Inorganic Chemistry Communications (v.6, #12)

Contents List (iii-iv).

A novel inclusion crystal, {[Rh(II)2(bza)4(pyz)] n  · 3n(N2O)} (1), was prepared and characterized by single-crystal X-ray diffraction analysis; linear alignment (N2O) n coherently generates in the channels of host rhodium benzoate pyrazine and there is a high possibility of the existence of an intermediate phase induced by a slight amount of adsorbed N2O inside the crystal even at room temperature.
Keywords: Phase transition; Host–guest inclusion; Crystal structure; Gas adsorption; One-dimensional polymer;

We report a new synthesis of Au2S3 by a sonochemical reaction between Au(CH3COO)3 and S in decalin at room temperature in nitrogen atmosphere. When gold acetate is sonicated under similar conditions without the presence of sulfur, nanocrystalline gold is formed. The products were characterized by X-ray powder diffraction, transmission electron microscope and thermal analysis (TG and DSC). The synthesis procedure is substantially simpler than the previously reported methods.
Keywords: Sonochemical reaction; Sulfides; Nanostructures;

The role of reaction medium on the coordination environment of terbium in complexes with 4-acylpyrazol-5-ones by Claudio Pettinari; Riccardo Pettinari; Fabio Marchetti; Andrey Drozdov; Ivan Timokhin; Sergey Semenov; Sergey I. Troyanov (1423-1425).
[Tb(Q)3(H2O)] and [Tb(Q)3(H2O)(EtOH)] derivatives of novel 1-phenyl-3-methyl-4-R-pyrazol-5-one (HQ=HQCP: R=cyclopentylcarbonyl, HQETCP: R=cyclopentylpropionyl) have been prepared and shown to be seven- and eight-coordinate, respectively, by IR, X-ray and elemental analyses. The role of the reaction medium on the coordination number of Tb is discussed.

A novel 3D structure of Ag-1,4-cyclohexanedicarboxylate coordination framework by Wenhua Bi; Rong Cao; Daofeng Sun; Daqiang Yuan; Xing Li; Maochun Hong (1426-1428).
A novel 3D polymeric complex, [Ag(chdc)0.5] n (1), (H2chdc = 1,4-cyclohexanedicarboxylate acid), was synthesized by self-assembly reaction of H2chdc with Ag(I) ions. The most interesting characteristic of 1 is that the distribution of Ag(I) ions in the crystal is similar to the carbon atoms in a layer of graphite.
Keywords: Crystal structure; 3D framework; Self-assembly; Ag(I) polymer;

A novel 3D network coordination polymer consisting of paddlewheel Co3 clusters connected by PO4 and 4-pyridinecarboxylate by Xiao-Guang Zhou; Zhan-Gang Han; Jun Peng; Jie-Sheng Chen; En-Bo Wang; Chun-Gui Tian; Li-Ying Duan; Ning-Hai Hu (1429-1432).
The synthesis, structural characterization and preliminary magnetic studies of a novel coordination polymer with paddlewheel Co3 clusters are reported firstly. In the polymer, Co3 clusters are covalently linked through PO4 tetrahedra and 4-pyridinecarboxylate (4-pya) ligands into interpenetrated three-dimensional network.
Keywords: Hydrothermal synthesis; Crystal structure; Co3 clusters; 4-Pyridinecarboxylate;

A novel 2D polymeric structure of Cu–Na complex, in which phthalate gives seven coordination sites by Xuanwen Liu; Chengzhi Xie; Xiaoqing Wang; Guangqiu Shen; Dezhong Shen (1433-1435).
A novel copper and sodium hetero-nuclear complex {[(H2O)Na]2Cu(phth)2} n (phth=phthalate) was synthesized and its crystal structure has been determined by X-ray diffraction methods. The complex structure consists of two-dimensional (2D) infinite layers, in which it is first observed that one phthalate ligand coordinates to five metal ions and gives seven coordination sites.
Keywords: Crystal structure; Cu–Na hetero-nuclear complex; 2D coordination layer; Phthalate acid;

Synthesis and spectroscopic investigation of the pyrazole complexes. The X-ray structure of [ReOBr3(OAsPh3)(pzH)] by B Machura; J.O Dzięgielewski; R Kruszynski; T.J Bartczak; J Kusz (1436-1440).
The [ReOX3(OAsPh3)(AsPh3)] complexes react with pyrazole in dry tetrahudrofuran to give new monomeric oxo rhenium(V) complexes – [ReOX3(OAsPh3)(pzH)]. This paper presents synthesis and spectroscopic characterisation of [ReOX3(OAsPh3)(pzH)] compounds and X-ray structure of the bromine analogue.
Keywords: Rhenium(V); Oxo; Pyrazole; Arsine complex;

