High-temperature reactions of metal triangles: The influence of counterion, ligand, and metal on the structure observed

A series of oxo-centered metal carboxylate triangles have been heated to 20 0-400 degreesC under a stream of N-2, The products of this treatment depend on the metal, carboxylate, and counterion present, Heating [Cr3O(O2CC6H4Cl )(6)(H2O)(3)] [NO3]to 200 degreesC gives a compound that crystallizes as [C r(OH)(O2CC6H4Cl)(2)](8) [Cr3O(O2CC6H4Cl)(6)](2)[O(2)CC(6)H4Cl], indicating incomplete dehydration of [Cr3O(O2CC6H4Cl)(6)(H2O)(3)][NO3] at this tempera ture. For [Cr3O(O2CCMe3)(6)][O2CCMe3] heating to 400 degreesC gives a new s alt containing the hexanuclear cages [Cr6O2(OH)(2) (O2CCMe3)(11)] [Cr6O4(O2 CCMe3)(11)]. For [Mn3O(O2CPh)(6) (NC5H5)(2)(H2O)] a reduction of the metal occurs and a polymeric complex [Mn-4(O2CPh)(8)(EtOH)(6)](n) can be crystall ized from EtOH, (C) 2001 Academic Press.