Preparation, properties, and X-ray crystal structure of a 1:1 complex of tetrathiafulvalene and p-dinitrobenzene

1982 ◽  
Vol 60 (16) ◽  
pp. 2057-2061 ◽  
Author(s):  
Martin R. Bryce ◽  
Anthony S. Secco ◽  
James Trotter ◽  
Larry Weiler
Keyword(s):  
Crystal Structure ◽  
Room Temperature ◽  
Direct Methods ◽  
X Ray Diffraction ◽  
Crystalline Complex ◽  
X Ray ◽  
Triclinic System ◽  
Donor Acceptor ◽  
Bulk Magnetic Susceptibility ◽  
R Value

A crystalline complex of tetrathiafulvalene and p-dinitrobenzene has been prepared and characterised by esr and ir spectroscopy, bulk magnetic susceptibility, dc conductivity, and an X-ray diffraction analysis. It is a neutral 1:1 complex which is an insulator at room temperature, σRT = 2.5 × 10−7 ohm−7 cm−1. The complex crystallizes in the triclinic system, space group [Formula: see text] with cell constants a = 6.915(1), b = 7.615(1), c = 8.149(1) Å, α = 79.39(1), β = 69.55(1), γ = 70.81(1)°, Z = 1. Data were collected on an Enraf-Nonius CAD-4 diffractometer. The structure was solved by direct methods and refined to an R-value of 0.028 for 1222 observed reflections. The structure consists of molecules stacked in an alternating donor–acceptor fashion along the c-axis. Mixed sheets parallel to [Formula: see text] are comprised of tetrathiafulvalene and p-dinitrobenzene molecules arranged end-on in the [021] direction.

Molecular conformation of di-o-anisylcarbinol: an X-ray diffraction study

1983 ◽  
Vol 61 (9) ◽  
pp. 2001-2005 ◽  
Author(s):  
C. Faerman ◽  
H. Negri ◽  
G. Punte ◽  
A. A. Vitale ◽  
N. S. Nudelman
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Diffraction Study ◽  
Molecular Conformation ◽  
Direct Methods ◽  
X Ray Diffraction ◽  
X Ray ◽  
Triclinic System ◽  
Phenyl Rings ◽  
R Factors

Di-o-anisylcarbinol crystallizes in the triclinic system, space group [Formula: see text] with a = 7.50 (4), b = 10.89 (4), c = 7.98 (3) Å, α = 101.9 (1), β = 94.1 (1), γ = 94.6 (1)°, Z = 2, V = 633.11 Å3, Dc = 1.28 mg m−3, Dm = 1.26 (1) mg m−3, CuKα radiation, λ = 1.54178 Å, μ(CuKα) = 0.633 mm−1, F(000) = 260. The structure has been determined by direct methods using single crystal X-ray data and refined by least-squares to the final R factors R = 5.89% and Rw = 5.35%. The molecule has a twist-skewed conformation with the phenyl rings on nearly orthogonal planes. The crystal structure shows a hydrogen-bonded dimer and a peculiar arrangement of the methoxy and phenyl groups.

scholarly journals X-ray crystal structure determination and NMR solution studies of 3′,3″5′,5″-tetrabromophenolphthalein ethyl ester

1991 ◽  
Vol 69 (8) ◽  
pp. 1298-1305 ◽  
Author(s):  
Antony C. Chiverton ◽  
Suzanne Fortier ◽  
John W. Bovenkamp ◽  
D. Thoraval ◽  
G. W. Buchanan ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Ethyl Ester ◽  
Room Temperature ◽  
Direct Methods ◽  
X Ray Diffraction ◽  
X Ray ◽  
Solution Studies ◽  
Central Carbon ◽  
Dark Blue ◽  
C Nmr

