Michael addition of phenylacetonitrile to the acrylonitrile group leading to diphenylpentanedinitrile. Structural data and theoretical calculations

2014 ◽  
Vol 68 (5) ◽  
Author(s):  
M. Percino ◽  
Margarita Cerón ◽  
Maria Castro ◽  
Guillermo Soriano-Moro ◽  
Victor Chapela ◽  
...  
Keyword(s):  
Michael Addition ◽  
Theoretical Calculations ◽  
Structural Data ◽  
Unit Cell ◽  
Structure Property ◽  
Unit Cell Parameters ◽  
Monoclinic System ◽  
Space Group ◽  
Cell Parameters ◽  
Structure Property Relationships

AbstractKnoevenagel condensation of phenylacetonitrile with 4-diphenylaminophenylacetonitrile in the presence of piperidine was carried out to obtain a novel conjugated compound. In addition to the expected compound 2-(phenyl)-3-(4-diphenylaminophenyl)acrylonitrile (I), the 3-((4-diphenylamino)phenyl)-2,4-diphenylpentanedinitrile (II) was also obtained with a good yield. Compound II was obtained as a result of the Michael addition of phenylacetonitrile with 2-(phenyl)-3-(4-diphenylaminophenyl)acrylonitrile (I). Conversely, when the same reaction was performed in the presence of KOH as catalyst, only the α,β-unsaturated nitrile (I) was afforded with a 92 % yield. The structures were confirmed with IR, EI-MS and NMR spectroscopy. Single crystals I and II were formed and their structures were determined by X-ray single-crystal diffraction analysis. Crystal I belongs to the monoclinic system with space group P21/n having unit cell parameters of a = 16.8589(5) Å, b = 6.68223(17) Å, c = 19.8289(7) Å, β = 111.133(4)○ and Z = 4. Crystal II belongs to the same monoclinic system with space group P21/c, having unit cell parameters of a = 10.8597(4) Å, b = 24.7533(10) Å, c = 9.7832(4) Å, β = 91.297(3)○ and Z = 4. In addition to the structural data analysis, some theoretical calculations that reveal the nature of relevant structure-property relationships are also reported.

scholarly journals Crystal structure of gluconate 5-dehydrogenase from Lentibacter algarum

2020 ◽  
Vol 76 (5) ◽  
pp. 228-234
Author(s):  
Dengke Tian ◽  
Xueqi Fu ◽  
Wenqiang Cao ◽  
Hong Yuan
Keyword(s):  
Crystal Structure ◽  
Escherichia Coli ◽  
Structural Similarity ◽  
Unit Cell ◽  
Unit Cell Parameters ◽  
Monoclinic System ◽  
Space Group ◽  
Cell Parameters ◽  
High Structural Similarity

Gluconate 5-dehydrogenase (Ga5DH; EC 1.1.1.69) from Lentibacter algarum (LaGa5DH) was recombinantly expressed in Escherichia coli and purified to homogeneity. The protein was crystallized and the crystal structure was solved at 2.1 Å resolution. The crystal belonged to the monoclinic system, with space group P1 and unit-cell parameters a = 55.42, b = 55.48, c = 79.16 Å, α = 100.51, β = 105.66, γ = 97.99°. The structure revealed LaGaDH to be a tetramer, with each subunit consisting of six α-helices and three antiparallel β-hairpins. LaGa5DH has high structural similarity to other Ga5DH proteins, demonstrating that this enzyme is highly conserved.

Synthesis and X-ray diffraction data of 1-N-(4-pyridylmethyl)amino naphthalene

2010 ◽  
Vol 25 (1) ◽  
pp. 72-74 ◽  
Author(s):  
H. A. Camargo ◽  
J. A. Henao ◽  
D. F. Amado ◽  
V. V. Kouznetsov
Keyword(s):  
Diffraction Pattern ◽  
Powder Diffraction ◽  
Diffraction Data ◽  
Unit Cell ◽  
X Ray Diffraction ◽  
Unit Cell Parameters ◽  
Monoclinic System ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters

1-N-(4-pyridylmethyl)amino naphtalene was synthesized by means of a reaction of alpha-naphthylamine, 4-pyridylcarboxyaldehyde, in anhydrous ethanol to obtainN-(4-pyridylen)-alpha-naphthylamine and that was reduced with NaBH4 to produce the wanted compound. The X-ray powder diffraction pattern for the new compound 1-N-(4-pyrydylmethyl)amino naphtalene was obtained. This compound crystallizes in a monoclinic system with refined unit cell parameters a=10.375(5) Å, b=17.665(6) Å, c=5.566(2) Å, β=100.11(3), and V=1004.3(5) Å3, with space group P2/m (No. 10).

