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Crystal System (crystal + system)
Kinds of Crystal System Selected AbstractsYarlongite: A New Metallic Carbide MineralACTA GEOLOGICA SINICA (ENGLISH EDITION), Issue 1 2009Nicheng SHI Abstract: Yarlongite occurs in ophiolitic chromitite at the Luobusha mine (29°5,N 92°5,E, about 200 km ESE of Lhasa), Qusum County, Shannan Prefecture, Tibet Autonomous Region, People's Republic of China. Associated minerals are: diamond, moissanite, wüstite, iridium ("osmiridium"), osmium ("iridosmine"), periclase, chromite, native iron, native nickel, native chromium, forsterite, Cr-rich diopside, intermetallic compounds Ni-Fe-Cr, Ni-Cr, Cr-C, etc. Yarlongite and its associated minerals were handpicked from a large heavy mineral sample of chromitite. The metallic carbides associated with yarlongite are cohenite, tongbaite, khamrabaevite and qusongite (IMA2007,034). Yarlongite occurs as irregular grains, with a size between 0.02 and 0.06 mm, steel-grey colour, H Mohs: 5½,6. Tenacity: brittle. Cleavage: {0 0 1} perfect. Fracture: conchoidal. Chemical formula: (Cr4Fe4Ni),9C4, or (Cr,Fe,Ni),9C4, Crystal system: Hexagonal, Space Group: P63/mc, a= 18.839(2) Å, c= 4.4960 (9) Å, V= 745.7(2) Å3, Z= 6, Density (calc.) = 7.19 g/cm3 (with simplified formula). Yarlongite has been approved as a new mineral by the CNMNC (IMA2007,035). Holotype material is deposited at the Geological Museum of China (No. M11650). [source] Configuration, conformation and crystal structure of rabdosianin bCRYSTAL RESEARCH AND TECHNOLOGY, Issue 8 2005Bao Lin Li Abstract Rabdosianin B, 7,20-epoxy-7,-hydroxy-1,,6,,11,,15,-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) [source] Characterization of Lead Precipitate Following Uptake by Roots of Brassica junceaENVIRONMENTAL TOXICOLOGY & CHEMISTRY, Issue 11 2009Donald E. R. Meyers Abstract Seedlings of Brassica juncea (L.) Czern. were grown in solution culture for 14 d prior to exposure to Pb2+ at an activity of 31 ,M for 72 h. Electron-dense deposits found within the apoplast and symplast were analyzed using scanning transmission electron microscopy/energy dispersive spectroscopy to determine the chemical identity of the deposits and potential toxicity resistance mechanisms. Irrespective of the cellular compartment in which they were found, the deposits contained Pb, O, P, and Cl. For the extracellular deposits, the average Pb:P:O atomic ratio was 1:0.54:3.0, which together with the hexagonal crystal system suggests that Pb is present as chloropyromorphite (Pb5(PO4)3Cl). A weak Ca signal also was detected in approximately half of the spectra, possibly indicating the presence of small concentrations of phosphohedyphane (Pb3Ca2(PO4)3Cl). The evidence suggests that B. juncea resists Pb toxicity by storing precipitated Pb in the vacuole. [source] Highly Symmetrical Tetranuclear Cluster Complexes Supported by p - tert -Butylsulfonylcalix[4]arene as a Cluster-Forming LigandEUROPEAN JOURNAL OF INORGANIC CHEMISTRY, Issue 9 2006Takashi Kajiwara Abstract Square-planar tetranuclear clusters [M4(L)(AcO)4(,4 -OH)], (M = MnII, CoII, and NiII) are synthesized using tetra-anionic p - tert -butylsulfonylcalix[4]arene (L4,) as a cluster-forming ligand. Three complexes are crystallographically isostructural, being crystallized in the triclinic crystal system with space group P. The calix[4]arene acts as a tetrakis fac -tridentate ligand through four phenoxo and four sulfonyl oxygen atoms to form square arrangement of four metal ions, which are further bridged by four chelating acetate ions and one hydroxo ion in a ,4 manner to complete the hexacoordination of each metal center. Although the whole molecule of each complex is crystallographically independent, the molecule is highly symmetrical with a pseudo-four-fold axis lying on the ,4 -OH, group. The tetranuclear clusters are stable enough to maintain the core structures even in highly dilute solution (,10 ,M), which was confirmed by mass spectroscopic study, however, bridging acetates were easily exchanged by other carboxylate chelates to form derivatives such as [M4(L)(BzO)4(OH)],. Metal,metal interactions were investigated by means of magnetic susceptibility, and it was revealed that both ferro- and antiferromagnetic interactions occur in the NiII complex depending on the bridging angles of Ni,O,Ni. (© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2006) [source] Advances