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  • Articles  (1,328)
  • Inorganic Chemistry  (1,210)
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  • 2005-2009  (75)
  • 1995-1999  (1,253)
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  • Articles  (1,328)
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  • 2005-2009  (75)
  • 1995-1999  (1,253)
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  • 1
    Electronic Resource
    Electronic Resource
    Masthead (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996) 
    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.19961290101
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  • 2
    Electronic Resource
    Electronic Resource
    Triferriothioxophosphoranes: First Structural Characterization of a μ3-P=S ComplexDedicated to Prof. Dr. M. Herberhold on the occasion of his 60th birthday. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 11-13 
    Details
    ISSN: 0009-2940
    Keywords: Triferriophosphane sulfide ; Metallothioxophosphorane ; PS complex ; Spiro compounds ; Decarbonylation ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The P-H-functional triferriophosphonium salts [{CpFe-(CO)2}3PH]2FeCl4 (1) and [{μ-CO(CpFeCO)2}{CpFe-(CO)2}PH]2FeCl4 (4) are easily deprotonated by DBU to the corresponding unstable triferriophosphanes 2, 5, which subsequently are oxidized by sulfur to the triferriophosphane sulfides {CpFe(CO)2}3P=S (3) and {μ-CO(CpFeCO)2}{CpFe-(CO)2}P=S (6), respectively. The photolysis of 3 results only in its decomposition by elimination of [CpFe(CO)2]2, whereas the photolysis of 6 cleaves off one CO ligand to give the new spiro compound (CpFeCO)(μ-η2-PS){μ-CO(CpFeCO)2} (7), where the P=S unit is η2-bonded to the 15-electron CpFeCO fragment, and the phosphorus atom bridges two 17-electron fragments. Compound 7 shows a new coordination mode of the PS unit where sulfur is also bound to one of the metal atoms. Compounds 6 and 7 can be regarded as first examples of a new class of PS complexes of transition metals. All compounds were characterized by IR, 31P{1H}- and 13C{1H}-NMR spectroscopy as well as mass spectrometry; for 6 the X-ray analytical data are given.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19961290104
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  • 3
    Electronic Resource
    Electronic Resource
    The Chemistry of 1,3,5-Triazacyclohexane Complexes, 3Part 2: Ref.. High Yield Synthesis of [Cr{N(SiMe3)2}3] and Accurate Structure Determination by Cocrystallization with Me6Si2 (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 25-27 
    Details
    ISSN: 0009-2940
    Keywords: Triazacyclohexanes ; Chromium complexes ; Amides ; Hexamethyldisilane ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reaction of N,N′,N′′-trimethyl-1,3,5-triazacyclohexane chromium trichloride ((Me3TAC)CrCl3, 1) with LiN(SiMe3)2 or NaN(SiMe3)2 in petroleum ether yields nearly quantitatively [Cr{N(SiMe3)2}3] (2) with loss of the Me3TAC ligand. Compound 2 could be crystallized from hexamethyldisilane as [Cr{N(SiMe3)2}3] · (Me6Si2)0,5 which allowed the refinement of the X-ray crystal structure in the trigonal space group P-31c (no. 163) (a = 16.012(3) Å, c = 8.4796(12) Å, V = 1882.8(6) Å3, Z = 2) without severe disorder.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19961290107
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  • 4
    Electronic Resource
    Electronic Resource
    Synthesis of Novel Tridentate N,O,S and N,N,O Ligands of the Tripod Type in Racemic and Enantiomerically Pure Form (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 59-68 
    Details
    ISSN: 0009-2940
    Keywords: Glyceraldehyde ; Ligands, tridentate ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A series of seven chiral, tripodal N,O,S and N,N,O ligands were prepared in which N stands for a secondary amine or imidazole donor, O for a phenol, and S for a thioether or thiol metal-binding group. Key steps are (1) the construction of ortho-hydroxyacetophenones bearing the phenolic binding group and either a thioether, a protected thiol or an imidazole substituent in the α-position, and (2) subsequent reductive amination with a primary amine. The modular synthesis allows a rapid construction of a variety of structurally related ligands. In three cases, the enantiomers of the racemic products could be separated after condensation with (R)-glyceraldehyde acetonide as chiral auxiliary. The relative configurations of the cyclic N,O- and N,N-acetals thus obtained were established by NOE spectroscopy. X-ray structural analysis of two crystalline N,O- and N,N-acetals allowed the assignment of absolute configurations. Hydrolysis of the dia-stereomerically pure acetals afforded the enantiomerically pure ligands in high yield. By comparison of their CD spectra, absolute configuration could also be assigned to the third pair of enantiomerically pure ligands.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19961290113
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  • 5
    Electronic Resource
    Electronic Resource
    Kinetic Investigations of the Hydrogenation of Diolefin Ligands in Catalyst Precursors for the Asymmetric Reduction of Prochiral Olefins, II[1] (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 85-89 
    Details
    ISSN: 0009-2940
    Keywords: Rhodium complexes, chiral ; Hydrogenation ; Bisolefins ; Thermodynamic stability ; Kinetic control ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Asymmetric hydrogenations of prochiral olefines by means of chiral rhodium(I) complexes of the type [Rh(L)(PP*)]A (L = COD, [(Z,Z)-cycloocta-1,5-diene], or NBD (norborna-2;5-diene), PP* = chiral bisphosphane forming seven-membered chelate rings, A = anion like BF4-) are often associated with induction periods caused by partial blocking of the catalyst. NBD complexes are hydrogenated faster than the corresponding COD complexes. Catalytic hydrogenation of COD/NBD mixtures and the determination of the ratio of the Michaelis constants showed that the steady-state concentration of the COD complex under hydrogen is higher than that of the NBD complex. However, under argon the NBD complex predominates owing to its higher thermodynamic stability compared with that of the COD complex as determined by 31P-NMR spectoscopy. This complete reversion of the ther-modynamically determined ratios of COD to NBD complex concentration under hydrogenation conditions was proven by means of UV/Vis spectroscopy.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19961290117
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  • 6
    Electronic Resource
    Electronic Resource
    1-Bromo-3,5-bis(trifluoromethyl)benzene: A Versatile Starting Material for Organometallic Synthesis (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 233-235 
    Details
    ISSN: 0009-2940
    Keywords: Positional selectivity ; Bromination ; Halogen/lithium exchange ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 1-Bromo-3,5-bis(trifluoromethyl)benzene (1) can be selectively prepared by treatment of 1,3-bis(fluoromethyl)benzene with N,N'-dibromo-5,5-dimethylhydantoin in strongly acidic media. A number of synthetically useful reactions via 3,5-bis(trifluoromethyl)phenylmagnesium, -lithium, and -copper intermediates were accomplished.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19961290219
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  • 7
    Electronic Resource
    Electronic Resource
    Lithiierte Phosphanimine. Synthese und Kristallstrukturen von [LiCH2PMe2NSiMe3]4 und [LiCMe2P(iPr)2NSiMe3]2 (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 253-257 
    Details
    ISSN: 0009-2940
    Keywords: Lithiated phosphane imines ; Phosphane imines, lithiated ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Lithiated Phosphane Imines. Synthesis and Crystal Structures of [LiCH2PMe2NSiMe3]4 and [LiCMe2P(iPr)2NSiMe3]2The title compounds were prepared by the reaction of Me3-SiNPMe3 and Me3SiNP(iPr)3, respectively, with n-Butylli-thium at 20°C in n-hexane solution. They form white, moisture- and oxygen-sensitive crystals, which were characterized by IR spectroscopy and by crystal structure determinations. - [LiCH2PMe2NSiMe3]4 (1) forms a Li4 tetrahedron, the faces of which are capped with CH2 groups with average Li-C distances of 233 and 251 pm, while the nitrogen atoms occupy the corners of the Li4 tetrahedron. - [LiCMe2P(iPr)2N-SiMe3]2 (2) forms molecules of symmetry C2 in which the lithium atoms have coordination number three by two carbon atoms and one nitrogen atom with Li-C distances of 215.2 and 237.9 pm and Li-N of 192.8 pm.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19961290223
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  • 8
    Electronic Resource
    Electronic Resource
    Synthesis and Characterization of a Novel Cyclobutadiene-octatetrayne Polymer (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 269-273 
    Details
    ISSN: 0009-2940
    Keywords: Organometallic polymers ; Coupling reactions ; Butadiynyl complexes ; Cobalt compounds ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The synthesis of 3a starting from compound 1 is described. Copper-catalyzed oxidative coupling of 3b under Hay conditions gives the novel polymer 9 with octatetrayne-cyclobutadiene units.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19961290304
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  • 9
    Electronic Resource
    Electronic Resource
    A Study on Electronic Interaction Between two [2.2]Metacyclophane Systems Connected with a C=C Bond: Preparation, Structure and Complexation of (E)- and (Z)-8,8′-(Ethene-1,2-diyl)bis(5-tert-butyl[2.2]metacyclophane) (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 289-296 
    Details
    ISSN: 0009-2940
    Keywords: Bis[2.2]metacyclophanes ; Stilbenes ; π-π Interaction ; Tricarbonylchromium complexes ; Charge-transfer ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: (E)-8,8′-(Ethene-1,2-diyl)bis(5-tert-butyl[2.2]metacyclo-phane) (2) was obtained from a McMurry reaction of 5-tert-butyl-8-formyl[2.2]metacyclophane (1). Irradiation of 2 with a high-pressure mercury lamp gave the corresponding (Z) isomer 3. X-ray crystallographic analyses of 2 and 3 show a certain degree of twisting of the bond connecting the meta-cyclophane unit and the central π system due to steric crowding. UV spectra of 2 and 3 and of the charge-transfer complexes [2/TCNE] and [3/TCNE] allow for a discussion of π-π interaction between the central stilbene subunit and the outer benzene rings of the metacyclophane units. Bis[2.2]meta-cyclophanes 2 and 3 reacted regioselectively with hexacar-bonylchromium on the outer benzene rings giving 1:1 and 1:2 complexes 9-14 with tricarbonylchromium. No 1:3 and 1:4 complexes formed due to steric restrictions. Analysis of UV spectral data of the complexed [2.2]metacyclophanes was performed for an indication of π-π interactions in the complexes.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19961290308
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  • 10
    Electronic Resource
    Electronic Resource
    Thermally Stable Self-assembling Open-Frameworks: Isostructural Cs+ and (CH3)4N+ Iron Germanium Sulfides (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 283-287 
    Details
    ISSN: 0009-2940
    Keywords: Self-assembling frameworks ; Thermal stability ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Here we report on investigations that have revealed for the first time that the Cs+ ion templates the same metal germanium sulfide open-framework as (CH3)4N+ (TMA+), and that metal complexing agents enhance crystal size by at least two orders of magnitude. The synthesis, structures and thermal properties of Cs2FeGe4S10 ·× H2O and TMA2FeGe4S10 are also described. Both have 3D zinc blende-type open-framework structures. These materials have the same connectivity as TMA2MnGe4S10. The tetrahedral sites in the lattice are alternately substituted by pseudo-tetrahedral Fe2+ and adamantanoid Ge4S104- building blocks, covalently linked together by Fe(μ-S)Ge bridge bonds, to give a tetragonal unit cell. The charge-balance of the anionic framework [Fe-Ge4S10]2- is maintained by either Cs+ or TMA+ ions in the cavity spaces. Synthesis of these materials demonstrates an interesting example of a self-assembly process in which a 3D framework is built from molecular precursors. Water adsorption-desorption cycling from room temperature to 200 °C reveals framework flexibility between larger and smaller tetragonal unit cell 14 isotypes. The compound TMA2FeGe4S10 is stable in nitrogen at 350 °C and under vacuum at 450 °C. The corresponding temperatures for Cs2FeGe4S10 are 530 °C and 630°C; it is stable on cooling to room temperature under vacuum, and after subsequent exposure to air. Six hundred thirty degrees celsius is the highest recorded temperature at which the integrity of a non-oxide framework has been maintained. The framework stability and flexibility of “all-inorganic” Cs2FeGe4S10 provides an encouraging example for researchers interested in developing sulfide-based framework materials with practical applications.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19961290307
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  • 11
    Electronic Resource
    Electronic Resource
    Complexes with S-Donor Ligands, 4Part 3: J. Vicente, M. T. Chicote, P. González-Herrero, P. G. Jones, J. Chem. Soc., Chem. Commun. 1995, 745.. Mono- and Di-Homo- and -Hetero-Nuclear Gold(I), Silver(I), and Palladium(II) Complexes with 2-(Methylthio)pyridine, Pyridine-2(1H)-thione, and Benzoxazole-2(3H)-thione. Some Examples of the Use of Complexes as Ligands (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 327-330 
    Details
    ISSN: 0009-2940
    Keywords: Gold complexes ; Silver complexes ; Palladium complexes ; S-Donor ; Thiones ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: AgClO4 reacts with bidentate ligands 2-(methylthio)pyridine (SMepy) or complexes PPN[Au(Spy)2] [PPN = N(PPh3)2, HSpy = pyridine-2(1H)-thione) or PPN[Au(Sbz)2] (HSbz = benzoxazole-2(3H)-thione), themselves acting as ligands, to give dinuclear complexes [Ag2(μ-SMepy)2](ClO4)2 (1), [AgAu(μ-Spy)2] (2), or [AgAu(μ-Sbz)2] (3), respectively. By treating 1 with [AuCl(tht)] (tht = tetrahydrothiophene), [Au(SMepy)(tht)]ClO4 (4) is obtained which, in turn, reacts with SMepy to give [Au(SMepy)2]ClO4 (5). Similarly, [PdCl2(NCPh)2] reacts with SMepy in 1:1 molar ratio to give [Pd2Cl2(μ-Cl)2(SMepy)2] (6) which reacts with SMepy in 1:2 molar ratio to give [PdCl2(SMepy)2] (7). On the other hand, HSpy reacts with Ag2CO3 to give [Ag2(μ-Spy)2] (8), and (SMepyH)ClO4 reacts with [Au(acac)PPh3] (acacH = acetyl-acetone) to give [Au(SMepy)PPh3]ClO4 (9).
