Inorganic Chemistry Communications (v.7, #4)

Contents list (iii-vi).

Synthesis of Cu(II) aminoalkoxide complexes and their unusual thermolysis to Cu(0) by Jung Woo Park; Hong Suk Jang; Minchan Kim; Kiwhan Sung; Sun Sook Lee; Taek-Mo Chung; Sangman Koo; Chang Gyoun Kim; Yunsoo Kim (463-466).
The “fluorine free” Cu(II) aminoalkoxide complexes Cu(OCMe2CH2NR2)2 (R=Me(I), Et(II)) are synthesized and characterized as a low melting solid (I) and a viscous liquid (II). The complexes are thermally decomposed at below 200 °C to produce metallic copper by unusual γ-hydrogen elimination reaction.
Keywords: Metal organic chemical vapor deposition (MOCVD); Aminoalkoxide ligands; Donor-functionalized ligands; Monomeric complexes; Crystal structure;

A novel 2D coordination polymer based on a copper(II) tetramer with p-sulfonated thiacalix[4]arene by Qian-Ling Guo; Wen-Xiang Zhu; Song Gao; Shu-Lan Ma; Shu-Jing Dong; Miao-Qiong Xu (467-470).
X-ray structural determination of the title complex shows it containing a phenoxy and sulfato-bridged Cu(II) tetramer coordinating to fully deprotonated p-sulfonated thiacalix[4]arene with its cavity occupied by a pyridinium cation and forming a 2D coordination polymer. Variable temperature susceptibility measurement reveals an antiferromagnetic coupling of four Cu(II) ions formed.
Keywords: Crystal structure; 2D Coordination polymer; Copper tetramer; p-Sulfonated thiacalix[4]arene;

A new 1-D mercury iodide coordination polymer [Hg(bpfb)I2]n  · 2DMF (bpfb=N,N-bis(4-pyridylformamide)-1,4- benzene) was prepared and characterized. Its optical responses to the incident light exhibit strong three-order nonlinear optical absorptive and refractive effects with α 2=3.148×10−16 m2 W−1 and n 2=6.854×10−18 m2 W−1 in a 2.48 × 10−4 mol dm−3 DMF solution. We find that a polymeric adduct may give better NLO properties than a monomeric adduct.A new 1-D mercury iodide coordination polymer [Hg(bpfb)I2] n  · 2DMF (1) (bpfb=N,N -bis(4-pyridyl formamide)-1,4-benzene) was prepared. Its optical responses to the incident light exhibit strong three-order nonlinear optical absorptive and refractive effects with α 2=3.148×10−16 m2 W−1 and n 2=6.854×10−18 m2 W−1 in a 2.48 × 10−4 mol dm−3 DMF solution, and we find that a polymeric adduct may give better NLO properties than a monomeric adduct.
Keywords: Mercury (II) complex; Crystal structure; Nonlinear optical properties;

Synthesis and structure of a new layered zinc phosphate [C6N2H16]3.5[Zn14(PO4)7(HPO4)7] in the presence of trans-1,4-diaminocyclohexane by Yan Xing; Guanghua Li; He Meng; Zhan Shi; Yunling Liu; Xinghui Wei; Yulin Yang; Wenqin Pang (475-477).
A novel two-dimensional layered zinc phosphate [C6N2H16]3.5[Zn14(PO4)7(HPO4)7], I, has been synthesized hydrothermally using trans-1,4-diaminocyclohexane(trans -1,4-DACH) as the structure-directing agent. The structure of I comprises a network of ZnO4, PO4, and PO3(OH) tetrahedral forming one-dimensional tubes. The tubes, in turn, are linked via oxygen atoms forming macroanionic inorganic layers.
Keywords: Hydrothermal synthesis; Zinc phosphate; Layer structure; Trans-1,4-diaminocyclohexane;