The crystal structure of 3′,3″,5′,5″-tetrabromophenolphthalein ethyl ester (TBPE) has been determined by X-ray diffraction at room temperature. This compound crystallizes in space group [Formula: see text], with a = 12.361(4), b = 12.533(4), c = 9.986(2) Å, α = 99.57(3), β = 112.76(2), γ = 100.73(3) °, and Z = 2. The structure was solved by direct methods and refined by full-matrix least-squares calculations to a residual of 0.034 for 1862 observed reflections. TBPE is propeller shaped about the central carbon and crstallizes with one molecule of benzene solvent per asymmetric unit. In 1:1 CD2Cl2:CDCl3 solution complete 1H and 13C NMR signal assignments have been made via 1H1H COSY and 1H13C HETCOR experiments. The quinoidal and phenolic integrities are retained on the NMR timescale. By contrast for an acetone-d6 solution only 14 13C resonances are found and the colour of the solution changed from green to dark blue. These changes in acetone solution are attributed to the presence of a trace of base which induces the loss of the phenolic proton of TBPE and the existence of resonance forms which render the phenolic and quinoidal rings equivalent. Key words: crystal structure, NMR, 3′3″5′5″-tetrabromophenolphthalein ethyl ester.

scholarly journals Spectral Characterization and Crystal Structure of 1,2-Bis-(1H-benzimidazol-2-yl)-ethane Dihydrochloride

2013 ◽  
Vol 2013 ◽  
pp. 1-5
Author(s):  
Aydin Tavman ◽  
Cigdem Sayil
Keyword(s):  
Crystal Structure ◽  
Nmr Spectroscopy ◽  
Nmr Spectra ◽  
Room Temperature ◽  
X Ray Diffraction ◽  
X Ray ◽  
Triclinic System ◽  
Ir And Nmr Spectroscopy ◽  
Ft Ir ◽  
System Characteristics

The crystal structure of 1,2-bis-(1H-benzimidazol-2-yl)-ethane dihydrochloride (1) was determined by X-ray diffraction at room temperature. The structure of1was also characterized by mass, elemental analysis, FT-IR, and NMR spectroscopy techniques. The title compound crystallizes in triclinic system and space group P-1,a=7.1350,b=9.6299(1),c=15.3340(7)Å,α=80.67(2),β=79.66(2),γ=68.395(11)∘,V=958.33(10)Å3,Z=2. Owing to theanticonformations of –CH2– groups, the entire molecule is relatively flat.H1-NMR spectra of1show AA′XX′system characteristics.

Crystal structure determination of the conformation of two bicyclo[3.3.1]nonan-ones

1985 ◽  
Vol 63 (6) ◽  
pp. 1166-1169 ◽  
Author(s):  
John F. Richardson ◽  
Ted S. Sorensen
Keyword(s):  
Crystal Structure ◽  
Direct Methods ◽  
Chair Conformation ◽  
Molecular Structures ◽  
Boat Conformation ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Final Agreement

The molecular structures of exo-7-methylbicyclo[3.3.1]nonan-3-one, 3, and the endo-7-methyl isomer, 4, have been determined using X-ray-diffraction techniques. Compound 3 crystallizes in the space group [Formula: see text] with a = 15.115(1), c = 7.677(2) Å, and Z = 8 while 4 crystallizes in the space group P21 with a = 6.446(1), b = 7.831(1), c = 8.414(2) Å, β = 94.42(2)°, and Z = 2. The structures were solved by direct methods and refined to final agreement factors of R = 0.041 and R = 0.034 for 3 and 4 respectively. Compound 3 exists in a chair–chair conformation and there is no significant flattening of the chair rings. However, in 4, the non-ketone ring is forced into a boat conformation. These results are significant in interpreting what conformations may be present in the related sp2-hybridized carbocations.

scholarly journals Exploring the Structural Chemistry of Pyrophosphoramides: N,N′,N″,N‴-Tetraisopropylpyrophosphoramide

