Citation: LIU Fang, WULAN Gerile, DA Lima, BAO Yong-Sheng, BAIYIN Meng He. Syntheses and Structural Characterization of Multi-component Chalcogenide Compounds Based on Pyridine/1,2-Ethanedithiol Solvent[J]. Chinese Journal of Structural Chemistry, ;2016, 35(6): 946-952. doi: 10.14102/j.cnki.0254-5861.2011-0963 shu

Syntheses and Structural Characterization of Multi-component Chalcogenide Compounds Based on Pyridine/1,2-Ethanedithiol Solvent

a.
a. College of Chemistry & Environmental Science, Innner Mongolia Normal University, Hohhot 010022, China;
b.
b. Key Laboratory for Physics and Chemistry of Functional Materials, Inner Mongolia, Hohhot 010022, China;
c.
c. Chemistry and Chemical Engineering College, Inner Mongolia University for the Nationalities, Tongliao 028043, China

Received Date: 28 August 2015
Available Online: 11 November 2015
Fund Project: This project was supported by the National Natural Science Foundation of China (No.21461019) (No.21461019)

Reactions of Sn powder, cadmium iodide, rubidium carbonate, and sodium sulfide yielded two new compounds: three-dimensional chalcogenide RbNa₃Cd₂Sn₂S₈ (1) and layered ternary compound Na₂CdS₂ (2). 1 and 2 have been determined by single-crystal X-ray diffraction: 1 belongs to the orthorhombic space group Pca2₁, with a = 13.486(3), b = 6.7310(14), c = 18.401(4) Å and Z = 4; 2 crystallizes in the R3m space group, with a = 3.718(3), c = 26.170(4) Å and Z = 3. Study of the yellow block shaped crystals of 1 reveals that the structure consists of tetrahedral CdS₄ and SnS₄. The {Cd₂Sn₂S₈} cluster shows a 12-numbered ring structure assembled by corner-sharing of alternating SnS₄and CdS₄, and the rubidium and sodium ions act as void-filling and charge compensating cations. The dark orange hexagonal crystal of compound 2 consists of a unique [CdS₂]^2- layer, which are separated by the Na⁺. UV/Vis absorption spectrum exhibits the materials 1 and 2 have semiconductor properties.
- solvothermal synthesis,
- tin,
- cadmium,
- crystal structure
1. [1]
  (1) Jing, H.; Wang, X.; Sheng, T.; Hu, S.; Fu, R.; Wu, X. Synthesis, structure, and characterization of a novel selenidoarsenate: incorporation of [Mn(phen)₂]²⁺ cations into [As^III₂Se₃(Se₂)]^2- chains. Inorg. Chem. Commun. 2012, 17, 5-8.
2. [2]
  (2) Zhou, J.; Liu, X.; Liang, G.; Liang, W.; Hu, F.; Zhu, L. [Ni(dien)₂]₃[Ge₃Sb₈S₂₁]·0.5H₂O: a new 2-D layered thiogermanate-thioantimonate with metal complexes as template ions. Inorg. Chem. Commun. 2013, 27, 92–96.
3. [3]
  (3) Liang, J.; Chen, J.; Zha, J.; Pan, Y.; Zhang, Y.; Jia, D. Solvothermal syntheses, crystal structures, and thermal properties of the first example of selenidostannates with mixed ethylene polyamine-coordinated transition metal complexes as counterions. Z. Anorg. Allg. Chem. 2011, 637, 445–449.
4. [4]
  (4) Wang, L.; Sheng, T.; Zhang, J.; Hu, S.; Fu, R.; Wu, X.; Li, Y.; Huang, X.; Xiang, S. A convenient method for the conversion of [Sn₃S₄]^2- to [Sn₃S₃(µ₃-OH)]^-: syntheses, structures and characterizations of (Bu₄N)[Sn₃(µ₃-OH)S₃(edt)₃]·DMF and (Bu₄N)[Sn₃(µ₃-OH)S₃(edt)₃]·H₂O (edt = 1,2-ethanedithiolate). Polyhedron 2007, 26, 1098–1104.
