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).     

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.     

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 cubic space group of tungstogallate acid,H<Subscript>5</Subscript>GaW<Subscript>12</Subscript>O<Subscript>40</Subscript>

The space group of tungstogallate acid, H₅GaW₁₂O₄₀, reported by Niu et al. (J. Chem. Crystallogr. 2003, 33, 799) should be I–43m instead of Cm; the monoclinic C-centered cell is transformed to the I-centered cubic cell by (1 0 0; ,– , 1; – , – , –1).     

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.     

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.     

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.     

Crystal Structure and IR Study of (C<Subscript>6</Subscript>H<Subscript>5</Subscript>NH<Subscript>3</Subscript>)[ZnCl(HPO<Subscript>3</Subscript>)]

Abstract  

A new hybrid phosphate, (C₆H₅NH₃)[ZnCl(HPO₃)], has been synthesized and its structure characterized from single-crystal X-ray diffraction. The title compound crystallizes in the orthorhombic space group Pbca (n. 61) with the unit-cell parameters: a = 9.8635(2) ?, b = 9.4516(10) ?, c = 22.2430(4) ?, Z = 8 and V = 2,073.62(6) ?³. The final R factors were R/ωR = 0.0361/0.0924. Its framework might be described as a layered structure with two (010)-parallel cationic and anionic layers. The IR spectrum of this phase shows characteristic bands of phosphite and anilinium groups.     

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.     

Crystal structure of the gold(I) complex [Au(tfp)Cl] with tfp = (C<Subscript>4</Subscript>H<Subscript>3</Subscript>O)<Subscript>3</Subscript>P

The Au(I) complex [Au(tfp)Cl] with tfp = (C₄H₃O)₃P has been prepared and characterised. It crystallises in the monoclinic P2₁/n space group with z = 4, a = 9.837(3), b = 12.684(4), c = 11.103(5)Å, = 91.58(2)° and V = 1384.8(2)ų. The structure of the complex consists of molecules connected in head-to-tail dimers by a metal-halogen contact as generally found in analogus complexes of lighter coinage metals. The typical feature of halogen gold compounds, the Au–Au interaction, seems prevented by the bulk of the tfp ligand.     

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.      

Vibrational modes of hydrogen in (NH<Subscript>4</Subscript>)H<Subscript>5</Subscript>(PO<Subscript>4</Subscript>)<Subscript>2</Subscript> (Neutron scattering and simulation)

The vibrational modes of hydrogen in (NH₄)H₅(PO₄)₂ have been investigated by inelastic incoherent neutron scattering at temperatures above (220 K) and below (160 and 5 K) the phase-transition point T _c = 180 K. Computer simulation of vibrational modes has been performed for the low-temperature phase (NH₄)H₅(PO₄)₂ at 5 K. The calculated generalized incoherent dynamic factor and the partial incoherent dynamic factors for all hydrogens make it possible to identify the observed modes from acid hydrogens and hydrogens of ammonium ions.     

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.     

X-Ray Crystal Structure of <Emphasis Type="Italic">trans</Emphasis>-PdCl<Subscript>2</Subscript>(PPh<Subscript>2</Subscript>C<Subscript>12</Subscript>H<Subscript>7</Subscript>S<Subscript>3</Subscript>)<Subscript>2</Subscript>, a New Morphology

Herein we report the crystal structure of trans-PdCl₂(PPh₂C₁₂H₇S₃)₂, 1, in a different morphology than has previously been reported [Stott et al. (Dalton Trans (4):652–653, 2005]. This structure crystallizes in a P-1 space group with a = 9.4249(19) Å, b = 11.540(2) Å, c = 12.559(3) Å, α = 79.07(3)°, β = 78.04(3)°, γ = 69.44(3)°, Z = 1. The earlier structure possessed a P2₁/n space group. Additionally the terthienyl moieties of 1 demonstrate the anti orientation exclusively while the P2₁/n space group structure has some syn and even syn/anti mixed geometries included.     

Intermolecular interactions involved in the crystal structure of 2-amino-5-methylpyridinium hexabromostannate (IV), (C<Subscript>6</Subscript>H<Subscript>9</Subscript>N<Subscript>2</Subscript>)<Subscript>2</Subscript>[SnBr<Subscript>6</Subscript>]

The salt bis(2-amino-5-methylpyridinium) hexabromostannate(IV) (C₆H₉N₂)₂[SnBr₆] is monoclinic, P2 ₁ /c, with the following cell parameters: a=9.1636(18) ?, b=28.767(7) ?, c=16.956(17) ?, β=101.008(5)°, V=4387.5(17) ?³, Z=8, formula units. X-ray crystallography revealed that the structure can be regarded as a semi-regular three-dimensional array of anions, with pairs of cations forming layers perpendicular to b axis in the cavities between the anions. The cohesion forces that connects molecules in the organic layers are hydrophilic N⋯HCH₂ and HN⋯HN hydrogen bonding as well as hydrophobic π-π stacking and CH₃⋯π interactions. Cations and anions are connected via strong Br⋯H hydrogen bonding. Supplementary material CCDC 276493 contains the supplementary crystallographic data. These data can be obtained free of charge via www.ccdc. cam.ac.uk/data_request/cif, by e-mailing data_ request@ccdc.cam.ac.uk, or by contacting The Cambridge Crystallographic Data Centre, 12 Union Road, Cambridge CB2 1EZ, UK; fax: +44(0)1223-336033.     

