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  • Inorganic Chemistry  (567)
  • 1995-1999  (567)
  • 1980-1984
  • 1955-1959
  • 1925-1929
  • 1995  (567)
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  • 1995-1999  (567)
  • 1980-1984
  • 1955-1959
  • 1925-1929
Year
  • 1
    Electronic Resource
    Electronic Resource
    Masthead (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995) 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951280101
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  • 2
    Electronic Resource
    Electronic Resource
    Tripodal Triamidostannates as Building Blocks in the Generation of Sn - M-Bonded Heterobimetallics (M = Fe, Ru) (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 29-34 
    Details
    ISSN: 0009-2940
    Keywords: Tripodal ligands ; Triamidostannates ; Metal-metal bonds ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: By in situ lithiation of the trifunctional amines H3CC(CH2NHSiMe3)3, PhC(CH2NHSiMe3)3, and HC{SiMe2NH(p-Tolyl)}3 and subsequent reaction with SnCl2 the corresponding triamidostannates were obtained. These were coupled with CpM(CO)2Cl (M = Fe, Ru) to yield the M - Sn-bonded heterobimetallics 9-14 of which H3CC(CH2NSiMe3)3SnFe(CO)2Cp (9) was characterized by a single-crystal X-ray structure analysis. Of the in situ-generated amidostannates only [HC{SiMe2N(p-Tolyl)}3Sn][Li(THF)3] (8) could be isolated as a uniform product and characterized analytically and spectroscopically.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951280105
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  • 3
    Electronic Resource
    Electronic Resource
    The Structures of [X2Y—N—YX2]+ Cations (X = F, Cl; Y = S, Se). A Comparison of X-ray and ab Initio Studies[1] (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 35-40 
    Details
    ISSN: 0009-2940
    Keywords: Selenium-nitrogen compounds ; Sulfur-nitrogen compounds ; Calculations, ab initio ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The structures of cationic species of the series [X2Y—N—YX2]+ (X = F, Cl; Y = S, Se) have been computed ab initio using all electron treatments for first-row elements and sulfur and quasi-relativistic pseudopotentials for Se and Cl. Splitvalence basis sets with polarization and diffuse functions were employed. The MP2 results for the (non-isostructural!) cations [Cl2Se—N—SeCl2]+ (1: Cs) and [F2S—N—SF2]+ (2: C2v) are in excellent agreement with the experimental (X-ray) observations. Both structures represent local minima. A deeper minimum for either of the cations is represented by another C2v isomer which for crystal lattice energy reasons is stable in the isolated state only. The geometries of the hitherto unknown species [Cl2S—N—SCl2]+ (3) and [F2Se—N—SeF2]+ (4) have been assessed by ab initio HF calculations. In analogy to 2, cations 3 and 4 are predicted to prefer C2v symmetry. Therefore, 1 exhibits unusual structural features. According to strictly localized natural bond orbital analysis (NBO), the central nitrogen atoms in 1 and 2 possess two lone pairs of electrons (LP: one sp hybrid and one p orbital). The relatively short Se—N and S—N bond distances in 1 (1.741-1.760 Å) and 2 (1.551 Å) can best be attributed to LP(N)→s̰*(Y—X) negative hyperconjugation (1: Y = Se, X = Cl; 2: Y = S, X = F).
    Additional Material: 8 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951280106
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  • 4
    Electronic Resource
    Electronic Resource
    Die fördernde Rolle von Phosphinoester-Liganden bei der Synthese neutraler Carben-, Vinyliden- und Allenyliden-Ruthenium(II)-KomplexeHerrn Professor Hubert Schmidbaur zum 60. Geburtstag gewidmet. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 49-62 
    Details
    ISSN: 0009-2940
    Keywords: Ruthenium(II) complexes, octahedral ; Phosphino esters as mono- and bidentate ligands ; Fluxional behaviour ; Carbene complexes ; Vinylidene complexes ; Allenylidene complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Vinylidene Transition-Metal Complexes, XXXV[1].  -  The Supporting Role of Phosphino Ester Ligands for the Synthesis of Neutral Carbene, Vinylidene and Allenylidene Ruthenium(II) ComplexesThe reaction of [RuCl2(PPh3)3] (1) with the phosphino esters iPr2P(CH2)nCO2R (2-4) leads to complete (n = 1; R = CH3, C2H5) or partial (n = 2; R =CH3) displacement of the PPh3 ligands and formation of the octahedral ruthenium(II) complexes [RuCl2{k2(P,O)-iPr2PCH2CO2R}2] (5, 6) and [RuCl2(PPh3){k(P)-iPr2PCH2CH2CO2Me}{k2(P,O)-iPr2PCH2CH2CO2Me}] (7). Treatment of 5 with LiBr and LiI affords the dibromo- and diiodoruthenium derivatives 8 and 9. While compound 5 reacts with CO and SO2 by cleavage of one Ru - O bond to yield the 1:1 adducts [RuCl2(L){k(P)-iPr2PCH2CO2Me}{k2(P,O)-iPr2PCH2CO2Me}] (10, 11), the reaction of the dibromo derivative 8 with CO in solution gives the dicarbonyl complex [RuBr2(CO)2{k(P)-iPr2PCH2CO2Me}2](13). If CO is passed over 8 in the solid state, the corresponding monocarbonyl compound 14 is formed. The hydridoruthenium(II) complex 16, which is obtained from equimolar amounts of [RuHCl(CO)(PiPr3)2] (15) and 2, reacts with HC≡CMe by insertion to give the vinyl derivative [RuCl{E - CH=CHMe}(CO)(PiPr3){k2(P,O)-iPr2CH2CO2Me}] (17). Treatment of 5 with HC̊' (R' = H, Me, tBu, Ph) and of 6, 8, 9 with HC≡CPh affords upon photochemical activation the octahedral vinylidene complexes [RuX2-(=C=CHR){k(P)-iPr2PCH2CO2R}{k2(P,O)-iPr2PCH2CO2R}] (18-21 and 23-25) in good to excellent yield. At room temperature, these compounds (with the exception of 25) are highly fluxional in solution. From 31P-NMR measurements, the free energies of activation ΔG
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951280108
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  • 5
    Electronic Resource
    Electronic Resource
    Reaktionen von R2Al—AlR2 (R = CH(SiMe3)2) mit Trimethylsilylazid  -  Insertion in die Al—Al-Bindung und Abbau zum trimeren Dialkylaluminiumazid (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 81-85 
    Details
    ISSN: 0009-2940
    Keywords: Aluminium-aluminium bond ; Insertion of trimethylsilyl azide ; Trimeric dialkylaluminium azide ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Reactions of R2Al—AlR2 (R = CH(SiMe3)2) with Trimethylsilyl Azide  -  Insertion into the Al—Al Bond and Formation of a Trimeric Dialkylaluminium AzideTetrakis[bis(trimethylsilyl)methyl]dialuminium(4) (1) reacts with trimethylsilyl azide under insertion of one nitrogen atom into the Al—Al bond. As shown by NMR spectra and crystal structure the product contains three and four coordinated Al atoms due to the coordination of the α-nitrogen atom of the azide group to one of the Al atoms. An electronically delocalized N3-system is formed with a N—N bond length of 132.0 pm and a bond order of 1.5 for both N—N bonds. With an excess of trimethylsilyl azide further reaction is observed only under mild irradiation conditions with an exchange of the azide group between Si and Al and formation of Me6Si2 and the dialkylaluminium azide 3, which is better synthesized by the reaction of Me3Si—N3 with Cl—Al[CH(SiMe3)2]2. The sterically highly shielded aluminium azide 3 is a trimer in the solid state showing a non-planar 12-membered Al3N9 heterocycle with short N—N bonds (114 pm).
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951280112
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  • 6
    Electronic Resource
    Electronic Resource
    Selective Activation of Aromatic C - H Bonds with Lithium Atoms at 77 K (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 91-92 
    Details
    ISSN: 0009-2940
    Keywords: C - H bond activation ; Lithum atoms ; Cocondensation ; Aryllithium ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: In the presence of donor bases like THF lithium atoms are able to activate benzene derivatives under cryogenic reaction conditions. Only ring-metalated products and solid lithium hydride are formed selectively. The thermodynamically favored product benzyllithium or biphenyl generated by dimerization of free phenyl radicals are not found. This is one of the very few examples of metal atoms undergoing a C - H activation without further photoexcitation.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19951280114
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  • 7
    Electronic Resource
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    Protolysis of Tri-tert-butylazadiboriridine: Formation of a B-H-B Bridge in Unusual Coordination (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 99-103 
    Details
    ISSN: 0009-2940
    Keywords: Tri-tert-butylazadiboriridine ; (Hydroboryl)(methoxyboryl)amine ; 2,3-μ-Hydro-1,2,3-azoniadiborata-l-cyclopropenes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The B—B bond of tri-tert-butylazadiboriridine [—NR—BR—BR—] (R = tBu; 1) is oxidized by MeOH to give the (hydroboryl)(methoxyboryl)amine H—BR=NR-BR(OMe) (2a). μ-2,3-Hydroazoniadiborata-1-cyclopropenes [=NR—BR(X)—μH—BR=] (3a, 3c-e) are formed by the action of the acids HX upon 1. A similar hydrogen bridge as in 3a-e is formed during the hydroboration of 1 by catecholborane, yielding 3f. A B atom is identified in the products 3a-f to be planarly coordinated by four atoms, two of which are forming a BHB three-center bond with that B atom. This is a novel bonding situation in boron chemistry. The structures of the products are deduced from 1H-, 11B-, and 13C-NMR spectra and are confirmed by X-ray structural analyses of 2a, 3a, and 3c.
    Additional Material: 2 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951280203
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  • 8
    Electronic Resource
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    Synthese und Struktur zweikerniger Kupfer(II)-Komplexe eines neuen Hexaaza-Makrocyclus mit verbrückenden Oxalat- und Acetat-Ionen (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 115-119 
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    ISSN: 0009-2940
    Keywords: Polyazamacrocycles ; Dinucleating ligands ; Copper complexes ; Oxalate complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Synthesis and Structure of Dinuclear Copper(II) Complexes of a Novel Hexaaza Macrocycle Containing Bridging Oxalate and Acetate IonsNon-template Schiff base [2 + 2] condensation of pyridine-2,6-dicarbaldehyde with 1,4-diamino-2-butyne yields the hexaazamacrocyclic ligand 1, which is converted to 2 by NaBH4 reduction of the imino groups. Two dinuclear copper(II) complexes of 2 containing oxalate and acetate ions, [(2)Cu2(μ-C2O4)](BPh4)2 (3) and [(2)Cu2(μ-CH3CO2)(OH2)](PF6)2.25-(NO3)0.75 (4), were characterized by X-ray crystallography. The oxalate ligand in 3 forms a (μ-η4:η4) bridge between the copper atoms. Compound 4 contains a syn-anti-bridging acetate ion. The Cu-Cu distances are 5.315 Å in 3 and 4.746 Å in 4, respectively. Oxalate can be separated from other carboxylates in aqueous solution by selective binding to the [(2)Cu2] unit and precipitation of 3.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951280205
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  • 9
    Electronic Resource
    Electronic Resource
    Synthesis, X-Ray Crystal Structure and Magnetic Characterization of the First “Ni3S4N3” Nickel Thiolate Cluster (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 125-129 
    Details
    ISSN: 0009-2940
    Keywords: Nickel cluster ; Nickel thiolate ; Hydrogenase ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The tridentate N,O,S-ligand (RS)-2-[(2-mercapto-1-methylamino)ethyl]phenol (rac-1) was prepared from ortho-hydroxy-chloroacetophenone in three steps. When this ligand was treated with nickel(II) acetate, the novel “Ni3S4N3” cluster rac-3 was obtained. The X-ray crystal structure of rac-3 unambiguously revealed the pseudo-C3 symmetric structure of this novel nickel cluster, which is made up by three nickel ions, one sulfide sulfur atom, and three homochiral ligand molecules, each contributing one thiolate sulfur atom and one amine nitrogen atom to the ligation of the metal ions. According to NMR-spectroscopic results, this highly symmetric structure is maintained in solution. The magnetic studies revealed diamagnetic behavior in the solid state, although antiferromagnetic interaction of the metal centers cannot absolutely be excluded.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951280207
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  • 10
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    Stereospecific Ligand Substitutions in Manganese(I) Complexes (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 151-155 
    Details
    ISSN: 0009-2940
    Keywords: Tripodal ligands ; Phosphane ligands ; Thioethers ; Manganese complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Treatment of fac-[(P2SPh-P,P')Mn(CO)3Br] and fac-[(PS2Ph-P,S)Mn(CO)3Br] [P2SPh: Z = PPh2; PS2Ph: Z = SPh in CH3C-(CH2PPh2)(CH2SPh)(CH2Z)] with silver hexafluorophosphate yields the η3-tripodal manganese complexes [(P2SPh-P,P',S)Mn(CO)3]PF6 (7) and [(PS2Ph-P,S,S')Mn(CO)3]PF6 (9), respectively, whereas the reaction of CH3C(CH2PPh2)2-(CH2SH) with Mn(CO)5Br gives directly [CH3C(Ph2-PCH2)2(CH2S)-P,P',S]Mn(CO)3 (11). Both ionic complexes 7 and 9 undergo stereospecifically ligand substitution upon treatment with Br-, I-, N-3, SCN- and CN- to give syn-fac-[(P2SPh-P,P')Mn(CO)3X] and syn-fac-[(PS2Ph-P,S)Mn(CO)3X] (X = Br, I, SCN, N3, CN) respectively, but the neutral complex 11 fails to undergo such a substitution reaction with these ions. However, reaction of I- with the complex [(PSMe)-P,P',S]Mn(CO)3]BF4 (20) [P2SMe = CH3C(CH2-PPh2)2(CH2SCH3)), which is obtained from the S-alkylation of 11 with (CH3)3OBF4, affords syn-fac-[(P2SMe)-P,P']Mn(CO)3I (22s) exclusively. The possible reaction mechanism of this ligand substitution is discussed.
    Additional Material: 1 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951280211
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  • 11
    Electronic Resource
    Electronic Resource
    Oxacycloalkenyliden-Komplexe von Chrom, Molybdän und Wolfram: Synthese, Anellierung mit Alkinen und Diels-Alder-Reaktionen mit Dienen (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 157-161 
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    ISSN: 0009-2940
    Keywords: Carbene ligands ; Chromium complexes ; Molybdenum complexes ; Tungsten complexes ; Annulation reaction ; Diels-Alder reaction ; Oxacyclopentenylidene ligands ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Reactions of Complex Ligands, LXI[1]. - Oxacycloalkenylidene Complexes of Chromium, Molybdenum, and Tungsten: Synthesis, Their Annulation with Alkynes and Diels-Alder Reaction with DienesLithiiated propargylic ether 1 reacts with M(CO)6 (M = Cr, Mo, W) to give the 2-oxacyclic carbene complexes 2-4 containing an α,β-double bond and a cyclic acetal structure which serves as a protected benzoyl group. Reaction of the chromium complex 2 with tolan leads to an acyl hydroquinone derivative 5. The tungsten complex 3 undergoes a [4 + 2] cycloaddition with cyclopentadiene to give two diastereomeric oxatricyclic carbene complexes 6 and 7 with an endo/exo selectivity of 3:1. The stereochemistry of the Diels-Alder reaction is controlled by the configuration of the acetal carbon center.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951280212
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  • 12
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    Electronic Resource
    Darstellung und Komplexierung von 1,4-Dimethyl-2,3-bis(isopropyliden)-1,4-diboratetralinHerrn Professor Nils Wiberg zum 60. Geburtstag gewidmet. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 183-185 
    Details
    ISSN: 0009-2940
    Keywords: 1,4-Diboranaphthalines ; 2,7-Diboradodeca-1,3,9,11-tetraenes ; Cobalt complexes ; Rhodium complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Synthesis and Complexation of 1,4-Dimethyl-2,3-bis(isopropylidene)-1,4-diboratetraline1,4-Dimethyl-2,3-bis(isopropylidene)-1,4-diboratetraline (2) is obtained from o-dilithiumbenzene and 2,5-dimethyl-3,4-bis(chloromethylboryl)-2,4-hexadiene in 61% yield. Its complexation with cyclopentadienylbis(ethene)cobalt leads to the triple-decker bis(η5-cyclopentadienylcobalt)-μ-η6,η6-1,4-dimethyl-2-isopropenyl-3-isopropyl-1,4-dihydro-1,4-dibora-naphthaline (3) in low yield. However, the reaction of 2 with (C5H5)Rh(C2H4)2 and (C5Me5)Co(C2H4)2 originates complexes of a tricyclic ligand formed from 2 via conrotatoric [2 + 2] cycloaddition of the isopropylidene groups. (η5-Cyclo-pentadienylrhodium)-η6-tricyclo-[6.4.0.03,6]-2,4,4,5,5,7-hexamethyl-2,7-diboradodeca-1,3,9,11-tetraene (4), (η5-pentamethylcyclopentadienylcobalt)-η6-tricyclo-[6.4.0.03,6]-2,4,4,5,5,7-hexamethyl-2,7-diboradodeca-1,3,9,11-tetraene (5) and its related dinuclear complex 6 could be isolated in 29, 10, and 31%, respectively. Their constitutions are derived from spectroscopic data and proven by X-ray structure analysis of 4.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19951280216
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  • 13
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    Zerfall von Nitrosylazid, N4O: Existieren auch cyclische Stickstoff-Oxide? (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 201-203 
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    ISSN: 0009-2940
    Keywords: Nitrogen oxides ; Calculations, ab initio ; Tetranitrogen monoxide ; Dinitrogen monoxide ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Decomposition of Nitrosyl Azide, N4O: Are Cyclic Nitrogen Oxides Existent?The unimolecular decomposition of nitrosyl azide (tetranitrogen monoxide), N4O, was studied at the electron-correlated, spin-restricted RMP2 level with the 6-31G(d,p) and 6-31+G* basis sets. Frequency calculations were performed at 6-31+G* on the optimized structures. It is demonstrated that the experimentally established trans-trans-N4O (Cs) may either interconvert into cis-cis-N4O which upon decomposition forms cyclic N4O (C2v) as an intermediate species to finally give N2O (C∞v) and N2, or trans-trans-N4O may directly dissociate into cyclic N2O (C2v) and N2. All structures determined were rationalized by energy hypersurface calculations.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19951280220
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  • 14
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    Synthesis and Characterization of Mononuclear Titanium Complexes Containing a Bis(phenoxy) Ligand Derived from 2,2′-Methylene-bis(6-tert-butyl-4-methylphenol) (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 221-227 
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    ISSN: 0009-2940
    Keywords: Titanium complexes ; Bidentate phenoxy ligands ; Bulky phenols ; Lewis acidity ; Pentacoordination ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A series of new titanium complexes of the general type Ti(mbmp)X2 (X = Br, I; OMe, OiPr, OtBu), containing a bidentate bis(phenoxy) ligand derived from 2,2′-methylenebis(6-tert-butyl-4-methylphenol) (mbmpH2), was prepared. The 1H-chemical shifts for the protons of the methylene link were found to vary considerably as a function of the ligand X. Reaction of Ti(OiPr)4 with two equivalents of mbmpH2 gave the C2-symmetric spiro-titanate complex Ti(mbmp)2. The crystalline labile solvent adducts of the dichloro complex Ti(mbmp)Cl2 with THF and DME were isolated and characterized. A single-crystal X-ray structural analysis revealed the THF adduct to be a mono(THF) adduct with a trigonal-bipyramidal configuration, the bidentate mbmp ligand spanning an apical and equatorial site and the THF ligand occupying the remaining apical position.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19951280304
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  • 15
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    Darstellung und Charakterisierung der Tetrahedrane [CpM(CO)2]3P (M = Mo, W) sowie der Derivate [CpMo(CO)2]3P-Mo(CO)5 und [CpW(CO)2]3P-W(CO)5 (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 197-199 
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    ISSN: 0009-2940
    Keywords: μ3-Phosphorus-trimolybdenum tetrahedrane ; μ3-Phosphorus-tritungsten tetrahedrane ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Synthesis and Characterization of the Tetrahedranes [CpM(CO)2]3P (M = Mo, W) and Their Derivatives [CpMo(CO)2]3P-Mo(CO)5 and [CpW(CO)2]3P-W(CO)5The reaction of Na[CpM(CO)3] (M = Mo, W) with PCl3 in diglyme yields the cluster compounds [CpMo(CO)2]3P-Mo(CO)5 (2a) and [CpW(CO)2]3P-W(CO)5 (2b) in good yields as well as the tetrahedranes [CpMo(CO)2]3P (3a) and [CpW(CO)2]3P (3b) as side products. Compounds 3a, b are obtained independently by the reaction of 2a, b with PPh3. The clusters 2a, b and 3a, b were characterized spectroscopically (IR, NMR, MS), and X-ray structure determinations were carried out on 2a, b.
