Crystal structure of semiorganic antimony thiourea bromide monohydrate crystals: a redetermination

2009 ◽  
Vol 87 (4) ◽  
pp. 345-348 ◽  
Author(s):  
Mahesha K. Upadhya ◽  
N. K. Udayashankar
Keyword(s):  
Crystal Structure ◽  
Single Crystals ◽  
Room Temperature ◽  
Direct Methods ◽  
Unit Cell ◽  
Unit Cell Parameters ◽  
Orthorhombic Space Group ◽  
Cell Parameters ◽  
Evaporation Technique ◽  
R Value

The growth of antimony thiourea bromide monohydrate (ATBM) single crystals by evaporation technique at room temperature is reported here. Antimony thiourea bromide monohydrate crystallizes in the orthorhombic space group Cmca with unit cell parameters a = 12.320(7) Å, b = 11.668(7) Å, c = 18.615(11), and z = 8. The structure has been solved by direct methods and refined to a final R value of 0.0239.

scholarly journals The crystal structure of alstonite, BaCa(CO3)2: an extraordinary example of ‘hidden’ complex twinning in large single crystals

2020 ◽  
Vol 84 (5) ◽  
pp. 699-704
Author(s):  
Luca Bindi ◽  
Andrew C. Roberts ◽  
Cristian Biagioni
Keyword(s):  
Crystal Structure ◽  
Single Crystals ◽  
Structure Determination ◽  
Unit Cell ◽  
Crystal Structure Determination ◽  
Unit Cell Parameters ◽  
Space Group ◽  
Cell Parameters ◽  
Structure Determinations

AbstractAlstonite, BaCa(CO3)2, is a mineral described almost two centuries ago. It is widespread in Nature and forms magnificent cm-sized crystals. Notwithstanding, its crystal structure was still unknown. Here, we report the crystal-structure determination of the mineral and discuss it in relationship to other polymorphs of BaCa(CO3)2. Alstonite is trigonal, space group P31m, with unit-cell parameters a = 17.4360(6), c = 6.1295(2) Å, V = 1613.80(9) Å3 and Z = 12. The crystal structure was solved and refined to R1 = 0.0727 on the basis of 4515 reflections with Fo > 4σ(Fo) and 195 refined parameters. Alstonite is formed by the alternation, along c, of Ba-dominant and Ca-dominant layers, separated by CO3 groups parallel to {0001}. The main take-home message is to show that not all structure determinations of minerals/compounds can be solved routinely. Some crystals, even large ones displaying excellent diffraction quality, can be twinned in complex ways, thus making their study a crystallographic challenge.

Tetra-n-butylammonium iodide: a space-group revision

2007 ◽  
Vol 63 (3) ◽  
pp. o1464-o1466 ◽  
Author(s):  
Wiesław Prukała ◽  
Bogdan Marciniec ◽  
Maciej Kubicki
Keyword(s):  
Crystal Structure ◽  
Room Temperature ◽  
Unit Cell ◽  
Unit Cell Parameters ◽  
Space Group ◽  
Cell Parameters ◽  
Temperature Determination

The crystal structure of tetra-n-butylammonium iodide, C16H36N+·I−, has been redetermined at room temperature and at 100 (1) K. In the low-quality (R = 0.142) room-temperature determination by Wang, Habenschuss, Xenopoulos & Wunderlich [Mol. Cryst. Liq. Cryst. Sci. Technol. Sect. A (1995), 264, 115–129], this structure was described as crystallizing in the space group C2 with Z′ = 2. Our results prove that the correct space group is C2/c (with the same unit-cell parameters as in the original determination) at both temperatures. In the crystal structure, the iodide anions fill the voids in the grid-like cationic structure. Weak C—H...I interactions (eight per anion) strengthen this packing.

