层状多硫代锑(Ⅲ)酸镉(Ⅱ)化合物(1,4-DABH2)Cd2Sb2S6的溶剂热合成与表征

引用本文: 刚刚, 白音孟和, 王晓靖, 娜仁吉如嘎, 徐效清, 白乌云, 斯琴达莱. 层状多硫代锑(Ⅲ)酸镉(Ⅱ)化合物(1,4-DABH₂)Cd₂Sb₂S₆的溶剂热合成与表征[J]. 无机化学学报, 2013, 29(5): 979-984. doi: 10.3969/j.issn.1001-4861.2013.00.176 shu

Citation: GANG Gang, BAIYIN Meng-He, WANG Xiao-Jing, NAREN Ji-Ru-Ga, XU Xiao-Qing, BAI Wu-Yun, SIQIN Da-Lai. Solvothermal Synthesis and Characterzation of (1,4-DABH₂)Cd₂Sb₂S₆ with Layer Structure[J]. Chinese Journal of Inorganic Chemistry, 2013, 29(5): 979-984. doi: 10.3969/j.issn.1001-4861.2013.00.176 shu

层状多硫代锑(Ⅲ)酸镉(Ⅱ)化合物(1,4-DABH₂)Cd₂Sb₂S₆的溶剂热合成与表征

通讯作者: 白音孟和,E-mail:baiymh@imnu.edu.cn

基金项目:
教育部科学技术研究重点项目(No.210041) (No.210041)

内蒙古自然科学基金(No.20080404MS021)资助项目。 (No.20080404MS021)

摘要: 利用溶剂热方法合成了层状多硫代锑(Ⅲ)酸镉(Ⅱ)化合物(1,4-DABH₂)Cd₂Sb₂S₆ (1)(1,4-DAB=1,4-丁二胺),并通过红外光谱、热重分析对其进行了表征,用X-射线衍射测定了化合物的单晶结构。单晶解析表明,化合物属正交晶系,Cmca空间群,M_r=750.77,a=0.860 3(5) nm,b=0.898 7(6) nm,c=2.273(2) nm,V=1.758(2) nm³,Z=4,λ=0.071 073 nm,R=0.032,wR=0.106 7。晶体结构中含有六元环的Cd₂SbS₃和八元环的Cd₂Sb₂S₄的阴离子网络层状[CdSbS₃]_n^n-,双质子化的有机阳离子在阴离子层之间以氢键N-H…S形式连接。另外紫外-可见漫反射光谱研究表明,化合物为半导体。

关键词:

溶剂热合成;多硫代锑酸盐;晶体结构;表征

English

Solvothermal Synthesis and Characterzation of (1,4-DABH₂)Cd₂Sb₂S₆ with Layer Structure

1.
1. College of Chemistry & Environmental Science, Inner Mongolia Normal University, Huhhot 010022, China;

Corresponding author: 白音孟和,E-mail:baiymh@imnu.edu.cn

Received Date: 25 July 2012
Fund Project:
教育部科学技术研究重点项目(No.210041)

内蒙古自然科学基金(No.20080404MS021)资助项目。

Abstract: A multiple thioantimonate compound, (1,4-DABH₂)Cd₂Sb₂S₆ (1) (1,4-DAB=1,4-diaminobutane) , was solvothermally synthesized at 160 ℃ and characterized by IR and TGA. Its crystal structure analysis reveals the compound was determined by single crystal X-ray diffraction. The crystal structure is orthorhombic in the space group Cmca. Crystallographic data: M_r=750.77, a=0.860 3(5) nm, b=0.898 7(6) nm, c=2.273(2) nm, V=1.758(2) nm³, Z=4, λ=0.071 073 nm, R=0.032 0, wR=0.106 7. The compound features two-dimensional (2D) grid layer of [CdSbS₃]_n^n- with six-membered Cd₂SbS₃ rings and eight-membered Cd₂Sb₂S₄ rings. The doubly protonated organic cations are located at the interlayer spaces of [CdSbS₃]_n^n- and form extensive N-H…S hydrogen bonds. In addition, UV-Vis diffusion reflectance spectra suggest that the compound is semiconductor with estimated band gap 2.10 eV. CCDC: 879803.

