#------------------------------------------------------------------------------ #$Date: 2010-01-30 13:59:17 +0000 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003779.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_2003779 _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' _chemical_formula_sum 'C16 H22 N2' _chemical_formula_weight 242.36 _symmetry_cell_setting Monoclinic _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _[local]_cod_cif_authors_sg_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.7871(9) _cell_length_b 10.3877(7) _cell_length_c 12.4807(8) _cell_angle_alpha 90.00 _cell_angle_beta 102.276(6) _cell_angle_gamma 90.00 _cell_volume 1493.2(2) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.078 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _cell_measurement_reflns_used 44 _cell_measurement_theta_min 12.5 _cell_measurement_theta_max 14.0 _exptl_absorpt_coefficient_mu 0.063 _cell_measurement_temperature 298(2) _exptl_crystal_description Plate _exptl_crystal_size_max 0.69 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.09 _exptl_crystal_colour 'Pale green' _diffrn_measurement_device 'Stoe Stadi-4 four circle diffractometer' _diffrn_measurement_method ; \w-2\q scans with \w width (0.8 + 0.35tan\q)\% ; _exptl_absorpt_correction_type None _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_reflns_number 1951 _reflns_number_total 1951 _reflns_number_observed 1265 _reflns_observed_criterion >2sigma(I) _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_theta_max 22.51 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _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 0.0435 _refine_ls_wR_factor_obs 0.1133 _refine_ls_wR_factor_all 0.1226 _refine_ls_goodness_of_fit_obs 1.219 _refine_ls_goodness_of_fit_all 1.035 _refine_ls_number_reflns 1945 _refine_ls_number_parameters 164 _refine_ls_weighting_scheme ;calc w = 1/[s^2^(Fo^2^) + (0.0640P)^2^ + 0.0239P] where P = (Fo^2^ + 2Fc^2^)/3 ; _refine_ls_shift/esd_max 0.000 _refine_diff_density_max 0.135 _refine_diff_density_min -0.110 _refine_ls_extinction_method 'SHELXL93 (Sheldrick, 1993)' _refine_ls_extinction_coef 0.017(3) 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 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 0.6171(2) 0.4349(2) 0.7211(2) 0.0628(7) H1 1 0.6738(2) 0.4599(2) 0.6777(2) 0.075 C1m 1 0.6145(3) 0.5381(3) 0.8073(2) 0.0982(9) H1MA 1 0.6912(3) 0.5499(3) 0.8511(2) 0.147 H1MB 1 0.5631(3) 0.5117(3) 0.8535(2) 0.147 H1MC 1 0.5874(3) 0.6176(3) 0.7717(2) 0.147 N2 1 0.6563(2) 0.3125(2) 0.77993(14) 0.0646(6) N3 1 0.7028(2) 0.2281(2) 0.73198(14) 0.0587(5) C4 1 