Crystal Structure of 14-Deoxy-11,12-Didehydroandrographolide — A Diterpenoid

The crystal structure of 14-deoxy-11,12-didehydroandrographolide has been determined by X-ray structure analysis. The compound crystallizes in the trigonal space group P3₁ with cell parameters a = b 15.860(3), c = 6.437(2) Å. The structure has been solved by direct methods and refined to R = 0.048. The six-membered rings are trans-fused and both are in the chair conformation. The furan ring is planar with maximum deviation −0.011 (4) Å for C(14). Molecular are held together by hydrogen bonds.     

The Crystal and Molecular Structure of Mesomorphic 1,4-Dipentadecanoyloxy-biphenyl (SYM-14)

The compound with the general formula C_nH_2n+1 –COO–C₆H₄–C₆H₄–OOC–C_nH_2n+1, n = 14 (SYM- 14) crystallizes in the triclinic space group P 1 , with a = 5.431(5), b = 9.346(8), c = 39.172(51) Å, α = 92.60(15), β = 90.65(15), γ = 100.364(8)°. The crystal structure was solved by direct methods. Least-squares refinement leads to a final R value of 0.092 for 1575 observed reflections, with I > 2σs(I). The packing arrangement follows the same building principles found recently for the first three members of the well known homologous series of liquid crystalline terephthalylidine-anilines (TBAA-n).     

Crystal structure of marmesin,C14H14O4, 2-(β-hydroxyisopropyl)-2,3-dihydro-6,7-furano-coumarin

The unit cell parameters of this compound were determined by least-squares calculations from the adjusted angular setting of 25 general reflections. The crystals are monoclinic with the following crystallographic data: a = 5.718(1), b = 13.794(4), c = 7.861(1) Å, β = 100.53(2)°, Z = 2 and D_x = 1.34 g · cm⁻³. The space group according to the systematic absences is P2₁. The structure of this compound was solved by direct methods and refined by full matrix least-squares with anisotropic temperature factors to R = 0.04. The refined atomic positions indicate a considerable strain within the molecule. The structure is built up from molecules connected by H-atoms forming infinite chains along b-axis.     

14-Hydroxy-14-phenyldibenzo[a,j]xanthene as a lattice host: crystal and molecular structure of its (1:1) complex with diethyl ether

The title compound 14-hydroxy-14-phenyldibenzo[a,j]xanthene 1 formed a (1:1) complex with diethyl ether. 1,4-Dioxane was also enclathrated, but with a variable stoichiometric ratio. Single crystal X-ray crystallography was used to elucidate the crystal structure of the 1·diethyl ether complex. Crystals are orthorhombic with space group P2₁2₁2₁, a = 8.532(3), b = 15.040(4), c = 18.491(5) Å, V = 2373(1) ų, d _c = 1.256 g/cm³, and Z = 4. Host and guest molecules were found to associate via hydrogen bonds, with the guest molecules residing in undulating channels lined by host molecules.     

Crystal and molecular structure of (21R)-3β-acetoxy-14,21-epoxy-5β,14β-card-20(22)-enolide

The title compound (21R)-3β-acetoxy-14,21-epoxy-5β,14β-card-20(22)-enolide crystallizes in the monoclinic space group P2₁ with 2 formular units C₂₅H₃₄O₅ in the unit cell. The lattice parameters are a = 13.471, b = 7.959, c = 10.514 Å and β = 102.73°. The crystal structure was determined by direct methods and refined by least-squares procedures to the discrepancy factor R = 0.045. Bond length, bond angles, ring conformations and the configuration at C(21) were determined. Intermolecular interactions are only of van der Waals type.     

Crystal and molecular structure of 3β-hydroxy-5β-estr-8(14)-en-17-one

The title compound crystallizes in the orthorhombic space group P2₁2₁2₁ with 4 formula units C₁₈H₂₆O₂ in the unit cell. The lattice constants are a = 10.356(2) Å, b = 19.743(3) Å, and c = 7.487(1) Å. The structure was solved by direct methods of phases determination and refined by least-squares calculations to the conventional R = 0.054. The configuration and conformation of the molecule were determined and compared with those of Δ-8,14-anhydrodigitoxigenin.     

