Structure of monoclinic acridine orange hydrochloride monohydrate,C17H19N3 · HCl · H2O

M_r = 319.82, monoclinic P2₁/a, Z = 4, a = 14.545(5), b = 15.562(6), c = 8.538(4) Å, β = 120.66(3)°, V = 1662(1) ų, D_m = 1.27 Mgm⁻³, D_x = 1.278 Mgm⁻³, λ(MoKα) = 0.71069 Å, μ(MoKα) = 0.24 mm⁻¹, T = 297 K. Final R = 0.049 for 1485 observed reflections. All hydrogen atoms were located and refined isotropically. Bond lengths (σ = 0.004 Å) and angles (σ = 0.3°) are normal. The substance is a derivative of acridine. The structure consists of chloride anions, bisdimethylaminoacridinium cations and water molecules. In the solid state the molecules are approximately planar. Pairs of cations form dimers with parallel planes connected by an I inversion centre and plane distances of 3.474 Å. They overlap with partial areas of all three six membered rings.     

Configuration,conformation and crystal structure of rabdosianin b

Rabdosianin B, 7,20‐epoxy‐7β‐hydroxy‐1α,6β,11α,15β‐tetraacetoxy‐ent‐kaur‐16‐ene, C₂₈H₃₈O₁₀, was the first isolated from Isodon henryi. It consists of three six‐membered rings A, B, C and one five‐membered ring D. The fused‐ring system A, B and C are in chair, boat and chair conformations, respectively, and ring D is in an envelope conformation, on the basis of NMR and X‐ray diffraction analysis. The crystal of rabdosianin B is in orthorhombic crystal system with space group P2₁2₁2₁, lattice constants: a = 9.969(1) Å, b = 15.400(3) Å, and c = 17.624(3) Å, Z = 4. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

3 β ‐Acetoxy‐5 α ‐cholestan‐6‐one: A Steroid

The crystal and molecular structure of 3 β ‐Acetoxy‐5 α ‐cholestan‐6‐one has been determined by X‐ray crystallographic techniques. The compound crystallizes in the space group P2₁ with cell parameters : a = 13.060(3), b=6.299(2), c=17.152(6)Å; β =96.47(3)o, V = 1402.02ų, Z = 2, R = 0.072 for 1921 observed reflections. The six‐membered rings (A, B and C) exist in the chair conformations while the five‐membered ring‐d assumes half‐chair. All rings of the steroid skeleton are trans connected.     

Interaction in the molten system Rb2O‐P2O5‐TiO2‐NiO. Crystal structure of the langbeinite‐related Rb2Ni0.5Ti1.5(PO4)3

The interaction in the molten system Rb₂O‐P₂O₅‐TiO₂‐NiO was investigated at different molar ratios Rb/P = 0.5‐1.3, fixed Ti/P = 0.15, Ti/Ni = 1.0 at temperature range 1073–953 K. The conditions of formation of complex phosphates RbTi₂(PO₄)₃, Rb₂Ni_0.5Ti_1.5(PO₄)₃ and RbNiPO₄ have been determined. The new phosphate Rb₂Ni_0.5Ti_1.5(PO₄)₃ (space group P2₁3, a = 9.9386(2) Å) has been obtained and investigated by the single crystal X‐ray diffraction and FTIR‐spectroscopy. It has langbeinite‐like structure, that is built up from mixed (Ni/Ti)O₆‐octahedra and РО₄‐tetrahedra. Rubidium atoms are located in closed cavities of 3D‐framework.     

Crystal structure of N‐(2‐methoxyphenyl)‐3,6‐diphenyl‐1,4‐dihydro‐1,2,4,5‐tetrazine‐1‐carbonamide

The title compound, C₂₂H₁₉N₅O₂, was prepared and its structure was determined by X‐ray diffraction [CCDC 216074]. The compound crystallizes from ethanol in the orthorhombic system, space group P2₁2₁2₁, with unit cell parameters: a =10.048(1) Å, b = 13.935 (2) Å, c =14.607(2) Å, Z =4, and V=2045.3(5) ų. The crystal structure was solved by direct methods and refined by full‐matrix least‐squares to a final R‐value of 0.0516 with 3621 unique reflections. The central six‐membered ring of the compound has a boat conformation and is not homoaromatic, in which adjacent atoms N1 and N4 deviate from the plane of the ring by 0.4546(33) Å and 0.3786(33) Å, respectively. (© 2005 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.     

Crystal Structure of 1,2,3‐Tribromoindane,C9H7Br3

The title compound (C₉H₇Br₃) crystallizes in the triclinic space group with Z = 2; R = 0.043 for 1518 observed reflections [I = 2σ (I)]. The average Br‐C distance is 1.974 Å, Br‐C‐C angle is 110.0°. The five‐membered ring adopts a somewhat flattened structure. The atoms C1 and C3 have opposite configurations. The whole molecule has approximate (non‐crystallographic) C_s‐symmetry.     

