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1.
The principles of complex phosphate crystallization in K2O-P2O5-TiO2-NiO solution melts are studied for the ratios K/P = 0.7?1.4, Ti/P = 0.15, and Ni/Ti = 0.1?2.0. The phase-formation field and parameters are determined for a new complex phosphate K4Ti3Ni(PO4)6, which is isostructural to langbeinite. A single-crystal X-ray diffraction experiments is carried out for this phosphate (space group P213, a = 9.8247(10) Å).  相似文献   

2.
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   

3.
(NH4)Sb4F13 crystals (I) are synthesized and their crystal structure (tetragonal crystal system: a = 9.6431(2) Å, c = 6.5503(2) Å, V = 609.11(3) Å3, Z = 2, d calc = 4.100 g/cm3, F(000) = 664, space group I4?) is determined. The main structural units of I are tetranuclear anionic [Sb4F13]? complexes and [NH4]+ cations. The anionic complexes are built of four SbF3 groups linked together by tetrahedral bridging fluorine atom. At room temperature the (NH4)Sb4F13 crystals are isostructural to previously studied МSb4F13 (М = K, Rb, Cs, and Tl). The study of 121,123Sb NQR spectra of compound I is performed in a range of 77-370 K, which shows that when the temperature decreases (<250 K) the substance exhibits piezoelectric properties, as do other compounds of this group, but with a violation of their isostructurality.  相似文献   

4.
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   

5.
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   

6.
The reaction of cyclopentylamine with 2-hydroxy-1-naphthaldehyde and 5-nitrosalicylaldehyde, respectively, in methanol affords two new Schiff bases, 1-(cyclopentyliminomethyl)naphthalen-2-ol (HL1) and 4-nitro-2-(cyclopentyliminomethyl)phenol (HL2). Two new zinc(II) complexes, [Zn(L1)2] (I) and [Zn(L2)2] (II), derived from the Schiff bases, have been prepared and characterized by single-crystal X-ray diffraction, FT-IR, and elemental analysis. Complex I crystallizes in the monoclinic space group P21/c with a = 17.834(4), b = 14.738(3), c = 9.868(2) Å, β = 91.20(3)°, V = 2593.1(9) Å3, Z = 4. Complex II crystallizes in the triclinic space group P \(\bar 1\) with a = 10.206(1), b = 10.502(1), c = 12.554(1) Å, α = 66.771(2)°, β = 78.133(2)°, γ = 76.292(2)°, V = 1191.8(1) Å3, Z = 2. The Zn atom in each complex is coordinated by two N and two O atoms from two Schiff base ligands, forming a tetrahedral geometry. The Schiff bases and the complexes were assayed for antibacterial activities.  相似文献   

7.
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   

8.
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   

9.
The structures of the Pd4(SBu)4(OAc)4 (I) and Pd6 (SBu)12 (II) palladium clusters are determined by the X-ray diffraction method. For cluster I: a = 8.650(2), b = 12.314(2), c = 17.659(4) Å, α = 78.03(3)°, β = 86.71(2)°, γ = 78.13(3)°, V = 1800.8(7) Å3, ρcalcd = 1.878 g/cm3, space group P \(\bar 1\), Z = 4, N = 3403, R = 0.0468; for structure II: a = 10.748(2), b = 12.840(3), c = 15.233(3) Å, α = 65.31(3)°, β = 70.10(3)°, γ = 72.91(3)°, V = 1767.4(6) Å3, ρ calcd = 1.605 g/cm3, space group P \(\bar 1\), Z = 1, N = 3498, R = 0.0729. In cluster I, four Pd atoms form a planar cycle. The neighboring Pd atoms are bound by two acetate or two mercaptide bridges (Pd…Pd 2.95–3.23 Å, Pd…Pd angles 87.15°–92.85°). In cluster II, the Pd atoms form a planar six-membered cycle with Pd···Pd distances of 3.09–3.14 Å, the PdPdPd angles being 118.95°–120.80°. The Pd atoms are linked in pairs by two mercaptide bridges. The formation of clusters I and II in solution is proved by IR spectroscopy and calorimetry. Analogous clusters are formed in solution upon the reaction of palladium(II) diacetate with thiophenol.  相似文献   

10.
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   

11.
A ternary salt system Rb2MoO4-Eu2(MoO4)3-Hf(MoO4)2 was studied in the subsolidus area by X-ray phase analysis. A novel ternary molybdate, Rb4.98Eu0.86Hf1.11(MoO4)6, formed in the system. The Rb4.98Eu0.86Hf1.11(MoO4)6 rubidium-europium-hafnium molybdate crystals were grown by solution-melt crystallization under the spontaneous nucleation conditions. The structure and composition of this compound were refined by single crystal X-ray diffraction (X8 APEX automated diffractometer, MoK α radiation, 1753 F(hkl), R = 0.0183). The crystals are trigonal, a = b = 10.7264(1) Å, c = 38.6130(8) Å, V = 3847.44(9) Å3, Z = 6, space group R \(\bar 3\) c. The three-dimensional mixed framework of the structure comprises Mo tetrahedra and two types of octahedra, (Eu,Hf)O6 and HfO6. The large cavities of the framework include two types of the rubidium atom. The distribution of the Eu3+ and Hf4+ cations over two crystallographic positions was refined.  相似文献   

