Crystal and molecular structure of 10,20-epoxy-grayanotoxin-II

The photooxidation with HgO in benzene and the hydrolysis with 2%-KOH in methanol of the grayanotoxin (GTX) derivative (4) gave a 10,20-epoxy-grayanotoxin-II(5). The crystal structure of (5) has been determined by X-ray diffraction at room temperature. The crystal is monoclinic, space group P2₁, with a = 14.248(10) Å, b = 6.670(10) Å, c = 9.990(10) Å, = 105.507(8)°, V = 914.9(2) ų, Z = 2. The structure was solved by direct methods and refined by full-matrix least squares methods to a final R1 = 0.046 (wR2 = 0.0833) for 1161 independent reflections. The molecule has a pentacyclic structure consisting of two five-membered, one six-membered, one seven-membered, and one three-membered rings. The three-membered ring is connected with the seven-membered ring by spiro-type bond.     

X-ray crystal structure of cytochalasin D produced by Tubercularia sp., a novel endophytic fungus of Taxus mairei

The crystal structure of cytochalasin D, which was isolated from Tubercularia sp., a novel endophytic fungus of Taxus mairei, and cocrystallized with dimethyl sulfoxide, is reported. The title compound crystallizes in the monoclinic space group P2₁, with a = 7.583(6) Å, b = 11.053(10) Å, c = 18.632(10) Å, = 95.79(6)°, V = 1553.6(3) ų, Z = 2. The structure was solved by direct methods and refined by least-squares methods to a final R factor of 0.103 for 2937 independent reflections.     

Crystal and molecular structure of 6-0-acetylgrayanotoxin III

The crystal and molecular structure of a grayanotoxin III derivative, 6-0-acetylgrayanotoxin III is presented. The crystal is orthorhombic, space group P2₁2₁2₁, witha=15.582(3),b=21.304(3),c=6.339(3)Å,V=2104(1) ų Z=4. The structure was solved by direct methods and refined by full matrix least-squares methods to a finalR=0.047 for 1763 independent reflections withF ₀>3 (F ₀) The molecule is based on a tetracyclic structure consisting of two five-membered, one six-membered, and one seven-membered ring with various conformations.     

Synthesis, crystal structures, and properties of copper complexes with tripodal ligands and azide anion

Two new Cu^II complexes, (CuL¹N₃)ClO₄ (1) and (CuL²N₃)ClO₄ (2), have been synthesized and characterized in the presence of NaN₃, where L¹ = tris[2-(6-methylpyridyl)methyl]amine and L² = tris[(3,5-dimethylpyrazol-l-yl)methyl]amine, and their crystal structures have been determined by X-ray diffraction methods. Compound 1 crystallizes in the triclinic space group P–1, with a = 8.258(2) Å, b = 11.481(2) Å, c = 14.158(3) Å, = 72.30(3)°, = 79.05(3)°, = 86.08(3)°, V = 1255.4(5) ų. Compound 2 crystallizes in the monoclinic space group C2/c, with a = 26.752(2) Å, b = 10.561(2) Å, c = 21.059(4) Å, = 120.51(3)°, V = 5126(3) ų. In both compounds, each Cu^II center is in a distorted trigonal–bipyramidal coordinated environment with four nitrogen atoms from the tripodal ligand and one nitrogen atom from the azide group. The coordination geometry around Cu^II center of 1 is axially compressed trigonal bipyramid, while that of 2 is an axially elongated trigonal bipyramid. The coordinated azide group is in the axial site in both complexes. A quasi-dimeric structure of 1 has been formed in the unit cell through hydrogen bonding. The electronic spectra of two complexes in solution have been further studied by UV–vis technique, and the coordination properties have been discussed.     

