X-ray diffraction study of Rb<Subscript>2</Subscript>[(UO<Subscript>2</Subscript>)<Subscript>2</Subscript>(CrO<Subscript>4</Subscript>)<Subscript>3</Subscript>(H<Subscript>2</Subscript>O)<Subscript>2</Subscript>] · 4H<Subscript>2</Subscript>O

The compound Rb₂[(UO₂)₂(CrO₄)₃(H₂O)₂] · 4H₂O was studied by X-ray diffraction. The crystals are monoclinic, a = 10.695(2) Å, b = 14.684(3) Å, c = 14.125(3) Å, β = 108.396(4)°, sp. gr. P2₁/c, Z = 4, V = 2104.9(7) ų, and R = 0.0491. The main structural units are layers consisting of [(UO₂)₂(CrO₄)₃(H₂O)₂]^2? anions belonging to the crystal-chemical group A ₂ T ₂ ³ B ²M ₂ ¹ (A = UL ₂ ²⁺ , T ³ and B ² are CrO ₄ ^2? , and M ¹ is H₂O) of uranyl complexes. The uranium-containing layered groups are held together by electrostatic interactions with rubidium cations, as well as by hydrogen bonds with the participation of inner- and outer-sphere water molecules.     

Synthesis and structure of [(NH<Subscript>2</Subscript>)<Subscript>2</Subscript>CSSC(NH<Subscript>2</Subscript>)<Subscript>2</Subscript>]<Subscript>2</Subscript>[OsBr<Subscript>6</Subscript>]Br<Subscript>2</Subscript> · 3H<Subscript>2</Subscript>O

The complex [(NH₂)₂CSSC(NH₂)₂]₂[OsBr₆]Br₂ · 3H₂O is synthesized by the reaction of K₂OsBr₆ with thiocarbamide in concentrated HBr and characterized using electronic absorption and IR absorption spectroscopy. Its crystal structure is determined by X-ray diffraction. The crystals are orthorhombic, a = 11.730(2) Å, b = 14.052(3) Å, c = 16.994(3) Å, space group Cmcm, and Z = 4. The [OsBr₆]^2? anionic complex has an octahedral structure. The Os-Br distances fall in the range 2.483–2.490 Å. The α,α′-dithiobisformamidinium cation is a product of the oxidation of thiocarbamide. The S-S and C-S distances are 2.016 and 1.784 Å, respectively. The H₂O molecules, Br^?ions, and NH₂ groups of the cation are linked by hydrogen bonds.     

Crystal growth and properties of Rb<Subscript>2</Subscript>Ni(SO<Subscript>4</Subscript>)<Subscript>2</Subscript> · 6H<Subscript>2</Subscript>O (RNSH)

Large single crystals of rubidium nickel hexahydrate Rb₂Ni(SO₄)₂ · 6H₂O (RNSH) of optical quality were grown for the first time. The atomic structure of RNSH crystals was refined. A comparative analysis of the crystal structures of (M ¹⁺)₂Ni(SO₄)₂ · 6H₂O, where M ¹⁺ is K, Rb, or Cs, was performed. The solubility curve of RNSH in water was measured. The optical and thermogravimetric properties of RNSH were investigated. The internal defect structure of RNSH crystals was studied by X-ray topography.     

Crystal structure and properties of K<Subscript>2</Subscript>[OsO<Subscript>2</Subscript>(C<Subscript>2</Subscript>O<Subscript>4</Subscript>)<Subscript>2</Subscript>] · 2H<Subscript>2</Subscript>O

The synthesis and X-ray diffraction study of the compound K₂[OsO₂(C₂O₄)₂] · 2H₂O are performed. The compound crystallizes in the triclinic crystal system, space group P \(\bar 1\), a = 6.545(1) Å, b = 6.835(2) Å, c = 7.595(2) Å, α = 85.76(2)°, β = 65.33(2)°, γ = 71.14(2)°, and Z = 1. The osmium atom is located at the center of symmetry and has a distorted octahedral coordination formed by oxygen atoms: two oxygen atoms of the osmyl group occupy the apical positions [Os-O, 1.730(2) Å], and four oxygen atoms of the oxalate ions lie in the equatorial plane. The K⁺ cation is surrounded by ten oxygen atoms located at different K-O distances in the range from 2.787(2) to 3.158(2) Å. The assignment of the absorption bands in the IR spectrum of K₂[OsO₂(C₂O₄)₂] · 2H₂O is performed. The electronic absorption spectra of the compound are recorded in different solvents, and the thermal behavior in air is studied.     

