Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Foreman, Mark R. St J.' 'Plater, M. John' 'Skakle, M. S.' _publ_contact_author_name 'Dr M John Plater' _publ_contact_author_address ; Dr M John Plater Department of Chemistry University of Aberdeen Meston Walk Aberdeen AB24 3UE UNITED KINGDOM ; _publ_contact_author_email 'che356@abdn.ac.uk' data_newm _database_code_CSD 158365 _publ_requested_journal test _audit_creation_method SHELXL-97 _chemical_name_systematic ; Lead succinate ; _chemical_name_common 'lead succinate' _chemical_formula_moiety 'C4 H4 O4 Pb' _chemical_formula_sum 'C4 H4 O4 Pb' _chemical_formula_weight 323.26 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' 'O' 'O' 0.0106 0.0060 '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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 6.8830(3) _cell_length_b 20.9508(13) _cell_length_c 7.5354(5) _cell_angle_alpha 90.00 _cell_angle_beta 92.8680(10) _cell_angle_gamma 90.00 _cell_volume 1085.28(11) _cell_formula_units_Z 8 _cell_measurement_temperature 303(2) _cell_measurement_reflns_used 5663 _cell_measurement_theta_min 1.94 _cell_measurement_theta_max 23.28 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 3.957 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1136 _exptl_absorpt_coefficient_mu 31.018 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.0387 _exptl_absorpt_correction_T_max 0.3061 _exptl_special_details ; ? ; _diffrn_ambient_temperature 303(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 SMART area CCD detector' _diffrn_measurement_method /f-/w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 5663 _diffrn_reflns_av_R_equivalents 0.0619 _diffrn_reflns_av_sigmaI/netI 0.0446 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 23.28 _reflns_number_total 1551 _reflns_number_gt 1157 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Oscail in ORTEX (McArdle, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0576P)^2^+6.0733P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patterson _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_number_reflns 1551 _refine_ls_number_parameters 143 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0523 _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_ref 0.1081 _refine_ls_wR_factor_gt 0.1029 _refine_ls_goodness_of_fit_ref 1.137 _refine_ls_restrained_S_all 1.137 _refine_ls_shift/su_max 0.000 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.01427(8) 0.18815(4) 0.30527(8) 0.0151(3) Uani 1 d . . . O1 O 0.3342(18) 0.1370(6) 0.4589(15) 0.023(3) Uani 1 d . . . O2 O 0.2003(17) 0.2050(6) 0.6338(15) 