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1.
Interactions in the ternary system K2MoO4-Lu2(MoO4)3-Hf(MoO4)2 have been studied by X-ray powder diffraction and differential thermal analysis. A new triple (potassium lutetium hafnium) molybdate with the 5: 1: 2 stoichiometry has been found. Single crystals of this molybdate have been grown. Its X-ray diffraction structure has been refined (an X8 APEX automated diffractometer, MoK α radiation, 1960 F(hkl), R = 0.0166). The trigonal unit cell has the following parameters: a = 10.6536(1) ?, c = 37.8434(8) ?, V = 3719.75(9) ?, Z = 6, space group R c. The mixed 3D framework of the structure is built of Mo tetrahedra sharing corners with two independent (Lu,Hf)O6 octahedra. Two sorts of potassium atoms occupy large framework voids. Original Russian Text ? E.Yu. Romanova, B.G. Bazarov, R.F. Klevtsova, L.A. Glinskaya, Yu.L. Tushinova, K.N. Fedorov, Zh.G. Bazarova, 2007, published in Zhurnal Neorganicheskoi Khimii, 2007, Vol. 52, No. 5, pp. 815–818.  相似文献   

2.
Phase relations have been investigated in the subsolidus region of the Na2MoO4-NiMoO4-Fe2(MoO4)3 system by X-ray diffraction, differential thermal analysis, and vibrational spectroscopy. The phase of variable composition Na1−x Ni1−x Fe1+x (MoO4)3(0≤x≤0.5) with the NASICON structure (space group R c) and the NaNi3Fe(MoO4)5 ternary molybdate crystallizing in the triclinic crystal system (space group P ) have been obtained. A high conductivity was found in Na1−x Ni1−x Fe1+x (MoO4)3, which allows one to consider this phase of variable composition as a promising solid electrolyte with sodium ion conduction. Original Russian Text ? N.M. Kozhevnikova, A.V. Imekhenova, 2009, published in Zhurnal Neorganicheskoi Khimii, 2009, Vol. 54, No. 4, pp. 695–700.  相似文献   

3.
The crystal structure of cesium diberyllium phosphate hydrophosphate Cs[Be2(PO4)(PO4H)] obtained hydrothermally is analyzed. Unit cell parameters are: a = 4.8860(5) ?, b = 10.7330(11) ?, c = 13.0061(15) ?, α = 92.540(10)°, β = 92.451(9)°, γ = 90.948(9)°, space group P . In the structural motif consisting of PO4 and BeO4 tetrahedra, Be,P two-link chains and ribbons are distinguished, typical of a short a-translation of ≈4.9 ?. The presence of ternary and terminal O ligands along with bridging ones determines the term interrupted super framework. The group of two Be tetrahedra with a common edge is detected for beryllium phosphates for the first time. Original Russian Text Copyright ? 2009 by V. V. Bakakin, Yu. V. Seretkin, and S. P. Demin __________ Translated from Zhurnal Strukturnoi Khimii, Vol. 50, No. 2, pp. 369–373, March–April, 2009.  相似文献   

4.
A new compound [MNII(Phen)3]2+(B6H7)2 is synthesized; its crystal structure is studied by XRD at 100 K. Crystallographic data: C36H38B12N6Mn, M = 739.39, triclinic symmetry, space group P , unit cell parameters: a = 10.3131(3) ?, b = 13.4839(4) ?, c = 15.1132(4) ?; α = 97.696(1)°, β = 108.324(1)°, γ = 102.211(1)°; V = 1903.9(1) ?3, Z = 2, d calc = 1.290 g/cm3. The structure is solved by direct and Fourier methods and refined by full-matrix LSM in the anisotropic (isotropic for hydrogen atoms) approximation to the final factor R 1 = 0.036 for 10169 I hkl ≥ 2σ I (Bruker-Nonius X8 APEX CCD diffractometer, λMoK α). The structure contains two crystallographically different anions. Original Russian Text Copyright ? 2009 by T. M. Polyanskaya, M. K. Drozdova, V. V. Volkov, and K. G. Myakishev __________ Translated from Zhurnal Strukturnoi Khimii, Vol. 50, No. 2, pp. 381–385, March–April, 2009.  相似文献   

