#------------------------------------------------------------------------------ #$Date: 2008-01-26 17:25:03 +0000 (Sat, 26 Jan 2008) $ #$Revision: 20 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003565.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_2003565 _journal_name_full 'Acta Crystallographica' _journal_year 1995 _journal_volume C51 _journal_page_first 1234 _journal_page_last 1240 _publ_section_title ; Five Salts of Berberine ; _chemical_formula_moiety 'C20 H18 N O4 1+, Br 1-, 2H2 O' _chemical_formula_sum 'C20 H22 Br N O6' _chemical_formula_weight 452.30 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z' 'x+1/2, y+1/2, z+1/2' 'x+1, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y, -z' '-x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z+1/2' _symmetry_space_group_name_H-M 'I 2/a' _cell_length_a 21.974(3) _cell_length_b 7.200(7) _cell_length_c 26.151(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.180(10) _cell_angle_gamma 90.00 _cell_volume 3883.4(38) _cell_formula_units_Z 8 _exptl_crystal_density_diffrn 1.547 _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 15 _exptl_absorpt_coefficient_mu 2.154 _cell_measurement_temperature 293(2) _exptl_crystal_description 'Plates' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_colour 'Orange' _diffrn_measurement_device 'Enraf Nonius CAD4' _diffrn_measurement_method '2\q/\w scans' _exptl_absorpt_correction_type 'None' _diffrn_reflns_number 3485 _reflns_number_total 3400 _reflns_number_observed 1454 _reflns_observed_criterion >2sigma(I) _diffrn_reflns_av_R_equivalents 0.0540 _diffrn_reflns_theta_max 24.97 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 31 _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0471 _refine_ls_wR_factor_obs 0.0839 _refine_ls_wR_factor_all 0.0971 _refine_ls_goodness_of_fit_obs 1.189 _refine_ls_goodness_of_fit_all 0.831 _refine_ls_number_reflns 3398 _refine_ls_number_parameters 267 _refine_ls_weighting_scheme ;calc w = 1/[\s^2^(F~o~^2^)+(0.0394P)^2^+0.0000P] where P = (F~o~^2^+2F~c~^2^)/3 ; _refine_ls_shift/esd_max -0.183 _refine_diff_density_max 0.340 _refine_diff_density_min -0.310 _refine_ls_extinction_method none 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 0.001 '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' 0.0061 0.003 'O' 'O' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0106 0.006 'Br' 'Br' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' -0.2901 2. 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 Br1 1 0.46789(3) 0.04315(9) 0.15465(2) 0.0550(2) N1 1 0.34419(15) 0.0578(6) 0.25951(15) 0.0329(9) O1 1 0.2990(2) 0.1342(6) 0.47653(15) 0.0673(12) O2 1 0.4105(2) 0.1272(6) 0.51686(14) 0.0680(12) O3 1 0.27591(14) -0.0250(5) 0.09475(13) 0.0531(10) O4 1 0.1487(2) -0.1000(5) 0.04144(13) 0.0583(11) O5 1 0.5670(2) 0.2033(6) 0.2741(2) 0.0682(13) H51 1 0.5320(26) 0.2101(84) 0.2445(23) 0.082 H52 1 0.5504(26) 0.3115(78) 0.2952(21) 0.082 O6 1 0.3699(2) 0.4000(7) 0.1663(2) 0.0785(15) H61 1 0.3916(29) 0.5211(86) 0.1773(24) 0.094 H62 1 0.3896(31) 0.3033(91) 0.1607(25) 0.094 C1 1 0.3505(3) 0.1613(9) 0.5260(2) 0.067(2) H11 1 0.3463(3) 0.0768(9) 0.5535(2) 0.080 H12 1 0.3498(3) 0.2875(9) 0.5388(2) 0.080 C2 1 0.3929(2) 0.1064(7) 0.4616(2) 0.0406(14) C3 1 