#------------------------------------------------------------------------------ #$Date: 2008-01-13 22:15:36 +0000 (Sun, 13 Jan 2008) $ #$Revision: 14 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003720.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_2003720 _journal_name_full 'Acta Crystallographica' _journal_year 1995 _journal_volume C51 _journal_page_first 1379 _journal_page_last 1381 _publ_section_title ; 11-(4-Methylpiperazin-1-yl)-5H-pyrido[3,4-b][1,5]benzodiazepine ; _chemical_formula_sum 'C17 H19 N5' _chemical_formula_weight 293.37 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' '-x, -y, -z' 'x-1/2, -y, -z-1/2' '-x-1/2, y-1/2, -z' '-x, -y-1/2, z-1/2' _symmetry_space_group_name_H-M 'P c a b' _cell_length_a 9.8098(5) _cell_length_b 16.5788(10) _cell_length_c 19.1759(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3118.7(3) _cell_formula_units_Z 8 _exptl_crystal_density_diffrn 1.250 _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54180 _cell_measurement_reflns_used 48 _cell_measurement_theta_min 31.5 _cell_measurement_theta_max 38.61 _exptl_absorpt_coefficient_mu 0.617 _cell_measurement_temperature 293(2) _exptl_crystal_description prismatic _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.19 _exptl_crystal_colour colourless _chemical_compound_source 'Laboratory of Medicinal Chemistry, Li\`ege' _diffrn_measurement_device 'Stoe Siemens AED 4-circle diffractometer' _diffrn_measurement_method '\w' _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min 0.75 _exptl_absorpt_correction_T_max 0.85 _diffrn_reflns_number 2134 _reflns_number_total 2134 _reflns_number_observed 1636 _reflns_observed_criterion >2sigma(I) _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_theta_max 57.58 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '60 min' _diffrn_standards_decay_% 2.7 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0370 _refine_ls_wR_factor_obs 0.1027 _refine_ls_wR_factor_all 0.1154 _refine_ls_goodness_of_fit_obs 1.224 _refine_ls_goodness_of_fit_all 1.095 _refine_ls_number_reflns 2131 _refine_ls_number_parameters 203 _refine_ls_hydrogen_treatment ;H atoms treated using a riding model ; _refine_ls_weighting_scheme 'calc w = 1/[\s^2^(Fo^2^)+(0.0661P)^2^+0.1626P] _refine_ls_shift/esd_max 0.000 _refine_diff_density_max 0.148 _refine_diff_density_min -0.162 _refine_ls_extinction_method 'SHELXL93 (Sheldrick, 1993)' _refine_ls_extinction_coef 0.0072(4) 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' 0.0181 0.009 'H' 'H' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0000 0.000 'N' 'N' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0311 0.018 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 N1 1 -0.2308(2) 0.94798(10) 0.61831(8) 0.0515(5) C2 1 -0.3149(2) 0.88699(12) 0.60314(10) 0.0523(5) H2 1 -0.3995(2) 0.88602(12) 0.62504(10) 0.0572(15) C3 1 -0.2852(2) 0.82595(12) 0.55769(9) 0.0471(5) H3 1 -0.3496(2) 0.78623(12) 0.54828(9) 0.0572(15) C4 1 -0.1576(2) 0.82361(10) 0.52549(9) 0.0393(4) N5 1 -0.12575(15) 0.76411(8) 0.47642(7) 0.0459(4) H5 1 -0.1925 0.7228 0.4722 0.034 C6 1 -0.0789(2) 0.79057(10) 0.40982(9) 0.0412(4) C7 1 -0.1474(2) 0.76692(13) 0.35018(10) 0.0577(6) H7 1 -0.2235(2) 0.73383(13) 0.35422(10) 0.0572(15) C8 1 -0.1055(2) 0.79119(13) 0.28503(10) 0.0617(6) H8 1 -0.1520(2) 0.77398(13) 0.24547(10) 0.0572(15) C9 1 0.0059(2) 0.84118(12) 0.27891(10) 0.0531(5) H9 1 0.0339(2) 0.85886(12) 0.23518(10) 0.0572(15) C10 1 0.0754(2) 0.86488(10) 0.33757(8) 0.0415(4) H10 1 0.1505(2) 0.89866(10) 0.33292(8) 0.0572(15) C11 1 0.0362(2) 0.83957(10) 0.40392(8) 0.0373(4) N12 1 0.12394(13) 0.85947(8) 0.45971(7) 0.0391(4) C13 1 0.0811(2) 0.88215(10) 0.52015(8) 0.0360(4) C14 1 -0.0635(2) 0.88327(10) 0.54433(9) 0.0371(4) C15 1 -0.1080(2) 0.94425(11) 0.58869(9) 0.0429(5) H15 1 -0.0471(2) 0.98575(11) 0.59848(9) 0.0572(15) N16 1 0.17548(14) 0.91386(9) 0.56580(7) 0.0416(4) C17 1 0.1763(2) 0.89719(12) 0.64087(9) 0.0471(5) H171 1 0.2310(2) 0.84966(12) 0.65021(9) 0.0572(15) H172 1 0.0841(2) 0.88673(12) 0.65676(9) 0.0572(15) C18 1 0.2341(2) 0.96830(13) 0.67948(10) 0.0512(5) H181 1 0.1766(2) 1.01511(13) 0.67206(10) 0.0572(15) H182 1 0.2358(2) 0.95681(13) 0.72907(10) 0.0572(15) N19 1 0.37189(14) 0.98554(9) 0.65519(8) 0.0471(4) C20 1 0.3679(2) 1.00373(12) 0.58129(10) 0.0500(5) H201 1 0.4593(2) 1.01604(12) 0.56508(10) 0.0572(15) H202 1 0.3114(2) 1.05090(12) 0.57357(10) 0.0572(15) C21 1 0.3116(2) 0.93342(12) 0.54006(9) 0.0479(5) H211 1 0.3070(2) 0.94740(12) 0.49100(9) 0.0572(15) H212 1 0.3710(2) 0.88701(12) 0.54511(9) 0.0572(15) C22 1 0.4337(2) 1.0518(2) 0.69402(11) 0.0732(7) H221 1 0.4340(14) 1.0391(4) 0.74286(14) 0.097(5) H222 1 0.3821(9) 1.1002(2) 0.6864(6) 0.097(5) H223 1 0.5257(6) 1.0597(6) 0.6783(5) 0.097(5) 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 N1 0.0385(9) 0.0039(8) 0.0078(7) 0.0608(10) -0.0054(8) 0.0552(10) C2 0.0351(10) -0.0005(10) 0.0094(9) 0.0703(13) 0.0026(10) 0.0515(12) C3 0.0341(11) -0.0096(9) 0.0029(8) 0.0560(11) 0.0034(9) 0.0512(11) C4 0.0379(10) -0.0004(8) -0.0002(8) 0.0406(9) 0.0058(8) 0.0393(10) N5 0.0483(9) -0.0093(7) 0.0067(7) 0.0404(8) -0.0009(7) 0.0489(9) C6 0.0376(10) -0.0015(8) 0.0015(8) 0.0425(9) -0.0015(7) 0.0436(11) C7 0.0521(12) -0.0196(10) -0.0013(10) 0.0656(13) -0.0098(10) 0.0553(12) C8 0.0606(13) -0.0164(12) -0.0069(10) 0.0801(15) -0.0104(10) 0.0445(12) C9 0.0537(12) -0.0012(10) -0.0006(9) 0.0663(13) -0.0006(9) 0.0393(10) C10 0.0378(10) 0.0002(8) 0.0027(8) 0.0456(10) -0.0002(8) 0.0412(10) C11 0.0319(10) 0.0022(8) -0.0009(7) 0.0392(9) -0.0008(7) 0.0408(10) N12 0.0304(8) -0.0003(6) 0.0000(7) 0.0472(8) 0.0006(7) 0.0397(8) C13 0.0314(9) 0.0017(8) -0.0002(7) 0.0395(9) 0.0031(7) 0.0370(10) C14 0.0316(9) 0.0021(8) -0.0010(8) 0.0426(9) 0.0050(7) 0.0373(9) C15 0.0364(10) 0.0013(8) -0.0004(8) 0.0457(10) -0.0024(8) 0.0467(11) N16 0.0300(8) -0.0074(7) -0.0008(6) 0.0605(9) 0.0010(7) 0.0342(8) C17 0.0384(10) 0.0000(9) -0.0024(8) 0.0654(12) 0.0075(9) 0.0373(10) C18 0.0410(11) 0.0025(10) -0.0036(8) 0.0739(13) -0.0027(10) 0.0388(10) N19 0.0381(9) -0.0017(7) -0.0076(7) 0.0617(10) -0.0050(7) 0.0416(9) C20 0.0389(11) -0.0058(9) -0.0017(9) 0.0625(12) 0.0020(9) 0.0486(12) C21 0.0339(10) -0.0082(9) 0.0011(8) 0.0687(12) -0.0032(9) 0.0412(10) C22 0.0632(14) -0.0099(13) -0.0122(12) 0.090(2) -0.0218(12) 0.0666(15)