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1.
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   

2.
Compounds described as V2O3(XO4)2, where X = S or Se, were prepared from vanadium(V) oxide mixtures with concentrated sulfuric and selenic acids. The physicochemical properties of the products were studied; for V2O3(SeO4)2, the crystal structure was determined by powder X-ray diffraction and neutron diffraction, and its key differences from the structure of V2O3(SO4)2 were identified. V2O3(SeO4)2 crystallizes in the monoclinic system with the unit cell parameters a = 15.3831(2)Å, b = 5.54096(5)Å, c = 9.71644(7)Å, β = 111.886(1)°, V = 768.51Å3, space group C2/c (no. 15).  相似文献   

3.
A new 3 D europium sulfate Eu2(H2O)4(SO4)3 1 is synthesized solvothermally and characterized by single crystal X-ray diffraction, IR spectrum, TG, powder XRD, and ultraviolet excitation and emission spectrum. This compound crystallizes in the triclinic system with the space group P-1, a = 6.7520(9) Å, b = 9.1077(12) Å, c = 10.5910(14) Å, α = 94.432(2)°, β = 107.1170(10)°, γ = 99.160(2)°, V = 609.17(14) Å3, Z = 2. The open framework of the title compound is an eight-membered ring channel along the crystallographic a-axis, which is built up by EuO8 polyhedra and SO4 tetrahedra.  相似文献   

4.
Synthesis was performed and physicochemical properties were studied for the M4V2O3(SO4)4 complexes, where M = K, Rb, or Cs. Their crystal structures were determined using the set of data from X-ray diffraction and neutron diffraction studies. All compounds crystallize in a triclinic lattice (space group \(P\bar 1\), Z = 2) with the parameters: a = 7.7688(2), 7.8487(1), 8.1234(1) Å; b = 10.4918(3), 10.8750(2), 11.1065(1) Å; c = 11.9783(4), 12.1336(2), and 11.8039(1) Å; α = 76.600(2)°, 77.910(1)°, 79.589(1)°; β = 75.133(2)°, 75.718(1)°, 87.939(1)°; γ = 71.285(2)°, 72.189(1)°, 75.567(1)°; V = 881.78(5), 945.42(3), 1014.34(2) Å3 for K, Rb, Cs, respectively. The structure of M4V2O3(SO4)4 was found to be formed by discrete complex anions V2O3(SO4) 4 4? incorporating two oxygen-bridged vanadium atoms in a distorted octahedral oxygen environment. The sulfate groups are coordinated by the vanadium atoms in the chelating mode with a large scatter of S-O interatomic distances and OSO angles. Every VO6 octahedron has a short terminal vanadium-oxygen bond with a length of about 1.6Å. The V2O3(SO4) 4 4? complex anions in potassium and rubidium compounds differ from that in Cs4V2O3(SO4)4 in the type of symmetry and mutual spatial orientation. The vibrational spectra were presented and interpreted in line with the structural analysis data.  相似文献   

5.
The KPb2Cl5 and KPb2Br5 crystals are monoclinic (P21/c) with a microtwinned structure. X-ray analysis of chloride resulted in the parameters a = 8.854(2) Å, b = 7.927(2) Å, c = 12.485(3) Å; β = 90.05(3)°, dcalc = 4.78(1) g/cm3 (STOE STADI4, MoKα, 2θmax = 80°), R1 = 0.0702 for 4094 F ≥ 4 σ(F) reflections. For bromide, a = 9.256(2) Å, b = 8.365(2) Å, c = 13.025(3) Å; β = 90.00(3)°, dcalc = 5.62(1) g/cm3 (Bruker P4, MoKα, 2θmax = 70°), R1 = 0.0692 for 3076 F ≥ 4 (F) reflections.  相似文献   

6.
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.
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   

