J. A. Henao

Synthesis and X-ray diffraction data of 2-morpholino-2-(3,4,5-trimethoxyphenyl)acetonitrile, (C15H20N2O4)

The α -aminonitrile, 2-morpholino-2-(3,4,5-trimethoxyphenyl)acetonitrile (C 15 H 20 N 2 O 4 ), was prepared through a silica sulfuric acid-catalyzed Strecker reaction between 3,4,5-trimethoxybenzaldehyde, morpholine, and two different cyanide sources. Molecular characterization was performed by Fourier transform infrared spectroscopy, gas chromatography–mass spectrometry, ( 1 H, 13 C – mono and bidimensional) nuclear magnetic resonance; crystallographic characterization was completed by X-ray powder diffraction of polycrystalline samples. The title compounds crystallized in a monoclinic system and unit-cell parameters are reported [ a = 13.904(2), b = 5.1696(6), c = 21.628(3) A, β = 104.31(1)°, unit-cell volume V = 1506.3(3) A 3 , Z = 4]. All measured lines were indexed with the P 2 1 / a (No. 14) space group.

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

1- N -(4-pyridylmethyl)amino naphtalene was synthesized by means of a reaction of alpha-naphthylamine, 4-pyridylcarboxyaldehyde, in anhydrous ethanol to obtain N -(4-pyridylen)-alpha-naphthylamine and that was reduced with NaBH 4 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) A, b =17.665(6) A, c =5.566(2) A, β=100.11(3), and V =1004.3(5) A 3 , with space group P2/m (No. 10).

X-ray powder diffraction data of (25R)-spirost-5-en-3β-ol(diosgenin)

The diosgenin, (25R)-spirost-5-en-3 β -ol, was isolated from rhizomes of dioscorea meridensis and characterized by X-ray powder diffraction, IR and MS. The diosgenin was found to be monoclinic, with refined unit cell parameters a =16.774(3), b =7.259(2), c =10.383(2) A, β =92.74(2)°, V =1262.9(3) (A 3 ), Z =2, D x ( g ∕cm− 3 )1.089, with space group P 2 1 (No. 4).

X-ray powder diffraction data and characterization of Mirabegron

Mirabegron, (C 21 H 24 N 4 O 2 S), is a β 3 -adrenoceptor agonist approved in Japan, the USA, Canada and Europe, for the treatment of overactive bladder symptoms. There are no entries for this important active pharmaceutical ingredient in the Cambridge Structural Database or the Powder Diffraction File-4/Organics database. In this contribution, the powder diffraction pattern of Mirabegron, an unreported phase, are presented with a study by spectroscopy methods (Fourier-transform infrared spectroscopy [FT-IR] and RAMAN) and thermal analysis (thermogravimetric analysis [TGA]-differential scanning calorimetry [DSC]).

Characterization by X-ray powder diffraction of alpha lipoic acid

Alpha lipoic acid (ALA) C 8 H 14 O 2 S 2 is a naturally occurring compound that is synthesized in small amounts by plants and animals, including humans. ALA is covalently bound to specific proteins, which function as cofactors for several important mitochondrial enzyme complexes and studies suggest that they might help with type 2 diabetes. In the Cambridge Structural Database, there are four entries related to this compound: two for lipoic acid and two for complexes. In the Powder Diffraction File-4, two experimental unindexed patterns are reported. The material crystallizes in a monoclinic crystal system, space group P 2 1 / a and cell parameters a = 9.237 (1) A, b = 9.960 (1) A, c = 11.787 (2) A, β = 109.13 (1)°, and V = 1024.6 (2) A 3 .

Synthesis and X-ray diffraction data for dibromo-dioxo-(1,10-phenanthroline-N,N′)-molybdenum(VI) (C12H8N2MoBr2O2)

The dibromo-dioxo-(1,10-phenanthroline-N,N′)-molybdenum(VI) complex (C 12 H 8 N 2 MoBr 2 O 2 ) was prepared from molybdic acid and 1,10-phenanthroline using hydrobromic acid as solvent. The molybdenum complex solid was separated by filtration and washed with ethyl ether. The X-ray powder diffraction pattern for the title compound was analyzed and found to crystallizes in monoclinic system, space group P 2 1 /c (No14) with refined unit-cell parameters a = 12.036 (1), b = 9.819 (1), c = 12.671 (2) A, and β = 110.44° (1). The volume of the unit cell is V = 1403.2 (3) A 3 .

CCDC 1507508: Experimental Crystal Structure Determination

Related Article: J.H. Quintana Mendoza, J.A. Henao, E. Robles Marin, J.M. Urbina Gonzalez|2016|IUCrData|1|x161538|doi:10.1107/S2414314616015388

4,6-Dimethyl-2-(3-pyridyl)quinolin-5-amine.

The title compound, C(16)H(15)N(3), shows a hindrance effect between adjacent amino and methyl groups that leads to a structural distortion, which is reflected in the non-planarity of the quinoline entity and in the bond angles and distances. The crystal packing consists of chains along the b axis sustained by an intermolecular hydrogen bond between the amino group and the N atom of the pyridyl ring.

X-ray powder diffraction analysis of 2-exo-(β-pyridyl)-6-exo-phenyl-7-oxa-1-azabicyclo[2.2.1]heptane

The X-ray powder diffraction pattern for a bridgehead heterocyclic system was determined. 2- exo -(β-pyridyl)-6- exo -phenyl-7- oxa -1-azabicyclo[2.2.1]heptane, C 16 H 16 N 2 O, is triclinic with refined unit cell parameters a =1.1012(2), b =1.3950(2), c =1.0074(3) nm, α=111.09(2)°, β=104.97(2)°, γ=77.38(2)°, V =1.3813(3) nm 3 , Z =4, and D x =1.212 g/cm 3 with space group P -1 (No. 2).