Synthesis, Characterization, and Crystal Structure of Negundoside (2′-p-Hydroxybenzoyl Mussaenosidic Acid)

The structure of title compound Negundoside (2′-p-hydroxybenzoyl mussaenosidic acid) was established by spectral and X-ray diffraction studies. The compound crystallizes in the monoclinic crystal system with space group P21 having unit cell parameters: a=11.6201 (5) Å, b=9.2500 (4) Å, c=12.2516 (5) Å, β=97.793 (4)°, and Z=2. The crystal structure was solved by direct method using single crystal X-ray diffraction data collected at room temperature and refined by full-matrix least-squares procedures to a final R value of 0.0520 for 3389 observed reflections.

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Synthesis, Characterization, and X-Ray Crystal Structure of Bis(O-amyl dithiocarbonato-κ2S,S′)bis(4-cyanopyridine-κN)nickel(II)

Journal of Crystallography ◽

10.1155/2014/748425 ◽

2014 ◽

Vol 2014 ◽

pp. 1-5

Author(s):

Kuldeep Singh ◽

Sanjay Kapoor ◽

Renu Sachar ◽

Vivek K. Gupta ◽

Rajni Kant

Keyword(s):

Crystal Structure ◽

Magnetic Moment ◽

Direct Methods ◽

Title Complex ◽

X Ray Diffraction ◽

Unit Cell Parameters ◽

Orthorhombic Space Group ◽

Full Matrix ◽

X Ray ◽

Cell Parameters

The [Ni(S2CO-n-C5H11)2(C6H4N2)2] adduct of 4-cyanopyridine with [Ni(S2CO-n-C5H11)2] was synthesized and characterized by elemental analysis, magnetic susceptibility measurement, IR, electronic spectral data, and X-ray diffraction analysis. The Ni atom in the title complex is octahedrally coordinated within a trans-N2S4 donor set, with the Ni atom located on a centre of inversion. The title compound exhibits magnetic moment value (3.20 B.M) which is in agreement with magnetic moment values observed for paramagnetic octahedral complexes of nickel(II). The title complex crystallizes in the orthorhombic space group Pbca with unit cell parameters a = 11.455(5), b = 9.602(4), and c = 26.374(1) Å. Crystal structure was solved by direct methods and refined by full matrix least-squares procedures to a final R value of 0.0499 for 2004 observed reflections. The amyl chain is disordered over two sets of sites, with occupancy ratios of 0.595 : 0.405. Infinite long chains of molecules are formed with the help of C–H⋯N hydrogen bond.

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X-ray powder diffraction data of LaNi0.5Ti0.45Co0.05O3, LaNi0.45Co0.05Ti0.5O3, and LaNi0.5Ti0.5O3 perovskites

Powder Diffraction ◽

10.1017/s0885715620000767 ◽

2021 ◽

pp. 1-6

Author(s):

Mariana M. V. M. Souza ◽

Alex Maza ◽

Pablo V. Tuza

Keyword(s):

Crystal Structure ◽

Rietveld Method ◽

Pechini Method ◽

Powder Diffraction Data ◽

X Ray Diffraction ◽

Unit Cell Parameters ◽

X Ray ◽

Cell Parameters ◽

Modified Pechini Method ◽

Scanning Electron

In the present work, LaNi0.5Ti0.45Co0.05O3, LaNi0.45Co0.05Ti0.5O3, and LaNi0.5Ti0.5O3 perovskites were synthesized by the modified Pechini method. These materials were characterized using X-ray fluorescence, scanning electron microscopy, and powder X-ray diffraction coupled to the Rietveld method. The crystal structure of these materials is orthorhombic, with space group Pbnm (No 62). The unit-cell parameters are a = 5.535(5) Å, b = 5.527(3) Å, c = 7.819(7) Å, V = 239.2(3) Å3, for the LaNi0.5Ti0.45Co0.05O3, a = 5.538(6) Å, b = 5.528(4) Å, c = 7.825(10) Å, V = 239.5(4) Å3, for the LaNi0.45Co0.05Ti0.5O3, and a = 5.540(2) Å, b = 5.5334(15) Å, c = 7.834(3) Å, V = 240.2(1) Å3, for the LaNi0.5Ti0.5O3.

