scholarly journals Synthesis, Structure, and Cyclocondensation of the 4,4,4-Trifluoro-3,3-dihydroxy-2-methyl-1-(thien-2-yl)-1-butanone with Hydroxylamine and Hydrazine

2018 ◽  
Vol 2018 ◽  
pp. 1-8
Author(s):  
Alex F. C. Flores ◽  
Bruna P. Kuhn ◽  
Darlene C. Flores ◽  
Mariano A. Pereira ◽  
Tatiane L. Balliano ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Structural Analysis ◽  
Torsion Angle ◽  
Trifluoroacetic Anhydride ◽  
X Ray ◽  
Disorder Effect

The synthesis of 4,4,4-trifluoro-3,3-dihydroxy-2-methyl-1-(thien-2-yl)butan-1-one (3) through acylation of 1,1-dimethoxy-1-(thien-2-yl)propane (1) with trifluoroacetic anhydride and its reactions with hydroxylamine and hydrazine was investigated. X-ray structural analysis of new trifluoromethyl-substituted dielectrophile 3 revealed that this hydrate exists as a racemate with inter- and intramolecular O-H·O bonds. The crystal structure shows alignment along axis b of pair molecules with the same configuration of the O2-H·O1 bond. For 5(3)-trifluoromethyl-4-methyl-3(5)-(thien-2-yl)-1H-pyrazole (4), obtained via cyclocondensation of precursor 2 and hydrazine hydrochloride, X-ray structural analysis indicated that its rings are almost planar (torsion angle N2-C5-C6-C7–5.4°) and that S1 at the thienyl moiety is anti-periplanar to N2 (torsion angle N2-C5-C6-S1 176.01); no disorder effect was observed for the thienyl ring.

The synthesis, molecular and crystal structure of the 1:1 adduct of triphenyltin chloride with 2,3-diphenylthiazolidin-4-one

1995 ◽  
Vol 73 (1) ◽  
pp. 95-99 ◽  
Author(s):  
Frank E. Smith ◽  
Rosemary C. Hynes ◽  
John Tierney ◽  
Ying Z. Zhang ◽  
George Eng
Keyword(s):  
Crystal Structure ◽  
Structural Analysis ◽  
Oxygen Atom ◽  
Dutch Elm Disease ◽  
Monoclinic Space Group ◽  
Monodentate Ligand ◽  
X Ray ◽  
Trigonal Bipyramidal ◽  
Triphenyltin Chloride ◽  
Mössbauer Data

The title compound was synthesized as part of an effort to produce a more effective fungicide to combat Dutch Elm Disease (DED), which is caused by the fungus Ceratocystisulmi. A full X-ray structural analysis of the 1:1 adduct has been carried out and the results are reported along with the Mössbauer data for the compound. The crystals are monoclinic, space group P21/a with a = 19.240(3) Å, b = 9.1463(24) Å, c = 19.3512(24) Å, β = 118.874(8)°, V = 2982.0(10) Å3, z = 4, and Dcalc = 1.427 Mg m−3. The final discrepancy factors are RF = 0.056 and Rw = 0.058 for 1915 significant reflections. The QS and IS values in the Mössbauer spectrum of the complex are 3.08 mm s−1 and 1.28 mm s−1, respectively. The 2,3-diphenylthiazolidin-4-one behaves as a monodentate ligand and coordinates to the tin through the oxygen atom. The complex exhibits a trigonal bipyramidal configuration with the three phenyl groups in equatorial positions and the chloride and ligand oxygen occupying the apical sites. Keywords: triorganotin, fungicide, Dutch Elm Disease, thiazolidin-4-one.

