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[(Mes3Sn)2MoO4], a Monomeric Triorganotin Molybdate Mes3SnBr (Mes = 1, 3, 5‐trimethylphenyl) reacts with (NBu4)2[Mo6O19] in the presence of (NBu4)OH (in CH3CN as solvent) to form [(Mes3Sn)2MoO4]. Alternatively the title compound can be obtained from the reaction of [MoO2(acac)2] (acac = 2, 4‐pentadionate) with Mes3SnOH in isopropanol. [(Mes3Sn)2MoO4] forms monoclinic crystals, space group C2/c, with a = 2271.6(3) pm, b = 825.2(1) pm, c = 2739.9(5) pm, β = 90.96(2)°. The crystal structure consists of isolated molecules in which a tetrahedral MoO4 unit is connected to two terminal Mes3Sn groups. The Mo‐O distances range from 169.6(4) to 181.1(3) pm and the Sn‐O distance is 204.8(3) pm. 相似文献
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[(Ph3Sn)3VO4]·CH3CN and [(Ph3Sn)3VO4]·2 DMF, Triphenyltin Vanadates with Novel Chain Structures The reaction of Na3VO4 with Ph3SnCl in a water/CH2Cl2 mixture leads to the formation of [(Ph3Sn)3VO4] ( 1 ). Recrystallization of 1 from toluene/CH3CN gives pale yellow crystals of [(Ph3Sn)3VO4]·CH3CN ( 2 ). 2 crystallizes as coordination polymer which consists of infinite chains composed of corner‐sharing VO4 tetrahedra and Ph3SnO2 trigonal bipyramides. Additionally the VO4 groups are connected to two terminal SnPh3‐Groups containing tin atoms in a tetrahedral environment. [(Ph3Sn)3VO4]·2 DMF ( 3 ) which is obtained from Na3VO4 and Ph3SnCl in a water/DMF mixture contains a polymeric chain structure similar to 2 and additionally one of the terminal SnPh3 groups is coordinated to a DMF solvent molecule. 相似文献
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(Me2NH2)[(Ph3Sn)3(MoO4)2], a Triorganotin Molybdate with Layer Structure The reaction of [(Ph3Sn)2MoO4] with (Me2NH2)Cl in an acetonitrile/water mixture leads to the formation of (Me2NH2)[(Ph3Sn)3(MoO4)2] ( 1 ). ( 1 ) crystallizes in the space group Pca21 with a = 1967.0(4), b = 1353.1(2) and c = 2176.6(5) pm. In the crystal structure of 1 Ph3SnO2 bipyramides and MoO4 tetrahedra are linked by corner sharing to give a layer structure. Additionally the layers are connected by O···H···N hydrogen bridges between MoO4 groups and [Me2NH2]+ ions to give a 3D network structure. 相似文献
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Treatment of copper(I) chloride with R2Si(NLiPh)2 (R = Me, Ph) in thf led to the formation of the octanuclear cluster compounds [Cu8{(R2Si(NPh)2}4] [R = Me ( 1 ), Ph ( 2 ).] Compound 1 crystallizes in the tetragonal space group P4/n, with a = 1505.41(5) and c = 1911.32(7) pm. The X‐ray crystal structure determination revealed a cube shaped Cu8 cluster core with μ4 bridging Me2Si(NPh)22– ligands. The copper atoms display an almost linear coordination with Cu–N distances in the range of 191.1(3)–191.4(3) pm. The Cu–Cu distances are 265.7(1)–267.3(1) pm. Compound 2 forms monoclinic crystals, space group P21/n, with a = 1461.87(4), b = 2483.77(6), c = 2725.49(8) pm, β = 100.77(1)°. The cluster core of compound 2 consists formally of two mutually perpendicular arranged trigonal prisms, which share a common square face. Like in the case of compound 1 the square faces of the cluster core are capped by μ4 bridging Ph2Si(NPh)22– ligands. The copper atoms adopt a nearly linear N–Cu–N coordination with Cu–N distances of 190.0(4)–195.1(4) pm. The Cu–Cu distances are 252.3(1)–305.6(1) pm. 相似文献
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Subhi A. Al-Jibori Rawaa A. Q. Al-Nassiry Ghassan H. H. Al-Jibori Kurt Merzweiler Christoph Wagner Harry Schmidt Sucharita Basak-Modi Graeme Hogarth 《Transition Metal Chemistry》2014,39(7):735-740
Reaction of Na2[PdCl4] with two equivalents of amino- or acetylamino-pyridines (LH) affords trans-[PdCl2-(LH)2] {LH = 2-amino-3-methylpyridine (2-ampyH), 3-aminopyridine (3-apyH), 2-acetylamino-3-methylpyridine (2-acmpyH), 3-acetylamino-pyridine (3-acpyH)}. An X-ray crystal structure of trans-[PdCl2(2-ampyH)2] shows that the 2-ampy-H ligands are coordinated in a monodentate fashion via the nitrogen atoms of the pyridine rings. Treatment of trans-[PdCl2(2-acmpyH)2] with NEt3 affords the cyclometalated complex, trans-[Pd(κ2-2-acmpy)2], the X-ray structure of which shows that the 2-acmpy ligand is coordinated to palladium in a bidentate fashion via the nitrogen atom of the pyridine ring and oxygen. Reaction of trans-[PdCl2(LH)2] with two equivalents of sodium saccharinate affords the bis(saccharinate) complexes, trans-[Pd(sac)2(LH)2], in which the saccharinate anions are coordinated via the amide nitrogen atom. 相似文献
