#------------------------------------------------------------------------------ #$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $ #$Revision: 176432 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/46/2014685.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2014685 loop_ _publ_author_name 'Li, Xin-Hua' 'Xiao, Hong-Ping' 'Zhang, Qiao' 'Hu, Mao-Lin' _publ_section_title ;catena-Poly[[bis[aqua(1,10-phenanthroline)lead(II)]-di-\m~3~-5-carboxy-3-sulfonatobenzoato] dihydrate] ; _journal_issue 3 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first m130 _journal_page_last m132 _journal_paper_doi 10.1107/S0108270105000132 _journal_volume 61 _journal_year 2005 _chemical_formula_iupac '[Pb (C8 H4 O7 S1) (C12 H8 N2) (H2 O1)] , H2 O1' _chemical_formula_moiety 'C20 H14 N2 O8 Pb S , H2 O' _chemical_formula_sum 'C20 H16 N2 O9 Pb S' _chemical_formula_weight 667.60 _chemical_name_systematic ; catena-poly[[bis[aqua(1,10-phenanthroline-\k^2^N,N')lead(II)]- di-\m^3^-5-carboxy-3-sulfonatobenzoato- 1:2:1'\k^4^O^3^:O^1^,O^1'^:O^1^;2':1:2\k^4^O^1^:O^1^,O^1'^:O^3^] dihydrate] ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL97 _cell_angle_alpha 98.2510(10) _cell_angle_beta 92.2790(10) _cell_angle_gamma 94.1960(10) _cell_formula_units_Z 2 _cell_length_a 7.2209(6) _cell_length_b 9.6252(7) _cell_length_c 15.0478(12) _cell_measurement_reflns_used 3639 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 25.10 _cell_measurement_theta_min 1.37 _cell_volume 1030.92(14) _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_collection 'SMART (Bruker, 2002)' _computing_data_reduction SAINT _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material 'SHELXTL (Bruker, 2002)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 298(2) _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measurement_device_type 'Bruker APEX area-detector' _diffrn_measurement_method '\f and \w' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0219 _diffrn_reflns_av_sigmaI/netI 0.0353 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 7489 _diffrn_reflns_theta_full 25.10 _diffrn_reflns_theta_max 25.10 _diffrn_reflns_theta_min 2.14 _diffrn_standards_decay_% 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 8.343 _exptl_absorpt_correction_T_max 0.43 _exptl_absorpt_correction_T_min 0.24 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details '(SADABS; Bruker, 2002)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 2.151 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 640 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _refine_diff_density_max 