5. [5]
  (5) Zhang, X.; Pu, Y.; You, L.; Bian, G.; Zhu, Q.; Dai, J. Wheel-shaped indium telluride nanoclusters co-crystallized with metal-phenanthroline complexes. Polyhedron 2013, 52, 645–649.
6. [6]
  (6) Zhou, J.; Liu, X.; An, L.; Hu, F.; Yan, W.; Zhang, Y. Solvothermal synthesis and characterization of a series of lanthanide thiostannates(IV): the first examples of inorganic-organic hybrid cationic lanthanide thiostannates(IV). Inorg. Chem. 2012, 51, 2283-2290.
7. [7]
  (7) Llanos, J.; Mujica, C.; Sánchez, V.; Peña, O. Physical and optical properties of the quaternary sulfides SrCu₂MS₄ and EuCu₂MS₄ (M = Ge and Sn). J. Solid State Chem. 2003, 173, 78–82.
8. [8]
  (8) Aitken, A.; Lekse, J. W.; Yao, J.; Quinones, R. Synthesis, structure an dphysicochemical characterization of a noncentrosymmetric, quaternarythiostannate: EuCu₂SnS₄. J. Solid State Chem. 2009, 182, 141–146.
9. [9]
  (9) Chen, R.; Zhou, J.; Liu, X.; Hu, F.; An, L.; Kan, Y.; Xue, C. A new polymorph telluridoindate [In(en)₃][In₅Te₉(en)₂] with photocatalytic properties. Inorg. Chem. Commun. 2013, 28, 55–59.
10. [10]
  (10) Fard, Z. H.; Kanatzidis, M. G. Phase-change materials exhibiting tristability: interconverting forms of crystalline α-, β-, and glassy K₂ZnSn₃S₈. Inorg. Chem. 2012, 51, 7963-7965.
11. [11]
  (11) Yue, C.; Lei, X.; Zang, H.; Zhai, X.; Feng, L.; Zhao, Z.; Zhao, J.; Liu, X. Two manganese-amine complexes incorporating thioantimonates and exhibiting diversiform roles of amine ligands. Cryst. Eng. Commun. 2014, 16, 3424–3430.
12. [12]
  (12) Löken, S.; Tremel, W. Syntheses, structures, and properties of new quaternary gold-chalcogenides: K₂Au₂Ge₂S₆, K₂Au₂Sn₂Se₆, and Cs₂Au₂SnS₄. Z. Anorg. Allg. Chem. 1998, 624, 1588–1594.
13. [13]
  (13) Jia, D.; Zhang, Y.; Dai, J.; Zhu, Q.; Gu, X. Solvothermal syntheses and characterization of thiostannates [M(en)₃]₂Sn₂S₆ (M = Mn, Co, Zn), the influence of metal ions on the crystal structure. Z. Anorg. Allg. Chem. 2004, 630, 313–318.
14. [14]
  (14) Xiong, W.; Ye, K.; Ye, L.; Zhang, Q. Syntheses, crystal structures, and properties of two new one-dimensional heterometallic selenides: [DBNH]₄[M₃Sn₄Se₁₁(Se₂)₂] (M = Cd, Hg). Inorg. Chem. Commun. 2013, 35, 337–341.
15. [15]
  (15) Jiang, T.; Lough, A.; Ozin, G. A.; Bedard, R. L.; Broach, R. Synthesis and structure of microporous layered tin(IV) sulfide materials. J. Mater. Chem. 1998, 8, 721–732.
16. [16]
  (16) Loose, A.; Sheldrick, W. S. Synthesis and structure of [Sn₄Se₁₁]^6-,[Sn₂Se₅^2-], and [Sn₃Se₇^2-] model anions for the solventothermal reaction pathway to lamellar selenidostannates(IV). Z. Anorg. Allg. Chem. 1999, 625, 233–240.
17. [17]
  (17) Wan, Y.; Feng, M.; Wang, K.; Li, J.; Wang, Z.; Zou, G.; Huang, X. Two novel one-dimensional mercury selenidostannates with transitionmetal complexes: [Fe(phen)₃]Hg₂Sn₂Se₇·1.5eta·0.25H₂O and [Ni₂(teta)₂(μ-teta)]HgSn₃Se₉. Inorg. Chem. Commun. 2013, 33, 10–14.
18. [18]
  (18) Sheldrick, W. S.; Wachhold, M. Solventothermal synthesis of solid-state chalcogenidometalates. Angwe. Chem. Int. Ed. Engl. 1997, 36, 206–224.
