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  • 1
    Electronic Resource
    Electronic Resource
    Preparation and Crystal Structures of Gold(I) Complexes of a Series of Benzenethiolates: Pair Formation by Gold-to-Gold Interactions of (Benzenethiolato)(triphenylphosphane)gold(I) (1993)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 126 (1993), S. 605-610 
    Details
    ISSN: 0009-2940
    Keywords: Gold(I) complexes ; Gold(I) thiolates ; Thiolato complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Chloro(triphenylphosphane)gold(I) reacts readily with benzenethiol C6H5SH and a series of sterically hindered (2,4,6-trialkylbenzene)thiols 2,4,6-R3C6H2SH in the presence of NEt3 to yield stable gold(I) complexes Ph3PAu(S - 2,4,6-C6H2R3) [R=H (1), Me (2), Et (3), iPr (4)]. The crystal structures of these complexes have been determined by single-crystal X-ray diffraction analysis. In all compounds the gold atoms are linearly two-coordinate with very similar bond lengths and angles. - While complexes 2 - 4 with bulky thiolate ligands are monomeric in the crystal lattice, complex 1 has been found to form pairs of molecules with intermolecular gold - gold contacts of 313.5(5) pm. The Mössbauer spectra of the complexes exhibit large isomer shifts (I.S.), ranging from 3.06 to 3.72 mm s-1, and quadrupole splittings (Q.S.), ranging from 7.90 to 8.68 mm s-1. These data can be attributed to the strong electron-donating properties of the benzenethiolate ligands. The gold - gold contacts in complex 1 lead to I.S. and Q.S. values which are slightly smaller than those of 2 - 4. The Au - S distances do not show a major influence of the S - Au - P pairing in complex 1 as compared to complexes 2 - 4.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19931260310
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  • 2
    Electronic Resource
    Electronic Resource
    Tetramethylguanidine and Benzophenoneimine as Ligands in Gold Chemistry (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1417-1422 
    Details
    ISSN: 0009-2940
    Keywords: Gold ; N ligands ; Gold(I) complexes ; (Imine)gold(I) complexes ; Guanidines ; Ketimines ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: (Tetramethylguanidine)gold(I) chloride (1) and bromide (2) are readily prepared in high yield from (Me2N)2C=NH and [AuCl(Me2S)] or [AuBr(tht) (tht = tetrahydrothiophene), repectively. NMR spectra of chloroform solutions of the two products indicate equilibria of the type 2 LAuX = L2Au+AuX2-. The cationic complex [Au(NH=C(NMe2)2)(PPh3)]+ is obtained as the triflate salt 3 from tetramethylguanidine and [Au(PPh3)]+O3SCF3-. In solution at low temperature (-60°C), this compound adopts a rigid structure whereby the NMe2 groups are rendered non-equivalent, but at ambient temperature there is coalescence of the NMe2 signals in the 1H- and 13C-NMR spectra. The related benzophenoneimine complex [Au{NH=CPh2}(PPh3)]+BF4- (4), which was synthesized as a reference3 compound, exhibits similar behaviour. In solution at low temperature (-60°C) the two phenyl rings of the ligand are diastereotopic. In contrast, the triisopropylphosphane derivative [Au[NH=CPh2](PiPr3)]+BF4- (5) is rigid on the NMR time scale, even at 25°C. Thbe solid-state structures of 2, 3, 4, and 5 have been determined by single-crystal X-ray diffraction. Compound 2 crystallizes in the ionic form with discrete Au … Au bonded ion pairs [Au[NH=C(NMe2)2]2]+ [AuBr2]- [Au … Au 3.1413(8) Å]. The cations of 3, 4, and 5 show the [Au(PPh3)]+ units N-coordinated to the imino groups, with the nitrogen atoms in a trigonal-planar configuration.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19971301010
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  • 3
    Electronic Resource
    Electronic Resource
    Hypercoordinate Carbon in Trigoldbis(silyl)methanium Cations (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 137-142 
    Details
    ISSN: 0009-2940
    Keywords: Hypercoordinate carbon ; Gold(I) complexes ; Methanium cations ; Trigoldbis(silyl)methanium cations ; Gold clustering ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reactions of organolithium compounds of the type (R3Si)2CHLi (R3 = Me3 or Me2Ph) with the gold(I) complex Ph3PAuCl afford the monoaurated bis(silyl)methanes (R3Si)2- CHAuPPh3 (1a, b) in high yield. These compounds are converted into complex salts with hypercoordinate methanium cations {(R3Si)2C[Au(PPh3)]3}+BF-4 (3a, b) by treatment with {[(Ph3P)Au]3O}+ BF-4. In the reaction mixtures small amounts of the neutral dinuclear intermediates {(R3Si)2C[Au(PPh3)]2} (2a, b) have been detected and characterized by their spectroscopic data. Compounds 1a, b and 3a, b have been studied by single crystal X-ray diffraction analyses. While the mononuclear molecules 1a, b have conventional structures with parameters representing classical types of bonding, the novel trinuclear complexes 3a, b feature cations with a pentacoordinate carbon atom in a distorted trigonal-bipyramidal environment of two silicon atoms and one gold atom in equatorial positions and the remaining two gold atoms at the axial vertices of the polyhedra. The main axis of the bipyramid is strongly bent at the central carbon atoms. This distortion leads to short axial/equatorial Au…Au distances indicating peripheral metal-metal bonding.