The preparation and crystal structures of some tricarbonylmanganese(I) octahedral complexes containing the 1,1-dimethylamino-2,2-diphenylphosphinoethane ligand

Four new complexes of (pn) the titled ligand have been prepared and characterized: (CO)₃Mn(pn)Br, 1; (CO)₃Mn(pn)N₃, 2; the triazalato (tz) complex, (CO)₃Mn(pn)(tz), 3 and [(CO)₄Mn(pn)]BF₄, 4. Crystal structures for the first three of these were determined. Crystal data for 1, monoclinic crystal system, space group = C2, a = 17.8587(6) Å, b = 7.9611(3) Å, c = 14.2349(4) Å, = 90.281(1)°, V = 2023.82(12) ų, Z = 4; for 2, monoclinic crystal system, space group = P2₁/c, a = 8.8933(14) Å, b = 13.844(2) Å, c = 16.361(3) Å, = 95.712(3)°, V = 2004.4(6) ų, Z = 4; for 3, orthorhombic crystal system, space group = Pbca, a = 17.9097(4) Å, b = 13.1308(4) Å, c = 21.2838(6) Å, V = 5005.3(2) ų, Z = 8.     

Synthesis and crystal structure of a nickel(II) complex involving imino nitroxide radicals

A new complex of formula [Ni(im2-py)₂(SCN)₂]CH₃OH (im2-py = 2-(2-pyridyl)-4,4,5,5-tetramethylimidazoline-1-oxyl) has been synthesized and the crystal structure determined by X-ray diffraction methods. The complex crystallizes in the monoclinic space group P2₁/n with a = 15.525(5) Å, b = 13.405(4) Å, c = 16.167(5) Å, = 113.324(5)°, V = 3089.6(16) ų, and Z = 4. The structure of this complex is mononuclear with the nickel(II) ion octahedrally coordinated and bound to the imino nitroxide radicals through the imino nitrogen atoms. The thiocyanate groups are coordinated to the metal by the nitrogen atoms.     

Crystal structure of 1-chloroanthraquinone

The X-ray crystal structure of 1-chloroanthraquinone is determined. The compound C₁₄H₇O₂Cl, is monoclinic in P2₁(#4) with a = 7.763(1), b = 3.973(2), c = 16.947(1) Å, = 95.13(1)°, V = 520.6(3) ų, D _calc = 1.548 g/cm³, and Z = 2. In the molecular structure, the Cl atom is obviously repelled by O(1). The major force of crystal formation comes from aromatic ring stacking and C–H-aromatic interaction.     

Crystal structure, thermal analysis, and IR spectrometric investigation of bis(tert-butylammonium) sulfate

Chemical preparation, X-ray single crystal, thermal analysis, and IR spectrometric investigation of (C₄H₁₂N)₂SO₄, denoted tBAS, are described. The compound crystallizes in the monoclinic system with C2/c space group. Its unit cell dimensions are a = 11.1585(5) Å, b = 6.2148(4) Å, c = 20.070(1) Å, = 102.004(4)°, V = 1361.4(1) ų, and Z = 4. The crystal structure of tBAS can be described as a typical thick layered organization built by all the components of the structure and centered by planes z = 1/4 and 3/4. Connection in these layers are established by N—H···O hydrogen bonds. Thermal analysis shows a reversible weak phase transition.     

Synthesis, crystal structure, and thermal analyses of triaqua-(1,10-phenanthroline-N,N′) succinatomanganese(II) dihydrate, [Mn(H2O)3(phen)(C4H4O4)]·2H2O

[Mn(H₂O)₃(phen)(C₄H₄O₄)]·2H₂O was obtained by reaction of freshly prepared MnCO₃, phen and succinic acid in CH₃OH/H₂O (1:1 v/v), and its crystal structure has been determined by single crystal X-ray diffraction methods. The title mixed ligand complex crystallizes in the triclinic space group with cell dimensions a = 7.590(1) Å, b = 9.324(1) Å, c = 13.917(1) Å, = 85.64(1)°, = 74.56(1)°, = 77.10(1)°, and D _calc = 1.584 g/cm³ for Z = 2. The crystal structure consists of the [Mn(H₂O)₃(phen)(C₄H₄O₄)] complex molecules and lattice H₂O molecules. The Mn atoms are each octahedrally coordinated by two N atoms of one phen ligand and four O atoms of three H₂O molecules and one succinato ligand with d(Mn—N) = 2.271 and 2.299 Å, and d(Mn—O) = 2.133–2.239 Å. Through intermolecular hydrogen bondings, the complex molecules are interlinked to form 2D layers, which are assembled by – stacking interactions into 3D framework with tunnels occupied by the lattice H₂O molecules. Thermal analyses showed that the title compound decomposes in two steps over the range 25–600°C upon heating in flowing Ar.     

