Synthesis and Structural Characterization of a Salt {[Co(Phen)_3][Mo_2S_2(μ-S)_2(edt)_2]}_2·(DMSO)_2·(Et_2O)(Phen = 1,10-Phenanthroline, edt=Ethane-1,2-dithiolate)  

作　　者：ZHANGWen-Hua RENZhi-Gang ZHANGYong 

机构地区：[1]SchoolofChemistryandChemicalEngineering,SuzhouUniversit） [2]Suzhou215006,China

出　　处：《Chinese Journal of Structural Chemistry》2005年第7期773-778,736,共7页结构化学（英文）

基　　金：This work was supported by the NNSFC (No. 20271036), the NSF of Jiangsu Province (No. BK2004205) and the State Key Laboratory of Structural Chemistry (030066)

摘　　要：Reaction of [Et4N]2[Mo2S2(μ-S)2(edt)2] with CoCl2?6H2O and Phen in MeCN followed by recrystallization in DMSO/Et2O gave rise to dark-red block crystals of {[Co(Phen)3]- [Mo2S2(μ-S)2(edt)2]}2?(DMSO)2?(Et2O) 1 (C88H86Co2Mo4N12O3S18). 1 crystallizes in the monoclinic system, space group P21/c with a = 24.631(4), b = 16.117(3), c = 24.791(4) ?, β = 92.835o, V = 9829.3(3) ?3, Z = 4, Mr = 2438.57, Dc = 1.648 g/cm3, F(000) = 4928, μ = 12.61 cm-1, R = 0.0936 and wR = 0.1682 for 12998 observed reflections with I > 2.0σ(I). In the structure of 1, the Co atom of the [Co(Phen)3]2+ dication is octahedrally coordinated by three Phen ligands. The Mo atom of the [Mo2S2(μ-S)2(edt)2]2- dianion is coordinated by two μ-S, one terminal S and two S atoms from edt, forming a distorted square pyramidal geometry. The mean Co–N and Mo…Mo bond distances are 2.139 and 2.872 ?, respectively.Reaction of [Et4N]2[Mo2S2(μ-S)2(edt)2] with CoCl2?6H2O and Phen in MeCN followed by recrystallization in DMSO/Et2O gave rise to dark-red block crystals of {[Co(Phen)3]- [Mo2S2(μ-S)2(edt)2]}2?(DMSO)2?(Et2O) 1 (C88H86Co2Mo4N12O3S18). 1 crystallizes in the monoclinic system, space group P21/c with a = 24.631(4), b = 16.117(3), c = 24.791(4) ?, β = 92.835o, V = 9829.3(3) ?3, Z = 4, Mr = 2438.57, Dc = 1.648 g/cm3, F(000) = 4928, μ = 12.61 cm-1, R = 0.0936 and wR = 0.1682 for 12998 observed reflections with I > 2.0σ(I). In the structure of 1, the Co atom of the [Co(Phen)3]2+ dication is octahedrally coordinated by three Phen ligands. The Mo atom of the [Mo2S2(μ-S)2(edt)2]2- dianion is coordinated by two μ-S, one terminal S and two S atoms from edt, forming a distorted square pyramidal geometry. The mean Co–N and Mo…Mo bond distances are 2.139 and 2.872 ?, respectively.

关 键 词：molybdenum cluster sulfur cobalt crystal structure SYNTHESIS 

分 类 号：TP301.6[自动化与计算机技术—计算机系统结构] G633.41[自动化与计算机技术—计算机科学与技术]