SYNTHESIS AND CRYSTAL-STRUCTURE OF MOCL4(1,2-DIMETHOXYETHANE).15-CROWN-5 AND MOCL4(1,2-DIMETHOXYETHANE)

被引:0
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作者
HEYHAWKINS, E
VONSCHNERING, HG
机构
来源
ZEITSCHRIFT FUR NATURFORSCHUNG SECTION B-A JOURNAL OF CHEMICAL SCIENCES | 1991年 / 46卷 / 03期
关键词
TETRACHLORO(1,2-DIMETHOXYETHANE)MOLYBDENUM(IV); TETRACHLORO(1,2-DIMETHOXYETHANE)MOLYBDENUM(IV).15-CROWN-5; CRYSTAL STRUCTURE;
D O I
暂无
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
NaSi reacts with MoCl5 and 15-crown-5 in toluene with reduction of Mo(V) to Mo(IV). Work-up in DME yields MoCl4(DME). 15-crown-5 (1). MoCl4(DME) (2) is prepared more conveniently from MoCl5/DME. 1 and 2 were characterized spectroscopically and by X-ray structure determination. Crystal data: 1, space group P2(1)2(1)2(1) (No. 19), Z = 4,2765 observed independent reflexions, R = 0.026, cell dimensions (110 K): a = 16.292(4), b = 12.884(3), c = 10.452(2)angstrom. 2, space group 142d (No. 122), Z = 8,558 observed independent reflexions, R = 0.037, cell dimensions (292 K): a = b = 9.56(2), c = 23.777(6) angstrom. The MoCl4(DME) molecule of 1 and 2 forms a distorted octahedron. There are four non-coordinating 15-crown-5 molecules present in the unit cell of 1. The UV/VIS spectrum and the magnetic properties of 2 are discussed.
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页码:307 / 314
页数:8
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