Chemistry ◽  
2021 ◽  
Vol 3 (1) ◽  
pp. 149-163
Author(s):  
Duncan Micallef ◽  
Liana Vella-Zarb ◽  
Ulrich Baisch
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Nuclear Magnetic Resonance ◽  
Hydrogen Bonding ◽  
Nmr Spectroscopy ◽  
Ir Spectroscopy ◽  
Room Temperature ◽  
Intermolecular Hydrogen Bonding ◽  
X Ray Diffraction ◽  
X Ray

N,N′,N″,N‴-Tetraisopropylpyrophosphoramide 1 is a pyrophosphoramide with documented butyrylcholinesterase inhibition, a property shared with the more widely studied octamethylphosphoramide (Schradan). Unlike Schradan, 1 is a solid at room temperature making it one of a few known pyrophosphoramide solids. The crystal structure of 1 was determined by single-crystal X-ray diffraction and compared with that of other previously described solid pyrophosphoramides. The pyrophosphoramide discussed in this study was synthesised by reacting iso-propyl amine with pyrophosphoryl tetrachloride under anhydrous conditions. A unique supramolecular motif was observed when compared with previously published pyrophosphoramide structures having two different intermolecular hydrogen bonding synthons. Furthermore, the potential of a wider variety of supramolecular structures in which similar pyrophosphoramides can crystallise was recognised. Proton (1H) and Phosphorus 31 (31P) Nuclear Magnetic Resonance (NMR) spectroscopy, infrared (IR) spectroscopy, mass spectrometry (MS) were carried out to complete the analysis of the compound.

Evolution of crystal structure of dual layered molecular conductor (ET)4ZnBr4(C6H4Cl2) with temperature

CrystEngComm ◽  
2021 ◽  
Author(s):  
Gennady V. Shilov ◽  
Elena I. Zhilyaeva ◽  
Sergey M. Aldoshin ◽  
Alexandra M Flakina ◽  
Rustem B. Lyubovskii ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Electrical Resistivity ◽  
Single Crystal ◽  
Room Temperature ◽  
Organic Conductor ◽  
X Ray Diffraction ◽  
X Ray ◽  
Resistivity Measurements ◽  
Molecular Conductor ◽  
Abrupt Changes

Electrical resistivity measurements of a dual layered organic conductor (ET)4ZnBr4(1,2-C6H4Cl2) above room temperature show abrupt changes in resistivity at 320 K. Single-crystal X-ray diffraction studies in the 100-350 K range...

CRYSTAL STRUCTURE OF ZIRCONIUM TRICHLORIDE

1964 ◽  
Vol 42 (10) ◽  
pp. 1886-1889 ◽  
Author(s):  
B. Swaroop ◽  
S. N. Flengas
Keyword(s):  
Crystal Structure ◽  
Room Temperature ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Main Cell ◽  
Diffraction Patterns

The crystal structure of zirconium trichloride was determined from X-ray diffraction patterns. Zirconium trichloride belongs to the [Formula: see text]space group. The dimensions of the main cell at room temperature are: a = 5.961 ± 0.005 Å and c = 9.669 ± 0.005 Å.The density of zirconium trichloride was measured and gave the value of 2.281 ± 0.075 g/cm3 while, from the X-ray calculations, the value was found to be 2.205 g/cm3.

The crystal structure of gatehouseite

2011 ◽  
Vol 75 (6) ◽  
pp. 2823-2832
Author(s):  
P. Elliott ◽  
A. Pring
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonding ◽  
Three Dimensional ◽  
Direct Methods ◽  
Chemical Analyses ◽  
X Ray Diffraction ◽  
X Ray ◽  
Manganese Phosphate ◽  
Phosphate Mineral ◽  
Unit Formula

