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PubMed2002

New alkaline earth aluminum hydride with one-dimensional zigzag chains of [AlH6]: synthesis and crystal structure of BaAlH5.

The title hydride and its deuteride were successfully synthesized. The crystal structure of the deuteride was determined by time-of-flight neutron powder diffraction. BaAlD(5) crystallizes with a new orthorhombic structure in space group Pna2(1) (No. 33), cell parameters a = 9.194(1) A, b = 7.0403(9) A, and c = 5.1061(6) A, Z = 4. BaAlH(5) is the first example that contains one-dimensional zigzag chains of [AlH(6)] along the crystallographic c axis.

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PubMed2003

Two new groups of homoleptic rare earth pyridylbenzimidazolates: (NC12H8(NH)2)[Ln(N3C12H8)4] with Ln = Y, Tb, Yb, and [Ln(N3C12H8)2(N3C12H9)2][Ln(N3C12H8)4](N3C12H9)2 with Ln = La, Sm, Eu.

The compounds (NC(12)H(8)(NH)(2))[Ln(N(3)C(12)H(8))(4)], Ln = Y, Tb, Yb, and [Ln(N(3)C(12)H(8))(2)(N(3)C(12)H(9))(2)][Ln(N(3)C(12)H(8))(4)](N(3)C(12)H(9))(2), with Ln = La, Sm, Eu, were obtained by reactions of the group 3 metals yttrium and lanthanum as well as the lanthanides europium, samarium, terbium, and ytterbium with 2-(2-pyridyl)-benzimidazole. The reactions were carried out in melts of the amine without any solvent and led to two new groups of homoleptic rare earth pyridylbenzimidazolates. The trivalent rare earth atoms have an eightfold nitrogen coordination of four chelating pyridylbenzimidazolates giving an ionic structure with either pyridylbenzimidazolium or [Ln(N(3)C(12)H(8))(2)(N(3)C(12)H(9))(2)](+) counterions. With Y, Eu, Sm, and Yb, single crystals were obtained whereas the La- and Tb-containing compounds were identified by powder methods. The products were investigated by X-ray single crystal or powder diffraction and MIR and far-IR spectroscopy, and with DTA/TG regarding their thermal behavior. They are another good proof of the value of solid-state reaction methods for the formation of homoleptic pnicogenides of the lanthanides. Despite their difference in the chemical formula, both types (NC(12)H(8)(NH)(2))[Ln(N(3)C(12)H(8))(4)], Ln = Y (1), Tb (2), Yb (3), and [Ln(N(3)C(12)H(8))(2)(N(3)C(12)H(9))(2)][Ln(N(3)C(12)H(8))(4)](N(3)C(12)H(9))(2), Ln = La (4), Sm (5), Eu (6), crystallize isotypic in the tetragonal space group I4(1). Crystal data for (1): T = 170(2) K, a = 1684.9(1) pm, c = 3735.0(3) pm, V = 10603.5(14) x 10(6) pm(3), R1 for F(o) > 4sigma(F(o)) = 0.053, wR2 = 0.113. Crystal data for (3): T = 170(2) K, a = 1683.03(7) pm, c = 3724.3(2) pm, V = 10549.4(14) x 10(6) pm(3), R1 for F(o) > 4sigma(F(o)) = 0.047, wR2 = 0.129. Crystal data for (5): T = 103(2) K, a = 1690.1(2) pm, c = 3759.5(4) pm, V = 10739(2) x 10(6) pm(3), R1 for F(o) > 4sigma(F(o)) = 0.050, wR2 = 0.117. Crystal data for (6): T = 170(2) K, a = 1685.89(9) pm, c = 3760.0(3) pm, V = 10686.9(11) x 10(6) pm(3), R1 for F(o) > 4sigma(F(o)) = 0.060, wR2 = 0.144.

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PubMed2002

Growth of compound Bi(III)- VI(A)-VII(A) crystals with special morphologies under mild conditions.

A series of crystals Bi(III)-VI(A)-VII(A), including the platelike crystals BiOCl, polygonal tubular crystals BiSCl, bundle-rodlike crystals Bi(19)S(27)Br(3), and BiSI, have been grown with use of mild solution routes in an ethanol system. The products are characterized by means of X-ray powder diffraction (XRD), electron diffraction (ED), scanning electronic microscopy (SEM), and Raman spectrum techniques. A possible mechanism of the reaction and of the growth of the crystals is proposed.