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19961290313
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  • 12
    Electronic Resource
    Electronic Resource
    Zinc Complexes of Amino Acids and Peptides, 6. Zinc Complexes of Oligopeptides Containing Histidine at Both Termini (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 347-353 
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    ISSN: 0009-2940
    Keywords: Histidine peptides ; Zinc complexes ; EXAFS analysis ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: One tripeptide, five tetrapeptides, and one pentapeptide, all containing His-Xn-His sequences and being blocked at the N and C termini with acyl and amide functions, respectively, were synthesized by solid-phase methods. With one exception their reaction with various zinc salts led to the precipitation of 1:1 (zinc/peptide) complexes. Analytically pure compounds were obtained from zinc tetrafluoroborate and His-Gly-His (1), from zinc chloride (resp. bromide) and His-Gly -Gly-His (2), His-Ala-Gly-His (3), His-Leu-Gly-His (4), His-Pro-Gly-His (5), and His-Pro-Asn-His (6) as well as from zinc sulfate and His-Leu-Gly-His (4) and His-Ala-Pro-Gly-His (7). 1H-NMR data, when available, indicate the coordination of both histidine units to zinc in all cases. The low solubility of the complexes points to their polymeric nature. The only 1:2 (zinc/peptide) complex in this series was obtained from zinc perchlorate and His-Gly-Gly-His (2). An EXAFS study revealed that it contains zinc symmetrically coordinated by four histidine imidazole ligands. Based on the available information it is proposed that all complexes are one-dimensional polymers containg [-Zn-His-Xn-His-Zn-]x backbones.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19961290316
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  • 13
    Electronic Resource
    Electronic Resource
    Masthead (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996) 
    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.19961290401
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  • 14
    Electronic Resource
    Electronic Resource
    Silanediols Derived from Silanetriols. X-ray Crystal Structures of (2,4,6-Me3C6H2)N(SiMe3)Si(OSiMe3)(OH)2 and (2,4,6-Me3C6H2)N(SiMe3)Si(OSiMe2R)(OH)2 [R = CH2 (2-NH2-3,5-Me2C6H2)] (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 391-395 
    Details
    ISSN: 0009-2940
    Keywords: Silanediols ; Silanetriols ; Siloxanes ; Hydrogen bonding ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The silanediols RN(SiMe3)Si(OSiMe3)(OH)2 (R = 2,4,6-Me3C6H2 4, 2,6-Me2C6H3 5, and 2,6-iPr2C6H3 6) were prepared by the reactions of the respective silanetriols RN(SiMe3)-Si(OH)3 1 - 3 with SiMe3Cl in THF/hexane. Silanetriol 1 in CH2Cl2/hexane solution converts over a period of 4 weeks into the silanediol (2,4,6-Me3C6H2)N(SiMe3)Si(OSiMe2 R)-(OH)2 [R = CH2(2-NH2-3,5-Me2C6H2)] (7). Compounds 4 - 7 were characterized by means of mass, IR and NMR (1H and 29Si) spectroscopy. Additionally, the molecular structures of 4 and 7 were determined by single-crystal X-ray diffraction studies. Compound 4 forms O — H…O hydrogen-bonded tetramers in the solid state. A nine-membered ring formed by an intermolecular O—H…N hydrogen bond is found in the solid-state structure of 7.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19961290405
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  • 15
    Electronic Resource
    Electronic Resource
    Novel trialkylstibane iridium(I) and iridium(III) complexes including the x-ray crystal structure of five-Coordinate [IrCl(C2H4)2(SbiPr3)2]Dedicated to Professor Erwin Weiss on the occasion of his 70th birthday. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 411-417 
    Details
    ISSN: 0009-2940
    Keywords: Iridium complexes ; Stibane complexes ; Hydrido complexes ; Ethene complexes ; Ligand displacement reactions ; Alkyne-to-vinylidene rearrangement ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reaction of [IrCl(C8H14)2]2 (2) with SbiPr3 in the presence of H2 yields the dihydridoiridium(III) complex cis,mer-[IrH2Cl(SbiPr3)3] (3) which on treatment with CO and with HC≡CR (R = Ph, CO2Me) affords the octahedral derivatives [IrH2Cl(CO)(SbiPr3)2] (4) and [IrHCl(C≡CR)(SbiPr3)3] (5, 6), respectively. The stibane ligand trans to hydride in 5 and 6 is rather labile and, therefore, 5 and 6 react with pyridine to give [IrHCl(C≡CR)(py)(SbiPr3)2] (7, 8). Five-coordinate bis-(stibane)iridium(I) complexes [IrCl(C2H4)2(SbR3)2] (10-12) were prepared from [IrCl(C2H4)2]2 (9) and four equiv. of SbR3 (R = iPr, Me, Ph). The X-ray crystal structural analysis of 10 reveals a distorted trigonal-bipyramidal geometry around the metal center with one stibane ligand and the two olefinic ligands in the equatorial plane. Compound 10 reacts with NaC5H5 to yield [C5H5Ir(C2H4)(SbiPr3)] (13) and with different alkynes by partial or complete displacement of the ethene ligands to give trans-[IrCl(PhC≡CPh)(SbiPr3)2] (14), [IrHCl(C≡CTol)(C2H4)(SbiPr3)2] (15), and trans-[IrCl-{=C=C(SiMe3)R}(SbiPr3)2] (16, 17), respectively.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19961290409
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  • 16
    Electronic Resource
    Electronic Resource
    Azolylborane adducts. Structural and conformational analysis by x-ray diffraction and NMR. Protic-hydric (C=Hδ+-δ-H=B) and Protic-Fluoride (C=Hδ+-δ-F=B) interactions (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 441-449 
    Details
    ISSN: 0009-2940
    Keywords: Azolylborane adducts ; Boron-imidazole adducts ; Boron-pyridine adducts ; Protic-hydric interactions ; Protic-fluoride interactions ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The preparation, NMR and X-ray diffraction studies of a series of azolylboron hydrides derived from pyrrole, indole, and carbazole coordinated with tetrahydrofuran, pyridine, and imidazole are reported. The azolyl substituents are very electroattractive leading to an acidic boron atom which strongly coordinates with the Lewis bases. The stabilization of the =BH2=groups against disproportionation could be explained in terms of the interactions found between the acidic hydrogen atoms of the heterocycles (C=Hδ+ acceptor) and the hydrides (B=Hδ- donors).
    Additional Material: 8 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19961290413
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  • 17
    Electronic Resource
    Electronic Resource
    Masthead (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996) 
    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.19961290501
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  • 18
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    Electronic Resource
    The Synthesis of Stabilized Dimetallated Thioimidate Complexes by the Insertion of Ethoxycarbonylisothiocyanate into a Rhenium-Rhenium Bond (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 485-487 
    Details
    ISSN: 0009-2940
    Keywords: Dimetallations ; Insertions ; Rhenium ; Isothiocyanates ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Molecules containing dimetallated hydrocarbyl groupings are of great chemical interest[1-3]. These groupings often represent intermediates in important catalytic processes[4]. Recently, we have shown that substituted dimetallated olefins can be formed by alkyne insertion into the metal-metal bonds of certain dinuclear complexes[2,5]. Complexes having dimetallated hydrocarbyl groups combined with heteroatoms are quite rare[6]. Herein is described the formation of a dimetallathioimidate grouping by the insertion of an organic isothiocyanates into an unsupported metal-metal bond. Organic isothiocyanates are useful reagents in organic synthesis[7], but the organometallic chemistry of these molecules is not yet well developed[8].
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19961290503
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    Electronic Resource
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    Supermolecules Containing a Tetrahedral Core: A New Class of Liquid-Crystalline Siloxanes (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 521-525 
    Details
    ISSN: 0009-2940
    Keywords: Liquid crystals ; Siloxanes ; Phase behaviors ; Defined topology ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: It is shown that supermolecules with a tetrahedral symmetry and appropriate side-chains exhibit liquid-crystalline phase behaviour. The use of an optimised hydrosylation reaction allows for the synthesis of materials that have four mesogenic groups attached to a siloxane core, where the conformation and the configuration are unambiguous. The materials show low glass transition temperatures and, depending on the spacer length, complex liquid-crystalline morphologies.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19961290508
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    Transition Metal Complexes with Sulfur Ligands, Part 119Part 118: D. Sellmann, H.-J. Kremitzl, F. Knoch, M. Moll, J. Biol. Anorg. Chem., in press.. Synthesis of Water Soluble Fe and Ru Complexes with Novel Multidentate Thioether Thiolate Ligands Containing Carboxylate Substituents (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 509-519 
    Details
    ISSN: 0009-2940
    Keywords: Iron and ruthenium complexes ; Water soluble complexes ; Sulfur ligands ; X-ray structure analyses ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: In search of water soluble transition metal complexes with sulfur dominated coordination spheres that model key reactions of nitrogenases, the benzenedithiol derivatives ‘CO2HS2’-H2 (1) and ‘CO2Me-S2’-H2 (2) were synthesized as precursors for multidentate sulfur ligands. The template alkylation of 2 by C2H4Br2 at [Fe(CO)2] fragments yielded a mixture of two diastereomeric C2 symmetrical [Fe(CO)2(‘CO2Me-S4’)] complexes (4a and 4b), which were separated by crystallization. The hydrolysis of the mixture of the diastereomers 4a and 4b led to the isomerically pure tetradentate thioether thiol ligand ‘CO2Me-S4’-H2 (5) proving the regioselectivity of the template alkylation of the asymmetrical dithiol 2. The C1 symmetrical [Fe(‘CO2Me-S2’)2]2- anion is an intermediate of the template alkylation and was isolated as (AsPh4)2 [Fe(‘CO2Me-S2’2] (11), 4a, 5 and 11 were characterized by X-ray structural analysis. Saponification of the methyl ester groups of 5 yielded ‘CO2H-S4’-H2 (7). Treatment of 7 with FeCl2 · 4 H2O in the presence of CO and LiOMe gave a mixture of two C2 symmetrical and water soluble diastereomers of Li2[Fe(CO)2(‘CO2-S4’)] (8). Upon treatment with [RuCl2 (PPh3)3] 7 yielded isomerically pure [Ru(PPh3)2-(‘CO2H-S4’)] (9). 9 also exhibits C2 symmetry and could be reversibly deprotonated to form the water soluble complex K2[Ru(PPh3)2 (‘CO2-S4’)] (10). Treatment of (NBu4)2 (‘CO2MeS2’) with “Ru(NO)Cl3” led to isomerically pure (NBu4)[Ru(NO)(‘CO2Me-S2’)2] (12).
    Additional Material: 6 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19961290507
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    Syntheses and Photochemistry of Fluorinated and Chlorinated Titanium Porphyrinates: Crystal Structure of Oxotitanium meso-Tetrakis(2,3,4,5,6-pentafluorophenyl)porphyrinate (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 833-836 
    Details
    ISSN: 0009-2940
    Keywords: Oxotitanium(IV) porphyrinate ; Peroxotitanium(IV) porphyrinate ; Photochemistry ; Singlet oxygen ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The syntheses of oxotitanium(IV) meso-tetrakis(2,3,4,5,6-pentafluorophenyl)porphyrinate O=Ti(TPPF20) (1), oxotitanium(IV) meso-tetrakis(2,6-difluorophenyl)porphyrinate O=Ti-(TPPF8) (3), and oxotitanium(IV) meso-tetrakis(2,6-dichlorophenyl)porphyrinate O=Ti(TPPCl8) (5) from titanium tetrachloride and the corresponding porphine are described. The structure of 1 was determined by single-crystal X-ray diffraction. The reaction of oxotitanium porphyrinates with aqueous hydrogen peroxide leads to the corresponding light-sensitive peroxotitanium(IV) complexes: Ti(O2)(TPPF20) (2), Ti(O2)-(TPPF8) (4), Ti(O2)(TPPCl8) (6). All complexes are efficient and stable photosensitizers for the generation of singlet oxygen.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19961290715
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    Syntheses of Hetero-sila-closo-boranes (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 837-839 
    Details
    ISSN: 0009-2940
    Keywords: Boron compounds ; Silaboranes ; Dihetero-closo-borane ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Addition of 3 equivalents of KH · BEt3 to [Me3NH][Me-SiB10H12] followed by addition of one equivalent of SnCl2 or SbI3 affords the stanna-sila-closo-borate(1-) 3 and stiba-sila-closo-borane 4, respectively. [MePh3P] · 3 crystallizes in the orthorhombic space group P212121.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19961290716
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  • 23
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    Intramolekular stabilisierte Übergangsmetallamide: 2-(Dimethylaminomethyl)pyrrolyl-Komplexe des Titan(III), Vanadium(III), Chrom(III), Cobalt(II) und Nickel(II) (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 853-857 
    Details
    ISSN: 0009-2940
    Keywords: Amides ; Pyrrolyl complexes ; Chelate complexes ; Transition-metal complexes ; Metallacycles ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Intramolecularly Stabilized Metal Amides: 2-(Dimethylaminomethyl)pyrrolyl Complexes of Titanium(III), Vanadium(III), Chromium(III), Cobalt(II) and Nickel(II)By the metallation of 2-(dimethylaminomethyl)pyrrol (HL) with butyllithium the lithium pyrrolide LiL (1) was obtained. The reactions of 1 with TiBr3 · 3 THF, VBr3 · 3 THF, CrBr3 · 3 THF, CoBr2 · 2 THF, and NiBr2 · 1.67 THF result in the formation of the 2-(dimethylaminomethyl)pyrrolyl complexes of type ML3 (2-4), and ML2 (5, 6), respectively. The structures of these new compounds are discussed on the basis of magnetic and visible absorption measurements. An X-ray crystal structure determination of 4 reveals a strongly distorted octahedral environment of the chromium atom with facial arrangement of the ligands.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19961290719
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  • 24
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    Stepwise Insertion of Alkylisocyanides into the Metal-Alkyne Bond of Half-Sandwich Type Rhodium Complexes: Synthesis and Structural Characterization of Metallacyclobutenes and MetallacyclopentenesDedicated to Professor Gerhard E. Herberich on the occasion of his 60th birthday. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 903-910 
    Details
    ISSN: 0009-2940
    Keywords: Rhodium complexes ; Alkyne complexes ; Insertion reactions ; Alkyl isocyanides ; Metallacycles ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The cyclopentadienyl complexes [C5H5Rh(RC≡CR′)(SbiPr3)] (5-8), which were prepared from trans-[RhCl-(RC≡CR′)(SbiPr3)2] (1-4) and NaC5H5 and which contain a labile Rh-SbiPr3 bond, reacted with CO and CNR″ (R″ = Me, tBu) to give the carbonyl and isocyanide derivatives [C5H5Rh(RC≡CR′)(CO)] (9-11) and [C5H5Rh(RC≡CR′)-(CNR″)] (12-16), respectively. On treatment of 12 (R = R′ = Ph; R″ = Me) with SbiPr3, the metallacyclobutene complex [C5H5Rh{κ2(C,C}-C( = NMe)CPh=CPh}(SbiPr3)] (17) was formed; it reacts with excess CNMe or CNtBu to yield the metallacyclopentenes [C5H5Rh{κ2(C,C)-C(=NMe)CPh=CPhC-(=NR)}(CNR)] (18, 19). Similar compounds 20-23 containing a five-membered RhC4 metallacycle were prepared either from [C5H5Rh(RC≡CR′)(SbiPr3)] (7, 8) or [C5H5Rh-(PhC≡CPh)(CNtBu)] (14) and excess isocyanide. The crystal and molecular structures of 17 and 18 (R = Me) have been determined.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19961290805
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    Isolation and Spectroscopic Characterization of Heteroleptic, Anionic and Neutral (Phthalocyaninato)(tetra-4-pyridylporphyrinato)lanthanide(III) Double-DeckersDedicated to Professor Shang-Wai Tam on the occasion of his retirement from The Chinese University of Hong Kong. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 933-936 
    Details
    ISSN: 0009-2940
    Keywords: Phthalocyanines ; Porphyrins ; Lanthanide(III) compounds ; Macrocyclic ligands ; Double-decker complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Treatment of 5,10,15,20-tetra-4-pyridylporphyrin [(TPyP)H2] with europium(III) or gadolinium(III) acetylacetonate [Ln(acac)3 · nH2O] (Ln = Eu, Gd) in 1,2,4-trichlorobenzene produced Ln(acac)(TPyP), which reacted with dilithium phthalocyaninate [Li2(Pc)] to give Li[Ln(Pc)(TPyP)] in moderate yields. Upon exposure to air, solutions of these compounds converted slowly to the corresponding neutral complexes Ln(Pc)(TPyP). The new compounds were spectroscopically characterized.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19961290809
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    Synthesis, Spectroscopic Characterization, and Crystal Structure Determination of Cationic [(Cyclopentadienyl)dicarbonyliron](alkynyl)-aminocarbene Complexes (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 937-944 
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    ISSN: 0009-2940
    Keywords: Iron acyl complexes ; (Alkynyl)carbene ligand ; Cationic aminocarbene complexes ; Iron (2-methoxyvinyl)aminocarbene complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: (Alkynoyl)iron complexes 1, Cp(CO)2Fe(O=CC≡CR) (R = CH3, Ph, SiMe3), were synthesized by applying a mixed anhydride procedure and transformed into the cationic methoxycarbene complexes 2, [Cp(CO)2 Fe(C(OMe)C≡CR)+]-[PF6-]. Primary amines H2NR′ react with the methoxycarbene complexes to furnish exclusively cationic aminocarbene complexes 3, [Cp(CO)2 Fe(C(NHR′)C≡CR)+][PF6-], or (2-methoxyvinyl)aminocarbene complexes 5. The spectroscopic properties of the new complexes are discussed. The (alkynyl)-aminocarbene complexes 3e and 3f were characterized by X-ray crystal structure analysis.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19961290810
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    Synthesis and Characterization of Novel Phthalocyanines with Four 16-Membered Diazadithia Macrocycles (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 967-971 
    Details
    ISSN: 0009-2940
    Keywords: Phthalocyanines, sulphonated ; Diazadithiamacrocycles ; Pentanuclear complex ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Metal phthalocyanines (M = Cu, Ni, Co) 3-5 bearing four 16-membered diazadithia macrocycles at the peripheral positions were prepared. Detosylation with concentrated sulfuric acid afforded products containing both sulfonated groups on the aromatic rings of the macrocyclic substituents which are excellently soluble in water and donor sites for binding four CuII ions to give a pentanuclear complex.
    Additional Material: 2 Tab.
