#------------------------------------------------------------------------------ #$Date: 2011-09-10 06:16:28 +0300 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2100236.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2100236 loop_ _publ_author_name 'Ryabova, Svetlana Yu.' 'Rastorgueva, Nina A.' 'Sonneveld, Eduard J.' 'Peschar, Rene' 'Schenk, Henk' 'Tafeenko, Viktor A.' 'Aslanov, Leonid A.' 'Chernyshev, Vladimir V.' _publ_section_title ; Structural characterization of [1,4]diazepino[6,5-b]indoles by powder diffraction ; _journal_issue 2 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 192 _journal_page_last 199 _journal_volume 61 _journal_year 2005 _chemical_formula_sum 'C17 H13 N3 O2' _chemical_formula_weight 291.30 _chemical_melting_point 555.6(5) _chemical_name_systematic ; 2-Oxo-1-phenyl-1,2,3,6-tetrahydro[1,4]diazepino[6,5-b]indole- 4-oxide ; _space_group_IT_number 19 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 23.97(2) _cell_length_b 10.609(8) _cell_length_c 5.457(3) _cell_measurement_temperature 295(2) _cell_volume 1387.7(17) _computing_cell_refinement 'LSPAID (Visser et al., 1986)' _computing_data_collection 'Johannson LS18 linescanner data collection program' _computing_data_reduction 'local program' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material ' MRIA, SHELXL93 (Sheldrick, 1997), PARST (Nardelli, 1995)' _computing_structure_refinement MRIA _computing_structure_solution 'MRIA (Chernyshev & Zlokazov, 1992)' _diffrn_ambient_temperature 295(2) _diffrn_measurement_device_type 'Enraf-Nonius Guinier Johannson camera FR 552' _diffrn_radiation_monochromator quartz _diffrn_radiation_type CuK\a~1~ _diffrn_radiation_wavelength 1.54059 _exptl_absorpt_coefficient_mu 0.768 _exptl_absorpt_correction_type none _exptl_crystal_density_diffrn 1.395 _exptl_crystal_F_000 608 _refine_diff_density_max 0.38 _refine_diff_density_min -0.35 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 2.946 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type fullcycle _refine_ls_number_constraints 21 _refine_ls_number_parameters 120 _refine_ls_number_restraints 95 _refine_ls_shift/su_max .032 _refine_ls_shift/su_mean .010 _refine_ls_structure_factor_coef Inet _refine_ls_weighting_scheme sigma _[local]_cod_data_source_file ws5016.cif _[local]_cod_data_source_block 1B _cod_depositor_comments ; The following automatic conversions were performed: '_chemical_melting_point' value '282-283 C' was changed to '555.6(5)' - it was converted from degrees Celsius(C) to Kelvins(K), the average value was taken and precision was estimated. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_original_cell_volume 1387.0(17) _cod_database_code 2100236 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_occupancy _atom_site_type_symbol C11 0.8705(4) 0.7791(8) 0.8016(16) 0.053(2) Uiso d 1 C C9 0.8031(3) 0.8642(9) 1.0901(13) 0.053(2) Uiso d 1 C C7 0.8374(4) 1.0002(7) 0.7592(16) 0.053(2) Uiso d 1 C C10 0.8358(4) 0.7651(8) 1.0135(17) 0.053(2) Uiso d 1 C C8 0.8034(3) 0.9817(8) 0.9645(18) 0.053(2) Uiso d 1 C C13 0.8713(3) 0.8972(8) 0.6837(15) 0.053(2) Uiso d 1 C C12 0.9096(4) 0.6984(7) 0.6746(16) 0.053(2) Uiso