    Additional Material: 1 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951280209
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  • 4
    Electronic Resource
    Electronic Resource
    Gold(1) Complexes of Ketiminophosphanes and -phosphane Sulfides (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1423-1426 
    Details
    ISSN: 0009-2940
    Keywords: Gold ; Gold(I) complexes ; (Imine)gold(I)complexes ; Ketiminophosphanes ; (Ketiminophosphane)gold(I) complexes ; Ketiminophosphane sulfides ; (Ketiminophosphanesulfide)gold(I) complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reactions of chloro(dimethyl sulfide)gold(I) with equivalent quantities of the ketiminophosphane diphenyl(diphenylmethyleneamino)phosphane (1a) or its sulfide (1aS) lead to high yields of stable, crystalline 1 : 1 complexes with AuCl units attached to the phosphorus and sulfur atom, respectively. Tris(diphenylmethyleneamino)phosphane (1c) gives the related complex (Ph2C=N)3PAuCl with the gold atom also selectively P-bound. Bis(diphenylmethyleneamino)phenyl-phosphane (1b) could not be used because of its limited stability. Single-crystal X-ray diffraction studies have shown that there is no auxiliary coordination of the metal center by the imino functions of the ligands. The geometry of the P/S—Au—Cl moieties deviates only very slightly from linearity. The angle at the sulfur atom in (Ph2C=N)Ph2PSAuCl is very small [94.30(3)°], but despite of the resulting rather open coordination there are no discernible intra- or intermolecular contacts in the lattice. Such contacts are also absent with (Ph2C=N)Ph2PAuCl and (Ph2C=N)3PAuCl owing to the bulk of the ligands. The 1 : 1 complexes do not react with an excess of (Me2S)AuCl. This finding, and the molecular structures of the 1 : 1 complexes, show very consistently that both phosphane and sulfide donors are far superior as ligands for gold(I) as compared to ketimine donor molecules.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19971301011
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  • 5
    Electronic Resource
    Electronic Resource
    The supramolecular structures of complex tri[gold(I)]sulfonium cations (1994)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 127 (1994), S. 2387-2391 
    Details
    ISSN: 0009-2940
    Keywords: Gold(I) complexes ; Sulfonium salts ; Trigoldsulfonium salts ; Au-Au interactions ; Supramolecular aggregation ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Tris[(trimethylphosphane)gold(I)]sulfonium tetrafluoroborate (1) has been prepared from the corresponding oxonium salt [(Me3P)Au]3O+ BF-4 and bis(trimethylsilyl) sulfide, (Me3Si)2S. The analogous triisopropylphosphane and methyldiphenylphosphane complexes (2, 3) have been obtained in a similar way. The products are stable crystalline solids, the structure of which has been determined by X-ray methods. They are composed of independent tetrafluoroborate anions and pyramidal tri(gold)sulfonium cations, which are aggregated to form dimeric units (as in 3) or even strings of dimers (as in 1). It is only in complex 2 that steric effects, originating from the bulky phosphane ligands, prevent the building of supra-molecular (supracationic) aggregates. In the independent pyramidal cations of 2 only short intracationic Au…Au contacts have been detected. These are complemented by intercationic gold-gold contacts of similar length in the structures of 1 and 3. - In the preparation of complex 1, the species [(Me3P)Au]4S2+ (BF-4)2 (4) with hypercoordinate sulfur atoms has also been detected by mass spectroscopy.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19941271208