8.
The hydrothermal reaction of a mixture of V2O5, VCl3, 2,5-pyridinedicarboxylic acid and diluted H2SO4 for 68 h at 180°C gives a blue colored solution which yields prismatic blue crystals of IV 2 IV O2(SO4)2(H2O)6] (1) in 32% yield (based on V). Complex 1 was investigated by means of elemental analysis (C, H and S), TGA, FT-IR, manganometric titration, Single Crystal X-ray Diffraction Methods and also comparative antimicrobial activities. Crystal data for the compound: monoclinic space group P21/c and unit cell parameters are a = 7.3850(12) Å, b = 7.3990(7) Å, c = 12.229(2) Å, β = 108.976(12)° and Z = 2. Although structure of 1 as a natural mineral has been previously determined, this work covers new preparation method and full characterization of 1 along with comparison of antibacterial activity between 1 and the commercial vanadium(IV) oxide sulfate hydrate compounds, VOSO4 · xH2O (Riedel-de Haën and Alfa Aesar brand names). 1 was evaluated for the antimicrobial activity against gram-positive, gram-negative bacteria, yeasts and mould compared with the commercial VOSO4 · xH2O compounds. 1 showed weak activity against bacteria Bacillus cereus, Nocardia asteroides and yeast Candida albicans. A good antimicrobial activity was recorded against Cirtobacter freundii (15 mm). There are only a few reproducible well-defined vanadium(IV) starting materials to use for exploring the synthesis of new materials. VCl4, VO(acac)2, VOSO4 · xH2O and [V(IV)OSO4(H2O)4] · SO4 · [H2N(C2H4)2NH2] are common starting materials for such applications. In addition to these compounds, 1 can be used as an oxovanadium precursor.  相似文献   

9.
The crystal structure of [Cu(En)2CrO4]n (En is ethylenediamine) is determined: a = 14.7359(4) Å, b = 9.8083(3) Å, c = 14.2664(4) Å, V = 2061.98(10) Å3, space group Cmce, Z = 8, dx = 1.931 g/cm3. It is demonstrated that the studied phase is isostructural with [Сu(Еn)2SO4]n. A pseudotetragonal copper atom coordination (Cu–N 2.0204 Å and 2.0244 Å, ∠N–Cu–N 84.73°) is completed to distorted octahedral by two oxygen atoms of chromate anions (Cu–O 2.433 Å and 2.380 Å).  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.
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   

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.
Single crystals of triple molybdate of composition 5:1:3 K5Pb0.5Hf1.5(MoO4)6 have been grown and their crystal structure has been solved from X-ray diffraction data (an automated diffractometer X8 APEX, MoK α -radiation, 2173 F(hkl), R = 0.0321). Trigonal unit cell parameters are: a = b = 10.739(2) Å, c = 37.933(9) Å; V = 3789(1) Å3, Z = 6, ρcalc = 4.014 g/cm3, space group \(R\bar 3\). Three-dimensional mixed framework of the structure is formed by two types of MoO4 tetrahedra and Pb and Hf octahedra linking via common O-vertices. Potassium atoms of three types occupy large vacancies in the framework.  相似文献   

15.
A novel one-dimensional chain complex [Cd(NITpPy)2(N(CN)2)2)] n (NITpPy = 2-(4′-pyridyl)-4,4,5,5-tetramethylimidazoline-1-oxyl-3-oxide) has been synthesized and characterized structurally. It crystallizes in the triclinic space group P \(\bar 1\) with a = 7.1742(13), b = 9.4913(17), c = 13.208(2) Å, α = 71.020(2)°, β=87.308(2)°, γ = 70.503(2)°, V = 799.8(3) Å3, C28H32CdN12O4, Mr = 713.06, Z = 1, ρ c = 1.48 g/cm3, μ(MoK α) = 0.736 mm?1, F(000) = 364, R = 0.0275 and wR = 0.0605 for 2702 observed reflections with I > 2σ(I). The crystal structure consists of infinite chains of [Cd(NITpPy)2(N(CN)2)2)] units linked by dicyanamide anions [N(CN)2]?. Each Cd2+ ion is six-coordinated with the geometry of a distorted octahedron.  相似文献   

16.
Powder and single crystal X-ray diffraction studies have been performed for anhydrous nitrate complexes Rb2[Pd(NO3)4] (I) and Cs2[Pd(NO3)4] (II). Crystal data for I: a = 7.843(1) Å, b = 7.970(1) Å, c = 9.725(1) Å; β = 100.39(1)°, V = 597.9(1) Å 3, space group P21/c, Z = 2, d calc = 2.918 g/cm3; for II: a = 10.309(2) Å, b = 10.426(2) Å, c = 11.839(2) Å; β = 108.17(3)°, V = 1209.0(4) Å3, space group P21/c, Z = 4, d calc = 3.408 g/cm3. The structures are formed by isolated [Pd(NO3)4]2? complex anions and alkali metal cations. The plane-square environment of the Pd atom is formed from the oxygen atoms of the monodentate nitrate groups. The geometrical characteristics of the complex anions are analyzed. Compound II has a short contact Pd...Cs 3.252 Å.  相似文献   

