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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.
A new Mo2O3(dpm)4 compound (I) is synthesized by the interaction of Mo(CO)6 with 2,2,6,6-tetramethylheptanedione-3,5 (dpm). The structure of complex I determined by the XRD method is as follows: triclinic crystal system, space group P–1, a = 10.1780(7) Å, b = 10.1817(6) Å, c = 13.3255(9) Å, α = 110.562(2)°, β = 102.233(2)°, γ = 93.9041(19)°, V = 1248.17(14) Å3. The compound is characterized by IR spectroscopy, mass-spectrometry and thermogravimetric analysis (TGA).  相似文献   

3.
Macrocyclic and supermolecular complexes [Cu2(NiL)2Cl4] (I) and [Cd2(CuL)2Cl4] (II) (H2L = 2,3-dioxo-5,6,14,15-dibenzo-1,4,8,12-tetraazacyclo-pentadeca-7,13-diene) have been synthesized and structurally determined by X-ray diffraction and IR spectrum. Complex I crystallizes in the monoclinic system with P21/n group, a = 10.9019(15), b = 14.3589(19), c = 12.4748(17) 0A, β = 108.645(2)°, Z = 4. Complex II crystallizes in the monoclinic system with P21/n group, a = 10.9784(16), b = 14.580(2), c = 12.8904(18) Å, β = 109.339(2)°, Z = 4.  相似文献   

4.
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   

5.
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   

6.
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   

7.
Single crystals of (NH4)(CN3H6)[UO2(SeO3)2] (I) are synthesized and studied by X-ray diffraction analysis. The compound crystallizes in the triclinic crystal system with the unit cell parameters: a = 7.0051(2) Å, b = 9.4234(3) Å, c = 9.5408(3) Å, α = 88.727(1)°, β = 70.565(1)°, γ= 77.034(1)°, space group P 1, Z = 2, R = 0.0224. The main structural units of crystals I are the [UO2(SeO3)2]2? chains of the crystal-chemical group AB2B11 (A = UO 2 2+ , B2= SeO3 2?, B11= SeO3 2?) of the uranyl complexes. The uranium-containing complexes are joined into a three-dimensional framework by the ammonium and guanidinium ions and a system of hydrogen bonds.  相似文献   

8.
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   

9.
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   

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.
Potassium oxosulfatovanadate(V) K3VO2(SO4)2 has been obtained by solid-phase synthesis from K2SO4, K2S2O7, and V2O5 (2: 1: 1), and its formation conditions, crystal structure, and physiochemical properties have been studied. The conversions of K3VO2(SO4)2 in contact with potassium vanadates and other potassium oxosulfatovanadates(V) are considered in terms of phase relations in the K2O-V2O5-SO3 system, which models the active component of vanadium catalysts for sulfur dioxide oxidation into sulfur trioxide. The X-ray diffraction pattern of K3VO2(SO4)2 is indexed in the monoclinic system (space group P21) with unit cell parameters of a = 10.0408(1) Å, b = 7.2312(1) Å, c = 7.3821(1) Å, β = 104.457(1)°, Z = 2, and V = 519.02 Å3. The crystal structure of K3VO2(SO4)2 is built from [VO2(SO4)2]3? complex anions, in which the vanadium atom is in an octahedral oxygen environment formed by two terminal oxygen atoms (V-O(6) = 1.605(7) Å, V-O(10) = 1.619(7) Å and four oxygen atoms of the two chelating sulfate anions. The vibrational spectra of K3VO2(SO4)2 are analyzed using these structural data.  相似文献   

12.
The double complex salt [Pd(NH3)4][AuCl4]2 was synthesized and studied by X-ray diffraction: a = 7.5234(6) Å, b = 7.7909(5) Å, c = 8.0247(6) Å, α = 108.483(2)°, β = 106.497(2)°, γ = 99.972(3)°, V = 409.43(5) Å3, space group P \(\overline 1 \), Z = 1, ρcalod = 3.456 g/cm3, R = 0.0267. The compound was characterized by powder X-ray diffraction, thermal analysis, and IR and Raman spectroscopy. The metal products of thermolysis of the complex were studied by powder X-ray diffraction.  相似文献   