Crystal and molecular structure of (E)-21-Methoxycarbonyl-19-nor-pregna-4,8(14),20-trien-3-one

The crystal and molecular structure of the title compound has been determined by X-ray diffraction techniques. It crystallizes in the orthorhombic space group P 2₁2₁2₁ with cell parameters a = 12.662 Å, b = 17.995 Å, c = 8.433 Å. The structure was solved by direct methods using MULTAN-78 and refined by least-squares calculations to the conventional R = 0.061. The ring conformations of the steroid skeleton and the 17β-side chain conformation are discussed in detail.     

Crystal and molecular structure of (20R)-19-nor-5β,14β-pregnane-3β,14,20-triol 3,20-diacetate

The title compound (20R)-19-nor-5β,14β-pregnane-3β,14,20-triol 3,20-diacetate crystallizes in the monoclinic space group P2₁ with 4 formula units C₂₄H₃₈O₅ in the unit cell. The lattice parameters are a = 14.324, b = 12.569, c = 12.685 Å, β = 90.21°. The crystal structure was determined by direct methods and refined by the least-squares procedure to the discrepancy factor R = 0.042. Bond length, bond angles, ring conformations, as well as the absolute configuration at C20 were determined. In the crystal the molecules are linked to infinite chains by two hydrogen bonds.     

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).     

The emission and structure of a new laser crystal Nd3+: NaY(WO4)2

A new laser Nd³⁺ : NaY(WO₄)₂ crystal rod of Φ 2.5 × 5 mm was pumped by a xenon flash lamp, and a 1.06 μm laser output was for the first time obtained in our laboratory, which has a threshold lower than 1 J. The crystal structure of NaY(WO₄)₂ was determined. The crystal is tetragonal, with the space group 14₁/a, a = 5.205(2) Å, c = 11.251(3) Å, V = 304.8(2) ų, Z = 2, D_calc = 6.62 g/cm³, D_obs = 6.51 g/cm³.     

Ba2.2Ca0.8Mg4F14, a new “solid solution stabilized” matrix for an intense blue phosphor

Barium calcium magnesium fluoride (Ba₂(Ba_xCa_1‐x)Mg₄F₁₄, x=0.19‐0.26) has been synthesized at 850 °C from precursors prepared by the solution precipitation method. Single crystals with composition of Ba_2.200(2)Ca_0.800(2)Mg₄F₁₄were obtained after prolonged heating. Lattice parameters from single crystal data are a = 12.4203(8) and c = 7.4365(5) Å [tetragonal, space group P4₂/mnm (No. 136)]. They increase with increasing barium concentration within a given stability window. The structure is built of a network of MgF₆ octahedra forming a pyrochlore related channel system and isolated fluorine ions. Within the channels, heavy alkaline earth ions are located. The wide channel is filled with off‐center positioned barium ions. The channel with a narrow cross section hosts both ions, Ca²⁺and Ba²⁺. The structure is isotypic with Pb₃Nb₄O₁₂F₂ but has a different coordination around Ba/Ca and Pb, respectively. Doped with ∼1% Eu(II), the compound shows intense blue luminescence under UV activation. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal and molecular structure of 3-methoxy-estra-1,3,5(10)-triene-14β,17β-diol,C19H26O3

The crystal and molecular structure of 3-methoxy-estra-1,3,5(10)-triene-14β,17β-diol has been determined by single crystal X-ray analysis. It crystallizes in the orthorhombic space group P2₁2₁2₁ with cell parameters a = 8.965(2), b = 30.520(7), and c = 6.031(2) A. The structure was solved by the POSIT system and refined by least-squares calculations to the conventional R factor of 0.075. The steroid rings A, B, and C have planar, 7α, 8β-half chair, and chair conformations, respectively. The ring D is intermediate between 13α, 14β-half chair and 13α-envelope. Rings B and C are trans-fused, and rings C and D are cis-fused. There are intra- as well as intermolecular hydrogen bonds between both hydroxyl groups of the steroid molecule.     

Die Molekül- und Kristallstruktur des N-Methyl-piperidinium-acet-para-brom-anilid-jodid

N-Methyl-piperidinium-acet-para-bromo-anilide-iodide crystallizes in the triclinic space group P 1 with two formula units C₁₄H₂₀N₂OBrJ and two H₂O molecules in the unit cell. The lattice constants are a = 8.950 Å, b = 14.721 Å, c = 7.440 Å, α = 80.19°, β = 112.57° and γ = 106.82°. The molecular structure of the compound was determined by the X-ray structure analysis and the interaction between the molecules in the crystal was investigated. Especially the influence of the water in the crystal on the form of the molecule was analysed.     

