双核钼铁硫簇合物[Fe(2,2’-联吡啶_3)][(S_2MoS_2FeCl_2]的合成与晶体结构  

SYNTHESIS AND CRYSTAL STRUCTURE OF MOLYBDENUM -IRON -SULFUR CLUSTER COMPLEX, [Fc(2,2'-Bpy)_3][S_2MoS_2FcCI_2]

作　　者：蔡进华[1] 康北笙[1] 庄伯涛[1] 

机构地区：[1]中国科学院福建物质结构研究所,结构化学开放实验室福州350002

出　　处：《无机化学学报》1991年第3期301-305,共5页Chinese Journal of Inorganic Chemistry

基　　金：国家自然科学基金;科学院自然科学基金资助

摘　　要：双核Mo-Fe-S原子簇配合物[Fe(2,2′-bpy)_3][S_2MoS_2FeCl_2],是(Et_4N)_2MoS_4、FeCl_2和2,2′-联吡啶在乙腈中反应得到的结晶化合物.晶体属单斜晶系,空间群P2_1/c;a=9.328(3),b=26.788(2),c=13.764(3)(?);β=95.38(3)°;V=3424.2(11)(?)~3;Z=4;D_c=1.698g/cm^3;F(000)=1752.晶体结构用直按法解出;经全矩阵最小二乘法修正,最后R=0.068,R_ω=0.071(3933个I>3(?)(I)的独立衍射).在晶体结构中配位阴离子[S_2MoS_2FeCl_2]^(2-)是排布在阳离子[Fe(2,2′-bpy)_3]^(2+)所形成的空腔中.它是以非统计分布的形式存在,从而较准确地测定了各项键参数.Mo…Fe距离为2.773(2)(?),Mo-S_b和Fe-S_b有大致相等的键长.Molybdcnum-iron-sulfur cluster complex, [Fc(2,2'-bpy)3][S2MoS2FcC12] was prepared from the reaction of (Et4N)2MoS4,FeC12 and 2,2'-bpy in acctonitrilc. The crystal belongs to monoclinic space group P21 / c with a = 9.328(3), b = 26.788(2), c= 13.764(3)A, β = 95.38(3)° ; V=3424.2(11)A3;Z = 4; Dc= 1.698gcm-3. The crystal structure was solved by direct methods and refined by full-matrix least-squares techniques for 3933 reflections with I>3δ(I0). The final R and Rω are 0.068 and 0.071, respectively. In the crystal, the [S2MoS2FeCl2]2-anion are situated at the vacancies formed by the cations. There is no disordered arrangement of metal atoms in the title anion. At a result, its structural parameters have been determined accurately. The core of the anion MoS2Fe is planar with Mo…Fe distance of 2.773(2)A, and the distances of bonds Mo-Sband Fe-Sbarc nearly equivalent within the range of 2.248-2.251 A

关 键 词：双核 钼铁硫 混簇 联吡啶 络合物 

分 类 号：O614.612[理学—无机化学]