0.020(3) Uani 1 d . . . C1 C 0.335(3) 0.1703(8) 0.603(2) 0.017(4) Uani 1 d . . . C2 C 0.505(3) 0.1617(9) 0.729(2) 0.016(4) Uani 1 d . . . H2A H 0.6233 0.1689 0.6670 0.019 Uiso 1 calc R . . H2B H 0.5072 0.1181 0.7720 0.019 Uiso 1 calc R . . C3 C 0.500(2) 0.2082(8) 0.890(2) 0.012(4) Uiso 1 d . . . H3A H 0.4903 0.2519 0.8481 0.014 Uiso 1 calc R . . H3B H 0.3876 0.1992 0.9583 0.014 Uiso 1 calc R . . C4 C 0.683(2) 0.2005(8) 1.007(2) 0.014(4) Uiso 1 d . . . O3 O 0.675(2) 0.1583(7) 1.1382(17) 0.032(3) Uani 1 d . . . O4 O 0.8292(18) 0.2310(7) 0.9901(17) 0.035(4) Uani 1 d . . . Pb2 Pb 0.50268(10) 0.06290(4) 0.26912(8) 0.0153(3) Uani 1 d . . . O5 O 0.1823(19) 0.1014(7) 0.1340(16) 0.031(4) Uani 1 d . . . O6 O 0.297(2) 0.0331(7) -0.0511(17) 0.036(4) Uani 1 d . . . C5 C 0.174(2) 0.0689(8) -0.020(2) 0.012(4) Uiso 1 d . . . C6 C 0.002(3) 0.0837(8) -0.139(2) 0.023(4) Uani 1 d . . . H6A H 0.0018 0.1287 -0.1689 0.028 Uiso 1 calc R . . H6B H -0.1157 0.0746 -0.0778 0.028 Uiso 1 calc R . . C7 C 0.004(3) 0.0434(10) -0.311(2) 0.022(4) Uiso 1 d . . . H7A H 0.1227 0.0521 -0.3713 0.026 Uiso 1 calc R . . H7B H 0.0027 -0.0016 -0.2810 0.026 Uiso 1 calc R . . C8 C -0.168(3) 0.0588(8) -0.431(2) 0.014(4) Uani 1 d . . . O7 O -0.1612(18) 0.1032(6) -0.5421(15) 0.023(3) Uani 1 d . . . O8 O -0.3205(18) 0.0266(6) -0.4181(15) 0.022(3) Uani 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 0.0154(4) 0.0171(4) 0.0124(4) -0.0007(3) -0.0037(3) -0.0001(3) O1 0.024(8) 0.021(7) 0.022(7) -0.001(5) -0.009(6) 0.007(6) O2 0.012(7) 0.028(8) 0.019(6) -0.009(5) -0.001(5) 0.011(6) C1 0.024(11) 0.024(11) 0.002(8) -0.002(7) 0.001(7) -0.008(9) C2 0.021(11) 0.014(10) 0.012(9) -0.005(7) -0.004(7) 0.005(7) O3 0.029(8) 0.040(8) 0.027(7) 0.005(6) -0.010(6) -0.007(7) O4 0.019(7) 0.052(10) 0.034(8) 0.019(7) -0.006(6) -0.013(7) Pb2 0.0158(4) 0.0182(4) 0.0113(4) 0.0007(3) -0.0042(3) -0.0010(3) O5 0.022(8) 0.054(10) 0.017(7) -0.007(6) -0.013(6) 0.011(7) O6 0.043(9) 0.035(8) 0.027(7) -0.018(6) -0.017(7) 0.023(7) C6 0.040(13) 0.007(9) 0.023(9) 0.007(8) 0.005(9) 0.007(9) C8 0.017(11) 0.011(10) 0.016(9) 0.002(8) 0.009(7) 0.000(8) O7 0.026(8) 0.025(8) 0.018(7) 0.004(6) -0.010(6) -0.006(6) O8 0.022(8) 0.024(7) 0.021(7) 0.005(5) -0.005(5) -0.005(6) _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 O7 2.467(12) 1_556 ? Pb1 O5 2.541(13) . ? Pb1 O4 2.571(13) 4_465 ? Pb1 O1 2.661(12) . ? Pb1 O3 2.669(13) 1_454 ? Pb1 O2 2.752(11) . ? O1 C1 1.29(2) . ? O1 Pb2 2.442(12) . ? O2 C1 1.21(2) . ? C1 C2 1.48(2) . ? C2 C3 1.56(2) . ? C3 C4 1.51(2) . ? C4 O4 1.20(2) . ? C4 O3 1.33(2) . ? O3 Pb2 2.550(14) 1_556 ? O3 Pb1 2.668(13) 1_656 ? O4 Pb1 2.571(13) 4_666 ? Pb2 O5 2.515(12) . ? Pb2 O8 2.548(12) 3 ? Pb2 O3 2.550(14) 1_554 ? Pb2 O8 2.707(11) 1_656 ? O5 C5 1.34(2) . ? O6 C5 1.16(2) . ? C5 C6 1.48(2) . ? C6 C7 1.55(3) . ? C7 C8 1.49(2) . ? C8 O7 1.25(2) . ? C8 O8 1.26(2) . ? O7 Pb1 2.467(12) 1_554 ? O8 Pb2 2.548(12) 3 ? O8 Pb2 2.707(11) 1_454 ? 