AbstractThe crystal structure of the manganese phosphate mineral gatehouseite, ideally Mn52+(PO4)2(OH)4, space group P212121, a = 17.9733(18), b = 5.6916(11), c = 9.130(4) Å, V= 933.9(4) Å3, Z = 4, has been solved by direct methods and refined from single-crystal X-ray diffraction data (T = 293 K) to an R index of 3.76%. Gatehouseite is isostructural with arsenoclasite and with synthetic Mn52+(PO4)2(OH)4. The structure contains five octahedrally coordinated Mn sites, occupied by Mn plus very minor Mg with observed <Mn—O> distances from 2.163 to 2.239 Å. Two tetrahedrally coordinated P sites, occupied by P, Si and As, have <P—O> distances of 1.559 and 1.558 Å. The structure comprises two types of building unit. A strip of edge-sharing Mn(O,OH)6 octahedra, alternately one and two octahedra wide, extends along [010]. Chains of edge- and corner-shared Mn(O,OH)6 octahedra coupled by PO4 tetrahedra extend along [010]. By sharing octahedron and tetrahedron corners, these two units form a dense three-dimensional framework, which is further strengthened by weak hydrogen bonding. Chemical analyses by electron microprobe gave a unit formula of (Mn4.99Mg0.02)Σ5.01(P1.76Si0.07(As0.07)Σ2.03O8(OH)3.97.

Study of thermal properties of Ga0.5In1.5Se3 by differential scanning calorimetry

2021 ◽  
pp. 2150407
Author(s):  
S. I. Ibrahimova
Keyword(s):  
Crystal Structure ◽  
Differential Scanning Calorimetry ◽  
Thermal Properties ◽  
Thermal Effects ◽  
Room Temperature ◽  
Structural Studies ◽  
X Ray Diffraction ◽  
Hexagonal Symmetry ◽  
Scanning Calorimetry ◽  
X Ray

The crystal structure and thermal properties of the [Formula: see text] compound have been investigated. Structural studies were performed by X-ray diffraction at room temperature. The crystal structure of this compound was found to correspond to the hexagonal symmetry of the space group P61. Thermal properties were studied using a differential scanning calorimetry (DSC). It was found in the temperature range [Formula: see text] that thermal effects occur at temperatures [Formula: see text] and [Formula: see text]. The thermodynamic parameters of these effects are calculated.

Ein tricyclisches Tetraboradisiladodecan aus Dimethyl-di-1-propinylsilan und Ethyldiboranen(6) / A Tricyclic Tetraboradisiladodecane from Dimethyl-di-1-propynylsilane and Ethyldiboranes(6)

1995 ◽  
Vol 50 (3) ◽  
pp. 439-447 ◽  
Author(s):  
Roland Köster ◽  
Günter Seidel ◽  
Roland Boese ◽  
Bernd Wrackmeyer
Keyword(s):  
Crystal Structure ◽  
Room Temperature ◽  
X Ray Diffraction ◽  
Space Group ◽  
X Ray ◽  
Structure Space ◽  
Thermal Elimination

The exhaustive hydroboration of the (C ≡ C )-groups in Me2Si(C ≡ CMe)2 (A ) by adding ethyldiboranes(6) at room temperature is presumed to lead initially to the formation of a mixture of the threo- and erythro-3,3,5,6-tetrakis(diethylboryl)-4,4-dimethyl-4-silaheptanes (1a , b). The threo-1a reacts further by borane catalysed intermolecular condensation to the substituted disilatetraboratricyclo[6.2.1.16.9]dodecane 2 with the formula , whose crystal structure [space group C2/c, a = 19.696(2), b = 10.371(1), c = 16.580(2) Å; β = 125.90(1)°; at 122 K] has been established by X -ray diffraction. In contrast, the erythro-1b undergoes intramolecular, thermal elimination of Et3B to give the 1,2-diethyl-2,4-bis(diethylboryl)- 3,3,5-trim ethyl-3-silaborolane (4). If A is added to an excess of undiluted B (“hydridebath”), then the two substituted diastereomers of the 1-carba-arachno-pentaboranes(10) (endo/exo-Et,SiH Me2) (3a, b), are formed preferentially as the result of an initial Si-C ≡-c le a v e d hydroboration.

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