The Crystal and Molecular Structure of 11,12‐dibromo‐ 7,8—benzo‐1,5‐di(p—tolylsulphonyl)‐1,5‐diazacyclononan

The crystal structure of the title compound, C₂₅H₂₆Br₂N₂O₄S₂ was determined by single crystal X‐ray diffraction technique. The crystals are monoclinic, space group C 2/c, with a=20.7142(2) Å b=11.7910(2) Å, c= 10.6735(3) Å, β=98.549(2)°, V=2577.94(9) ų, Z=4. The structure was solved by direct methods and refined by least‐squares methods to a final R=0.046 for 1866 observed reflections with I>2sigma(I). The title compound, displays disordered geometry around the C1 atom located almost on twofold axis. The nine‐membered heterocylic ring is close to the half‐chair conformation. The dihedral angle between phenyl rings is 34.2(1)°.     

Crystal structure,thermal and compositional deformations of β‐CsB5O8

The crystal structure of β‐CsB₅O₈ has been determined from X‐ray powder diffraction data using synchrotron radiation: Pbca, a = 7.8131(3) Å, b = 12.0652(4) Å, c = 14.9582(4) Å, Z = 8, ρ_calc = 2.967 g/cm³, R‐p = 0.076, R‐wp = 0.094. β‐CsB₅O₈ was found to be isostructural with β‐KB₅O₈ and β‐RbB₅O₈. The crystal structure consists of a double interlocking framework built up from B‐O pentaborate groups. The crystal structure exhibits a highly anisotropic thermal expansion: α_a = 53, α_b = 16, α_c = 14 · 10^‐6/K; the anisotropy may be caused by partial straightening of the screw chains of the pentaborate groups. The similarity of the thermal and compositional (Cs‐Rb‐K substitution) deformations of CsB₅O₈ is revealed: increasing the radius of the metal by 0.01 Å leads to the same deformations of the crystal structure as increasing the temperature by 35°C. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal and Molecular Structure of Desmodin

The crystal structure of the title compound has been determined from X‐ray diffraction. The compound crystallizes from benzene in the orthorhombic system, space group P2₁2₁2₁, with unit cell parameters: a = 8.485(2), b = 9.816(2), c = 22.597(4) Å, Z = 4, V = 1881.9(7) ų. The structure was determined by direct methods and refined to a final R‐factor of 0.04. Six membered rings B and E are planar. Ring A and ring C are in slightly distorted sofa conformation. Ring D is in envelope conformation. The structure is stabilised by weak intermolecular C‐H...O hydrogen bonds.     

Crystal and molecular structures of 11-hydroxy-7-oxodrim-8(9)-ene

The crystal structure of 11-hydroxy-7-oxodrim-8(9)-ene is determined. The crystals are monoclinic. The unit cell parameters are a = 16.716(4) Å, b = 11.052(3) Å, c = 7.542(3) Å, γ = 76.11°, Z = 4, μ = 1.476 cm⁻¹, ρ_calcd = 1.147 g/cm³, and space group P2₁. The structure is solved by the direct method and refined by the least-squares procedure to R = 0.045. There are two molecules of 11-hydroxy-7-oxodrim-8(9)-ene in the asymmetric unit. Both molecules have the same conformation of the skeleton and can be described as rotomers differing in orientation of the OH groups with respect to the skeleton. In both molecules, the cyclohexane rings have a usual chair conformation. In the crystal, two independent molecules are linked by a hydrogen bond. The molecular pairs related by the twofold screw axes are linked by hydrogen bonds into helices running along the z-axis of the crystal. The helices are bound through van der Waals interactions. __________ Translated from Kristallografiya, Vol. 45, No. 2, 2000, pp. 275–278. Original Russian Text Copyright ? 2000 by Chumakov, Simonov, Mazus, Popa, Vlad. Deceased.     

Synthesis,Crystal and Molecular Structure of 2‐Pyridylethanolbis(saccharinato)mercury(II)

2‐Pyridylethanolbis(saccharinato)mercury(II), [Hg(sac)2(pyet)], where sac and pyet are the saccharinate anion and the 2‐pyridylethanol molecule, respectively, crystallizes in the triclinic space group P (No. 2) with a = 10.4518(6), b = 11.3796(6) (5), c = 19.9945(12) Å, a = 102.758(3)° b = 98.146(3)°, g = 104.751(3)°, Z = 4, V = 2193.0(2) ų. The unit cell contains two crystallographically independent [Hg(sac)2(pyet)] units in which the mercury(II) ion is tetrahedrally coordinated by two nitrogen atoms of two sac ligands, and one nitrogen and one oxygen atoms of one neutral pyet ligands. The pyet acts as a bidentate N‐ and O‐donor ligand forming a six‐membered chelate ring, while sac behaves as a monodentate N‐donor ligand. The average bite angle of the pyet ligand is 75.8(5)°. The Hg‐N_sac bond distances are in the range 2.0874(18) and 2.1931(18) Å, whereas the Hg‐N_pyet and Hg‐O_pyet bond distances are 2.2452(19)‐2.3202(19) and 2.6036(17)‐2.5902(16) Å, respectively. The crystal exhibits two strong hydrogen bonds between the hydroxyl O atom of pyet and sulfonyl O atoms of sac and the C‐H…O type weak hydrogen bonds between H atoms of the aromatic rings of the pyet and the sulfonyl O atoms of the sac ligands. Furthermore, packing of the molecules in the solid‐state results in aromatic π‐π interactions associated with the aromatic rings of sac‐sac and py‐py.     

