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Single cubane-like clusters, MFe_3S_4(R_2dtc)_5 (M=Mo, R_2=—(CH_2)_4—, Bz_2; M=W, R_2=Me_2, —(CH_2)4—; dtc=dialkyldithiocarbamate) were synthesized by assembly reaction of (NH_4)_2MS_4 (M=Mo, W), FeCl_2 with R_2dtcNa (or NH_4) in DMF. The structure, IR, EPR and cyclic voltammogram are described and discussed. MoFe_3S_4(C_4H_8dtc)_5 was also obtained from the conversion of linear cluster Fe(DMF)_6[(FeCl_2)_2MoS_4] in the presence of C_4H_8dtc NH_4. Both clusters MoFe_3S_4(C_4H_8dtc)_4·2C_2H_5CN and WFe_3S_4(C_4H_8dtc)_5·2DMF crystallize in the monoclinic space group C2/c with a=12.544(2), (Mo-cluster), 12.533(4) (W-cluster); b=20.478(4), 20.121(6); c=19.582(7), 19.659(2);β=102.82(2), 102.96(3)°; and Z=4, 4. Their structures were refined to R=0.057 and 0.064 with use of 2690 and 2179 reflections (ι>3Q(I)), respectively. Many similarities in structure for Mo and W clusters indicate that both Mo and W play a very similar role in the clusters. 相似文献
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本文根据分子碎片结合原理, 用直接法由简单的单质元素, 金属盐类及配体, 通过控制反应温度、压力, 时间及配体用量在CO气氛下一步合成含羰基和不含羰基的簇合物: Pd3(SC6H4OH)3(PPh3)3(OH)2Cl(1),Fe2S2(CO)5Pd(PPh3)3(2), Fe2S2(CO)5Pt(PPh3)3(3)。对它们进行了IR, NMR,EDS, 元素分析, 金属分析和化合物1的X光单晶衍射结构分析。化合物1属单斜晶系, 离子型, P21/n空间群, 晶胞参数a=1.4629(3)nm, b=1.9263(3)nm,c=2.4908(7)nm, β=94.53(2)°, Z=4, R=0.053。 相似文献
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Three types of unit combinations, FeS2Fe + FeS2Fe, FeS2Fe + MoS2Fe and MoS2Mo + MoS2Mo, lead to Fe4S4, MoFe3S4 and Mo2Fe2S4 cubane-like clusters, respectively. A new doubly bridged single cubane cluster [Mo2Fe2S4(C4H8dtc)6]·3.5C2H2Cl4 has been obtained and its structure is discussed. 相似文献
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经由零价双核钼含SR桥的配合物的氧化反应合成了一系列含各种SR桥的双核钼(Ⅰ)配合物Mo_2-(CO)_(8-n)(μ-SR)_2L_n[R=Bu~t,Ph,Bz(C_6H_5CH_2),CH_2CO_2Et;L=MeCN,PPh_3;n=0,2]。并应用红外光谱、元素分析等进行表征,讨论了新的合成途径。[含MeCN配位体配位到Mo(Ⅰ)上的配合物,Mo_2(CO)_6(SPh)_2(MeCN)_2经X射线结构测定,系属单斜晶系,空间群P2_1/c,a=9.241(2),b=9.330(3),c=15.458(4)A:β=105.77(2)°;V=1283(1)A~3;Z=2;R=0.033。Mo—Mo距离为2.978A,表明其Mo-Mo键的形成,Mo-S键长为2.469A。比较同系物Mo_2(CO)_8(μ-SCH_2CO_2-Et)_2,Mo_2(CO)_6(μ-SCH_2CO_2Et)_2(MeCN)_2和Mo_2(CO)_8(μ-SBu~t)_2的结构,并讨论其结构与化学。 相似文献
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