SYNTHESIS AND STRUCTURE OF O6NA)(2)NA-2[NB6CL12(OCH3)(6)]CENTER-DOT-15CH(3)OH

Citation
U. Bech et al., SYNTHESIS AND STRUCTURE OF O6NA)(2)NA-2[NB6CL12(OCH3)(6)]CENTER-DOT-15CH(3)OH, Croatica chemica acta, 68(4), 1995, pp. 837-848
Citations number
19
Categorie Soggetti
Chemistry
Journal title
ISSN journal
00111643
Volume
68
Issue
4
Year of publication
1995
Pages
837 - 848
Database
ISI
SICI code
0011-1643(1995)68:4<837:SASOO>2.0.ZU;2-O
Abstract
By the reaction of Nb(6)Cl(14)6CH(3)OH with sodium methoxide in methan ol 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)O H 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 = 1.6 17 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 24 9.8 pm, respectively, being longer than expected for [Nb6Cl12](2+) uni ts, are not fully understood.