# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name 'Kou-Lin Zhang' 'Yan Chang' 'Seik Weng Ng' _publ_contact_author_name 'Kou-Lin Zhang' _publ_contact_author_email koulinzhang2002@yahoo.com data_pb _database_code_depnum_ccdc_archive 'CCDC 789897' #TrackingRef 'PB DMF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H13 Br3 N2 O7 Pb' _chemical_formula_weight 732.15 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' Br Br -0.2901 2.4595 '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' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P41212 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+1/4' 'y+1/2, -x+1/2, z+3/4' '-x+1/2, y+1/2, -z+1/4' 'x+1/2, -y+1/2, -z+3/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 9.227 _cell_length_b 9.227 _cell_length_c 43.990(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3745.20(25) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9954 _cell_measurement_theta_min 2.2552 _cell_measurement_theta_max 26.6010 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.597 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2688 _exptl_absorpt_coefficient_mu 15.443 _exptl_absorpt_correction_type EMPIRICAL _exptl_absorpt_correction_T_min 0.011 _exptl_absorpt_correction_T_max 0.039 _exptl_absorpt_process_details EMPIRICAL _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEXII area-detector' _diffrn_measurement_method '\f and \w' _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32334 _diffrn_reflns_av_R_equivalents 0.0632 _diffrn_reflns_av_sigmaI/netI 0.0387 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -57 _diffrn_reflns_limit_l_max 56 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4289 _reflns_number_gt 3931 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'SAINT (Bruker, 2004)' _computing_data_reduction 'SAINT (Bruker, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond (CRYSTAL IMPACT, 2001)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0401P)^2^+12.3069P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment CONSTR _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.291(11) _refine_ls_number_reflns 4289 _refine_ls_number_parameters 220 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0396 _refine_ls_R_factor_gt 0.0341 _refine_ls_wR_factor_ref 0.0826 _refine_ls_wR_factor_gt 0.0805 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 1.01374(3) 0.71538(3) 0.023978(6) 0.02432(8) Uani 1 1 d . . . Br1 Br 0.80044(9) 1.11571(12) 0.11237(2) 0.0463(2) Uani 1 1 d . . . Br2 Br 0.19001(9) 1.03465(13) 0.11057(2) 0.0542(3) Uani 1 1 d . . . Br3 Br 0.53940(10) 0.75610(9) 0.022944(19) 0.0370(2) Uani 1 1 d . . . O1 O 0.8635(6) 0.8007(8) 0.06892(13) 0.0440(17) Uani 1 1 d . . . O2 O 0.8383(6) 0.9706(7) 0.03402(13) 0.0361(14) Uani 1 1 d . . . O3 O 0.2055(6) 0.7279(6) 0.06344(12) 0.0347(13) Uani 1 1 d . . . O4 O 0.2012(7) 0.9125(7) 0.03162(14) 0.0458(16) Uani 1 1 d . . . O5 