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The reaction of CuCl, LiAs(SiMe3)2 and dppb (Bis(diphenylphosphino)butane) leads to the formation of ionic cluster complexes. Depending on the reaction conditions one can isolate [Cu8As3(AsSiMe3)2(dppb)4]+[Cu{As2(SiMe3)2}{As4(SiMe3)4}]‐ ( 1 ) and [Cu8As3(AsSiMe3)2(dppb)4]+[Cu{As(SiMe3)2}2]‐ ( 2 ). The same reaction of CuCl, dppm (Bis(diphenylphosphino)methane) and LiSb(SiMe3)2 leads to the neutral cluster complex [Cu10(Sb3)2(SbSiMe3)2(dppm)6] ( 3 ). The structures of 1‐3 have been solved by X‐ray single crystal analyses. 相似文献
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Ulrike Riese Naim Faza Werner Massa Kurt Dehnicke 《Angewandte Chemie (International ed. in English)》1999,38(4):528-531
Unusual, highly symmetrical cubes are formed by the dodecameric cationic phosphoraneiminato complexes of copper(I ) and silver(I ) [M12(NPEt3)8]4+, in which the metal atoms occupy the edges and the N atoms of NPEt 3−3 groups the corners of the cube (see figure). The structures can be understood as molecular sections of the Cu3N structure, which is inverse to the ReO3‐type structure. 相似文献
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Barbaro P Di Vaira M Peruzzini M Seniori Costantini S Stoppioni P 《Chemistry (Weinheim an der Bergstrasse, Germany)》2007,13(23):6682-6690
The reaction of [CpRu(PPh(3))(2)Cl] (1) with half an equivalent of P(4) or P(4)S(3) in the presence of AgCF(3)SO(3) as chloride scavenger affords the stable dimetal complexes [{CpRu(PPh(3))(2)}(2)(micro,eta(1:1)-P(4))][CF(3)SO(3)](2).3 CH(2)Cl(2) (2) and [{CpRu(PPh(3))(2)}(2)(micro,eta(1:1)-P(apical)-P(basal)-P(4)S(3))][CF(3)SO(3)](2).0.5 C(7)H(8) (3), in which the tetrahedral P(4) and mixed-cage P(4)S(3) molecules are respectively bound to two CpRu(PPh(3))(2) fragments through two phosphorus atoms. The coordinated cage molecules, at variance with the free ligands, readily react with an excess of water in THF under mild conditions. Among the hydrolysis products, the new, remarkably stable complexes [{CpRu(PPh(3))(2)}(2)(micro,eta(1:1)-P(2)H(4))][CF(3)SO(3)](2) (4) and [CpRu(PPh(3))(2)(eta(1)-PH(2)SH)]CF(3)SO(3) (8) were isolated. In the former, diphosphane, P(2)H(4), is coordinated to two CpRu(PPh(3))(2) fragments, and in the latter thiophosphinous acid, H(2)PSH, is coordinated to the metal centre through the phosphorus atom. All compounds were characterised by elemental analyses and IR and NMR spectroscopy. The crystal structures of 2, 3, 4 and 8 were determined by X-ray diffraction. 相似文献
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A new polymorph of the iminophosphorane Ph2P(CH2Py)(NSiMe3), ( 1 ), is compared to a just recently published. The reaction of the starting material, the phosphane Ph2P(CH2Py) with N3SiMe3 in the presence of water gives [Ph2P(CH2Py)(NH2)][N3], ( 2 ). A comparison of the structural and NMR parameters of 2 with previously reported derivatives of 1 , suggests that 2 is best described as a phosphonium salt in which the negatively charged imino nitrogen atom is protonated, according to [Ph2(CH2Py)P+—NH2][N3]—, rather than as an iminiumphosphane salt [Ph2(CH2Py)P=+NH2][N3]—. 相似文献