Cyano-Bridged Bimetallic Complexes of Copper(II) with Nitroprusside. Crystal Structure of [Cu(H2NCH2CH(NH2)CH3)2Fe(CN)5NO] . H2O

2000 ◽  
Vol 53 (3) ◽  
pp. 225 ◽  
Author(s):  
Zdenek Smékal ◽  
Zdenek Trávnícek ◽  
Jaromír Marek ◽  
Milan Nádvornik
Keyword(s):  
Crystal Structure ◽  
Structural Analysis ◽  
Magnetic Measurements ◽  
X Ray ◽  
Cyanide Group ◽  
Cyanide Ligand ◽  
Binuclear Structure ◽  
Tetragonal Pyramidal ◽  
Cyanide Ligands ◽  
Diamine Ligands

Five new complexes of compositions [Cu(1,2-pn)2Fe(CN)5NO]·H2O (1,2-pn = propane-1,2-diamine) and [Cu(L)Fe(CN)5NO]·xH2O (L = tmen (N,N,N′,N′-tetramethylethane-1,2-diamine), x = 0.5; L = trimeen (N,N,N′-trimethylethane-1,2-diamine), x = 1; L = dien (N-(2-aminoethyl)ethane-1,2-diamine), x = 0; L = medpt (N-(3-aminopropyl)-N-methylpropane-1,3-diamine), x = 2) have been isolated from the reaction mixture of Cu(ClO4)2·6H2O (or CuCl2·2H2O), the amine and Na2 [Fe(CN)5NO]·2H2O in water. The complexes have been characterized by infrared and ultraviolet–visible spectroscopies, and magnetic measurements. Single-crystal X-ray structural analysis revealed that the [Cu(1,2-pn)2Fe(CN)5NO]·H2O complex assumes a cyanide-bridged binuclear structure in which iron(II) is six-coordinated by five cyanide ligands and one nitrosyl group (the nitrosyl group lies cis to the bridging cyanide group), while copper(II) is five-coordinated by two propane-1,2-diamine ligands and a bridging cyanide ligand in a distorted tetragonal pyramidal arrangement.

scholarly journals Unusual formation of (E)-11-(aminomethylene)-8,9,10,11-tetrahydropyrido[2′,3′:4,5]pyrimido[1,2-a]azepin-5(7H)-one and its crystal structure

2017 ◽  
Vol 73 (10) ◽  
pp. 1497-1500
Author(s):  
Khamid U. Khodjaniyazov ◽  
Utkir S. Makhmudov ◽  
Kambarali K. Turgunov ◽  
Burkhon Z. Elmuradov
Keyword(s):  
Crystal Structure ◽  
Structural Analysis ◽  
Aqueous Ammonia ◽  
Boat Conformation ◽  
X Ray ◽  
First Time ◽  
Twist Boat ◽  
Unusual Formation

Selective C-formylation of 8,9,10,11-tetrahydropyrido[2′,3′:4,5]pyrimido[1,2-a]-azepin-5(7H)-one has been studied for the first time. It was revealed that formylation proceeds by the formation of an intermediate salt, which due to the re-amination process on treatment with aqueous ammonia transformed into the corresponding (E)-11-(aminomethylene)-8,9,10,11-tetrahydropyrido[2′,3′:4,5]-pyrimido[1,2-a]azepin-5(7H)-one, C13H14N4O, as anE-isomer. Formylation was carried out by Vilsmeier–Haack reagent and the structure of the synthesized compound was confirmed by X-ray structural analysis, spectroscopic and LC–MS methods. In the molecule, the seven-membered pentamethylene ring adopts a twist-boat conformation.