Key words:

solvothermal synthesis;multiple thioantimonate;crystal structure;characterization

1. [1] Wu T, Bu X H, Feng P Y, et al. J. Am. Chem. Soc., 2011, 133:9616-9625[1] Wu T, Bu X H, Feng P Y, et al. J. Am. Chem. Soc., 2011, 133:9616-9625
2. [2] Powell A V, Lees R J E, Chippindale A M. J. Phys. Chem. Solids, 2008,69:1000-1006[2] Powell A V, Lees R J E, Chippindale A M. J. Phys. Chem. Solids, 2008,69:1000-1006
3. [3] Wang X, Sheng T L, Wu X T, et al. J. Solid State Chem., 2009,182:913-919[3] Wang X, Sheng T L, Wu X T, et al. J. Solid State Chem., 2009,182:913-919
4. [4] JIANG Hao(姜浩), WANG Xin(王欣), WU Xin-Tao(吴新涛), et al. Sci. China Chem.(Zhongguo Kexue: Huaxue), 2011,41 (4):726-731[4] JIANG Hao(姜浩), WANG Xin(王欣), WU Xin-Tao(吴新涛), et al. Sci. China Chem.(Zhongguo Kexue: Huaxue), 2011,41 (4):726-731
5. [5] Ren J, Wagner T, Chen G R, et al. J. Appl. Phys., 2011, 109:33105-33111[5] Ren J, Wagner T, Chen G R, et al. J. Appl. Phys., 2011, 109:33105-33111
6. [6] Glitzendanner R L, Disalvo F J. Inorg. Chem., 1996,35:2623 -2626[6] Glitzendanner R L, Disalvo F J. Inorg. Chem., 1996,35:2623 -2626
7. [7] Pienack N, Näther C, Bensch W, et al. Inorg. Chem., 2008, 47:9606-9611[7] Pienack N, Näther C, Bensch W, et al. Inorg. Chem., 2008, 47:9606-9611
8. [8] Zhang R C, Zhang C, An Y L, et al. J. Solid State Chem., 2012,186:94-98[8] Zhang R C, Zhang C, An Y L, et al. J. Solid State Chem., 2012,186:94-98
9. [9] Iban M, Fairbrother A, Cabotdx A, et al. Chem. Mater., 2012,24:562-570[9] Iban M, Fairbrother A, Cabotdx A, et al. Chem. Mater., 2012,24:562-570
10. [10] Bedard R L, Wilson S T, Vail L D. Zeolites: Facts, Figures, Future, Proceedings of the 8th International Zeolite Confere- nce. Jacobs P A, Santen R A Ed., Amsterdam: Elsevier Science, 1989:375-387[10] Bedard R L, Wilson S T, Vail L D. Zeolites: Facts, Figures, Future, Proceedings of the 8th International Zeolite Confere- nce. Jacobs P A, Santen R A Ed., Amsterdam: Elsevier Science, 1989:375-387
11. [11] Liu X, Zhou J. Inorg. Chem. Commun., 2011,14:1286-1289[11] Liu X, Zhou J. Inorg. Chem. Commun., 2011,14:1286-1289
12. [12] Wang X, Sheng T L, Wu X T, et al. J. Mol. Struct., 2009, 936:142-146[12] Wang X, Sheng T L, Wu X T, et al. J. Mol. Struct., 2009, 936:142-146
13. [13] Liu Y, Tian Y F, Zhang Q C, et al. Inorg. Chem. Commun., 2011,14:884-888[13] Liu Y, Tian Y F, Zhang Q C, et al. Inorg. Chem. Commun., 2011,14:884-888
14. [14] Spetzler V, Näther C, Bensch W, et al. Z. Anorg. Allg. Chem., 2004,630:142-148[14] Spetzler V, Näther C, Bensch W, et al. Z. Anorg. Allg. Chem., 2004,630:142-148
15. [15] Spetzler V, Näther C, Bensch W. Inorg. Chem., 2005,44: 5805-5812[15] Spetzler V, Näther C, Bensch W. Inorg. Chem., 2005,44: 5805-5812