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PubMed2002

Identification of a near-linear supramolecular water dimer, (H2O)2, in the channel of an inorganic framework material.

Supramolecular water dimer, (H(2)O)(2), is fundamentally important. During the course of our work on polyoxometalates, we have been able to identify the existence of hydrogen-bonded, near-linear water dimers in the "sinuous" channels of an inorganic framework material, Na(3)(n)(H(2)O)(6)(n)[Al(OH)(6)Mo(6)O(18)](n)() x 2nH(2)O, 1. The three-dimensional network structure of 1 in the solid state is assembled by the Anderson type of heteropolyanions as building blocks sharing sodium cations. Vibrational spectroscopy, X-ray powder diffraction technique, TG-DSC analyses, and single-crystal X-ray structure analysis have characterized this host-guest system, 1. Crystal data for 1: triclinic space group Ponemacr;, a = 12.0618 (3) A, b = 13.1570 (4) A, c = 14.1563 (4) A, alpha = 80.7850 (10) degrees, beta = 75.2660 (10) degrees, gamma = 68.9210 (10) degrees, and Z = 3.

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PubMed2002

Room-temperature synthesis and crystal, magnetic, and electronic structure of the first silver copper oxide.

Ag(2)Cu(2)O(3) is the first known silver copper oxide. It was prepared by coprecipitation at room temperature and ambient pressure and shows an increased thermal stability compared with silver oxides. The crystal structure (tetragonal, a = 5.8862(2) A, c = 10.6892(4) A, Z = 4, I4(1)/amd) was refined from neutron and X-ray powder diffraction data, and it is related to that of the mineral paramelaconite (Cu(4)O(3)). In addition to a thorough characterization (chemical and TG analyses, XPS, crystal structure, and electrochemical, magnetic, and transport properties), we have carried out band structure calculations [extended Hückel tight binding (EHTB) and spin polarized density functional (DFT) band calculations] for the title silver copper oxide and for the related paramelaconite structure (Cu(II)-Cu(I) mixed-valence system) with special incidence into the magnetic behavior and coupling constants in these magnetically novel 3-D compounds. This new oxide represents an important precedent in solid state inorganic chemistry but also has potential interest concerning its magnetic, electrochemical, and catalytic properties.

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PubMed2003

Dimorphism of a new CuI coordination polymer:synthesis, crystal structures and properties of catena[CuI(2-iodopyrazine-N)] and poly[CuI(mu2-2-iodopyrazine-N,N')].

Two modifications of the new copper(I) iodide coordination polymer CuI(2-iodopyrazine) were obtained by the reaction of CuI and 2-iodopyrazine in acetonitrile. During this reaction, intensely yellow crystals of form I appear first which transform within several minutes to intensely red crystals of form II which is the thermodynamically most stable form at room temperature. In catena[CuI(2-iodopyrazine-N)] (form I; a = 4.1830 (6) A; b = 10.814 (1) A; c = 17.961 (4) A; V = 812.5 (2) A(3); orthorhombic; P2(1)2(1)2(1); Z = 4), corrugated CuI double chains are found in which each copper atom is coordinated by one additional 2-iodopyrazine ligand. In poly[CuI(mu-2-iodopyrazine-N,N')] (form II; a = 4.2679 (5) A; b = 13.942 (2) A; c = 13.017 (2) A; b = 92.64 (1) degrees; V = 773.76 (2) A(3); monoclinic; P2(1)/c; Z = 4), CuI single chains occur which are connected via mu-N,N' coordination by the 2-iodopyrazine ligands to layers parallel to (010). The thermal behavior of both forms was investigated using simultaneous differential thermoanalysis, thermogravimetry, and mass spectrometry as well as differential scanning calorimetry and temperature resolved X-ray powder diffraction. On heating, both forms decompose to copper(I) iodide, and the decomposition temperature of form I is significantly lower than that of form II. From all experiments, there is no indication of a phase transition of one form into the other or for the formation of a phase with lower amine content.

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PubMed2003

Mixed valence in YBaFe(2)O(5).

