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  • Gold(I) complexes  (7)
  • Silicon  (3)
  • (Phosphane)gold(I) complexes  (2)
  • Aminosilanes  (2)
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  • 1
    Electronic Resource
    Electronic Resource
    (Triphenylphosphane)gold(I) Scrambling in a Hexanuclear Complex of Phenylene-1,2-bis(phosphane) (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 217-219 
    Details
    ISSN: 0009-2940
    Keywords: Gold compounds ; (Phosphane)gold(I) complexes ; Clusters ; P Ligands ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Phenylene-1,2-bis(phosphane) reacts with two mole-equivalents of tris[(triphenylphosphane)gold(I)]oxonium tetrafluoroborate in dichloromethane at -78°C to give high yields of a hexanuclear complex {C6H4]P(AuPPh3)3]2}2+ · 2 BF-4 (1). The variable-temperature 31P{1H}-NMR spectra of the product in CD2Cl2 at - 80°C are compatible with a static structure featuring three Ph3PAu units associated with each of the two C6H4P2 phosphide functions, as derived from a clear doublet/quartet pattern. At 50°C in CDCl3, however, there is rapid intramolecular scrambling of these Ph3PAu units, which gives rise to a triplet/septet pattern with the J(P,P) value reduced to exactly one half of the value at the low temperature limit.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19971300212
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  • 2
    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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  • 3
    Electronic Resource
    Electronic Resource
    Synthesis Structure and Photoluminescence of 1,2-Disila-acenaphthene Si2C10H10 and 1,2-Diaryldisilane Reference Compounds (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1671-1676 
    Details
    ISSN: 0009-2940
    Keywords: Silicon ; Disilanes ; Diaryldisilanes ; Disilanyl-arenes ; 1,2-Disila-acenaphthene ; Fluorescence spectroscopy ; UV/Vis spectroscopy ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: For the synthesis of the diaryldisilanes Ar-SiH2SiH2-Ar (1a, Ar = phenyl; 1b, Ar = p-tolyl 1c, Ar = mesityl; 1d, Ar = p-anisyl) two convenient preparative routes are reported. The crystal structures of 1c and 1d have been determined in X-ray diffraction studies; the disilanes have a staggered transconformation with a crystallographically imposed center of inversion. For 1a-d no photoluminescence phenomena can be observed. 1,2-Disila-acenaphthene (2) is synthesized in acceptable yield by treatment of 1,8-dilithionaphthalene with 1 equivalent of 1,2-bis[((trifluoromethyl)sulfonyl)oxy]disilane Tf-SiH2SiH2-Tf. The crystal structure of 2 has been determined by X-ray diffraction. The molecule has no crystallographically imposed symmetry but closely follows the symmetry elements of points group C2v. Solutions of 2 exhibit intense fluorescence in the near UV region at room temperature. The fluorescence spectra are discussed in comparison with data on acenaphthene and naphthalene.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19971301119
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  • 4
    Electronic Resource
    Electronic Resource
    The Molecular Structures of Tetra(amino)silanes (1997)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 130 (1997), S. 1167-1174 
    Details
    ISSN: 0009-2940
    Keywords: Silicon ; Configuration determination ; Aminosilanes ; Tetra(amino)silanes ; Molecular conformation ; Conformation analysis ; Nitrogen ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: In a search for crystalline homoleptic tetra(amin)silanes with (mirror)-symmetrical NR2 substituents, tetrakis( 1-pyrrolidinyl)silane (1) was prepared by an improved synthetic route, and tetrakis(morpholino)silane (2) was synthesized from SiBr4 and morpholine/Li-morpholide via the intermediate BrSi[N(CH2CH2)2O]3 (4). With SiCl4 only the monochloro stage, 3, is reached. Tetrakis(4-methyl-1-piperazinyl)silane (5) was prepared similarly, using 4-methylpiperazine. With (CH2)6NH or (CH2)6NLi and SiBr4 only [(CH2)6N]3SiBr (6) was obtained. The structures of 1, 2 and 5 were determined by single-crystal X-ray diffraction. While compound 1 has an irregular molecular geometry following no symmetrical pattern, molecules of 2 and 5 have similar structures with almost superimposable Si(NC2)4 cores of approximate D2d symmetry. The overall molecular symmetry of 2 is reduced only by incongruous folding of the heterocycles, which are all in a chair conformation. The core structures of 2 and 5 are in excellent agreement with the results of density function calculations for Si(NH2)4. Si(NMe2)4 (the crystal structure of which could not be determined) was converted into (Me2N)3SiO-SO2CF3 (7) by treatment with two equivalents of triflic acid. Reaction of 7 with 1-naphthylamine/triethylamine affords (Me2N)3SiNHC9H7 (8). With 2,4-difluoroaniline/NEt3 the analogous derivative (Me2N)3SiNHC6H3F2 (9) is obtained, but with 4-bromoaniline the product is a silane with the ligands redistributed to give (Me2N2),Si(NHC6H4Br), (10), the structure of which was also determined. It has a non-standard geometry with very flat nitrogen pyramids at all four substituents.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19971300821
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  • 5
    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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  • 6
    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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  • 7
    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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  • 8
    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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  • 9
    Electronic Resource
    Electronic Resource
    Synthesis and Structure of a Cyclic Complex of Digold Sulfide Au2S and of Related Compounds (1995)
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 128 (1995), S. 901-905 
    Details
    ISSN: 0009-2940
    Keywords: Gold sulfide complexes ; Gold thiolates ; (Phosphane)gold(I) complexes ; Digoldsulfonium salts ; Digoldchloronium salt ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 1,4-Bis(diphenylphosphanylmethyl)benzene (1) was converted into its bis[chlorogold(I)] complex [1 · (AuCl)2] upon treatment with two equivalents of chloro(dimethyl sulfide)-gold(I). The reaction of 1 · (AuCl)2 with one equivalent of silver tetrafluoroborate afforded a cyclic di[gold(I)]chloronium tetrafluoroborate [1 · Au2Cl+ BF-4]. Substitution of chloride in 1 · (AuCl)2 by sodium methanethiolate in wet chloroform, gave the bis[methylthiogold(I)] complex 1 · (AuSMe)2], while with sodium sulfide a cyclic complex 1 · Au2S was obtained. Reaction of 1 · (AuCl)2 with two equivalents of AgBF4 followed by treatment with diphenyldisulfide or sodium methanethiolate yielded the cyclic methyl/phenylsulfonium tetrafluoroborates 1 · Au2SPh+ BF-4 and 1 · Au2SMe+BF-4, respectively. All compounds were identified on the basis of their analytical and spectroscopic data. The crystal structures of 1 · (AuCl)2, 1 · (AuSMe)2, and 1 · Au2S have been determined. The Au2S complex has a cyclic structure with a narrow Au-S-Au angle of 86.7(1)° indicating a significant intraannular Au…Au interaction.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/cber.19951280908
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  • 10
    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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