5.
Subsolidus phase relations in the Ag2MoO4-CuO-MoO3 oxide-salt ternary system were determined. T-x diagram was plotted for the Ag2MoO4-CuMoO4 quasi-binary join. Double molybdate Ag2Cu2(MoO4)3 was found to exist on this join. This compound is a superstructure derived from orthorhombic Li3Fe(MoO4)3. Its structure was solved in terms of a subcell (a = 5.0749(3), b = 11.300(2), c = 18.127(3) ?, space group Pnma, Z = 4, R = 0.0678). In the true unit cell, the parameter a is tripled; suggested space group is P212121. A characteristic feature of the Ag2Cu2(MoO4)3 structure is infinite columns (extended along axis a) of face-sharing oxygen octahedra, in which disordered silver atoms are located (Ag(21), Ag(22), and Ag(23)) with various degrees of irregularity of their octahedral coordination and a strong anisotropy of thermal vibrations. Distorted CuO6 octahedra form zigzag ribbons extended in the same direction. MoO4 tetrahedra, which are arranged according to the pseudo-hexagonal law, link the aforementioned major structural elements into a three-dimensional framework. Trigonal-prismatic voids of the framework are occupied by silver atoms Ag (1). Presumably, the disorder of the silver ions in octahedral columns can be responsible for the increased ion conductivity of silver copper molybdate. A partial order of the same ions is the most likely reason for the appearance of superstructure with the tripled unit cell volume. Original Russian Text ? G.D. Tsyrenova, S.F. Solodovnikov, E.T. Pavlova, E.G. Khaikina, Z.A. Solodovnikova, 2009, published in Zhurnal Neorganicheskoi Khimii, 2009, Vol. 54, No. 5, pp. 802–809.  相似文献   

6.
Subsolidus phase relations in the Cs2MoO4-MMoO4-Zr(MoO4)2 (M = Mn, Zn) ternary systems were determined, and two groups of new isostructural triple molybdates were synthesized: Cs2MZr(MoO4)4 and Cs2MZr2(MoO4)6 (M = Mn, Mg, Co, Zn). Cs2MnZr2(MoO4)6 and Cs2MnZr(MoO4)4 crystals were grown by spontaneous flux crystallization and used in structure solution for both groups of compounds. The Cs2MnZr2(MoO4)6 structure (a =13.4322(2) ?, c = 12.2016(3) ?, group R3, Z = 3, R = 0.0367) is a new structure type characterized by a mixed three-dimensional framework built of corner-sharing MoO4 tetrahedra and (M, Zr)O6 octahedra where large channels are occupied by cesium cations. Cs2MnZr2(MoO4)4 (a =5.3890(1) ?, c = 8.0685(3) ?, space group P $ \bar 3 $ \bar 3 m1, Z = 0.5, R = 0.0247) has the layered glaserite-like KAl(MoO4)2 type structure, where Al3+ octahedral positions are randomly occupied by a 0.5M2+ + 0.5Zr4+ mixture.  相似文献   

7.
Phase relations have been studied for the subsolidus region of the Dy2O3-HfO2-MoO3 system; binary molybdates, Dy2Hf(MoO4)5 and Dy2Hf2(MoO4)7, were found to form. The crystal structure of the latter has been solved (a = 20.661(3) , b = 9.816(1) , c = 13.796(3) , = 113.47(1)°, Z = 4, space group C2/c, R = 0.023) and found to be a new type of structure. In the structure, MoO4 tetrahedra are linked by their vertices with HfO6 octahedra and DyO8 tetragonal antiprisms to form a 3D open-work, in which one can isolate double-row tetrahedral and octahedral chains extended down the c axis.Original Russian Text Copyright © 2004 by S. F. Solodovnikov, B. G. Bazarov, E. Yu. Badmaeva, Yu. L. Tushinova, E. S. Zolotova, and Zh. G. BazarovaTranslated from Zhurnal Strukturnoi Khimii, Vol. 45, No. 4, pp. 692–697, July–August, 2004.This revised version was published online in April 2005 with a corrected cover date.  相似文献   

