The crystal structure of hexaammonium diacetyl‐octa‐molybdate tetrahydrate

The crystal structure of hexaammonium diacetyl‐octa‐molybdate tetrahydrate, (NH₄)₄₂[Mo₁₃₂O₃₇₂ (CH₃COO)₃₀(H₂O)₇₂] is documented. The crystals are triclinic, space group P‐1, with a=8.1018(16) Å, b=10.334(2) Å, c=12.238(2) Å, α=68.20(3)°, β=74.98(3)°, γ=67.25(3)°, V=869.3(3) ų, Z=1. The structure was solved by direct methods and refined by least squares methods to a Final R1 = 0.0374 and wR2 = 0.1074 for 3805 observed reflections with I > 2σ(I). The structure contains ammonium cations and isolated acetyl octamolybdate(6‐) anions, [Mo₈O₂₈(CH₃CO)₂]^6‐. The crystallographic data of the structure was deposited with the Cambridge Data Center as No. CCDC 249565. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal structure and electrochemical properties of the supramolecular compound [Himi]6[As2Mo18O62]·11H2O

A supramolecular compound, [Himi]₆[As₂Mo₁₈O₆₂]·11H₂O ( 1 ) (imi = imidazole), has been synthesized and characterized by single crystal X‐ray analysis, IR spectra, thermal gravimetric analysis, electrochemical and elemental analysis. The crystals are monoclinic, P 2(1)/n, a = 14.9529(8) Å, b = 20.9521(11) Å, c = 25.2464(13) Å, β = 93.8130(10)°, V = 7892.1(7) ų, Z = 4. X‐ray diffraction indicated that protonated imidazole cation and polyanion were linked together through electrostatic interactions and intermolecular forces (hydrogen bonding). (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal structure of 2‐(2'‐hydroxyphenyl)‐6‐tributylstannyl‐4‐(3H )‐quinazolinone and 2‐(2'‐hydroxyphenyl)‐6‐iodo‐4‐(3H)‐quinazolinone

The structures of the title compounds C₂₆H₃₇N₂O₂Sn ( I ) and C₁₄H₉IN₂O₂ ( II ) were determined by single‐crystal X‐ray diffraction technique. Compound I crystallizes in the triclinic space group P1 with a = 9.560(3) Å, b = 16.899(6) Å, c = 17.872(5) Å, α = 65.957(7)°, β = 83.603(5)°, γ ( = 75.242(5)°, V = 2549.8(13) ų, Z = 4, and D =1.374 g/cm³. The compound consists of a quinazolinone ring with phenol and tributylstannyl moieties. Compound II crystallizes in the monoclinic space group P2₁/c with a = 7.6454(12) Å, b = 5.9270(9) Å, c = 27.975(4) Å; α = 90°, β = 95.081(3)°, γ = 90°, V = 1262.7(3) ų, Z = 4, and D = 1.915 g/cm³. The compound consists of a quinazolinone ring with phenol and iodine substituents. For both I and II , the short intramolecular O–H…N and two long intermolecular N–H…O hydrogen bonds are highly effective in holding the molecular system in a stable state. (© 2006 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Structure and conformation of n‐ (t‐butoxycarbonyl)‐l‐valine‐l‐phenylalanine‐methyl ester (Boc‐Val‐Phe‐OMe)

The crystal structure of N‐ (t‐butoxycarbonyl) ‐ L‐valine‐L‐phenylalanine‐methyl ester (Boc‐Val‐Phe‐OMe), C₂₀H₃₀N₂O₅ was determined by X‐ray diffraction methods. The dipeptide crystallizes in orthorhombic space group P2₁2₁2₁, with cell parameters a = 5.0680(1) Å, b = 13.8650(1) Å and c = 28.2630(1) Å, V = 2143.8(5) ų, F.W. = 378.46, Z = 4, D_calc = 1.173 Mg/m³, μ = 0.687 mm^‐1, F₀₀₀ = 816, CuKα = 1.5418 Å. The structure was solved by direct methods and final R1 and wR2 are 0.0659 and 0.1654, respectively. The peptide unit is in trans conformation [ω = 177.4(9)°]. The conformation angles ϕ₁, ψ₁, ϕ₂ and ψ₂ for the peptide backbone are: ‐96.5(13)°, 101.2(13)°, ‐123.9(12)° and 34.0(15)°. The N‐H…O and C‐H…O hydrogen bondings influence the packing of the molecules in the dipeptide crystal. (© 2004 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

