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Chromium(II) Complexes of o-Phenylenediamine. The Crystal and Molecular Structures of Bis(o-phenylenediamine-κN)bis(thiocyanato-κN)chromium(II) and Bis(o-phenylenediamine-κ2N,N')bis(o-phenylenediamine-κN)chromium(II) Trifluoromethanesulphonate

DOI: 10.1039/DT9910002045

Source and publish data:

Journal of the Chemical Society, Dalton Transactions p. 2045 - 2050 (1991)

Update date:2022-09-26

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Authors:

Jubb, JayneJubb, Jayne

Larkworthy, Leslie F.Larkworthy, Leslie F.

Oliver, Lee F.Oliver, Lee F.

Povey, David C.Povey, David C.

Smith, Gallienus W.Smith, Gallienus W.

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Article abstract of DOI:10.1039/DT9910002045

The following chromium(II) complexes of o-phenylenediamine (opd) have been isolated: , Br2, *1.5EtOH, , Cl2 and 2.From the patterns of bands assigned to NH2 and CN stretching vibrations in the infrared spectra the first two complexes contain monodentate diamine, the next two bidentate diamine and the last two both mono- and bi-dentate diamine; thus Cl2 is more correctly formulated as Cl2*2opd.Crystal-structure determinations confirm the assignments for and Cr(opd)4>2.The thiocyanato complex crystallises in the monoclinic space group P21/c with a = 11.027(3), b = 5.828(2), c = 13.431(2) Angstroem, β = 103.93(2) deg and Z = 2.The structure was refined to R = 0.040 for 1551 observed reflections.There are trans-planar units in which the bond distances are Cr-NH2 (monodentate diamine) 2.160(2) and Cr-NCS 2.036(2) Angstroem, with S atoms of isothiocyanato groups of adjacent units in the axial positions, Cr-S 2.972(2) Angstroem forming a thiocyanato-bridged structure.The triflate crystallises in the orthorhombic space group Pbca, with a = 8.978(8), b = 22.455(7), c = 16.842(2) Angstroem and Z = 4.The structure was refined to R = 0.061 for 1863 observed reflections.The co-ordination sphere consists of two bidentate diamine molecules, mean Cr-N 2.119 Angstroem, with two more distant, axially positioned, monodentate molecules at 2.669(5) Angstroem.In accordance with its structure exhibits antiferromagnetic behaviour as does which is a chloride-bridged polymer.The triflate and the remaining complexes show simple paramagnetic behaviour (90-300 K).Attempts to prepare a chromium(II) complex of a tetraazamacrocyclic ligand by reaction of the o-phenylenediamine complexes with acetylacetone were unsuccessful; either no reaction took place or the benzodiazepinium chloride was isolated.

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Product name:bis(o-phenylenediamine-κN)-bis(thiocyanato-κN)chromium(II)

Cas No:124858-20-4

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