Synthesis and Crystal Structure of Complex [Nd(2-FC<Subscript>6</Subscript>H<Subscript>4</Subscript>COO)<Subscript>3</Subscript>·(2-FC<Subscript>6</Subscript>H<Subscript>4</Subscript>COOH)·H<Subscript>2</Subscript>O]<Subscript>2</Subscript>

The neodymium complex with 2-fluorobenzoic acid was synthesized and characterized by X-ray diffraction. The complex crystallizes in the triclinic system with space group Pī, lattice parameters: a = 9.2747(10) Å, b = 11.7594(13) Å, c = 13.5158(14) Å, α = 110.220(2)°, β = 93.930(2)°, γ = 90.894(2)°, V = 1378.8(3) Å³, Z = 1, Dcalc = 1.733 Mg/m³. The complex is a binuclear molecule in which four 2-fluorobenzoato groups act as bidentate and tridentate bridges between the two Nd³⁺ ions. Each Nd³⁺ ion is additionally chelated by one 2-fluorobenzoato group and coordinated by one 2-fluorobenzoic acid and one water molecule.     

Na(H<Subscript>2</Subscript>O)[Mn(H<Subscript>2</Subscript>O)<Subscript>2</Subscript>(BP<Subscript>2</Subscript>O<Subscript>8</Subscript>)]: Crystal structure refinement

The crystal structure of synthetic manganese sodium borophosphate hydrate Na(H₂O)[Mn(H₂O)₂(BP₂O₈)] was refined based on X-ray diffraction data. The compound was prepared by soft hydrothermal synthesis in the MnCl₂-Na₃PO₄-B₂O₃-H₂O system. The unit-cell parameters are a= 9.602(1) Å, c= 16.037(3) Å, sp. gr. P6₅22, Z= 6, D _x = 2.57 g/cm³. The water molecules were found to be statistically distributed in the channels of the mixed anionic paraframework consisting of (BO₄) and (PO₄) tetrahedra and [MnO₄(H₂O)₂] octahedra. The hydrogen atoms of the water molecules coordinated to the Mn²⁺ cations were located and their positional and thermal parameters were refined. The crystal-chemical features of borophosphates of the general formula A _x M(H₂O)₂(BP₂O₈)(H₂O) are considered.     

The synthesis and structure of a novel alternating 1-D cobalt coordination polymer [Co(2,5-PDC)<Subscript>2</Subscript>(H<Subscript>2</Subscript>O)<Subscript>2</Subscript>Co(H<Subscript>2</Subscript>O)<Subscript>4</Subscript>]·4H<Subscript>2</Subscript>O

A novel cobalt complex [Co(2,5-PDC)₂(H₂O)₂Co(H₂O)₄]·4H₂O (2,5-PDCH₂ = 2,5-pyridinedicarboxylic acid) was synthesized and its crystal structure has been determined by X-ray diffraction. The crystallographic data are: triclinic P−1, a = 7.112(2) ?, b = 8.939(3) ?, c = 9.719(3) ?, α = 91.153(5)°, β = 101.136(5)°, γ = 108.001(4)°, V = 574.4(3) ?³, Z = 1. The compound [Co(2,5-PDC)₂(H₂O)₂Co(H₂O)₄]·4H₂O exhibits a novel one-dimensional network constructed from the interconnection of Co(2,5-PDC)₂(H₂O)₂ and Co(H₂O)₄, in which two kinds of six-coordinated Co(II) atoms have both octahedral coordination environments. Each 2,5-PDC anion connects two different coordinated cobalt ions alternately in an one-dimensional chain. The zigzag 1D alternating chains are linked by extensive hydrogen bonds to form a three-dimensional (3D) supramolecular structure, in which uncoordinated solvate molecules act as space filling particles. Supplementary data CCDC-264249 contains the supplementary crystallographic data for this paper. Copies of this information may be obtained free of charge from the Director, CCDC, 12 Union Road, Cambridge, CB2 1EZ, UK (fax: t44–1223–336033; e-mail: deposit@ccdc.cam.ac.uk or ) or also available from the author Xiaoqing Wang.     