Redefinition of satimolite

2018 ◽  
Vol 82 (5) ◽  
pp. 1033-1047 ◽  
Author(s):  
Igor V. Pekov ◽  
Natalia V. Zubkova ◽  
Dmitry A. Ksenofontov ◽  
Nikita V. Chukanov ◽  
Vasiliy O. Yapaskurt ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Rietveld Method ◽  
Three Dimensional ◽  
Direct Methods ◽  
Salt Dome ◽  
Unit Cell ◽  
Unit Cell Parameters ◽  
Cell Parameters ◽  
Octahedral Clusters

ABSTRACTThe borate mineral satimolite, which was first described in 1969 and remained poorly-studied until now, has been re-investigated (electron microprobe analysis, single-crystal and powder X-ray diffraction studies, crystal-structure determination, infrared spectroscopy) and redefined based on the novel data obtained for the holotype material from the Satimola salt dome and a recently found sample from the Chelkar salt dome, both in North Caspian Region, Western Kazakhstan. The revised idealized formula of satimolite is KNa2(Al5Mg2)[B12O18(OH)12](OH)6Cl4·4H2O (Z = 3). The mineral is trigonal, space group R$\bar{3}$m, unit-cell parameters are: a = 15.1431(8), c = 14.4558(14) Å and V = 2870.8(4) Å3 (Satimola) and a = 15.1406(4), c = 14.3794(9) Å and V = 2854.7(2) Å3 (Chelkar). The crystal system and unit-cell parameters are quite different from those reported previously. The crystal structure of the sample from Chelkar was solved based on single-crystal data (direct methods, R = 0.0814) and the structure of the holotype from Satimola was refined on a powder sample by the Rietveld method (Rp = 0.0563, Rwp = 0.0761 and Rall = 0.0667). The structure of satimolite is unique for minerals. It contains 12-membered borate rings [B12O18(OH)12] in which BO3 triangles alternate with BO2(OH)2 tetrahedra sharing common vertices, and octahedral clusters [M7O6(OH)18] with M = Al5Mg2 in the ideal case, with sharing of corners between rings and clusters to form a three-dimensional heteropolyhedral framework. Each borate ring is connected with six octahedral clusters: three under the ring and three over the ring. Large ellipsoidal cages in the framework host Na and K cations, Cl anions and H2O molecules.

Crystal structure and topological affinities of magbasite, KBaFe3+Mg7Si8O22(OH)2F6: a trellis structure related to amphibole and carpholite

2014 ◽  
Vol 78 (1) ◽  
pp. 29-45 ◽  
Author(s):  
M. D. Welch ◽  
R. H. Mitchell ◽  
A. R. Kampf ◽  
A. R. Chakhmouradian ◽  
D. Smith ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Unit Cell ◽  
Unit Cell Parameters ◽  
Carbonatite Complex ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
Cell Parameters ◽  
Structural Relations ◽  
Final Agreement

AbstractThe crystal structure of magbasite from the Eldor carbonatite complex, Quebec, Canada, has been determined and indicates that the currently accepted formula should be revised to KBaFe3+Mg7Si8O22(OH)2F6. Magbasite is orthorhombic, space group Cmme (Cmma), with unit-cell parameters a 18.9506(3) Å, b 22.5045(3) Å, c 5.2780(1) Å, V 2250.93(6) Å3 (Z = 4). The structure has been solved and refined to final agreement indices R1 = 0.026, wR2 = 0.052, GooF = 1.116 for a total of 2379 unique reflections, and is a new kind of trellis motif related to amphibole and carpholite topologies. An amphibole-like I-beam ‖(100) of edge-sharing octahedrally-coordinated M(1,2,3) sites, which are filled by Mg, is sandwiched between double-chains of SiO4 tetrahedra ‖c. This I-beam is connected to side-ribbons ‖(010) of edge-sharing (Mg,Fe2+)O4(OH,F)2 and Fe3+O4(OH)2 octahedra to form a tunnelled box or trellis structure very like that of carpholite, for which the I-beams are pyroxene-like. K occupies a tunnel site analogous to the A site of amphibole. Ba occupies a cavity site at the corners where the I-beam and side-ribbon meet, and corresponds to the A site of carpholite. The structural relations between magbasite and carpholite are discussed.

scholarly journals Synthesis, Crystal structure, Vibrational, Optical and Dielectric properties Of 2-(2-Aminoethyl)-1-methylpyrrolidinum chloride hexachlorobismuthate (III) monohydrate [C7H18N2]2ClBiCl6.H2O