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Novel Silver‐Telluride Clusters Stabilised with Bidentate Phosphine Ligands: Synthesis and Structure of {[Ag5(TePh)6(Ph2P(CH2)2PPh3)](Ph2P(CH2)2PPh2)}∞, [Ag18Te(TePh)15(Ph2P(CH2)3PPh2)3Cl], and [Ag38Te13(Te t Bu)12(Ph2P(CH2)2PPh2)3] Bidentate phosphine ligands have been found effective to stabilise polynuclear cores containing silver and chalcogenide ligands. They can act as intra and intermolecular bridges between the silver centres. The clusters {[Ag5(TePh)6(Ph2P(CH2)2PPh3)](Ph2P(CH2)2PPh2)}∞ ( 1 ), [Ag18Te(TePh)15(Ph2P(CH2)3PPh2)3Cl] ( 2 ), and [Ag38Te13(TetBu)12(Ph2P(CH2)2PPh2)3] ( 3 ) have been prepared and their molecular structure determined. Compound 2 and 3 are molecular structures with separated cluster cores while 1 forms a polymeric chain bridged by phosphine ligands. ( 1 : space group P21/c (No. 14), Z = 4, a = 3518,1(7) pm, b = 2260,6(5) pm, c = 3522,1(7) pm, β = 119,19(3)°; 2 : space group R3 (No. 148), Z = 6, a = b = 3059,4(4) pm, c = 5278,8(9) pm; 3: space group Pccn (No. 56), Z = 4, a = 3613,0(9) pm, b = 3608,6(7) pm, c = 2153,5(8) pm) 相似文献
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Gómez-Ruiz S Wolf R Bauer S Bittig H Schisler A Lönnecke P Hey-Hawkins E 《Chemistry (Weinheim an der Bergstrasse, Germany)》2008,14(15):4511-4520
[Na{cyclo-(P(5)tBu(4))}] (1) reacts with [CuCl(PCyp(3))(2)] (Cyp=cyclo-C(5)H(9)) and [CuCl(PPh(3))(3)] (1:1) to give the corresponding copper(I) complexes with a tetra-tert-butylcyclopentaphosphanide ligand, [Cu{cyclo- (P(5)tBu(4))}(PCyp(3))(2)] (2) and [Cu{cyclo-(P(5)tBu(4))}(PPh(3))(2)] (3). The CuCl adduct of 2, [Cu(2)(mu-Cl){cyclo-(P(5)tBu(4))}(PCyp(3))(2)] (4), was obtained from the reaction of 1 with [CuCl(PCyp(3))(2)] (1:2). Compounds 2 and 3 rearrange, even at -27 degrees C, to give [Cu(4){cyclo- (P(4)tBu(3))PtBu}(4)] (5), in which ring contraction of the [cyclo-(P(5)tBu(4))](-) anion has occurred. The reaction of 1 with [AgCl(PCyp(3))](4) or [AgCl(PPh(3))(2)] (1:1) leads to the formation of [Ag(4){cyclo-(P(4)tBu(3))PtBu}(4)] (6). Intermediates, which are most probably mononuclear, "[Ag{cyclo-(P(5)tBu(4))}(PR(3))(2)]" (R=Cyp, Ph) could be detected in the reaction mixtures, but not isolated. Finally, the reaction of 1 with [AuCl(PCyp(3))] (1:1) yielded [Au{cyclo-(P(5)tBu(4))}(PCyp(3))] (7), whereas an inseparable mixture of [Au(3){cyclo-(P(5)tBu(4))}(3)] (8) and [Au(4){cyclo-(P(4)tBu(3))PtBu}(4)] (9) was obtained from the analogous reaction with [AuCl(PPh(3))]. Complexes 3-7 were characterised by (31)P NMR spectroscopy, and X-ray crystal structures were determined for 3-9. 相似文献
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Syntheses and Crystal Structures of [Cu4(As4Ph4)2(PRR′2)4], [Cu14(AsPh)6(SCN)2(PEt2Ph)8], [Cu14(AsPh)6Cl2(PRR′2)8], [Cu12(AsPh)6(PPh3)6], [Cu10(AsPh)4Cl2(PMe3)8], [Cu12(AsSiMe3)6(PRR′2)6], and [Cu8(AsSiMe3)4(PtBu3)4] (R, R′ = Organic Groups) Through the reaction of CuSCN with AsPh(SiMe3)2 in the presence of tertiary phosphines the compounds [Cu4(As4Ph4)2(PRR′2)4] ( 1 – 3 ) ( 1 : R = R′ = nPr, 2 : R = R′ = Et; 3 : R = Me, R′ = nPr) and [Cu14(AsPh)6(SCN)2(PEt2Ph)8] ( 4 ) can be synthesised. Using CuCl instead of CuSCN results to the cluster complexes [Cu14(AsPh)6Cl2(PRR′2)8] ( 5–6 ) ( 5 : R = R′ = Et; 6 : R = Me, R′ = nPr), [Cu12(AsPh)6(PPh3)6] ( 7 ) and [Cu10(AsPh)4Cl2(PMe3)8] ( 8 ). Through reactions of CuOAc with As(SiMe3)3 in the presence of tertiary phosphines the compounds [Cu12(AsSiMe3)6(PRR′2)6] ( 9 – 11 ) ( 9 : R = R′ = Et; 10 : R = Ph, R′ = Et; 11 : R = Et, R′ = Ph) and [Cu8(AsSiMe3)4(PtBu3)4] ( 12 ) can be obtained. In each case the products were characterised by single‐crystal‐X‐ray‐structure‐analyses. As the main structure element 1 – 3 each have two As4Ph42–‐chains as ligands. In contrast 4 – 12 contain discrete AsR2–ligands. 相似文献