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    A Search for Thionitrosyl Chloride (Cl-N=S) in the Gas Phase (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1379-1381 
    Details
    ISSN: 0009-2940
    Keywords: Thionitrosyl chloride ; Thiazyl chloride ; Neutralization-reionization mass spectrometry ; Calculations, ab initio ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Ab initio MO calculations at the QCISD(T)/6-311++G(3df,2p) + ZPE level show that the thionitrosyl chloride ion, ClNS+•, is 36 kJ/mol more stable than the thiazyl chloride ion, NSCl+•, whereas neutral NSCl is 77 kJ/mol more stable than ClNS [IEa (ClNS) = 9.2 ± 0.3 eV, IEa (NSCl) = 10.5 ± 0.3 eV]. Mild flash-vacuum pyrolysis of the thiazyl chloride trimer (NSCl)3 followed by electron impact ionization resulted in the formation of [N,S,Cl]+• ions (m/z 81). The fragments observed in the CA spectrum of these ions indicate the formation of both NSCl+• and ClNS+• ions. A very weak recovery signal is observed in a neutralizationreionization experiment. This signal is tentatively assigned to the neutral thionitrosyl chloride.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19961291111
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    Synthesis and Reactivity of Some Nitroaryl Complexes of HgII and AuIII  -  Synthesis of a Substituted Biphenyl by C-C Coupling - Crystal Structure of [Hg(C6H4NO2-3, OnBu-6)2] (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1395-1399 
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    ISSN: 0009-2940
    Keywords: Gold ; Mercury ; Nitroaryl ; Transmetallation ; Biaryl ; C-C Coupling ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 4-Butoxynitrobenzene reacts with [Hg(O2CCF3)2] and LiCl to give [Hg(R)Cl] [R = C6H3NO2-3, OnBu-6 (1)] which is symmetrized by Me4NCl to give [HgR2] (2), the crystal structure of which has been determined. The reaction of 2 with Me4N[AuCl4] affords Me4N[Au(R)Cl3] (3) by a facile transmetallation process. Complex 3 reacts with PPh3 (1:1) to give cis-[Au(R)(PPh3)Cl2] (4). The diaryl complex [-Ph-2)(R)Cl] (5) is obtained by reaction of 3 with [Hg-(C6H4N=NPh-2)2] through a second transmetallation reaction. Complex 5 and PPh3 (1:1) give [AuClPPh3] and the C-C coupling biphenyl RC6H4N=NPh-2 (6).
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    URL: http://dx.doi.org/10.1002/cber.19961291114
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    Sulfenato, Thiosulfinato, and Thiosulfonato Transition Metal ComplexesDedicated to Professor M. Herberhold on the occasion of his 60th birthday. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1409-1419 
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    ISSN: 0009-2940
    Keywords: Sulfenic acid anions ; Thiosulfinic acid anions ; Thiosulfonic acid anions ; Transition metal complexes ; Stereochemistry ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The synthesis and coordination chemistry of sulfenic, thiosulfinic, and thiosulfonic acid anions are reviewed. Different approaches, which yield the platinum(II) and ruthenium(II) complexes containing the anionic sulfur(0), sulfur(II), and sulfur(IV) oxid ligands, are described. The oxidative addition of thiosulfinates or N-sulfinyl phthalimides to platinum(0) complexes L2Pt(C2H4) [L = PPh3, 1/2 PPh2CH2CH2PPh2, 1/2 (R,R)-(-)-DIOP, 1/2 (C5H4PPh2)Fe(C5H4PPh2) leads to sulfenato complexes; those of N-thiosulfinyl phthalimidies or trisulfid 1-oxides afford the thiosulfinato complexes. Moreover, the reactions of CpRu(PPh3)(L)(SH) (L = CO, PPh3) with N-sulfinyl phthalimides forming the thiosulfinato moiety, are reported. The spectroscopic, structural and chemical properties of these complexes are discussed.
    Additional Material: 5 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19961291202
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    Cationic Iron Aminocarbene Complexes as Dienophiles in Diels-Alder Reaction with Cyclopentadiene (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1057-1059 
    Details
    ISSN: 0009-2940
    Keywords: (Alkynyl)carbene ligands ; Iron acyl complexes ; Cationic iron aminocarbene complexes ; Diels-Alder reactions ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The cationic iron (alkynyl)aminocarbene complexes [Cp(CO)2Fe(C(NHR)C≡CSiMe3][PF6], (R = C6H5, p-CH3C6H4) 1 derived from aromatic amines smoothly react with cyclopentadiene in dichloromethane to yield the cycloadducts 2. No reaction was observed for complexes derived from sterically demanding aliphatic amines, like L-alanine tert-butyl ester. For comparison, the alkynyl-substituted acyl iron compounds Cp(CO)2Fe(C=O)C≡C̊ (R = SiMe3, C6H5) 3 were investigated, requiring TiCl4 catalysis to undergo the cycloaddition reaction. The structures of the cycloadducts 4 were determined by X-ray crystallography.
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    URL: http://dx.doi.org/10.1002/cber.19961290913
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    Synthesis, Structure and Reactions of the Homoleptic Alkyne Nickel(0) Complex (Alkyne)4Ni3 (Alkyne: 2-methyl-4-trimethylsilyl-3-butyn-2-ol)Dedicated to Professor Walter Siebert on the occasion of his 60th birthday. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1457-1461 
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    ISSN: 0009-2940
    Keywords: Nickel(0) ; Alkyne complexes ; Hydrogen bonds ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Treatment of (cdt)Ni (cdt: cyclododeca-1,5,9-triene) with 2 equivalents of 2-methyl-4-trimethylsilyl-3-butyn-2-ol leads to the selective formation of the homoleptic complex (alkyne)4Ni3 (compound 3), which can be isolated in excellent yields. The solid-state structure of 3 exhibits three Ni centers, forming a bent Ni3 chain connected by two bridging alkynes. The other two alkynes are terminally coordinated. Additionally, the trimeric units are stabilized by three intramolecular hydrogen bonds. Two intermolecular hydrogen bonds connect the trimeric units to form a polymer rope. According to the 13C- and 1H-NMR spectra in THF the structure of the complex 3 in solution is very similar to that in the solid state. The reaction of 3 with some alkynediols and with 2,5,5-trimethylhex-3-yn-2-ol affords compounds of the type (alkyne)2Ni. Cot (cot: 1,3,5,7-cyclooctatetraene) converts 3 into [(cot)Ni]2, which in turn reacts with 2,5-dimethylhex-3-yne-2,5-diol to form the dimeric complex (alkyne)2Ni2(cot) 6. X-ray analysis of 6 reveals a very symmetrical structure in which cot connects both Ni(0) centers at opposite sides of the ring system.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19961291210
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    Control of the SO2 Coordination Mode at the (Monochelate)rhodium Complex ClRh(P∼O) with the Hemilabile Ligand Cy2PCH2CH2OCH3Dedicated to Professor Michael Hanack on the occasion of his 65th birthday. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1103-1105 
    Details
    ISSN: 0009-2940
    Keywords: Sulfur dioxide ; Rhodium complexes ; Ether-phosphanes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The SO2 coordination mode at the rhodium complex [ClRh(P∼O)()] (1) [ = η2(O,P)-chelated Cy2PCH2CH2OCH3 ligand; P∼O = =1(P)-coordinated] is controlled by the hemilabile ligand Cy2PCH2CH2OCH3 and shows a dependence on the polarity of the solvent. In polar organic solvents (e.g. acetone) the addition of sulfur dioxide results in the formation of a trigonal-pyramidal oriented SO2 group in [ClRh(η1-SO2)(P∼O)()] (2a). However, in nonpolar media (e.g. n-hexane) a trigonal-coplanar geometry of the SO2 unit in [ClRh(η1-SO2)(P∼O)2] (2b) is favored.
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    Masthead (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996) 
    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.19961291001
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    Hydrogen Bonding and Conformational Analysis of Chelate-Stabilized Alkoxopalladium(II) Complexes Derived from Amino Alcohol Ligands (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 35-44 
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    ISSN: 0009-2940
    Keywords: Alkoxopalladium(II) ; Conformational analysis ; Hydrogen bonding ; Two-dimensional and cage structures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reaction of palladium acetate with two equivalents of di- and triethanolamines RN(CH2CH2OH)2 in the presence of a base affords the new chelate-stabilized alkoxo Pd(II) complexes [Pd(OCH2CH2N(R)CH2CH2OH)2] [R = Me (1), Et (2), n-Bu (3), benzyl (4) or CH2CH2OH (5)]. These N,O-ligated complexes are isolated in high yield as yellow, crystalline solids and are thermally stable despite the presence of several β-hydrogen atoms in the ligand system. Both complexes possess a square-planar palladium coordination geometry with the two oxygen atoms positioned mutually trans. The most notable difference in the molecular structures is that 1 forms a two dimensional network of intermolecular O-H≡O hydrogen bonds, whereas 5 forms intramolecular O-H⃛O hydrogen bonds, which cage the palladium center. In solution 1-4 exist as a diastereoisomeric mixture (a racemic enantiomeric pair SNSN, RNRN and a mesomeric form RNSN) in a 1:1 molar ratio, and this ratio is independent of temperature in nonalcoholic solvents, When complexes 1-4 are dissolved in protic solvents (e.g. MeOH) the diastereomeric excess is temperature-dependent due to an exchange process between the meso diastereoisomer and the (racemic) enantiomeric pair. Thermodynamic parameters for this process in a mixture of MeOH-toluene have been determined with NMR and show this process to be influenced by the steric nature of the alkyl substituent (R) on nitrogen. A conformational analysis based on 1H-NMR coupling constants within the N,O-chelate ring of complexes 1-4 provides details on the solution structure of the ring in both diastereoisomers.
    Additional Material: 9 Ill.
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    Synthesis of Functionalized Carbamates through a Palladium-Catalyzed Reductive Carbonylation of Substituted Nitrobenzenes (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 13-22 
    Details
    ISSN: 0009-2940
    Keywords: Carbamates ; Catalysis ; Substituted nitrobenzenes ; Palladium ; Reductive carbonylation ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The palladium-catalyzed reductive carbonylation of ortho and para-substituted nitrobenzenes has proven to be an attractive route for the synthesis of functionalized carbamates. For the Pd(1, 10-phenanthroline)2(triflate)2 catalyst system, the scope of the reaction has been studied. Substrates with electron-donating substituents at the para position were found to decrease the catalytic activity, most probably as a result of their relatively low oxidizing capacity. the selectivity towards the desired carbamate, however, was increased for these substrates. Under the influence of electron-withdrawing substituents the azoxybenzene and azobenzene derivatives became important side products. Introduction of large steric hindrance at the ortho position of the nitro substrates gave rise to an interesting side reaction, viz. methoxylation of the aromatic ring. The methoxylation reaction appeared to occur on an intermediate species in the catalytic cycle. Several functionalities have shown to be resistant to the reaction conditions required for the conversion ot the nitro group. Especially with 4-nitrobenzoic acid, an extremely high activity and selectivity was found, thus yielding a very convenient synthesis for N-protected amines containing carboxylic acid function.
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    Dimeric Silver(I) Complexes of Some Isothiazole-Based LigandsDedicated to Prof. Dr. Rolf Gleiter on the occasion of this 60th birthday. (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 95-100 
    Details
    ISSN: 0009-2940
    Keywords: Isothiazole complexes ; Dinuclear silver(I) complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A series of isothiazole-based potential ligands bearing substituents with additional donor sites in the 5-position of the heterocycle was synthesized [3-Me-5-R-C3HNS; R = CH=N(CH2)2py (1), CH=NCH2py (2), CH2N(CH2CH2NEt2)2 (4), (CH2)2SMe (5)]. Upon reaction with AgO3SCF3 they formed complexes [(1)AgOSO2CF3]2 (6), [(2)AgOSO2CF3]2 (7), [(4)Ag]2+2(O3SCF-3)2 (8) and [(5)AgOSO2CF3]2 (9), respectively. 6, 8 and 9 were shown by X-ray structural analyses to consist of dimeric units L2Ag2+2, either discrete (8), coordinated by terminal CF3SO-3 units (6). In 8 and 9 the isothiazole moiety is bonded to the metal center via the ring-N. The coordination potential of the isothiazole heterocycle is discussed.
    Additional Material: 5 Ill.
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    Synthesis and Structure of Binuclear Single-Bridged Bis[(phosphane)gold(I)]halogenonium Complexes (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 115-118 
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    ISSN: 0009-2940
    Keywords: Gold complexes ; Bromonium complex ; Halogenonium complex ; Halogen, two-coordinate ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Reactions of (R3P)AuX (X = Cl, Br, I) with [(R3P)Au]+ BF-4 obtained from (R3P)AuCl and AgBF4 in tetrahydrofuran, lead to cationic binuclear gold(I) complexes of the general formula ([(R3P)Au]2X}+ BF-4. A number of chloro- (R = Ph, o-Tol, Mes, Bzl, Et), bromo- (R = Ph, o-Tol, Mes) and iodo-bridged (R = Ph, Mes) complexes of this type have been isolated and identified on the basis of their analytical and spectroscopic data. The crystal structure of bis[(triphenylphosphane)gold(I)]bromonium tetrafluoroborate was determined by single-crystal X-ray diffraction. The cations contain two-coordinate bromine atoms with an Au-Br-Au angle of 96.83(3)°.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19971300119
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    A Specific Route to Enantiomerically Pure Asymmetric (η6-Arene)(η4-1,5-cyclooctadiene)Ru(0) ComplexesDedicated to Professor Rolf Gleiter on the occassion of his 60th birthday. (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 123-130 
    Details
    ISSN: 0009-2940
    Keywords: Arene complexes ; Ruthenium compounds ; Electrophilic substitution ; Lithiation ; Catalysis ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Chiral or achiral (arene)(COD)Ru complexes can be made by replacing the η6-ligands of (η4-1,5-COD)(η6-1,3,5-cyclooctatriene)Ru (1) or (η4-1,5-COD)(η6-naphthalene)Ru (2) by a suitable arene. This well known reaction has been extended to mono- and dibromoarenes and we report a novel route to substituted (arene)(COD)Ru species, utilizing (bromoarene)-(COD)Ru as starting materials. These facilitate a rapid bromine-lithium exchange reaction with nBuLi at low temperatures and the lithiated species react readily with alkyl chloroformates as electrophiles. By using chiral electrophiles [alkyl = (-)-menthyl] enantiomerically pure or diastereomeric complexes containing CO2R* groups are formed, depending on the symmetry of the original complex. A diastereomeric 1:1 mixture was separated by recrystallization. All (arene)-(COD)Ru complexes tested so far are useful as catalysts for the hydrogenation of simple alkenes at room temperature.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19971300121
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    Recent Advances in C-F Bond Activation (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 145-154 
    Details
    ISSN: 0009-2940
    Keywords: Fluorocarbons ; C-F bond activation ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The main reaction pathways which lead to the breaking of C-F bonds in perfluoroalkanes and -arenes are discussed. Emphasis is placed on recent developments and on the mechanistic patterns that emerge.
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    URL: http://dx.doi.org/10.1002/cber.19971300203
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    Metal Atoms in the Synthesis of Metal Clusters, VIII.On the Reaction of Sterically Demanding Cyclopentadiene Ligands with Cobalt Atoms: Synthesis, Crystal Structure, Spectroscopic Behavior, and Reactivity of Di-, Tri- and Tetranuclear Hydrido Clusters of CobaltDedicated to Professor IV Siehert on the occasion of his 60th birthday. (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 161-170 
    Details
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The metal-vapor reactions of Co atoms with 1,3-tBu2CpH (1a), 1,3-tBu2CpH (1a), 1,2,4-tBu3CpH (1b) and EtMe4CpH (1c) are described. With 1a the two mononuclear complexes [(η5-tBu2Cp) (η4-tBu2-1,3-cyclopentadiene)Co] (2a) and [(η5-tBu2Cp)2Co] (3a) were isolated, together with the dinuclear cobalt cluster [{(η5-tBu2Cp)Co}2H3] (4a) and trace amounts of the tetranuclear cluster [{(η5-tBu2Cp)CoH}4] (5a). The molecular structures of 3a and 4a were determined by X-ray diffraction. Reaction of 1b with Co atoms afforded a single product, the dinuclear cluster [{(η5-tBu3Cp)Co}2H3] (4b), whose molecular structure was determined by single-crystal X-ray diffraction. Both, 4a and 4b exhibit extremely short Co-Co distances [2.244(1) (4a) and 2.242(1) Å (4b)], as found for the Me5Cp analog [{(η5-Me5Cp)Co}2H3] (4c). Reaction of an isomeric mixture of Me4EtCpH (1c) with Co atoms furnished the mononuclear sandwich [ (η5-Me4EtCp)(η4-Me4Et-1,3- cyclopentadiene)Co] (2b), the trinuclear hydridocobalt cluster [{(η5-Me4EtCp)Co}3H4] (6a) and the tetranuclear hydridocobalt cluster [{(η5-Me4EtCp)Co}4H4] (5c). The molecular structure of 5c was determined by X-ray crystallography and revealed a tetrahedral arrangement of the cobalt atoms. The electrochemical behavior of the dinuclear complexes 4a-4c was studied by cyclic voltammetry. Reversible redox couples were found for all three compounds, with a correlation between the degree of alkyl substitution and their respective cathodic shifts. Compounds 4a and 4b react with CO to yield the mononuclear and dinuclear complexes [ (η5- CpR)Co(CO)2] (R=1,3-tBu2, 1,2,4-tBu3) (7a and 7b) as well as [{(η5-CpR)CO}2(CO)2] (8a and 8b). Reaction of the trinuclear hydridocobalt cluster 6a and its Me5Cp analog 6b with AgBF4 in the presence of PEt3 yielded the heteronuclear clusters [{η5-Me4CPR)Co}3AgP(Et)3H4]+[BF4]- (R=Et, Me) (9a and 9b). 9a was structurally characterized by X-ray crystallography.
