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  • 1
    Electronic Resource
    Electronic Resource
    (N-lithioamino)diorganophosphanes and Bis(N-Lithioamino)organophosphanes: Synthesis and Structures (1999)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 1999 (1999), S. 2355-2368 
    Details
    ISSN: 1434-1948
    Keywords: Phosphane complexes ; Lithium ; Aminophosphanes ; Hydrazides ; (N-lithioamino)diorganophosphanes ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Butyllithium (nBuLi) deprotonates Ph2P-NHtBu in ether to give (Ph2P-NLitBu)2·OEt2. There is no Li···P interaction in this molecule. Three compounds of the type R′P(NLiR)2 have been obtained by lithiation of R′P(NHR)2, isolated as [BuP(NLitBu)2·OEt2]2, [PhP(NLiPh)2·OEt2]2 and [PhP(NLiPh)2]2. Reaction of nBuLi with MeP(NHiPr)2 in hexane/THF leads to [MeP{N(Li)iPr]2·THF}4 with an asymmetric cluster structure comprising one LiP3, three LiPN2, three LiP2N and one LiN3 cluster units. The molecular structures of these compounds as determined by X-ray structure analysis show that they are best depicted as N-lithioaminophosphanes and not as the isomeric P-lithioiminophosphoranes.
    Additional Material: 13 Ill.
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  • 2
    Electronic Resource
    Electronic Resource
    Solvates of Sodium Bis(borane)dimethylamide (1999)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 1999 (1999), S. 1373-1379 
    Details
    ISSN: 1434-1948
    Keywords: Sodium bis(borane)dimethylamide solvates ; X-ray structure ; Reduction ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reaction of sodium metal with dimethylamine-borane in THF yields Na[(H3B)2NMe2] (1) which can be isolated as {Na[(H3B)2NMe2]}5·THF or as Na[(H3B)2NMe2]·15-crown-5 (2) and Na[(H3B)2NMe2]·benzo-15-crown-5 (3) after addition of the appropriate crown ether to the THF solution of 1. Reaction of 1 with ZrCl4 yields Me2HN-BH2-NMe2-BH3 (4), the structure of which has been determined. In THF solution, 1 reduces aldehydes, ketones, acyl chlorides, and esters to the corresponding alcohols. It also reacts slowly with nitriles and allylbenzene. Compound (1)5·THF crystallizes in an extended three-dimensional lattice, in which the Na atoms are coordinated by 6-9 hydridic H atoms, while 3 is a molecular compound in the solid state. Only one hydrogen atom of each BH3 group coordinates to the sodium center. On the other hand, 4 forms dimeric associates in the solid state through N-H···H-B interactions.
    Additional Material: 6 Ill.
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  • 3
    Electronic Resource
    Electronic Resource
    Formation of Calcium-Carbon Bonds From a Lewis Acid-Base Reaction of Calcium Bis[bis(trimethylsilyl)amide] and Tris(trimethylsilylmethyl)alane (1999)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 1999 (1999), S. 2209-2214 
    Details
    ISSN: 1434-1948
    Keywords: Aluminium ; Amides ; Calcium ; Metallacycles ; Phosphorus ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Treatment of calcium bis[bis(trimethylsilyl)amide] with two equivalents of tris(trimethylsilylmethyl)alane yields (Me3SiCH2)2Al-N(SiMe3)2 (1) and the dimer [(Me3Si)2N-Ca(μ-CH2SiMe3)2Al(CH2SiMe3)2]2 (2). The five-coordinate bridging carbon atoms show Ca-C bond lengths of 264 and 268 pm. A similar reaction with calcium bis[bis(trimethylsilyl)phosphanide] gives the dimer [(Me3SiCH2)2Al-P(SiMe3)2]2 (3) with crystallographic C2 symmetry. A calcium-containing species is not isolable, however, in the presence of DME - ether cleavage reactions and the formation of the centrosymmetric dimer [(Me3SiCH2)2Al-OCH2CH2OMe]2 (4) are observed. The central moiety is an Al2O2 cycle with fivefold coordinated aluminium centers.
    Additional Material: 4 Ill.