0.3273(2) 0.1134(7) 0.4375(2) 0.0405(14) C4 1 0.4330(2) 0.0865(7) 0.4317(2) 0.0423(14) H41 1 0.4779(2) 0.0856(7) 0.4483(2) 0.051 C5 1 0.4036(2) 0.0678(7) 0.3754(2) 0.0328(11) C6 1 0.2968(2) 0.0953(6) 0.3829(2) 0.0406(14) H611 1 0.2519(2) 0.0982(6) 0.3673(2) 0.049 C7 1 0.3365(2) 0.0720(7) 0.3510(2) 0.0341(12) C8 1 0.3057(2) 0.0432(7) 0.2920(2) 0.0311(11) C9 1 0.4121(2) 0.1229(7) 0.2853(2) 0.0431(14) H91 1 0.4124(2) 0.2568(7) 0.2894(2) 0.052 H92 1 0.4365(2) 0.0929(7) 0.2618(2) 0.052 C10 1 0.4439(2) 0.0347(8) 0.3399(2) 0.0394(12) H101 1 0.4868(2) 0.0871(8) 0.3571(2) 0.047 H102 1 0.4486(2) -0.0977(8) 0.3355(2) 0.047 C11 1 0.3225(2) 0.0231(7) 0.2067(2) 0.0351(12) H111 1 0.3510(2) 0.0283(7) 0.1875(2) 0.042 C12 1 0.2575(2) -0.0212(6) 0.1793(2) 0.0308(11) C13 1 0.2421(2) -0.0031(6) 0.2662(2) 0.0330(13) H131 1 0.2155(2) -0.0161(6) 0.2870(2) 0.040 C14 1 0.2153(2) -0.0317(7) 0.2100(2) 0.0311(11) C15 1 0.1500(2) -0.0728(7) 0.1818(2) 0.0407(13) H151 1 0.1216(2) -0.0853(7) 0.2010(2) 0.049 C16 1 0.1277(2) -0.0948(6) 0.1269(2) 0.0405(13) H161 1 0.0839(2) -0.1188(6) 0.1091(2) 0.049 C17 1 0.1690(2) -0.0823(7) 0.0961(2) 0.0427(14) C18 1 0.2340(2) -0.0496(7) 0.1221(2) 0.0371(11) C19 1 0.0805(2) -0.1067(8) 0.0108(2) 0.064(2) H191 1 0.0742(2) -0.1196(8) -0.0272(2) 0.095(12) H192 1 0.0604(2) 0.0059(8) 0.0165(2) 0.095(12) H193 1 0.0615(2) -0.2109(8) 0.0226(2) 0.095(12) C20 1 0.2958(3) -0.1895(10) 0.0755(3) 0.087(2) H201 1 0.3252(3) -0.1588(10) 0.0568(3) 0.144(17) H202 1 0.2586(3) -0.2518(10) 0.0509(3) 0.144(17) H203 1 0.3172(3) -0.2696(10) 0.1057(3) 0.144(17) 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 Br1 0.0457(3) -0.0022(4) 0.0244(2) 0.0645(4) -0.0008(4) 0.0597(4) N1 0.029(2) -0.006(2) 0.022(2) 0.034(2) -0.004(2) 0.043(2) O1 0.061(2) 0.004(2) 0.028(2) 0.107(3) -0.002(2) 0.042(2) O2 0.062(3) 0.007(2) 0.019(2) 0.100(4) -0.003(2) 0.042(2) O3 0.046(2) -0.006(2) 0.028(2) 0.074(3) 0.003(2) 0.048(2) O4 0.040(2) -0.003(2) 0.007(2) 0.090(3) -0.001(2) 0.040(2) O5 0.065(3) 0.001(3) 0.024(2) 0.074(3) -0.008(3) 0.067(3) O6 0.061(3) 0.001(2) 0.026(3) 0.070(4) -0.001(3) 0.102(4) C1 0.072(4) 0.007(4) 0.032(4) 0.089(5) -0.003(4) 0.048(4) C2 0.051(3) 0.003(3) 0.010(3) 0.040(4) 0.003(3) 0.029(3) C3 0.048(3) 0.000(3) 0.024(3) 0.042(4) 0.002(3) 0.038(3) C4 0.034(3) -0.004(3) 0.010(2) 0.045(4) -0.002(3) 0.045(3) C5 0.042(3) -0.003(3) 0.019(2) 0.029(3) -0.004(3) 0.031(3) C6 0.038(3) 0.002(2) 0.019(3) 0.045(4) -0.002(3) 0.042(3) C7 0.030(2) 0.000(3) 0.016(2) 0.032(3) 0.006(3) 0.043(3) C8 0.033(3) 0.002(3) 0.018(2) 0.021(3) 0.002(3) 0.043(3) C9 0.033(3) -0.010(3) 0.019(2) 0.057(4) -0.008(3) 0.044(3) C10 0.027(2) 0.006(3) 0.010(2) 0.048(3) -0.002(3) 0.042(3) C11 0.034(3) 0.001(2) 0.015(2) 0.036(4) -0.005(3) 0.037(3) C12 0.031(3) 0.001(2) 0.015(2) 0.024(3) -0.002(2) 0.039(3) C13 0.032(3) 0.004(2) 0.022(2) 0.028(4) 0.002(2) 0.046(3) C14 0.027(2) 0.001(2) 0.015(2) 0.026(3) 0.002(3) 0.043(3) C15 0.026(3) -0.005(3) 0.018(2) 0.045(4) 0.006(3) 0.055(4) C16 0.027(3) -0.003(2) 0.007(2) 0.042(4) 0.002(3) 0.048(3) C17 0.040(3) -0.002(3) 0.010(3) 0.046(4) 0.008(3) 0.039(3) C18 0.036(3) 0.001(3) 0.021(2) 0.036(3) 0.000(3) 0.045(3) C19 0.049(4) -0.012(3) 0.004(3) 0.068(5) 0.001(3) 0.062(4) C20 0.083(5) -0.006(5) 0.059(4) 0.110(6) -0.032(5) 0.092(5)