scholarly journals Synthesis and X-ray Crystal Structure of New Substituted 3-4’-Bipyrazole Derivatives. Hirshfeld Analysis, DFT and NBO Studies

Crystals ◽  
2021 ◽  
Vol 11 (8) ◽  
pp. 953
Author(s):  
Ahmed T. A. Boraei ◽  
Matti Haukka ◽  
Ahmed A. M. Sarhan ◽  
Saied M. Soliman ◽  
Abdullah Mohammed Al-Majid ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Thermal Conditions ◽  
Chemical Yield ◽  
Triclinic Crystal System ◽  
X Ray ◽  
Hirshfeld Analysis ◽  
Intermolecular Contacts ◽  
New Compounds ◽  
Spectral Characterizations ◽  
Good Agreement

A new compounds named 3-4’-bipyrazoles 2 and 3 were synthesized in high chemical yield from a reaction of pyran-2,4-diketone 1 with aryl hydrazines under thermal conditions in MeOH. Compound 2 was unambiguously confirmed by single-crystal X-ray analysis. It crystalizes in a triclinic crystal system and space group P-1. Its crystal structure was found to be in good agreement with the spectral characterizations. With the aid of Hirshfeld calculations, the H...H (54.8–55.3%) and H...C (28.3–29.2%) intermolecular contacts are the most dominant, while the O...H (5.8–6.5%), N...H (3.8–4.6%) and C...C (3.0–4.9%) are less dominant. The compound has a polar nature with a net dipole moment of 6.388 Debye. The BD(2)C31-C32→BD*(2)N4-C34 (27.10 kcal/mol), LP(1)N5→BD*(2)C31-C32 (36.90 kcal/mol), BD(1)C32-C34→BD*(1)C18-C31 (6.78 kcal/mol) and LP(1)N4→BD*(1)N5-C31 (7.25 kcal/mol) are the strongest π→π*, n→π*, σ-σ* and n→σ* intramolecular charge transfer processes, respectively.

Synthesis and Crystal Structure of Tetraphenylarsonium Pentachlorocarbonylosmate(IV), (Ph4As)[OsCl5(CO)]

1997 ◽  
Vol 52 (8) ◽  
pp. 978-980 ◽  
Author(s):  
M Höhling ◽  
W Preetz
Keyword(s):  
Crystal Structure ◽  
Complex Anion ◽  
Structure Type ◽  
Close Packing ◽  
Cation Sublattice ◽  
X Ray Diffraction ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
Positional Disorder ◽  
Intermolecular Contacts

The structure of tetraphenylarsonium pentachlorocarbonylosmate(IV), (Ph4As)[OsCl5(CO)], the first example of a halogenocarbonyl complex with osmium in the oxidation state +IV, has been determined at 208 K by single crystal X-ray diffraction: tetragonal, space group P4/n with a = 12.821 , c = 8.084 Å, Z = 2. There are short intermolecular contacts between neighbouring anions along the tetragonal axis c and unusually large displacement ellipsoids of the carbonyl group and the four equatorial Cl ligands arising from a positional disorder of the complex anion. By analogy with a variety of reported structures of the (Ph4As)[RuNCl4] structure type this is attributed to the close packing of the cation sublattice. Compared to other monocarbonylosmates the Os-C bond of 1.94(2) Å is extraordinaryly long while the bond between Os and the trans coordinated Cl ligand of 2.286(3) Å is rather short.

scholarly journals Synthesis and X-ray Crystal Structures of Novel Spiro 1,3-benzoxazine Dimers

2002 ◽  
Vol 2002 (10) ◽  
pp. 473-474 ◽  
Author(s):  
H.Z. Alkhathlan ◽  
M.A. Al-Saad ◽  
H.M. Al-Hazimi ◽  
K.A. Al-Farhan ◽  
A.A. Mousa
Keyword(s):  
Crystal Structure ◽  
Crystal Structures ◽  
Mass Spectra ◽  
X Ray ◽  
New Compounds

Novel spiro 1,3-benzoxazine dimers are obtained when hydrazones of 2-hydroxyacetophenone are treated with triphosgene. An X-ray crystal structure, and the NMR and mass spectra of these new compounds, are reported and discussed.