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 new radical cation salt (<Emphasis Type="Italic">DOET</Emphasis>)<Subscript>4</Subscript>[Fe(CN)<Subscript>5</Subscript>NO]<Subscript>1.25</Subscript>(C<Subscript>6</Subscript>H<Subscript>5</Subscript>Cl)<Subscript>0.75</Subscript>

A new radical cation salt based on 4,5-(1,4-dioxanediyl-2,3-dithio)-4′,5′-ethylenedithiotetrathiafulvalene (DOET) with the photochromic anion [Fe(CN)₅NO]^2?, namely, (DOET)₄[Fe(CN)₅ NO]_1.25(C₆H₅Cl)_0.75, is synthesized. Single crystals of this salt are studied using X-ray diffraction [a = 10.398(2) Å, b = 11.168(2) Å, c = 18.499(4) Å, α = 103.14(3)°, β = 92.80(3)°, γ = 106.02(3)°, V = 1996.3(7) ų, space group \(P\bar 1\), and Z = 1]. In the structure, radical cation layers alternate with anion layers along the c axis. The centrosymmetric dimers are formed by DOET radical cations in the donor layer with packing of the β type. Like the vast majority of DOET-based salts, the new salt possesses semiconductor properties.     

Synthesis and an X-ray diffraction study of Rb<Subscript>2</Subscript>[(UO<Subscript>2</Subscript>)<Subscript>2</Subscript>(C<Subscript>2</Subscript>O<Subscript>4</Subscript>)<Subscript>3</Subscript>]

The synthesis and X-ray diffraction study of compound Rb₂[(UO₂)₂(C₂O₄)₃], which crystallizes in the monoclinic crystal system, are performed. The unit cell parameters are as follows: a = 7.9996(6) Å, b = 8.8259(8) Å, c = 11.3220(7) Å, β = 105.394(2)°, and V = 770.7(1) ų; space group P2₁/n, Z = 2, and R ₁ = 0.0271. [(UO₂)₂(C₂O₄)₃]^2? layers belonging to the AK _0.5 ⁰² T ¹¹ crystal chemical group of uranyl complexes (A = UO ₂ ²⁺ , K ⁰² = C₂O ₄ ^2? , and T ¹¹ = C₂O ₄ ^2? ) are uranium-containing structural units of the crystals. The layers are connected with outer-sphere rubidium cations by electrostatic interactions.     

Microhardness and fracture toughness of Y<Subscript>2</Subscript>O<Subscript>3</Subscript>-and Y<Subscript>3</Subscript>Al<Subscript>5</Subscript>O<Subscript>12</Subscript>-based nanocrystalline laser ceramics

The microhardness and fracture toughness of laser nanocrystalline ceramics based on the cubic oxides Y₂O₃ and Y₃Al₅O₁₂ are determined experimentally. It is shown by comparative measurements that the fracture toughness and microhardness of Y₂O₃ ceramics exceed the corresponding parameters of Y₂O₃ single crystals by factors of 2.5 and 1.3, respectively. The fine morphology of grains and grain boundaries in fractures is investigated. It is ascertained that changes in the mechanical properties of the nanocrystalline ceramics under study are related to both the sizes and structure of grains and the structure of grain boundaries. It is suggested that twinning processes determine the mechanisms of formation of nanocrystalline ceramics.     

Crystal structure of (Al,V)<Subscript>4</Subscript>(P<Subscript>4</Subscript>O<Subscript>12</Subscript>)<Subscript>3</Subscript>, archetype of double cubic ring tetraphosphate

The crystal structure of the (Al,V)₄(P₄O₁₂)₃ solid solution, obtained in the single-crystal form by hydrothermal synthesis in the Al(OH)₃-VO₂-NaCl-H₃PO₄-H₂O system, has been solved by X-ray diffraction analysis (Xcalibur-S-CCD diffractometer, R = 0.0257): a = 13.7477(2) Å, sp. gr. I \(\bar 4\)3d, Z = 4, and ρ_calcd = 2.736 g/cm³. It is shown that the crystal structure of the parent cubic Al₄(P₄O₁₂)₃ modification can formally be considered an archetype for the formation of double isosymmetric tetraphosphates on its basis.