共查询到20条相似文献,搜索用时 15 毫秒
1.
Michael I Bruce Andrew C Meier Allan H White 《Journal of organometallic chemistry》2004,689(5):965-970
The reaction between Ru3(μ-H){μ3-C2CPh2(OH)}(CO)9 and HCCPh, carried out in the presence of HBF4 · Me2O, afforded the cluster complexes Ru3(μ-H)(μ3-CPh2CCCCPh)(CO)9 (5) and Ru3{μ3-CPhCHCC(CPh2)CHCPh}(μ-CO)(CO)8 (6), both of which were characterised by single-crystal X-ray studies. 相似文献
2.
María G. Hernández-Cruz Micaela Hernández-Sandoval María J. Rosales-Hoz Verónica Salazar Francisco J. Zuno-Cruz 《Journal of organometallic chemistry》2011,696(10):2177-4078
The reaction between [Ru3(CO)10(NCMe)2] and [AuClPPh3] gave compound [Ru3(CO)10(μ-Cl)(μ-AuPPh3)] (1) in quantitative yield under very mild conditions. The reaction of 1 with 4-mercaptopyridine (4-pyS) using ultrasonic reaction conditions gave the heteronuclear compound [Ru3(CO)10(μ-AuPPh3)(μ-SC5H4N)] (2) in moderate yield. There was no spectroscopic evidence that indicates the formation of the hydride isolobal analog in this reaction. The homonuclear cluster [Ru3(CO)8(μ-H)(μ-SC5H4N)(μ-dppe)] (3) was prepared by a selective reaction employing the ruthenium-diphosphine derivative [Ru3(CO)10(μ-dppe)] (dppe = 1,2-bis(diphenylphosphine)ethane) with 4-pyS in THF solution. The isolobal analog to compound 3, compound [Ru3(CO)8(μ-AuPPh3)(μ-SC5H4N)(μ-dppe)] (4) was synthesized by the reaction between compound 2 and dppe in refluxing dichloromethane. Compounds 1-4 were characterized in solution by spectroscopic methods and the molecular structure of compounds 2 and 3 in the solid state was obtained by single crystal X-ray diffraction studies. 相似文献
3.
Mien Wei Lum 《Journal of organometallic chemistry》2003,687(1):203-208
Reaction of the cluster Os3(μ-H)(μ-OH)(CO)10 (1) with 1-naphthol afforded the isomeric clusters 2a and 3a with the formulae Os3(μ-H)2(μ3-1-OC10H6)(CO)9. A similar reaction with 2-naphthol, however, gave Os3(μ-H)(μ-2-OC10H7)(CO)10, 4b, and the analogue of 2a. These clusters have been structurally characterised to confirm the mode of anchoring of the naphthols. 相似文献
4.
Md. Iqbal Hyder Md. Delwar H. Sikder Graeme Hogarth Shariff E. Kabir Christian J. Richard 《Journal of organometallic chemistry》2009,694(2):304-174
Reaction of [Ru3(CO)10(μ-dppm)] (1) with H2S at 66 °C affords high yields of the sulfur-capped dihydride [Ru3(CO)7(μ-H)2(μ-dppm)(μ3-S)] (2), formed by oxidative-addition of both hydrogen-sulfur bonds. Hydrogenation of [Ru3(CO)7(μ-dppm)(μ3-CO)(μ3-S)] (3) at 110 °C also gives 2 in similar yields, while hydrogenation of [Ru3(CO)7(μ-dppm)(μ3-CO)(μ3-Se)] (4) affords [Ru3(CO)7(μ-H)2(μ-dppm)(μ3-Se)] (5) in 85% yield. The molecular structures of 2 and 5 reveal that the diphosphine and one hydride simultaneously bridge the same ruthenium-ruthenium edge with the second hydride spanning one of the non-bridged edges. Both 2 and 5 are fluxional at room temperature being attributed to hydride migration between the non-bridged edges. Addition of HBF4 to 2 affords the cationic trihydride [Ru3(CO)7(μ-H)3(μ-dppm)(μ3-S)][BF4] (6) in which the hydrides are non-fluxional due to the blocking of the free ruthenium-ruthenium edge. 相似文献
5.
6.
