12-钨磷酸钙与丁二酰亚胺加合物的制备和性质研究

SYNTHESIS AND PROPERTIES OF ADDUCT BETWEEN CALCIUM DODECATUNGSTOPHOSPHATE WITH SUCCINIMIDE

本文研究了12-钨磷酸钙与丁二酰亚胺和邻苯二甲酰亚胺的加合反应,制备了12-钨磷酸钙的丁二酰亚胺加合物Ca_(3/2)PW_(12)O_(40)·4(CH_2CO)_2NH·7H_2O,测定了加合物的红外光谱、拉曼光谱和热重差热分析曲线,用X射线粉末衍射方法研究了加合物的结晶学特征.结果表明.配体丁二酰亚胺以一个羰基氧与金属阳离子配位,加合物的形成对杂阴离子的Kcggin结构没有明显影响.但WO_6八面体发生一定的畸变.其中W-O_d键减弱,W-O_c键增强.加合物属单斜晶系,晶胞参数为:a=25.839(6).b=13.223(2),c=18.438(2)(?),β=97.06(2)°,V=6251.88(?)~3,可能的空间群为C_2h^5-P2_1/c或C_2h^2-P2_1/m或C_2~2-P2_1,品质因子F_(30)=54(0.012,45).

This paper reports the synthesis of adduct between calcium dodccatungstophosphate with succinimidc. The properties were characterized by IR, Raman spectra, TG-DTA thermal analysis, and X-ray powder diffraction analysis. The compound is monoclinic with crystal data: a=25.839(6), b=13.223(2), c=18.438(3)A, 0 = 97.06(2)° , V=6251.88A3. The possible group is C52h-P21 / c or C22h-P21/ m or C22-P21. The figure of merit F30 = 54 (0.012, 45). Because of its large stcro effect, the ligand succinimidc coordinates to the cation with only one oxygen of the two C = O bonds, causing the vc=o vibration peak splits into three pcaks, and the coordination number of cation decreases from six in DMF adducts to three.