Synthesis, Spectroscopic Properties and Crystal Structure of Optically Active dimalato dioxomolybdenum(VI) Complexes

YAN Wenbin, HOU Shuya#, ZHAO Hong#, ZHOU Zhaohui#*, WAN Huilin#
(Department of Chemistry, Jishou University, Jishou 416000, # Department of Chemistry, Xiamen University, Xiamen 361005)

Abstract  The complexes Na2[MoO2(S-Hmal)2]·4H2O (1) and K2[MoO2(S- Hmal)2]·2H2O 2 were prepared from the reaction of S-malic acid and molybdate. The two complexes were characterized by elemental analysis, conductivity measurement, optical rotation and IR measurement. 1 was characterized by NMR and X-ray diffraction method. It crystallizes in orthorhombic space group P 212121 with unit cell parameters: a=2.1000 (1), b=1.07569 (8), c=0.79356 (6) nm, V=1.7926 (4)nm3, Z=4，Dc=1.890g.cm-3, F(000)=1024, m＝8.355cm-1, R=0.0309 and Rw=0.0366 for 1900 reflections with I≥3s (I). The molybdenum atom is coordinated by two bidentate S-malato ligands through a-alkoxy and a-carboxy group. The polymeric coordinated anion is connected by strong hydrogen bonding. The absolute configuration of the coordinated anion is D-S,S.
Key words  Malic acid, Malate, Oxomolybdenum(VI) complex, Crystal Structure

　

光学活性苹果酸氧钼(VI)配合物的合成、表征和晶体结构*

颜文斌 侯书雅# 赵 宏# 周朝晖#** 万惠霖#
(吉首大学化学系 吉首 416000  #厦门大学化学系 厦门 361005)

摘要 合成了苹果酸氧钼(VI)配合物D -Na2[MoO2(S-Hmal)2]·4H2O (1) 和K2[MoO2(S-Hmal)2]·2H2O (2)，通过元素分析、电导率、旋光度和红外光谱对配合物进行了表征，对配合物1进行了核磁共振和X衍射晶体结构分析。结果表明，配合物1晶体属正交晶系，空间群为P 212121，a=2.1000 (1)，b=1.07569 (8)，c=0.79356 (6) nm，V=1.7926 (4)nm3，Z=4，Dc=1.890g·cm-3，F(000)=1024，m＝8.355cm-1 ，R=0.0309，Rw=0.0366。中心钼为扭曲的六配位八面体结构，阴离子通过分子间强氢键形成聚合结构，配阴离子的绝对构型为D-S,S。
关键词 苹果酸 苹果酸盐 钼(VI)配合物 晶体结构

颜文斌 男，36岁，硕士，副教授，从事无机化合物、金属有机化合物的合成、结构和性质研究。**联系人 E-mail:zhzhou@xmu.edu.cn
国家自然科学基金项目(29933040)和高等学校骨干教师资助计划项目
2000-12-21收稿，2001-04-22修回

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