Synthesis and Crystal Structure of 2D Supramolecular Compound [Co(phth)(phen) (H<Subscript>2</Subscript>O)<Subscript>3</Subscript>]·H<Subscript>2</Subscript>O

Abstract  

A 2D supramolecular compound [Co(phth)(phen) (H₂O)₃]·H₂O has been synthysized by the reactions of Co(NO₃)₂·6H₂O, 1, 10-phenanthroline(phen) and phthalate acid(H₂phth) in NaOH solution with pH 7.0.The complex has been characterized by elemental analysis, IR, and single-crystal X-ray diffraction analysis which shows it belongs the monoclinic space group P2(1)/n, a = 7.571(2) ?, b = 13.737(3) ?, c = 20.015(4) ?, β = 95.56(1)°. V = 2071.9(8) ?³, Mr = 475.31, Dc = 1.524 g/cm⁻³, Z = 4, F(000) = 980, μ(MoKa) = 0.879 mm⁻¹. The final R1 and wR2 are 0.0348 and 0.0711, respectively. The cobalt(II) ion is six-coordinated in a distorted octahedron to form a unit. Every unit is connected by hydrogen bonds forming 1D chain and 2D supramolecular network by π–π stacking interaction between adjoining chains.     

Synthesis and Crystal Structure of [Ni(L)(Phen)(H<Subscript>2</Subscript>O)]·3.75H<Subscript>2</Subscript>O

Abstract  

The title compound, [Ni(L)(Phen)(H₂O)]·3.75H₂O, where L = (E)-2-(5-formyl-2-oxidobenzylideneamino)ethanesulfonate, was synthesized in aqueous methanol in the presence of Ni(II), Phen and the potassium salt of 2-{[(E)-(2-hydroxy-5{[(2-sulfoethyl)imino]methyl}phenyl)methylidene]amino}-1-ethanesulfonic acid. The complex crystallized in the space group of P-1 with a = 13.751 (2) ?, b = 14.797 (2) ?, c = 15.543 (2) ?, α = 105.86 (1)°, β = 103.51 (1)°, γ = 114.38 (1)°, and Z = 2. In [Ni(L)(Phen)(H₂O)], the Ni(II) was six coordinated with two O and one N from L, two N from Phen and one O from coordinated water, forming an octahedral geometry. There are two molecules in the asymmetric unit and concomitant differences in the Ni-ligand bond lengths.     

Synthesis,Crystal Structure and Spectral Properties of [Fe<Subscript>3</Subscript>(2,2′-bipy)<Subscript>6</Subscript>(ox)<Subscript>3</Subscript>]·12.25H<Subscript>2</Subscript>O Complex

A novel iron (II) complex of formula [Fe₃(2,2′-bipy)₆(ox)₃]·12.25H₂O (2,2′-bipy = 2,2′-bipyridine, ox = oxalate) has been prepared and structurally characterized by X-ray crystallography. In the complex, the metal atoms are six-coordinated in distorted octahedral environment. In the complex [Fe(ox)₃]^4? anions and water molecules are linked together into 1D chain structure by hydrogen interaction. The red crystal of the complex is monoclinic, space group P2₁/c, with a = 22.932(6) Å, b = 13.715(4) Å, c = 22.493(6) Å, β = 93.177(5)°, and V = 7063(3) Å³ with Z = 4.     

Synthesis and Crystal Structure of a Novel Supramolecular Complex: [Co(2-Me-3,4-qudc)(Phen)<Subscript>2</Subscript>(H<Subscript>2</Subscript>O)]·4.5H<Subscript>2</Subscript>O

Abstract  

A novel 3D supramolecular complex, [Co(2-Me-3,4-qudc)(Phen)₂(H₂O)] 4.5H₂O (2-Me-3,4-qudc = 2-methylquinoline-3,4-dicarboxylate dianion, phen = 1,10-phenanthroline), has been synthesized under mild condition and characterized by elemental analyses, IR spectrum, thermogravimetric analysis and single-crystal X-ray diffraction. The complex crystallizes in the monoclinic space group P2₍₁₎ /n with unit cell parameters a = 13.1701(12) ?, b = 18.6728(19) ?, c = 15.0683(16) ?, β = 13.617(2), V = 3395.3(6) ?³, Z = 4. The 3D framework of the title compound is formed via O–H⋯O hydrogen-bonds and π–π stacking interactions. The lattice waters are stable at room temperature, but when thermally decomposed, the water loss is irreversible.     

