Synthesis and characterization of rhenium(III) organohydrazide compounds. Crystal and molecular structures of [ReCl(PPh3)2(NHNC5H4N)(HNNC 5H4N)]Cl2, [Re{2-(Ph2P)C6H4S}{2-(Ph2PO)C 6H4S}]

Paulo Pérez-Lourido; Jaime Romero; J. A. García-Vázquez; Antonio Sousa; Kevin P. Maresca; Jon Zubieta

doi:10.1021/ic980953m

Synthesis and characterization of rhenium(III) organohydrazide compounds. Crystal and molecular structures of [ReCl(PPh₃)₂(NHNC₅H₄N)(HNNC ₅H₄N)]Cl₂, [Re{2-(Ph₂P)C₆H₄S}{2-(Ph₂PO)C ₆H₄S}]

Paulo Pérez-Lourido, Jaime Romero, J. A. García-Vázquez, Antonio Sousa, Kevin P. Maresca, Jon Zubieta

Department of Chemistry

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Abstract

The reduction of ReO₄^- with 2-hydrazinopyridine dihydrochloride and PPh₃ gives [ReCl(PPh₃)₂(NHNC₅H₄N)-(HNNC ₅H₄N)]Cl₂ (2). A similar reaction using 2-hydrazino-2-imidazoline and PPh₃ in methanol hydrochloric acid allows the preparation of [ReCl₃(PPh₃)₂(NNC₃H ₄N₂)] (3). The reaction of the Re(III) complex [ReCl₃(NNC₅H₄-NH)(HNNC₅H ₄N)] (1), with 2-(Ph₂P)C₆H₄SH in methanol yields [Re{2-(Ph₂P)C₆H₄S}{2-(Ph₂PO)C ₆H₄S}-(NNC₅H₄N)(HNNC ₅H₄N)] (4) and [Re{2-(Ph₂P)C₆H₄S}₂(NNC ₅H₄N)] (5). The same precursor with 2-(Ph₂PO)-6-(Me₃Si)C₆H₃SH gives [ReCl{2-(Ph₂PO)-6-(Me₃Si)C₆H ₃S}(NNC₅H₄N)(HNNC₅H₄N)] (6) and with PhP(C₆H₄SH-2)₂ yields [Re{PhP(C₆H₄S-2)₂}(NNC₅H ₄N)(HNNC₅H₄N)] (7). Crystal data: 2, C₄₆H₃₉N₆P₂Cl₃Re, orthorhombic, Pnma, a = 19.6381(7) Å, b = 15.1861(6) Å, c = 15.0711(5) Å, V = 4494.6(3) Å³, Z = 6, 5646 reflections, R = 0.0655; 4, C₄₆H₃₇N₆OP₂S₂Re, triclinic, P1̄, a = 9.4233(2) Å, b = 15.8308(3) Å, c = 16.3530(2) Å, α = 61.88(10)°, β= 80.9220(10)°, γ = 85.1350(10)°, V = 2124.40(7) Å³, Z = 2, 8728 reflections, R = 0.0757; 5, monoclinic, P2₁/c, a = 10.0006(2) Å,b= 18.1857(1) Å, c = 19.8595(2) Å, β= 94.09(1)°, V= 3598.08(8) Å³, Z = 4, 8406 reflections, R = 0.0359.

Original language	English (US)
Pages (from-to)	1511-1519
Number of pages	9
Journal	Inorganic Chemistry
Volume	38
Issue number	7
DOIs	https://doi.org/10.1021/ic980953m
State	Published - 1999

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Physical and Theoretical Chemistry
Inorganic Chemistry

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10.1021/ic980953m

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Synthesis and characterization of rhenium(III) organohydrazide compounds. Crystal and molecular structures of [ReCl(PPh₃)₂(NHNC₅H₄N)(HNNC ₅H₄N)]Cl₂, [Re{2-(Ph₂P)C₆H₄S}{2-(Ph₂PO)C ₆H₄S}]. / Pérez-Lourido, Paulo; Romero, Jaime; García-Vázquez, J. A. et al.
In: Inorganic Chemistry, Vol. 38, No. 7, 1999, p. 1511-1519.

