scholarly journals Two Compounds of 1-((4-Bromothiophen-2-Yl)Methylene)-2-(Perfluorophenyl)Hydrazine, and 1-((4-Bromo-5-Methylthiophen-2-Yl)Methylene)-2-(Perfluorophenyl)Hydrazine and They Crystal, Molecular and Electronic Properties

2021 ◽  
Author(s):  
Július Sivý ◽  
Dušan Bortňák ◽  
Daniel Végh ◽  
Erik Rakovský
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Solid Phase ◽  
Diffraction Method ◽  
Monoclinic Space Group ◽  
Boat Conformation ◽  
Compound I ◽  
Space Group ◽  
Centrosymmetric Space Group ◽  
Compound Ii

The crystals, C11H4BrF5N2S, (I), 1-((4-bromothiophen-2-yl)methylene)-2-(perfluorophenyl)hydrazine and C12H6BrF5N2S, (II), 1-((4-bromo-5-methylthiophen-2-yl)methylene)-2-(perfluorophenyl)hydrazine are molecules with two rings and hydrazone part like a centre of the molecule. The compounds have been synthesized and characterized by elemental, spectroscopic (1H-NMR) analysis. The crystal structures of the solid phase were determined by single crystal X-ray diffraction method. They crystallize in the monoclinic space group with Z = 4 and Z = 2 molecules per unit-cell. The compound (I) crystallizes as a racemate in the centrosymmetric space group and the compound (II) crystallizes as a non-racemate in the non-centrosymmetric space group. The “absolute configuration and conformation for bond values” were derived from the anomalous dispersion (ad) for (II). The crystal structures are revealed diverse non-covalent interactions such as intra- and interhydrogen bonding, π-ring···π-ring, C-H···π-ring and they were investigated. The expected stereochemistry of hydrazones atoms C7, N2 and N1 were confirmed for (I) and (II). The hole molecule of the (I), and (II) possesses “a boat conformation” like a 6-membered ring. The results of the single crystal studies are reproduced with the help of Hirshfeld surface study and Gaussian software.

The Dichloroplatinum(II) and Dichloropalladium(II) Complexes of 1,4-Diazacycloheptane: Preparative, Structural and Conformational Studies

1996 ◽  
Vol 49 (12) ◽  
pp. 1301 ◽  
Author(s):  
GW Allen ◽  
ECH Ling ◽  
LV Krippner ◽  
TW Hambley
Keyword(s):  
Crystal Structures ◽  
Chelate Ring ◽  
Chair Conformation ◽  
Monoclinic Space Group ◽  
Boat Conformation ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
Membered Chelate Ring ◽  
Alternative Conformation

The preparation and purification of [Pt( hpip )Cl2] and [Pd( hpip )Cl2] ( hpip = homopiperazine = 1,4-diazacycloheptane) are described. Crystal structures of [Pt( hpip )Cl2] and [Pd( hpip )Cl2] have been determined by X-ray diffraction methods and refined to R values of 0.023 (932 F) and 0.023 (948 F). The crystals of [Pt( hpip )Cl2] are orthorhombic, space group Pbcm , a 7.7019(8), b 9.8080(12), c 12.1944(14) Ǻ, and those of [Pd( hpip )Cl2] are monoclinic, space group P21/m, a 6.1001(9), b 11.527(2), c 6.458(I) Ǻ, β 106.30(2)°. The seven- membered rings of the ligands in both complexes adopt boat-like conformations in which the five- membered chelate ring has an eclipsed N-C-C-N group and the six- membered chelate ring adopts a chair conformation. Molecular mechanics methods were used to investigate whether this conformation was a crystallographic artefact but it was found to be real. An alternative conformation in which the six-membered chelate ring adopts a skew-boat conformation was also investigated. It was found to be less stable than the conformation observed in the crystal structures, but to a degree that depends on whether non-bonded interactions involving the metal atom were included or not.

