Synthesis and X-ray diffraction data of (4R)-methyl-3-(1-(4-chlorophenyl)-1H-1,2,3-triazole-4-carbonyl)thiazolidin-4-carboxylate, C14H13ClN4O3S

The new compound (4R)-methyl-3-(1-(4-chlorophenyl)-1H-1,2,3-triazole-4-carbonyl)thiazolidin-4-carboxylate was synthesized by the 1,3-dipolar cycloaddition reaction between (4R)-methyl-3-propionyl-thiazolidin-4-carboxylate (1) and 4-chlorophenylazide using the click chemistry approach. Molecular characterization was carried out by infrared spectroscopy and mass spectrometry. The X-ray powder diffraction study determined that the title compound crystallized in an orthorhombic system with unit-cell parameters a = 20.876 (2) Å, b = 12.111 (1) Å, and c = 6.288 (9) Å. The volume of the unit cell is V = 1589.7 (2) Å3. All measured diffraction maxima were indexed and are consistent with the P2221 space group (No. 17). No detectable impurities were observed.

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Synthesis and X-ray diffraction data of 2-ethyl-6-(pyridin-4-yl)-7H-indeno[2,1-c]quinoline

Powder Diffraction ◽

10.1017/s0885715613000730 ◽

2013 ◽

Vol 29 (1) ◽

pp. 53-57

Author(s):

H.A. Camargo ◽

A. Sánchez ◽

J.A. Henao ◽

Arnold R. Romero Bohórquez ◽

Vladimir V. Kouznetsov

Keyword(s):

Elemental Sulfur ◽

Cycloaddition Reaction ◽

Unit Cell ◽

Gas Chromatography Mass Spectrometry ◽

X Ray Diffraction ◽

Unit Cell Parameters ◽

Monoclinic System ◽

X Ray ◽

Cell Parameters ◽

Xrpd Pattern

The compound 2-ethyl-6-(pyridin-4-yl)-7H-indeno[2,1-c]quinoline (2) (chemical formula C23H22N2) was synthesized through the free-solvent oxidation reaction mediated by elemental sulfur from the corresponding 2-ethyl-6-(pyridin-4-yl)-5,6,6a,11b-tetrahidro-7H-indeno[2,1-c]quinoline (1), an adduct easily obtained, using the Lewis acid-promoted [4 + 2] cycloaddition reaction. Preliminary molecular characterization was performed by Fourier transform-infrared and gas chromatography-mass spectrometry. The X-ray powder diffraction (XRPD) pattern for the title compound was analyzed and found to be crystallized in monoclinic system, space groupP21/n(N° 14) with refined unit-cell parametersa = 20.795 (8) Å,b = 7.484 (2) Å,c = 10.787 (2) Å andß = 93.96° (2). The volume of the unit cell isV = 1674.8 (6) Å3.

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Powder diffraction investigations of 2,2′-Thiobis(4-methyl-6-tert-butylphenol) and 2,2′-Methylenebis(4-methyl-6-tert-butylphenol)

Powder Diffraction ◽

10.1154/1.1835961 ◽

2005 ◽

Vol 20 (1) ◽

pp. 67-70

Author(s):

B. Lasocha ◽

M. Grzywa ◽

W. Lasocha

Keyword(s):

Room Temperature ◽

Unit Cell ◽

X Ray Diffraction ◽

Unit Cell Parameters ◽

Monoclinic System ◽

Orthorhombic System ◽

Space Group ◽

X Ray ◽

Cell Parameters ◽

Phenol Derivatives

X-ray diffraction investigations of two phenol derivatives - 2,2′-Thiobis(4-methyl-6-tert-butylphenol) and 2,2′-Methylenebis(4-methyl-6-tert-butylphenol) were carried out. Both compounds at room temperature have similar cell volume and the same number of molecules in an unit cell. However, 2,2′-Thiobis(4-methyl-6-tert-butylphenol) crystallizes in the monoclinic system with unit cell parameters refined to a=0.8278(2) nm, b=1.2968(4) nm, c=1.9493(7) nm, β=90.93(2)°, space group P21∕n(14), whereas 2,2′-Methylenebis(4-methyl-6-tert-butylphenol) crystallizes in the orthorhombic system with unit cell parameters refined to a=1.6203(5) nm, b=1.2827(5) nm, c=1.0197(3) nm, space group Pna21(33). The investigated C22H30O2S turned out to be a new polymorph of 2,2′-Thiobis(4-methyl-6-tert-butylphenol).

