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1.
By single crystal X-ray analysis, the atomic structure of the crystals of bis-phenanthrolinium hexachlorotellurate(IV) dihydrate (C12H9N2)2 TeBr6·2H2O (a = 7.4846(5) Å, b = 13.792(1) Å, c = 14.532(1) Å, β = 99.857(2)°, space group P21/c, Z = 2, d x = 2.259 g/cm3) is determined. The crystal structure is formed from separate anions [TeBr6]2?, cations of phenanthrolinium (C12H9N2)+, and water molecules. The electronic and geometrical aspects determining the spectral-luminescent and thermochromic properties of the complex are discussed.  相似文献   

2.
The crystal structure of (C2H5)4N)2TeCl6 was determined by X-ray diffraction (a = 14.130(2) Å, b = 14.547(2)Å, c = 13.296(2)Å, β= 90.356(3)°; space group C2/c, Z = 4, ρ(calcd) = 1.387 g/cm3). The crystal structure is composed of the [TeCl6]2? anions and tetraethylammonium cations ((C2H5)4N)+. The electronic and geometric aspects that determine the spectral luminescence and thermochromic properties of the complex are discussed.  相似文献   

3.
The synthesis, vibrational spectra, and X-ray diffraction analysis results for 2-(diphenylphosphinylmethoxy) aniline, 2-[(C6H5)2P(O)OCH2]C6H4NH2(I), are described. The crystals are monoclinic: a = 18.4515(17) Å, b = 10.5421(12) Å, c = 17.897(2) Å, β = 104.479(8)°, V = 3370.7(6) Å3, Z = 8, space group P21/c, R = 0.0546 for 1770 reflections with I > 2σ(I). The unit cell contains two crystallographically independent molecules Ia and Ib joined by an N-H …O hydrogen bond between a hydrogen atom of the amino group of aniline in molecule Ia (Ib) and the phosphoryl oxygen atom of molecule Ib (Ia) (O…H 2.18 and 2.19 Å, N…O, 2.979(5) and 3.000(5) Å; NHO angle, 154° and 157°).  相似文献   

4.
Slow evaporation of solutions of Sc and Eu nitrates with macrocyclic cavitand cucurbit[6]uril gives crystals of isostructural complexes [Sc(NO3)(H2O)4(C36H36N24O12)](NO3)2 ? 8.5H2O (space group Pna21, a = 32.0065(18) Å, b = 14.7904(8) Å, c = 11.5774(6) Å, V = 5480.6(5) Å3, Z = 4) and [Eu(NO3)(H2O)4(C36H36N24O12)](NO3)2 ? 6.75H2O (space group Pna21, a = 31.9525(17) Å, b = 14.7203(8) Å, c = 11.8592(6) Å, V = 5578.0(5) Å3, Z = 4). The metal to ligand ratio in these complexes is 1 : 1; the complexes are obtained at 0.025–0.1 mol/l concentrations of the metals in solutions. With higher lanthanide concentrations (0.7–1 mol/l), the 2 : 1 complex with cucurbit[6]uril is formed of the composition [{ Gd(NO3)(H2O)5}2(C36H36N24O12)](NO3)4 ? 6.5H2O (space group \(P\bar 1\), a = 13.3972(6) Å, b = 14.4994(5) Å, c = 18.3290(8) Å, α = 73.5610(10)°, β = 87.2590(10)°, γ = 87.5540(10)°, V = 3409.4(2) Å3, Z = 2) and isotypical complex [{Gd(NO3)(H2O)5}2{(C5H5N) ? (C36H36N24O12)}](NO3)4 ? 8H2O with a pyridine molecule inside the cucurbit[6]uril cavity (space group P21/n, a = 14.8263(6) Å, b = 13.3688(7) Å, c = 18.5970(9) Å, β = 107.5860(10)°, V = 3513.8(3) Å3, Z = 2). According to X-ray diffraction data, the metal atoms of the title complexes coordinate the O atoms in portals of cucurbit[6]uril molecules.  相似文献   

