Synthesis and Characterization of Rhenium(III) Organohydrazide Compounds. Crystal and Molecular Structures of [ReCl(PPh3)2(NHNC5H4N)(HNNC5H4
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- 作者：Paulo Pé ; rez-Lourido ; Jaime Romero ; J. A. Garcí ; a-Vá ; zquez ; Antonio Sousa ; Kevin P. Maresca ; and Jon Zubieta
- 刊名：Inorganic Chemistry
- 出版年：1999
- 出版时间：April 5, 1999
- 年：1999
- 卷：38
- 期：7
- 页码：1511 - 1519
- 全文大小：108K
- 年卷期：v.38,no.7(April 5, 1999)
- ISSN：1520-510X
文摘
The reduction of ReO4- with 2-hydrazinopyridine dihydrochloride and PPh3 gives [ReCl(PPh3)2(NHNC5H4N)(HNNC5H4N)]Cl2 (2). A similar reaction using 2-hydrazino-2-imidazoline and PPh3 in methanol hydrochloricacid allows the preparation of [ReCl3(PPh3)2(NNC3H4N2)] (3). The reaction of the Re(III) complex [ReCl3(NNC5H4NH)(HNNC5H4N)] (1), with 2-(Ph2P)C6H4SH in methanol yields [Re{2-(Ph2P)C6H4S}{2-(Ph2PO)C6H4S}(NNC5H4N)(HNNC5H4N)] (4) and [Re{2-(Ph2P)C6H4S}2(NNC5H4N)] (5). The same precursor with 2-(Ph2PO)-6-(Me3Si)C6H3SH gives [ReCl{2-(Ph2PO)-6-(Me3Si)C6H3S}(NNC5H4N)(HNNC5H4N)] (6) and with PhP(C6H4SH-2)2 yields [Re{PhP(C6H4S-2)2}(NNC5H4N)(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, P
, a = 9.4233(2) Å, b = 15.8308(3) Å, c = 16.3530(2) Å, 
=61.88(10)
, 
= 80.9220(10), 
= 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, = 94.09(1), V = 3598.08(8) Å3,Z = 4, 8406 reflections, R = 0.0359.
, a = 9.4233(2) Å, b = 15.8308(3) Å, c = 16.3530(2) Å, =61.88(10), = 80.9220(10), = 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, = 94.09(1), V = 3598.08(8) Å3,Z = 4, 8406 reflections, R = 0.0359.