YBaFe(2)O(5) has been synthesized by heating a nanoscale citrate precursor in a carefully controlled reducing environment. Successful synthesis of a single-phase sample can only be achieved in a narrow window of oxygen partial pressures and temperatures. YBaFe(2)O(5) adopts an oxygen-deficient perovskite-type structure, which contains double layers of corner sharing FeO(5) square pyramids separated by Y(3+) ions. At T(N) congruent with 430 K, tetragonal (P4/mmm) and paramagnetic YBaFe(2)O(5) orders antiferromagnetically (AFM) experiencing a slight orthorhombic distortion (Pmmm). Around this temperature, it can be characterized as a class-III mixed valence (MV) compound, where all iron atoms exist as equivalent MV Fe(2.5+) ions. The magnetic structure is characterized by AFM Fe-O-Fe superexchange coupling within the double layers and a ferromagnetic Fe-Fe direct-exchange coupling between neighboring double layers. Upon cooling below approximately 335 K, a premonitory charge ordering (2Fe(2.5+) --> Fe(2.5+delta) + Fe(2.5)(-delta)) into a class-II MV phase takes place. This transition is detected by differential scanning calorimetry, but powder diffraction techniques fail to detect any volume change or a long-range structural order. At approximately 308 K, a complete charge ordering (2Fe(2.5+) --> Fe(2+) + Fe(3+)) into a class-I MV compound takes place. This charge localization triggers a number of changes in the crystal, magnetic, and electronic structure of YBaFe(2)O(5). The magnetic structure rearranges to a G-type AFM structure, where both the Fe-O-Fe superexchange and the Fe-Fe direct-exchange couplings are antiferromagnetic. The crystal structure rearranges (Pmma) to accommodate alternating chains of Fe(2+) and Fe(3+) running along b and an unexpectedly large cooperative Jahn-Teller distortion about the high-spin Fe(2+) ions. This order of charges does not fulfill the Anderson condition, and it rather corresponds to an ordering of doubly occupied Fe(2+) d(xz) orbitals. Comparisons with YBaMn(2)O(5) and YBaCo(2)O(5) are made to highlight the impact of changing the d-electron count.

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PubMed2003

New low-temperature preparations of some simple and mixed co and ni dispersed sulfides and their chemical behavior in reducing atmosphere.

A series of simple (CoS(2), Co(9)S(8), NiS(2), NiS, Ni(3)S(2)) and mixed sulfides (NiCo(2)S(4), Ni(0.33)Co(0.67)S(2), Ni(3)Co(6)S(8), CuCo(2)S(4), Cu(0.33)Co(0.67)S(2)) was prepared using low-temperature procedures. To obtain the mixed sulfides, the mixtures of the solutions of the corresponding salts were precipitated by Na(2)S and then heated in a sulfiding atmosphere at 300 degrees C. It has been found that the product phase composition depends on the sulfiding atmosphere. Using a H(2)S/Ar mixture leads to pyrite type sulfides, whereas treatment in H(2)S/H(2) flow allowed the preparation of Ni-Co and Cu-Co thiospinels. The as prepared highly dispersed single-phase materials were characterized by X-ray powder diffraction, scanning electron microscopy, temperature-programmed reduction (TPR), elemental analysis, and BET surface area measurements.

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PubMed2003

Complexation of beryllium(II) ion by phosphinate ligands in aqueous solution. Synthesis and XRPD structure determination of Be[(PhPO2)2CH2](H2O)2.

Two bifunctional ligands, phenyl(carboxymethyl)phosphinate (ccp(2-) and P,P'-diphenylmethylenediphosphinate (pcp(2-)), have been tested as chelating agents of beryllium(II). Both ligands have the same charge and a similar chelating structure, but whereas the 1:1 adduct of pcp(2-), Be(pcp)(H(2)O)(2), could be isolated as a white powder, no pure compound could be isolated from solutions containing beryllium(II) and ccp(2-). Instead, the solutions were examined by means of potentiometry and (9)Be NMR spectroscopy. Analysis of the potentiometric titration data with the program HYPERQUAD suggested the formation of the complex species BeL, [BeHL](+), [BeL(2)](2-), and [BeHL(2)](-) (L = ccp). The formation constants for these species were determined at 25 degrees C and I = 0.5 mol dm(-3) NaClO(4). The (9)Be NMR spectra are consistent with this model. The formation constants found for the ccp(2-) complexes are lower than those reported for related phosphonate ligands. However, the effective stability constant (which gives a better indication of the intrinsic coordinating capacity of the ligand at a particular pH) of the complex [Be(ccp)(2)](2-) at pH < 4 is greater than the effective constants of the corresponding phosphonoacetate and methylenediphosphonate complexes. The structure of Be(pcp)(H(2)O)(2) was determined by X-ray powder diffraction methods and consists of discrete molecules interconnected by an extended 2D network of hydrogen bonds, resulting in a stacking of doublelayers with a polar core and a lipophilic surface. Crystal data: C(13)H(16)BeO(6)P(2), fw 339.21, monoclinic P2(1)/c, a = 16.174(1) A, b = 8.979(1) A, c = 10.929(1) A, beta = 90.398(9) degrees, V = 1587.2(3) A(3), Z = 4.