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 O7 Pb1 O5 88.1(5) 1_556 . ? O7 Pb1 O4 87.4(4) 1_556 4_465 ? O5 Pb1 O4 175.5(5) . 4_465 ? O7 Pb1 O1 85.4(4) 1_556 . ? O5 Pb1 O1 62.9(4) . . ? O4 Pb1 O1 116.8(4) 4_465 . ? O7 Pb1 O3 67.3(4) 1_556 1_454 ? O5 Pb1 O3 90.1(4) . 1_454 ? O4 Pb1 O3 88.0(4) 4_465 1_454 ? O1 Pb1 O3 142.7(4) . 1_454 ? O7 Pb1 O2 83.7(4) 1_556 . ? O5 Pb1 O2 110.2(4) . . ? O4 Pb1 O2 69.5(4) 4_465 . ? O1 Pb1 O2 47.4(4) . . ? O3 Pb1 O2 144.2(4) 1_454 . ? C1 O1 Pb2 148.6(12) . . ? C1 O1 Pb1 96.7(11) . . ? Pb2 O1 Pb1 114.1(4) . . ? C1 O2 Pb1 94.3(9) . . ? O2 C1 O1 121.1(16) . . ? O2 C1 C2 122.5(15) . . ? O1 C1 C2 116.4(16) . . ? C1 C2 C3 112.3(14) . . ? C4 C3 C2 109.9(14) . . ? O4 C4 O3 119.8(16) . . ? O4 C4 C3 123.8(15) . . ? O3 C4 C3 116.3(15) . . ? C4 O3 Pb2 147.8(11) . 1_556 ? C4 O3 Pb1 97.4(10) . 1_656 ? Pb2 O3 Pb1 114.5(5) 1_556 1_656 ? C4 O4 Pb1 147.9(12) . 4_666 ? O1 Pb2 O5 66.5(4) . . ? O1 Pb2 O8 87.2(4) . 3 ? O5 Pb2 O8 88.5(4) . 3 ? O1 Pb2 O3 88.4(4) . 1_554 ? O5 Pb2 O3 90.5(4) . 1_554 ? O8 Pb2 O3 175.6(4) 3 1_554 ? O1 Pb2 O8 82.8(4) . 1_656 ? O5 Pb2 O8 142.1(4) . 1_656 ? O8 Pb2 O8 67.6(4) 3 1_656 ? O3 Pb2 O8 111.0(4) 1_554 1_656 ? C5 O5 Pb2 100.6(10) . . ? C5 O5 Pb1 143.2(11) . . ? Pb2 O5 Pb1 115.9(4) . . ? O6 C5 O5 120.2(15) . . ? O6 C5 C6 125.5(16) . . ? O5 C5 C6 114.4(16) . . ? C5 C6 C7 110.5(15) . . ? C8 C7 C6 110.5(15) . . ? O7 C8 O8 120.6(16) . . ? O7 C8 C7 120.9(16) . . ? O8 C8 C7 118.5(15) . . ? C8 O7 Pb1 151.8(12) . 1_554 ? C8 O8 Pb2 149.5(11) . 3 ? C8 O8 Pb2 97.0(10) . 1_454 ? Pb2 O8 Pb2 112.4(4) 3 1_454 ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 23.28 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 3.062 _refine_diff_density_min -2.039 _refine_diff_density_rms 0.380 data_js040c _database_code_CSD 158366 _publ_requested_journal test _audit_creation_method SHELXL-97 _chemical_name_systematic ; Pb-Ph- ; _chemical_name_common 'C56 H36 O13 Pb3' _chemical_formula_moiety 'C56 H36 O13 Pb3' _chemical_formula_sum 'C56 H36 O13 Pb3' _chemical_formula_weight 1538.42 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' 'Pb' 'Pb' -3.3944 10.1111 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, -z-1/2' _cell_length_a 16.8880(7) _cell_length_b 17.5052(7) _cell_length_c 17.0201(7) _cell_angle_alpha 90.00 _cell_angle_beta 93.8450(10) _cell_angle_gamma 90.00 _cell_volume 5020.