新型杂多酸(H_3NCH_2CH_2NHCH_2CH_2NH_3)_2[(HPO_4)_2Mo_5O_(15)]的水热合成与晶体结构

Hydrothermal synthesis and crystal structure of a novel complex(H_3NCH_2CH_2NHCH_2CH_2NH_3)_2[(HPO_4)_2Mo_5O_(15)]

合成了一种未见报道的标题化合物((H3NCH2CH2NHCH2CH2NH3)2[(HPO4)2Mo5O15],Mr=1121.99)并得到单晶,晶体衍射实验发现其属于三斜晶系,P-1空间群,晶体学参数:a=0.980 6(2)nm,b=0.995 2(2)nm,c=1.468 0(3)nm,α=95.46(3)°,β=98.88(3)°,γ=95.70(3)°,V=1.399 6(5)nm3,Z=1,Dc=2.648 mg/m3,(MoKα)=1.199 mm-1,F000=528,最终R=0.042 1,wR=0.099 7,GooF=1.034.配体由一个[(HPO4)2Mo5O15]4-簇阴离子和两个质子化的二乙烯三胺组成,化合物中端基氧与有机胺之间存在大量的氢键作用,使其连成一种新的有机-无机杂化的超分子化合物.

The title compound（（H3NCH2CH2NHCH2CH2NH3）2[（HPO4）2Mo5O15],Mr=1121.99） is synthesized by hydrothermal reaction.It crystallizes in a triclinic system with space group P-1 and unit cell parameters ：a= 0.980 6（2）nm,b= 0.995 2（2）nm,c=1.468 0（3）nm,α= 95.46（3）°,β= 98.88（3）°,γ= 95.70（3）°,V=1.399 6（5）nm3,Z=1,Dc = 2.648 mg/m3,（MoKα） = 1.199 mm-1,F000=528,the final R = 0.042 1,wR=0.099 7,GooF=1.034.The structure of title compound consists of a [（HPO4）2Mo5O15]4-cluster and 2 protonated diethylenetriamine molecular ions,those intermolecular hydrogen bonds between the O atoms and diethylenetriamine develop a supermolecular structure.