Tetrahalogenotellurate(II): Synthese und Kristallstrukturen von Verbindungen mit den Ionen TeX42- (X = Cl, Br, I)/Tetrahalotellurates(II): Syntheses and Crystal Structures of Compounds with TeX42- Ions (X = Cl, Br, I)

1985 ◽  
Vol 40 (2) ◽  
pp. 251-257 ◽  
Author(s):  
Siegfried Pohl ◽  
Wolfgang Saak ◽  
Bernt Krebs
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Acetonitrile Solution ◽  
Monoclinic Space Group ◽  
Space Group ◽  
X Ray ◽  
Bond Lengths ◽  
Square Planar

Abstract The compounds [(C6H5)4As]2 TeCl4 (1), [(C2H5)4 N]2 TeBr4 · CH3CN (2), and [(C2H5)4N]2TeI4 (3) were prepared by the reaction of Te, X2 , and excess (C2H5)4NX (X = Br, I) in acetonitrile solution or by heating of [(C6H5)4 As]2TeCl6 , Te, and (C6H5)4 ASCl for several hours in the same solvent.The structures of 1-3 were determined from single crystal X-ray data.1 crystallizes in the monoclinic space group P21/n with a = 1061.8(2), b = 1614.2(3), c = 1341.7(3) pm, β = 94.21° and Z = 2; 2: tetragonal, P4/mmm, a = 1039.7(2), c = 690.5(1), Z = 1; 3: tetragonal, I4/mmm, a = 1061.7(2), c = 1342.8(4), Z = 2. In 1-3 Te(II) exhibits a square planar coordination. The Te -CI, Te -Br, and Te-I bond lengths were found to be 260.7 (mean), 275.3, and 298.5 pm, respectively.

On racemic and L-malates: a comparison of their crystal structures

2004 ◽  
Vol 219 (2) ◽  
Author(s):  
Michel Fleck ◽  
Ekkehart Tillmanns ◽  
Ladislav Bohatý ◽  
Peter Held
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Monoclinic Space Group ◽  
Powder Diffraction Data ◽  
X Ray Diffraction ◽  
Powder Diffraction File ◽  
Space Group ◽  
X Ray

AbstractThe crystal structures of eight different L-malates have been determined and refined from single-crystal X-ray diffraction data. The compounds are the monoclinic (space groupIn addition, for all the compounds, powder diffraction data were collected, analysed and submitted to the powder diffraction file (PDF).

scholarly journals Polymorphism and pseudosymmetry of 10,10′-oxybis(9-thia-10-hydro-10-boraanthracene)

2019 ◽  
Vol 75 (5) ◽  
pp. 690-694
Author(s):  
Julian Radtke ◽  
Hans-Wolfram Lerner ◽  
Michael Bolte
Keyword(s):  
Title Compound ◽  
The Other ◽  
Asymmetric Unit ◽  
Compound I ◽  
Unit Cell Parameters ◽  
Space Group ◽  
Cell Parameters ◽  
Compound C ◽  
Centrosymmetric Space Group ◽  
Compound Ii

We have encountered two polymorphs of the title compound, C24H16B2OS2, both of which display almost the same unit-cell parameters. Compound (I) crystallizes in the non-centrosymmetric space group P21 with four molecules in the asymmetric unit. These molecules are related by pseudosymmetry. As a result, the space group looks like P21/c, but the structure cannot be refined successfully in that space group. Compound (II) on the other hand crystallizes in the centrosymmetric space group P21/c with only two molecules in the asymmetric unit. The crystals studied for (I) and (II) were both non-merohedral twins.

