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1.
G. Haxhillazi 《Journal of solid state chemistry》2004,177(9):3045-3051
The compounds (NH4)3[Ta(O2)4], K3[Ta(O2)4], Rb3[Ta(O2)4] and Cs3[Ta(O2)4] have been prepared and investigated by X-ray powder methods as well as Raman- and IR-spectroscopy. In the case of Rb3[Ta(O2)4] the structure has been solved from single crystal data. It is shown that all these compounds are isotypic and crystallize in the K3[Cr(O2)4] type (SG , No. 121). The infrared- and Raman spectra (recorded on powdered samples) are discussed with respect to the internal vibrations of the peroxo-group and the dodecahedral [Ta(O2)4]3− ion. Symmetry coordinates for the [Ta(O2)4]3− ion are given from which the vibrational modes of the O-O stretching vibrations of the O22− groups, the Ta-O stretching vibrations and the Ta-O bending vibrations are deduced. 相似文献
2.
D. P. Domonov S. I. Pechenyuk N. L. Mikhailova A. T. Belyaevskii 《Russian Journal of Inorganic Chemistry》2007,52(7):1027-1032
The thermolysis of the complexes [Co(NH3)6]2C2O4[Cu(C2O4)2]2 (I) and [Co(NH3)6]Cl[Cu(C7H4O3)2] (II) in air and hydrogen at 200, 350, and 500°C and the composition and properties of the thermolysis products are considered.
The oxidative thermolysis of the complexes yields mixtures of cobalt and copper oxides, including mixed ones. The reductive
thermolysis of the complexes yields a Co + Cu bimetallic powder in the case of compound I and a Co + Cu + C powder in the
case of compound II. The thermal behavior of the complexes is governed by the nature of the ligand coordinated to the copper
atom. The observed data are explicable in terms of the properties of this ligand. The chemistry of the oxidative and reductive
thermolysis is discussed.
Original Russian Text ? D.P. Domonov, S.I. Pechenyuk, N.L. Mikhailova, A.T. Belyaevskii, 2007, published in Zhurnal Neorganicheskoi
Khimii, 2007, Vol. 52, No. 7, pp. 1104–1110. 相似文献
3.
Double complex salts (DCSs) [Co(NH3)6][Fe(CN)6] (I) and [Co(NH3)6]2[Cu(C2O4)2]3 (II) and complex [Co(NH3)6]2(C2O4)3·4H2O (III) are synthesized and investigated by single crystal XRD, crystal optics, and elemental analysis. The crystalline phases of
I, II, and III (R-3, P21/c, and Pnnm space groups respectively) have the following crystallographic characteristics: a = 10.9804(2) ?, b = 10.9804(2) ?, c = 10.8224(3) ?, V = 1130.03(4) ?3, Z = 3, d
x = 1.65 g/cm3 (I); a = 9.6370(2) ?, b = 10.2452(2) ?, c = 13.2108(3) ?, V = 1932.90(9) ?3, Z = 2, d
x= 1.97 g/cm3 (II), and a = 11.7658(3) ?, b = 11.7254(3) ?, c = 14.1913(4) ?, V = 1304.34(5) ?3, Z = 2, d
x = 1.68 g/cm3 (III). This paper investigates the products of DCS thermolysis in a hydrogen atmosphere: the intermetallic compound CoFe with
the bcc parameter a = 2.852 ? for I and a heterogeneous mixture of Co and Cu in the decomposition of II. The coordinated CN− and C2O42− groups then turn into NH3, hydrocarbons, and CO2. The dominant hydrocarbon is methane. 相似文献
4.