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Crystal Structure Refinements of Four Monazite Samples from Different Localities

Minerals ◽

10.3390/min10111028 ◽

2020 ◽

Vol 10 (11) ◽

pp. 1028 ◽

Cited By ~ 1

Author(s):

M. Mashrur Zaman ◽

Sytle M. Antao

Keyword(s):

Crystal Structure ◽

Electron Probe ◽

Unit Cell Volume ◽

Unit Cell ◽

X Ray Diffraction ◽

Unit Cell Parameters ◽

X Ray ◽

Cell Parameters ◽

Large Unit Cell ◽

A Site

This study investigates the crystal chemistry of monazite (APO4, where A = Lanthanides = Ln, as well as Y, Th, U, Ca, and Pb) based on four samples from different localities using single-crystal X-ray diffraction and electron-probe microanalysis. The crystal structure of all four samples are well refined, as indicated by their refinement statistics. Relatively large unit-cell parameters (a = 6.7640(5), b = 6.9850(4), c = 6.4500(3) Å, β = 103.584(2)°, and V = 296.22(3) Å3) are obtained for a detrital monazite-Ce from Cox’s Bazar, Bangladesh. Sm-rich monazite from Gunnison County, Colorado, USA, has smaller unit-cell parameters (a = 6.7010(4), b = 6.9080(4), c = 6.4300(4) Å, β = 103.817(3)°, and V = 289.04(3) Å3). The a, b, and c unit-cell parameters vary linearly with the unit-cell volume, V. The change in the a parameter is large (0.2 Å) and is related to the type of cations occupying the A site. The average <A-O> distances vary linearly with V, whereas the average <P-O> distances are nearly constant because the PO4 group is a rigid tetrahedron.

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Refinement of the crystal structure of sieleckiite and revision of its symmetry

Mineralogical Magazine ◽

10.1180/minmag.2016.080.143 ◽

2017 ◽

Vol 81 (4) ◽

pp. 917-922

Author(s):

Peter Elliott

Keyword(s):

Crystal Structure ◽

Synchrotron Radiation ◽

Single Crystal ◽

Diffraction Data ◽

X Ray Diffraction ◽

Aluminium Phosphate ◽

Unit Cell Parameters ◽

X Ray ◽

Cell Parameters ◽

Phosphate Mineral

AbstractThe crystal structure of the copper aluminium phosphate mineral sieleckiite, Cu3Al4(PO4)2 (OH)12·2H2O, from the Mt Oxide copper mine, Queensland, Australia was solved from single-crystal X-ray diffraction data utilizing synchrotron radiation. Sieleckiite has monoclinic rather than triclinic symmetry as previously reported and is space group C2/m with unit-cell parameters a = 11.711(2), b = 6.9233(14), c = 9.828(2) Å, β = 92.88(3)°, V = 795.8(3) Å3and Z = 2. The crystal structure, which has been refined to R1 = 0.0456 on the basis of 1186 unique reflections with Fo > 4σF, is a framework of corner-, edge- and face- sharing Cu and Al octahedra and PO4 tetrahedra.

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Synthesis and crystal structure of (Ag,Pd)22Se6

Powder Diffraction ◽

10.1017/s0885715612000929 ◽

2013 ◽

Vol 28 (1) ◽

pp. 13-17 ◽

Cited By ~ 1

Author(s):

F. Laufek ◽

A. Vymazalová ◽

D.A. Chareev ◽

A.V. Kristavchuk ◽

J. Drahokoupil ◽

...

Keyword(s):

Crystal Structure ◽

Diffraction Data ◽

Glass Tube ◽

Structure Type ◽

X Ray Diffraction ◽

Unit Cell Parameters ◽

Synthesis And Crystal Structure ◽

X Ray ◽

Cell Parameters ◽

Silica Glass Tube

The (Ag,Pd)22Se6 phase was synthesized from individual elements by silica glass tube technique and structurally characterized from powder X-ray diffraction data. The (Ag,Pd)22Se6 phase crystallizes in Fm$\overline3$m symmetry, unit-cell parameters: a = 12.3169(2) Å, V = 1862.55(5) Å3, Z = 4, and Dc = 10.01 g/cm3. The crystal structure of the (Ag,Pd)22Se6 phase represents a stuffed 3a.3a.3a superstructure of the Pd structure (fcc), where only 4 from 108 available octahedral holes are occupied. Its crystal structure is related to the Cr23C6 structure type.