Domain Structure and Orientational Ordering of NO<Subscript>2</Subscript> Groups in K<Subscript>2</Subscript>Ba(NO<Subscript>2</Subscript>)<Subscript>4</Subscript> Crystals

Polarization-optical studies of the domain structure of K₂Ba(NO₂)₄ crystals and differentialscanning calorimetric measurements have been performed in the vicinity of the high-temperature phase transition. The orientational ordering of NO₂ atomic groups is analyzed and the temperature dependence of the birefringence coefficient is theoretically described.     

Synthesis and Structure of [Fe<Subscript>3</Subscript>O(O<Subscript>2</Subscript>CCH<Subscript>2</Subscript>OMe)<Subscript>6</Subscript>(H<Subscript>2</Subscript>O)<Subscript>3</Subscript>][FeCl<Subscript>4</Subscript>]

Abstract  The structure of [Fe₃O(O₂CCH₂OMe)₆(H₂O)₃][FeCl₄] · 2.5H₂O has been determined. The three iron atoms and the μ₃-oxo are coplanar. Each carboxylic ligand is bidentate and links two iron atoms in the cluster. The clusters are linked by intra-trimer hydrogen bonding to form a zigzag motif that forms sheets via hydrogen bonding involving disordered waters of hydration. The [FeCl₄]⁻ anion is intercalated between the hydrogen-bonded sheets. Crystal data: space group P2₁/n, a = 10.276(2), b = 22.793(5), c = 17.091(3) ?, β = 96.66(3)°, V = 3976(1) ?³, Z = 4, R = 0.0837, wR ₂ = 0.1836. Graphical Abstract  The structure of [Fe₃O(O₂CCH₂OMe)₆(H₂O)₃][FeCl₄] · 2.5H₂O has been determined in which the clusters are linked by intra-trimer hydrogen bonding to form a zigzag motif that forms sheets via hydrogen bonding involving disordered waters of hydration.      

Synthesis and characterization of a lead(II) complex [Pb(phen)(H<Subscript>2</Subscript>O)(NO<Subscript>3</Subscript>)<Subscript>2</Subscript>] (phen = 1,10-phenanthroline)

The monomeric lead(II) complex, [Pb(phen)(H₂O)(NO₃)₂] was prepared by a hydrothermal reaction of Pb(NO₃)₂, nitrilotriacetic acid, NaOH, 1,10-phenanthroline, and H₂O. The structure was determined by X-ray crystallography. It crystallizes in monoclinic P2(1)/n space group with the crystal cell parameters of a = 6.3568(6), b = 20.2345(19), c = 11.2722(9) Å, β = 98.337(4)^°, V = 1434.6(2) ų, and Z = 4. The crystal X-ray analysis shows that the lead atom is six-coordinated by two N atoms of phen ligand, three oxygen atoms of nitrate anions and one water molecule. Owing to the presence of a lone pair of electrons of lead atom, a significant gap occurs in the coordination geometry around Pb ion. A 3D architecture is formed through the strong hydrogen bonding and π–π stacking interactions.     

Synthesis and crystal structure of bis(malonato)tetra (aqua)barium(II)cobalt(II): [BaCo(C<Subscript>3</Subscript>H<Subscript>2</Subscript>O<Subscript>4</Subscript>)<Subscript>2</Subscript>(H<Subscript>2</Subscript>O)<Subscript>4</Subscript>]

The title compound [BaCo(C₃H₂O₄)₂(H₂O)₄] was synthesized and its crystal structure was determined. The compound is orthorhombic, space group Pccn with a = 18.974(3) Å, b = 6.783(2) Å, c = 9.394(4) Å. The structure is polymeric and consists of edge-sharing BaO₈ polyhedra and CoO₆ octahedra linked together by the malonate groups. The geometry around the Ba(II) centres is a slightly distorted square-antiprism with Ba–O distances ranging from 2.789(4) to 2.843(4) Å. Around the Co(II) centres, the coordination forms a distorted octahedron with Co–O bonds between 2.040(3) and 2.238(4) Å.     