Molecular and Crystal Structure of Sildenafil Base

2012 ◽  
Vol 67 (5) ◽  
pp. 491-494 ◽  
Author(s):  
Dmitrijs Stepanovs ◽  
Anatoly Mishnev
Keyword(s):  
Crystal Structure ◽  
Erectile Dysfunction ◽  
Crystal Structures ◽  
Unit Cell ◽  
Sildenafil Citrate ◽  
Unit Cell Parameters ◽  
Monoclinic System ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters

Sildenafil citrate monohydrate, well known as Viagra®, is a drug for the treatment of erectile dysfunction. Here we present the X-ray crystal structure of the sildenafil base, C22H30N6O4S. The compound crystallizes in the monoclinic system, space group P21/c with the unit cell parameters a = 17:273(1), b=17:0710(8), c=8:3171(4) Å , b =99:326(2), Z = 4, V = 2420:0(3) Å3. A comparison with the known crystal structures of sildenafil citrate monohydrate and sildenafil saccharinate is also presented.

scholarly journals Synthesis and Crystal Structure of 1-Methyl-3-(2-pyridyl)imidazolium Hexafluorophosphate

2014 ◽  
Vol 2014 ◽  
pp. 1-4
Author(s):  
Elango Kandasamy
Keyword(s):  
Crystal Structure ◽  
Solid State ◽  
Weak Interactions ◽  
Unit Cell ◽  
State Structure ◽  
Unit Cell Parameters ◽  
Monoclinic System ◽  
Synthesis And Crystal Structure ◽  
Space Group ◽  
Cell Parameters

Compound 1-Methyl-3-(2-pyridyl)imidazolium hexafluorophosphate was crystallized in monoclinic system with space group P21/c and unit cell parameters a=7.3740(8) Å, b=15.5931(16) Å, c=10.4787(11) Å, β= 105.3102°, and  ν=1162.12Å3. The obtained solid state structure of 1-Methyl-3-(2-pyridyl)imidazolium hexafluorophosphate shows CH⋯F type weak interactions and was analyzed.

Synthesis and X-ray diffraction data of 6,8-dimethyl-cis-2-vinyl-2,3,4,5-tetrahydro-1H-benzo[b]azepin-4-ol and 8-chloro-9-methyl-cis-2-(prop-1-en-2-yl)-2,3,4,5-tetrahydro-1H-benzo[b]azepin-4-ol

2011 ◽  
Vol 26 (4) ◽  
pp. 346-349 ◽  
Author(s):  
M. A. Macías ◽  
J. A. Henao ◽  
Lina María Acosta ◽  
Alirio Palma
Keyword(s):  
Unit Cell ◽  
Chemical Formula ◽  
X Ray Diffraction ◽  
Unit Cell Parameters ◽  
Monoclinic System ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters ◽  
Diffraction Patterns ◽  
New Compounds

The 6,8-dimethyl-cis-2-vinyl-2,3,4,5-tetrahydro-1H-benzo[b]azepin-4-ol (2a) (Chemical formula C14H19NO) and 8-chloro-9-methyl-cis-2-(prop-1-en-2-yl)-2,3,4,5-tetrahydro-1H-benzo[b]azepin-4-ol (2b) (Chemical formula C14H18ClNO) were prepared via the reductive cleavage of the bridged N-O bond of the corresponding 1,4-epoxytetrahydro-1-benzazepines. The X-ray powder diffraction patterns for the new compounds were obtained. The compound 2a was found to crystallize in an orthorhombic system with space group Pmn21 (No. 31), refined unit-cell parameters a = 19.422(6) Å, b = 6.512(3) Å, c = 9.757(4) Å and V = 1234.0(5) Å3. The compound 2b was found to crystallize in a monoclinic system with space group P21/m (No. 11), refined unit-cell parameters a = 17.570(4) Å, b = 8.952(3) Å, c = 14.985(4) Å, β = 101.66(2)°, and V = 2308.3(9) Å3.