O 1.1911(9) 0.5657(9) -0.00632(17) 0.068(2) Uani 1 1 d . . . O1W O 0.9754(10) 0.4821(8) 0.05382(16) 0.063(2) Uani 1 1 d . . . H1W1 H 0.9975 0.4089 0.0435 0.095 Uiso 1 1 d R . . H1W2 H 1.0259 0.4881 0.0697 0.095 Uiso 1 1 d R . . O2W O 1.0385(10) 0.2241(9) 0.02776(19) 0.075(2) Uani 1 1 d . . . H2W1 H 0.9910 0.1530 0.0343 0.112 Uiso 1 1 d R . . H2W2 H 1.0159 0.2368 0.0094 0.112 Uiso 1 1 d R . . N1 N 0.4857(8) 1.1335(10) 0.13500(17) 0.051(2) Uani 1 1 d . . . H11 H 0.5620 1.1664 0.1438 0.061 Uiso 1 1 calc R . . H12 H 0.4016 1.1493 0.1428 0.061 Uiso 1 1 calc R . . N2 N 1.3340(10) 0.5212(10) -0.04626(19) 0.051(2) Uani 1 1 d . . . C1 C 0.7947(8) 0.9016(9) 0.05676(16) 0.0266(15) Uani 1 1 d . . . C2 C 0.6489(8) 0.9404(8) 0.07041(16) 0.0233(15) Uani 1 1 d . . . C3 C 0.6320(7) 1.0278(8) 0.09519(16) 0.0212(15) Uani 1 1 d . . . C4 C 0.4979(8) 1.0565(8) 0.10875(17) 0.0247(15) Uani 1 1 d . . . C5 C 0.3769(7) 0.9955(8) 0.09449(16) 0.0227(15) Uani 1 1 d . . . C6 C 0.3867(7) 0.9098(9) 0.06909(16) 0.0248(15) Uani 1 1 d . . . C7 C 0.5235(8) 0.8792(8) 0.05770(15) 0.0211(15) Uani 1 1 d . . . C8 C 0.2529(7) 0.8455(9) 0.05409(17) 0.0251(17) Uani 1 1 d . . . C9 C 1.2661(14) 0.6156(11) -0.0278(3) 0.062(3) Uani 1 1 d . . . H9 H 1.2745 0.7150 -0.0307 0.074 Uiso 1 1 calc R . . C10 C 1.3255(17) 0.3697(15) -0.0442(4) 0.093(5) Uani 1 1 d . . . H10A H 1.2589 0.3436 -0.0283 0.140 Uiso 1 1 calc R . . H10B H 1.4196 0.3311 -0.0396 0.140 Uiso 1 1 calc R . . H10C H 1.2922 0.3308 -0.0632 0.140 Uiso 1 1 calc R . . C11 C 1.4218(15) 0.5835(19) -0.0710(3) 0.094(5) Uani 1 1 d . . . H11A H 1.4039 0.6858 -0.0723 0.141 Uiso 1 1 calc R . . H11B H 1.3960 0.5382 -0.0899 0.141 Uiso 1 1 calc R . . H11C H 1.5226 0.5671 -0.0669 0.141 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.02237(14) 0.02818(15) 0.02240(13) -0.00490(12) -0.00127(11) 0.00116(10) Br1 0.0213(4) 0.0732(7) 0.0445(5) -0.0170(5) -0.0076(4) -0.0037(4) Br2 0.0200(4) 0.0828(8) 0.0597(6) -0.0283(6) 0.0178(4) 0.0005(4) Br3 0.0407(4) 0.0372(5) 0.0332(4) -0.0133(3) 0.0126(4) -0.0053(3) O1 0.040(3) 0.060(4) 0.032(3) 0.014(3) 0.010(3) 0.027(3) O2 0.023(3) 0.049(4) 0.036(3) 0.014(3) 0.011(2) 0.000(2) O3 0.034(3) 0.040(3) 0.031(3) 0.005(3) 0.000(3) -0.010(3) O4 0.035(3) 0.055(4) 0.048(4) 0.023(3) -0.014(3) -0.011(3) O5 0.087(6) 0.067(5) 0.048(4) -0.001(4) 0.023(4) 0.037(5) O1W 0.095(6) 0.040(4) 0.054(4) -0.002(3) -0.006(5) -0.011(4) O2W 0.105(7) 0.048(4) 0.072(5) 0.001(4) -0.025(5) -0.005(5) N1 0.027(4) 0.081(6) 0.045(5) -0.030(4) 0.001(3) 0.001(4) N2 0.051(5) 0.058(5) 0.044(5) -0.006(4) 0.003(4) 0.013(4) C1 0.019(4) 0.036(4) 0.024(4) -0.001(3) 0.003(3) 0.005(3) C2 0.026(4) 0.021(4) 0.023(4) 0.007(3) 0.002(3) 0.009(3) C3 0.017(3) 0.028(4) 0.019(3) 0.000(3) -0.002(3) -0.001(3) C4 0.021(3) 0.030(4) 0.023(4) 0.002(3) 0.002(3) 0.000(3) C5 0.017(3) 0.031(4) 0.020(3) -0.002(3) 0.003(3) 0.001(3) C6 0.014(3) 0.038(4) 0.022(4) 0.007(3) 0.000(3) -0.006(3) C7 