8.
Phases of variable composition K1−x A1−x R1+x (MoO4)3) (0 ≤ x ≤ 0.2–0.6), where A = Ni, Mg, Co, or Mn and R = Yb, Lu, or Sc, which crystallize in a NASICON-type structure (space group R c) were synthesized by solid-phase reactions. Their crystal parameters were calculated, and IR and Raman spectra described. Original Russian Text ? N.M. Kozhevnikova, T.N. Khamaganova, 2008, published in Zhurnal Neorganicheskoi Khimii, 2008, Vol. 53, No. 5, pp. 864–865.  相似文献   

9.
Two new mixed organic-inorganic uranyl molybdates, (C6H14N2)3[(UO2)5(MoO4)8](H2O)4 (1) and (C2H10N2)[(UO2)(MoO4)2] (2), have been obtained by hydrothermal methods. The structure of 1 [triclinic, , Z=1, a=11.8557(9), b=11.8702(9), c=12.6746(9) Å, α=96.734(2)°, β=91.107(2)°, γ=110.193(2)°, V=1659.1(2) Å] has been solved by direct methods and refined on the basis of F2 for all unique reflections to R1=0.058, which was calculated for the 5642 unique observed reflections (|Fo|?4σF). The structure contains topologically novel sheets of uranyl square bipyramids, uranyl pentagonal bipyramids, and MoO4 tetrahedra, with composition [(UO2)5(MoO4)8]6−, that are parallel to (−101). H2O groups and 1,4-diazabicyclo [2.2.2]-octane (DABCO) molecules are located in the interlayer, where they provide linkage of the sheets. The structure of 2 [triclinic, , Z=2, a=8.4004(4), b=11.2600(5), c=13.1239(6) Å, α=86.112(1)°, β=86.434(1)°, γ=76.544(1)°, V=1203.14(10) Å] has been solved by direct methods and refined on the basis of F2 for all unique reflections to R1=0.043, which was calculated for 5491 unique observed reflections (|Fo|?4σF). The structure contains topologically novel sheets of uranyl pentagonal bipyramids and MoO4 tetrahedra, with composition [(UO2)(MoO4)2]2−, that are parallel to (110). Ethylenediamine molecules are located in the interlayer, where they provide linkage of the sheets. All known topologies of uranyl molybdate sheets of corner-sharing U and Mo polyhedra can be described by their nodal representations (representations as graphs in which U and Mo polyhedra are given as black and white vertices, respectively). Each topology can be derived from a simple black-and-white graph of six-connected black vertices and three-connected white vertices by deleting some of its segments and white vertices.  相似文献   

10.
Phase equilibria in the subsolidus region of the Na2MoO4-Hf(MoO4)2 system have been investigated. The existence of Na2Hf(MoO4)3 was confirmed, and a new binary molybdate, Na8Hf(MoO4)6, has been found, whose crystal structure with dimensions a = 20.661(3) Å, b = 9.816(1) Å, c = 13.796(3) Å, β = 113.47(1)°, Z = 4, space group C2/c, R = 0.023 is similar to that of K8Hf(MoO4)6. In the structure, each HfO6 octahedron is linked (through common vertices) to six MoO4 tetrahedra, forming [Hf(MoO4)6]8− cluster groups. Between the groups are Na+ ions having considerably distorted tetragonal pyramidal or octahedral oxygen surroundings; c.n. of sodium here is 5 or 6 versus c.n. = 7–9 of potassium in K8Hf(MoO4)6. The open irregular environment of sodium and the continuous three-dimensional openwork of oxygen polyhedra around sodium suggest that Na8Hf(MoO4)6 or its analogs may be good ion conductors.Original Russian Text Copyright © 2004 by S. F. Solodovnikov, B. G. Bazarov, L. V. Balsanova, Z. A. Solodovnikova, and Zh. G. Bazarova__________Translated from Zhurnal Strukturnoi Khimii, Vol. 45, No. 6, pp. 1044–1048, November–December, 2004.  相似文献   