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 303(2) _cell_measurement_reflns_used 38963 _cell_measurement_theta_min 2.01 _cell_measurement_theta_max 32.52 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.035 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2888 _exptl_absorpt_coefficient_mu 10.102 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_process_details '(SADABS; Sheldrick, 1997)' _exptl_absorpt_correction_T_min 0.652 _exptl_absorpt_correction_T_max 0.928 _exptl_special_details ; ? ; _diffrn_ambient_temperature 303(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 SMART area CCD detector' _diffrn_measurement_method /f-/w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38963 _diffrn_reflns_av_R_equivalents 0.0657 _diffrn_reflns_av_sigmaI/netI 0.0875 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 32.52 _reflns_number_total 17968 _reflns_number_gt 10956 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortex in OSCAIL (McArdle, 1995)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0308P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17968 _refine_ls_number_parameters 649 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0790 _refine_ls_R_factor_gt 0.0362 _refine_ls_wR_factor_ref 0.0742 _refine_ls_wR_factor_gt 0.0638 _refine_ls_goodness_of_fit_ref 0.859 _refine_ls_restrained_S_all 0.859 _refine_ls_shift/su_max 0.003 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.058251(10) 0.168706(10) 0.934175(11) 0.03053(4) Uani 1 d . . . Pb2 Pb -0.141662(10) 0.080835(11) 0.891702(11) 0.03119(5) Uani 1 d . . . Pb3 Pb 0.031826(10) -0.047565(10) 0.910869(10) 0.02754(4) Uani 1 d . . . O1 O -0.02136(16) 0.06556(16) 0.95479(17) 0.0239(6) Uani 1 d . . . O2 O -0.0212(2) 0.2193(2) 1.0338(2) 0.0461(9) Uani 1 d . . . O3 O -0.1352(2) 0.2050(2) 0.9623(2) 0.0538(10) Uani 1 d . . . C1 C -0.0916(3) 0.2387(3) 1.0121(3) 0.0369(11) Uani 1 d . . . C2 C -0.1222(3) 0.3097(3) 1.0492(3) 0.0373(11) Uani 1 d . . . C3 C -0.2007(3) 0.3126(3) 1.0672(3) 0.0455(13) Uani 1 d . . . H3 H -0.2350 0.2730 1.0519 0.055 Uiso 1 calc R . . C4 C -0.2282(4) 0.3740(4) 1.1077(4) 0.0663(19) Uani 1 d . . . H4 H -0.2807 0.3750 1.1210 0.080 Uiso 1 calc R . . C5 C -0.1793(5) 0.4333(4) 1.1284(5) 0.078(2) Uani 1 d . . . H5 H -0.1984 0.4751 1.1551 0.093 Uiso 1 calc R . . C6 C -0.1015(4) 0.4312(4) 1.1097(5) 0.067(2) Uani 1 d . . . H6 H -0.0681 0.4717 1.1244 0.081 Uiso 1 calc R . . C7 C -0.0724(3) 0.3709(3) 1.0699(3) 0.0484(14) Uani 1 d . . . C8 C 0.0148(4) 0.3747(4) 1.0517(4) 0.0565(16) Uani 1 