Crystal structure from laboratory X-ray powder diffraction data, DFT-D calculations, Hirshfeld surface analysis, and energy frameworks of a new polymorph of 1-benzothiophene-2-carboxylic acid

2021 ◽  
pp. 1-12
Author(s):  
Analio J. Dugarte-Dugarte ◽  
Jacco van de Streek ◽  
Graciela Díaz de Delgado ◽  
Alicja Rafalska-Lasocha ◽  
José Miguel Delgado
Keyword(s):  
Crystal Structure ◽  
Carboxylic Acid ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Rietveld Method ◽  
Hirshfeld Surface ◽  
Powder Diffraction Data ◽  
Pharmacological Activities ◽  
X Ray ◽  
Acid Acid

Several benzothiophene-based compounds, including 1-benzothiophene-2-carboxylic acid, exhibit a wide variety of pharmacological activities. They have been extensively used to treat various types of diseases with high therapeutic effectiveness. In this contribution, the crystal structure of a new polymorph of 1-benzothiophene-2-carboxylic acid (BTCA) was determined from laboratory X-ray powder diffraction data with DASH, refined by the Rietveld method with TOPAS-Academic, and optimized using DFT-D calculations. The new form of 1-benzothiophene-2-carboxylic acid crystallizes in space group C2/c (No. 15) with a = 14.635(4), b = 5.8543(9), c = 19.347(3) Å, β = 103.95(1)°, V = 1608.8(6) Å3, and Z = 8. The structure is a complex 3D arrangement which can be described in terms of hydrogen-bonded dimers of BTCA molecules, joined by the acid–acid homosynthon, which interact through C–H⋯O hydrogen bonds to produce tapes further connected through head-to-tail π⋯π and edge-to-face C–H⋯π interactions. A comparison with a previously reported triclinic polymorph and with the related 1-benzofuran-2-carboxylic acid (BFCA) is also presented.

Crystallographic study of ternary ordered skutterudite IrGe1.5Se1.5

2010 ◽  
Vol 25 (3) ◽  
pp. 247-252 ◽  
Author(s):  
F. Laufek ◽  
J. Návrátil
Keyword(s):  
Crystal Structure ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Rietveld Method ◽  
Crystallographic Data ◽  
Powder Diffraction Data ◽  
X Ray ◽  
Crystallographic Study ◽  
Related Phase ◽  
The Ideal

The crystal structure of skutterudite-related phase IrGe1.5Se1.5 has been refined by the Rietveld method from laboratory X-ray powder diffraction data. Refined crystallographic data for IrGe1.5Se1.5 are a=12.0890(2) Å, c=14.8796(3) Å, V=1883.23(6) Å3, space group R3 (No. 148), Z=24, and Dc=8.87 g/cm3. Its crystal structure can be derived from the ideal skutterudite structure (CoAs3), where Se and Ge atoms are ordered in layers perpendicular to the [111] direction of the original skutterudite cell. Weak distortions of the anion and cation sublattices were also observed.

Powder diffraction data of two tricydic diazonia diiodide salts used in silver iodide solid electrolytes

1993 ◽  
Vol 8 (3) ◽  
pp. 175-179
Author(s):  
J. Estienne ◽  
O. Cerclier ◽  
J. J. Rosenberg
Keyword(s):  
Crystal Structure ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Silver Iodide ◽  
Solid Electrolytes ◽  
Rietveld Method ◽  
Powder Diffraction Data ◽  
Organic Salts ◽  
X Ray ◽  
Structure Determinations

Indexed X-ray powder diffraction data are reported for two organic salts with carbon rings having two quaternary nitrogens: diazonia-6,9 dispiro [5.2.5.2] hexadecane and diazonia-6,9 dispiro [5.2.5.3] heptadecane diiodides. For these compounds, which give solid electrolytes when associated with AgI, powder diffraction diagrams calculated by the Rietveld method from single crystal structure determinations are presented and are compared to the experimental diffraction data.