in space-group determination from powder diffraction dataJOURNAL OF APPLIED CRYSTALLOGRAPHY, Issue 4 2007Angela Altomare The space-group determination process by powder diffraction data is not straightforward. The low accuracy of the reflection intensities may invalidate the calculation of the probability associated to each extinction group that is compatible with the crystal system determined in the indexation step. Here the combination of the z statistics with two new algorithms is reported: the first checks the quality of each 2, interval in order to omit doubtful z estimates from the calculations; the second creates a list of reflections with peaks that weakly overlap with any other peak, in order to check if any of them violates the extinction rules of the extinction symbol. The new approach has been applied to a large set of test structures and proved to be much more efficient than the procedure based only on the z statistics. [source] Synthesis of processible doped polyaniline-polyacrylic acid compositesJOURNAL OF APPLIED POLYMER SCIENCE, Issue 2 2009Bhavana Gupta Abstract Processible composites of emeraldine salt form of polyaniline (PANI) with polyacrylic acid (PAA) are synthesized and studied for their structural, electrical, mechanical, thermal, and electrochemical properties. The processible conducting composites of various weight percentage from 20 wt % to 90 wt % (of PANI) have been prepared by mixing the PANI and PAA under vigorous stirring and sonication conditions. Self-standing films of electroactive homogeneous composites are obtained by solution casting method. A significant improvement in processibility, crystallinity, and thermal stability is observed in the composites; however, the electrical conductivity decreased remarkably as the percentage of PANI is decreased in the composites. The 60 wt % PANI-PAA composite showed crystalline structural property with orthorhombic crystal system and cell parameters as a = 5.93Å, b = 7.57Å, and c = 10.11Å. The 60 wt % PANI-PAA composite also showed better thermal stability and highest capacitance amongst all the composites and used as an active material for development of electrochemical capacitors (parallel plate assembly). The processible composites based electrochemical capacitors using 0.5 M NaClO4 -Acetonitril electrolyte showed super capacitance with ease in fabrication and cost effectiveness in comparison to other similar materials based capacitors. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2009 [source] On the purity of 2-[ortho -anilinyl]-1,3-benzoxazole derived from 2H -3,1-benzoxazine-2,4(1H)dione (isatoic anhydride) [1,2],JOURNAL OF HETEROCYCLIC CHEMISTRY, Issue 2 2010Karen M. Button The Lewis acid catalyzed synthesis and chromatographic purification of isatoic anhydride-derived 2-(2,-anilinyl)-1,3-benzoxazole (2) can result in the co-isolation of 2 and a light pink colored impurity (<5%). This latter species has been identified (NMR, single crystal X-ray diffraction, mp) as 2,-hydroxy-2-aminobenzanilide (3), which represents a predictable intermediate in the formation of 2. Compound 3 crystallizes in an orthorhombic crystal system of space group P212121 with four molecules in the unit cell (, = , = , = 90°; a = 6.715 (2) Å, b = 12.100 (4) Å, c = 13.321 (4) Å; V = 1082.2 (6) Å3). Pure 2 is characterized as a colorless, high-melting solid; unlike the dark colored oil that is isolated if 2 contains traces of 3. J. Heterocyclic Chem., (2010). [source] Manipulation of crystal shape by cycles of growth and dissolutionAICHE JOURNAL, Issue 6 2007Ryan C. Snyder Abstract A method for the manipulation of crystal shape by using cycles of growth and dissolution is presented, representing a unique process-based solution to an important product quality concern. Using 3-D shape evolution models for faceted crystal growth and dissolution, results are reported for cycling both an illustrative crystal system, as well as a physical plate-like system. The results show that crystal shape can be manipulated by cycling when the relative growth and dissolution rates are anisotropic, which can be caused by differences in growth mechanism, asymmetry in super/undersaturation, and by the use of surface active additives. Since this method of crystal shape enhancement uses the existing liquid solution, it could be a valuable alternative to the traditional methods which often require changes in the chemical