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    URL: http://dx.doi.org/10.1002/cber.19951280219
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  • 16
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    Photocatalytic Oxygenation of Selected Cycloalkenes in Aqueous Solutions Induced by Water-Soluble Metal Porphyrin Complexes (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 229-234 
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    ISSN: 0009-2940
    Keywords: Photooxygenation ; Dioxygen activation ; Metalloporphyrins ; Epoxidation ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Water-soluble manganese(III) as well as iron(III) porphyrinates are introduced as light-sensitive precursor compounds for the photocatalytic activation of dioxygen in aqueous solutions. It is shown that in the presence of α-pinene (4) and the further cycloalkenes 11-13 photocatalytic oxygenation reactions occur. The dependence of the selectivity of the oxygen transfer to the olefin on both the presence of water and the variation of the substrate-to-catalyst ratio is discussed. The catalyst may be conveniently separated from the substrates/products by using aqueous solvent systems.
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    URL: http://dx.doi.org/10.1002/cber.19951280305
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    Carbohydratocarbene Complexes of Manganese and RheniumDedicated to Prof. Hans H. Brintzinger on the occasion of his 60th birthday. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 373-378 
    Details
    ISSN: 0009-2940
    Keywords: Carbene complexes ; Carbyne complexes ; Carbohydrates ; Diastereoselective addition ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The cationic carbyne complexes [Cp(CO)2M≡CR]+ [BX4]- [M = Mn, X = F: R = Ph (1), Tol (2); M = Re, X = 3,5-C6H2(CF3)2: R = Ph (3)] add the anion of monodeprotonated protected mannofuranose (4a), glucofuranose (4b), and fructopyranose (4c) to the carbyne carbon atom to form the carbohydratocarbene complexes 5a-c, 6a, b, and 7a. With 5b, 5c, and 6b the addition proceeds with retention of configuration at the anomeric center. Due to inversion of configuration in the deprotonation step the complexes 5a, 6a, and 7a are obtained as β-glycosides. The carbene ligand is oxidatively cleaved from the metal by trimethylamine N-oxide or air. Cleavage of the C(carbene)—O bond with reformation of the cation of the carbyne complex 2 is achieved by reaction of 6a with BCl3. Photolysis of [Cp(CO)2Mn=C(Ph)OEt] in the presence of L affords the carbene complexes [Cp(CO)(L)Mn=C(Ph)OEt] [L = P(OMe)3 (11), P(Tol)3 (12)]. Ethoxide abstraction from 11 and 12 by BF3 gives the chiral cationic carbyne complexes [Cp(CO)(L)Mn=CPh]+[EF4]- (13, 14) which add 4a to form the corresponding mannofura-nosylcarbene complexes (15, 16). When 0.5 equivalents of 4a are employed in the reaction with 13, 14 the ratio of diastereomers is 3:2, both for 15 and 16. Complex 11 was characterized by an X-ray structural analysis.
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    Metallorganische Verbindungen der Lanthanoide, 89. Cyclooctatetraenyl-Komplexe der frühen Übergangsmetalle und Lanthanoide, 6. (Cyclooctatetraenyl)[N,N′-bis(trimethylsilyl)benzamidinato]-und -[diphenylbis(trimethylsilylimido)phosphinato]-Komplexe der Seltenen Erden; Röntgenstrukturanalyse von (C8H8)Tm[PhC(NSiMe3)2](THF), (C8H8)Lu[4-MeOC6H4C(NSiMe3)2](THF) und (C8H8)Nd[Ph2P(NSiMe3)2](THF) (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 395-404 
    Details
    ISSN: 0009-2940
    Keywords: Lanthanides, organo-, complexes ; Cyclooctatetraenyl complexes ; Benzamidinate ligands ; Diimidophosphinate ligands ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Organometallic Compounds of the Lanthanoids, 89. - Cyclooctatetraenyl Complexes of the Early Transition Metals and Lanthanoids, 6. - (Cyclooctatetraenyl)[N,N′-bis(trimethylsilyl)benzamidinato]- and -[diphenylbis(trimethylsilylimido)-phosphinato] Complexes of the Rare Earths; X-Ray Structural Analyses of (C8H8)Tm[PhC(NSiMe3)2](THF), (C8H8)Lu[4-MeOC6H4C(NSiMe3)2](THF), and (C8H8)Nd[Ph2P(NSiMe3)2](THF)[(C8H8)Ln(μ-Cl)(THF)2]2 or [(C8H8)Ln(μ-O3SCF3)(THF)2]2 (Ln = Y, Ce, Pr, Nd, Sm, Tm, Lu) react with Na[4-RC6H4C(NSiMe3)2] (R = H, OMe, CF3) or Li[PhC(NSiMe3)2] to give the monomeric (cyclooctatetraenyl)lanthanide benzamidinates (C8H8)Ln[4-RC6H4C(NSiMe3)2](THF) [R = H, Ln = Y (1), Ce (4), Pr (6), Nd (8), Sm (10), Tm (12), Lu (15); R = OMe, Ln = Y (2), Ce (5), Pr (7), Nd (9), Sm (11), Tm (13), Lu (16); R = CF3, Ln = Y (3), Tm (14), Lu (17)]. The reaction of [(C8H8)Ln(μ-Cl)(THF)2]2 (Ln = Ce, Pr, Nd, Sm) with Li[Ph2P(NSiMe3)2] in THF leads directly to the monomeric compounds (C8H8)Ln[Ph2P(NSiMe3)2](THF) [Ln = Ce (18), Pr (19), Nd (20), Sm (21)] in good yields. The 1H-, 13C-, 31P- and 29Si-NMR and mass spectra of the new compounds as well as the molecular structures of 12, 16, and 20 are discussed. The Raman spectra of the complexes 1-3, 12, and 14-17 have been studied in detail.
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    Perfluororganochalkogensäuren in hohen Oxidationsstufen (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 423-428 
    Details
    ISSN: 0009-2940
    Keywords: Perfluoroethylselenoic acid, -salts, -esters ; Bis(pentafluorophenyl)tellurium(IV) acid, mixed anhydrides, -tellurium(VI) oxide, -tetrakis(trifluoromethylsulfonate), -dihydroxybis(trifluoromethylsulfonate) ; Pentafluorophenyltellurium(IV) oxoacid ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Perfluoroorganochalcogenic Acids in Higher Oxidation StatesPentafluoroethylseleninic acid is oxidized by KMnO4 in slightly alkaline aqueous solution to give K[C2F5SeO3]. With HClO4 the salt is converted into the free acid. Neutralisation of C2F5SeO3H with NaOH, Ag2O, NH3 + H2O provides the corresponding salts. The ethyl ester is made from Ag[C2F5SeO3] and C2H5I. Oxidation of C6F5TeC6F5 with concd. HNO3 yields C6F5Te(OH)ONO2 which on controlled hydrolyses gives (C6F5)2Te(OH)2. Strong acids like HClO4 or H2SO4 form mixed anhydrides like (C6F5)2Te(OH)ClO4 or (C6F5)2Te(OH)OS(O)2OTe(OH)(C6F5)2. For the latter compound a cyclic or noncyclic polycondensate form cannot be ruled out. Acidic 35% H2O2 solution oxidizes (C6F5)2Te(OH)2 at 40°C (48 h) to give (C6F5)2TeO2. This anhydride dissolves only in CF3SO3H forming (C6F5)2Te(OSO2CF3)4. It is soluble in CH3CN and reacts in solution with water to yield (C6F5)2Te(OH)2(OSO2CF3)2. Oxidation of C6F5TeTeC6F5 with concd. HNO3 provides oligomeric [C6F5Te(O)OH]x which still contains some HNO3. A single-crystal X-ray structure determination carried out on [(C6H5)4As][C2F5SeO3] shows convincingly that the central selenium atom is coordinated by three equivalent oxygen atoms with d(Se-O) = 1.614(3) Å, proving that Se has the oxidation state VI.
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    Molecular Modeling, a Tool for Predicting Structural Effects on the Macrocyclization Reaction between Bis(vinyl or allyl) Dialdehydes and Thiophosphonic Bis(hydrazides) (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 443-447 
    Details
    ISSN: 0009-2940
    Keywords: Phosphorus macrocycles ; Molecular modeling ; Cyclocondensation ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reaction of new phosphorus dialdehydes PhP(O)-[(CH2)nCH=CHC6H4CHO]2 (4a-c, 5a) (n = 0:4, n = 1:5; a:para, b:meta, c:ortho), with thiophosphonic bis(hydrazide) PhP(S)[NMeNH2]2 (6) yields macrocyclic compounds 9b′, c′, 10a′, 9a″, b″, c″, 10a″ and 9c′″, arising from the cyclocondensation of one, two, or three equivalents of each reagent, respectively. Molecular modeling of 4a-c, 5a, 6 and of the intermediate monocondensation products 7a-c, 8a was carried out and points out the importance of the geometry of the starting reagents in the competition between inter- and intramolecular cyclocodensation.
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    Synthesis, Structures and Properties of CF3S-Substituted Tellurium Compounds (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 477-480 
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    ISSN: 0009-2940
    Keywords: Tellurium, bis(sulfinylamido)-, bis(trifluoromethylthio)- ; Thiachalcogenadiazole ; Ditelluradiazetidine ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: New preparations for the following compounds are described: Te(SCF3)2, Te(NSO)2, and Cl2Te(NSO)2. The catalytic or thermal SO2 elimination from Cl2Te(NSO)2 affords a coordinated or non-coordinated thiachalcogenadiazole. Conversions of these compounds are reported. Evidence for the proposed mechanism for the reaction between Te(NSO)2 and SbCl5 is provided. Cl4Te2N2(SCF3)2, prepared from TeCl4 and CF3SN(SiMe3)2, reacts with LiN(SiMe3)2 to form [(Me3Si)2N]4Te2N2(SCF3)2. An X-ray structural analysis of Cl4Te2N2(SCF3)2 is presented.
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    Syntheses and Structures of Intramolecularly Stabilized Organoaluminium CompoundsDedicated to Professor Peter Paetzold on the occasion of his 60th birthday. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 493-497 
    Details
    ISSN: 0009-2940
    Keywords: Organoaluminium compounds ; Alanes, 2-[(dimethylamino)methyl]phenyl- ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reaction of LiAr (Ar = 2-[(dimethylamino)methyl]phenyl) with AlCl3, MeAlCl2, and Me2AlCl in a 1:1 ratio yields the corresponding organoaluminium compounds ArAlCl2, ArAl(Cl)Me, and ArAlMe2 (1-3). The alanes Ar2AlCl and Ar2AlMe (4 and 5) were synthesized from AlCl3 and MeAlCl2 with two equivalents of LiAr. The products ArAl(Cl)R [R = tBu, C(SiMe3)3] 6 and 7 are formed by the reaction of LiR with 1. The Lewis acid 1 adds the bases iPrNH2 and THF to yield the adducts 1 · iPrNH2 and 1 · THF. The structures of the products were deduced from the 1H-, 13C-, and 27Al-NMR spectra and were confirmed by X-ray structural determinations of 5 and 1 · iPrNH2.
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    Metallkomplexe unsymmetrisch überbrückter [N4]-Makrocyclen: Synthese, Struktur und Redoxverhalten (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 503-514 
    Details
    ISSN: 0009-2940
    Keywords: Cu, Ni, Co, Fe complexes ; Template synthesis ; Tetraaza macrocycles ; X-ray structure, H bridges, ID-coordination polymers ; Electrochemistry ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Metal Complexes of Unsymmetrically Bridged [N4] Macrocycles: Synthesis, Structure and Redox BehaviourMetal complexes M-5a (M = Cu, Ni, Co, Fe, and I-Fe11) of 6,13-Di(ethoxycarbonyl)-7,12-dimethyl-benzo[b]-1,4,8,11-tetraaza-cyclotetradeca-2,5,7,11,13-pentaene and the free ligand H2-5a have been synthesized. The crystals of Cu-5a · H2O and Ni-5a · H2O consist of planar complex molecules which are linked by H bridges between the water molecules and the peripheric ester groups to give 1D chains. The average M-N distances are equal for both complexes (Cu 1.928, Ni 1.924 Å), being unexpectedly large for the nickel complex. The redox properties of all the new compounds as well as some acetyl derivatives M-5b have been examined by cyclic voltammetry and compared with those of the previously reported symmetrically phenylene (M-4) and ethylene (M-6) bridged derivatives. All complexes give a reversible single electron reduction which clearly shows the increasing electron density around the central atom in the order M-4 〈 M-5 〈 M-6. Like the carbonyl substituted tetraazaannulenes M-4 the copper complexes Cu-5 give two, the cobalt complexes Co-5 three, and the iron complex Fe-5a probably four reversible single electron oxidations. They can be attributed to the species [MIIIL-II]+, [MIILo]2+, [MIIILo]3+, and [FeIVLo]4+ with Lo being a “non innocent” neutral 1,2-quinodiimine ligand. Very surprisingly, since in contrast to Ni-4 and Ni-6, the nickel complexes Ni-5 gave no reversible oxidation.
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    Zinc Complexes of Histidine-Containing Di- and Tripeptides (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 541-550 
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    ISSN: 0009-2940
    Keywords: Histidine peptides ; Zinc complexes ; Composition ; Solid-state structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Nine dipeptides and one tripeptide containing histidine were converted into analytically pure zinc complexes. Four different compositions were observed. The peptides used as or converted into the monoacids LH (HisGly, GlyHis, HisPhe, HisHis) form the compounds ZnL2 (11a, 12-14) and alternatively (HisGly, HisGlyGly) the compounds ZnL(BF4) (11b, 20). The peptides used as amides (HisGlyNH2, HisMetNH2) act as neutral ligands in the compounds ZnL2(ClO4)2 (15, 16). The three remaining peptides (HisAsp, AlaHis, β-AlaHis) behave like diprotonic acids LH2 forming the compounds ZnL (17-19). Spectra and solubilities indicate that complexes 11a, 13, 15, and 16 are mononuclear containing two chelating peptides bound by their amino and imidazole nitrogen atoms. All other complexes seem to be coordination polymers in some of which the amide N and O atoms are involved in the coordination. This was proven by a structure determination for Zn(GlyHis)2 (12) in which the zinc ions are coordinated octahedrally by two histidine N, two amino N, and two amide O atoms of four peptide residues.
