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Title: Synthesis and characterization of rhenium(III) organohydrazide compounds. Crystal and molecular structures of [ReCl(PPh{sub 3}){sub 2}(NHNC{sub 5}H{sub 4}N)(HNNC{sub 5}H{sub 4}N)]Cl{sub 2}, [Re{l_brace}2-(Ph{sub 2}P)C{sub 6}H{sub 4}S{r_brace}{l_brace}2-(Ph{sub 2}PO)C{sub 6}H{sub 4}S{r_brace}(NNC{sub 5}H{sub 4}N)(HNNC{sub 5}H{sub 4}N)], and [Re{l_brace}2-(Ph{sub 2}P)C{sub 6}H{sub 4}S{r_brace}{sub 2}(NNC{sub 5}H{sub 4}N)]

Abstract

The reduction of ReO{sub 4}{sup {minus}} with 2-hydrazinopyridine dihydrochloride and PPh{sub 3} gives [ReCl(PPh{sub 3}){sub 2}(NHNC{sub 5}H{sub 4}N)-(HNNC{sub 5}H{sub 4}N)]Cl{sub 2} (2). A similar reaction using 2-hydrazino-2-imidazoline and PPh{sub 3} in methanol hydrochloric acid allows the preparation of [ReCl{sub 3}(PPh{sub 3}){sub 2}(NNC{sub 3}H{sub 4}N{sub 2})] (3). The reaction of the Re(III) complex [ReCl{sub 3}(NNC{sub 5}H{sub 4}NH)(HNNC{sub 5}H{sub 4}N)] (1), with 2-(Ph{sub 2}P)C{sub 6}H{sub 4}SH in methanol yields [Re{l_brace}2-(Ph{sub 2}P)C{sub 6}H{sub 4}S{r_brace}-{l_brace}2-(Ph{sub 2}PO)C{sub 6}H{sub 4}S{r_brace}(NNC{sub 5}H{sub 4}N)(HNNC{sub 5}H{sub 4}N)] (4) and [Re{l_brace}2-(Ph{sub 2}P)C{sub 6}H{sub 4}S{r_brace}{sub 2}(NNC{sub 5}H{sub 4}N)] (5). The same precursor with 2-(Ph{sub 2}PO)-6-(Me{sub 3}Si)C{sub 6}H{sub 3}SH gives [ReCl{l_brace}2-(Ph{sub 2}PO)-6-(Me{sub 3}Si)C{sub 6}H{sub 3}S{r_brace}(NNC{sub 5}H{sub 4}N)(HNNC{sub 5}H{sub 4}N)] (6) and with PhP(C{sub 6}H{sub 4}SH-2){sub 2} yields [Re{l_brace}PhP(C{sub 6}H{sub 4}S-2){sub 2}{r_brace}(NNC{sub 5}H{sub 4}N)(HNNC{sub 5}H{sub 4}N)] (7).

Authors:
; ; ;  [1]; ;  [2]
  1. Univ. de Santiago de Compostela (Spain). Dept. de Quimica Inorganica
  2. Syracuse Univ., NY (United States). Dept. of Chemistry
Publication Date:
Sponsoring Org.:
USDOE, Washington, DC (United States)
OSTI Identifier:
343687
Resource Type:
Journal Article
Journal Name:
Inorganic Chemistry
Additional Journal Information:
Journal Volume: 38; Journal Issue: 7; Other Information: PBD: 5 Apr 1999
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE; 55 BIOLOGY AND MEDICINE, BASIC STUDIES; RHENIUM COMPOUNDS; HYDRAZIDES; CRYSTAL STRUCTURE; MOLECULAR STRUCTURE; RADIOPHARMACEUTICALS; SYNTHESIS

