Crystal structure of a new basic nitrate of neodymium(III), [Nd6O(OH)8(H2O)14(NO3)6](NO3)2 · 2H2O

A new basic Nd³⁺ nitrate, [Nd₆O(OH)₈(H₂O)₁₄(NO₃)₆](NO₃)₂ · 2H₂O (I), is isolated in the crystal form and studied. Compound I differs from the basic Ln nitrates containing [Ln ₆O(OH)₈] clusters in that it involves a larger number of water molecules. The incorporation of additional water molecules is accompanied by changes in the coordination environment of one of the three crystallographically independent Nd³⁺ cations. Two cations have coordination polyhedra in the form of a monocapped tetragonal antiprism with a coordination number of 9, and the third cation has a polyhedron in the form of a bicapped tetragonal antiprism with a coordination number of 10. Original Russian Text ? I.A. Charushnikova, C. Den Auwer, 2007, published in Kristallografiya, 2007, Vol. 52, No. 2, pp. 248–251.     

Growth and shape control of orthorhombic Fe5(PO4)4(OH)3·2H2O single crystalline dendrites

Orthorhombic Fe₅(PO₄)₄(OH)₃·2H₂O single crystalline dendritic nanostructures have been synthesized by a facile and reproducible hydrothermal method without the aid of any surfactants. The influences of synthetic parameters, such as reaction time, temperature, the amount of H₂O₂ solution, pH values, and types of iron precursors, on the crystal structures and morphologies of the resulting products have been investigated. The formation process of Fe₅(PO₄)₄(OH)₃·2H₂O dendritic nanostructures is time dependent: amorphous FePO₄·nH₂O nanoparticles are formed firstly, and then Fe₅(PO₄)₄(OH)₃·2H₂O dendrites are assembled via a crystallization-orientation attachment process, accompanying a color change from yellow to green. The shapes and sizes of Fe₅(PO₄)₄(OH)₃·2H₂O products can be controlled by adjusting the amount of H₂O₂ solution, pH values, and types of iron precursors in the reaction system.     

Electrosynthesis and characterization of [Cu(Taab)(H2O)2](L)2 non-crystalline thin films

Molecular-material thin films of diaqua tetrabenzo (b,f,j,n) {1,5,9,13} tetraazacyclohexadecine copper (II) bisanthraflavates and base organic molecules L have been electrodeposited on Corning 7059 glass slices, quartz substrates with tin oxide film and (100) single-crystalline silicon (c-Si) wafers. The surface morphology and structure of the deposited films were studied by atomic force microscopy (AFM), energy-dispersive spectrophotometry (EDS), ultraviolet-visible (UV-Vis) and Fourier-transform infrared (FT-IR) spectroscopies. The IR-spectra show that compounds obtained by chemical synthesis have the same absorption bands as the amorphous thin films obtained by electrosynthesis. The conductivities and the electrical-conduction mechanisms in the thin films were also investigated. Cubic nonlinear optical (NLO) characterizations of the film samples were performed with the Z-Scan technique, with some samples exhibiting remarkably high nonlinear activity.     

Syntheses, Characterizations and Crystal Structures of Two Copper Coordination Polymers Both Having Cu2Cl2 Bridging Subunit [CuI(bipy)1/2Cl]n(1) and {[(CuII)4(phen)4(SSA)2Cl2](H2O)2(DMF)2}n(2)

Abstract  

Two copper coordination polymers [Cu^I(bipy)_1/2Cl] _n (1) and {[(Cu^II)₄(phen)₄(SSA)₂Cl₂] (H₂O)₂(DMF)₂} _n (2)(bipy = 4,4′-bipyridine, phen = 1,10-phenanthroline, H₃SSA = 5-sulfosalicylic acid, DMF = N,N-dimethylformamide) have been prepared and characterized by X-ray diffraction, elemental analysis, IR spectrum and 2 was also studied by cyclic voltammetric method. X-ray analysis indicates that both of them have Cu₂Cl₂ bridging subunit. Complex 1 is a two dimensional network structure. While 2 shows a one dimensional zigzag chain. Electrochemistry studies reveal that complex 2 undergo a quasi reversible one-electron metal-centered redox process at E _1/2 = +0.062 V.     