0.019(3) 0.032(4) 0.012(3) 0.000(3) 0.004(3) -0.001(3) C8 0.019(4) 0.040(4) 0.016(4) -0.004(3) 0.003(3) -0.003(3) C9 0.087(9) 0.037(5) 0.062(7) 0.003(5) -0.009(7) 0.019(5) C10 0.099(12) 0.071(9) 0.110(12) -0.015(9) -0.014(10) 0.027(8) C11 0.066(9) 0.122(13) 0.095(11) 0.027(10) -0.022(8) 0.000(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 O3 2.482(6) 1_655 ? Pb1 O5 2.523(7) . ? Pb1 O4 2.533(6) 1_655 ? Pb1 O1 2.540(6) . ? Pb1 O1W 2.546(7) . ? Pb1 C8 2.840(7) 1_655 ? Br1 C3 1.909(7) . ? Br2 C5 1.898(7) . ? Br3 C7 1.910(7) . ? O1 C1 1.247(9) . ? O2 C1 1.252(9) . ? O3 C8 1.240(10) . ? O3 Pb1 2.482(6) 1_455 ? O4 C8 1.260(9) . ? O4 Pb1 2.533(6) 1_455 ? O5 C9 1.257(13) . ? N1 C4 1.361(10) . ? N2 C9 1.347(13) . ? N2 C10 1.403(16) . ? N2 C11 1.473(16) . ? C1 C2 1.516(10) . ? C2 C3 1.365(10) . ? C2 C7 1.404(10) . ? C3 C4 1.399(10) . ? C4 C5 1.399(10) . ? C5 C6 1.372(10) . ? C6 C7 1.388(10) . ? C6 C8 1.520(10) . ? C8 Pb1 2.840(7) 1_455 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Pb1 O5 86.1(2) 1_655 . ? O3 Pb1 O4 52.18(18) 1_655 1_655 ? O5 Pb1 O4 91.2(3) . 1_655 ? O3 Pb1 O1 80.23(19) 1_655 . ? O5 Pb1 O1 159.3(2) . . ? O4 Pb1 O1 92.7(2) 1_655 . ? O3 Pb1 O1W 77.2(2) 1_655 . ? O5 Pb1 O1W 84.2(3) . . ? O4 Pb1 O1W 129.3(2) 1_655 . ? O1 Pb1 O1W 77.6(2) . . ? O3 Pb1 C8 25.8(2) 1_655 1_655 ? O5 Pb1 C8 88.5(3) . 1_655 ? O4 Pb1 C8 26.3(2) 1_655 1_655 ? O1 Pb1 C8 86.0(2) . 1_655 ? O1W Pb1 C8 103.0(3) . 1_655 ? C1 O1 Pb1 100.1(4) . . ? C8 O3 Pb1 93.5(5) . 1_455 ? C8 O4 Pb1 90.6(5) . 1_455 ? C9 O5 Pb1 123.6(7) . . ? C9 N2 C10 125.4(11) . . ? C9 N2 C11 116.7(11) . . ? C10 N2 C11 117.9(11) . . ? O1 C1 O2 124.0(7) . . ? O1 C1 C2 117.2(7) . . ? O2 C1 C2 118.8(7) . . ? C3 C2 C7 117.5(6) . . ? C3 C2 C1 123.8(7) . . ? C7 C2 C1 118.6(6) . . ? C2 C3 C4 123.6(7) . . ? C2 C3 Br1 118.3(5) . . ? C4 C3 Br1 118.1(5) . . ? N1 C4 C3 122.3(7) . . ? N1 C4 C5 121.6(7) . . ? C3 C4 C5 116.0(7) . . ? C6 C5 C4 123.0(6) . . ? C6 C5 Br2 118.2(5) . . ? C4 C5 Br2 118.8(5) . . ? C5 C6 C7 118.1(7) . . ? C5 C6 C8 121.7(6) . . ? C7 C6 C8 120.2(7) . . ? C6 C7 C2 121.6(6) . . ? C6 C7 Br3 118.7(6) . . ? C2 C7 Br3 119.7(5) . . ? O3 C8 O4 123.8(7) . . ? O3 C8 C6 118.9(7) . . ? O4 C8 C6 117.2(7) . . ? O3 C8 Pb1 60.7(4) . 1_455 ? O4 C8 Pb1 63.1(4) . 1_455 ? C6 C8 Pb1 176.7(5) . 1_455 ? O5 C9 N2 118.2(10) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.622 _refine_diff_density_min -1.684 _refine_diff_density_rms 0.188 data_pb _database_code_depnum_ccdc_archive 'CCDC 789898' #TrackingRef 'pb CH3OH.