Synthesis and characterization of volatile trifluoromethyl alkyl tellurides (original) (raw)
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Crystal Structures of a Series of 1,1-Spiro-bis(1,2,3,4-tetrahydronaphthalene)-Based Derivatives
Journal of Chemical Crystallography, 2012
The structures of four spirobisnaphthalenes based monomers 1, 2, 3a and 3b are reported. Each compound represents a methoxylated precursor which after deprotection led to the formation of a monomer successfully used for the synthesis of Polymers of intrinsic microporosity. The spiro-centre represents the site of contortion that, since its rigidity, leads to inefficient packing in the solid state inducing microporosity in the final polymer. Compound 1 crystallized in the monoclinic P2/c space group with unit cell parameters a = 8.1659(19) Å , b = 7.5298(18) Å , c = 19.130(5) Å , b = 97.935(4)°, V = 1165.0(5) Å 3 , Z = 2, D = 1.210 Mg m -3 . Compound 2 crystallized in the monoclinic P2 1 /n space group with unit cell parameters a = 12.6940(9) Å , b = 7.7267(6) Å , c = 19.9754(15) Å , b = 97.220(1)°, V = 1943.7(3) Å 3 , Z = 4, D = 1.355 Mg m -3 . Compound 3a crystallized in the monoclinic P2 1 /c space group with unit cell parameters a = 16.8137(14) Å , b = 10.5577(9) Å , c = 31.344(3) Å , b = 103.618(1)°, V = 5407.5(8) Å 3 , Z = 8, D = 1.308 Mg m -3 . Compound 3b crystallized in the monoclinic Pc space group with unit cell parameters a = 15.594 Å , b = 12.564 Å , c = 18.339 Å , b = 90.224(1)°, V = 3593.0 Å 3 , Z = 4, D = 1.236 Mg m -3 .
Journal of Molecular Structure, 1999
The IR (4000-400 cm Ϫ1) and Raman (4000-50 cm Ϫ1) spectra of 3-methoxymethylene-2,4-pentanedione (H 3 CO -CHyC (COCH 3) 2) in the liquid and solute forms in various solvents of different polarity were recorded at ambient temperature. Additional IR and Raman spectra were obtained for amorphous and crystalline solid at low temperature. The vibrational spectra revealed that compound exists atleast in two dominant conformers with different polarity and that conformer present in the solid phase is less polar. NMR spectra in various solvents at different temperatures were also obtained.The compound can exist in several conformers as a result of rotation around O-Cy and both yC-C bonds with planar or nonplanar arrangement of the heavy atoms. Semiempirical (AM1, PM3, MNDO, MINDO3) and ab initio using TZP and 6-31G** basis sets calculations were carried out. According to ab initio calculations at least five conformational structures with the methoxy group oriented as anti or syn and carbonyl groups oriented as Z or E towards the CyC double bond were obtained at energy surface. The calculated ab initio and AM1 energies of all conformers suggest as the most stable anti-ZE conformer where Z and E regard of the trans and cis acetyl group, respectively. As the second most stable conformer with energy at least 10 kJ mol Ϫ1 higher was calculated anti-EZ conformer. Assignments of the vibrational spectra for the studied compound were made with the aid of normal coordinate calculations employing scaled ab initio force field constants. The scaled ab initio frequencies as well as calculated energies indicate that the conformer present in the solid phase is anti-ZE.
Zeitschrift für Kristallographie - Crystalline Materials, 2008
In each of the title compounds, R[Ph(Cl)C=(H)C]TeCl2, R = nBu (1) and Ph (2), the primary geometry about the TeIV atom is a pseudo-trigonal-bipyramidal arrangement, with two Cl atoms in apical positions, and the lone pair of electrons and C atoms in the equatorial plane. As the TeIV is involved in two, an intra- and an inter-molecular, Te···Cl interactions the coordination geometry might be considered as a ψ-pentagonal bipyramid in each case. In addition, in (2) there is a hint of a Te···π interaction (Te···C = 3.911(3) Å). The key feature in the crystal structure of both compounds is the formation of supramolecular chains mediated by Te···Cl contacts.(1): C12H15Cl3Te, triclinic, P-1, a = 5.9471(11), b = 10.7826(22), c = 11.7983(19) Å, α = 75.416(12), β = 78.868(13), γ = 80.902(14)°, V = 713.6(2) Å3, Z = 2, R 1 = 0.021; (2): C14H11Cl3Te, orthorhombic, Pcab, a = 7.7189(10), b = 17.415(2), c = 21.568(3) Å, V = 2899.3(6) Å3, Z = 8, R 1 = 0.027.