Two new potassium uranyl molybdates K2(UO2)2(MoO4)O2 and K8(UO2)8(MoO5)3O6 have been obtained by solid state chemistry . The crystal structures were determined by single crystal X-ray diffraction data, collected with MoKα radiation and a charge coupled device (CCD) detector. Their structures were solved using direct methods and Fourier difference techniques and refined by a least square method on the basis of F2 for all unique reflections, with R1=0.046 for 136 parameters and 1412 reflections with I?2σ(I) for K2(UO2)2(MoO4)O2 and R1=0.055 for 257 parameters and 2585 reflections with I?2σ(I) for K8(UO2)8(MoO5)3O6. The first compound crystallizes in the monoclinic symmetry, space group P21/c with a=8.250(1) Å, b=15.337(2) Å, c=8.351(1) Å, β=104.75(1)°, ρmes=5.22(2) g/cm3, ρcal=5.27(2) g/cm3 and Z=4. The second material adopts a tetragonal unit cell with a=b=23.488(3) Å, c=6.7857(11) Å, ρmes=5.44(3) g/cm3, ρcal=5.49(2) g/cm3, Z=4 and space group P4/n.In both structures, the uranium atoms adopt a UO7 pentagonal bipyramid environment, molybdenum atoms are in a MoO4 tetrahedral environment for K2(UO2)2(MoO4)O2 and MoO5 square pyramid coordination in K8(UO2)8(MoO5)3O6. These compounds are characterized by layered structures. The association of uranyl ions (UO7) and molybdate oxoanions MoO4 or MoO5, give infinite layers [(UO2)2(MoO4)O2]2− and [(UO2)8(MoO5)3O6]8− in K2(UO2)2(MoO4)O2 and K8(UO2)8(MoO5)3O6, respectively. Conductivity properties of alkali metal within the interlayer spaces have been measured and show an Arrhenius type evolution. 相似文献
5.
J. K. Ghosh G. V. Jere 《Journal of photochemistry and photobiology. A, Chemistry》1987,40(2-3):295-306
The compounds K4Ti(O2)4·2H2O, K3Ta(O2)2F4 and K2V2O3(O2)2F2 undergo photolysis in the solid state. The photolysis kinetics obey the parabolic rate equation p = kt1/2 and indicate a monoexcitation process for the photolysis. These features are similar to those reported previously for peroxo complexes. The mechanism of evolution of oxygen reported earlier appears to be the same in all these solids. 相似文献
6.
7.
Infrared spectra of K3[ReO2(CN)4] have been recorded using polarized radiation and oriented single crystals. The dichroic behaviour of the bands is analyzed and discussed on the basis of molecular geometry and the oriented molecular model. Experimentally determined dichroic ratios are used to obtain a full set of vibrational frequencies. By combining these data with those obtained from Raman spectra, the fundamental internal and lattice vibrations are assigned. 相似文献
8.
9.
S. I. Pechenyuk D. P. Domonov D. L. Rogachev A. T. Belyavskii 《Russian Journal of Inorganic Chemistry》2007,52(7):1033-1038
The thermolysis of complexes [Co(NH3)6][Fe(CN)6] and [Co(NH3
6]4[Fe(CN)6]3 under an air or hydrogen atmosphere at 200, 350, and 500°C is studied. The composition and properties of thermolysis products
are determined. The oxidative thermolysis yields mixtures of oxides of the central metals; the reductive thermolysis yields
intermetallic compounds CoFe. The density of the complexes and the specific surface area of the intermetallic compounds are
measured. Average particle sizes are calculated. The morphology and dispersion of the powders are dictated by the shape and
density of the crystals of the precursor double salts and the thermolysis temperature. The thermolysis chemism in the oxidative
and reductive atmospheres is discussed in the context of the nature of the complex anion.
Original Russian Text ? S.I. Pechenyuk, D.P. Domonov, D.L. Rogachev, A.T. Belyavskii, 2007, published in Zhurnal Neorganicheskoi
Khimii, 2007, Vol. 52, No. 7, pp. 1110–1115. 相似文献
10.
The synthesis and crystal structure of Cs3Mn[Nb6Cl9O3(CN)6]0.6H2O are described in this work. It crystallizes in the cubic system (space group Fm-3m; a=15.708(5) Å) and is characterized by a static orientational disorder of the [Nb6Cl9O3(CN)6]5− cluster units. It results in a framework structurally related to that encountered in the well known Prussian Blue family prepared for different hexacyanometallates. The charge of the framework is compensated by cesium cations that are located in the tetrahedral cavities of the c.f.c. lattice of units along with water molecules. We will evidence the features that act in the crystallization of solid state compounds built up from ordered or disordered units as well as the influence of orientational disorder on interatomic distances obtained from single-crystal X-ray diffraction investigations. 相似文献
11.
N. V. Izarova M. N. Sokolov A. V. Virovets H. G. Platas V. P. Fedin 《Journal of Structural Chemistry》2005,46(1):147-153
A complex of the composition KNa3[Fe3O(CH3COO)6(H2O)3]3 [α-P2W17Fe(H2O)O61]·32.5H2O (I) was obtained by interaction of FeCl3·6H2O and phosphotungstate K10[α2-P2W17O61]·20H2O in an acetate buffer with a yield of 52%. Compound I was characterized by single crystal X-ray phase analysis and IR spectroscopy. In the crystal structure, the Na and K cations
bind [Fe3O(CH3COO)6(H2O)3]+ trinuclear cations and [α-P2W17Fe(H2O)O61]7− heteropolytungstate anions into infinite zigzag chains.