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H10 Br3 N O7 Pb' _chemical_formula_weight 691.10 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' Br Br -0.2901 2.4595 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 9.0731(8) _cell_length_b 6.9348(6) _cell_length_c 11.9935(11) _cell_angle_alpha 90.00 _cell_angle_beta 95.7160(10) _cell_angle_gamma 90.00 _cell_volume 750.88(12) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3412 _cell_measurement_theta_min 2.69 _cell_measurement_theta_max 27.49 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.057 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 628 _exptl_absorpt_coefficient_mu 19.246 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.114 _exptl_absorpt_correction_T_max 0.260 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEXII area-detector' _diffrn_measurement_method '\f and \w' _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6507 _diffrn_reflns_av_R_equivalents 0.0357 _diffrn_reflns_av_sigmaI/netI 0.0350 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 27.50 _reflns_number_total 1848 _reflns_number_gt 1685 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'SAINT (Bruker, 2004)' _computing_data_reduction 'SAINT (Bruker, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond (CRYSTAL IMPACT, 2001)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0315P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1848 _refine_ls_number_parameters 128 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0280 _refine_ls_R_factor_gt 0.0242 _refine_ls_wR_factor_ref 0.0602 _refine_ls_wR_factor_gt 0.0586 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.36382(2) 0.2500 0.52779(2) 0.02102(9) Uani 1 2 d S . . Br1 Br 0.92699(8) 0.2500 0.48980(6) 0.03757(18) Uani 1 2 d S . . Br2 Br 0.48324(7) 0.2500 0.12520(7) 0.03877(19) Uani 1 2 d S . . Br3 Br 1.09122(7) 0.2500 0.04576(6) 0.03724(18) Uani 1 2 d S . . O1 O 1.2068(3) 0.4111(4) 0.3284(3) 0.0307(7) Uani 1 1 d . . . O2 O 0.5618(3) 0.0924(4) 0.4075(3) 0.0295(7) Uani 1 1 d . . . O3 O 0.2413(6) 0.2500 0.7193(5) 0.0463(14) Uani 1 2 d S . . H3O H 0.1384 0.2500 0.7160 0.08(4) Uiso 1 2 calc SR . . O1W O 0.5926(5) 0.2500 0.6624(4) 0.0335(12) Uani 1 2 d S . . H1W H 0.6366 0.1475 0.6576 0.040(16) Uiso 1 1 calc R . . O2W O 0.0511(6) 0.7500 0.2381(5) 0.0426(14) Uani 1 2 d S . . H2W H 0.093(7) 0.643(8) 0.270(5) 0.06(2) Uiso 1 1 d . . . N1 N 0.7535(7) 0.2500 -0.0132(5) 0.0394(15) Uani 1 2 d S . . H1A H 0.6614 0.2500 -0.0383 0.047 Uiso 1 2 calc SR . . H1B H 0.8205 0.2500 -0.0591 0.047 Uiso 1 2 calc SR . . C1 C 0.6105(6) 0.2500 0.3751(6) 0.0209(12) Uani 1 2 d S . . C2 C 0.7255(6) 0.2500 0.2924(5) 0.0203(13) Uani 1 2 d S . . C3 C 0.6870(6) 0.2500 0.1781(6) 0.0217(13) Uani 1 2 d S . . C4 C 0.7935(7) 0.2500 0.0998(6) 0.0252(13) Uani 1 2 d S . . C5 C 0.9432(6) 0.2500 0.1456(5) 0.0211(12) Uani 1 2 d S . . C6 C 0.9851(6) 0.2500 0.2597(6) 0.0205(12) Uani 1 2 d S . . C7 C 0.8762(7) 0.2500 0.3323(5) 0.0207(12) Uani 1 2 d S . . C8 C 1.1474(7) 0.2500 0.3060(5) 0.0223(13) Uani 1 2 d S . . C9 C 0.3225(10) 0.2500 0.8261(7) 0.047(2) Uani 1 2 d S . . H9A H 0.2552 0.2500 0.8830 0.070 Uiso 1 2 calc SR . . H9B H 0.3837 0.3630 0.8340 0.070 Uiso 0.50 1 calc PR . . H9C H 0.3837 0.1370 0.8340 0.070 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.01688(13) 