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Observed Reflections (observed + reflection)
Selected AbstractsNeutron and electron diffraction studies of La(Zn1/2Ti1/2)O3 perovskiteACTA CRYSTALLOGRAPHICA SECTION B, Issue 4 2006Yi Hu The crystallography and microwave dielectric properties of La(Zn1/2Ti1/2)O3 (LZT) ceramics prepared via the mixed-oxide route were investigated in this study. While samples were largely single phase, small amounts of ZnO impurity were detected in sintered pellets. Observed reflections in electron and neutron diffraction patterns indicate that the symmetry of LZT is P21/n. The B site is ordered on {110} or pseudocubic {111}, but the presence of the pseudocubic (111) reflection is in itself insufficient to indicate the existence of such order. Rietveld refinements of the neutron diffraction data yield an excellent fit for such a model. The structure is highly twinned, with variants related through common {211} composition planes and 90° rotations about ,011,. The microwave dielectric properties measured were ,r = 34, Qf = 36,090 and ,f = ,70,MK,1. [source] Synthesis and crystal structure investigation of pyridine-2-(3,-mercaptopropanoic acid)- N -oxideCRYSTAL RESEARCH AND TECHNOLOGY, Issue 10 2007R. Ramasubramanian Abstract Pyridine-2-(3,-mercaptopropanoic acid)- N -oxide (I), is a higher homologue of 1-oxopyridinium-2-thioacetic acid (II) [1]. It crystallizes in monoclinic space group P21 with a = 9.2168(2) Å, b = 4.1423(2) Å, c = 11.3904(4) Å, , = 98.65(2)°, V = 429.93(3) Å3 and Z = 2. The least-squares refinement gave residual index R = 0.024 for 1070 observed reflections. The introduction of an additional methylene group in (II) causes a flip in the carboxylic acid group of (I) that facilitates the molecules to align infinite antiparallel chains through strong C,H···O interactions. The molecules are interlinked by O,H···O hydrogen bonding across the chains and forming an infinite screw chain along y-direction. The molecular packing is stabilized by O,H···O and C,H···O hydrogen bonding and ,-, electron interactions. This is an important facet of the crystal packing. (© 2007 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Synthesis and crystal structure of a new inorganic , organic complex: (4-ClC7H6NH3)9[Nd(P6O18)2]·9H2OCRYSTAL RESEARCH AND TECHNOLOGY, Issue 9 2007O. Amri Abstract Single crystals of (4-ClC7H6NH3)9[Nd(P6O18)2]·9H2O were synthesized in aqueous solution. This compound crystallizes in a triclinic P1 unit-cell, with a = 14.898(6), b = 18.049(7), c = 20.695(6)Å, , = 102.04(3), , = 100.49(3), , = 98.82(3)°, V = 5245(4) Å3 and Z = 2. The crystal structure has been solved and refined to R = 0.043 (Rw = 0.061) for 20420 observed reflections. The atomic arrangement of the title compound can be described as infinite layers built by complex of Neodyme [Nd(P6O18)2] and nine water molecules. The organic cations are located in the space delimited by the successive inorganic layers. (© 2007 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Crystal structure of a ternary mononuclear copper (II) complex: 4-chloro-3-methyl-6[(N-2-picolyl)-1,-iminomethyl]phenolato copper(II)perchlorateCRYSTAL RESEARCH AND TECHNOLOGY, Issue 5 2006S. M. Malathy Sony Abstract The complex crystallizes in monoclinic space group P21/n with unit cell parameters a = 7.295(4), b = 19.627(5), c = 12.770(4) Å, , = 101.25(4)º, V = 1793.2(12) Å3, Z = 4, , = 1.684 Mg/m3 at T = 293(2)K. The structure was solved by Patterson method and refined by full-matrix least-squares procedures to final R = 0.0387 using 2906 observed reflections. The asymmetric unit of the complex contains a mononuclear tridentate ligand, a perchlorate group and a methanol molecule. The compound crystallizes as parallel layers of polymeric complex bridged through perchloarate groups. The molecular CuN2OO,O,,2 chromophore involves an