The triphenylphosphine adduct of a copper(I) complex involving an incompletely bound N2S2 macrocyclic ligand
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The highly distorted tetrahedral copper(1) complex of the 14-membered trans-N,S, macrocyclic ligand 6,7,15,16-tetrahydrodibenzo[f,m] [I,8 ,4,11 ]dithiadiazacyclotetradecine (L) undergoes reaction with triphenylphosphine to form an adduct in which one of the two sulphur donors of the macrocycle has been displaced from the primary co-ordination sphere of the metal ion, resulting in tetrahedral co-ordination via an N,PS donor array. The triphenylphosphine molecule is labile allowing the parent complex to be recovered upon recrystallization from an acetone-ethanol mixture. Crystal structures of both [CuL] CIO, (1 ) and [CuL( PPh,)] CIO4-0.5Me,CO (2) are reported. For (1): space group P6, a = 17.610(7), c = 5.377(2) A, Z = 3, R = 0.061 for 947 'observed' reflections. For (2): space group PT, a = 15.74(2), b = 12.29(1), c = 9.91 (1 ) A, O! = 82.07(9), p = 84.88(8), y = 84.43(9)", Z = 2, R = 0.1 0 for 1 796 'observed' reflections. The solid-state 31P n.m.r. spectrum for (2) shows a quartet centred on 2.3 p.p.m. with line spacings of 1.41, 1.55, and 1.65 kHz.
Journal of the Chemical Society, Dalton Transactions
Copyright 1988 Royal Society of Chemistry. This is the author-manuscript version of the paper. Reproduced in accordance with the copyright policy of the publisher.