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1.
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   

2.
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   

3.
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   

4.
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   

5.
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   

6.
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   

7.
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   

8.
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   

9.
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   

10.
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   

11.
Phase formation in the BaB2O4-NaBO2-MBO3 (M = Sc, La, Y) system was studied using solid-phase synthesis, visual polythermal analysis, and spontaneous crystallization. This system was shown to be suitable for growing LaBO3. A new compound, ScBaNa(BO3)2, was obtained (trigonal crystal system; space group R \(\bar 3\) unit cell parameters: a = 5.239(1) Å, c = 34.591(1) Å, and V = 822.38(4) Å3).  相似文献   

12.
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   

13.
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   

14.
Ytterbium alkali-metal chromites YbMCr2O5 (M = Li, Na, K, Cs) were synthesized by a ceramic procedure from the corresponding oxides and carbonates. Their crystal systems and unit cell parameters were determined by the homology method: for YbLiCr2O5, a = 10.34 Å, b = 10.62 Å, c = 15.05 Å, Z = 16, V o = 1653.74 Å3, ρX-ray = 5.85 g/cm3, ρpycn = 5.81 ± 0.03 g/cm3; for YbNaCr2O5, a = 10.30 Å, b = 10.56 Å, c = 16.46 Å, Z = 16, V o = 1790.32 Å3, ρX-ray = 5.64 g/cm3, ρpycn = 5.59 ± 0.07 g/cm3; for YbKCr2O5, a = 10.33 Å, b = 10.63 Å, c = 19.93 Å, Z = 16, V o = 2188.47 Å3, ρX-ray = 5.95 g/cm3, ρpycn = 5.91 ± 0.03 g/cm3; and for YbCsCr2O5, a = 10.34 Å, b = 10.63 Å, c = 18.43 Å, Z = 16, V o = 2025.72 Å3, ρX-ray = 5.19 g/cm3, ρpycn = 5.16 ± 0.05 g/cm3.  相似文献   

15.
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   

16.
The complex [UO2(SeO4)(C5H12N2O)2(H2O)] (I) was synthesized and studied by thermal analysis, IR spectroscopy, and X-ray crystallography. The crystals are orthorhombic: a = 13.1661(3) Å, b = 16.4420(5) Å, c = 17.4548(6) Å, Pbca, Z = 8, R = 0.0423. The structural units of crystal I are chains with the composition coinciding with that of the compounds of the AB2M 3 1 crystal chemical group of the uranyl complexes (A = UO 2 2+ , B2 = SeO 4 2? , M1 = C5H12N2O and H2O).  相似文献   

17.
Two complexes [Zn(SALIMP)(CH3CO2)]2 (1) and [Cu(SALIMP)Cl] (2) are obtained by the reactions of zinc(II) and copper(II) salts with a tridentate Schiff base ligand 2-[[(2-pyridinylmethyl) imino]methyl]phenol (HSALIMP). Their structure is determined by single crystal X-ray diffraction. Data for complex 1: C30H28N4O6Zn2, CCDC number: 668213, M r = 671.3, monoclinic, C2/c, with a = 34.670(5) Å, b = 15.266(2) Å, c = 23.464(4) Å, β = 114.045(2)°, V = 11341(3) Å3, Z = 16, F(000) = 5504, GOOF(F 2) = 0.894, the final R = 0.0520 and wR = 0.1272 for 10515 observed reflections with I > 2σ(I); complex 2: C13H12N2OClCu, CCDC number: 668211, M r = 311.24, triclinic, P-1, with a = 7.4050(8) Å, b = 10.2369(11) Å, c = 16.2873(17) Å, α = 87.728(2)°, β = 87.818(2)°, γ = 78.279(2)°, V = 1207.4(2) Å3, Z = 4, F(000) = 632, GOOF(F 2) = 1.077, the final R = 0.0326 and wR = 0.0381 for 4209 observed reflections with I > 2σ(I).  相似文献   

18.
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   

19.
New ferrites ErMFe2O5 (M = Li, Na, K) were synthesized from erbium and iron(III) oxides and lithium, sodium, and potassium carbonates by solid-state annealing. According to X-ray powder diffraction, these compounds crystallize in the orthorhombic system with the following unit cell parameters: ErLiFe2O5, a = 10.510 Å, b = 10.776 Å, c = 14.270 Å, V 0 = 1616.16 Å3; Z = 16, V subcell 0 = 101.01 Å3, ρX = 6.01 g/cm3, ρpycn = 5.97 ± 0.05 g/cm3; ErNaFe2O5, a = 10.519 Å, b = 10.785 Å, c = 15.510 Å, V 0 = 1759.56 Å3, Z = 16, V subcell 0 = 109.90 Å3, ρX = 5.77 g/cm3, ρpycn = 5.72 ± 0.08 g/cm3; ErKFe2O5, a = 10.050 Å, b = 11.320 Å, c = 15.480 Å, V 0 = 1937.33 Å3, Z = 16, V subcell 0 = 121.08 Å3, ρX = 5.46 g/cm3, ρpycn = 5.41 ± 0.04 g/cm3.  相似文献   

20.
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   

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