scholarly journals Chemical Preparations and X-ray Diffraction Data of Cyclotriphosphates Type MnMII2(P3O9)2.nH2O with MII Alkaline Earths

2021 ◽  
Vol 12 (5) ◽  
pp. 6021-6031
Keyword(s):  
Diffraction Data ◽  
Ion Exchange Resin ◽  
Unit Cell ◽  
Unit Cell Parameters ◽  
Monoclinic System ◽  
Preparation Methods ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters ◽  
Alkaline Earths

Chemical preparation methods and X-ray powder diffraction data, XPRD, are reported for four cyclotriphosphates associated with manganese MnMII2(P3O9)2.nH2O with MII alkaline earths. These phosphates are MnCa2(P3O9)2.10H2O, MnCa2(P3O9)2, MnSr2(P3O9)2.4H2O and MnBa2(P3O9)2.6H2O. The condensed phosphates MnSr2(P3O9)2.4H2O and MnBa2(P3O9)2.6H2O were prepared by the method of ion-exchange resin, whereas MnCa2(P3O9)2.10H2O was prepared by using nitrates and MnCa2(P3O9)2 was obtained by total thermal dehydration of MnCa2(P3O9)2.10H2O. MnSr2(P3O9)2.4H2O crystallizes in the triclinic system, space group is P-1, Z = 1, the unit-cell parameters are : a = 6,653(1)Å, b = 7,110(1)Å, c = 5,123(1)Å, α = 103,37(2)°, β = 95,81(2)°, γ = 93,04(2)° and the factors of merit, M(20) = 29.6 and F(30) = 34.4. MnCa2(P3O9)2.10H2O crystallizes in the monoclinic system, space group is P21/n, the unit-cell parameters of MnCa2(P3O9)2.10H2O are : a = 9.631 (5) Å, b = 18.173 (7) Å, c = 7.976 (4) Å, β = 109.438 (4), Z = 2 and V = 1045,1 (3) Å3. MnCa2(P3O9)2 an hexagonal symetry, Z = 2, the space group is P3 and the unit-cell parameters are a = 7.392 Å (9) and c = 20.134 (2) Å. MnBa2(P3O9)2.6H2O crystallizes in the triclinic unit cell, , Z = 2, the space group is P-1 and its unit-cell parameters are : a = 7,479 (6)Å, b = 11,942 (8)Å, c = 12,786 (9)Å, α = 105,94(7)°, β = 98,40°(7), γ = 98,16 (7)° and V = 1046,8 (2)Å3.

Powder diffraction investigations of 2,2′-Thiobis(4-methyl-6-tert-butylphenol) and 2,2′-Methylenebis(4-methyl-6-tert-butylphenol)

2005 ◽  
Vol 20 (1) ◽  
pp. 67-70
Author(s):  
B. Lasocha ◽  
M. Grzywa ◽  
W. Lasocha
Keyword(s):  
Room Temperature ◽  
Unit Cell ◽  
X Ray Diffraction ◽  
Unit Cell Parameters ◽  
Monoclinic System ◽  
Orthorhombic System ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters ◽  
Phenol Derivatives

X-ray diffraction investigations of two phenol derivatives - 2,2′-Thiobis(4-methyl-6-tert-butylphenol) and 2,2′-Methylenebis(4-methyl-6-tert-butylphenol) were carried out. Both compounds at room temperature have similar cell volume and the same number of molecules in an unit cell. However, 2,2′-Thiobis(4-methyl-6-tert-butylphenol) crystallizes in the monoclinic system with unit cell parameters refined to a=0.8278(2) nm, b=1.2968(4) nm, c=1.9493(7) nm, β=90.93(2)°, space group P21∕n(14), whereas 2,2′-Methylenebis(4-methyl-6-tert-butylphenol) crystallizes in the orthorhombic system with unit cell parameters refined to a=1.6203(5) nm, b=1.2827(5) nm, c=1.0197(3) nm, space group Pna21(33). The investigated C22H30O2S turned out to be a new polymorph of 2,2′-Thiobis(4-methyl-6-tert-butylphenol).

scholarly journals X-ray, Hirshfeld surface analysis, spectroscopic and DFT studies of polycyclic aromatic hydrocarbons: Fluoranthene and acenaphthene

