Synthesis and structure of (C18H36N2O6Na)(2)Na-2[Nb6Cl12(OCH3)(6)]center dot 15CH(3)OH

被引:0
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作者
Bech, U
Simon, A
Brnicevic, N
Sirac, S
机构
[1] MAX PLANCK INST FESTKORPERFORSCH,D-70569 STUTTGART,GERMANY
[2] RUDJER BOSKOVIC INST,ZAGREB 10000,CROATIA
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O6 [化学];
学科分类号
0703 ;
摘要
By the reaction of Nb(6)Cl(14)6CH(3)OH with sodium methoxide in methanol at 254 K, the triclinic cluster compound Na-4[Nb6Cl12(OCH3)(6)] nCH(3)OH 1 with a = 1125.2(11), b = 1156.9(11), c = 1294.9(13) pm, a = 89.66(8)degrees, beta = 71.46(8)degrees, gamma = 68.19(8)degrees and V = 1471.7 x 10(6) pm(3) has been prepared. Reacting 1 with 222-cryptand yields triclinic crystals (cryptNa)(2)Na-2[Nb6Cl12(OCH3)(6)]. 15CH(3)OH 2 with space group <P(1)over bar>(No. 2), a = 1325.6(4), b = 1669.2(6), c = 2442.1(9) pm, alpha = 81.70(3)degrees, beta = 77.09(3)degrees, gamma = 77.95(3)degrees; V = 5123.8(31) x 10(6) pm(3) Z = 2, Dc = 1.617 g/cm(3) The structure of 2 is built from (C18H36N2O6Na)(+) and [Na-2(CH3OH)(8)](2+) cations and [Nb6Cl12(OCH3)(6)](4-) anions. The Nb-Nb and Nb-Cli distances in the range of 295.2 to 298.0 pm and 246.6 to 249.8 pm, respectively, being longer than expected for [Nb6Cl12](2+) units, are not fully understood.
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页码:837 / 848
页数:12
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