5.
Crystal structures are determined by X-ray crystallography for tetrafluoroantimonates(III) of single and double protonated 3-amino-1,2,4-triazolium cations of the composition (C2H5N4)SbF4 (I) (monoclinic: a = 4.7723(6) Å, b = 19.643(2) Å, c = 7.6974(9) Å, β = 97.239(2)°, Z = 4, Cc space group) and (C2H6N4)(SbF4)2 (II) (monoclinic: a = 4.7617(3) Å, b = 15.512(1) Å c = 7.4365(5)Å β = 107.706(1)°, Z = 2, P21/n space group). The structure of I is built from complex [SbF4]? anions and single charged (C2H5N4)+ cations; the structure of II is built from the same anion and double charged 3-amino-1,2,4-triazolium cation: (C2H6N4)2+. In the structure, weak interactions Sb…F join the anions in polymeric layers [SbF4] n n? that are assembled in a 3D framework by N-H…F hydrogen bonds. The formation of the double protonated 3-amino-1,2,4-triazolium cation (C2H6N4)2+, found in the crystal structure of II, is observed for the first time.  相似文献   

6.
N,N-Diethylanilinium dicitratoborate [C6H5NH(C2H5)2][(C6H6O7)2B] (I) has been synthesized for the first time. Single crystals has been synthesized in an aqueous solution to study the crystal structure of complex I by single-crystal X-ray diffraction. Crystals are triclinic, space group Р1 a = 9.6183(2) Å, b = 10.3153(3) Å, c = 13.7364(4) Å, α = 69.0304(12)°, β = 77.0394(13)°, γ = 89.5518(10)°, V = 1236.25(6) Å3, Z = 2, ρcalcd = 1.454 g/cm3. Structural units in a crystal of complex I are large complex dicitratoborate anions with a spirane structure and N,N-diethylanilinium cations. The crystal packing is a three-dimensional framework implemented via a system of hydrogen bonds like О–Н…О, О–Н…О, ОI, and N–Н…О.  相似文献   

7.
A crystal-chemical study of dimethylgold(III) complexes with 8-hydroxyquinoline (CH3)2Au(OR) and 8-mercaptoquinoline (CH3)2Au(SR) (R = C9H6N) was performed. Crystal data for (CH3)2Au(OR): a = 8.7133(17) Å, b = 27.875(6) Å, c = 8.6688(17) Å, β = 102.76(3)°, Z = 8, ρ(calc) = 2.401 g/cm3, space group P21/c, R = 0.0909; for (CH3)2Au(SR): a = 3.5401(7) Å, b = 15.689(3) Å, c = 19.910(4) Å, β = 99.81(3)°, Z = 4, ρ(calc) = 2.361 g/cm3, space group P21/c, R = 0.0712. Both structures are molecular and involve neutral (CH3)2Au(L) molecules, L = C9H6NO or C9H6NS. In the structures, the molecules are arranged in stacks joined by van der Waals interactions. The average Au…Au intrastack distances are 3.57 Å and 4.34 Å for (CH3)2Au(OR) and 3.5 Å for (CH3)2Au(SR).  相似文献   

8.
Double ionic complexes [M(C5H5NCOO)3(H2O)2][Cr(NCS)6] · nH2O, where M = Eu (I), n = 1.15; Dy (II), Er (III), n = 1.5; M = Yb (IV), n = 2, have been synthesized by the reaction between M(NO3)3, M = Eu, Dy, Er, Yb, K3[Cr(NCS)6], and nicotinic acid (C5H5NCOO) in an aqueous solution and studied by chemical analysis, IR spectroscopy, and X-ray diffraction. Crystals of complexes IIV are monoclinic, space group P21/n, Z = 4; a = 9.5358(2) Å, b = 25.4871(5) Å, c = 15.4303(4) Å, β = 105.513(1)°, V = 3613.6(1) Å3, ρcalcd = 1.799 g/cm3 for I, a = 9.5901(5) Å, b = 25.8599(15) Å, c = 15.6316(9) Å, β = 106.829(2)°, V = 3710.6(4) Å3, ρcalcd = 1.782 g/cm3 for II, a = 9.5640(3) Å, b = 25.8936(11) Å, c = 15.6498(7) Å, β = 106.895(2)°, V = 3708.3(3) Å3, ρcalcd = 1.791 g/cm3 for III, and a = 9.5049(2) Å, b = 25.6378(4) Å, c = 15.5120(3) Å, β = 106.934(1)°, V = 3616.1(1) Å3, ρcalcd = 1.864 g/cm3 for IV.  相似文献   

