Synthesis and crystal structure of [Co(phen)(H2O)4](SO4)⋅2(H2O)

The title complex, [Co(phen)(H₂O)₄](SO₄)2(H₂O) (phen = 1,10-phenanthroline) was prepared in aqua tert-butylperoxohydrogen solution. X-ray single crystal structure determination reveals that the complex consists of a phenanthrolinatocobalt(II)tetrahydrate dication, two uncoordinated water molecules and a sulfate anion. It crystallizes in the orthorhombic space group Pbca with a = 8.856(1), b = 18.318(3), c =21.918(5) Å, V = 3555.6(11) ų. The coordination geometry at each cobalt(II) atom is a slightly distorted octahedron.     

Interferometric study of the growth kinetics of K2Co(SO4)2 · 6H2O and K2Ni(SO4)2 · 6H2O crystals

Crystallography Reports - The growth kinetics of the (001) and (110) faces of K2Co(SO4)2 · 6H2O and K2Ni(SO4)2 · 6H2O crystals in the kinetic mode has been in situ investigated for the...     

[Co(H2O)6](C18H15O4SO3)2·4H2O的合成和晶体结构

以芒柄花素为先导化合物,合成了水溶性的[Co(H2O)6](C18H15O4SO3)2·4H2O,并采用IR, 1H NMR, TG-DTA, XRD和单晶X射线衍射法对其结构进行了表征.单晶X射线衍射结果表明:[Co(H2O)6]2+、C18H15O4SO 3和H2O之间存在多种氢键,形成晶体结构中的亲水区.异黄酮骨架间反平行排列,面对面和边对面芳香堆积作用同时存在于其中,构成晶体结构中的疏水区.磺酸根是连接亲水区和疏水区的桥梁.氢键、芳香堆积作用以及阴阳离子之间的静电引力共同将标题化合物组装成具有三维网络结构的超分子.     

Crystal structures of acid ethylenediaminetetraacetates [Cd(H2 Edta)(H2O)] · 2H2O and [Mn(H2O)4][Mn(HEdta)(H2O)]2 · 4H2O

The crystal structures of [Cd(H₂ Edta)(H₂O)] · 2H₂O (I) and [Mn(H₂O)₄][Mn(HEdta)(H₂O)]₂ · 4H₂O (II) are studied by X-ray diffraction [R ₁ = 0.0209 (0.0272), wR ₂ = 0.0571 (0.0730) for 2551 (4025) reflections with I > 2σ(I) in I (II), respectively]. Structure I contains mononuclear [Cd(H₂ Edta)(H₂O)] complexes with the C ₂ symmetry, and structure II contains centrosymmetric trinuclear [Mn(H₂O)₄][Mn(HEdta)(H₂O)]₂ complexes. In I and II, the protonated ligands are hexadentate (2N + 4O), and the water molecule increases the coordination number of the metal atom to seven. The acid protons participate in short intermolecular hydrogen bonds, which are symmetric in II and asymmetric in I.     

Synthesis and structure of (NH4)3[UO2(C3H2O4)2(NCS)] · 2H2O

Malonate-thiocyanate complex (NH₄)₃[UO₂(C₃H₂O₄)₂(NCS)] · 2H₂O is synthesized and studied by X-ray diffraction. The compound crystallizes in the monoclinic system: a = 13.9983(4) Å, b = 8.1947(2) Å, c = 16.4678(4) Å, β = 100.846(1)°, space group Cc, Z = 4, and R = 0.0158. The main structural units of the crystal are mononuclear [UO₂(C₃H₂O₄)₂(NCS)]^3? groups belonging to the AB ₂ ⁰¹ M ₁ crystal chemical group of uranyl complexes (A = UO ₂ ²⁺ , B ⁰¹ = C₃H₂O ₄ ^2? , M ¹ = NCS^?). Discrete uranium-containing groups are connected by electrostatic interactions with ammonium ions and by hydrogen bonds. Some specific structural features of crystals containing [UO₂(L)₂(NCS)]^3? complexes, where L is the oxalate or malonate ion, are discussed.     

