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1.
D. O. Savinykh S. A. Khainakov A. I. Orlova S. Garcia-Granda 《Russian Journal of Inorganic Chemistry》2018,63(6):714-724
NaZr2–xBx(PO4)3–2x(SO4)2x (0 ≤ x ≤ 1.25, B = Mg, Co, Ni, Cu, Zn), and NaZr2–xRx(PO4)3–x(SO4)x (0 ≤ x ≤ 1.25, R = Al, Fe) phosphate-sulfates series have been prepared by a sol–gel process. These compounds belong to the NaZr2(PO4)3 (NZP) structure family and crystallize in hexagonal crystal system, space group R\(\bar 3\)c. Limited solid solution series were found to exist; their formation temperatures and thermal stability limits were determined. Particle sizes as determined by microstructure observation were 50–200 nm, and for Cu- and Zn-containing samples, 200–500 nm. The thermal expansion of phosphate-sulfate NaZr1.25Cu0.75(PO4)1.5(SO4)1.5 was studied in the range 25–700°C. Thermal expansion coefficients and thermal expansion anisotropy were found to be αa =–5.40 × 10–6 °C–1, αс = 18.88 × 10–6 °C–1, αavg = 2.69 × 10–6 °C–1, and Δα = 24.28 × 10–6 °C–1. 相似文献
2.
T. S. Sysoeva E. A. Asabina V. I. Pet’kov V. S. Kurazhkovskaya 《Russian Journal of Inorganic Chemistry》2009,54(6):829-839
Phase formation in the A1 + x Al x Ti2 ? x P3O12 (A = Li, Na, K, Rb, or Cs; 0 ≤ x ≤ 2.0) and B0.5(l + x)Al x Ti2 ? x P3O12 (B = Mg, Ca, Sr, or Ba; 0 ≤ x ≤ 2.0) systems was studied using X-ray powder diffraction, electron probe microanalysis, and IR spectroscopy. The following double and triple orthophosphates were found to exist: A1 + x Al x Ti2 ? x (PO4)3 with A = Li (0 ≤ x ≤ 0.3), Na (0 ≤ x ≤ 1.0), K (x = 0, 1.0, or 2.0), Rb (x = 0, 1.0, or 2.0), or Cs (0 ≤ x ≤ 1.0) and B0.5(l + x)Al x Ti2 ? x (PO4)3 with B = Mg and Ba (x = 0), Ca and Sr (0 ≤ x ≤ 0.2). These orthophosphates crystallize in the structure types of kosnarite, langbeinite, cesium titanium arsenate, potassium aluminum phosphate, or rubidium aluminum phosphate. Their crystal parameters were calculated. For CsTi2(PO4)3 (x = 0), Rietveld refinement was carried out: space group Ia \(\bar 3\) d, Z = 32, a = 19.909(5) Å, V = 7892(1) Å3. This compound has a framework structure. The framework is built of TiO6 octahedra and PO4 tetrahedra; eight- and 12-coordinated Cs+ cations populate interstices. 相似文献
3.
V. I. Pet’kov A. S. Shipilov A. V. Markin N. N. Smirnova 《Russian Journal of Physical Chemistry A, Focus on Chemistry》2018,92(4):646-652
The temperature dependence of heat capacity C° p = f(T) of crystalline arsenate Mg0.5Zr2(AsO4)3 was studied by precision adiabatic vacuum and differential scanning calorimetry in the temperature range 8?670 K. The standard thermodynamic functions C° p (T), H°(T)–H°(0), S°(T), and G°(T)–H°(0) of the arsenate for the range from Т → 0 to 670 K and the standard formation entropy at Т = 298.15 K were calculated from the obtained experimental data. Based on the low-temperature capacity data (30–50 K) the fractal dimension D of the arsenate was determined, and the topology of its structure was characterized. The results were compared with the thermodynamic data for the structurally related crystalline phosphates M0.5Zr2(PO4)3 (M = Mg, Ca, Sr, Ba, Ni) and arsenate NaZr2(AsO4)3. 相似文献
4.