Synthesis and X-ray diffraction analysis of the tetrazole peptide analogue Pro-LeuΨ[CN4]Gly-NH2

1988 ◽  
Vol 53 (11) ◽  
pp. 2863-2876 ◽  
Author(s):  
Giovanni Valle ◽  
Marco Crisma ◽  
Kuo-Long Yu ◽  
Claudio Toniolo ◽  
Ram K. Mishra ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bond ◽  
Diffraction Analysis ◽  
Dopamine Receptor ◽  
Torsion Angle ◽  
Peptide Bond ◽  
X Ray Diffraction ◽  
X Ray ◽  
Conformationally Restricted ◽  
Bond Characteristic

The synthesis of an analogue of the neuropharmacologically active peptide Pro-Leu-Gly-NH2 in which the Leu-Gly peptide bond has been replaced with a tetrazole moiety was carried out. The molecular and crystal structure of the tetrazole analogue Pro-Leuψ[CN4]Gly-NH2 was determined by X-ray diffraction and a comparison was made with the published X-ray structure of Pro-Leu-Gly-NH2. The tetrazole annular system turns out to be a good conformationally-restricted replacement for the cis-peptide bond in terms of bond lengths, bond angles and the ω torsion angle. The molecule was found to be folded at the -Leuψ[CN4]Gly- sequence, but it did not form the intramolecular N-H···O=C hydrogen bond characteristic of the type Vla β-bend conformation. In contrast to Pro-Leu-Gly-NH2, Pro-Leuψ[CN4]Gly-NH2 was found to be unable to enhance the binding of dopamine receptor agonists to the dopamine receptor.

Synthesis and1H NMR Structural Analysis of 11-Aryl/Heteroarylnaphtho[2,1-b]furans: X-Ray Crystal Structure of 11-(4′-Pyridyl)naphtho[2,1-b]furan.

ChemInform ◽  
2005 ◽  
Vol 36 (47) ◽  
Author(s):  
Sabir H. Mashraqui ◽  
Mamta B. Patil ◽  
Yogesh Sangvikar ◽  
Mohamed Ashraf ◽  
Hitesh D. Mistry ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Structural Analysis ◽  
X Ray

Synthesis, Crystal Structure and Photoluminescence of 1,2-Bis(phenylselenyl)-1,2-dicarba-closo-dodecaborane(12)

2011 ◽  
Vol 66 (1) ◽  
pp. 65-68
Author(s):  
Jinling Miao ◽  
Hongwei Chen ◽  
Meiling Xu ◽  
Bin Peng ◽  
Yong Nie ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Single Crystal ◽  
Torsion Angle ◽  
Title Compound ◽  
Uv Light ◽  
X Ray Diffraction ◽  
Violet Emission ◽  
X Ray

The reaction of dithio-o-carborane with diphenyldiselenide (PhSeSePh) affords the title compound, closo-1,2-(PhSe)2C2B10H10 (1), which has been characterized by IR and NMR (1H, 11B) spectroscopy and by single-crystal X-ray diffraction. The phenylselenyl groups are bonded to the cage carbon atoms of the o-carborane cluster with a Ccage-Ccage distance of 1.751(6) Å and an Se-Ccage- Ccage-Se torsion angle of 10.1(3)°. Compound 1 displays a violet emission on excitation with UV light. For comparison the photoluminescence of the known analog closo-1,2-(PhS)2C2B10H10 (2) was also studied

The crystal structure of nickel(II) dimethyldithiocarbamate

1980 ◽  
Vol 45 (8) ◽  
pp. 2147-2151 ◽  
Author(s):  
Jan Lokaj ◽  
Ján Garaj ◽  
Viktor Kettmann ◽  
Viktor Vrábel
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Structural Analysis ◽  
Least Squares ◽  
Least Squares Method ◽  
Crystal And Molecular Structure ◽  
Unit Cell ◽  
Special Position ◽  
X Ray ◽  
Triclinic Unit Cell

Crystal and molecular structure of nickel(II) dimethyldithiocarbamate, Ni[S2CN(CH3)2]2 was solved by X-ray structural analysis and refined by the least squares method to R = 0.06 for 1065 reflections. The compound crystallizes in a space group P I and the triclinic unit cell has the dimensions: a = 6.521 (7), b = 6.798 (9), c = 7.633 (4), α = 67.21 (8)°, β = 67.34 (6)° γ =85.59 (9)°. The experimentally observed density is 1.75 g cm-3 and the calculated value for Z = 1 is 1.73 g cm-3. In the structure , the Ni atom occupies a special position in the centre of symmetry and is coordinated by four sulphur atoms in a plane: Ni-S 0.2218 (4) and 0.2198 nm S1-Ni-S2 angle 79.62 (8)°. The ligand S2CNC2 is nearly planar.