Growth and properties of mixed K2Ni x Co1−x (SO4)2 · 6H2O crystals

Optically homogeneous mixed K₂Ni _x Co_{(1 ? x)}(SO₄)₂ · 6H₂O crystals are grown from solutions of different compositions by the temperature-reduction technique in static and dynamic regimes. The optical characteristics of the grown crystals are measured: transmittance reaches 80% in the wavelength range of 240–290 nm and no more than 9% in the visible spectral range. The thermal stability of the crystals is studied. It is established that the thermal stability of mixed K₂Ni _x Co_{1 ? x} (SO₄)₂ · 6H₂O crystals is higher than that of K₂Co(SO₄)₂ · 6H₂O crystal. The defects of the mixed crystals grown in static and dynamic regimes are investigated by X-ray topography.     

Crystal structures of mixed ligand complexes containing saccharinate and nicotinamide: [Cu(saccharinato)2 (nicotinamide) (H2O)]⋅(H2O) and [M(nicotinamide)2 (H2O)4]⋅(saccharinate)2 (M = Ni2+, Co2+)

[M(saccharinato)₂(H₂O)₄] (M = Cu²⁺, Ni²⁺, Co²⁺) react with nicotinamide to form mixed ligand complexes, [Cu(saccharinato)₂(nicotinamide)(H₂O)](H₂O) (1) and [M(nicotinamide)₂(H₂O)₄](saccharinate)₂ (2: M = Ni²⁺; 3: M = Co²⁺), and their crystal structures have been determined by X-ray diffraction. In 1, the Cu²⁺ atom in an octahedral configuration is coordinated by two monodentate saccharinato ligands in the trans arrangement through the deprotonated ring nitrogens, by two bidentate nicotinamide ligands, one through the pyridyl ring nitrogen and the other through the amide oxygen, and by a water molecule, thus forming a nicotinamide-bridged one-dimensional extended structure. In the isomorphous complexes 2 and 3, the octahedral metal atom, which rides on a crystallographic center of symmetry, is coordinated by two monodentate nicotinamide ligands through the ring nitrogens and four water molecules to form a discrete [M(nicotinamide)₂(H₂O)₄]^{2 +} structural unit, which captures up and down two saccharinate ions, each through three hydrogen bonds: two hydrogen bonds between two water ligands and the ring N and the carbonyl O atoms and one between the amide N of the nicotinamide ligand and the carbonyl O.     

Synthesis and structure of (H2O·HBF4)2(18-crown-6)

The title compound has been prepared by the addition of fluoroboric acid to 18-crown-6 in toluene. The compound crystallizes in the triclinic space group P¯1 witha=7.341(2),b=8.364(2),c=10.631(3)Å,=71.48(2),=67.91(2), =67.94(2)°, andD _c =1.44 g cm^–3 forZ=1. The final conventionalR value was 0.079 based on 1575 observed reflections. The molecule resides on a center of inversion. The (H₂O·HBF₄) moieties are best viewed as fluoroboric acid monohydrate molecules hydrogen bonded to the crown ether, one above and one below the plane of the crown. The FO(water) hydrogen bond separation is 2.474(5)Å, and the O(crown)O(water) separations are 2.834(5) and 2.841(6) Å. The oxygen atoms of the crown ether are planar to 0.23 Å.     