A. Yu. Ledneva N. G. Naumov A. V. Virovets S. Cordier Y. Molard 《Journal of Structural Chemistry》2012,53(1):132-137
The structures of three novel octahedral rhenium cluster compounds [Re6S8(CN)2(py)4]·H2O (1), [Re6S8(CN)2(4-Mepy)4] (2), [Re6S8(CN)2(4-Mepy)4]·4-Mepy (3) (py = pyridine, 4-Mepy = 4-methylpyridine) are determined by X-ray crystallography. Crystal data are: C2/m space group, a = 14.813(1) Å, b = 14.772(1) Å, c = 9.2122(6) Å, β = 119.085(2)°, V = 1761.7(2) Å3, d x = 3.318 g/cm3, R = 0.0585 (1); I41/amd space group, a = 16.0018(3) Å, c = 14.7186(5) Å, V = 3768.81(16) Å3, d x = 3.169 g/cm3, R = 0.0489 (2); P21/c space group, a = 9.0452(4) Å, b = 15.8065(7) Å, c = 15.2951(6) Å, β = 103.700(2)°, V = 2124.57(16) Å3, d x = 2.957 g/cm3, R = 0.0245 (3). Molecular cluster complexes interact via π-π stacking affording 3D frameworks in 1 and 2 and chains in 3. 相似文献
5.
S. N. Vorob’eva I. A. Baidina A. V. Belyaev N. I. Alferova 《Journal of Structural Chemistry》2012,53(1):125-131
The crystal structures of compounds of the composition [Rh(H2O)6]2(SO4)3·5H2O (I) and [Rh(H2O)6]PO4 (II) are determined. Crystallographic data for I: a = 7.272(9) Å, b = 27.047(1) Å, c = 12.464(9) Å, β = 97.038(10)°, P21 space group, Z = 4, d x = 2.184 g/cm3; for II: a = 9.746(6)Å, b = 6.877(7) Å, c = 23.623(6) Å, β = 100.601(10)°, C2/c space group, Z = 8, d x = 2.611 g/cm3. Compounds are analyzed by IR spectroscopy and powder XRD. Crystalline phase I is well soluble in water, whereas II is almost insoluble. 相似文献
6.
P. E. Plyusnin E. Yu. Semitut I. A. Baidina L. A. Sheludyakova S. V. Korenev 《Journal of Structural Chemistry》2009,50(3):479-484
The crystal structures of compounds from the series [M(NH3)5Cl](NO3)2, (M = Ir, Rh, Ru) were described. The compounds crystallized in the tetragonal crystal system, space group I4, Z = 2. Crystal data for [Ir(NH3)5Cl](NO3)2 (I): a = 7.6061(1) Å, b = 7.6061(1) Å, c = 10.4039(2) Å, V = 601.894(16) Å3, ρcalc = 2.410 g/cm3, R = 0.0087; [Rh(NH3)5Cl](NO3)2 (II): a = 7.5858(5) Å, b = 7.5858(5) Å, c = 10.41357(7) Å, V = 599.24(7) Å3, ρcalc = 1.926 g/cm3, R = 0.0255; [Ru(NH3)5Cl](NO3)2 (III): a = 7.5811(6) Å, b = 7.5811(6) Å, c = 10.5352(14) Å, V = 605.49(11) Å3, ρcalc = 1.896 g/cm3, R = 0.0266. The compounds were defined by IR spectroscopy and XRPA and thermal analyses. 相似文献
7.
