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1.
《Journal of organometallic chemistry》1991,407(2):C13-C15
The dianion [Ru10C(CO)24]2− in CH2Cl2 reacts with CO under ambient conditions to produce quantitative amounts of the species [Ru3(CO)12] and [Ru6C(CO)16]2−; the hydrido-anion [HRu10C(CO)24]− reacts similarly to form [Ru6C(CO)16]−. 相似文献
2.
3.
《Journal of organometallic chemistry》1989,377(1):C17-C22
X-ray structural studies of new thermolysis products from the reaction of Ru3(CO)12 in heptane in the presence of 1,3,5-trimethylbenzene (mesitylene) confirm that they are the decaruthenium carbido-cluster dianion [Ru10C(CO)24]2− (I) and the hydrido decaruthenium carbido-cluster monoanion [HRu10C(CO)24]− (II). Both anions have the giant tetrahedron Ru10 metal framework, and the monohydride provides the first example of a hydrido ligand in a tetrahedral Ru4 cavity. 相似文献
4.
Angelo J. Amoroso Brian F. G. Johnson Jack Lewis Chi-Keung Li Catherine A. Morewood Paul R. Raithby Maria D. Vargas Wing-Tak Wong 《Journal of Cluster Science》1995,6(1):163-173
Reduction of the heptaosmium cluster [Os7(CO)21] With [Et4N][NH4) gives the cluster dianion [Os7(CO)20]2–,1, in high yield. The reaction of the dianion with [AuPR
3Cl] (R=Et or Ph) in the presence of TlPF6 forms [Os7((CO)20(AuPR
3)2] [R=Et (2a);R = Ph(2b)] in 80% yield, while the corresponding reaction with (Os(C6H6)(CH3CN)3]2+ gives [Os8(CO)20 (
6-C6H6)] (3) in reasonable yield (ca. 30%). The dianion,1, and the clusters2 and3 have been fully characterized by bout spectroscopic and crystallographic methods. The crystal structure of the [Ph4P]+ salt of1 shows that the metals in the anion adopt a capped octahedral geometry, with all twenty carbonyl ligands in terminal sites. The metal core geometry in2a is best described as a tricapped octahedron, and is based on the structure of the dianion1 with two adjacent octahedral faces capped by the Au atoms of the two AuPEt3 groups. In a similar fashion, the geometry of3 is related to that of1 with the addition of an Os(C6H6) unit capped to a triangular face, to give a bicapped octahedral framework. 相似文献
5.
Thomas E. Concolino Judith L. Eglin Chad E. Hadden Rickey P. Hicks Richard J. Staples Edward J. Valente Jeffrey D. Zubkowski 《Journal of Cluster Science》2000,11(1):109-123
The complex Re2Cl6(P-n-Bu3)2 prepared in situ reacts with CH3CN to form a blue-green solution. Addition of the chelating phosphine bis(diphenylphosphino)methane (dppm) results in the formation of the complex [Re2Cl3(-dppm)2(NCCH3)2][Cl] (1) upon heating. The two acetonitrile molecules adopt a trans geometry on the rhenium center with the axially coordinated chlorine. The analogous trans benzonitrile species [Re2Cl3(-dppm)2(NCC6H5)2][Cl]·2CH2Cl2 (2) is synthesized under the same reaction conditions. The coupling constants of the AABB 31P{1H} NMR spectra of the compounds were elucidated from 31P–31P homonuclear J-resolved NMR experiments. Additional characterization methods include 31P{1H} NMR spectroscopy, UV-vis spectroscopy, and X-ray crystallography. 相似文献
6.
《Polyhedron》1999,18(26):3533-3544
[Tris(1,3-dithiole-2-thione-4,5-dithiolato)stannate]2−, [Q]2[Sn(C3S5)3], [tris(1,3-dithiole-2-one-4,5-dithiolato)stannate]2−, [Q]2[Sn(C3S4O)3], and [tris(1,3-dithiole-2-thione-4,5-diselenolato)stannate]2− [Q]2[Sn(C3S3Se2)3], complexes, have been synthesised and characterised. Crystal structure determinations of [Q]2[Sn(C3S5)3] (Q=1,4-dimethylpyridinium, monoclinic and orthorhombic forms; NMe4, NEt4, and PPh4) and [NEt4]2[Sn(C3S4O)3] revealed variations in the overall dianion structures. The geometry about tin in each case is essentially octahedral with the chelate bite angles in the range 80.7(5)–87.45(4)°: the range of Sn–S distances is 2.5207(18)–2.571(17) Å. A statistical analysis, carried out on the crystal structure data for the six complexes, indicated that the most critical factors in controlling the overall shape of the dianion were the distances of the Sn atom from the dithiolate ligand planes [Sn–OOP]. Interanionic S⋯S interactions, within the sum of the van der Waals’ radii for two S atoms, are affected by the size of the cation, Q; the secondary connectivity is 3-dimensional for the smallest cations, Q=1,4-dimethylpyridinium and NMe4, in chains for the somewhat larger cation, NEt4 and is absent for the still larger, PPh4 cation. 相似文献
7.