Gloria Sánchez-Cabrera Francisco J. Zuno-Cruz María J. Rosales-Hoz 《Journal of organometallic chemistry》2007,692(11):2138-2147
The compound [Os3(CO)10(μ-Cl)(μ-AuPPh3)] (2) was prepared from the reaction between [Os3(CO)10(NCMe)2] (1) and [AuClPPh3] under mild conditions. The reaction of 2 with 4-mercaptopyridine (4-pyS) ligand yielded compounds [Os3(CO)10(μ-H)(μ-SC5H4N)] (4), formed by isolobal replacement of the fragment [AuPPh3]+ by H+ and [Os3(CO)10(μ-AuPPh3)(μ-SC5H4N)] (5). [Os3(CO)10(μ-H)(μ-SC5H4N)] (4) was also obtained by substitution of two acetonitrile ligands in the activated cluster 1 by 4-pyS, at room temperature in dichloromethane. Compounds 2-5 were characterized spectroscopically and the molecular structures of 4 and 5 in the solid state were obtained by single crystal X-ray diffraction studies. 相似文献
7.
Tobias Mayer 《Journal of organometallic chemistry》2011,696(21):3415-3420
A convenient synthesis and the characterization of six new electronically and coordinatively unsaturated complexes of the formula [Ru2(CO)4(μ-H)(μ-PtBu2)(μ-L2)] (2b-g) (RuRu) is described exhibiting a close relation to the known [Ru2(CO)4(μ-H)(μ-PtBu2)(μ-dppm)] (2a). The complexes 2b-g were obtained in a kind of one-pot synthesis starting from [Ru3(CO)12] and PtBu2H in the first step followed by the reaction with the bidentate bridging ligand in the second step. The method was developed for the following bridging ligands (μ-L2): dmpm (2b, dmpm = Me2PCH2PMe2), dcypm (2c, dcypm = Cy2PCH2PCy2), dppen (2d, dppen = Ph2PC(=CH2)PPh2), dpppha (2e, dpppha = Ph2PN(Ph)PPh2), dpppra (2f, dpppra = Ph2PN(Pr)PPh2), and dppbza (2g, dppbza = Ph2PN(CH2Ph)PPh2). The molecular structures of all new complexes 2b−g were determined by X-ray diffraction. 相似文献
8.
Md. Iqbal Hossain Graeme Hogarth Shariff E. Kabir 《Journal of organometallic chemistry》2011,696(18):3036-3039
Allene reacts with the benzothiazolide clusters [Os3(CO)9(μ3-NSC7H3R)(μ-H)] (R = H, Me) to afford the bridging allyl complexes [Os3(CO)7(μ-CO)2(μ-NSC7H3R)(μ-η1:η2:η1-CH2CHCH2)] resulting from insertion of allene into the metal-hydride. Both have been crystallographically characterized and differ with respect to the relative arrangement of allyl and benzothiazolide at the triosmium centre. 相似文献
9.
A. A. Pasynskii I. V. Skabitskii Yu. V. Torubaev I. M. Krylov G. G. Aleksandrov 《Russian Journal of Coordination Chemistry》2011,37(8):613-618
A reaction of the dimer [Mn(CO)4(SPh)]2 with (PPh3)2Pt(C2Ph2) gave the heterometallic complex (CO)4Mn(μ-SPh)Pt(PPh3)2 (I) and its isomer (CO)3(PPh3)Mn(μ-SPh)Pt(PPh3)(CO) (II). A reaction of complex I with a diphosphine ligand (Dppm) yielded the heterometallic complex (CO)3Mn(μ-SPh)Pt(PPh3)(Dppm) (III). Complexes I–III were characterized by X-ray diffraction. In complex I, the single Mn-Pt bond (2.6946(3) ?) is supplemented with a thiolate bridge with the shortened Pt-S and Mn-S bonds (2.3129(5)
and 2.2900(6) ?, respectively). Unlike complex I, in complex II, one phosphine group at the Pt atom is exchanged for one CO group at the Mn atom. The Mn-Pt bond (2.633(1) ?) and the thiolate
bridge (Pt-S, 2.332(2) ?; Mn-S, 2.291(2) ?) are retained. In complex III, the Mn-Pt bond (2.623(1) ?) is supplemented with thiolate (Pt-S, 2.341(2) ?; Mn-S, 2.292(2) 0?) and Dppm bridges (Pt-P,
2.240(1)?; Mn-P, 2.245(2) ?). Apparently, the Pt atom in complexes I–III is attached to the formally double bond , as in Pt complexes with olefins. 相似文献
10.
