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The coordination geometries about the Cu II ions in both [3,9-dimethyl-4,8-diaza-3,8-undecadiene-2,10-dione dioximato(1−)](thiocyanato)copper(II), [Cu(C 11 H 19 N 4 O 2 )(SCN)] (1), and [3,6,6,9-tetramethyl-4,8-diaza-3,8-undecadiene-2,10-dione dioximato(1−)](isothiocyanato)copper(II), [Cu(C 13 H 23 N 4 O 2 )(NCS)] (2), are distorted square pyramidal with the four diazadioxime N atoms in equatorial positions and the monodentate ligand axial. This monodentate axial ligand is an S-bonded thiocyanato group in complex (1) and an N-bonded isothiocyanato group in (2). The intramolecular O...O hydrogen-bond lengths are 2.530 (4) and 2.490 (2) A in complexes (1) and (2), respectively

Two slightly different complex ions, related by a pseudo-twofold axis, exist in the asymmetric unit of the title compound, [Ni(C 2 H 8 N 2 )(C 10 H 24 N 4 )](ClO 4 ) 2 . There is a mirror plane passing through the Ni and four ligand N atoms in each complex ion. The Ni II ion is six-coordinate in a distorted octahedral arrangement, with the tetradentate macrocyclic ligand in a folded conformation. The two five-membered rings of the macrocyclic ligand have envelope conformations and the two six-membered rings are in chair conformations. The complex has 1SR and 7RS configurations at the two chiral N-atom centres and the C atoms of the ethylenediamine ligands are disordered.

The coordination geometry about the Co III ion in the title compound, chloro[(1RS,7SR,11SR,14RS)-1,4,7,11,14-pentaazacycloheptadecane]cobalt(III) chloride perchlorate, is distorted square bipyramidal with four tetraamine N atoms equatorial and a Cl and an N atom axial. The equatorial N atoms are nearly coplanar with the largest deviation from the least-squares plane of 0.018 A; the deviation of the Co III ion from the plane is 0.039 A. Both six-membered rings are in chair forms and all three five-membered rings in gauche forms

The coordination geometry about Co III is slightly distorted octahedral. The four donor N atoms of the tetraamine form the equatorial plane of the coordination octahedron and two Cl ligands occupy the apices. The alternate five-, six- and five-membered chelate rings have stable skew, chair and skew conformations, respectively. The perchlorate group binds the tetraamine groups through weak hydrogen bonds