Synthesis and crystal structure of [copper(1,10-phenanthroline)2(pyridine)]perchlorates

The complex [Cu(phen)(2)py](ClO4)(2) was obtained by the reaction of 1,10-p henanthroline with Cu(ClO4)(2) . 6H(2)O in water and by recrystallization f rom pyridine. A single-crystal X-ray study shows that the complex is a squa re pyramidal arrangement of five nitrogen atoms from the two 1,10-phenanthr oline ligands and one pyridine ligand, respectively. The compound is orthor hombic, C29H21N5Cl2O8Cu, M-r = 701.958, with space group Pbcn, a = 29.9593( 3), b = 16.1240(3), c = 11.9183(6) Angstrom, V = 5757.3(3) Angstrom (3), Z = 8, D-c = 1.409g/cm(3) mu = 1.121 mm(-1), F(000) = 2465, R = 0.0539, R-w = 0.1380 for 4293 reflections with I >2 sigma (I). The bond lengths of Cu(1) - N(1), Cu(1) - N(2), Cu(1) - N(3) and Cu(1) - N(4) are 2.223(3), 2.017(3) , 2.013(3) and 2.038(3) Angstrom, respectively. The distance from copper to pyridine N(5) is 2.012(3) Angstrom. The angles N(2) - Cu(1) - N(3) and N(4 ) - Cu(1) - N(5) are 176.1(1) degrees and 160.9(1)degrees, respectively. Th e angles between axial position nitrogen atom N (1) and four square positio n nitrogen atoms N(2), N(3), N(4), N(5) are 79.3(1), 98.3(1), 90.7(1), 108. 4(1)degrees, respectively.