Crystal structure of a salt of the pyridinium-pyridine ion by X-ray and neutron diffraction

The crystal structure of [(C₅H₅N)₂H]⁺[ZnBr_3/2Cl_3/2(C₅H₅N)]^– has been determined and refined by full-matrix least-squares methods using X-ray (R, on ¦F _o¦, = 0.045 with 2291 reflections) and neutron (¯R, on ¦F _o¦, = 0.035 with 2030 reflections) diffraction data. The crystals of the compound are monoclinic, space groupP2₁/c witha = 12.728(1),b = 11.600(1),c = 13.354(1) Å, = 107.38(1) °,Z = 4,D _x = 1.68, andD _m(flotation) = 1.69 g cm^–3. The X-ray and neutron intensities were measured by the counter -2 scan technique with CuK X-rays ( = 1.5418 Å) and neutrons with = 1.109 Å, respectively. An intramolecular N--H hydrogen bond holds pairs of pyridine molecules together in the lattice [N N, 2.737(3) Å]. The hydrogen atom is very asymmetrically disposed with N-H distances of 1.086(7) Å and 1.658(6) Å. The coordination about the zinc atom is tetrahedral with the nitrogen atom of the pyridine molecule in one tetrahedral position and different mixtures of the two halogen atoms in the other three positions. The important average bond distances from the neutron study are Zn-N [2.073(3) Å], Zn-Cl [2.251(2) Å], Zn-Br [2.394(3) Å], N-C [1.334(5) Å], C-C [1.378(5) Å], and C-H [1.075(7) Å].     

Synthesis and crystal structure of 3,5-di(2-propenyl)-6-phenyl-1,3,5-triazine-2,4-dione and 2-dimethylamino-4-ethoxycarbonylmethoxy-6-phenyl-1,3,5-triazine

The title compound 3,5-di(2-propenyl)-6-phenyl-1,3,5-triazine-2,4-dione has been synthesized by the reaction of 6-phenyl-1,3,5-triazine-2,4-dione with allyl bromide. Its structure was determined by X-ray single crystal diffraction. The crystal belongs to orthorhombic, space group Pbca with the following crystallographic parameters: a = 16.282(4) Å, b = 8.888(2) Å, c = 19.281(5) Å, = 90°, = 90°, = 90°, = 0.088 mm^–1, V = 2790.1(13) ų, z = 8, Dx = 1.282 mg/m³, F(000) = 1136, T = 293(2) K, 2.11° 25.02°, the final R factor: R ₁ = 0.0430, wR₂ = 0.0981. The X-ray results demonstrate that the reaction of 6-phenyl-1,3,5-triazine-2,4-dione with allyl bromide in the presence of N,N-dimethylformamide and potassium carbonate yields the N-alkylated product. The title compound 2-dimethylamino-4-ethoxycarbonylmethoxy-6-phenyl-1,3,5-triazine has been synthesized by a new reaction, in which the solvent N,N-dimethylformamide involves. Its structure was determined by X-ray single crystal diffraction. The crystal belongs to triclinic, space group P-1 with the following crystallographic parameters: a = 7.977(2) Å, b = 10.394(3) Å, c = 10.837(3) Å, = 111.774(5)°, = 104.050(5)°, = 99.446(5)°, = 0.093 mm^–1, V = 776.6(4) ų, z = 2, Dx = 1.293 mg/m³, F(000) = 320, T = 293(2) K, 2.14° 25.03°, the final R factor: R ₁ = 0.0582, wR ₂ = 0.1399. The distance of N(4) C(2) (1.339 Å) is much shorter than the length of normal C N (1.47 Å) and very close to that of C-N (1.33 Å), which is indicative of the significant double bond character.     

