#------------------------------------------------------------------------------ #$Date: 2008-01-13 22:15:36 +0000 (Sun, 13 Jan 2008) $ #$Revision: 14 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003567.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_2003567 _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 '2(C20 H18 N O4 1+), O4 S 2-, 7H2 O' _chemical_formula_sum 'C40 H50 N2 O19 S' _chemical_formula_weight 894.88 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, z' '-x, -y, -z' '-x-1/2, y-1/2, -z' _symmetry_space_group_name_H-M 'P 21/a' _cell_length_a 23.198(30) _cell_length_b 6.918(10) _cell_length_c 24.963(30) _cell_angle_alpha 90.00 _cell_angle_beta 96.65(9) _cell_angle_gamma 90.00 _cell_volume 3979.0(91) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.494 _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 0.169 _cell_measurement_temperature 293(2) _exptl_crystal_description 'Needles' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.1 _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 5360 _reflns_number_total 5193 _reflns_number_observed 1319 _reflns_observed_criterion >2sigma(I) _diffrn_reflns_av_R_equivalents 0.1112 _diffrn_reflns_theta_max 22.51 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time 180 _diffrn_standards_decay_% 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0764 _refine_ls_wR_factor_obs 0.1649 _refine_ls_wR_factor_all 0.2046 _refine_ls_goodness_of_fit_obs 1.321 _refine_ls_goodness_of_fit_all 0.732 _refine_ls_number_reflns 5193 _refine_ls_number_parameters 380 _refine_ls_weighting_scheme ;calc w = 1/[\s^2^(F~o~^2^)+(0.0844P)^2^+3.7773P] where P = (F~o~^2^+2F~c~^2^)/3 ; _refine_ls_shift/esd_max 0.003 _refine_diff_density_max 0.342 _refine_diff_density_min -0.308 _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 'S' 'S' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.1246 0.123 'O' 'O' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0106 0.006 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 S1 1 0.87341(13) 0.4785(5) 0.23974(11) 0.0371(8) N1 1 0.3051(3) 0.3843(13) 0.0715(3) 0.029(2) N2 1 0.2078(3) 0.6378(13) 0.5709(3) 0.030(2) O1 1 0.0483(3) 0.3566(12) 0.1055(3) 0.042(2) O2 1 0.0792(3) 0.4295(12) 0.1949(3) 0.050(2) O3 1 0.4349(3) 0.4082(12) -0.0296(3) 0.046(2) O4 1 0.4065(3) 0.3962(11) -0.1370(2) 0.042(2) O5 1 0.4721(3) 0.6220(12) 0.6034(3) 0.047(2) O6 1 0.4630(3) 0.6712(12) 0.6950(3) 0.051(2) O7 1 0.0514(2) 0.6003(12) 0.4685(2) 0.036(2) O8 1 0.0513(3) 0.6313(11) 0.3626(2) 0.037(2) O9 1 0.9012(4) 0.5459(16) 0.1942(3) 0.097(4) O10 1 0.8919(3) 0.2842(13) 0.2556(3) 0.070(3) O11 1 0.8099(3) 0.4814(13) 0.2263(3) 0.059(3) O12 1 0.8905(3) 0.6161(12) 0.2854(3) 