11.
The [Ni(DDM)2(NO3)2(H2O)2] complex (DDM is 4,4-diaminodiphenylmethane [CH2(C6H4NH2)2]) is synthesized, and its structure is determined. The crystals are triclinic, space group P , a = 5.846(1) ?, b = 9.450(2) ?, c = 13.390(3) ?, α = 105.63(3)°, β = 98.13(3)°, γ = 105.84(3)°, V = 666.6(2) ?3, ρcalcd = 1.553 g/cm3, Z = 2. The Ni(II) ion (in the inversion center) is bound to a distorted octahedral array formed by the nitrogen atoms of the primary amino groups of the DDM molecules and the oxygen atoms of the monodentate nitrato groups and water molecules (Ni(1)-N(3) 2.119(2) ?, Ni(1)-O(1) 2.122(2) ?, Ni(1)-O(w) 2.047(2) ?, angles at the Ni atoms vary in the 85.08(9)°–94.92(9)° interval). The structure contains supramolecular metallacycles formed by the O(w)-H…N(2) hydrogen bonds between the coordinated H2O molecules and the terminal amino groups of DDM. The metallacycles are joined by the Ni2+ ions into infinite chains running in the [111] direction. Original Russian Text ? Yu.V. Kokunov, V.V. Kovalev, Yu.E. Gorbunova, 2008, published in Zhurnal Neorganicheskoi Khimii, 2008, Vol. 53, No. 11, pp. 1838–1843.  相似文献   

12.
The subsolidus area of Cs2MoO4-Al2(MoO4)3-Zr(MoO4)2 system was studied by X-ray powder diffraction. Two new molybdates with component molar ratios of 1: 1: 1 (S1) and 5:1:2 (S2) were synthesized for the first time. The crystallographic parameters of the 5:1:2 compound were determined. Solution- melt crystallization and spontaneous nucleation yielded crystals of new 1:1:1 cesium aluminum zirconium molybdate Cs(AlZr0.5)(MoO4)3. Its formula unit and crystal structure were refined by X-ray diffraction (1592 reflections, R=0.0249). Trigonal crystals: a=12.9441(2) ?, c=12.0457(4) ?, V=1747.86(7) ?3, Z = 6, space group R $ \bar 3 $ \bar 3 . The three-dimensional combined framework of this structure is formed by MoO4 tetrahedrons linked through common vertices to (Al,Zr)O6 octahedrons. Cesium atoms occupy large cavities of the framework. Crystallographic position M(1) is occupied by randomly distributed Al3+ and Zr4+ cations.  相似文献   

13.
The complexes of CdI2 with acetamide (AA) and propaneamide (PrA) of the composition [Cd(AA)6][Cd2I6] (I) and [Cd(PrA)6][Cd2I6] (II) were synthesized and studied by X-ray diffraction. Isostructural crystals I and II are triclinic: a = 7.285(3) and 8.066(6), b = 11.266(4) and 11.649(3), c = 11.554(3) and 12.063(2) ?, α = 100.96(2)° and 102.74(2)°, β = 91.59(2)° and 91.73(4)°, γ = 100.76(3)° and 101.05(4)°, V = 912.5 and 1081.9 ?3, respectively; space group , Z = 1. Original Russian Text ? I.A. Zamilatskov, E.V. Savinkina, D.V. Al’bov, 2007, published in Koordinatsionnaya Khimiya, 2007, Vol. 33, No. 6, pp. 407–410.  相似文献   