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Expression, purification, crystallization and X-ray diffraction studies of the molecular chaperone prefoldin fromHomo sapiens

Acta Crystallographica Section F Structural Biology Communications ◽

10.1107/s2053230x15013990 ◽

2015 ◽

Vol 71 (9) ◽

pp. 1189-1193 ◽

Cited By ~ 3

Author(s):

Yoshiki Aikawa ◽

Hiroshi Kida ◽

Yuichi Nishitani ◽

Kunio Miki

Keyword(s):

Crystal Structure ◽

Protein Folding ◽

Diffraction Data ◽

Molecular Chaperone ◽

X Ray Diffraction ◽

Unit Cell Parameters ◽

X Ray ◽

Cell Parameters ◽

Native Proteins ◽

Group Ii Chaperonin

Proper protein folding is an essential process for all organisms. Prefoldin (PFD) is a molecular chaperone that assists protein folding by delivering non-native proteins to group II chaperonin. A heterohexamer of eukaryotic PFD has been shown to specifically recognize and deliver non-native actin and tubulin to chaperonin-containing TCP-1 (CCT), but the mechanism of specific recognition is still unclear. To determine its crystal structure, recombinant human PFD was reconstituted, purified and crystallized. X-ray diffraction data were collected to 4.7 Å resolution. The crystals belonged to space groupP21212, with unit-cell parametersa= 123.2,b= 152.4,c= 105.9 Å.

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A first Mn member in the struvite morphotropic series, CsMn(H2O)6(PO4): hydrothermal synthesis, crystal structure and interconnections within the family of related phosphates

Acta Crystallographica Section C Structural Chemistry ◽

10.1107/s2053229618009798 ◽

2018 ◽

Vol 74 (8) ◽

pp. 936-943

Author(s):

Galina V. Kiriukhina ◽

Olga V. Yakubovich ◽

Ekaterina M. Kochetkova ◽

Olga V. Dimitrova ◽

Anatoliy S. Volkov

Keyword(s):

Crystal Structure ◽

Ionic Radius ◽

The Novel ◽

X Ray Diffraction ◽

Unit Cell Parameters ◽

Hydrothermal Conditions ◽

X Ray ◽

Cell Parameters ◽

Structural Relationships ◽

The Family

Caesium manganese hexahydrate phosphate, CsMn(H2O)6(PO4), was synthesized under hydrothermal conditions. Its crystal structure was determined from single-crystal X-ray diffraction data. The novel phase crystallizes in the hexagonal space group P63 mc and represents the first manganese member in the struvite morphotropic series, AM(H2O)6(TO4). Its crystal structure is built from Mn(H2O)6 octahedra and PO4 tetrahedra linked into a framework via hydrogen bonding. The large Cs atoms are encapsulated in the framework cuboctahedral cavities. It is shown that the size of the A + ionic radius within the morphotropic series AM(H2O)6(XO4) results is certain types of crystal structures and affects the values of the unit-cell parameters. Structural relationships with Na(H2O)Mg(H2O)6(PO4) and the mineral hazenite, KNa(H2O)2Mg2(H2O)12(PO4)2, are discussed.

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Crystal Chemistry and High-Temperature Behaviour of Ammonium Phases NH4MgCl3·6H2O and (NH4)2Fe3+Cl5·H2O from the Burned Dumps of the Chelyabinsk Coal Basin

Minerals ◽

10.3390/min9080486 ◽

2019 ◽

Vol 9 (8) ◽

pp. 486 ◽

Cited By ~ 2

Author(s):

Andrey A. Zolotarev ◽

Elena S. Zhitova ◽

Maria G. Krzhizhanovskaya ◽

Mikhail A. Rassomakhin ◽

Vladimir V. Shilovskikh ◽

...

Keyword(s):

