含一价铜配合物的新型双金属钼氧簇合物[5-(4-Br-Ph)-2,4′-Hbpy]_2·[Cu~Ⅰ(5-(4-Br-Ph)-2,4′-bpy)_2]_2[Mo_8O_(26)]的水热合成及晶体结构

Hydrothermal Synthesis and Crystal Structure of a New Bimetallic Oxide Cluster Constructed from β-Octamolybdate and Copper(Ⅰ)-organonitrogen Complexes

采用水热法合成出一种含一价铜配合物的新型双金属钼氧簇合物[5-(4-Br-Ph)-2,4′-Hbpy]2[Cu(5-(4-Br-Ph)-2,4′-bpy)2]2[Mo8O26],并通过X射线单晶结构分析、红外光谱分析、元素分析以及X射线粉末衍射分析对该化合物的结构进行了表征.结果表明,该化合物属单斜晶系,P21/c空间群,晶胞参数a=1.4411(3)nm,b=1.3924(3)nm,c=2.5183(5)nm,β=99.06(3)°,V=4.990(17)nm3,Z=2;该化合物是由一价铜配合物{Cu(5-(4-Br-Ph)-2,4′-bpy)2}+与{β-Mo8O26}4-簇通过共价配位键连接形成的新型多金属钼酸盐,其中游离的质子化配体作为抗衡阳离子.

A new bimetallic oxide cluster [5-(4-Br-Ph)-2,4′-Hbpy]_2[Cu~Ⅰ(5-(4-Br-Ph)-2,(4′-bpy)_2]_2·)[Mo_8O_(26)] (1) was hydrothermally synthesized and structurally solved by single-crystal X-ray diffraction analysis. Crystal data for compound 1: monoclinic, P2_1/c, a=1.441 1(3) nm, b=(1.392 4(4)) nm, c=2.518 3(5) nm, β=99.06(3)°, V=4.990 3(17) nm^3, and Z=2. The structure of compound 1 consists of a cluster anion {[Cu~Ⅰ(5-(4-Br-Ph)-2,4′-bpy)_2]_2[Mo_8O_(26)]}^(2-), which is constructed from β-octamolybdate subunit (Mo_8O_(26))^(4-) covalently bonded to two coordinated complexes {Cu~Ⅰ(5-(4-Br-Ph)-2,4′-bpy)_2}^+. Discrete protonated ligand {5-(4-Br-Ph)-2,4′-Hbpy}^+ acts as the charge-compensating cation.