Journal of the Chemical Society, Dalton Transactions p. 751 - 762 (1981)
Update date:2022-08-05
Topics:
Howard, Judith A. K.
Jeffery, John C.
Laguna, Mariano
Navarro, Rafael
Stone, F. Gordon A.
full title: Chemistry of di- and tri-metal complexes with bridging carbene or carbyne ligands. Part 7. Interconversion of carbene and carbyne ligands at a dimetal centre. X-Ray crystal structures of [CrPt{μ-C(CO2Me)Ph}(CO)4(PMe3)3] and [ MnPt(μ-CC6H4Me-4)(CO)2(PMe3) 2(η-C5H5)][BF4]·CH 2Cl2 Reaction of the dimetal complexes [MPt{μ-C(OMe)Ph}(CO)5(PMe3)2] with [OMe3][BF4] followed by addition of Li[C6H4Me-4] or Na[OEt] afforded the compounds [MPt{μ-C(Ph)R}(CO)5(PMe3)2] (M = Cr, R = C6H4Me-4 or OEt; M = W, R = OEt). Treatment of the compounds [MPt{μ-C(OMe)R}(CO)4(PMe3)3] (M = Cr, R = Ph; M = W, R = C6H4Me-4) with [OMe3][BF4] allowed isolation and characterization of the salts [CrPt(μ-CPh)-(CO)4(PMe3)3][BF4] and [PtW(μ-CC6H4Me-4) (CO)4(PMe3)3][BF4] respectively. Reaction of [CrPt(μ-CPh)-(CO)4(PMe3)3] [BF4] with Na[OMe] gave the alkylidene-bridged compound [CrPt{μ-C(CO2Me)Ph}(CO)4-(PMe3) 3], the strucure of which was established by X-ray diffraction. Crystals are monoclinic, space group A2/a, Z = 8, in a unit cell with lattice parameters a = 18.27(3), b = 9.84(1), c = 31.93(5) A, β = 106.2(1)°. The structure has been refined to R 0.12 (R′ 0.12) for 2 292 independent absorption corrected intensities to 2.9 ≤ 2θ ≤ 50° (Mo-Kα X-radiation) collected at room temperature. The chromium-platinum bond [2.646(7) A] is bridged by the μ-C(CO2Me)Ph group [C-Pt 1.98(3), C-Cr 2.27(4) A]. One of the CO ligands is semi-bridging to the platinum [Cr-C-O 157(3)°]. Related platinum-tungsten compounds [PtW{μ-C(CO2R)Ph}(CO)4(PMe3)3] (R = Me or Et) have also been prepared. The platinum-manganese and -rhenium compounds [MPt(μ-CC6H4Me-4)(CO)2(PR3) 2(η-C5H5)][BF4] (M = Mn, PR3 = PMe3; M = Re, PR3 = PMe3 or PMe2Ph) have been synthesized and an X-ray diffraction study made on the manganese compound which crystallises with a molecule of CH2Cl2 per molecule of complex in the asymmetric unit. Crystals are monoclinic, space group P21/c, Z = 4, in a unit cell of dimensions a = 10.434(4), b = 19.334(7), c = 14.901(7) A, and β = 94.42(4)°. The structure has been refined to R 0.044 (R′ 0.046) for 4 223 independent reflections to 2.9 ≤ 2θ ≤ 55° (Mo-Kα X-radiation) collected at 300 K. In the cation the manganese-platinum bond [2.628(1) A] is bridged by the CC6H4Me-4 group [C-Pt 1.968(8), C-Mn 1.829(8) A] forming a dimetallacyclopropene ring, the C-Mn separation being indicative of a double bond. The 1H, 31P, and 13C (1H decoupled) n.m.r. spectra of the new compounds are reported and discussed.
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