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Synthesis and characterization of manganese and rhenium metallacycles

Journal Article · · Organometallics; (USA)
DOI:https://doi.org/10.1021/om00116a019· OSTI ID:6985567

Reactions of manganese or rhenium formyl complexes bearing phosphine or phosphite ligands with protonic acids have been utilized in developing synthetic routes to new five- and six-membered metallacyclic compounds, Mn(CO){sub 4}(P(Ph){sub 2}(o-C{sub 6}H{sub 4}CH{sub 2})) and M(CO){sub 3}(L) (P(OPh){sub 2}(o-OC{sub 6}H{sub 4}CH{sub 2})) (M = Mn, L = CO or P(OPh){sub 3}; M = Re, L = P(OPh){sub 3}). The synthetic route makes use of the ability of formyl complexes to transfer hydride in the presence of a protonic acid without transferring it to the acid. Two of the manganese compounds have been characterized by X-ray crystallography: (i) crystal data for Mn-(CO){sub 4}(P(Ph){sub 2}(o-C{sub 6}H{sub 4}CH{sub 2})), a = 13.519 (3) {angstrom}, b = 8.295 (2) {angstrom}, c = 18.199 (3) {angstrom}, {beta} = 90.82 (1){degree}, Z = 4, d{sub c} = 1.44 g cm{sup {minus}3}, space group P2{sub 1}/c, and R = 0.029; (ii) crystal data for Mn(CO){sub 3}(P(OPh){sub 3}) (P(OPh){sub 2}(o-OC{sub 6}H{sub 4}CH{sub 2})), a = 15.977 (8) {angstrom}, b = 26.554 (10) {angstrom}, c = 8.523 (6) {angstrom}, {beta} = 87.12 (5){degree}, Z = 4, d{sub c} = 1.42 g cm{sup {minus}3}, space group P2{sub 1}/n, and R = 0.039. The IR and {sup 1}H and {sup 13}C NMR spectral properties of all four metallacycles are reported.

OSTI ID:
6985567
Journal Information:
Organometallics; (USA), Journal Name: Organometallics; (USA) Vol. 9:2; ISSN 0276-7333; ISSN ORGND
Country of Publication:
United States
Language:
English