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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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Compressibility of β-As4S4: an in situ high-pressure single-crystal X-ray study

Mineralogical Magazine ◽

10.1180/minmag.2012.076.4.12 ◽

2012 ◽

Vol 76 (4) ◽

pp. 963-973 ◽

Cited By ~ 6

Author(s):

G. O. Lepore ◽

T. Boffa Ballaran ◽

F. Nestola ◽

L. Bindi ◽

D. Pasqual ◽

...

Keyword(s):

Pressure Range ◽

Substantial Reduction ◽

Structural Data ◽

Unit Cell ◽

Van Der Waals Interactions ◽

X Ray Diffraction ◽

Unit Cell Parameters ◽

X Ray ◽

Cell Parameters ◽

Intermolecular Distances

AbstractAmbient temperature X-ray diffraction data were collected at different pressures from two crystals of β-As4S4, which were made by heating realgar under vacuum at 295ºC for 24 h. These data were used to calculate the unit-cell parameters at pressures up to 6.86 GPa. Above 2.86 GPa, it was only possible to make an approximate measurement of the unit-cell parameters. As expected for a crystal structure that contains molecular units held together by weak van der Waals interactions, β-As4S4 has an exceptionally high compressibility. The compressibility data were fitted to a third-order Birch–Murnaghan equation of state with a resulting volume V0 = 808.2(2) Å3, bulk modulus K0 = 10.9(2) GPa and K' = 8.9(3). These values are extremely close to those reported for the low-temperature polymorph of As4S4, realgar, which contains the same As4S4 cage-molecule. Structural analysis showed that the unit-cell contraction is due mainly to the reduction in intermolecular distances, which causes a substantial reduction in the unit-cell volume (∼21% at 6.86 GPa). The cage-like As4S4 molecules are only slightly affected. No phase transitions occur in the pressure range investigated.Micro-Raman spectra, collected across the entire pressure range, show that the peaks associated with As–As stretching have the greatest pressure dependence; the S–As–S bending frequency and the As–S stretching have a much weaker dependence or no variation at all as the pressure increases; this is in excellent agreement with the structural data.

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Crystallization and X-ray diffraction analysis of native and selenomethionine-substituted PhyH-DI fromBacillussp. HJB17

Acta Crystallographica Section F Structural Biology Communications ◽

10.1107/s2053230x17015102 ◽

2017 ◽

Vol 73 (11) ◽

pp. 607-611

Author(s):

Fang Lu ◽

Bei Zhang ◽

Yong Liu ◽

Ying Song ◽

Gangxing Guo ◽

...

Keyword(s):

Unit Cell ◽

Diffusion Method ◽

Data Sets ◽

Asymmetric Unit ◽

X Ray Diffraction ◽

Unit Cell Parameters ◽

Solvent Content ◽

Space Group ◽

X Ray ◽

Cell Parameters

Phytases are phosphatases that hydrolyze phytates to less phosphorylatedmyo-inositol derivatives and inorganic phosphate. β-Propeller phytases, which are very diverse phytases with improved thermostability that are active at neutral and alkaline pH and have absolute substrate specificity, are ideal substitutes for other commercial phytases. PhyH-DI, a β-propeller phytase fromBacillussp. HJB17, was found to act synergistically with other single-domain phytases and can increase their efficiency in the hydrolysis of phytate. Crystals of native and selenomethionine-substituted PhyH-DI were obtained using the vapour-diffusion method in a condition consisting of 0.2 Msodium chloride, 0.1 MTris pH 8.5, 25%(w/v) PEG 3350 at 289 K. X-ray diffraction data were collected to 3.00 and 2.70 Å resolution, respectively, at 100 K. Native PhyH-DI crystals belonged to space groupC121, with unit-cell parametersa = 156.84,b = 45.54,c = 97.64 Å, α = 90.00, β = 125.86, γ = 90.00°. The asymmetric unit contained two molecules of PhyH-DI, with a corresponding Matthews coefficient of 2.17 Å3 Da−1and a solvent content of 43.26%. Crystals of selenomethionine-substituted PhyH-DI belonged to space groupC2221, with unit-cell parametersa = 94.71,b= 97.03,c= 69.16 Å, α = β = γ = 90.00°. The asymmetric unit contained one molecule of the protein, with a corresponding Matthews coefficient of 2.44 Å3 Da−1and a solvent content of 49.64%. Initial phases for PhyH-DI were obtained from SeMet SAD data sets. These data will be useful for further studies of the structure–function relationship of PhyH-DI.