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Chloroberyllates with Nitrogen Donor Ligands. Crystal Structures of (Ph4P)[BeCl3(py)], (Ph4P)2[(BeCl3)2(tmeda)], (Ph4P)[BeCl2{(Me3SiN)2CPh}], and (Ph4P)2[BeCl4] · 2CH2Cl2 The title compounds were obtained as colourless, moisture sensitive crystals by reactions of (Ph4P)2[Be2Cl6] with pyridine, tmeda (N, N′‐tetramethylethylendiamine), or with the silylated benzamidine PhC—[N(SiMe3)2(NSiMe3)], whereas the tetrachloro beryllate was isolated as a by‐product from a solution in dichloromethane in the presence of the silylated phosphaneimine Me3SiNP(tol)3. All compounds were characterized by crystal structure determinations and by IR spectroscopy. (Ph4P)[BeCl3(Py)] ( 1 ): Space group Pbcm, Z = 4, lattice dimensions at 193 K: a = 756.2(1), b = 1739.2(2), c = 2016.3(2) pm, R1 = 0.0626. The complex anion contains tetrahedrally coordinated beryllium atom with a Be—N distance of 176.5 pm. (Ph4P)2[(BeCl3)2(tmeda)]·2CH2Cl2 ( 2 ·2CH2Cl2). Space group P1¯, Z = 1, lattice dimensions at 193 K: a = 1072.7(1), b = 1132.6(1), c = 1248.9(1) pm, α = 95.34(1)°, β = 92.80(1)°, γ = 90.81(1)°, R1 = 0.0344. Both nitrogen atoms of the tmeda molecule coordinate with BeCl3— units forming the centrosymmetric complex anion with Be—N distances of 181.3 pm. (PPh4)[BeCl2{(Me3SiN)2CPh}] ( 3 ). Space group C2, Z = 2, lattice dimensions at 193 K: a = 1255.4(2), b = 1401.9(2), c = 1085.2(2) pm, R1 = 0.0288. In the complex anion the benzamidinato ligand {(Me3SiN)2CPh}— acts as chelate with Be—N distances of 174.9 pm. (Ph4P)2[BeCl4]·2CH2Cl2 ( 4 ·2CH2Cl2). Space group P2/c, Z = 4, lattice dimensions at 193 K: a = 2295.4(1), b = 982.5(1), c = 2197.2(2) pm, β = 99.19(1)°, R1 = 0.0586. 4 ·2CH2Cl2 contains nearly ideal tetrahedral [BeCl4]2— ions, like the previously described 4 ·2, 5CH2Cl2, which crystallizes in the space group P1¯, with Be—Cl distances of 203.4 pm on average. 相似文献
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Luis Adrio Gemma Alberdi Adriana Amoedo Darío Lata Alberto Fernndez Javier Martínez M. Teresa Pereira Jos M. Vila 《无机化学与普通化学杂志》2005,631(11):2197-2203
Reaction of the thiosemicarbazone ligands C4H4NC(H)=NN(H)C(S)NHR (R = Me, a ; Et, b ) with Li2[PdCl4] gave the dinuclear complexes [Pd{C4H4NC(H)=NNC(S)NHR}(μ‐Cl)]2 (R = Me, 1a ; Et, 1b ) with a central Pd2Cl2 core and with deprotonation of the thiosemicarbazones at the hydrazinic nitrogen atom. Treatment of 1a and 1b with triphenylphosphine gave the mononuclear compounds [Pd{C4H4C(H)=NNC(S)NHR}(Cl)(PPh3)] (R = Me, 2a ; Et, 2b ), whereas reaction of 1a and 1b with tertiary diphosphines gave mono‐ and dinuclear compounds, as appropriate, with the corresponding diphosphine acting as a monodentate ( 6b ), chelating ( 3a ) and bridging ligand ( 4a, 5a , 4b, 5b ). Treatment of 1a and 1b with (Ph2PCH2CH2PPh2)W(CO)5 gave the new heterobimetallic complexes 7a and 7b . The crystal structures of complexes 3a and 4a are described. 相似文献