Darstellung, Schwingungsspektren und Normalkoordinatenanalyse der 10B-und 11B-Isotopomeren von [B2(NCS)6]2- sowie Kristallstruktur von (Ph3P=N=PPh3)2[B2(NCS)6] / Preparation, Vibrational Spectra and Normal Coordinate Analysis of the 10B and 11B Isotopomers of [B2(NCS)6]2- and Crystal Structure of (Ph3P=N=PPh3)2[B2(NCS)6]

1996 ◽  
Vol 51 (4) ◽  
pp. 551-556 ◽  
Author(s):  
W. Preetz ◽  
B. Steuer
Keyword(s):  
Crystal Structure ◽  
Normal Coordinate Analysis ◽  
Force Constants ◽  
Potential Energy Distribution ◽  
X Ray Diffraction ◽  
Normal Coordinate ◽  
Triclinic Space Group ◽  
X Ray ◽  
Fractionated Crystallization ◽  
Good Agreement

Abstract By reaction of [B6H6]2- with a solution of (SCN)2 in dichloromethane in the presence of solid KOH the hexaisothiocyanatodiborate anion [B2(NCS)6]2- is formed and can be isolated by fractionated crystallization. The crystal structure of (PNP)2[B2(NCS)6] has been determined by single crystal X-ray diffraction analysis; triclinic space group P1̄ with a=12,282(5), b=12,416(5), c=14,155(5)Å, a=68,36(5), β=70,59(5), γ=80,93(5)°.The [B2(NCS)6]2- anion reveals a staggered conformation with nearly local D3d symmetry and a B-B bond length of 1,73(2) Å. Using the crystallographic data a normal coordinate analysis has been performed. With a set of 12 force constants (e.g. fd(BB)=3,62, fd(BN)=4,21 mdyn/Å) a good agreement between observed and calculated frequencies for the 10B and 11B isotopomers has been achieved. The potential energy distribution on the force constants reveals strong vibrational couplings within the B2N6 framework.

scholarly journals X-ray Single-Crystal Structural Analysis of a Magnetically Oriented Monoclinic Microcrystal Suspension of α-Glycine

Crystals ◽  
2019 ◽  
Vol 9 (11) ◽  
pp. 561 ◽  
Author(s):  
Tatsuya Tanaka ◽  
Chiaki Tsuboi ◽  
Kazuaki Aburaya ◽  
Fumiko Kimura ◽  
Masataka Maeyama ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Magnetic Susceptibility ◽  
Single Crystal ◽  
Magnetic Energy ◽  
Powder Sample ◽  
Single Crystal Structure ◽  
X Ray ◽  
Crystal Structural ◽  
The Relationship ◽  
Good Agreement

We previously reported on a method for X-ray single-crystal structure determination from a powder sample via a magnetically oriented microcrystal suspension (MOMS). The method was successfully applied to orthorhombic microcrystals (L-alanine, P212121). In this study, we apply this method to monoclinic microcrystals. Unlike most of the orthorhombic MOMSs, monoclinic MOMSs exhibit two or four orientations with the same magnetic energy (we refer to this as twin orientations), making data processing difficult. In this paper, we perform a MOMS experiment for a powder sample of monoclinic microcrystal (α-glycine, P21/n) to show that our method can also be applied to monoclinic crystals. The single-crystal structure determined in this work is in good agreement with the reported one performed on a real single crystal. Furthermore, the relationship between the crystallographic and magnetic susceptibility axes is determined.

scholarly journals 4-Benzyl-1-(4-nitrophenyl)-1H-1,2,3-triazole: crystal structure and Hirshfeld analysis

2017 ◽  
Vol 73 (11) ◽  
pp. 1716-1720 ◽  
Author(s):  
Julio Zukerman-Schpector ◽  
Sofia Dallasta Pedroso ◽  
Lucas Sousa Madureira ◽  
Márcio Weber Paixão ◽  
Akbar Ali ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Torsion Angle ◽  
Title Compound ◽  
Three Dimensional ◽  
Hirshfeld Surface ◽  
Aromatic Rings ◽  
Compound C ◽  
Centroid Distance ◽  
Hirshfeld Analysis ◽  
Intermolecular Contacts