0.7105(2) 0.2348(2) 0.6208(2) 0.0491(6) C41 1 0.8141(2) 0.1641(2) 0.5949(2) 0.0558(6) H41 1 0.8023(2) 0.1642(2) 0.5147(2) 0.067 C42 1 0.8097(2) 0.0221(2) 0.6280(2) 0.0829(8) H42A 1 0.8753(2) -0.0226(2) 0.6116(2) 0.124 H42B 1 0.7393(2) -0.0162(2) 0.5879(2) 0.124 H42C 1 0.8119(2) 0.0165(2) 0.7052(2) 0.124 C43 1 0.9328(2) 0.2307(2) 0.6374(2) 0.0641(7) C44 1 0.9265(2) 0.3675(3) 0.5930(3) 0.1028(10) H44A 1 0.9043(2) 0.3655(3) 0.5144(3) 0.154 H44B 1 1.0012(2) 0.4078(3) 0.6147(3) 0.154 H44C 1 0.8701(2) 0.4155(3) 0.6217(3) 0.154 C45 1 0.9681(2) 0.2336(3) 0.7621(2) 0.1037(10) H45A 1 0.9721(2) 0.1473(3) 0.7900(2) 0.156 H45B 1 0.9118(2) 0.2817(3) 0.7910(2) 0.156 H45C 1 1.0428(2) 0.2739(3) 0.7839(2) 0.156 C46 1 1.0267(2) 0.1595(3) 0.5918(3) 0.1023(10) H46A 1 1.0329(2) 0.0725(3) 0.6184(3) 0.153 H46B 1 1.0999(2) 0.2024(3) 0.6155(3) 0.153 H46C 1 1.0059(2) 0.1591(3) 0.5132(3) 0.153 C5 1 0.6189(2) 0.2687(2) 0.5418(2) 0.0541(6) H5 1 0.6263(2) 0.2556(2) 0.4699(2) 0.065 C5a 1 0.5105(2) 0.3233(2) 0.5560(2) 0.0558(6) C6 1 0.4074(2) 0.2963(3) 0.4794(2) 0.0751(7) H6 1 0.4098(2) 0.2465(3) 0.4180(2) 0.090 C7 1 0.3035(2) 0.3428(3) 0.4948(3) 0.0929(9) H7 1 0.2354(2) 0.3234(3) 0.4444(3) 0.111 C8 1 0.2994(3) 0.4178(3) 0.5840(3) 0.0988(11) H8 1 0.2281(3) 0.4484(3) 0.5939(3) 0.119 C9 1 0.3980(3) 0.4485(3) 0.6586(2) 0.0798(8) H9 1 0.3937(3) 0.4998(3) 0.7186(2) 0.096 C9a 1 0.5049(2) 0.4031(2) 0.6449(2) 0.0577(6) 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 0.087(2) 0.0002(13) 0.0291(13) 0.0512(15) -0.0026(12) 0.0567(14) C1m 0.136(3) 0.008(2) 0.040(2) 0.078(2) -0.025(2) 0.088(2) N2 0.0861(14) 0.0108(11) 0.0208(10) 0.0668(14) 0.0044(10) 0.0439(11) N3 0.0724(13) 0.0094(10) 0.0194(9) 0.0606(12) 0.0042(10) 0.0462(11) C4 0.0633(14) 0.0004(11) 0.0176(11) 0.0443(13) 0.0004(10) 0.0424(12) C41 0.0655(15) 0.0064(12) 0.0159(11) 0.0543(14) -0.0003(11) 0.0493(13) C42 0.088(2) 0.0056(13) 0.034(2) 0.055(2) -0.0059(15) 0.111(2) C43 0.062(2) 0.0014(12) 0.0154(12) 0.060(2) 0.0030(12) 0.071(2) C44 0.089(2) -0.0079(15) 0.034(2) 0.068(2) 0.018(2) 0.155(3) C45 0.092(2) -0.012(2) -0.004(2) 0.126(3) -0.008(2) 0.084(2) C46 0.076(2) 0.011(2) 0.039(2) 0.101(2) -0.007(2) 0.136(3) C5 0.0667(15) 0.0013(11) 0.0160(11) 0.0543(14) 0.0013(11) 0.0431(12) C5a 0.0626(15) 0.0028(12) 0.0147(11) 0.0544(14) 0.0135(11) 0.0515(14) C6 0.072(2) 0.0040(15) 0.0061(14) 0.076(2) 0.0142(14) 0.073(2) C7 0.061(2) 0.006(2) 0.004(2) 0.104(2) 0.033(2) 0.108(2) C8 0.082(2) 0.026(2) 0.044(2) 0.098(3) 0.039(2) 0.126(3) C9 0.085(2) 0.019(2) 0.039(2) 0.076(2) 0.018(2) 0.087(2) C9a 0.067(2) 0.0085(12) 0.0269(13) 0.0514(14) 0.0140(12) 0.060(2) _cod_database_code 2003779