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PubMed2003

New two-dimensional metal-organic networks constructed from 1,2,4,5-benzenetetracarboxylate and chelate ligands.

Two novel nickel coordination polymers [Ni(2)(2,2'-bipy)(2)(OH)(2)(H(2)btec)](3)(n)(1) and [Ni(2)(1,10'-phen)(2)(H(2)O)(2)(btec)](n)(2) (btec = 1,2,4,5-benzenetetracarboxylate) have been hydrothermally synthesized and characterized by elemental analyses, IR and XPS spectra, TG analysis, X-ray powder diffraction, and single crystal X-ray diffraction. Crystal data for 1: C(90)H(66)N(12)O(30)Ni(6), monoclinic P2(1)/c, a = 10.905(2) A, b = 18.006(4) A, c = 20.551(4) A, beta = 94.91(3) degrees, Z = 2. Crystal data for 2: C(34)H(22)N(4)O(10)Ni(2), monoclinic P2(1)/n, a = 10.122(2) A, b = 9.3106(19) A, c = 15.690(3) A, beta = 92.03(3) degrees, Z = 2. Compound 1 exhibits a novel one-dimensional chainlike structure, in which the dinuclear Ni centers are linked by the btec ligands. Furthermore, the adjacent chains are linked into a 2-D wavelike layer via the strong OH.O hydrogen bonding interactions. Compound 2 possesses an unusual two-dimensional steplike network with interesting rhombic grids. Both compounds exhibit unprecedented metal-organic ligand construction modes in [M/btec/L] (M = transition metal; L = chelate ligands) systems. The magnetic behaviors of compounds 1 and 2 have been studied.

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PubMed2004

New insights into the structural and dynamical features of lithium hexaoxometalates Li7MO6 (M = Nb, Ta, Sb, Bi).

We present a (re)investigation of the hexaoxometalates Li(8)MO(6) (M = Sn, Pb, Zr, Hf) and Li(7)MO(6) (M = Nb, Ta, Sb, Bi). Lithium motion and ionic conductivity in the hexaoxometalates were studied using impedance spectroscopy (for Li(7)MO(6), M = Sb, Bi, Ta) and (6)Li and (7)Li solid-state nuclear magnetic resonance (for Li(7)TaO(6)). The NMR data indicate a considerable exchange of Li among the tetrahedral and octahedral voids even at ambient temperature. In an investigation of the crystal structures using laboratory and synchrotron X-ray powder diffraction techniques, the structures of Li(7)TaO(6), Li(7)NbO(6), and Li(7)SbO(6) could be solved and refined. All three reveal a triclinic metric (Li(7)SbO(6), triclinic, P1, a = 5.38503(6) A, b = 5.89164(7) A, c = 5.43074(6) A, alpha = 117.2210(6) degrees, beta = 119.6311(6) degrees, gamma = 63.2520(7) degrees, V = 127.454(3) A(3), Z = 1; Li(7)NbO(6), triclinic, P1, a = 5.37932(9) A, b = 5.91942(11) A, c = 5.37922(9) A, alpha = 117.0033(9) degrees, beta = 119.6023(7) degrees, gamma = 63.2570(9) degrees, V = 126.938(4) A(3), Z = 1; Li(7)TaO(6), triclinic, P1, a = 5.38486(2) A, b = 5.92014(3) A, c = 5.38551(2) A, alpha = 117.0108(2) degrees, beta = 119.6132(2) degrees, gamma = 63.2492(2) degrees, V = 127.208(1) A(3), Z = 1.

