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1.
Michael I. Bruce Paul A. Humphrey Allan H. White 《Journal of organometallic chemistry》2004,689(15):2558-2561
The reaction between AuMe(PPh3) and Ru3(μ-H)3(μ3-CBr)(CO)9 (1) affords the novel heptanuclear cluster Au4Ru3(μ3-CMe)(Br)(CO)9(PPh3)3 (2), containing an Au/Ru3/Au trigonal pyramidal cluster face-capped by two Au(PPh3) groups and a CMe ligand, together with Au2Ru3(μ-H)(μ3-CMe)(CO)9(PPh3)2 (3), formed by isolobal replacement of two of the three μ-H atoms in 1 by Au(PPh3) groups. The latter co-crystallises with the analogous μ3-CH complex, as also shown spectroscopically. 相似文献
2.
Oxo/hydoxo zirconium(IV) complex of the general formula [Zr6(μ3-O)4(μ3-OH)4(OOCCH2tBu)9(μ2-OH)3]2 has been isolated, when Zr(OiPr)4 reacted with a 2-fold excess of 3,3-dimethylbutyric acid. Single crystal X-ray diffraction data, collected at 103 and 153 K, showed that the studied compound crystallizes in hexagonal system (P63/m (no. 176)). Structure consists of dimers composed of [Zr6(μ3-O)4(μ3-OH)4(OOCCH2tBu)9] sub-units, linked by six μ2-OH bridges. Infrared spectroscopic studies proved the presence of hydroxo groups in the structure of studied clusters and formation of different types of oxo/hydroxo bridges. The application of variable temperature infrared spectroscopy and differential scanning calorimetry revealed that the structure of this complex undergoes the phase transitions at 143–183 and 203–293 K. Comparison of spectral and crystallographic data suggests that these phase transitions might be related to changes in the strength of Zr–O bonds of μ2-OH bridges linking complex sub-units, and change in symmetry of the crystal lattice (from hexagonal to trigonal). Analysis of thermogravimetric data showed that decomposition of [Zr6(μ3-O)4(μ3-OH)4(OOCCH2tBu)9(μ2-OH)3]2 proceeds with complete conversion to ZrO2 (monoclinic form) between 603 and 803 K. 相似文献
3.
A new polymer azido-bridged copper(II) complex [Cu4(En)2(μ1,1-N3)4(μ1,1,1-N3)2(μ1,3-N3)2]
n
(I) (En = ethylenediamine) has been synthesized and crystallography characterized. Complex I shows one-dimensional coordination polymeric structure based on a tetranuclear cluster unit [Cu4(En)2(μ1,1-N3)4(μ1,1,1-N3)2(μ1,3-N3)2], in which the azido ions display three different bridging modes. 相似文献
4.
Charles E. Ellul 《Journal of organometallic chemistry》2010,695(1):6-2376
The reduction of trans-[Pd(NHC)2Cl2] (NHC = IMes, 1,3-bis(2,4,6-trimethylphenyl)imidazol-2-ylidene; IiPr2 = 1,3-bis-isopropylimidazol-2-ylidene) with potassium graphite under an atmosphere of CO affords the palladium NHC carbonyl clusters [Pd3(μ-CO)3(NHC)3] (NHC = IMes, 1; IiPr2, 3). Treatment of 1 with SO2 at room temperature yields the bridging SO2 complex [Pd3(μ-SO2)3(IMes)3] (4) in quantitative yield. Complexes 1, 3 and 4 have been structurally characterised by X-ray crystallography. 相似文献
5.
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
6.
P. A. Abramov M. N. Sokolov A. V. Virovets V. P. Fedin 《Journal of Structural Chemistry》2009,50(1):162-165
The crystal structure of [(C5Me4Et)3Rh3(μ3-Se)2](PF6)2 and [(C5Me4Et)2Rh2(μ2-Cl)3]PF6, obtained in the reaction of [(C5Me4Et)Rh(C6H6)](PF6)2 with ZnSe in 4M HCl under hydrothermal conditions, is determined. In agreement with the 18VE rule, the triangular cluster
contains single metal-metal bonds (Rh-Rh 2.864(1) ?), whereas they are absent in the binuclear complex (Rh ...Rh 3,216(1)
?).
Original Russian Text Copyright ? 2009 by P. A. Abramov, M. N. Sokolov, A. V. Virovets, and V. P. Fedin
__________
Translated from Zhurnal Strukturnoi Khimii, Vol. 50, No. 1, pp. 169–172, January–February, 2009. 相似文献
7.