Yong Leng Kelvin Tan 《Journal of organometallic chemistry》2006,691(9):2048-2054
The heteronuclear cluster RuOs3(μ-H)2(CO)13 (4) reacts with refluxing toluene to form the clusters Ru2Os3(μ-H)2(CO)16 (5) RuOs3(CO)9(μ-CO)2(η6-C6H5Me) (6) and Ru2Os3(CO)12(μ-CO)(η6-C6H5Me) (7). Cluster 5 exists as a mixture of five isomers. The inter-relationship among the clusters has also been investigated. 相似文献
11.
Yong Leng Kelvin Tan 《Journal of organometallic chemistry》2007,692(11):2253-2269
The heteronuclear cluster RuOs3(μ-H)2(CO)13 (1) reacted readily with a number of ditertiary phosphines under chemical activation with trimethylamine-N-oxide. The solid-state and solution structures of these derivatives have been examined. Six structural types have been characterized crystallographically, including one in which a phenyl group migrates from the ditertiary phosphine ligand to the metal framework. There are many more isomers present in solution, most of which are rapidly inter-converting via hydride migrations. 相似文献
12.
Yong Leng Kelvin Tan 《Journal of organometallic chemistry》2007,692(4):768-773
The heteronuclear cluster RuOs3(μ-H)2(CO)13 (1) reacts with indene under thermal activation to afford the novel clusters RuOs3(μ-H)(CO)9(μ-CO)2(η5-C9H7) (3), RuOs3(μ-H)(CO)9(μ3,η5:η2:η2-C9H7) (4) and Ru2Os3(μ-H)(CO)11(μ3,η5:η2:η2-C9H7) (5), the latter two possessing indenyl ligands in the μ3,η5:η2:η2 bonding mode. Cluster 5 exists as a mixture of two isomers. The inter-relationship among the clusters has also been investigated. 相似文献
13.
Pt(P-t-Bu3)2 reacts with the bismuthtrirhenium complex Re3(CO)12(μ-BiPh2)(μ-H)2, 1 at 68 °C to give eight complexes PtRe2(CO)9P(t-Bu3)(μ-H)2, 2, PtRe3(CO)12P(t-Bu3)(μ-Ph)(μ-H)(μ4-Bi), 3, PtRe3(CO)13P(t-Bu3)(μ4-Bi)(μ-H)2, 4, PtRe4(CO)16P(t-Bu3)(μ-H)2(μ4-Bi)(μ3-Bi), 5, Pt2Re5(CO)21[P(t-Bu)3]2(μ-H)3(μ4-Bi)2, 6, trans-Pt2Re5(CO)22[P(t-Bu)3]2(μ-H)3(μ4-Bi)2,trans-7, cis-Pt2Re5(CO)22[P(t-Bu)3]2(μ-H)3(μ4-Bi)2, cis-7, (an isomer of trans-7) and Re3(CO)13[PtPBut3]2(μ-H)2(μ4-Bi), 8, all in low yields. When 4 was treated with Pt(P-t-Bu3)2 at 68 °C, compounds 2, trans-7, cis-7, and Pt2Re4(CO)18[P(t-Bu)3]2(μ-H)2(μ4-Bi)2, 9 were formed. When 8 was treated with CO at 25 °C, compounds 2, trans-7, 9, and PtRe3(CO)9P(t-Bu)3(μ3-Bi)(μ4-Bi2), 10 were formed. In all of the products both of the phenyl rings from the bridging BiPh2 ligand of 1 were cleaved from the bismuth atom. Only compound 3 contains a phenyl ligand and that ligand was a bridging ligand across the Pt-Re bond. All of the products, except 10, and the known compound 2, contain spiro, μ4-Bi ligands. The higher nuclearity complexes 5, 6, trans-7, cis-7, and 9 contain two bismuth ligands. Compound 10 contains three bismuth atoms. Two of the bismuth atoms in 10 are part of an octahedrally-shaped Re3PtBi2 cluster. The third bismuth atom is a triply-bridging ligand on the triangular Re3 face of the cluster. When a mixture of 4 and 8 was heated to 68 °C in the presence of CO, the new compound PtRe4(CO)17(P-t-Bu3)(μ-H)2(μ4-Bi), 11 was formed. The molecular structures of all of the new complexes were characterized by single-crystal X-ray diffraction analyses. 相似文献
14.
