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首页> 外文期刊>Zeitschrift fur Anorganische und Allgemeine Chemie >TWO NEW CYCLIC THIOANIONS - (PPH4)(2)[1,3-P2S8] AND (PPH4)(2)[SI2S6CL2] - NEW SYNTHETIC ACCESS ROUTES TO PPH4[PS2CL2] AND PPH4[PS2BR2] [German]
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TWO NEW CYCLIC THIOANIONS - (PPH4)(2)[1,3-P2S8] AND (PPH4)(2)[SI2S6CL2] - NEW SYNTHETIC ACCESS ROUTES TO PPH4[PS2CL2] AND PPH4[PS2BR2] [German]

机译:两种新型环硫酮-(PPH4)(2)[1,3-P2S8]和(PPH4)(2)[SI2S6CL2]-PPH4 [PS2CL2]和PPH4 [PS2BR2]的新合成途径[德语]

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摘要

(PPh4)(2)[P2S8] was obtained from tetraphenylphosphonium polysulfide and white phosphorus in acetonitrile. According to its X-ray crystal structure analysis (4229 reflexions, R=0.079) the P2S82- ion consists of a six-membered ring in chair conformation made up from four sulfur and two phosphorus atoms in 1,3 positions; in addition, each P atom has two terminal sulfur atoms. (PPh4)(2)[Si2S6Cl2]. 2CH(2)Cl(2) was obtained from Na2S4, PPh4Cl and SiCl4 in dichloromethane. The Si2S6Cl22- ion also has a six-membered ring structure, consisting of four sulfur and two silicon atoms in 1,4 positions (X-ray structure analysis, 2694 reflexions, R=0.032). PPh4[PS2Cl2] is accessible by the following reactions: 1. P4S3+PPh4Cl+chlorine in CH2Cl2; 2. PSCl3+Na2S4+PPh4Cl in CH2Cl2; 3. PCl5+Na2S4+PPh4Cl in acetonitrile; 4. PCl3+Na2S4+PPh4Cl in acetonitrile; 5. P4S10+Na2S4+PPh4Cl in acetonitrile. P4S3 or P4S10 react with PPh4Cl and bromine to yield PPh4[PS2Br2]. PPh4[PS2Cl2] crystallizes isotypic to PPh4[PS2Br2] in the BiPh4[ClO4] structure type with orientational disorder of the PS2Cl2- ions in positions with site symmetry (4) over bar. [References: 28]
机译:(PPh4)(2)[P2S8]是由多硫化四苯基and和白磷在乙腈中制得的。根据其X射线晶体结构分析(4229反射,R = 0.079),P2S82-离子由六面环构象环组成,该环由1,3位的四个硫和两个磷原子组成;另外,每个P原子具有两个末端硫原子。 (PPh4)(2)[Si2S6Cl2]。从二氯甲烷中的Na2S4,PPh4Cl和SiCl4获得2CH(2)Cl(2)。 Si 2 S 6 Cl 22-离子还具有六元环结构,由位于1,4位的四个硫和两个硅原子组成(X射线结构分析,2694反射,R = 0.032)。 PPh4 [PS2Cl2]可通过以下反应获得:1. P4S3 + PPh4Cl +氯的CH2Cl2中; 2.在CH 2 Cl 2中的PSCl 3 + Na 2 S 4 + PPh 4 Cl; 3. PCl5 + Na2S4 + PPh4Cl的乙腈溶液; 4. PCl3 + Na2S4 + PPh4Cl的乙腈溶液; 5.乙腈中的P4S10 + Na2S4 + PPh4Cl。 P4S3或P4S10与PPh4Cl和溴反应生成PPh4 [PS2Br2]。 PPh4 [PS2Cl2]结晶成BiPh4 [ClO4]结构类型的PPh4 [PS2Br2]同型,在棒上具有位置对称性(4)的位置中PS2Cl2-离子取向紊乱。 [参考:28]

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