Original Russian Text Copyright ? 2005 by N. V. Izarova, M. N. Sokolov, A. V. Virovets, H. G. Platas, and V. P. Fedin
__________
Translated from Zhurnal Strukturnoi Khimii, Vol. 46, No. 1, pp. 149–155, January–February, 2005. 相似文献
12.
The rare-earth dicarboxylate hybrid materials [Ce(H2O)]2[O2C(CH2)2CO2]3 ([Ce(Suc)]) and [Sm(H2O)]2[O2C(CH2)2CO2]3·H2O ([Sm(Suc)]) have been hydrothermally synthesized (200°C, 3 days) under autogenus pressure. [Ce(Suc)] is triclinic, a=7.961 (3) Å, b=8.176 (5) Å, c=14.32 (2) Å, α=97.07° (7), β=96.75° (8), γ=103.73° (6), and z=2. The crystal structure of this compound has been determined using 3120 unique single crystal data. The final refinements let the agreement factors R1 and wR2(F2) converge to 0.0138 and 0.0363, respectively. [Ce(Suc)] is built up from infinite chains of edge-sharing nine-fold coordinated cerium atoms running along [100]. These chains are interconnected by the carbon atoms of the succinate anions, leading to a three-dimensional hybrid framework. The cell constants of [Sm(Suc)], isotypic with monoclinic C2/c [Pr(H2O)]2[O2C(CH2)2CO2]3·H2O ([Pr(Suc)]), were refined starting from X-ray powder data: a=20.275 (3) Å, b=7.919 (6) Å, c=14.130 (3) Å, and β=121.45° (1). Despite its lower symmetry, [Ce(Suc)] presents an important structural filiation with [Sm(Suc)] 相似文献
13.
Thioantimonate compounds of [Mn(en)3]2Sb2S5 (1) and [Ni(en)3(Hen)]SbS4 (2) (en=ethylenediamine) were prepared by reaction of transition metal chloride with Sb and S8 powders under solvothermal conditions. Compound 1 consists of discrete [Sb2S5]4− anion, which is formed by corner-sharing SbS3 trigonal pyramids. Compound 2 is composed of discrete tetrahedral [SbS4]3− anion. The compounds 1 and 2 are charge compensated by [M(en)3]2+ cations, whereas in the crystal of 2 there is another counter ion of [Hen]+. The results of the synthesis suggest that the temperature, the concentration and the existing states of the starting materials and so on are important for the structure and composition of the final products. In addition, the oxidation-state of antimony might be related to the molar ratio of the reactants. Excess amount of elemental S is beneficial to the higher oxidation-state of thioantimonate (V). Compound 1 decomposes from 150°C to 350°C, while compound 2 decomposes from 200°C to 350°C remaining Sb2S3 and NiSbS as residues. 相似文献
14.
The hydrothermal reactions of As, Mn, S, phen (phen=1,10-phenanthroline), and en (en=ethylenediamine) yield two manganese As(III) and As(V) thioarsenates, [Mn2(phen)(AsIII2S5)]n (1) and [Mn3(phen)3(AsVS4)2]n·nH2O (2), respectively. Single-crystal X-ray diffraction analyses reveal that compound 1 is a two-dimensional (2D) layer of (6,3) topology. The 18-membered rings within the 2D porous layers are formed by corner-, edge-, and face-sharing cubane-like [Mn2As2S4] units along the [100] direction. Whereas compound 2 is a one-dimensional (1D) chain structure. They are both characterized by IR, elemental analysis, EDS, and X-ray powder diffraction. The thermogravimetric analysis of 1 and 2 are discussed. Both the compounds are semiconductors with the band gap of Eg (compound 1)=2.01 eV (617 nm) and Eg (compound 2)=1.97 eV (629 nm), respectively. In addition, the variable-temperature magnetic susceptibility data suggest weak antiferromagnetic interactions between the Mn2+ ions in these two compounds. 相似文献
15.
Peter Schwendt Alena Oravcová Jarmila Tyršelová František Pavel?ík Jaromír Marek 《Polyhedron》1996,15(24):4507-4511
The vanadium(V) peroxo phosphato complex K7[V4O4(O2)8(PO4)]·9H2O has been obtained from the KVO3---KH2PO4---KOH---H2O2---H2O---C2H5OH system. The X-ray structural analysis revealed a tetranuclear anionic structure in which two dinuclear [V2O2(O)2)2(μ-η1 : η2-O2)2] units are connected by the μ4-PO4 group. 相似文献
16.