Darstellung und Kristallstruktur von Cs2Sn3Se7, ein Cäsium-selenostannat(IV) mit fünffach koordiniertem Zinn / Preparation and Crystal Structure of Cs2Sn3Se7, a Cesium Selenostannate(IV) with Pentacoordinated Tin

1990 ◽  
Vol 45 (12) ◽  
pp. 1643-1646 ◽  
Author(s):  
W. S. Sheldrick ◽  
H.-G. Braunbeck
Keyword(s):  
Crystal Structure ◽  
Structural Analysis ◽  
Asymmetric Unit ◽  
X Ray ◽  
Coordination Numbers

Methanolothermal reaction of Cs2CO3 with SnSe, in the presence of SnSe at 160 C and 13 bar yields the selenostannates(IV) Cs4Sn2Se6 and Cs,Sn3Se7. The structure of the latter phase was established by X-ray structural analysis. The crystal structure contains polyselenostannate(IV) sheet anions [Sn3Se72-]∞2, for which the basic elements are trigonal SnSe5-bipyramids. Six of the seven independent selenium atoms in the asymmetric unit are coordinated by two tin atoms, one by three atoms. Neighbouring anion sheets are so placed that channels are formed which contain two independent cesium cations; these display coordination numbers of, respectively, eight and seven.

Synthesis and1HNMR structural analysis of 11-aryl/heteroarylnaphtha[2,1-b]furans: X-ray crystal structure of 11-(4′-pyridyl)naphtho[2,1 -b]furan

2005 ◽  
Vol 42 (5) ◽  
pp. 947-954 ◽  
Author(s):  
Sabir H Mashraqui ◽  
Mamta B Patil ◽  
Yogesh Sangvikar ◽  
Mohamed Ashraf ◽  
Hitesh D Mistry ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Structural Analysis ◽  
X Ray

The crystal and molecular structure of aqua-bis(ethylenediamine)cupric-tris(cyano)-selenocyanatodicuprate

1982 ◽  
Vol 47 (10) ◽  
pp. 2623-2632 ◽  
Author(s):  
Viktor Vrábel ◽  
Jan Lokaj ◽  
Ján Garaj ◽  
František Pavelčík
Keyword(s):  
Molecular Structure ◽  
Crystal Structure ◽  
Structural Analysis ◽  
Least Squares Method ◽  
Crystal And Molecular Structure ◽  
Three Dimensional ◽  
Monoclinic System ◽  
Space Group ◽  
X Ray ◽  
Triclinic System

The crystal structure of [Cu(H2O)(en)2][Cu2(CN)3(SeCN)] was solved by single crystal X-ray structural analysis in the triclinic system with a space group of P1 and in the monoclinic system with a space group of C2. In the triclinic system the unit cell has dimensions of a = 0.8445(3), b = 0.7903(3), c = 0.8444(3) nm, α = 119.58(2), β = 118.59(2) and γ = 93.63(3)° and, in the monoclinic system, a = 1.3331(4), b = 0.8670(2), c = 0.8267(3), β = 122.60(2)°. The structure was refined by the least squares method to final value of R = 5.5% in the triclinic system and R = 7.8% in the monoclinic system. The coordination sphere around the Cu(II) atom is square pyramidal, formed of two ethylenediamine molecules and one water molecule. The Cu(I) atoms are tetrahedrally coordinated by bridging SeCN and CN ligands to form infinite three-dimensional chains. The SeCN group is bonded to the Cu(I) atoms through the Se atom at distances of 0.2731(3) and 0.2745(3) nm.

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