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PubMed2004

Two-dimensional metallic chain compounds Y5M2Te2 (M = Fe, Co, Ni) that are related to Gd3MnI3. The hydride derivative Y5Ni2Te2D0.4.

Y(5)M(2)Te(2) (M = Fe, Co, Ni) have been prepared by high-temperature solid-state techniques and shown to be isostructural and orthorhombic Cmcm (No. 63), Z = 4. The structure was established by single crystal X-ray methods at 23 degrees C for M = Fe, with a = 3.9594(3) A, b = 15.057(1) A, and c = 15.216(1) A. The new structure contains zigzag chains of the late transition metal sheathed by a column of yttrium atoms that are in turn condensed through trans vertices on the latter to yield 2D bimetallic layers separated by single layers of tellurium atoms. Reaction of hydrogen with Y(5)Ni(2)Te(2) causes a rumpling of the Y-Ni layers as determined by both single X-ray crystal means at 23 degrees C and neutron powder diffraction at -259 degrees C for Y(5)Ni(2)Te(2)D(0.41(1)), Pnma (No. 62), Z = 4. Lattice constants from the former study are a = 14.3678(7) A, b = 4.0173(2) A, and c = 15.8787(7) A. The hydrogen is accommodated in tetrahedral yttrium cavities generated by bending the formerly flat sheets at the trans Y vertices. A higher hydride version also exists. Band structure calculations confirm the 2D metal-bonded character of the compounds and also help illustrate the bonding/matrix changes that accompany the bonding of hydrogen. The ternary structures for both Y(5)M(2)Te(2) and Sc(5)Ni(2)Te(2) can be derived from that of Gd(3)MnI(3), the group illustrating three different kinds of metal chain condensation.

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PubMed2003

The structure of magnesium alanate.

Mg(AlH(4))(2) was produced as a nanocrystalline powder by metathesis of NaAlH(4) and MgCl(2). Starting with a structure estimation which was developed from an evaluation of FTIR data and comparison of structural properties of two solvent adducts, quantum chemical calculations were performed on the density functional theory (DFT) level. The calculated atomic positions were used to simulate an X-ray powder diffraction pattern, based on a trigonal unit cell. The simulated pattern was congruent to experimental data. Thus, magnesium alanate exhibits a CdI(2) layer structure, the layers being formed by Mg atoms occupying the Cd sites and AlH(4) tedrahedra occupying the sites of the iodine atoms in CdI(2).

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PubMed2003

Sonochemical fabrication and characterization of stibnite nanorods.

Regular stibnite (Sb(2)S(3)) nanorods with diameters of 20-40 nm and lengths of 220-350 nm have been successfully synthesized by a sonochemical method under ambient air from an ethanolic solution containing antimony trichloride and thioacetamide. The as-prepared Sb(2)S(3) nanorods are characterized by employing techniques including X-ray powder diffraction, X-ray photoelectron spectroscopy, scanning electron microscopy, energy-dispersive X-ray analysis, transmission electron microscopy, selected area electron diffraction, high-resolution transmission electron microscopy, and optical diffuse reflection spectroscopy. Microstructural analysis reveals that the Sb(2)S(3) nanorods crystallize in an orthorhombic structure and predominantly grow along the (001) crystalline plane. High-intensity ultrasound irradiation plays an important role in the formation of these Sb(2)S(3) nanorods. The experimental results show that the sonochemical formation of stibnite nanorods can be divided into four steps in sequence: (1) ultrasound-induced decomposition of the precursor, which leads to the formation of amorphous Sb(2)S(3) nanospheres; (2) ultrasound-induced crystallization of these amorphous nanospheres and generation of nanocrystalline irregular short rods; (3) a crystal growth process, giving rise to the formation of regular needle-shaped nanowhiskers; (4) surface corrosion and fragmentation of the nanowhiskers by ultrasound irradiation, resulting in the formation of regular nanorods. The optical properties of the Sb(2)S(3) amorphous nanospheres, irregular short nanorods, needle-shaped nanowhiskers, and regular nanorods are investigated by diffuse reflection spectroscopic measurements, and the band gaps are measured to be 2.45, 1.99, 1.85, and 1.94 eV, respectively.