elongated rhombic octahedral structure and the Cu-ligand bond shows greater disparity. The five-membered chelate ring and the pyridine ring lie in the same plane while the six membered chelate ring assumes sofa conformation. A strong O-H,O inter molecular interaction plays a key role in the formation of dimer along b-axis. (© 2006 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Crystal structure of 4-(1-methyl-1-mesitylcyclobutane-3-yl)-2-aminothiazoleCRYSTAL RESEARCH AND TECHNOLOGY, Issue 3 2006. Aksoy Abstract The crystal structure of 4-(1-methyl-1-mesitylcyclobutane-3-yl)-2-aminothiazole (C17H22N2S1) has been determined by X-ray crystallographic techniques. The compound crystallizes in the triclinic space group P-1 with Z = 6. The crystal structure was solved by direct methods and refined by full-matrix least squares to a final R-value of 0.052 for 2298 observed reflections [I > 2, ( I ) ]. There are three crystallographically independent molecules, I, II and III. These molecules are held together by intermolecular N-H...N hydrogen bonds. © 2006 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim [source] Crystal structure of N-[(1Z)-1-(3-methyl-3-phenylcyclobutyl)-2-thiomorpholin-4-ylethylidene] thioureaCRYSTAL RESEARCH AND TECHNOLOGY, Issue 7 2005U. Sar Abstract The crystal structure of N-[(1Z)-1-(3-methyl-3-phenylcyclobutyl)-2-thiomorpholin-4-ylethylidene] thiourea (C18H26N4S2) has been determined by X-ray crystallographic techniques. The compound crystallizes in the orthorhombic space group Pbca, with unit cell parameters: a = 15.692(3), b = 20.803(8), c = 11.979(6)Å, Z = 8, V = 3911(7)Å3. The crystal structure was solved by direct methods and refined by full-matrix least squares to a final R-value of 0.084 for 1447 observed reflections [I > 2, ( I ) ]. In the thiosemicarbazide moiety, the S = C bond length is 1.656(6), N-C-N angle is 115.6(5)°. The crystal structure is stabilized by the intermolecular N-H...S hydrogen bonds. (© 2005 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Structure and conformation of a nickel complex: {2-Hydroxo-3-piperidine-1-yl-methyl-N,N,(bis-5-bromobenzylpropylenediimine)nickel(II)perchlorate}CRYSTAL RESEARCH AND TECHNOLOGY, Issue 2 2004S. M. Malathy Sony Abstract The title compound, a nickel complex [C23H26N3O2Br2Ni.(ClO4)] (CCDC 199520) crystallizes in triclinic space group P with the cell parameters a = 10.2560(4), b = 10.8231(4), c = 12.0888(5)Å, , = 99.404(1), , = 99.780(1), , = 92.252(1)° and V = 1301.49(9)Å3. The structure was solved by Patterson method and refined by full-matrix least-squares procedures to a final R = 0.0497 using 6287 observed reflections. In the complex, the piperidine ring takes chair conformation and the geometry around the Ni ion is slightly distorted square planar. The dihedral angle between the planes [N-Ni-N and O-Ni-O] is 9.4(1)°. The chelate ring containing both the nitrogen atoms adopts twisted boat conformation. The molecules in the crystal are stabilized by N-H,O and C-H,O types of hydrogen bonds in addition to a C-H,, interaction. (© 2004 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Crystal structure of ,-phenoxo bridged dicopper complex: {N-[(2-hydroxylato-5-methyl)benzyl-(2,-hydroxylato-3,,5,-dimethylbenzyl)]ethyl amine dicopper(II)}CRYSTAL RESEARCH AND TECHNOLOGY, Issue 12 2002S. M. Malathy Sony Abstract The title compound crystallizes in monoclinic space group C2/c with cell parameters a = 21.404(2), b = 13.962(1), c = 17.917(1)Å, , = 124.394(2)°, V = 4418.3(6)Å3, Z = 8, Dcal = 1.193Mg/m3 and T = 293 K. The structure was solved by Patterson method and refined by full-matrix least-squares procedures to final R = 0.0882 using 5253 observed reflections. The tetra coordinated copper atom have a slight distorted square planar geometry with the Cu-Cu distance of 2.987(1)Å. The two six membered rings containing copper