Inorganic Chemistry, Vol.33, No.25, 5864-5871, 1994
Synthesis, Spectroscopy, and Structural Characterization of 6-Coordinate bis(Aryldiazenido)Rhenium and bis(Diarylhydrazido)Rhenium Complexes - X-Ray Structures of (Et(4)N)(Re(Nnph)(2)(O2C6H4)(2)), (Et(4)N)(Re(Nnph(2))(2)(O2C6H4)2), and Na(Re(Nnph)(2)(O2C6H4)2)Center-Dot-CH3CN
The reactions of the cis-dioxorhenium(VII)-catecholate complex [(CH3CH2)(4)N][ReO2(O2C6H4)(2)] (1) With either monosubstituted organohydrazines (C6H5NHNH2; 4-BrC6H4NHNH2) or 1,1-disubstituted organohydrazines (Ph(2)-NNH2) yield the cis-bis(diazenido) core complexes [(CH3CH2)(4)N][Re(NNR)(2)(O2C6H4)(2)] (5, R = C6H5; 6, R = 4-BrC6H4) and the cis-bis(hydrazido) core species [(CH3CH2)(4)N][Re(NNPh(2))(2)(O(2)C36H(4))(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) : P2(1)/c, a = 14.458(3) Angstrom, b = 10.436(2) Angstrom, c = 21.767(4) Angstrom, beta = 107.04(3)degrees, V = 3140(2) Angstrom(3), Z = 4, D-calc = 1.572 g cm(-3); structure solution and refinement based on 3256 reflections with I-0 greater than or equal to 3 sigma(I-0) converged at R = 0.053. Crystal data for C44H48N5O4Re (7) : P ($) over bar 1, a = 11.660(2) Angstrom, b = 11.864(2) Angstrom, c = 15.400(2) Angstrom, alpha = 107.12(3)degrees, beta = 94.99(3)degrees, gamma = 97.61(3)degrees, V = 2000(1) Angstrom(3), Z = 2, D-calc = 1.490 g cm(-3); 3702 reflections, R = 0.0534. Crystal data for C26H18N5NaO(4)Re (8) : P2/n, a = 5.785(1) Angstrom, b = 9.670)2) Angstrom, c = 23.142(5) Angstrom, beta = 90.91(3)degrees, V = 1294.4(7) Angstrom(3), Z = 2, D-calc = 1.737 g cm(-3); 1517 reflections, R = 0.049.
Keywords:MOLECULAR-STRUCTURES;CRYSTAL-STRUCTURES;CHEMISTRY;TECHNETIUM;LIGANDS;PROTEINS;(TCCL2(C8H5N4)(PPH3)2).0.75C7H8;DERIVATIVES;MOLYBDENUM;ELEMENTS