Citation Formats

Perez-Lourido, P., Romero, J., Garcia-Vazquez, J.A., Sousa, A., Maresca, K.P., and Zubieta, J. Synthesis and characterization of rhenium(III) organohydrazide compounds. Crystal and molecular structures of [ReCl(PPh{sub 3}){sub 2}(NHNC{sub 5}H{sub 4}N)(HNNC{sub 5}H{sub 4}N)]Cl{sub 2}, [Re{l_brace}2-(Ph{sub 2}P)C{sub 6}H{sub 4}S{r_brace}{l_brace}2-(Ph{sub 2}PO)C{sub 6}H{sub 4}S{r_brace}(NNC{sub 5}H{sub 4}N)(HNNC{sub 5}H{sub 4}N)], and [Re{l_brace}2-(Ph{sub 2}P)C{sub 6}H{sub 4}S{r_brace}{sub 2}(NNC{sub 5}H{sub 4}N)]. United States: N. p., 1999. Web. doi:10.1021/ic980953m.
Perez-Lourido, P., Romero, J., Garcia-Vazquez, J.A., Sousa, A., Maresca, K.P., & Zubieta, J. Synthesis and characterization of rhenium(III) organohydrazide compounds. Crystal and molecular structures of [ReCl(PPh{sub 3}){sub 2}(NHNC{sub 5}H{sub 4}N)(HNNC{sub 5}H{sub 4}N)]Cl{sub 2}, [Re{l_brace}2-(Ph{sub 2}P)C{sub 6}H{sub 4}S{r_brace}{l_brace}2-(Ph{sub 2}PO)C{sub 6}H{sub 4}S{r_brace}(NNC{sub 5}H{sub 4}N)(HNNC{sub 5}H{sub 4}N)], and [Re{l_brace}2-(Ph{sub 2}P)C{sub 6}H{sub 4}S{r_brace}{sub 2}(NNC{sub 5}H{sub 4}N)]. United States. doi:10.1021/ic980953m.
Perez-Lourido, P., Romero, J., Garcia-Vazquez, J.A., Sousa, A., Maresca, K.P., and Zubieta, J. Mon . "Synthesis and characterization of rhenium(III) organohydrazide compounds. Crystal and molecular structures of [ReCl(PPh{sub 3}){sub 2}(NHNC{sub 5}H{sub 4}N)(HNNC{sub 5}H{sub 4}N)]Cl{sub 2}, [Re{l_brace}2-(Ph{sub 2}P)C{sub 6}H{sub 4}S{r_brace}{l_brace}2-(Ph{sub 2}PO)C{sub 6}H{sub 4}S{r_brace}(NNC{sub 5}H{sub 4}N)(HNNC{sub 5}H{sub 4}N)], and [Re{l_brace}2-(Ph{sub 2}P)C{sub 6}H{sub 4}S{r_brace}{sub 2}(NNC{sub 5}H{sub 4}N)]". United States. doi:10.1021/ic980953m.
@article{osti_343687,
title = {Synthesis and characterization of rhenium(III) organohydrazide compounds. Crystal and molecular structures of [ReCl(PPh{sub 3}){sub 2}(NHNC{sub 5}H{sub 4}N)(HNNC{sub 5}H{sub 4}N)]Cl{sub 2}, [Re{l_brace}2-(Ph{sub 2}P)C{sub 6}H{sub 4}S{r_brace}{l_brace}2-(Ph{sub 2}PO)C{sub 6}H{sub 4}S{r_brace}(NNC{sub 5}H{sub 4}N)(HNNC{sub 5}H{sub 4}N)], and [Re{l_brace}2-(Ph{sub 2}P)C{sub 6}H{sub 4}S{r_brace}{sub 2}(NNC{sub 5}H{sub 4}N)]},
author = {Perez-Lourido, P. and Romero, J. and Garcia-Vazquez, J.A. and Sousa, A. and Maresca, K.P. and Zubieta, J.},
abstractNote = {The reduction of ReO{sub 4}{sup {minus}} with 2-hydrazinopyridine dihydrochloride and PPh{sub 3} gives [ReCl(PPh{sub 3}){sub 2}(NHNC{sub 5}H{sub 4}N)-(HNNC{sub 5}H{sub 4}N)]Cl{sub 2} (2). A similar reaction using 2-hydrazino-2-imidazoline and PPh{sub 3} in methanol hydrochloric acid allows the preparation of [ReCl{sub 3}(PPh{sub 3}){sub 2}(NNC{sub 3}H{sub 4}N{sub 2})] (3). The reaction of the Re(III) complex [ReCl{sub 3}(NNC{sub 5}H{sub 4}NH)(HNNC{sub 5}H{sub 4}N)] (1), with 2-(Ph{sub 2}P)C{sub 6}H{sub 4}SH in methanol yields [Re{l_brace}2-(Ph{sub 2}P)C{sub 6}H{sub 4}S{r_brace}-{l_brace}2-(Ph{sub 2}PO)C{sub 6}H{sub 4}S{r_brace}(NNC{sub 5}H{sub 4}N)(HNNC{sub 5}H{sub 4}N)] (4) and [Re{l_brace}2-(Ph{sub 2}P)C{sub 6}H{sub 4}S{r_brace}{sub 2}(NNC{sub 5}H{sub 4}N)] (5). The same precursor with 2-(Ph{sub 2}PO)-6-(Me{sub 3}Si)C{sub 6}H{sub 3}SH gives [ReCl{l_brace}2-(Ph{sub 2}PO)-6-(Me{sub 3}Si)C{sub 6}H{sub 3}S{r_brace}(NNC{sub 5}H{sub 4}N)(HNNC{sub 5}H{sub 4}N)] (6) and with PhP(C{sub 6}H{sub 4}SH-2){sub 2} yields [Re{l_brace}PhP(C{sub 6}H{sub 4}S-2){sub 2}{r_brace}(NNC{sub 5}H{sub 4}N)(HNNC{sub 5}H{sub 4}N)] (7).},
doi = {10.1021/ic980953m},
journal = {Inorganic Chemistry},
number = 7,
volume = 38,
place = {United States},
year = {1999},
month = {4}
}