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    1,3-Heterobinuclear Cyclobutenylidene Complexes with an Exocyclic C=C bond  -  Synthesis, Structure, and Spectroscopic Properties (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1475-1482 
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    ISSN: 0009-2940
    Keywords: Allenylidene complexes ; Alkynyl complexes ; Cyclobutenylidene complexes ; Cycloadditions ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Pentacarbonyl(allenylidene)chromium and -tungsten, [(CO)5—M=C=C=CR2] (M=Cr, R=C6H4CH3-p(1a), C6H4OCH3 (1b); M=W, R=C6H4CH3-p (1c), react with the alkynyl complexes [Cp(CO)2Fe—C≡CR′] (R′ = nBu (2), Ph (4)), [Cp*(CO)2Fe—C≡CnBu] (6), [Cp(CO){P(OMe)3}-Fe—C≡CnBu] (8) and [Cp(PPh3)Ni—C≡CnBu] (10) by cycloaddition of the C≡C bond of the alkynyl complexes to the Cα=Cβ bond of the allenylidene ligand to give 3a-c), (5), (7), and respectively. The cycloaddition is highly selective. The spectroscopic data of these 1,3-heterobinuclear complexes indicate a delocalized π-system (M=Cr, W; Y=[Fe(CO)2Cp], [Fe(CO)(P{OMe}3)Cp], [Fe(CO)2Cp*], [Ni(PPh3)-Cp]). X-ray structural analyses of the compounds 3a, 9a, and 11c reveal a “butterfly” conformation of the four-membered ring. Its puckering angle is 142° (3a), 152° (9a), and 151° (11c). All Complexes exhibit a moderate to strong negative solvatochromic behavior. The extent of the solvatochromic effect depends on [(CO)5M] and Y and considerably decreases when C=CR2 is replaced by e.g. CMe2.
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    The Phosphonate-Phosphate- and Phosphate-Phosphonate Rearrangement and Their Applications, 4Part 3: Ref.[1].. Deprotonation of Secondary Benzylic Phosphates  -  Configurationally Stabile Benzylic Carbanions with a Diethoxyphosphoryloxy Substituent and Their Rearrangement to Optically Active Tertiary α-Hydroxyphosphonates (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1503-1508 
    Details
    ISSN: 0009-2940
    Keywords: Phosphate - Phosphonate rearrangement ; Carbanions, benzylic, configurational stability of ; α-Hydroxyphosphonates, tertiary, chiral, non-racemic ; t-Butyl(phenyl)phosphinothioic acid, homochiral ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Optically active alcohols (ee ≥ 98%) such as 1-phenylpropanol, 1-(2-naphthyl)ethanol, 1-tetralol, and 1-indanol were transformed into diethyl phosphates 7a-d. sBuLi/TMEDA  -  induced phosphate - phosphonate rearrangement in diethyl ether furnished tertiary α-hydroxyphosphonates 8a-d of high enantiomeric purity (ee 94-98%) in yields of 43-83% with retention of configuration. The enantiomeric excesses were determined by using homochiral t-butyl(phenyl)phosphinothioic acid as chiral solvating agent.
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    URL: http://dx.doi.org/10.1002/cber.19961291217
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    Hydride Addition to Coordinated S2CPR3 Ligands in Mononuclear Mn and Re Complexes: Phosphane-dithioformate Adducts as Five-electron Bridging Ligands (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1535-1540 
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    ISSN: 0009-2940
    Keywords: 1,1-Dithiolate ; Manganese complexes ; Rhenium complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The cationic tetracarbonyl complex cis-[Mn(CO)4-(S2CPCy3)]+ undergoes addition of hydride ion to the central carbon of the S2CPR3 ligand to afford, after spontaneous dimerization with loss of CO, the dimer [Mn2(CO)6{μ-S2C(H)PCy3}2] (5a), which was characterized by analytical and spectroscopic methods as well as by X-ray diffraction. In the molecule of 5a each S2C(H)PCy3- ligand is coordinated to one manganese in an η2-S,S′ chelate fashion, and one sulfur of each ligand serves as a bridge to bind the other manganese atom, thus forming a distorted Mn2S2 square. This appears to be a very stable arrangement. Compound 5a can be more easily prepared by treating the perchlorato complex [Mn(CO)3(S2CPCy3)(OClO3)] (2a) with NaBH4. This procedure is general and can be used for the preparation of several derivatives containing either manganese or rhenium [M2(CO)6{μ-S2C(H)PR3}2] 5a-d. The reaction of cationic tricarbonyl complexes [M(CO)3(S2CPR3)(PPh3)]PF6 (M = Mn, Re) with NaBH4 produced the same dimers 5a or 5c by displacement of the PPh3 ligand. Treatment of the dimer 5a with excess PEt3 or P(OMe)3 leads to the cleavage of the bridges and loss of one CO and the PR3 group from the S2C(H)PR3 unit to afford ultimately the dithioformate complexes [Mn(CO)2(S2CH)(L)2] [L = PEt3, P(OMe)3].
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    Zinkorganische Phosphaniminato-Komplexe mit Heterocuban-StrukturHerrn Prof. Dr. Armin Berndt zum 60. Geburtstag gewidmet. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1621-1625 
    Details
    ISSN: 0009-2940
    Keywords: Organo-zinc compounds ; Phosphaneiminato complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Organo-Zinc Phosphaneiminato Complexes with Heterocubane StructureThe organo-zinc heterocubanes [ZnR(NPMe3)]4 with R = CH3 (1) and n-C4H9 (2) were prepared by the reaction of [ZnBr(NPMe3)]4 with MeLi and nBuLi, respectively, in hexane solution. In a similar reaction of nBuLi with [ZnI(NPMe3]4 the phosphaneiminato complex [Zn4I(nBu)4(NPMe3)3] (3) is formed. 1-3 were characterized by IR, NMR and MS spectroscopy, and by crystal-structure determinations. 1 and 2 possess heterocubane structures in which the zinc atoms are linked via μ3-N bridges of the phosphaneiminato groups, and all bond angles in the Zn4N4 core are close to 90°. A distorted heterocubane structure is observed for 3 with one of the NPMe3 moieties replaced by an iodine atom.
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    Generation and Synthetic Application of Metallated Methyl Isopropenyl Ether, A Substitute for Acetone Enolate (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 45-48 
    Details
    ISSN: 0009-2940
    Keywords: Metallated methyl isopropenyl ether ; Tetrahydrofurans ; 1-Oxabicyclo[4.3.0]heptanes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Methyl isopropenyl ether (1) has been metallated at low temperature with a 1:1 molar mixture of n-BuLi/t-BuOK in THF-hexane, and subsequently functionalized with a variety of electrophilic reagents. At temperatures higher than - 30°C, the metallated methyl isopropenyl ether (2) decomposes with formation of allene. When the suspension of 2 is allowed to warm up to room temperature in the presence of an additional equivalent of n-BuLi, the intermediary allene is converted into 1-propynyllithium (2c), which reacts with propylthiocyanate to give 1-propylthio-1-propyne (4). Some of the functionalization products were subjected to acidic hydrolysis affording the expected methyl ketones.
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    Asymmetric Catalysis, 105Part 104: Ref.. Stereoselective Hydrogenation of Folic Acid with Immobilized Optically Active Rhodium(I)/Diphosphane Catalysts (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 55-62 
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    ISSN: 0009-2940
    Keywords: Diastereoselective hydrogenation ; Folic acid ; Immobilized optically active rhodium(I)/diphosphane catalysts ; Leucovorin ; HPLC analysis of 5-formyltetrahydrofolic acid derivatives ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: For the hydrogenation of the C=N bonds in the pyrazine ring of the vitamin folic acid (1) optically active rhodium(I)/diphosphane complexes immobilized on supports such as silica gel or Al2O3 were used. The reduction was carried out at 50 bar hydrogen pressure in an aqueous solution buffered to pH 7. Thus, 5,6,7,8-tetrahydrofolic acid (2) was obtained which contains a new asymmetric center at C-6 of the pterine system. Therefore, in combination with the (S) configuration of the natural L-glutamic acid part of the molecule two diastereomers with (6S,S) and (6R,S) configuration arise. The relatively unstable tetrahydrofolic acid (2) was converted into its 5-formyl derivative folinic acid (4) by treatment with methyl formate/formic acid in a 5:1 mixture of DMSO/pyridine. The Ca salt of folinic acid (4) is the widely used drug leucovorin. The diastereomers were separated by silica gel HPLC. To the column bovine serum albumine (BSA) is covalently bound. With optically active rhodium(I)/diphosphane catalysts, immobilized on silica gel supports, a diastereoselectivity of up to 90% could be achieved in the hydrogenation of folic acid (1).
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    Hexahydro-closo-hexaborane as a Ligand in Coordination Compounds: Syntheses and Crystal Structures of [M2(μ-bis-η3-B6H6)(PPh3)2] )M = Cu, Au) (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 405-408 
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    ISSN: 0009-2940
    Keywords: Hexahydro-closo-hexaborates ; Boron ; Bridging ligands ; NMR spectroscopy ; Gold ; Copper ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: By reaction of (PPh3)3 CuCl and PPh3AuCl with [B6H6]2- in organic media, dinuclear complexes are formed containing the hexaborate as a bridging ligand coordinated to the metal centers by opposite B3 facets of the B6 cluster in a trihapto mode. This is verified by single-crystal X-ray structural analysis of the isotypical (Paā) compounds [Cu2μ-bis-η3-B6H6)(PPh3)2] (1) and [Au2(μ-bis-η3-B6H6)(PPh3)2)] (2) which showed the metal centers to be very close to the B3 plane [1.92 (1), 2.10 (2) Å. The 11B NMR spectra of the two compounds feature doublets, at δ= -15.32 in 1 and at -11.51 in 2, which are significantly shifted downfield in comparison to [B6H6]2- (δ= -17.2).
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    Crown Thioether Chemistry: Novel Silver(I) Complexes of 1,3-Dithiole-Annelated 1,4,7-Trithiacyclononane (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 425-429 
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    ISSN: 0009-2940
    Keywords: Silver complexes ; Crown compounds ; Thioethers ; 1,3-Dithioles ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The coordination chemistry of two crown thioethers 2,5,8,10,12-pentathiabicyclo[7.3.0]dodeca-1)9)-ene-11-thione (L) and -11-one (L') with Ag1 has been investigated by structural methods. Both thioethers act as tridentate ligands coordinating the silver ion in a trigonal fashion. In the case L, the 11- thione sulfur is coordinated additionally by another silver ion, to yield a polymeric chain with a distorted-tetrahedral geometry about the metal ion. Despite differing only in its carbonyl chalcogen, L' forms six-coordinated, monomeric complexes.
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    Unsymmetric Dinucleating Ligands for Metallobiosite Modelling (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 433-442 
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    ISSN: 0009-2940
    Keywords: Metallobiosites ; Metalloproteins ; Metalloenzymes ; Dinucleating ligands ; Transition metals ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Awareness of the asymmetric nature of numerous dinuclear metallobiosites and of the ability of the individual metal ions to have quite distinct roles in the functioning of the metalloenzyme concerned has led to a search for carefully designed unsymmetric dinucleating ligands that will give dinuclear complexes capable of acting as models for the metallobiosites. This review surveys progress made in the design and synthesis of complexes capable of serving as models for donor atom, coordination number and geometric asymmetries found at dinuclear metal centres.
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    URL: http://dx.doi.org/10.1002/cber.19971300402
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    Chemie polyfunktioneller Moleküle, 125Part 124: Ref. Synthese und Kristallstruktur von N,N,N′,N“,N-Pentamethyl-diethylentriamin-cokoordiniertem Kalium-bis(diphenylphosphanyl)amidHerrn Prof. Dr. Gerhard Herberich zum 60. Geburtstage gewidmet. (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 141-144 
    Details
    ISSN: 0009-2940
    Keywords: Alkali metal organophosphanylamide ; Carbon-potassium bonding ; Phosphazane ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The metalation of bis(diphenylphosphanyl)amine [HN-(PPh2)2,1 with KOtBu at 95°C in toluene affords a pale yellow precipitate of potassium bis(diphenylphosphanyl)amide (3a). On addition of liquid N,N,N′,N“,N“-pentamethyldiethylenetriamine (PMDTA, 4) the precipitate dissolves in toluene at 115°C to give a yellow solution, from which yellow-green blocks of [(Ph2P)2NK·PMDTA] (3b) are obtained. X-ray analysis reveals that the coordination sphere of potassium consists of the chelating triamine ligand and [N(PPh2)2]- as N-donor as well as η1 and η2 C-donor with two phenyl fragments. No phosphorus coordination of [N(PPh2)2]- is observed.
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    Organophosphorus Compounds, 114. Tetracyclic Phosphorus-Aluminium-Carbon Compounds - Synthesis by Cooligomerization of Kinetically Stabilized Phosphaalkynes with Trialkylaluminium CompoundsDedicated to Professor Michael Hanack on the occasion of his 65th birthday. (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 255-259 
    Details
    ISSN: 0009-2940
    Keywords: Phosphaalkynes ; Triorganoaluminium compounds ; Cooligomerization ; Cage compounds ; Aluminium compounds ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: When the trialkylaluminium reagents 5 are allowed to react with phosphaalkynes 4 in n-pentane, a highly selective phosphaalkyne cyclotrimerization with incorporation of two organometallic units occurs (→ 6). The tetracyclooctane derivatives 6a-e represent the first examples of phosphorus-aluminium-carbon cage compounds. The polycyclic products 6 are able to function as ligands in transition-metal complexes (→ 7), which is illustrated by the reactions of 6b, c with nonacarbonyldiiron and pentacarbonyl(tetrahydrofuran)tungsten, respectively.
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    URL: http://dx.doi.org/10.1002/cber.19971300219
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    On the Ligating Properties of Sulfonate and Perchlorate Anions Towards Zinc (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 283-289 
    Details
    ISSN: 0009-2940
    Keywords: Zinc ; Sulfonate ligands ; Perchlorates ; Coordination modes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Attempts are reported to incorporate sulfonate and perchlorate anions as ligands in zinc complexes of tripodal ligands. Using tris(benzimidazolylmethyl)amine (BIMA) only the aqua complexes [ (BIMA)Zn-OH2](RSO3)(ClO4) and [(BIMA)Zn-OH2](RSO3)2(R=CH3, CF3, p-tolyl) were accessible. Using substituted pyrazolylborates (Tp*), the same three sulfonate anions were found to be ligands in the complexes Tp*Zn-OSO2R. Spectroscopic evidence for perchlorate coordination in Tp*ZnClO4 · 2 DMSO conflicts with crystallograpic evidence against it in Tp*ZnClO4 · pyridine. The crystal structures of [(BIMA)Zn-OH2](CH3SO3)2, TpCum,MeZn-OS02CH3, TPtBu,MeZn-OSO2C6H4-p-CH3, and [TpCum,MeZn · NC5H5]ClO4 were determined.
    Additional Material: 4 Ill.
