The structure of bis(cis-1,3-diaminocyclohexane) palladium(II) chloride has been determined from X-ray diffraction data collected by the counter method. The crystal is orthorhombic with space group Pnnm, a=17.728(5), b=6.418(4), c=6.914(2) Å, and Z=2. The crystal structure has been determined by Patterson and Fourier techniques and refined by a least-squares method to R=0.026 for 1151 independent reflections for which Fo2>3σ(Fo2). The Pd atom has a planar coordination of 4N atoms and the complex cation has a crystallographically imposed C2h symmetry, the two cis-1,3-diaminocyclohexane ligands being related to each other by a two fold axis. The six-membered chelate ring (Remark: Graphics omitted.) is of the envelope conformation. The structural features of the ligating cis-1,3-diaminocyclohexane have been described. The crystal of bis(cis-1,3-diaminocyclohexane)platinum(II) (orthorhombic, a=17.727(8), b=6.371(3), c=6.965(2) Å) was found to be isomorphous with that of the palladium analogue.
The crystal structures of wine-red [Cu(1,3-chxn)2]Br2 (1), [Cu(1,3-chxn)2](NO3)2 (2), and blue-violet [CuCl(1,3-chxn)2]ClO4 (3) (1,3-chxn=cis-1,3-cyclohexanediamine) have been determined from the diffractometer data measured by the use of Mo Kα radiation. The structures were solved by the Patterson–Fourier method and refined by the least-squares method to R=0.042 (1), 0.033 (2), and 0.057 (3) for 1309, 1210, and 776 nonzero reflections respectively. The Cu atoms in 1 and 2 have a square-planar coordination by 4 N atoms, while the complex ion in 3 has a 5-coordinate square-pyramidal geometry, with the Cl atom at the apical position. The 6-membered chelate rings in 1, 2, and 3 are of the chair, flattened-chair, and envelope conformations respectively. The complex ions in 1 and 2 have virtually a C2h symmetry, the two-fold axis of which lies on the CuN4 plane. The virtual symmetry for [CuCl(1,3-chxn)2]+ is C2v, the approximate two-fold axis being coincident with the Cu–Cl bond. The cyclohexane rings (chair conformation) in 2 and 3 are roughly perpendicular to the coordination plane, but that in 1 leans toward the central Cu(II) atom. The formation of such coordinatively unsaturated Cu(II) complexes as 1–3 is attributable to the steric hindrance of the bulky cyclohexane ring to the axial coordination site.
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