Three-Dimensional X-Ray Powder Diffraction from Disordered Illite

2015 ◽  
pp. 43-78 ◽  
Keyword(s):  
Powder Diffraction ◽  
Three Dimensional ◽  
X Ray

Crystal structure of (Z)-cefprozil monohydrate, C18H19N3O5S(H2O)

2019 ◽  
Vol 34 (4) ◽  
pp. 379-388
Author(s):  
Zachary R. Butler ◽  
James A. Kaduk ◽  
Amy M. Gindhart ◽  
Thomas N. Blanton
Keyword(s):  
Crystal Structure ◽  
Powder Diffraction ◽  
Density Functional ◽  
Three Dimensional ◽  
Ion Pair ◽  
Powder Diffraction Data ◽  
Powder Diffraction File ◽  
X Ray ◽  
Dimensional Network ◽  
Acid Proton

The crystal structure of cefprozil monohydrate has been solved and refined using synchrotron X-ray powder diffraction data and optimized using density functional techniques. Cefprozil monohydrate crystallizes in space group P21 (#4) with a = 11.26513(6), b = 11.34004(5), c = 14.72649(11) Å, β = 90.1250(4)°, V = 1881.262(15) Å3, and Z = 4. Although a reasonable fit was obtained using an orthorhombic model, closer examination showed that many peaks were split and/or had shoulders, and thus the true symmetry was monoclinic. DFT calculations revealed that one carboxylic acid proton moved to an amino group. The structure thus contains one ion pair and one pair of neutral molecules. This protonation was confirmed by infrared spectroscopy. There is an extensive array of hydrogen bonds resulting in a three-dimensional network. The powder pattern has been submitted to ICDD® for inclusion in the Powder Diffraction File™.

scholarly journals Reinvestigation of trilithium divanadium(III) tris(orthophosphate), Li3V2(PO4)3, based on single-crystal X-ray data

2013 ◽  
Vol 69 (2) ◽  
pp. i11-i12 ◽  
Author(s):  
Yongho Kee ◽  
Hoseop Yun
Keyword(s):  
Single Crystal ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Title Compound ◽  
Three Dimensional ◽  
Structure Type ◽  
Powder Diffraction Data ◽  
Charge Balance ◽  
X Ray ◽  
Anisotropic Displacement Parameters

The structure of Li3V2(PO4)3has been reinvestigated from single-crystal X-ray data. Although the results of the previous studies (all based on powder diffraction data) are comparable with our redetermination, all atoms were refined with anisotropic displacement parameters in the current study, and the resulting bond lengths are more accurate than those determined from powder diffraction data. The title compound adopts the Li3Fe2(PO4)3structure type. The structure is composed of VO6octahedra and PO4tetrahedra by sharing O atoms to form the three-dimensional anionic framework∞3[V2(PO4)3]3−. The positions of the Li+ions in the empty channels can vary depending on the synthetic conditions. Bond-valence-sum calculations showed structures that are similar to the results of the present study seem to be more stable compared with others. The classical charge balance of the title compound can be represented as [Li+]3[V3+]2[P5+]3[O2−]12.

scholarly journals Crystal structure of anhydrous tripotassium citrate from laboratory X-ray powder diffraction data and DFT comparison

2016 ◽  
Vol 72 (8) ◽  
pp. 1159-1162 ◽  
Author(s):  
Alagappa Rammohan ◽  
James A. Kaduk
Keyword(s):  
Crystal Structure ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Density Functional ◽  
Three Dimensional ◽  
Carboxylate Group ◽  
Powder Diffraction Data ◽  
Coordination Polyhedra ◽  
X Ray ◽  
Graph Set

The crystal structure of anhydrous tripotassium citrate, [K3(C6H5O7)]n, has been solved and refined using laboratory X-ray powder diffraction data, and optimized using density functional techniques. The three unique potassium cations are 6-, 8-, and 6-coordinate (all irregular). The [KOn] coordination polyhedra share edges and corners to form a three-dimensional framework, with channels running parallel to thecaxis. The only hydrogen bond is an intramolecular one involving the hydroxy group and the central carboxylate group, with graph-set motifS(5).

scholarly journals Crystal structure of trirubidium citrate from laboratory X-ray powder diffraction data and DFT comparison