The reaction of CuSO4  · 5H2O with 4,4-bipyridine and malic acid at 140 °C under solvothermal conditions afforded a mixed valence three-dimensional coordination polymer [CuICuII 2(mal)(SO4)(bpy)2  · H2O] n , (1). The building unit consists of a Cu2+-dimer in which copper centers are bridged by malate and sulphate anions. SO4 2− anion further connects dimeric unit with the Cu1+ center. Building units are linked by 4,4-bipyridine ligands to form double chains, that are interconnected into 3D network through additional sulphate bridge.
Keywords: Mixed-valence copper complex; Malate anion; μ4-Sulphate bridge; Bipyridine; Polymeric structure; Solvothermal synthesis;

Controllable growth of In(OH)3 nanorods with rod-in-rod structure in a surfactant solution by Xian-Hua Zhang; Su-Yuan Xie; Zi-Mian Ni; Xuan Zhang; Zhi-Yuan Jiang; Zhao-Xiong Xie; Rong-Bin Huang; Lan-Sun Zheng (1445-1447).
The In(OH)3 nanorods (25–55 nm in diameter and 120–200 nm in length) bearing parallel subunit nanorods (diameters ranging from 8 to 10 nm) were synthesized by controlling hydrolysis of indium nitrate in the presence of hexamethylene tetraamine and cetyltrimethylammonium bromide.
Keywords: Nanorods; Indium hydroxide; Surfactant; Template;

One novel dysprosium coordination polymer [Dy(PIC)3(H2O)2]n (HPIC = pyridine-4-carboxylic acid) has been synthesized. X-ray analysis reveals that it forms the chain-like molecular structure through the bridged oxygen atoms of the carbonyl groups. The title coordination polymer crystallizes in the monoclinic system, space group C2/c, with lattice parameters: a=20.243(9) Å, b=11.576(5) Å, c=9.834(4) Å, β=110.601(2)°, V=2078(2) Å3, D c=1.805 mg/m3, Z=4, F(000)=1100, GOF = 1.11, R1=0.0404. The photophysical property has been studied with ultraviolet absorption spectrum, excitation and emission spectrum. The luminescence spectra show the stronger blue emission than yellow emission.
Keywords: Dysprosium (III); Chain-like coordination polymer; Molecular structure; Photophysical property;

Two copper(I) iodide complexes with polydentate bis(ethylamidophosphine) ligands were synthesized, characterized with crystal structures. They include a dimeric complex [Cu(μ-I)(CH2NHCOC2H4PPh2)2]2 1 containing a planar Cu2I2 rhombohedron with two doubly bridged ligands and a tetrameric complex {Cu4(μ-I)4[(CH2NHCOC2H4PPh2)2]2} 3 with all the coppers and iodines forming a highly distorted cubane geometry.
Keywords: Copper(I) iodide complex; Bis(ethylamidophosphine); Cubane; Crystal structure;

Ten-vertex osmamonocarbaboranes via arachno and nido {CB9} monocarbaboranes. Polyhedral contraction promoted by [OsCl2(PPh3)3] in MeOH and the crystal and molecular structure of [1-H-1,1-(PPh3)2-2-Ph-3-(OMe)-isocloso-1,2-OsCB8H7] by Vitalii E. Konoplev; Irina V. Pisareva; Eugenii V. Vorontsov; Fedor M. Dolgushin; Andreas Franken; John D. Kennedy; Igor T. Chizhevsky (1454-1458).
Reactions of [OsCl2(PPh3)3] 1 with the [NEt4]+ salts of the [6-Ph-nido-6-CB9H11] anion 2 and the [arachno-6-CB9H14] anion 3 each proceed selectively in methanol solution with the elimination of one boron-containing fragment from the starting cluster polyhedron, yielding together a short series of three novel 10-vertex hydridoosmamonocarbaboranes of isocloso {OsCB8} cluster geometry.
Keywords: Borane cluster; Isocloso geometry; Metallamonocarbaborane; Carbaborane; Monocarbaborane; Cluster-dismantling reaction; X-ray structure; NMR spectroscopy;

Surfactant-assisted growth and characterization of CdS nanorods by Qitao Zhao; Lisong Hou; Ruian Huang; Shuzhi Li (1459-1462).
Well-defined CdS nanorods were synthesized using hydrothermal process with ethylenediamine as a bidentate ligand to form Cd2+ complexes and polyoxyethylene 20 cetyl ether providing an effective control over the crystal uniformity of CdS nanorods. The photoluminescence (PL) spectrum of the nanorods indicated that they have potential applications in light-emission devices.
Keywords: Nanorods; CdS; Surfactant-assisted; Synthesis; Microstructures; Photoluminescent properties;