1.125 _refine_diff_density_min -0.770 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 306 _refine_ls_number_reflns 3638 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.042 _refine_ls_R_factor_all 0.0255 _refine_ls_R_factor_gt 0.0238 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0433P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0576 _refine_ls_wR_factor_ref 0.0583 _reflns_number_gt 3454 _reflns_number_total 3638 _reflns_threshold_expression I>2\s(I) _cod_data_source_file ga1091.cif _cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'not measured' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas ; _cod_original_sg_symbol_Hall -P1 _cod_original_sg_symbol_H-M P-1 _cod_database_code 2014685 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Pb1 0.91506(2) 0.564015(14) 0.871257(9) 0.02809(7) Uani d . 1 . . Pb C1 0.7127(6) 0.2721(5) 0.9492(3) 0.0400(11) Uani d . 1 . . C H1 0.7060 0.3397 0.9995 0.048 Uiso calc R 1 . . H C2 0.6687(7) 0.1312(6) 0.9569(4) 0.0483(13) Uani d . 1 . . C H2 0.6360 0.1058 1.0118 0.058 Uiso calc R 1 . . H C3 0.6736(7) 0.0319(5) 0.8844(4) 0.0495(13) Uani d . 1 . . C H3 0.6468 -0.0624 0.8896 0.059 Uiso calc R 1 . . H C4 0.7191(6) 0.0702(5) 0.8010(3) 0.0381(10) Uani d . 1 . . C C5 0.7193(7) -0.0279(5) 0.7204(4) 0.0468(13) Uani d . 1 . . C H5 0.6877 -0.1228 0.7221 0.056 Uiso calc R 1 . . H C6 0.7640(7) 0.0137(5) 0.6427(4) 0.0489(13) Uani d . 1 . . C H6 0.7610 -0.0524 0.5910 0.059 Uiso calc R 1 . . H C7 0.8161(6) 0.1575(5) 0.6377(3) 0.0406(11) Uani d . 1 . . C C8 0.8653(8) 0.2056(6) 0.5580(3) 0.0563(14) Uani d . 1 . . C H8 0.8627 0.1425 0.5049 0.068 Uiso calc R 1 . . H C9 0.9173(9) 0.3449(6) 0.5573(4) 0.0633(16) Uani d . 1 . . C H9 0.9494 0.3775 0.5043 0.076 Uiso calc R 1 . . H C10 0.9210(8) 0.4361(5) 0.6371(3) 0.0489(12) Uani d . 1 . . C H10 0.9579 0.5305 0.6364 0.059 Uiso calc R 1 . . H C11 0.8215(5) 0.2575(4) 0.7149(3) 0.0305(9) Uani d . 1 . . C C12 0.7681(5) 0.2146(4) 0.7988(3) 0.0296(9) Uani d . 1 . . C C13 1.2218(5) 0.9930(4) 0.7652(3) 0.0272(9) Uani d . 1 . . C C14 1.1949(6) 1.0665(4) 0.8493(3) 0.0274(9) Uani d . 1 . . C H14 1.1564 1.0183 0.8955 0.033 Uiso calc R 1 . . H C15 1.2258(5) 1.2125(4) 0.8645(3) 0.0284(9) Uani d . 1 . . C C16 1.2840(5) 1.2830(4) 0.7956(3) 0.0284(9) Uani d . 1 . . C H16 1.3055 1.3806 0.8058 0.034 Uiso calc R 1 . . H C17 1.3107(5) 1.2095(4) 0.7109(3) 0.0283(9) Uani d . 1 . . C C18 1.2777(5) 1.0632(4) 0.6961(3) 0.0280(9) Uani d . 1 . . C H18 1.2935 1.0131 0.6397 0.034 Uiso calc R 1 . . H C19 1.3765(6) 1.2893(4) 0.6391(3) 0.0305(9) Uani d . 