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Title: Synthesis and characterization of rhenium thiolate complexes. Crystal and molecular structures of [NBu{sub 4}][ReO(H{sub 2}O)Br{sub 4}]{center_dot}2H{sub 2}O, [Bu{sub 4}N][ReOBr{sub 4}(OPPh{sub 3})], [ReO(SC{sub 5}H{sub 4}N){sub 3}], [ReO(SC{sub 4}H{sub 3}N{sub 2}){sub 3}][ReO(OH)(SC{sub 5}H{sub 4}N-3,6-(SiMe{sub 2}Bu{sup t}){sub 2}){sub 2}], [Re(N{sub 2}COC{sub 6}H{sub 5})(SC{sub 5}H{sub 4}N)Cl(PPh{sub 3}){sub 2}], and [Re(PPh{sub 3})(SC{sub 4}H{sub 3}N{sub 2}){sub 3}]

Abstract

The syntheses and characterization of six monomeric rhenium thiolate complexes and the structural characterization of two useful rhenium starting materials are presented. Pyridine-2-thiol (2), 3,6-bis(dimethyl-tert-butylsilyl)pyridine-2-thiol (3), and pyrimidine-2-thiol (4) were reacted with [Bu{sub 4}N][ReOBr{sub 4}(H{sub 2}O)]{center_dot}2H{sub 2}O (5), [Bu{sub 4}N][ReOBr{sub 4}(OPPh{sub 3})] (6), [ReO{sub 2}(C{sub 5}H{sub 5}N){sub 4}], and [Re(N{sub 2}CO(C{sub 6}H{sub 5}))Cl{sub 2}(PPh{sub 3}){sub 2}] to give [ReO(C{sub 5}H{sub 4}NS){sub 3}] (7), [ReO(C{sub 8}H{sub 12}NSiS){sub 3}] (8), [ReO(OH)(C{sub 11}H{sub 20}NSi{sub 2}S){sub 2}] (9), [Re(N{sub 2}-CO(C{sub 6}H{sub 5}))Cl(PPh{sub 3}){sub 2}(C{sub 5}H{sub 4}NS)] (10), [ReO(C{sub 4}H{sub 3}N{sub 2}S){sub 3}] (11), and [Re(P(C{sub 6}H{sub 5}){sub 3})(C{sub 4}H{sub 3}N{sub 2}S){sub 3}] (12). Crystal structures are reported for the compounds.

Authors:
; ;  [1]
  1. Syracuse Univ., NY (United States) [and others
Publication Date:
OSTI Identifier:
477556
Resource Type:
Journal Article
Journal Name:
Inorganic Chemistry
Additional Journal Information:
Journal Volume: 35; Journal Issue: 12; Other Information: PBD: 5 Jun 1996
Country of Publication:
United States
Language:
English
Subject:
40 CHEMISTRY; RHENIUM COMPLEXES; CRYSTAL STRUCTURE; CHEMICAL PREPARATION; MOLECULAR STRUCTURE; MONOCLINIC LATTICES; TRICLINIC LATTICES; ORTHORHOMBIC LATTICES