Arun K. Raha Md. Manzurul Karim Noorjahan Begum Edward Rosenberg 《Journal of organometallic chemistry》2008,693(24):3613-3621
Treatment of unsaturated [Os3(CO)8{μ3-Ph2PCH2P(Ph)C6H4}(μ-H)] (2) with tBuNC at room temperature gives [Os3(CO)8(CNBut)){μ3-Ph2PCH2P(Ph)C6H4}(μ-H)] (3) which on thermolysis in refluxing toluene furnishes [Os3(CO)7(CNBut){μ3-Ph2PCHP(Ph)C6H4}(μ-H)2] (4). Reaction of the labile complex [Os3(CO)9(μ-dppm)(NCMe)] (5) with tBuNC at room temperature affords the substitution product [Os3(CO)9(μ-dppm)(CNBut)] (6). Thermolysis of 6 in refluxing toluene gives 4. On the other hand, the reaction of unsaturated [Os3(CO)9{μ3-η2-C7H3(2-Me)NS}(μ-H)] (7) with tBuNC yields the addition product [Os3(CO)9(CNBut){μ-η2-C7H3(2-Me)NS}(μ-H)] (8) which on decarbonylation in refluxing toluene gives unsaturated [Os3(CO)8(CNBut){μ3-η2-C7H3(2-Me)NS}(μ-H)] (9). Compound 9 reacts with PPh3 at room temperature to give the adduct [Os3(CO)8(PPh3)(CNBut){μ-η2-C7H3(2-Me)NS(μ-H)] (10). Compound 8 exists as two isomers in solution whereas 10 occurs in four isomeric forms. The molecular structures of 3, 6, 8, and 10 have been determined by X-ray diffraction studies. 相似文献
15.
Javier A. Cabeza Ignacio del Río Daniel Miguel 《Journal of organometallic chemistry》2007,692(16):3583-3587
The hexaruthenium cluster complexes [Ru6(μ3-H)(μ5-κ2-L)(μ- CO)(CO)15], HL = 2-mercaptopyridine (1) and 2-mercapto-6-methylpyridine (2), have been prepared by heating [Ru3(CO)12] with 0.5 equiv. of HL in THF at reflux temperature. An X-ray diffraction study on a crystal of complex 2 has determined that its metallic skeleton, a basal-edge-bridged square pyramid, is hold up by a (6-methylpyrid-2-yl)thiolate ligand. This ligand is attached to the four basal ruthenium atoms of the pyramid through the sulfur atom and to the edge-bridging ruthenium atom through the nitrogen atom. Such a coordination mode is unprecedented for (pyrid-2-yl)thiolate ligands. 相似文献
16.
Dafa Chen 《Journal of organometallic chemistry》2006,691(18):3823-3833
Thermal treatment of C9H7SiMe2C9H7 and C9H7Me2SiOSiMe2C9H7 with Ru3(CO)12 in refluxing xylene gave the corresponding diruthenium complexes (E)[(η5-C9H6)Ru(CO)]2(μ-CO)2 [E = Me2Si (1), Me2SiOSiMe2 (2)]. A desilylation product [(η5-C9H7)Ru(CO)]2(μ-CO)2 (3) was also obtained in the latter case. Similar treatment of C9H7Me2SiSiMe2C9H7 with Ru3(CO)12 gave a novel indenyl nonanuclear ruthenium cluster Ru9(μ6-C)(CO)14(μ3-η5:η2:η2-C9H7)2 (5) with carbon-centered tricapped trigonal prism geometry, in addition to the diruthenium complex (Me2SiSiMe2)[(η5-C9H6)Ru(CO)]2(μ-CO)2 (4) and the desilylation product 3. Complex 4 can undergo a thermal rearrangement to form the product [(Me2Si)(η5-C9H6)Ru(CO)2]2 (6). The molecular structures of 1, 2, 4, 5, and 6 were determined by X-ray diffraction. 相似文献
17.