1 . . C C20 1.1991(6) 1.2922(4) 0.9564(3) 0.0307(9) Uani d . 1 . . C O1 1.1977(6) 1.2270(4) 1.0222(2) 0.0558(10) Uani d . 1 . . O O2 1.1765(4) 1.4220(3) 0.9622(2) 0.0378(7) Uani d . 1 . . O O3 1.4370(5) 1.4119(3) 0.6542(2) 0.0429(8) Uani d . 1 . . O O4 1.3628(5) 1.2157(3) 0.5586(2) 0.0461(8) Uani d . 1 . . O H4 1.4066 1.2637 0.5225 0.069 Uiso calc R 1 . . H O5 1.2325(6) 0.7609(3) 0.6578(2) 0.0569(10) Uani d . 1 . . O O6 1.0023(5) 0.7662(3) 0.7677(3) 0.0519(9) Uani d . 1 . . O O7 1.3214(5) 0.7635(3) 0.8146(2) 0.0568(10) Uani d . 1 . . O O8 0.6029(4) 0.5857(4) 0.8107(2) 0.0497(9) Uani d . 1 . . O H8B 0.5872 0.5384 0.7607 0.075 Uiso calc R 1 . . H H8A 0.5716 0.6649 0.8280 0.075 Uiso d R 1 . . H O9 0.4703(7) 0.3456(4) 0.4299(3) 0.0690(13) Uani d D 1 . . O N1 0.7641(5) 0.3138(4) 0.8722(2) 0.0319(8) Uani d . 1 . . N N2 0.8751(5) 0.3968(4) 0.7143(2) 0.0354(8) Uani d . 1 . . N S1 1.19291(15) 0.80538(10) 0.74953(7) 0.0313(2) Uani d . 1 . . S H9A 0.553(7) 0.308(6) 0.406(4) 0.047 Uiso d D 1 . . H H9B 0.473(7) 0.423(4) 0.426(4) 0.047 Uiso d D 1 . . H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pb1 0.03739(11) 0.02172(10) 0.02432(10) -0.00027(7) 0.00194(6) 0.00170(7) C1 0.040(3) 0.040(3) 0.039(3) -0.010(2) -0.006(2) 0.011(2) C2 0.051(3) 0.048(3) 0.049(3) -0.011(2) -0.009(2) 0.026(3) C3 0.044(3) 0.029(3) 0.075(4) -0.010(2) -0.015(3) 0.019(3) C4 0.030(2) 0.026(2) 0.058(3) 0.0021(17) -0.009(2) 0.009(2) C5 0.040(3) 0.022(2) 0.074(4) 0.0010(19) -0.011(2) -0.003(2) C6 0.046(3) 0.032(3) 0.062(3) -0.001(2) 0.002(2) -0.014(2) C7 0.034(2) 0.035(3) 0.046(3) 0.0005(19) -0.002(2) -0.012(2) C8 0.069(4) 0.058(3) 0.033(3) -0.006(3) 0.003(2) -0.018(2) C9 0.090(4) 0.061(4) 0.034(3) -0.016(3) 0.011(3) 0.000(3) C10 0.068(3) 0.042(3) 0.034(3) -0.009(2) 0.008(2) 0.003(2) C11 0.029(2) 0.028(2) 0.034(2) 0.0045(17) -0.0038(17) 0.0002(18) C12 0.025(2) 0.027(2) 0.036(2) 0.0028(16) -0.0059(17) 0.0038(18) C13 0.027(2) 0.021(2) 0.031(2) 0.0009(16) -0.0014(16) 0.0010(17) C14 0.031(2) 0.026(2) 0.026(2) 0.0048(16) 0.0034(16) 0.0059(17) C15 0.027(2) 0.028(2) 0.031(2) 0.0066(16) 0.0011(16) 0.0022(18) C16 0.029(2) 0.024(2) 0.032(2) 0.0027(16) 0.0008(16) -0.0002(17) C17 0.025(2) 0.029(2) 0.030(2) 0.0003(16) -0.0012(16) 0.0046(18) C18 0.032(2) 0.025(2) 0.025(2) 0.0014(16) 0.0014(16) -0.0013(17) C19 0.037(2) 0.024(2) 0.030(2) 0.0024(17) 0.0009(17) 0.0015(18) C20 0.035(2) 0.028(2) 0.029(2) 0.0085(17) 0.0034(17) 0.0004(18) O1 0.100(3) 0.041(2) 0.0307(18) 0.0291(19) 0.0070(18) 0.0075(16) O2 0.0517(18) 0.0265(16) 0.0341(16) 0.0037(14) 0.0064(14) -0.0004(13) O3 0.060(2) 0.0326(18) 0.0346(17) -0.0063(15) 