Synthesis and Crystal Structure of NdCaGaO4

The crystal structure of the NdCaGaO₄ compound was investigated by means of X-ray structure analysis (powder diffractometer HZG-4, CuK_α): structure type LaCuO₄, space group Cmca, a = 5.3700(2) Å, b = 12.1058(3) Å, c = 5.3937(2) Å, Z = 4, R_I = 0.126. The shortest interatomic distances are: Nd(Ca)—O — 2.240(14) Å; Ga—O — 1.913(2) Å, O—O — 2.6852(2) Å, Nd(Ca)—Nd(Ca) — 3.442(3) Å, Nd(Ca)—Ga — 3.154(4) Å, Ga—Ga — 3.8056(2) Å. Atoms have the following coordination numbers: Nd(Ca) — 8; Ga — 6; O1 — 14(6); O2 — 9(5).     

Crystal and molecular structure of N-(Diethylaminothiocarbonyl)-N′-phenyl-benzamidine

The crystal structure of the title compound has been determined by X-ray diffractometer data collected on a CAD-4 diffractometer. C₁₈H₂₁N₃S crystallizes monoclinic, space group P 2₁/n with a = 8.939(1) Å, b = 18.992(3) Å, c = 10.416(2) Å, β = 97.29(2) Å and Z = 4. Least-squares refinement gave a value of R = 0.107 for 2647 observed reflections. The molecule has a configuration which can be described best by Z, E′ and exists in the tautomeric enamine form. The molecules form infinite chains connected by intermolecular N—H … S interactions, with H … S distances of 2.46 Å.     

Crystal Structure of a Complex of Sarcosine with Barium Chloride

Single crystals of sarcosine barium chloride tetrahydrate were crystallised from a saturated aqueous solution containing stoichiometric amounts of sarcosine and barium chloride, in 2: 1 proportion. The intensity data were collected using a CAD-4 diffractometer with graphite monochromated MoKα radiation. The crystal data are as follows: a = 7.235(1) Å, b = 10.668(4) Å, c = 15.686(3) Å, V = 1210.7 ų, F.W. = 369.33, d_expt, = 2.02 g · cm⁻³, d_calc = 2.026 g · cm⁻³, Z = 4 and the space group is P2₁2₁2₁. The structure has been solved to an R value of 0.02 for all the 1239 reflections with I > 2σ(I). The sarcosine molecule exists as zwitterion in the structure. The barium ion is found to have 10-fold coordination with nine oxygens and a chlorine taking part in coordination. All the water oxygens and chlorines take part in hydrogen bonds except carboxyl oxygens.     

Crystal and molecular structure of the chiral compound 4–(2–methylbutyloxy)phenyl–4–(2-propenyloxy)-benzoate,C21H24O4

The enantiomeric [(S)-(–)-MBP3B] and the racemic form [(±)-MBP3B] of the title compound with the formula C₃H₅O–C₆H₄–CO₂–C₆H₄–OC₅H₁₁ were studied by single crystal analysis at room temperature. (S)-(–)-MBP3B crystallizes in the orthorhombic space group P2₁2₁2₁ with a = 7.835(3) Å, b = 11.093(6) Å, c = 44.820(3) Å and 8 molecules per unit cell. The structure was determined from 966 reflections with intensities > 3σ. The refinement with isotropic temperature factors leads to R = 0.094. The crystals of the racemic form are monoclinic, space group P2₁/a with a = 7.899(5) Å, b = 11.046(6) Å, c = 22.845(12) Å, β = 99.28(3)°, Z = 4.1236 diffractometer data (I > 3σ) were refined by least-squares methods with anisotropic temperature factors for the non-H atoms to R = 0.070. The packing arrangement for both forms shows a layer-like structure with very similar packing coefficients, k = 0.7085 for the pure enantiomer and k = 0.7014 for the racemic form.     

Crystal and molecular structures of 4-N-morpholino-7-phenyl 1,3-isobenzofurandione

The crystal and molecular structures of 4-N-morpholino-7-phenyl-1,3-isobenzofurandione have been determined by X-ray diffraction analysis (Nicolet R3m automated diffractometer, MoK _α radiation, graphite monochromator, θ/2θ scan mode). It is found that the compound crystallizes in the orthorhombic system, space group Pbca. The unit cell parameters are as follows: a = 7.773(2) Å, b = 14.652(3) Å, c = 25.614(5) Å, and Z = 8. The structure is solved by the direct method and refined to R1 = 0.0504 [I > 2σ(I)]. The conformational and geometric characteristics of the studied compound and the molecular packing in the crystal are discussed.     