16. [16] Vaqueiro P, Cowley A R, Powell A P, et al. Inorg. Chem., 2003,42:7846-7851[16] Vaqueiro P, Cowley A R, Powell A P, et al. Inorg. Chem., 2003,42:7846-7851
17. [17] Lin Z E, Bu X H, Feng P Y. Microporous Mesoporous Mater., 2010,132:328-334[17] Lin Z E, Bu X H, Feng P Y. Microporous Mesoporous Mater., 2010,132:328-334
18. [18] Kong D N, Xie Z L, Huang X Y, et al. Cryst. Growth Des., 2010,10(3):1364-1372[18] Kong D N, Xie Z L, Huang X Y, et al. Cryst. Growth Des., 2010,10(3):1364-1372
19. [19] Kiebach R, Näther C, Bensch W. Z. Anorg. Allg. Chem., 2002,628:2176[19] Kiebach R, Näther C, Bensch W. Z. Anorg. Allg. Chem., 2002,628:2176
20. [20] Schaefer M, Näther C, Bensch W. Solid State Sci., 2003,5: 1135-1139[20] Schaefer M, Näther C, Bensch W. Solid State Sci., 2003,5: 1135-1139
21. [21] Stähler R, Bensch W. Eur. J. Inorg. Chem., 2001:3073-3078[21] Stähler R, Bensch W. Eur. J. Inorg. Chem., 2001:3073-3078
22. [22] Stähler R, Mosel B D, Bensch W, et al. Angew. Chem. Int. Ed., 2002,41(23):4487-4489[22] Stähler R, Mosel B D, Bensch W, et al. Angew. Chem. Int. Ed., 2002,41(23):4487-4489
23. [23] Stähler R, Näther C, Bensch W. J. Solid State Chem., 2003, 174:264-275[23] Stähler R, Näther C, Bensch W. J. Solid State Chem., 2003, 174:264-275
24. [24] Stähler R, Näther C, Bensch W. Eur. J. Inorg. Chem., 2001: 1835-1840[24] Stähler R, Näther C, Bensch W. Eur. J. Inorg. Chem., 2001: 1835-1840
25. [25] Schaefer M, Engelke L, Bensch W. Z. Anorg. Allg. Chem., 2003,629:1912-1918[25] Schaefer M, Engelke L, Bensch W. Z. Anorg. Allg. Chem., 2003,629:1912-1918
26. [26] Vaqueiro P, Chippindale A M, Powell A P. Inorg. Chem., 2004,43:7963-7965[26] Vaqueiro P, Chippindale A M, Powell A P. Inorg. Chem., 2004,43:7963-7965
27. [27] Powell A P, Lees R J E, Chippindale A M. J. Phys. Chem. Solids, 2008,69:1000-1006[27] Powell A P, Lees R J E, Chippindale A M. J. Phys. Chem. Solids, 2008,69:1000-1006
28. [28] Vaqueiro P, Chippindale A M, Powell A P. Polyhedron, 2003,22:2839-2845[28] Vaqueiro P, Chippindale A M, Powell A P. Polyhedron, 2003,22:2839-2845
29. [29] Lees R J E, Powell A P, Chippindale A M. Polyhedron, 2005,24:1941-1948[29] Lees R J E, Powell A P, Chippindale A M. Polyhedron, 2005,24:1941-1948
30. [30] Jia D X, Jin Q Y, Chen J F, et al. Inorg. Chem., 2009,48 (17):8286-8293[30] Jia D X, Jin Q Y, Chen J F, et al. Inorg. Chem., 2009,48 (17):8286-8293
31. [31] WANG Jiao(王娇), PAN Ying-Li(潘迎利), JIA Ding-Xian(贾定光), et al. Chinese J. Inorg. Chem.(Wuji Huaxue Xuebao), 2010,26(8):1339-1344[31] WANG Jiao(王娇), PAN Ying-Li(潘迎利), JIA Ding-Xian(贾定光), et al. Chinese J. Inorg. Chem.(Wuji Huaxue Xuebao), 2010,26(8):1339-1344
32. [32] Jia D X, Zhang Y, Zhao Q X, et al. Inorg. Chem., 2006,45: 9812-9817[32] Jia D X, Zhang Y, Zhao Q X, et al. Inorg. Chem., 2006,45: 9812-9817