E. A. Asabina V. I. Pet’kov E. R. Gobechiya Yu. K. Kabalov K. V. Pokholok V. S. Kurazhkovskaya 《Russian Journal of Inorganic Chemistry》2008,53(1):40-47
Triple phosphates A2FeTi(PO4)3 (A = Na, Rb) were synthesized by the solid-phase method and studied by electronic microscopy, electron probe X-ray microanalysis, and IR and Mössbauer spectroscopy. The crystal structure of the obtained compounds was refined by X-ray powder diffraction (the Rietveld method). The unit-cell parameters are as follows: for Na2FeTi(PO4)3 (space group R \(\overline 3 \) c, Z = 6), a = 8.6015(1) Å, c = 21.718(1) Å, V = 1391.52(1) Å3; for Rb2FeTi(PO4)3 (space group P213, Z = 4), a = 9.8892(2) Å, V = 967.12(1) Å3. The base of the crystal structures is a mixed octahedral-tetrahedral framework {[FeTi(PO4)3]2?}3∞. Na+ and Rb+ cations are arranged in cavities of the framework. The influence of cationic substitutions on the change of the structural type of the isoformular compounds A2FeTi(PO4)3 (A = Na, Rb) was considered. 相似文献
8.
M. K. Khosa P. T. Wood S. M. Humphrey W. T. A. Harrison 《Journal of Structural Chemistry》2015,56(6):1130-1135
The syntheses and crystal structures of the layered coordination polymers M(C8H8NO2)2 [M = Mn (1), Co (2), Ni (3) and Zn (4)] are described. These isostructural compounds contain centrosymmetric trans-MN2O4 octahedra as parts of infinite sheets; the ligand bonds to three adjacent metal ions in μ3-N,O,O′ mode from both its carboxylate O atoms and its amine N atom. In each case, weak intra-sheet N–H?O and C–H?O hydrogen bonds may help to consolidate the structure. Crystal data: 1, C16H16MnN2O4, M r = 355.25, monoclinic, P21/c (No. 14), a = 10.6534(2) Å, b = 4.3990(1) Å, c = 15.5733(5) Å, β = 95.1827(10)°, V = 726.85(3) Å3, Z = 2, R(F) = 0.026, wR(F 2) = 0.067. 2, C16H16CoN2O4, M r = 359.24, monoclinic, P21/c (No. 14), a = 10.6131(10) Å, b = 4.3374(4) Å, c = 15.3556(17) Å, β = 95.473(4)°, V = 703.65(12) Å3, Z = 2, R(F) = 0.041, wR(F 2) = 0.091. 3, C16H16N2NiO4, M r = 359.02, monoclinic, P21/c (No. 14), a = 10.6374(4) Å, b = 4.2964(2) Å, c = 15.2827(8) Å, β = 95.9744(14)°, V = 694.66(6) Å3, Z = 2, R(F) = 0.028, wR(F 2) = 0.070. 4, C16H16N2O4Zn, M r = 365.68, monoclinic, P21/c (No. 14), a = 10.6385(5) Å, b = 4.2967(3) Å, c = 15.2844(8) Å, β = 95.941(3)°, V = 694.89(7) Å3, Z = 2, R(F) = 0.038, wR(F 2) = 0.107. 相似文献
9.
New compounds Pb4La(GeO4)2(VO4)(I) and Sr5La5(GeO4)5(VO4)O(II) were prepared and identified. Compound I has the structure of apatite, a = 10.108(1) Å, c = 7.369(1) Å, V = 652.1(2) Å3. Compound II has the structure of oxyapatite, a = 9.9028(5) Å, c = 7.3162(4) Å, V = 621.34(6) Å3. 相似文献
10.
K. V. Yusenko I. V. Korolkov S. A. Gromilov S. V. Korenev 《Journal of Structural Chemistry》2007,48(2):379-382
The crystal structure of [Os(NH3)5Cl][ReCl6] has been refined by X-ray powder analysis: a = 11.645(3) Å, b = 8.3788(2) Å, c = 15.277(4) Å, β = 91.029(6)°, V = 1490(1) Å3, d x = 3.163 g/cm3, space group P21/m, Z = 4. The thermolysis product of the salt in a hydrogen atmosphere is a solid substitution solution Os0.5Re0.5: a = 2.753(2) Å, c = 4.366(3) Å, space group P63/mmc; coherent scattering region (CSR) is ~230 Å. 相似文献
11.