2015 ◽  
Vol 80 (12) ◽  
pp. 1489-1504 ◽  
Author(s):  
Wioleta Śmiszek-Lindert ◽  
Anna Michta ◽  
Aleksandra Tyl ◽  
Grzegorz Małecki ◽  
Elżbieta Chełmecka ◽  
...  
Keyword(s):  
Theoretical Calculations ◽  
Unit Cell ◽  
Computational Method ◽  
Orthorhombic Crystal ◽  
Monoclinic System ◽  
Space Group ◽  
X Ray ◽  
Cell Parameters ◽  
Hirshfeld Surfaces ◽  
Polycyclic Aromatic

The X-ray structure, theoretical calculation, Hirshfeld surfaces analysis, IR and Raman spectra of fluoranthene and acenaphthene were reported. Acenaphthene crystallizes in the orthorhombic crystal system and space group P21ma, with crystal parameters a = 7.2053 (9) ?, b = 13.9800 (15) ?, c = 8.2638 (8) ?, Z = 4 and V = 832.41 (16) ?3. In turn, the grown crystals of fluoranthene are in monoclinic system with space group P21/n. The unit cell parameters are a = 18.3490 (2) ?, b = 6.2273 (5) ?, c = 19.8610 (2) ?, ? = 109.787 (13)?, Z = 8 and unit cell volume is 2135.50 (4) ?3. Theoretical calculations of the title compounds isolated molecule have been carried out using DFT at the B3LYP level. The intermolecular interactions in the crystal structure, for both the title PAHs, were analyzed using Hirshfeld surfaces computational method.

Crystal and molecular structure of fenspiride, C15H20N2O2

2020 ◽  
Vol 35 (2) ◽  
pp. 144-146
Author(s):  
Silvina Pagola
Keyword(s):  
Molecular Structure ◽  
General Position ◽  
Crystal And Molecular Structure ◽  
Unit Cell ◽  
Unit Cell Parameters ◽  
Monoclinic System ◽  
Inflammatory Drug ◽  
Space Group ◽  
Cell Parameters ◽  
Independent Molecules

The crystal and molecular structure of fenspiride, a bronchodilator and anti-inflammatory drug, are reported. Fenspiride crystallizes in the monoclinic system, with two crystallographically independent molecules in the general position of the space group P21/n (No. 14) and Z = 8. Rietveld refined unit cell parameters are a = 11.52013(8) Å, b = 5.614091(31) Å, c = 44.1567(4) Å, α = 90°, β = 93.0885(6)°, γ = 90°, and V = 2851.69(4) Å3.

scholarly journals New crystal structures of adenylate kinase fromStreptococcus pneumoniaeD39 in two conformations

2014 ◽  
Vol 70 (11) ◽  
pp. 1468-1471
Author(s):  
Trung Thanh Thach ◽  
Sangho Lee
Keyword(s):  
Crystal Structures ◽  
Adenylate Kinase ◽  
Bound States ◽  
Critical Role ◽  
Unit Cell ◽  
Unit Cell Parameters ◽  
Space Group ◽  
Cell Parameters ◽  
Ligand Free ◽  
Adenylate Kinases

Adenylate kinases (AdKs; EC 2.7.3.4) play a critical role in intercellular homeostasis by the interconversion of ATP and AMP to two ADP molecules. Crystal structures of adenylate kinase fromStreptococcus pneumoniaeD39 (SpAdK) have recently been determined using ligand-free and inhibitor-bound crystals belonging to space groupsP21andP1, respectively. Here, new crystal structures of SpAdK in ligand-free and inhibitor-bound states determined at 1.96 and 1.65 Å resolution, respectively, are reported. The new ligand-free crystal belonged to space groupC2, with unit-cell parametersa= 73.5,b= 54.3,c= 62.7 Å, β = 118.8°. The new ligand-free structure revealed an open conformation that differed from the previously determined conformation, with an r.m.s.d on Cαatoms of 1.4 Å. The new crystal of the complex with the two-substrate-mimicking inhibitorP1,P5-bis(adenosine-5′-)pentaphosphate (Ap5A) belonged to space groupP1, with unit-cell parametersa= 53.9,b= 62.3,c= 63.0 Å, α = 101.9, β = 112.6, γ = 89.9°. Despite belonging to the same space group as the previously reported crystal, the new Ap5A-bound crystal contains four molecules in the asymmetric unit, compared with two in the previous crystal, and shows slightly different lattice contacts. These results demonstrate that SpAdK can crystallize promiscuously in different forms and that the open structure is flexible in conformation.

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