Molecular structure of [(C<Subscript>5</Subscript>H<Subscript>5</Subscript>)<Subscript>2</Subscript>(C<Subscript>5</Subscript>H<Subscript>4</Subscript>CH<Subscript>3</Subscript>)(C<Subscript>4</Subscript>H<Subscript>8</Subscript>O)Sm]

The mixed tris-cyclopentadienyl tetrahydrofuranato samarium complex bis-(cyclopentadienyl) methylcyclopentadienyl tetrahydrofuranato samarium (I) was synthesized by reaction of (C₅H₅)₂SmCl with methyl cyclopentadienyl sodium in THF. [(C₅H₅)₂(C₅H₄CH₃)(C₄H₈O)Sm] (I) was characterized by elemental analyses—IR spectra and MS spectra. The structure of [(C₅H₅)₂(C₅H₄CH₃)(C₄H₈O)Sm] (I), which has two slightly different independent molecules per asymmetric unit, has been elucidated through complete X-ray analysis. The crystals are monoclinic, with a = 12.791(3) Å, b = 10.467(2) Å, c = 26.108(5) Å, β = 98.22(2)°, and space group Cc, R = 0.0381 for 2103 observed-reflection with I ≥ 3σ(I).     

Li<Subscript>2</Subscript>HPO<Subscript>3</Subscript>, H<Subscript>2</Subscript>O: Crystal Structure and IR Spectrum

Abstract  

Crystal structure of Li₂HPO₃,H₂O was determined by single-crystal X-Ray diffraction analysis at 173(2) K. It crystallizes in the monoclinic system (P2_1/c) with the parameters: a = 5.0322(9) ?, b = 8.9795(17) ?, c = 17.088(4) ?, β = 92.672(16)° and Z = 8. The structure was refined to R = 0.0237 and ωR = 0.0650 for 1449 reflexions. The framework of Li₂HPO₃, H₂O can be described as layers perpendicular to the crystallographic c axis. The structure contains two types of Li-tetrahedrons. In one kind each O atom belongs to one HPO₃ group, while in the second kind one apex is an O from water. A network of hydrogen bonds interactions insures the connection between the layers.     

Synthesis,Crystal Structure and Luminescence Property of a Chiral Magnesium (II) Mixed-ligand Complex [Mg(H<Subscript>2</Subscript>O)<Subscript>2</Subscript>(phen)(HBDC)<Subscript>2</Subscript>](phen)

Abstract  

A new mixed-ligand complex of [Mg(H₂O)₂(phen)(HBDC)₂](phen) (phen = 1, 10-phenanthroline, H₂BDC = 1,3-benzene dicarboxylic acid) has been synthesized and its crystal structure determined by single-crystal X-ray diffraction. It is noteworthy that this complex was formed from achiral reactants, and found to crystallize in the chiral space group C2. Structure analysis shows that each Mg(II) ion is coordinated by the two nitrogen atoms of phen, one oxygen atom from each of the two 1,3-HBDC molecules and one oxygen atom from each of the two water molecules, leading to a distorted octahedral geometry. The mixed-ligand complexes are assembled into a two-dimensional supramolecular network through the formation of intermolecular hydrogen bonds. The luminescence property and thermal stability behavior of the complex were also investigated. The complex shows a strong blue luminescence emission. Crystal data: a = 24.5856(16), b = 10.1598(6), c = 7.1460(4) ?, β = 105.226(2)o, V = 1722.30(18)?³, Z = 2, R ₁ = 0.0367, wR ₂ = 0.0833 [I>2σ(I)].     

Synthesis and Crystal Structure of [Li(THF)<Subscript>4</Subscript>]Cu<Subscript>2</Subscript>Br<Subscript>4</Subscript>

The mixed-valence compound [Li(THF)₄]Cu₂Br₄ was synthesized in a redox reaction from 1,4-dihydroxynaphthalene, CuBr₂ and LiNtBuSiMe₃ in THF. X-ray quality crystals of [Li(THF)₄]Cu₂Br₄ (monoclinic, P2₁/c) are obtained from the mother liquor at ambient temperature. In the solid state, infinite chains of anionic [Cu₂Br₄]⁻ units are established. These chains are separated by [Li(THF)₄]⁺ cations.     