atom assume distorted sofa conformation. C-H,, and C-H,O type of intermolecular interactions play a role in stabilizing the crystal packing in addition to van der Waals forces. [source] Ab initio structure solution by iterative phase-retrieval methods: performance tests on charge flipping and low-density eliminationJOURNAL OF APPLIED CRYSTALLOGRAPHY, Issue 1 2010Frank Fleischer Comprehensive tests on the density-modification methods charge flipping [Oszlányi & Süt, (2004). Acta Cryst. A60, 134,141] and low-density elimination [Shiono & Woolfson (1992). Acta Cryst. A48, 451,456] for solving crystal structures are performed on simulated diffraction data of periodic structures and quasicrystals. A novel model-independent figure of merit, which characterizes the reliability of the retrieved phase of each reflection, is introduced and tested. The results of the performance tests show that the quality of the phase retrieval highly depends on the presence or absence of an inversion center and on the algorithm used for solving the structure. Charge flipping has a higher success rate for solving structures, while low-density elimination leads to a higher accuracy in phase retrieval. The best results can be obtained by combining the two methods, i.e. by solving a structure with charge flipping followed by a few cycles of low-density elimination. It is shown that these additional cycles dramatically improve the phases not only of the weak reflections but also of the strong ones. The results can be improved further by averaging the results of several runs and by applying a correction term that compensates for a reduction of the structure-factor amplitudes by averaging of inconsistently observed reflections. It is further shown that in most cases the retrieved phases converge to the best solution obtainable with a given method. [source] Advances in the free lunch methodJOURNAL OF APPLIED CRYSTALLOGRAPHY, Issue 5 2007Rocco Caliandro The most critical limit of macromolecular crystallography, the experimental data resolution, is partially `tricked' by the `free lunch method' (non-measured reflection extrapolation). The best electron density map available when only observed data are used may be employed to extrapolate moduli and phases of unobserved reflections behind and beyond the experimental resolution limit. The method is able to reduce the mean phase error of the observed reflections and to produce a more interpretable (in terms of a molecular model) electron density map. The main features of the free lunch method have been studied and its performance has been enhanced; it is beneficial even if data resolution is about 2,Å. Furthermore, the technique has been parameterized so that it may be routinely used by other phasing programs. [source] The first crystal structure of a gramicidin complex with sodium: high-resolution study of a nonstoichiometric gramicidin D,NaI complexACTA CRYSTALLOGRAPHICA SECTION D, Issue 8 2010A. Olczak The crystal structure of the nonstoichiometric complex of gramicidin D with NaI has been studied using synchrotron radiation at 100,K. The limiting resolution was 1.25,Å and the R factor was 16% for 19,883 observed reflections. The general architecture of the antiparallel two-stranded gramicidin dimers in the studied crystal was a right-handed antiparallel double-stranded form that closely resembles the structures of other right-handed species published to date. However, there were several surprising observations. In addition to the significantly different composition of linear gramicidins identified in the crystal structure, including the absence of the gramicidin C form, only two cationic sites were found in each of the two independent dimers (channels), which were partially occupied by sodium, compared with the seven sites found in the RbCl complex of gramicidin. The sum of the partial occupancies