13.
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   

14.
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   

15.
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   

16.
The crystal structure of a new bismuth aluminoborate Bi0.96Al2.37(B4O10)O is studied by single-crystal X-ray diffraction. The Bi0.96Al2.37(B4O10)O single crystals are hexagonal (space group \(P\bar 6\) 2m). The unit cell parameters are as follows: a = b = 4.587(4) Å, c = 2.253(9) Å, α = β = 90°, γ = 120°, V = 168.60 Å3, Z = 1.  相似文献   

17.
A chelate compound Pb[(iso-C4H9)2PS2]2 is synthesized. Using X-ray diffraction data, the crystal structures of two modifications of this compound are determined (X8 APEX diffractometer, MoK α radiation, 14169 F hkl , R = 0.0480 for the low temperature α-form and 6261 F hkl , R = 0.0387 for the β-form studied at ambient temperature). The crystals are triclinic: a = 11.047(2) Å, b = 14.486(3) Å, c = 32.048(6) Å; α = 91.30(3)°, β = 99.73(3)°, γ = 101.61(3)°, V = 4942.9(17) Å3, Z = 8, ρcalc = 1.682 g/cm3 (α-modification) and a = 11.2124(5) Å, b = 14.6989(7) Å, c = 17.1644(6) Å; α = 109.393(1)°, β = 94.989(2)°, γ = 101.649(1)°, V = 2576.83(19) Å3, Z = 4, ρcalc = 1.613 g/cm3 (β-modification), space group \(P\bar 1\) for both polymorphs. The structures are molecular, coordination cores of PbS4 are tetragonal pyramids with Pb atoms in the vertices and S atoms in the base. In both structures intermolecular Pb...S contacts yield supramolecular ensembles comprising by four molecules, where PbS4+2 cores form planar aggregates of edge-sharing octahedra. The ensembles are joined by weak intermolecular S...S interactions resulting in the development of polymeric chains along the a axis.  相似文献   

18.
Coordination polymers [AgCF3CO2(2,3-Et2Pyz)](I)(2,3-Et2Pyz-C8H12N2) and [AgCF3CO2(Bpeta)] (II) (Bpeta is 4′4-bipyridylethane, C12H12N2) are synthesized. Their structures are determined. The crystals of compound I are monoclinic, space group P2(1)/n, a = 7.185(1), b = 14.754(1), c = 12.317(1)Å, β = 97.09(1)°, V = 1295.7(2) Å3, ρcalcd = 1.831 g/cm3, Z = 4. Structure I consists of infinite chains of doubled polymeric chains joined by silver carboxylate dimers [[Ag2(CF3CO2)2(Et2Pyz)2]. The coordination polyhedron of Ag+ is a distorted tetrahedron. The crystals of compound II are orthorhombic, space group Pbca, a = 13.555(3), b = 13.991(3), c = 16.449(3) Å, V = 3119.5(11) Å3, ρcalcd = 1.725 g/cm3, Z = 8. Doubled polymeric chains with the Ag…Ag bond (3.16 Å) are also formed in structure II. Supramolecular layers are formed in the structure due to the weak π-π-stacking interaction between the aromatic groups of chains. The CF3CO 2 ? anion is weakly bound to Ag+ (Ag-Oavg 2.790 Å).  相似文献   

19.
The U(VI) complex with cyanoacetic acid, [UO2(H2O)2(NCCH2COO)2] (I), was synthesized from an aqueous solution, and its X-ray diffraction analysis was carried out. The crystals are orthorhombic: space group Pca2 1, a = 25.9605(7) Å, b = 6.7634(2) Å, c = 6.3398(2) Å, V = 1113.15(6) Å3 at 100 K, and Z = 4. The coordination polyhedron of the uranium atom is a distorted pentagonal bipyramid. The cations UO 2 2+ are bound into infinite zigzag chains by the bridging carboxyl groups of one of the anions of cyanoacetic acid. The carboxyl oxygen atom of the second anion, which is not involved in coordination, and the nitrogen atoms of the cyano groups form hydrogen bonds with the coordination water molecules. The layer structure of the compound is formed through the hydrogen bonds. The absorption spectra in the visible and infrared ranges of the crystalline compound are measured and analyzed.  相似文献   

20.
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 /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   

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