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Synthesis and Characterization of New Oxidopolysulfidovanadates

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posted on 29.11.2001, 00:00 by Mehtap Emirdag-Eanes, James A. Ibers
The alkali-metal oxidopolysulfidovanadates Cs4[(VO)2(η2-S2)4(μ-S2)] (I), Cs5[(VO)3(η2-S2)6(μ-S4)] (II), and K6[(VO)4(η2-S2)8(μ-S3)]·2CH3OH·0.6H2O (III) have been synthesized by means of methanothermal methods at 170 °C or 175 °C. These compounds each contain a V5+ ion coordinated by an oxo ligand and two η2-S22- groups. In I, two such [VO(η2-S2)2]- units are bridged by an S22- unit. In II and III, two such [VO(η2-S2)2]- units are joined by a V−S−V bond to form [(VO(η2-S2)2)2]2- units; in II, such a [(VO(η2-S2)2)2]2- unit is bridged to a [VO(η2-S2)2]- unit by an S42- group; in III, two such [(VO(η2-S2)2)2]2- units are bridged by an S32- group. Crystallographic data at T = 153 K (compound, space group, Z, a, b, c, β):  I, P21/n, 2, 7.4366(3), 10.3743(5), 13.1151(6) Å, 101.097(1)°; II, P21/c, 4, 8.4451(6), 24.5144(18), 14.0995(10) Å, 101.325(1)°; III, C2/c, 4, 31.037(3), 12.5355(11), 8.7822(8) Å, 93.127(2)°.