Acta Crystallographica Section E Crystallographic Communications
In this study, four new piperazinium salts, namely, 4-phenylpiperazin-1-ium 4-ethoxybenzoate monohydrate, C9H9O3·C10H15N2·H2O (I); 4-phenylpiperazin-1-ium 4-methoxybenzoate monohydrate, C10H15N2·C8H7O3·H2O (II); 4-phenylpiperazin-1-ium 4-methylbenzoate monohydrate, C10H15N2·C8H7O2·H2O (III); and 4-phenylpiperazin-1-ium trifluoroacetate 0.12 hydrate, C10H15N2·C2F3O2·0.12H2O (IV), have been synthesized. The single-crystal structures of these compounds reveal that all of them crystallize in the triclinic P\overline{1} space group and the crystal packing of (I)–(III) is built up of ribbons formed by a combination of hydrogen bonds of type N—H...O, O—H...O and other weak interactions of type C—H...O and C—H...π, leading to a three-dimensional network. In the crystal of (IV), the cations and the anions are connected by C—H...O, N—H...O and C—H...F hydrogen bonds and by C—H...π interactions, forming sheets which in turn interact to maintain the crystal structure by linking through the oxyg...
Journal of the American Chemical Society, 1992
the dry nitrogen atmosphere of a glovebox. Reactions involving NF,' salts were carried out in 3/4 in. 0.d. Teflon-FEP ampules closed by a stainless steel valve. The I9F and ' H NMR spectra were measured at 84.6 and 90 MHz, respectively, on a Varian Model EM390 spectrometer, with 4-mm Teflon-FEP tubes (Wilmad Glass Co.) as sample containers and CFCI, and TMS, respectively, as internal standards, with negative shifts being upfield from the standards. Raman spectra were recorded on either a Cary Model 83 or a Spex Model 1403 spectrophotometer by use of the 488-nm exciting line of an Ar ion or the 647.1-nm line of a Kr ion laser, respectively. Baked-out Pyrex melting point capillaries were used as sample holders. Infrared spectra were recorded on a Perkin-Elmer Model 283 spectrophotometer as AgCl disks that were pressed in a Wilks minipress inside the drybox. The NF,BF,-N(CH,),F-CH,CN System. NF4BF4 (0.54 mmol) and N(CH,)4F (0.60 mmol) were loaded inside the drybox into a '/, in. Teflon-FEP ampule. On the vacuum line, dry CH,CN (3 mL liquid) was added at-196 "C, and the mixture was warmed to-31 "C for 30 min. The ampule was cooled to-78 "C, and the volatile material (0.45 mmol) was expanded into the vacuum line and shown by fractional condensation at-210 "C and infrared spectroscopy to consist mainly of NF, (0.40 mmol). The mixture in the ampule was then warmed for 3 h to-31 "C and for 1 h to room temperature, and an additional amount of NF, (0.13 mmol) was evolved. The solid residue (90.9 mg, weight calculated for 0.54 mmol of N(CH,),BF, and 0.06 mmol of unreacted N(CH,),F = 92.9 mg) was shown by vibrational spectroscopy to consist mainly of N(CH3),BF4. When the reaction was repeated using a 5-fold excess of N(CH,),F at-31 OC, the NF, evolution was 95% complete after 30 min. The NF4BF4-N(CH3),F-CHF3 System. NF4BF4 (2.19 mmol) and N(CH,),F (2.24 mmol) were combined in a Teflon ampule, and CHF, (50.26 mmol) was added at-196 OC. The mixture was warmed to-78 OC for 3 h and then cooled again to-196 "C, and the noncondensable gases (0.45 mmol of F2) were measured. Subsequently, the ampule was warmed to the melting point of CHF, (-155 "C), and the volatile material was removed in a dynamic vacuum by fractional condensation through traps kept at-186 and-210 "C. The-210 "C trap contained NF, (2.16 mmol). The solid residue, after being pumped on at room temperature (360 mg), consisted mainly of N(CH,)4BF4 (weight calculated for 2.19 mmol of N(CH,),BF, and 0.05 mmol N(CH,),F = 357 mg). When the reaction was repeated at-142 "C, only 10% of the theoretical amount of NF, was evolved in 3 h.