Crystal structure of the solid solution NH<Subscript>4</Subscript>Al<Subscript>0.62</Subscript>Cr<Subscript>0.38</Subscript>(SO<Subscript>4</Subscript>)<Subscript>2</Subscript> · 12H<Subscript>2</Subscript>O

The solid solution NH₄Al_0.62Cr_0.38(SO₄)₂ · 12H₂O was studied by X-ray diffraction. The crystal structure was determined in a series of the maximal subgroups Pa3? > R3? > P1? > P1. Reflections forbidden in sp. gr. Pa3? are indicative of symmetry lower than cubic. In the centrosymmetric models under consideration, all sulfate groups are oppositely oriented with respect to each other. In non-centrosymmetric sp. gr. P1, four of the eight sulfate groups have the same orientation, whereas the other four groups are oriented in an opposite direction.     

Crystal structure of CoUO<Subscript>2</Subscript>(SO<Subscript>4</Subscript>)<Subscript>2</Subscript> · 5H<Subscript>2</Subscript>O at 293 K

Single crystals of cobalt uranyl sulfate are grown. The crystal structure is established by X-ray diffraction: the orthorhombic system, sp. gr. Pmc2₁, a = 6.452(2) Å, b = 8.295(2) Å, c = 11.288(3) Å, R₁ = 0.0303, wR₂ = 0.0735 for reflections with I > 2σ(I). The structure of CoUO₂(SO₄)₂ · 5H₂O consists of infinite two-dimensional uncharged [CoUO₂(SO₄)₂H₂O]_2∞ layers, which are linked to each other by hydrogen bonds.     

Crystal structure and properties of [OsO<Subscript>2</Subscript>(NH<Subscript>3</Subscript>)<Subscript>4</Subscript>]SO<Subscript>4</Subscript> · H<Subscript>2</Subscript>O

The structure of a single crystal of tetraammindioxoosmium(VI) sulfate [OsO₂(NH₃)₄]SO₄ · H₂O, which is synthesized by the reaction of K₂[OsO₂(OH)₄] with (NH₄)₂SO₄ in an aqueous solution, is investigated using X-ray diffraction analysis. The compound crystallizes in the monoclinic crystal system, space group P2₁/c, a = 13.102(2) Å, b = 6.158(3) Å, c = 11.866(2) Å, β = 98.13(2)°, and Z = 4. The [OsO₂(NH₃)₄]SO₄ · H₂O compound has an island structure. Two crystallographically independent osmium atoms are situated at the centers of symmetry, and their octahedral coordination includes two oxygen atoms and four nitrogen atoms of the ammonia molecules. In both octahedra, the osmyl group is linear. The Os-O distances in the octahedra are identical within the standard deviations [Os(1)-O, 1.762(2) Å; Os(2)-O, 1.769(2) Å]. The Os-N bond lengths vary from 2.082(3) to 2.101(3) Å. The cationic complexes, SO₄ groups, and water molecules are linked via the system of hydrogen bonds. The assignment of the absorption bands in the IR spectrum of the compound synthesized is performed, and its thermal behavior in air is studied.     

Crystal and molecular structure of phenanthrolinium peroxodisulfate dihydrate (C<Subscript>12</Subscript>H<Subscript>9</Subscript>N<Subscript>2</Subscript>)<Subscript>2</Subscript>S<Subscript>2</Subscript>O<Subscript>8</Subscript> · 2H<Subscript>2</Subscript>O

The crystal structure of (HPhen)₂S₂O₈ · 2H₂O is studied using X-ray diffraction. The crystals are monoclinic, a = 23.716(5) Å, b = 10.220(2) Å, c = 13.103(3) Å, β = 128.03(2)°, V = 2501.6(9) ų, Z = 4, space group C2/c, and R = 0.0745 for 1579 reflections with I > 2σ(I). The crystal is built of S₂O ₈ ^2? centrosymmetric anions, HPhen ⁺ cations, and molecules of crystallization water. Hydrogen bonds link the structural units into chains. Within a chain, stacking interactions are observed between the phenanthroline rings (the interplanar spacing between the rings is 3.8 Å, and the dihedral angle between their planes is 8°). The data of IR spectroscopy confirm the formation of the N(Phen)-H bond.     