The Crystal Structure of Hydrated Barium Copper Oxalate

BaCu(C₂O₄₂.6 H₂O is triclinic, P1 , with a = 6.5405(9), b = 9.202(3), c = 10.939(1) Å, α = 85.46(2), β = 79.22(1), γ = 80.45(2), V = 636.99(1) ų, Z = 2, D₀ = 2.14, D_c = 2.465 g. cm⁻³, R = 0.074, wR = 0.0746 for 2219 significant reflections |F₀|≧ 6.0σF₀. The barium has eleven coordinations and the coordination polyhedra is a capped antiprism. Six water oxygen atoms are coordinated whereas the other five are coming from the oxalate group. In the unit cell the molecules form a polymeric network. One lattice water molecule belongs to the coordinating water. The barium oxygen distances vary from 2.75 Å to 3.15 Å.     

Crystal structures of four inclusion compounds of 2,2′-dithiosalicylic acid and tetraalkylammonium

Herein four inclusion compounds of 2,2′-dithiosalicylic acid and tetraalkylammonium, 2(CH₃)₄N⁺·C₁₄H₈O₄S₂^2?·H₂O (1), (C₂H₅)₄N⁺·C₁₄H₉O₄S₂^?·0.25H₂O(2), (n-C₃H₇)₄N⁺·C₁₄H₉O₄S₂^? (3) and (n-C₄H₉)₄N⁺·C₁₄H₉O₄S₂^?(4) are prepared and characterized by X-ray single crystal diffraction. As shown in the results, compounds 1 and 3 belong to orthorhombic crystal system with different space groups of P2₁2₁2₁ and Pca2₁, and 2 and 4 are monoclinic system with similar groups of P2₁/n and P2₁/c. The crystallography data are displayed below: 1: a = 10.5903(7) Å, b = 10.6651(7) Å, c = 21.9476(13) Å, V = 2478.9(3) ų, Z = 4, R₁ = 0.0359; 2: a = 8.13340(1) Å, b = 22.0741(3)Å, c = 13.2143(2)Å, β = 101.6360(1) °, V = 2323.70(6) ų, Z = 1, R₁ = 0.0385; 3: a = 15.7857(2) Å, b = 8.24830(1) Å, c = 20.2599(2) Å, V = 2637.94(5) ų, Z = 4, R₁ = 0.0308_degree4: a = 11.7476(2) Å, b = 17.1346(1) Å, c = 16.3583(3)Å, β = 109.4560(1) °, V = 3104.74(9)ų, Z = 4, R₁ = 0.0562. Interestingly, although the carbon chains of the guest templates vary from methyl group to butyl group, the host molecules of 2,2′-dithiosalicylic acid all construct the similar 2D hydrogen-bonded host layers with or without the existence of water molecules to contain the guest templates to yield analogous sandwich-like inclusion compounds. Obviously, although the guest templates will have certain effects on the ultimate formation of these crystal structures, the host molecule of 2,2′-dithiosalicylic acid is a controlling factor to form these four inclusion compounds.     

The crystal and molecular structure of three homologue 1,4-dialkanoyloxy-biphenyls (SYM-n)

The three homologue compounds with the general formula C_nH_2n+1 COO C₆H₄ C₆H₄ OOC C_nH_2n+1 (SYM-n) crystallize in the following space groups: SYM-1: triclinic, P1 , a = 7.400(6), b = 9.227(3), c = 10.579(3) Å, α = 85.97(3), β = 89.09(3), γ = 71.47(3)°; SYM-2; monoclinic, P2₁/c, a = 11.712(7), b = 5.648(1), c = 12.408(6), Å, β = 103.84(3)°; SYM-5: triclinic, P1, a = 5.505(4), b = 8.342(8), c = 24.79(2) Å, α = 86.67(3), β = 85.45(6), γ = 71.74(7)°. The structures have been solved by direct methods and refined to R = 0.075, 0.061 and 0.053, respectively. The packing arrangements show a layer-like structure. The layers are almost separated for SYM-1 as well as for SYM-2 and interdigitated for the structure of SYM-5.     