Synthesis and characterization of the first aryltellurium(II) halide complex stabilized by a Te–Te bond from a tellurium ether by Gabriela N. Ledesma; Ernesto Schulz Lang; Ezequiel M. Vázquez–López; Ulrich Abram (478-480).
(MesTe)2 reacts with equivalent amounts of iodine to produce a crystalline powder. Attempts to crystallize mesityltellurenyl monoiodide (MesTeI) were unsuccessful and we always obtained Mes(I)Te(TeMes2) from the recrystallization of the crude solid. The structure of the new organotellurium(II) halide has been studied by means of single crystal X-ray diffractometry. The three-centre system Te2–Te1–I1 is approximately linear, suggesting the occurrence of a charge transfer complex. The geometry about the Te1 atom is a distorted T-shape, indicating the presence of a stereochemically active lone pair.
Keywords: Organotellurium(II) halide; X-ray structure; Tellurium–tellurium bond;

A general synthetic approach to the design of bis(ethylamine) derivatives of single amino acid chelates has been developed. In general, protection of diethylenetriamine as the phthalimide, followed by reaction with the appropriate bromoalkylcarboxylate and deprotection, yields the bifunctional reagents (H2NCH2CH2)2N–R–CO2H. Reaction of the bis(aminoethyl)aminovaleric acid derivative with (NEt4)2[Re(CO)3Br3] in methanol yields [Re(CO)3{(H2NCH2CH2)2N(CH2)4CO2Me}]Br (1Br), the first example of the {Re(CO)3}+ core ligated to exclusively aliphatic amine donors. Crystal data: C13H23BrN3O5Re (1Br), monoclinic P21/c, a=8.3419(5) Å, b=9.4018(6) Å, c=23.569(1) Å, β=99.165(1)°, V=1824.9(2) Å3, Z=4, D calc=2.065 g cm−3.
Keywords: Bifunctional chelates; {M(CO)3}+ core; Single amino acid chelates;

Efficient mechanochemical synthesis of tris(pyrazolylborate) complexes of manganese(II), cobalt(II) and nickel(II) by Sergey V Kolotilov; Anthony W Addison; Swiatoslaw Trofimenko; William Dougherty; Vitaly V Pavlishchuk (485-488).
A mechanochemical synthesis of Mn(II), Co(II) and Ni(II) tris(pyrazolylborates) (Tp) was developed, which enabled preparation of metal complexes of the type TpMCl and TpMCl · Hpz type (Hpz is the substituted pyrazole generated by hydrolysis of the corresponding Tp ligand). The X-ray structure of a new Co(II) tris(pyrazolylborate) and the electronic spectra of these coordination compounds are discussed.
Keywords: Mechanochemistry; Tris(pyrazolylborate); 3d-Metals; X-ray structure; Electronic spectra;

Action of triphenylphosphine on [Rh(HCOO)(PPh3)2(CO)]. A novel synthetic route to [HRh(PPh3)3(CO)] by Yuri S Varshavsky; Tatiana G Cherkasova; Ivan S Podkorytov (489-491).
Rhodium(I) carbonyl formato complex, trans-[Rh(HCOO)(PPh3)2(CO)], on heating in propanol-2 in the presence of excess triphenylphosphine converts into carbonyl hydride complex, [HRh(PPh3)3(CO)], with a good yield. The reaction provides a new and attractive method of synthesis of [HRh(PPh3)3(CO)].
Keywords: Rhodium; Format; Carbonyl hydride;

The intermediate [Zn(4-PTZ)2(H2O)4] (4-PTZ=5-(4-pyridyl N-oxide)tetrazolate) (1) in the synthesis of 4-H-PTZ (2) from cycloaddition reaction of 4-cyanopyridine N-oxide with NaN3 in water catalyzed by ZnCl2 was structurally characterized. The catalysis role of Zn2+ in the synthesis of tetrazole stems from the formation of tetrazolate zinc complex 1.
Keywords: Zinc; Tetrazole; Cycloaddition; Crystal structure;