19. [19]
  (19) Eisenmann, B.; Schwerer, H.; Schäfer, H. Plane, zu ketten verknopfte [Te₅]^6--anionen im K₂SnTe₅ Mater. Res. Bull. 1983, 18, 383–387.
20. [20]
  (20) Dhingra, S. S.; Haushalter, R. C. One-dimensional inorganic polymers: synthesis and structural characterization of the main-group metal polymers K₂HgSnTe₄, (EtdN)₂HgSnTe₄,(Ph₄P)GeInTe₄, and RbInTe₂. Chem. Mater. 1994, 6, 2376–2381.
21. [21]
  (21) Pienack, N.; Möller, K.; Näther, C.; Bensch, W. (1,4-dabH)₂MnSnS₄: the first thiostannate with integrated Mn²⁺ ions in an anionic chain structure. Solid State Sciences 2007, 9, 1110–1114.
22. [22]
  (22) Pienack, N.; Bensch, W. The new silver thiostannate (1,4-dabH₂)Ag₂SnS₄: solvothermal synthesis, crystal structure and spectroscopic properties. Z. Anorg. Allg. Chem. 2006, 632, 1733–1736.
23. [23]
  (23) Pienack, N.; Näther, C.; Bensch, W. Two new copper thiostannates synthesized under solvothermal conditions: crystal structures, spectroscopic and thermal properties of (DBUH)CuSnS₃ and (1,4-dabH₂)Cu₂SnS₄. Solid State Sciences 2007, 9, 100–107.
24. [24]
  (24) Baiyin, M.; Naren, J.; Gang, G.; Wang, X.; Xu, X. Two new quaternary selenostannates synthesized under solvothermal conditions: crystal structure and reflectance spectra of (1,4-dabH)₂MnSnSe₄ and (1,4-dabH₂)Cu₂SnSe₄. Inorg. Chem. Commun. 2013, 35, 135–139.
25. [25]
  (25) ([1]) Pienack, N.; Puls, A.; Näther, C.; Bensch, W. The layered thiostannate (dienH₂)Cu₂Sn₂S₆: a photoconductive inorganic-organic hybrid compound. Inorg. Chem. 2008, 47, 9606–9611.
26. [26]
  (26) Xiong, W.; Miao, J.; Li, P.; Zhao, Y.; Liu, B.; Zhang, Q. [enH][Cu₂AgSnS₄]: a quaternary layered sulfide based on Cu–Ag–Sn–S composition. Cryst. Eng. Commun. 2014, 16, 5989–5992.
27. [27]
  (27) Xiong, W.; Miao, J.; Li, P.; Zhao, Y.; Liu, B.; Zhang, Q. {[M(NH₃)₆][Ag₄M₄Sn₃Se₁₃]}_∞ (M = Zn, Mn): three-dimensional chalcogenide frameworks constructed from quaternary metal selenide clusters with two different transitionmetals. J. Solid State Chem. 2014, 218, 146–150.
28. [28]
  (28) Behrens, M.; Ordolff, M.; Näther, C.; Bensch, W.; Becker, K. New three-dimensional thiostannates composed of linked Cu₈S₁₂ clusters and the first example of a mixed-metal Cu₇SnS₁₂ cluster. Inorg. Chem. 2010, 49, 8305–8309.
29. [29]
  (29) An, Y.; Ji, M.; Baiyin, M.; Liu, X.; Jia, C.; Wang, D. A solvothermal synthesis and the structure of K₄Ag₂Sn₃S₉·2KOH. Inorg. Chem. 2003, 42, 4248–4249.
30. [30]
  (30) Baiyin, M.; An, Y.; Liu, X.; Ji, M.; Jia, C.; Ning, G. K₂Ag₆Sn₃S₁₀: quaternary sulfide composed of silver sulfide layers pillared by zigzag chains [SnS3]^2-. Inorg. Chem. 2004, 43, 3764–3765.
31. [31]
  (31) ([1]) An, Y.; Ye, L.; Ji, M.; Liu, X.; Menghe, B.; Jia, C. A solvothermal synthesis and structure of a novel open-framework K₄Ag₂Ge₃S₉·H₂O. J. Solid State Chem. 2004, 177, 2506–2510.
32. [32]
  (32) Sheldrick, G. M. SHELXS-97, Program for X-ray Crystal Structure Solution. University of Göttingen, Germany 1997.
33. [33]