I. Yu. Prikhod’ko V. P. Kirin V. A. Maksakov A. V. Virovets A. V. Golovin 《Journal of Structural Chemistry》2008,49(4):719-723
The complex Ru4(μ4-S)(μ,η3-C3H5)2(CO)12 is prepared and examined by IR and NMR spectroscopy; its crystal structure is determined (an automatic Bruker-Nonius X8 Apex
four-circle diffractometer equipped with a 2-D CCD-detector, 100 K, graphite-monochromated molybdenum source, λ = 0.71073
?). The crystal belongs to the orthorhombic crystal system with unit cell parameters a = 19.3781(9) ?, b = 12.2898(7) ?, c = 10.1726(4) ?, V = 2422.6(2) ?3, space group Pnma, Z = 4, composition C18H10O12Ru4S, d
x = 2.343 g/cm3. The molecule of point symmetry C
1 is situated on the mirror plane of the space group Pnma, two carbonyl groups at Ru2 and Ru3 atoms overlapping with the allylic ligand with a weight of 50% so that carbon atoms coincide.
Thus, we have a racemic structure with two overlapping enantiomers of the molecule of Ru4(μ4-S)(μ,η3-C3H5)2(CO)12.
Original Russian Text Copyright ? 2008 by I. Yu. Prikhod’ko, V. P. Kirin, V. A. Maksakov, A. V. Virovets, and A. V. Golovin
__________
Translated from Zhurnal Strukturnoi Khimii, Vol. 49, No. 4, pp. 748–752, May–June, 2008. 相似文献
8.
T. Yu. Glazunova A. I. Boltalin S. I. Troyanov 《Russian Journal of Coordination Chemistry》2005,31(4):247-252
Novel anhydrous trinuclear 3-oxo complexes of Cr(III), Cr3(3-O)(CF3COO)6(CH3COOH)2(CF3COO) (I) and of Cr(III,III,II), Cr3(3-O)(CF3COO)6(CH3COOH)2(THF) (II) (where THF is (CH2)4O) are synthesized by anodic dissolution of metallic chromium in solutions of trifluoroacetic acid in acetonitrile and in tetrahydrofuran and their structures are studied by X-ray diffraction analysis. Complex I forms orthorhombic crystals with space group Pna21, a = 9.778(1) , b = 16.042(2) , c = 22.851(4) , Z = 4, R
1 = 0.0332; complex II crystallizes in monoclinic system: space group P21/c, a = 9.866(1) , b = 17.895(2) , c = 21.167(4) , = 100.75(2)°, Z = 4, R = 0.0422. The average Cr-(3-O) distances in compounds I and II are almost equal (1.943(3) and 1.927(3) ). An average length of the Cr-O bond in octahedral surrounding of metal atoms is different in complexes I and II (1.985(4) and 2.003(3) , respectively), which is specified by different oxidation states of the metal atom. The CrCr distances lie in an interval of 3.366(1)–3.337(1) .__________Translated from Koordinatsionnaya Khimiya, Vol. 31, No. 4, 2005, pp. 266–272.Original Russian Text Copyright © 2005 by Glazunova, Boltalin, Troyanov. 相似文献
9.
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
10.
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
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.
Todd W. Graham 《Journal of organometallic chemistry》2007,692(21):4481-4485
The reaction of CpTi(μ2-Me)(μ2-NPi-Pr3)(μ4-C)(AlMe2)3 with ClSnMe3 and MeO3SCF3 affords the species CpTi(μ2-Cl)(μ2-NPi-Pr3)(μ4-C)(μ2-Cl)(AlMe)(AlMe2)21 and CpTi(μ2-Me)(μ2-NPi-Pr3)(μ4-C)(μ2-O3SCF3)(AlMe)(AlMe2)22, respectively. Both 1 and 2 have been structurally characterized. 相似文献
13.
Reactions of platinum(II) chloro-phosphine complexes with Co3(μ3-CCCCCSiMe3)(μ-dppm)(CO)7 in the presence of NaOMe have given the compounds Pt{CCCC-μ3-C[Co3(μ-dppm)(CO)7]}2(dppe) (1), trans-Pt{CCCC-μ3-C[Co3(μ-dppm)(CO)7]}2(PEt3)2 (2) and trans-Pt{CCCC-μ3-C[Co3(μ-dppm) (CO)6(PPh3)]}2(PPh3)2 (3), each of which contains two Co3 clusters linked by C5 chains to the Pt centre. Electrochemical studies (CVs) show the presence of both oxidation and reduction processes, the latter probably occurring on the CCo3 cores. Ready reductive elimination of {Co3(μ-dppm)(CO)7}2(μ3:μ3-C10) occurs from 1 upon heating. The X-ray study of 3 was carried out using synchrotron radiation (Advanced Photon Source, Argonne, IL) to confirm its structure. 相似文献
14.
15.
16.
Van An Du Gregor N. Stipicic Maria Bendova Ulrich Schubert 《Monatshefte für Chemie / Chemical Monthly》2010,10(2):671-675
Abstract
Thermolysis of cis-Fe(CO)4(SiCl3)2 results in the formation of the novel compound Fe2(CO)6(μ2-SiCl2)3, which was characterized by single crystal X-ray diffraction. Density functional theory calculations were carried out to elucidate possible reaction steps leading to the formation of Fe2(CO)6(SiCl2)3, including CO dissociation and chlorine abstraction by a SiCl3 radical generated from homolytic Fe–Si bond cleavage involving a singlet–triplet intersystem crossing. 相似文献17.