Cristobalite-Related Phases in the NaAlO2–NaAlSiO4 System. II. A Commensurately Modulated Cubic Structure

1998 ◽  
Vol 54 (5) ◽  
pp. 547-557 ◽  
Author(s):  
R. L. Withers ◽  
J. G. Thompson ◽  
A. Melnitchenko ◽  
S. R. Palethorpe
Keyword(s):  
Crystal Structure ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Rietveld Method ◽  
Powder Diffraction Data ◽  
Tetrahedral Framework ◽  
X Ray ◽  
Sodium Aluminosilicate ◽  
Vacancy Ordering ◽  
Cubic Structure

The crystal structure of a new cubic cristobalite-related sodium aluminosilicate Na1.45Al1.45Si0.55O4 [P213, a = 14.553 (1) Å] has been modelled using a modulation wave approach and the model tested against X-ray powder diffraction data using the Rietveld method. Owing to there being 64 independent positional parameters and eight independent Na sites, refinement of the tetrahedral framework atom positions and Na occupancies was not possible. The framework was modelled successfully in terms of q 1 = 1\over 4〈020〉_p^*-type (p = parent) modulation waves with the requirement that the MO4 (M = Al0.725Si0.275) tetrahedra be as close to regular as possible. Na/vacancy ordering was modelled successfully in terms of q 2 = 1\over 4〈220〉_p^* modulation waves. Only the Na-atom positions were refined. The significance of this unique modulated cubic cristobalite-related structure and the possible insight it provides to understanding β-cristobalite are discussed.

Ab initio determination and Rietveld refinement of the crystal structure of Ni0.50TiO(PO4)

1999 ◽  
Vol 14 (1) ◽  
pp. 10-15 ◽  
Author(s):  
P. Gravereau ◽  
J. P. Chaminade ◽  
B. Manoun ◽  
S. Krimi ◽  
A. El Jazouli
Keyword(s):  
Crystal Structure ◽  
Ab Initio ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Rietveld Method ◽  
Heavy Atom ◽  
Monoclinic Space Group ◽  
Powder Diffraction Data ◽  
X Ray ◽  
Heavy Atom Method

The structure of the oxyphosphate Ni0.50TiO(PO4) has been determined ab initio from conventional X-ray powder diffraction data by the “heavy atom” method. The cell is monoclinic (space group P21/c, Z=4) with a=7.3830(5) Å, b=7.3226(5) Å, c=7.3444(5) Å, and β=120.233(6)°. Refinement of 46 parameters by the Rietveld method, using 645 reflexions, leads to cRwp=0.152, cRp=0.120, and RB=0.043. The structure of Ni0.50TiO(PO4) can be described as a TiOPO4 framework constituted by chains of tilted corner-sharing TiO6 octahedra running parallel to the c axis, crosslinked by phosphate tetrahedra and in which one-half of octahedral cavities created are occupied by Ni atoms. Ti atoms are displaced from the center of octahedra units in alternating long (2.231) and short (1.703 Å) Ti–O bonds along chains.

Rietveld Structure Refinement of Metastable Lithium Disilicate Using Synchrotron X-Ray Powder Diffraction Data From the Daresbury SRS 8.3 Diffractometer

1990 ◽  
Vol 5 (3) ◽  
pp. 137-143 ◽  
Author(s):  
R.I. Smith ◽  
A.R. West ◽  
I. Abrahams ◽  
P.G. Bruce
Keyword(s):  
Crystal Structure ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Rietveld Method ◽  
Structure Refinement ◽  
Powder Diffraction Data ◽  
X Ray ◽  
New Instrument ◽  
Diffraction Peaks

AbstractThe crystal structure of metastable Li2Si2O5, Fw = 150.05, has been refined by the Rietveld method using high resolution X-ray powder diffraction data recorded at the Daresbury Synchrotron Radiation Source on the new 8.3 diffractometer. Li2Si2O5, in keeping with many compounds of interest to the materials scientist, exhibits relatively broad diffraction peaks. It is important to establish the quality of crystal structure data that may be obtained from such materials on this new instrument. Various functions were used to model the peak shape from this instrument; a split-Pearson VII function appeared to be marginally superior to Pearson VII or Pseudo-Voigt functions. Refinement was carried out using the split-Pearson VII in the space group Pbcn (60) and terminated with a = 5.6871(6), b = 4.7846(5), c = 14.645(1) Å, V = 398.50 Å3, Z=4, Dc= 2.502 gcm−3, Rwp = 17.06, Rex = 14.48 and Χ2 = 1.39. The refined parameters are compared with those obtained from a previous single crystal X-ray determination.

