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首页> 外文期刊>Polyhedron: The International Journal for Inorganic and Organometallic Chemistry >Synthesis, characterization and structural comparisons of phosphonium and arsenic dithiocarbamates with alkyl and phenyl substituents
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Synthesis, characterization and structural comparisons of phosphonium and arsenic dithiocarbamates with alkyl and phenyl substituents

机译：具有烷基和苯基取代基的phospho和二硫代氨基甲酸砷酯的合成，表征和结构比较

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摘要

The synthesis and characterization of the new arsenic dithiocarbamate complex As[S_2CNPh_2]_3 and three new phosphonium dithiocarbamates [PPh_4][S_2CNR_2], where R_2 = Et_2, (CH_2)_5 and Ph_2, are reported. As[S_2CNPh_2]_3 was prepared by treating AsI_3 with three equivalents of NaS_2CNPh_2 in a 2:1 mixture of H_2O and EtOH. The precipitate that formed was recrystallized from hot toluene to yield yellow prisms of As[S_2CNPh_2]_3 suitable for single-crystal X-ray diffraction (XRD). Attempts to prepare the known compound As[S_2CN(CH_2)_5]_3 using a similar route resulted in a mixture of As[S_2CN(CH_2)_5]_3 and the mixed iodide species As[S_2CN(CH_2)_5]_2I. Single-crystals of both compounds were isolated from concentrated Et_2O/CHCl_3 solutions and their structures are described here for the first time. [PPh_4][S_2CNR_2] salts were prepared for comparison to arsenic dithiocarbamates by metathesis reactions with PPh_4Br and NaS_2CNR_2 in acetonitrile. All three salts could be obtained in high-purity from MeCN/Et_2O solutions and crystal structures of [PPh_4][S_2CNEt_2] and [PPh_4][S_2CN(CH_2)_5] reveal charge-separated phosphonium cations and dithiocarbamate anions. The five new crystal structures are used to compare dithiocarbamate bond distances and angles in the presence and absence of arsenic. Nuclear magnetic resonance (NMR) spectra, infrared (IR) spectra, microanalyses, and melting points of the compounds are reported.
机译：报道了新的二硫代氨基甲酸砷配合物As [S_2CNPh_2] _3和三种新的二硫代氨基甲酸phospho [PPh_4] [S_2CNR_2]的合成和表征，其中R_2 = Et_2，（CH_2）_5和Ph_2。通过在H_2O和EtOH的2：1混合物中用三当量的NaS_2CNPh_2处理AsI_3来制备As [S_2CNPh_2] _3。将形成的沉淀物从热甲苯中重结晶，以生成适合于单晶X射线衍射（XRD）的As [S_2CNPh_2] _3的黄色棱镜。尝试使用相似的路线制备已知化合物As [S_2CN（CH_2）_5] _3导致As [S_2CN（CH_2）_5] _3和混合碘化物As [S_2CN（CH_2）_5] _2I的混合物。从浓Et_2O / CHCl_3溶液中分离出这两种化合物的单晶，并在此首次描述其结构。制备了[PPh_4] [S_2CNR_2]盐，用于通过与PPh_4Br和NaS_2CNR_2在乙腈中的复分解反应与二硫代氨基甲酸砷进行比较。可以从MeCN / Et_2O溶液中高纯度地获得所有三种盐，[PPh_4] [S_2CNEt_2]和[PPh_4] [S_2CN（CH_2）_5]的晶体结构揭示了电荷分离的phospho阳离子和二硫代氨基甲酸酯阴离子。这五个新的晶体结构用于比较在存在和不存在砷的情况下二硫代氨基甲酸酯键的距离和角度。报告了化合物的核磁共振（NMR）光谱，红外（IR）光谱，微量分析和熔点。

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