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    1,4,2-Diazaphospholothiazoles and -pyridines by a Hantzsch-Type Condensation Using Chloromethyldichlorophosphane (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 581-587 
    Details
    ISSN: 0009-2940
    Keywords: Anellated azaphospholes ; Hantzsch-type [3 + 2] cyclocondensation ; Chloromethyldichlorophosphane ; Regioselectivity ; 31P-, 1H-, 13C-NMR spectra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The [3 + 2] cyclocondensation of 2-amino-1,3-thiazoline, 2-aminopyridines, 2- and 4-aminopyrimidines, 2-aminopyrazine, and 2-aminoquinoline with chloromethyldichlorophosphane in the presence of triethylamine yields regiospecifically 5,6-dihydrothiazolo[2,3-e][1,4,2]diazaphosphole (3), 1,4,2-diazaphospholo[4,5-α]pyridines (12), 1,4,2-diazaphospholo[4,5-α]pyrimidines (15), 1,4,2-diazaphospholo[4,5-e]pyrimidine (17), 1,4,2-diazaphospholo[4,5-α]pyrazine (19), and [1,4,2]diazaphospholo[4,5-α]quinoline (22), respectively. Using 2-amino-1,3-thiazole (4) and 2-aminobenzothiazoles 8, we obtained mixtures of the 1,5- and 4,5-anellated 1,4,2-diazaphospholes 5/6, 9a/10a and 9b/10b, while in the case of the methyl derivative 8c only the [1,4,2]diazaphospholo[5,4-b][1,3]benzothiazole 10c was formed. In the reaction of 2-aminothiazole and 2-aminopyrazine with Chloromethyldichlorophosphane the bis(diazaphospholo)-substituted chloromethylphosphanes 7 and 20 could be detected. The new anellated 1,4,2-diazaphospholes are colorless to pale yellow crystalline moisture-sensitive solids.
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    Reactions at Silicon-Silicon Bonds, V. Selective Trichlorosilylation of Alkyl(diorganylamino)chlorophosphanes with Hexachlorodisilane or with Trichlorosilane/Triethylamine. - Two Routes to New Functional Trichlorosilylphosphanes (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 615-619 
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    ISSN: 0009-2940
    Keywords: Reductive silylation ; Aminochlorophosphanes ; Silylphosphanes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reaction of alkyl(diorganylamino)chlorophosphanes R(R2′N)PCl 1 (1a: R = tBu, R′ = Et, 1b: R = iPr, R′ = iPr; 1c: R = iPr, R′ = Ph) with hexachlorodisilane, afforded alkyl(diorganylamino)trichlorosilylphosphanes R(R2′N)PSiCl3 2 (2a: R = tBu, R′ = Et; 2b: R = iPr, R′ = iPr; 2c: R = iPr, R′ = Ph) and silicon tetrachloride. An intermediate formed in the reaction of 1b with hexachlorodisilane, the adduct iPr(iPr2N)(Cl)P-Si(Cl)3-SiCl3 (3b = 1b · Si2Cl6), was detected by 31P- and 29Si-NMR spectra that indicate pentacoordinated silicon bound to tetracoordinated phosphorus and tetracoordinated silicon. Trichlorosilylphosphanes 2 are also available from 1 under very mild conditions by reductive trichlorosilylation with trichlorosilane in the presence of triethylamine. Compounds 2 were identified analytically, by mass spectroscopy, multinuclear NMR, and an X-ray structure determination of 2c.
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    Reactions of Complex Ligands, LXIVPart LXIII: Ref.. Synthesis of 5,5′-Diphenyl-2,2′-bifuran, a Biaryl Compound with Remarkable Fluorescence Properties (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 641-643 
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    ISSN: 0009-2940
    Keywords: Carbene ligands ; Tungsten complexes ; 2,2′-Bifuran ; Copper coupling reaction ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The 2-oxacyclic α,β-unsaturated carbene complex 1 reacts with an excess of dimethylamine to give the diphenylbifuran 2. The structure of 2 was established by independent synthesis from 2-phenylfuran (4) via regioselective lithiation and transmetalation to zinc and tin organometallics 6a-c and final oxidative copper coupling reactions.
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    Ligandgesteuerte P2-Verknüpfung zu einem acyclischen P4-LigandenHerrn Prof. Peter Puetzold zum 60. Geburtstag gewidmet. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 635-639 
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    ISSN: 0009-2940
    Keywords: P2 and P4 ligands ; Ligand-induced P2 coupling ; Cobalt complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Ligand-Induced P2 Coupling to an Acyclic P4 LigandThe further terminal coordination of M(CO)5 (M = Cr, Mo W) to [(Cp‴Co)2(μ-η2:2-P2)2] (1), Cp‴ = 1,2,4-tBu3C5H2, affords the polynuclear cobalt complexes [(Cp‴Co)2(μ3(4)-η4:4:1:(1)-P4){M(CO)5}n], n = 1; M = Cr (2a), Mo (2b), W (2c) and n = 2, M = W (3). The X-ray crystal structure analyses as well as low-temperature 31P-NMR studies show that in 1 the two P2 ligands are rectangularly oriented while in 2b, 2c, and 3 they are coupled to an acyclic, trapezoidally arranged P4 chain.
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    Formation and Structure of a New Dinuclear Rhodium Complex [(iPr3P)RhCl]2[P3C3tBu3] (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 737-739 
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    ISSN: 0009-2940
    Keywords: Rhodium complex, dinuclear ; Phosphaalkyne ; Trimerization ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The new dinuclear rhodium complex 4 was synthesized by reaction of [(iPr3P)2RhCl]2 (1) or [(iPr3P)2(CH2=CH2)RhCl] (2) with 2-tert-butyl-1-phosphaacetylene (3) in 58% yield. An X-ray analysis reveals that in 4 a 1,3,6-triphosphahexadiene-1,6-diyl chain is bound to each of the two rhodium atoms in an η1,η3 manner.
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    Synthesis of Structures of (Acyloxy)boranesDedicated to Prof. Dr. A. Schmidpeter on the occasion of his 65th birthday.Synthesis of Structures of (Acyloxy)boranes (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 751-762 
    Details
    ISSN: 0009-2940
    Keywords: Trifluoroacyloxy-9-borabicyclo[3.3.1]nonane ; Pivaloyloxy-9-borabicyclo[3.3.1]nonane dimer ; Bis(9-borabicyclo[3.3.1]nonyl]oxalate ; Tetrakis(9-borabicyclo[3.3.1]nonyl)-dihydroxyoxalate ; Bis(9-borabicyclo[3.3.1]nonyl)-2,2-dimethylmalonate tetramer ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 9-Borabicyclo[3.3.1]nonane (9-BBNH) reacts with monocarboxylic acids to afford 9-(acyloxy)-9-borabicyclo[3.3.1]nonanes which are dimers in the solid state as shown by X-ray crystal structures of the benzoate and pivalate. More complex reactions were observed by allowing 9-BBNH to react with dicarboxylic acids in THF or monoglyme. Thus, (9-BBN)2 oxalate 3 contains a fully delocalized oxalate unit with equal C-O and B-O bond lengths. Traces of water convert it into the tetrakis(9-BBN) oxalate 5. A rather unusual structure is veryfied by 9-BBN 2,2-dimethylmalonate 7 which according to its molecular structure is a tetramer featuring a 32-membered ring system. In contrast, reactions of oxalic acid with thexylborane leads to reduction of the acid and formation of a bicyclic dioxaborolo-dioxaborolane 10. Several intermediates were detected by 11B-NMR spectroscopy as well as in reactions of BH3 · THF or BH3 · SMe2 with oxalic acid.  -  It follows from the present study that (acyloxy)boranes derived from dicarboxylic acids are strong Lewis acids with an unexpected variety of structural features.
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    β-Alkoxy- and β-Hydroxyalkylphosphanes as Ligands in the Stereoselective Hydrogenation  -  A Comparison (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 767-773 
    Details
    ISSN: 0009-2940
    Keywords: Ether phosphanes ; Hydroxyalkylphosphanes ; Rhodium ; Asymmetric hydrogenation ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Optically pure 1,4-bis(diphenylphosphanyl)-2-hydroxy-butane (2) and its methyl ether 1 can be conveniently prepared by starting from chiral pool substances such as malic or L-ascorbic acid. Different pathways to these compounds were elucidated. In one case an interesting migration of an acetalic OH-protective group was observed. The reaction of the bisphosphanes with Rh1 or PdII gave uniform metal complexes. On the basis of X-ray structural analysis, NMR and IR data it was concluded that in the investigated precatalysts of the type [Rh(COD)(bisphosphane)]BF4 a coordination of the alkoxy or hydroxy oxygen to the metal does not take place. Nevertheless, significant differences in enantioselectivity and activity could be observed when several prochiral substrates were hydrogenated.
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    Substituted Variants of the Cluster Type Fe3(CO)9(μ3-η2-RC≡N) (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 793-797 
    Details
    ISSN: 0009-2940
    Keywords: Triiron clusters ; Capping nitrile ligands ; Phosphine substitutions ; Structure determination ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Various aromatic nitriles were used for the preparation of the nitrile-capped clusters Fe3(CO)9(μ3-η2-RC≡N) (2) by reaction with Fe3(CO)12 under hydrogen. Electron-rich nitriles decrease, electron-poor nitriles increase the thermal stability of clusters 2. With CN-substituted pyridines only traces of clusters 2 could be obtained. CO replacement in Fe3(CO)9(PhCN) (2a) by isonitriles also causes a lowering of the stability. Conversely, more stable products were obtained by substitution reaction with trimethyl phosphite. One PPh3 and two dppm derivatives were also obtained. The structure of Fe3(CO)8-P(OMe)3(μ3-η2-PhC=N) (5a) was determined.
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    Zinc Complexes of Drugs Containing Nitrogen Heterocycles (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 779-785 
    Details
    ISSN: 0009-2940
    Keywords: Zinc complexes ; Drug ligands ; Captopril ; Isoniazid ; Nalidixic acid ; Mercaptopurine ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Four drugs whose actions have a relation to the status of zinccontaining species in the human body were used as ligands in zinc complexes. Captopril (H2Cap) forms the compound [ZnCap] (1) presumed to be a coordination polymer with O and S coordination. Isoniazid, in the presence of zinc salts, is converted to 1,2-diisonicotinoyl hydrazide (H2Nih) which forms polymeric [Zn(Nih)NH3] (2) with trigonal-bipyramidal ZnO2N3 coordination. Nalidixic acid (HNal) and zinc perchlorate yield [Zn(HNal)2(H2O)2](ClO4)2 · 2 H2O (3) containing zinc in an octahedral ZnO6 environment. Mercaptopurine (H2Mer), in the presence of ammonia, forms [Zn(Mer)(NH3)2] . H2O (4) which is a coordination polymer containing tetrahedral ZnN4 units. The structures of [Zn(Nih)NH3], [Zn(HNal)2(H2O)2](ClO4)2 . 2 H2O, and [Zn(Mer)(NH3)2] . 2 H2O were determined diffractometrically.
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    Enantioselective Deprotonation of Benzyl Phosphates by Homochiral Lithium Amide Bases  -  Configurational Stability of Benzyl Carbanions with a Dialkoxyphosphoryloxy Substituent and Their Rearrangement to Optically Active α-Hydroxy Phosphonates (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 823-830 
    Details
    ISSN: 0009-2940
    Keywords: Phosphate-phosphonate rearrangement ; Carbanions, benzylic, configurational stability of ; Phosphonaes Lithium amides, homochiral ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Benzyl dialkyl phosphates are deprotonated enantioselectively by homochiral lithium amides of isopropyl(1-phenylethyl)amine or bis(1-phenylethyl)amine. The short-lived benzylic carbanions formed are virtually configurationally stable relative to the rearrangement to optically active phenyl-hydroxymethylphosphonates. The enantiomeric excesses are up to 50%. The pro-(S) hydrogen is removed by amides having (S) configuration. Homochiral diethyl (S)-phenyl[D1]-methyl phosphate [(S)-16c] is deprotonated by both LDA and n-BuLi with a high primary kinetic isotope effect (kH/D ≍ 50) and isomerizes to the corresponding α-hydroxy phosphonate with an enantiomeric excess of up to 85%.
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    Tris(1,10-phenanthroline)iron(II) Complexes  -  Broad Variation of the Redox Potential by 4,7-Substitution at the Phenanthroline Ligands[1] (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 845-850 
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    ISSN: 0009-2940
    Keywords: Phenanthroline synthesis ; Tris(phenanthroline)iron(II) complexes ; Redox potential ; Cyclic voltammetry ; Electron transfer, outer-sphere ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The new 4,7-donor-substituted phenanthrolines 2a-h were synthesized and the corresponding tris(1,10-phenanthroline)iron(II) complexes 3a-h studied by cyclic voltammetry. In more detail three novel aza-crown ether-linked (phenanthroline)iron complexes were investigated, the redox potentials of which could be fine-tuned by the addition of group-Ia,IIa metal cations. All iron(II) complexes showed reversible waves at scan rates between 50 and 500 mV · s-1 and could be reversibly oxidized and reduced by chemical means.
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    Bis(cyclopentadienyl)methane-Bridged Dinuclear Complexes, 10Part 9: B. Stempfle, H. Werner, Gazz. Chim. Ital., 1995, 125, in press. The Bis(cyclopentadienyl)methane Link between Lewis Basic and Lewis Acidic Metal CentersDedicated to Prof. Dr. Herbert Schumann on the occasion of his 60th birthday. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 877-881 
    Details
    ISSN: 0009-2940
    Keywords: Bis(cyclopentadienyl)methane ; Heterobimetallic complexes ; Imido complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The mononuclear rhodium complexes [(C5H5CH2C5H4)-Rh(CO)2] (1) and [(C5H5CH2C5H4)Rh(PhC≡CPh)(PiPr3)] (2) readily react with nBuLi or TlOEt to yield the corresponding lithium salts 3 and 4 or thallium salts 5 and 6. The reaction of these salts with [(C5H5)Nb(NtBu)Cl2] (7) leads to the formation of the heterodinuclear compounds [{CH2(C5H4)2}-{Rh(CO)2}{(C5H5)Nb(NtBu)Cl}] (8) and [{CH2(C5H4)2}-{Rh(PhC≡CPh)(PiPr3)}{(C5H5)Nb(NtBu)Cl}] (9), respectively. Treatment of 3-6 with [Mo(NtBu)2Cl2] (10) gives the heterodinuclear Rh/Mo complexes [{CH2(C5H4)2}{Rh(CO)2}-{Mo(NtBu)2Cl}] (11) and [{CH2(C5H4)2}{Rh(PhC≡CPh)-(PiPr3)}{Mo(NtBu)2Cl}] (12). The analogous reaction of [Mo(NMes)2Cl2(DME)] (13) with 3-6 yields the corresponding complexes [{CH2(C5H4)2}{Rh(CO)2}{Mo(NMes)2Cl}] (14) and [{CH2(C5H4)2}{Rh(PhC≡CPh)(PiPr3)}{Mo(NMes)2Cl}] (15). From the monometallated ligand [(C5H5CH2C5H4)M] (M = Li: 16; M = Tl: 17) and the imidometal compounds 7, 10 and 13, the mononuclear complexes [(C5H5CH2C5H4)(C5H5)Nb-(NtBu)Cl] (18) and [(C5H5CH2C5H4)Mo(NR)2Cl] (R = tBu: 19; R = Mes: 20) have been obtained.
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    Synthesis of 7-Alkyl/aryl-1,3,5-triaza-7-phosphonia-adamantane Cations and Their Reductive Cleavage to Novel N-Methyl-P-alkyl/aryl[3.3.1]bicyclononane Ligands (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 891-900 
    Details
    ISSN: 0009-2940
    Keywords: 1,3,5-Triaza-7-phospha-adamantane ; Reductive cleavage of phosphonium salts ; Ambidentate P,N-ligands ; P,N-[3.3.1]bicyclononane systems ; Phosphanes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Two reaction pathways for the synthesis of 1,3,5-triaza-7-phosphoniaadamantane salts, RP[(CH2)6N3]+X- (1), were followed. Route 1 starts with commercial tetrakis(hydroxymethyl)phosphonium chloride, which is converted into P(CH2OH)3 by treatment with a base. Subsequent quaternization with alkyl halides RX and cyclization with formaldehyde and ammonia afford [R-TPA]+X-. This process is only applicable for R = Me (1a) and Et (1b), however. Route 2 is more general and starts with primary phosphanes RPH2, which are converted into organotris(hydroxymethyl)phosphonium salts with formaldehyde and hydrochloric acid followed by ring closure with CH2O/NH3 to give compounds 1c-1f (R = t-Bu, c-Hex, Bz, and Ph, respectively, and X = Cl, I, PF6, or BPh4). Reductive cleavage of compounds 1 by sodium in liquid ammonia proceeds with either external (P-R) or internal (P-CH2) bond rupture. P-R cleavage affords the 1,3,5-triaza-7-phosphaadamantane (TPA), while cage cleavage leads to new bowl- or helmet-shaped ligand systems with peripheral amine and phosphane functions (2). Yields of the cage-opening reaction are highest for R = Ph (2f), moderate for R = Me and Et (2a, 2b), and poor with the remaining R groups (2c-2e). A radical mechanism is proposed for this reaction, the leaving group properties of R determining the direction of the cleavage. The crystal and molecular structures of compounds 2a and 2f were determined by X-ray diffraction studies. Exo positions were found for the N-Me and P-R groups. The isomers with the R group in the endo position are also present in solution in small amounts, as detected by NMR spectroscopy. Isomer interconversion by P inversion is slow on the NMR time scale. Compounds 2a, 2b and 2f were oxidized with elemental sulfur and selenium to give the monosulfides and selenides, respectively (2aS, 2aSe, 2bS, 2bSe, 2fS, 2fSe). Oxidation with H2O2 led to degradation. Compound 2a was quaternized at the P atom by treatment with Mel to give the corresponding phosphonium salt. Treatment with equimolar quantities of (Me2S)AuCl led to the 1:1 complexes 2aAucl, 2bAuCl and 2fAuCl, with the AuCl units solely P-bonded, as determined by X-ray diffraction of 2aAuCl and 2fAuCl. Compound 2a forms an ionic 2:1 complex with AuCl, composed of the ions [(2a)2Au]+ Cl- (with unidentate ligands), while its reaction with [Me2AuCl]2 leads to [Me2Au(2a)]+ [Me2AuCl2]- (with a chelating 2a ligand), as again confirmed by crystal structure analysis in both cases. Ligands 2a, 2b and 2f also act as chelating ligands in their tetracarbonylmolybdenum complexes obtained in the reactions with (C7H8)Mo(CO)4.