New Diphosphopentamolybdate K<Subscript>5</Subscript>[HP<Subscript>2</Subscript>Mo<Subscript>5</Subscript>O<Subscript>23</Subscript>] · 10H<Subscript>2</Subscript>O: Synthesis,Structure, and Characterization

A new diphosphopentamolybdate(VI) K₅[HP₂Mo₅O₂₃] · 10H₂O has been prepared employing solution method and characterized by single crystal X-ray diffraction, energy dispersive analysis, infrared spectroscopy, thermal stability analysis, cyclic voltammetry analysis, and ultraviolet visible spectroscopy. The compound crystallizes in the orthorhombic sp. gr. Pcab: a = 15.9661(10) Å, b = 19.0832(10) Å, c = 20.0970(9) Å, V = 6123.27(10) Å3, Z = 8. The crystal structure contains the polyanion units [HP₂Mo₅O₂₃]^5– around the potassium cations and lattice water. The [HP₂Mo₅O₂₃]^5– subunits are connected together through K?O?Mo bridges and hydrogen bonds. The crystal shape morphology was simulated using the Bravais–Friedel–Donnay–Harker model.     

Synthesis and Crystal Structure of [Na(H<Subscript>2</Subscript>O)<Subscript>1.5</Subscript>][Na(H<Subscript>2</Subscript>O)<Subscript>3.5</Subscript>] X<Subscript>2</Subscript>·2H<Subscript>2</Subscript>O (X = 4′-Methoxy-7-Hydroxyisoflavone-3′-Sulfonate)

Abstract  

Water-soluble derivative of formononetin, [Na(H₂O)_1.5][Na(H₂O)_3.5] X₂·2H₂O(X = 4′-methoxy-7-hydroxyisoflavone-3′-sulfonate) was synthesized by sulfonation reaction. It was characterized by IR, ¹H NMR and single-crystal X-ray diffraction analysis. Single-crystal X-ray diffraction analysis showed that the title compound crystallized in a triclinic space group P-1 with cell parameters a = 6.9642(15) ?, b = 13.343(3) ?, c = 20.634(5) ?, α = 107.115(3)˚, β = 93.121(4)˚, γ = 91.911(3)˚, V = 1827.3(7) ?⁻³, D _c  = 1.575 Mg m ⁻³, Z = 2. There are two conformers of 4′-methoxy-7-hydroxyisoflavone-3′-sulfonate anions, two kinds of sodium cations, five coordinated water molecules and two lattice water molecules in the crystal structure. The sodium atoms coordinated with the oxygen atoms from water molecules, hydroxyl groups and sulfo-groups to form a Na–O coordinated network. Aromatic π···π stacking interactions and hydrogen bonding existed in the crystal structure of title compound, which together with coordinated interactions and electrostatic interactions between sodium cations and anions sulfonates C₁₆H₁₀O₄SO₃ ⁻ lead to the moieties into a three-dimensional network.     

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 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.     

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 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.     

Ordering of calcium and vacancies in calcium catapleiite CaZr[Si<Subscript>3</Subscript>O<Subscript>9</Subscript>] • 2H<Subscript>2</Subscript>O

A sample of holotypic calcium catapleiite from the Burpala alkaline massif (Northern Baikal, Russia) is studied by single crystal X-ray analysis at 120 K and IR spectroscopy. The empirical formula of calcium catapleiite is Ca_0.97Na_0.02Zr_1.01Si₃O₉ ? 2H₂O (Z = 4). The X-ray diffraction study confirms the orthorhombic unit cell with the following parameters: a = 7.406(1), b = 12.687(1), and c = 10.112(1) Å; V = 950.1(2) ų; space group Pbnn. The crystal structure is refined in the anisotropic approximation of atomic displacement parameters using 1177 reflections with I > 2σ(I) to the final R = 2.91%. The structure of calcium catapleiite under study is based on the microporous heteropolyhedral framework formed by ZrO₆ octahedra and threemembered silicon–oxygen rings [Si₃O₉]. It is on the whole analogous to the structures of the samples studied earlier, but differs from them by a high degree of ordering of calcium and vacancies at extraframework positions. The distribution of calcium over Ca1 and Ca2 positions in the calcium catapleiite structure leads to the formation of zigzag chains of the …Сa1–Zr–Ca1–Zr… and …Сa2–h–Ca2–□… types. Low occupancy of the Ca2 position and its alternation with the vacancy are prerequisites for potential Ca²⁺ cationic conduction.     

Synthesis and structure of a new hybrid vanadium arsenate: [VO<Subscript>2</Subscript>(phen)]<Subscript>2</Subscript>(H<Subscript>2</Subscript>AsO<Subscript>4</Subscript>)⋅H<Subscript>3</Subscript>O

A new hybrid vanadium arsenate [VO₂(phen)]₂(H₂AsO₄)H₃O 1 (phen = 1,10-phenanthroline) was synthesized under hydrothermal reaction conditions and structurally characterized by single-crystal X-ray diffraction, thermogravimetric analysis (TGA), IR and elemental analyses. Crystal data for 1: monoclinic, P2₁/n, a = 9.175(2) Å, b = 18.638(5) Å, c = 14.482(4) Å, = 102.333(3), V = 2419(1) ų, Z = 4. Compound 1 is composed of discrete tricyclic (VO₂)₂(H₂AsO₄) cluster decorated with two phen ligands. The discrete arsenic–vanadium clusters are extended into three-dimensional supramolecular arrays via – stacking interactions of phen groups.     

