Tek Kristal X-Işınları Kırınımı Yöntemiyle C15h13cln4o, C21h19no3 ve C21h20n2o3 Moleküllerinin Kristal Yapı Analizleri

Abstract

TEK KRİSTAL X-ISINLARI KIRINIMI YÖNTEMİYLE CısfltaCDM), C21H19NO3 VE C2ıH2oN203 MOLEKÜLLERİNİN KRİSTAL YAPI ANALİZLERİ ÖZET Bu çalışmada, (C15H13CIN4O) 3-Fenil-4-(m-klorobenzilamino)-4,5-dihidro-l//-l,2,4- triazol-5-on, (C21H19NO3) l-Fenil-l-metil-3-(2-N-ftalimido-l-oksoetil)siklobutan ve (C21H20N2O3) 2-[2-Hdroksiimino-2-(3-metil-3-fenilsiklobutil)-etil]-izoindol-l,3-dion maddelerinin kristal ve moleküler yapılan X-ışınlan kırınımı yöntemiyle tayin edilmiştir. Kristallerin şiddet verileri Stoe IPDS II difraktometresi ile toplanmış ve kristallerin yapı faktörlerine Lorentz ve polarizasyon düzeltmeleri yapılmıştır. Yapı çözümleri aşamasında kristaller SHELXS-86 (Sheldrick, 1990) paket programı ile direkt yöntemler kullanılarak çözülmüş, yapı arıtımı aşamasında ise çözülen yapıların atomik parametreleri SHELXL-97 (Sheldrick, 1997) paket programı ile tam-matris en küçük kareler ve fark-Fourier yöntemleri kullanılarak antılmıştır. CısHuCÎNA Triklinik, PÎ, a=7.1819(10) Â, b=7.4204(9) A, c=14.3295(19) Â,ıu SINGLE CRYSTAL X-RAY STRUCTURE ANALYSIS OF THE C15H13CIN4O, C21H19NO3 AND C2iH2oN203 MOLECULES ABSTRACT In this study, the crystal and molecular structures of (C15H13CIN4O) 3-Phenyl-4-(m- cMorobenzylamino)-4,5-dihydro-lif-l,2,4-triazol-5-one, (C21H19NO3) 1 -Phenyl-1 -methyl-3-(2- N-phmalimido-l-oxoethyl)cyclobutane and (C21H2ÜN2O3) 2-[2-Hydroxyimino-2-(3-methyl-3- phenylcyclobutyl)-ethyl]-isoindole-l,3-dione crystals have been determined by X-ray diffraction technique. The data of the crystals have been obtained in the Stoe BPDS n diffractometer and corrections of Lorentz and polarization have been applied. The structures were solved by SHELXS-86 (Sheldrick, 1990) using direct methods and the atomic parameters were refined by SHELXL-97 (Sheldrick, 1997) using full-matrix least-squares and difference-Fourier methods. Ci5Hi3ClN40, Triclimc, PT, a=7.1819(10) A, b=7.4204(9) A. c=14.3295(19) A, 0=88.224(10)°, 0=80.974(11)°, 7=72.945(10)°, V=720.94(16) A3, Z=2, Dx=1.385 gr/cm3, A(MoKa>=0.71073 A, u=0.27 mm'1, T=293(2)° K, R=0.039, wR=0.126, S=1.07, F(000)=312. C21H19NO3, Orthorhombic, P2mb, a=9.1755(9) A, b=9.4488(7) A, c=19.7807(18) A, a=90°, P=90°, y=90°, V=1714.9(3) A3, Z=4, Dx=1.291 gr/cm3, X(MoKa)=0.71073 A, u-0.09 mm'1, T=293(2)° K, R=0.035, wR=0.075, S=0.84, F(000)=704. CaHatoOa, Monoclinic, P2i/c, a=14.6497(14) A, b=5.6976(3) A, c=21. 965(2) A, a=90°, p=109.095(7)°, y=90°, V=1732.5(3) A3, Z=4, Dx=1.336 gr/cm3, X(MoKa)=0.71073 A, u=0.09 mm'1, T=293(2)° K, R=0.052, wR=0.1351, S=0.855, F(000)= 736. The C15H13CIN4O molecule has four planar fragments. The dihedral angles between the ttiazole ring plane and the benzene ring (C1-C6) and the phenyl ring (C10-C15) planes are 2.95(14) and 16.43(12)°, respectively. There are two independent N-H...0 hydrogen bonds in the structure involving two active hydrogen atoms. Each of the two H-bonds is responsible for the formation of typical H-bonded centrosymmetric motive. The 01 atom acts as a single acceptor for both H-bonds. Such arrangement results in the formation of infinite chains running along the b-axis of the crystal.IV In the C21H19NO3 molecule, the plane of the cyclobutane ring forms a dihedral angle of 64.93(15)° with the plane of the phthalimido group. The molecule has C-H...O interactions (intermolecular). The C...0 intermolecular contact distances are 3.322(3) and 3.436(3) Â, respectively. In the C21H20N2O3 molecule, there are bom C-H...O, C-H...N, O-H...O type interactions and %?% interaction between the molecules. Key Words: X-ray diffraction, 1,2,4-Triazol, Phthalimido, Cyclobutane, Oxime.