0.02434(13) 0.02204(15) 0.000 0.00298(9) 0.000 Br1 0.0275(4) 0.0685(5) 0.0167(4) 0.000 0.0021(3) 0.000 Br2 0.0164(3) 0.0651(5) 0.0339(4) 0.000 -0.0019(3) 0.000 Br3 0.0225(3) 0.0673(5) 0.0234(4) 0.000 0.0092(3) 0.000 O1 0.0236(17) 0.0323(17) 0.036(2) -0.0027(15) -0.0001(14) -0.0058(13) O2 0.0287(17) 0.0245(15) 0.037(2) 0.0054(14) 0.0119(15) 0.0009(12) O3 0.042(3) 0.064(4) 0.035(3) 0.000 0.014(3) 0.000 O1W 0.026(3) 0.035(3) 0.039(3) 0.000 -0.002(2) 0.000 O2W 0.034(3) 0.052(3) 0.039(4) 0.000 -0.011(2) 0.000 N1 0.025(3) 0.078(4) 0.016(3) 0.000 0.003(2) 0.000 C1 0.016(3) 0.022(3) 0.024(4) 0.000 0.000(2) 0.000 C2 0.020(3) 0.017(3) 0.024(4) 0.000 0.006(2) 0.000 C3 0.010(3) 0.029(3) 0.025(4) 0.000 -0.001(2) 0.000 C4 0.020(3) 0.033(3) 0.022(4) 0.000 -0.002(2) 0.000 C5 0.015(3) 0.029(3) 0.019(3) 0.000 0.002(2) 0.000 C6 0.016(3) 0.022(3) 0.024(3) 0.000 0.003(2) 0.000 C7 0.018(3) 0.026(3) 0.018(3) 0.000 0.003(2) 0.000 C8 0.017(3) 0.034(3) 0.016(3) 0.000 0.004(2) 0.000 C9 0.057(5) 0.051(5) 0.035(5) 0.000 0.014(4) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 O1W 2.499(5) . ? Pb1 O2 2.567(3) 2_656 ? Pb1 O2 2.567(3) 3_656 ? Pb1 O3 2.649(5) . ? Pb1 O2 2.650(3) . ? Pb1 O2 2.650(3) 4_565 ? Br1 C7 1.899(6) . ? Br2 C3 1.893(6) . ? Br3 C5 1.887(6) . ? O1 C8 1.258(4) . ? O2 C1 1.255(4) . ? O2 Pb1 2.567(3) 3_656 ? O3 C9 1.413(10) . ? O3 H3O 0.9300 . ? O1W H1W 0.8200 . ? O2W H2W 0.91(6) . ? N1 C4 1.367(9) . ? N1 H1A 0.8600 . ? N1 H1B 0.8600 . ? C1 O2 1.255(4) 4_565 ? C1 C2 1.510(8) . ? C2 C3 1.381(9) . ? C2 C7 1.403(8) . ? C3 C4 1.413(9) . ? C4 C5 1.413(8) . ? C5 C6 1.382(9) . ? C6 C7 1.381(8) . ? C6 C8 1.522(8) . ? C8 O1 1.258(4) 4_565 ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1W Pb1 O2 68.18(8) . 2_656 ? O1W Pb1 O2 68.18(8) . 3_656 ? O2 Pb1 O2 135.28(15) 2_656 3_656 ? O1W Pb1 O3 80.42(18) . . ? O2 Pb1 O3 81.84(9) 2_656 . ? O2 Pb1 O3 81.84(9) 3_656 . ? O1W Pb1 O2 77.71(13) . . ? O2 Pb1 O2 111.98(7) 2_656 . ? O2 Pb1 O2 67.12(11) 3_656 . ? O3 Pb1 O2 146.92(11) . . ? O1W Pb1 O2 77.71(13) . 4_565 ? O2 Pb1 O2 67.12(11) 2_656 4_565 ? O2 Pb1 O2 111.98(7) 3_656 4_565 ? O3 Pb1 O2 146.92(11) . 4_565 ? O2 Pb1 O2 48.73(13) . 4_565 ? C1 O2 Pb1 144.0(3) . 3_656 ? C1 O2 Pb1 95.0(3) . . ? Pb1 O2 Pb1 112.88(11) 3_656 . ? C9 O3 Pb1 124.1(5) . . ? C9 O3 H3O 118.0 . . ? Pb1 O3 H3O 118.0 . . ? Pb1 O1W H1W 109.5 . . ? C4 N1 H1A 120.0 . . ? C4 N1 H1B 120.0 . . ? H1A N1 H1B 120.0 . . ? O2 C1 O2 121.2(6) 4_565 . ? O2 C1 C2 119.4(3) 4_565 . ? O2 C1 C2 119.4(3) . . ? C3 C2 C7 118.7(5) . . ? C3 C2 C1 121.9(5) . . ? C7 C2 C1 119.4(5) . . ? C2 C3 C4 122.5(5) . . ? C2 C3 Br2 118.3(4) . . ? C4 C3 Br2 119.2(5) . . ? N1 C4 C3 121.8(6) . . ? N1 C4 C5 122.4(6) . . ? C3 C4 C5 115.8(6) . . ? C6 C5 C4 123.0(6) . . ? C6 C5 Br3 119.0(4) . . ? C4 C5 Br3 118.0(5) . . ? C7 C6 C5 118.7(6) . . ? C7 C6 C8 119.8(6) . . ? C5 C6 C8 121.5(5) . . ? C6 C7 C2 121.3(6) . . ? C6 C7 Br1 120.6(5) . . ? C2 C7 Br1 118.1(4) . . ? O1 C8 O1 125.3(6) . 