nature of the solution, for example, by changing solvent. © 2007 American Institute of Chemical Engineers AIChE J, 2007 [source] Geometrical theory of triple junctions of CSL boundariesACTA CRYSTALLOGRAPHICA SECTION A, Issue 4 2001V. Y. Gertsman When three grain boundaries having misorientations generating coincidence site lattices (CSLs) meet at a triple junction, a common (triple-junction) CSL is formed. A theory is developed as a set of theorems establishing the relationships between the geometrical parameters of the grain-boundary and triple-junction CSLs. Application of the theory is demonstrated in detail for the case of the cubic crystal system. It is also shown how the theory can be extended to an arbitrary crystal lattice. [source] Two novel bis-azomethines derived from quinoxaline-2-carbaldehydeACTA CRYSTALLOGRAPHICA SECTION C, Issue 12 2009Digna Varghese The Schiff base compounds N,N,-bis[(E)-quinoxalin-2-ylmethylidene]propane-1,3-diamine, C21H18N6, (I), and N,N,-bis[(E)-quinoxalin-2-ylmethylidene]butane-1,4-diamine, C22H20N6, (II), crystallize in the monoclinic crystal system. These molecules have crystallographically imposed symmetry. Compound (I) is located on a crystallographic twofold axis and (II) is located on an inversion centre. The molecular conformations of these crystal structures are stabilized by aromatic ,,, stacking interactions. [source] Synthetic, spectral as well as in vitro antimicrobial studies on some bismuth(III) bis(N,N -dialkyldithiocarbamato) alkylenedithiophosphatesAPPLIED ORGANOMETALLIC CHEMISTRY, Issue 4 2010H. P. S. Chauhan Abstract Mixed sulfur donor ligand complexes of the type bismuth(III) bis(N,N -dialkyldithiocarbamato) alkylenedithiophosphate, [R2NCS2]2BiS2POGO [where R = CH3 and C2H5; G = -CH2 -C(C2H5)2 -CH2 -, -CH2 -C(CH3)2 -CH2 -, -CH(CH3)-CH(CH3)- and -C(CH3)2 -C(CH3)2 -] were synthesized in 1:1 molar ratio of bismuth(III) bis(N,N -dialkyldithiocarbamate) chloride and ammonium alkylenedithiophosphate in refluxing benzene and characterized by melting point, molecular weight determinations, elemental analysis (C, H, N, Bi and S) and spectral [UV, IR,NMR (1H,13C and 31P) and powder X ray diffraction] studies; all these studies were in good agreement with the synthesized complexes. These newly synthesized derivatives are yellow and brown colored solids and are soluble in common organic solvents like benzene, chloroform, dichloromethane and DMF. Based on the physicochemical and spectral studies, a tentative structure of these newly synthesized complexes was assigned and the average particle size of the synthesized complexes determined by powder XRD, showing that nano range polycrystalline particles were formed with a monoclinic crystal system. These complexes were also screened for their antimicrobial activities using the well diffusion method. The free ligands as well as their mixed metal complexes were tested in vitro against four bacterial strains: two Gram-positive, Staphylococcus aureus (ATCC 9144) (G+) and Bacillus subtilis (ATCC 6051), (G+) and two Gram-negative, Escherichia coli (ATCC 9637) (G,) and Pseudomonas aeruginosa (ATCC 25619) (G,) to assess their antimicrobial properties. The results were indeed positive and exhibited good antibacterial effects. Chloroamphenicol used as a standard for comparison and synthesized complexes showed good antibacterial effects over chloroamphenicol. On the basis of these studies, the synthesized complexes help to understand the different structural and biological properties of main group elements with sulfur donor ligands. Copyright © 2010 John Wiley & Sons, Ltd. [source] Two hydrates of 6-methoxypurineACTA CRYSTALLOGRAPHICA SECTION C, Issue 1 2004Natalya Fridman 6-Methoxypurine crystallizes from N,N -methylformamide as the hemihydrate, C6H6N4O·0.5H2O, and from water as the trihydrate, C6H6N4O·3H2O. Both forms crystallize in the triclinic crystal system. Upon heating the trihydrate, molecules of water are liberated successively; the hemihydrate is formed at 383,K. In the hemihydrate, the H atom on the imidazole N atom is disordered between the two N atoms. The water molecule in the hemihydrate and the H atoms of a water molecule in the trihydrate are also disordered. In the hemihydrate, the organic moieties are connected by N,H,N hydrogen bonds, while they are connected via water molecules in the trihydrate. [source] Two dimorphs of 5-methylsulfanyl-1H -tetrazoleACTA