17.
The complex [Co(2-Me-Pyz)2(H2O)4](NO3)2 is synthesized and its structure is determined. The crystals are monoclinic: space group P21/n, a = 10.685(2) Å, b = 6.837(1), c = 12.515(3) Å, β = 91.84(3)°, V = 913.8(3) Å3, ρcalcd = 1.042 g/cm 3, Z = 2. The Co2+ ion (in the inversion center) is coordinated at the vertices of the distorted octahedron by two nitrogen atoms of methylpyrazine and four oxygen atoms of the water molecules (Co(1)–N(1) 2.180(3), average Co(1)–O(w) 2.079(3) Å, angles at the Co atom 87.9(1)–92.1(1)°). Supramolecular pseudometallocycles are formed in the structure through the O(w)–H…N(1) hydrogen bonds between the coordinated H2O molecules and the terminal nitrogen atoms of the 2-methylpyrazine molecules. Their interaction results in the formation of supramolecular layers joined by the NO3 groups into a three-dimensional framework.  相似文献   

18.
The heat capacities of Pb2V2O7 and Pb3(VO4)2 as a function of temperature in the range 350–965 K have been studied by the differential scanning calorimetry method. The CP = f(T) curve for Pb2V2O7 is described by the equation Cp = (230.76 ± 0.51) + (73.60 ± 0.50)×10-3T ? (18.38 ± 0.54)×105T-2 in the entire temperature range. For Pb3(VO4)2, there is a well-pronounced extreme point in the CP = f(T) curve at T = 371.5 K, which is caused by the existence of a structural phase transition. The thermodynamic properties of the oxide compounds have been calculated.  相似文献   

19.
The characteristics of crystal structures of the titanium(IV) diammonium (Ti(NH4)2P4O13) and tin(IV) diammonium (Sn(NH4)2P4O13) tetraphosphates, which are isostructural with similar silicon(IV) and germanium(IV) salts, have been obtained by the Rietveld method using X-ray powder diffraction data. The compounds crystallize in the triclinic system, space group P \(\overline 1 \), Z = 2, a = 15.0291(7) Å, b = 7.9236(4) Å, c = 5.0754(3) Å, α = 99.168(3)°, β = 97.059(3)°, γ = 83.459(3)° for Ti(NH4)2P4O13 and a = 15.1454(7) Å, b = 8.0103(5) Å, c = 5.1053(3) Å, α = 99.898(6)°, β = 96.806(3)°, γ = 83.881(4)° for Sn(NH4)2P4O13. The structure is refined in the isotropic approximation using the pseudo-Voigt function: R p = 0.077, R Bragg = 0.045, R F = 0.057 for Ti(NH4)2P4O13; R p = 0.082, R Bragg = 0.044, R F = 0.046 for Sn(NH4)2P4O13. The hydrogen atoms of the ammonium cations are placed in the calculated positions. A comparative analysis of the structures of the compounds of the MIV(NH4)2P4O13 (MIV = Si, Ge, Ti, Sn) series has been carried out.  相似文献   

20.
The coordination polymers [AgPF6(Me4Pyz)2] (I) and [AgPF6(2,3-Et2Pyz)2] (II) were synthesized, and their structures were determined. Crystals of I are monoclinic, space group C2/c, a = 10.213(2) Å, b = 16.267(3) Å, c = 12.663(3) Å, β = 92.90(3)°, V = 2102.1(7) Å3, ρcalcd = 1.660 g/cm3, Z = 4. The structure of I is built of polymeric zigzag [Ag(C8H12N2)] + chains and octahedral [PF6] anions. The coordination polyhedron of the Ag+ ion is a flat triangle. Crystals of II are tetragonal, space group P \(\bar 4\)2(1)/c,a = b = 10.641(1) Å, c = 18.942(1) Å, V = 2144.6(2) Å3, ρcalcd = 1.627 g/cm3, Z = 4. In the structure of II, 2D cationic layers of fused square rings exist; the rings consist of four Ag+ cations linked by four bridging ligands of diethylpyrazine Et2Pyz. The coordination polyhedron of the Ag+ ion is an irregular four-vertex polyhedron.  相似文献   

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