A comparison of the crystal structures of (dabcoH2)CuCl4 and (dabcoH2)CuCl4⋅H2O

The crystal structures of the anhydrous and monohydrated (dabcoH₂)CuCl₄nH₂O salts (n = 0,1) have been determined and a comparison of their crystal structures has been reported. The anhydrous salt is monoclinic P2₁/c with a = 9.045(2) Å, b = 6.9270(10) Å, c = 18.767(4) Å and = 90.07(3)° with V = 1175.8(4) ų. The hydrated salt is also monoclinic P2₁/c with a = 9.266(2) Å, b = 9.395(2) Å, c = 14.386(3) Å and = 93.32(3)° with V = 1250.3(5) ų. The structures of the two salts are closely related. Both compounds contain isolated distorted (compressed) tetrahedral CuCl₄ ^2– anions, diprotonated dabco cations, and in the case of the hydrated salt, lattice H₂O molecules. In the anhydrous salt, each of the two N–H⁺ groups of the dabcoH₂ ²⁺ dications form bifurcated hydrogen bonds to chloride ions on adjacent CuCl₄ ^2– anions along the c axis, thus forming chains running parallel to the c axis. In the hydrated salt, a water molecule is inserted into one of the pair of bifurcated hydrogen bonds, forming instead N–H O–H CuCl₄ ^2– linkages. The chains thus formed are cross-linked by O–H Cl hydrogen bonds between the chains. Because of this additional hydrogen bonding, the CuCl₄ ^2– anions in the hydrated salt are distorted further from tetrahedral geometry.     

Effect of growth conditions on the functional properties of K2Co(SO4)2·6H2O crystals

K₂Co(SO₄)₂ · 6H₂O single crystals of optical quality have been grown and the effect of solution pH on their solubility and transmission spectra has been investigated. A kinetic growth curve is obtained for the (110) face and the onset temperature of dehydration is established for single-crystal samples. The structural quality of single crystals grown at different supersaturations is analyzed.     

Metal-hydroxycarboxylate interactions: syntheses and structures of K2[VO2(C6H6O7)]2·4H2O and (NH4)2[VO2(C6H6O7)]2·2H2O

Potassium and ammonium dimeric (citrato)dioxovanadium(V) hydrate K₂[VO₂(H₂cit)]₂·4H₂O1 and (NH₄)₂[VO₂(H₂cit)]₂·2H₂O2 (H₄cit=citric acid) have been prepared and characterized by X-ray structure analyses. Vanadate1 crystallizes in the monoclinic space groupP2₁/n (No. 14) with unit cell parameters:a=9.304(2),b=11.756(2),c=11.911(2)Å, =111.72(3)°, andD _c=1.911 g/cm³,Z=2; Vanadate2 also crystallizes in the monoclinic space groupP2₁/n with unit cell parameters:a=9.719(2),b=11.111(3),c=11.294(2)Å, =109.03(2)°, andD _c=1.781 g/cm³,Z=2. Each dimer contains a centro-symmetric planar four-member V₂O₂ ring with two exocyclic citrate entities coordinated by the oxygen atoms of the hydroxy-and -carboxylate ligands, while the other two -carboxylate groups remain uncomplexed. Principal dimensions of the V–O bonds are 1.986(4)_av (hydroxy) and 1.980(3)Å(-carboxyl) for vanadate1, 1.988(2)_av (hydroxy) and 1.974(3)Å(-carboxyl) for vanadate2.     

Synthesis and crystal structure of [Ni(H2O)6](C19H17O9S)2·2H2O

A water soluble flavonoid sulfate, [Ni(H₂O)₆](C₁₉H₁₇O₉S)₂·2H₂O was synthesized and its structure was determined by single-crystal X-ray diffraction analysis. The crystal of it belongs to triclinic crystal system, space group P–1. The results show that the title compound consists of [Ni(H₂O)₆]²⁺, C₁₉H₁₇O₆SO₃ ⁻ and H₂O. Ni(II) is located on the symmetry center and octahedrally coordinated by six water molecules. A variety of hydrogen bonds among [Ni(H₂O)₆]²⁺, C₁₉H₁₇O₆SO₃ ⁻ and the lattice water molecules build a hydrophilic region. Aromatic π–π stacking interactions assemble isoflavone skeletons into a column and the columns form a hydrophobic region of the title compound. The sulfo-groups bridge the hydrophilic regions and the hydrophobic regions as well as the inorganic components and organic components. Hydrogen bonds, stacking interactions and the electrostatic interactions between cation [Ni(H₂O)₆]²⁺ and anion sulfonate C₁₉H₁₇O₆SO₃ ⁻ lead the moieties to a three-dimensional structure.     