Crystal Structure ◽

High Temperature ◽

Unit Cell ◽

X Ray Diffraction ◽

Coal Basin ◽

Unit Cell Parameters ◽

Space Group ◽

X Ray ◽

Cell Parameters ◽

Mineral Phases

The technogenic mineral phases NH4MgCl3·6H2O and (NH4)2Fe3+Cl5·H2O from the burned dumps of the Chelyabinsk coal basin have been investigated by single-crystal X-ray diffraction, scanning electron microscopy and high-temperature powder X-ray diffraction. The NH4MgCl3·6H2O phase is monoclinic, space group C2/c, unit cell parameters a = 9.3091(9), b = 9.5353(7), c = 13.2941(12) Å, β = 90.089(8)° and V = 1180.05(18) Å3. The crystal structure of NH4MgCl3·6H2O was refined to R1 = 0.078 (wR2 = 0.185) on the basis of 1678 unique reflections. The (NH4)2Fe3+Cl5·H2O phase is orthorhombic, space group Pnma, unit cell parameters a = 13.725(2), b = 9.9365(16), c = 7.0370(11) Å and V = 959.7(3) Å3. The crystal structure of (NH4)2Fe3+Cl5·H2O was refined to R1 = 0.023 (wR2 = 0.066) on the basis of 2256 unique reflections. NH4MgCl3·6H2O is stable up to 90 °C and then transforms to the less hydrated phase isotypic to β-Rb(MnCl3)(H2O)2 (i.e., NH4MgCl3·2H2O), the latter phase being stable up to 150 °C. (NH4)2Fe3+Cl5·H2O is stable up to 120 °C and then transforms to an X-ray amorphous phase. Hydrogen bonds provide an important linkage between the main structural units and play the key role in determining structural stability and physical properties of the studied phases. The mineral phases NH4MgCl3·6H2O and (NH4)2Fe3+Cl5·H2O are isostructural with natural minerals novograblenovite and kremersite, respectively.

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Bosoite, a new silica clathrate mineral from Chiba Prefecture, Japan

Mineralogical Magazine ◽

10.1180/mgm.2020.91 ◽

2020 ◽

pp. 1-8

Author(s):

Koichi Momma ◽

Takuji Ikeda ◽

Toshiro Nagase ◽

Takahiro Kuribayashi ◽

Chibune Honma ◽

...

Keyword(s):

Crystal Structure ◽

Sedimentary Rocks ◽

X Ray Diffraction ◽

Unit Cell Parameters ◽

Average Model ◽

Guest Molecules ◽

Calculated Density ◽

X Ray ◽

Cell Parameters ◽

Chiba Prefecture

Abstract Bosoite (IMA2014-023) is a new silica clathrate mineral containing hydrocarbon molecules in its crystal structure. Bosoite can be considered structurally as a silica analogue of the structure-H gas hydrate, where guest molecules are trapped in cage-like voids constructed of the host framework. The mineral occurs in the Miocene tuffaceous sedimentary rocks at Arakawa, Minami-boso City, Chiba Prefecture, Japan. Bosoite is hexagonal, and it crystallises as an epitaxial intergrowth on chibaite crystals, with the {0001} of bosoite parallel to octahedral {111} form of chibaite. Crystals are colourless and transparent with vitreous lustre. The calculated density is 2.04 g/cm3. The empirical formula (based on 2 O apfu and guest molecules assumed as CH4) is Na0.01(Si0.98Al0.02)Σ1.00O2⋅0.50CH4; the end-member formula is SiO2⋅nC x H2x+2. Bosoite has the space group P6/mmm, with the unit-cell parameters a = 13.9020(3) Å, c = 11.2802(2) Å, V = 1887.99(6) Å3 and Z = 34. The crystal structure of bosoite was refined by single-crystal X-ray diffraction and converged to R1 = 4.26% for the average model and R1 = 2.96% for the model where all oxygen sites are split.

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Synthesis, Crystal Structure, and Solubility Analysis of a Famotidine Cocrystal

Crystals ◽

10.3390/cryst9070360 ◽

2019 ◽

Vol 9 (7) ◽

pp. 360 ◽

Cited By ~ 3

Author(s):

Yan Zhang ◽

Zhao Yang ◽

Shuaihua Zhang ◽

Xingtong Zhou

Keyword(s):

Crystal Structure ◽

Malonic Acid ◽

X Ray Diffraction ◽

Unit Cell Parameters ◽

H2 Receptor Antagonist ◽

Single Crystal Diffraction ◽

Intermolecular Hydrogen Bonds ◽

X Ray ◽

Cell Parameters ◽

Cocrystal Structure

A novel cocrystal of the potent H2 receptor antagonist famotidine (FMT) was synthesized with malonic acid (MAL) to enhance its solubility. The cocrystal structure was characterized by X-ray single crystal diffraction, and the asymmetry unit contains one FMT and one MAL connected via intermolecular hydrogen bonds. The crystal structure is monoclinic with a P21/n space group and unit cell parameters a = 7.0748 (3) Å, b = 26.6502 (9) Å, c = 9.9823 (4) Å, α = 90, β = 104.2228 (12), γ = 90, V = 1824.42 (12) Å3, and Z = 4. The cocrystal had unique thermal, spectroscopic, and powder X-ray diffraction (PXRD) properties that differed from FMT. The solubility of the famotidine-malonic acid cocrystal (FMT-MAL) was 4.2-fold higher than FMT; the FAM-MAL had no change in FMT stability at high temperature, high humidity, or with illumination.

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