CRYSTALLOGRAPHICA SECTION C, Issue 1 2004Natalya Fridman 5-Methylsulfanyl-1H -tetrazole, C2H4N4S, crystallizes in dimorphic forms; the ,-form crystallizes at room temperature in the monoclinic crystal system, space group P21/m, and the ,-form crystallizes by sublimation at 423,K in the orthorhombic crystal system, space group Pbcm. In both forms, the molecules occupy crystallographic mirror planes and are connected to one another via N,H,N hydrogen bonds, the amino H atoms being disordered. The two forms differ from one another in their packing; there are polar layers in the ,-form and non-polar layers in the ,-form. [source] Structure of d -tyrosyl-tRNATyr deacylase using home-source Cu,K, and moderate-quality iodide-SAD data: structural polymorphism and HEPES-bound enzyme statesACTA CRYSTALLOGRAPHICA SECTION D, Issue 5 2010Manickam Yogavel d -Tyrosyl-tRNATyr deacylase (DTD) is an editing enzyme that removes d -amino acids from mischarged tRNAs. The crystal structure of Plasmodium falciparum DTD (PfDTD) was determined using the iodide-SAD phasing method. Iodide-derivatized PfDTD crystals were obtained using the quick cryo-soaking procedure in which native crystals were soaked for a short period of 10,30,s in cryoprotectant solution containing 0.2,1,M NaI. Iodide-SAD data sets were collected to 3.3 and 2.74,Å resolution from PfDTD crystals that belonged to two different space groups, P43 and P1, using an in-house X-ray copper-anode source. This is the first report to detail structure solution using low iodide anomalous signal, modest resolution and redundancy and average solvent content for SAD phasing of 984 and 1312 amino acids in the triclinic P1 and tetragonal P43 space groups, respectively. A total of 85% and 56% of the residues were automatically built into the iodide-phased electron-density maps using PHENIX AutoBuild. The structure of HEPES-bound PfDTD was subsequently determined by molecular replacement and refined to 2.83,Å resolution. The crystals obtained from various batches of crystallization trials of PfDTD exhibited polymorphism in terms of belonging to different crystal forms and space groups. Even within a given crystal system the unit-cell parameters showed high non-isomorphism. These packing variations were exploited in order to conduct a systematic study of conformational changes in PfDTD. It is shown that the disposition of a ten-residue insertion loop affects packing within the PfDTD crystals and seems to determine the non-isomorphism in unit-cell parameters. By tracking the changes in PfDTD unit cells, it was possible to map conformational differences within PfDTD that may be of significance for enzyme activity. [source] The interdependence of wavelength, redundancy and dose in sulfur SAD experimentsACTA CRYSTALLOGRAPHICA SECTION D, Issue 12 2008Michele Cianci In the last decade, the popularity of sulfur SAD anomalous dispersion experiments has spread rapidly among synchrotron users as a quick and streamlined way of solving the phase problem in macromolecular crystallography. On beamline 10 at SRS (Daresbury Laboratory, UK), a versatile design has allowed test data sets to be collected at six wavelengths between 0.979 and 2.290,Å in order to evaluate the importance and the interdependence of experimental variables such as the Bijvoet ratio, wavelength, resolution limit, data redundancy and absorbed X-ray dose in the sample per data set. All the samples used in the experiments were high-quality hen egg-white lysozyme crystals. X-radiation damage was found to affect disulfide bridges after the crystals had been given a total dose of 0.20 × 107,Gy. However, with such a total dose, it was still possible in all cases to find a strategy to collect data sets to determine the sulfur substructure and produce good-quality phases by choosing an optimum combination of wavelength, exposure time and redundancy. A ,|,ano|/,(,ano), greater than 1.5 for all resolution shells was a necessary requirement for successful sulfur SAD substructure location. Provided this is achieved, it seems possible to find an optimum compromise between wavelength, redundancy and dose to provide phasing information. The choice of the wavelength should then follow the sample composition and the diffracting properties of the crystal. For strongly diffracting crystals, wavelengths equal or shorter than 1.540,Å can be selected to capture the available data (provided the Bijvoet ratio is