2013 ◽  
Vol 9 (3) ◽  
pp. 2005-2022 ◽  
Author(s):  
Fayçal Ben Tahar ◽  
Chakib Hrizi ◽  
Slaheddine Chaabouni ◽  
Nassira Chniba-Boudjada ◽  
Nicolas Ratel Ramond ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Dielectric Properties ◽  
Room Temperature ◽  
Three Dimensional ◽  
Free Water ◽  
Unit Cell ◽  
Water Molecules ◽  
Unit Cell Parameters ◽  
Cell Parameters ◽  
Vis Spectroscopy

Synthesis, crystal structure, vibrational and dielectric properties of [C7H18N2]2ClBiCl6.H2O are reported. The compound crystallizes at room temperature in the orthorhombic system, space group P212121, with the following unit cell parameters : a = 7.5500(6) Å, b = 18.3780(2) Å, c = 19.8980(13) Å, V = 2760.9(4) Å3 and four molecules per unit cell. The structure has been solved by three-dimensional Patterson synthesis and refined by least-squares analysis (R1 = 0.0463, wR2 = 0.0764). The crystal structure of the title compound, [C7H18N2]2ClBiCl6.H2O consists of 2-(2-Aminoethyl)-1-methylpyrrolidinium cations, [BiCl6]3- anions, Cl- anions and free water molecules. The Bi(III) cation is coordinated by six Cl- anions in slightly distorsed octahedral geometry. In the crystal, extensive intermolecular N-H…Cl hydrogen bonds occur. The charge-transfer (CT) interactions between 2-(2-Aminoethyl)-1-methylpyrrolidinium cation and the anionic hosts have been revealed by structural analysis and UV-vis spectroscopy. The dielectric properties have been investigated at temperature range from 100 to 300 K at various frequencies (1 KHz – 1 MHz). The evolution of dielectric constant as a function of temperature and frequency of pellet has been investigated in order to determine some related parameters.

The crystal structure of Cu2GeSe3 and the structure-types of the I2-IV-VI3 family of semiconducting compounds

2021 ◽  
Vol 77 (1) ◽  
pp. 158-167
Author(s):  
Analio Dugarte-Dugarte ◽  
Nahum Ramírez Pineda ◽  
Luis Nieves ◽  
José Antonio Henao ◽  
Graciela Díaz de Delgado ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
Unit Cell Parameters ◽  
Orthorhombic Space Group ◽  
Initial Report ◽  
Space Group ◽  
Cell Parameters ◽  
Semiconducting Compounds ◽  
Bond Valence Model

Almost 50 years after the initial report, the crystal structure of Cu2GeSe3, a I2-IV-VI3 semiconductor, has been revised using modern single-crystal X-ray diffraction data. The structure of this material can be properly described in the monoclinic space group Cc (No. 9) with unit-cell parameters a = 6.7703 (4) Å, b = 11.8624 (5) Å, c = 6.7705 (4) Å, β = 108.512 (6)°, V = 515.62 (5) Å3, Z = 4, rather than in the orthorhombic space group Imm2 (No. 44) with unit-cell parameters a = 11.860 (3), b = 3.960 (1), c = 5.485 (2) Å, V = 257.61 Å3, Z = 2, as originally proposed [Parthé & Garín (1971). Monatsh. Chem. 102, 1197–1208]. Contrary to what was observed in the orthorhombic structure, the distortions of the tetrahedra in the monoclinic structure are consistent with the distortions expected from considerations derived from the bond valence model. A brief revision of the structures reported for the I2-IV-VI3 family of semiconducting compounds (I: Cu, Ag; IV: Si, Ge, Sn; and VI: S, Se, Te) is also presented.

scholarly journals Synthesis, Crystal structure of hepta (pyridinium) bis (hexachlorobismuthate (III)) nitrate [C5H6N]7(BiCl6)2(NO3)

2013 ◽  
Vol 9 (2) ◽  
pp. 1975-1987
Author(s):  
Ben Tahar Fayçal ◽  
Perez Olivier ◽  
Slaheddine Chaabouni
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Title Compound ◽  
Room Temperature ◽  
Three Dimensional ◽  
Unit Cell ◽  
Unit Cell Parameters ◽  
Monoclinic System ◽  
Cell Parameters ◽  
Dimensional Network