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    Multiple Bonds Between Main-Group Elements and Transition Metals, CLXIV. Alkylrhenium(VI) Oxides-Synthesis and Characterization (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 295-298 
    Details
    ISSN: 0009-2940
    Keywords: Rhenium ; Oxides ; Alkyl ligands ; Dirhenium compounds ; Metal-metal interactions ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Most alkylrhenium(VII) oxides, e.g. ((cyclo)-C3H5)Re03 (2) are rather sensitive to temperature and moisture with the prominent exception of methyltrioxorhenium (1). The corresponding alkylrhenium(VI) oxides of formula [RR′(O)- Re(μ-O)]2 [R=R′=(cyclo)-C3H5 (3), iPr (4); R=CH3, R′=C2H5 (5), R=CH3, R′=iPr (6)] are much more stable in this regard. They can be handled in air at room temperature. They were synthesized from Re207 and dialkylzinc precursors, fully characterized and are available in much higher yields than their ReVII congeners. Mixed tetraalkyltetraoxodirhenium(VI) complexes (R # R′) synthesized from 1 and dialkylzinc compounds form as a mixture of cis/trans isomers. They are oily liquids at room temperature. The Re=O and Re-Re stretching force constants as a measure of the bond strengths, were determined from IR and Raman data.
    Additional Material: 3 Tab.
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    Hydroxy- and Carboxy-Substituted Allylsilanes: A Simple and Stereoselective Method of Preparation (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 335-340 
    Details
    ISSN: 0009-2940
    Keywords: Allylsilanes ; Superbases ; Metalations ; Stereoselectivity ; Cyclizations ; Silicon ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: When treated with two equivalents of a butyllithium/potassium tert-butoxide mixture, terminal olefins carrying unprotected hydroxy or carboxy groups generate allylmetal intermediates which can be trapped with chlorotrimethylsilane to afford functionalized (Z)-2-alkenyltrimethylsilanes. One equivalent of the superbasic reagent suffices if the unsaturated alcohols are first protected as acetals before being subjected to the metalation/silylation/hydrolysis sequence.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19971300306
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    Preparation, Properties, and Reactions, of Metal-Containing Heterocycles, XCVIPart XCV: E. Lindner, E. Bosch, R. Fawzi, M. Steimann, H.A. Mayer, K. Gierling, Chem. Ber. 1996, 129, 945-951.. Mono-, Di- and Trinuclear Metallacycloalkanes of the Iron-TriadDedicated to Professor Wolfgang Beck on the occasion of his 65th birthday. (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 347-356 
    Details
    ISSN: 0009-2940
    Keywords: Metallacycloalkanes ; Metallacycloalkenes ; Osmium ; Iron ; Cyclic ketones ; Metallacycles ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reaction of the bis(triflates) [F3CSO3-(CH)m-O3SCF3] [m = 5-10, 12, 14, 16 (1a-i) with Na2[Os(CO)4] in dimethyl either affords the osmacycloalkanes 2a, 2b and 2f-i (m = 5, 6, 10, 12, 14, 16), diosmacycloalkanes 3a-i (m = 5-10, 12, 14, 16), and triosmacycloalkanes 4a-i (m = 5-10, 12, 14, 16). The structure of 3f was investigated by an X-ray structural analysis. This 22-membered disomacycle crystallizes in the space group Pā with Z = 1. If the unsaturated cis-4-octen-1,8-diyl bis(trifluoromethanesulfonate) (5) is treated with Na2[Os(CO)4] the diosmacyclooctadeca-5,14-diene 6 is obtained. By treating the bis(triflates) 1a, b with Na2[Fe(CO)4] the corresponding ferracycloalkanes are formed only in situ. Insertion of carbon monoxide into the M-C σ bonds leads to the cyclic ketones 7a, d and to the diketone 8d.
    Additional Material: 4 Ill.
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    Enantioselective Catalysis, XIIIPart XII: U. Nagel, J. Leipold, Chem. Ber., 1996, 129815-821.. Preparative and Structural Chemistry of Chiral 3-(Diphenylphosphanyl)-pyrrolidiens and Their Palladium(II) Complexes (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 385-398 
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    ISSN: 0009-2940
    Keywords: Pyrrolidinephosphanes ; 3-Hydroxypyrrolidine ; 3-Diphenylphosphanylpyronlidine ; Salt effects ; Polymorphism ; Homogeneous catalysis ; Palladium ; Asymmetric catalysis ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The preparation of both enantiomers of 3-diphenylphosphanulpyrrolidiine (2) and several N-substituted derivatives together with two PdIi complexes of this ligand is reported. Form L-malic acid and L-hydroxyproline both enantiomers of 3-hydroxypyrrolidine are prepared without any problems due to epimerization. KPPh2 in the presence of LiCl is shown to be the most effective reagent for the synthesis of 2. The reported X-ray structure determination sof Pdl2 complexes show a rather rigid bicyclic hetero-norbornane skeleton. The flexibility of the other parts of the molecules is obvious in several polymorphs revealed by this method. This polymorphism is additionally investigated by a 31P-CP-MAS study. From solution 1-, 13C- and 31P-NMR studies it is concluded that the bicyclic hetero-norbornane skeleton is retained in solution.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19971300313
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    Reactions of Silicon-Silicon Bonds, VIFor part V, see ref.[1].. Reductive Trichloroslilylation Reactions Leading to Alkyl- and Dialkylaminobis(trichlorosilyl)phosphanesDedicated to Professor Walter Siebert on the occasion of his 60th birthday. (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 377-384 
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    ISSN: 0009-2940
    Keywords: Trichlorosilylation ; Dichlorophosphanes ; Silylphosphanes ; Amino(silyl)phosphanes ; Silicon /Reductions ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Reactions of hexachlorodisilane and of trichlorosilane/triethylamine with alkyl-and dialkylaminodichlorophosphanes RPCl2 1a-i [R = iPr: a; (Me3Si)2CH: b; R=1-adamantly: c: R=tBu: d; R=Et2N: e; R=iPr2M: f] furnish bis(trichlorosilyl)-phosphanes RP(SiCl3)2 3a-f. However, when less bulky substituents are attached to the phosphorus atom, so that there is little steric crowding, the double reductive silylations leading from 1 to 3 are accompanied by side reactions and decomposition of 3. Therefore, only 3b, 3c, 3d, and 3f wre isolated in a pure state. These compounds are more readily prepared by the; trichlorosilane/triethylamine method. 1H-, 31P- and 29Si-Nmr spectra confirm their constitution. The structure of solid 3f, the first aminobis(trichlorosilyl)phosphane, was determined by X-ray crystallography. 3f contains a phosphorus atom in a pyramidal environment surrounded by two silicon atoms and a planar nitrogen atom of the diisopropylamino group.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19971300312
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    Formation of the Digallium Compound [(C5C6)2N3](R)Ga-Ga(R)[N3(C6H5)2] with Two Bis(trimethylsilyl)methyl Groups and Two Terminal Chelating Diphenyltriazenido Ligands (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 417-420 
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    ISSN: 0009-2940
    Keywords: Gallium ; Low-valent compounds ; Gallium-gallium bond ; Terminal triphenytriazenido ligand ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Tetrakis[bis(trimethylsilyl)methyl]digallane (4) 1 reacts with 1,3-diphenyltriazene to yield two compounds, which were both characterized by a crystal structure determination. The gallium-gallium bond is retained in the yellow derivate [(H5C6)2N3](R)Ga-Ga(R)[N3(C6H5)2 2 [R = CH(SiMe3)2], which is formed by a ligand exchange reaction and shows two terminal chelating triazenido ligands besides two bis(trimethylsilyl)methyl groups; the Ga—Ga bond length is 245.79(6) pm. The second product is the orange dialkyl(diphenyltriazenido)gallium derivative R2Ga[N3(C6H5)2] 3, where the triazene has reacted as an oxidant by the cleavage of the Ga—Ga bond and probably by release of elemental hydrogen.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19971300317
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    The Electronic Structure of [Te15Br4][MoOBr4]2 and Some General Aspects of Bonding in “Classical” and Hypervalent Tellurium Halides (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 463-472 
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    ISSN: 0009-2940
    Keywords: Hypervalent compounds ; Tellurium ; Polycations ; Molecular Orbital Theory ; Band structure ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Approximate MO and band structure calculation are used to analyze the bonding in the recently synthesized paramagnetic, semiconducting phase [Te15Br4]2+. The [Te15Br4]2+ chains are very similar to those in the tellurium subhalide Te2Br. The electronic structure and bonding within these chains is analysed and the possibility of hypervalency in both [Te15Br4][MoOBr4]2 and Te2Br is discussed. The bonding in the classically hypervalent molecule TeBr42- and a model Te3Br24- is compared to that of the infinite system. Our calculations indicate that both [Te15Br4][MoOBr4]2 and Te2Br contain weakly hypervalent Te atoms and that the interesting electronic properties of [Te15Br4][MoOBr4]2 arise within the distinct sublattices, which do not interact significantly.
    Additional Material: 12 Ill.
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    Heterobimetallic Complexes with a Propynylidene C3-Bridge: General Synthetic Routes to Bimetallic Ethynylcarbene Complexes (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 479-488 
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    ISSN: 0009-2940
    Keywords: Heterobimetallic complexes ; Carbene complexes ; Alkynes ; Coupling reaction ; Bridging ligands ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Sequential reaction of the dimethylamino(trimethylsilylethylnyl)carbene complexes [(CO)5M'=C(NMe2)C≡CSiMe3] [M' = W (1a)] with KF/THFMeOH, nBuLi and transition metal halides, [XMLn], affords heterobimetallic propynyliden complexes of the type [(CO)5M'=C(N-Me2)C≡CMLn] [MLn = Ni(PPh3) Cp (4a, b). Ni(PMe2Ph)2- {Mes) (Mes=2,4,6-C6H2Me3) (5a), Rh(CO)(PPh3)2 (6a), Fe(CO)2Cp (7a,b)]. In contrast, reaction of 1a with MeLi · LiBr and [IFe(CO)2Cp] yields the novel N-metallated complex [(CO)5W=C{N(ME)Fe(CO)2Cp}C≡CSiMe3] (8a). The complexes [(CO)5M'=C(NMe2)C≡CMLn=Fe(CO)2Cp (7a, b), Ru(CO)2Cp (10a,b), Ru(CO)(PPh3)Cp (11a), Mn(CO)5 (12a), Re(CO)5 (13a)] are accessible by Pd-catalyzed coupling of the C-stannylated carbene complexes [(CO)5M'=C-(NMe2)C≡CSnBu3] (9a, b) with [XMLn]. The related monomethylaminocarbene complexes [(CO)5M'=C(NHMe)C≡ CSnBu3] (16a, b), obtained by stannylation of [(C))5M'=C(NHMe)C=CH] (15a, B) with Bu3SnNEt2, react with [IFe(CO)2Cp] to give the bimetallic complexes [(CO)5M'=C(NHMe)C≡CFe(CO)2Cp] (17a, b). The complexes 4a, 5a, 7a and 10a were characterized by X-ray structural analysis. The spectroscopic and structural data suggest that the two metal centers in 4-7, 10-13, and 17 interact only weakly.
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    Synthesis and Molecular Structure of a Rhenium Complex Derived from 8a-Amino-6-methyl-ergolineDedicated to Professor Roland Mayer on the occasion of his 70th birthday. (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 839-841 
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    ISSN: 0009-2940
    Keywords: Rhenium ; Technetium ; 8a-Amino-6-methyl-ergoline ; Chelates ; Structure elucidation ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Current research in radiopharmaceutical chemistry is aimed at the design of technetium-based receptor-binding radiotracers because of the excellent nuclide properties of the isotope 99mTc. Tc tracers and the corresponding complexes of rhenium, as the inactive surrogate of Tc, are required to imitate organic agonists or antagonists of the receptor. We have started studies with ergolines, which are known to be dopamine substitutes. The present report deals with the functionalization of 8α-amino-6-methyl-ergoline (2) with a 2-mercaptoacetyl group, and the subsequent synthesis of the first rhenium complex containing a pendent ergoline moiety [Re- O(SSS)(RS)] (HSSSH = HS-CH2CH2-S-CH2CH2-SH and RSH = 8a-amino-N-(2-mercaptoacetyl)-6-methyl-ergoline) (4). The molecular structure of the rhenium complex was determined by X-ray crystal structure analysis.
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    Aminotroponimines as Ligands for Yttrium and Lanthanide Complexes (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 859-862 
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    ISSN: 0009-2940
    Keywords: Yttrium ; Lanthanum ; Samarium ; Lanthanides ; Aminotroponiminate ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reaction of N-isopropyl-2-(isopropylamino)troponimine, [(i-Pr)2ATI]H, with KH in THF affords [(i-Pr)2ATI]K. This is a useful starting material for the preparation of the mono-, bis- and tris-substituted compounds [[i-Pr)2ATI]YCl2-(THF)2}2, [(i-Pr)2ATI2Y[O(2,6,t-Bu2C6H3)] and [(i-Pr)2-ATI]3Ln (Ln = Y, La, Sm), which can be obtained from ([i-Pr)2ATI]K and LnX3 and LnX3 (X = Cl, I), or Y[O(2,6-t-BuC6H3)]3. All compounds have been characterized by spectroscopic methods. The monosubstituted yttrium complex {[(i-Pr)2ATI]YCl2(THF)2}2 has also been investigated by single crystal X-ray diffraction.
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    On the Synthesis of Sulfoxonium Ylides: New Aspects of the Chemistry of 1,3-Dithietane 1,1,3,3-Tetraoxide and 1,3,5-Trithiane 1,1,3,3,5,5-Hexaoxide (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 161-167 
    Details
    ISSN: 0009-2940
    Keywords: Sulfoxonium ylides ; 1,3-Dithietane 1,1,3,3-tetraoxide, silylated ; 1,3,5-Trithiane 1,1,3,3,5,5-hexaoxide, silylated ; Disulfenes, unsaturated ; Disulfenes, dianions of ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Sulfoxonium ylides 3a-h were synthesized by silylation of the cyclic methylene disulfones 1,3-dithietane 1,1,3,3-tetraoxide (1) and 1,3,5-trithiane 1,1,3,3,5,5-hexaoxide (4) with the silylating agents silyl nonafluorobutanesulfonates. The structure and constitution of the ylides were established with 1H-NMR, 13C-NMR, 29Si-NMR spectroscopy, mass spectrometry, and elemental analysis. On the route to the sulfoxonium ylides a new class of unsaturated disulfenes 7, 8, 12, 13 of 1 and 4 were synthesized via Knoevenagel and substitution reactions. Dianions of newly formed alkyl disulfenes 16a, b, e, f, and the trianion 17 were prepared and characterized by 1H-NMR and 13C-NMR spectroscopy and compared with the results of the ylides.
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    URL: http://dx.doi.org/10.1002/cber.19961290209
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    C-H Bond Activation of Simple Alkenes with (C5H5)CO Fragments: Preparation, Molecular Structure, and Dynamical Behaviour of Tri- and Tetranuclear Cyclopentadienylcobalt Cluster complexes with μ-Cycloalkyne Ligands (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 593-603 
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    ISSN: 0009-2940
    Keywords: C-H activation ; Alkyne complexes ; Cyclopentadienyl cobalt ; Fluxionality ; Hydrido complexes ; Clusters ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Vicinal C-H bonds of the cycloalkenes CnH2n (n = 5-8) were activated upon treatment under mild conditions with reactive sources of the (C5H5)CO fragment. With [C5H5)CO(C2H4)2] (2a), the trinuclear cluster complexes [H2((C5H5)CO)3(μ3-C2(CH2)n-2)] (5a: n = 5; 5c: n = 5d: n = 8) were formed. Using the more reactive [(C5H5)2Co]/K, 5a-5dwere obtained, along with small amounts of the tetranuclear [{(C5H5)CO}4r{μ4-C2(CH2)n-2}] (8a-c: n = 5-7). X-ray structure analyses of 5c, d and 8b, c were performed. A μ-‖ (orμ3-η1:η2:η1) coordination of the cycloalkyne ligands was found in the trinuclear cluster complexes. The tetranuclear 8b, c had the cycloalkynes quadruply bridging (μ4-η1:η2:η2:η1_ a butterfly arrangement of the metal atoms. The acetylenic carbon-carbon bonds are considerably lengthened upon coordination [1.392(4), 1.398(3) å in 5c d; 1.464(8), 1.499(5) Å in 8b, c]. Three dynamic processes - alkyne “walk” on top of the CO3 triangle, μ2-hydride migration, and μ2/μ3-hydride exchange - are operational in the trinuclear 5a-d. Dynamic NMR data for 5a are consistent with a “windshield-wiper” mechanism for the alkyne migration. Hydride exchange is associated with a higher energy barrier, and is probably and independent dynamic process.
    Additional Material: 6 Ill.