Synthesis and crystal structure of the [Co<Subscript>2</Subscript>(Nicotinamide)<Subscript>4</Subscript>(C<Subscript>4</Subscript>H<Subscript>9</Subscript>COO)<Subscript>4</Subscript>(H<Subscript>2</Subscript>O)] complex

The [Co₂ L ₄(C₄H₉COO)₄(H₂O)] coordination compound of cobalt(II) valerate with nicotinamide (L) is synthesized and studied by IR spectroscopy. The crystal structure of the synthesized compound is determined. The crystals are triclinic, and the unit cell parameters are as follows: a = 10.2759(10) Å, b = 16.3858(10) Å, c = 16.4262(10) Å, α = 100.538(10)°, β = 101.199(10)°, γ = 90.813 (10)°, Z = 2, and space group P \(\bar 1\). The structural units of the crystal are dimeric molecular complexes in which pairs of cobalt atoms are linked by triple bridges formed by oxygen atoms of two bidentately coordinated valerate anions and a water molecule. The octahedral coordination of each cobalt atom is complemented by the pyridine nitrogen atoms of two nicotinamide ligands and the oxygen atom of the monodentate valerate group. The hydrocarbon chains of the valerate anions are disordered over two or three positions each.     

Synthesis and Crystal Structure of a Cyano-Bridged Bimetallic Nickel(II)–Silver(I) Complex, [Ni(dmen)<Subscript>2</Subscript>{Ag(CN)<Subscript>2</Subscript>}<Subscript>2</Subscript>] · 0.5H<Subscript>2</Subscript>O

A cyano-bridged heteronuclear bimetallic complex [Ni(dmen)₂{Ag(CN)₂}₂] · 0.5H₂O (dmen = N,N′-dimethylethylenediamine) has been prepared and characterized by IR spectroscopy and X-ray Crystallography. The compound crystallizes in the monoclinic space group P2₁/c. The crystal structure of the complex consists of two independent centrosymmetric trinuclear molecules made up of a [Ni(dmen)₂] ⁺² unit linked to two [Ag(CN)₂]⁻ anions in a trans configuration. The trinuclear units are joined by hydrogen bonding to form irregular chains.     

Synthesis and structure of the stoichiometric sodium bis(dihydrotellurato)cuprate(III) Na<Subscript>5</Subscript>[Cu(H<Subscript>2</Subscript>TeO<Subscript>6</Subscript>)<Subscript>2</Subscript>] · 16H<Subscript>2</Subscript>O

Stoichiometric sodium bis(dihydrotellurato)cuprate(III) of the composition Na₅[Cu(H₂TeO₆)₂] · 16H₂O is synthesized, and its crystal structure is studied. The site occupancy of the Na(3) atom at the center of symmetry is refined to 0.493(8). Since this value is close to 0.5, the position is considered to be completely occupied.     

Crystal structure of the binary complex of cobalt and zinc chlorides with carbamide [Co(OCN<Subscript>2</Subscript>H<Subscript>4</Subscript>)<Subscript>5</Subscript>(H<Subscript>2</Subscript>O)][ZnCl<Subscript>4</Subscript>]

Mixed single crystals of [Co(OCN₂H₄)₅(H₂O)][ZnCl₄] were grown by the isothermal evaporation of an aqueous solution. The crystal structure of this complex was established by X-ray diffraction (R = 0.052 based on 7003 reflections). The crystals consist of [Co(OCN₂H₄)₅(H₂O)]²⁺ cations containing Co atoms in an octahedral coordination and [ZnCl₄]²⁻] anions containing Zn atoms in a tetrahedral coordination. The carbamide molecules are involved in both intramolecular and interionic hydrogen bonds. The H₂O molecule forms hydrogen bonds with the anions.     

Structure and some properties of [UO<Subscript>2</Subscript>(C<Subscript>5</Subscript>H<Subscript>12</Subscript>N<Subscript>2</Subscript>O)<Subscript>5</Subscript>](ClO<Subscript>4</Subscript>)<Subscript>2</Subscript>

Compound [UO₂(C₅H₁₂N₂O)₅](ClO₄)₂ is synthesized and characterized by thermogravimetry, IR spectroscopy, and X-ray diffraction. The compound crystallizes in the monoclinic crystal system; a = 15.2985(9) Å, b = 26.9676(15) Å, c = 20.6962(11) Å, β = 100.697(1)°, space group P2₁/c, Z = 8, and R = 0.0445. Discrete [UO₂(C₅H₁₂N₂O)₅]²⁺ groups belonging to the AM ₅ ¹ crystal chemical group of uranyl complexes (A = UO ₂ ²⁺ and M ¹=C₅H₁₂N₂O) are uranium-containing structural units of the crystals.     