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The structures of marialite (Me6) and meionite (Me93) in space groups P42/n and I4/m, and the absence of phase transitions in the scapolite series

Powder Diffraction ◽

10.1154/1.3582802 ◽

2011 ◽

Vol 26 (2) ◽

pp. 119-125 ◽

Cited By ~ 1

Author(s):

Sytle M. Antao ◽

Ishmael Hassan

Keyword(s):

Phase Transitions ◽

High Resolution ◽

Crystal Structures ◽

Unit Cell ◽

X Ray Diffraction ◽

Unit Cell Parameters ◽

X Ray ◽

Space Groups ◽

Cell Parameters ◽

The Mean

The crystal structures of marialite (Me6) from Badakhshan, Afghanistan and meionite (Me93) from Mt. Vesuvius, Italy were obtained using synchrotron high-resolution powder X-ray diffraction (HRPXRD) data and Rietveld structure refinements. Their structures were refined in space groups I4/m and P42/n, and similar results were obtained. The Me6 sample has a formula Ca0.24Na3.37K0.24[Al3.16Si8.84O24]Cl0.84(CO3)0.15, and its unit-cell parameters are a=12.047555(7), c=7.563210(6) Å, and V=1097.751(1) Å3. The average ⟨T1-O⟩ distances are 1.599(1) Å in I4/m and 1.600(2) Å in P42/n, indicating that the T1 site contains only Si atoms. In P42/n, the average distances of ⟨T2-O⟩=1.655(2) and ⟨T3-O⟩=1.664(2) Å are distinct and are not equal to each other. However, the mean ⟨T2,3-O⟩=1.659(2) Å in P42/n and is identical to the ⟨T2′-O⟩=1.659(1) Å in I4/m. The ⟨M-O⟩ [7]=2.754(1) Å (M site is coordinated to seven framework O atoms) and M-A=2.914(1) Å; these distances are identical in both space groups. The Me93 sample has a formula of Na0.29Ca3.76[Al5.54Si6.46O24]Cl0.05(SO4)0.02(CO3)0.93, and its unit-cell parameters are a=12.19882(1), c=7.576954(8) Å, and V=1127.535(2) Å3. A similar examination of the Me93 sample also shows that both space groups give similar results; however, the C–O distance is more reasonable in P42/n than in I4/m. Refining the scapolite structure near Me0 or Me100 in I4/m forces the T2 and T3 sites (both with multiplicity 8 in P42/n) to be equivalent and form the T2′ site (with multiplicity 16 in I4/m), but ⟨T2-O⟩ is not equal to ⟨T3-O⟩ in P42/n. Using different space groups for different regions across the series implies phase transitions, which do not occur in the scapolite series.

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The solid solution TbNiIn1−x Ga x

Zeitschrift für Naturforschung B ◽

10.1515/znb-2021-0167 ◽

2021 ◽

Vol 0 (0) ◽

Author(s):

Myroslava Horiacha ◽

Galyna Nychyporuk ◽

Rainer Pöttgen ◽

Vasyl Zaremba

Keyword(s):

Solid Solution ◽

Unit Cell ◽

Type Structure ◽

X Ray Diffraction ◽

Unit Cell Parameters ◽

Space Group ◽

X Ray ◽

Cell Parameters ◽

Structure Space ◽

Arc Melting

Abstract Phase formation in the solid solution TbNiIn1−x Ga x at 873 K was investigated in the full concentration range by means of powder X-ray diffraction and EDX analysis. The samples were synthesized by arc-melting of the pure metals with subsequent annealing at 873 K for one month. The influence of the substitution of indium by gallium on the type of structure and solubility was studied. The solubility ranges have been determined and changes of the unit cell parameters were calculated on the basis of powder X-ray diffraction data: TbNiIn1–0.4Ga0–0.6 (ZrNiAl-type structure, space group P 6 ‾ 2 m $P‾{6}2m$ , a = 0.74461(8)–0.72711(17) and c = 0.37976(5)–0.37469(8) nm); TbNiIn0.2–0Ga0.8–1.0 (TiNiSi-type structure, space group Pnma, а = 0.68950(11)–0.68830(12), b = 0.43053(9)–0.42974(6), с = 0.74186(10)–0.73486(13) nm). The crystal structures of TbNiGa (TiNiSi type, Pnma, a = 0.69140(5), b = 0.43047(7), c = 0.73553(8) nm, wR2=0.0414, 525 F 2 values, 21 variables), TbNiIn0.83(1)Ga0.17(1) (ZrNiAl type, P 6 ‾ 2 m $P‾{6}2m$ , a = 0.74043(6), c = 0.37789(3) nm, wR2 = 0.0293, 322 F 2 values, 16 variables) and TbNiIn0.12(2)Ga0.88(2) (TiNiSi type, Pnma, a = 0.69124(6), b = 0.43134(9), c = 0.74232(11) nm, wR2 = 0.0495, 516 F 2 values, 21 variables) have been determined. The characteristics of the solid solutions and the variations of the unit cell parameters are briefly 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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Layer stacking disorder in Mg-Fe chlorites based on powder X-ray diffraction data