A Novel Polyoxometalate-Based Hybrid Materials Composed of Octamolybdate and Hexamuclear Copper Cluster Units

Self-assemble of aqueous solution of the Cu²⁺/molybdate/glyc-ine system results in {[NaCu₆(Gly)₈(H₂O)₂][Mo₈O₂₆Cu(Gly)₂]₂}_n·n{NaCu₆(Gly)₈(H₂O)₂}·n{Mo₈O₂₆[Cu(Gly)(GlyH)(H₂O)₂]₂} 15nH₂O 1, which exhibits the 0-D + 1-D supramolecular framework and in which the copper atoms show three kinds of coordination models: (1) in quadrilateral geometry, (2) in square-pyramidal geometry, and (3) in distorted octahedral geometry. The space group of the compound is P–1, with the lattice parameters: α = 89.036(5)°, β = 89.384(4)°, γ = 88.337(5) °, a = 12.559(4) Å, b = 14.441 (4)Å, c = 23.063(6) Å, and Z = 1.     

Synthesis,crystal structure and vibrational characterization of bis‐μ‐peroxo‐hexacarbonatodicerate(IV) complexes of rubidium and cesium

The new compounds Rb₈[Ce(O₂)(CO₃)₃]₂ · 12 H₂O (1) and Cs₈[Ce(O₂)(CO₃)₃]₂ · 10 H₂O (2) were obtained from the reaction of hydrogen peroxide and Ce(III) in saturated alkali carbonate solutions. The crystal structures and the unit cell parameters of (1) triclinic, P‐1 with a = 8.973(2) Å, b = 10.815(2) Å, c = 11.130(3) Å, α = 66.992(2)°, β = 68.337(2)°, γ = 74.639(2)°, V_EZ = 914.7(4) ų, Z = 2, and (2) orthorhombic, Pbca, a = 19.3840(16) Å, b = 18.528(2) Å, c = 10.487(3) Å, V_EZ = 3766.4(13) ų, Z = 8, were determined. Both compounds contain the bis‐µ‐peroxo‐hexacarbonatodicerate(IV)‐ion, [(CO₃)₃Ce(O₂)₂Ce(CO₃)₃]^8‐. IR and Raman spectra were measured and discussed. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

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.     

Pyroxenoids of pyroxmangite–pyroxferroite series from xenoliths of Bellerberg paleovolcano (Eifel,Germany): Chemical variations and specific features of cation distribution

The pyroxferroite and pyroxmangite from xenoliths of aluminous gneisses in the alkaline basalts of Bellerberg paleovulcano (Eifel, Germany) have been studied by electron-probe and X-ray diffraction methods and IR spectroscopy. The parameters of the triclinic unit cells are found to be a = 6.662(1) Å, b = 7.525(1) Å, c = 15.895(2) Å, α = 91.548(3)°, β = 96.258(3)°, and γ = 94.498(3)° for pyroxferroite and a = 6.661(3) Å, b = 7.513(3) Å, c = 15.877(7) Å, α = 91.870(7)°, β = 96.369(7)°, and γ = 94.724(7)° for pyroxmangite; sp. gr. \(P\overline 1 \). The crystallochemical formulas (Z = 2) are, respectively, ^M(1–2)(Mn_0.5Ca_0.4Na_0.1)₂^M(3–6)(Fe, Mn)₄^M7[Mg_0.6(Fe, Mn)_0.4][Si₇O₂₁] and ^M(1–3)(Mn, Fe)₃^M(4–6)[(Fe, Mn)_0.7Mg_0.3]₃^M7[Mg_0.5(Fe, Mn)_0.5][Si₇O₂₁]. For these and previously studied representatives of the pyroxmangite structural type, an analysis of the cation distribution over sites indicates wide isomorphism of Mn²⁺, Fe²⁺, and Mg in all cation M(1–7) sites and the preferred incorporation of Сa and Na into large seven-vertex M1O₇ and M2O₇ polyhedra and Mg into the smallest five-vertex M7O₅ polyhedron.     

