MACROCYCLIC POLYPHOSPHANE LIGANDS : SYNTHESIS AND CHARACTERISATION OF THREE DIASTEREOISOMERS OF 5,8,16,19-TETRAPHENYL-1,12-DITHIA-5,8,16,19-TETRAPHOSPHACYCLODOCOSANE AND THE X-RAY CRYSTAL STRUCTURE OF A DINUCLEAR NICKEL(II) COMPLEX OF THE β ISOMER

DOI: 10.1039/DT9840002265

Source and publish data:

Journal of the Chemical Society, Dalton Transactions p. 2265 - 2270 (1984)

Update date:2022-08-05

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Authors:

Ciampolini, Mario

Nardi, Nicoletta

Orioli, Pier Luigi

Mangani, Stefano

Zanobini, Fabrizio

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Article abstract of DOI:10.1039/DT9840002265

The macrocycle 5,8,16,19-tetraphenyl-1,12-dithia-5,8,16,19-tetraphosphacyclodocosane, L³, has been synthesised in 13percent yield.Three of the five possible diastereoisomers are isolated and one of them (β) is used to form cobalt(II) and nickel(II) complexes with 1 : 1 and 2 : 1 metal-ligand ratios.The compound 3)>2*MeOH crystallises in the orthorhombic space group Pbca with a = 17.791(4), b = 20.993(4), c = 22.758(5) Angstroem, and Z = 4.Least-squares refinement gave R =0.092, for the 917 observed reflections.The cation 3)>²⁺ contains two nickel atoms in a slightly distorted square-planar environment related by a crystallographic centre of symmetry.Each nickel atom is co-ordinated by two phosphorus and one sulphur atoms of the macrocycle and by one bromide ion.The Ni...Ni separation within the cation is 5.13 Angstroem.The stereochemistries of some cobalt(II) and nickel(II) complexes of β-L³ have been investigated in solution and in the solid state by electronic and 31P n.m.r. spectroscopy, and by magnetic measurements.