14.
1-Allyl-4-aminopyridinium chloride reacts with Cu(NO3)2 · 3H2O in an ethanolic solution under the conditions of ac electrochemical synthesis at copper electrodes to form crystals of compound [(NH2C5H4N(C3H5))2Cu3Cl3(NO3)2] (I). The crystals of compound I are monoclinic: space group P21/c, Z = 4, a = 25.770(7), b = 7.230(4), c = 12.505(5) ?, β = 92.58(3)°, V = 2328(2) ?3. The direct interaction of 1-allylquinolinium nitrate with Cu(NO3)2 · 3H2O in a methanolic solution in the presence of metallic copper yields crystals of compound [C9H7N(C3H5)Cu(NO3)2] (II). The crystals of compound II are triclinic: space group P , a = 6.756(3), b = 8.391(4), c = 12.489(5) ?, α = 77.18(3)°, β = 89.48(4)°, γ = 73.32(3)°, V = 662.0(5) ?3. The structure of compound I is built of infinite linear anions: polymeric fragments {(NH2C5H4N(C3H5))2Cu3Cl3(NO3)2} n . Each of two copper atoms (Cu(1) and Cu(2)) π-coordinates the C=C bonds of the allyl groups of the 1-allyl-4-aminopyridinium cations, the oxygen atom of the nitrate ions, and two chlorine atoms. The third copper atom Cu(3) is linearly linked with two chlorine atoms. Particular polymeric fragments are additionally joined by the N-H…O, C-H…O, C-H…Cl hydrogen bonds. The crystal structure of compound II is built-up of the isolated L2Cu2(NO3)4 fragments (L is the 1-allylquinolinium cation). The metal atom is localized in the trigonal pyramidal coordination environment of three oxygen atoms of the nitrate ions and of the C=C bond of the allyl group of the cation. The particular L2Cu2(NO3)4 fragments are additionally joined by the C-H…O hydrogen bonds. Original Russian Text ? A.V. Pavlyuk, T. Lis, M.G. Mys’kiv, 2009, published in Koordinatsionnaya Khimiya, 2009, Vol. 35, No. 6, pp. 458–462.  相似文献   

15.
Triple molybdate NaCoCr(MoO4)3, a phase of variable composition Na2MoO4-CoMoO4-Cr2(MoO4)3 (0 ≤ x ≤ 0.5) having nasicon structure (space group R $ \bar 3 $ \bar 3 c), and triple molybdate NaCo3Cr(MoO4)5 crystallizing in triclinic space group P $ \bar 1 $ \bar 1 were synthesized in the subsolidus region of the Na2MoO4-CoMoO4-Cr2(MoO4)3 ternary salt system. Crystal parameters were calculated for the newly synthesized molybdates and phases. The vibration spectra of Na1 − x Co1 − x Cr1 + x (MoO4)3 and electrophysical properties were studied. Upon Na + Co → Cr(III) substitution, chromium cations are distributed to cobalt sites and additional vacancies are generated in the sodium sublattice.  相似文献   

16.
The subsolidus region of the Cs2MoO4-Bi2(MoO4)3-Zr(MoO4) system was studied by X-ray powder diffraction. Quasi-binary sections were elucidated, and triangulation performed. Triple molybdates with the component ratios 5: 1: 2 (S 1) and 2: 1: 4 (S 2) were prepared for the first time. Crystals of cesium bismuth zirconium molybdate of the 5: 1: 2 stoichiometry (Cs5BiZr(MoO4)6) were grown from fluxed melts with spontaneous nucleation. The composition and crystal structure of this triple molybdate were refined using X-ray diffraction data (collected on X8 APEX automated diffractometer, MoK α radiation, 2348 F(hkl), R = 0.0226). The trigonal unit cell parameters were as follows: a = b = 10.9569(2), c = 39.804(4) Å, V = 4138.4(4) Å3, Z = 6, space group R $ \bar 3 The subsolidus region of the Cs2MoO4-Bi2(MoO4)3-Zr(MoO4) system was studied by X-ray powder diffraction. Quasi-binary sections were elucidated, and triangulation performed. Triple molybdates with the component ratios 5: 1: 2 (S 1) and 2: 1: 4 (S 2) were prepared for the first time. Crystals of cesium bismuth zirconium molybdate of the 5: 1: 2 stoichiometry (Cs5BiZr(MoO4)6) were grown from fluxed melts with spontaneous nucleation. The composition and crystal structure of this triple molybdate were refined using X-ray diffraction data (collected on X8 APEX automated diffractometer, MoK α radiation, 2348 F(hkl), R = 0.0226). The trigonal unit cell parameters were as follows: a = b = 10.9569(2), c = 39.804(4) ?, V = 4138.4(4) ?3, Z = 6, space group R c. The mixed-metal three-dimensional framework in this structure is built of Mo tetrahedra and two sorts of (Bi,Zr)O6 octahedra. Large interstices accommodate two sorts of cesium atoms. The Bi3+ and Zr4+ cation distributions over two positions were refined during structure solution. Original Russian Text ? B.G. Bazarov, T.V. Namsaraeva, R.F. Klevtsova, A.G. Anshits, T.A. Vereshchagina, R.V. Kurbatov, L.A. Glinskaya, K.N. Fedorov, Zh.G. Bazarova, 2008, published in Zhurnal Neorganicheskoi Khimii, 2008, Vol. 53, No. 9, pp. 1585–1589.  相似文献   

