无机化学学报
無機化學學報
무궤화학학보
JOURNAL OF INORGANIC CHEMISTRY
2005年
1期
25-29
,共5页
付明来%郭国聪%刘冰%吴阿清%黄锦顺
付明來%郭國聰%劉冰%吳阿清%黃錦順
부명래%곽국총%류빙%오아청%황금순
水热合成%硫代锡酸盐%晶体结构
水熱閤成%硫代錫痠鹽%晶體結構
수열합성%류대석산염%정체결구
solvothermal synthesis%thiostannates%crystal structures
利用溶剂热方法在温和的条件下合成了二个新的硫代锡酸盐[Mn(en)3]2Sn2S6·2H2O(eh=H2NC2H4NH2)(1)和[Mn(dien)2]2Sn2S6(dien=H2NC2H4NHC2H4NH2)(2),通过X-射线衍射分析表征其晶体结构.化合物1的晶体学参数:C12H48Mn2N12S6Sn2·2H2O,Mr=936.28,单斜晶系,P21/c,a=1.0129(3),b=1.5746(4),c=1.1524(3)nm,β=102.36(1)°,V=1.795 5(8)nm3,Z=2,Dc=1.732 g·cm-3,μ(MoKα)=2.442 mm-1,F(000)=940,R=0.0633,wR=0.081 4;化合物2的晶体学参数:C16H52Mn2N12S6Sn2,Mr=952.32,单斜晶系,P21/c,a=1.248 12(3),b=0.937 60(4),c=1.776 17(7)nm,β=121.752(2)°,V=1.767 5(1)nm3,Z=2,Dc=1.789 g·cm-3,μ(MoKα)=2.479 mm-1,F(000)=956,R=0.0579,wR=0.1374.在两个化合物中存在的[Sn2S6]4-阴离子均由共边的两个SnS4四面体构成.在1中,锰离子螯合3个乙二胺做为阳离子模板,而在2中锰离子螯合2个二乙烯三胺做为阳离子模板.金属配合物作为模板对阴离子[Sn2S6]4-在晶体结构中的排列产生重要的影响.
利用溶劑熱方法在溫和的條件下閤成瞭二箇新的硫代錫痠鹽[Mn(en)3]2Sn2S6·2H2O(eh=H2NC2H4NH2)(1)和[Mn(dien)2]2Sn2S6(dien=H2NC2H4NHC2H4NH2)(2),通過X-射線衍射分析錶徵其晶體結構.化閤物1的晶體學參數:C12H48Mn2N12S6Sn2·2H2O,Mr=936.28,單斜晶繫,P21/c,a=1.0129(3),b=1.5746(4),c=1.1524(3)nm,β=102.36(1)°,V=1.795 5(8)nm3,Z=2,Dc=1.732 g·cm-3,μ(MoKα)=2.442 mm-1,F(000)=940,R=0.0633,wR=0.081 4;化閤物2的晶體學參數:C16H52Mn2N12S6Sn2,Mr=952.32,單斜晶繫,P21/c,a=1.248 12(3),b=0.937 60(4),c=1.776 17(7)nm,β=121.752(2)°,V=1.767 5(1)nm3,Z=2,Dc=1.789 g·cm-3,μ(MoKα)=2.479 mm-1,F(000)=956,R=0.0579,wR=0.1374.在兩箇化閤物中存在的[Sn2S6]4-陰離子均由共邊的兩箇SnS4四麵體構成.在1中,錳離子螯閤3箇乙二胺做為暘離子模闆,而在2中錳離子螯閤2箇二乙烯三胺做為暘離子模闆.金屬配閤物作為模闆對陰離子[Sn2S6]4-在晶體結構中的排列產生重要的影響.
이용용제열방법재온화적조건하합성료이개신적류대석산염[Mn(en)3]2Sn2S6·2H2O(eh=H2NC2H4NH2)(1)화[Mn(dien)2]2Sn2S6(dien=H2NC2H4NHC2H4NH2)(2),통과X-사선연사분석표정기정체결구.화합물1적정체학삼수:C12H48Mn2N12S6Sn2·2H2O,Mr=936.28,단사정계,P21/c,a=1.0129(3),b=1.5746(4),c=1.1524(3)nm,β=102.36(1)°,V=1.795 5(8)nm3,Z=2,Dc=1.732 g·cm-3,μ(MoKα)=2.442 mm-1,F(000)=940,R=0.0633,wR=0.081 4;화합물2적정체학삼수:C16H52Mn2N12S6Sn2,Mr=952.32,단사정계,P21/c,a=1.248 12(3),b=0.937 60(4),c=1.776 17(7)nm,β=121.752(2)°,V=1.767 5(1)nm3,Z=2,Dc=1.789 g·cm-3,μ(MoKα)=2.479 mm-1,F(000)=956,R=0.0579,wR=0.1374.재량개화합물중존재적[Sn2S6]4-음리자균유공변적량개SnS4사면체구성.재1중,맹리자오합3개을이알주위양리자모판,이재2중맹리자오합2개이을희삼알주위양리자모판.금속배합물작위모판대음리자[Sn2S6]4-재정체결구중적배렬산생중요적영향.
Two new thiostannates [Mn(en)3]2Sn2S6·2H2O (en=ethylenediamine) (1) and [Mn(dien)2]2Sn2S6 (dien=diethylenetriamine) (2) have been prepared under mild solvothermal conditions and structurally characterized by XF(000)=940, R=0.063 3, wR=0.0814; and for 2: [Mn(dien)2]2Sn2S6, Mr=952.32, monoclinic P21/c, a=1.248 12(3), b=F(000)=956, R=0.057 9, wR=O. 137 4. In each complex [Sn2S6]4- anions is composed of two SnS4 tetrahedra sharing a common edge. In the complex 1 the transition metal Mn cations are coordinated each by three en ligands, while in complex 2 the Mn cations are coordinated each by two dien ligands. The metal complex templates make a significant influence on the arrangement of [Sn2S6]4- anions in their crystal structures. CCDC: 246260, 246261.