Crystal structure of Sr(AsUO<Superscript>6</Superscript>)<Subscript>2</Subscript> · 8H<Subscript>2</Subscript>O

The crystal structure of the compound Sr(AsUO₆)₂ · 8H₂O is determined by X-ray diffraction analysis (monoclinic system, sp. gr. Pc, unit-cell parameters a = 7.154(1) Å, b = 7.101(1) Å, c = 18.901(7) Å, β = 92.67(2)°, Z = 2). The structure is built by (001)-parallel [AsUO₆]^? layers formed by flattened square UO₆ bipyramids and AsO₄ tetrahedra. The neighboring layers are connected via SrO₈ square antiprisms. The cavities of the polyhedral framework thus formed are occupied by H₂O molecules. The displacements of the anion complexes by a half-translation with respect to one another along only one lattice period is a characteristic feature of this polymorphous modification of the uran-mica group.     

Synthesis and X-ray diffraction study of [UO<Subscript>2</Subscript>(NO<Subscript>3</Subscript>)<Subscript>2</Subscript>(H<Subscript>2</Subscript>O)<Subscript>2</Subscript>] · 2C<Subscript>12</Subscript>H<Subscript>18</Subscript>O

The compound [UO₂(NO₃)₂(H₂O)₂] · 2C₁₂H₁₈O was synthesized and studied by IR spectroscopy and X-ray diffraction. The structure consists of the neutral island groups [UO₂(NO₃)₂(H₂O)₂], which belong to the crystal-chemical group AB ⁰¹ ₂ M ¹ ₂ (A = UO₂ ²⁺, B ⁰¹ = NO₃⁻, M ¹ = H₂O) of uranyl complexes, and 1-adamantyl methyl ketone molecules. The characteristic features of the association of the complexes [UO₂(NO₃)₂(H₂O)₂] and 1-adamantyl methyl ketone molecules in the crystal structure via hydrogen bonds are considered with the use of Voronoi-Dirichlet polyhedra.     

Synthesis and Crystal Structure of Ethylenediammonium bis iodate tetra iodic Acid: [C<Subscript>2</Subscript>H<Subscript>10</Subscript>N<Subscript>2</Subscript>] (IO<Subscript>3</Subscript>)<Subscript>2</Subscript>·4HIO<Subscript>3</Subscript>

Abstract  

The synthesis and crystal structure are presented for the ethylenediammonium bis iodate tetra iodic acid. An X-ray investigation has shown that this compound crystallizes in a centrosymmetric monoclinic system, space group P2₁/c with the lattice parameters: a = 7.2536(2) ?, b = 18.5351(5) ?, c = 7.5685(2) ?, β = 107.937(1)°, V = 968.10(3) ?³. The structure was solved from 5281 independent reflections with R ₁ = 0.0229 and wR ₂ = 0.0428, and refined with 156 parameters. The structure is built up of [(CH₂)₂(NH₃)₂]²⁺ cations connected to the one-dimensional [HIO₃]_n chains and to the [H₂I₄O₁₂]²⁻ clusters by a weak N–H···O hydrogen bonds.     

Investigation of the structure and properties of K<Subscript>9</Subscript>H<Subscript>7</Subscript>(SO<Subscript>4</Subscript>)<Subscript>8</Subscript> · H<Subscript>2</Subscript>O single crystals

The features of the conductivity of K₉H₇(SO₄)₈ · H₂O single-crystal samples in the temperature range of superprotonic phase transition have been investigated. The K₉H₇(SO₄)₈ · H₂O crystal structure is determined and refined taking into account hydrogen atoms by X-ray diffraction analysis at a temperature of 295 K: monoclinic symmetry, sp. gr. P2₁/c, Z = 4, a = 7.059(1), b = 19.773(1), c = 23.449(1) Å, β = 95.33(1)°, R ₁/wR ₂ = 2.71/1.71. The structural data obtained suggest that the occurrence of high conductivity in K₉H₇(SO₄)₈ · H₂O crystals with an increase in temperature is related to the diffusion of crystallization water and motion of K ions, as well as to the transformation of the system of hydrogen bonds and protonic motion. The stabilization of the high-temperature superprotonic phase and its supercooling to low temperatures are due to the presence of channels for the motion of K ions and slow backward diffusion of water in the crystal.     

