Jian-Feng Zhang, Shu-Jiao Chen, Fangfei Xu
Jun 1, 2011
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Zeitschrift für Kristallographie - New Crystal Structures
Abstract
C11H12Cl2N4OZn, triclinic, P1 (no. 2), a = 7.487(2) Å, b = 8.604(2) Å, c = 11.952(2) Å, * = 69.13(3)°, ) = 80.47(3)°, & = 84.03(3)°, V = 708.6 Å, Z = 2, Rgt(F) = 0.048, wRref(F ) = 0.167, T = 296 K. Source of material A solution of the 3-[3-(pyridin-2-yl)-1H-pyrazol-1-yl]propanamide ligand (0.0432 g, 0.2 mmol) in acetonitrile (15 ml) was added dropwise to a solution of ZnCl2 (0.0272 g, 0.2 mmol) in methanol (10 ml) in a 50 ml beaker. The mixture was stirred for 30 min at 323 K, then filtered. The resulted solution was kept at room temperature. Colorless block-shaped single crystals suitable for X-ray diffraction were obtained after two weeks (yield 25 % based on Zn). Elemental analysis — found: C, 37.59 %; H, 3.21 %; Cl, 20.26 %; N, 15.97 %; Zn, 18.69 %; calculated for C11H12Cl2N4OZn: C, 37.84 %; H, 3.43 %; Cl, 20.11 %; N, 15.89 %; Zn, 18.55 %. Discussion In recent years, 3-(2-pyridyl)pyrazole-based ligands have been found for a wide range of application in coordination chemistry, because they can act as bridging or chelating ligands and exhibit a series of intriguing structures and potential applications as functional materials [1,2]. Nowadays, much attention has been focused on the synthetic approach and the structural control of coordination architectures [3,4]. The synthesis and crystallographic description of the 3-[3-(pyridin-2-yl)-1H-pyrazol-1yl]propan-amide ligand were first put forward in our laboratory [5], but its coordination complexes with metals have not been yet reported. In the title complex, the dihedral angle between pyrazole and pyridine ring is 2.8(4)°, and the torsion angle of N3–C6–C7–C8 is 176.7(6)°. The Zn(II) centre is four-coordinated by two N atoms from one 3-(3-(pyridin-2-yl)-1H-pyrazol-1-yl)propanamide ligand and two Cl atoms. The complexes are interconnected into a three-dimensional supermolecular network through intermolecular N–H···O and N–H···Cl hydrogen bonds. The crystal structure is also stabilized by slipped ,-, stacking interactions between the N2–N3–C6–C5–C4 and the N4–C11–C10–C9– C8–C7 rings with centroid-to-centroid distance of 3.626(1) Å and interplanar distance of 3.474(1) Å. Z. Kristallogr. NCS 226 (2011) 221-222 / DOI 10.1524/ncrs.2011.0102 221 © by Oldenbourg Wissenschaftsverlag, München Crystal: colorless block, size 0.06 × 0.18 × 0.38 mm Wavelength: Mo Kα radiation (0.71073 Å) -: 21.06 cm−1 Diffractometer, scan mode: Rigaku R-AXIS RAPID, % 2+max: 54.92° N(hkl)measured, N(hkl)unique: 6977, 3219 Criterion for Iobs, N(hkl)gt: Iobs > 2 ((Iobs), 1936 N(param)refined: 173 Programs: SHELXS-97, SHELXL-97 [6] Table 1. Data collection and handling. H(1A) 2i −0.0132 1.3687 0.4656 0.071 H(1B) 2i 0.0804 1.2128 0.4535 0.071 H(2A) 2i 0.4361 1.2091 0.4441 0.064 H(2B) 2i 0.3303 1.0918 0.5637 0.064 H(3A) 2i 0.6153 1.1364 0.5978 0.063 H(3B) 2i 0.5716 1.3291 0.5539 0.063 H(4A) 2i 0.4816 1.4306 0.7348 0.065 H(5A) 2i 0.3436 1.3059 0.9488 0.059 H(8A) 2i 0.1825 1.0740 1.1305 0.067 H(9A) 2i 0.0545 0.8483 1.2852 0.079 H(10A) 2i 0.0335 0.6055 1.2488 0.082 H(11A) 2i 0.1416 0.5908 1.0599 0.068 Table 2. Atomic coordinates and displacement parameters (in Å). Atom Site x y z Uiso