The molecule in the title compound, C15H12N4O2, has a twistedL-shape with the dihedral angle between the aromatic rings of the N-bound benzene and C-bound benzyl groups being 70.60 (9)°. The nitro group is co-planar with the benzene ring to which it is connected [C—C—N—O torsion angle = 0.4 (3)°]. The three-dimensional packing is stabilized by a combination of methylene-C—H...O(nitro), methylene-C—H...π(phenyl), phenyl-C—H...π(triazolyl) and nitro-O...π(nitrobenzene) interactions, along with weak π(triazolyl)–π(nitrobenzene) contacts [inter-centroid distance = 3.8386 (10) Å]. The importance of the specified intermolecular contacts has been verified by an analysis of the calculated Hirshfeld surface.

Untersuchungen an Stickstoff-Brom-Verbindungen, IV / Studies on Nitrogen-Bromine Compounds, IV

1977 ◽  
Vol 32 (12) ◽  
pp. 1416-1420 ◽  
Author(s):  
Omar Jabay ◽  
Hans Pritzkow ◽  
Jochen Jander
Keyword(s):  
Crystal Structure ◽  
Nitrogen Atom ◽  
Structure Analysis ◽  
Electron Acceptors ◽  
Molecular Structures ◽  
Hydrogen Atoms ◽  
X Ray ◽  
Crystal And Molecular Structures ◽  
Solid Nitrogen ◽  
Intermolecular Contacts

The crystal and molecular structures of N-bromobenzamide (NBB), N-bromosuccinimide (NBS), and N,N-dibromobenzenesulfonamide (NBBS) were determined by X-ray structure analysis. The nitrogen atoms in NBB and NBS have a trigonal planar coordination (sp2) and the N—Br distances lie in the same range (1.82 A, 1.84 A). The N—Br distance in NBBS, where the nitrogen atom is sp3-hybridized, is somewhat longer (1.88 A). In these structures the molecules are connected by O···H—N (NBB), O···Br—N (NBS) or N···Br—N (NBBS) intermolecular bonds forming endless chains; positivated hydrogen atoms or, in case that they are absent, positivated bromine atoms act as electron acceptors with oxygen or sp3- hybridized nitrogen atoms. These results suggest, that in solid nitrogen tribromide, the crystal structure of which cannot be determined, the nitrogen atoms will be sp3-hybridized and intermolecular contacts via N—Br···N will occur.

The crystal and molecular structure of copper(II) bis-(ethylenediamine)nitrate selenocyanate

1982 ◽  
Vol 47 (2) ◽  
pp. 409-420 ◽  
Author(s):  
Viktor Vrábel ◽  
Ján Garaj
Keyword(s):  
Crystal Structure ◽  
Least Squares Method ◽  
Crystal And Molecular Structure ◽  
Central Atom ◽  
Covalent Bond ◽  
Axial Direction ◽  
Analysis Method ◽  
Monoclinic System ◽  
X Ray ◽  
Intermolecular Contacts

The crystal structure of [Cuen2(NO3)]SeCN was solved by the single-crystal X-ray structural analysis method. The compound crystallizes in the monoclinic system with space group Pc. The unit cell has dimensions: a = 0.9254(3), b = 1.4018(3), c = 0.9722(5) nm, β = 99.20(3)°. The structure was refined by the least squares method to a final value of R = 6.8% for 1965 observed reflections. The crystal structure consits of polymeric cation chain [Cuen2(NO3)]+ and of free uncoordinated SeCN- anions. The nitrate ion NO-3 forms a bridging unit between two [Cuen3]2+ cations. The coordination polyhedron around the Cu(II) atom is a deformed octahedron, formed of two ethylendiamine molecules and two oxygen atoms of the NO-3 ions, bonded to divalent copper in the axial direction along the long coordinates. The crystal structure contains selenocyanate which is not bonded through a covalent bond to the central atom, but there are intermolecular contacts with its immediate surroundings.

