夹心型钼磷酸盐的水热合成与晶体结构  

Hydrothermal Synthesis and Crystal Structure of SandwichLike Heteropolymolybdophosphates

作　　者：刘宗瑞[1,2] 王恩波[1,2] 王力 胡长文[1,2] 许林[1,2] 邢彦 贾恒庆[3] 林永华 

机构地区：[1]东北师范大学化学系 [2]内蒙古民族师范学院 [3]中国科学院长春应化所

出　　处：《Chinese Journal of Structural Chemistry》1999年第3期182-187,共6页结构化学（英文）

基　　金：吉林大学教育部无机合成与制备开放实验室资助

摘　　要：采用水热法合成了首例含过渡金属铬的夹心型钼磷酸盐〔Ｈ３Ｎ（ＣＨ２）６ＮＨ３〕２Ｈ３｛Ｃｒ〔Ｍｏ６Ｏ１５（ＨＰＯ４）（Ｈ２ＰＯ４）３〕２｝·４Ｈ２Ｏ超分子化合物，用单晶Ｘ－射线测定其晶体结构，该晶体属三斜晶系，空间群Ｐ１。晶胞参数ａ＝１２．１５６（２），ｂ＝１２．８０９（３），ｃ＝１３．５３０（３），α＝１０２．４６（３）°，β＝９３．６７（３）°，γ＝９３．４６（３）°．Ｖ＝２０４６．９（７）３，Ｚ＝１，Ｍｒ＝２７６８．６９，Ｄｃ＝２．２４６ｇ／ｃｍ３，Ｆ（０００）＝１３３７，μ＝２．１６２ｍｍ－１，全矩阵最小二乘法修正至Ｒ＝０．０６６６，ｗＲ＝０．１７４５，独立可观测点数为７１４２。化合物是分别由质子化的１，６－己二胺、水和｛Ｃｒ〔Ｍｏ６Ｏ１５（ＨＰＯ４）（Ｈ２ＰＯ４）３〕２｝７－阴离子构成。Sandwichlike heteropoly molybdochromophosphates of supermolecular compound NH3(CH2)6NH32H3{CrMo6O15(HPO4)(H2PO4)32}4H2O has been hydrothermally synthesized and the single crystal structure has been determined by Xray diffraction. The crystal data are has follows: triclinic, space group P1 , a=12.156(2), b=12.809(3), c=13.530(3) , =10246(3), =93.67(3), =93.46(3), V=2046.9(7) 3, Z=1, Mr=2768.69, Dc=2246 g/cm-3, F(000)=1337, =2.162 mm-1. The structure has been refined to R=0.0666 and wR=0.1745 by fullmatrix leastsquares method. The title compound is composed of 1, 6diaminohexane, water molecules, and {CrMo6O15(HPO4)(H2PO4)32}7- anion which consists of six oxygen atoms from two Mo6P4 units with a sandwichlike transition metal atom Cr located at the center of symmetry.

关 键 词：水热合成 晶体 超分子化合物 夹心型 钼磷酸盐 

分 类 号：O641.4[理学—物理化学]