Crystal structure of PbUO2(CH3COO)4(H2O)3

Single crystals of PbUO₂(CH₃COO)₄(H₂O)₃ have been investigated by X-ray diffraction (R = 0.029 for 3175 reflections). The structure of this compound is formed by [Pb(CH₃COO)(H₂O)₃]⁺ chains, which are oriented along the [100] axis and limited by one-core complexes [UO2(CH₃COO)₃]⁻. The coordination numbers of the Pb(II) and U(VI) atoms are 8, and the coordination polyhedron of uranium is a hexagonal bipyramid whose vertices contain oxygen atoms of three bidentate cyclic acetate groups and the uranyl group. Taking into account the different crystallographic roles of acetate ions, the crystal-chemical formula of [PbUO₂(CH₃COO)₄(H₂O)₃] chains can be written as AA′B ²¹ B ¹¹(B ⁰¹)₂ M ₃¹, where A = Pb; A′ = UO₂²⁺; M ¹ = H₂O; and B ²¹, B ¹¹, and B ⁰¹ are CH₃COO⁻ groups.     

The Structure and Fluorescence Property of a 3D Supramolecular Network [Cd2(2-mBIM)2Cl2(C4H4O4)(H2O)2(H2O)]n

Abstract  

A cadmium(II) coordination polymer [Cd₂(2-mBIM)₂Cl₂(C₄H₄O₄)(H₂O)₂(H₂O)] _n (1) (wherein 2-mBIM = bis(2-methylimidazo-1-yl) methane, C₄H₄O₄ = succinate anion) has been synthesized and characterized by X-ray diffraction. Complex 1 crystallizes in the monoclinic space group C2/c with a = 23.5265(15) ?, b = 7.3558(5) ?, c = 17.4771(11) ?, β = 90.3560(10)°, V = 3024.5(3) ?³, Z = 4. Each Cd(II) atom is octahedrally coordinated and connected with two adjacent Cd(II) atoms by two individual 2-mBIM ligands in a trans-configuration to form one-dimensional (1D) helical structure. Such 1D helical chain structures were connected to each other via the succinate anion ligands and result in the formation of a two-dimensional (2D) framework. Meanwhile, an overall three-dimensional (3D) supramolecular network was formed via the weak hydrogen bond interactions between metal-coordination and free water molecules.     

Synthesis and crystal structure of (NH4)3[UO2(CH3COO)3]2[UO2(CH3COO)(NCS)2(H2O)]

Single crystals of the compound (NH₄)₃[UO₂(CH₃COO)₃]₂[UO₂(CH₃COO)(NCS)₂(H₂O)] (I) are synthesized, and their structure is investigated using X-ray diffraction. Compound I crystallizes in the monoclinic system with the unit cell parameters a = 18.3414(6) ?, b = 16.3858(7) ?, c = 12.4183(5) ?, β = 92.992(1)°, space group C2/c, Z = 4, V = 3727.1(3) ?³, and R = 0.0253. The uranium-containing structural units of crystals I are mononuclear complexes of two types with an island structure, i.e., the [UO₂(CH₃COO)₃]⁻ anionic complexes belonging to the crystal-chemical group (AB ₃⁰¹ = UO₂²⁺, B ⁰¹ = CH₃COO⁻) of the uranyl complexes and the [UO₂(CH₃COO)(NCS)₂(H₂O)]⁻ anionic complexes belonging to the crystal-chemical group AB ⁰¹M₃¹ (A = UO₂²⁺, B ⁰¹ = CH₃COO⁻, M ¹ = NCS⁻ or H₂O).     

Synthesis and X-ray diffraction study of complex neptunium(VI) potassium chromate K2[(NpO2)2(CrO4)3(H2O)] · 3H2O

The crystal structure of the K₂[(NpO₂)₂(CrO₄)₃(H₂O)] · 3H₂O compound was established. The structure consists of anionic layers [(NpO₂)₂(CrO₄)₃(H₂O)] _n ²ⁿ , between which K+ ions and crystallization water molecules are located. The coordination polyhedra of Np atoms are distorted pentagonal bipyramids. All chromate ions are bound in a tridentate-bridging fashion. __________ Translated from Kristallografiya, Vol. 49, No. 4, 2004, pp. 676–680. Original Russian Text Copyright ? 2004 by Grigor’ev, Fedoseev, Budantseva, Bessonov, Krupa.     