Growth of filamentary KDP crystals from solution with the addition of Al(NO<Subscript>3</Subscript>)<Subscript>3</Subscript> · 9H<Subscript>2</Subscript>O

To elucidate the mechanism of nucleation and growth of filamentary crystals on the bipyramid faces of KH₂PO₄ (KDP) crystals from solution with the addition of Al(NO₃)₃ · 9H₂O, the growth rates and transverse dimensions of the crystals were measured at various supersaturations, temperatures, and impurity concentrations. The dependences obtained can be interpreted with due regard for the competition between the intrinsic and impurity particles in the presence of Cabrera-Vermilyea stoppers.     

Crystal and Molecular Structure of Dichloro(ethylenediamine)gold(III) Nitrate: [Au(NH<Subscript>2</Subscript>CH<Subscript>2</Subscript>CH<Subscript>2</Subscript>NH<Subscript>2</Subscript>)Cl<Subscript>2</Subscript>]NO<Subscript>3</Subscript>

Abstract  The gold(III) atom in [Au(NH₂CH₂CH₂NH₂)Cl₂]NO₃ is chelated by the ethylenediamine (en) ligand and the approximately square planar geometry is completed by two chloride atoms. Weak Au···O and Au···Cl contacts are noted above and below the square plane leading to a tetragonally distorted octahedron for the gold(III) center. Extensive charge-assisted hydrogen bonding of the type N–H···O leads to the formation of a 2-D array and layers are consolidated into a 3-D network via C–H···O and C–H···Cl contacts. The compound crystallizes in the orthorhombic space group Pbca with a = 10.3380(11) ?, b = 8.2105(7) ?, c = 19.625(2) ?, and Z = 8. Index Abstract  Square planar complex cations form additional Au···O and Au···Cl interactions to form a tetragonally distorted octahedron for gold. The ionic components are connected into a 2-D array via charge-assisted N–H···O hydrogen bonding interactions.      

Structure of Cs<Subscript>4</Subscript>(HSO<Subscript>4</Subscript>)<Subscript>3</Subscript>(H<Subscript>2</Subscript>PO<Subscript>4</Subscript>) single crystals

Single crystals of Cs₄(HSO₄)₃(H₂PO₄) are synthesized and studied for the first time. The new compound is found in the course of studies of the phase diagram of the CsHSO₄–CsH₂PO₄–H₂O triple system. Data on the atomic crystal structure of single-crystalline and powder specimens, as well as on structural phase transitions, are obtained.     

Synthesis and Structure of Bis(3-dimethylammonium-1-propyne)pentachlorobismuthate(III) (C<Subscript>5</Subscript>H<Subscript>10</Subscript>N)<Subscript>2</Subscript>BiCl<Subscript>5</Subscript>

Abstract  

The synthesis and crystal structure are given for the bis(3-dimethylammonium-1-propyne)pentachlorobismuthate(III) salt. An X-ray investigation has shown that the title compound crystallizes at 298 K in a centrosymmetric monoclinic system, space group C2/c with the following lattice parameters a = 12.6215(4) ?, b = 18.9228(5) ?, c = 8.3134(2) ?, β = 104.100(2)°, V = 1925.70(9) ?³. The structure was solved from 7,716 independent reflections with R ₁ = 0.0457 and wR ₂ = 0.0906, and refined with 85 parameters. The structure consists of disordered 3-dimethylammonium-1-propyne, C₅H₉NH⁺ cations and polynuclear anions in which slightly distorted (BiCl₅)²⁻ anions, sharing an apex are interconnected in chains. These chains are themselves interconnected by means of N–H···Cl originating from the C₅H₉NH⁺ entities, forming a three-dimensional network.