d . . . O4 O 0.0649(3) 0.3867(5) 1.1037(3) 0.114(3) Uani 1 d . . . C9 C 0.0367(3) 0.3684(3) 0.9689(4) 0.0468(13) Uani 1 d . . . C10 C -0.0174(4) 0.3779(4) 0.9051(4) 0.0615(17) Uani 1 d . . . H10 H -0.0704 0.3870 0.9134 0.074 Uiso 1 calc R . . C11 C 0.0067(5) 0.3738(4) 0.8284(4) 0.074(2) Uani 1 d . . . H11 H -0.0306 0.3797 0.7860 0.088 Uiso 1 calc R . . C12 C 0.0841(5) 0.3613(4) 0.8149(5) 0.075(2) Uani 1 d . . . H12 H 0.1000 0.3588 0.7637 0.090 Uiso 1 calc R . . C13 C 0.1394(4) 0.3523(4) 0.8790(4) 0.0634(18) Uani 1 d . . . H13 H 0.1925 0.3436 0.8707 0.076 Uiso 1 calc R . . C14 C 0.1153(4) 0.3562(4) 0.9542(4) 0.0557(16) Uani 1 d . . . H14 H 0.1528 0.3506 0.9964 0.067 Uiso 1 calc R . . O5 O 0.1404(2) 0.0573(2) 0.8943(2) 0.0448(9) Uani 1 d . . . O6 O 0.1867(2) -0.0402(2) 0.9655(2) 0.0434(9) Uani 1 d . . . C15 C 0.1967(3) 0.0177(3) 0.9249(3) 0.0357(11) Uani 1 d . . . C16 C 0.2807(3) 0.0389(3) 0.9074(3) 0.0428(12) Uani 1 d . . . C17 C 0.2945(4) 0.1075(4) 0.8688(4) 0.073(2) Uani 1 d . . . H17 H 0.2522 0.1401 0.8559 0.088 Uiso 1 calc R . . C18 C 0.3680(5) 0.1277(6) 0.8498(5) 0.105(3) Uani 1 d . . . H18 H 0.3766 0.1737 0.8245 0.126 Uiso 1 calc R . . C19 C 0.4297(5) 0.0787(7) 0.8687(6) 0.109(4) Uani 1 d . . . H19 H 0.4808 0.0920 0.8564 0.131 Uiso 1 calc R . . C20 C 0.4176(4) 0.0106(5) 0.9051(5) 0.082(3) Uani 1 d . . . H20 H 0.4603 -0.0223 0.9159 0.098 Uiso 1 calc R . . C21 C 0.3428(3) -0.0104(4) 0.9265(4) 0.0528(15) Uani 1 d . . . C22 C 0.3351(3) -0.0858(4) 0.9667(4) 0.0494(14) Uani 1 d . . . O7 O 0.3297(3) -0.1435(3) 0.9273(3) 0.0768(14) Uani 1 d . . . C23 C 0.3421(3) -0.0873(3) 1.0548(3) 0.0432(13) Uani 1 d . . . C24 C 0.3482(3) -0.0200(4) 1.0971(4) 0.0495(14) Uani 1 d . . . H24 H 0.3475 0.0267 1.0711 0.059 Uiso 1 calc R . . C25 C 0.3553(4) -0.0225(5) 1.1778(4) 0.0659(19) Uani 1 d . . . H25 H 0.3570 0.0226 1.2067 0.079 Uiso 1 calc R . . C26 C 0.3598(4) -0.0924(6) 1.2164(5) 0.075(2) Uani 1 d . . . H26 H 0.3665 -0.0942 1.2711 0.090 Uiso 1 calc R . . C27 C 0.3544(4) -0.1583(5) 1.1739(5) 0.072(2) Uani 1 d . . . H27 H 0.3566 -0.2050 1.1999 0.087 Uiso 1 calc R . . C28 C 0.3459(4) -0.1568(4) 1.0938(4) 0.0590(17) Uani 1 d . . . H28 H 0.3427 -0.2022 1.0654 0.071 Uiso 1 calc R . . O8 O -0.0555(2) 0.1582(2) 0.8050(2) 0.0416(9) Uani 1 d . . . O9 O -0.0509(2) 0.0343(2) 0.78050(19) 0.0384(8) Uani 1 d . . . C29 C -0.0371(3) 0.1028(3) 0.7621(3) 0.0312(10) Uani 1 d . . . C30 C 0.0003(3) 0.1187(3) 0.6876(3) 0.0339(11) Uani 1 d . . . C31 C 0.0159(3) 0.1933(3) 0.6661(3) 0.0464(13) Uani 1 d . . . H31 H 0.0051 0.2329 0.7001 0.056 Uiso 1 calc R . . C32 C 0.0474(4) 0.2100(4) 0.5949(4) 