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    Metal Tetrahydroborates and Tetrahydroborato Metalates. 20Contribution 19: M. Bremer, H. Nöth, M. Thomann, M. Schmidt, Chem. Ber. 1995, 128, 455-460.. Reactions of Cadmium Tetrahydroborate with Alcoholates and Phenolates - X-ray Structure of [MeCd(OCMe3)]4 (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 923-927 
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    ISSN: 0009-2940
    Keywords: 11B-NMR spectroscopy ; 113Cd-NMR spectroscopy ; tert-Butoxy(methyl)cadmium tetramer ; Organyloxy(tetrahydroborato)cadmates ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Cadmium tetrahydroborate reacts with alkali metal alcoholates or phenolates in THF solution either with formation of addition products [Cd(BH4)2OR]- or by ligand exchange to produce Cd(BH4)OR. Different oligomers of the latter are formed depending on concentration. The reaction of Cd(BH4)2 with Cd(Omes)2 (mes = mesityl) leads to an equilibrium of the starting materials with Cd(BH4)(Omes) as shown by 113Cd-NMR spectroscopy. The crystal structure of Me-Cd(OCMe3), a molecule which can be regarded as a model for Cd(OCMe3)(BH4), proved to be a tetramer with a cubane-type Cd4O4 core.
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    Preparation, Properties, and Reactions of Metal-Containing Heterocycles, XCIPart XC: Ref.[1]. Insertion of Activated Alkynes and Sulfur into the P-P Bond of DiphosphamolybdacyclopropanesDedicated to Professor Herbert Schumann on the occasion of his 60th birthday (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 973-982 
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    ISSN: 0009-2940
    Keywords: Molybdenum heterocycles ; P - P bonds ; Activated alkynes ; Sulfur ; Insertion reactions ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The insertion of the alkynes ZC≡CZ (2a-i) [Z = Co2R: R = Me (a), Et (b), nPr (c), iPr (d), nBu (e), tBu (f), neo-Pent (g), cyc-Hex (h); Z = CF3 (i)] into the P1-P2 bond of the diphos-phamolybdacyclopropane Mes (1) (Mes = 2,4,6-trimethylphenyl) results in the formation of the diphosphamolybdacyclopentenes Mes (3a-i). According to an X-ray structural analysis, 3a crystallizes in the space group P21/c with the mesityl function at P2 and the cyclopentadienyl fragment at the metal atom on the opposite side of the planar five-membered ring. The same orientation is found in solution by NMR experiments (NOE; 2D 1H, 13C HETCOR). Kinetic investigations confirm that the rate constants decrease in the sequence R = Me 〉 Et 〉 nPr 〉 isoProp 〉 Cy 〉 nBu 〉 neo-Pent 〉 tBu. The second-order reaction and the strongly negative activation entropy which was determined in the case of the reaction 1 + 2e → 3e are consistent with a nucleophilic attack of P2 at one of the triply bonded carbon atoms of the alkyne. The reaction of 3a, h with sulfur affords the diastereomeric compounds Mes (4a, h). An X-ray structural analysis of the heterocycle 4h, which crystallizes in the space group P1, shows the presence of the enantiomeric pair SR/RS. The reaction of 1 with alkynes is hindered if this heterocycle is oxidized by sulfur to give Mes (5). Further reaction of 5 with sulfur leads to the ring-expanded heterocyclic intermediate (6) which crystallizes in the space group P1. The five-membered ring in 6 has an envelope conformation. Upon thermally induced cleavage of the P2S2Mes fragment from 6 the three-membered ring (7) is formed as the final product.
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    Correction (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1271-1271 
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    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    URL: http://dx.doi.org/10.1002/cber.19951281221
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    Metal Complexes of Functional Isocyanides, XXV. Amino(hydrazino)carbene Complexes (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1061-1068 
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    ISSN: 0009-2940
    Keywords: N-Isocyanides ; N-Isocyanodialkylamine complexes ; Carbene complexes ; Imaging-Plate data collection ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The N-isocyanodialkylamine metal complexes [M(CO)5CN-NR2] (M = Cr, W), trans-[MI2(CNNR2)2] (M = Pd, Pt), trans-[Pt(Cl)(CNNR2)(PPh3)2]BF4, and cis-[PtCl2(CNNR2)(PPh3)] [R = Et, iPr; 2 R = -{CHMe(CH2)3CHMe}-] react with primary amines to give the amino(hydrazino)carbene metal complexes [M(CO)5(C(NHR′)NHNR2}] (R′ = Me, nPr, Cy) (1-9), trans-[PtI2{C(NHMe)NHNR2}2] (10-12) and trans, and the amine adducts cis-[PtCl2{C(NHMe)NHNC(H)(Me) (CH2)3CHMe}(PPh3)] H2NMe (14), and trans-[PdI2{C (NHMe)NHNC(H)(Me)(CH2)3CHMe}2] 2 H2NMe (15). With secondary amines the amino(hydrazino)carbene metal complexes trans (18) and trans-[PtCl{C(NEt2)NHNEt2} (PPh3)2]BF4 (19) Were isolated. The complexes trans-[PtI2{C(NHCy)NHNiPr2}CNNiPr 2] (20) and trans-[PdI2 (NH2Cy){C(NHCy)NHNiPr2}] (21) were obtained by reaction of trans-[MI2(CNNiPr2)2] (M = Pd, Pt) with cyclohexylamine. The structures were assigned on the basis of IR, NMR- (1H, 13C, 31P), and mass spectroscopy as well as an X-ray structural analysis of 21.
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    Metallocenophanes, VIIPart VI: Ref.. Preparation and Characterisation of the Disilver(I) Complexes of Conjugated Polyenes with [2.2.2]Paracyclophanyl End Groups (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1079-1082 
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    ISSN: 0009-2940
    Keywords: [2.2.2]Paracyclophanes ; Polyenes ; Silver complexes ; X-Ray structural analysis ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The preparation of the disilver(I) complexes 3 and 4, polyene metal complexes that are terminally substituted with [2.2.2]paracyclophanyl units, is described. NMR spectro-scopic studies on the disilver perchlorate complex 3b showed that (a) the sites of complexation are the cyclophane groups and (b) the olefinic spacers do not overly perturb the overall complexation properties of the individual [2.2.2]paracyclo-phanyl groups. The crystal structures of the disilver hexafluo-roantimonate complexes 4a-b were determined. The use of the hexafluoroantimonate counterion and solvent mixtures containing toluene both proved crucial in obtaining single crystals; toluene is incorportated into the crystal lattices.
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    Highly Substituted Tris(pyrazolyl)methane Ligands and Some Zinc Complexes Thereof (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1095-1103 
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    ISSN: 0009-2940
    Keywords: Zinc complexes ; Tridentate ligands ; Tris(pyrazolyl)methane ; Reactivity ; Structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Tris(pyrazolyl)methane ligands in which two or three of the pyrazole carbon atoms bear organic substituents (L1-L7) were synthesized from chloroform and the corresponding pyrazole under phase transfer conditions. Their behavior towards zinc salts was found to span the range from no reaction at all to hydrolytic destruction. One hydrolysis product isolated and structurally characterized was the perchlorate complex [(HPz5)3Zn-OClO3]ClO4 (1), other ones were the 2:1 complexes (HPz3)2ZnBr2 (2) and (HPz6)2Zn(NO3)2 (3, HPzn = substituted pyrazole). Zinc perchlorate and tris(trimethylpy-razolyl)methane (L2) formed the octahedral binary complex [L22Zn](ClO4)2 (4) as evidenced by a structure determination. Zinc halides produced the 1:1 complexes L1 · ZnBr2 (5), L4 · ZnCl2 (6), and L4 · ZnBr2 (7), which according to the structure determinations of 6 and 7 contain tetrahedral ZnN2Hal2 units with only bidentate tris(pyrazolyl)methane ligands. In contrast, the zinc nitrate complex L4 · Zn(NO3)2 (8) was found to have an octahedral structure with mono- and bidentate nitrate and tridentate L4. The bromide complex 7 was converted by silver perchlorate hydrate into the labile compound [L4 · ZnBr]ClO4 (9) and then into the unstable product [L4 · Zn-OH2](ClO4)2 (10), both presumed to contain zinc in a tetrahedral ZnN3Br or ZnN3O environment, respectively. The ease of hydrolytic self-destruction prevented the exploitation of the reactivity of 9 and 10 in analogy to that of the corresponding tris(pyrazolyl)borate zinc complexes.
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    The 13C Chemical Shift of the ipso Carbon Atom in Phenyllithium (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1183-1186 
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    ISSN: 0009-2940
    Keywords: Phenyllithium ; Solid-state NMR ; Chemical shift anisotropy ; Calculations, IGLO ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Phenyllithium was labeled with 6Li and 13C at the ipso carbon atom, and the tetramer was measured by solid-state NMR. The chemical shift tensor data were obtained by a moment analysis of the spinning side bands and were compared with the results obtained by calculations with the IGLO method. Although no splitting by dipolar spin coupling to 6Li was found the very good agreement between IGLO predictions and experimental results allowed alignment of the tensor axis to the molecular frame and interpretation of the data. The large deshielding of the isotropic chemical shift is mainly due to a decrease of the ΔE term in s̰.
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    Synthesis and Characterization of Copper(II) Complexes of a 14-Membered cis-N2S2 Dibenzo Macrocycle and of Its Bis-acetato and Bis(methylpyridyl) Derivatives (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1199-1205 
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    ISSN: 0009-2940
    Keywords: Copper(I) complexes ; Copper(II) complexes ; N,S-Donor ligands ; Macrocyclic ligands ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The synthesis and characterization of seven copper coordination compounds with the 14-membered macrocyclic cis-N2S2 dibenzo ligand 6,7,13,14,15,16,17,18-octahydrodibenzo[e,m]-[1,4,8,11]dithiadiazacyclotetradecine (L1) and its N,N'-bisacetato and -bis(methylpyridyl) functionalized derivatives H2L2 and L3 are described. The structures of five compounds were determined by single-crystal X-ray diffraction. The tetrahedrally distorted square-planar coordination geometry of [CuL1](ClO4)2 (1) changes upon reduction of copper to a severely distorted tetrahedral geometry in [CuL1]Br · MeCN (2). The Cu-N bond lengths increase from 1.988(3) to 2.029(5) Å; the Cu-S bond lengths decrease from 2.293(1) to 2.255(2) Å. Copper(II) is hexacoordinated in [CuHL2]HSO4 · 2.5 H2O (5) and [CuHL2]ClO4 · H2O (6). Both compounds exhibit very similar overall structures in the cationic part. The macrocyclic ring of the ligand is folded along an N⃜S axis, the octahedral geometry is strongly Jahn-Teller distorted, with O and S donor atoms in the apical positions. Compound 5 contains one very short [2.271(3) Å] and one long [2.701(3) Å] Cu-S (thioether) bond. In [CuL3](ClO4)2 · 2 H2O (7) one thioether group of the ligand L3 remains uncoordinated. The coordination polyhedron is rather irregular: Cu-S 2.506(3) and Cu-N 1.960(7)-2.107(8) Å. The compounds were further characterized by electronic and EPR spectroscopy and by cyclic voltammetry. Some relationships to the structural and spectroscopic properties of “blue” copper proteins were found.
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    Chiral Ligands for Transition Metal Complexation (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 449-454 
    Details
    ISSN: 0009-2940
    Keywords: Chiral ligands ; Transition metal complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Novel chiral salen- or salphen-type ligands with stereogenic centres in the 1,3-dicarbonyl moiety 2 as well as in the amino bridge in 15-18 were synthesized from the enantiomerically pure Hajos-Wiechert ketone.
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    Synthesis and Characterization of β-Phosphaenones An Investigation on the Conjugative Properties of the P=C Bond (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 465-476 
    Details
    ISSN: 0009-2940
    Keywords: Phosphaalkenes, C-halo, C-metal ; Phosphaacrylic acid ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Thermally and air-stable β-phosphaenones were synthesized by functionalization of Mes*P=CCl2 (1; Mes* = supermesityl = 2,4,6-tri-tert-butylphenyl). At low temperature, 1 was lithiated by halogen-metal exchange with n-butyllithium to give the phosphanylidene carbenoid (Z)-Mes*P=C(Cl)Li [(Z)-2] which reacted with acid chlorides to furnish the C-carbonyl-substituted phosphaalkenes (Z)-Mes*P=C(Cl)R (3: P = COtBu; 4: R = COPh; 5: R = COOEt). The reaction of (Z)-2 with carbon dioxide furnished the carboxylate 6, which was converted by treatment with pivaloyl chloride or trimethylsilyl chloride into the phosphaalkenes 7 and 8 functionalized at the carbon atom by an anhydride or a trimethylsilyl ester function, respectively. Acidification of 6 or hydrolysis of 8 with water in chloroform solution afforded the novel carboxylic acid (Z)-Mes*P=C(Cl)COOH (9). Spectroscopic investigations (NMR, UV, IR) of 3-9 and the X-ray structures of 3 and 4 are presented. Based on these properties and on theoretical calculations, the occurrence of conjugation in the β-phosphaenone system is discussed and compared with the well-known conjugation in normal enones.
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    Reactions of Phosphaalkenes with HexafluoroacetoneDedicated to Professor H. M. R. Hoffmann on the occasion of his 60th birthday. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 499-502 
    Details
    ISSN: 0009-2940
    Keywords: Phosphaalkenes ; Cycloadditions ; Insertion reactions ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The dimethylamino-substituted phosphaalkene 1 reacts with hexafluoroacetone (HFA) with addition at the P=C bond to form the 1,5,2-dioxaphosphorinane 2. The structure of 2 was confirmed by an X-ray crystal structure analysis. The six-membered ring displays an envelope conformation with the phosphorus atom out of the plane, but the phosphorus is disordered over two sites. Reaction of P-trimethylsilyl-substituted phosphaalkenes with HFA proceeds with retention of the P=C double bond and insertion of HFA into the P—Si bond. Two isomeric products are obtained and are characterized by 1H-, 13C-, 19F-, and 31P-NMR spectroscopy, IR spectroscopy, mass spectrometry, and elemental analysis.
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    Zinc Complexes of S,N Ligands Derived from Thiazolines (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 787-791 
    Details
    ISSN: 0009-2940
    Keywords: Zinc complexes ; Sulfur and nitrogen ligands ; Structure determinations ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Three different thiazoline derivatives or their tautomeric mercaptoethylamine derivatives were used for the preparation of zinc complexes containing S,N ligands. 2-(2-pyridyl)-3-(2-pyridylmethyl)-1,3-thiazolidine (PPMT) could not be opened reductively but acted as a tridentate nitrogen ligand in (PPMT)ZnX2 (1a, b, X = Br, NO3). The thiazolidine tautomer N-(2-mercaptoethyl)salicylideneimine (MESIH2) yielded polymeric (MESI)Zn (2) and, after oxidation, monomeric (MESI)2Zn (3) containing a disulfide unit. The 2-aryl-benzo-1,3-thiazoline tautomers N-(2-mercaptophenyl)-p-fluoroben-zylideneimine (MPFBH) and N-(2-mercaptophenyl)-p-meth-oxybenzylideneimine (MPMBH) underwent reaction with diethyl zinc resulting in the unstable L . Zn-Et complexes 4a and b, which are probably dimeric and the stable 2:1 complex (MPFB)2Zn (5). The structures of 3 and 5 were determined and were found to exhibit distorted tetrahedral ZnN2O2 and ZnN2S2 coordinations, respectively.
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    Synthesis and Reactivity of Silicon-Transition Metal Complexes, 3l30. Mitteilung: Lit.[1e].. Metallosilanols and Metallosiloxanes, 61.-5. Mitteilung: Lit.[1a-e].. Die ersten Hydroxysilandiyl-verbrückten Zweikernkomplexe: Selektive Oxygenierung der Silicium-Brücke in Silandiyleisen-Komplexen mit Dimethyldioxiran (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 963-965 
    Details
    ISSN: 0009-2940
    Keywords: Dimethyldioxirane ; Oxofunctionalization ; Si-H bonds ; Iron complexes, silanediyl-bridged ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Synthesis and Reactivity of Silicon-Transition Metal Complexes, 31  -  Metallosilanols and Metallosiloxanes, 6.  -  The First Hydroxysilanediyl-Bridged Binuclear Complexes: Selective Oxofunctionalization of the Silicon Bridge in Silanediyliron Complexes with DimethyldioxiraneOxygenation of [μ-(R)(H)Si][Fe(CO)2Cp]2 [R = Me (1a), pTol (1b)] with dimethyldioxirane (2) yields the μ-(hydroxysilanediyl)bisiron complexes [μ-(R)(HO)Si][Fe(CO)2Cp]2 [R = Me (3a), pTol (3b)]. In an analogous manner the cyclic complex (μ-OC)[μ-(Mes)(H)Si][Fe(CO)Cp]2(Fe-Fe) (6) obtained by photochemical reaction of Cp(OC)2Fe-Me (4) with MesSiH3, (5) is converted into (μ-OC)[μ-(Mes)(HO)Si][Fe(CO)Cp]2-(Fe-Fe) (7). 6 and 7 are obtained as a mixture of cis(Mes), cis(H or OH), and trans isomers.
