Synthesis and structural characterization of three new compounds containing [Nb6Cl12]2+ units as hydrated hydroxides

N. Brničević, P. Planinić, R. Mccarley, S. Antolić, M. Luić, B. Kojić-Prodić
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引用次数: 9

Abstract

Conditions have been established for the preparation of three different hydrated chloroniobium cluster hydroxide compounds from alkaline solutions: triclinic [Nb6Cl12(OH)2(H2O)4]·4H2O 1 and two cubic compounds whose structures are uncertain with regard to the co-ordination of OH– ions, Nb6Cl12(OH)2(H2O)142 and Nb6Cl12(H2O)14(OMe)23. Based upon structural data 2 and 3 may contain either the cation [Nb6Cl12(H2O)6]2+ or the neutral cluster [Nb6Cl12(OH)2(H2O)4] containing hydroxo ligands. In 1 distinct distances of 2.147(5) for Nb–OH, and 2.250(5) and 2.289(5)A for Nb–OH2 were found. In 2 and 3 only distances of 2.19(1) and 2.193(7)A, respectively, were found for the Nb–O bonds of co-ordinated water (or hydroxide-water averaged). Compound 1 is triclinic, space group P1, a= 8.930(3), b= 9.195(2), c= 9.118(1)A, α= 104.37(2), β= 99.51(2) and γ= 116.99(2)°, U= 611.9(3)A3, Z= 1, R= 1, R= 0.036. Compound 2 is cubic, space group Fm3m, a= 14.59(2)A, U= 3105.7(1)A3, Z= 4, R= 0.028. Compound 3 is also cubic, space group Fm3m, a= 14.627(1)A, U= 3129.3(1)A3, Z= 4, R= 0.031. IR spectra of 1 show strong O–H and Nb–O stretching bands that reflect the presence of co-ordinated OH– groups. In 2 and 3 the IR spectra are less definitive about possible co-ordination of hydroxide.
以[Nb6Cl12]2+为水合羟基的三种新化合物的合成及结构表征
建立了从碱性溶液中制备三种不同水合氯铌簇氢氧化物的条件:三斜[Nb6Cl12(OH)2(H2O)4]·4H2O 1和两种结构不确定的立方化合物:Nb6Cl12(OH)2(H2O)142和Nb6Cl12(H2O)14(OMe)23。根据结构数据2和3可能含有阳离子[Nb6Cl12(H2O)6]2+或含有羟基配体的中性簇[Nb6Cl12(OH)2(H2O)4]。Nb-OH和Nb-OH2分别在2.147(5)和2.250(5)和2.289(5)A的不同距离上被发现。在2和3中,发现配位水(或氢氧根-水平均)的Nb-O键的距离分别为2.19(1)和2.193(7)A。化合物1为三斜体,空间群P1, a= 8.930(3), b= 9.195(2), c= 9.118(1) a, α= 104.37(2), β= 99.51(2), γ= 116.99(2)°,U= 611.9(3)A3, Z= 1, R= 1, R= 0.036。化合物2为立方,空间群为Fm3m, a= 14.59(2) a, U= 3105.7(1)A3, Z= 4, R= 0.028。化合物3也是立方,空间群为Fm3m, a= 14.627(1) a, U= 3129.3(1)A3, Z= 4, R= 0.031。1的红外光谱显示出强的O-H和Nb-O拉伸带,反映了配位OH -基团的存在。在2和3中,红外光谱对氢氧化物可能的配位不太确定。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
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