Research output: Contribution to journal › Article › peer-review

@article{632fb4976a3945a58d9add23e6003504,

title = "Synthesis and characterization of rhenium(III) organohydrazide compounds. Crystal and molecular structures of [ReCl(PPh3)2(NHNC5H4N)(HNNC 5H4N)]Cl2, [Re{2-(Ph2P)C6H4S}{2-(Ph2PO)C 6H4S}]",

abstract = "The reduction of ReO4- with 2-hydrazinopyridine dihydrochloride and PPh3 gives [ReCl(PPh3)2(NHNC5H4N)-(HNNC 5H4N)]Cl2 (2). A similar reaction using 2-hydrazino-2-imidazoline and PPh3 in methanol hydrochloric acid allows the preparation of [ReCl3(PPh3)2(NNC3H 4N2)] (3). The reaction of the Re(III) complex [ReCl3(NNC5H4-NH)(HNNC5H 4N)] (1), with 2-(Ph2P)C6H4SH in methanol yields [Re{2-(Ph2P)C6H4S}{2-(Ph2PO)C 6H4S}-(NNC5H4N)(HNNC 5H4N)] (4) and [Re{2-(Ph2P)C6H4S}2(NNC 5H4N)] (5). The same precursor with 2-(Ph2PO)-6-(Me3Si)C6H3SH gives [ReCl{2-(Ph2PO)-6-(Me3Si)C6H 3S}(NNC5H4N)(HNNC5H4N)] (6) and with PhP(C6H4SH-2)2 yields [Re{PhP(C6H4S-2)2}(NNC5H 4N)(HNNC5H4N)] (7). Crystal data: 2, C46H39N6P2Cl3Re, orthorhombic, Pnma, a = 19.6381(7) {\AA}, b = 15.1861(6) {\AA}, c = 15.0711(5) {\AA}, V = 4494.6(3) {\AA}3, Z = 6, 5646 reflections, R = 0.0655; 4, C46H37N6OP2S2Re, triclinic, P{\=1}, a = 9.4233(2) {\AA}, b = 15.8308(3) {\AA}, c = 16.3530(2) {\AA}, α = 61.88(10)°, β= 80.9220(10)°, γ = 85.1350(10)°, V = 2124.40(7) {\AA}3, Z = 2, 8728 reflections, R = 0.0757; 5, monoclinic, P21/c, a = 10.0006(2) {\AA},b= 18.1857(1) {\AA}, c = 19.8595(2) {\AA}, β= 94.09(1)°, V= 3598.08(8) {\AA}3, Z = 4, 8406 reflections, R = 0.0359.",

author = "Paulo P{\'e}rez-Lourido and Jaime Romero and Garc{\'i}a-V{\'a}zquez, {J. A.} and Antonio Sousa and Maresca, {Kevin P.} and Jon Zubieta",

year = "1999",

doi = "10.1021/ic980953m",

language = "English (US)",

volume = "38",

pages = "1511--1519",

journal = "Inorganic Chemistry",

issn = "0020-1669",

publisher = "American Chemical Society",

number = "7",

}

TY - JOUR

T1 - Synthesis and characterization of rhenium(III) organohydrazide compounds. Crystal and molecular structures of [ReCl(PPh3)2(NHNC5H4N)(HNNC 5H4N)]Cl2, [Re{2-(Ph2P)C6H4S}{2-(Ph2PO)C 6H4S}]

AU - Pérez-Lourido, Paulo

AU - Romero, Jaime

AU - García-Vázquez, J. A.

AU - Sousa, Antonio

AU - Maresca, Kevin P.