reasonable), while a longer wavelength, to gain as high a Bijvoet ratio as possible, must be used for more weakly diffracting crystals. These results suggest that an approach to a sulfur SAD experiment based on a complete description of the crystal system and the instrument for data collection is useful. [source] Crystallization of a core fragment of the flagellar hook protein FlgEACTA CRYSTALLOGRAPHICA SECTION D, Issue 11 2004Fadel A. Samatey A core fragment of the bacterial flagellar hook protein FlgE was overexpressed, purified and crystallized. The crystal diffracted to 1.6,Å resolution using synchrotron X-radiation. The crystal belongs to the orthorhombic crystal system, with space group P21212 and unit-cell parameters a = 128.4, b = 48.8, c = 96.7,Å. SeMet protein was also overexpressed, purified, crystallized and a set of 2.3,Å MAD data was collected. [source] A new crystal form of XT6 enables a significant improvement of its diffraction quality and resolutionACTA CRYSTALLOGRAPHICA SECTION D, Issue 3 2004Maya Bar Xylanases (1,4-,- d -xylan xylanhydrolases; EC 3.2.1.8) hydrolyze the 1,4-,- d -xylopyranosyl linkage of xylans. The detailed structural characterization of these enzymes is of interest for the elucidation of their catalytic mechanism and for their rational modification toward improved stability and specificity. An extracellular xylanase from Geobacillus stearothermophilus T-6 (XT6) has recently been cloned, overexpressed, purified and biochemically characterized. Previous crystallographic efforts resulted in a hexagonal crystal form, which subsequently proved to be of limited use for structural analysis, mainly because of its relatively poor diffraction quality and resolution. A systematic search for more suitable crystals of XT6 recently resulted in a new crystal form of this enzyme with significantly improved diffraction characteristics. The new crystals belong to a C -centred monoclinic crystal system (space group C2), with unit-cell parameters a = 121.5, b = 61.7, c = 89.1,Å, , = 119.7°. These crystals diffract X-rays to better than 1.5,Å resolution, showing a very clear diffraction pattern of relatively high quality. The crystals are mechanically strong and exhibit excellent radiation-stability when frozen under cold nitrogen gas. A full diffraction data set to 1.45,Å resolution (94.1% completeness, Rmerge = 7.0%) has been collected from flash-frozen crystals of the native enzyme at 95,K using synchrotron radiation. Crystals of the E159A/E265A catalytic double mutant of XT6 were found to be isomorphous to those of native XT6. They were used for a full measurement of 1.8,Å resolution diffraction data at 100,K (90.9% completeness; Rmerge = 5.0%). These data are currently being used for the high-resolution structure determination of XT6 and its mutant for mechanistic interpretations and rational introduction of thermostability. [source] Crystallization and preliminary X-ray data investigation of the bacterial enterocin A immunity protein at 1.65,Å resolutionACTA CRYSTALLOGRAPHICA SECTION D, Issue 7 2003Bjørn Dalhus Crystals of the bacterial enterocin A immunity protein have been prepared by the hanging-drop vapour-diffusion technique at 293,K. The crystals diffract to better than 1.7,Å resolution and X-ray diffraction data to 1.65,Å have been collected at 110,K using synchrotron radiation. The enterocin A immunity protein crystals belong to the monoclinic crystal system, with unit-cell parameters a = 116.32, b = 42.35, c = 66.17,Å, , = 111.3°. The symmetry and systematic absences in the diffraction pattern are consistent with space group C2. The presence of two molecules in the asymmetric unit with a molecular weight of ,12.2,kDa gives a crystal volume per protein mass (VM) of ,3.1,Å3,Da,1 and a solvent content of ,60% by volume. [source] Crystallization and preliminary crystallographic analysis of N -acetylglucosamine 6-phosphate deacetylase from Escherichia coliACTA CRYSTALLOGRAPHICA SECTION D, Issue 5 2000F. M. Ferreira N -Acetylglucosamine 6-phosphate deacetylase (E.C. 3.5.1.25), an enzyme from Escherichia coli involved in aminosugar catabolism, has been crystallized by the vapour-diffusion technique using phosphate as precipitant. X-ray diffraction experiments show the crystals to belong to the orthorhombic crystal system, with space group P21212. The unit-cell parameters are a = 82.09,(2), b = 114.50,(1), c = 80.17,(1),Å. The crystals diffract