9.
A new copper(II) complex of 1,10-phenanthroline (C12H8N2) and the meta-aminobenzoate ion (m-amb; C7H6NO 2 ? ), having the formula Cu(C12H8N2)(C7H6NO2)Cl?0.5H2O, is prepared and characterized by elemental analysis, IR spectroscopy, and single crystal X-ray diffraction. The structure is built up from monomeric units in which the coordination environment around the metal ion is a square plane arising from a bidentate 1,10-phenanthroline molecule, a monodentate m-amb anion, and a chloride ion. A very long (Cu–N = 2.856(5) Å) bond to the nitrogen atom of an adjacent m-amb ion generates [101] polymeric chains in the crystal. The crystal structure is consolidated by N–H???O and O–H???O hydrogen bonds and C–H???O, C–H???Cl, and aromatic π–π stacking interactions. Crystal data: C19H15ClCuN3O2.5, M r = 424.33, monoclinic, P21/n (No. 14), a = 9.8200(5) Å, b = 10.9291(7) Å, c = 16.3803(9) Å, β = 105.293(3)°, V = 1695.74(17) Å3, Z = 4, R(F) = 0.043, wR(F 2) = 0.122.  相似文献   

10.
Crystal structure of (C6H5NH3)3[SbCl5]Cl·H2O is determined by X-ray analysis (a = 9.4155(13) Å, b = 11.4344(16) Å, c = 13.1584(18) Å, α = 113.483(2)°, β = 90.383(2)°, γ = 97.323(2)°, space group P \(\bar 1\), Z = 2, ρcalc = 1.642 g/cm3). The crystal structure is based on [SbCl5]2? anions, anilinium cations (C6H5NH3)+, isolated Cl? anions, and water molecules. Structural features responsible for spectral and luminescent properties of the complex are discussed.  相似文献   

11.
Two dinuclear complexes [Zn(μ-L)(NO3)(H2O)]2 (1) and [Cu2(μ-L)2(HL)2](NO3)2(C12H8Br2)0.5·H2O (2), (HL = 3-(2-pyridyl)pyrazole, C12H8Br2 = 4,4′-dibromobiphenyl) are synthesized under hydrothermal conditions and characterized by elemental analysis and X-ray single crystal diffraction. Crystal data for 1: triclinic, \(P\bar 1\), a = 8.8478(7) Å, b = 15.0550(11) Å, c = 16.4310(12) Å, α = 107.588(4)°, β = 112.498(3)°, γ = 115.595(3)°, V = 2099.8(9) Å3, Z = 2; for 2: triclinic, \(P\bar 1\), a = 7.2870(15) Å, b = 8.6840(17) Å, c = 9.3290(19) Å, α = 107.588(4)°, β = 112.498(3)°, γ = 115.595(3)°, V = 528.77(18) Å3, Z = 1. Complex 1 and 2 are both dinuclear structures which are further packed into a 1D supramolecular chain and a 3D supramolecular framework via weak C–H…O hydrogen bond interactions respectively.  相似文献   

12.
In the work, isomeric complexes of platinum(II) with the (ptac)–1 pivaloyltrifluoroacetonate ion (Pt((CH3)3–CO–CH–CO–CF3)2) are studied. The synthesis and chromatographic separation of Pt(ptac)2 isomers are described, TGA data for the separated isomers are given, and the crystal structures of the solid phases are studied. The cis-Pt(ptac)2 complex crystallizes in the space group P-1, a = 10.7091(4) Å, b = 12.7787(6) Å, c = 16.0154(8) Å, α = 92.389(2)°, β = 90.868(2)°, γ = 112.1260(10)°, V = 2027.39(16) Å3, Z = 4, d calc = 1.918 g/cm3. The trans-Pt(ptac)2 complex crystallizes in the space group C2/m, a = 13.3235(5) Å, b = 8.5515(3) Å, c = 9.6694(3) Å, β = 118.5880(10)°, V = 967.38(6) Å3, Z = 2, d calc = 2.010 g/cm3. The structures of the complexes are molecular, the Pt atom has a square coordination of four oxygen atoms of two ligands; for cis-Pt(ptac)2, the Pt–Oav distance is 1.968 Å, for trans-Pt(ptac)2 it is 1.980 Å.  相似文献   