Complexation and proton transfer by hydroxamic acids in model inhibited metallohydrolases: formation of metal hydroxamate trimers by D.A. Brown; G.J. Clarkson; N.J. Fitzpatrick; W.K. Glass; A.J. Hussein; T.J. Kemp; H. Müller-Bunz (495-498).
Reaction between the dimeric metal complexes, [M2(μ-OAcF)2(OAcF)2(μ-H2O)(tmen)2], M=Co(II), Ni(II), and aceto- and benzohydroxamic acids (AHA, BHA) gives the novel trimeric complexes, [M3(μ-OAcF)4(μ-RA)2(tmen)2], M=Co(II), Ni(II); RA=AA, BA, in which each hydroxamate bridges two metal centres via its deprotonated hydroxyl and the carbonyl oxygen bonds one metal centre only together with the doubly protonated salt [(tmen) · 2H][OAcF]2. In contrast, self-assembly from M(OAcF)2  · 4H2O, tmen and RHA gives the dibridged hydroxamate dimers [M2(μ-OAcF)(μ-RA)2(tmen)2] [OAcF].
Keywords: Crystal structures; Trinuclear cobalt; Nickel hydroxamates; Model inhibited complexes;

The dinucleating ligand 4,6-dimethyl-2-hydroxy-isophthalic acid, H3L, forms the tetracopper(II) complex Cu4L2(O2CCH3)2(py)4(CH3OH)2, 1. The single crystal X-ray structure of 1  · 2CH3OH reveals that this complex is a carboxylate bridged dimer of dinuclear copper(II) subunits, in which the copper(II) centres adopt square-based pyramidal geometries.
Keywords: Copper complexes; Carboxylate ligands; Tetranuclear complexes;

Acyclic tellurated Schiff base [4-MeOC6H4TeCH2CH2N=C(CH3)C6H4-2-OH (L 1 H)] has been synthesized by reacting 2-(4-methoxyphenyltelluro)ethylamine with o-hydroxyacetophenone. The L 1 H on reaction with Na2PdCl4 forms a complex [PdCl(L 1 )] in which the tellurated Schiff base coordinates in a tridentate mode. The proton and carbon-13 NMR spectra of L 1 H and the complex are characteristic. The single crystal structure of the complex is solved. The Pd–Te, Pd–Cl, Pd–O and Pd–N bond distances are 2.504(1), 2.290(4), 2.03(1) and 2.01(1) Å, respectively.
Keywords: Palladium; Acyclic tellurated Schiff base; Complex; Synthesis; Single crystal structure;

A novel route for the preparation of monodisperse silver nanoparticles via a pulsed sonoelectrochemical technique by Li-Ping Jiang; An-Ning Wang; Yu Zhao; Jian-Rong Zhang; Jun-Jie Zhu (506-509).
Monodisperse silver nanoparticles stabilized with PVP have been prepared in a saturated solution of silver citrate (Ag3C6H5O7) in the presence of poly(vinyl pyrrolidone) (PVP) by a pulsed sonoelectrochemical technique.
Keywords: Sonoelectrochemistry; Silver; Nanoparticles; PVP;

A novel metal-organic hybrid compound [Co(OOC(CH2)4COO)(4,4-bipy)] 1, has been hydrothermally synthesized and structurally characterized. Compound 1 exhibits a novel three-dimensional interpenetrating network with mixed adipate and 4,4-bipy ligands constructed by covalent bonds.
Keywords: Hydrothermal synthesis; Interpenetration; Metal-organic; Crystal structure;

Cleavage of the SiO–Si(CH3)2H bond in Si8O20[Si(CH3)2H]8 by Isao Hasegawa; Wataru Imamura; Toshio Takayama (513-515).
Si8O20[Si(CH3)2H]8 reacts with methanol or H2O, resulting in fission of the SiO–Si(CH3)2H bond. The double eight-membered ring silicate core of Si8O20[Si(CH3)2H]8 is retained during the reactions. Si8O20[Si(CH3)3]8 undergoes neither alcoholysis nor hydrolysis under the same reaction conditions, indicating that stability of the Si–O–Si bond depends on the type of functional groups attached to a Si atom.
Keywords: Silicate anion; Si8O20 8−; Silyl derivatives; Siloxane bond; Alcoholysis; Hydrolysis;

Reactions of pyridinum hydrogenmaleate with mononuclear oxohalomolybdates produced (PyH)3[Mo2O4X4(OOCCH=CHCOOH)] (X=Cl, Br), the first molybdenum(V) complexes with hydrogenmaleato ligand. The X-ray structure analysis revealed in both the {Mo2O4}2+ core with hydrogenmaleate in a μ2-bis(monodentate) binding mode forming a third bridge between a pair of molybdenum atoms linked by a single metal–metal bond. A pair of halo ligands completes a distorted octahedral environment of each metal in the {Mo2O4}2+ unit.
Keywords: Molybdenum; Dinuclear molybdenum(V) species; Dicarboxylato complexes; Hydrogenmaleato ligand;