Conformation of azaphosphorinane ring. Crystal structures of 2,2,6,6-tetramethyl-4,4-diphenyl-1,4-azaphosphorinanium perchlorate and 2,2,6,6-tetramethyl-4-oxo-4-phenyl-1,4-azaphosphorinan-1-oxyl (stable nitroxy radical)

1983 ◽  
Vol 61 (3) ◽  
pp. 427-433 ◽  
Author(s):  
Miroslaw Cygler ◽  
Janusz Skolimowski
Keyword(s):  
Crystal Structures ◽  
Heavy Atom ◽  
Phenyl Group ◽  
Direct Methods ◽  
Chair Conformation ◽  
Monoclinic Space Group ◽  
Compound I ◽  
Orthorhombic Space Group ◽  
Space Group ◽  
Unit Cell Dimensions

Crystal structures of 2,2,6,6-tetramethyl-4,4-diphenyl-1,4-azaphosphorinanium perchlorate (I) and 2,2,6,6-tetramethyl-4-oxo-4-phenyl-1,4-azaphosphorinan-1-oxyl (II) were determined. Compound I crystallizes in the monoclinic space group C2/c with unit cell dimensions a = 18.2967(7), b = 10.9413(6), c = 20.8714(13) Å, β = 90.79(1)° (at 115 K), and II crystallizes in the orthorhombic space group Pn21a with a = 8.076(1), b = 10.139(1), c = 17.894(1) Å. Intensity data were measured on a diffractometer at 115 K for I and at the room temperature for II. The structures were solved by a combination of heavy-atom and direct methods and refined to R = 0.036 (3968 reflections) for I and 0.039 (1451 reflections) for II.The azaphosphorinane ring adopts a chair conformation in both molecules, being flattened in the P part in I and in the N part in II. In molecule I the equatorial phenyl group is nearly parallel to the approximate plane of symmetry of the molecule, and the axial phenyl group is perpendicular to that plane. In molecule II the P=O bond is axial and the phenyl group is equatorial. The CN(O)C group is not planar. The N—O bond makes an angle of 18.0(3)° with the CNC plane. The CNC angle of 129.3(3)° is larger than that found in nitroxypiperidine analogues.

scholarly journals The crystal structures of three 3-methyl-1H-1,2,4-triazole-5-thiones, including a second polymorph of 4-[(E)-(5-bromo-2-hydroxybenzylidene)amino]-3-methyl-1H-1,2,4-triazole-5(4H)-thione and a redetermination of 4-amino-3-methyl-1H-1,2,4-triazole-5(4H)-thione

2015 ◽  
Vol 71 (9) ◽  
pp. 1003-1009 ◽  
Author(s):  
Padmanabha S. Manjula ◽  
Balladka K. Sarojini ◽  
Hemmige S. Yathirajan ◽  
Mehmet Akkurt ◽  
Cem Cüneyt Ersanlı ◽  
...  
Keyword(s):  
Hydrogen Bond ◽  
Hydrogen Bonds ◽  
Crystal Structures ◽  
Dihedral Angle ◽  
Compound I ◽  
Methyl Group ◽  
Space Group ◽  
Improved Model ◽  
Compound Ii

The structures of three 3-methyl-1H-1,2,4-triazole-5-thione derivatives are reported. The structure of 4-amino-3-methyl-1H-1,2,4-triazole-5(4H)-thione, C3H6N4S, (I), has been redetermined with an improved model for the H atoms: the non-H atoms of (I) all lie on mirror planes in space groupPbcm, and the H atoms of the methyl group are disordered over two sets of reflection-related atomic sites having occupancy 0.5: two independent N—H...S hydrogen bonds link the molecules of compound (I) into complex sheets. The non-H atoms in the molecules of 4-[(E)-(3,4-dimethoxybenzylidene)amino]-3-methyl-1H-1,2,4-triazol-5(4H)-thione, C12H14N4O2S, (II), despite lying in general positions are close to planar, with a dihedral angle between the two rings of 6.31 (10)°: the molecules of compound (II) are linked by a three-centre N—H...(O)2hydrogen bond into aC(10)C(11)[R12(5)] chain of rings. A second polymorph of 4-[(E)-(5-bromo-2-hydroxy-5-bromobenzylidene)amino]-3-methyl-1H-1,2,4-triazole-5(4H)-thione, C10H9BrN4OS, (III), has been identified; the non-H atoms are nearly co-planar with a dihedral angle between the two rings of 1.9 (4)°. There is an intramolecular O—H...N hydrogen bond and the molecules are linked by N—H...S hydrogen bonds, forming centrosymmetricR22(8) dimers. Comparisons are made with some related structures.

