Molecular-Structure of bis(ethane-1,2-diolato)( tetraphenylporphyrinato )phosphorus(V) chloride: [P( tpp )(OCH2CH2OH)2]+Cl -

Abstract

The structure of bis(ethane-1,2-diolato)( tetraphenylporphyrinato )phosphorus(V) chloride, [P( tpp )(OCH2CH2OH)2]+Cl -, has been confirmed by X-ray diffraction. The cation displays an octahedral coordination about the phosphorus atom and exhibits a ruffled porphyrin geometry with a core size of 1.841 Ǻ. It crystallizes in the orthorhombic space group P212121, with a 12.524(3), b 25.177(5), c 14.275(3) Ǻ, and Z = 4. Refinement based on 4194 observed reflections led to a final R value of 5.1%. The displacement of the phosphorus atom from the porphyrin mean plane is 0.014 Ǻ. The geometry around the phosphorus centre of the [P( tpp )(OCH2CH2OH)2]+Cl- molecule has P-O(1) 1.643(4), P-O(3) 1.642(4) and P- Np 1.841(4) Ǻ. n.m.r. spectroscopy provides a complementary method for the investigation of the ethane-1,2-diolate ligand. The 13C resonances (24°C) of this axial ligand were observed at 62.9 [P-O-C-C-OH, with 2J(P,C) 16.1 Hz] and 57.8 ppm [P-O-C-C-OH with 3J(P,C) 19.1 Hz].