A new compound [(Gly)2Cu][Na(H2O)4Cr(OH)6Mo6O18] · 9.5H2O 1, has been synthesized and structurally characterized. Compound 1 exhibits an unusual two-dimensional (2D) window-like network constructed from [Cr(OH)6Mo6O18]3− as building blocks, Na+ ions and Cu2+ coordination complexes as linkers, representing the first example of a 2D extended framework based on Anderson type polyanions.
Keywords: Organic–inorganic hybrid; Anderson type polyanions; Sodium ions; Copper (II) coordination complexes;

A novel bifunctionalized arylimido derivative of hexamolybdate, (Bu4N)2[Mo6O17(NAr)2]2− (Ar=o-CH3C6H4) 1, in which the two o-tolylimido groups are bounded to hexamolybdate at the cis positions, was synthesized by self-assembled metathesis of α-type octamolybdate ion and o-toluidine with DCC as a dehydration agent. The most interesting characteristic of 1 is that the cluster anions form dimers via the π–π stacking between one of its two phenyl rings, and four such dimers are linked in turn via C–H⋯O hydrogen bonding involving terminal hexamolybdate oxygen atoms into ring-like tetramers in the solid state.
Keywords: Polyoxometalates; Organoimido derivatives; DCC; Supramolecular assembly; Crystal structure;

The compounds Tl(hfac), Pb(hfac)2 and Bi(hfac)3 with hfac=hexafluoroacetylacetonate show a green phosphorescence (λ max≈500 nm) under ambient conditions. This emission which is facilitated by the heavy atom effect of the metals originates from the lowest-energy hfac intraligand triplet.
Keywords: Thallium compounds; Lead compounds; Bismuth compounds; Phosphorescence;

Synthesis, structure and electrical conductivity of (PyMe)[Ni(dmit)2]2 by Wen Xu; Qi Fang; Hong-Yu Chen; Gang Xue; Guo-Qun Liu; Wen-Tao Yu; Jin-Biao Zhang; Cui-Ying Xu; De-Qing Zhang; Dao-Ben Zhu (531-533).
A new molecular conductor (PyMe)[Ni(dmit)2]2 (PyMe = N-methylpyridinium, dmit = 2-thioxo-1,3-dithiole-4,5-dithiolato) has been synthesized and its structure been determined. The temperature-dependent conductivities in the range of 290–20 K reveal a semi-conducting behavior of the crystal with a small activation energy of 0.067 eV and a quite high room temperature conductivity of 2 S cm−1.
Keywords: Nickel complex; Synthesis; X-ray crystal structure; Semiconductors;

Alkyne oxidation by nonheme iron catalysts and hydroperoxides by Ju Yeon Ryu; Soonyoung Heo; Philsung Park; Wonwoo Nam; Jinheung Kim (534-537).
Alkynes were oxidized by hydrogen peroxide and tert-butyl hydroperoxide catalyzed by nonheme iron complexes under aerobic and anaerobic conditions: the formation of diketone and α,β-acetylenic oxidation products was significantly affected by the oxidants, and product yields were markedly influenced by the presence of O2.
Keywords: Nonheme iron complex; Hydroperoxide; Alkyne oxidation; Oxygen activation;

Synthesis and structures of two luminescent Zn(II) complexes with pyrazole and carboxylate ligands by Jing Li; Jian-Hao Zhou; Yi-Zhi Li; Lin-Hong Weng; Xue-Tai Chen; Zhi Yu; Ziling Xue (538-541).
Two new Zn(II) complexes with pyrazole and carboxylate ligands, [Zn(μ-pz)(pzH)(O2CCH2CH3)]2 (pzH = pyrazole), 1 and [Zn(bet)2(pzH)2](ClO4)2 (bet = Me3NCH2CO2), 2, were prepared and structurally characterized. Both compounds exhibit blue emission at room temperature in solid state.
Keywords: Zinc; Pyrazole; Betaine; Crystal structure; Luminescence;