Double complex salts (DCS) [RuNO(NH3)4(H2O)]2[MCl4]Cl4·2H2O, M = Pt (I) and Pd (II), are prepared and characterized using IR spectroscopy, single crystal and powder X-ray diffraction, and thermogravimetric analysis. Crystalline phases of I and II are isostructural (P2(1)/n space group) and have the following crystallographic characteristics: a = 6.689 Å, b = 15.609 Å, c = 12.348 Å, V = 1289.1 Å3, Z = 2, d x = 2.425 g/cm3 (I) and a = 6.637 Å, b = 15.521 Å, c = 12.244 Å, V = 1261.2 Å3, Z = 2, d x = 2.255 g/cm3 (II). The thermolysis of the obtained DCS in the hydrogen atmosphere affords two-phase mixtures of limited solid solutions of the metals: hcp for ruthenium-based ones and fcc for Pt or Pd based solutions. On decomposition in the helium atmosphere the products contain a minor amount of RuO2. For the phases obtained during thermolysis the parameters are determined and the compositions are estimated. The heating of I to 400°C in the helium-air atmosphere yields a nanocrystalline composite Pt+RuO2 with CSR of ~20 nm. 相似文献
12.
Thermal decomposition of [Pt(NH3)4][ReHlg6] binary complex salts (Hlg = Cl, Br) in a hydrogen atmosphere has been studied. Polycrystal X-ray diffractometry indicated that two-phase metallic systems are the final products of thermolysis. Structure refinement was performed for [Pt(NH3)4][ReCl6] by the combined technique involving decomposition of the diffractogram into individual reflections, isolation of reflections most sensitive to the position of separate light atoms, and full-profile analysis. Crystal data for PtReN4Cl6H12: a = 11.616(1) Å, b = 10.998(1) Å, c = 10.377(1) Å, V = 1148.1 Å3, space group Cmca, Z = 4, d x = 3.831 g/cm3. The indices are Rp = 5.48%, Rwp = 10.01%, R(F2) = 12.62%. The coordination polyhedron of Re is an almost regular octahedron: Re-Cl 2.34–2.36 Å, ∠ Cl-Re-Cl 86.9–90.3°; the coordination polyhedron of Pt is a square: Pt-N 2.04 Å, ∠N-Pt-N 90.4°. 相似文献
13.
K. É. Miminoshvili A. N. Sobolev É. B. Miminoshvili L. A. Beridze É. R. Kutelia 《Journal of Structural Chemistry》2005,46(3):560-565
X-ray structural analysis has been performed for two complex compounds: Cu(en)2(o-HB)2H2O (I) (a = 16.873(4) Å, b = 8.713(2) Å, c = 14.803(3) Å, β = 91.15(2)°, V = 2175.8(8) Å3, C2/c, Z = 4, R(F) = 0.0263, 1516 reflections with I > 3σ (I)) and [Cu(en)2(OH2)2]2+(o-AB?)2 (II) (a = 7.488(5) Å, b = 22.122(8) Å, c = 7.856(5) Å, β = 118.77(2)°, V = 1140.7(11) Å3, P21/n, Z = 2, R(F) = 0.0432, 1684 reflections with I > 3σ(I)) synthesized under identical conditions (en is ethylenediamine, o-HB is o-hydroxybenzoate, and o-AB is o-aminobenzoate). Although the compounds were assumed to have similar structures and the Cu-Lig bond lengths and the cis and trans angles are acceptable for an octahedral structure, the geometric parameters of o-HB suggest that the copper atom has a plane square environment. 相似文献
14.