American Mineralogist ◽

10.2138/am-2020-6982 ◽

2020 ◽

Vol 105 (3) ◽

pp. 353-362

Author(s):

Katarzyna Luberda-Durnaś ◽

Marek Szczerba ◽

Małgorzata Lempart ◽

Zuzanna Ciesielska ◽

Arkadiusz Derkowski

Keyword(s):

Accurate Determination ◽

Unit Cell ◽

Powder Xrd ◽

X Ray Diffraction ◽

Unit Cell Parameters ◽

Xrd Pattern ◽

X Ray ◽

Cell Parameters ◽

Layer Stacking

Abstract The primary aim of this study was the accurate determination of unit-cell parameters and description of disorder in chlorites with semi-random stacking using common X-ray diffraction (XRD) data for bulk powder samples. In the case of ordered chlorite structures, comprehensive crystallographic information can be obtained based on powder XRD data. Problems arise for samples with semi-random stacking, where due to strong broadening of hkl peaks with k ≠ 3n, the determination of unit-cell parameters is demanding. In this study a complete set of information about the stacking sequences in chlorite structures was determined based on XRD pattern simulation, which included determining a fraction of layers shifted by ±1/3b, interstratification with different polytypes and 2:1 layer rotations. A carefully selected series of pure Mg-Fe tri-trioctahedral chlorites with iron content in the range from 0.1 to 3.9 atoms per half formula unit cell was used in the study. In addition, powder XRD patterns were carefully investigated for the broadening of the odd-number basal reflections to determine interstratification of 14 and 7 Å layers. These type of interstratifications were finally not found in any of the samples. This result was also confirmed by the XRD pattern simulations, assuming interstratification with R0 ordering. Based on h0l XRD reflections, all the studied chlorites were found to be the IIbb polytype with a monoclinic-shaped unit cell (β ≈ 97°). For three samples, the hkl reflections with k ≠ 3n were partially resolvable; therefore, a conventional indexing procedure was applied. Two of the chlorites were found to have a monoclinic cell (with α, γ = 90°). Nevertheless, among all the samples, the more general triclinic (pseudomonoclinic) crystal system with symmetry C1 was assumed, to calculate unit-cell parameters using Le Bail fitting. A detailed study of semi-random stacking sequences shows that simple consideration of the proportion of IIb-2 and IIb-4/6 polytypes, assuming equal content of IIb-4 and IIb-6, is not sufficient to fully model the stacking structure in chlorites. Several, more general, possible models were therefore considered. In the first approach, a parameter describing a shift into one of the ±1/3b directions (thus, the proportion of IIb-4 and IIb-6 polytypes) was refined. In the second approach, for samples with slightly distinguishable hkl reflections with k ≠ 3n, some kind of segregation of individual polytypes (IIb-2/4/6) was considered. In the third approach, a model with rotations of 2:1 layers about 0°, 120°, 240° was shown to have the lowest number of parameters to be optimized and therefore give the most reliable fits. In all of the studied samples, interstratification of different polytypes was revealed with the fraction of polytypes being different than IIbb ranging from 5 to 19%, as confirmed by fitting of h0l XRD reflections.

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Structure and properties of solid solutions in the Mg-Al-B system

Open Physics ◽

10.2478/s11534-011-0013-8 ◽

2012 ◽

Vol 10 (1) ◽

Cited By ~ 4

Author(s):

Ludmila Sevastyanova ◽

Olga Gulish ◽

Vladimir Stupnikov ◽

Vladimir Genchel ◽

Oleg Kravchenko ◽

...

Keyword(s):

Solid Solutions ◽

Unit Cell ◽

Superconducting Transition ◽

Structure And Properties ◽

X Ray Diffraction ◽

Unit Cell Parameters ◽

X Ray ◽

Cell Parameters ◽

Resistivity Measurements ◽

Ceramic Synthesis

AbstractCompounds with the general formula Mg1−x AlxB2 were obtained by two-step ceramic synthesis. All compounds were characterized by X-ray diffraction, NMR spectroscopy, and by four point probe resistivity measurements in various magnetic fields method. The diborides unit cell parameters were determined as a function of the Al mole fraction. With the vaues of x up to 0.40 (where x is the composition of the stock prepared for sintering), the unit cell parameters of Mg1−x AlxB2 are similar to those of pure MgB2 and the superconducting transition temperature was lowered. For stock compositions of 0:25 ≤ x ≤ 0:60, the products contain a superstructure, also superconducting phase, which becomes the only product at x = 0:50, and at x > 0:60 this phase is replaced by AlB2-based solid solutions.

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