d 1 C C14 0.9300(3) 0.7683(8) 0.4714(15) 0.053(2) Uiso d 1 C N6 0.9067(3) 0.8895(6) 0.4825(13) 0.053(2) Uiso d 1 N N1 0.9227(3) 0.5715(6) 0.7259(14) 0.053(2) Uiso d 1 N C5 0.9694(4) 0.7336(7) 0.2886(17) 0.053(2) Uiso d 1 C N4 1.0126(3) 0.6574(6) 0.3393(12) 0.053(2) Uiso d 1 N C2 0.9748(4) 0.5142(7) 0.6674(15) 0.053(2) Uiso d 1 C C3 1.0197(4) 0.6060(9) 0.5915(15) 0.053(2) Uiso d 1 C O15 1.0475(2) 0.6164(4) 0.1744(9) 0.053(2) Uiso d 1 O O16 0.9802(2) 0.3977(5) 0.6573(9) 0.053(2) Uiso d 1 O C17 0.8804(4) 0.4883(7) 0.8345(18) 0.053(2) Uiso d 1 C C18 0.8927(4) 0.4171(9) 1.0478(16) 0.053(2) Uiso d 1 C C19 0.8528(4) 0.3386(8) 1.1426(16) 0.053(2) Uiso d 1 C C20 0.7974(4) 0.3382(9) 1.0478(17) 0.053(2) Uiso d 1 C C21 0.7857(4) 0.4095(9) 0.8375(16) 0.053(2) Uiso d 1 C C22 0.8266(4) 0.4854(8) 0.7333(18) 0.053(2) Uiso d 1 C H9 0.7803 0.8538 1.2264 0.050 Uiso d 1 H H7 0.8378 1.0769 0.6761 0.050 Uiso d 1 H H10 0.8353 0.6896 1.1000 0.050 Uiso d 1 H H8 0.7807 1.0466 1.0189 0.050 Uiso d 1 H H6 0.9132 0.9495 0.3803 0.050 Uiso d 1 H H5 0.9651 0.7648 0.1307 0.050 Uiso d 1 H H31 1.0556 0.5640 0.6015 0.050 Uiso d 1 H H32 1.0201 0.6756 0.7067 0.050 Uiso d 1 H H18 0.9274 0.4236 1.1224 0.050 Uiso d 1 H H19 0.8620 0.2847 1.2708 0.050 Uiso d 1 H H20 0.7695 0.2915 1.1239 0.050 Uiso d 1 H H21 0.7503 0.4059 0.7673 0.050 Uiso d 1 H H22 0.8183 0.5342 0.5965 0.050 Uiso d 1 H loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C13 C11 C10 118.0(9) C13 C11 C12 107.4(8) C10 C11 C12 134.6(9) C10 C9 C8 121.2(9) C10 C9 H9 119 C8 C9 H9 119 C8 C7 C13 116.9(9) C8 C7 H7 122 C13 C7 H7 121 C9 C10 C11 119.9(9) C9 C10 H10 120 C11 C10 H10 120 C7 C8 C9 120.9(9) C7 C8 H8 120 C9 C8 H8 120 N6 C13 C11 108.4(8) N6 C13 C7 128.5(9) C11 C13 C7 123.0(9) N1 C12 C14 125.0(8) N1 C12 C11 128.0(8) C14 C12 C11 106.9(8) N6 C14 C5 121.7(9) N6 C14 C12 108.0(8) C5 C14 C12 130.2(9) C13 N6 C14 109.2(7) C13 N6 H6 125 C14 N6 H6 125 C12 N1 C2 123.9(8) C12 N1 C17 119.9(8) C2 N1 C17 116.2(7) N4 C5 C14 121.5(9) N4 C5 H5 119 C14 C5 H5 119 O15 N4 C5 123.9(8) O15 N4 C3 116.1(7) C5 N4 C3 119.8(8) O16 C2 N1 121.8(9) O16 C2 C3 123.4(9) N1 C2 C3 114.5(8) N4 C3 C2 114.0(8) N4 C3 H31 109 C2 C3 H31 109 N4 C3 H32 109 C2 C3 H32 109 H31 C3 H32 108 C22 C17 C18 120.2(9) C22 C17 N1 119.3(8) C18 C17 N1 120.4(8) C19 C18 C17 119.1(9) C19 C18 H18 120 C17 C18 H18 120 C18 C19 C20 121.0(9) C18 C19 H19 119 C20 C19 H19 120 C21 C20 C19 119.0(9) C21 C20 H20 121 C19 C20 H20 121 C20 C21 C22 120.0(9) C20 C21 H21 120 C22 C21 H21 120 C17 C22 C21 120.3(9) C17 C22 H22 120 C21 C22 H22 120 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C11 C13 1.411(14) C11 C10 1.428(14) C11 C12 1.446(14) C9 C10 1.376(14) C9 C8 1.423(14) C9 H9 0.93 C7 C8 1.403(14) C7 C13 1.419(14) C7 H7 0.93 C10 H10 0.93 C8 H8 0.93 C13 N6 1.398(12) C12 N1 1.411(12) C12 C14 1.422(14) C14 N6 1.403(13) C14 C5 1.419(14) N6 H6 0.86 N1 C2 1.426(12) N1 C17 1.464(12) C5 N4 1.343(12) C5 H5 0.93 N4 O15 1.303(10) N4 C3 1.492(12) C2 O16 1.242(12) C2 C3 1.514(14) C3 H31 0.97 C3 H32 0.97 C17 C22 1.394(14) C17 C18 1.418(14) C18 C19 1.377(14) C18 H18 0.93 C19 C20 1.423(14) C19 H19 0.93 C20 C21 1.399(14) C20 H20 0.93 C21 C22 1.401(14) C21 H21 0.93 C22 H22 0.93