Synthesis, Crystal Structure and Properties of the Binuclear Complex [Sm2(C10H9N2O4)2(C10H8N2O4)2(H2O)4]

Abstract  A novel binuclear Smarium (III) complex with N-(2-propionic acid)-salicyloyl hydrazone (C₁₀H₁₀N₂O₄, H₃L) was prepared and characterized. The crystal structure of [Sm₂(H₂L)₂(HL)₂(H₂O)₄] (1) was determined by X-ray single crystal diffractometry. 1 crystallizes in the monoclinic systerm, space group P2(1)/c, with a = 0.10229(2), c = 31.549(7), b = 0.70599(15) nm, and Z = 4. In the structure, Sm(III) is nine-coordinated by carboxyl O and acyl O atoms and imido N atoms of two ligands (H₂L and HL forms) and O atoms from two water molecules. H₂L and HL act as tridentate ligands which form two stable five-numbered chelating rings sharing one edge in the keto form for each ligand, and the carboxyl groups of two ligands were coordinated via bidentated bridging form. The coordination polyhedron around Sm (III) was described as a monocapped square antiprism. The inter- and intramolecular hydrogen bonds resulted in a three-dimensional network and provided extra stability for the structure. The complex was researched the interaction with calf thymus DNA by electronic absorption titration and emission titration. The results show that the complex is bound to calf thymus DNA mainly by intercalation .The complex also shows good fluorescence property. Index Abstract  The title compound, [Sm₂(H₂L)₂(HL)₂(H₂O)₄] was synthesized by the treatment of N-(2-propionic acid)-salicyloyl hydrazone (C₁₀H₁₀N₂O₄, H₃L) and Sm(NO₃) · 4H₂O and its crystal structure determined. Single crystal X-ray diffraction analysis reveals that Sm (III) is nine-coordinated by carboxyl O and acyl O atoms and imido N atoms of two ligands (H₂L and HL forms) and O atoms from two water molecules. The carboxyl groups of two ligands were coordinated via bidentated bridging form. The coordination polyhedron around Sm (III) was described as a monocapped square antiprism. The inter- and intramolecular hydrogen bonds resulted in a three-dimensional network and provided extra stability for the structure.      

Synthesis and crystal structure of rare earth selenates Nd(HSeO4)3, Sm(HSeO4)3, and Nd2(SeO4)3 · 5H2O

Single crystals of rare earth (RE) selenates of the compositions Nd(HSeO₄)₃, Sm(HSeO₄)₃, and Nd₂(SeO₄)₃ · 5H₂O are synthesized and studied by X-ray diffraction analysis at T = 297 and 180 K. It is established that Nd and Sm hydrogen selenates are isostructural to one another and to the corresponding hydrogen sulfates. Neodymium selenate pentahydrate is not isostructural to the analogous RE sulfates, although their structural motifs are similar. __________ Translated from Kristallografiya, Vol. 49, No. 5, 2004, pp. 835–840. Original Russian Text Copyright ? 2004 by Zakharov, Troyanov, Kemnitz.     

Synthesis, characterization and crystal structure of [Ni(DACH)2](H2O)2(CH3COO)2 (DACH = 1,4-diazacycloheptane): a three-dimensional (3-D) hydrogen-bonded network embodying 1-D water chains

The mononuclear complex [Ni(DACH)₂](H₂O)₂(CH₃COO)₂ (DACH = 1,4-diazacyclo-heptane) has been synthesized and characterized by IR, UV-Vis, elemental analysis and single crystal X-ray diffraction. The complex crystallizes in monoclinic system, P2₁/n space group with a=7.500(3) ?, b=8.788(3) ?, c=16.429(6) ?, β=93.395(5)°, D _c =1.269 g cm⁻³, μ=0.930 mm⁻¹, V=1080.9(6) ?³, Z=2. The central Ni^II atom is in a square-planar coordination geometry formed by four N atoms of two DACH chelated ligands. The notable feature of the title compound resides in the formation of a three-dimensional network through hydrogen bonds between the [Ni(DACH)₂]²⁺ cations, the CH₃COO⁻ counter anions and the guest water molecules trapped in the crystal lattice.     

Synthesis and Crystal Structure of Copper II and Silver I Complex with 1,4-diazabicyclo[2.2.2]octane[Cu(CBC)2(Dabco)(H2O)] n (1) and [Ag2(HBC)2(Dabco)] n (2)

