SCHEDULED MAINTENANCE
Tri-, tetra-, penta-, and hexa-nuclear phenylphosphinidene-capped products from the reaction of dodecacarbonyltriruthenium with phenylphosphine: crystal structures of [Ru4(µ4-PPh)2(µ-CO)(CO)10], [Ru5(µ4-PPh){µ-PPh(OPrn)}(µ-H)(CO)13], [Ru6(µ4-PPh)2(µ3-PPh)2(CO)12], and [Ru6(µ4-PPh)3(µ3-PPh)2(CO)12]
Abstract
The reaction of [Ru3(CO)12] with PPhH2 in toluene under reflux affords a range of products, the nature and yields of which are dependent on the reaction times and the molar ratios employed. Compounds isolated and characterised include not only the trinuclear derivatives [Ru3(µ-PPhH)(µ-H)(CO)10], [Ru3(µ3-PPh)(µ-H)2(CO)9], and [Ru3(µ3-PPh)2(CO)9] but the tetra-, and penta-, and hexanuclear species [Ru4(µ4-PPh)2(µ-CO)(CO)10], [Ru4(µ4-PPh)2(µ-PPhH)2(CO)8], [Ru5(µ4-PPh)(CO)15], [Ru6(µ-PPh)2(CO)n](n= 14 or 15), [Ru6(µ4-PPh)2(µ3-PPh)2(CO)12], and [Ru6(µ4-PPh)3(µ3-PPh)2(CO)12] as well as the pentanuclear by-product [Ru5(µ4-PPh){µ-PPh(OPrn)}(µ-H)(CO)13]. Crystal-structure determinations have revealed that [Ru4(µ4-PPh)2(µ-CO)(CO)10] contains an approximately square-planar array of ruthenium atoms capped on both sides by phenylphosphinidene ligands, that [Ru6(µ4-PPh)2(µ3-PPh)2(CO)12] and [Ru6(µ4-PPh)3(µ3-PPh)2(CO)12] have distorted trigonal-prismatic skeletal geometries, and that the ruthenium atom framework in [Ru5(µ4-PPh){µ-PPh(OPrn)}(µ-H)(CO)13] adopts a square-pyramidal configuration with the basal plane being capped by a phenylphosphinidene ligand and a basal edge being bridged by a phosphido group.
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