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    Organoamido- and Aryloxolanthanoids, 15Part 14: Ref. [1a].. Organometallic Compounds of the Lanthanoids, 116Part 115: Ref. [1b].. Syntheses of Low Coordination Number Divalent Lanthanoid Organoamide Complexes, and the X-ray Crystal Structures of Bis[(N-2,6-diisopropylphenyl)(N-trimethylsilyl)amido]bi(tetrahydrofuran)samarium(II)and -ytterbium(II) (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 409-415 
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    ISSN: 0009-2940
    Keywords: Mercury ; Lanthanides ; Lanthanoid(II) complexes ; (N-2,6-Diisopropylphenyl)(N-trimethylsily)amide complexes ; Bis(trimethylsilyl)amide complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The Mercury(II) amide complex Hg[N(SiMe3)(2,6-iPr2C6H3)]2 (1) was prepared by reaction of HgBr2 with Li[N(SiMe3) 2,6-iPr2C6H3)] in diethyl ether solvent. Redox transmetallation reactions of 1 with elemental samarium, europium or ytterbium in THF solvent (THF = tetrahydrofuran), generated the novel divalent complexes Ln[N(SiMe3)(2,6-iPr2C6H3]2(THF)2 with Ln = Sm (2), Eu (3) and Yb (4). 4 was also synthesized by reaction of elemental ytterbium, HgPh2 and HN(SiMe3)(2,6-Me3)2]2(THF)2 [Ln = Sm (5), Yb (6)] by reaction of the metals with HgPh2 and HN(SiMe3)2. Thermal desolvation of 4 under high vacuum gave Yb(N)(SiMe3)2,6-iPr2C6H3)]2 (THF) (7), whereas under identical conditions 6 yielded the solvent-free complex [Yb[N{SiMe3)2]2]2. (8). The new compounds 1-4 and 7 are hydrocarbon soluble and 171Yb-NMR spectra were recorded for 4, 6, 7 and 8. X-ray crystal structure determinations of 2 and 4 revealed four-coordinate, distorted tetrahedral metal environments augmented by weak Ln…ipso-C(aryl) interactions.
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    Synthesis and Structure of 2,2′ -Boryl-, Germyl-Silyl-, and Stannyl-Substituted 1,1′ -Binaphthyl SystemsDedicated to Professor Hans Paulsen on the occasion of his 75th birthday. (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 923-932 
    Details
    ISSN: 0009-2940
    Keywords: Biaryls ; Boron ; Chirality ; Cooperative Effects ; Lewis acids ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A number of Lewis acid binaphthyl systems, substituted in 2-or 2,2′-position, are synthesized by lithiation of 2,2′-dibromo-1,l ′-binaphthyl (5), followed by addition of various electrophiles. Stepwise lithiation and subsequent borylation with trimethyl borate leads to the bromoboronic acid 6, which can be stabilized by esterification with pinacol giving 7. By increasing the reaction mixture to 2 equiv. of n-butyllithium and 2 equiv. of methyl borate the path to the binaphthylmonoboronic acid ester 9 is opened up. A further increase in the quantity of electrophile also leads to the binaphthylbisboronic acid ester 12. The 2,2′-disubstituted silyl, germyl, and stannyl derivatives 13a-15a are accessible in good yields. Treatment with boron halides leads exclusively to methyl/halogen exchange, giving the bidentate Lewis acids 13b-15b, the former of which can be bridged by oxygen.Only in case of the bis(tributylstannyl)binaphthyl 16a does ipso substitution occur in the presence of boron trichloride, giving the bis(dichloroboryl)-substituted binaphthyl 16b which can then be hydrolysed to 11. The structures of the majority of the compounds were investigated by X-ray diffraction. In case of the 2,2′-disubstituted compounds 13a-15a the naphthyl groups are orientated perpendicular to each other. The intra- and intermolecular interactions are dominated by this binaphthyl system. In case of the oxygenbridged compounds 13c and 14c the angle between the naphthyl planes decreases to about 70°. This also has an effect on the packing of the molecule; in this instance the orientation of two naphthyl in neighbouring molecules is nearly parallel. The structure of the diboronic acid is dominated by intra- and intermolecular hydrogen bonding.
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    Temperature-dependent Ring-Opening and -Closure of a Cyclic Phosphane-BoraneDedicated to Professor Gottfried Huttner on the occasion of his 65th birthday. (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 951-954 
    Details
    ISSN: 0009-2940
    Keywords: Phosphane-boranes ; Medium-sized rings ; Ring opening and closure ; Temperature-dependent NMR studies ; Phosphorus ; Boron ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A phosphane-borane (3) with the P-B bond integrated into a seven-membered ring was prepared from 4-pentenyl-diphenylphosphane (4) by hydroboration using 9-borabicyclononane (9-BBN). The product was confirmed to have a ring structure in the solid state by single crystal X-ray diffraction. The P-B distance of 2.057(2) Å is indicative of a standard donor-acceptor bond similar to the type found in homologous five- and six-membered rings. The room-temperature 31P-NMR signal of the compound in various solvents (δ ≈ - 15) is not compatible with the cyclic structure and suggests that ring opening occurs as the compound is dissolved. Variable-temperature NMR work corroborated this assumption, and the enthalpy of ring closure was determined to be ΔH = -30.5(4) kJmol-l. In CD2C12 at -90°C, δ31P is shifted to +3.5 ppm to low field, suggesting virtually complete ring closure under these conditions.
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    The Coordination Chemistry of Fluorocarbons: Group-I and Group- II Metal Ion Complexes of Fluoro Macrocycles (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 963-968 
    Details
    ISSN: 0009-2940
    Keywords: Fluorine ; Macrocycles ; Complexes ; Sodium ; Barium ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Two new fluoro macrocycles BenzoFN2O3 and F(N2O2)2C2H4 were synthesized in the reactions of 1,3-bis(bromomethyl)-2-fluorobenzene with benzo-diaza-15-crown-5 and 1,2-bis(diaza-12-crown-4)ethane, respectively, in 30% yield each. Close CF...metal ion interactions in the respective alkaline metal complexes in solution are evidenced by characteristic shifts of the 19F-NMR resonances of up to δ = 18.7 relative to the free ligand and by a decrease of the 1J(CF) coupling constant of up to 20 Hz, which is most pronounced in BenzoFN2O3 · Li+ and F(N2O2)2C2H4 · K+. In BenzoFN2O3· Li+ a1J(19F-7Li) of 15.5 Hz was observed, which is indicative very close CF...Li+ interactions in solution. In the X-ray crystal structures of BenzoFN2O3 · Na+ [CF⃛Na+ 246.8(2) pm], 26-fluoro-4,7,13,16-tetraoxa-1, 10-diazatricyclo[ 8.8.7.1 20,24 ] - hexacosa-20,22,24(26)triene · Na+ (CF⃛Na+ 267.1(2) pm) and 21 -fluoro-3,6,9,12,15,18-hexaoxabicyclo[ 18.3.1 1,20]heneicosa- l(24),20,22-triene. Ba2+ [CF⃛Ba2+ 299.0(3) pm] short CF⃛metal interactions were found. Such close CF⃛metal ion interactions do not result in a lengthening of the C-F bonds, which is not a sign of weak CF⃛metal ion interactions, since a Cambridge Structural Database search revealed that a shortening of the C-O bond length is also not observed in crown ether complexes of alkaline metals.
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    Organophosphorus Compounds, 118Part 2: 117: Ref1. Reactions of 1-Chloro-1H-phosphirenes with Nucleophiles (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 711-723 
    Details
    ISSN: 0009-2940
    Keywords: Phosphorus heterocycles ; 1H-Phosphirenes ; Nucleophilic substitution reactions at 1H-phosphirenes ; Metal-complexation of functionalized 1H-phosphirenes ; Carbonyl complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The halogen atoms in the 1-chloro-1H-phosphirenes, 5a-c, are easily substituted on reaction with organolithium and Grignard reagents, 14a-p, with formation of the corresponding O-, N-, C-, Si-, and Ge-substituted 1H-phosphirenes, 15a-t. C1/H exchange reactions also occur on reaction with lithium metal hydrides (5a → 17). Furthermore, substitution reactions are also realized with the alkali metal borates, 18a-g (→19a-g); the same is true for reactions with trimethylsilyl cyanide and azide (→22a-d). Some of the substitution products have been characterized in the form of their metal complexes, 16, 23, 24, and 25.
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    Synthesis of Germatranyl Derivatives of Esters of Carboxylic Acids via Organometallic (Si, Ge, Sn) Reagents (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 739-746 
    Details
    ISSN: 0009-2940
    Keywords: Germatranes ; Organotrihalogenogermanes ; Organometallic (Si, Ge, Sn) reagents ; Transmetallation ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Trialkylstannyl esters of tris(2-hydroxyalkyl)amines, N(CH2CHROSnAlk3)3 (9-11 (R = H, Me; Alk = Et, Bu), react with X3GeC(R1)(R2)COOR3 (12-17) (X = Cl or Br; R1, R2=H, Me, Ph, SiMe3, COOEt; R3=Me, Et) to give esters of α-germatranylcarboxylic acids, N(CH2CHRO)3GeC(R1)(R2)-COOR3 (1-8), in high yields. The synthesis of esters 12-17 is reported. Esters of α-germatranyldiphenylacetic acid 24 and 25 can be obtained by treatment of diphenylketene with Et3SnOMe to give in situ Et3SnC(Ph2)COOMe (23), followed by reaction with GeCl4 to give in situ Cl3GeC(Ph2)COOMe (22 and further reactions with 9 or 11, respectively. Reduction of germatrane 6 with LiAlH4 in diethyl ether leads to cleavage of the germanium-carbon bond with subsequent formation of (2-hydroxyethyl)trimethylsilane. The crystal structures of 3, 6 and 7 are reported. 1-Acyloxygermatranes 26 and 27 are obtained by treatment of 1-methoxygermatrane (28) with diphenyl- and dichloroacetic acid, respectively.
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    Base-Induced Synthesis of a Tetrastannatriazabicyclo[3.1.1]heptane from Tris)dimethylchlorostannyl)amineDedicated to Professor W. Sieber on the occasion of his 60th birthday. (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 765-769 
    Details
    ISSN: 0009-2940
    Keywords: Tin - Nitrogen cage compounds ; Sn—X—Sn intramolecular bridges ; Distannylamine pyridine adduct ; Tin ; Moessbauer spectroscopy ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Tris(dimethylchlorostannyl)amine (2a) reacts with pyridine in a 3:4 molar ratio to produce the tin-nitrogen containing bicyclo[3.1.1]heptane (3) with elimination of the adduct Me2SnCl2·2 py. Treatment of the distannylamine 2,6-[Pr2H3N(SnMe2Cl)2 (4) with pyridine, however, leads to the formation of the 1:1 pyridine adduct 4 and this can be regarded as a model to explain the route to 3. The molecular structures of 3 and 5 were determined by multinuclear magnetic resonance spectroscopy in solution, as well as by X-ray structure analysis of their crystals. Typical structural features for both compounds are intramolecular Sn—X—Sn bridges. Support for the structures comes from MS fragmentation patterns, IR spectra, and the Mössbauer spectra.
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    Thermal Reactions of 5-Alkylidene-4,5-dihydro-3H-1,2,4(λ3)-diazaphospholes (4-Phosphapyrazolines) - A Route to Various P—Heterocycles and to 2-PhosphabutadienesDedicated to Professor M. Hanack on the occasion of his 65th birthday. (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 779-788 
    Details
    ISSN: 0009-2940
    Keywords: 1,2,4-Diazaphospholes ; Phosphiranes, alkylidene- ; 2-Phosphabutadienes ; Phosphorus heterocycles ; pyrazolines, thermolysis ; Rearrangements ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The 5-alkylidene-4,5-dihydro-3H-1,2,4(λ3)-diazaphospholes (4-phosphapyrazolines) are thermally much more stable than related compounds without the exocyclic double bond. Thermolysis reactions typically occur in the range 110-150°C in toluene solution, and different, mostly competing, reaction pathways are observed. Thermal extrusion of nitrogen from 8a-g gives rise to β-phosphanaylsiloxyalkenes 10, benzo[c]-phosphole derivatives 11, 14 and 115, (β-siloxyalkylidene)-Phosphiranes 12, and dihydro-1,3-oxaphospholes 13. The thermolysis of 5-alkylidene-4,5-dihydro-4-trimethylsilyl-3-trimethylsilyloxy-3H-1,2,4-dizaphospholes 17 afforded three products, including the highly substituted and stable 2-phosphabutadienes 18 formed by nitrogen extrusion and rearrangement. Finally, the 4-chloro-3-trimethylsilyloxy-substituted heterocycle 21 was transformed at 170°C into 4H-1,2,4-diazaphosphole 23. The structures of 13c and 18a were determined by single-crystal X-ray diffraction.
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    Addition von CS2 und anderen Heteroallenen an die 16-Elektronen-Osmium(0)-Komplexe trans-[OsCl(NO)(PiPr2R)2] (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 405-410 
    Details
    ISSN: 0009-2940
    Keywords: Osmium(0) complexes ; Nitrosyl complexes ; CS2, COS, SCNPh, and Ph2C=C=O as bidentate ligands ; Protonation and methylation reactions ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Addition of CS2 and Other Heteroallenes to the 16-Electron Osmium(0) Complexes trans-[OsCl(NO)(PiPr2R)2]The coordinatively unsaturated 16-electron compounds trans-[OsCl(NO)(PiPr2R)2] (1: R = iPr; 2: R = Ph) react with CS2 and COS to form the 1:1 adducts [OsCl(NO){κ2(C,S)-S=C=S}(PiPr2R)2)] (3, 4) and [OsCl(NO){κ2(C,S)-S=C=O}-(PiPr2R)2] (6, 7), respectively. While compounds 3, 4 are inert toward PMe3, the Os(COS) complexes 6, 7 react with tri-methylphosphane by abstraction of sulfur to give (OsCl(NO)-(CO)(PiPr2R)2] (8, 9). From 1 or 2 and phenylisothiocyanate the corresponding 1:1 adducts (OsCl(NO){κ2(C,S)-S=C=NPh}(PiPr2R)2] (10, 11) are obtained. Protonation and methylation reactions of 10 (R = iPr) with HBF4 or CF3SO3Me lead, by addition of the electrophile to the C=N nitrogen atom, to the formation of [OsCl(NO){κ2(C,S)-S=CNHPh}-(PiPr3)2]BF4 (12) and [OsCl(NO){κ2(C,S)-S=CN(Me)Ph}-(PiPr3)2]CF3SO3 (13). Treatment of 1 with diphenylketene yields [OsCl(NO){κ2(C,O)-O=C=CPh2}(PiPr3)2] (14). The X-ray structure analyses of 10 and 14 confirm the coordination of phenylisothiocyanate via S and C and of diphenylketene via O and C, respectively.
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    8-quinolylcyclopentadienyl, a ligand with a tailored fit for chelate complexes (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 459-463 
    Details
    ISSN: 0009-2940
    Keywords: Cyclopentadienes ; Half-sandwich complexes ; Intramolecular nitrogen donors ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 8-Lithioquinoline reacts with 2,3,4,5-tetramethylcyclopentenone to give 8-quinolylcyclopentadiene (1/2) after acidic workup and treatment with ammonia. Two of the possible three isomers are formed; the acidic protons on the Cp rings show unusual downfield shifts in the 1H-NMR spectra. Treatment with strong bases led to the intensely coloured anionic 4 which was converted into the trimethylsilyl derivative 5. This is a suitable starting compound for the trihalotitanium and -zirconium compounds 6 and 7. The two complexes were investigated by crystal structure analyses. In both cases the quinolyl nitrogen atom is coordinated to the metal.