Two 1D polymeric complex, [Cu(CBC)₂(Dabco)(H₂O)] _n (1) and [Ag₂(HBC)₂(Dabco)] _n (2) have been synthesized and characterized by X-ray single crystal analysis, where CBCH is p-chlorobenzoic acid, HBCH 2 is 2-hydroxybenzoic acid and Dabco is 1,4-diazabicyclo[2.2.2]octane. Complex 1 has been obtained in high yield by hydrothermal synthesis from CuO and CBCH and Dabco, and complex 2 has been obtain by evaporation of the solvent from silver salicylate and Dabco, 1 crystallizes in the orthorhombic space group Pmn2 ₁ with a = 24.3310(5) ?, b = 6.9050(6) ?, c = 5.9980(5) ?, Z = 2, V = 1007.70(4) ?³ and Dx = 1.657 g cm⁻³, 2 crystallizes in the monoclinic space group P2 ₁ /m with a = 10.292(3) ?, b = 6.913(2) ?, c = 14.417(4) ?, β = 95.660(5), Z = 2, V = 1020.8(5) ?³ and Dx = 1.959 g cm⁻³. The final R value is 0.0302 for 1323 measured reflections for 1 and the final R value is 0.0684 for 1545 measured reflections for 2. The atomic arrangement is built by infinite one-dimensional polymeric chain in both complexes. These chains are cross-linked by hydrogen bonds involving the coordinated water molecules to form a two-dimensional framework in complex 1.     

Structures of mixed-ligand Manganese(II) compounds [Mn(Heida)(Phen)]2 · 7H2O and [Mn2(Edta)(Phen)] · 4H2O

The crystal structures of [Mn(Heida)(Phen)]₂ · 7H₂O (I) and [Mn₂(Edta)(Phen)] · 4H2O (II) are studied by X-ray diffraction [R ₁ = 0.0375 (0.0283) and wR ₂ = 0.0954 (0.0662) for 5449 (3176) observed reflections in I (II), respectively]. Structure I contains mononuclear mixed-ligand complexes [Mn(Heida)(Phen)] and [Mn(Heida)(Phen)(H₂O)]. In structure II, the [Mn(Edta)]²⁻ anionic complexes and the [Mn(Phen)(H₂O)₂]²⁺ cationic complexes are linked by the bridging carboxyl groups into the tetramers with C ₂ symmetry. In both compounds, two independent Mn atoms have different coordination numbers (6 and 7). __________ Translated from Kristallografiya, Vol. 47, No. 2, 2002, pp. 280–285. Original Russian Text Copyright ? 2002 by Polyakova, Sergienko, Poznyak.     

Crystal structure refinement of bifluorides MHF2 (M = Na, NH4, Rb). Crystal structures of Rb5F4(HF2) · 2H2O and RbF · H2O

The crystal structures of alkali metal and ammonium bifluorides MHF₂ (M = Na, NH₄, or Rb) are refined using single-crystal X-ray diffraction. In all the crystals of acid fluorides studied, HF ₂ ^t- anions have a linear structure with F⋯F distances ranging from 2.277 to 2.281 Å. The crystal structures of the Rb₅F₄(HF₂) · 2H₂O and RbF · H₂O compounds are determined. It is established that, in these structures, the O-H⋯F hydrogen bonds whose lengths are equal to 2.55–2.57 and 2.63 Å participate in the formation of trinuclear bent anions and zigzag anionic chains, respectively. __________ Translated from Kristallografiya, Vol. 50, No. 5, 2005, pp. 834–839. Original Russian Text Copyright ? 2005 by Troyanov.     

Palladium (II) compounds with diaminocarboxylic acids: Crystal structures of [Pd(H2Cdta)] · H2O, [Pd(H3Edtp)Cl] · 2H2O, and (H6Edtp)[PdCl4] · 4H2O

The crystal structures of three Pd(II) compounds with diamine tetracarboxylates in different protonation states are determined, namely, [Pd(H₂ Cdta)] · H₂O (I), [Pd(H₃ EdtpCl] · 2H₂O (II), and (H₆ Edtp)[PdCl₄] · 4H₂O (III) (R ₁ = 0.0230, 0.0313, and 0.0277 for 3040, 3377, and 3809 reflections with I > 2σ(I) for I–III, respectively). Crystals I and II are built of neutral complexes [Pd(H₂ Cdta)] and [Pd(H₃ Edtp)Cl], respectively, and crystallization water molecules. Crystal III consists of [PdCl₄]²⁻ anionic complexes, H₆ Edtp ²⁺ cations, and water molecules. In I, one of the protonated acetate groups of the H₂ Cdta ²⁻ ligand forms a very weak additional Pd-O bond [2.968(2) Å] over the 2N + 2O coordination square. In II and III, the protonated propionate groups of the H₃ Edtp ⁻ ligand and the H₆ Edtp ²⁺ cation are not involved in Pd coordination and the coordination squares consist of the 2N + O + Cl and 4Cl atoms, respectively. __________ Translated from Kristallografiya, Vol. 48, No. 2, 2003, pp. 278–282. Original Russian Text Copyright ? 2003 by Polyakova, Poznyak, Sergienko.     