to a maximum resolution of 1.8,Å and an initial data set was collected to 2.0,Å. [source] Production, purification, crystallization and preliminary X-ray diffraction studies of the nucleoside diphosphate kinase b from Leishmania majorACTA CRYSTALLOGRAPHICA SECTION F (ELECTRONIC), Issue 11 2009Celisa Caldana Costa Tonoli Nucleoside diphosphate kinases (NDKs; EC 2.7.4.6) play an essential role in the synthesis of nucleotides from intermediates in the salvage pathway in all parasitic trypanosomatids and their structural studies will be instrumental in shedding light on the biochemical machinery involved in the parasite life cycle and host,parasite interactions. In this work, NDKb from Leishmania major was overexpressed in Escherichia coli, purified to homogeneity and crystallized using the sitting-drop vapour-diffusion method. The NDK crystal diffracted to 2.2,Å resolution and belonged to the trigonal crystal system, with unit-cell parameters a = 114.2, c = 93.9,Å. Translation-function calculations yielded an unambiguous solution in the enantiomorphic space group P3221. [source] Inclusion Behavior of ,-Cyclodextrin with Bipyridine Molecules: Factors Governing Host-Guest Inclusion GeometriesCHEMISTRY - AN ASIAN JOURNAL, Issue 3 2009Yan-Li Zhao Dr. Abstract Guest Effect: The differences of nitrogen atom positions and the bridge bonds linked to two pyridine rings of some bipyridine guests can significantly affect the binding abilities and inclusion geometries of ,-cyclodextrin with the guests in both the solution and solid states. The 1:1 complexation of ,-cyclodextrin (,-CD) with structurally similar bipyridine guests which lead to the formation of six inclusion complexes (1,6) of ,-CD with 4,4,-vinylenedipyridine, 2,2,-vinylenedipyridine, 1-(2-pyridyl)-2-(4-pyridyl)ethylene, 4,4,-ethylene-dipyridine, 4,4,-dithiodipyridine, and 2,2,-dithiodipyridine has been investigated comprehensively by X-ray crystallography in the solid state and by 1H,NMR spectroscopy and microcalorimetric titration in aqueous solution. The complex formation constants (KS) for the stoichiometric 1:1 host,guest inclusion complexation of ,-CD with the bipyridine derivatives were determined in aqueous solution by microcalorimetry and the host,guest inclusion geometries of the complexes were deduced from 1H ROESY NMR spectroscopy. It transpires that the guest bipyridine molecules are included in the ,-CD cavity with a range of different inclusion geometries. In the solid state, the crystal superstructures for the ,-CD complexes 1, 4, and 5 are characterized by the triclinic crystal system (space group P1) commensurate with AAAA type supramolecular aggregation. By contrast, the ,-CD complexes 2, 3, and 6 display either monoclinic (space group P21) or orthorhombic (space group C2221) crystal systems, characteristic of ABAB type supramolecular aggregation. The results demonstrate that the relative locations of the nitrogen atom positions and the bridge-bond links between the two pyridine rings in these bipyridine guests, not only lead to distinct crystal systems and space groups, but also to different binding geometries and thermodynamical parameters on complexation of the bipyridines with ,-CD. The knowledge obtained from this research improves our understanding of the molecular recognition and self-assembly processes exhibited by ,-CD, both in the solid state and in aqueous solution. [source] Nitrogen-rich 6-(3,5-Dimethylpyrazol-1-yl)-3-(2,4,6-trinitro-anilino)-1,2,4,5-tetrazin: Synthesis, Crystal Structure and Thermal PropertyCHINESE JOURNAL OF CHEMISTRY, Issue 10 2007Wan-Long PAN Abstract 6-(3,5-Dimethylpyrazol-1-yl)-3-(2,4,6-trinitroanilino)-1,2,4,5-tetrazin (1) has been synthesized and characterized by 1H NMR, MS, elemental analysis, infrared spectra and thermal analyses. The crystal structure was determined by X-ray diffraction method. 