Crystal Structure of Sarcosine Cadmium Chloride

Single crystals of sarcosine cadmium chloride were crystallised from a saturated aqueous solution containing stoichiomeric amounts of sarcosine and cadmium chloride, in 1:1 proportion. The intensity data were collected using a CAD-4 diffractometer with graphite monochromated MoK_α, radiation. The crystal data are as follows: a = 6.916(1) Å, b = 13.855(3) Å, c = 7.981(1) Å, V = 764.1 Å · F.W. = 272.4, d_expt = 2.39 g · cm⁻³, d_calc = 2.368 g · cm⁻³, Z = 4 and the space group is P2₁/n. The structure has been solved to an R value of 0.023 for all the 1323 reflections with I > 2σ(I). The sarcosine molecule exists as zwitterion in the structure. The conformation of the sarcosine molecule is significantly changed due to the complexation of the molecule with cadmium chloride. The cadmium ion is found to have an octahedral coordination with both the oxygens of the carboxyl group of the amino acid and chlorines taking part in it. Since the complex has no water of hydration, only two hydrogen bonds of the types N H ‥ O and N H ‥ Cl are found.     

Yttrium barium heptaoxocobaltate YBaCo4O7+δ: Refinement of the structure and determination of the composition

Parameters of the crystal structure of compound YBaCo₄O₇ are refined. The experimental data [3917 reflections measured, 469 unique I _hkl , and 420 observed reflections with I > 2σ(I)] are obtained on a Bruker X8APEX automated diffractometer equipped with a CCD detector [MoK _α, graphite monochromator, θ_max = 33.09°, space group P6₃ mc, a = 6.3058(4) Å, c = 10.2442(7) Å, V = 352.77 ų, Z = 2, d _calcd = 5.404 g/cm³, R ₁ = 0.0183 for 420 observed reflections and 0.0216 for all unique reflections]. The refinement shows that the occupancy factors of all sites of the space group correspond within three standard deviations to the standard values, that is, to the Y: Ba: Co: O = 1: 1: 4: 7 whole-number ratio of elements in the formula of the compound and to the absence of an aluminum impurity in the crystal.     

Molecular and crystal structures of 3-methyl-3-[1,7-dicarba-closo-dodecaborane(12)-1-oyl-peroxy]-but-1-yne

The crystal and molecular structures of 3-methyl-3-[1,7-dicarba-closo-dodecaborane(12)-1-oylperoxy]-but-1-yne (I) are determined by X-ray diffraction analysis (Nicolet R3m automated diffractometer, MoK _α radiation, θ/2θ scan mode). It is found that the compound crystallizes in the orthorhombic crystal system, space group P2₁2₁2₁. The unit cell parameters are as follows: a = 7.355(2) Å, b = 9.773(3) Å, c = 21.938(7) Å, and Z = 4. The structure is solved by the direct method and refined to R = 0.0658. The structural features of the molecule and the C-H?O contacts in the structure are discussed.     

Formation of Hydrogen-Bonding Adduct between 1-Phyenyl-2-Amino Pyrimidine and Vaniline,C17H13N3O2

The adduct compound was prepared by condensation of equimolar quantities of analar vaniline and 1-phenyl-2-amino pyrimidine in absolute ethyl alcohol. Prismatic crystals were obtained with the crystallographic data: a = 12.901 (6), b = 19.297 (9), c = 6.828 (3) Å, γ = 102.67 (2)°, V = 1657.9 ų, Z = 4, F.W. = 291.31, D_x = 1.17 g/cm³, space group P2/n, R = 0.038 and R_w = 0.036. The intensity data were collected on an Enraf Nonius CAD-4 computer controlled diffractometer using MoKα radiation. The structure was solved by direct method and refined by full matrix least-squares using anisotropic temperature factor of all atoms, except for hydrogen ones, which were treated isotropically. A full discussion was given to explain: a) the occurrence of the condensation process between the OH-group of vaniline and the heterocyclic N-atom in position 5 of the pyrimidine cycle and b) why this condensation does not take place between the amino-group of the pyrimidine compound and the aldehydic group of vaniline to give a Schiff base.     

Crystal structure refinement of the ternary compound Cu2SnTe3 by X‐ray powder diffraction

The ternary compound Cu₂SnTe₃ crystallizes in the Imm2 (Nº 44) space group, Z = 2, with a = 12.833(4) Å, b = 4.274(1) Å, c = 6.043(1) Å, V = 331.5(1) ų. Its structure was refined from X‐ray powder diffraction data using the Rietveld method. The refinement of 25 instrumental and structural variables led to R_p = 10.2%, R_wp = 11.8%, R_exp = 7.7%, R_B = 10.6%, S = 1.6 and χ² = 2.6, for 5501 step intensities and 163 independent reflections. This compound is isostructural with Cu₂GeSe₃, and consists of a three‐dimensional arrangement of slightly distorted CuTe₄ and SnTe₄ tetrahedra connected by common corners. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

