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Title: Synthesis and characterization of rhenium phosphinothiolate complexes. Crystal and molecular structures of [HNEt{sub 3}][Re{l_brace}P(C{sub 6}H{sub 4}S){sub 3}{r_brace}{sub 2}], [ReOCl{l_brace}OP(C{sub 6}H{sub 5}){sub 2}(C{sub 6}H{sub 4}S){r_brace}{l_brace}P(C{sub 6}H{sub 5}){sub 2}(C{sub 6}H{sub 4}S){r_brace}], [Re{sub 2}O{sub 5}{l_brace}P(C{sub 6}H{sub 5}){sub 2}(C{sub 6}H{sub 4}S){r_brace}{sub 2}], and [ReOCl{l_brace}OP(C{sub 6}H{sub 5}){sub 2}(2-SC{sub 6}H{sub 3}-3-SiMe{sup 3}){r_brace}{sub 2}]

Abstract

The reactions of ammonium perrhenate, HCl(aq), and the phosphinothiol ligands (2-HSC{sub 6}H{sub 4})P(C{sub 6}H{sub 4}X){sub 2}, where X = H or SH [abbreviated P-(SH){sub x} (x = 1, 3)], in alcohol have led to the isolation of a series of rhenium complexes containing the [M(P{minus}S{sub x}){sub 2}] core, represented by [Re[P(C{sub 6}H{sub 4}S){sub 3}] [P(C{sub 6}H{sub 4}S){sub 2}(C{sub 6}H{sub 4}SH)]] (1), [ReOCl-[OP(C{sub 6}H{sub 5}){sub 2}(C{sub 6}H{sub 4}S)][P(C{sub 6}H{sub 5}){sub 2}(C{sub 6}H{sub 4}S)]] (3), and [ReOCl[OP(C{sub 6}H{sub 5}){sub 2}(2-SC{sub 6}H{sub 3}-3-SiMe{sub 3})]{sub 2}] (5). The reaction of 1 with NEt{sub 3}results in the formation of [HNEt{sub 3}][Re[P(C{sub 6}H{sub 4}S){sub 3}]{sub 2}] (2) by deprotonation of a thiol ligand. The reaction of ammonium perrhenate with P-(SH) also led to the isolation of the binuclear species [ReOCl[OP(C{sub 6}H{sub 5}){sub 2}(2-SC{sub 6}H{sub 3}-3-SiMe{sub 3})]{sub 2}] (4). Crystal data are given.

Authors:
; ; ;  [1]; ; ;  [2]
  1. Univ. de Santiago de Compostela, Santiago (Spain). Dept. de Quimica Inorganica
  2. Syracuse Univ., NY (United States). Dept. of Chemistry
Publication Date:
OSTI Identifier:
642402
Resource Type:
Journal Article
Journal Name:
Inorganic Chemistry
Additional Journal Information:
Journal Volume: 37; Journal Issue: 13; Other Information: PBD: 29 Jun 1998
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE; 55 BIOLOGY AND MEDICINE, BASIC STUDIES; RHENIUM COMPLEXES; CRYSTAL STRUCTURE; MOLECULAR STRUCTURE; RADIOPHARMACEUTICALS; RHENIUM 186; RHENIUM 188; THIOLS; CHEMICAL PREPARATION; EXPERIMENTAL DATA

