Tek Kristal X-ışınları Kırınım Yöntemiyle C16h12n2o2, C17h12n2o3 ve C18h15no2 Kristallerinin Yapı Analizleri

Abstract

IV ÖZET Bu çalışmada, Schiff bazı olan (C16H12N2O2) l-[(3-Hidroksipiridin-2- ilamino)-metilen]-lH-naftalen-2-on, (C17H12N2O3) l-[(4-Nitro-fenilamino)- metilen]-lH-naftalen-2-on maddeleri ile (C18H15NO2) l-[(2-Hidroksi-5-metil- fenilamino)-metilen]-lH-naftalen-2-on maddesinin kristal ve moleküler yapılan x- ışınlan kırınım yöntemiyle tayin edilmiştir. Her üç kristalin şiddet verileri STOE IPDS II difraktometresiyle toplanmış ve kristallerin yapı faktörlerine Lorentz ve kutuplanma düzeltmeleri yapılmıştır. Doğrudan yöntemler kullanılarak çözülen yapıların atomik parametreleri tam-matris en küçük kareler ve Fark-Fourier yöntemleri kullanılarak antılmıştır. C16H12N2O2, Monoklinik, P2,, a=8.8268(14)Â, b=5.9191(6)Â, c=12.1670(19)Â,VI ABSTRACT In this study, the crystal and molecular structures of (C16H12N2O2) l-[(3- Hydroxy-pyridin-2-ylamino)-methylene]-lH-naphthalen-2-one, (C17H12N2O3) 1- [(4-Nitrophenylamino)methylene]-lH-napthalen-2-one (known as Schiff bases) and (C18H15NO2) l-[(2-Hydroxy-5-methyl-phenylamino)-methylene]-lH-naphthalen-2- one crystals have been determined by x-ray diffraction technique. The data of cystals have been obtained in the STOE IPDS II diffractometer and corrections of Lorentz and Polarization have been applied. The structures were solved by direct methods and the atomic parameters were refined by full-matrix least-squares and difference-Fourier methods. Cı6Hi2N202, Monoclinic, P2ı, a=8.8268(14)Â, b=5.9191(6)Â, c=12.1670(19)Â, a=90°, (3=90.277(13)°, y=90°, V=65.68(16)Â3, Z=2, Dx=1.381 g/cm3, X(Mo BCa)=0.71073 Â, n=0.093mm'1, T=293(2)°K, F000 =276, R=0.034, Rw=0.071, S=0.98, crystal size: 0.56x0.25x0. 1 1 mm., plate and orange. C16H12N2O2 molecule is almost planar with a 2.24(8)° dihedral angle between the two aromatic rings. The N-H...O hydrogen bonded ring is almost planar and coupled with the naphtaldimine ring. In the molecule, intramolecular N-H...O and intermolecular O-H...O hydrogen bonds were observed. The molecules are linked by intermolecular O-H...O hydrogen bonds and C-H...7I interactions, forming a three-dimensional network. C17Hi2N203, Monoclinic, P21/c, a=8.0124(13)Â, b=7.3743(8)Â, c=22.690(4)Â, a=90°, p=93.043(13)°, y=90°, V=1338.8(4)Â3, Z=4, Dx=1.450gcm'3, X(Mo Ka)=0.71073 Â, u=0. 101mm'1, T=293(2)°K, F000 =608, R=0.053, Rw=0.145, S=0.82, crystal size: 0.60x0.30x0.06mm., plate and red. C17H12N2O3 molecule is almost planar, with a dihedral angle of 4.63(1)° between ring naphtalen and phenyle ring. The N-H...0 hydrogen bonded ring is almost planar and coupled with the naphtaldimine ring. In the molecule, intramolecular N-H...0 hydrogen bonds were observed. C18Hi5N02, Triclinic, P-l, a=7.1260(10)Â, b=7.8975(9)Â, c=13.6846(17)Â, a=77.698(9)°, p=85. 429(10)°, y=65.210(9)°, V=683.07(15)Â3, Z=2, Dx=1.348gcm'3, X(Mo Ka)=0.71073 Â, u^O.OSSmnV1, T=293(2)°K, F000 =292, R=0.047, Rw=0.121, S=0.88, crystal size: 0.3 1x0.2 1x0.08mm., plate and orange.vıı Intramolecular N-H...O and intermolecular O-H...O hydrogen bonds were observed in the molecule C18H15NO2. The molecule is not exactly planar, with a dihedral angle of 12.37(9)° between the two aromatic rings. The N-H...O hydrogen bonded ring is almost planar and coupled with the naphtaldimine ring. The molecules are linked by intermolecular O-H...O hydrogen bonds into a three- dimensional network. Key words: o-hydroxy schiff bases, o- hydroxy naphthaldimine, tautomerism, thermochromism.