1 is crystallized in P21/c space group of monoclinic crystal system, and exhibits good physical properties, such as high densities (>1.55 g·cm,3) and good thermal stabilities (Td>220 °C). The intrermolecular hydrogen bonds construct the P - and M -helices from organic molecules and may contribute to the high melting points. [source] Crystal Structure and Characterization of a Large Polyoxotungstate (NH4)21{La(H2O)5[Ni(H2O)]2As4W40O140}·53H2OCHINESE JOURNAL OF CHEMISTRY, Issue 3 2003Xue Gang-Lin Abstract The heteropolytungstate (NH4)21{La(H2O)5[Ni(H2O)]2As4W40O140}·53H2O is obtained by the reaction of Na27[NaAs4W40O140]· 60H2O with NiCl2·6H2O, La(NO3)3·6H2O and NH4Cl at pH-4.5. The structure and chemical composition are determined by X-ray diffraction analysis and elemental analysis. The crystal data and main structure refinement are a = 1.9551(3) nm, b = 2.4156(4) nm, c= 3.7068(6) nm, , = 91.505(3)°, V = 17.500 (5) nm3, monoclinic crystal system with space group P21/n, Z = 4, R1 = 0.0573, wR2 = 0.0717 [I >2 Crystal Structure of Complex Tris(4,4,4-trifluoro-1-pheny1,1,3-butanedione) (1, 10-phenanthroline) Europium (III)CHINESE JOURNAL OF CHEMISTRY, Issue 2 2003Guo Qian-Ling Abstract The complex Eu(btfa)3 (phen) (btfa=4,4,4-trifluoro-1-phenyl-1, 3-butanedione, phen = 1,10-phenanthroline) has been prepared and characterized by elemental analysis, IR and UV spectroscopies. The crystal and molecular structures of the complex have been determined by X-ray diffraction analysis. It belongs to the monoclinic crystal system, space group P21/c with a = 0.9700(2) nm, b = 3.7450(5) nm, c = 1.0917(3) nm, , = 92.51(2)°, V = 3.962(1) nm5, Z = 4, Dc = 1.639 g/cm3, , = 1.676 mm,1, F(000) = 1936, R1, = 0.0388, wR2 = 0.0775. Structure analysis shows that the europium(III) ion is coordinated to six oxygen atoms of ,-diketonate anions and two nitrogen atoms of phenanthroline molecule. The coordination polyhedron is an approximate square antiprism. [source] Channel-like crystal structure of cinchoninium L - O -phosphoserine salt dihydrateCHIRALITY, Issue 6 2010Aleksandra Wese, ucha-Birczy Abstract Studies on the interactions between L - O - phosphoserine, as one of the simplest fragments of membrane components, and the Cinchona alkaloid cinchonine, in the crystalline state were performed. Cinchoninium L - O -phosposerine salt dihydrate (PhSerCin) crystallizes in a monoclinic crystal system, space group P21, with unit cell parameters: a = 8.45400(10) Å, b = 7.17100(10) Å, c = 20.7760(4) Å, , = 90°, , = 98.7830(10)°, , = 90°, Z = 2. The asymmetric unit consists of the cinchoninium cation linked by hydrogen bonds to a phosphoserine anion and two water molecules. Intermolecular hydrogen bonds connecting phosphoserine anions via water molecules form chains extended along the b axis. Two such chains symmetrically related by twofold screw axis create a "channel." On both sides of this channel cinchonine cations are attached by hydrogen bonds in which the atoms N1, O12, and water molecules participate. This arrangement mimics the system of bilayer biological membrane. Chirality 2010. © 2009 Wiley-Liss, Inc. [source] Advances in powder diffraction pattern indexing: N-TREOR09JOURNAL OF APPLIED CRYSTALLOGRAPHY, Issue 5 2009Angela Altomare Powder pattern indexing can still be a challenge, despite the great recent advances in theoretical approaches, computer speed and experimental devices. More plausible unit cells, belonging to different crystal systems, are frequently found by the indexing programs, and recognition of the correct one may not be trivial. The task is, however, of extreme importance: in case of failure a lot of effort and computing time may be wasted. The classical figures of merit for estimating the unit-cell reliability {i.e.M20 [de Wolff (1968). J. Appl. Cryst.1, 108,113] and FN [Smith & Snyder (1979). J. Appl. Cryst.12, 60,65]} sometimes fail. For this reason, a new figure of merit has been introduced in N-TREOR09, the updated version of the indexing package N-TREOR [Altomare, Giacovazzo, Guagliardi, Moliterni, Rizzi & Werner (2000). J. Appl. Cryst. 33, 1180,1186], combining the information supplied by M20 with additional parameters such as the number of unindexed lines, the degree of overlap in the pattern (the so-called number of statistically independent observations), the symmetry deriving from the automatic evaluation of the extinction group, and the agreement between the calculated and observed profiles. The use of the new parameters requires a dramatic modification of the procedures used worldwide: in the approach presented here, extinction symbol and unit-cell determination are simultaneously estimated. N-TREOR09 benefits also from an improved indexing procedure in the triclinic system and has been integrated into EXPO2009, the updated version of EXPO2004 [Altomare, Caliandro, Camalli, Cuocci, Giacovazzo, Moliterni & Rizzi (2004). J. Appl. Cryst. 