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.
基金
吉林大学教育部无机合成与制备开放实验室资助
关键词
水热合成
晶体
超分子化合物
夹心型
钼磷酸盐
hydrothermal synthesis, crystal structure, molybdenum, supermolecular compound