4_565 ? O1 C8 C6 117.2(3) . . ? O1 C8 C6 117.2(3) 4_565 . ? O3 C9 H9A 109.5 . . ? O3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? O3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1W Pb1 O2 C1 -85.5(3) . . . . ? O2 Pb1 O2 C1 -25.4(3) 2_656 . . . ? O2 Pb1 O2 C1 -156.8(4) 3_656 . . . ? O3 Pb1 O2 C1 -135.2(4) . . . . ? O2 Pb1 O2 C1 -1.2(3) 4_565 . . . ? O1W Pb1 O2 Pb1 71.28(12) . . . 3_656 ? O2 Pb1 O2 Pb1 131.41(17) 2_656 . . 3_656 ? O2 Pb1 O2 Pb1 0.0 3_656 . . 3_656 ? O3 Pb1 O2 Pb1 21.6(3) . . . 3_656 ? O2 Pb1 O2 Pb1 155.62(8) 4_565 . . 3_656 ? O1W Pb1 O3 C9 0.000(2) . . . . ? O2 Pb1 O3 C9 -69.11(8) 2_656 . . . ? O2 Pb1 O3 C9 69.11(8) 3_656 . . . ? O2 Pb1 O3 C9 49.1(2) . . . . ? O2 Pb1 O3 C9 -49.1(2) 4_565 . . . ? Pb1 O2 C1 O2 -139.6(3) 3_656 . . 4_565 ? Pb1 O2 C1 O2 2.1(6) . . . 4_565 ? Pb1 O2 C1 C2 42.6(9) 3_656 . . . ? Pb1 O2 C1 C2 -175.6(5) . . . . ? O2 C1 C2 C3 -88.9(5) 4_565 . . . ? O2 C1 C2 C3 88.9(5) . . . . ? O2 C1 C2 C7 91.1(5) 4_565 . . . ? O2 C1 C2 C7 -91.1(5) . . . . ? C7 C2 C3 C4 0.0 . . . . ? C1 C2 C3 C4 180.0 . . . . ? C7 C2 C3 Br2 180.0 . . . . ? C1 C2 C3 Br2 0.0 . . . . ? C2 C3 C4 N1 180.0 . . . . ? Br2 C3 C4 N1 0.0 . . . . ? C2 C3 C4 C5 0.0 . . . . ? Br2 C3 C4 C5 180.0 . . . . ? N1 C4 C5 C6 180.0 . . . . ? C3 C4 C5 C6 0.0 . . . . ? N1 C4 C5 Br3 0.0 . . . . ? C3 C4 C5 Br3 180.0 . . . . ? C4 C5 C6 C7 0.0 . . . . ? Br3 C5 C6 C7 180.0 . . . . ? C4 C5 C6 C8 180.0 . . . . ? Br3 C5 C6 C8 0.0 . . . . ? C5 C6 C7 C2 0.0 . . . . ? C8 C6 C7 C2 180.0 . . . . ? C5 C6 C7 Br1 180.0 . . . . ? C8 C6 C7 Br1 0.0 . . . . ? C3 C2 C7 C6 0.0 . . . . ? C1 C2 C7 C6 180.0 . . . . ? C3 C2 C7 Br1 180.0 . . . . ? C1 C2 C7 Br1 0.0 . . . . ? C7 C6 C8 O1 -86.8(5) . . . . ? C5 C6 C8 O1 93.2(5) . . . . ? C7 C6 C8 O1 86.8(5) . . . 4_565 ? C5 C6 C8 O1 -93.2(5) . . . 4_565 ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.822 _refine_diff_density_min -1.402 _refine_diff_density_rms 0.215 data_pb _database_code_depnum_ccdc_archive 'CCDC 789899' #TrackingRef 'PB DMA.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H10 Br3 N O8 Pb' _chemical_formula_weight 695.09 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' Br Br -0.2901 2.4595 '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' _symmetry_cell_setting TRICLINIC _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.5364(6) _cell_length_b 9.2515(7) _cell_length_c 12.6753(9) _cell_angle_alpha 70.7600(10) _cell_angle_beta 73.9090(10) _cell_angle_gamma 66.4000(10) _cell_volume 753.76(10) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4402 _cell_measurement_theta_min 2.480 _cell_measurement_theta_max 27.468 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.063 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 632 _exptl_absorpt_coefficient_mu 19.178 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.004 _exptl_absorpt_correction_T_max 0.026 