V. N. Krasil’nikov A. P. Tyutyunnik V. G. Zubkov I. F. Berger L. A. Perelyaeva I. V. Baklanova 《Russian Journal of Inorganic Chemistry》2010,55(9):1331-1338
Vanadium(V) complexes of general composition M3VO2(SO4)2 (M = Rb, Cs) were synthesized by a solid-state route. The individuality of the synthesized compounds was proved by X-ray and neutron diffraction, vibrational spectroscopy, and microscopic analysis. The X-ray diffraction patterns of M3VO2(SO4)2 were indexed to fit the monoclinic system (space group P2/c, Z = 4) with the following unit cell parameters: a = 11.6487(2) Å, b = 8.4469(2) Å, c = 12.1110(2) Å, β = 109.483(1)°, V = 1123.43 Å3 (Rb); a = 12.0546(3) Å b = 8.7706(2) Å, c = 12.6496(3) Å, β = 109.843(2)°, V = 1257.99 Å3 (Cs). In the crystal structure of M3VO2(SO4)2, [VO2(SO4)2]3? complex anions can be discerned in which the vanadium atom is surrounded by five oxygen atoms: two oxygen atoms form short terminal V–O bonds, and three oxygen atoms are from the two sulfato groups, one of which acts as a monodentate ligand and the other acts as a bidentate chelating ligand. 相似文献
15.
A. R. Zaripov V. A. Orlova V. I. Pet’kov O. M. Slyunchev D. D. Galuzin S. I. Rovnyi 《Russian Journal of Inorganic Chemistry》2009,54(1):45-51
The new phosphate Cs2Mn0.5Zr1.5(PO4)3 was synthesized for the first time and characterized by X-ray diffraction. Its crystal structure was refined in space group P213, Z = 4 at 25°C (a = 10.3163(1) Å, V = 1097.93(1) Å3), by the Rietveld method using the powder X-ray diffraction data. The structure is built of an octahedral-tetrahedral framework {[Mn0.5Zr1.5(PO4)3]2?}3∞ with cesium atoms being located in large cavities. The hydrolytic stability of the powdered phosphate containing 137Cs radionuclide was studied. The minimum achieved 137Cs leaching rate was 4 × 10?8 g/cm2 day. 相似文献
16.
Novel complex salts [Au(en)2]Cl(ReO4)2 (I) and [Au(en)2](ReO4)3 (II), en = ethylenediamine, are obtained. Their crystal structures are determined by single crystal X-ray diffraction. Complex I crystallizes in the triclinic crystal system: a = 6.2172(7) Å, b = 7.1644(8) Å, c = 8.8829(8) Å, α = 96.605(4)°, β = 110.000(4)°, γ = 97.802(4)°, P-1 space group, Z = 1, d x = 3.905 g/cm3; complex II crystallizes in the monoclinic crystal system: a = 15.244(2) Å, b = 7.6809(8) Å, c = 9.3476(12) Å, β = 127.004(3)°, C2 space group, Z = 4, d x = 4.057 g/cm3. 相似文献
17.
D. A. Rusakov A. A. Filaretov A. P. Bobylev V. P. Danilov L. N. Komissarova 《Russian Journal of Inorganic Chemistry》2007,52(12):1844-1854
Indium strontium hydrogen nitrate SrIn2[PO3(OH)]4 was synthesized under mild hydrothermal conditions (T = 180 or 200°C) and characterized using IR spectroscopy, chemical analysis, and thermal analysis. A structure model obtained ab initio was refined by the Rietveld method: a= 9.6412(1) Å, b = 13.763(1) Å, c = 9.3579(1) Å, R obs = 0.0183, R p = 0.0493 (space group B2212, Z = 4). The acentricity of the structure was confirmed by SHG tests (I 2ω/I 2ω(SiO2) ≈ 2.0). In the SrIn2[PO3(OH)]4 structure, indium atoms reside in distorted InO6 octahedra and form, together with PO3(OH) tetrahedra, a mixed 3D structure {In2[PO3(OH)]4} 3∞ 2? whose voids are occupied by Sr2+ cations (CN = 8). The block-dimer In2(HPO4)10 is the most informative unit of the framework. Blocks are condensed into infinite columns running in the [101] direction. The compound is thermally stable up to 400°C. 相似文献
18.