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    URL: http://dx.doi.org/10.1002/cber.19951280920
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    Organophosphorus Compounds, 103Part 102: Ref.[1]. Thermal Transformation of Kinetically Stabilized Phosphaalkynes with Phosphinidene Precursors. Synthesis of Phosphorus-Carbon Cage Compounds by Cocyclooligomerization ProcessesDedicated to Professor H.-J. Bestmann on the occasion of his 70th birthday (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 991-997 
    Details
    ISSN: 0009-2940
    Keywords: Phosphaalkynes ; Phosphinidenes ; Phosphinidene Complexes ; Cocyclooligomerization ; Cage compounds, phosphorus-carbon ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Phosphaalkynes 2 undergo cocyclooligomerization reactions with the phosphinidene 14 or the phosphinidene-W(CO)5 complex 18 to furnish the phosphorus-carbon cage compounds 16 or 23. The phosphinidene 14 is generated by the thermal reaction of 2a-c with the phosphole 11, a process in which the initially formed 7-phosphanorbornadienes 12a-c decompose to the λ3-phosphinines 13a-c and the desired reactive intermediate. When three further equivalents of the phosphaalkynes 2a-c are employed, the tetraphosphahomoquadricyclanes 16a-c can be isolated in 53-65% yields. The second approach is based on the thermal fragmentation of 17 to generate the phosphinidene-W(CO)5 complex 18 which, in turn, reacts with four equivalents of the phosphaalkynes 2a or b to produce the pentaphosphadeltacyclanes 23a or b. The constitutions of these novel phosphorus-carbon cage compounds were confirmed by X-ray crystal structure analyses of 16a and 23a.
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    Masthead (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995) 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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    URL: http://dx.doi.org/10.1002/cber.19951281101
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    Chiral Carbanions, 1. Configurational Stability and Reactions of α-Acyloxy-Substituted α-Methylbenzyllithium Compounds (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1069-1077 
    Details
    ISSN: 0009-2940
    Keywords: Esters, 1-phenylethyl ; Carbanions, α-methyl-α-oxybenzyl, Configurational stability ; Ester - hydroxy ketone rearrangement ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Racemic and optically active 1-phenylethyl esters of pivalic, ( - )-camphanic and 2,4,6-triisopropylbenzoic acid were prepared. The esters 7a of pivalic acid were deprotonated with lithium 2,2,6,6-tetramethylpiperidide (Li-TMP) to form α-oxy-α-methylbenzyllithium compounds which are partly con-figurationally stable prior to acylation with starting material. Camphanic ester (-)-7b cannot be deprotonated by Li-TMP and tBuLi is added to the ester function to afford ketone (-)-12a. 1-Phenylethyl 2,4,6-triisopropylbenzoates 16 were transformed within minutes to carbanions 19 by using sBuLi/TMEDA in THF, hexane, toluene and sBuLi without TMEDA in toluene/20% diethyl ether at -78°C. The carbanions are configurationally stable only in toluene/20% diethyl ether and racemise partly in the other solvents. They react with a variety of electrophiles with either retention [MeOD, AcOD, (MeO)2CO, CICO2Me] or inversion (Me3SnCl) of configuration. Carbanions 19 rearrange on warming to -20°C to hydroxy ketone 24 with racemisation.
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    Metal Complexes with Tetrapyrrole Ligands, LXIX. Facile Synthesis and 13C-NMR Spectrum of Dichloro(octaethylporphyrinato)zirconium(IV) (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1131-1133 
    Details
    ISSN: 0009-2940
    Keywords: Zirconium(IV) octaethylporphyrin complex ; Dichlorozirconium(IV) porphyrin complex ; Precursor of organometallic compounds ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The synthesis of dichloro(2,3,7,8,12,13,17,18-octaethylpor-phyrinato)zirconium(IV), Zr(oep)Cl2, from zirconium tetrachloride and octaethylporphyrin, H2(oep), is described. The reported synthesis is a new and simple route to this precursor of organometallic compounds. Zr(oep)Cl2 was characterized by elemental analyses, 1H- and 13C-NMR, UV/Vis, and mass spectra. Hydrolysis yielded a mixture of mono- and binuclear hydroxy zirconium(IV) porphyrins.
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    Auf- und Abbau von Azadecaboranen; Aza-nido-nonaboratFrau Professor Marianne Baudler zum 75. Geburtstag gewidmet. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1221-1224 
    Details
    ISSN: 0009-2940
    Keywords: 10-Organo-10-aza-nido-nonaborates ; 6-Alkylamine-4-aryl-4-aza-arachno-nonaboranes ; 1-Orgaro-1-aza-closo-decaboranes ; 6-Aryl-6-aza-nido-decaboranes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Synthesis and Degradation of Azadecaboranes; Aza-nido-nonaborateThe boranes arachno-B9H13(NRH2 (1a-c: R = p-ClC6H4, p-MeC6H4, PhCH2) are dehydrogenated at 140°C to give nido-RNB9H11 (2a-c), from which the azaboranes closo-RNB9H9 (3a-c) are formed on further dehydrogenation at 460°C. These azaboranes are deboronated either by the attack of the amine iPrNH2 or by one of the fluorides [NBu4]F or [S(NMe2)3][Me3SiF2] in THF. One of the four boron atoms adjacent to nitrogen in the closo species is removed and then detected in the borazine (HNBiPr)3 or the borate BF4, respectively, whereas the novel anions nido-RNB8H9 (4a-c) remain. The structure of 4a-c corresponds to that of nido-SB8-H9-, according to NMR spectra. Primary amines R'NH2 deboronate the closo-boranes 3a, b in a solvent less polar than THF to give the amine - azanonaboranes arachno-RNB8H10-(NR'H2) (5a-c: R' = iPr, Pr, Bu). The nido product [iPrNH3][(p-ClC6H4)NB8H9 is converted into a mixture of the arachno products 5a and (p-ClC6H4)NB8H10(NPrH2) (5d) by the action of PrNH2, making plausible that anions of type 4 are intermediates during the transformation of 3 into 5.
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    Thermische Stabilisierung des Silaethens Ph2Si=C(SiMe3)2Frühere Mitteilungen: Lit.Herrn Prof. Dr. Manfred Regitz zum 60. Geburtstag gewidmet. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1241-1250 
    Details
    ISSN: 0009-2940
    Keywords: Methyl and phenyl group migrations in Ph2Si=C(SiMe3)2 ; Silaethenes Me2Si=C(SiMePh2)(SiMe3), PhMeSi=(SiMe2Ph)(SiMe3), Me2Si=C(SiMe2Ph)2 ; Silaethene dimers ; Disilaindanes ; Silaethene reactions with Et2O and with Ph2SiBr-CLi(SiMe3)2 ; Insertions of silaethenes into SiN bond of Ph2C=N-SiMe3 ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Thermal Stabilization of the Silaethene Ph2Si=C(SiMe3)2Frühere Mitteilungen: Lit. Herrn Prof. Dr. Manfred Regitz zum 60. Geburtstag gewidmet.Silaethene Ph2Si=C(SiMe3)2 (3) (generated from Ph2SiBr-C-Li(SiMe3)2 = 3 · LiBr in Et2O at -78·C) reversibly isomerizes fast by methyl migration, then a bit slower by phenyl migration, and finally fast by methyl migration into thermodynamically more stable Me2Si=C(SiMePh2)(SiMe3) (3a), then into medium stable PhMeSi=C(SiMe2Ph)(SiMe3) (3b), and finally into most stable Me2Si=C(SiMe2Ph)2 (3c) (cf. Schemes 1 and 2; Figure 1). Simultaneously with isomerization 3a · 3c [2 + 2] cycloadditions (dimerizations) of 3a and 3c occur (formation of 3a · 3a, 3a · 3c, 3c · 3c; cf. Scheme 2). Over and above that, silaethenes 3a and 3c irreversibly isomerize into disilaindanes 4a, 4b, and 4c (cf. Scheme 6). Certainly, the latter reactions are even slow at 100·C. Thermolysis of 3a · 3a, 3a · 3c, 3c · 3c at 340·C, on the other hand, leads by way of [2 + 2] cycloreversion and the intermediate formation of an equilibrium mixture of 3, 3a, 3b, 3c almost quantitatively to 4. In addition to the thermolysis products mentioned above, products of 3 and its isomers 3a, 3b, 3c with the solvents (for example Et2O; cf. Scheme 7), with the silaethene sources (for example 3 · LiBr; cf. Scheme 8), or with products formed from sources besides silaethene 3 (for example Ph2,C=N-SiMe3;cf. Scheme 4) are observed.
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    (η8-Cyclooctatetraene)(η4-1,2- and -1,3-diphosphacyclobutadiene)titanium: Preparation, Structure, and Reactivity (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1261-1265 
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    ISSN: 0009-2940
    Keywords: (Cyclooctatetraene)titanium complexes ; Diphosphacyclobutadiene ; Cyclodimerization ; Phosphaalkyne ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The synthesis of the (η8-cyclooctatetraene)(η4-1,3- and -1,2-diphosphacyclobutadiene)titanium complexes 3a-c and 4a, b by cyclodimerization of the phosphaalkynes 2a-c [a: R = tBu, b: R = adamantyl (ad), and c: R = (iPr)(Me3Si)N] in the coordination sphere of the (η8-cyclooctatetraene)titanium complex 1 is described. The molecular structures of 3a-c and 4a, b were determined by spectroscopic methods (31P, 1H, and 13C NMR). In the case of 3a and 4a, X-ray analyses were carried out. The increased reactivity of 4a compared to 3a was utilized to separate 3a from 4a. Displacement of the 1,2-diphosphete (isolated as its cyclodimer 5) from 3b was achieved by reaction with hexachlorethane.
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    Synthese und Komplexchemie funktionalisierter Tripod-Liganden RC(CH2PPh2)3Manfred Ziegler zum Gedenken. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 63-70 
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    ISSN: 0009-2940
    Keywords: Tripod ligand synthesis ; Tripod nickel chloro complexes ; Tripod iron tris(acetonitrile) complexes ; Tripod cobalt acetate complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Synthesis and Complex Chemistry of Functionalised Tripod Ligands RC(CH2PPh2)3Malonic ester 1 is alkylated and converted into the triols RC(CH2OH)3 (5). These are easily converted into the corresponding functionalised tripodal ligands RC(CH2PPh2)3 (7) with R = Bzl (a), n-C12H25 (b), (CH3)2CH(CH2)2 (c). Crystals suitable for X-ray crystallography have been obtained of the ligand 7a. In addition, the tripod ligands 7a and 7c have been further characterized by the syntheses and X-ray analyses of the nickel complex [(7a)NiCl] (8a), the iron complex [(7c)Fe(NCCH3)3](BF4)2 [9 · (BF4)2], and the cobalt complex [(7c)Co{O(O)CCH3}](BPh4) (10 · BF4).
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    Übertragung eines cyclo-E5-Liganden (E = P, As) von einem Eisen- auf ein Ruthenium- und ein Osmium-ZentrumHerrn Professor Hubert Schmidbaur zum 60. Geburtstag gewidmet. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 71-73 
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    ISSN: 0009-2940
    Keywords: cyclo-E5 ligands (E = P, As) ; Transfer reaction ; Iron complexes ; Ruthenium complexes ; Osmium complexes ; Sandwich complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Transfer of a cyclo-E5 Ligand (E = P, As) from an Iron to a Ruthenium and an Osmium Center⋆The thermolysis of [Cp*Fe(η5-E5)] (1) and [{Cp*M(CO)2}2] (2, 3) affords by cyclo-E5 transfer the sandwich complexes [Cp* M(η5-E5)] (4a, b: M = Ru, E = P, As; 4c: M = Os, E = P). The crystal-structure analysis of [(C5Me4Et)Os(η5-P5)] (4c') confirms its sandwich-type structure.
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    Structural Chemistry of Lithium HydrazidesDedicated to Professor Ernst Biekert on the occasion of his 70th birthday. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 105-113 
    Details
    ISSN: 0009-2940
    Keywords: Lithium N,N'-diethylhydrazide hexamer ; Dilithium N,N'-bis(trimethylsilyl)hydrazide tetramer ; [Lithium N,N-bis(trimethylsily)hydrazide]-[dilithium N,N'-bis(trimethylsilyl)hydrazide] dimer ; Dilithium N-phenyl-N-trimethylsilylhydrazide tetramer ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Deprotonation of NH protons, of four diorgano-, organo(trimethylsilyl)- and bis(trimethylsilyl)hydrazines by n-butyllithium in hexane led to the following lithium hydrazides: [Et-(Li)N-N(H)Et]6, (1)6, [Me3Si(Li)N-N(Li)SiMe3]4, (2)4, [Me3Si-(Li)N-N(Li)SiMe3 · (Me3Si)2N-N(Li)SiMe3]2 (3)2, and [Ph-(Li)N-N(Li)SiMe3]4, (4)4, respectively. The structure determination by X-ray methods at low temperature reveals butterfly-shaped Li2N2 structural monomeric units which associate through “laddering” to the observed oligomers thereby generating penta- and hexacoordinated Li centers. N-N bonds lengths of up to 1.556 Å suggest that negative charge accumulates at the nitrogen atoms of (1)6, (2)4, and (3)2. An amazing structure shows the red compound 4 where two Li ions are π-sandwiched between two phenyl groups each. The compound can be looked at as a new type of a lithium lithiate complex, Li2[Li6N8Ph4(SiMe3)4], but short N-C and N-N bonds in the Li6N8 core indicate that its negative charge is transferred to the phenyl groups.
    Additional Material: 7 Ill.
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    Ion Pair Charge-Transfer Complexes of Dithiolene Metalates with Diquaternary 2,2′-BiimidazolesDedicated to Professor Dr. Heinz Dürr on the occasion of his 60th birthday. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 131-136 
    Details
    ISSN: 0009-2940
    Keywords: Dithiolene metalates ; Biimidazolium dications ; Charge-transfer complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Cycloalkylated biimidazolium dications (A2+) of reduction potentials from -0.4 to -1.4 V form ion pair charge-transfer complexes {A2+ [M(mnt)2]2-} with dithiolene metalates, M = Zn, Ni, Pd, Pt, mnt2- = maleonitrile-2,3-dithiolate. X-ray analyses of {P2BBIm2+[Ni(mnt)2]2-} [P2BBIm2+ = 1,1′,3,3′-bis(propane-1,3-diyl)bibenzimidazolium] and {B2Blm2+ [Pd(mnt)2]2-} [B2BIm2+ = 1,1′,3,3′-bis(butane-1,4-diyl)biimidazolium] reveal that the solid-state structure is largely determined by the geometry of the acceptor. When the latter is strongly twisted, the usually observed mixed donor-acceptor columns are modified to a chain-like arrangement. In the case of the bibenzimidazolium dication P2BBIm2+ the otherwise planar [Ni(mnt)2]2- becomes tetrahedrally distorted. By the application of the Hush model a reorganization energy of about 67 kJ/mol is estimated for the thermal electron transfer from [M(mnt)2]2- to A2+ when M = Ni, Pd, Pt, but considerable deviations from this model are observed when M = Zn. Irradiation of the free biimidazolium acceptors in the presence of EDTA affords the strongly reducing radical cations which reduce water to hydrogen in the presence of colloidal platinum. Attempts to sensitize this reaction by irradiating into the charge-transfer band of {A2+ [M(mnt)2]2-} have failed until now. The molar absorptivity of one biimidazolium radical cation is measured by spectroelectrochemistry.
    Additional Material: 6 Ill.
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    Synthesis of Transient Silenes by a Modified Peterson Reaction (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 143-149 
    Details
    ISSN: 0009-2940
    Keywords: Silenes ; Silene dimerization ; 1,2-Disilacyclobutanes ; 2,3-Disilanaphthalene, tetrahydro- ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Tris(trimethylsilyl)silylmagnesium bromide, obtained in situ from tris(trimethylsilyl)silyllithium and magnesium bromide, reacts with acetone, pivalaldehyde, or 2,4,6-trimethylbenzaldehyde to give the (1-hydroxyalkyl)tris(trimethylsilyl)silanes (Me3Si)3SiC(OH)Me2 (1a), (Me3Si)3CH(OH)tBu (1b), and (Me3Si)3SiC(OH)Mes (1c), resp. After deprotonation with methyllithium in ether at -78°C 1a-c eliminate trimethylsilanolate according to a modified Peterson mechanism to form transient silenes (Me3Si)2Si=CR1R2 (6a: R1 = R2 = Me; 6b: R1 = H, R2 = tBu; 6c: R1 = H, R2 = Mes). In the absence of trapping agents these silenes dimerize, 6a leading to the linear dimer 1-isopropenyl-2-isopropyl-1,1,2,2-tetrakis(trimethylsilyl)disilane (7) and 6b giving the head-to-head cyclodimerization product (E)-3,4-di-tert-butyl-1,1,2,2-tetrakis(trimethylsilyl)-1,2-disilacyclobutane (8), whereas 6c in a very unusual cyclodimerization step affords (E)-1,2,3,8a-tetrahydro-1-mesityl-5,7,8a-trimethyl-2,2,3,3-tetrakis(trimethylsilyl)-2,3-disilanaphthalene (9). Compound 9 is the result of an unexpected [2 + 4] reaction, in which the silene formally acts as the monoene and - involving the aromatic substituent - simultaneously also as the diene. The reaction of 1a-c with methyllithium in THF at low temperature initiates 1,3-Si,O-trimethylsilyl migrations leading to (trimethylsiloxy)-[bis(trimethylsilyl)silyl]alkanes (Me3Si)2SiH-CR1R2OSiMe3 3a-c. Reaction of 1a-c with an excess of methyllithium, tert-butyllithium, or phenyllithium, leads to trisilanes (Me3Si)2-SiR3-CHR1R2 11a-e, formed by the addition of the organolithium reagent to the Si=C bond of the transient silences 6a-c. Deprotonation of 1b and 1c in the presence of 2,3-dimethyl-1,3-butadiene gives the [2 + 4] cycloadducts 6-tert-butyl-3,4-dimethyl-1,1-bis(trimethylsilyl)-1-sila-3-cyclohexene (12a) and 6-mesityl-3,4-dimethyl-1,1-bis(trimethylsilyl)-l-sila-3-cyclohexene (12b). For 8 and 9 the results of the X-ray analyses are given.
