Synthesis and structures of (13-hydroxylamino-5,7,7,13-tetramethyl-1,4,8,11-tetraazacyclotetradec-4-ene-κ)nickel(II) tetrachlorozincate(II) and (13-azonium-5,5,7,13-tetramethyl-1,4,8,11-tetraazacyclotetradecane-κ)nickel(II) tetrachlorozincate(II) chloride 2.25 water |
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Authors: | Neil F Curtis Horst Puschmann Ward T Robinson |
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Institution: | aSchool of Chemical and Physical Sciences, Victoria University of Wellington, P.O. Box 600, Wellington 6140, New Zealand;bDurham University Chemical Crystallography Group, Durham DH1 3LE, United Kingdom;cChemistry Department, University of Canterbury, Christchurch, New Zealand |
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Abstract: | Zinc/acid reduction of the nitro function of (5,7,7,13-tetramethyl-13-nitro-1,4,8,11-tetraazacyclotetradec-4-ene)nickel(II) yields (13-hydroxylamino-5,7,7,13-tetramethyl-1,4,8,11-tetraazacyclotetradec-4-ene)nickel(II), isolated as the tetrachlorozincate salt, for which the structure is reported. This has singlet ground state nickel(II) in square-planar coordination by the three amine and the imine nitrogen atoms of the macrocycle. There is no interaction between the nickel(II) ion and the axially oriented hydroxylamino group.Zinc/acid reduction of the nitro function of (5,5,7,13-tetramethyl-13-nitro-1,4,8,11-tetraazacyclotetradecane)nickel(II) yields (13-amino-5,5,7,13-tetramethyl-1,4,8,11-tetraazacyclotetradecane)nickel(II), isolated from acid solution as (13-azonium-5,5,7,13-tetramethyl-1,4,8,11-tetraazacyclotetradecane-κ4)nickel(II) tetrachlorozincate(II) chloride 2.25 water, for which the structure is reported. The two independent cations have singlet ground state nickel(II) in square-planar coordination by the four secondary amine nitrogen atoms of the macrocycle, with the protonated amine substituent axially oriented.The cations of both compounds show disorder in the location of the axial methyl component of the gem-dimethyl group, manifest as reversal of the trimethyl substituted 1,3-amine-imine or 1,3-diamine chelate rings, arising from co-crystallisation of enantiomers. |
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Keywords: | Azamacrocycle Cyclic tetraamine hydroxylamine compound Reduction of nitro group Nickel(II) compound Crystal structure |
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