The crystal structure of dichlorobis(dimethylsulfoxide-O)copper(II), [CuCl2(DMSO)2] (I), previously determined by Willett and Chang, is reinvestigated. It crystallizes in the orthorhombic system with the space group Pnma (N°62), Z = 4, and unit cell parameters a = 8.053(1) Å, b = 11.642(5) Å, c = 11.347(3) Å. Our structure determination is of a significantly higher precision in terms of bond lengths, angles, and R factors (e.g., Cu1–O1 = 1.9737(24) Å, O1–Cu1–O1i = 173.08(13)° (symmetry code: I x, 1/2–y, z) and R(F 2) = 0.046 compared to 1.955(4) Å, 173.0(3)° and R(F) = 0.075). In contrast to the previous investigation, all H atoms are placed at calculated positions. In the title molecule, the CuII atom is five coordinated in a distorted square pyramidal geometry. Thus, as reported previously, it can be shown that the crystal structure consists of [CuCl2(DMSO)2] molecules which, by virtue of long Cu–Cl interactions, are tied together to form chains parallel to the [100] direction. The density functional theory (DFT) optimized structure at the B3LYP/6-311++G(2d,2p) level is compared with the experimentally determined molecular structure. The HOMO-LUMO energy gap and other related molecular properties are also calculated. Comprehensive experimental and theoretical structural studies on the studied complex are carried out by FT-IR and UV-visible spectroscopies. 相似文献
19.
The subsolidus region of the Ag2MoO4-MgMoO4-Al2(MoO4)3 ternary salt system has been studied by X-ray phase analysis. The formation of new compounds Ag1 ? x Mg1 ? x Al1 + x (MoO4)3 (0 ≤ x ≤ 0.4) and AgMg3Al(MoO4)5 has been determined. The Ag1 ? x Mg1 ? x Al1 + x (MoO4)3 variable-composition phase is related to the NASICON type structure (space group R \(\bar 3\) c). AgMg3Al(MoO4)5 is isostructural to sodium magnesium indium molybdate of the same formula unit and crystallizes in triclinic system (space group P \(\bar 1\), Z = 2) with the following unit cell parameters: a = 9.295(7) Å, b = 17.619(2) Å, c = 6.8570(7) Å, α = 87.420(9)°, β = 101.109(9)°, γ = 91.847(9)°. The compounds Ag1 ? x Mg1 ? x Al1 + x (MoO4)3 and AgMg3Al(MoO4)5 are thermally stable up to 790 and 820°C, respectively. 相似文献
20.
A. V. Oreshkina G. Z. Kaziev T. Yu. Glazunova 《Russian Journal of Inorganic Chemistry》2008,53(10):1552-1556
Tetramminenickel hydrogen hexamolybdoaluminate and hexamolybdogallate(III) of compositions [Ni(NH3)4] · H[AlMo6O18(OH)6] · 10H2O (I) and [Ni(NH3)4] · H[GaMo6O18(OH)6] · 10H2O (II) were synthesized and characterized by mass spectrometry, thermogravimetry, X-ray powder diffraction, and IR spectroscopy. Their crystals are triclinic. For compound I, a= 17.30 Å, b= 14.69 Å, c= 10.45 Å, α = 129.07, β = 65.91°, γ = 138.01°, V = 1338.7l Å3, ρcalcd = 2.75g/cm3, Z = 2; for compound II, a = 17.38 Å, b= 14.75 Å, c= 10.51 Å, α = 131.38°, β= 65.96°, γ = 138.09, V = 1338.15 Å3, ρcalcd = 2.68 g/cm3, Z = 2. 相似文献