Two organic‐inorganic hybrids with Keggin polyanions

Two new Keggin polyoxometalates [Co(phen)₃]₂[SiW₁₂O₄₀]·6H₂O (1) and (ppy)₆ H₄SiMo₁₂O₄₀·0.4H₂O (2) (phen = 1,10′‐phenanthroline, ppy = 4‐(5‐phenylpyridin‐2‐yl)pyridine) have been synthesized by the hydrothermal method. Single crystal X‐ray analysis revealed that compound 1 crystallizes in the monoclinic crystal system with cell parameters of a = 13.344(2) Å, b = 17.191(3) Å, c = 22.002(4) Å, α = 90.00°, β = 99.566(2)°, γ = 90.00°, V = 4977 ų, Z = 2, and compound 2 crystallizes in the triclinic crystal system with cell parameters of a = 11.297(2) Å, b = 12.341(3) Å, c = 19.354(4) Å, α = 107.60(3)°, β = 95.80(3)°, γ = 94.16(3)°, V = 2543.7(9) ų, Z = 1. Both 1 and 2 represent organic ligand molecules and inorganic Keggin anions, which are further interconnected to a 3D framework by supramolecular interactions. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal and molecular structures of 2-amino-5-(m-nitrophenyl)-1,3,4-Thiadiazole

2-Amino-5-(m-nitrophenyl)-1,3,4-thiadiazole (C₈H₆N₄O₂S) is studied using IR and ¹H NMR spectroscopy and X-ray diffraction (CAD4 automated diffractometer, λMoK _α, graphite monochromator, 957 unique reflections, Patterson method, R = 0.0326). The crystals are monoclinic, a = 11.832 Å, b = 9.862 Å, c = 8.353 Å, β = 110.40(3)°, V = 913.6(3) ų, d _calcd = 1.212 g cm^?3, μ(MoK _α) = 0.253 mm^?1, Z = 4, and space group P2₁/c. In the crystal, the C₈H₆N₄O₂S molecules form infinite layers parallel to the xz plane. Each layer contains aromatic rings with nitro groups that deviate from the layer plane on either side of the layer. In the packing, the aromatic rings with nitro groups of one layer fill spaces between aromatic rings with nitro groups of the adjacent layers.     

The Crystal and Molecular Structure of tert‐Butoxycarbonyl ‐ α‐aminoisobutyryl ‐ isoleucyl ‐methylester

The crystal structure of the synthetic peptide Boc — Aib — Ile ‐ OMe (C₁₆ H₃ 0 N₂ O₅ ) has been determined from three‐dimensional X — ray diffraction data. The peptide crystallizes in triclinic space group P1 with a = 9.570(9), b = 10.261(7), c = 10.610(2) Å , α = 101.9(0), β = 91.7(0), γ = 98.6(0)° V = 1006.1(12) ų, Z = 2, D_calc = 1.09 Mg m^‐3. The structure was solved by direct methods and refined by full‐matrix least‐squares method to an R value of 0.072 (λ = 1.5418Å). The conformation of Aib residue in molecule A is αL and in molecule B is αR. The Ile residue in molecule A adopts folded conformation, while in molecule B it is in the extended region. The peptide units are trans and show significant deviations from planarity.     

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 Fibrillar Sodium Trimolybdate Hydrate by Powder Diffraction Method

The crystal structure of polycrystalline fibrillar sodium trimolybdate Na₂Mo₃O₁₀. 3 H₂O, has been solved ab initio by Powder Diffraction – Direct Methods package POWSIM. The structure was refined by the Rietveld method with final discrepancy factors R_F = 6.9 and R_wp = 17.1%. The structure consists of polymeric chains of Mo-O polyhedra parallel to the b axis. The space group is C2/m (12), a = 17.179(1), b = 3.7757(3), c = 10.8571(8) Å, β = 115.417(6)°, V = 636.06(6) ų, Z = 2.     

Crystal structure of (2,2′-bipyrimidine)-dinitratopalladium(II) acetone solvate

(2,2′-bipyrimidine)dinitratopalladium(II) forms a triclinic crystal in space groupP?1 witha=7.605(5) Å,b=8.791(4) Å,c=12.632(5) Å, α=85.11(3)⁰, β=78.79(4)⁰, γ=77.45(4)⁰,V=807.7(7) ų, andZ=2. The Pd atom exhibits square planar coordination geometry with mean Pd?O=2.206(7) Å, Pd?N=1.990(5) Å, O?Pd?O=92.0(2)⁰, and N?Pd?N=81.0(2)⁰. The complexes associate across an inversion center with Pd...Pd=3.190(2) Å. The bipyrimidine ligand is bowed with a 5.9(2)⁰ dihedral angle between the C₄N₂ rings. The nitrate ions are on the same side of the N₂O₂ donor atoms plane and make 60.4(2)⁰ and 66.6(2)⁰ dihedral angles with that plane.     