The dilithium bis-azaallyl complex [CH2 =C(NAr)C(NAr)=CH2]Li2(THF)4 (Ar=2,6- i Pr2C6H3) was synthesized by the reaction of ArN=C(CH3)C(CH3)=NAr with 2 equiv. of lithium diisopropylamide. This complex exhibits good catalytic activity and stereoselectivity for the anionic polymerization of methyl methacrylate (MMA).
Keywords: Lithium amide; Synthesis; Crystal structure; Anionic polymerization; Methyl methacrylate;

AlN serrated nanoribbons synthesized by chloride assisted vapor–solid route by Ting Xie; Yu Lin; Guosheng Wu; Xiaoyou Yuan; Zhi Jiang; Changhui Ye; Guowen Meng; Lide Zhang (545-547).
A novel morphology of nanoribbons – serrated nanoribbons of pure crystalline AlN – was obtained by chloride assisted vapor–solid (VS) route, in which there exist some stacking faults. The growth direction of these serrated nanoribbons is along [0 0 1].
Keywords: Aluminum nitride; Nanoribbon; Stacking fault; Vapor–solid process;

Copper(II) salts react with 3,5-dinitrosalicylic acid to give complex of the composition [Cu3{3,5-(NO2)2sal2−}2{3,5-(NO2)2sal1−}2(H2O)4] · 4H2O (3,5-(NO2)2sal x=3,5-dinitrosalicylato anion). The complex was characterized by elemental microanalysis, electronic, IR and EPR spectra and magnetic susceptibility measurements and the crystal structure of the complex has been determined and refined. Structure of the complex comprises of the centrosymmetric [Cu3{3,5-(NO2)2sal2−}2{3,5-(NO2)2sal1−}2(H2O)4] molecules and the water molecules which are held together by system of different types of hydrogen bonds and van der Waals interactions. The Cu(1) atom is centrosymmetrically coordinated by two 3,5-dinitrosalicylato dianions, thus forming the square planar CuO4 chromophore. The satellite Cu(2) atom is coordinated by one oxygen atom of bridging 3,5-dinitrosalicylato dianion, two oxygen atoms of chelating 3,5-dinitrosalicylato monoanion (in the phenolato form), and by two water oxygen atoms in the square pyramidal coordination polyhedron. Variable-temperature magnetic susceptibility measurements (1.9–300 K) show the occurrence of significant ferromagnetic interactions caused by syn–anti conformation of carboxylato bridges within the trimer. The EPR spectroscopy is in agreement with the molecular structure of the complex and magnetic properties, indicating superposition spectra of copper centres (S=1/2) with square-planar and square pyramidal coordination polyhedrons (g =2.32, g =2.05).
Keywords: Copper; 3,5-Dinitrosalicylate complex; Crystal structure; Trimer; Spectral; Magnetic properties;

Rapid synthesis of nanocrystalline CeVO4 by microwave irradiation by Hao Wang; YongQiang Meng; Hui Yan (553-555).
Size-controlled CeVO4 nanoparticles have been synthesized by a simple microwave irradiation processing. The products were characterized by X-ray diffraction, transmission electron microscopy, and UV–Vis spectroscopy. The results showed that the size of as-synthesized CeVO4 powders was in the range of 6–18 nm and was extremely dependent on the solution pH value. The optical absorption measurements displayed the obvious quantum-size effect of the products.
Keywords: Nanomaterials; CeVO4; Microwave irradiation;

A novel dimeric pentamolybdate [4,4-H2bipy]3[4,4-Hbipy]2[(Mo5O17)2(4,4-bipy)], the first example of a 4,4-bipyridine bridging dumbbell-like polyoxomolybdates, has been prepared by hydrothermal synthesis and characterized by X-ray crystallography.
Keywords: Polyoxometalates; Hydrothermal synthesis; Crystal structure; Molybdenum;