Synthesis and crystal structure of Schiff base transition metal complex [Co(PMBP-smdtc)2]⋅2H2O

A cobalt(II) complex, [Co(PMBP-smdtc)₂]2H₂O, in which PMBP-smdtc is the l-phenyl-3-methyl-4-benzoyl-5-pyrazolone Schiff base of S-methyldithiocarbazate, has been synthesized and characterized by IR spectrum and single crystal X-ray diffraction. The crystal is monoclinic: space group C2/c, with a = 12.455(2) Å, b = 16.024(2) Å, c = 20.513(3) Å, = 101.18(1)°, V = 4016.3(10) ų, and Z = 4. The cobalt ion is octahedrally coordinated by two tridentate Schiff base ligands with ONS donor atoms. The molecules are bridged together by two water molecules through H-bond along b axis and one-dimensional indented chain structure is formed.     

Growth of faces of K2Co x Ni1 – x(SO4)2 · 6H2O mixed crystals

Data on the morphology and normal growth rate of the (110) and (001) faces, velocities of step motion, and slopes of dislocation hillocks on the (001) face of K₂Co _x Ni₁– _x (SO₄)₂ · 6H₂O crystals at different supersaturations of solutions with a Co/Ni ratio equal to 1: 1 or 1: 2 have been obtained using a Michelson interferometer. The morphology of the (110) faces is found to be the same for solutions of both compositions. Powerful dislocation sources with large Burgers vectors dominate on the (001) face. The morphology of the (001) surface is rougher than that of (110), especially in a 1: 2 solution at high supersaturation. The (110) faces grow more slowly as compared with (001). The kinetic coefficients of steps on the (001) face are identical in the 1: 1 and 1: 2 solutions. The influence of the kinetic and morphological characteristics of (001) faces on the single-crystal quality is analyzed.

     

Complexation between molybdenum(VI) and oxalate: Crystal and molecular structure of [(−)Co(en)3][MoO3(C2O4)OH2]I·2 H2O

The crystal structure of the product of the reaction between [(–)Co(en)₃]I₃ and a mixture of Na₂MoO₄ and NaHC₂O₄ in aqueous solution is reported: [(–)Co(en)₃][MoO₃(C₂O₄)OH₂]I·2H₂O, space groupP2₁2₁2₁,a=8.131(2),b=14.590(4),c=17.509(4) Å;Z=4. FinalR=0.048,R _w=0.050,w=( ² F)^–1 for 1899 reflections. The configuration of the Mo(VI) oxalate complex differs notably from that proposed previously on the basis of chemical analysis and equilibrium studies.     

Synthesis, crystal structure, and thermal property of a novel supramolecular assembly: (NH4)2(C8H10N4O2)4 [H4V10O28]·2H2O, constructed from decavanadate and caffeine

A novel 3D supramolecular assembly constructed from decavanadate and caffeine building blocks, (NH₄)₂(C₈H₁₀N₄O₂)₄[H₄V₁₀O₂₈]·2H₂O (1), has been synthesized in aqueous solution and characterized by elemental analysis, IR, ¹H NMR, ⁵¹V NMR, TG-DTA, and single crystal X-Ray diffraction. The compound 1 crystallizes in monoclinic system, space groupP2 ₁/n, a = 15.801(1) Å, b = 12.914(1) Å, c = 15.913(2) Å, = 113.55°,V = 2976.4 (5)ų, Z = 2, R = 0.0498 with 6818 reflections. Water molecules, ammonium ions, and caffeine act as cement linking the polyanions into 1D chain along the c-axis by hydrogen bonding. In compound 1, extensive hydrogen-bond contacts and strong – interactions lead to an ordered 3D supramolecular framework. TG-DTA curves indicate that the weight loss of the complex can be divided into three stages.     

