Thermolysis of [Pt(NH3)4][ReHlg6] (Hlg = Cl, Br). Structure refinement for [Pt(NH3)4][ReCl6]

Thermal decomposition of [Pt(NH3)4][ReHlg6] binary complex salts (Hlg = Cl, Br) in a hydrogen atmosphere has been studied. Polycrystal X-ray diffractometry indicated that two-phase metallic systems are the final products of thermolysis. Structure refinement was performed for [Pt(NH3)4][ReCl6] by the combined technique involving decomposition of the diffractogram into individual reflections, isolation of reflections most sensitive to the position of separate light atoms, and full-profile analysis. Crystal data for PtReN4Cl6H12: a = 11.616(1) Å, b = 10.998(1) Å, c = 10.377(1) Å, V = 1148.1 Å3, space group Cmca, Z = 4, dx = 3.831 g/cm3. The indices are Rp = 5.48%, Rwp = 10.01%, R(F2) = 12.62%. The coordination polyhedron of Re is an almost regular octahedron: Re-Cl 2.34–2.36 Å, ∠ Cl-Re-Cl 86.9–90.3°; the coordination polyhedron of Pt is a square: Pt-N 2.04 Å, ∠N-Pt-N 90.4°.