0.0071(15) 0.0042(14) O4 0.074(2) 0.0334(18) 0.0289(17) -0.0117(16) 0.0107(16) 0.0028(14) O5 0.101(3) 0.0278(18) 0.0383(19) -0.0037(18) 0.0193(19) -0.0060(15) O6 0.052(2) 0.0321(18) 0.075(2) -0.0030(15) 0.0127(18) 0.0201(18) O7 0.072(2) 0.039(2) 0.061(2) 0.0244(18) -0.0156(19) 0.0053(17) O8 0.0462(19) 0.043(2) 0.054(2) 0.0123(16) -0.0085(16) -0.0151(17) O9 0.111(4) 0.045(2) 0.060(3) 0.015(2) 0.039(2) 0.026(2) N1 0.0360(19) 0.0287(19) 0.0310(19) -0.0043(15) -0.0015(15) 0.0084(16) N2 0.044(2) 0.031(2) 0.0303(19) -0.0009(16) 0.0011(16) 0.0035(16) S1 0.0437(6) 0.0204(5) 0.0295(5) 0.0020(4) 0.0039(4) 0.0027(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O8 Pb1 N1 . . 78.88(12) no O8 Pb1 O1 . 2_777 76.52(12) yes N1 Pb1 O1 . 2_777 119.70(12) yes O8 Pb1 O2 . 2_777 95.36(11) yes N1 Pb1 O2 . 2_777 78.81(10) no O1 Pb1 O2 2_777 2_777 50.35(10) yes O8 Pb1 N2 . . 73.39(11) no N1 Pb1 N2 . . 63.34(11) yes O1 Pb1 N2 2_777 . 148.40(12) yes O2 Pb1 N2 2_777 . 141.79(10) no O8 Pb1 O6 . . 82.14(12) no N1 Pb1 O6 . . 145.22(12) no O1 Pb1 O6 2_777 . 83.15(11) yes O2 Pb1 O6 2_777 . 132.11(10) yes N2 Pb1 O6 . . 83.43(11) no O8 Pb1 O2 . 1_545 151.86(11) yes N1 Pb1 O2 . 1_545 73.96(10) no O1 Pb1 O2 2_777 1_545 110.87(10) no O2 Pb1 O2 2_777 1_545 72.43(10) yes N2 Pb1 O2 . 1_545 100.26(10) no O6 Pb1 O2 . 1_545 125.03(10) yes N1 C1 C2 . . 122.4(5) ? N1 C1 H1 . . 118.8 ? C2 C1 H1 . . 118.8 ? C3 C2 C1 . . 119.7(5) ? C3 C2 H2 . . 120.1 ? C1 C2 H2 . . 120.1 ? C2 C3 C4 . . 120.3(4) ? C2 C3 H3 . . 119.9 ? C4 C3 H3 . . 119.9 ? C3 C4 C12 . . 116.9(4) ? C3 C4 C5 . . 123.6(4) ? C12 C4 C5 . . 119.5(4) ? C6 C5 C4 . . 121.4(4) ? C6 C5 H5 . . 119.3 ? C4 C5 H5 . . 119.3 ? C5 C6 C7 . . 120.9(5) ? C5 C6 H6 . . 119.5 ? C7 C6 H6 . . 119.5 ? C11 C7 C8 . . 117.1(4) ? C11 C7 C6 . . 120.0(5) ? C8 C7 C6 . . 122.9(4) ? C9 C8 C7 . . 120.5(5) ? C9 C8 H8 . . 119.8 ? C7 C8 H8 . . 119.8 ? C8 C9 C10 . . 118.5(5) ? C8 C9 H9 . . 120.8 ? C10 C9 H9 . . 120.8 ? N2 C10 C9 . . 123.7(5) ? N2 C10 H10 . . 118.2 ? C9 C10 H10 . . 118.2 ? N2 C11 C7 . . 122.4(4) ? N2 C11 C12 . . 118.0(4) ? C7 C11 C12 . . 119.6(4) ? N1 C12 C4 . . 122.4(4) ? N1 C12 C11 . . 119.1(4) ? C4 C12 C11 . . 118.5(4) ? C18 C13 C14 . . 120.7(4) ? C18 C13 S1 . . 120.5(3) ? C14 C13 S1 . . 118.8(3) ? C13 C14 C15 . . 119.9(4) ? C13 C14 H14 . . 120.0 ? C15 C14 H14 . . 120.0 ? C16 C15 C14 . . 119.6(4) ? C16 C15 C20 . . 120.6(4) ? C14 C15 C20 . . 119.9(4) ? C15 C16 C17 . . 120.7(4) ? C15 C16 H16 . . 119.7 ? C17 C16 H16 . . 119.7 ? C16 C17 C18 . . 119.3(4) ? C16 C17 C19 . . 118.9(4) ? C18 C17 C19 . . 121.8(4) ? C13 C18 C17 . . 119.9(4) ? C13 C18 H18 . . 