The crystal structure of the title compound has been determined from three-dimensional X-ray data collected on Weissenberg photographs, using CuKα radiation. The intensities were estimated visually with a standard scale. The structure was solved by the heavy-atom method and refined by the least-squares method. The final R value was 0.118 for 1835 observed reflections. The space group is C2/c, with a=22.58(2), b=7.23(1), c=16.58(2) Å, β=123.6(1)°, and Z=4. The crystal is composed of [Cu(H2O)(phen)2]2+ cations with C2-symmetry and NO3− anions. The copper atom is surrounded by four nitrogen atoms of the two phenanthroline ligands (average Cu–N=2.01 Å) and a water-oxygen atom (Cu–O=2.18 Å) in a distorted trigonal-bipyramidal arrangement. One oxygen atom and two nitrogen atoms of two different phenanthroline ligands are coplanar with the central copper atom, and lines linking the copper atom with each of the axial nitrogen atoms make angles of about 10°, with the normal to the basal N–N–O plane. The electronic reflectance spectrum of this complex shows a characteristic band at about 12.5×103 cm−1, which is analogous to that of [CuI(bipy)2]I.
The crystal data for p-nitrobenzylidene-p-dimethylaminoaniline (I) are: monoclinic, space group P21/c; a= 11.065 (2), b=7.759 (2), c= 16.488 (2)/~,, fl= 106"53 (3) °, Z=4. The crystal data for p-dimethylaminobenzylidene-p-nitroaniline (II) are: triclinic, space group P]'; a=9.509 (1), b= 16.200 (1), c= 9-505 (1) ~, e=91.69 (1), fl= 107.52 (1), 9,= 101"04 (1) °, Z=4 (two independent molecules in the asymmetric unit). The intensity data were collected on a four-circle diffractometer using Zr-filtered Mo Ke radiation. The structures were refined by a block-diagonal least-squares method to R indices of 0.081 for (I) and 0.070 for (II). The molecule (I), as a whole, is in a nearly planar conformation, and (II) in a non-planar one. The twist angles of the aniline ring out of the C-N=C-C plane are 9.2 ° for (I), and 41.5 and 49.0 ° for (II). The twist angles of the benzylidene ring range from 4.1 to 11"4 °.
The crystal of the title compound is monoclinic, with a=19.099(6), b=8.100(3), c=16.177(5) Å, β=100.54(5)°, the space group of C2/c, and Z=4. The structure was determined from the counter data and was refined to R=0.083 for 1736 non-zero reflections. The coordination geometry of the copper atom is best described as a distorted trigonal bipyramid, in which the equatorial plane is composed of Cu, two N, and water O atoms, and the axial positions are occupied by two N atoms. The complex has a crystallographically imposed twofold axis which passes through the copper and the water oxygen atoms at the equatorial plane. The two phenanthroline ligands are related with each other by this axis.
The structure of bis(2,2′-bipyridine)copper(II) perchlorate, Cu(bipy)2(ClO4)2, has been determined from three-dimensional X-ray data collected by the photographic method. The compound forms triclinic crystals with a=7.44(1), b=14.93(1), c=15.32(1) Å, α=136.3(0.1), β=103.7(0.1), γ=83.2(0.1)°, and Z=2 in the space group P\bar1. The structure was solved by the usual Patterson and Fourier techniques and was refined by the least-squares method to an R value of 0.134. The crystal is composed of an infinite chain of [Cu(ClO4)(bipy)2+]∞ and ClO4−; a perchlorate ion in the chain bridges two adjacent copper atoms through its two oxygen atoms. Roughly speaking, the coordination polyhedron around the copper atom is a tetragonally-distorted octahedron; the four nitrogen atoms of bipyridine molecules are arranged in a flattened tetrahedral manner (average Cu–N=1.99 Å), the least-squares plane of these atoms making an equatorial plane, while the polar positions are occupied by the two oxygen atoms of perchlorate anions, the Cu–O distances being 2.45 and 2.73 Å. The two pyridine rings are twisted slightly to each other in both of the bipyridine molecules; the dihedral angle between the pyridine planes is 13° in one bipyridine ligand and 4° in the other.
The crystal structure of the title compound has been determined from three-dimensional X-ray data. The crystal is composed of the nitrate anions and the distorted-octahedral [Cu(NO3)(H2O)3(bipy)]+ cations, where the nitrato-groups act as a monodentate ligand and the three coordinated water molecules occupy a facet of the octahedron.
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