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.     

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.     

Synthesis and structure of the [Os<Emphasis Type="Italic">Thio</Emphasis><Subscript>6</Subscript>]Br<Subscript>3</Subscript> · H<Subscript>2</Subscript>O complex

A complex of the composition [OsThio ₆]Br₃ · H₂O is synthesized by the reaction of H₂OsBr₆ with thiourea in a 0.5 M HBr solution. The [OsThio ₆]Br₃ · H₂O complex is characterized using electronic absorption and infrared spectroscopy. The structure of the complex is determined by X-ray diffraction analysis. The crystals are orthorhombic with the unit cell parameters a = 20.510(4) Å, b = 11.186(2) Å, c = 11.892(2) Å, space group Pccn, and Z = 4. The thiourea molecules are coordinated to the osmium atom through the sulfur atom. The osmium atom has an octahedral coordination. The Os-S distances fall in the range 2.39–2.40 Å. The outersphere H₂O molecules and Br^? anions are involved in hydrogen bonds with the NH₂ groups of the thiourea molecules.     

Synthesis and Crystal Structure of the Coordination Polymer [Cu(ppca′)<Subscript>2</Subscript>(H<Subscript>2</Subscript>O)(HgI<Subscript>2</Subscript>)](H<Subscript>2</Subscript>O) (ppca′ = 3,4′-bipyridine-6-carboxylic acid)

Abstract  

The coordination complex Cu(ppca′)₂(H₂O)₂ (1) was synthesized hydrothermally using the ligand 3,4′-bipyridine-6-carboxylic acid (ppca′). Complex 1 consists of pseudo-octahedral copper (II) units hydrogen bonded into a three-dimensional network that crystallizes in the monoclinic P2₁/n space group. In complex 1, a = 5.3429(4) ?, b = 29.343(2) ?, c = 6.7940(5) ?, and β = 110.635(2)°.     

Crystal structure of the (Mg,Fe)[UO<Subscript>2</Subscript>(P,As)O<Subscript>4</Subscript>]<Subscript>2</Subscript> · 10H<Subscript>2</Subscript>O solid solution—A novel mineral variety of saléeite

The crystal structure of a novel variety {[(Mg_0.81Fe_0.19)(H₂O)₆](H₂O)₄}{(UO₂)[(P_0.67As_0.33)O₄]}₂ of the mineral saléeite is determined using X-ray diffraction (Bruker Smart diffractometer, λMoK _α, graphite monochromator, 2θ_max = 56.62°, R = 0.0321 for 2317 reflections, T = 100 K). The main crystal data are as follows: a = 6.952(6) Å, b = 19.865(5) Å, c = 6.969(2) Å, β = 90.806(4)°, space group P12₁/n1, Z = 2, and ρ_calcd = 3.34 g/cm³. It is shown that the structure is formed by alternating (along the [010] direction) anionic layers, which are composed of uranium bipyramids and T(P,As) tetrahedra, and cation layers consisting of M(Mg,Fe) octahedra and water molecules, which are joined through a system of asymmetric hydrogen bonds. The hydrogen atoms are located, the scheme of hydrogen bonds is established, and their geometric characteristics are calculated.     

Crystal Structure and Vibrational Spectra of Erbium Trisodium Bis(Cyclotriphosphate) Nonahydrate,ErNa<Subscript>3</Subscript>(P<Subscript>3</Subscript>O<Subscript>9</Subscript>)<Subscript>2</Subscript> · 9H<Subscript>2</Subscript>O

Abstract The cyclotriphosphate salt, ErNa₃(P₃O₉)₂ · 9H₂O, has been characterized by single-crystal X-ray diffraction [hexagonal, space group , with unit cell parameters of a = b = 30.8451(14), c = 12.8063(8) ?; Z = 18]. The structure consists of alternating layers of [P₃O₉]³⁻ groups, ErO₈ dodecahedra, Na(1)O₆ and Na(2)O₇ polyhedra linked together by water molecules. The P₃O₉ rings are grouped along the c-axis in a P₃O₉–ErO₈ arrangement thereby producing broad, hexagonal channels of diameter of 6.65 ? with a side dimension of 3.907 ?. The absence of coincidences for the majority of the IR and Raman bands observed for the cyclotriphosphate salt is in accord with the centrosymmetric structure of the material. The vibrational spectra have been interpreted on the basis of factor group effects. Graphical abstract We report the crystal structure and vibrational spectra of erbium trisodium bis(cyclotriphosphate)nanohydrate salt ErNa ₃ (P ₃ O ₉ ) ₂ · 9H ₂ O H. Assaaoudi, M. Ijjaali, A. Ennaciri, I. S. Butler* and J. A. Kozinski Crystal structure and vibrational spectra of erbium trisodium bis(cyclotriphosphate) nonahydrate,ErNa₃(P₃O₉)₂ · 9H₂O. Projection of the coordination polyhedra of ErNa₃(P₃O₉)₂ · 9H₂O down the c axis