Optical properties of Sr3TaGa3Si2O14 single crystal

The specific rotation ρ of strontium tantalum gallium silicate Sr₃TaGa₃Si₂O₁₄ (STGS) piezoelectric single crystal was determined from 350 to 850 nm by measuring the optical transmission between parallel polarisers in Z direction. It is shown that Sr₃TaGa₃Si₂O₁₄ has quite large a value of ρ which is a little smaller than that of strontium niobium gallium silicate Sr₃NbGa₃Si₂O₁₄ (SNGS). The crystal with ordered structure which is isostructural to calcium gallium germanate Ca₃Ga₂Ge₄O₁₄ (CGG) was grown by Czochraiski technique. And its birefringence was also determined. (© 2004 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

A new dabco templated metal sulfate, (C6H14N2)[Mn (H2O)6](SO4)2. Chemical preparation, hydrogen-bonded structure and thermal decomposition

The crystal structure of manganese sulfate templated by 1,4-diaza-bicyclo[2.2.2]octane (abbreviated dabco), (C₆H₁₄N₂)[Mn(H₂O)₆](SO₄)₂, was investigated using single crystal X-ray diffraction data. It crystallises in the monoclinic system (space group P2₁/c) with the following unit-cell parameters: a = 12.1392(2) ?, b = 12.3117(2) ?, c = 12.2765(2) ?, β = 104.607(1)°, V = 1775.47(5) ?³ and Z = 4. The structure has been solved using direct methods and refined by least-squares analysis [R ₁ = 0.0381, wR ₂ = 0.1082]. The crystal structure of the title compound is built from isolated [Mn(H₂O)₆]²⁺ octahedral cations, 1,4-diaza-bicyclo[2.2.2]octandiium cations (C₆H₁₄N₂)²⁺ and sulfate anions (SO₄)²⁻ connected by a three-dimensional hydrogen-bond network. The thermal decomposition of the precursor, studied by thermogravimetry and temperature-dependent X-ray powder diffraction, proceeds through four stages giving rise to the mixture of Mn₂O₃and Mn₃O₄. Supplementary Material CCDC 620298 contains the supplementary crystallographic data for this paper. These data can be obtained free of charge from The Cambridge Crystallographic Data Centre via www.ccdc.cam.ac.uk/data_request/cif.     

Imidazolium based ionic liquid crystals: structure,photophysical and thermal behaviour of [Cnmim]Br·xH2O (n = 12, 14; x=0, 1)

The long chain imidazolium halides [C_nmim]Br·xH₂O (n = 10, 12; x = 0, 1) have been synthesized and their structural and thermal behaviour together with their photophysical properties characterized. X‐ray structure analyses of the monohydrates ([C₁₂mim]Br·H₂O: triclinic, P1, no. 2, Z = 2, Pearson code aP112, a = 550.0(5) pm, b = 779.4(5) pm, c = 2296.1(5) pm, α = 81.89(5)°, β = 83.76(5)°, γ = 78.102(5)°, 3523 unique reflections with I_o > 2σ(I_o), R₁ = 0.0263, wR₂ = 0.0652, GooF = 1.037, T = 263(2) K; [C₁₄mim]Br•H₂O: triclinic, P1, no. 2, Z = 12, Pearson code aP11, a = 549.86(8) pm, 782.09(13) pm, c = 2511.3(4) pm, α = 94.86(2)°, β = 94.39(2)°, γ = 101.83(2)°, 2063 unique reflections with I_o > 2σ(I_o), R₁ = 0.0429, wR₂ = 0.0690, GooF = 0.770, T = 293(2) K) show for both compounds similar bilayered structures. Sheets composed of hydrophilic structure regions constituted by positively charged imidazolium head groups, bromide anions and hydrogen bonded water alternate with hydrophobic areas formed by interdigitated long alkyl chains belonging to imidazolium cations with different orientation. Combined differential scanning calorimetry and polarizing optical microscopy shows that the monohydrates as well as the anhydrous imidazolium salts are thermotropic liquid crystals which adopt smectic mesophases. The mesophase region is larger in case of the monohydrates when compared to the anhydrous compounds indicating that water obviously stabilizes the mesophase. All compounds show an intense whitish photoluminescence with short lived (¹π←¹π*) and long lived (¹π←³π*) transitions. (© 2008 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis and Crystal Structure of 2-Amino-4-(4-hydroxyphenyl)-5-propylthiazole Ethanol Solvate 0.25 Hydrate

