Crystal Structure of [Co 2 ( μ‐dmg ) 2 ( μ‐dmg H)( dmg H)(Pø 3 )] 1/2 dmg H 2 · 1/2 CH 3 OH: A Crystal Containing Various Forms of dmg Ligand

The crystal structure of [Co 2 ( μ‐dmg ) 2 ( μ‐dmg H)( dmg H)(Pø 3 )] · 1/2 dmg H 2 · 1/2 CH 3 OH has been determined by single crystal X‐ray diffraction. The title complex crystallizes in triclinic space group P&1bar; with a =10.859(3), b =13.299(3), c =15.247(3)Å, α=98.52(2), β=99.26(2), γ=97.80(2)° and Z =2. The agreement indices are R ( F )=0.062 and R w ( F )=0.085 for 5231 observations and 515 variables. Both cobalt atoms have an oxidation state of 3+ and are both six‐coordinated; one Co(III) atom is bonded to a phosphorous atom of triphenylphosphine, four nitrogen atoms of two planar ligands, dmg 2− and dmg H − , and one oxygen atom of another dmg 2− ligand. The other Co(III) atom is coordinated by four nitrogen atoms of two cis nonplanar ligands, dmg 2− , dmg H − , and two oxygen atoms of the other dmg 2− and dmg H − ligands. There are three N‐O bridged ligands namely two dmg 2− and one dmg H − between two Co(III) atoms. A free molecule of dmg H 2 and a molecule of CH 3 OH are also found in the crystal lattice. The structure interestingly demonstrates the possible various forms of dmg , not only on their charge but also in different conformations upon coordination.