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The thioether functionalized aminosilanes Me2Si(NH‐C6H4‐2‐SR)2 (R = Ph, Me) were lithiated with nBuLi and subsequently reacted with AgCl in the presence of PMe3 or with [AuCl(PMe3)]. In the case of Me2Si(NH‐C6H4‐2‐SPh)2 the dinuclear complexes [M2{Me2Si(NC6H4‐2‐SPh)2}(PMe3)2] (M = Ag; Au) were isolated. The analogous reactions starting from Me2Si(NH‐C6H4‐SMe)2 afforded the dinuclear gold complex [Au2{Me2Si(NC6H4‐2‐SMe)2}(PMe3)2] and the tetranuclear silver complex [Ag4{Me2Si(NC6H4‐2‐SMe)2}2(PMe3)2]. In the dinuclear compounds of the type [M2{Me2Si(NC6H4‐2‐SR)2}(PMe3)2], each of the silylamide N atoms is connected to a M(PMe3) group to give a nearly linear N–M–P arrangement with Ag–N and Au–N bonds in the range of 212.0(4)–213.3(4) pm and 205.3(3)–208.1(9) pm, respectively. [Ag4{Me2Si(NC6H4‐2‐SMe)2}2(PMe3)2] consists of a central Si2N4Ag2 ring with linearly coordinated Ag atoms (Ag‐N: 223.1(4)–222.1(4) pm) and two peripheral Ag(PMe3) units, which are connected to the amido N atoms in a chelating mode. The relatively short transannular Ag ··· Ag separation (277.6(1) pm) within the Si2N4Ag2 ring hints for argentophilic interactions. The peripheral Ag atoms are three coordinated with Ag–N distances of 233.9(4)–242.8(4) pm. 相似文献
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Copper(I) Clusters with Trifunctional Silyl Amide Ligands. Synthesis and Crystal Structures of [Li(THF)4]2[Cu10{RSi(NPh)3}4] (R = Me,Ph, Vin)
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Treatment of CuCl with the lithiated silyl amides RSi(NLiPh)3 (R = Me, Ph, Vin) in THF as solvent led to the formation of the novel CuI cluster compounds [Li(THF)4]2[Cu10{RSi(NPh)3}4]. For each of the three compounds the X‐ray crystal structure analysis revealed similar Si4N12Cu10 cores which are based on cubane like Cu8 cores bearing two additional peripheral copper atoms. The copper atoms are coordinated nearly linearly by the μ5‐bridging silyl amide ligands with Cu–N distances in the range of 187.1(3) to 194.5(4) pm and N–Cu–N angles of 171.6(1) to 178.7(1)°. For each of the compounds the structural parameters are very similar which indicates that the structures are barely influenced by the different steric requirements of the organic groups bound to silicon. 相似文献
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Christian Albrecht Christoph Wagner Kurt Merzweiler Tadeusz Lis Dirk Steinborn 《应用有机金属化学》2005,19(11):1155-1163
The platina‐β‐diketone [Pt2{(COMe)2H}2(µ‐Cl)2] ( 1 ) was found to react with monodentate phosphines to yield acetyl(chloro)platinum(II) complexes trans‐[Pt(COMe)Cl(PR3)2] (PR3 = PPh3, 2a ; P(4‐FC6H4)3, 2b ; PMePh2, 2c ; PMe2Ph, 2d ; P(n‐Bu)3, 2e ; P(o‐tol)3, 2f ; P(m‐tol)3, 2g ; P(p‐tol)3, 2h ). In the reaction with P(o‐tol)3 the methyl(carbonyl)platinum(II) complex [Pt(Me)Cl(CO){P(o‐tol)3}] ( 3a ) was found to be an intermediate. On the other hand, treating 1 with P(C6F5)3 led to the formation of [Pt(Me)Cl(CO){P(C6F5)3}] ( 3b ), even in excess of the phosphine. Phosphine ligands with a lower donor capability in complexes 2 and the arsine ligand in trans‐[Pt(COMe)Cl(AsPh3)2] ( 2i ) proved to be subject to substitution by stronger donating phosphine ligands, thus forming complexes trans‐[Pt(COMe)Cl(L)L′] (L/L′ = AsPh3/PPh3, 4a ; PPh3/P(n‐Bu)3, 4b ) and cis‐[Pt(COMe)Cl(dppe)] ( 4c ). Furthermore, in boiling benzene, complexes 2a – 2c and 2i underwent decarbonylation yielding quantitatively methyl(chloro)platinum(II) complexes trans‐[Pt(Me)Cl(L)2] (L = PPh3, 5a ; P(4‐FC6H4)3, 5b ; PMePh2, 5c ; AsPh3, 5d ). The identities of all complexes were confirmed by 1H, 13C and 31P NMR spectroscopy. Single‐crystal X‐ray diffraction analyses of 2a ·2CHCl3, 2f and 5b showed that the platinum atom is square‐planar coordinated by two phosphine ligands (PPh3, 2a ; P(o‐tol)3, 2f ; P(4F‐C6H4)3, 5b ) in mutual trans position as well as by an acetyl ligand ( 2a, 2f ) and a methyl ligand ( 5b ), respectively, trans to a chloro ligand. Single‐crystal X‐ray diffraction analysis of 3b exhibited a square‐planar platinum complex with the two π‐acceptor ligands CO and P(C6F5)3 in mutual cis position (configuration index: SP‐4‐3). Copyright © 2005 John Wiley & Sons, Ltd. 相似文献
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