An hepta (pyridinium) bis (hexachlorobismuthate (III)) nitrate, (C5H6N)7(BiCl6)2(NO3) crystallizes at room temperature in the monoclinic system, space group P21/n, with the following unit-cell parameters: a = 9.555(1) Å, b = 16.847(1) Å, c = 32.522(1) Å, β = 94.37° , V = 5219.8 Å3 and four molecules per unit cell. Its crystal structure was determined and refined down to R1 = 0.0504, wR2 = 0.0667. The structure of the title compound, (C5H6N)7(BiCl6)2(NO3) consists of seven monoprotonated pyridinium (C5H6N)+ cations, two independent octahedron [BiCl6]3- and an isolated NO3- anion. These entities are linked together through N-H.....Cl and N-H.....O hydrogen bonds, originating from the (C5H6N)+ groups and the isolated anion of nitrate to forming a three dimensional network.

Synthesis and Spectroscopic Characterization of Mixed Diamidophosphoric Acid Esters: X-Ray Crystal Structure of [(CH3)2N]-[p-H3C-C6H4-O]P(O)X (X = NHC(CH3)3 and p-H3C-C6H4-NH)

2009 ◽  
Vol 64 (5) ◽  
pp. 565-569 ◽  
Author(s):  
Saied Ghadimi ◽  
Mehrdad Pourayoubi ◽  
Ali Asghar Ebrahimi Valmoozi
Keyword(s):  
Spectroscopic Characterization ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
Unit Cell Parameters ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters ◽  
R Value ◽  
Acid Esters

Mixed diamidophosphoric acid esters [(CH3)2N][p-H3C-C6H4-O]P(O)X, where X = NH(CH3) (1), NHCH(CH3)2 (2), NHC(CH3)3 (3) and p-H3C-C6H4-NH (4) were synthesized and characterized by 31P, 31P{1H}, 13C, 1H NMR, and IR spectroscopy and mass spectrometry, and single crystal X-ray diffraction analysis for the compounds 3 and 4. Compound 3 crystallizes in the monoclinic, space group P21/c with unit cell parameters a = 9.006(3), b = 16.286(5), c = 10.319(3) A° , β = 99.633(6)◦, V = 1492.2(8) °A3, Z = 4. The final R value is 0.0622 for 2074 reflections [I ≥ 2σ (I)]. Compound 4 crystallizes in the orthorhombic, space group Pna21 with unit cell parameters a = 7.0459(14), b = 20.934(4), c = 10.436(2) ° A, V = 1539.3(5) °A3, Z = 4. The final R value is 0.0530 for 3025 reflections [I ≥ 2σ (I)].

The Crystal Structure of S-Methyl 1-[Dicyclohexyl(thiophosphoryl)]-dithioformate: (c-C6H11)2P(S)C(S)Sme

1988 ◽  
Vol 41 (3) ◽  
pp. 405 ◽  
Author(s):  
BF Hoskins ◽  
ERT Tiekink
Keyword(s):  
Crystal Structure ◽  
Title Compound ◽  
Direct Methods ◽  
Mirror Plane ◽  
Unit Cell Parameters ◽  
Orthorhombic Space Group ◽  
Interatomic Distances ◽  
Full Matrix ◽  
Cell Parameters ◽  
Compound C

The crystal structure of the title compound, (c-C6H11)2P(S)C(S)SMe , has been determined and shows that the P(S)C(S)SC chromophore is situated on a crystallographic mirror plane with the cyclohexyl groups related to each other across this plane. Significant interatomic distances are: P=S 1.951(1), P-C 1.860(4), C=S 1.632(4) and C-S 1.700(4)Ǻ. A resonance scheme involving the delocalization of π-electrons over the CS2 moiety has been invoked to account for the observed C-S bond distances in the molecule. Crystals are orthorhombic, space group Pnma with unit cell parameters a 10.196(2), b 10.612(1) and c 15.370(3)Ǻ, and Z 4. The structure was solved by direct methods and refined by a full-matrix least-squares procedure to final R 0.045, Rw 0.047 for 1191 reflections with I ≥ 3.0σ(I).

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

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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