Abstract  

2-Amino-4-(4-hydroxyphenyl)-5-propylthiazole was synthesized by the reaction of α-bromo-1-(4-hydroxyphenyl)-1-pentone with thiourea. The crystal structure of its ethanol solvate 0.25 hydrate, C₁₂H₁₄N₂OS···C₂H₅OH···0.25·H₂O, was determined by X-ray diffraction analysis. The crystal belongs to monoclinic system, space group C2/c with a = 20.9046(10), b = 10.1057(5), c = 30.0017(15) ?, β = 105.5850(10)°, Z = 8, M _r = 569.77, V = 6105.0(5) ?³, D _c = 1.240 g/cm³, μ = 0.214 mm⁻¹, F(000) = 2440, the final R = 0.0598 and wR = 0.1825 for 5,911 observed reflections [I > 2σ(I)]. Compound (1) is composed by two non-coplanar ring systems of phenol and thiazole. The structure displays extensive O–H···N, N–H···O and O–H···O intermolecular hydrogen bonds.     

Synthesis of a new dibenzo-14-crown-4 lariat ether and structure of its sodium perrhenate complex

A dibenzo-14-crown-4 ether with a novel monooxyacetone sidearm is prepared and its structure with sodium perrhenate is determined. The structure crystallizes in P2₁/c with cell dimensions: a = 8.107(2) Å, b = 28.138(3) Å, c = 10.293(2) Å, and = 104.173(9)°; giving a volume of 2276.6(7) ų. This structure is compared to other sodium complexes of dibenzo-14-crown-4 lariat ethers and is found to be the only one with intramolecular bonding between the sidearm and the cation. Possible reasons for this observation are discussed.     

Crystal structure of britvinite [Pb7(OH)3F(BO3)2(CO3)][Mg4.5(OH)3(Si5O14)]: A new layered silicate with an original type of silicon-oxygen networks

The crystal structure of a new mineral britvinite Pb_7.1Mg_4.5(Si_4.8Al_0.2O₁₄)(BO₃)(CO₃)[(BO₃)_0.7(SiO₄)_0.3](OH, F)_6.7 from the Lángban iron-manganese skarn deposit (V?rmland, Sweden) is determined at T = 173 K using X-ray diffraction (Stoe IPDS diffractometer, λMoKα, graphite monochromator, 2θ_max = 58.43°, R = 0.052 for 6262 reflections). The main crystal data are as follows: a = 9.3409(8) ?, b = 9.3579(7) ?, c = 18.8333(14) ?, α = 80.365(6)°, β = 75.816(6)°, γ = 59.870(5)°, V = 1378.7(2) ?³, space group P1, Z = 2, and ρ_calcd = 5.42 g/cm³. The idealized structural formula of the mineral is represented as [Pb₇(OH)₃F(BO₃)₂(CO₃)][Mg_4.5(OH)₃(Si₅O₁₄)]. It is demonstrated that the mineral britvinite is a new representative of the group of mica-like layered silicates with structures in which three-layer (2: 1) “sandwiches” composed of tetrahedra and octahedra alternate with blocks of other compositions, such as oxide, oxide-carbonate, oxide-carbonate-sulfate, and other blocks. The tetrahedral networks (Si₅O₁₄)_∞∞ consisting of twelve-membered rings are fragments of the britvinite structure. Similar networks also form crystal structures of the mineral zeophyllite and the synthetic phase Rb₆Si₁₀O₂₃. In the crystal structures under consideration, the tetrahedral networks differ in the rotation of tetrahedra with respect to the layer plane. Original Russian Text ? O.V. Yakubovich, W. Massa, N.V. Chukanov, 2008, published in Kristallografiya, 2008, Vol. 53, No. 2, pp. 233–242.     

Die Änderung der Molekül- und Kristallstruktur des N-Methyl-piperidinum-acet-meta-chlor-anilid-jodid durch Einlagerung von Wasser

N-Methyl-piperidinium-acet-meta-chloro-anilide-iodide crystallizes from water in the space group Pna2₁ with 4 formula units C₁₄H₂₀N₂OClJ and 4 H₂O molecules in the unit cell. The lattice constants are a = 12.413 Å, b = 19.798 Å and c = 6.919 Å. The change of the molecular conformation caused by water molecules was investigated by X-ray structure analysis.