  (33) Banerjee, S.; Malliakas, C. D.; Kanatzidis, M. G. New layered tin(II) thiophosphates ASnPS₄ (A = K, Rb, Cs): synthesis, structure, glass formation, and the modulated CsSnPS₄. Inorg. Chem. 2012, 51, 11562-11573.
34. [34]
  (34) Deng, B.; Chan, G. H.; Huang, F. H.; Gray, D. L.; Ellisa, D. E.; Van Duyne, R. P.; Ibers, J. A. Synthesis, structure, optical properties, and electronic structure of NaLiCdS₂. J. Solid State Chem. 2007, 180, 759-764.
1. [1]
  Yao HUANG , Yingshu WU , Zhichun BAO , Yue HUANG , Shangfeng TANG , Ruixue LIU , Yancheng LIU , Hong LIANG . Copper complexes of anthrahydrazone bearing pyridyl side chain: Synthesis, crystal structure, anticancer activity, and DNA binding. Chinese Journal of Inorganic Chemistry, 2025, 41(1): 213-224. doi: 10.11862/CJIC.20240359
2. [2]
  Lulu DONG , Jie LIU , Hua YANG , Yupei FU , Hongli LIU , Xiaoli CHEN , Huali CUI , Lin LIU , Jijiang WANG . Synthesis, crystal structure, and fluorescence properties of Cd-based complex with pcu topology. Chinese Journal of Inorganic Chemistry, 2025, 41(4): 809-820. doi: 10.11862/CJIC.20240171
3. [3]
  Xiumei LI , Linlin LI , Bo LIU , Yaru PAN . Syntheses, crystal structures, and characterizations of two cadmium(Ⅱ) coordination polymers. Chinese Journal of Inorganic Chemistry, 2025, 41(3): 613-623. doi: 10.11862/CJIC.20240273
4. [4]
  Yan XU , Suzhi LI , Yan LI , Lushun FENG , Wentao SUN , Xinxing LI . Structure variation of cadmium naphthalene-diphosphonates with the changing rigidity of N-donor auxiliary ligands. Chinese Journal of Inorganic Chemistry, 2025, 41(2): 395-406. doi: 10.11862/CJIC.20240226
5. [5]
  Chao LIU , Jiang WU , Zhaolei JIN . Synthesis, crystal structures, and antibacterial activities of two zinc(Ⅱ) complexes bearing 5-phenyl-1H-pyrazole group. Chinese Journal of Inorganic Chemistry, 2024, 40(10): 1986-1994. doi: 10.11862/CJIC.20240153
6. [6]
  Xiaoxia WANG , Ya'nan GUO , Feng SU , Chun HAN , Long SUN . Synthesis, structure, and electrocatalytic oxygen reduction reaction properties of metal antimony-based chalcogenide clusters. Chinese Journal of Inorganic Chemistry, 2024, 40(6): 1201-1208. doi: 10.11862/CJIC.20230478
7. [7]
  Xiaoling WANG , Hongwu ZHANG , Daofu LIU . Synthesis, structure, and magnetic property of a cobalt(Ⅱ) complex based on pyridyl-substituted imino nitroxide radical. Chinese Journal of Inorganic Chemistry, 2025, 41(2): 407-412. doi: 10.11862/CJIC.20240214
8. [8]
  Kaimin WANG , Xiong GU , Na DENG , Hongmei YU , Yanqin YE , Yulu MA . Synthesis, structure, fluorescence properties, and Hirshfeld surface analysis of three Zn(Ⅱ)/Cu(Ⅱ) complexes based on 5-(dimethylamino) isophthalic acid. Chinese Journal of Inorganic Chemistry, 2024, 40(7): 1397-1408. doi: 10.11862/CJIC.20240009
9. [9]
  Huan ZHANG , Jijiang WANG , Guang FAN , Long TANG , Erlin YUE , Chao BAI , Xiao WANG , Yuqi ZHANG . A highly stable cadmium(Ⅱ) metal-organic framework for detecting tetracycline and p-nitrophenol. Chinese Journal of Inorganic Chemistry, 2024, 40(3): 646-654. doi: 10.11862/CJIC.20230291
10. [10]
