#------------------------------------------------------------------------------ #$Date: 2010-01-30 13:59:17 +0000 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003782.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_2003782 _journal_name_full 'Acta Crystallographica Section C' _journal_year 1995 _journal_volume 51 _journal_page_first 1621 _journal_page_last 1627 _publ_section_title ; 4-Substituted 1-Methyl-1H-2,3-benzodiazepine Compounds ; _chemical_formula_moiety 'C16 H22 N2 O' _chemical_formula_sum 'C16 H22 N2 O' _chemical_formula_weight 258.36 _symmetry_cell_setting Triclinic loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _symmetry_space_group_name_H-M 'P -1' _cell_length_a 7.7357(9) _cell_length_b 9.4583(10) _cell_length_c 11.0128(13) _cell_angle_alpha 102.929(8) _cell_angle_beta 101.797(6) _cell_angle_gamma 100.792(5) _cell_volume 745.48(15) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.151 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _cell_measurement_reflns_used 20 _cell_measurement_theta_min 15 _cell_measurement_theta_max 16 _exptl_absorpt_coefficient_mu 0.072 _cell_measurement_temperature 298(2) _exptl_crystal_description Tabular _exptl_crystal_size_max 1.23 _exptl_crystal_size_mid 1.04 _exptl_crystal_size_min 0.46 _exptl_crystal_colour Colourless _diffrn_measurement_device 'Stoe Stadi-4 four-circle diffractometer' _diffrn_measurement_method ; \w-2\q scans with \w width (0.99 + 0.35tan\q)^o^ ; _exptl_absorpt_correction_type None _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_reflns_number 2054 _reflns_number_total 1950 _reflns_number_observed 1777 _reflns_observed_criterion >2sigma(I) _diffrn_reflns_av_R_equivalents 0.0036 _diffrn_reflns_theta_max 22.52 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 11 _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0336 _refine_ls_wR_factor_obs 0.0925 _refine_ls_wR_factor_all 0.0991 _refine_ls_goodness_of_fit_obs 1.132 _refine_ls_goodness_of_fit_all 1.096 _refine_ls_number_reflns 1942 _refine_ls_number_parameters 173 _refine_ls_weighting_scheme ;calc w = 1/[s^2^(Fo^2^) + (0.0466P)^2^ + 0.1211P] where P = (Fo^2^ + 2Fc^2^)/3 ; _refine_ls_shift/esd_max 0.000 _refine_diff_density_max 0.125 _refine_diff_density_min -0.105 _refine_ls_extinction_method 'SHELXL93 (Sheldrick, 1993)' _refine_ls_extinction_coef 0.120(9) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag 'C' 'C' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0033 0.0016 'H' 'H' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0000 0.0000 'N' 'N' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0061 0.0033 'O' 'O' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0106 0.0060 loop_ _atom_site_label _atom_site_occupancy _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv C1 1 0.2840(2) 0.5722(2) 0.43458(13) 0.0511(4) H1 1 0.4060(2) 0.6170(2) 0.42895(13) 0.061 C1m 1 0.2833(2) 0.6031(2) 0.57589(14) 0.0650(5) H1MA 1 0.3198(2) 0.7090(2) 0.61536(14) 0.098 H1MB 