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
Pb. Kettler et al., 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, Inorganic chemistry, 33(25), 1994, pp. 5864-5871
The reactions of the cis-dioxorhenium(VII)-catecholate complex [(CH3CH
2)(4)N][ReO2(O2C6H4)(2)] (1) With either monosubstituted organohydrazi
nes (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, b
eta = 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) A
ngstrom, b = 11.864(2) Angstrom, c = 15.400(2) Angstrom, alpha = 107.1
2(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) Ang
strom, b = 9.670)2) Angstrom, c = 23.142(5) Angstrom, beta = 90.91(3)d
egrees, V = 1294.4(7) Angstrom(3), Z = 2, D-calc = 1.737 g cm(-3); 151
7 reflections, R = 0.049.