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Volumn 48, Issue 3, 2009, Pages 810-812

Zero-dimensional units of ligand-bridged gallium-sulfide supertetrahedra

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EID: 61549115912     PISSN: 00201669     EISSN: None     Source Type: Journal    
DOI: 10.1021/ic8020723     Document Type: Article
Times cited : (40)

References (31)
  • 24
    • 61549100991 scopus 로고    scopus 로고
    • Compound 1 was prepared by mixing of gallium metal (Alfa Aesar; 99.99, 139.4 mg, sulfur (Alfa Aesar; 99.5, 144 mg, DPE (Fluka > 98, 182 mg, FeCl2·4H2O (Aldrich; 99, 59.6 mg, and 3,5-dimethylpyridine (Aldrich; 98, 3 mL) in a 23 mL Teflon-lined stainless steel autoclave. This corresponds to a molar ratio of Ga:S: DPE:FeCl 2:3,5-dimethylpyridine, 2:4.5:1:0.3:26. After the vessel was sealed, the reaction mixture was heated at 200 °C for 10 days and then allowed to cool to room temperature at 1 °C min-1. The product consisted of a mixture of white crystals of 1 (yield 50, and a darkgray polycrystalline powder. For the synthesis of 2, bipy Aldrich; 98, was used as the organic linker. Crystals of 2 were produced by heating of a mixture with an approximate molar composition of Ga: S:bipy:3,5-dimethylpyridine, 2:4.5:1:22 at 200 °C for 20 days. The reaction product contained orange needles of
    • -1. The product consisted of a mixture of white crystals of 1 (yield 50%) and a darkgray polycrystalline powder. For the synthesis of 2, bipy (Aldrich; 98%) was used as the organic linker. Crystals of 2 were produced by heating of a mixture with an approximate molar composition of Ga: S:bipy:3,5-dimethylpyridine = 2:4.5:1:22 at 200 °C for 20 days. The reaction product contained orange needles of 2 (yield 90%), together with a small amount of unreacted gallium. Elem anal. Caled for 1: C, 26.3; H, 2.9; N, 4.5. Found: C, 25.9; H, 2.8; N, 4.6. Caled for 2: C, 25.05; H, 2.5; N, 5.4. Found: C, 27.1; H, 2.9; N, 5.7.
  • 25
    • 61549109336 scopus 로고    scopus 로고
    • 8)]
    • merg = 0.0421; 10 626 observed with I > 3σ(I), which were used in all calculations]. Final values of R(F) and wR(F) [with I > 3σ(Z)] were 0.0431 and 0.0478, respectively. Data collections using a Bruker X2 APEX 2 diffractometer (Mo Kα; λ = 0.71073 Å), at 100 K. The structures were solved by direct methods using the program SIR92 and models refined using CRYSTALS. Carbon and nitrogen atoms were located in the difference Fourier maps. Hydrogen atoms on the organic moieties were placed geometrically. Data for 2 were treated with SQUEEZE to correct die effect of the disordered organic cations. Those that could be located in the difference Fourier maps were modeled isotropically because their large thermal parameters suggest a certain degree of disorder.
  • 27
    • 61549100667 scopus 로고    scopus 로고
    • 4 powder was used as a reference, and the absorption data were calculated from the reflectance data using the Kubelka-Munk function.
    • 4 powder was used as a reference, and the absorption data were calculated from the reflectance data using the Kubelka-Munk function.


* 이 정보는 Elsevier사의 SCOPUS DB에서 KISTI가 분석하여 추출한 것입니다.