Synthesis, Spectroscopy, and Structural Characterization of Six-Coordinate Bis(aryldiazenido)rhenium and Bis(diarylhydrazido)rhenium Complexes. X-ray Structures of (Et4N)[Re(NNPh)2(O2C6H4)2], (Et4N)[Re(NNPh2)2(O2C6H4)2], and Na[Re(NNPh)2(O2C6H4)2]·CH3CN

Peter B. Kettler, Yuan Da Chang, Jon Zubieta

Research output: Contribution to journalArticle

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Abstract

The reactions of the di-dioxorhemum(VII)-catecholate complex [(CH3CH2)4N] [ReO2(O2C6H4)2] (1) with either monosubstituted organohydrazines (C6H5NHNH2; 4-BrC6H4NHNH2) or 1,1-disubstituted organohydrazines (Ph2- NNH2) yield the cis-bis(diazenido) core complexes [(CH3CH2)4N] [Re(NNR)2(O2C6H4)2] (5, R = C6H5; 6, R = 4-BrC6H4) and the cis-bis(hydrazido) core species [(CH3CH2)4N] [Re(NNPh2)2(O2C36H4)2] (7). Elution of 5 in a 3:1 mixture of toluene/methanol on a column of silica gel resulted in cation exchange to give Na[Re(NNPh)2- (O2C6H4)2]-CH3CN (8) as a one-dimensional polymer {[Na(CH3CN)]+[Re(NNPh)2(O2C6H4)2]-}2· Crystal data for C32H38N5O4Re (5): P21/c, a = 14.458(3) Å, b = 10.436(2) Å, c = 21.767(4) Å, β= 107.04(3)°, V= 3140(2) Å3, Z = 4, Dcalc = 1.572 g cm-3; structure solution and refinement based on 3256 reflections with Io ≥ 3 σ (Io) converged at R = 0.053. Crystal data for C44H48N5O4Re (7): P1, a = 11.660(2) Å, b = 11.864(2) Å, c = 15.400(2) Å, α = 107.12(3)°, β = 94.99(3)°, γ = 97.61(3)°, V = 2000(1) Å3, Z = 2, Dcalc = 1.490 g cm-3; 3702 reflections, R = 0.0534. Crystal data for C26H18N5NaO4Re (8): P2/n, a = 5.785(1) Å, b = 9.670)2) Å, c = 23.142(5) Å, β = 90.91(3)°, V = 1294.4(7) Å3, Z = 2, Dcalc = 1.737 g cm-3; 1517 reflections, R = 0.049.

Original languageEnglish (US)
Pages (from-to)5864-5871
Number of pages8
JournalInorganic Chemistry
Volume33
Issue number25
DOIs
StatePublished - Dec 1 1994

ASJC Scopus subject areas

  • Physical and Theoretical Chemistry
  • Inorganic Chemistry

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