The complex [Cu(C10H24N4)(ClO4)]ClO4, where C10H24N4=1,4-bis(3-aminopropyl)piperazine was synthesized and characterized, and its molecular structure was established by X-ray diffraction. The complex crystallizes in orthorhombic Pbca (no. 61) with Z=8, a=14.417(3) Å, b=15.067(3) Å, and c=16.101(3) Å. The structure consists of isolated [Cu(C10H24N4)(ClO4)]+ cations and perchlorate counter anions. The coordination geometry of the Cu(II) center may be described as square pyramidal (SP) with ClO4 group at the apical site and the N donor atoms of the neutral tetradentate ligand occupy the basal sites. The Cu–N bond distances are 2.069(4), 2.020(3) Å for the internal chelate rings, and 2.033(4) and 1.996(3) Å for the outer rings. The Cu–O(1) distance is 2.454(3) Å. The central six-membered ring of the tetradentate ligand has a boat conformation, whereas the two terminal six-membered chelate rings of the amine ligand adopt the chair conformation.
Keywords: Copper(II) complexes; Perchlorato complexes; 1,4-Bis(3-aminopropyl)piperazine; Piperazine; Crystal structure;

Large-scale growth of porous CuInS2 microspheres by Hanmei Hu; Baojun Yang; Xinyuan Liu; Rui Zhang; Yitai Qian (563-565).
Uniform CuInS2 porous microspheres were synthesized on a large scale using CuCl2  · 2H2O, InCl3  · 4H2O and KSCN as starting reagents in ethylene glycol at 200 °C for 12 h. XRD result reveals that the obtained products are well crystallized. FESEM observation reveals that the prepared microspheres are composed of sheet-like nanocrystals. The possible formation mechanism was simply discussed.
Keywords: Semiconductor; Copper indium disulfide; Solvothermal synthesis; Porous microspheres;

Ligand effect on the periodic properties of trivalent organolanthanide complexes: a density functional study by Yi Luo; Parasuraman Selvam; Michihisa Koyama; Momoji Kubo; Akira Miyamoto (566-568).
For the first time, density functional calculations on a series of organolanthanides of the type Cp3Ln, Cp2LnCl, Cp2LnCl(THF) and CpLnCl2 (Ln=La, Ce, Eu, Gd, Yb and Lu; Cp=cyclopentadienyl, C5H5; THF=tetrahydrofuran, OC4H8), which showed a periodic trend and the influence of ligands on the molecular properties for a set of tailored lanthanide complexes. The replacement of the ligands by another alters the bond lengths and has irregular trends along the lanthanide series. The increase in the (Hirshfeld) charges on going from La to Lu indicates an increase in ionic character, which is in line with the chemical hardness and softness concept while Mulliken charges failed to describe the same.
Keywords: Organolanthanide; DFT; Ligand effect; Lanthanide contraction; Hirshfeld charge;

Revised preparation procedure of calcium hydroxyapatite with sol consisting of sodium alginate and sodium diphosphate by Shigeru Sugiyama; Minako Fujii; Hiromu Hayashi; Katsuki Kusakabe (569-571).
Calcium hydroxyapatite (Ca10(PO4)6(OH)2; CaHAp) was prepared from the cation-exchange of Na+ in the gel consisting of sodium alginate and Na4P2O7 with Ca2+ from the mixture of Ca(CH3COO)2 and Ca(NO3)2 in an aqueous solution at pH 10 although it had been already reported that CaHAp could be prepared with the employment of CaCl2 at pH 6.5, which rather afforded calcium chlorapatite (Ca10(PO4)6Cl2).
Keywords: Calcium hydroxyapatite; Calcium chlorapatite; Sol–gel method; Preparation;

Shape controlled synthesis of PbS nanocrystals by a solvothermal–microemulsion approach by Junhua Xiang; Shu-Hong Yu; Bianhua Liu; Yang Xu; Xin Gen; Lei Ren (572-575).
Shape controlled synthesis of PbS nanoparticles, cubes, and nanowires has been realized by a so-called solvothermal–microemulsion technique in a sodium dodecyl sulfate (SDS)/hexane/hexanol/water microemulsion system using different sulfur source. The effect of different sulfur source and temperature on the shape of PbS nanocrystallites was investigated. The results demonstrated that the combination of solvothermal process and microemulsion technique could provide a useful tool for the synthesis of other nanocrysals with unusual shape and structures.
Keywords: Solvothermal; Microemulsion; Synthesis; Shape control;