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEXII area-detector' _diffrn_measurement_method '\f and \w' _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5372 _diffrn_reflns_av_R_equivalents 0.0363 _diffrn_reflns_av_sigmaI/netI 0.0523 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 25.50 _reflns_number_total 2718 _reflns_number_gt 2479 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker, 2004)' _computing_cell_refinement 'SAINT (Bruker, 2004)' _computing_data_reduction 'SAINT (Bruker, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond (CRYSTAL IMPACT, 2001)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1027P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2718 _refine_ls_number_parameters 162 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0511 _refine_ls_R_factor_gt 0.0467 _refine_ls_wR_factor_ref 0.1355 _refine_ls_wR_factor_gt 0.1223 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.64644(5) 0.54390(3) 0.59835(3) 0.02080(18) Uani 1 1 d . . . Br1 Br 0.24460(16) 1.05071(12) 0.58937(8) 0.0302(3) Uani 1 1 d . . . Br2 Br -0.02506(15) 1.34659(11) 0.95581(8) 0.0292(3) Uani 1 1 d . . . Br3 Br 0.51257(15) 0.69654(11) 1.00979(9) 0.0302(3) Uani 1 1 d . . . O1 O 0.4218(10) 0.6462(8) 0.7598(6) 0.0260(15) Uani 1 1 d . . . O2 O 0.6559(10) 0.7574(8) 0.7007(7) 0.0326(17) Uani 1 1 d . . . O3 O -0.1740(9) 1.3164(8) 0.7212(6) 0.0272(16) Uani 1 1 d . . . O4 O 0.0602(11) 1.4284(8) 0.6552(7) 0.0375(19) Uani 1 1 d . . . O1W O 0.4489(10) 0.3644(8) 0.6810(7) 0.0360(18) Uani 1 1 d . . . H1WB H 0.5511 0.2947 0.6554 0.054 Uiso 1 1 d R . . H1WA H 0.3484 0.3665 0.6618 0.054 Uiso 1 1 d R . . O2W O 0.7325(14) 0.3163(9) 0.4748(6) 0.040(2) Uani 1 1 d . . . H2WA H 0.7270 0.2222 0.5115 0.060 Uiso 1 1 d R . . H2WB H 0.8519 0.3145 0.4609 0.060 Uiso 1 1 d R . . O3W O 0.7234(12) 0.0484(9) 0.6573(7) 0.040(2) Uani 1 1 d D . . H3WA H 0.6750(13) -0.0192(11) 0.6553(7) 0.061 Uiso 1 1 d RD . . H3WB H 0.8415(16) -0.0023(10) 0.6689(7) 0.061 Uiso 1 1 d RD . . O4W O 0.9770(12) 0.2570(10) 0.2601(8) 0.047(2) Uani 1 1 d D . . H4WA H 0.8720(15) 0.2505(10) 0.2528(8) 0.071 Uiso 1 1 d RD . . H4WB H 1.0756(15) 0.1976(11) 0.2230(8) 0.071 Uiso 1 1 d RD . . N1 N 0.2359(13) 1.0097(10) 1.0801(6) 0.0279(18) Uani 1 1 d . . . H11 H 0.3078 0.9229 1.1210 0.034 Uiso 1 1 calc R . . H12 H 0.1622 1.0912 1.1085 0.034 Uiso 1 1 calc R . . C1 C 0.4897(14) 0.7541(11) 0.7543(8) 0.023(2) Uani 1 1 d . . . C2 C 0.3570(13) 0.8938(10) 0.8091(7) 0.0181(8) Uani 1 1 d . . . C3 C 0.2412(13) 1.0345(10) 0.7438(7) 0.0181(8) Uani 1 1 d . . . C4 C 0.1267(13) 1.1691(10) 0.7879(7) 0.0181(8) Uani 1 1 d . . . C5 C 0.1284(13) 1.1617(10) 0.8983(7) 0.0181(8) Uani 1 1 d . . . C6 C 0.2387(13) 1.0180(10) 0.9691(7) 0.0181(8) Uani 1 1 d . . . C7 C 0.3553(13) 0.8895(10) 0.9188(7) 0.0181(8) Uani 1 1 d . . . C8 C -0.0056(13) 1.3206(10) 0.7142(7) 0.0180(18) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.0249(3) 0.0164(2) 