Synthesis,characterization and crystal structure of a novel Ni(II) coordination polymer with dipyrido[3,2‐a:2′,3′‐c]phenazine and 4,4′‐oxy(bisbenzoate)

A novel coordination polymer, [Ni(dppz)(oba)(H₂O)]·0.5H₂O (dppz = dipyrido[3,2‐a:2′,3′‐c]phenazine and oba = 4,4′‐oxy(bisbenzoate)) has been synthesized through hydrothermal method and characterized by IR, and single‐crystal X‐ray diffraction. It crystallizes in monoclinic, space group C2/c with a = 23.163(5), b = 18.211(4), c = 14.460(3) Å, α = γ = 90°, β = 100.45(3)°, V = 5998(2) ų, Z = 2. The structure was solved by direct methods and refined to R = 0.0866 (wR₂ = 0.1836). The compound exhibits interesting one‐dimensional chain structures, which are further stacked through π‐π interactions to form supramolecular double chains. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis and characterization of a layered chlorozincophosphate templated by protonated 4‐methylpiperidine

A chlorozincophosphate with the composition Zn(HPO₄)Cl·[C₆H₁₄N] has been synthesised under mild conditions in water medium in presence of 4‐methylpiperidine as organic template. The structure was determinated by single crystal X‐ray diffraction. The unit cell is orthorhombic (space group Pcab) with a = 8.743(9), b = 9.592(6), c = 26.573(6) Å, Z = 8 and V = 2228.91(12) ų. The structure involves a network of ZnO₃Cl and PO₃(OH) tetrahedra forming macroanionic inorganic layers with four and eight‐membered rings. Charge balance is achieved by the protonated amine which is trapped in the interlayers space and interacts with the organic framework through hydrogen bonding. Solid state ³¹P and ¹³C MAS‐NMR spectroscopies are in full agreement with the X‐ray structure. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Si modified Ge10 cluster: the preparation and characterization of single crystal Na4(Ge,Si)9O20

A Si modified Ge₁₀ cluster with structure Na₄(Ge,Si)₉O₂₀ (denoted as HUT‐1) was synthesized by hydrothermal synthesis at 160 °C with a sodium silicate source. The compound was characterized by single crystal, powder X‐ray diffraction and TGA‐DSC analysis. HUT‐1 crystallizes in space group I4₁ (80) with calculated unit cell (a=14.966(5) Å, c=7.343(2) Å, V=1644.8(9) ų), which has the same structure as Na₄Ge₉O₂₀. HUT‐1 has a high Si/Ge ratio with an approximate formula of Na₄Ge_7.68Si_1.32O₂₀. Single crystal X‐ray structure refinements together with results from X‐ray powder diffraction (XRPD) confirm the occupancy of Si at two tetrahedral sites. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Powder study of propanthioamide dervative C8H6N2S2

The crystal structure of 2‐cyano‐3‐(2‐thienyl)prop‐2‐enethioamide (C₈H₆N₂S₂), a propanethioamide derivative was solved from high resolution laboratory X‐ray powder diffraction data collected at ambient conditions. Structure determination was performed by means of the global optimization method of simulated annealing at a resolution of 1.5 Å. Rietveld refinement yielded an R_WP value of 4.02% (P2₁/a, a = 15.8174(2) Å, b = 5.6502(1) Å, c = 11.0952(1) Å, β = 116.9923(7)°, V = 883.6(5) ų, Z = 4). The molecules are stacked in parallel layers and are stabilized by hydrogen bonds. (© 2009 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

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.     

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)     

Synthesis and structure of the three‐dimensional coordination polymer [Ag3hmt3(μ3 ‐btc)]·5H2O

A new coordination polymer, [Ag₃hmt₃(μ₃ ‐btc)]·5H₂O (1) (hmt = hexamethylenetetramine, btc=1,3,5‐benzenetricarboxlic), has been successfully synthesized. Crystal data: P2₁/a, a = 11.9906(2) Å, b = 17.3689(2) Å, c = 16.96100(10) Å, β = 101.9820(14)°, V = 3455.40(7) ų, Z = 4, Dc = 2.002 Mg/m³. In the hexagonal structure of Ag‐hmt unit, each Ag‐hmt unit comprises three Ag atoms and three hmt ligands. The μ₃ ‐btc ligands bridge adjacent two‐dimensional honeycomb‐like Ag‐hmt layers to form three‐dimensional networks. Structure analysis show that hydrogen bonds play a key role for the stable structure in the compounds. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

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)