DISCRETE TRIGONAL-PYRAMIDAL LEAD(II) COMPLEXES - SYNTHESES AND X-RAY STRUCTURE ANALYSES OF [(C6H5)4AS][PB(SC6H5)3] [(C6H5)4AS][PB(SEC6H5)3]
DISCRETE TRIGONAL-PYRAMIDAL LEAD(II) COMPLEXES - SYNTHESES AND X-RAY STRUCTURE ANALYSES OF [(C6H5)4AS][PB(SC6H5)3] [(C6H5)4AS][PB(SEC6H5)3]
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DOI：
10.1021/ic00193a027
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发表时间：
1984-01-01
影响因子：
4.6
通讯作者：
PAYNE, NC
中科院分区：
文献类型：
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作者：
DEAN, PAW;VITTAL, JJ;PAYNE, NC
(1)A，对于2，用全矩阵最小二乘法对F进行修正，使结构符合因子R=0.026(用F0>；2o(F0))和R=0.034(用Fa>；3a(F0))。离散的[Pb(EC_6H_5)_3]“阴离子是同构的；三个S或Se原子形成一个三角金字塔的底部，顶端被铅原子占据。化合物1的铅-S距离分别为2.619(1)、2.647(1)和2.623(1)A，而化合物2的铅-硒距离分别为2.762(1)、2.727(1)和2.733(1)。这些盐代表了三配位铅(II)的三角-锥体配位几何构型的第一个明确的例子。铅-207核磁共振谱证实了[Pb(EC6H5)3]“离子是最近在溶液中原位合成的阴离子铅(II)物种。
(1) A, and ß= 105.84 (1) for 2. The structures havebeen refined by full-matrix least-squares techniques on F to agreement factors R= 0.026 (4866 observations with F0> 2o (F0)) for 1 and R= 0.034 (3074 observations with Fa> 3a (F0)) for 2. The discrete [Pb (EC6H5) 3]" anions are isostructural; the three S or Se atoms form the base of a trigonal pyramid whose apex is occupied by the Pb atom. The Pb-S distances in 1 are 2.619 (1), 2.647 (1), and 2.623 (1) A, while in 2 the Pb-Se distances are 2.762 (1), 2.727 (1), and 2.733 (1) A. Angles at the Pb atom range from 90.32 (4) to 96.14 (5) in 1 and from 88.82 (4) to 96.57 (4) in 2. In both anions all three phenyl groups adopt a propeller-like conformation and are disposed in equatorial positions above the basal plane of chalcogen atoms. These salts represent the first unambiguous examples of the trigonal-pyramidal coordination geometryexpected for isolated three-coordinated Pb (II). Lead-207 NMR spectra confirm that the [Pb (EC6H5) 3]" ions are the anionic lead (II) species recently prepared in situ in solution.