1 0.3666(2) 0.5555(2) 0.61882(14) 0.098 H1MC 1 0.1629(2) 0.5643(2) 0.58281(14) 0.098 N2 1 0.1523(2) 0.64690(14) 0.37097(12) 0.0559(4) N3 1 0.1771(2) 0.68256(14) 0.27155(11) 0.0543(4) C4 1 0.3074(2) 0.6394(2) 0.20650(12) 0.0480(4) C41 1 0.3852(2) 0.7549(2) 0.14410(12) 0.0505(4) H41 1 0.3016(2) 0.8203(2) 0.13571(12) 0.061 O41 1 0.39882(14) 0.68759(12) 0.01798(9) 0.0601(3) C42 1 0.2287(3) 0.6396(2) -0.0758(2) 0.0785(6) H42A 1 0.2463(3) 0.5955(2) -0.1584(2) 0.118 H42B 1 0.1777(3) 0.7239(2) -0.0803(2) 0.118 H42C 1 0.1472(3) 0.5670(2) -0.0522(2) 0.118 C43 1 0.5749(2) 0.8544(2) 0.22186(13) 0.0526(4) C44 1 0.7176(2) 0.7631(2) 0.2267(2) 0.0671(5) H44A 1 0.6849(2) 0.6853(2) 0.2668(2) 0.101 H44B 1 0.8342(2) 0.8272(2) 0.2757(2) 0.101 H44C 1 0.7237(2) 0.7194(2) 0.1406(2) 0.101 C45 1 0.5666(3) 0.9269(2) 0.35905(14) 0.0691(5) H45A 1 0.4765(3) 0.9843(2) 0.35543(14) 0.104 H45B 1 0.6834(3) 0.9915(2) 0.40696(14) 0.104 H45C 1 0.5348(3) 0.8505(2) 0.40066(14) 0.104 C46 1 0.6249(2) 0.9788(2) 0.1583(2) 0.0648(5) H46A 1 0.5342(2) 1.0356(2) 0.1558(2) 0.097 H46B 1 0.6308(2) 0.9357(2) 0.0721(2) 0.097 H46C 1 0.7413(2) 1.0435(2) 0.2071(2) 0.097 C5 1 0.3254(2) 0.4978(2) 0.17842(13) 0.0519(4) H5 1 0.3897(2) 0.4731(2) 0.11733(13) 0.062 C5a 1 0.2562(2) 0.3798(2) 0.23245(14) 0.0519(4) C6 1 0.2187(2) 0.2300(2) 0.1614(2) 0.0670(5) H6 1 0.2383(2) 0.2074(2) 0.0795(2) 0.080 C7 1 0.1536(2) 0.1162(2) 0.2109(2) 0.0772(5) H7 1 0.1286(2) 0.0173(2) 0.1625(2) 0.093 C8 1 0.1252(2) 0.1489(2) 0.3332(2) 0.0747(5) H8 1 0.0811(2) 0.0715(2) 0.3665(2) 0.090 C9 1 0.1614(2) 0.2943(2) 0.4054(2) 0.0630(4) H9 1 0.1401(2) 0.3147(2) 0.4869(2) 0.076 C9a 1 0.2301(2) 0.4119(2) 0.35787(13) 0.0504(4) loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 C1 0.0454(8) 0.0171(7) 0.0184(6) 0.0691(10) 0.0183(7) 0.0448(8) C1m 0.0651(10) 0.0195(9) 0.0211(7) 0.0875(12) 0.0193(8) 0.0464(9) N2 0.0566(8) 0.0251(6) 0.0247(6) 0.0712(8) 0.0185(6) 0.0499(7) N3 0.0552(7) 0.0255(6) 0.0220(6) 0.0676(8) 0.0185(6) 0.0496(7) C4 0.0479(8) 0.0215(7) 0.0153(6) 0.0628(9) 0.0137(6) 0.0384(7) C41 0.0596(9) 0.0262(7) 0.0184(7) 0.0630(9) 0.0152(7) 0.0372(7) O41 0.0703(7) 0.0212(6) 0.0184(5) 0.0776(7) 0.0140(5) 0.0353(5) C42 0.0920(13) 0.0176(10) 0.0033(9) 0.0911(13) 0.0173(8) 0.0434(9) C43 0.0605(9) 0.0186(7) 0.0162(7) 0.0598(9) 0.0169(7) 0.0421(8) C44 0.0604(10) 0.0218(8) 0.0154(8) 0.0764(11) 0.0273(9) 0.0698(11) C45 0.0872(12) 0.0127(9) 0.0164(8) 0.0707(11) 0.0113(8) 0.0443(9) C46 0.0751(11) 0.0196(8) 0.0218(8) 0.0685(10) 0.0250(8) 0.0578(10) C5 0.0521(8) 0.0215(7) 0.0200(6) 0.0661(10) 0.0141(7) 0.0435(8) C5a 0.0465(8) 0.0205(7) 0.0150(7) 0.0607(9) 0.0152(7) 0.0525(8) C6 0.0709(11) 0.0263(8) 0.0222(8) 0.0648(11) 0.0118(8) 0.0681(10) C7 0.0731(12) 0.0212(9) 0.0192(10) 0.0592(10) 0.0166(10) 0.0978(15) C8 0.0639(11) 0.0132(9) 0.0184(10) 0.0715(12) 0.0365(11) 0.0935(14) C9 0.0513(9) 0.0155(8) 0.0167(8) 0.0784(12) 0.0309(9) 0.0655(10) C9a 0.0393(8) 0.0176(7) 0.0141(6) 0.0654(9) 0.0210(7) 0.0519(9) _cod_database_code 2003782