Synthesis and crystal structure of Na<Subscript>3</Subscript>(H<Subscript>3</Subscript>O)[UO<Subscript>2</Subscript>(SeO<Subscript>3</Subscript>)<Subscript>2</Subscript>]<Subscript>2</Subscript>· H<Subscript>2</Subscript>O

Single crystals of the compound Na₃(H₃O)[UO₂(SeO₃)₂]₂ · H₂O (I) have been synthesized, and their structure has been investigated using X-ray diffraction. Compound I crystallizes in the triclinic system with the unit cell parameters a = 9.543(6)Å, b = 9.602(7)Å, c = 11.742(8)Å, α = 66.693(16)°, β = 84.10(2)°, γ = 63.686(14)°, space group P \(\bar 1\), Z = 2, and R = 0.0734. The uranium-containing structural units of the crystals are [UO₂(SeO₃)₂]^2? chains, which belong to the crystal-chemical group AB ² B ¹¹ (A = UO ₂ ²⁺ , B ² = SeO ₃ ^2? , B ¹¹ = SeO ₃ ^2? ) of the uranyl complexes. The structures of the compounds containing the [UO₂(SeO₃)₂]^2? anionic complexes are compared.     

Structural Studies of the Isomorphous MCl<Subscript>2</Subscript>(PMe<Subscript>3</Subscript>)<Subscript>4</Subscript> (M = Mo,W) Complexes

Abstract  

The structure of WCl₂(PMe₃)₄ has been determined in order to allow for a comparison with its molybdenum analogue. The complexes are isomorphous, and exhibit trans-pseudooctahedral coordination, with crystallographically imposed [`4]2m\overline{4}2m (D<sub>2d</sub>) symmetry. A significant distortion occurs involving the PMe<sub>3</sub> ligands, through which one opposing pair tilts upward toward one axial chloride ligand, while the other pair tilts in an opposite manner, by 9.33°. The complex crystallizes in the tetragonal space group I[`4]2mI\overline{4}2m, with a = b = 9.4987(4) ?, c = 12.1058(5) ?, V = 1092.25(8) ?³, D _calc = 1.700 at 150(1) K. For a better comparison, the structure of the molybdenum complex was redetermined, at a low temperature. Its space group is also I[`4]2mI\overline{4}2m with a = b = 9.5193(3) ?, c = 12.1083(5) ?, V = 1097.22 ?³, D _calc = 1.426 at 150(1) K. In accord with the larger cell volume, the molybdenum complex possesses slightly longer M–Cl and M–P bonds.     

Crystal Structure and Characterization of [Ni(RPOEt)<Subscript>2</Subscript>(C<Subscript>2</Subscript>H<Subscript>5</Subscript>OH)<Subscript>2</Subscript>](ClO<Subscript>4</Subscript>)<Subscript>2</Subscript> [RPOEt = bis{(diphenylphosphinyl)methyl}ethyl phosphinate]

Abstract  

The compound [Ni(RPOEt)₂(C₂H₅OH)₂](ClO₄)₂ (1) [RPOEt = bis{(diphenylphosphinyl)methyl}ethyl phosphinate] has been prepared in the form of single crystals and characterized by elemental and thermal analyses, IR spectroscopy and by a single crystal X-ray diffraction study. The complex crystallizes in the triclinic P[`1] P\bar{1} space group with a = 9.8773(5), b = 13.741(1), c = 14.287(1) ?, α = 64.313(9), β = 70.280(5), γ = 89.973(7)o, V = 1620.5(2) ?³, and Z = 1. The nickel(II) atom in 1, situated at the centre of symmetry, is coordinated by four oxygen atoms from two RPOEt ligands and two oxygen atoms from two ethanol molecules in a slightly distorted octahedral environment. The third phosphoryl-oxygen atom from the phosphinate ligand is hydrogen bonded to the oxygen atom of the ethanol molecule coordinated to nickel(II). The complex [Ni(RPOEt)₂(C₂H₅OH)₂]²⁺ cations are linked by the C–H···O hydrogen bonds into one-dimensional chains and by the composite π···π and C–H···π phenyl interactions into a final three-dimensional structure.     