12.
Double phosphate Ba1.5Fe2(PO4)3 was synthesized and structurally studied. Single crystals were synthesized by the fusion method. Cubic crystals, Z = 4, space group P213, a = 9.866(1) Å. This structure is built of polyhedrons of four types: PO4 tetrahedrons, two virtually regular FeO6 octahedrons, BaO12 twelve-vertex polyhedrons, and BaO9 nine-vertex polyhedrons. These polyhedrons share common oxygen vertices to form three-dimensional [Fe2(PO4)3]3∞ framework containing barium atoms in cavities.  相似文献   

13.
The single crystals of [UO2SO4{(CH3)HNCONH(CH3)}2] (I) were synthesized and studied by X-ray diffraction. The crystals are monoclinic, a = 6.847(1) Å, b = 14.259(3) Å, c = 14.297(3) Å, β = 93.451(4)°, space group P21/n, Z = 4. The main structural units of crystals I are ribbons whose composition coincides with the composition of the compound. The crystal chemical formula of the complex is AT3M 2 1 (A = UO 2 2+ ).  相似文献   

14.
A new complex [UO2CrO4{CH3CON(CH3)2}2] (I) was studied by thermal analysis, IR spectroscopy, and X-ray crystallography. The crystals are monoclinic: a = 13.8108(11) Å, b = 8.6804(7) Å, c = 13.0989(10) Å, β = 104.777(1)°, V = 1518.4(2) Å3, space group P21/c, Z = 4, R = 2.39%. The structure of I contains infinite chains of the [UO2CrO4{CH3CON(CH3)2}2] composition running along [001]; the complex belongs to the AT11M1 2 crystal-chemical group (A = UO 2 2+ , T11 = CrO 4 2? , M1 = CH3CON(CH3)2) of uranyl complexes. The chains are linked into a three-dimensional framework due to hydrogen bonds between oxygen atoms of chromate ions and hydrogen atoms of methyl groups of the dimethylacetamide.  相似文献   

15.
Crystals of double polyphosphates EuCs5(PO3)8 (I) and GdCs5(PO3)8 (II) have been studied by X-ray diffraction. The isostructural crystals of I and II are monoclinic, space group C2. Only unit cell parameters have been determined for the crystals of double Pr and Cs polyphosphate (III). This crystal is isostructural with earlier studied La3Cs15P24O72 · 6H2O (IV). The crystals of compounds III and IV are triclinic, space group P1, Z = 1; a = 11.987(2) and 12.178(5) Å, b = 14.754(8) and 14.740(8) Å, c = 14.692(8) and 14.847(9) Å, α = 60.15(4)° and 60.87(5)°, β = 67.04(4)° and 66.35(4)°, γ = 78.76(3)° and 77.54(4)°, respectively. In compounds I and II, the polyphosphate anions exist as infinite chains. The MIIIO8 polyhedra are isolated from each other but share edges and faces with the CsO n polyhedra.  相似文献   

16.
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   

17.
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   

18.
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   

19.
A new reduced ferrous molybdophosphate composite solid of the formula, [(C10H14N2)H]4[FeII 10MoV 24(H2PO4)4(HPO4)12(PO4)4(H2O)16(OH)16O44]·12H2O, has been synthesized from a reaction mixture of MoO3, FeSO4·7H2O, C2H2O4·2H2O, nicotine, H3PO4, and H2O under hydrothermal conditions. The crystal data: monoclinic, space group C2/m, a = 24.4349(124), b = 12.9935(66), c = 14.7281(74) Å, β = 104.87(1) Å, V = 4520(4) Å3, Z = 2, R 1  = 0.0874, wR 2  = 0.2179. The structure is built from the building blocks of the formula, {FeII[Mo6P4O31]2}, consisting of a network of MO6 (M = Fe, Mo) octahedral and PO4 tetrahedral linked through their vertices. The connectivity of the building blocks with two pairs of face-sharing dinuclear Fe(II) clusters of the formula of [FeII 2(H2O)4O5] on which a phosphate group is hanging gives rise to one-dimensional chains with eight-membered apertures. The remarkable hydrogen bonded interactions between the chains form a unique and interesting framework with three-dimensional intersecting tunnels where the protonated nicotine molecules as structuring templates and crystallization water molecules are situated.  相似文献   

20.
The low-temperature heat capacity of Na2Lu (MoO4)(PO4) was measured by adiabatic calorimetry in the range of 7.47–345.74 K. The experimental data were used to calculate the thermodynamic functions of Na2Lu (MoO4)(PO4). At 298.15 K, the following values were obtained: C p 0 (298.15 K) = 237.7 ± 0.1 J/(K mol), S 0(298.15 K) = 278.1 ± 0.8 J/(K mol), H 0(298.15 K) ? H 0 (0 K) = 42330 ± 20 J/mol, and Φ0(298.15 K) = 136.1 ± 0. 3 J/(K mol). A heat capacity anomaly was found in the range of 10-67 K with a maximum at T tr = 39.18 K. The entropy and enthalpy of transition are ΔS = 12.39 ± 0.75 J/(K mol) and ΔH = 403 ± 16 J/mol. The thermal investigation of sodium lutetium molybdate phosphate in the high-temperature range (623–1223 K) was performed using differential scanning calorimetry. It was found that during melting in the range of 1030–1200 K, Na2Lu(MoO4)(PO4) degrades to simpler compounds; the degradation scenario is verified by X-ray powder diffraction.  相似文献   

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