Leonard Joachim Pereira 《Journal of organometallic chemistry》2005,690(4):1033-1043
TMNO-activated reaction of the heteronuclear cluster Os3Ru(μ-H)2(CO)13 (1) with diphenylphosphine afforded the novel phosphido-bridged clusters Os3Ru(μ-PPh2)(μ-H)3(CO)11 (2), Os3Ru(μ-PPh2)2(μ-H)2(CO)10 (3), Os3Ru(μ-PPh2)2(μ-H)4(CO)9 (4), and Os3Ru(μ-PPh2)(μ-H)3(CO)11(PPh2H) (5). The formation of 2-5 proceeded via P-H bond cleavage in the adduct Os3Ru(μ-H)2(CO)12(PPh2H) (6). Reaction of 2 with PPh3 afforded the adduct Os3Ru(μ-PPh2)(μ-H)3(CO)11(PPh3) (7) and the substituted derivative Os3Ru(μ-PPh2)(μ-H)3(CO)10(PPh3) (8). 相似文献
18.
The title complex is obtained by reacting Ru3(CO)12 with 1,4-dichloro-but-2-yne (ClCH2CCCH2Cl, DCB) in CH3OH/KOH solution (followed by acidification with HCl). The X-ray structure analysis shows that (μ-H)2Ru3(CO)9{μ3-η2-[H2CC(H)CCC(O)OCH3]} complex contains a “parallel” ene-yne acetyl substituent, H2CC(H)CCC(O)OCH3; the formation of such a ligand starting from DCB is - to our knowledge - unprecedented. The synthesis of complex (μ-H)2Ru3(CO)9{μ3-η2-[H2CC(H)CCC(O)OCH3]} occurs through the activation of CO and methanol. This process has been found for other reactions of functionalized alkynes with M3(CO)12 carbonyls (M = Fe, Ru) under basic methanolic conditions.The known hydridic cluster, (μ-H)Ru3(CO)9[μ3-η3-(MeCCHCH)] has been identified as the minor reaction product. 相似文献
19.
Yury Torubaev Pradeep Mathur Alexander Pasynskii. 《Journal of organometallic chemistry》2011,696(4):832-834
Treatment of ruthenium carbonyl, [Ru3(CO)12] with phenylseleno tribromide PhSeBr3 afforded a new triruthenium cluster, [(CO)10Br4Ru3(μ-SePh)2] (1). Its molecular structure was determined by single crystal XRD method (P21/c; a = 10.514(3) Å; b = 10.814(3) Å; c = 19.063(5) Å; β = 105.064(4)°; V = 2093.1(10) Å3) and shown to have two lateral Ru(CO)3Br2 units attached via two PhSe bridges to a Ru(CO)4 center forming a chain-like Ru-Se-Ru-Se-Ru cluster core. This is in contrast with a recently reported reaction of PhTeBr3 with [Ru3(CO)12] which formed a monomeric complex of ruthenium-dicarbonyl-dibromo fragment coordinating two PhTeBr ligands, [(CO)2RuBr2(PhTeBr)2]. 相似文献
20.
Rubén A. Machado María C. Goite Ysaura De Sanctis Lindora D’Ornelas 《Journal of organometallic chemistry》2005,690(3):622-628
Treatment of the labile compound [Os3(CO)10(CH3CN)2] with 2,3-bis(2-pyridyl)pyrazine (C14H10N4) in dichloromethane at room temperature gave the cluster [Os3(C14H10N4)(CO)10] (1), which contains the chelating ligand co-ordinated axially through one of the pyridine rings and equatorially through a pyrazine nitrogen atom while one of the pyridine rings remains unco-ordinated. Thermolysis of 1 leads to loss of CO and yields two structural isomers of [Os3(μ-H)(μ,η3-C14H9N4)(CO)9] (2) and (3). Isomer 2 contains an orthometallated 2-pyridyl group and a co-ordinated 2-pyridyl which is not orthometallated. A seven-membered chelate ring is formed and the pyrazine ring is uncoordinated. On the other hand, isomer 3 contains a 2-pyridyl-1,4-pyrazine fragment metallated in the pyrazine ring to form a five-membered chelate ring with the one pyridine ring remaining unco-ordinated. The molecular structures of 1-3 were confirmed by X-ray crystallographic studies. 相似文献