0.058(3) O13 1 0.1303(3) 0.1173(15) 0.5779(3) 0.077(3) O14 1 0.0526(3) 0.0554(13) 0.7891(3) 0.063(3) O15 1 0.7533(3) 0.2426(13) 0.7220(3) 0.059(3) O16 1 0.1060(3) 0.3965(17) -0.0838(3) 0.092(4) O17 1 0.8519(3) 0.9743(13) 0.3092(3) 0.058(3) O18 1 0.5672(3) 1.0621(13) -0.3898(3) 0.052(2) O19 1 0.0363(3) 0.0530(14) -0.1028(3) 0.065(3) C1 1 0.0297(5) 0.404(2) 0.1563(4) 0.060(4) H11 1 0.0055(5) 0.3012(20) 0.1678(4) 0.071 H12 1 0.0070(5) 0.5221(20) 0.1531(4) 0.071 C2 1 0.1255(4) 0.4232(16) 0.1641(4) 0.032(3) C3 1 0.1073(4) 0.3841(16) 0.1110(4) 0.030(3) C4 1 0.1815(4) 0.4493(17) 0.1841(4) 0.040(3) H41 1 0.1925(4) 0.4725(17) 0.2205(4) 0.048 C5 1 0.2229(4) 0.4395(16) 0.1459(4) 0.028(3) C6 1 0.1449(4) 0.3694(16) 0.0745(4) 0.030(3) H61 1 0.1320(4) 0.3429(16) 0.0386(4) 0.036 C7 1 0.2047(4) 0.3948(16) 0.0915(4) 0.027(3) C8 1 0.2465(4) 0.3958(16) 0.0525(4) 0.028(3) C9 1 0.3225(4) 0.3566(17) 0.1298(3) 0.034(3) H91 1 0.3629(4) 0.3925(17) 0.1383(3) 0.041 H92 1 0.3188(4) 0.2209(17) 0.1386(3) 0.041 C10 1 0.2862(3) 0.4748(16) 0.1635(4) 0.030(3) H101 1 0.2950(3) 0.6109(16) 0.1597(4) 0.035 H102 1 0.2952(3) 0.4399(16) 0.2012(4) 0.035 C11 1 0.3465(4) 0.3902(15) 0.0378(3) 0.026(3) H111 1 0.3852(4) 0.3894(15) 0.0527(3) 0.032 C12 1 0.3346(4) 0.3973(15) -0.0178(3) 0.024(3) C13 1 0.2311(4) 0.4026(16) -0.0022(4) 0.033(3) H131 1 0.1921(4) 0.4089(16) -0.0157(4) 0.039 C14 1 0.2743(4) 0.4001(15) -0.0389(4) 0.024(3) C15 1 0.2604(4) 0.4080(17) -0.0954(4) 0.040(3) H151 1 0.2218(4) 0.4131(17) -0.1104(4) 0.048 C16 1 0.3034(4) 0.4082(16) -0.1280(4) 0.036(3) H161 1 0.2942(4) 0.4156(16) -0.1652(4) 0.044 C17 1 0.3624(4) 0.3970(18) -0.1056(4) 0.039(3) C18 1 0.3777(4) 0.3931(16) -0.0522(4) 0.028(3) C19 1 0.3925(4) 0.4228(16) -0.1952(4) 0.042(3) H191 1 0.4276(4) 0.4191(16) -0.2121(4) 0.117(15) H192 1 0.3738(4) 0.5455(16) -0.2021(4) 0.117(15) H193 1 0.3670(4) 0.3212(16) -0.2095(4) 0.117(15) C20 1 0.4632(4) 0.2323(19) -0.0129(5) 0.055(4) H201 1 0.5023(4) 0.2591(19) 0.0021(5) 0.117(15) H202 1 0.4635(4) 0.1478(19) -0.0434(5) 0.117(15) H203 1 0.4428(4) 0.1713(19) 0.0139(5) 0.117(15) C21 1 0.5035(5) 0.636(2) 0.6567(4) 0.057(4) H211 1 0.5245(5) 0.5174(20) 0.6657(4) 0.069 H212 1 0.5313(5) 0.7415(20) 0.6578(4) 0.069 C22 1 0.4092(4) 0.6735(17) 0.6649(4) 0.032(3) C23 1 0.4135(4) 0.6463(16) 0.6098(4) 0.032(3) C24 1 0.3578(4) 0.7044(17) 0.6830(4) 0.039(3) H241 1 0.3553(4) 0.7300(17) 0.7192(4) 0.047 C25 1 0.3066(4) 0.6965(15) 0.6443(3) 0.023(3) C26 1 0.3668(4) 0.6434(16) 0.5719(4) 0.039(3) H261 1 0.3706(4) 0.6272(16) 0.5355(4) 0.047 C27 1 0.3119(4) 0.6662(15) 0.5906(3) 0.023(3) C28 1 0.2601(4) 0.6612(16) 0.5525(4) 0.034(3) C29 1 0.2064(4) 0.6105(18) 0.6290(4) 0.042(3) H291 1 0.2141(4) 0.4758(18) 0.6379(4) 0.050 