2017 ◽  
Vol 73 (2) ◽  
pp. 250-253 ◽  
Author(s):  
Alagappa Rammohan ◽  
James A. Kaduk
Keyword(s):  
Crystal Structure ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Density Functional ◽  
Three Dimensional ◽  
Powder Diffraction Data ◽  
Coordination Polyhedra ◽  
X Ray ◽  
Methylene Groups ◽  
Graph Set

The crystal structure of trirubidium citrate, 3Rb+·C6H5O73−, has been solved and refined using laboratory X-ray powder diffraction data, and optimized using density functional techniques. The two independent Rb+cations are seven- and eight-coordinate, with bond-valence sums of 0.99 and 0.92 valence units. The coordination polyhedra share edges and corners to form a three-dimensional framework. The only hydrogen bond is an intramolecular one between the hydroxy group and the central carboxylate, with graph setS(5). The hydrophobic methylene groups lie in pockets in the framework.

scholarly journals Crystal structure of trirubidium citrate monohydrate from laboratory X-ray powder diffraction data and DFT comparison

2017 ◽  
Vol 73 (2) ◽  
pp. 227-230 ◽  
Author(s):  
Alagappa Rammohan ◽  
James A. Kaduk
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bond ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Density Functional ◽  
Three Dimensional ◽  
Powder Diffraction Data ◽  
Hydrogen Bond Donor ◽  
X Ray ◽  
Intramolecular Hydrogen

The crystal structure of the title compound, 3Rb+·C6H5O73−·H2O, has been solved and refined using laboratory X-ray powder diffraction data, and optimized using density functional techniques. The hydroxy group participates in an intramolecular hydrogen bond to the deprotonated central carboxylate group with graph-set motifS(5). The water molecule acts as a hydrogen-bond donor to both terminal and central carboxylate O atoms. The three independent rubidium cations are seven-, six- and six-coordinate, with bond-valence sums of 0.84, 1.02, and 0.95, respectively. In the extended structure, their polyhedra share edges and corners to form a three-dimensional network. The hydrophobic methylene groups occupy channels along thebaxis.

scholarly journals RbCa2Nb3O10from X-ray powder data

2009 ◽  
Vol 65 (6) ◽  
pp. i44-i44 ◽  
Author(s):  
Zhen-Hua Liang ◽  
Kai-Bin Tang ◽  
Qian-Wang Chen ◽  
Hua-Gui Zheng
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Solid State Reaction ◽  
Perovskite Structure ◽  
Three Dimensional ◽  
Rietveld Analysis ◽  
Powder Diffraction Data ◽  
X Ray

Rubidium dicalcium triniobate(V), RbCa2Nb3O10, has been synthesized by solid-state reaction and its crystal structure refined from X-ray powder diffraction data using Rietveld analysis. The compound is a three-layer perovskite Dion–Jacobson phase with the perovskite-like slabs derived by termination of the three-dimensional CaNbO3perovskite structure along theabplane. The rubidium ions (4/mmmsymmetry) are located in the interstitial space.

scholarly journals Synthesis, crystal structure and thermal properties of poly[bis[μ2-3-(aminomethyl)pyridine]bis(thiocyanato)cobalt(II)]

2021 ◽  
Vol 77 (4) ◽  
pp. 428-432
Author(s):  
Christoph Krebs ◽  
Inke Jess ◽  
Christian Näther
Keyword(s):  
Crystal Structure ◽  
Differential Scanning Calorimetry ◽  
Hydrogen Bonding ◽  
Thermal Properties ◽  
Powder Diffraction ◽  
Title Compound ◽  
Three Dimensional ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Dimensional Network

The reaction of Co(NCS)2 with 3-(aminomethyl)pyridine as coligand leads to the formation of crystals of the title compound, [Co(NCS)2(C6H8N2)2] n , that were characterized by single-crystal X-ray analysis. In the crystal structure, the CoII cations are octahedrally coordinated by two terminal N-bonded thiocyanate anions as well as two pyridine and two amino N atoms of four symmetry-equivalent 3-(aminomethyl)pyridine coligands with all pairs of equivalent atoms in a trans position. The CoII cations are linked by the 3-(aminomethyl)pyridine coligands into layers parallel to the ac plane. These layers are further linked by intermolecular N—H...S hydrogen bonding into a three-dimensional network. The purity of the title compound was determined by X-ray powder diffraction and its thermal behavior was investigated by differential scanning calorimetry and thermogravimetry.

