Crystal Structure of Monoaquobis (1,10-phenanthroline)nickel(II) Chloride
Analytical Sciences X-ray Structure Analysis Online
The transition metal complexes with polypyridyl bridging ligands are of considerable interest because of their potential as building blocks for supramolecular assemblies directed by either metal coordination or other intermolecular electronic interactions. 1 Polypyridyl ligands such as phenanthroline and bipyridine can act as a bridge or node to assemble multidimensional supramolecular architecture through polydentate ligands or aromatic ring stacking and hydrogen bonds. 2 Here, we report a
... re, we report a mononuclear nickel complex [Ni(phen)2(H2O)Cl]Cl·H2O·CH3CN, in which the anion groups are self-assembled via hydrogen bonds while the aromatic rings groups are stacked via π-π interactions, giving the twodimentional structure. The title compound was prepared by a homogenized mixture of NiCl2·2H2O and phenanthroline. The mixture was ground in a agate mortar with a pestle at room temperature. Light blue crystals suitable for X-ray analysis were obtained by recrystallization from CH3CN solution. A blue cubic crystal with dimensions of 0.20 mm × 0.30 mm × 0.35 mm was mounted on a BRUKER SMART 1000 CCD diffractometer equipped with a graphite monochromator for data collection. The determination of unit cell parameters and data collections were performed with Mo Kα radiation (λ = 0.71073 Å). A total of 5268 reflections (4416 independent ones) with Rint = 0.0201 and 3296 observed reflections with I > 2σ(I) were collected in the range of 1.77 < θ < 25.02˚ by an ω/θ scan mode at 293(2)K. All data were corrected by using SADABS method. The structure was solved by direct methods with SHELXS-97 program. 3 The final refinement was performed by full-matrix least-squares methods with anisotropic thermal parameters for non-hydrogen atoms on F 2 . Ni(II) atom in the complex was located from E-maps. The hydrogen atoms were added theoretically, riding on the concerned atoms and being refined with fixed thermal factors. The weighting scheme was w = 1/[σ 2 (Fo 2 ) + (0.0743P) 2 ], where P = (Fo 2 + 2Fc 2 )/3. The refinement converged to the final R = 0.0471 and wR = 0.1184. S = 1.022. Molecular graphics were drawn with the program package XP. Crystallographic data and experimental details for structural analyses are summarized in Table 1 . Positional parameters and atomic coordinates are given in Table 2 , whereas the selected bond distances and angles are listed in Table 3 , respectively. The ORTEP view of the title complex with atom labeling is shown in Fig. 2(a) . It consists of a discrete [Ni(II)(phen)2(H2O)Cl] + cation and the uncoordinated Clanion, H2O and CH3CN molecules. The Ni(II) center is coordinated with four nitrogen donors of organoamine ligand phenanthroline, which thus binds metal ion in a bidentate x63 ANALYTICAL SCIENCES 2004, VOL. 20 X-ray Structure Analysis Online The title complex [Ni(phen)2(H2O)Cl]Cl·H2O·CH3CN (phen = 1,10-phenanthroline) has been synthesized in solid phase reaction and characterized by X-ray diffraction analysis. The Ni(II) center is six-coordinated in a distorted octahedral geometry. The complexes form a dimeric structure through the two O-H···Cl hydrogen bonds, and neighboring π-π interactions link the dimer segments into a quasi-two-dimensional structure.