Li-Cheng Song Hua-Wei Cheng Qing-Mei Hu Zhi Wang 《Journal of organometallic chemistry》2004,689(1):139-145
The monoanions (η5-RC5H4)(CO)3Cr− (1, R=H; 2, R=Me; 3, R=CO2Et) reacted with tetrahedral cluster FeCo2(μ3-S)(CO)9 to give single isolobal displacement products (η5-RC5H4)FeCrCo(μ3-S)(CO)8 (4, R=H; 5, R=Me; 6, R=CO2Et) in 86-89% yields, whereas monoanion (η5-RC5H4)(CO)3Cr− (7, R=C(O)Me) reacted with FeCo2(μ3-S)(CO)9 to afford the expected single isolobal displacement product (η5-RC5H4)FeCrCo(μ3-S)(CO)8 (8, R=C(O)Me) in 5% yield and an unexpected square pyramidal cluster FeCo2(μ3-S)2(CO)9 (9) in 45% yield. Similarly, the dianions [η5-C5H4CH2(CH2OCH2)nCH2C5H4-η5][(CO)3Cr−]2 (10, n=1; 11, n=2; 12, n=3) reacted with two molecules of FeCo2(μ3-S)(CO)9 to produce double isolobal displacement products [η5-C5H4CH2(CH2OCH2)nCH2C5H4-η5][FeCrCo(μ3-S)(CO)8]2 (13, n=1; 14, n=2; 15, n=3) in 32-36% yields, while treatment of dianion [η5-C5H4C(O)CH2]2[(CO)3Cr−]2 (16) with two molecules of FeCo2(μ3-S)(CO)9 gave the unexpected square pyramidal cluster FeCo2(μ3-S)2(CO)9 (9) in 42% yield and the corresponding double isolobal displacement product [η5-C5H4C(O)CH2]2[FeCrCo(μ3-S)(CO)8]2 (17) in 8% yield. Products 4-6, 8, 9, 13-15 and 17 were characterized by elemental analyses, IR and 1H NMR spectroscopy, as well as for 4, 6 and 9 by X-ray diffraction techniques. 相似文献
18.
Reactions of [(dtc)2Mo2(S)2(μ-S)2] with one or two equivalents of CuBr in CH2Cl2 afforded two new heterobimetallic sulfide clusters, [(dtc)2Mo2(μ3-S)(μ-S)3(CuBr)] (1) and [(dtc)2Mo2(μ3-S)4(CuBr)2] (2). Both compounds were characterized by elemental analysis, IR, UV-vis and X-ray analysis. Compound 1 contains a butterfly-shaped Mo2S4Cu core in which one CuBr unit is coordinated by one bridging S and two terminal S atoms of the [(dtc)2Mo2(S)2(μ-S)2] moiety. In the structure of 2, one [(dtc)2Mo2(S)2(μ-S)2] moiety and two CuBr units are held together by six Cu-μ3-S bonds, forming a cubane-like Mo2S4Cu2 core. 相似文献
19.
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
20.
Bojan Kozlevčar Lea Glažar Gordana Pirc Zvonko Jagličić Amalija Golobič Primož Šegedin 《Polyhedron》2007
Two novel polynuclear complexes with methanoate anions and 3-hydroxypyridine ligands [Cu(μ-HCO2)2(3-pyOH)]n (1) and [Cu2(μ-HCO2)2(μ-3-pyOH)2(3-pyOH)2(HCO2)2]n (2), respectively, were synthesized and characterized. The central copper atom in 1 is surrounded by four methanoates and a 3-pyOH molecule, forming a square-pyramidal CuO3NO chromophore. All the methanoates are bidentate and serve as bridges between the adjacent copper ions via syn-anti and anti–anti coordination. The basal square coordination axes are formed by O(syn), N(3-pyOH) (1.974(2), 2.016(2) Å) and O(anti), O(anti) (1.945(2), 1.960(2) Å), while the third O(anti) (2.247(2) Å) is on the top of the pyramid. A ferromagnetic transition with an exchange constant 2J/kB = 9.2 cm−1 is found for 1 below 20 K. This interaction probably takes place through two syn-anti methanoates extended in a chain through the 2D structure. On the other hand, two monoatomic Cu–O–Cu intra-dinuclear asymmetric (1.986(2), 2.415(2) Å) bridges of two methanoates in [Cu2(HCO2)4(3-pyOH)4] (2) are present. An elongated distorted octahedral coordination sphere around each copper(II) atom is completed by an additional monodentate terminal methanoate (1.975(2) Å), two N-coordinated 3-pyOH (2.005(2), 2.002(2) Å) and the third weakly O-coordinated 3-pyOH (2.732(2) Å). Although a shorter Cu?Cu distance is noticed in 2 than in 1 (4.690(1) Å 1, 3.442(1) Å 2), much weaker ferromagnetism is found in 2. 相似文献