#------------------------------------------------------------------------------ #$Date: 2008-01-26 13:05:32 +0000 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003780.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_2003780 _journal_name_full 'Acta Crystallographica' _journal_year 1995 _journal_volume C51 _journal_page_first 1621 _journal_page_last 1627 _publ_section_title ; 4-Substituted 1-Methyl-1H-2,3-benzodiazepine Compounds ; _chemical_formula_moiety 'C17 H24 N2' _chemical_formula_sum 'C17 H24 N2' _chemical_formula_weight 256.38 _symmetry_cell_setting Monoclinic 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' _symmetry_space_group_name_H-M 'P 21/c' _cell_length_a 12.852(6) _cell_length_b 10.605(5) _cell_length_c 12.331(6) _cell_angle_alpha 90.00 _cell_angle_beta 111.07(3) _cell_angle_gamma 90.00 _cell_volume 1568.3(13) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.086 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _cell_measurement_reflns_used 10 _cell_measurement_theta_min 11 _cell_measurement_theta_max 12 _exptl_absorpt_coefficient_mu 0.064 _cell_measurement_temperature 298(2) _exptl_crystal_description Lath _exptl_crystal_size_max 0.82 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.04 _exptl_crystal_colour 'Lemon yellow' _diffrn_measurement_device 'Stoe Stadi-4 four-circle diffractometer' _diffrn_measurement_method ; \w-2\q scans with on-line profile fitting (Clegg, 1981) ; _exptl_absorpt_correction_type None _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_reflns_number 2030 _reflns_number_total 2027 _reflns_number_observed 1245 _reflns_observed_criterion >2sigma(I) _diffrn_reflns_av_R_equivalents 0.0465 _diffrn_reflns_theta_max 22.50 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% <1 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0486 _refine_ls_wR_factor_obs 0.1251 _refine_ls_wR_factor_all 0.1433 _refine_ls_goodness_of_fit_obs 1.208 _refine_ls_goodness_of_fit_all 1.054 _refine_ls_number_reflns 2026 _refine_ls_number_parameters 173 _refine_ls_weighting_scheme ;calc w = 1/[s^2^(Fo^2^) + (0.0651P)^2^ + 0.1325P] where P = (Fo^2^ + 2Fc^2^)/3 ; _refine_ls_shift/esd_max 0.000 _refine_diff_density_max 0.159 _refine_diff_density_min -0.143 _refine_ls_extinction_method 'SHELXL93 (Sheldrick, 1993)' _refine_ls_extinction_coef 0.009(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 0.6403(2) 0.4540(3) -0.1505(2) 0.0647(8) H1 1 0.6968(2) 0.4722(3) -0.0741(2) 0.078 C1m 1 0.6333(3) 0.5652(4) -0.2308(3) 0.1008(12) H1M1 1 0.7055(3) 0.5810(4) -0.2344(3) 0.151 H1M2 1 0.6085(3) 0.6386(4) -0.2013(3) 0.151 H1M3 1 0.5813(3) 0.5462(4) -0.3072(3) 0.151 N2 1 0.6762(2) 0.3410(3) -0.2002(2) 0.0736(8) N3 1 0.7260(2) 0.2544(2) -0.1317(2) 0.0681(7) C4 1 0.7381(2) 