Crystal and Molecular Structure of mer-Co(4-CH3C5H4N)3(N3)3

The crystal structure of mer-Co(4-CH₃C₅H₄N)₃(N₃)₃has been determined by single crystal X-ray methods at 300 K. The compound crystallizes in the monoclinic space group C 2/c, a = 19.087(6), b = 16.769(4), c = 15.845(4) Å, β = 119.04(2)°, V = 4434(2) ų, M_r = 464.42. Z = 8, D_x = 1.391 Mgm⁻³, F(000) = 1920, λ (MoKα) = 0.71069 Å, μ = 0.802 mm⁻¹. The cobalt(III) ions are octahedrally coordinated to three azide groups and to three 4-methyl-pyridine molecules to form isolated coordination polyhedra.     

Crystal structure of 4-phenyl-3,5-dioxacyclohexyl-1, 1′-cyclopentane-2′,3″-(1,5,8,11-tetraoxacyclotridecane)

The structure of the title compound is determined by X-ray diffraction (DAR-UMB diffractometer, θ-θ/2θ scan mode, MoK _α radiation, direct method). The crystal is monoclinic, a = 24.582(6) Å, b = 22.812(8) Å, c = 8.647(3) Å, γ = 60.64(2)°, ρ _calcd = 1.232 g/cm³ space group A2/a, and Z = 8 for C₂₂H₃₂O₆. The molecule consists of four fragments: 13-crown-4 (A), 1,3-dioxane (B), a five-membered ring (C) acting as a bridge between fragments A and B, and a phenyl ring (D). Introduction of the bulky ring C as a bridge into the molecule results in significant deviations (up to ±0.014 Å) of the ether O atoms from planarity. The conformation of the macrocyclic fragment is [3433] according to the Dale notation. The C—H?O 1,4-interactions, which are energetically favorable occur in the propylene part of 13-crown-4: the C(2)?O(5) and C(4)?O(1) distances are 2.82 Å. The molecules in the structure form planar networks parallel to the xy plane. The intermolecular contacts correspond to the van der Waals interactions.     

The Crystal and Molecular Structure of Mesogenic Malonates (II)

The crystal and molecular structures of three diethyl-2-{n-[4-(4-nitrophenylazo)-phenoxy]alkyl}malonate with n = 5 (5 PhNO₂), 7 (7PhNO₂), 9 (9 PhNO₂) and an analogous diethyl-2-[4(4-cyanophenylazo)phenoxy]pentylmalonate (5 PhCN) have been determined with CuK_a or MoK_a: 5 PhNO₂: a = 8.007(6) Å, b = 11.960(8) Å, c = 13.516(9) Å, α = 77.10(6)°, β = 81.80(5)°, γ = 83.15(5)°; R = 0.053; 7PhNO₂: a = 8.074(4) Å, b = 11.592(5) Å, c = 14.422(7) Å, α = 87.43(3)°, β = 82.46(3)°, γ = 85.43(3)°; R = 0.072; 9 PhNO₂: a = 5.520(5) Å, b = 13.628(9) Å, c = 20.220(11) Å, α = 100.02(4)°, β = 95.49(4)°, γ = 101.02(4)°; R = 0.042; 5 PhCN: a = 8.018(6) Å, b = 11.960(8) Å, c = 13.566(7) Å, α = 77.82(5)°, β = 81.89(5)°, γ = 82.69(5)°; R = 0.067 (isotropically refined). All these structures belong to the triclinic space groups P1 . The arrangements of the molecules in the crystal of the homologous series of nPhNO₂ suggest two different types of packing independent of n even, odd or large, small. 5 PhCN represents an isomorphous structure to 5 PhNO₂. Isomophism between 7 PhNO₂ and 7 PhCN was confirmed by cocrystallization of these two compounds whose crystal structure was also determined.