Crystal and molecular structure analysis of 4-o-(4-methoxybenzoyl)-2-methyl-N-(2-pyridal)-2H-1,2-benzothiazine-3-carboxamide-1,1-dioxide from laboratory X-ray powder data (original) (raw)
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2012
Crystal structures of methyl 2-pentyl-4-hydroxy-2 H -1,2-benzothiazine-3-carboxylate-1,1-dioxide 1 and methyl 2-pentenyl-4-hydroxy-2 H -1,2-benzothiazine-3-carboxylate-1,1-dioxide 2 have been determined after their synthesis from saccharin. 1 and 2 crystallize in a monoclinic and orthorhombic crystal system, respectively. The asymmetric unit of both contains one molecule of each compound and shows intramolecular O-H×××O interactions generating six membered ring motifs S 1 1 (6). Intermolecular hydrogen bonding interactions have been observed in the molecule with the pentyl side chain. The thiazine ring in both molecules adopts a half chair conformation with a r.m.s. deviation of 0.2049 A and 0.2161 A.
Molecular and Crystal Structures of Two 1,2,4-BENZOTHIADIAZINE Derivatives
Журнал структурной химии, 2015
The synthesis of two 1,2,4-benzothiadiazine derivatives, namely, 6-bromo-4H-spiro[1,2,4-benzothiadiazine-3,1c-cyclobutane] 1,1-dioxide (1) and 6-bromo-1c-ethyl-4H-spiro[1,2,4-benzothiadiazine-3,4c-piperidine] 1,1-dioxide (2) is described in the present work. The synthesized compounds were studied by IR, 1 H and 13 C NMR, and single crystal X-ray diffraction to determine their molecular and crystal structure. In both structures the conformation of the 1,2,4thiadiazinane ring is a twisted chair and is stabilized by the intramolecular interaction of the C-H…O type. Compound 1 crystallizes in the monoclinic crystal system and space group C2/c with the unit cell parameters a = 15.8690(17) Å, b = 12.1453(16) Å, c = 12.0152(15) Å, E = 99.686(7)q, Z = 8 and V = 2282.7(5) Å 3. Compound 2 crystallizes in the monoclinic crystal system and space group P 2 1 /c with the unit cell parameters a = 14.5748(6) Å, b = 9.3340(5) Å, c = 12.4283(6) Å, E = 112.757(2)q, Z = 4 and V = 1559.14(13) Å 3. In the crystal structures different packing motifs are implemented with the formation of supramolecular assemblies of different types due to classical hydrogen bonds such as N-H…O and intermolecular interactions of N-H…Br, N-H…N, C-H…O types and S…S stacking.
Journal of Chemical Crystallography, 2010
Abstract The crystal structures of four derivatives of pyrazolo[4,3-c][1,2]benzothiazine-2,4-dihydro-3,4-dimethyl-,5,5-dioxide containing benzothiazine dioxide and pyrazolo fused rings that have been synthesized were determined. (C11 H11 N3 O2 S): Mr = 249.29, monoclinic, P21/c, a = 8.3070(3), b = 13.6331(5), c = 10.1661(3) Å, β = 106.924(2)°, V = 1101.45(7) Å3, Z = 4. (C12 H13 N3 O2 S): Mr = 263.31, monoclinic, P21/n, a = 9.729(3), b = 11.224(4), c = 11.436(3) Å, β = 98.85(2)°, V = 1233.9(7) Å3, Z = 4. (C14 H15 N3 O4 S): Mr = 321.35, monoclinic, P21/c, a = 9.2534(3), b = 19.3920(7), c = 7.9489(2) Å, β = 95.323(2)°, V = 1420.21(8) Å3, Z = 4. (C14 H15 N3 O3 S): Mr = 305.35, monoclinic, P21 /c, a = 13.816(7), b = 7.464(3), c = 14.674(8) Å, β = 109.05(3)°, V = 1430.3(12) Å3, Z = 4. The heterocyclic thiazine rings adopt half-chair conformations, and the mean-planes of the phenyl and pyrazolo rings lie between 10.43(11) and 15.93(16)° with respect to each other. In each case, the geometry about thiazine N-atom is trigonal pyramidal and only the first compound containing a donor N-atom shows classical hydrogen bonds. However, non-classical H-bonding of the type C–H···O is observed in all structures. Graphical Abstract The synthesis, crystal structures and molecular packing of four pyrazolo[4,3-c][1,2]benzothiazine-2,4-dihydro-3,4-dimethyl-5,5-dioxide derivatives have been presented.
European Journal of Chemistry, 2020
A combined theoretical and experimental investigation on a pharmaceutically important binary complex 3,3'-[(3-benzimidazolyl)methylene]bis(4-hydroxy-2H-1-benzopyran-2-one): 5-methyl-1,3-thiazol-2(3H)-imine is presented in this manuscript. The compound crystallizes in the monoclinic crystal system with space group Cc with unit cell parameters: a = 19.8151(8) Å, b = 15.2804(6) Å, c = 8.3950(4) Å, β = 94.0990(10)°, V = 2535.36(19) Å3, Z = 4, T = 296(2) K, μ(MoKα) = 0.184 mm-1, Dcalc = 1.490 g/cm3, 35833 reflections measured (5.332° ≤ 2Θ ≤ 56.678°), 6168 unique (Rint = 0.0467, Rsigma = 0.0388) which were used in all calculations. The final R1 was 0.0435 (I > 2σ(I)) and wR2 was 0.1073 (all data). The crystal structure has been determined by the conventional X-ray diffraction method, solved by direct methods and refined by the full matrix least squares procedure. Intramolecular hydrogen bonding of the type C–H⋅⋅⋅O and O–H⋅⋅⋅O is present and the crystal structure stabilizes via N–H…...