    Additional Material: 2 Ill.
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    Platin(II)-Komplexe mit Porphyrinliganden: Synthese und Synergismen bei der photodynamischen Tumortherapie (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 173-181 
    Details
    ISSN: 0009-2940
    Keywords: Porphyrins ; Platinum(II) complexes ; Photodynamic therapy ; Antitumor activity ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Platinum(II) Complexes with Porphyrin Ligands: Synthesis and Synergisms in the Photodynamic Tumor TherapyTwelve porphyrin ligands (2-5, 8, 13-16, 19, 27, 28) and their platinum(II) complexes (29-40) were synthesized and characterized. Nine of the porphyrins are derived from hemin, and three are based on tetraphenylporphyrin. The ligands were transformed into diammine-dicarboxylatoplatinum(II) complexes and diamine-dichloroplatinum(II) complexes. The antitumor activity in the photodynamic therapy of the ligands and their complexes was tested in vitro towards the MDA-MB-231 mammary carcinoma cell line. The results obtained showed an additive effect of the photodynamic activity of the porphyrin skeleton when irradiated with visible red light and the cytotoxic activity of the platinum moiety in the complexes.
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    URL: http://dx.doi.org/10.1002/cber.19951280215
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    Zwei Extreme in der Zinnchemie: Ein nichtbindender Sn-Sn-Abstand von 285 pm und eine 119Sn-NMR-Verschiebung δ = 3301 in metallorganischen Derivaten von Sn(0)Herrn Prof. Dr. G. P. Schiemenz gewidmet. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 187-191 
    Details
    ISSN: 0009-2940
    Keywords: Tin complexes ; Transition metal complexes ; NMR, 119Sn ; Sn(0) compounds ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Two Extremes in Tin Chemistry: A Non-bonding Sn-Sn Distance of 285 pm and a 119Sn-NMR Shift δ = 3301 in Organome-tallic Derivatives of Sn(0)The reaction of Na[{Cp'(CO)2Mn}2H] with SnCl2, which produces the inidene compound [Cp'(CO)2Mn\documentclass{article}\usepackage{amsmath}\pagestyle{empty}\begin{document}$ {\rm C}\ddot - {\rm C} $\end{document}Sn(Cl)\documentclass{article}\usepackage{amsmath}\pagestyle{empty}\begin{document}$ {\rm C}\ddot - {\rm C} $\end{document}Mn-(CO)2Cp']- under standard workup procedures, results in the formation of [{Cp'(CO)2MnSn}2{μ2-Mn(CO)2Cp'}2{μ2-Cl}]- (1) when quenched with unpolar solvents. While, formally, 1 contains tin in its oxidation state zero, it may be conceived as composed of an Sn2-2 entity, which is linearly end-on coordinated to two Cp'(CO)2Mn 16-electron species; in addition the tin centers are bridged by two μ2-Mn(CO)2Cp' moieties and a μ2-Cl function. The resulting connectivity Sn2{μ2-Mn(CO)2Cp'}2{μ2-Cl} thus corresponds to a [1.1.1]propellane scaffolding. While there is no obvious need for a tin-tin bond in this propellane-type cage, a short Sn-Sn contact of only 285 pm is observed. While the 119Sn-NMR signal of 1 could not be recorded, the peculiar bonding in this type of compounds is generally mirrored in their unconventional 119Sn-NMR shift whereever signals can be observed: it is found that [{Cp*(CO)2Mn}3(μ3-Sn)], which contains trigonally planar-coordinated μ3-Sn as a naked ligand atom, has its 119Sn-NMR resonance at δ = 3301 well beyond the known range of 119Sn-NMR shifts. This finding is interpreted in terms of a relatively week Snpπ-Mndπ π bonding which leads to low-energy unoccupied molecular orbitals as the prerequisit for a large paramagnetic contribution to the NMR shift.
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    URL: http://dx.doi.org/10.1002/cber.19951280217
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    Pn-Liganden mit maximaler Elektronendonorfähigkeit, 7. Dreikomponentenreaktion von P4-Phosphor mit [CpxRh(CO)2] in Gegenwart von [Cr(CO)5THF] oder [CpMn(CO)2THF]. - Eine Methode zum Studium des Transformationsweges vom P4-Tetraeder zum planaren cyclo-P4-LigandenHerrn Professor Gerhard Fritz zum 75. Geburtstag gewidmet. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 251-257 
    Details
    ISSN: 0009-2940
    Keywords: Tetraphosphorus ligands ; Bond cleavage in P4, stepwise ; Rhodium P4 complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Pn Ligands with Maximum Electron-Donor Capacity, 7. - Three-Component Reaction of P4-Phosphorus with [CpxRh(CO)2] in the Presence of [Cr(CO)5THF] or [CpMn(CO)2THF]. - A Method of Studying the Pathway from Tetrahedral P4 to the Planar cyclo-P4 LigandHerrn Professor Gerhard Fritz zum 75. Geburtstag gewidmet.The reaction of P4 with [CpxRh(CO)2] (Cpx = Cp′, Cp′′; Cp′ = η5-C5H4tBu, Cp′′ = η5-C5H3tBu2-1,3) in the presence of [Cr(CO)5THF] leads to [CpxRh(CO)(η1:1-P4){Cr(CO)5}4] (1a, b), [Cp′′Rh(η4-P4){Cr(CO)5}3] (2b), and [Cp′Rh(η4-P4){Cr-(CO)5}4] (3a). In the corresponding reaction with [CpMn-(CO)2THF] no P4 takes part, and [(Cp′′RhCO)(CpMnCO)(μ-CO)2] (4) is formed. An X-ray structure determination of [CpxRh(CO)(η1:1-P4){Cr(CO)5}4] (1) and [Cp′Rh(η4-P4)-{Cr(CO)5}4] (3a) indicates a stepwise (PP) bond cleavage as the transformation pathway from the P4 tetrahedron to the cyclo-P4 ligand by passing a bicyclotetraphosphane. In the cyclo-P4 ligand complex 3a all P atoms are able to coordinate to [Cr(CO)5] groups. However, in [Cp′′Rh(η4-P4){Cr(CO)5}3] (2b) the additional tBu group at the Cpx ligand sterically influences the coordination behavior of the P atoms, and only three of them are able to coordinate to [Cr(CO)5] units. In these syntheses the [Cr(CO)5] moieties promote the reaction and stabilise intermediates along the reaction pathway. Variable-temperature 31P{1H}-NMR measurements indicate for 2b the freezing of the Cp′′ rotation at low temperature and reveals a ΔG≠c (at the coalescence temperature) of 36 kJ mol-1. Surprisingly, in [(Cp′′RhCO)(CpMnCO)(μ-CO)2]-(Rh-Mn) (4) the Cpx ligands are cis-oriented whereas in [(Cp*RhCO)(CpMnCO)(μ-CO)2](Rh-Mn) a trans arrangement is observed. This indicates the unusual behavior of the Cp′′ ligand as a “rod” and not as an “enlarged disk” like Cp* in the crystal lattice of these compounds.
    Additional Material: 5 Ill.
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    Wasserlösliche Phosphane, IV. Tertiäre Alkylphosphane mit Ammoniumgruppen in den Seitenketten - Amphiphile mit basischen P-Atomen (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 275-279 
    Details
    ISSN: 0009-2940
    Keywords: Aminoalkylphosphanes ; N-Quaternisation ; P-Alkylation ; Cationic tertiary phosphanes ; Amphiphiles ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Water-Soluble Phosphanes, IV. - Tertiary Alkylphosphanes with Ammonium Groups in the Side Chains  -  Amphiphiles with Basic P-AtomsBy stepwise aminoalkylation of PH3 with Me2N—(CH2)2—Cl in the superbasic medium DMSO/KOH the secondary phosphane [Me2N—(CH2)2]2PH (2) is obtained in good yields. Metallation of 2 with n-BuLi and subsequent reaction with Me2N—(CH2)2]2Cl affords the basic tertiary phosphane [Me2N—(CH2)2]2]3P (3), which on protonation with Ph3P · HBr in CH2Cl2 gives {[HNMe2 - (CH2)2]3P}3+ 3 Br- (4a) with an extremely high solubility in water. By oxidation of 3 with H2O2 and N-quaternisation with Me3O+ BF-4 the cationic phosphane oxide {[Me3N—(CH2)2]3P=O}3+ 3 BF-4 (5a) is formed, which could, however, not be reduced with SiHCl3 or Si2Cl6/NEt3 to the corresponding tricationic phosphane. Tertiary cationic phosphanes of type [RMe2N—(CH2)2—P(Oct)2]+ X- (8a, 8b, R = Me, C8H17; X = Br, I) are accessible by free radical addition of 1-octene to 7b and 7d. Addition of formaldehyde to 7a gives the hydroxymethyl phosphane 10a. By methylation of [RMe2N—(CH2)2—PH2]+I- (7d and 7e, R = CnH2n+1, n = 8, 12) with Mel under controlled condition and subsequent deprotonation of the phosphonium salts 12b and 12c the cationic tertiary phosphanes 13a and 13b with long alkyl side chains may be obtained in good yields.
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    Fe(NCMe)2+3-Komplexe von chiralen Tripodliganden mit drei verschiedenen Donorgruppen: Dynamik und StrukturHerrn Prof. Dr. Herrmann Schildknecht gewidmet. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 293-301 
    Details
    ISSN: 0009-2940
    Keywords: Tripodal ligands, chiral ; Iron tris(acetonitrile) tripod complexes ; Chiral triphosphanes ; Conformational analysis ; Ligand exchange ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Fe(NCMe)2+3 Complexes of Chiral Tripod Ligands Bearing three Different Donor Groups: Dynamics and StructureChiral tripod ligands [tripod = CH3C(CH2PR2)(CH2PR′2)(CH2-PR′′2), 1a-d] with three different donor groups react with Fe(NCMe)6(BF4)2 to yield the complexes tripodFe(NCMe)3(BF4)2 (2a-d). These complexes show an idealized octahedral coordination based on a facial coordination of the tripod ligand. The asymmetry of the chiral tripod ligands a-d induces a differentiation of the remaining coordination sites at iron. The structure and the dynamic behaviour of the compounds 2a, b is elucidated by X-ray structural analyses and 2D-NMR techniques.
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    URL: http://dx.doi.org/10.1002/cber.19951280314
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    Masthead (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995) 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951280401
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    Synthesis and Application of Ring-Substituted Analogues of the [4-(η-Cyclopentadienylidene)-4,7,7-trimethyl-4,5,6,7-tetrahydro-η5-indenyl]-ZrCl2 Ansa-Metallocene System (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 357-364 
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    ISSN: 0009-2940
    Keywords: Ansa-metallocene ; Ziegler catalyst, homogeneous ; Propene polymerization ; Fulvenes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Reaction of the 2,5-hexanedione-derived bisfulvene 1 with R—Li reagents (R = phenyl or n-butyl) yields the ring-closed [4-(cyclopentadienylidene)-7-R-4,7-dimethyl-4,5,6,7-tetrahydroindenyl]dilithium reagents 3. Their reaction with MCl4 (M = Ti, Zr, Hf) gives the corresponding ansa-group-4-metallocene dichloride complexes 4, 6, or 7. In a similar way the [7-allyl-4-(η-cyclopentadienylidene)-4,7-dimethyl-4,5,6,7-tetrahydro-η5-indenyl]metal dihalides (M = Ti, Zr) (6d, 4d) are prepared. Two diastereomers are formed in most cases, some of which could be separated. The five representative examples cis- and trans-4c, trans-4d, cis-6c, and trans-7c of these complexes were characterized by X-ray diffraction. All these six-membered ring-annulated C1-bridged ansa-metallocene dichlorides exhibit extremely small D1—Zr—D2 angles (D1 and D2 denote the centroids of the cyclopentadienyl rings) of 116.5°, i.e., they are characterized by a very open bite of the bent metallocene wedge. The homogeneous Ziegler-type catalysts derived from these ansa-zirconocenes by activation with methylalumoxane have high activities and all produce low-molecular mass atactic polypropylenes or propene oligomers.
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    Ionenpaarbildung und Cyclisierungsreaktionen an koordinierten Oxalamidinen (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 405-412 
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    ISSN: 0009-2940
    Keywords: Sodium oxalamidinates ; 2-Imidazolidinone ; Ionic molybdenum carbonyl complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Ion Pairing and Cyclization on Coordinatively Bound OxalamidinesThe tetraphenyloxalamidine ligand of complex 8a reacts easily in the presence of bases with elementorganic dichlorides (R2MCl2) to form coordinated metalacycles. The cyclization with phosgene gives the (CO)4Mo-coordinated 1,3-diphenyl-4,5-bis(phenylimino)-2-imidazolidinones 10. In contrast to the reaction forming the piperazine derivative 2, the reaction of 8a with oxalyl chloride also proceeds to 10 by decarbonylation. The product of this cyclization, (CO)4Mo(OCTPOA) (10), and two possible intermediates, the dinuclear sodium salts Na2(THF)8[(CO)4Mo(HTPOA)]2 (11a) and Na(THF)4[(CO)4Mo(EtO2COCTTOA)]2 (15) have been characterized by X-ray analyses. 11a contains the coordinated oxalaminate anion. The structure of the ionic complex 15 shows the simultaneous attack at both sp3-hybridized nitrogen atoms and the selective formation of the five-membered 2-imidazolidinone heterocycle by coordination of the oxalamidine. Both sodium complexes 11a and 15 are dimeric and centrosymmetric ion pairs. Complex 11a contains two C≡O—Na—O≡C bridges while compound 15 has a central [Na2O2] four-membered ring consisting of sodium alcoholate bridges.
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    Syntheses of Cyclic and Acyclic Bis(perfluoroalkylthio)nitronium Salts (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 429-433 
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    ISSN: 0009-2940
    Keywords: Nitronium ions ; One-electron oxidation ; Superacidic systems ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: (F3CS)3N (1) is oxidized quantitatively by AsF5 to the first bis(perfluoroalkylthio)nitronium salt (F3CS)2N+AsF-6 (2). Addition of halide ions (F-, Cl-, Br-, l-) to the cation of 2 destroys the S—N—S chain. (F2CSCl)2 undergoes with ammonia a cyclization reaction to S—CF2—CF2—S—N—H (3), which can be derivatized with F3CSCl or (F2CSCl)2 to S—CF2—CF2—S—N—SCF3 (3a) and (S—CF2—CF2—S—N—SCF2—)2 (3b), respectively. Oxidation of 3a with AsF5 yields (S—CF2—CF2—S—N+AsF-6 (4) and byproducts, which suggest formation of a {3a}+• radical cation as an intermediate in this reaction. Pure 4 is accessible by reaction of 3 with AsF5 in 54% yield. The chemical and spectroscopic properties of the new species are discussed.
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    Masthead (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995) 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951280501
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    Structure and Conformation of Bis(trifluoromethylthio)methane, CH2(SCF3)2 (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 461-464 
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    ISSN: 0009-2940
    Keywords: Bis(trifluoromethylthio)methane ; Gas-phase structure ; Conformational properties ; Electron diffraction ; Calculations, ab initio ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The geometric structure and conformational properties of bis(trifluoromethylthio)methane, CH2(SCF3)2' were determined by gas electron diffraction. The main conformer (70 ± 15%) possesses C2 symmetry with dihedral angles Φ(SCSC) = 79.1(10)°. The second conformer possesses C1 symmetry. The following skeletal geometric parameters (distances ra [pm] and angles 〈α[°] with 3-σ uncertainties) were obtained: C—S 183.6(3), S—CF3, 179.3(3), S—C—S 112.1(6), and C—S—C 98.2(10). The geometric structures and relative conformational stabilities were well reproduced by ab initio calculations at the HF/3-21G* level.
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    Pyridyl-Functionalised Cyclopentadienyl Ligands: Building Blocks for Oligonuclear Organometallic Assemblies (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 481-485 
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    ISSN: 0009-2940
    Keywords: Cyclopentadienyl ligands, functionalised ; Hemilabile ligands ; Cyclopentadienes, pyridyl-functionalised ; Ferrocenes, pyridyl-functionalised ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Lithiated 2-methylpyridine reacts with 2,3,4,5-tetramethylfulvene (TMF) to give 2-[2-(2,3,4,5-tetramethylcyclopenta-1,4-dien-1-yl)ethyl]pyridine (2H) after aqueous work-up. Similarly, a mixture of 2-methyl-6-[2-(2,3,4,5-tetramethylcyclopenta-1,4-dien-1-yl)ethyl]pyridine (3H) and 2,6-bis[2-(2,3,4,5-tetramethylcyclopenta-1,4-dien-1-yl)ethyl]pyridine (4H2) was obtained from monolithiated 2,6-dimethylpyridine and TMF. All three compounds were obtained as a roughly statistical mixture of double-bond isomers. 2-Lithiopyridine reacts with 2,3,4,5-tetramethylcyclopent-2-enone to yield 2-(2,3,4,5-tetramethylcyclopenta-1,3-dien-1-yl)pyridine (5H) after acidic work-up. This compound was obtained as a non-statistical mixture of double-bond isomers, which is presumably due to intramolecular hydrogen-bond interactions. The lithiated derivatives 2Li, 3Li and 5Li react with iron(II) chloride to afford the respective ferrocenes (2)2Fe (8), (3)2Fe (9) and (5)2Fe (10). The structure of 10 was determined by a single-crystal X-ray diffraction study. The cyclopentadienyl ligands adopt a staggered conformation; the pyridyl rings are arranged in a stacked fashion with the closest ring-ring contact being 3.16 Å. The distance between the iron atom and the cyclopentadienyl ring centroids is 1.66 Å.