13.
Arsenic 4-methoxy-8-mercaptoquinolinate As[C9H5(4-OCH3)NS]3 (I) was synthesized and studied by X-ray diffraction. Crystals are trigonal: space group R3, a = b = 13.9867(4) Å, c = 12.4991(5) Å, γ = 120°, V = 2117.58(12) Å3, ρ = 1.519 g/cm3, Z = 3. An arsenic atom in the crystal structure occupies a special position on axis 3. The structural unit of the crystal (neutral complex I) has symmetry C3. 4-Methoxy-8-mercaptoquinoline acts as a bidentate (N,S-) ligand. The coordination polyhedron of the arsenic atom is a symmetric octahedron (3S + 3N) or, with allowance for the lone electron pair, ψ-one-capped octahedron (3S + 3N + E). Bond lengths are as follows: As-S, 2.3179(7)Å; As…N 2.688(3) Å. The geometries of coordination polyhedra of arsenic atoms are compared in the crystal structures of As(C9H6NS)3, As[C9H5(2-CH3)NS]3, and As[C9H5(4-CH3)NS]3.  相似文献   

14.
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   

15.
The syntheses and crystal structures of two one-dimensional coordination polymers, [Mn(C5HO2F6)2(C16H20N2)] n (1) and [Mn(C5HO2F6)2(C20H20N2)] n (2), are described, where C5HO2F6 ? is the hexafluoro acetylacetonate anion, C16H20N2 is 1,6-bis(4-pyridyl)-hexane, and C20H20N2 is 1,4-bis[2-(3-pyridyl)ethyl]-benzene. In both phases, the metal ion lies on a crystallographic twofold axis and is coordinated by two chelating C5HO2F6 ? anions and two bridging bipyridyl ligands to generate a cis-MnN2O4 octahedron. The bridging ligands, which are completed by crystallographic inversion symmetry in both compounds, connect the metal nodes into zigzag [20 1 ] chains in 1 and contorted [001] chains in 2. Intrachain C–H???O interactions occur in 1 but not in 2, which may be correlated with the relative orientations of the ligands. Crystal data: 1, C26H22F12MnN2O4, M r = 709.40, monoclinic, C2/c (No. 15), a = 9.3475(2) Å, b = 16.6547(3) Å, c = 18.3649(4) Å, β = 91.1135(8)°, V = 2858.50(10) Å3, Z = 4, R(F) = 0.030, w R(F 2) = 0.075. 2, C30H22F12MnN2O4, M r = 757.44, monoclinic, C2/c (No. 15), a = 19.9198(2) Å, b = 10.6459(2) Å, c = 16.8185(3) Å, β = 119.8344(8)°, V = 3093.91(9) Å3, Z = 4, R(F) = 0.032, w R(F 2) = 0.078.  相似文献   

16.
A complex [Zn(C8H7O3)2(H2O)2] (C8H8O3 is vanillin) has been synthesized and characterized by IR, elemental analysis, and X-ray diffraction single-crystal analysis. The crystals are monoclinic, space group C2/c, a = 22.236(8) Å, b = 10.594(2) Å, c = 7.8190(16) Å, α = 89.90(3)°, β = 106.87(4)°, γ = 89.99(3)°, V = 1762.6(8) Å3, Z = 4, F(000) = 832, S = 1.079, ρ c = 1.521g cm?3, R = 0.0221, R w = 0.0604, μ = 1.433 mm?1. The Zn2+ ion is six-coordinated with a distorted octahedron geometry. The complex forms a three-dimensional network through intermolecular hydrogen bonds. The thermal decomposition kinetics of the complex for the second stage was studied under non-isothermal conditions by the TG and DTG methods. The kinetic equation can be expressed as dα/dt = Ae?E/RT 2(1 ? α)[1 ? ln(1 ? α)]1/2. The kinetic parameters (E, A), activation entropy ΔS , and activation free-energy ΔG were also gained.  相似文献   