Crystal structure of byelorussite-(Ce) NaMnBa<Subscript>2</Subscript>Ce<Subscript>2</Subscript>(TiO)<Subscript>2</Subscript>[Si<Subscript>4</Subscript>O<Subscript>12</Subscript>]<Subscript>2</Subscript>(F,OH) · H<Subscript>2</Subscript>O

The crystal structure of the mineral byelorussite-(Ce) NaMnBa₂Ce₂Ti₂Si₈O₂₆(F,OH) · H₂O belonging to the joaquinite group was solved and refined to R = 0.033 based on 4813 reflections with I > σ2(I). The parameters of the orthorhombic unit cell are a = 22.301(4) Å, b = 10.514(2) Å, c = 9.669(2) Å, V = 2267.1(8) ų, sp. gr. Ama2, and Z = 4. The structure is composed of three-layer sheets, which consist of dimers of edge-sharing Ti octahedra located between isolated four-membered [Si₄O₂] rings. The sheets are linked to each other by Mn 5-vertex polyhedra to form a heteropolyhedral framework. Large cavities in the framework are occupied by Na 6-vertex polyhedra, Ba 11-vertex polyhedra, and REE 9-vertex polyhedra.     

New crystals of the CsHSO<Subscript>4</Subscript>–CsH<Subscript>2</Subscript>PO<Subscript>4</Subscript>–H<Subscript>2</Subscript>O system

Cs₆H(HSO₄)₃(H₂PO₄)₄ crystals, grown for the first time based on an analysis of the phase diagram of the CsHSO₄–CsH₂PO₄–H₂O ternary system, have been investigated by structural analysis using synchrotron radiation. The atomic structure of the crystals is determined and its specific features are analyzed.     

Synthesis and crystal structure of binuclear molecule Ho<Subscript>2</Subscript>(2-FC<Subscript>6</Subscript>H<Subscript>4</Subscript>COO)<Subscript>6</Subscript>⋅4H<Subscript>2</Subscript>O

The complex Ho₂(2-FC₆H₄COO)₆?4H₂O has been synthesized and structurally characterized by single crystal X-ray diffraction methods. The complex crystallizes in the triclinic system with space group P \(\bar 1\), lattice parameters a = 9.293(8) Å, b = 9.845(8) Å, c = 12.703(11) Å, α = 85.470(14)^°, β = 87.537(12)^°, γ = 62.485(11)^°, V = 1027.5(15) ų, Z = 1, D_calc = 1.998 Mg/m³. The Ho³⁺ ion is in distorted monocapped square-antiprism coordination environment and is coordinated by nine oxygen atoms, seven from five 2-FC₆H₄COO^2? groups, two from two water molecules. Two Ho³⁺ ions are linked together by four bridging carboxylate groups to form a binuclear molecule with inversion center.     

Base-Stabilized Monomeric Stibinoalane dmap–Al(Et<Subscript>2</Subscript>)Sb(<Superscript>t</Superscript>Bu)<Subscript>2</Subscript>

Abstract  

The six-membered heterocycle [Me₂AlSb(t-Bu)₂]₃ was reacted with the strong Lewis-base 4-dimethylaminopyridine (dmap), yielding the first completely alkyl-substituted monomeric complex dmap–Al(Me₂)Sb(t-Bu)₂ 1. 1 was characterized by NMR spectroscopy and single crystal X-ray diffraction. 1 is monoclinic, space group P2 ₁ /n with a = 9.9004(2) ?, b = 16.8166(3) ?, c = 13.8400(3) ?, β = 100.746(1)° and Z = 4.     

The Crystal Structures of Bis(2-amino-5-methylpyridinium) Tetrabromometallate(II): Intermolecular Interactions in (C<Subscript>6</Subscript>H<Subscript>9</Subscript>N<Subscript>2</Subscript>)<Subscript>2</Subscript>[MBr<Subscript>4</Subscript>]; M = Cd and Co

Abstract The crystallization and structures of a triclinic (henceforth T) (C₆H₉N₂)₂[CdBr₄] and a monoclinic (henceforth M) of (C₆H₉N₂)₂[CoBr₄] are reported. The crystal packing of both solids is analyzed and compared: both contain parallel chains of cations and stacks of anions. In both T and M, each [MBr₄]²⁻ is hydrogen bonded non-symmetrically to surrounding cations in a ladder chains that run along b axis, with planar cations in both structures falling in parallel to the planes to anions. In T the cation chains are further involved in classical π···π stacking, while in M the cation chains show less significant stacking, with longer repeat distance. Index Abstract Extensive N–H···Br hydrogen bonds link both anions and cations into chains of the ladder type parallel to the crystallographic b axis. The crystal structures of bis(2-amino-5-methylpyridinium) tetrabromometallate(II): Intermolecular interactions in (C6H9N2)2[MBr4]; M = Cd and Co Rawhi Al-Far and Basem Fares Ali