0.0601(17) Uani 1 d . . . H32 H 0.0586 0.2602 0.5818 0.072 Uiso 1 calc R . . C33 C 0.0619(4) 0.1514(4) 0.5437(4) 0.0592(17) Uani 1 d . . . H33 H 0.0809 0.1625 0.4950 0.071 Uiso 1 calc R . . C34 C 0.0486(3) 0.0765(4) 0.5641(3) 0.0466(14) Uani 1 d . . . H34 H 0.0609 0.0372 0.5302 0.056 Uiso 1 calc R . . C35 C 0.0165(3) 0.0596(3) 0.6359(3) 0.0369(11) Uani 1 d . . . C36 C 0.0003(3) -0.0237(3) 0.6526(3) 0.0372(11) Uani 1 d . . . O10 O -0.0579(3) -0.0542(2) 0.6209(2) 0.0526(10) Uani 1 d . . . C37 C 0.0601(4) -0.0704(3) 0.6994(3) 0.0416(13) Uani 1 d . . . C38 C 0.0412(4) -0.1446(4) 0.7197(3) 0.0592(17) Uani 1 d . . . H38 H -0.0084 -0.1647 0.7044 0.071 Uiso 1 calc R . . C39 C 0.0972(5) -0.1891(4) 0.7636(4) 0.072(2) Uani 1 d . . . H39 H 0.0842 -0.2383 0.7787 0.087 Uiso 1 calc R . . C40 C 0.1715(5) -0.1600(5) 0.7843(4) 0.073(2) Uani 1 d . . . H40 H 0.2088 -0.1904 0.8121 0.087 Uiso 1 calc R . . C41 C 0.1911(4) -0.0869(4) 0.7646(4) 0.0604(18) Uani 1 d . . . H41 H 0.2413 -0.0677 0.7791 0.072 Uiso 1 calc R . . C42 C 0.1345(3) -0.0408(4) 0.7220(3) 0.0474(14) Uani 1 d . . . H42 H 0.1470 0.0092 0.7091 0.057 Uiso 1 calc R . . O11 O 0.1588(2) 0.1781(2) 1.0432(2) 0.0535(10) Uani 1 d . . . O12 O 0.1157(2) 0.0688(2) 1.0888(2) 0.0492(10) Uani 1 d . . . C43 C 0.1589(3) 0.1279(3) 1.0966(3) 0.0357(11) Uani 1 d . . . C44 C 0.2061(3) 0.1420(3) 1.1718(3) 0.0317(10) Uani 1 d . . . C45 C 0.1792(3) 0.1122(3) 1.2413(3) 0.0435(13) Uani 1 d . . . H45 H 0.1348 0.0807 1.2390 0.052 Uiso 1 calc R . . C46 C 0.2180(4) 0.1291(3) 1.3139(4) 0.0539(15) Uani 1 d . . . H46 H 0.2002 0.1086 1.3599 0.065 Uiso 1 calc R . . C47 C 0.2830(4) 0.1765(4) 1.3165(4) 0.0539(15) Uani 1 d . . . H47 H 0.3082 0.1897 1.3649 0.065 Uiso 1 calc R . . C48 C 0.3114(3) 0.2047(3) 1.2481(3) 0.0468(13) Uani 1 d . . . H48 H 0.3567 0.2351 1.2512 0.056 Uiso 1 calc R . . C49 C 0.2736(3) 0.1886(3) 1.1741(3) 0.0351(11) Uani 1 d . . . C50 C 0.3106(3) 0.2149(3) 1.1011(3) 0.0454(13) Uani 1 d . . . O13 O 0.3455(3) 0.1683(3) 1.0635(3) 0.0864(17) Uani 1 d . . . C51 C 0.3079(3) 0.2962(3) 1.0804(3) 0.0417(12) Uani 1 d . . . C52 C 0.2744(3) 0.3498(3) 1.1281(4) 0.0506(14) Uani 1 d . . . H52 H 0.2531 0.3345 1.1746 0.061 Uiso 1 calc R . . C53 C 0.2727(4) 0.4266(4) 1.1066(5) 0.0647(18) Uani 1 d . . . H53 H 0.2525 0.4629 1.1398 0.078 Uiso 1 calc R . . C54 C 0.3005(4) 0.4481(4) 1.0372(5) 0.0662(19) Uani 1 d . . . H54 H 0.2967 0.4989 1.0216 0.079 Uiso 1 calc R . . C55 C 0.3336(4) 0.3966(5) 0.9905(5) 0.072(2) Uani 1 d . . . H55 H 0.3539 0.4126 0.9438 0.087 Uiso 1 calc R . . C56 C 0.3379(4) 0.3209(4) 1.0109(4) 0.0565(16) Uani 1 d . . . H56 H 0.3609 0.2860 