33. [33] BIAN Guo-Qing(卞国庆), ZHOU Jian(周健), DAI Jie(戴洁), et al. Chem. Res. Appl. (Huaxue Yanjiu Yu Yingyong), 2008, 20(1):54-57[33] BIAN Guo-Qing(卞国庆), ZHOU Jian(周健), DAI Jie(戴洁), et al. Chem. Res. Appl. (Huaxue Yanjiu Yu Yingyong), 2008, 20(1):54-57
34. [34] Zhou J, Yin X H, Zhang F. Inorg. Chem., 2010,49:9671- 9676[34] Zhou J, Yin X H, Zhang F. Inorg. Chem., 2010,49:9671- 9676
35. [35] Wood P T, Schimek G L, Kolis J W. Chem. Mater., 1996,8: 721-726[35] Wood P T, Schimek G L, Kolis J W. Chem. Mater., 1996,8: 721-726
36. [36] Huang F Q, Ibers J A. J. Solid State Chem., 2005,178:212- 217[36] Huang F Q, Ibers J A. J. Solid State Chem., 2005,178:212- 217
37. [37] Li J, Chen Z, Wang X X, Proserpio D M. J. Alloys Compd., 1997,262-263:28-33[37] Li J, Chen Z, Wang X X, Proserpio D M. J. Alloys Compd., 1997,262-263:28-33
38. [38] CHEN Zhen(陈震), WANG Ru-Ji(王如骥). Acta Chim. Sinica (Huaxue Xuebao), 2000,58(3):326-331[38] CHEN Zhen(陈震), WANG Ru-Ji(王如骥). Acta Chim. Sinica (Huaxue Xuebao), 2000,58(3):326-331
39. [39] Yao H G, Zhou P, An Y L, et al. Inorg. Chem., 2010,49: 1186-1190[39] Yao H G, Zhou P, An Y L, et al. Inorg. Chem., 2010,49: 1186-1190
40. [40] Lekse J W, Moreau M A, Aitken J A, et al. Inorg. Chem., 2009,48:7516-7518[40] Lekse J W, Moreau M A, Aitken J A, et al. Inorg. Chem., 2009,48:7516-7518
41. [41] Zhang L D, Han C Y, Guo H Y, et al. Chem. Res. Chinese Universities, 2010,26(4):514-516[41] Zhang L D, Han C Y, Guo H Y, et al. Chem. Res. Chinese Universities, 2010,26(4):514-516
42. [42] CHEN Zhen(陈震), WANG Ru-Ji(王如骥). Chinese J. Inorg. Chem.(Wuji Huaxue Xuebao), 1999,15(5):662-666[42] CHEN Zhen(陈震), WANG Ru-Ji(王如骥). Chinese J. Inorg. Chem.(Wuji Huaxue Xuebao), 1999,15(5):662-666
43. [43] Sheldrick G M. SHELXTL, Program for the Solution and the Refinement of Crystal Structures, Universitt Gtötingen, Germany, 1997.[43] Sheldrick G M. SHELXTL, Program for the Solution and the Refinement of Crystal Structures, Universitt Gtötingen, Germany, 1997.
44. [44] Pienack N, Näther C, Bensch W. Solid State Sci., 2007,9: 100-107[44] Pienack N, Näther C, Bensch W. Solid State Sci., 2007,9: 100-107
45. [45] Wendlandt W W, Hecht H G. Reflectance Spectroscopy. New York: Interscience Publishers, 1966.[45] Wendlandt W W, Hecht H G. Reflectance Spectroscopy. New York: Interscience Publishers, 1966.

扫一扫看文章

计量

PDF下载量: 251
文章访问数: 1343
HTML全文浏览量: 159

通讯作者: 陈斌, bchen63@163.com

1.
沈阳化工大学材料科学与工程学院沈阳 110142

层状多硫代锑(Ⅲ)酸镉(Ⅱ)化合物(1,4-DABH₂)Cd₂Sb₂S₆的溶剂热合成与表征

通讯作者: 白音孟和,E-mail:baiymh@imnu.edu.cn

English

Solvothermal Synthesis and Characterzation of (1,4-DABH₂)Cd₂Sb₂S₆ with Layer Structure

Corresponding author: 白音孟和,E-mail:baiymh@imnu.edu.cn

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南：你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

计量

通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处