17.
The crystals of [C9H7NC3H5]Cu(SCN)2 (I) and [C9H7NC3H5]Cu2(SCN)3 (II) were obtained in the reaction of N-allylquinolinium bromide with CuSCN and NH4SCN in a methanol solution. The crystals of I are triclinic: space group P , Z = 2, a = 8.619(2), b = 8.755(2), c = 10.463(3) ?, α = 77.18(3), β = 69.95(3), γ = 79.38(3)°, V = 718.1(3) ?3. The crystals of II are opthorhombic: space group P212121, Z = 4, a = 5.744(2), b = 16.799(4), c = 17.980(5), V = 1735.9(9) ?3. The structure of compound I is built of infinite linear {Cu(SCN)2} anions and the N-allylquinolinium cations bonded additionally by relatively weak hydrogen contacts C-H...S. The [C9H7NC3H5]+ cations are located between the corrugated layers of the {Cu2(SCN)3} anions in compound II. As in the case of the previously studied copper(I) halide complexes, the C=C bond of the allyl group in the N-allylquinolinium cation of complexes I, II does not interact with Cu(I). Original Russian Text ? A.V. Pavlyuk, V. Kinzhybalo, T. Lis, M.G. Mys’kiv, 2008, published in Koordinatsionnaya Khimiya, 2008, Vol. 34, No. 10, pp. 764–769.  相似文献   

18.
19.
Physicochemical analysis (XRPA, DTA) was used to study phase equilibria in a ternary salt system Rb2MoO4-Fe2(MoO4)3-Hf(MoO4)2 in the subsolidus region. Ternary molybdates with compositions 5:1:3, 5:1:2, and 1:1:1 have been found and synthesized. Crystal and thermal characteristics have been determined. Single crystals of the ternary molybdate Rb5FeHf(MoO4)6 with a composition of 5:1:2 were grown. The crystal structure of the compound was solved using X-ray diffractometry (CAD-4 automatic diffractometer, MoK α radiation, 1766 F(hkl), R = 0.0298). Hexagonal crystals with unit cell dimensions: a = b = 10.124(1) Å, c =15.135(3) Å, V = 1343.4(4) Å3, Z = 2, ρcalc = 4.008 g/cm3, space group P63. The mixed three-dimensional framework of the structure is formed from two sorts of MoO4 tetrahedra and Fe and Hf octahedra linked through their common O-vertices. Rubidium atoms of three varieties occupy the large voids of the framework.Original Russian Text Copyright © 2004 by B. G. Bazarov, R. F. Klevtsova, A. D. Tsyrendorzhieva, L. A. Glinaskaya, and Zh. G. Bazarova__________Translated from Zhurnal Strukturnoi Khimii, Vol. 45, No. 6, pp. 1038–1043, November–December, 2004.  相似文献   

20.
The structure of Ir(CO)2(acac) is determined by XRD at room temperature. Crystallographic data for C7H7IrO4 are: a = 6.4798(5) ?, b = 7.7288(5) ?, c = 9.1629(10) ?, α = 105.738(2)°, β = 90.467(3)°, γ = 100.658(2)°, space group 1, P , V= 433.24(6) ?3, Z = 2, d calc = 2.662 g/cm3, R = 0.0167. The structure is built of isolated mononuclear molecules. The central iridium atom has a square coordination environment formed by two oxygen atoms that belong to the acetylacetonate ligand and two carbon atoms of carbonyl groups. The average Ir-O and Ir-C bond lengths are 2.045(3) ? and 1.832(6) ? respectively. Molecules are stacked in such a way that the planes of coordination squares turn out to be parallel to the Ir...Ir distances between the nearest neighbors in the stack of 3.242 ? and 3.260 ?. Original Russian Text Copyright ? 2009 by K. V. Zherikova, N. V. Kuratieva, and N. B. Morozova __________ Translated from Zhurnal Strukturnoi Khimii, Vol. 50, No. 3, pp. 595–597, May–June, 2009.  相似文献   

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