Structural trends and the electronic structure of the rare-earth oxomolybdates RMo5O8 (R = La, Ce, Pr, Nd, Sm, Eu and Gd) containing chains of bioctahedral Mo10 clusters

2003 ◽  
Vol 59 (4) ◽  
pp. 472-478 ◽  
Author(s):  
P. Gougeon ◽  
P. Gall ◽  
J.-F. Halet ◽  
R. Gautier
Keyword(s):  
Crystal Structure ◽  
Electronic Structure ◽  
Rare Earth ◽  
Single Crystal ◽  
Crystal Structures ◽  
Monoclinic Space Group ◽  
Space Group ◽  
Theoretical Investigations ◽  
Bonding Mode ◽  
The Rare Earth

The crystal structures of the rare-earth members of the series RMo5O8 (R = Ce to Eu) have been investigated and compared with those of the La and Gd members previously published in order to understand the influences of the size and the charge of the cation on the different Mo—Mo bonds. The RMo5O8 compounds crystallize in the monoclinic space group P21/c. Their crystal structure is characterized by bioctahedral Mo10 clusters forming extended chains. The results of our single-crystal studies show that the modification of charge predominantly affects the Mo—Mo bonds between the Mo10 clusters and, to a lesser extent, the intra-cluster distances, while the cationic size induces only small variations. Theoretical investigations confirm this statement and allow the understanding of the bonding mode in these compounds.

scholarly journals The crystal structures of two chalcones: (2E)-1-(5-chlorothiophen-2-yl)-3-(2-methylphenyl)prop-2-en-1-one and (2E)-1-(anthracen-9-yl)-3-[4-(propan-2-yl)phenyl]prop-2-en-1-one

2016 ◽  
Vol 72 (8) ◽  
pp. 1153-1158 ◽  
Author(s):  
Marisiddaiah Girisha ◽  
Hemmige S. Yathirajan ◽  
Jerry P. Jasinski ◽  
Christopher Glidewell
Keyword(s):  
Hydrogen Bond ◽  
Hydrogen Bonds ◽  
Crystal Structures ◽  
The Other ◽  
Single Type ◽  
Compound I ◽  
Space Group ◽  
Compound Ii

In the crystal of compound (I), C14H11ClOS, molecules are linked by C—H...O hydrogen bonds to form simpleC(5) chains. Compound (II), C26H22O, crystallizes withZ′ = 2 in space groupP-1; one of the molecules is fully ordered but the other is disordered over two sets of atomic sites having occupancies 0.644 (3) and 0.356 (3). The two disordered components differ from one another in the orientation of the isopropyl substituents, and both differ from the ordered molecules in the arrangement of the central propenone spacer unit, so that the crystal of (II) contains three distinct conformers. The ordered and disordered conformers each form aC(8) chain built from a single type of C—H...O hydrogen bond but those formed by the disordered conformers differ from that formed by the ordered form.