Ching-Juh Way Yun Chi Ipe J. Mavunkal Sue-Lein Wang Fen-Ling Liao Shie-Ming Peng Gene-Hsiang Lee 《Journal of Cluster Science》1997,8(1):87-100
Treatment of carbido cluster Ru5(μ 5-C)(CO)15 with Me3NO in acetonitrile solution followed by addition of dimethyl maleate or dimethyl acetylene dicarboxylate affords new clusters Ru5(μ 5-C)(CO)13[C2H2(CO2Me)2] (1) and Ru5(μ 5-C)(CO)15[C2(CO2Me)2] (2), respectively. Single crystal X-ray structural studies reveal that both complexes contain a wingtip-bridged butterfly pentametallic skeleton. In complex1 the maleate fragment is coordinated to one wingtip Ru atom through its carbon-carbon double bond and to the adjacent Ru atom by the formation of two O → Ru dative bonding interactions, while the acetylene dicarboxylate fragment in2 is best considered as acis-dimetallated alkene, linking one hinge Ru atom and the nearby Ru atom at the bridged position. Crystal data for1: space group P 42/n;a=20.199(6),c=13.941(3) Å,Z=8; finalR F=0.025,R w=0.026 for 3963 reflections withI>2σ(I). Crystal data for2: space group P21/n;a=9.634(3),b=20.062(6),c=17.372(5) Å,β=90.62(2)°,Z=4; finalR F=0 033,R w=0.036 for 4683 reflections withI>3σ(I). 相似文献
8.
《Polyhedron》2001,20(9-10):1107-1113
The reactions of dipropargyl manolate and terephthalate, respectively, with Co2(CO)8 in THF at room temperature gave four new compounds [R(CO2CH2C2H-μ)2][Co2(CO)6]2 (R=CH2, 1a; R=C6H4, 1b) and [(HC2CH2OCO)R(CO2CH2C2H-μ)][Co2(CO)6] (R=CH2, 2a; R=C6H4-1,4-, 2b), and compounds 2a and b reacted with RuCo2(CO)11 to form two new linked clusters [R(CO2CH2C2H-μ)2][Co2(CO)6][RuCo2(CO)9] (R=CH2, 3a; R=C6H4-1,4-, 3b). The treatment of two dipropargyl esters, respectively, with RuCo2(CO)11 afforded another two new clusters [R(CO2CH2C2H-μ)2][RuCo2(CO)9]2 (R=CH2, 4a; R=C6H4-1,4-, 4b). The reactions of dipropargyl manolate, terephalate with Mo2Cp2(CO)4 gave rise to the formation of dinuclear complexes [(HC2CH2OCO)R(CO2CH2C2H-μ)][Mo2Cp2(CO)4] (R=CH2, 5a; R=C6H4-1,4-, 5b), compound 5a reacted with Co2(CO)8 to produce the cluster [CH2(CO2CH2C2H-μ)2][Co2(CO)6][Mo2Cp2(CO)4] 6a. All the new clusters have been characterized by C/H elemental analysis, IR and 1H NMR spectroscopies. The structure of [CH2(CO2CH2C2H-μ)2][Co2(CO)6]2 1a and [p-(HC2CH2OCO)C6H4(CO2CH2C2H-μ)][Co2(CO)6] 2b have been determined by single crystal X-ray diffraction methods. 相似文献
9.
WANG Tao FAN Yu-guo 《高等学校化学研究》1993,9(2):99-103
A cobalt complex with mixed valence state [Co( Ⅰ ) (dppe)2CO]2 [Co2 ( Ⅱ )(dppe) Cl]6O2] (dppe = 1,2 - bis(diphenylphosphino) ethane) has been prepared. The compound crystallizes in triclinic space group P1 with unit cell parameters: a=1. 1763(3) nm, b = 1. 2943(6) nm, c=2. 1507(9) nm, a=81. 44(4)°? ,β=82. 58(3)°, r = 79. 82(3)°, V = 3. 1691 nm3 and Z=1. The structure was solved by direct method according to ALPHA criterion and was refined by a block diagonal matrix least-squares procedure to final R= 0.084, Moreover, infared spectra, electronic reflection spectra and cyclic voltammetry curve were mearsured. 相似文献
10.