The Structure of 4-n-Hexyle-6-(4-cyanophenyl)-1,5-diazobicyclo [3.1.0]-hexanone-(2), C17H21N3O

M_r = 283.2; monoclinic, P 2₁/c, a = 9.631(7), b = 21.268(16), c = 8.488(8) Å, β = 107.13(9)°, Z = 4, V = 1661.8(9) ų, D_x = 1.42 Mg m⁻³, final R = 0.134 for 605 independent reflections excluding those with |F_o| < 3σ|F_o|). Intensities were measured with an automatic diffractometer. The compound is a product of a photoreaction. The five membered ring and the three membered ring of the bicyclic diaziridine group and the six membered ring of the 4-cyanophenyl group are nearly perpendicular one to another. The 4-cyanophenyl group is in exo-position to the five membered ring of the bicyclic diaziridine group. The C(4) atom and the aliphatic hexyle group are in respect to the five ring in trans-position.     

Hydrothermal synthesis and the crystal structure of borate cancrinite (Na,Ca)2[Na6(AlSiO4)6](BO3) · 2H2O

Transparent prismatic single crystals of borate cancrinite (Na,Ca)₂[Na₆(AlSiO₄)₆](BO₃) · 2H₂O are prepared through hydrothermal crystallization. The parameters of the hexagonal unit cell and intensities of 10806 reflections are measured on an Enraf—Nonius CAD4 automated diffractometer. The compound crystallizes in the hexagonal crystal system with the unit cell parameters a = 12.745(4) Å, c = 5.180(2) Å, V = 728.6(4) ų, and space group P6₃. The structure is determined by direct methods and refined using the full-matrix least-squares procedure in the anisotropic approximation for the non-hydrogen atoms. The refinement of the structure is performed to the final discrepancy factor R ₁ = 0.027 for 2889 unique reflections with I > 2 σ (I). In the structure of the borate cancrinite, the AlO₄ and SiO₄ tetrahedra form a zeolite-like framework in which twelve-membered hexagonal channels are occupied by sodium atoms and BO₃ groups, whereas six-membered channels are filled with sodium and calcium atoms and water molecules. The mean interatomic distances are found to be as follows: (Si-O)_mean = 1.614 Å and (Al-O)_mean = 1.741 Å in the AlO₄ and SiO₄ tetrahedra, (Na-O)_mean = 2.542 Å in the seven-vertex sodium polyhedra, and [(Na,Ca)-O]_mean = 2.589 Å in the ditrigonal bipyramids.     

Crystal structures of double vanadates, Ca9 R(VO4)7 ⋅ III. R = Nd, Sm, Gd, or Ce

The crystal structures of Ca₉ R(VO₄)₇ (R = Nd (I), Sm (II), or Gd (III)) were studied by the Rietveld method. The compounds are isostructural to Ca₃(VO₄)₂ and are crystallized in the trigonal system (sp. gr. R3c, Z = 6). The unit-cell parameters are as follows: for I, a = 10.8720(5) Å, c = 38.121(1) Å; for II, a = 10.8652(5) Å, c = 38.098(1) Å; and for III, a = 10.8631(5) Å, c = 38.072(1) Å. In the structures of I and II, the M(1), M(2), and M(3) positions are statistically occupied by the rare-earth cations and calcium anions. In the structure of III, the Gd³⁺ cations occupy the _M(1) and _M(2) positions. The distributions of the R ³⁺ cations over the positions are characteristic of each structure. The composition of the cerium-ontaining compound Ca_9.81Ce_0.42(VO₄)₇ (a = 10.8552(5) Å, c = 38.037(1) Å) was refined and its crystal structure was solved from the X-ray powder data. In this compound, cerium atoms are in the oxidation states +3 and +4.     

α-substituted Phosphoryl Compounds (II). The Crystal and Molecular Structure of Diphenyl-[5,6-dichloro-1, 3-benzodioxol-(2)]-phosphine-oxide,C19H13O3PCl2

The compound crystallizes in the monoclinic space group P 2₁/c with four molecules per unit cell, and with the lattice parameters a = 11.807 Å, b = 13.070 Å, c = 11.312 Å, β = 96.74°. With X-ray diffraction data collected on a four circle diffractometer, the crystal structure has been determined by direct methods and refined to an R-value of 0.061 for 2735 measured and symmetrically independent reflections. The substance is a derivative of acetales of formyl diphenyl phosphine oxides. Correlations between the geometry of the structure and NMR-data are of interest.     