scholarly journals Whole-pattern fitting technique in serial femtosecond nanocrystallography

IUCrJ ◽  
2016 ◽  
Vol 3 (2) ◽  
pp. 127-138 ◽  
Author(s):  
Ruben A. Dilanian ◽  
Sophie R. Williams ◽  
Andrew V. Martin ◽  
Victor A. Streltsov ◽  
Harry M. Quiney
Keyword(s):  
Powder Diffraction ◽  
Diffraction Data ◽  
Three Dimensional ◽  
Monte Carlo Integration ◽  
Data Set ◽  
X Ray ◽  
X Ray Crystallography ◽  
Small Crystals ◽  
Crystallite Structure ◽  
Serial Crystallography

Serial femtosecond X-ray crystallography (SFX) has created new opportunities in the field of structural analysis of protein nanocrystals. The intensity and timescale characteristics of the X-ray free-electron laser sources used in SFX experiments necessitate the analysis of a large collection of individual crystals of variable shape and quality to ultimately solve a single, average crystal structure. Ensembles of crystals are commonly encountered in powder diffraction, but serial crystallography is different because each crystal is measured individually and can be orientedviaindexing and merged into a three-dimensional data set, as is done for conventional crystallography data. In this way, serial femtosecond crystallography data lie in between conventional crystallography data and powder diffraction data, sharing features of both. The extremely small sizes of nanocrystals, as well as the possible imperfections of their crystallite structure, significantly affect the diffraction pattern and raise the question of how best to extract accurate structure-factor moduli from serial crystallography data. Here it is demonstrated that whole-pattern fitting techniques established for one-dimensional powder diffraction analysis can be feasibly extended to higher dimensions for the analysis of merged SFX diffraction data. It is shown that for very small crystals, whole-pattern fitting methods are more accurate than Monte Carlo integration methods that are currently used.

Crystal structure of new triple molybdate AgMg3Ga(MoO4)5 from Rietveld refinement

2017 ◽  
Vol 32 (4) ◽  
pp. 255-260
Author(s):  
Irina Yu. Kotova ◽  
Aleksandra A. Savina ◽  
Elena G. Khaikina
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Three Dimensional ◽  
Polycrystalline Sample ◽  
Powder Diffraction Data ◽  
Structural Refinement ◽  
X Ray ◽  
Triple Molybdate

A polycrystalline sample of a new triple molybdate AgMg3Ga(MoO4)5 was obtained by solid-state reaction techniques. Structural refinement based on X-ray powder diffraction data showed that the crystal structure is isotypic with NaMg3In(MoO4)5 (sp. gr. P$\bar 1$). In the structure pairs of edge-shared (Mg, Ga)O6,  octahedra are connected by common vertices to form a three-dimensional framework. Large framework cavities involve Ag+ cations. The title compound was found to melt at 1079 K.

Crystal structure of the three-dimensional magnetic network of type Mek[Fe(CN)6]l·mH2O, where Me=Cu, Ni, Co

1995 ◽  
Vol 10 (4) ◽  
pp. 300-305 ◽  
Author(s):  
A. Ratuszna ◽  
S. Juszczyka ◽  
G. Małecki
Keyword(s):  
Crystal Structure ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Three Dimensional ◽  
Powder Diffraction Data ◽  
Bridging Ligands ◽  
X Ray ◽  
C And N ◽  
Fe Sites ◽  
Magnetic Network

The crystal structures of Mek[Fe(CN)6];l·mH2O where Me = Cu, Ni and Co, have been refined from X-ray (CuKa) powder diffraction data by means of Rietveld analyses in space group . The Fe and Me ions are octahedrally coordinated by C and N atoms respectively, forming three-dimensional bimetallic networks with the CN-groups as bridging ligands. The Me(l) sites (k = 2, l=1) and the Fe sites (k = 3, l = 2) are partially occupied. Water oxygens were placed in alternative, empty metal sites.

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