Crystal structure and characterization of [Co(saccharinate)2(L1)(H2O)2] n solvate: A new microporous coordination polymer generated from 1,4-bis(3-pyridyl)-2,3-diaza-1,3-butadiene (L1) and [Co(saccharinate)2·4H2O]·2H2O

A new microporous coordination polymer, [Co(saccharinate)₂(L1)(H₂O)₂] _n solvate, has been prepared from the reaction of the N,N bidentate ligand 1,4-bis(3-pyridyl)-2,3-diaza-1,3-butadiene (L1) with [Co(saccharinate)₂·4H₂O]·2H₂O in a methylene chloride/ethanol solvent mixture. The compound crystallizes in the triclinic system, space group P-1, with lattice parameters a = 7.6893(5) Å, b = 11.0169(7) Å, c = 11.2369(7) Å, = 66.2610(10)°, = 74.4160(10)°, = 74.6740(10)°. The structure consists of one-dimensional chains composed of octahedrally coordinated Co(II) centers linked by L1. The packing of these chains, along with intrachain and interchain hydrogen bonds, generates a 3-D framework with infinite channels that are occupied by disordered guest molecules. The compound was further characterized by IR spectroscopy and DTA/TGA.     

Growth and Study of Properties of Mixed Crystals (NH4)2NixCo1 –x(SO4)2 · 6H2O

Crystallography Reports - Mixed crystals (NH4)2NixCo1 –x(SO4)2 · 6H2O have been grown from aqueous solutions of different compositions by reducing the solution temperature in two growth...     

Synthesis and structural characterization of [Co(tren)(Tsal)]ClO4·H2O and [Ni(pn)(py)2(NCS)2]

Complexes [Co(tren)(Tsal)]ClO₄·H₂O 1 and [Ni(pn)(py)₂(NCS)₂] 2, (tren = tris(2-aminoethyl)amine, Tsal = thiosalicylate ion, pn = 1, 2-diamino propane and py = pyridine) have been synthesized and structurally characterized. Both complexes crystallize in the monoclinic space group C2/c with a = 21.3340(6), b = 11.7754(2), c = 14.8076(5) Å, = 100.3831(10)°, Z = 8 (1), and a = 7.2573(8), b = 17.8810(11), c = 15.2681(12) Å, = 101.170(2)°, Z = 4 (2). The metal atoms in both cases have distorted octahedral geometry. In 1, the tren ligand is quadridentate and Tsal is bidentate chelate. In 2, the pn ligand forms a bidentate chelate with the NCS ligands in trans positions. Complex 1 is diamagnetic whereas 2 shows paramagnetism with a magnetic moment of 3.10 B. M.     

Synthesis and crystal structure of hexaaquamagnesium hydrogen phosphododecatungstate tetrahydrate [Mg(H2O)6][HPW12O40]·4H2O

Crystals suitable for X-ray structure analysis were obtained after the slow evaporation of the reaction mixture containing equimolar quantities of magnesium chloride and dodecatungstophosphoric acid aqueous solution insuring pH of the solution between 1.0 and 1.2. This simple synthetic route yielded stability of Keggin anion and high quality [Mg(H₂O)₆][HPW₁₂O₄₀]·4H₂O single crystals. The obtained compound belongs to the group of heteropoly compounds and its structure is composed of Keggin [PW₁₂O₄₀]^3– anions, [Mg(H₂O)₆]²⁺ cations and lattice water molecules. Zigzag arrangement of Keggin anions along c-axis creates irregular channels occupied by [Mg(H₂O)₆]²⁺ cations and lattice H₂O molecules. The calculation of the total potential solvent volume indicated the presence of 4.1 lattice H₂O lattice molecules per formula unit, which is in agreement with the here presented structural model. The position of one lattice water molecule is well defined, while each of three other molecules is statistically distributed over two locations. Hydrogen bonds involve all coordinated and lattice H₂O molecules, as well as some oxygen atoms from the Keggin anion. (© 2007 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim)