New niobium complexes with alkynes. 1. Mono- and dinuclear complexes

New niobium complexes with alkynes. 1. Mono- and dinuclear complexes
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新的铌与炔烃的配合物。

DOI:
10.1021/ic00328a035
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发表时间:
1990
影响因子:
4.6
通讯作者:
M. Shang
M. Shang
中科院分区:
化学2区
文献类型:
--
作者:
F. Cotton;M. Shang

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报道了四种Nb的炔类配合物,并用X-射线单晶衍射法测定了它们的结构。由NbCl4(THF)2、汞齐钠和PhCCPh在四氢呋喃中反应得到的NbCl3(PhCCPh)(Thf)2(1)属于P2+/n空间群,晶胞参数为a=12.013(3)A,6=15.265(4)A,c=13.520(3)A,?=110.83(2),K=2317(1)A3,Z=4。由NbCl4(THF)2、Mg和PhCCPh在四氢呋喃中反应得到P2n空间群,a=13.751(3)k,b=10.867(2)A,c=14.592(2),?=116.91(1),V=1944.5(6)a3,Z=4.[Mg2Cl3(Thf)6][NbCl4(PhCCPh)(Thf)]-0.5THf(3)由NbCl4(Thf)2,Mg和PhCCPh在四氢呋喃中反应得到,在PI空间群中结晶,a=10.310(2)A,b=15.117(2)A,C=17.148(4)A,a=80.46(2),?=89.79(2),=87.24(1),V=2633(1)A3,Z=2。Nb2OCl4(PhCCPh)(四氢呋喃)4(4),通过与3相同的反应或其他两个反应,在C2/c空间群中结晶,a=20.581(3)A,b=9.829(2)A,c=19.176(3)A,?=19.176(9),V=3379(2)A3,Z=4。
Four alkyne complexes of niobium are reported, and their structures, determined by X-ray crystallography, are presented. NbCl3 (PhCCPh)(THF) 2 (1), prepared by the reaction of NbCl4 (THF) 2, sodium amalgam, and PhCCPh in THF, crystallizes in the P2¡/n space group with a= 12.013 (3) A, 6= 15.265 (4) A, c= 13.520 (3) A, ß= 110.83 (2), K= 2317 (1) A3, and Z= 4. NbCl3 (PhCCMe)(THF) 2 (2), prepared by the reaction of NbCl4 (THF) 2, sodium amalgam, and PhCCMe in THF, crystallizes in the P2\/n space group with a= 13.751 (3) k, b= 10.867 (2) A, c= 14.592 (2), ß= 116.91 (1), V= 1944.5 (6) A3, and Z= 4.[Mg2Cl3 (THF) 6][NbCl4 (PhCCPh)(THF)]-0.5 THF (3), preparedby the reaction of NbCl4 (THF) 2, Mg, and PhCCPh in THF, crystallizes in the Pi space group with a= 10.310 (2) A, b= 15.117 (2) A, c= 17.148 (4) A, a= 80.46 (2), ß= 89.79 (2),= 87.24 (1), V= 2633 (1) A3, and Z= 2. Nb2OCl4 (PhCCPh)(THF) 4 (4), prepared by the same reaction as for 3, or two other reactions, crystallizes in the C2/c space group with a= 20.581 (3) A, b= 9.829 (2) A, c= 19.176 (3) A, ß= 119.406 (9), V= 3379 (2) A3, and Z= 4.