Zhong-Feng Li

Tris(2,2'-bi-1H-imidazole-κN,N)-nickel(II) dinitrate N,N-dimethyl-formamide monosolvate.

The reaction of nickel salts and 4,4′-bipyridine with 2,2′-biimidazole (H2biim) yielded the title complex, [Ni(C6H6N4)3](NO3)2·C3H7NO. The NiII atom is chelated by three H2biim ligands in a distorted octahedral coordination geometry. The two nitrate anions and one dimethylformamide (DMF) molecule are not coordinated. The compound has a three-dimensional structure, formed by extensive hydrogen bonding between [Ni(H2biim)3]2+ cations and nitrate anions, each nitrate anion forming hydrogen bonds with an R 1 2(4) motif. The DMF molecule is disordered over three sets of sites, with occupancy ratios of 0.341 (16):0.350 (17):0.309 (19).

Lanthanide contraction and chelating effect on a new family of lanthanide complexes with tetrakis(O-isopropyl)methyle-nediphosphonate: synthesis, structures and terahertz time-domain spectroscopy

Sixteen lanthanide–diphosphate complexes [LnL2(H2O)4Cl]Cl2 (Ln = La3+ for 1, Ln = Ce3+ for 2), [LnL2(H2O)4]Cl3·6H2O (Ln = Nd3+ for 3, Ln = Sm3+ for 4, Ln = Eu3+ for 5, Ln = Gd3+ for 6, Ln = Tb3+ for 7, Ln = Dy3+ for 8, Ln = Er3+ for 9), {[LaL2(H2O)4Cl]Cl2}2 (10), [PrL2(OH)2(H2O)Cl] [PrL2(H2O)4Cl]Cl2 (11), [LaL2(H2O)5Cl]Cl2·2H2O (12), [YbL2(H2O)3Cl]Cl2·H2O (13), [NdL2(H2O)3Cl]Cl2·3H2O (14), [HoL2(H2O)Cl2]Cl·H2O (15), [Sc2L2(H2O)4(OH)2]Cl4·4H2O·2CH3OH (16) (L = tetrakis(O-isopropyl)methylenediphosphonate) have been synthesized by the reaction of lanthanide chlorides and L ligand in the solvent of acetonitrile (with ethanol or DMF) at room temperature. The title complexes were characterized by IR, elemental analysis, single-crystal X-ray diffraction analysis, thermal analysis, 1HNMR and 31PNMR spectroscopy. Complexes 1–15 are mononuclear complexes and complex 16 is a binuclear cluster complex. Complex 12 is the intermediate of complex 1. Complexes 11–13 display a one-dimensional chain formed by hydrogen bonds and the structures of complexes 14, 16 can be simplified as two-dimensional mesh 63 topology formed by hydrogen bonds. In those lanthanide complexes, the lanthanide ion with an atomic number smaller than Pr element tends to form a nine-coordinated structure and that with the atomic number larger than Pr element tends to form an eight or lower number-coordinated structure. Pr element has two kinds of coordination situations, with coordination numbers of nine or eight. The terahertz (THz) time-domain spectra of these complexes were also studied.

Crystal structure of (μ-(bis(diphenylphosphino)ethane dioxide-kO,O′)-bis([2,3-f]-pyrazino-[1,10]phenanthroline-2,3-dicarbonitrile-kN,N′)- bis(dibromido)dicopper(II) — acetonitrile (1:2.5), [Cu2(C26H24P2O2)(C16H6N6)2Br4] · 2.5CH3CN

C63H43.50Br4Cu2N14.50O2P2, monoclinic, C12/c1 (no. 15), a = 31.63(3) Å, b = 9.680(1) Å, c = 24.650(2) Å, + = 119.995(2)°, V = 6536.7 Å, Z = 4, Rgt(F) = 0.056, wRref(F ) = 0.164, T = 298 K.

Crystal structure of bis(triphenylphospine-kP)-dichloropalladium( II) —acetonitrile (1:1), [PdCl2(C18H15P)2] · CH3CN

C38H33Cl2NP2Pd, monoclinic, C12/c1 (no. 15), a = 12.056(1) Å, b = 14.393(1) Å, c = 20.002(2) Å, * = 92.372(1)°, V = 3467.8 Å, Z = 4, Rgt(F) = 0.070, wRref(F ) = 0.178, T = 298 K.

Crystal structure of (μ-bis(diphenylphosphino methane-)k2P,P'))-bis(1,10- phenanthroline-) k2N,N')-bis(thiocyanate-)N)copper(I) — water (1:0.25), [Cu2(C25H22P2)(C12H8N2)2(CNS)2]2 · 0.5H2O

C102H77Cu4N12O0.5P4S4, monoclinic, C12/c1 (no. 15), a = 44.599(3) Å, b = 9.769(1) Å, c = 22.370(2) Å, / = 110.832(2)°, V = 9109.0 Å, Z = 4, Rgt(F) = 0.049, wRref(F ) = 0.142, T = 298 K.