  Jia JI , Zhaoyang GUO , Wenni LEI , Jiawei ZHENG , Haorong QIN , Jiahong YAN , Yinling HOU , Xiaoyan XIN , Wenmin WANG . Two dinuclear Gd(Ⅲ)-based complexes constructed by a multidentate diacylhydrazone ligand: Crystal structure, magnetocaloric effect, and biological activity. Chinese Journal of Inorganic Chemistry, 2025, 41(4): 761-772. doi: 10.11862/CJIC.20240344
11. [11]
  Ruikui YAN , Xiaoli CHEN , Miao CAI , Jing REN , Huali CUI , Hua YANG , Jijiang WANG . Design, synthesis, and fluorescence sensing performance of highly sensitive and multi-response lanthanide metal-organic frameworks. Chinese Journal of Inorganic Chemistry, 2024, 40(4): 834-848. doi: 10.11862/CJIC.20230301
12. [12]
  Lu LIU , Huijie WANG , Haitong WANG , Ying LI . Crystal structure of a two-dimensional Cd(Ⅱ) complex and its fluorescence recognition of p-nitrophenol, tetracycline, 2, 6-dichloro-4-nitroaniline. Chinese Journal of Inorganic Chemistry, 2024, 40(6): 1180-1188. doi: 10.11862/CJIC.20230489
13. [13]
  Xiaowei TANG , Shiquan XIAO , Jingwen SUN , Yu ZHU , Xiaoting CHEN , Haiyan ZHANG . A zinc complex for the detection of anthrax biomarker. Chinese Journal of Inorganic Chemistry, 2024, 40(10): 1850-1860. doi: 10.11862/CJIC.20240173
14. [14]
  Xiumei LI , Yanju HUANG , Bo LIU , Yaru PAN . Syntheses, crystal structures, and quantum chemistry calculation of two Ni(Ⅱ) coordination polymers. Chinese Journal of Inorganic Chemistry, 2024, 40(10): 2031-2039. doi: 10.11862/CJIC.20240109
15. [15]
  Meirong HAN , Xiaoyang WEI , Sisi FENG , Yuting BAI . A zinc-based metal-organic framework for fluorescence detection of trace Cu²⁺. Chinese Journal of Inorganic Chemistry, 2024, 40(8): 1603-1614. doi: 10.11862/CJIC.20240150
16. [16]
  Shuyan ZHAO . Field-induced Co^Ⅱ single-ion magnet with pentagonal bipyramidal configuration. Chinese Journal of Inorganic Chemistry, 2024, 40(8): 1583-1591. doi: 10.11862/CJIC.20240231
17. [17]
  Yinling HOU , Jia JI , Hong YU , Xiaoyun BIAN , Xiaofen GUAN , Jing QIU , Shuyi REN , Ming FANG . A rhombic Dy₄-based complex showing remarkable single-molecule magnet behavior. Chinese Journal of Inorganic Chemistry, 2025, 41(3): 605-612. doi: 10.11862/CJIC.20240251
18. [18]
  Xiaofen GUAN , Yating LIU , Jia LI , Yiwen HU , Haiyuan DING , Yuanjing SHI , Zhiqiang WANG , Wenmin WANG . Synthesis, crystal structure, and DNA-binding of binuclear lanthanide complexes based on a multidentate Schiff base ligand. Chinese Journal of Inorganic Chemistry, 2024, 40(12): 2486-2496. doi: 10.11862/CJIC.20240122
19. [19]
  Zhaodong WANG . In situ synthesis, crystal structure, and magnetic characterization of a trinuclear copper complex based on a multi-substituted imidazo[1,5-a]pyrazine scaffold. Chinese Journal of Inorganic Chemistry, 2025, 41(3): 597-604. doi: 10.11862/CJIC.20240268
20. [20]
  Jing REN , Ruikui YAN , Xiaoli CHEN , Huali CUI , Hua YANG , Jijiang WANG . Synthesis and fluorescence sensing of a highly sensitive and multi-response cadmium coordination polymer. Chinese Journal of Inorganic Chemistry, 2025, 41(3): 574-586. doi: 10.11862/CJIC.20240287

Get Citation

PDF

XML

Metrics

PDF Downloads(1)
Abstract views(2237)
HTML views(22)

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