of Na+ was only 1.26 per two dimers and was confirmed by the similar content of iodine ions (1.21 ions distributed over seven sites), which was easily visible from their anomalous signal. Another surprising observation was the significant asymmetry of the distributions and occupancies of cations in the gramicidin dimers, which was in contrast to those observed in the high-resolution structures of the complexes of heavier alkali metals with gramicidin D, especially that of rubidium. [source] An Unprecedented 2D 4f-3d-5d Multimetal-Isonicotinic Acid Complex: Synthesis, Structural Characterization and Magnetic PropertiesCHINESE JOURNAL OF CHEMISTRY, Issue 9 2008Wen-Tong CHEN Abstract A novel heterometallic metal-isonicotinic acid inorganic-organic hybrid complex [Zn0.5(H2O)]{(Hg2Cl5)- [Er(C6NO2H4)3(H2O)2]}(HgCl2)·0.5CH3OH·0.5H2O (1) has been successfully synthesized via a hydrothermal reaction and structurally characterized by single-crystal X-ray diffraction. Complex 1 crystallizes in the space group C2/c of the monoclinic system with eight formula units in a cell: a=34.165(4) Å, b=9.4692(8) Å, c=24.575(3) Å, , =115.090(5)°, V=7200(1) Å3, C18.50H21Cl7ErHg3N3O10Zn0.50, Mr=1495.25, Dc=2.759 g/cm3, T=293(2) K, µ(Mo K,) =15.954 mm,1, F(000) =5400 and R1/wR2=0.0561/0.0909 for 3157 observed reflections [I>2,(I)] and 6468 unique reflections. Complex 1 is characteristic of a novel 2D {(Hg2Cl5)[Er(C6NO2H4)3(H2O)2]} layered structure constructed from the [Er(C6NO2H4)3(H2O)2] chains interconnected by the Hg2Cl5, linkers. The 2D {(Hg2Cl5)[Er(C6NO2H4)3(H2O)2]} layers, mercury chloride and the lattice water molecules are held together via hydrogen bonds to form a three-dimensional framework with the methanol molecules and the hydrated zinc ions located in the cavities. The magnetic properties show that complex 1 exhibits antiferromagnetic-like interactions. [source] Synthesis and Structural Characterization of 1,4-Di(2-methoxyphenyl)-2,5-piperazinedioneCHINESE JOURNAL OF CHEMISTRY, Issue 5 2007Shu-Sheng Zhang Abstract A new derivative of 2,5-piperazinedione, 1,4-di(2-methoxyphenyl)-2,5-piperazinedione (I), was synthesized by the cyclocondensation reaction of N -2-methoxyphenyl chloroacetamide, and its structure was characterized by elemental analysis, IR, 1H NMR and single crystal X-ray diffraction method. The crystal belongs to monoclinic system, space group P21/c with unit cell dimensions a=0.56934(10) nm, b=1.3880(2) nm, c=1.00329(17) nm, ,=90.376(3)°, V=0.7928(2) nm3, Z=2, Dc=1.367 g·cm,3, ,=0.98 cm,1, R and wR being 0.0606 and 0.1564 respectively for 1549 unique reflections with 1247 observed reflections [I>2,(I)]. The molecule has a crystallographically imposed symmetry center. The three rings in the molecule are each coplanar with their attached groups, excluding methyl H atoms and the H atoms attached to the piperazinedione ring, while the whole molecule is not planar, with dihedral angles of 74.7(1)° between the piperazinedione and each of the two aromatic rings. The crystal structure is stabilized by van der Waals and dipole-dipole forces. [source] New Type of Polymeric Chain Constructed by Exo-bidentate Binaphthol DerivativeCHINESE JOURNAL OF CHEMISTRY, Issue 10 2005Ya-Qiong Gong Abstract The self-assembly of a racemic exo-bidentate ligand 2,2,-bis(4-pyridylmethyloxy)-1,1,-binaphthyl, namely Rac -L, with cadmium(II) salt gave rise to a new one-dimensional polymer, which has been characterized by single crystal X-ray diffraction analysis. The polymer crystallizes in a triclinic space group P -1 with unit cell parameters: a=0.6976(1) nm, b=1.30160(14) nm, c=1.71146(17) nm,,=105.141(3) °,,=94.263(5)°,,=100.405(4)°, V=1.4633(2) nm3, Z=2, C32H29CdCl2N2O4.5, M=696.88, Dc=1.584 g/cm3, F(000) =708, ,(Mo K,) =0.972 mm,1. The final R and wR are 0.0498 and 0.1282 for 5079 observed reflections with I,,(I). [source] | ||||||||||