Cheng-Jun Hao, Yao Wang, Songwei Chen
Dec 1, 2010
Citations
0
Influential Citations
0
Citations
Journal
Zeitschrift für Kristallographie - New Crystal Structures
Abstract
C13H17N3O2, orthorhombic, P212121 (no. 19), a = 6.548(1) Å, b = 12.609(3) Å, c = 16.605(3) Å, V = 1371.0 Å, Z = 4, Rgt(F) = 0.043, wRref(F) = 0.130, T = 293 K. Source of material 3-(5-Methyl-3-phenyl-1H-pyrazol-1-yl)propanamide was prepared according to [1]. A total of 1.99 g (10 mmol) 3-iodopropanamide and 1.58 g (10 mmol) 5-methyl-3-phenyl-1H-pyrazole were dissolved in 4 ml of DMSO. A sodium carbonate was then added to this solution. The mixture was heated at 60 °C for 5 h. Crystals suitable for X-ray structure analysis were obtained by recrystallization of the solid row product from ethanol solution by slow evaporation for a week at room temperature. Discussion Pyrazole and ist derivatives exhibit herbicidal and fungicidal activities. The title crystal structure is build up of the neutral molecules C13H17N3O2 and lattice water. Three intra-molecular O2– H22···O1, N3–H31···N2, N3–H32···O2 and an inter-molecular O2–H21···O1 hydrogen bonds give rise to a molecular onedimensional chain, parallel to [011]. Aromatic --stacking interactions exist between chains. The dihedral angle between the benzene ring and the 1H-pyrazole ring (C7/C8/C9/N1/N2) is 26.75°. There exist -···interaction with a plane-to-plane separation of 3.699 Å and a centroid-to-centroid distance of 6.548 Å. Z. Kristallogr. NCS 225 (2010) 727-728 / DOI 10.1524/ncrs.2010.0321 727 © by Oldenbourg Wissenschaftsverlag, München Crystal: yellow prism, size 0.09 × 0.12 × 0.29 mm Wavelength: Mo K+ radiation (0.71073 Å) .: 0.83 cm−1 Diffractometer, scan mode: Rigaku Mercury CCD, % 2,max: 49.98° N(hkl)measured, N(hkl)unique: 10726, 2400 Criterion for Iobs, N(hkl)gt: Iobs > 2 )(Iobs), 1855 N(param)refined: 167 Programs: SHELXS-97, SHELXL-97 [2] Table 1. Data collection and handling. H(21) 4a 0.0874 0.2358 0.4875 0.143 H(22) 4a −0.0547 0.1594 0.5220 0.103 H(3A) 4a −0.2067 0.4279 0.3987 0.083 H(3B) 4a −0.1668 0.5368 0.4228 0.083 H(1) 4a 1.2898 0.9416 0.3944 0.109 H(2) 4a 1.0499 0.8750 0.4831 0.090 H(3) 4a 0.7872 0.7713 0.4362 0.070 H(5) 4a 1.0113 0.7940 0.2122 0.072 H(6) 4a 1.2670 0.9016 0.2604 0.100 H(8) 4a 0.6503 0.7383 0.1674 0.062 H(10A) 4a 0.3380 0.5083 0.1459 0.115 H(10B) 4a 0.3381 0.6207 0.1056 0.115 H(10C) 4a 0.1813 0.5946 0.1741 0.115 H(11A) 4a 0.4367 0.4550 0.3622 0.059 H(11B) 4a 0.2956 0.4540 0.2859 0.059 H(12A) 4a 0.0834 0.5789 0.3432 0.068 H(12B) 4a 0.2299 0.5901 0.4174 0.068 Table 2. Atomic coordinates and displacement parameters (in Å). Atom Site x y z Uiso