[C_6N_2H_(18)]_2[Mo_5O_(15)(HPO_4)_2]·H_2O的水热合成与结构表征

Hydrothermal Synthesis and Characteristic of [C_6N_2H_(18)]_2[Mo_5O_(15)(HPO_4)_2]·H_2O

通过水热法合成了一个新化合物 [C6 N2 H18]2 [Mo5O15(HPO4 ) 2 ]· H2 O,并通过 IR光谱、ICP、元素分析、差热与热重分析和 X射线单晶衍射分析等手段进行了表征 .结果表明 ,晶体属三方晶系 ,P3 (2 ) 2 1空间群 ,a=1 .1 2 3 1 (1 ) nm,c=2 .2 80 2 (5 ) nm,V=2 .4 91 1 (7) nm3,Dx=2 .83 5 Mg/m3,Z=6,最后的一致性因子 R=0 .0 2 2 7,w R=0 .0 675 .阴离子中 Mo5O15构成一环状结构 ,2个 HPO4 一个连在环的下方 ,一个连在环的上方 ,形成类似于“飞碟”状的结构 ,阳离子为

C_6N_2H_ 18]_2[Mo_5O_ 15(HPO_4)_2]·H_2O has been obtained by using hydrothermal synthesis, and the results of X-ray single crystal diffraction show that the compound crystalliized in space group {P3(2)21} of trigonal system with a=1.123 1(1) nm, c=2.280 2(5) nm, V=2.491 1(7) nm 3, D_x=2^835 {Mg/m 3}, Z=6 and R=0.022 7, wR=0.067 5. The crystal structure of [C_6N_2H_ 18]_2[Mo_5O_ 15(HPO_4)_2]·H_2O is composed of two protoned tertramethyldiamine, [C_6N_2H_ 18] 4+_2, [Mo_5O_ 15(HPO_4)_2] 4- and one molecule water. In the anion H_2Mo_5P_2O 4-_ 23, five octahedral MoO_6 are connected by sharing-angle to form a pentagon and three oxygen atoms of two PO_4 tetrahedral is connected to five Mo atoms. Five octahedral MoO_6 and two PO_4 tetrahedral are connected to form this anion like flying saucer.