132540-96-6Relevant articles and documents
Synthesis and structure of seven-coordinate rhenium(III) mixed halo-phosphine isocyanide complexes
Warner, Steve,Cheatham, Linda K.,Tulip, Thomas H.,Williams, Ian D.,Lippard, Stephen J.
, p. 1221 - 1226 (2008/10/08)
The synthesis of mixed halo-phosphine isocyanide complexes of general formula [ReCl2(CNR)3(PMePh2)2]+ is described. The crystal structure of a representative member of this class, [ReCl2(CN-t-Bu)3(PMePh2)2](SbF 6) (1), has been determined. This complex adopts the C2υ capped trigonal prismatic geometry with close nonbonded contacts of 2.341 (8) and 2.330 (9) A? between coordinated isocyanide carbon atoms. Such distances in seven-coordinate compounds reveal that they are good candidates for reductive coupling of the isocyanide ligands, a reaction previously studied for 1. The syntheses of [ReCl3(CN-t-Bu)2(PMePh2)2] and [ReCl3(CN-2,6-Me2Ph)3(PMePh2)] are also reported. Red crystals of [Re(O)(OEt)Cl2(PMePh2)2] (2) were isolated in 25% yield as a side product during the preparation of [ReCl3(PMePh2)3] starting material from AgReO4. The identity of 2 was established by IR spectroscopy, elemental analysis, and X-ray crystallography. The Re-O bond distance of 1.699 (5) A? is characteristic of a metal-oxygen triple bond. Crystal data: for 1, a = 10.486 (2) A?, b = 13.201 (2) A?, c = 17.559 (2) A?, α = 76.21 (1)°, β = 89.73 (1)°, γ = 87.05 (1)°, triclinic, P1 (Ci1; Z = 2); for 2, a = 11.015 (1) A?, b = 12.745 (1) A?, c = 21.035 (3) A?, β = 105.19 (1)°, monoclinic, P21/n (C2h5; Z = 4).
