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Synthesis and Crystal Structure of Ho_4S_3Si_2O_7

Synthesis and Crystal Structure of Ho_4S_3Si_2O_7
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摘要 In an attempt to synthesize the homologous sulfide of KHo2CuSe4 by using KBr as flux in a sealed evacuated quartz tube, transparent crystals of Ho4S3Si2O7 (Mr = 924.08) were isolated. The crystal structure of Ho4S3Si2O7 was determined by single-crystal X-ray diffraction method. Ho4S3Si2O7 crystallizes in a tetragonal system, space group I41/amd (No. 141) with a = 11.666(4), c = 13.593(5) ? V = 1850(2) ?, Z = 8, Dc = 6.64g/cm3, F(000)= 3200, m(MoKa) = 34.79mm-1, final R = 0.0355 and Rw = 0.0378 for 851 reflections with I > 3s(I). The structure of Ho4S3Si2O7 contains two crystallographically independent Ho3+ cations that are interconnected by S2 anions and the isolated [Si2O7]6 units. Ho(1) is coordinated by three O atoms and three S atoms to form a trigonal prismatic geometry, while Ho(2) is coordinated by six O atoms and three S atoms to form a tricapped trigonal prismatic geometry. The Si2O7 double tetrahedra are in the eclipsed configuration with non-linear SiOSi bridges (angle : 129.2(9)). In an attempt to synthesize the homologous sulfide of KHo2CuSe4 by using KBr as flux in a sealed evacuated quartz tube, transparent crystals of Ho4S3Si2O7 (Mr = 924.08) were isolated. The crystal structure of Ho4S3Si2O7 was determined by single-crystal X-ray diffraction method. Ho4S3Si2O7 crystallizes in a tetragonal system, space group I41/amd (No. 141) with a = 11.666(4), c = 13.593(5) ? V = 1850(2) ?, Z = 8, Dc = 6.64g/cm3, F(000)= 3200, m(MoKa) = 34.79mm-1, final R = 0.0355 and Rw = 0.0378 for 851 reflections with I > 3s(I). The structure of Ho4S3Si2O7 contains two crystallographically independent Ho3+ cations that are interconnected by S2 anions and the isolated [Si2O7]6 units. Ho(1) is coordinated by three O atoms and three S atoms to form a trigonal prismatic geometry, while Ho(2) is coordinated by six O atoms and three S atoms to form a tricapped trigonal prismatic geometry. The Si2O7 double tetrahedra are in the eclipsed configuration with non-linear SiOSi bridges (angle : 129.2(9)).
出处 《Chinese Journal of Structural Chemistry》 SCIE CAS CSCD 北大核心 2002年第2期157-160,共4页 结构化学(英文)
基金 Supported by the Director Fund of Fujian Institute of Research on the Structure of Matter (No. 200196).
关键词 FLUX rare earth pyrosilicate chalcogenide crystal structure flux, rare earth, pyrosilicate chalcogenide, crystal structure
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