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  • 4
    Electronic Resource
    Electronic Resource
    Magnesiation of Triisopropylsilylphosphane: Synthesis and Structures of New Mg2nP2m Polyhedra (1999)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 1999 (1999), S. 2215-2220 
    Details
    ISSN: 1434-1948
    Keywords: Magnesium ; Metalation ; Phosphorus ; Polyhedra ; X-ray structures ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The magnesiation of triisopropylsilylphosphane with dibutylmagnesium in toluene yields the octanuclear complex [Mg8(PSiiPr3)6{P(H)SiiPr3}4] (1) which consists of MgPSiiPr3 units forming a hexagonal Mg6P6 prism, with two opposite Mg2P2 moieties capped by additional Mg[P(H)SiiPr3]2 groups. If a small amount of THF is present during the metalation reaction [(THF)4Mg6(PSiiPr3)6] (2) also containing a hexagonal Mg6P6 prism can be isolated. The magnesiation of H2P-SiiPr3 in tetrahydrofuran leads to the formation of the tetrameric complex [(THF)MgPSiiPr3]4(3) with a slightly distorted Mg4P4 cubane-like structure.The structures depend strongly on the steric strain caused by the trialkylsilyl substituents and the neutral coligands at the magnesium center. The highest steric strain, which is induced by coordination to every magnesium atom, leads to the smallest MgnPn polyhedron - the central Mg4P4 heterocubane moiety. In compounds 1 and 2 the hexagonal Mg6P6 prism is formed, however, with reduced steric strain as observed for 2 where the Mg-P bond lengths become more similar.
    Additional Material: 4 Ill.
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  • 5
    Electronic Resource
    Electronic Resource
    Synthesis and Characterization of the Heterometallic Aggregate Pb2Al5(μ3-O)(μ4-O)(μ-OiPr)9(OiPr)3(μ-OAc)3 (1999)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 1999 (1999), S. 1291-1293 
    Details
    ISSN: 1434-1948
    Keywords: Aluminum ; Lead ; O ligands ; Alkoxy carboxylates ; Structure elucidation ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A novel heterometallic aggregate Pb2Al5(μ3-O)(μ4-O)(μ-OiPr)9(OiPr)3(μ-OAc)3 obtained from the interaction of Pb(OAc)2 and Al(O-iPr)3 is the first structurally characterized example based on lead and aluminum. This compound has been isolated in high yield and examined by 1H-, 13C-, and 27Al NMR, and in the solid state by X-ray crystallography.
    Additional Material: 2 Ill.
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  • 6
    Electronic Resource
    Electronic Resource
    Diphosphonio Dihydrophosphetide and 1,2-Diphospholide CationsDedicated to Professor Rolf Appel on the occasion of his 75th birthday (1996)
    Weinheim : Wiley-Blackwell
    Chemistry - A European Journal 2 (1996), S. 221-227 
    Details
    ISSN: 0947-6539
    Keywords: heterocycles ; organic syntheses ; phospholes ; phosphorus ylides ; ring expansions ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Condensation of a 1,3-diphosphoniopropenide cation at its reactive 1,3-positions with a dichlorophosphine in the presence of triethylamine provides a route to 2,4-diphosphoniodihydrophosphetide cations. An excess of dichlorophosphine in the presence of an additional reducing agent results in a ring expansion and yields 3,5-diphosphoniodihydro-1,2-diphospholide cations. The chlorosubstituted cation derived from PCl3 can be further reduced to the hydrolytically stable 3,5-diphosphonio-1,2-diphospholide cation. It adds halogen to the P=P bond and can easily be regained from the halogen adduct. Structural comparison of the 1,2-diphenyl- and 1,2-dichlorodihydro-1,2-diphospholide cation with the 1,2-diphospholide cation shows three stages of interaction of the C3 and the P2 entities of the ring: no conjugation in the first case, hyperconjugative extension of the allylic system to include the phosphorus atoms in the second case and cyclic π conjugation in the third.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/chem.19960020215
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  • 7
    Electronic Resource
    Electronic Resource
    The Molecular Structure of Some Transition-Metal Complexes with 1,2,3,4-Tetrazole-5-thiolate Anions (1998)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 1998 (1998), S. 93-99 
    Details
    ISSN: 1434-1948
    Keywords: 2-Methyl-1,2,3,4-tetrazole-5-thiolates ; 2-Phenyl-1,2,3,4-tetrazole-5-thiolates ; Palladium ; Platinum ; Copper ; Silver ; Gold ; Molecular structures ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The molecular structures of nine transition metal tetrazolethiolates have been determined by X-ray structure determinations. The ligand is invariably coordinated through its sulfur atom to the metal center [M = PdII, CuI, AgI, AuI, AuIII, and Hg]. The M-S-C bond angles vary considerably, but this cannot be correlated with variations in the C-S bond lengths. Intermolecular association occurs for Ph3PAu(SCN4Me) via Au-S contacts, leading to dimeric strands in the solid state. The copper compound (Ph3P)3Cu4(SCN4Me)4 (5), possesses a rather asymmetric structure: one Cu atom is tricoordinated by 3 sulfur atoms, the other three are tetracoordinated by P and N as well as by S atoms.
