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1.  Synthesis, Structure, and Antiproliferative Activity of Three Gallium(III) Azole Complexes 
As part of our interest into the bioinorganic chemistry of gallium, gallium(III) complexes of the azole ligands 2,1,3-benzothiadiazole (btd), 1,2,3-benzotriazole (btaH), and 1-methyl-4,5-diphenylimidazole (L) have been isolated. Reaction of btaH or btd with GaBr3 or GaCl3 resulted in the mononuclear complexes [GaBr3(btaH)2] (1) and [GaCl3(btd)2] (2), respectively, while treatment of GaCl3 with L resulted in the anionic complex (LH)2[GaCl4] (3). All three complexes were characterized by single-crystal X-ray crystallography and IR spectroscopy, while their antiproliferative activities were investigated against a series of human and mouse cancer cell lines.
PMCID: PMC2913727  PMID: 20721278
2.  Hydrogen-Bonded Networks Based on Cobalt(II), Nickel(II), and Zinc(II) Complexes of N,N'-Diethylurea 
N,N'-diethylurea (DEU) was employed as a ligand to form the octahedral complexes [M(DEU)6]2+ (M=Co, Ni and Zn). Compounds [Co(DEU)6](BF4)2 (1), [Co(DEU)6](CIO4)2 (2), [Ni(DEU)6](CIO4)2 (3), and [Zn(DMU)6](CIO4)2 (4) have been prepared from the reactions of DEU and the appropriate hydrated metal(II) salts in EtOH in the presence of 2,2-dimethoxypropane. Crystal structure determinations demonstrate the existence of [M(DEU)6]2+ cations and CIO4− (in 2–4) or BF4− (in 1) counterions. The [M(DEU)6]2+ cations in the solid state are stabilized by a pseudochelate effect due to the existence of six strong intracationic N-H ⋯ O(DEU) hydrogen bonds. The [M(DEU)6]2+ cations and counterions self-assemble to form hydrogen-bonded 2D architectures in 2–4 that conform to the kgd (kagome dual) network, and a 3D hydrogen-bonded rtl (rutile) network in 1. The nature of the resulting supramolecular structures is influenced by the nature of the counter-ion. The complexes were also characterized by vibrational spectroscopy (IR).
PMCID: PMC2905724  PMID: 20689706
3.  Synthesis, X-Ray Structure, and Characterization of a Complex Containing the Hexakis(urea)cobalt(II) Cation and Lattice Urea Molecules 
The 12: 1 reaction of urea (U) with CoI2 in EtOH yielded the “clathrate-coordination” compound [CoU6]I2·4U (1). The complex crystallizes in the monoclinic space group P21/c. The lattice constants are a = 9.844(4), b = 7.268(3), c = 24.12(1) Å, and β=98.12(1)∘. The crystal structure determination demonstrates the existence of octahedral [CoU6]2+ cations, I- counterions, and two different types (two U1 and two U2) of hydrogen-bonded, lattice urea molecules. The [CoU6]2+ cations and the U1 lattice molecules form two-dimensional hydrogen-bonded layers which are parallel to the ab plane. The I- anions are placed above and below each layer, and are hydrogen bonded both to U1 molecules and [CoU6]2+ cations. Each U2 molecule is connected to a [CoU6]2+ cation through an N–H⋯O hydrogen bond resulting in a three-dimensional network. Room temperature magnetic susceptibility and spectroscopic (solid-state UV/Vis, IR, Raman) data of 1 are discussed in terms of the nature of bonding and the known structure.
PMCID: PMC2235932  PMID: 18288263
4.  A Mononuclear and a Mixed-Valence Chain Polymer Arising from Copper(II) Halide Chemistry and the Use of 2,2′-Pyridil 
Reactions of 2,2′-pyridil (pyCOCOpy) with CuCl2 · 2H2O and CuBr2 in EtOH yielded the mononuclear complex [Cu(pyCOOEt)2Cl2] · H2O (1) and the one-dimensional, mixed-valence complex [Cu2ICuII(pyCOOEt)2Br4]n (2), respectively. Both complexes crystallize in the triclinic space group P 1¯. The lattice constants are a = 8.382(2), b = 9.778(2), c = 7.814(2), α = 101.17(1), β = 114.55(1), γ = 94.14(1)° for 1 and a = 8.738(1), b = 9.375(2), c = 7.966(1), α = 79.09(1), β = 64.25(1), γ = 81.78(1)° for 2. 2,2′-pyridil undergoes a metal-assisted alcoholysis and oxidation leading to decomposition and yielding the ethyl picolinate (pyCOOEt) ligand. The autoredox process associated with the reduction of copper(II) to copper(I) in the case of complex 2 is discussed in terms of the increased redox activity of the copper(II) bromide system relative to the copper(II) chloride system.
PMCID: PMC1939912  PMID: 18253464

Results 1-4 (4)