17.
X-ray structural analysis has been performed for two complex compounds: Cu(en)2(o-HB)2H2O (I) (a = 16.873(4) Å, b = 8.713(2) Å, c = 14.803(3) Å, β = 91.15(2)°, V = 2175.8(8) Å3, C2/c, Z = 4, R(F) = 0.0263, 1516 reflections with I > 3σ (I)) and [Cu(en)2(OH2)2]2+(o-AB?)2 (II) (a = 7.488(5) Å, b = 22.122(8) Å, c = 7.856(5) Å, β = 118.77(2)°, V = 1140.7(11) Å3, P21/n, Z = 2, R(F) = 0.0432, 1684 reflections with I > 3σ(I)) synthesized under identical conditions (en is ethylenediamine, o-HB is o-hydroxybenzoate, and o-AB is o-aminobenzoate). Although the compounds were assumed to have similar structures and the Cu-Lig bond lengths and the cis and trans angles are acceptable for an octahedral structure, the geometric parameters of o-HB suggest that the copper atom has a plane square environment.  相似文献   

18.
A new mixed-ligand one-dimensional copper(II) coordination polymer [Cu(en)(sal)Cl] n where en = ethylenediamine(C2H8N2) and Hsal = 2-hydroxybenzoic acid (salicylic acid; C7H6O3) is synthesized and characterized by FTIR spectroscopy and single crystal X-ray diffraction. The structure contains Cu2+ ions in two different distorted octahedral coordination environments: an axially extended CuN4Cl2 moiety arising from a pair of bidentate en ligands and a CuO4Cl2 moiety arising from a pair of asymmetrically coordinated sal anions. The chloride ions bridge the copper ions into a zigzag chain propagating in [001]. The structure is consolidated by N–H???O and N–H???Cl hydrogen bonds which generate a layered network. Crystal data: C9H13ClCuN2O3, M r = 296.20, monoclinic, P21/c, a = 13.9179(10) Å, b = 10.4900(8) Å, c = 8.5181(6) Å, β = 105.518(4)°, V = 1198.30(15) Å3, Z = 4, R(F) = 0.026, w R(F 2) = 0.068.  相似文献   

19.
Compounds with compositions [Rh(H2O)6]2(SO4)3·4H2O (I), (H3O)[Rh(H2O)6](SO4)2 (II), [Rh(H2O)5OH](SO4)·0.5H2O (III), and [Rh(H2O)6]2(SO4)·(H2SO4) x ·5H2O (IV) have been studied. The crystal structures of II, III, and IV were determined. All compounds crystallized in the monoclinic crystal system. Crystal data for II: a = 7.279(2) Å, b = 10.512(7) Å, c = 15.806(3) Å, β = 96.71(3)°, space group P21/n, Z = 2, d calc = 2.334 g/cm3; III: a = 20.433(4) Å, b = 7.820(2) c = 11.215(2) Å, β = 114.14(1)°, space group C2/c, Z = 8, d calc = 2.559 g/cm3; IV: a = 6.2250(4 Å), b = 27.0270(12) Å, c = 7.2674(5) Å, β = 97.04(3)°, space group P21/c, Z = 4, d calc = 2.143 g/cm3. The compounds were studied by IR spectroscopy and powder X-ray diffraction. All of the isolated crystalline phases are sparingly soluble in ethanol and well soluble in water.  相似文献   

20.
The crystal structure of an antimony(III) fluoride complex of the composition (C5H12NO2)SbF4·H2O (I) involving a cation of α-amino isovaleric acid (DL-valine, Val) is determined. Crystals are monoclinic: a = 12.2024(2) Å, b = 6.1636(1) Å, c = 15.5167(3) Å, Z = 4, space group P21/c. The structure is formed of DL-valinium (C5H12NO2)+ cations, complex [SbF4]nn? anions having a polymeric chain structure, and crystallization water molecules. The [SbF4]nn? complex anions consist of trigonal SbF4E bipyramids joined together by asymmetric bridging Sb–F(3)···Sb bonds. The structural units are organized into a threedimensional framework via N–H···F, N–H···O, and O–H···F hydrogen bonds.  相似文献   

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