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PubMed2003

Metathetical conversion of Nd2O3 nanoparticles into NdS2 polysulfide nanoparticles at low temperatures using boron sulfides.

A new simple metathetical sulfidation method using boron sulfides has been developed to prepare nanoparticles of NdS(2) via conversion of ca. 50-nm-sized nanoparticles of Nd(2)O(3) at 450 degrees C, in which boron and sulfur powders form boron sulfides in situ and evaporate to sulfidize the oxide. The X-ray powder diffraction analysis revealed that the products were purely NdS(2), and the atomic absorption spectrometric analysis confirmed nonexistence of boron in the products after washing with water. The detailed TEM studies showed that the NdS(2) nanoparticles maintained the original size of the oxide particles without fusion during the low-temperature sulfidation process.

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PubMed2003

Synthesis and characterization of two polymorphic crystalline phases and an amorphous powder of nickel(II) bisimidazolate.

Nickel(II) bisimidazolate is polymorphic. Depending on the synthetic strategy adopted, two crystalline phases (alpha- and beta-Ni(im)(2)) or an amorphous material of the same composition can be prepared. The thermodynamically stable alpha-Ni(im)(2) phase, which can be prepared in water at elevated temperatures, contains a two-dimensional polymer (of nearly square meshes) with square-planar NiN(4) chromophores and exo-bidentate imidazolate ligands bridging nickel atoms that are ca. 5.73 A apart. The beta-Ni(im)(2) phase can be kinetically stabilized at lower temperatures, but the structural complexity and the lack of single crystals prevented its full structural characterization, even in the presence of an indexed powder diffraction pattern. The spectroscopic features of these crystalline phases are compared with those of the amorphous material.

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PubMed2003

A porous supramolecular architecture from a copper(II) coordination polymer with a 3D four-connected 8(6) net.

A novel coordination polymer [[Cu(L(1))(L(2))(H(2)O)].5H(2)O](n) (1), where L(1) =1,1'-(1,4-butanediyl)bis(imidazole) and L(2) = m-phthalate anion, has been obtained by using an unusual crystallization process. It crystallizes in the orthorhombic space group Pna2(1), which belongs to the crystal class mm2, with a = 9.0521(18), b = 15.401(3), and c = 17.141(3) A, alpha = beta = gamma = 90 degrees, V = 2389.7(8) A(3), and Z = 4. The complex 1 composing a porous supramolecular architecture displays unprecedented four-connected topology of an 8(6) net in coordination polymer chemistry. Thermal gravimetric analysis (TGA) and X-ray powder diffraction (XRPD) patterns for 1 are discussed in detail.

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PubMed2004

Synthesis, characterization, and luminescent properties of dinuclear gold(I) xanthate complexes: X-ray structure of [Au2(nBu-xanthate)2].

The synthesis and characterization of gold(I) complexes of butyl xanthate [Au(2)((n)()Bu-xanthate)(2)], 1, and ethyl xanthate [Au(2)(Et-xanthate)(2)], 2, are described. These complexes are readily prepared from the reaction between Au(THT)Cl (THT = tetrahydrothiophene) and the corresponding xanthate ligands as the potassium salts. The two xanthate complexes are characterized by (1)H NMR, IR, mass spectrometry, elemental analysis, and UV-vis techniques. Thermal gravimetric analysis (TGA) and differential thermal analysis (DTA) show that the gold xanthate complexes decompose to yield mainly gold metal at approximately 200 degrees C, confirmed by X-ray powder diffraction. Excitation of the complexes at 450 nm in the solid state at 77 K produces a strong red emission at ca. 690 nm with a broad asymmetric profile tailing to 850 nm. The dinuclear gold(I) xanthate complex, [Au(2)(nBu-xanthate)(2)], 1, is the first structurally characterized binary Au(I) xanthate. The Au...Au distance in the eight-membered ring is 2.8494(15) A while the shortest intermolecular Au...Au interaction between independent units is 3.64 A. The angle between the planes containing the molecules in the unit cell is approximately 69.56 degrees. The light green plates of [Au(mu-S(2)COBu(n))](2) crystallize in the orthorhombic space group P2(1)2(1)2 with a = 37.254(14) A, b = 7.287(3) A, c = 6.054(2) A, alpha = beta = gamma = 90 degrees, Z = 4, and V = 1643.4(11) A(3).

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