The first specimen of tetranuclear (FeIII, LnIII) clusters assembled by carboxylate ligands: synthesis, structure, Mössbauer spectra, and magnetic properties of [Fe3EuO2(CCl3COO)8H2O(THF)3] · THF by Constantin Turta; Denis Prodius; Valeriu Mereacre; Sergiu Shova; Maria Gdaniec; Yurii A. Simonov; Victor Kuncser; George Filoti; Andrea Caneschi; Lorenzo Sorace (576-579).
The reaction of the neutral cluster [Fe2BaO(CCl3COO)6(THF)6] with Eu(NO3)3  · 6H2O in methanol affords novel tetranuclear Fe–Eu complex [Fe3EuO2(CCl3COO)8H2O(THF)3] · THF (1), which displays interesting Mössbauer spectra and magnetic behaviour.
Keywords: Iron(III) europium(III) heterocluster; Crystal structure; Ferromagnetic interaction;

Novel crystal structure and mesomorphism appeared in oxovanadium(IV) salen complexes with 4-substituted long alkoxy chains by Yuriko Abe; Kyoko Nakabayashi; Nahoko Matsukawa; Masayasu Iida; Tomoaki Tanase; Makiko Sugibayashia; Kazuchika Ohta (580-583).
A series of V(IV) complexes with 4-substituted salen ligands, formulated as [VO((4-C n H2n+1O)2salen)] (n=12 (1), 14 (2), 16 (3), 18 (4), and 20 (5)), which formed a novel biomembrane-like bilayer crystal structure, exhibited an unprecedented bilayer mesophase having symmetry Pa21 in the layers.
Keywords: Oxovanadium(IV) complexes; Salen with 4-substituted long alkoxy chains; Novel biomembrane-like bilayer crystal structure; Metallomesogen; Liquid crystal;

A new complex containing two different discrete trinuclear oxo-centered [Fe3O] units has been synthesized and characterized by single crystal X-ray diffraction analysis and Mössbauer spectra. The Mössbauer spectra of the complex are typical of high spin iron(III) complexes.
Keywords: Synthesis; New iron(III) oxide cluster; Crystal structure; Mössbauer spectra;

Heterometallic nanocomposite oxide catalysts have been obtained by impregnation of NaY zeolite with toluene solutions of a structurally characterized heterometallic heteroleptic alkoxide, Co2Nb2(acac)2(OMe)12. EXAFS studies showed the molecular structure of the complex to be preserved and the coordination of the late transition metal atom in the ready nanocomposite very close to that in the original complex. A silsesquioxane complex has been used in order to prepare a zeolite nanocomposite analogue and this proved successful with very similar EXAFS spectra to the ready nanocomposite, indicating the usefulness of the silsesquioxanes as molecular analogues of zeolites.
Keywords: Nanocomposite; Zeolite; Bis-silsesquioxane complex; Molecular analogue; Late transition metal alkoxide; EXAFS;

A novel hydrothermal route to synthesize boron nitride nanocrystals by Xiaopeng Hao; Shouyi Dong; Wei Fang; Jie Zhan; Ling Li; Xiangang Xu; Minhua Jiang (592-594).
Boron nitride (BN) nanocrystals have been synthesized by a novel hydrothermal method. The results of measurement indicated that the sample is a mixture of orthorhombic (o) and cubic (c) BN nanocrystals.
Keywords: Boron nitride; Nanocrystals; Hydrothermal synthesis;

Using rare earth coordination polymers with salicylic acid as precursors for the luminescent species Gd2SiO5:Tb3+, composing with the polyacrylamide as dispersing media, nanophosphor of Gd2SiO5 doped with Tb3+ was synthesized by the sol–gel technique. X-ray diffraction and scanning electronic microscope show that these materials have the nanometer size of 40–100 nm. These nanometer materials exhibit strong green emission at 542 nm.
Keywords: Optical materials; Luminescence; Nanostructures; Gd2SiO5; Nanophosphors; Doped Tb3+; In situ composition; Hybrid precursors;