A new dabco templated metal sulfate, (C6H14N2)[Mn (H2O)6](SO4)2. Chemical preparation, hydrogen-bonded structure and thermal decomposition

The crystal structure of manganese sulfate templated by 1,4-diaza-bicyclo[2.2.2]octane (abbreviated dabco), (C₆H₁₄N₂)[Mn(H₂O)₆](SO₄)₂, was investigated using single crystal X-ray diffraction data. It crystallises in the monoclinic system (space group P2₁/c) with the following unit-cell parameters: a = 12.1392(2) ?, b = 12.3117(2) ?, c = 12.2765(2) ?, β = 104.607(1)°, V = 1775.47(5) ?³ and Z = 4. The structure has been solved using direct methods and refined by least-squares analysis [R ₁ = 0.0381, wR ₂ = 0.1082]. The crystal structure of the title compound is built from isolated [Mn(H₂O)₆]²⁺ octahedral cations, 1,4-diaza-bicyclo[2.2.2]octandiium cations (C₆H₁₄N₂)²⁺ and sulfate anions (SO₄)²⁻ connected by a three-dimensional hydrogen-bond network. The thermal decomposition of the precursor, studied by thermogravimetry and temperature-dependent X-ray powder diffraction, proceeds through four stages giving rise to the mixture of Mn₂O₃and Mn₃O₄. Supplementary Material CCDC 620298 contains the supplementary crystallographic data for this paper. These data can be obtained free of charge from The Cambridge Crystallographic Data Centre via www.ccdc.cam.ac.uk/data_request/cif.     

Hydrothermal Synthesis, Structural Characterization and Luminescent Property of a New 1-D Chain-like [Er(NC6H4O2)3(H2O)2]n

Abstract  

Erbium (III) coordination compound with the formula [Er(IN)₃(H₂O)₂]_n 1 (HIN = isonicotinic acid) was synthesized by mixing Er₂O₃ with isonicotinic acid under hydrothermal condition. The structure of the title compound was determined by single crystal X-ray diffraction analysis, which reveals that the 1-D chain-like structure is formed by the erbium polyhedra through the carboxyl groups of IN. It crystallizes in the monoclinic system, possesses space group C2/c, with lattice parameters: a = 20.229(10) ?, b = 11.594(6) ?, c = 9.871(5) ?, α = γ=90°, β = 115.509(6)°, V = 2089.3(18) ?³, and D _calc = 1.811 mg/cm³ for Z = 4, F(000) = 1108, GOF = 1.109, R1 = 0.0675. Compound 1 has been characterized by IR absorption spectroscopy, ultraviolet excitation and emission spectrum.     

Growth of single crystals of NaH2PO4 (NaDP), NaH2PO4 · H2O (NaDP · H2O), and NaH2PO4 · 2H2O (NaDP · 2H2O) sodium dihydrogenphosphate based on the analysis of the Na2O-P2O5-H2O phase diagram

The crystallization conditions for the NaH₂PO₄, NaH₂PO₄ · H₂O, and NaH₂PO₄ · 2H₂O solid phases have been established from the analysis of the phase diagram of solubility of the ternary Na₂O-P₂O₅-H₂O system in the temperature range from 0 to 100°C. Based on these data, the methods for growing sodium dihydrogenphosphate single crystals of the above compositions are developed. The initial components for preparing mother solutions were H₃PO₄ and NaOH solutions taken in certain weight ratios. For the first time, NaDP, NaDP · H₂O, and NaDP · 2H₂O single crystals were grown on a seed by the method of temperature decrease. The habits of the NaDP and NaDP · H₂O single crystals are determined. __________ Translated from Kristallografiya, Vol. 47, No. 5, 2002, pp. 937–944. Original Russian Text Copyright ? 2002 by Soboleva, Voloshin.     

Crystallization behavior of (GeS2)0.1(Sb2S3)0.9 glass

The crystal growth kinetics of antimony trisulfide in (GeS₂)_0.1(Sb₂S₃)_0.9 glass has been studied by microscopy and DSC. The linear crystal growth kinetics has been confirmed in the temperature range 492 ? T ? 515 K (E_G = 405 ± 7 kJ mol⁻¹). The applicability of standard growth models has been assessed. From the crystal growth rate corrected for viscosity plotted as a function of undercooling it has been found that the most probable mechanism is interface controlled 2D nucleated growth. The non-isothermal DSC data, corresponding to the bulk sample, can be described by the Johnson-Mehl-Avrami equation.