The structures of some (hexamethyl-1,5,9,13-tetraazacyclohexadecadiene)copper(II) compounds |
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Authors: | Neil F Curtis Kelly Flood Clifton E Rickard Ward T Robinson Joyce M Waters |
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Institution: | 1. School of Chemical and Physical Sciences, Victoria University of Wellington, Box 600, Wellington, New Zealand;2. Department of Chemistry, University of Canterbury, Christchurch, New Zealand;3. Department of Chemistry, University of Auckland, Auckland, New Zealand;4. Institute of Fundamental Sciences – Chemistry, Albany Campus, Massey University, Auckland, New Zealand |
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Abstract: | The structure of the crystalline azamacrocyclic product formed by reaction of bis(propane-1,3-diamine)copper(II) perchlorate with acetone has been determined as N-rac-(6,8,8,14,16,16-hexamethyl-1,5,9,13-tetraazacyclohexadeca-5,13-diene)copper(II) · N-meso-(6,8,8,14,14,16-hexamethyl-1,5,9,13-tetraazacyclohexadeca-5,16(1)-diene)copper(II) perchlorate, with the cis, 5,16(1)-diene, and trans, 5,13-diene, isomeric cations co-crystallised. The structures of three compounds crystallised from solutions of this mixture have been determined. N-rac-(6,8,8,14,14,16-hexamethyl-1,5,9,13-tetraazacyclohexadeca-5,16(1)-diene)copper(II) tetrachlorozincate has an irregular flattened tetrahedral coordination geometry with trans-N-Cu-N angles of 139.27(8)° and 155.94(8)°. (Hexamethyl-1,5,9,13-tetraazacyclohexadecadiene)(thiocyanato-N)copper(II) perchlorate has twofold symmetrical square-pyramidal cations. A (μ-cyano)-tetracyanonickelate(II) compound has two (hexamethyl-1,5,9,13-tetraazacyclohexadecadiene)copper(II) cations each with a single axially coordinated tetracyanonickelate(II) group. The compounds, except for the tetrachlorozincate(II) salt, show disorder in the location of the imine functions and axial methyl substituents, attributed to co-crystallisation of enantiomers for the N-rac-trans isomer and/or of rotated arrangements of the N-meso-cis isomer. For the thiocyanato and tetracyanonickelato compounds this disorder precluded unambiguous assignment of configuration. |
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Keywords: | Copper(II) compounds Azamacrocycle Tetraazacyclotetradecadiene Thiocyanate Tetracyanonickelato Tetrachlorozincate Crystal structures |
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