0.0234(3) -0.00396(16) -0.00666(16) -0.00846(17) Br1 0.0395(6) 0.0304(5) 0.0207(5) -0.0089(4) -0.0064(4) -0.0090(4) Br2 0.0306(6) 0.0228(5) 0.0362(5) -0.0169(4) -0.0054(4) -0.0036(4) Br3 0.0332(6) 0.0190(5) 0.0361(5) 0.0003(4) -0.0173(4) -0.0047(4) O1 0.026(4) 0.025(3) 0.033(4) -0.015(3) 0.002(3) -0.013(3) O2 0.022(4) 0.029(4) 0.051(5) -0.024(3) 0.007(3) -0.011(3) O3 0.020(3) 0.025(3) 0.036(4) -0.001(3) -0.008(3) -0.009(3) O4 0.037(4) 0.017(3) 0.046(4) 0.008(3) -0.011(4) -0.008(3) O1W 0.022(4) 0.028(4) 0.060(5) -0.007(4) -0.005(3) -0.015(3) O2W 0.057(5) 0.022(4) 0.031(4) -0.003(3) -0.006(4) -0.008(4) O3W 0.047(5) 0.030(4) 0.048(5) 0.007(3) -0.019(4) -0.024(4) O4W 0.040(5) 0.042(5) 0.064(6) -0.006(4) -0.022(4) -0.014(4) N1 0.038(5) 0.032(4) 0.018(4) -0.008(3) -0.002(3) -0.017(4) C1 0.024(5) 0.017(4) 0.024(5) -0.005(4) -0.011(4) 0.001(4) C2 0.0194(18) 0.0150(17) 0.0227(18) -0.0051(15) -0.0037(15) -0.0084(14) C3 0.0194(18) 0.0150(17) 0.0227(18) -0.0051(15) -0.0037(15) -0.0084(14) C4 0.0194(18) 0.0150(17) 0.0227(18) -0.0051(15) -0.0037(15) -0.0084(14) C5 0.0194(18) 0.0150(17) 0.0227(18) -0.0051(15) -0.0037(15) -0.0084(14) C6 0.0194(18) 0.0150(17) 0.0227(18) -0.0051(15) -0.0037(15) -0.0084(14) C7 0.0194(18) 0.0150(17) 0.0227(18) -0.0051(15) -0.0037(15) -0.0084(14) C8 0.016(4) 0.016(4) 0.021(4) -0.007(3) -0.003(3) -0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 O3 2.327(6) 1_645 ? Pb1 O1 2.454(6) . ? Pb1 O1W 2.457(7) . ? Pb1 O2 2.728(7) . ? Pb1 O2W 2.798(8) . ? Br1 C3 1.908(9) . ? Br2 C5 1.888(9) . ? Br3 C7 1.905(8) . ? O1 C1 1.267(12) . ? O2 C1 1.256(12) . ? O3 C8 1.263(11) . ? O3 Pb1 2.327(6) 1_465 ? O4 C8 1.224(12) . ? N1 C6 1.378(11) . ? C1 C2 1.525(13) . ? C2 C7 1.375(12) . ? C2 C3 1.386(12) . ? C3 C4 1.392(12) . ? C4 C5 1.382(12) . ? C4 C8 1.539(11) . ? C5 C6 1.416(11) . ? C6 C7 1.394(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Pb1 O1 90.5(2) 1_645 . ? O3 Pb1 O1W 73.4(2) 1_645 . ? O1 Pb1 O1W 75.4(2) . . ? O3 Pb1 O2 93.6(2) 1_645 . ? O1 Pb1 O2 50.5(2) . . ? O1W Pb1 O2 124.5(2) . . ? O3 Pb1 O2W 82.2(2) 1_645 . ? O1 Pb1 O2W 142.3(3) . . ? O1W Pb1 O2W 67.1(3) . . ? O2 Pb1 O2W 166.2(3) . . ? C1 O1 Pb1 97.9(6) . . ? C1 O2 Pb1 85.5(6) . . ? C8 O3 Pb1 110.8(5) . 1_465 ? O2 C1 O1 123.6(9) . . ? O2 C1 C2 118.1(9) . . ? O1 C1 C2 118.2(9) . . ? C7 C2 C3 118.5(8) . . ? C7 C2 C1 122.7(7) . . ? C3 C2 C1 118.7(8) . . ? C2 C3 C4 120.9(8) . . ? C2 C3 Br1 120.5(7) . . ? C4 C3 Br1 118.6(6) . . ? C5 C4 C3 119.4(8) . . ? C5 C4 C8 121.3(8) . . ? C3 C4 C8 119.2(8) . . ? C4 C5 C6 121.4(8) . . ? C4 C5 Br2 118.7(6) . . ? C6 C5 Br2 119.9(6) . . ? N1 C6 C7 122.4(8) . . ? N1 C6 C5 121.2(8) . . ? C7 C6 C5 116.3(8) . . ? C2 C7 C6 123.3(8) . . ? C2 C7 Br3 119.0(7) . . ? C6 C7 Br3 117.6(6) . . ? O4 C8 O3 127.3(8) . . ? O4 C8 C4 118.8(8) . . ? O3 C8 C4 113.9(8) . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 3.180 _refine_diff_density_min -5.000 _refine_diff_density_rms 0.424