《Polyhedron》2003,22(25-26):3383-3387
Three new octahedral rhenium chalcocyanide cluster compounds [CuNH3(trien)]2[Re6S8(CN)6] · 7H2O (1), [CuNH3(trien)]2[Re6Se8(CN)6] (2) and [CuNH3(trien)]2[Re6Te8(CN)6] · H2O (3) exhibiting ionic structures have been obtained by the diffusion of an ammonia solution of KCs3[Re6S8(CN)6] (for 1), K4[Re6Se8(CN)6] · 3.5H2O (for 2) or Cs4[Re6Te8(CN)6] · 2H2O (for 3) into a glycerol solution of CuCl2 · 2H2O in the presence of trien (trien=triethylenetetramine). The compounds have been characterized by single-crystal X-ray diffraction. All three compounds contain a cationic complex [CuNH3(trien)]2+ which was not described previously. 相似文献
11.
Elena Lucenti Dominique Roberto Carmen Roveda Renato Ugo Elena Cariati 《Journal of Cluster Science》2001,12(1):113-122
New high yield routes to the high nuclearity hydrido carbonyl clusters [H5Os10(CO)24]- and [H4Os10(CO)24]2-, model systems for the chemisorption of CO and H2 on metal surfaces, are reported. [H5Os10(CO)24]- is obtained in good yields by hydrogenation (1 atm) at 200°C of physisorbed [Os(CO)3(OH)2]n whereas in refluxing ethylene glycol solution, that is less acidic than the silica surface, [H4Os10(CO)24]2- is obtained in high yield starting from [Os(CO)3(OH)2]n or, more conveniently, from -[Os(CO)3Cl2]2 in the presence of the stoichiometric amount of sodium carbonate. The quantitative equilibrium
is confirmed. 相似文献
12.
《Journal of Coordination Chemistry》2012,65(1-3):163-172
Abstract The kinetics of the transformation of [Ru6(CO)18]2? into [Ru6C(CO)16]2? in diglyme over the temperature range 130–160°C have been determined. The results are consistent with reversible loss of a carbonyl ligand from [Ru6(CO)18]2?, followed by formation of carbon dioxide and reassociation of carbon monoxide to give the observed product. Mass spectral analysis of the evolved carbon dioxide trapped as barium carbonate supports an intramolecular pathway for the disproportionation of carbon monoxide. 相似文献
13.
The title compound [Co3(CO)9(μ3-C)C(O)OCH2]2 was synthesized by the reaction of [Cl3CC(O)OCH2]2 with Co2(CO)8 at 40~50 ℃. Crystal data: C24H4O22Co6, Mr=997.88, monoclinic, space group P21/n(#14), a=9.330(2), b=15.197(4), c=11.783(4), β=91.16(2)°, V=1670.4(7) 3, Z=2, Dc=1.984 g/cm3, μ(MoKα)=30.01 cm-1, F(000)=972.00, T=293K, final R=0.045, Rw=0.051 for 1936 observed reflections with I>2σ(I). The structure contains two centrosymmetric dimeric molecules in a unit cell, each of which has two tetrahedral skeletons (CCo3) connected through a C(O)OCH3CH2OC(O) bridge. 相似文献
14.
Cp2Cr2(CO)4( - 2 - P2), 1, reacts with one molar equivalent of Fe2(CO)9 in THF to yield the mono- and di-iron complexes, Cp2Cr2(CO)4P2[Fe(CO)4], 2, (16.5% yield) and Cp2Cr2(CO)4P2[Fe(CO)4]2, 3, (16.9% yield), as dark magenta brown and dark greenish brown crystals, respectively. Both complexes were characterized by single-crystal X-ray diffraction analysis. Crystal data –2: space group =P21/c,a=17.024(1) Å,b=8.180(1) Å,c=30.891(2) Å, =100.953(5)°,V=4223.4(7)Å3,Z=8, 3743 observed reflections,R
F=0.033; 3: space group P1,a=10.209(2) Å,b=10.212(2) Å,c=15.989(3) Å, =106.93(1)°, =91.87(1)°, =119.50(1)°,V=1356.5(4) Å3,Z=2, 3489 observed reflections,R
F=0.029. 相似文献
15.