    Additional Material: 3 Ill.
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    Tin for Organic Synthesis, 12. Synthesis of Aromatic and Olefinic Sodium Sulfonates by Electrophilic Destannylation with Trimethylsilyl Chlorosulfonate (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 575-580 
    Details
    ISSN: 0009-2940
    Keywords: Electrophilic aromatic substitution ; Electrophilic vinylic substitution ; Trialkylstannanes, application of ; Arylsulfonates, sodium salts of ; Vinylsulfonates, sodium salts of ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A mild and effective method for the preparation of a variety of aromatic, olefinic, and acetylenic sodium sulfonates is described. The reaction of trialkylaryl- (2a-k) and -heteroarylstannanes (4a-d), bis-(1-alkenyl)dibutylstannanes (6a-f), or trialkylalkynylsta manes with trimethylsilyl chlorosulfonate (1) followed by hydrolysis with aqueous NaHCO3 provides the sodium sulfonates in an ipso-specific and in the case of vinylic stannanes stereospecific manner. A comparison of the reactivity of stannylated and silylated olefinic compounds 13 and 14 underlines the greater leaving ability of the stannyl moiety. The in situ preparation of the stannanes makes it possible to apply the synthetic method to natural products such as N-substituted apocodeine (17).
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    URL: http://dx.doi.org/10.1002/cber.19951280609
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    On the Regioselectivity and Stereoselectivity of the Carbene Transfer from Fischer Carbene Complexes to Trisubstituted Electron-Deficient 1,3-DienesDedicated to Professor Rolf Huisgen on the occasion of his 75th birthday. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 605-614 
    Details
    ISSN: 0009-2940
    Keywords: Chromium complexes ; Carbene complexes ; 1,3-Dienes, electron-deficient ; [2 + 1] Cycloadditions ; Vinylcyclopropanes, donor-acceptor-substituted ; Diastereoselectivity ; Regioselectivity ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Thermal reactions of Fischer carbene complex 1 with trisubstituted electron-deficient 1,3-dienes 7, 8, 23, 25, 32, and 35 provided highly substituted vinylcyclopropanes in good yields. The carbene transfer proceeds highly regioselectively favouring cyclopropanation of the double bond not bearing the ester function. In addition, the diastereoselectivity is generally fairly high in preference of cyclopropanes with the methoxy group cis-positioned with respect to the olefin moiety. The reaction of methylcarbene complex 2 with diene ester 8 displays inversed regioselectivity. These observations are discussed together with solvent effects, and a mechanistic rationale is presented.
    Additional Material: 5 Tab.
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    URL: http://dx.doi.org/10.1002/cber.19951280613
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  • 77
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    Synthesis and Characterization of Copper, Nickel and Cobalt Complexes of N,N′-Dimethyl-2,11-diaza[3,3](2,6)pyridinophane (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 531-539 
    Details
    ISSN: 0009-2940
    Keywords: 2,11-Diaza[3,3](2,6)pyridinophane ; N,N′-dimethyl- ; Tetraazamacrocyclic complexes ; cis-Octahedral coordination geometry ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The properties of the tetraazamacrocyclic compound N,N′-dimethyl-2,11-diaza[3,3](2,6)pyridinophane (L-N4Me2) as a ligand for some selected metal chlorides have been examined. The crystal structure of the uncoordinated ligand reveals a syn chair-chair conformation. In solution, the ligand displays fluctional behavior. Reaction of L-N4Me2 with the chlorides of copper(II), nickel(II), and cobalt(II) affords the complexes [Cu(L-N4Me2)Cl2] · H2O (3), [Ni(L-N4Me2)(H2O)Cl]Cl · H2O (4), and [Co(L-N4Me2)Cl2] · 2 H2O (5) in which the ligand adopts a syn boat-boat conformation. The crystal structures of 4 and 5 are presented. Due to the small cavity of the 12-membered ring of the ligand, exclusively distorted cis-octahedral coordination geometries are found at the metal sites. A comparison of structural data of several complexes with this ligand shows that the extent of the distortions from ideal octahedral geometry is mainly determined by the M-Npy bond strength. The electronic as well as the solution properties of the described complexes have been investigated by electronic absorption spectroscopy. ESR spectroscopy, and electrochemical methods.
    Additional Material: 6 Ill.
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  • 78
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    Synthesis and Crystal and Molecular Structure of Tris(dimethylphenylsilyl)antimony (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 565-567 
    Details
    ISSN: 0009-2940
    Keywords: Antimony, tris(dimethylphenylsilyl)- ; Antimony, trisilyl- ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Tris(dimethylphenylsilyl)antimony (1) was prepared in moderate yield from dimetallic “Na3Sb” (generated in situ) and chlorodimethylphenylsilane in tetrahydrofuran at reflux temperature. The product was identified by standard analytical and spectroscopic techniques, and the crystal structure was determined by single-crystal X-ray diffraction (triclinic, space group P1, Z = 2). The SbSi3 skeleton is pyramidal (average Si-Sb-Si angle 100.2°, average Sb-Si bond length 2.558 Å), and the Me2PhSi groups are in a staggered conformation.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19951280607
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    Chirotopic and Stereogenic Metal Centers in [M(L)(L')(‘RS4’)] Complexes with Chiral Thioether-Thiolate Ligands ‘RS4’-H2 [‘MeS4’2- = 1,2-bis(2-mercaptophenylthio)propanato(2-), ‘CH3(CH2)2S4’2- = 1,2-bis(2-mercaptophenylthio)pentanato(2-), ‘HO(CH2)9S4’2-10 (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 653-663 
    Details
    ISSN: 0009-2940
    Keywords: Chirality ; Stereogenicity ; Diastereoselectivity ; Ligand stereospecificity ; Metal sulfur complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: In order to investigate the stereochemistry of substitution reactions of chiral pseudo-octahedral complexes the chiral thioether-thiolate ligands ‘RS4’-H2 (= HSC6H4SCHRCH2-SC6H4SH) with R = CH3- (5), CH3(CH2)2- (6), HO(CH2)9- (7), and PhCH2- (8) were synthesized by template alkylation of Na2[Ni(‘S2’)2] [‘S2’2- = 1,2-benzenedithiolate(2-)] with 1,2-dibromoalkanes BrCHRCH2Br (R = CH3-, 1; R = CH3(CH2)2-, 2; R = HO(CH2)9-, 3; R = PhCH2-, 4) and isolated after hydrolyses. Reactions of ‘RS4’-H2 with [RuCl2(PPh3)3] or [Mo(O)2(acac)2] yielded [Ru(PPh3)2(‘RS4’)] (R = CH3-, 9; R = HO(CH2)9-, 10; R = PhCH2-, 11) and [Mo(O)2(‘MeS4’)] (12). [Ru(PPh3)2(‘MeS4’)] · 2 CH2Cl2 (9 · 2 CH2Cl2) and [Mo(O)2(‘MeS4’)] (12) were characterized by X-ray structure determination. In both complexes, the metal centers are surrounded pseudo-octahedrally by four sulfur donors of the ‘MeS4’ ligand and two cis coligands. The methyl substituent at the stereogenic C* atom of the C2 bridge of the ‘MeS4’ ligands assumes an equatorial position. In addition, the metal centers of these complexes are chirotopic and prostereogenic. Crystal data of 9 · 2 CH2Cl2 in comparison with [Ru(PBu3)2(‘S4’) 11-bis(2-mercaptophenylthio)-1-undecanolato(2-), ‘PhCH2S4’2-1,2-bis(2-mercaptophenylthio)-3-phenylpropanato(2-)] ] and those of 12 in comparison with [Mo(O)2(‘S4’)] show that distances and angles of the coordination cores are not influenced by the substituents on the C2 bridge. Reactions of the [Ru(PPh3)2(‘RS4’)] complexes (9-11) with the achiral substrates CO and PMe3, however, yielded diastereomers of [Ru(PPh3)(L)(‘RS4’)] (L = CO, R = CH3-, 13; L = CO, R = HO(CH2)9-, 14; L = CO, R = PhCH2-, 15; L = PMe3, R = CH3-, 16; L = PM R = HO(CH2)9-, 17; L = PMe3, R = PhCH2-, 18) in diastereomeric excesses between 60 and 82%. The diastereomer of [Ru(PPh3)CO)(‘MeS4’)] (13) which could be characterized by X-ray structure determination exhibits the CO ligand in trans position to the thioether donor which is bound to the stereogenic C* atom of the C2 bridge. Reaction of 9 · 2 CH2Cl2 with the optically pure bidentate diphosphine (+)-(S,S)-DIOP [= (+)-2,3-O-isopropylidene-2,3-dihydroxy-1,4-bis(diphenylphosphino)butane] yielded 1:1 mixtures of two diastereomers of [Ru(DIOP)(‘MeS4’)] (19) one of which was separated in pure form by HPLC.
    Additional Material: 5 Ill.
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    A Deceiving X-ray Single-Crystal Structure Determination: Amino-Hydrogen Exchange in Amino-alkynylboranes and ab initio Investigations of Alkynylboranes, Borirenes, and Boraallenes (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 711-717 
    Details
    ISSN: 0009-2940
    Keywords: Alkynylboranes ; Borirenes ; Boraallenes ; Calculations, ab initio ; Hydroboration ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Dimeric(dimethylamino)(phenylethynyl)borane (2)2 is formed by the reaction of bis(dimethylamino)(phenylethynyl)-borane (1) with 9-BBN-H. An X-ray single-crystal diffraction study revealed a central B2N2 four-membered ring for (2)2 with both alkynyl groups pointing to the same side in a cisoid arrangement. However, solution and solid-state NMR as well as ab initio calculations on model compounds show that the cis arrangement in the crystal chosen for X-ray diffraction is not representative of the bulk material, which consists of both cis and trans isomers. Further investigations of the competition between hydrogen-amino group exchange and hydroboration in the reaction of amino-alkynylboranes with hydroborating agents (9-BBN-H and catB-H) show the exchange to be much faster even in the presence of Wilkinson's catalyst and with cyclic amino-alkynylboranes such as 1,3-dimethyl-2-[(trimethylsily1)ethynyl]-1,3,2-diazaborolidine (3). Ab initio calculations on alkynylboranes I, borirenes II, and boraallenes III, which are all geometrical isomers, show alkynylboranes to be the most stable isomers only if strongly π-donating groups X (X = NH2, F) are attached to the boron atom. In any case, boraallenes are highest in energy.
    Additional Material: 1 Ill.
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    A T-Shaped Selenenyl Halide: Synthesis and Characterisation of a Proposed Reaction Intermediate (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 741-742 
    Details
    ISSN: 0009-2940
    Keywords: Selenenyl halides ; Nucleophilic substitution ; Complex intermediate ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The T-shaped selenenyl halide (1), which may be regarded as a model substance for the transition state in nucleophilic displacement at divalent chalcogen atoms, has been isolated and subjected to X-ray structure determination.
    Additional Material: 1 Tab.
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    URL: http://dx.doi.org/10.1002/cber.19951280715
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    Masthead (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995) 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951280801
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    Synthesis of 2- and 3-Stannolenes via Addition of Trimethyltin Alkoxides to 3-Diethylboryl-4-ethyl-1,1-dimethylstannole (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 679-687 
    Details
    ISSN: 0009-2940
    Keywords: Stannole, diethylboryl-substituted ; Trimethyltin alkoxides ; 2-, 3-Stannolenes, organometallic-substituted ; NMR, coupling constants, 2J(Sn,Sn), sign determination ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Trimethyltin alkoxides (2) react stereoselectively with 3-diethylboryl-4-ethyl-1,1-dimethylstannole (1) via addition of the Me3Sn group to C(2) to the C(2) = C(3) bond and a 1,2 shift of an ethyl group from boron to C(3) to give the 2-stannolenes 3. The molecular structure of 3f' [R = (S)-2-Bu] was determined by single-crystal X-ray analysis, confirming the cis positions of the Et(RO)B and the Me3Sn group. These 2-stannolenes 3 undergo, upon heating to ca. 80°C, facile rearrangement by irreversible allylic migration of the Et(RO)B group to the 3-stannolenes 4 in which the cis positions of the boryl and the stannyl group are retained. All 2-stannolenes (in contrast to the 3-stannolenes) are readily deprotoborylated to give the 3-stannolene 5. The structures of 3, 4, and 5 follow conclusively from 1H-, 11B-, 13C-, and 119Sn-NMR spectra. The negative sign of the geminal coupling constants 2J(SnSn) was determined in the case of 3, 4, and 5 by 2D 119Sn/1H heteronuclear shift correlations.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19951280705
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    A New Synthesis of P-Substituted 2,3-Dihydro-1,3-dimethyl-1,3,2δ3-benzodiazaphosphorin-4(1H)-ones and Alkylaminodifluorophosphanes with Chlorodifluorophosphane.  -  Synthesis and Structure of {cis-Bis[bis(2-chloroethyl)aminodifluorophosphane]dichloro}platinum(II)Dedicated to Professor Wilhelm Preetz on the occasion of his 60th birthday. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 695-701 
    Details
    ISSN: 0009-2940
    Keywords: 2,3-Dihydro-1,3-dimethyl-1,3,2-benzodiazaphosphorin-4-(1H)-ones, 2-trimethylsiloxy-, 2-oxo-, and 2-fluoro-substituted ; Equilibrium reaction ; Aminodifluorophosphanes ; Platinum complex ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 2,3-Dihydro-1,3-dimethyl-2-oxo-1,3,2δ4-benzodiazaphosphorin-4(1H)-one 1 reacted with diethylaminotrimethylsilane to give solely the 2-trimethylsiloxy-δ3-diazaphosphorinone 2. The reaction of 2 with the 2-chloro-δ3-diazaphosphorinone 3 yielded the P - O - P-bridged compound 4 in an equilibrium reaction with elimination of trimethylchlorosilane. The synthesis of the P-difluorophosphite-substituted δ3-benzodiaza-phosphorinone 6 was effected by the reaction of chlorodifluorophosphane (5) with 1 in the presence of triethylamine in a 1:1 molar ratio, or in the reaction of 5 with 2 or 4. The reaction of 5 with 6 led, with elimination of μ-oxo-bis(difluoro-phosphane), to the P(III)Cl species 3, 5 reacted with N,N'-dimethylanthranilamide in the presence of triethylamine in a 2:1:2 molar ratio to give the N,N'-bis(difluorophosphane) derivative 9, as evidenced by low temperature (-30°C) 19F-and 31P-NMR data. At room temperature the 2-fluoro-δ3-diazaphosphorinone 10 was formed from 9 with intramolecular elimination of phosphorus trifluoride. 2-Chloroethyl- or bis(2-chloroethyl)aminodifluorophosphane 11 and 12 were obtained in the reaction of 5 with 2-chloroethyl- or bis(2-chloroethyl)amine hydrochloride in the presence of triethylamine in a 1:1:2 molar ratio. 12 reacted with (COD)PtCl2 (COD = 1,5-cyclooctadiene) in a 2:1 molar ratio to give the {cis-bis[bis(2-chloroethyl)aminodifluorophosphane]dichloro}platinum(II) complex 13. The characterization of 2, 4, 6, and 11-13 is based on their NMR and mass spectra. The structures of 10 and 13 were established by single-crystal X-ray analysis. 10 crystallizes with two independent molecules. Both six-membered heterocycles display an envelope conformation with the phosphorus atoms 36.9 and 50.4 pm, respectively, out of the plane. The phosphorus atoms have pyramidal coordination geometry. The cis-configuration at platinum(II) in the complex 13 was confirmed; two ligands (12) are coordinated to PtII via phosphorus. The platinum atom has a distorted square-planar coordination geometry.
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    Mo(CO)2(PPh3)2(O3SCF3)2: Ein neuer Vorläufer einer dikationischen, metallorganischen Lewis-Säure mit drei freien Koordinationsstellen (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 729-734 
    Details
    ISSN: 0009-2940
    Keywords: Lewis acids, organometallic ; 12-e- Systems ; Alkyne complexes ; Molybdenum complexes ; Tungsten complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Organometallic Lewis Acids, LIV.  -  Mo(CO)2(PPh3)2(O3SCF3)2: A New Precursor for an Organometallic Dicationic Lewis Acid with Three Accessible Coordination SitesThe reaction of Mo(CO)2(PPh3)2Br2 (1) with AgO3SCF3 gives the bis(triflate) complex Mo(CO)2(PPh3)2(O3SCF3)2 (3) which can be considered as a precursor for the 12-e- system “Mo-(CO)2(PPh3)2+2”. According to the spectroscopic data one of the two coordinated CF3SO-3 anions is acting as a chelate ligand. Treatment of 3 and of the in situ generated W(CO)2(PPh3)2(O3SCF3)2 (4) with H2O affords the dinuclear hydroxo-bridged complexes [M2(μ-OH)3(CO)4(PPh3)4][CF3SO3] (5: M = Mo; 6: M = W). Acetonitrile replaces the CF3SO-3 ligands in 3 and 4 to afford the cationic complexes [M(CO)2(PPh3)2(NCMe)3][CF3SO3]2 (7: M = Mo; 8: M = W). The reaction of 3 with an excess of 2-butyne and 1-phenyl-1-propyne leads to the monoalkyne complexes Mo(CO)(MeC≡CR)(PPh3)2(O3SCF3)2 (9: R = Me; 10: R = Ph) in moderate yield. In contrast, the bisalkyne complexes [M(CO)(MeC≡CMe)2(PPh3)2(O3SCF3)][CF3SO3] (11: M = Mo; 12: M = W) are formed in high yield when a CH2Cl2 solution of 2-butyne is added to 1 and 2 in the presence of AgO3SCF3. At room temperature, 11 and 12 are highly fluxional in solution, while 9 and 10 are stereochemically rigid. Treatment of 11 with acetonitrile yields [Mo(CO)(MeC≡CMe)2(PPh3)2(NCMe)][CF3SO3]2 (13). Compounds 3-13 (except 4) are characterized by IR, 1H-, 13C-, 19F-, and 31P-NMR spectrescopy.