0.9781 0.068 Uiso 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 0.02731(8) 0.02981(9) 0.03414(10) 0.00166(8) -0.00037(7) -0.00200(7) Pb2 0.02258(8) 0.03861(10) 0.03158(10) -0.00160(8) -0.00396(6) 0.00245(7) Pb3 0.02599(8) 0.02995(9) 0.02670(9) -0.00445(7) 0.00203(6) 0.00080(7) O1 0.0183(14) 0.0264(16) 0.0258(16) -0.0019(12) -0.0066(11) 0.0009(11) O2 0.041(2) 0.046(2) 0.051(2) -0.0115(18) 0.0039(17) 0.0116(17) O3 0.055(2) 0.050(2) 0.053(2) -0.016(2) -0.0205(19) 0.015(2) C1 0.039(3) 0.035(3) 0.037(3) 0.002(2) 0.002(2) 0.008(2) C2 0.039(3) 0.033(3) 0.039(3) -0.005(2) 0.001(2) 0.006(2) C3 0.039(3) 0.044(3) 0.053(3) -0.008(3) 0.003(2) 0.001(2) C4 0.041(3) 0.069(5) 0.090(5) -0.019(4) 0.010(3) 0.011(3) C5 0.077(5) 0.049(4) 0.108(6) -0.031(4) 0.019(5) 0.008(4) C6 0.056(4) 0.051(4) 0.094(6) -0.034(4) -0.002(4) 0.001(3) C7 0.050(3) 0.040(3) 0.054(4) -0.013(3) -0.003(3) 0.003(3) C8 0.039(3) 0.064(4) 0.066(4) -0.014(3) -0.003(3) -0.009(3) O4 0.050(3) 0.220(8) 0.072(4) -0.058(4) -0.004(3) -0.035(4) C9 0.039(3) 0.047(3) 0.054(4) -0.009(3) -0.001(3) -0.010(2) C10 0.053(4) 0.062(4) 0.068(5) 0.010(4) -0.004(3) -0.012(3) C11 0.076(5) 0.084(5) 0.060(5) 0.011(4) -0.001(4) -0.021(4) C12 0.090(6) 0.071(5) 0.067(5) -0.006(4) 0.026(4) -0.028(4) C13 0.050(4) 0.065(4) 0.076(5) -0.014(4) 0.010(3) -0.014(3) C14 0.048(4) 0.058(4) 0.060(4) -0.002(3) -0.002(3) -0.012(3) O5 0.0302(19) 0.048(2) 0.056(2) -0.0053(18) 0.0006(16) 0.0088(16) O6 0.0282(18) 0.059(2) 0.044(2) 0.0023(19) 0.0065(15) -0.0020(17) C15 0.023(2) 0.050(3) 0.034(3) -0.009(2) 0.0020(19) 0.002(2) C16 0.026(2) 0.055(3) 0.048(3) -0.002(3) 0.006(2) -0.004(2) C17 0.060(4) 0.081(5) 0.080(5) 0.031(4) 0.012(4) -0.012(4) C18 0.062(5) 0.140(9) 0.115(7) 0.060(6) 0.012(5) -0.038(5) C19 0.035(4) 0.179(10) 0.115(7) 0.054(7) 0.011(4) -0.029(5) C20 0.023(3) 0.137(8) 0.085(5) 0.027(5) 0.006(3) 0.001(4) C21 0.026(3) 0.078(4) 0.055(4) -0.009(3) 0.008(2) 0.000(3) C22 0.026(3) 0.059(4) 0.062(4) -0.008(3) -0.001(2) 0.012(3) O7 0.072(3) 0.077(3) 0.080(3) -0.031(3) -0.003(3) 0.021(3) C23 0.026(2) 0.053(3) 0.050(3) 0.001(3) -0.006(2) 0.005(2) C24 0.045(3) 0.051(3) 0.053(4) 0.000(3) -0.001(3) 0.004(3) C25 0.054(4) 0.080(5) 0.062(5) -0.013(4) -0.008(3) -0.007(4) C26 0.051(4) 0.115(7) 0.058(4) 0.013(5) 0.000(3) -0.010(4) C27 0.056(4) 0.075(5) 0.084(6) 0.034(4) -0.009(4) -0.006(4) C28 0.044(3) 0.058(4) 0.075(5) 0.005(4) 0.001(3) 0.003(3) O8 0.052(2) 0.036(2) 0.037(2) 0.0007(16) 0.0052(17) 0.0057(16) O9 0.049(2) 0.039(2) 0.0289(18) 0.0006(15) 0.0084(15) -0.0005(16) C29 0.030(2) 0.039(3) 0.025(2) 0.002(2) -0.0011(18) 0.0045(19) C30 0.032(2) 0.040(3) 