AU - Zubieta, Jon

PY - 1999

Y1 - 1999

N2 - The reduction of ReO4- with 2-hydrazinopyridine dihydrochloride and PPh3 gives [ReCl(PPh3)2(NHNC5H4N)-(HNNC 5H4N)]Cl2 (2). A similar reaction using 2-hydrazino-2-imidazoline and PPh3 in methanol hydrochloric acid allows the preparation of [ReCl3(PPh3)2(NNC3H 4N2)] (3). The reaction of the Re(III) complex [ReCl3(NNC5H4-NH)(HNNC5H 4N)] (1), with 2-(Ph2P)C6H4SH in methanol yields [Re{2-(Ph2P)C6H4S}{2-(Ph2PO)C 6H4S}-(NNC5H4N)(HNNC 5H4N)] (4) and [Re{2-(Ph2P)C6H4S}2(NNC 5H4N)] (5). The same precursor with 2-(Ph2PO)-6-(Me3Si)C6H3SH gives [ReCl{2-(Ph2PO)-6-(Me3Si)C6H 3S}(NNC5H4N)(HNNC5H4N)] (6) and with PhP(C6H4SH-2)2 yields [Re{PhP(C6H4S-2)2}(NNC5H 4N)(HNNC5H4N)] (7). Crystal data: 2, C46H39N6P2Cl3Re, orthorhombic, Pnma, a = 19.6381(7) Å, b = 15.1861(6) Å, c = 15.0711(5) Å, V = 4494.6(3) Å3, Z = 6, 5646 reflections, R = 0.0655; 4, C46H37N6OP2S2Re, triclinic, P1̄, a = 9.4233(2) Å, b = 15.8308(3) Å, c = 16.3530(2) Å, α = 61.88(10)°, β= 80.9220(10)°, γ = 85.1350(10)°, V = 2124.40(7) Å3, Z = 2, 8728 reflections, R = 0.0757; 5, monoclinic, P21/c, a = 10.0006(2) Å,b= 18.1857(1) Å, c = 19.8595(2) Å, β= 94.09(1)°, V= 3598.08(8) Å3, Z = 4, 8406 reflections, R = 0.0359.

AB - The reduction of ReO4- with 2-hydrazinopyridine dihydrochloride and PPh3 gives [ReCl(PPh3)2(NHNC5H4N)-(HNNC 5H4N)]Cl2 (2). A similar reaction using 2-hydrazino-2-imidazoline and PPh3 in methanol hydrochloric acid allows the preparation of [ReCl3(PPh3)2(NNC3H 4N2)] (3). The reaction of the Re(III) complex [ReCl3(NNC5H4-NH)(HNNC5H 4N)] (1), with 2-(Ph2P)C6H4SH in methanol yields [Re{2-(Ph2P)C6H4S}{2-(Ph2PO)C 6H4S}-(NNC5H4N)(HNNC 5H4N)] (4) and [Re{2-(Ph2P)C6H4S}2(NNC 5H4N)] (5). The same precursor with 2-(Ph2PO)-6-(Me3Si)C6H3SH gives [ReCl{2-(Ph2PO)-6-(Me3Si)C6H 3S}(NNC5H4N)(HNNC5H4N)] (6) and with PhP(C6H4SH-2)2 yields [Re{PhP(C6H4S-2)2}(NNC5H 4N)(HNNC5H4N)] (7). Crystal data: 2, C46H39N6P2Cl3Re, orthorhombic, Pnma, a = 19.6381(7) Å, b = 15.1861(6) Å, c = 15.0711(5) Å, V = 4494.6(3) Å3, Z = 6, 5646 reflections, R = 0.0655; 4, C46H37N6OP2S2Re, triclinic, P1̄, a = 9.4233(2) Å, b = 15.8308(3) Å, c = 16.3530(2) Å, α = 61.88(10)°, β= 80.9220(10)°, γ = 85.1350(10)°, V = 2124.40(7) Å3, Z = 2, 8728 reflections, R = 0.0757; 5, monoclinic, P21/c, a = 10.0006(2) Å,b= 18.1857(1) Å, c = 19.8595(2) Å, β= 94.09(1)°, V= 3598.08(8) Å3, Z = 4, 8406 reflections, R = 0.0359.

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UR - http://www.scopus.com/inward/citedby.url?scp=0001733156&partnerID=8YFLogxK

U2 - 10.1021/ic980953m

DO - 10.1021/ic980953m

M3 - Article

AN - SCOPUS:0001733156

SN - 0020-1669

VL - 38

SP - 1511

EP - 1519

JO - Inorganic Chemistry

JF - Inorganic Chemistry

IS - 7

ER -

Synthesis and characterization of rhenium(III) organohydrazide compounds. Crystal and molecular structures of [ReCl(PPh₃)₂(NHNC₅H₄N)(HNNC ₅H₄N)]Cl₂, [Re{2-(Ph₂P)C₆H₄S}{2-(Ph₂PO)C ₆H₄S}]

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