120.0 ? C17 C18 H18 . . 120.0 ? O3 C19 O4 . . 123.3(4) ? O3 C19 C17 . . 122.7(4) ? O4 C19 C17 . . 113.9(3) ? O1 C20 O2 . . 123.4(4) ? O1 C20 C15 . . 118.8(4) ? O2 C20 C15 . . 117.8(4) ? C20 O1 Pb1 . 2_777 93.3(2) yes C20 O2 Pb1 . 2_777 92.1(2) yes C19 O4 H4 . . 109.5 ? S1 O6 Pb1 . . 121.72(19) yes Pb1 O8 H8B . . 109.5 ? Pb1 O8 H8A . . 109.5 ? H8B O8 H8A . . 129.2 ? H9A O9 H9B . . 113(6) ? C1 N1 C12 . . 118.2(4) ? C1 N1 Pb1 . . 120.4(3) ? C12 N1 Pb1 . . 120.2(3) ? C10 N2 C11 . . 117.9(4) ? C10 N2 Pb1 . . 124.1(3) ? C11 N2 Pb1 . . 117.6(3) ? O5 S1 O7 . . 114.5(2) ? O5 S1 O6 . . 112.2(2) ? O7 S1 O6 . . 111.3(2) ? O5 S1 C13 . . 105.66(19) ? O7 S1 C13 . . 105.3(2) ? O6 S1 C13 . . 107.21(19) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pb1 O8 . 2.432(3) yes Pb1 N1 . 2.572(3) yes Pb1 O1 2_777 2.588(3) yes Pb1 O2 2_777 2.605(3) yes Pb1 N2 . 2.653(4) yes Pb1 O6 . 2.717(3) yes Pb1 O2 1_545 2.831(3) yes C1 N1 . 1.336(5) ? C1 C2 . 1.392(7) ? C1 H1 . 0.9300 ? C2 C3 . 1.346(8) ? C2 H2 . 0.9300 ? C3 C4 . 1.402(7) ? C3 H3 . 0.9300 ? C4 C12 . 1.414(6) ? C4 C5 . 1.426(7) ? C5 C6 . 1.333(7) ? C5 H5 . 0.9300 ? C6 C7 . 1.421(7) ? C6 H6 . 0.9300 ? C7 C11 . 1.395(6) ? C7 C8 . 1.396(7) ? C8 C9 . 1.367(8) ? C8 H8 . 0.9300 ? C9 C10 . 1.380(7) ? C9 H9 . 0.9300 ? C10 N2 . 1.319(6) ? C10 H10 . 0.9300 ? C11 N2 . 1.370(5) ? C11 C12 . 1.442(6) ? C12 N1 . 1.355(5) ? C13 C18 . 1.376(6) ? C13 C14 . 1.386(6) ? C13 S1 . 1.783(4) ? C14 C15 . 1.390(6) ? C14 H14 . 0.9300 ? C15 C16 . 1.382(6) ? C15 C20 . 1.509(6) ? C16 C17 . 1.394(6) ? C16 H16 . 0.9300 ? C17 C18 . 1.396(5) ? C17 C19 . 1.486(6) ? C18 H18 . 0.9300 ? C19 O3 . 1.214(5) ? C19 O4 . 1.309(5) ? C20 O1 . 1.246(5) ? C20 O2 . 1.263(5) ? O1 Pb1 2_777 2.588(3) yes O2 Pb1 2_777 2.605(3) yes O4 H4 . 0.8200 ? O5 S1 . 1.431(3) yes O6 S1 . 1.448(3) yes O7 S1 . 1.442(3) yes O8 H8B . 0.8200 ? O8 H8A . 0.8200 ? O9 H9A . 0.79(4) ? O9 H9B . 0.75(4) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA O4 H4 O9 1_665 0.82 1.76 2.567(5) 169 O8 H8B O3 1_445 0.82 2.08 2.851(5) 156 O8 H8A O7 1_455 0.82 2.12 2.749(5) 134 O9 H9A O5 2_766 0.79(4) 1.96(4) 2.749(6) 172(6) O9 H9B O3 2_776 0.75(4) 2.21(4) 2.862(5) 145(5) loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag N1 C1 C2 C3 . . -1.4(7) ? C1 C2 C3 C4 . . -1.3(7) ? C2 C3 C4 C12 . . 3.3(7) ? C2 C3 C4 C5 . . -177.1(4) ? C3 C4 C5 C6 . . -179.9(5) ? C12 C4 C5 C6 . . -0.3(7) ? C4 C5 C6 C7 . . 1.1(7) ? C5 C6 C7 C11 . . 0.1(7) ? C5 C6 C7 C8 . . 179.5(5) ? C11 C7 C8 C9 . . 0.5(8) ? C6 C7 C8 C9 . . -178.9(5) ? C7 C8 C9 C10 . . 0.4(9) ? C8 C9 C10 N2 . . -0.8(9) ? C8 C7 C11 N2 . . -1.0(7) ? C6 C7 C11 N2 . . 