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四核银原子簇化合物Ag_4(α-C_(10)H_7CS_2)_4(Py)_4·2Py由α-萘荒酸与硝酸银在有机溶剂中反应,经吡啶重结晶获得单晶。由于反应中采用不同的银盐与α-萘荒酸的投料比(1:2与1:4),得到了两种颜色的晶体(甲和乙)。用X射线单晶衍射法测定了它们的晶体结构。晶体甲的空间群为C_(2h)~5—P2_1/a。晶胞参数:a=2.2822(4)(?),b=12.803(4)(?),c=24.444(7)(?),β=103.90(2)°,V=6933.14(?)~3,Z=4。晶体乙的空间群为c_(2h)~6—c2/c。晶胞参数:a=29.150(2)(?),b=12.789(3)(?),c=24.413(2)(?),β=130.56(4)°,V=6914.38(?)~3,Z=4。Ag_4(α-C_(10)H_7CS_2)_4(Py)_4在两种晶体中的空间构型基本相同,差别只在于分子的对称性上。晶体乙中,分子处在二重轴上,分子的对称性较高。本文只报道晶体乙的结构测定和结构参数.3338个反射参与修正,最终的偏差因子R=0.093。分子中Ag_4呈压扁的四面体构型。六个Ag—Ag距离可分成两类,硫桥相连的Ag—Ag平均键长为2.924(?)(2.875—2.972(?)),表明有相当程度的金属键相互作用。不与硫桥相连的Ag—Ag距离为3.563(?)。
The tetranuclear silver cluster compound Ag_4 (α-C_ (10) H_7CS_2) _4 (Py) _4 · 2Py is synthesized from α-naphthalene-lanthanide and silver nitrate in organic solvent and recrystallized from pyridine to obtain single crystal. Two different colors of crystals (A and B) were obtained due to the different dosing ratios (1: 2 and 1: 4) of the silver salt to α-naphthalene-deficient acid in the reaction. Their crystal structures were determined by X-ray single crystal diffraction. Crystal A space group C_ (2h) ~ 5-P2_1 / a. Cell parameters: a = 2.2822 (4) (?), B = 12.803 (4) (?), C = 24.444 (7) ?,? = 103.90 (2) °, V = 6933.14? , Z = 4. Crystal B space group c_ (2h) ~ 6-c2 / c. Cell parameters: a = 29.150 (2) (?), B = 12.789 (3) (?), C = 24.413 (2) ?, β = 130.56 (4) °, V = 6914.38 , Z = 4. The spatial configurations of Ag_4 (α-C_ (10) H_7CS_2) _4 (Py) _4 are basically the same, the only difference is the symmetry of the molecule. Crystal B, the molecules in the double axis, the molecular symmetry higher. In this paper, only the crystal structure and structure parameters of B were reported, 3338 reflections were involved in the correction, and the final deviation factor was R = 0.093. Molecular Ag_4 was squashed tetrahedral configuration. The six Ag-Ag distances can be divided into two groups, and the average bond length of Ag-Ag connected by the sulfur bridge is 2.924 (?) (2.875-2.972 (?)), Indicating a considerable degree of metal-metal interaction. The Ag-Ag distance to the sulfur bridge is 3.563 (?).