Crystal structure of benzimidazolium dichromate

The X-ray crystal structure of benzimidazolium dichromate is determined. The compound C₁₄H₁₄Cr₂N₄O₇ is Triclinic in P-1 with a = 8.2722(8) Å, b = 10.0269(10) Å, c = 11.7001(11) Å, = 102.073(2)°, =100.483(2)°, = 67.288(2)°, V = 869.88(15) ų, D _calc = 1.734 g/cm³, and Z = 2. A dichromate ion connects two benzimidazolium rings via hydrgen bonds, as leads to face-to-face intramolecular aromatic stacking. The major force of crystal formation comes from hydrogen bonds, and an intermolecular hydrogen bridge is formed to connect two neighbored dichromate ions.     

Crystal and molecular structure of dihydro-8b,8c-diphenyl-1H,3H,4H,5H,7H,8H,-2,6-dioxa-3a,4a,7a,8a-tetraazacyclopenta[def]fluorene-4,8-dithione

The title compound C₂₀H₁₈N₄O₂S₂ crystallizes in the monoclinic space group P2₁/n witha=8.4930(1) Å,b=11.4880(1) Å,c=20.0709(2) Å, =94.933(1)°,V=1951.01(3) ų,Z=4. The crystal structure has been solved by vector search methods and refined by fullmatrix least-squares toR=0.04 for 2888 reflections and 116 restraints. The title compound has a suitable geometry for synthesizing receptor molecules with a cleft for selective complexation.     

Tetra-n-butylammonium bromide-thiourea (1/2), a layer-type inclusion compound

The inclusion compound built of tetra-n-butylammonium bromide-thiourea (1/2), [(n-C₄H₉)₄N⁺Br^– 2(NH₂)₂CS], has been prepared and characterized by X-ray crystallography. The compound crystalline in orthorhombic space group Pbca, with a = 16.872(6) Å, b = 17.214(6) Å, c = 18.561(6) Å, V = 5390(3) ų, Z = 8. The compound features a sandwich-like crystal structure built up from planar layers. In the crystal structure, zigzag hydrogen-bonded thiourea ribbons are linked by bromide anions to generate puckered layers matching the (100) planes, and the (n-C₄H₉)₄N⁺ cations occupy the intervening space.     

The crystal structure of a N-(2-thiophenyl)-salicylaldiminopiperidino nickel(II) complex

The crystal and molecular structure of the title complex, C₁₈H₁₉N₂OSNi, has been determined by direct methods. The compound crystallizes in monoclinic crystal system witha=11.968(1),b=12.182(1),c=12.399(1) Å, =115.23(1)°, space group P2₁/n. Nickel is in a slightly distorted square-planar environment of two nitrogens [1.881(2) and 1.952(2) Å] and one oxygen [1.856(3) Å] and one sulphur [2.138(2) Å] atom. Ni is 0.005 Å out of the plane of its ligands.     

Crystal structure of quinoline-2-carboxylic acid ⋅ quinolinium-2-carboxylate

Quinoline-2-carboxylic acid (quinaldic acid), C₁₀H₇NO₂, crystallizes in the monoclinic space group P2₁/c, a =9.724(1) Å, b = 5.937(1) Å, c = 27.545(2) Å, = 90.15(1)°, z = 4, and occurs in the crystal in two tautomeric forms: the neutral molecule and the zwitterion, with molecular ratio 1:1. The compound can be named quinoline-2-carboxylic acid quinolinium-2-carboxylate. The crystal structure is built up of tautomeric pairs consisting of C₉H₆NCOOH and C₉H₆NH⁺COO^– moieties, held up together by hydrogen bonds.     

Crystal structures of a series of 3,7-bis-(arylazo)-1,3,5,7-tetraazabicyclo[3.3.1]nonanes