H292 1 0.1678(4) 0.6409(18) 0.6379(4) 0.050 C30 1 0.2492(4) 0.7325(16) 0.6621(4) 0.029(3) H301 1 0.2390(4) 0.8679(16) 0.6574(4) 0.035 H302 1 0.2498(4) 0.7000(16) 0.7000(4) 0.035 C31 1 0.1585(4) 0.6267(16) 0.5379(4) 0.033(3) H311 1 0.1240(4) 0.6073(16) 0.5527(4) 0.040 C32 1 0.1563(4) 0.6433(15) 0.4814(3) 0.024(3) C33 1 0.2588(4) 0.6696(16) 0.4974(4) 0.031(3) H331 1 0.2944(4) 0.6762(16) 0.4838(4) 0.037 C34 1 0.2090(4) 0.6691(16) 0.4597(4) 0.030(3) C35 1 0.2082(4) 0.6810(16) 0.4034(4) 0.034(3) H351 1 0.2427(4) 0.6954(16) 0.3881(4) 0.041 C36 1 0.1565(4) 0.6712(15) 0.3716(4) 0.024(3) H361 1 0.1566(4) 0.6799(15) 0.3345(4) 0.029 C37 1 0.1029(4) 0.6486(17) 0.3921(4) 0.034(3) C38 1 0.1040(4) 0.6295(16) 0.4475(4) 0.027(3) C39 1 0.0482(4) 0.6567(16) 0.3033(3) 0.039(3) H391 1 0.0089(4) 0.6405(16) 0.2874(3) 0.117(15) H392 1 0.0724(4) 0.5621(16) 0.2888(3) 0.117(15) H393 1 0.0615(4) 0.7840(16) 0.2955(3) 0.117(15) C40 1 0.0244(4) 0.7713(18) 0.4887(4) 0.052(4) H401 1 -0.0112(4) 0.7354(18) 0.5022(4) 0.117(15) H402 1 0.0164(4) 0.8632(18) 0.4600(4) 0.117(15) H403 1 0.0502(4) 0.8281(18) 0.5173(4) 0.117(15) 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 S1 0.049(2) -0.001(2) 0.0042(13) 0.032(2) -0.002(2) 0.030(2) O1 0.034(4) -0.005(5) 0.002(3) 0.059(7) -0.006(5) 0.032(4) O2 0.042(5) -0.006(5) 0.003(4) 0.076(7) -0.024(5) 0.030(4) O3 0.042(5) 0.010(5) 0.003(3) 0.057(7) 0.003(5) 0.038(4) O4 0.045(5) -0.006(5) 0.008(3) 0.056(6) -0.001(4) 0.025(4) O5 0.035(5) -0.001(5) 0.006(4) 0.055(7) -0.005(5) 0.052(5) O6 0.036(5) 0.009(5) 0.006(4) 0.064(7) 0.000(5) 0.054(5) O7 0.021(4) -0.004(4) 0.007(3) 0.051(6) -0.003(4) 0.036(4) O8 0.038(5) 0.006(4) 0.002(3) 0.043(6) -0.003(4) 0.030(4) O9 0.118(7) -0.033(8) 0.056(6) 0.122(10) 0.009(6) 0.060(6) O10 0.068(6) 0.003(5) -0.024(5) 0.032(6) 0.020(5) 0.101(7) O11 0.031(5) 0.023(5) -0.012(4) 0.056(7) -0.013(5) 0.085(6) O12 0.070(6) 0.005(5) -0.025(4) 0.048(6) -0.032(5) 0.050(5) O13 0.064(5) 0.009(6) 0.020(4) 0.116(9) -0.020(6) 0.056(5) O14 0.055(5) -0.008(5) 0.000(4) 0.080(8) 0.009(5) 0.052(5) O15 0.046(5) -0.020(5) 0.004(4) 0.078(7) -0.013(5) 0.052(5) O16 0.064(6) -0.007(7) -0.008(4) 0.151(11) -0.022(7) 0.057(6) O17 0.053(5) 0.016(5) 0.009(4) 0.075(7) 0.005(5) 0.047(5) O18 0.039(4) 0.009(5) 0.017(4) 0.065(7) -0.006(5) 0.055(5) O19 0.044(5) 0.002(5) 0.003(4) 0.084(8) 0.021(5) 0.065(5) C1 0.054(8) -0.022(9) 0.008(7) 0.071(12) 0.010(8) 0.054(8) C19 0.067(8) -0.008(7) 0.021(6) 0.039(9) 0.011(6) 0.025(6) C20 0.036(7) 0.002(8) -0.006(6) 0.052(10) 0.009(8) 0.075(9) C21 0.054(8) -0.004(8) -0.012(7) 0.053(11) 0.005(8) 0.060(8) C39 0.058(8) -0.012(7) -0.019(5) 0.032(9) 0.004(6) 0.021(6) C40 0.047(8) 0.031(8) 0.022(6) 0.062(11) -0.009(8) 0.051(8)