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    URL: http://dx.doi.org/10.1002/cber.19951280712
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    Chalcogen Polycations with Mononuclear Divalent Anions from Chalcogen Subhalides and Tetrachlorides of Zr and Hf: Syntheses and Crystal Structures of Se4(MCl6) (M = Zr, Hf) and Te4(HfCl6) (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 763-766 
    Details
    ISSN: 0009-2940
    Keywords: cyclo-Tetraselenium(2+) ; cyclo-Tetratellurium(2+) ; Hexachlorozirconate(IV) ; Hexachlorohafnate(IV) ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Selenium, SeCl4, and MCl4 (M = Zr, Hf) react in a sealed evacuated glass ampoule at 130°C to afford red, moisture sensitive crystals of Se2+4(ZrCl2-6) and Se2-6(HfCl2-6). The isotypic crystal structures (tetragonal, P42/ncm, Z = 4) consist of square-planar Se2+4 cations and slightly distorted octahedral MCl2-6 (M = Zr, Hf) anions. The ions are packed corresponding to the NaCl structure type with the centres of gravity of the Se4 rings and the metal atoms of the MCl6 octahedra in the Na and Cl positions. From Te, TeCl4, and HfCl4 one obtains under similar conditions at 200°C Te2+4 (HfCl2-6) in form of dark violet crystals. The crystal structure (triclinic, P1, Z = 1) is built of nearly square-planar Te2+4 ions and octahedral HfCl2-6 ions. The packing of the ions corresponds to a rhombohedrally distorted CsCl structure type.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19951280804
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    Electronic Structure of Planar-Tricoordinated Phosphorus in Titanium-Boron Complexes (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 775-778 
    Details
    ISSN: 0009-2940
    Keywords: Phosphorus, planar-tricoordinated ; Calculations, RHF, MP2 ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The electronic structure of the recently synthesized complex 5 obtained by the reaction of Cp2Ti(PMe3)(tBu-CP) with (Et2BH)2 was analyzed by means of molecular orbital (MO) calculations. The methods applied were the extended Hückel and the ab initio Hartree-Fock procedures. The highest occupied MOs were derived from molecular fragments. The geometrical parameters calculated for a simplified model (6) are close to those obtained from an X-ray investigation of 5. The analysis of the results shows a strong donor-acceptor interaction between the P-B ó bond and the Ti center. The phosphorus lone pair is not involved in bonding.
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    URL: http://dx.doi.org/10.1002/cber.19951280806
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    Locating the Position of Lithium in Solution by Combined 13C,6Li and 1H,6Li HOESY Measurements (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 799-802 
    Details
    ISSN: 0009-2940
    Keywords: 13C,6Li HOESY ; 1H,6Li HOESY ; Organolithium compounds ; Distance determination ; Spin lattice relaxation ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 13C,6Li HOESY Measurements were developed and performed for the first time on the 13C-labeled benzyllithium compound 1. 1D NOE difference, 1H,6Li HOESY, and spin lattice relaxation measurements were used to obtain information on the position of the lithium, ion in solution.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19951280810
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    Synthesis and Structures of Magnesium TetrahydridoaluminatesDedicated to Dr. R. Bauer, who first synthesized magnesium tetrahydridoaluminate, on the occasion of his 70th birthday. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 999-1006 
    Details
    ISSN: 0009-2940
    Keywords: Magnesium tetrahydridoaluminate ; Magnesium halide tetrahydridoaluminate ; (Organyloxo)magnesium tetrahydridoaluminates ; X-ray structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The molecular structures of XMg(A1H4) · 4 THF (1a, 2, 3a) (X = A1H4, Cl, Br) have been determined by X-ray structural analysis. Each compound possesses a hexacoordinated Mg center and AlH4- groups bound to this center via a single hydride bridge bond. Attempts to prepare ROMg(AlH4) compounds were successful only for sterically demanding groups R (R = CMe3, CPh3, naph, mes, smes). The 2-naphthoxy derivative 7, a compound with the composition (naphO)Mg-(AlH4) · 2.5 THF, is a dimer with a central Mg2O2 ring. One of its two AlH4- groups is terminally bound to one Mg atom, the other bridges the two Mg centers. This structure indicates how AlH4- transfer may occur from ROMg(AlH4) compounds to form Mg(OR)2 and Mg(AlH4)2.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19951281007
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    Ylidyl 1,2,4-Thiadiphosphetane and 1,2,4-Selenadiphosphetane Sulfides and Selenides (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1015-1020 
    Details
    ISSN: 0009-2940
    Keywords: 1,2,4-Thiadiphosphetanes ; 1,2,4-Selenadiphosphetanes ; Thioxophosphanes ; Selenoxophosphanes ; Ylides ; Phosphane elimination ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Phosphoniumylidyl thioxophosphanes and selenoxophosphanes, the only known monomeric chalcogenoxophosphanes, react in a 2:1 ratio with triphenylphosphonium ylides. With loss of PPh3 the 1,2,4-thia(or selena)diphosphetane monosulfides (or selenides) are formed. Their prominent structural feature are the very different PS bond lengths in the ring. They can be oxidized to the corresponding disulfides or sulfide selenides. The latter rearrange to the isomer in which the selenium atom has become a ring member.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19951281009
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    Polare Iminoborane: Reaktionen des (tert-Butylimino)(pentafluorphenyl)borans (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1037-1043 
    Details
    ISSN: 0009-2940
    Keywords: Iminoborane ; Triazadiboracyclohexane ; Borazine ; Diazadiboracyclobutane ; Azaboracyclobutane ; Diazadiboracyclopentane ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Polar Iminoboranes: Reactions of (tert-Butylimino)(pentafluorophenyl)boraneThe reactions of the iminoborane C6F5-B≡N-tBu (1) with nitriles and isonitriles are studied. Nitriles RCN give cycloadducts either of the triazadiboracyclohexane type (3a; R = iPr) or of the tetrazatriborabicyclo[4.2.0]octane type [4b-d; R = Ph, p-C6H4Me, p-C6H4(CF3)] or of the (iminomethyl)borazine type (5e, f; R = Me, Et). Isonitriles RNC yield mainly adducts of RNC to a cycloaddition product of the diazadiboracyclopentane type (6a, b; R = 2,6-C6H3Me2, tBu); the adduct of RNC to a diazadiboracyclobutane may be a side-product (7b; R = tBu). The iminoborane Me3Si(tBu)N-B=NtBu reacts with two molecules of (2,6-C6H3Me2)NC to give the corresponding azaboracyclobutane 8. The iminoborane tBu-B≡N-C6F5 (1′), formed by gas-phase elimination of ClSiMe3 from Cl(tBu)B = N(C6F5)SiMe3 (9), cyclodimerizes more readily than the isomeric borane 1. The cyclodimer 2′ gives 1:1-addition reactions with tBuNC, PMe3, and MeNC, respectively; the added components fluctuate in solutions of the products 7b'-d'. A similar fluctuation is observed with the 1:1 adduct 7c from PMe3 and the cyclodimer 2 of the iminoborane 1. The products 3a, 5e, 6a, 8 crystallize in the space groups P21/c, P21/n, Pbca, and P21/c, respectively.
    Additional Material: 3 Ill.
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    Addition von Hydrofullerid [C60H]- an koordinierte, ungesättigte Kohlenwasserstoffe: Bindung von Fulleren an Metallkomplexe über KohlenwasserstoffbrückenHerrn Professor Herbert Walter Roesky zum 60. Geburtstag gewidmet (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1059-1060 
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    ISSN: 0009-2940
    Keywords: Fullerene ; Hydrofulleride ; Manganese complex ; Rhenium complex ; Iron complexes ; Ruthenium complex ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Addition of Hydrofulleride [C60H]- to Coordinated, Unsaturated Hydrocarbons: Binding of Fullerene to Metal Complexes through Hydrocarbon BridgesHerrn Professor Herbert Walter Roesky zum 60. Geburtstag gewidmet.Hydrofulleride [C60H]- is added to the hydrocarbon ligands of the cationic complexes [(OC)5Re(η2-C2H4)]+, [(OC)3Mn-(η6-C6H6)]+, [(OC)3M(η5-C6H7)]+ (M = Fe, Ru), [(OC)3Fe(η5-C7H9)]+, and [(η5-C5H5)Fe(η6-C5H4CH2)]+.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951281017
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    Controlled Conversion of the Transient 2-Mesityl-1,1-bis(trimethylsilyl)silene into a Tetrahydro-2,3-disilanaphthalene, a 1,2-Disilacyclobutane, or a 1,3-Disilacyclobutane (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1083-1088 
    Details
    ISSN: 0009-2940
    Keywords: Silenes ; Silene dimerization ; 1,2-Disilacyclobutanes ; 1,3-Disilacyclobutanes ; 2,3-Disilanaphthalene, tetrahydro- ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Mesityl[tris(trimethylsilyl)silyl]methanol (1) reacts with strong bases with elimination of trimethylsilanolate according to a Peterson-type mechanism, the outcome of the reaction being dependent on solvent, temperature, and nature of the organometallic base applied. Thus, 1 was converted by treatment with MeLi in ether at -78°C to (E)-1,2,3,8a-tetra -hydro-1-mesityl-5,7,8a-trimethyl-2,2,3,3-tetrakis (trimethylsi-lyl)-2,3-disilanaphthalene (3), formally a [2 + 4] cyclodimer of the transient silene (Me3Si)2Si=CHMes (2). The reaction of 1 with PhMgBr in THF after some days resulted in the formation of (Z)-3,4-dimesityl-1,1,2,2-tetrakis(trimethylsilyl) -1,2-disilacyclobutane (6) as the main product besides small quantities of 3, the polysilane (Me3SiSi(SiMe3)2CH2Mes (10), and the alkoxysilane (Me3Si)3SiCH(Mes)OSi(Si-Me3)2CH2Mes (7). Compound 6, the formal [2 + 2] cycloadduct of 2, can also be obtained by thermal treatment of 3 and is considered to be the thermodynamically more stable silene dimer whereas 3 is the kinetically preferred product. At high LiBr concentrations in the reaction mixture 1 was converted by PhMgBr in THF to (E)-2,4-dimesityl-1,1,3,3-tetrakis(tri- methylsilyl)-1,3-disilacyclobutane (13) besides 6 and [bis(tri-methylsilyl)silyl]mesityl(trimethylsiloxy)methane (11). The unforeseen formation of 13 is discussed as proceeding via the silene-lithium bromide adduct (Me3Si)2Si(Br)CH(Li)Mes (12). In the absence of LiBr 1 was converted by MeLi in THF at -78°C to 11 and the trisilane (Me3Si)2Si(Me)CH2Mes (4b). Probable pathways of the formation of all new compounds are discussed. For 6 and 13 the results of the X-ray structural analyses are given.
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    URL: http://dx.doi.org/10.1002/cber.19951281105
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    Metallkomplexe mit biologisch wichtigen Lisganden, LXXXLXXIX. Mitteilung: Lit.. (η3:η3-C10H16)Ru(IV)-Komplexe mit α-Aminocarboxylaten, α-Aminosäureestern und Peptidestern als Liganden (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1117-1125 
    Details
    ISSN: 0009-2940
    Keywords: 1,7-Dimethylocta-2,6-diene-1,8-diyl ; Ruthenium complexes ; α-Amino carboxylates ; α-Amino acid esters ; Peptide esters ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Metal Complexes Containing Biologically Important Ligands, LXXXLXXIX. Mitteilung: Lit. .  -  (η3:η3-C10H16)Ru(IV) Complexes with α-Amino Carboxylates, α-Amino Acid Esters, and Peptide Esters as LigandsReactions of the chloro-bridged bis(allyl) complex [(η3:η3-C10H16)Ru(Cl)(μ-Cl)]2 with α-amino carboxylates and α-amino acid esters afford the complexes (η3:η3-C10H16)(Cl)RuNH2CHRCO2 (2) and (η3:η3-C10H16)(Cl)2-RuNH2CHRCO2R′ (3). Abstraction of chloride from 3 by Ag+ gives the N,O-chelates [(η3:η3-C10H16)(Cl)RuNH2CHRCO2R′]+BF4 (4). Cysteine methyl ester forms the N,S-chelate complex (η3:η3-C10H16)(Cl)RuNH2CH(CO2CH3)CH2S (5), and with histidine methyl ester a dinuclear complex 6 with N,N-histidine bridge is obtained. Compound 3d with L-PheOEt as ligand was characterized by X-ray diffraction.
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    URL: http://dx.doi.org/10.1002/cber.19951281110
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    [MeO(CH2CH2O)3(CH2)3C5Me4]FeCl: A Halfsandwich Iron (II) Chloride Complex of Remarkable Stability (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1135-1136 
    Details
    ISSN: 0009-2940
    Keywords: Hemilabile ligands ; Cyclopentadienyl ligands, functionalised ; Iron compounds ; Halfsandwich complex ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Reaction of iron(II) chloride with one equivalent of [MeO-(CH2CH2O)3(CH2)3C5Me4]Li in THF yields the title halfsand-wich complex 1, which is stable in solution up to room temperature. Compound 1 reacts with C5H5Li and CO to give [MeO(CH2CH2O)3(CH2)3C5Me4]Fe(C5H5) (2) and [MeO-(CH2CH2O)3(CH2)3C5Me4]Fe(CO)2CI (3), respectively, in high yields.
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    URL: http://dx.doi.org/10.1002/cber.19951281113
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    [Cp4Fe4(E2)2] Clusters with Triangulated Dodecahedral Fe4E4 Skeletons (E = P, As)Dedicated to Professor Herbert Schumann on the occasion of his 60th birthday. (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1145-1148 
    Details
    ISSN: 0009-2940
    Keywords: P2, As2, P2S2, and P2Se2 ligands ; Iron complexes ; Triangulated dodecahedra ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The thermolysis of [CpFe(CO)2]2 (1) and P4 or As4 affords the iron clusters [Cp4Fe4(E2)2], E = As (2a), P (2b), the Fe4E4 skeleton of which consists of a triangulated dodecahedron. S8 and gray Se oxidize the P2 ligands of 2b with formation of [Cp4Fe4(P2X2)2], X = S (3a), Se (3b), complexes with the hitherto unknown P2X2 ligands, 2a, b and 3a, b have been characterized by X-ray crystallography.
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    URL: http://dx.doi.org/10.1002/cber.19951281202
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    LiClO4-Promoted Addition of Alkyl Grignard and Alkynyllithium Reagents to Ketones. Comparison of a 5 M LiClO4/Diethyl Ether Solution with CeCl3 (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1171-1174 
    Details
    ISSN: 0009-2940
    Keywords: Nucleophilic addition ; Lewis acid ; Enolizable ketones ; Alkyl Grignard ; Alkynyllithium reagent ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The influence of a 5 M ethereal LiClO4 solution as solvent on the addition of different alkyl Grignard and alkynyllithium reagents to highly enolizable ketones was studied. A comparison with the results in the presence of CeCl3 shows a similar improvement in the yield.
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    Thiaaza-arachno-pentaboran SNB3H2tBu3R (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1105-1108 
    Details
    ISSN: 0009-2940
    Keywords: Azadiboriridine, tri-tert-butyl- ; Mercaptoborane ; Thiaaza-arachno-pentaborane, 1,4,5-tri-tert-butyl-2-organo- ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Thiaaza-arachno-pentaborane SNB3H2tBu3RThe azadiboriridine [-B(tBu)-N(tBu)-B(tBu)-] (1) gives 1:1 adducts with the mercaptoboranes BH2(SR), which can be generated from their cyclotrimers by the action of THF. The adduct 4a (R = Ph), a nido cluster with an NB3 skeleton, forms an equilibrium with an adduct 5a, an arachno cluster with an SNB3 skeleton, whose S-bound ligand Ph is found in an endo position by an X-ray structural analysis. The equilibrium 4a · 5a involves a Lewis acid-base reaction, which is electronically coupled to a reduction of a three-center to give a two-center π bond. The reaction of 1 with BH2(SPr) gives the corresponding arachno cluster 5b only.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19951281108
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    Metallkomplexe mit biologisch wichtigen Lisganden, LXXXIPart LXXX: Ref.. Synthese und Kristallstruktur von Rh(I)-Komplexen mit α-Aminocarboxylat-Liganden (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 1127-1130 
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    ISSN: 0009-2940
    Keywords: Rhodium(I) ; α-Aminocarboxylate ; Crystal structure ; Hydrogen bonding ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Metal Complexes Containing Biologically Important Ligands, LXXXPart LXXX: Ref. .  -  Synthesis and Crystal Structure of Rhodium(I) Chelates with α-Amino Carboxylates Part LXXX: Ref.The α-amino carboxylate complexes were prepared from Rh(Cl)(CO)(PPh3)2 and H2NC(H)(R)CO2 in the presence of AgBF4 and characterized by X-ray diffraction. In the crystal the complexes form chains by hydrogen bridges between amino and carboxylate groups of adjacent molecules.
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    URL: http://dx.doi.org/10.1002/cber.19951281111
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    Masthead (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995) 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951281201
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