Syntheses, Spectra, and Structures of (Diphosphine)platinum(II) Carbonate Complexes.
Syntheses, Spectra, and Structures of (Diphosphine)platinum(II) Carbonate Complexes.
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DOI：
10.1021/ic9603159
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发表时间：
1996-09
影响因子：
4.6
通讯作者：
M. A. Andrews;G. Gould;W. Klooster;Kristina S. Koenig;E. J. Voss
中科院分区：
文献类型：
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作者：
M. A. Andrews;G. Gould;W. Klooster;Kristina S. Koenig;E. J. Voss
在有水存在的情况下，用碳酸银在二氯甲烷溶液中处理相应的（二膦）铂（II）碳酸配合物（LL）Pt（CO(3)）可以很容易地制得各种（二膦）铂（II）碳酸配合物（LL）Pt（CO(3)）。该反应还允许易于制备类似的（13）c标记配合物。用红外光谱和（13）C核磁共振光谱对这些配合物中的碳酸盐配体进行了表征。备选的制备路线包括将前驱物二氯化物转化为相应的二氧化物或二苯氧化物，然后用水和二氧化碳处理。在后一种合成中，各种反应中间体已被光谱观察到。用单晶x射线衍射研究了(Ph(2)PCH(2)CH(2)CH(2)PPh(2) Pt（CO(3)）的两种结晶修饰，一种是有二氯甲烷溶剂化，另一种是无二氯甲烷溶剂化。PtP(2)O(3)C(28)H（26）的晶体数据：P2(1)/ C, Z = 4, T = 200 K, a = 10.362(8) Å， b = 14.743(6) Å， C = 19.183（10） Å， β = 122.69(6)度。PtP(2)O(3)C(28)H（26）的晶体数据。CH(2)Cl(2): P2(1)/c, Z = 4， T约298 K， a = 11.744(2) Å， b = 15.526(3) Å， c = 15.866(3) Å， β = 101.58(1)度。
A variety of (diphosphine)platinum(II) carbonate complexes, (LL)Pt(CO(3)), are readily prepared from the corresponding (diphosphine)platinum dichlorides by treatment with silver carbonate in dichoromethane solution provided that water is present. This reaction also permits facile preparation of analogous (13)C-labeled complexes. The carbonate ligands in these complexes have been characterized by IR and (13)C NMR spectroscopy. Alternative preparative routes involve conversion of the precursor dichlorides to the corresponding dialkoxides or diphenoxides, followed by treatment with water and carbon dioxide. Various reaction intermediates have been spectroscopically observed in the latter syntheses. Two crystalline modifications of (Ph(2)PCH(2)CH(2)CH(2)PPh(2))Pt(CO(3)), one with and one without a dichloromethane of solvation, have been studied by single-crystal X-ray diffraction. Crystal data for PtP(2)O(3)C(28)H(26): P2(1)/c, Z = 4, T = 200 K, a = 10.362(8) Å, b = 14.743(6) Å, c = 19.183(10) Å, beta = 122.69(6) degrees. Crystal data for PtP(2)O(3)C(28)H(26).CH(2)Cl(2): P2(1)/c, Z = 4, T approximately 298 K, a = 11.744(2) Å, b = 15.526(3) Å, c = 15.866(3) Å, beta = 101.58(1) degrees.