scholarly journals Structure and Optical Properties of B'- Phase of Ag8SnSe6

2016 ◽  
Vol 17 (3) ◽  
pp. 346-349
Author(s):  
І.V. Semkiv
Keyword(s):  
Crystal Structure ◽  
Optical Properties ◽  
Absorption Spectrum ◽  
Optical Absorption ◽  
Experimental Studies ◽  
Energy Dispersive Spectrum ◽  
Energy Dispersive ◽  
Interatomic Distances ◽  
X Ray ◽  
Good Agreement

Energy dispersive x-ray spectroscopy of lowtemperature b¢-Ag8SnSe6 crystalcarried out. Energy dispersive spectrum shows only peaks related to Ag8SnSe6. Experimental optical absorption spectrum and band gap value 0.82 eV are determined. Theoretical calculation of absorption spectrum shows good agreement with experimental studies. Modeling of crystal structure of Ag8SnSe6 argyrodite and interatomic distances calculation are carried out.

Interaction of the Components in the {Ce, Gd}-{Ti, Zr}-Sb Systems

2019 ◽  
Vol 289 ◽  
pp. 3-11
Author(s):  
Oleksandr Senchuk ◽  
Roman E. Gladyshevskii
Keyword(s):  
Crystal Structure ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Ternary Systems ◽  
The Other ◽  
Powder Diffraction Data ◽  
Isothermal Sections ◽  
X Ray ◽  
Ternary Compounds ◽  
New Compounds

The phase equilibria in the ternary systems {Ce, Gd}–{Ti, Zr}–Sb were investigated by means of X-ray powder diffraction and energy-dispersive X-ray spectroscopy. The isothermal sections of the phase diagrams at 600°C were constructed. The formation of three ternary compounds (Ce2Ti7Sb12, Ce3TiSb5, and Gd2Ti11Sb14) was confirmed in the {Ce, Gd}–Ti–Sb systems and no more ternaries were found. The investigation of the {Ce, Gd}–Zr–Sb systems revealed several new ternary compounds and confirmed the known ones. The crystal structure of the new compound Ce0.08(3)Zr1.92(3)Sb was determined from X-ray powder diffraction data. The other new compounds in the Ce–Zr–Sb system were found to have compositions close to ~CeZrSb4and ~Ce2Zr3Sb5. In the Gd–Zr–Sb system the existence of a large homogeneity range was established for the GdZrSb compound along the isoconcentrate 33.3 at.% Sb: Gd1-xZr1+xSb (x= 00.905(18) at 600°C), and a new compound, ~Gd3Zr3Sb14, was discovered. The crystal structures at the boundary compositions of the Gd1-xZr1+xSb phase were refined from X-ray powder diffraction data.

Simple Synthesis of New Mixed Isocyanide-NHC-Platinum(II) Complexes and Their Catalytic Activity

2014 ◽  
Vol 67 (3) ◽  
pp. 469 ◽  
Author(s):  
Christoph Hubbert ◽  
Marcus Breunig ◽  
Kristen J. Carroll ◽  
Frank Rominger ◽  
A. Stephen K. Hashmi
Keyword(s):  
Crystal Structure ◽  
Catalytic Activity ◽  
Structural Data ◽  
Simple Synthesis ◽  
X Ray ◽  
New Family ◽  
Catalytically Active ◽  
Convergent Approach ◽  
New Compounds

Using the new modular and convergent approach to isocyanide-N-hetrocyclic carbene-platinum(ii) complexes, eight new compounds have been synthesised. For three of these, detailed structural data could be obtained by X-ray crystal structure analyses. This new family of organoplatinum complexes is catalytically active for hydrosilylation reactions; styrene and phenylacetylene could be used as substrates; triethylsilane and 1,1,1,3,5,5,5-heptamethyltrisiloxane could be used as reagents. With some of the new platinum pre-catalysts, excellent regioselectivities of up to 98 : 2 could be obtained, and turnover numbers up to 840 were achieved.

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