Synthesis of the neutral (CuF(NC5H5)(4))(2)NbOF5 cluster

Composition space diagrams can be used to study the stability and variety o f mixed transition metal oxide fluorides prepared under hydro(solvato)therm al conditions. Prior to this work the neutral (CuF(NC5H5)(4))(2)NbOF5 clust er had not been observed but it was expected because of the nucleophilic ch aracter of the oxygen and trans fluorine in the [NbOF5](2-) species, [H3O]( 2)[(CuF(NC5H5)(4))(2)NbOF5][F](2), a compound containing the 2:1 (Cu: Nb) c luster, was synthesized from the concentration variables, [CuO . 0.5 Nb2O5] , [(HF), pyridine], and [H2O], by adding a fourth, [pyridine], and extendin g the composition space from a two-dimensional triangle to a three-dimensio nal prism. Crystal Data: [H3O](2)[(CuF(NC5H5)(4))(2)NbOF5][F](2), tetragona l, space group I4(1)/acd (no, 142), with a = 24.691(1) Angstrom, c = 14.556 (1) Angstrom, Z = 8.