A. I. Yanovsky F. M. Dolgushin Yu. T. Struchkov V. S. KaganovicH M. I. Rybinskaya 《Russian Chemical Bulletin》1995,44(6):1072-1079
It has been established by X-ray structural study that the bicluster cobalt -arene complex of diphenylmethane [6-PhCo4CO9]2CH2 and binuclear complex [6-PhCr(CO)3]2CH2 have ans-trans-s-trans conformation in their crystals.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 6, pp. 1111–1117, June, 1995.This work was supported by the Russian Foundation for Basic Research (Projects No. 93-03-4028 and 94-03-08338). 相似文献
16.
《Journal of organometallic chemistry》1998,571(2):289-295
Antimony is reduced when [SbPh2BrO]2 is treated with Na[Mo(CO)3(η5-C5H5)] to produce [μ-SbPh2]2[Mo(CO)2(η5-C5H5)]2. A structure determination shows diphenylstibido groups bridging between two Mo(CO)2(η5-C5H5) moieties giving a central ‘butterfly’ shaped Sb2Mo2 ring. The cyclopentadiene rings are trans to each other and Mo–Sb and Sb–Sb separations are both short. An iron analogue could not be obtained from [SbPh2BrO]2 and Na[Fe(CO)2(η5-C5H5)] but a mixture of SbPh[Fe(CO)2(η5-C5H5)]2 and SbPh2[Fe(CO)2(η5-C5H5)] was obtained using SbPh2Cl. An X-ray structure for SbPh[Fe(CO)2(η5-C5H5)]2 shows an open stibinidine structure. 相似文献
17.
《Journal of organometallic chemistry》1991,407(2):C9-C12
The reaction in THF of Na2[Fe(CO)4·xTHF with InBr3 in an approximate 3.5:1 molar ratio affords the new [In{Fe(CO)4}3]3− trianion, which has been isolated as its trimethylbenzylammonium salt and structurally characterized by single-crystal X-ray diffraction studies. On oxidation with two equivalents of AgBF4 it stepwise affords the anions [In2Fe6(CO)24]x− with x = 4 and 2, respectively. Its reaction with InBr3 gives species of the composition [InBr3−x{Fe(CO)4x}]x− (x = 1,2), and the anion with the composition [InBr2{Fe(CO)4}]− has been structurally characterized as the dimeric species [InBr2Br4{η-Fe(CO)4}2]2−. 相似文献
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19.
Stéphanie M. Cornet Michael P. Redmond David Collison Clint A. Sharrad Madeleine Helliwell John Warren 《Comptes Rendus Chimie》2010,13(6-7):832-838
The [NpO2(DPPMO2)2Cl][NpO2Cl4] complex (where DPPMO2 = bis(diphenylphosphino)methanedioxide) contains the linear neptunyl group, {NpO2}2+, with two bidentate P=O donor ligands. Coordinating anion Cl? fills the fifth equatorial coordination site yielding a complex of general formula [NpO2(DPPMO2)2X]2[Y] (1) (where X = Cl? and Y = [NpO2Cl4]2?. Reaction between our newly prepared neptunium starting material [NpO2Cl2(thf)]n and phosphinimine ligand produced crystals of [Ph3PNH2]2[NpO2Cl4] (2). Compounds 1 and 2 have been structurally characterised. 相似文献
20.
Simonov Yu. A. Gerbeleu N. V. Gdaniec M. Bourosh P. N. Koropchanu E. B. Bologa O. A. 《Russian Journal of Coordination Chemistry》2001,27(5):341-352
Compounds that form in the CoSiF6· 6H2O–NioxH2–A–water–alcohol system, where A is thiourea (Thio) or triphenylphosphine (PPh3) and NioxH2is 1,2-cyclohexanedione dioxime, were synthesized and characterized by X-ray diffraction analysis. Crystal structures of the [Co(NioxH)2(PPh3)2]SiF5and [Co(NioxH)2(Thio)2]2SiF6· 3H2O complexes were established. In octahedral Co(III) complexes, two radicals of 1,2-cyclohexanedione dioxime are bound by a hydrogen bond and are located in the equatorial plane. The intramolecular (– and H bonds) and intermolecular (C–H···F and H bonds) interactions in the crystal are discussed. 相似文献