178.4(4) ? C8 C7 C11 C12 . . 178.6(4) ? C6 C7 C11 C12 . . -2.0(6) ? C3 C4 C12 N1 . . -2.9(6) ? C5 C4 C12 N1 . . 177.5(4) ? C3 C4 C12 C11 . . 178.0(4) ? C5 C4 C12 C11 . . -1.5(6) ? N2 C11 C12 N1 . . 3.2(6) ? C7 C11 C12 N1 . . -176.4(4) ? N2 C11 C12 C4 . . -177.7(4) ? C7 C11 C12 C4 . . 2.7(6) ? C18 C13 C14 C15 . . -0.4(6) ? S1 C13 C14 C15 . . 176.7(3) ? C13 C14 C15 C16 . . -0.3(6) ? C13 C14 C15 C20 . . -179.2(4) ? C14 C15 C16 C17 . . 0.4(6) ? C20 C15 C16 C17 . . 179.3(4) ? C15 C16 C17 C18 . . 0.1(6) ? C15 C16 C17 C19 . . -178.9(4) ? C14 C13 C18 C17 . . 1.0(6) ? S1 C13 C18 C17 . . -176.1(3) ? C16 C17 C18 C13 . . -0.8(6) ? C19 C17 C18 C13 . . 178.2(4) ? C16 C17 C19 O3 . . 12.4(6) ? C18 C17 C19 O3 . . -166.6(4) ? C16 C17 C19 O4 . . -167.5(4) ? C18 C17 C19 O4 . . 13.5(6) ? C16 C15 C20 O1 . . -160.3(4) ? C14 C15 C20 O1 . . 18.5(6) ? C16 C15 C20 O2 . . 20.7(6) ? C14 C15 C20 O2 . . -160.4(4) ? O2 C20 O1 Pb1 . 2_777 9.1(5) ? C15 C20 O1 Pb1 . 2_777 -169.8(3) ? O1 C20 O2 Pb1 . 2_777 -9.0(5) ? C15 C20 O2 Pb1 . 2_777 169.9(3) ? O8 Pb1 O6 S1 . . -168.1(3) no N1 Pb1 O6 S1 . . -110.8(3) no O1 Pb1 O6 S1 2_777 . 114.7(2) no O2 Pb1 O6 S1 2_777 . 101.8(2) no N2 Pb1 O6 S1 . . -94.0(2) no O2 Pb1 O6 S1 1_545 . 3.9(3) no C2 C1 N1 C12 . . 1.8(6) ? C2 C1 N1 Pb1 . . -165.7(3) ? C4 C12 N1 C1 . . 0.4(6) ? C11 C12 N1 C1 . . 179.4(4) ? C4 C12 N1 Pb1 . . 167.9(3) ? C11 C12 N1 Pb1 . . -13.0(5) ? O8 Pb1 N1 C1 . . -104.3(3) ? O1 Pb1 N1 C1 2_777 . -36.9(4) ? O2 Pb1 N1 C1 2_777 . -6.5(3) ? N2 Pb1 N1 C1 . . 178.9(4) ? O6 Pb1 N1 C1 . . -162.4(3) ? O2 Pb1 N1 C1 1_545 . 68.3(3) no O8 Pb1 N1 C12 . . 88.5(3) ? O1 Pb1 N1 C12 2_777 . 155.8(3) ? O2 Pb1 N1 C12 2_777 . -173.7(3) ? N2 Pb1 N1 C12 . . 11.6(3) ? O6 Pb1 N1 C12 . . 30.3(4) ? O2 Pb1 N1 C12 1_545 . -99.0(3) no C9 C10 N2 C11 . . 0.2(8) ? C9 C10 N2 Pb1 . . 173.2(4) ? C7 C11 N2 C10 . . 0.7(6) ? C12 C11 N2 C10 . . -178.9(4) ? C7 C11 N2 Pb1 . . -172.8(3) ? C12 C11 N2 Pb1 . . 7.6(5) ? O8 Pb1 N2 C10 . . 91.7(4) ? N1 Pb1 N2 C10 . . 177.3(4) ? O1 Pb1 N2 C10 2_777 . 73.4(5) ? O2 Pb1 N2 C10 2_777 . 168.9(4) ? O6 Pb1 N2 C10 . . 7.9(4) ? O2 Pb1 N2 C10 1_545 . -116.5(4) no O8 Pb1 N2 C11 . . -95.3(3) ? N1 Pb1 N2 C11 . . -9.6(3) ? O1 Pb1 N2 C11 2_777 . -113.6(3) ? O2 Pb1 N2 C11 2_777 . -18.1(4) ? O6 Pb1 N2 C11 . . -179.1(3) ? O2 Pb1 N2 C11 1_545 . 56.5(3) no Pb1 O6 S1 O5 . . 110.0(2) ? Pb1 O6 S1 O7 . . -19.8(3) ? Pb1 O6 S1 C13 . . -134.4(2) ? C18 C13 S1 O5 . . -1.9(4) ? C14 C13 S1 O5 . . -179.0(3) ? C18 C13 S1 O7 . . 119.7(4) ? C14 C13 S1 O7 . . -57.5(4) ? C18 C13 S1 O6 . . -121.7(3) ? C14 C13 S1 O6 . . 61.2(4) ?