The crystal and molecular structure of a series of 3,7-bis(arylazo)-1,3,5,7-tetraazabicyclo[3.3.1] nonanes (1a–d) have been determined by single crystal X-ray diffraction analysis. All four compounds have the same feature, that the tetraazabicyclononane unit assumes a cage-like structure with the aryltriazene moieties lying parallel to one another so that the aryl rings are held together by – stacking. Crystal data: 1a C₁₇H₁₈N₁₀O₄, triclinic, space group P – 1, a = 9.8899(10), b = 13.0845(13), c = 16.458(2) Å, = 94.095(2)°, = 107.004(2)°, = 111.027(2)°, V = 1863.5(3) ų and Z = 4; 1b, C₁₉H₁₈F₆N₈, orthorhombic, space group Pbca, a = 15.3210(8), b = 10.9512(6), c = 24.5698(13) Å, V = 4122.4(4) ų and Z = 8; 1c C₁₉H₁₈N₁₀, monoclinic, space group P2₁/n a = 6.3742(6), b = 13.7343(13), c = 21.542(2)Å, = 97.738(2)°, V = 1868.8(3) ų, and Z = 4; 1d, C₁₉H₁₈N₁₀, monoclinic, space group P2₁/c, a = 18.205(2), b = 17.398(2), c = 12.784(12) Å, = 109.480(2)°, V = 3818.0(6) ų, and Z = 8.     

Crystal and molecular structures of tin(IV) dithiocarbamates: II. Tris (N,N-diethyldithiocarbamato) methyltin(IV), a seven-coordinated pentagonal bipyramidal complex

The crystal structure of the title compound has been determined from 2919 independent reflections measured by scintillation methods. The crystals are monoclinic, space groupP2_1/n , with cell parametersa = 10.041(3),b = 10.712(4),c = 24.295(7) Å, = 93.17(5), andZ = 4. The structure was solved by Patterson and Fourier techniques, and refined by full-matrix least-squares methods toR = 0.058. The crystal structure consists of discrete, neutral, mononuclear, seven coordinated tin complexes. The geometry around the tin is a distorted pentagonal bipyramid with the methyl group axial, two dithiocarbamate ligands equatorial, and one dithiocarbamate bridging axial-equitorial. For the equatorial dithiocarbamates, each ligand has a short Sn-S distance [2.618(2) Å] and a longer Sn-S distance [2.761(12) Å]. For the other dithiocarbamate ligand there is a short axial Sn-S distance [2.481(2) Å] and a long equatorial Sn-S distance[2.817(2) Å]. The Sn-C distance has a rather normal value of 2.148(8) Å.     

Crystal structure and conformation of the antimalarial drug 5,7-methoxy-8-(3-methyl-1-buten-3-ol)-coumarin

The crystal and molecular structure of the antimalarial compound 5,7-methoxy-8-(3-methyl-1-buten-3-ol)-coumarin, C₁₆H₁₈O₅, M _r = 290.3 Da, has been determined from X-ray diffraction data. The material crystallizes in the monoclinic space group P2₁/c with 4 molecules per unit cell of dimensions a = 8.9044(9), b = 17.623(1), c = 10.175(1) Å, = 113.97(1)°, crystal density D _c = 1.322 g/cm³. The structure was determined using direct methods and refined by full-matrix least squares to a conventional R index of 0.066 for 2416 measured reflections and 206 parameters.The coumarin ring system is almost planar with the methoxy C atoms rotated slightly out of the coumarin mean plane. Apart from the terminal CH₃ groups C(12) and C(13), which are 1.184(3) Å above and –1.315(3) Å below the plane, the 3-methyl-1-buten-3-ol substituent is planar (rms deviation 0.009 Å) making an angle of 6.31(7)° with the phenyl ring. One intermolecular hydrogen bond is present in the crystal structure between O(5)–HO(5) and the symmetry related O(2) oxygen, generated by the symmetry operation (x, 1/2 – y, –1/2 + z).     

Design, synthesis, and structure of novel cesium receptors

The podand, bis(2-methoxyphenoxy)m-xylene (1), was designed and synthesized as a potential host for the cesium ion. Its structure was determined by single crystal X-ray diffraction. It crystallizes in P2₁/c with cell dimensions: a = 8.5723(7) Å, b = 8.3931(14) Å, c = 25.2879(26) Å, = 96.224(9), and V = 1808.7(4) ų. A crown derivative, tribenzo-21-crown-6 (2), was also prepared and structurally characterized. It also crystallizes in P2₁/c with cell dimensions: a = 15.5825(13) Å, b = 15.8648(16) Å, c = 8.8266(7) Å, = 95.247(6), and V = 2172.9(3) ų. The structures exhibit hydrogen bonding, and are evaluated in terms of complementarity and preorganization for cesium binding.