[(C_2H_5)_4N]_2{Fe_4S_4[S_2CN(C_2H_5)_2]_4}的晶体和分子结构

Crystal and Molecular Structure of [(C_2H_5)_4N]_2 {Fe_4S_4[S_2CN(C_2H_5)_2]_4}

[(C_2H_5)_4N]_2{Fe_4S_4[S_2CN(C_2H_5)_2]_4}单晶样品在Nicolet-R3四圆衍射仪上收集X射线衍射数据。分析结果给出其晶胞参数:a=22.125(6),b=11.313(3),c=25.053(8)A;β=118.05(2)°;V=5534.19A^3,Z=4,空间群Cc。衍射数据经过Lp因子和经验吸收效应校正。分子中铁原子的位置从三维Patterson图上得到。接着经过若干轮Fourier和差Fourier电子云密度合成,发现全部其余非氢原子的坐标。氢原子位置根据理论模型计算。结构修正最后收敛至R=0.073,R_w=0.069.标题化合物是由[(C_2H_5)_4N]^+和{Fe_4[S_2CN(C_2H_5)_2]}^(2-)组成的离子型化合物。结构的主要特点表现在阴离子上,而在阴离子中含有类立方烷型簇核Fe_4S_4。该簇核中每个铁原子与五个硫原子配位,其配位多面体构型均为畸变的四方锥。

Crystal of the title compound was shown to have the cell parameters a=22.125(6), b=11.313 (3), c=25.053 (8) A, β=118.05 (2)°, V=5534.19A^3, Z=4 and space group Cc. Reflection data were undertaken Lp factor and empirical absorption corrections. The position of Fe atoms were obtained from three-dimensional Patterson function analysis. The remaining non-hydrogen atoms were located by subsequent Fourier and difference Fourier syntheses following least-squares refinements of the input atomic coordinates. The coordinates of hydrogen atoms were calculated by Sheoretical models. Structure refinement converged finally to R=0.073, R_w=0.069. The molecule of the title compound consists of [(C_2H_5)_4N]^+ and {Fe_4S_4[S_2CN(C_2H_5)_2]_4}^(2-). Of special interest is the anion which contains Fe_4S_4 cluster with cubane-like configuration. Each Fe atom in the cluster is coordinated wish five S atoms which situate on vertices of a distored square-pyramid.