Co-crystallization of C-propyl-pyrogallolarene (PgC3) with 4,4′-bipyridine (bpy) in ethanol afforded a multi-component complex (PgC3) · 3(bpy) ·(EtOH) (1) that consists of a one-dimensional brick-wall framework, which was formed by four pyrogallolarene molecules and two juxtaposed bpy molecules, entrapping two other bpy molecules as guests within each cavity. Heating a mixture of PgC3 and trans-1,2-bis-(4-pyridyl)ethylene (bpe) in an ethanol-water mixed solvent allowed the isolation of a multi-component complex (PgC3) ·(bpe) · 2(EtOH) ·(H2O) (2), which has a two-dimensional wave-like polymer structure with the bpe molecules embedded in the wave trough between two PgC3 molecules. Single-crystal X-ray crystallography was utilized to investigate the hydrogen bonding networks of the multi-component complexes 1 and 2.
Ag2CdSnS4 was synthesized by a two step mechanochemical synthesis route. From a detailed analysis of the observed reflections in the X-ray powder diffraction pattern, the crystal structure proposed in the literature (space group Cmc21 [E. Parthé, K. Yvon, R. H. Deitch, Acta Crystallogr.1969, B25, 1164–1174; O. V. Parasyuk, I. D. Olekseyuk, L. V. Piskach, S. V. Volkov, V. I. Pekhnyo, J. Alloys Compd.2005, 399, 173–177]) is questionable. Our structural investigations presented in this contribution point to the fact that Ag2CdSnS4 crystallizes in the monoclinic wurtzkesterite-type structure (space group Pn). At around T = 200°C, a phase transition to the orthorhombic wurtzstannite-type structure (space group Pmn21) is observed.
A new polymerizable naphthalene derivative has been designed, prepared, and characterized by 1H, 13C NMR, and MS. The new monomer synthesis has successfully been accomplished from a cheap commercially available raw material, in only four steps with good yields. The four steps can be easily scaled up for manufacturing purposes. It is anticipated that the new precursor can be very useful in the preparation of valuable materials with high refractive index for numerous opto-electronic applications.
Condensation of 3,6-dichloropyridazine or 3,6-dichloro-4,5-dimethyl- pyridazine with 3-methyl-1H-pyrazole or 4-methyl-1H-pyrazole with the assistance of sodium metal in tetrahydrofuran at reflux afforded three 3,6-bis(pyrazolyl)- pyridazine-type ligands: 3,6-bis(3-methylpyrazolyl)pyridazine (L1), 3,6-bis(4-methyl- pyrazolyl)pyridazine (L2) and 4,5-dimethyl-3,6-bis(4-methylpyrazolyl)pyridazine (L3). Reactions of cis-[RuCl2(bpy)2] · 2H2O (bpy = 2,2′-bipyridine) and L1, L2 or L3 in the presence of NH4PF6 produced the heteroleptic cationic ruthenium(II) complexes [Ru(L1)(bpy)2](PF6)2 (1), [Ru(L2)(bpy)2](PF6)2 (2) and [Ru(L3)(bpy)2](PF6)2 (3), respectively. The three complexes have been characterized by UV/Vis and luminescence spectroscopy. The crystal structures of 1 · EtOH, 2 · EtOH and 3 have been determined by single-crystal X-ray diffraction.
A new metal-organic framework, [Pb(hmpcaH)2]n (1), has been hydrothermally synthesized from Pb(OAc)2 · 3H2O and 2-hydroxy-6-methylpyridine-4-carboxylic acid (hmpcaH2; 2), and characterized by IR spectroscopy, elemental and thermogravimetric analysis, and single-crystal X-ray diffraction. In complex 1, each hmpcaH− ligand represents a three-connected node to combine with the hexacoordinated Pb(II) ions, generating a 3D binodal (3,6)-connected ant network. The crystal structure of 2 was determined. The solid-state fluorescence properties of 1 and 2 were investigated.
A new Cu(II) metal-organic framework, [Cu(BMIOPE)(Br-BDC)]n (1) [Br-H2BDC = 5-bromo-isophthalic acid, BMIOPE = 4,4′-bis(2-methylimidazol-1-yl)diphenyl ether], has been hydrothermally synthesized and characterized through IR spectroscopy, elemental and thermal analysis, and single-crystal X-ray diffraction. Complex 1 possesses a unique two-fold interpenetrating two-dimensional framework with sql topology. The photocatalytic property of complex 1 for oxidative degradation of methyl orange and methylene blue with hydrogen peroxide was examined under UV irradiation.
Reaction of 1,4-bis(benzo[d]oxazol-2-yl)butane (BBO) with [Ag(CH3CN)4(ClO4)] afforded a new binuclear silver(I) complex, with composition [Ag2(BBO)2(ClO4)2], characterized by elemental analysis, UV/Vis and IR spectroscopy, and single-crystal X-ray diffraction. The results show that the Ag(I) complex consists of a centrosymmetric dimetallacyclic structure assembled from two Ag(I) atoms and two bridging BBO ligands. The coordination environment of silver(I) complex can be described as distorted trigonal planar, with one oxygen atom from a perchlorate anion and two nitrogen atoms from two BBO ligands. The luminescence properties of the ligand and the Ag(I) complex were studied in the solid state. The emission peaks of the Ag(I) complex are attributed to ligand-centered transitions. There is no effect of the complexation except for a partial quenching. The cyclic voltammograms of the Ag(I) complex indicated an irreversible Ag+/Ag couple.
The synthesis, characterisation and properties of several divalent metal complexes (Co, Ni, Pd) containing 2-oxazoline ligands L1–L3, appended with long chain alkyl and/or ester groups, is reported. The X-ray crystal structure aspects of one such complex, trans-PdCl2(rac-2-heptadecyl-4,5-dihydro-5-methyl-2-oxazole)2 (i.e. PdCl2(L1)2: 3), is described. This latter material contains one of the longest alkyl chains to be crystallographically characterised appended to an oxazoline ligand. The complexes reported herein represent the first transition metal derivatives of these high molecular weight, long chain and presumably low polarity monodentate oxazoline ligands. A combination of spectral and theoretical calculations (semi-empirical PM6(tm) level of theory) are used to support the proposed structure in the case of the hydrates of NiCl2 and CoBr2 complexes derived from L1. A trio of PdCl2 complexes of the ligand set are likewise detailed. Complex 3 is shown to be a useful pre-catalyst for the promotion of a Heck coupling reaction between bromobenzene and styrene under typical conditions.