Citation Formats

Perez-Lourido, P., Romero, J., Garcia-Vazquez, J., Sousa, A., Maresca, K.P., Rose, D.J., and Zubieta, J. Synthesis and characterization of rhenium phosphinothiolate complexes. Crystal and molecular structures of [HNEt{sub 3}][Re{l_brace}P(C{sub 6}H{sub 4}S){sub 3}{r_brace}{sub 2}], [ReOCl{l_brace}OP(C{sub 6}H{sub 5}){sub 2}(C{sub 6}H{sub 4}S){r_brace}{l_brace}P(C{sub 6}H{sub 5}){sub 2}(C{sub 6}H{sub 4}S){r_brace}], [Re{sub 2}O{sub 5}{l_brace}P(C{sub 6}H{sub 5}){sub 2}(C{sub 6}H{sub 4}S){r_brace}{sub 2}], and [ReOCl{l_brace}OP(C{sub 6}H{sub 5}){sub 2}(2-SC{sub 6}H{sub 3}-3-SiMe{sup 3}){r_brace}{sub 2}]. United States: N. p., 1998. Web. doi:10.1021/ic9715299.
Perez-Lourido, P., Romero, J., Garcia-Vazquez, J., Sousa, A., Maresca, K.P., Rose, D.J., & Zubieta, J. Synthesis and characterization of rhenium phosphinothiolate complexes. Crystal and molecular structures of [HNEt{sub 3}][Re{l_brace}P(C{sub 6}H{sub 4}S){sub 3}{r_brace}{sub 2}], [ReOCl{l_brace}OP(C{sub 6}H{sub 5}){sub 2}(C{sub 6}H{sub 4}S){r_brace}{l_brace}P(C{sub 6}H{sub 5}){sub 2}(C{sub 6}H{sub 4}S){r_brace}], [Re{sub 2}O{sub 5}{l_brace}P(C{sub 6}H{sub 5}){sub 2}(C{sub 6}H{sub 4}S){r_brace}{sub 2}], and [ReOCl{l_brace}OP(C{sub 6}H{sub 5}){sub 2}(2-SC{sub 6}H{sub 3}-3-SiMe{sup 3}){r_brace}{sub 2}]. United States. doi:10.1021/ic9715299.
Perez-Lourido, P., Romero, J., Garcia-Vazquez, J., Sousa, A., Maresca, K.P., Rose, D.J., and Zubieta, J. Mon . "Synthesis and characterization of rhenium phosphinothiolate complexes. Crystal and molecular structures of [HNEt{sub 3}][Re{l_brace}P(C{sub 6}H{sub 4}S){sub 3}{r_brace}{sub 2}], [ReOCl{l_brace}OP(C{sub 6}H{sub 5}){sub 2}(C{sub 6}H{sub 4}S){r_brace}{l_brace}P(C{sub 6}H{sub 5}){sub 2}(C{sub 6}H{sub 4}S){r_brace}], [Re{sub 2}O{sub 5}{l_brace}P(C{sub 6}H{sub 5}){sub 2}(C{sub 6}H{sub 4}S){r_brace}{sub 2}], and [ReOCl{l_brace}OP(C{sub 6}H{sub 5}){sub 2}(2-SC{sub 6}H{sub 3}-3-SiMe{sup 3}){r_brace}{sub 2}]". United States. doi:10.1021/ic9715299.
@article{osti_642402,
title = {Synthesis and characterization of rhenium phosphinothiolate complexes. Crystal and molecular structures of [HNEt{sub 3}][Re{l_brace}P(C{sub 6}H{sub 4}S){sub 3}{r_brace}{sub 2}], [ReOCl{l_brace}OP(C{sub 6}H{sub 5}){sub 2}(C{sub 6}H{sub 4}S){r_brace}{l_brace}P(C{sub 6}H{sub 5}){sub 2}(C{sub 6}H{sub 4}S){r_brace}], [Re{sub 2}O{sub 5}{l_brace}P(C{sub 6}H{sub 5}){sub 2}(C{sub 6}H{sub 4}S){r_brace}{sub 2}], and [ReOCl{l_brace}OP(C{sub 6}H{sub 5}){sub 2}(2-SC{sub 6}H{sub 3}-3-SiMe{sup 3}){r_brace}{sub 2}]},
author = {Perez-Lourido, P. and Romero, J. and Garcia-Vazquez, J. and Sousa, A. and Maresca, K.P. and Rose, D.J. and Zubieta, J.},
abstractNote = {The reactions of ammonium perrhenate, HCl(aq), and the phosphinothiol ligands (2-HSC{sub 6}H{sub 4})P(C{sub 6}H{sub 4}X){sub 2}, where X = H or SH [abbreviated P-(SH){sub x} (x = 1, 3)], in alcohol have led to the isolation of a series of rhenium complexes containing the [M(P{minus}S{sub x}){sub 2}] core, represented by [Re[P(C{sub 6}H{sub 4}S){sub 3}] [P(C{sub 6}H{sub 4}S){sub 2}(C{sub 6}H{sub 4}SH)]] (1), [ReOCl-[OP(C{sub 6}H{sub 5}){sub 2}(C{sub 6}H{sub 4}S)][P(C{sub 6}H{sub 5}){sub 2}(C{sub 6}H{sub 4}S)]] (3), and [ReOCl[OP(C{sub 6}H{sub 5}){sub 2}(2-SC{sub 6}H{sub 3}-3-SiMe{sub 3})]{sub 2}] (5). The reaction of 1 with NEt{sub 3}results in the formation of [HNEt{sub 3}][Re[P(C{sub 6}H{sub 4}S){sub 3}]{sub 2}] (2) by deprotonation of a thiol ligand. The reaction of ammonium perrhenate with P-(SH) also led to the isolation of the binuclear species [ReOCl[OP(C{sub 6}H{sub 5}){sub 2}(2-SC{sub 6}H{sub 3}-3-SiMe{sub 3})]{sub 2}] (4). Crystal data are given.},
doi = {10.1021/ic9715299},
journal = {Inorganic Chemistry},
number = 13,
volume = 37,
place = {United States},
year = {1998},
month = {6}
}