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  • 6
    Electronic Resource
    Electronic Resource
    Gold Coordination by Tertiary Phosphane Sulfides (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 955-958 
    Details
    ISSN: 0009-2940
    Keywords: Phosphane sulfides ; Gold(I) complexes ; Sulfide coordination ; Phosphorus ; Sulfur ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Treatment of the ditertiary phosphane sulfides (CH2)n[PPh2S]2, 1a-1d, n = 1-4, with equivalent amounts of (dimethylsulfide)gold(I) chloride (Me2S)AuC1 affords the dinuclear complexes 2a-2d with an AuCl unit attached to each sulfur atom. The chlorides can be converted into the bromides 3a-3c by metathesis using KBr, or by reacting 1d with (tetrahydrothiophene)gold bromide. With [(Ph3P)Au]+ O3SCF3 as the aurating agent for the diphosphane disulfides, the corresponding dicationic products are obtained: {(CH2)n[SPPh2AuPPh3]2}2+ · 2 O3SCF3 (4b-4d, n = 2-4). An excess of the reagents does not lead to polygold clustering at the sulfur atoms, and P-S cleavage occurs instead to give sulfonium salts {S[Au(PPh3)]3}+ X-. The reaction of Ph3PS with equimolar quantities of [ (Ph3P)Au]O3SCF3 leads to the cationic 1:1 complex 5, and with an excess of the agent the P-S bond is ruptured. The structures of compounds 4b and 4d were determined by single-crystal X-ray diffraction. The dications have crystallographic centers ot inversion, the coordination at the gold atoms is linear [4b: 179.03(3)° 4d: 175.29(2)°] and the angles at the sulfur atoms are acute [4b: 97.76(4)° 4d: 96.37(3)°], but there are no short Au-Au contacts.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19971300723
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  • 7
    Electronic Resource
    Electronic Resource
    Neutral Gold(I) Complexes with Mixed Phosphorus LigandsDedicated to Professor Wolfgang Beck on the occasion of his 65th birthday. (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1333-1338 
    Details
    ISSN: 0009-2940
    Keywords: Gold ; Gold(I) complexes ; Phosphinite complexes ; Phosphite complexes ; Configuration determination ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The reaction of compounds (R3P) AuMe with diphenylphosphinous acid Ph2P(O)H affords methane and neutral complexes of the type (R3P(O)Ph2 (1a: R = Me; 1b: R = Ph, lc: R = o-Tol). 1a, b are obtained in high yield, but the yield of lc is lower owing to a side-reaction which leads to a different product: Ph2P(OH)-Au-P(O)Ph2 (2). The crystal structure of 1a was determined by a single-crystal X-ray diffraction study. The compounds is a monomer with a linear P-Au-P′ axis and the phosphane and phosphinite ligands in a staggered conformation. In solution (CHCl3, CH2Cl 2/) compounds 1a-c undergo a ligand redistribution, establishing equilibria that involve ionic isomers of the type [R3P)2Au]+ [Au-(P(O)Ph2)2]-, which are readily identified through their NMR data. The analogous reaction of (R3P)b AuMe with dimethylphosphite (MeO)2P(O)H gives methane and the corresponding dimethylphosphites of the type (R3P)AuP(O)(OMe)2 (3a: R = Me; 3b: R = Ph; 3c: R= o-Tol). The crystal structure of 3b has also been determined. It features a linear structure with an eclipsed conformation of the ligands. In polar solvents (CHCl3, methanol) there is again an eqilibrium between neutral and ionic isomers, the latter comprising bis(phosphane)gold cations [(R3P)2Au]+ and {Au[P(O)-(OMe)2]2)- anions, as confirmed by NMR spectroscopy and mass spectrometry.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19971300925
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