【摘要】 草酸与钼（Ⅵ）反应可以生成多种络合物。根据文献［１］方法，我们制得无色透明块状的ｃｉｓ－（ＱＨ）２［ＭｏＯ２（Ｃ２Ｏ４）２］晶体（式中ＱＨ＋＝Ｃ９ＮＨ８＋）。该晶体属斜方晶系，空间群为Ｐｃｃ２；晶胞参数：ａ＝１２．４９７（４），ｂ＝１０．２６２（３），Ｃ＝１６．７５０（３）Ａ；Ｖ＝２１４８．０８Ａ；Ｍ＝５６４．３２；晶体密度：ｄｏｂｓ＝１．７３ｇｃｍ－３；晶胞分子数Ｚ＝４（ｄｃａｌｃ＝１．７４５ｇｃｍ－３）。晶体在ＣＡＤ－４ 四园衍射仪上用Ｍ０Ｋａ射线收集三维衍射点强度数据，通过三维Ｐａｔｔｅｒｓｏｎ函数和Ｆｏｕｒｉｅｒ函数合成方法，确定了ｃｉｓ－（ＱＨ）２［ＭｏＯ２）Ｃ２Ｏ４）２］的晶体和分子结构。最后，根据Ｉ＞２σ（Ｉ）的１３６３个独立衍射点的强度数据、用最小二乘法把结构精修到Ｒ＝０．０６０，Ｒｗ＝０．０５９。该晶体的阴离子由六个氧原子围绕着Ｍ０原子形成扭曲的八面体。分子具有Ｃ２对称性（ＱＨ）＋和［Ｍ０Ｏ２）Ｃ２Ｏ４）２］２－之间组成了Ｎ－Ｈ…Ｏ类的氢键。更多还原

【Abstract】 Various complexes can be formed by the reaction of oxalic acid with Mo (Ⅵ). We have prepared the cis-(C9H8N)2 [M0O2(C2O4)2] crystal by spittle and Wardlaw’s method[1]. X-ray data were collected on an Enraf Nonious CAD-4 four-circle x-ray diffractometer with M0 Ka radiation. The title comp- ound crystallized in the orthorhobic system, with space group Pcc2 .The unit cell parameters are as follows: a=12. 497(4), b= 10. 262(3), c=16. 750(3)A; V= 2148. 08A3; M=564. 32 dobs = 1. 73gcm-3. whereby Z=4, dcalc =1. 745gcm-3. The structure was solved by three dimensional patterson and Fourier synthesis me- thods and refined by least-squates procedures to a final R =0. 060 Rw = 0. 059 for 1363 independent reflexions with 1>2σ(I). Six O atoms form a distorted octahedral coordination around Molybdenum atom. The Molecular symmetry is C2. The hydrogen bonds (N-H…O) are formed between quionlinium cation and the anion[MoO2 (C2O4)2]2 .更多还原