37, 1025,1028]. The application of the new procedure to a large set of test structures is described. [source] Synthesis and functional properties of green fluorescent poly(methylmethacrylate) for use in liquid crystal systemsPOLYMERS FOR ADVANCED TECHNOLOGIES, Issue 9 2003Ivo Grabchev Abstract The copolymerization of six 4-aminosubstituted-1,8-naphthalimide dyes comprising an allylic polymerizable group with methylmethacrylate has been investigated. The utility of the copolymers prepared as fluorescent component in polymer/liquid crystal systems has been examined. The photophysical and photochemical properties of the systems monomeric dye/liquid crystal and copolymer/liquid crystal have been also discussed. It has been shown that in a liquid crystal mixture 1,8-naphthalimide dyes and respective copolymer/liquid crystals have yellow,green fluorescent color with good photostability. Copyright © 2003 John Wiley & Sons, Ltd. [source] Deposition of crystalline copper films from tetranuclear copper (II) complexes without application of reducing atmosphereAPPLIED ORGANOMETALLIC CHEMISTRY, Issue 10 2010Muhammad Shahid Abstract Crystalline copper films were deposited by aerosol-assisted chemical vapor deposition (AACVD) in the absence of hydrogen from two newly synthesized complexes [Cu(deae)(TFA)]4·1.25THF (1) and [Cu4(OAc)6(bdmap)2(H2O)2]·4H2O (2) [deae = N, N -diethylaminoethanolate, TFA = trifloroacetate, OAc = acetate and bdmap = 1,3-bis(dimethylamino)-2-propanolato]. These precursors were prepared in high yield using mixed ligands and crystallized in tetragonal and triclinic crystal systems with space groups 141/a and P , 1. Complexes 1 and 2 thermally decomposed at 290 and 250 °C, respectively, to yield copper films which were characterized by SEM/EDX for their morphology and composition and PXRD for their crystallinity and phase. These films have smooth morphologies with particle sizes within the range of 0.3,0.6 µm and may find applications in fabrication of ultralarge-scale integrated circuits. Copyright © 2010 John Wiley & Sons, Ltd. [source] Two polymorphs of aqua[N,N,-ethylenebis(salicylideneaminato- N,O)]oxovanadium(V) nitrateACTA CRYSTALLOGRAPHICA SECTION C, Issue 3 2001Alan Hazell The title compound, aqua[bis(salicylidene)ethylenediaminato- O,N,N,,O,]oxovanadium(V) nitrate, [VO(C16H14N2O2)(H2O)]NO3, crystallizes as two polymorphs in the triclinic and monoclinic crystal systems. In both, the V atom has a distorted octahedral coordination geometry with a long V,Owater bond trans to V=O. The coordinated water molecules are hydrogen bonded to the nitrate ions so that pairs of cations are linked to give neutral centrosymmetric dimers. The V=O and V,Owater distances are 1.598,(2) and 2.257,(2),Å, respectively, in the triclinic form, and 1.588,(3) and 2.230,(3),Å, respectively, in the monoclinic form. In the triclinic form, the dimers pack so that the salen [bis(salicylidene)ethylenediaminate] ligands are parallel to each other, whereas in the monoclinic form, which is the denser, there is a herring-bone arrangement. [source] Type II dehydroquinase: molecular replacement with many copiesACTA CRYSTALLOGRAPHICA SECTION D, Issue 1 2008Kirsty Anne Stewart Type II dehydroquinase is a small (150-amino-acid) protein which in solution packs together to form a dodecamer with 23 cubic symmetry. In crystals of this protein the symmetry of the biological unit can be coincident with the crystallographic symmetry, giving rise to cubic crystal forms with a single monomer in the asymmetric unit. In crystals where this is not the case, multiple copies of the monomer are present, giving rise to significant and often confusing noncrystallographic symmetry in low-symmetry crystal systems. These different crystal forms pose a variety of challenges for solution by molecular replacement. Three examples of structure solutions, including a highly unusual triclinic crystal form with 16 dodecamers (192 monomers) in the unit cell, are described. Four commonly used molecular-replacement packages are assessed against two of these examples, one of high symmetry and the other of low symmetry; this study highlights how program performance can vary significantly depending on the given problem. In addition, the final refined structure of the 16-dodecamer triclinic crystal form is analysed and shown not to be a superlattice structure, but rather an F -centred cubic crystal with frustrated crystallographic symmetry. [source]
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