A 2D Layered Thiostannate: Synthesis and Crystal Structure of [tmdpH_2]Sn_3S_7  

作　　者：王欣 盛天录 项生昌 胡胜民 傅瑞标 吴新涛 

机构地区：[1]State Key Laboratory of Structural Chemistry,Fujian Institute of Research on the Structure of Matter,Chinese Academy of Sciences [2]Graduate School of the Chinese Academy of Sciences

出　　处：《Chinese Journal of Structural Chemistry》2010年第2期260-264,共5页结构化学（英文）

基　　金：supported by the 973 Program (2007CB815301 and 2006CB932904);the National Natural Science Foundation of China (20333070, 20673118, 20871114);the Science Foundation of CAS (KJCX2-YW-M05);Fujian Province (2006L2005, 2006J0014, 2006F3132)

摘　　要：A new thiostannate,[tmdpH2]Sn3S7 1（tmdp = 4,4＇-trimethylenedipiperidine）,has been synthesized under solvothermal conditions and characterized by elemental analysis,IR spectroscopy,and single-crystal X-ray diffraction analysis.In 1,the Sn3S4 secondary incomplete cubane-like building units are bridged by μ2-S atoms to form Sn12S12 rings which are then joined parallelly to the [001] plane,giving the final 2D（Sn3S7^2-）n layer of（6,3） network.The layers are stacked along the c axis so that 24-membered ring channels are generated,in which the organic cations are accommodated.The compound crystallizes in monoclinic,space group C2/c,with a=23.052（3）,b=13.4039（12）,c=18.412（2）A,β=120.112（4）°,V=4921.3（9）A^3,C13H28N2S7Sn3,Mr=792.86,Z=8,Dc=2.140 g/cm^3,F（000）=3056,μ=3.619 mm^-1,the final R=0.0488 and wR=0.1125 for 4607 observed reflections with I〉2σ（I）.A new thiostannate,[tmdpH2]Sn3S7 1（tmdp = 4,4＇-trimethylenedipiperidine）,has been synthesized under solvothermal conditions and characterized by elemental analysis,IR spectroscopy,and single-crystal X-ray diffraction analysis.In 1,the Sn3S4 secondary incomplete cubane-like building units are bridged by μ2-S atoms to form Sn12S12 rings which are then joined parallelly to the [001] plane,giving the final 2D（Sn3S7^2-）n layer of（6,3） network.The layers are stacked along the c axis so that 24-membered ring channels are generated,in which the organic cations are accommodated.The compound crystallizes in monoclinic,space group C2/c,with a=23.052（3）,b=13.4039（12）,c=18.412（2）A,β=120.112（4）°,V=4921.3（9）A^3,C13H28N2S7Sn3,Mr=792.86,Z=8,Dc=2.140 g/cm^3,F（000）=3056,μ=3.619 mm^-1,the final R=0.0488 and wR=0.1125 for 4607 observed reflections with I〉2σ（I）.

关 键 词：thiostannate tmdp crystal structure 2D layer （6 3） network 

分 类 号：O621.2[理学—有机化学]