Guo-Biao Cao, Bing-Qin Yang
Dec 1, 2010
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Zeitschrift für Kristallographie - New Crystal Structures
Abstract
C16H17N3O6, monoclinic, P121/c1 (no. 14), a = 10.997(9) Å, b = 12.46(1) Å, c = 12.67(1) Å, * = 108.80(1)°, V = 1643.3 Å, Z = 4, Rgt(F) = 0.060, wRref(F) = 0.158, T = 298 K. Source of material 3-Hydroxy-6-nitrobenzaldehyde and 4-methoxybenzohydrazide of AR grade were purchased from Aldrich and were used as received. The compound was prepared by refluxing 3-hydroxy-6nitrobenzaldehyde (0.1 mmol, 16.7 mg) with 4-methoxybenzohydrazide (0.1 mmol, 16.6 mg) in methanol (30 ml). Colorless block-like single crystals were obtained by slow evaporation of the solution in air. Experimental details H2 and H3 were located in the difference Fourier map and refined with d(O—H) = 0.85(1) Å and d(N—H) = 0.90(1) Å. The remaining H atoms were placed in idealized positions and constrained to ride on their parent atoms, with d(C—H) = 0.93 0.96 Å, d(O—H) = 0.82 0.85 Å, and with Uiso(H) = 1.2 Ueq(C) and 1.5 Ueq(O,Cmethyl). Discussion Hydrazone compounds derived from the condensation of aldehydes with benzohydrazides have been widely investigated, either for their crystal structures [1-4] or for their biological properties [5-7]. The asymmetric unit of the title crystal structure consists of a hydrazone molecule and a methanol molecule of crystallization. The bond lengths are within normal values [8], and are comparable to the values observed in similar hydrazone compounds [1-4]. The dihedral angle between the two aromatic rings in the hydrazone molecule is 8.2(2)°, indicating that the molecule is approximately coplanar. The molecular structure is stabilized by inter-molecular O–H···O, N–H···O, and O–H···N hydrogen bonds. Z. Kristallogr. NCS 225 (2010) 715-716 / DOI 10.1524/ncrs.2010.0315 715 © by Oldenbourg Wissenschaftsverlag, München Crystal: colorless block, size 0.23 × 0.27 × 0.30 mm Wavelength: Mo K+ radiation (0.71073 Å) .: 1.09 cm−1 Diffractometer, scan mode: Bruker SMART 1000 CCD, % 2,max: 54° N(hkl)measured, N(hkl)unique: 9224, 3485 Criterion for Iobs, N(hkl)gt: Iobs > 2 )(Iobs), 1732 N(param)refined: 235 Programs: SHELXS-97, SHELXL-97 [9] Table 1. Data collection and handling. H(6) 4e 0.7552 0.3012 0.2308 0.104 H(3A) 4e 0.9153 0.6558 0.8066 0.058 H(4) 4e 1.0385 0.5801 0.7101 0.059 H(6A) 4e 0.9851 0.2911 0.8250 0.059 H(7) 4e 0.8272 0.3608 1.0097 0.054 H(10) 4e 0.7641 −0.1396 0.9743 0.060 H(11) 4e 0.6751 −0.2548 1.0710 0.064 H(13) 4e 0.5497 −0.0032 1.2014 0.060 H(14) 4e 0.6413 0.1116 1.1072 0.053 H(15A) 4e 0.5187 −0.3414 1.1332 0.132 H(15B) 4e 0.5187 −0.3425 1.2569 0.132 H(15C) 4e 0.6483 −0.3299 1.2314 0.132 H(16A) 4e 0.5527 0.3516 0.1540 0.137 H(16B) 4e 0.5935 0.3822 0.0502 0.137 H(16C) 4e 0.6527 0.4437 0.1631 0.137 H(2) 4e 0.767(3) 0.199(2) 1.047(2) 0.080 H(3) 4e 1.124(3) 0.422(2) 0.667(2) 0.080 Table 2. Atomic coordinates and displacement parameters (in Å). Atom Site x y z Uiso