Li-Hua Bi 《Journal of solid state chemistry》2009,182(6):1401-1407
The first RuIII-supported tungstoantimonate [RuII(bpy)3]2[Sb2W20RuIII2(H2O)2(dmso)6O68]·3dmso (bpy=bi-pyridine) (1a) has been successfully isolated as [Ru(bpy)3]2+ (Rubpy) salt by routine synthetic reaction in mixed solutions with dmso and water. Single-crystal X-ray analysis was carried out on 1a, which crystallizes in the triclinic system space group P-1 with a=16.804 (6), b=16.988 (6), c=17.666 (6) Å, α=107.397 (13)°, β=106.883 (13)°, γ=103.616 (12)°. V=4309 (3) Å3, Z=1 with R1=0.0773. The compound 1a reveals the following features: (1) Rubpy is firstly used as an alternative ruthenium-source for the synthesis of Ru-substituted heteropolytungstate; (2) the structure of 1a consists of four RuIII-O-S(CH3)2 and two W-O-S(CH3)2 bonds resulting in an assembly with C2 symmetry; (3) the RuIII ions are linked to two dmso groups via two RuIII-O-S(CH3)2 bonds, which represents the other dmso-coordination mode to RuIII in POM chemistry. The cyclic voltammetry studies of 1a in dmso/H2SO4 (3/1 v/v) at pH 2.5 medium using the glassy carbon electrode as a working electrode show the respective electrochemical behaviors of the W-centers and the Ru-centers within 1a, which could be separated clearly. In addition, the compound 1a exhibits photoluminescence arising from π*−t2g ligand-to-metal transition of Rubpy. 相似文献
17.
The actual structure of the vanadium phosphate K6(VO)2(V2O3)2(PO4)4(P2O7) has been determined, using a much larger single crystal than previously used for the isostructural Rb-phase. The actual supercell is four times larger than the corresponding orthorhombic subcell with , , , α=β=γ=90°. The structure resolution, performed in the triclinic space group C-1, shows that the P2O7 groups alone are responsible for the superstructure, all the other atoms keeping the atomic positions of the orthorhombic subcell. This structural study shows a perfect ordering of the P2O7 groups in the actual structure, in contrast to the results obtained from the subcell. Concomitantly, the V4+ and V5+ are found to be ordered in the form of [110] stripes. 相似文献
18.
The new compound Sr5(As2O7)2(AsO3OH) was synthesized under hydrothermal conditions. It represents a previously unknown structure type and belongs to a group of a few compounds in the system SrO-As2O5-H2O; (As2O7)4− besides (AsO3OH)2− groups have not been described yet. The crystal structure of Sr5(As2O7)2(AsO3OH) was determined by single-crystal X-ray diffraction (space group P21/n, a=7.146(1), b=7.142(1), , β=93.67(3)°, , Z=4). One of the five symmetrically unique Sr atoms is in a trigonal antiprismatic (Inorg. Chem. 35 (1996) 4708)—coordination, whereas the other Sr atoms adopt the commonly observed (“Collect” data collection software, Delft, The Netherlands, 1999; Methods Enzymol. 276 (1997) 307)—coordination. The position of the hydrogen atom was located in a difference Fourier map and subsequently refined with an isotropic displacement parameter. Worth mentioning is the very short hydrogen bond length Oh-H?O(1) of 2.494(4) Å; it belongs to the shortest known examples where the donor and acceptor atoms are crystallographically different. This hydrogen bond was confirmed by IR spectroscopy. In addition, Raman spectra were collected in order to study the arsenate groups. 相似文献
19.
20.
Single crystals of Ca3Cu3(PO4)4 synthesized hydrothermally at 420°C and 55 kpsi (3.8 kbar) were found to occur in the space group (No. 14) with a = = 17.619(2), b = 4.8995(4), c = 8.917(1)Å, β = 124.08(1)°, and Z = 2. Full-matrix least-squares refinement of the structure using diffractometer data converged to a final anisotropic R = 0.037 (Rw = 0.046). The two calcium atoms are in six- and nine-coordination and the two copper-containing polyhedra (four- and five-coordinated) are similar to those previously found in Cu3(PO4)2. 相似文献