期刊
ZEITSCHRIFT FUR ANORGANISCHE UND ALLGEMEINE CHEMIE
卷 632, 期 10-11, 页码 1681-1686出版社
WILEY-V C H VERLAG GMBH
DOI: 10.1002/zaac.200600007
关键词
beryllium; antimony; beryllium crown ether complex; antimony trichloride; crown ether complexes
Beryllium chloride reacts in dichloromethane suspension in the presence of the equimolar amount of 12-crown-4 with antimony pentachloride exothermically to give [BeCl(12-crown4)][SbCl4] (1), which is characterized by IR spectroscopy and by single crystal structure determination. Space group P2(1)/c, Z = 8, lattice dimensions at 193 K: a = 1116.4(2), b = 1735.4(2), c = 1709.8(3)pm, beta = 91.31(1)degrees, R-1 = 0.0301. 1 contains cations [BeCl(12-crown-4)](+) with coordination number five at the beryllium atom, and polymeric anions [SbCl4-](infinity), forming zigzag chains along [001] with coordination number five at the antimony atoms, thus showing the steric effect of the lone pair. I can also be obtained by using the twofold amounts of 12-crown-4 and antimony pentachloride, however, accompanied by forming [SbCl3(12-crown-4)] (2). With respect to the wrong crystal structure determinations previously reported in the literature, we solved the X-ray structure of 2 in the space group P2(1)/c, Z = 4, lattice dimensions at 173 K: a = 1191.4(1), b = 783.7(1), c = 1489.7(2) pm, beta = 90.83(1)degrees, R-1 = 0.0243.
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