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  • 8
    Electronic Resource
    Electronic Resource
    Oxidative Addition of α-Bromoglycine to Palladium(0) and Platinum(0) Complexes: α-Metallated Amino Acids as Models for Intermediates in the Metal-Catalyzed Hydrogenation of Dehydroamino Acids (1998)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 1998 (1998), S. 375-379 
    Details
    ISSN: 1434-1948
    Keywords: α-Metallated amino acids ; Palladium ; Platinum ; Oxidative addition ; α-Bromoglycinate ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Oxidative addition of methyl N-benzoyl-2-bromoglycinate to bis(dibenzylideneacetone)palladium, in the presence of 2,2′-bipyridyl, and to (Ph3P)2Pt(η2-C2H4) gives the α-metallated glycine esters 1a and 2a. Abstraction of bromide from 1a, 2a, using AgSbF6 or AgBF4, affords the cationic C,O-chelate complexes [(bpy)Pd-CH(CO2Me)NHC(Ph)O]+ (1b,c) and [(Ph3P)2Pt-CH(CO2Me)NHC(Ph)O]+ (2b), respectively, featuring coordination of the amide O atom. The complexes 1b and 2b have been characterized by X-ray diffraction.
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  • 9
    Electronic Resource
    Electronic Resource
    Rearrangement of Bis(dimethylamino)bis(1-indenyl)diborane(4) into Bis(dimethylamino)bis(3-indenyl)diborane(4) (1998)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 1998 (1998), S. 505-509 
    Details
    ISSN: 1434-1948
    Keywords: Chlorobis(dimethylamino)(3-indenyl)diborane(4) ; Bis(dimethylamino)bis(1-indenyl)diborane(4) ; Bis(dimethylamino)(1-indenyl)(3-indenyl)diborane(4) ; Bis(dimethylamino)bis(3-indenyl)diborane(4) ; Rearrangement ; X-ray structures ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Indenyllithium reacts with dichlorobis(dimethylamino)diborane(4) with formation of bis(dimethylamino)bis(1-indenyl)diborane(4) which rearranges on heating to the isomer bis(dimethylamino)bis(3-indenyl)diborane(4). The „mixed” bis(dimethylamino)(1-indenyl)(3-indenyl)diborane(4) is obtained from indenyllithium and chlorobis(dimethylamino)(3-indenyl)diborane(4). The main structural differences between the two isomers 3 and 4 are a slightly shorter B-B bond in 4, as well as a stronger twist about the B-B bond (89.9° vs. 67.4°) and, as expected, a shorter B-C bond. There is, however, no significant B-C π bonding.
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  • 10
    Electronic Resource
    Electronic Resource
    Oligomeric Solvent-Free Magnesium Bis(phosphanides) - Molecular Structure of Trimeric Magnesium Bis[bis(trimethylsilyl)phosphanide] (1998)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 1998 (1998), S. 517-521 
    Details
    ISSN: 1434-1948
    Keywords: Bis(silyl)phosphanes ; Magnesium ; NMR spectroscopy ; Oligomers ; Phosphorus ; Chemistry ; General Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The metathesis reaction of (dme)LiPH2 and chlorodiisopropylsilane yields HP(SiHiPr2)2 (1) and P(SiHiPr2)3 (2). The metalation of 1 by n/sec-dibutylmagnesium in heptane leads to the formation of dimeric magnesium bis[bis(diisopropylsilyl)phosphanide] [(3)2]. A toluene solution of magnesium bis[bis(trimethylsilyl)phosphanide] (4) shows a dimer-trimer equilibrium in the 31P{1H}-NMR spectrum at -40°C with an increasing amount of the dimer with increasing temperature. A molecular mass determination by freezing-point depression in benzene yields a value of 516 g·mol-1, which lies between a monomeric and a dimeric molecule. Cooling of the toluene solution to -30°C leads to the precipitation of single crystals of monoclinic {(Me3Si)2P-Mg[μ-P(SiMe3)2]2}2Mg [(4)3].
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