Citation Formats

Rose, D.J., Maresca, K.P., and Kettler, P.B. Synthesis and characterization of rhenium thiolate complexes. Crystal and molecular structures of [NBu{sub 4}][ReO(H{sub 2}O)Br{sub 4}]{center_dot}2H{sub 2}O, [Bu{sub 4}N][ReOBr{sub 4}(OPPh{sub 3})], [ReO(SC{sub 5}H{sub 4}N){sub 3}], [ReO(SC{sub 4}H{sub 3}N{sub 2}){sub 3}][ReO(OH)(SC{sub 5}H{sub 4}N-3,6-(SiMe{sub 2}Bu{sup t}){sub 2}){sub 2}], [Re(N{sub 2}COC{sub 6}H{sub 5})(SC{sub 5}H{sub 4}N)Cl(PPh{sub 3}){sub 2}], and [Re(PPh{sub 3})(SC{sub 4}H{sub 3}N{sub 2}){sub 3}]. United States: N. p., 1996. Web. doi:10.1021/ic950881o.
Rose, D.J., Maresca, K.P., & Kettler, P.B. Synthesis and characterization of rhenium thiolate complexes. Crystal and molecular structures of [NBu{sub 4}][ReO(H{sub 2}O)Br{sub 4}]{center_dot}2H{sub 2}O, [Bu{sub 4}N][ReOBr{sub 4}(OPPh{sub 3})], [ReO(SC{sub 5}H{sub 4}N){sub 3}], [ReO(SC{sub 4}H{sub 3}N{sub 2}){sub 3}][ReO(OH)(SC{sub 5}H{sub 4}N-3,6-(SiMe{sub 2}Bu{sup t}){sub 2}){sub 2}], [Re(N{sub 2}COC{sub 6}H{sub 5})(SC{sub 5}H{sub 4}N)Cl(PPh{sub 3}){sub 2}], and [Re(PPh{sub 3})(SC{sub 4}H{sub 3}N{sub 2}){sub 3}]. United States. doi:10.1021/ic950881o.
Rose, D.J., Maresca, K.P., and Kettler, P.B. Wed . "Synthesis and characterization of rhenium thiolate complexes. Crystal and molecular structures of [NBu{sub 4}][ReO(H{sub 2}O)Br{sub 4}]{center_dot}2H{sub 2}O, [Bu{sub 4}N][ReOBr{sub 4}(OPPh{sub 3})], [ReO(SC{sub 5}H{sub 4}N){sub 3}], [ReO(SC{sub 4}H{sub 3}N{sub 2}){sub 3}][ReO(OH)(SC{sub 5}H{sub 4}N-3,6-(SiMe{sub 2}Bu{sup t}){sub 2}){sub 2}], [Re(N{sub 2}COC{sub 6}H{sub 5})(SC{sub 5}H{sub 4}N)Cl(PPh{sub 3}){sub 2}], and [Re(PPh{sub 3})(SC{sub 4}H{sub 3}N{sub 2}){sub 3}]". United States. doi:10.1021/ic950881o.
@article{osti_477556,
title = {Synthesis and characterization of rhenium thiolate complexes. Crystal and molecular structures of [NBu{sub 4}][ReO(H{sub 2}O)Br{sub 4}]{center_dot}2H{sub 2}O, [Bu{sub 4}N][ReOBr{sub 4}(OPPh{sub 3})], [ReO(SC{sub 5}H{sub 4}N){sub 3}], [ReO(SC{sub 4}H{sub 3}N{sub 2}){sub 3}][ReO(OH)(SC{sub 5}H{sub 4}N-3,6-(SiMe{sub 2}Bu{sup t}){sub 2}){sub 2}], [Re(N{sub 2}COC{sub 6}H{sub 5})(SC{sub 5}H{sub 4}N)Cl(PPh{sub 3}){sub 2}], and [Re(PPh{sub 3})(SC{sub 4}H{sub 3}N{sub 2}){sub 3}]},
author = {Rose, D.J. and Maresca, K.P. and Kettler, P.B.},
abstractNote = {The syntheses and characterization of six monomeric rhenium thiolate complexes and the structural characterization of two useful rhenium starting materials are presented. Pyridine-2-thiol (2), 3,6-bis(dimethyl-tert-butylsilyl)pyridine-2-thiol (3), and pyrimidine-2-thiol (4) were reacted with [Bu{sub 4}N][ReOBr{sub 4}(H{sub 2}O)]{center_dot}2H{sub 2}O (5), [Bu{sub 4}N][ReOBr{sub 4}(OPPh{sub 3})] (6), [ReO{sub 2}(C{sub 5}H{sub 5}N){sub 4}], and [Re(N{sub 2}CO(C{sub 6}H{sub 5}))Cl{sub 2}(PPh{sub 3}){sub 2}] to give [ReO(C{sub 5}H{sub 4}NS){sub 3}] (7), [ReO(C{sub 8}H{sub 12}NSiS){sub 3}] (8), [ReO(OH)(C{sub 11}H{sub 20}NSi{sub 2}S){sub 2}] (9), [Re(N{sub 2}-CO(C{sub 6}H{sub 5}))Cl(PPh{sub 3}){sub 2}(C{sub 5}H{sub 4}NS)] (10), [ReO(C{sub 4}H{sub 3}N{sub 2}S){sub 3}] (11), and [Re(P(C{sub 6}H{sub 5}){sub 3})(C{sub 4}H{sub 3}N{sub 2}S){sub 3}] (12). Crystal structures are reported for the compounds.},
doi = {10.1021/ic950881o},
journal = {Inorganic Chemistry},
number = 12,
volume = 35,
place = {United States},
year = {1996},
month = {6}
}