0.2494(2) -0.0130(2) 0.0520(7) C5 1 0.6501(2) 0.2710(2) 0.0202(2) 0.0538(7) H5 1 0.6592(2) 0.2476(2) 0.0957(2) 0.065 C5a 1 0.5436(2) 0.3264(3) -0.0479(2) 0.0544(7) C6 1 0.4470(2) 0.2937(3) -0.0265(3) 0.0676(9) H6 1 0.4520(2) 0.2365(3) 0.0323(3) 0.081 C7 1 0.3450(3) 0.3447(3) -0.0911(3) 0.0790(10) H7 1 0.2815(3) 0.3215(3) -0.0765(3) 0.095 C8 1 0.3377(3) 0.4303(4) -0.1773(3) 0.0854(11) H8 1 0.2689(3) 0.4647(4) -0.2214(3) 0.102 C9 1 0.4306(3) 0.4650(3) -0.1986(3) 0.0737(9) H9 1 0.4241(3) 0.5228(3) -0.2574(3) 0.088 C9a 1 0.5345(2) 0.4162(3) -0.1348(2) 0.0562(7) C41 1 0.8432(2) 0.1857(2) 0.0648(2) 0.0549(7) H41 1 0.8317(2) 0.1688(2) 0.1378(2) 0.066 C42 1 0.8581(2) 0.0553(3) 0.0169(3) 0.0691(9) H42A 1 0.8578(2) 0.0656(3) -0.0614(3) 0.083 H42B 1 0.9302(2) 0.0214(3) 0.0644(3) 0.083 C43 1 0.7690(3) -0.0377(3) 0.0144(3) 0.0852(10) H43A 1 0.7827(3) -0.1167(3) -0.0161(3) 0.128 H43B 1 0.6974(3) -0.0059(3) -0.0340(3) 0.128 H43C 1 0.7698(3) -0.0501(3) 0.0919(3) 0.128 C44 1 0.9484(2) 0.2714(3) 0.0979(3) 0.0616(8) C45 1 1.0477(2) 0.2066(3) 0.1914(3) 0.0828(10) H45A 1 1.0643(2) 0.1287(3) 0.1613(3) 0.124 H45B 1 1.0292(2) 0.1899(3) 0.2588(3) 0.124 H45C 1 1.1117(2) 0.2609(3) 0.2124(3) 0.124 C46 1 0.9816(3) 0.3016(3) -0.0069(3) 0.0873(10) H46A 1 0.9958(3) 0.2244(3) -0.0400(3) 0.131 H46B 1 1.0477(3) 0.3526(3) 0.0178(3) 0.131 H46C 1 0.9221(3) 0.3465(3) -0.0641(3) 0.131 C47 1 0.9259(3) 0.3944(3) 0.1503(3) 0.0875(11) H47A 1 0.9051(3) 0.3758(3) 0.2160(3) 0.131 H47B 1 0.8665(3) 0.4393(3) 0.0930(3) 0.131 H47C 1 0.9921(3) 0.4454(3) 0.1749(3) 0.131 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 0.077(2) 0.003(2) 0.025(2) 0.070(2) 0.006(2) 0.049(2) C1m 0.122(3) 0.022(2) 0.052(2) 0.101(3) 0.043(2) 0.091(3) N2 0.088(2) 0.016(2) 0.0290(14) 0.089(2) 0.0046(15) 0.0479(15) N3 0.080(2) 0.0123(14) 0.0290(13) 0.078(2) -0.0005(14) 0.051(2) C4 0.061(2) 0.0036(14) 0.0201(13) 0.055(2) -0.0017(13) 0.042(2) C5 0.066(2) 0.0028(14) 0.0210(14) 0.051(2) 0.0006(13) 0.046(2) C5a 0.056(2) 0.0008(14) 0.0189(14) 0.055(2) -0.0097(15) 0.052(2) C6 0.068(2) -0.008(2) 0.027(2) 0.064(2) -0.015(2) 0.072(2) C7 0.053(2) -0.005(2) 0.021(2) 0.080(2) -0.028(2) 0.098(3) C8 0.064(2) 0.011(2) 0.004(2) 0.083(3) -0.024(2) 0.090(3) C9 0.072(2) 0.008(2) 0.009(2) 0.078(2) -0.008(2) 0.059(2) C9a 0.062(2) 0.0067(14) 0.0105(14) 0.056(2) -0.0059(14) 0.044(2) C41 0.066(2) 0.0093(14) 0.0272(14) 0.054(2) 0.0044(14) 0.050(2) C42 0.079(2) 0.008(2) 0.033(2) 0.053(2) -0.001(2) 0.079(2) C43 0.101(2) -0.011(2) 0.036(2) 0.061(2) 0.001(2) 0.095(3) C44 0.064(2) 0.0070(14) 0.0235(15) 0.054(2) 0.0020(15) 0.067(2) C45 0.071(2) 0.005(2) 0.019(2) 0.083(2) 0.003(2) 0.087(2) C46 0.091(2) -0.009(2) 0.043(2) 0.091(2) 0.015(2) 0.088(2) C47 0.089(2) 0.005(2) 0.020(2) 0.065(2) -0.018(2) 0.098(3)