Crystal structure of Cu doped La0.67Ca0.33MnO3 by Rietveld refinement

2004 ◽  
Vol 19 (4) ◽  
pp. 329-332
Author(s):  
H. L. Cai ◽  
X. S. Wu ◽  
F. Z. Wang ◽  
A. Hu ◽  
S. S. Jiang ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Magnetic Properties ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Structural Changes ◽  
Rietveld Method ◽  
Crystal Data ◽  
Powder Diffraction Data ◽  
Orthorhombic System ◽  
X Ray

The crystal structure of La0.67Ca0.33Mn0.80Cu0.20O3 (LCMCO) compound was determined from laboratory X-ray powder diffraction data and refined by the Rietveld method. LCMCO is isostructural with La0.67Ca0.33MnO3 (LCMO). The crystal data are: La0.64Ca0.36Mn0.82Cu0.18O3.01, Mr=843.80, orthorhombic system, space group Pnma, a=5.4364(1) Å, b=7.6725(2) Å, c=5.4452(1) Å, V=227.124(8)Å3, Z=4, Dx=6.168 g∕cm3. In comparing with the Cu-free compound, subtle structural changes such as bond lengths and bond angles found in the Cu-doped compound may be responsible for the larger effects on the transport and magnetic properties when Cu partially substitutes for Mn in CMCO.

Crystal structure and powder diffraction pattern of high-temperature modification of Pd73Sn14Te13

2007 ◽  
Vol 22 (4) ◽  
pp. 334-339 ◽  
Author(s):  
F. Laufek ◽  
A. Vymazalová ◽  
J. Plášil
Keyword(s):  
Crystal Structure ◽  
High Temperature ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Title Compound ◽  
Rietveld Method ◽  
Powder Diffraction Data ◽  
X Ray ◽  
Temperature Modification ◽  
High Temperature Modification

Crystal structure of high-temperature modification of Pd73Sn14Te13 has been refined by the Rietveld method from laboratory X-ray powder diffraction data. Refined crystallographic data of Pd73Sn14Te13 are a=7.6456(3) Å, c=13.9575(9) Å, V=706.75(6) Å3, space group P63cm (No. 185), Z=6, and Dx=10.71 g/cm3. The title compound is isostructural with Pd5Sb2 and Ni5As2; it can be considered as a stacking and filling variant of the Ni2In structure. An important structural feature in the high-temperature modification of Pd73Sn14Te13 is the presence of various Pd-Pd bonds.

Structure Re-determination of LASSBio-294 – a cardioactive compound of the N-acylhydrazone class – using X-ray powder diffraction data

2013 ◽  
Vol 28 (S2) ◽  
pp. S491-S509 ◽  
Author(s):  
Fanny N. Costa ◽  
Fabio Furlan Ferreira ◽  
Tiago F. da Silva ◽  
Eliezer J. Barreiro ◽  
Lídia M. Lima ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Goodness Of Fit ◽  
Rietveld Method ◽  
Therapeutic Interventions ◽  
Powder Diffraction Data ◽  
X Ray ◽  
Cell Parameters

Many N-acylhydrazone derivatives synthetized in LASSBio® cannot be prepared as single crystals of sufficient size and/or quality for structure determination to be carried out using single crystal X-ray diffraction techniques. This article highlights the opportunity for determining crystal structures of this class of compounds directly from powder diffraction data. For this task, the crystal structure of LASSBio-294 was re-determined by means of conventional X-ray powder diffraction data and so, compared with the crystal structure already determined for single crystal data. LASSBio-294 is a cardioactive compound of the N-acylhydrazone class, which can become part of the therapeutic interventions designed to decrease exertional fatigue, and, consequently, improve the quality of life of patients suffering from chronic heart failure. Its final crystal structure was refined by means of the Rietveld method (Rietveld, 1967; 1969). This drug crystallizes in a monoclinic (P21/c) space group, with unit cell parameters a = 11.3413(3) Å, b = 12.3573(4) Å, c = 9.0158(3) Å, β = 89.821(2)°, V = 1263.55(7) Å3, Z = 4, Ź = 1 and ρcalc = 1.4419(1) g cm−3. The goodness-of-fit indicator and R-factors were, respectively: χ2 = 1.203, RBragg = 0.696%, Rwp = 5.59%, Rexp = 4.65% and Rp = 4.18%. The molecules in LASSBio-294 are H-bonded along the c-axis involving the atoms N(3)–H(8)···O(4).

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