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    Über das Silaethen tBu2Si=C(SiMe3)2 und die Struktur sowie Reaktivität seines [4 + 2]-Cycloaddukts mit Ph2C=OFrau Prof. Marianne Baudler zum 75. Geburtstag gewidmet. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 471-478 
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    ISSN: 0009-2940
    Keywords: Silaethenes ; [4 + 2] Cycloadditions ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: On the Silaethene tBu2Si=C(SiMe3)2, and the Structure and Reactivity of Its [4 + 2] Cycloadduct with Ph2C=OFrom tBu2SiF—CLi(SiMe3)2 by LiF elimination only Me2Si= C(SiMe3)(SiMetBu2) (1b) instead of tBu2Si=C(SiMe3)2 (1a) is isolated. With benzophenone, silaethene 1b (from its THF adduct 1b · THF) forms at -78 °C a yellow [4 + 2] cycloadduct (5) and a colorless [2 + 2] cycloadduct (6). With increasing temperature 5 transforms into 6, and 6 transforms -more slowly - into the yellow [4 + 2] cycloadduct (7) of 1a and Ph2CO. It follows from this that the migration equilibrium 1a ⇄ 1b really exists. The structure of 7 shows a planar —O—CPh=C6H5-framework with the cycloadded atoms Si and C from -tBu2Si—C(SiMe3)2- located above the plane. The =C6H5—C bond (1.62 Å) is exceptionally long. 7 is a source for 1a which is trapped by acetone (formation of an ene product) and by benzaldehyde [formation of a [2 + 2] cycloadduct, unstable against cycloreversion into PhHC=C(SiMe3)2 and tBu2SiO-containing substances]. Reaction of 7 with trimethylsilyl azide, less reactive than acetone or benzaldehyde, leads - by way of 1a which transforms into 1b - to a trapping product of 1b (formation of a [3 + 2] cycloadduct, unstable against transformation into (RMe2Si)(Me3Si)CN2 with R = (Me3Si)2N, or cycloreversion into (tBu2MeSi)(Me3Si)CN2 and Me2SiNSiMe3-containing substances). Reaction of 1b or 1b · THF with acetone leads only to an ene reaction product of 1b. This means, that only undetectable amounts of 1a or 1a · THF are in equilibrium with 1b or 1b · THF. A minor substance which is shown by NMR at low temperatures besides 1b or 1b · THF is interpreted as a rotamer of 1b or 1b · THF.
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    Organophosphorus Compounds, 112Part 111: Ref.[1].. Lewis Acid Mediated Spirocyclotrimerization of Kinetically Stabilized Phosphaalkynes - Key Step for the Selective Generation and Trapping of Triphospha Dewar BenzenesDedicated to Professor H. W. Roesky on the occasion of his 60th birthday. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 489-494 
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    ISSN: 0009-2940
    Keywords: Phosphaalkynes ; Phosphaalkenes ; Spirocyclotrimerization ; Triphospha Dewar benzenes ; Phosphaalkyne cyclooligomers ; Cage compounds, phosphorus-carbon ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: In the presence of Lewis acidic derivatives of group 13 elements, phosphaalkynes 7 undergo spirocyclotrimerization with incorporation of the corresponding Lewis acids to form 10a-f. Scope and limitations of this novel cyclooligomerization process are examined. Starting from the spirocyclotrimer 10a reaction with the Lewis base dimethyl sulfoxide, we have in hand for the first time a method for the selective generation of two isomeric triphospha Dewar benzene derivatives (18, 19). Both can be trapped efficiently by further reaction with the phosphaalkyne to furnish the two novel phosphaalkyne cyclotetramers 20 and 21, both still possessing a phosphorus-carbon double bond. In the case of 21, further functionalization of the phosphaalkene unit is possible by [3 + 2] cycloaddition with a nitrile oxide (→ 23).
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    Reaction of 1,3-Dialkyl-4,5-dimethylimidazol-2-ylidenes with 2-Bromo-2,3-dihydro-1H-1,3,2-diazaboroles (Alkyl=iPr and tBu)Dedicated to professor Adolf Zschunke on the occasion of his 60th birthday. (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 705-710 
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    ISSN: 0009-2940
    Keywords: Boron ; Diazaboroles ; Carbenes ; Heterocycles ; Imidazoles ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 2-Bromo-2,3-dihydro-1H-1,3,2-diazaboroles (3a-c) were synthesized by cyclocondensation of dilithiated 1,4-diazabutadienes (5a-c) with boron tribromide in hexane. 3a was also obtained by sodium amalgam reduction was conducted in ether solvents, diboroxane (2) resulted as the main product. Compound 3a and 1,3-dialkyl-4,5-dimethylimidazol2-ylidenes (6a, b) underwent halide displacement to afford the borolylimidazolium salts 7a, b. Compounds 2, 3a-c, and 7a, b were characterized by elemental analyses and spectroscopic methods (1H, 11B, 13C NMR; Ir; MS). The molecular structures of 2 and 7a were established by single-crystal X-ray diffraction analyses.
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    Well-Defined Metallodendrimers by Site-Specific Complexation (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 725-728 
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    ISSN: 0009-2940
    Keywords: Dendrimers ; Metal complexes ; Nanostructures ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Strong multiple complexation of transition metal ions, Cu(II), Zn(II) and Ni(II) with different generations of well-defined poly(propylene imine) dendrimers as multi(tridentate) ligands has been used to construct nanoscopic assemblies of defined structure and size incorporating a distinct number of metal ions from 2 up to 32.
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    Compounds of Germanium and Tin, 2lPart 20: Ref.[1]. A Tetraaryldigermene with a Short Germanium-Germanium Double Bond and a Nearly Planar Environment of Both Germanium AtomsDedicated to Professor Hans Bürger on the occasion of his 6oth birthday (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 735-738 
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    ISSN: 0009-2940
    Keywords: Germanium ; Digermenes ; Tin ; Germylenes ; Stannylenes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Treatment of GeCl2 · dioxane with the Grignard reagent RMgBr (R=2-tBu-4,5,6-Me3C6H) furnishes the tetraaryldigermene R2Ge=GeR2 (8). X-ray structure-analysis of 8 reveals a short Ge=Ge double bond, a nearly planar environment of both germanium atoms and extremely widened C—Ge—C angles of 128°. In solution, 8 dissociates into two germylene molecules R2Ge, which can be trapped with oxygen or by [4+1] cycloaddition reactions with 1,4-dihetero-1,3-dienes. A similar cycloadduct of a stannylene wa obtained by thermolysis of (R′2Sn)3 (R′=2,4,6-iPr3C6H2), in the presence of a 1,4-diazabutadiene and characterized by an X-ray structure-analysis.
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    Synthesis and Crystal Structure of tert-Butylamino)di-tert-butyl)siliceniotrichloroaluminate, (Me3C)2Si=NCMe3·AlCl3, and Dimethylazomethine-Aluminium Trichloride, Me2C=NH·AlCl3Dedicated to Prof. A. Meller on the occasion of his 65th birthday. (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 753-755 
    Details
    ISSN: 0009-2940
    Keywords: Silicenium ion ; Iminosilane ; Aluminate ; Silicon ; Aluminium ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Lithiated text-butylaminolfluorosilanes react with aluminum trichloride in ether, eliminating LiF to give AlCl3 adducts of iminosilanes  -  aminosiliceniotrichloroaluminates {R2Si-NCMe3·AlCl3}, which thermally form the dimethylazomethine- aluminium trichloride, Me2C=NH·AlCl3.
    Additional Material: 2 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19971300613
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    Sulfur Compounds, 199Part 198: R. Steudel, Y Drozdova, K. Miaskiewicz, R. H. Hertwig, W. Koch, J Am. Chem. Soc. 1997, 119, 1990.. Novel Titanocene Thiolato Complexes and Their Application in Preparing New Sulfur-Containing Heterocycles (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 757-764 
    Details
    ISSN: 0009-2940
    Keywords: Titanocene complexes ; S ligands ; Organic polysulfanes ; Ligand transfer reactions ; Sulfur heterocycles ; Chalcogens ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Treatment of Cp2Ti(CO)2 (3) with the di- and polysulfanes 1,2,4-(CH2)2S3, C4S6 (9), C,7H10S3 (11), 1,2,4,6-(CH2)3S4 (16), C6H10S6(19), and S6 affords the titanocene chelate complexes Cp2TiS3(CH2)2 (8), (Cp2Ti)2C4S6 (10), Cp2TiS3C7H10 (13), Cp2TiS2C7H10 (14), Cp2TiS4(CH2)3 (17), Cp,2TiS6C6H6H10 (20), and Cp2TiS8 (23). 14 is also obtained from Cp2TiCl2 (1) and the geminal dithiol of norbornene. The analogous reaction with the dithiol of dicyclopentadiene yields Cp2TiS2C10H12 (15). In ligand transfer reactions, 8 reacts with SCl2 to give 1,2,3,5-tetrathiane (25), 10 provides 9 on reaction with Cl2, 13 when treated with S2Cl2 affords C7H10S5 (12), 15 reacts with S2Cl2Cl2 to give C10H12S4. 17 and SCl2 yield 1,2,3,5,7-pentathiepane (18), 20 is converted to C6H10S7 (22) on reaction with SCl2, and 23 yields S10 and 1,2,-C6H4(SCl)2, respectively. With phosgene, thiophosgene, and thionyl chloride, compound 15 yields the corresponding dithiocarbonate 26, the trithiocarbonate 27 and the trisulfane 2-oxide 28. The structure of 27 was determined by X-ray crystallography.
    Additional Material: 1 Ill.
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    Synthesis of a Bisdienophilic Phthalocyanine and of Precursors for Repetitive Diels-Alder Reactions Based on Hemiporphyrazines and Phthalocyanines (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 801-806 
    Details
    ISSN: 0009-2940
    Keywords: Unsymmetrical phthalocyanines ; Hemiporphyrazines ; Macrocyclic bisdienes and bisdienophiles ; Diels-Alder reactions ; Ladder polymers ; Cycloaddition ; Macrocycles ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The specific synthesis of a metal-free bisdienophilic phthalocyanine 193, suitable for repetitive Diels-Alder reactions, is reported. This was achieved by condensation of 191,3,3-trichloro-6/7-nitroioindolenine (191) and 4,9-dibutoxy-2,3,5,8-tetrahydro-1,3-diimino-1H-5,8-epoxybenz[f]isoindoline (2). The ability of 3 to undergo Diels-Alder reactions was tested by reaction with an excess of 1,2,3,4-tetraphenylcyclopentadienone (5). Experimental data of the hemiporphyrazines 9, 10, and 11, which can be used as precursors for the synthesis of ladder polymers, are also given in the Experimental Section.
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  • 84
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    Pseudoelement Compounds, XPart IX: Ref. Synthesis and Crystal Structure of New Complexes of the Type trans-[Pt(H)X(PPh3)2 with Cyanamide and Cyanomethanide LigandsDedicated to Professor S. Engels on the occasion of his 65th birthday. (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1007-1012 
    Details
    ISSN: 0009-2940
    Keywords: Platinum ; Nitrocyanamide ; Nitrosodicyanomethanide ; 1,1,3, 3-Tetracyano-2-azapropenide ; 1,1,2,3,3-Pentacyanopropenide ; Hydrido complexes ; Coordination modes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The new coordination compounds trans-[Pt(H)X(PPh3)2] with NCN- and C(CN)2-functionalized anions (X- = [N(O)C(CN)2]-, [NO2NCN]-, [N{C(CN)2}2]-, [NCC{C-(CN)2}2]-, have been characterized by 1H-, 31P-, 13C-NMR, and IR spectroscopy and elemental analyses the crystal structures of trans-[Pt(H)N(O)C(CN)2(PPh3)2], trans- [Pt(H)N{C(CN)2}2(PPh3)2], and trans-[Pt(H)NCC{C(CN)2}2-(PPh3)2) have been determined by X-ray diffraction. Remarkably, [N(O)C(CN)2]- is coordinated through the central nitrogen atom, while [N{C(CN)2}2]- and [NCC(C(CN)2]2]- are bonded through terminal nitrogen atoms of a C(CN)2 unit.
    Additional Material: 4 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19971300730
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  • 85
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    New Coupling Reactions and Phosphorylations Using Organozinc Reagents (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1021-1027 
    Details
    ISSN: 0009-2940
    Keywords: Zinc ; Chirality ; Cross-coupling ; Phosphorylations ; Catalysis ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: This Microreview on the chemistry of organozinc reagents starts by briefly showing the methods of preparation of organozinc compounds and then discusses the considerable synthetic utility of zinc organometallics for the formation of new carbon-carbon bonds in the presence of transition-metal catalysts. Finally, the use of organozinc chemistry for the preparation of polyfunctional and chiral phosphanes is described.
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    URL: http://dx.doi.org/10.1002/cber.19971300802
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  • 86
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    Synthesis and Structures of Bis(tetramethylipiperidino)aluminum Halides-X-ray Crystal Structures of tmp2AlX (X = Cl, Br, I) and [tmp2A1(μ-F)l2 (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1047-1052 
    Details
    ISSN: 0009-2940
    Keywords: Bis(tetramethylipiperidino)aluminum halides ; Alkoxy((tetramethylpiperidino)aluminum halides ; 27Al-NMR spectra ; Aluminum ; Amides ; Synthetic methods ; Bridging ligands ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: N-Lithio-2,2,6,6-tetramethylpiperidine [Li(tmp)] reacts with AlX3 (X = Cl, Br) in diethyl ether/ n-hexane solution to generate the products of substitution and ether cleavage, [tmpAl(X)(μ-OEt)], (la, X = Cl; 1b, X = Br). However, when the reaction is allowed to proceed in n-hexane alone, an almost quantitative yield of compounds tmp2AlX (2a, X = Cl; 2b, X = Br; 2c, X = I) is obtained. According to 27AI-NMR spectroscopy, mass spectroscopy, cryoscopy, and X-ray crystal structure determinations, these compounds are monomeric in the solid state, in solution, and in the gas phase. 2b reacts with AgBF4 yielding the fluoride-bridged dimer (tmp2AlF), 2d, as shown by X-ray crystal structure determination.
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    URL: http://dx.doi.org/10.1002/cber.19971300805
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  • 87
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    Synthesis, Structure, and Dynamic Behavior of (μ-Aldimido)(μ-η1: η2-alkyne)- biszirconocene Cation Complexes That Contain Planar-Tetracoordinate Carbon (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1069-1077 
    Details
    ISSN: 0009-2940
    Keywords: Planar-tetracoordinate carbon ; Dynamic organometallic systems, μ-alkyne complexes ; π-Agostic systems ; Zirconium ; Metallocenes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The benzonitrile hydrozirconation product Cp2ZrCl(N—CHPh) 8 was treated with propynyl lithium to yield the (propynyl)(benzaldimido)ZrCp; complex 9. Subsequent treatment with trityl tetraphenylborate generated [Cp2Zr(C—C—CH3)-BPh-4] that instantaneously added to 9 to eventually form the (μ-aldimido)(μ-η1:η2-hexadiyne)ZrCp2 cation 11. The X-ray crystal structure analysis showed that 11 contains a planar-tetracoordinate carbon atom that is stabilized by forming a three-center-two-electron bond with the two adjacent metal atoms. Similarly, complex 9 reacted with [Cp2Zr(CH3)+CH3B(C6F5)3 1 to yield the planar-tetracoordinate carbon containing (μ-aldimido)(μ-η1:η2-2-butyne) Cp; cation 12. Both complexes 11 and 12 exhibit dynamic NMR spectra due to their rapid reorganization of the dimetallabicyclic frameworks (ΔG* = 10 kcal mol-1) in addition to an anchimerically assisted C—N bond rotation (ΔG* =15 kcal mol-1).
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19971300808
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    Isolation and Characterization of a Porphinatomanganese(IV) Complex from the Reaction of Dichloro Monoxide with 5,10,15,20-Tetrakis-(2,6-dichloropheny)porphinatomanganese(III) Chloride [Mn(EDCPP)CI] (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1099-1103 
    Details
    ISSN: 0009-2940
    Keywords: Porphyrinatomanganese(IV) ; Monooxygenase model ; Dichloro monoxide ; Catalytic alkene epoxidation ; Catalytic alkane oxygenation ; Catalytic alkane chlorination ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The isolation at -78°C and characterization of the novel crystalline reactive porphinatomanganese(IV) complex Mn-(TDCPP)(OCl)2 (5) is described. 5 is compared with the porphinatomanganese(IV) complexes Mn(TDCPP)(C6H5IOCl)2 (2), Mn(TDCPP)(C6F510C1)CI (3) and Mn(TDCPP)(OCH3)2, (4). The stoichiometric reaction of 5 with triphenylphosphane yields 2.5 equivalents of triphenylphosphane oxide and 1.0 equivalent of Mn(TDCPP)Cl (1). Complex 5 epoxidizes stilbene, and oxygenates and chlorinates cyclohexane.
    Additional Material: 2 Tab.
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    URL: http://dx.doi.org/10.1002/cber.19971300811
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  • 89
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    Synthesis and Structure of Allenyl-Substituted η6-Benzene(tricarbonyl)-chromium Complexes (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1135-1139 
    Details
    ISSN: 0009-2940
    Keywords: Arene complexes ; Chromium ; Allenes ; Rearrangements ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The Cr(CO)3-complexed η6-phenylpropargylic alcohols 3 react in a displacement rearrangement with thionyl chloride or chlorodiphenylphosphane to give the chloro- or phosphoryl allenyl substituted η6-phenyl complexes 4 and 6, respectively. In the X-ray crystal structure of the novel organometallic allenic derivatives 4b and 6b the vicinal chloro or phosphoryl substituent and the benzene(tricarbonyl)chromium fragment are arranged coplanarily. Palladium/copper-catalyzed couplings of the chloroallene 4b with terminal alkynes disclose a facile access to ynallene derivatives 8, novel carbon-rich organometallic π-systems.