The structure of Dimethylaminomethanediphosphonic Acid,C3H11NO6P2

M_r = 218.9, monoclinic, P 2₁/c, a = 6.870(1), b = 10.824(2), c = 11.337(2) Å, β = = 94.59(2)⁰, Z = 4, V = 840.5(3) ų, D_x = 1.73 Mgm⁻³. Final R = 0.033 for 2648 independent reflections, excluding those with |F₀| < 3σ(F₀). Intensities were measured with an automatic diffractometer. This organophosphorous compound is characterized by two P C bonds. Four symmetrically independent intermolecular hydrogen bonds determine the threedimensional packing of the molecules and the unique chemical properties of the campound.     

Structures of Azomethine Imines of the Pyrazolidone-(3)-type, (III) The Structure of 1-[Anthryl-(9)-methylene]-pyrazolidone-(3)-betaine

C₁₈H₁₄N₂O, Pbca, a = 19.541(4) Å, b = 14.800(2) Å, c = 9.572(3) Å, Z = 8, U = 2768.3 ų, D_x = 1.32 g cm⁻³, μ(MoKα) = 0.93 cm⁻⁻¹, crystal size 0.5 × 0.2 × 0.1 mm, colourless. Final R = 0.077 for 1177 independent reflections excluded those with |F₀| < 8 σ(F₀). The intensities were measured with an automatic diffractometer. The azomethine imine unit of the molecule has a geometry in approximate agreement with a polymethinic electron structure. The conjugation of the azomethine imine unit with the anthryl unit is only small. The anthryl ring and the five membered pyrazolidone ring include a dihedral angle of 65.4°. The main intermolecular forces are C–H … N hydrogen bridges.     

The Crystal and Molecular Structure of 2-(2′-Cyano-2′-amido-ethylenyl)-pyridine

The title compound (C₉H₇N₃O) has been determined from three dimensional X-ray diffraction data. The crystals are monoclinic, a = 4.858(3) Å, b = 15.008(7) Å, c = 11.787(2) Å, ß = 94.107(2)°, V= 857.2(4) ų, z = 4, D_calc = 1.342 g. cm⁻³, space group P2_1/c. The structure was solved by direct methods and refined by full-matrix least-squares method (γ MoK_α′, R = 0.0766).     

The Crystal and Molecular Structure of 1,18-dibromooctadecane

The crystal and molecular structures of 1,18-dibromooctadecane are determined precisely by X-ray diffraction method. The results obtained are as follows: empirical formula, C₁₈H₃₆Br₂, formula weight Mr = 412.27, crystal system, monoclinic, space group, P2₁/n, lattice parameters, a = 5.496(1), b = 5.403(1), c = 34.374(4) Å, β = 94.50(1)°, volume of unit cell, V = 1017.6(3) ų, Z value, Z = 2, calculated density, D_x = 1.346 g/cm³, wave length of X-ray, λ(CuKα) = 1.5418 Å, absorption coefficient, μ(CuKα) = 49.64 cm⁻¹, F(000) = 428.00, temperature, T = 293 ± 1 K, R factor, R = 0.052, weighted R factor, R_w = 0.078 for 1019 unique observed reflection [I > 3σ (I)]. There are no unusual bond distances or angles. The structure obtained here is quite similar to that of 1,12-dibromododecane.     

The crystal structure of zinc azide · 2-methylpyridine at 98 K

The crystal structure of the title compound has been determined by single crystal X-ray diffraction methods at 98 K. Zinc azide · 2-methyl pyridine crystallizes in the space group P1 with a = 6.028(2) Å, b = 7.610(3) Å, c = 10.052(4) Å, α = 92.81(3)°, β = 101.08(2)·, γ = 94.64(3)° and Z = 2. Least-squares refinement gave an R value of R_w = 0.039 for 2096 observed reflections. Each zinc atom is surrounded by four nitrogen atoms of different azide groups and one nitrogen atom of the pyridine adduct in a distorted trigonal bipyramidal fashion. The ZnN₅-polyhedra share common edges to form chains along the crystallographic a-axis.     

Crystal structure of hydrazine 5-amino-1-benzyl-1,2,3-triazole-4-carboxylate hexafluorosilicate trihydrate

Hydrazine 5-amino-1-benzyl-1,2,3-triazole-4-carboxylate hexafluorosilicate trihydrate (I) is synthesized. The crystal structure of the compound synthesized is determined. Crystals I are monoclinic, a = 13.353(1) Å, b = 21.094(2) Å, c = 20.233(2) Å, β = 94.05(3)°, space group P2₁/c, and R = 0.0584 for 16 601 reflections with I > 2σ(I). In the asymmetric part of the unit cell, four organic cations protonated at the terminal hydrazine nitrogen atoms, two hexafluorosilicate anions, and six water molecules are linked into a three-dimensional framework through hydrogen bonds of the N-H?F, N-H?O, and O-H?F types.