One-pot green synthesis of biologically relevant novel spiro[indolin-2-one-3,4′-pyrano[2,3-c]pyrazoles] and studies on their spectral and X-ray crystallographic behaviors

2016 ◽  
Vol 72 (3) ◽  
pp. 335-343
Author(s):  
Sakshi Sharma ◽  
Goutam Brahmachari ◽  
Rajni Kant ◽  
Vivek K. Gupta
Keyword(s):  
Hydrogen Bonds ◽  
Single Crystal ◽  
Dimethyl Sulfoxide ◽  
Monoclinic Space Group ◽  
Boat Conformation ◽  
Pyran Ring ◽  
One Pot ◽  
Structural Investigations ◽  
Space Group ◽  
X Ray

Synthesesviagreen route and single-crystal X-ray structural investigations have been carried out for three spiro[indolin-2-one-3,4′-pyrano[2,3-c]pyrazole] derivatives, 6′-amino-2-oxo-3′-propyl-2′H-spiro[indoline-3,4′-pyrano[2,3-c]pyrazole]-5′-carbonitrile dimethyl sulfoxide monosolvate (5a), 6′-amino-5-fluoro-2-oxo-3′-propyl-2′H-spiro[indoline-3,4′-pyrano[2,3-c]pyrazole]-5′-carbonitrile dimethyl sulfoxide monosolvate (5b) and methyl 6′-amino-5-cyano-1-methyl-2-oxo-3′-propyl-2′H-spiro[indoline-3,4′-pyrano[2,3-c]pyrazole]-3′-carboxylate 0.25 hydrate (5c), respectively. Compounds (5a) and (5b) crystallize in the triclinic space group P\bar 1, whereas compound (5c) crystallizes in the monoclinic space groupC2/c. In molecules (5a) and (5b) all the rings are practically flat, while in (5c), the heterocyclic pyran ring adopts a flattened-boat conformation. In (5a) and (5b) the cyanide group is oriented in a (−ap)conformation, while the amino group is oriented in a (+ap)conformation with a pyran ring, but in (5c) both the cyanide and amino groups are oriented in a (−ap) conformation with the pyran ring. In the crystal structure of (5a) and (5b), the molecules are linked by an elaborate system of N—H...O and N—H...N hydrogen bonds to generate a zigzag-like construct. In (5c) molecules are linked by N—H...O hydrogen bonds, thereby generating extended chains. The present communication focuses on the detailed and comparative information about spectral behaviors, single-crystal X-ray crystallographic properties and solid-state supramolecular architectures of these synthesized compounds of potential biological interests.

Hydratisierte Cyanoelpasolithe: Bis(tetramethylammonium)diaquaIithium-hexacyanometallate(III) des Mangans, Eisens und Cobalts / Hydrated Cyanoelpasolites: Bis(tetramethylammonium)diaqualithium-hexacyanometallates(III) of Manganese, Iron and Cobalt

1988 ◽  
Vol 43 (10) ◽  
pp. 1311-1318 ◽  
Author(s):  
M Witzel ◽  
B Ziegler ◽  
D Babel
Keyword(s):  
Single Crystal ◽  
Crystal Structures ◽  
Monoclinic Space Group ◽  
Lithium Ions ◽  
Space Group ◽  
Distorted Octahedral ◽  
Face Centered

The crystal structures of three isotypic hexacyanometallates(III) (NMe4)2LiM(CN)6·2H2O have been determined and refined in the monoclinic space group C2/c, Z = 4, to wR = 0.053 (M = Mn, 959 independent single crystal reflections), 0.041 (M =Fe, 2002 reflections) and 0.037 (M = Co, 1881 reflections). The stucture is elpasolite-related by its face-centered pseudocubic arrangement of M atoms within nearly undistorted M(CN)63- octahedra, six of which form strongly distorted octahedral N6 cavities occupied by dihydrated lithium ions. The resulting average distances for the M(CN)63- octahedra are Mn-C = 201, Fe-C = 194.7, Co-C = 190.3, and C-N = 114 pm. The lithium coordination is distorted tetrahedral, consisting of LiO2N2 units with distances of about Li-O = 194, Li -N = 209 pm (for M = Fe, Co). The remaining four N atoms of the N6 cavity are bound by hydrogen bridges from the two aqua ligands, O-H···N = 283 and 295 pm. The relations to the hydrated elpasolite structure of (NMe4)2NaFe(CN)6·H2O are discussed.

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