    Additional Material: 1 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19971300816
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    Raman and Infrared Spectra and Quantum Chemical Calculations for Trichlorophosphoranylidenesulfamoyl Chloride, CISO2N=PCI3 (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1141-1145 
    Details
    ISSN: 0009-2940
    Keywords: Trichlorophosphoranylidenesulfamoyl chloride ; Vibrational spectroscopy ; Conformational properties ; Quantum chemical calculations ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Raman (3500-50 cm-l) and infrared (4000-400 cm-l) spectra of the title compound, ClSO2N=PCl3, were recorded for the solid and liquid phase. Additionally, the Raman spectrum of the compound dissolved in CCl4 was obtained and qualitative depolarization values were determined. The spectra of the liquid and solid phase were interpreted in terms of the existence of only one conformation possessing C1 symmetry, as predicted by quantum chemical calculations. A complete vibrational assignment is proposed based on the relative intensities, on group frequencies along with support from the normal coordinate analysis. The experimental fundamental vibrational modes are compared to those obtained from theoretical approaches employing the ab initio MP2/6-31G* method and a density functional approximation (B3PW91/6-31G*).
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19971300817
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    Ab Initio Studies on Disubstituted closo-Icosahedral Heteroboranes, X2B10H10 [X = CH, SiH, N, P, and Sb] (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1147-1150 
    Details
    ISSN: 0009-2940
    Keywords: Icosahedral heteroboranes ; Ab initio calculation ; Bonding models ; Aromaticity ; Nucleus Independent Chemical Shift [NICS] ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Ab initio theoretical studies on X2B10H10 (X = CH, SiH, N, P and Sb) have been done for all the three possible isomers. Unlike lower-vertex heteroboranes, all the hetero derivatives have shown similar trends in the relative stabilities, the 1,12-isomer being more stable followed by 1,7- and 1,2-isomers, except for N and Sb. No conventional 1,2-isomer for N could be found. Instead, a new nido isomer which is 18.1 kcal/mol higher in energy than the most stable isomer has been located. Any hetero group substitution to icosahedral R12H122- is found to be thermodynamically destabilizing. However, the Nucleus Independent Chemical Shift criterion shows that all compounds, except for 8, have similar aromaticity.
    Additional Material: 2 Tab.
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    URL: http://dx.doi.org/10.1002/cber.19971300818
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    The Molecular Structures of Triaminosilanes (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1159-1166 
    Details
    ISSN: 0009-2940
    Keywords: Aminosilantes ; Structure elucidation ; Molecular conformations ; Configuration determination ; Nitrogen Planarity/Silanes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The structural chemistry of a series of triaminosilanes XSi(NR2)3 has been investigated in order to determine the ground-state configuration and conformation of these molecules. Theoretical studies and analogy with the isoelectronic XP(NR2)3 (X = CH2, O, Se, NSiMe3 etc.) and P(NR2)3 molecules suggest structures of Cs or C3 symmetry, with small energy differences between them. The molecular structure of HSi(NMe2)3 (1) has been determined by a single-crystal X-ray diffraction study at low temperature. Surprisingly, the molecules have a non-standard conformation with an irregular orientation of the three NMe2 groups. The hydrido-, chloro-, methyl-, and vinyltris(morpholino)silanes XSi[N(CH2CH2)2O]3 (X = H, Cl, Me, Vi; 2-5) were prepared from the corresponding chlorosilanes and morpholine (2, 3) or lithium morpholide (4,5). Their variable-temperature NMR spectra were studied and the molecular structures determined by single crystal X-ray diffraction. Compound 2 has a molecular geometry approaching mirror symmetry with one morpholino group significantly different from the other two. This structure resembles that of isoelectronic tris(amino)phosphines. Compounds 3-5 have structures with a propeller-like arrangement of the three morpholino rings approaching C3 symmetry for this part of the molecules. The chloro compound 3 shows the shortest Si-N bond lengths (average 1.690 Å), followed by 2 (1.708Å),5 (1.709Å) and 4 (l.712Å). The configuration of all nitrogen atoms is almost planar, with sums of the angles close to 360°, and the morpholino rings adopt a chair conformation. According to the solution NMR spectra the ring inversion is slow at low temperature, but the rings rotate freely about the Si-N bonds on the NMR time scale. The molecular structures are discussed in terms of steric and electronic effects of the substituents. Other model compounds, including (Me2N)3SiC6H4-4-Br (6), MeSi[N(CH2CH2)2NMe]3 (7) and PhSi[N(CH2)4]3 (8), could not be crystallized, but were characterized by their analytical and spectroscopic data.
    Additional Material: 7 Ill.
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    Self-Assembly of Substituted 6-Hydroxy-trans-3-hexenoic Acids - Formation of Extended Ribbon-Like Structures by Hydrogen Bonds (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1029-1034 
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    ISSN: 0009-2940
    Keywords: Hydrogen bonding ; Hydroxy carboxylic acids, self-assembly of ; Crystal engineering ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The substituted 6-hydroxy-trans-3-hexenoic acids 2a and 2b are prepared by an organometallic template reaction involving a sequence of CC coupling reactions between a CO2 equivalent, butadiene, and 3-cyclopenten-1-one or 3,4-diphenyl-3-cyclopenten-1-one, respectively. In the crystal 2a assembles to form an infinite ribbon-type structure, exhibiting an alternating array of 12 and 18 atom-containing loops. The former are each constructed by an alternating CO2H/OH/CO2H/OH sequence, originating from four different monomeric units, that are linked together by means of hydrogen bonds. Two complementary ribbons of 2a are connected by van der Waals interactions to form staples that constitute the microscopic building blocks of the true (2a)n structure in the crystal. Stacks of cyclopentene π bonds are oriented inside the columnar structure of 2a. Acid 2b also forms a related ribbon-like assembly in the solid state. Here the bulky 3,4-diphenylcyclopentadienylidene moieties are oriented laterally at the ribbons, and van-der-Waals interactions with adjacent ribbons construct a three-dimensional hydroxyhexenoic acid network.
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    Preparation and Structure of Dithioxo- and Diselenoxophosphoranes Stabilized by Intramolecular Coordination with a Dialkylamino GroupDedicated to Prof. Dr. Marianne Baudler on the occasion of her 75th birthday. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1049-1055 
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    ISSN: 0009-2940
    Keywords: Dithioxophosphoranes ; Diselenoxophosphoranes ; Internal coordination ; Steric protection ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Some dithioxophosphoranes 3 stabilized by intramolecular coordination with a dialkylamino group were prepared, and their structures were analyzed by X-ray crystallography involving [2,4-di-tert-butyl-6-(isopropylmethylamino)phenyl]- (3c), {2,4-di-tert-butyl-6-[(dimethylamino)methyl]phenyl}- (3f), and {2,4-di-tert-butyl-6-[2-(dimethylamino)-1,1-dimethylethyl]phenyl}dithioxophosphorane (3h). The bond between the phosphorus atom and the aromatic ring is flexible and the angle narrows with decreasing ring size of the intramolecular coordination. The 31P-NMR signals are shifted to higher field with increasing ring size of the intramolecular coordination or strength of coordination. Similarly, the corresponding diselenoxophosphoranes 4 were prepared. Both their 31P- and 77Se-NMR signals are shifted to higher field with increasing contribution of intramolecular coordination.
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    Structural Studies on Indium and Tin Thiobenzoates (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1093-1098 
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    ISSN: 0009-2940
    Keywords: Indium tris(thiobenzoate) ; Triethylammonium tetrakis(thiobenzoato)indate ; Tin, butyl-, tris(thiobenzoate) ; Tin, dichloro-, bis(thiobenzoate) ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Indium(III) and tin(IV) thiocarboxylates were prepared and characterized on the basis of their IR, 13C- and 19Sn-NMR data. Indium tris(thiobenzoate) (1) decomposes into a sulfido complex In (S)[S(O)CPh] (2a). The corresponding tris(thioacetate) In[S(O)CMe]3 is thermally too unstable to be isolated. The anionic tetrakis complex [Et3NH]{In[S(O)CPh]4} (3) was characterized by X-ray crystallography which revealed a distorted tetrahedral coordination at the In atom. X-ray diffraction analysis of the complexes BuSn[S(O)CPh]3 (4) and Cl2Sn[S(O)CPh]2 (7) showed distorted tetrahedral and cis-octahedral structures, respectively.
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    Reaktionen des Tripod-Co-Templats CH3C(CH2PPh2)3Co(II) mit funktionalisierten HydrazinenMax Herberhold zum 60. Geburtstag gewidmet. (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1107-1113 
    Details
    ISSN: 0009-2940
    Keywords: Tripod ligands ; Hydrazines, substituted ; Diazenes ; Cobalt(III), fivefold coordination of ; Cobalt(II), fivefold coordination of ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The coordination behaviour of ligands having the same basic constitution RN=NC(=X)R′ (X = O, NR″, S) in their tripod cobalt derivatives has been analyzed. The ligands themselves may be considered as neutral heterodiene compounds and are in this respect vinylogues to diazenes RN=NRy′. Two- electron reduction of these neutral species results in dianionic heterosubstituted heteroolefins RN- -N=C(X-)R′. Due to their redox ambiguity the oxidation state of the metal M in chelate complexes is not a priori evident. Compounds tripod [5: X, R′ = O, Ph; 6; (X, R′) = (py); 7: X, R′ = S, NH2] are best described as containing low-spin Co(III) and dianionic ligands. Co(II) species are obtained with diethyl azodicarboxylate EtOOCN=NCOOEt as the ligand. In the mononuclear compound, with only one nitrogen and one carbonyl oxygen of the ligand acting as donor groups, the neutral ligand is coordinated to give the high-spin cobalt(II) species tripod (8). In the dinuclear compound 9 with both of the nitrogen atoms and carbonyl groups involved in coordination the dianionic ligand bridges two high-spin cobalt(II) centers to give tripod (9) as a derivative with two fused five-membered chelate rings. In addition to the conventional analytical techniques X-ray structure analyses, cyclovoltametric measurements, magnetic susceptibility and ESR data are used to characterize the compounds.
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    URL: http://dx.doi.org/10.1002/cber.19961290921
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    Übergangsmetall-Stannyl Komplexe, 10[1]. Molybdocen- und Wolframocen-Derivate mit zwei unterschiedlichen Liganden der 4. Hauptgruppe (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1131-1142 
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    ISSN: 0009-2940
    Keywords: Stannyl complexes ; Plumbyl complexes ; Tungsten complexes ; Molybdenum complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Transition-Metal Stannyl Complexes, 10 - Molybdocen and Wolframocen Derivatives with Two Different Main-Group-4 LigandsReactions of Li[Cp2MSnPh3] (M = Mo, W) with CH3I, BuBr, PhCH2Br, PhC(O)Cl or Br(CH2)nBr (n = 4,5) yield Cp2M(R)SnPh3 [R = CH3, Bu, CH2Ph, C(O)Ph, (CH2)nBr], while tBuBr or CH3C(O)Cl give the hydrido complexes Cp2M(H)SnPh3. A silyl stannyl complex is only obtained from Li[Cp2WSnPh3] and Me3SiOSO2CF3, but not with Me3SiCl or from the anionic Mo complex. In contrast, the reactions of chlorostannanes provide the bis(stannyl) complexes Cp2M(SnR′3)SnPh3 or Cp2M(SnR′2Cl)SnPh3. R/Cl exchange at the tin atom is observed when an excess of the chlorostannane is used. Upon reaction of Li[Cp2MSnPh3] with Ph3PbCl only Cp2M(PbPh3)SnPh3 is formed, while a mixture of Cp2M(PbMe3)SnPh3 and Cp2M(PbMe2Cl)SnPh3 is obtained with Me3PbCl due to redistribution reactions. The structures of Cp2W(SnPh3)C(O)Ph, Cp2W(SnPh3)SntBu2Cl and Cp2W(SnPh3)PbMe2Cl were determined by X-ray structure analyses.
    Additional Material: 1 Tab.
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    URL: http://dx.doi.org/10.1002/cber.19961290924
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    Thietane and Selenetane Complexes by Thermal Cycloaddition of Vinyl Ethers to Transition-Metal-Coordinated Thio- and Selenoaldehydes - Crystal Structure of Pentacarbonyl(7-phenyl-2-oxa-8-thiabicyclo[4.2.0]octane-S)tungsten(0)Dedicated to Professor Max Herberhold on the occasion of his 60th birthday (1996)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 129 (1996), S. 1169-1175 
    Details
    ISSN: 0009-2940
    Keywords: Thioaldehyde complexes ; Selenoaldehyde complexes ; Thietane complexes ; Selenetane complexes ; Rearrangements ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Pentacarbonyl(thiobenzaldehyde)tungsten und pentacarbonyl(selenobenzaldehyde)tungsten (1a and 1b) undergo a thermal [2 + 2] cycloaddition with several vinyl ethers to give highly substituted transition metal-coordinated thietanes and selenetanes. The addition is highly regio- and stereospecific. The products undergo acid-catalyzed rearrangements, which lead to thermodynamically more stable diastereomers of the thietanes and selenetanes. The stereochemistry of both addition and rearrangement was established by reaction of deuterium-labeled vinyl ethers and by reaction of the cis and trans isomers of ethyl propenyl ether. The crystal structure of the bicyclic addition product of 1a and 3,4-dihydro-2H-pyran is reported.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19961291005
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  • 99
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    A Monomeric Bis(arena)lead(II) Complex with a Plumbocene-like Bent Sandwich Structural Unit  -  Structure of [Pb(1,2-C6H4Me2)2(AlCl4)2Dedicated to Professor C. G. Kreiter on the occasion of his 60th birthday. (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1731-1732 
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    ISSN: 0009-2940
    Keywords: Lead ; Tetrachloroaluminate ; Arenes ; o-Xylene ; Bis(arene) Complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Bis(o-xylene)lead(II) bis(tetrachloroaluminate), obtained from lead(II) chloride and aluminium trichloride in o-xylene, has been shown by X-ray crystallography to be a mononuclear lead complex with point group symmetry C2 The two aromatic ligands are arranged similarly to those in monomeric plumbocene. The coordination sphere is completed by two bidentate AlCl4-ions. The lead center uses about a quarter of its bonding capability for each of the four ligands
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19971301204
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  • 100
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    Titanium and Zirconium Complexes Containing a Novel Dianionic Trifunctional Amido Ligand (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1751-1759 
    Details
    ISSN: 0009-2940
    Keywords: Amido complexes ; Titanium ; Zirconium ; Alkylmetal compounds ; Amido complexes ; Titanium ; Zirconium ; Alkylmetal compounds ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The novel tridentate diamidoamine ligands [RC(2C5H4N)(CH2NSiMe3)2)2- (R = H, CH3) have been synthesized and coordinated to TiIV giving the pentacoordinate complexes [MX2(RC(2-C5H4N)(CH2NSiMe3)2}] (M = Ti, Zr; X = Cl, Br). The crystal structure analysis of [TiBr2{HC(2-C5H4N)(CH2)2}] (M = Ti, Zr; X = Cl, Br). The crystal structure analysis of [TiBr2{HC(2-C5H4N)(CH2NSiMe3))] (10b) confirmed the involvement of the pyridyl function in the coordination to the meta centre occupying an apical position in the trigonal bipyramidal ligand polyhedron. alkylation of [TiCl2{H3CC(2-C5H4N)(CH2NSiMe3)2)] (12a) with one or two molar equivalents of [RMgCl](R = PhCH2, Me3SiC2) yielded the mono- and dialkyl complexes [TiClR{H3CC(2-C5H4N)(CH2NSiMe3)2)] and [TiR2(H3CC(2-C5H4N)(CH2NSiMe3)2)] and [TiR2(H3CC(2-C5H4N)(CH2NSiMe3)2}] in good yields. Depending on the steric demand of the alkyl group coordination or decoordination of the pyridyl group leads to four- or five-coordinate species. A crystal structure analysis of the pentacoordinate complex [TiCl(CH2SiMe3){H3CC(2-C5H4N)(CH2NSiMe3)2}] (16) was carried out.
    Additional Material: 3 Ill.
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    URL: http://dx.doi.org/10.1002/cber.19971301208
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