International journal of chemistry and technology, 2021
The molecular structure optimization of 3-Methyl-4-[3-ethoxy-(2-p-metilbenzenesulfonyloxy)-benzylidenamino]-4,5-dihydro-1H-1,2,4-triazol-5-one was obtained using the HF method and "B3LYP, B3PW91" functionals in the DFT method at the 6-31G (d, p) basis sets. The structure characterization performed using infrared (FT-IR), 13 C-NMR and 1 H-NMR spectral tools. Computational IR data was obtained at the Veda4f program. Theoretical 1 H/ 13 C-NMR(DMSO) isotropic shift values were assigned according to the GIAO method in the DMSO solvent. All the experimental data were available in the literature, these values are consistent with the calculated. Also, the theoretical results of different functionals were compared with each other. The HOMO-LUMO energies and energy difference (eV) were calculated and three-dimensional images are drawn. The no need to use the electronic parameters have been found using the energy difference (ΔE). The thermodynamics properties, mulliken atomic charges, geometric properties, dipole moments, total energy were calculated. The non linear optical (NLO) analysis was carried out. Additionally, with the MEP surface map, the nucleophilic and electrophilic regions of the molecule were determined.
Zeitschrift für Kristallographie - New Crystal Structures, 2015
C 65 H 67 Cl 2 O 5 P, monoclinic, P2 1 /c (no. 14), a =16.118(1) Å, b =10.0843(7) Å, c =35.113(2) Å, b =104.009(3)°, V =5537.5 Å 3 , Z =4,R gt (F) =0.0930, wR ref (F 2) =0.1855, T =173 K. Source of material To as olution of 5-bromo-25,26,27,28-tetrabenzyloxycalix[4]arene (2.270 g, 2.63 mmol) in THF (100 mL) at-78°C was slowly added n-buthyllithium (5.26 mmol). After 0.5 h, the resulting organolithium compound was quenched with chloro(ditert-butyl)-phosphane (0.951 g, 5.26 mmol). The solution was allowed to reach room temperature and was stirred for an additional 16 h. Hydrogen peroxide (30% in water, 20 mL) was then added, and the mixture was stirred for 1h .T he aqueous phase was washed with CH 2 Cl 2 (2´20 mL). Thecombined organic phases were dried over Na 2 SO 4 and evaporated under reduced pressure. The phosphane oxide was purified by columnchromatography on silica gel using CH 2 Cl 2 /MeOH (95 :5,v/v)aseluent(R f =0.45).
Journal of Molecular Structure, 1999
The IR (4000-400 cm Ϫ1) and Raman (4000-50 cm Ϫ1) spectra of 3-methoxymethylene-2,4-pentanedione (H 3 CO -CHyC (COCH 3) 2) in the liquid and solute forms in various solvents of different polarity were recorded at ambient temperature. Additional IR and Raman spectra were obtained for amorphous and crystalline solid at low temperature. The vibrational spectra revealed that compound exists atleast in two dominant conformers with different polarity and that conformer present in the solid phase is less polar. NMR spectra in various solvents at different temperatures were also obtained.The compound can exist in several conformers as a result of rotation around O-Cy and both yC-C bonds with planar or nonplanar arrangement of the heavy atoms. Semiempirical (AM1, PM3, MNDO, MINDO3) and ab initio using TZP and 6-31G** basis sets calculations were carried out. According to ab initio calculations at least five conformational structures with the methoxy group oriented as anti or syn and carbonyl groups oriented as Z or E towards the CyC double bond were obtained at energy surface. The calculated ab initio and AM1 energies of all conformers suggest as the most stable anti-ZE conformer where Z and E regard of the trans and cis acetyl group, respectively. As the second most stable conformer with energy at least 10 kJ mol Ϫ1 higher was calculated anti-EZ conformer. Assignments of the vibrational spectra for the studied compound were made with the aid of normal coordinate calculations employing scaled ab initio force field constants. The scaled ab initio frequencies as well as calculated energies indicate that the conformer present in the solid phase is anti-ZE.