0.029(3) 0.000(2) 0.0021(19) -0.003(2) C31 0.046(3) 0.044(3) 0.049(3) -0.001(3) 0.004(3) -0.009(2) C32 0.066(4) 0.056(4) 0.060(4) 0.016(3) 0.013(3) -0.021(3) C33 0.062(4) 0.070(4) 0.048(4) 0.009(3) 0.022(3) -0.013(3) C34 0.042(3) 0.068(4) 0.031(3) 0.002(3) 0.007(2) -0.003(3) C35 0.039(3) 0.040(3) 0.032(3) 0.004(2) 0.007(2) -0.002(2) C36 0.045(3) 0.040(3) 0.028(3) -0.004(2) 0.008(2) -0.002(2) O10 0.058(3) 0.052(2) 0.048(2) -0.0040(19) 0.005(2) -0.015(2) C37 0.060(4) 0.042(3) 0.023(3) -0.004(2) 0.006(2) 0.006(3) C38 0.089(5) 0.052(4) 0.038(3) -0.005(3) 0..013(3) 0.000(3) C39 0.117(7) 0.051(4) 0.047(4) 0.002(3) -0.004(4) 0.030(4) C40 0.094(6) 0.072(5) 0.049(4) -0.001(4) -0.015(4) 0.040(4) C41 0.058(4) 0.080(5) 0.041(3) -0.011(3) -0.011(3) 0.028(4) C42 0.054(3) 0.053(3) 0.035(3) -0.002(3) 0.006(2) 0.010(3) O11 0.059(3) 0.051(2) 0.048(2) 0.001(2) -0.0155(19) -0.004(2) O12 0.0317(19) 0.057(2) 0.059(3) -0.020(2) -0.0006(17) -0.0139(17) C43 0.028(2) 0.031(3) 0.048(3) -0.008(2) 0.000(2) 0.0084(19) C44 0.027(2) 0.030(2) 0.037(3) -0.006(2) -0.0067(19) -0.0009(19) C45 0.037(3) 0.040(3) 0.053(3) -0.005(3) 0.000(2) -0.011(2) C46 0.078(5) 0.044(3) 0.039(3) 0.004(3) -0.004(3) -0.004(3) C47 0.056(4) 0.061(4) 0.041(3) -0.007(3) -0.020(3) -0.002(3) C48 0.032(3) 0.045(3) 0.061(4) 0.000(3) -0.015(2) -0.007(2) C49 0.028(2) 0.036(3) 0.040(3) -0.004(2) -0.009(2) -0.003(2) C50 0.033(3) 0.049(3) 0.053(4) -0.005(3) -0.004(2) -0.012(2) O13 0.102(4) 0.058(3) 0.105(4) -0.013(3) 0.052(3) 0.007(3) C51 0.028(2) 0.050(3) 0.047(3) -0.001(3) -0.001(2) -0.012(2) C52 0.045(3) 0.052(4) 0.055(4) 0.008(3) 0.001(3) -0.008(3) C53 0.071(5) 0.048(4) 0.077(5) -0.003(3) 0.014(4) -0.009(3) C54 0.060(4) 0.052(4) 0.085(5) 0.015(4) -0.007(4) -0.016(3) C55 0.063(5) 0.089(6) 0.065(5) 0.018(4) 0.005(4) -0.030(4) C56 0.049(4) 0.069(4) 0.051(4) 0.001(3) 0.003(3) -0.016(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 O1 2.292(3) . ? Pb1 O2 2.401(3) . ? Pb1 O11 2.435(4) . ? Pb1 O5 2.513(3) . ? Pb1 O8 2.827(4) . ? Pb2 O1 2.249(3) . ? Pb2 O3 2.483(4) . ? Pb2 O8 2.532(3) . ? Pb2 O9 2.643(3) . ? Pb2 O12 2.673(4) 3_557 ? Pb2 O6 2.690(4) 3_557 ? Pb2 Pb3 3.6898(3) . ? Pb3 O1 2.319(3) . ? Pb3 O1 2.327(3) 3_557 ? Pb3 O12 2.519(4) 3_557 ? Pb3 O5 2.622(4) . ? Pb3 O6 2.720(3) . ? Pb3 Pb3 3.6840(3) 3_557 ? O1 Pb3 2.327(3) 3_557 ? O2 C1 1.267(6) . ? O3 C1 1.235(6) . ? C1 C2 1.502(7) . ? C2 C3 1.381(7) . ? C2 C7 1.393(8) . ? C3 C4 1.374(8) . ? C4 C5 1.358(10) . ? C5 C6 1.373(10) . ? C6 C7 1.365(8) . ? C7 C8 1.526(8) . ? C8 O4 1.200(8) . ? C8 C9 1.485(8) . ? C9 C10 1.381(8) . ? C9 C14 1.384(8) . ? C10 C11 1.395(9) . ? C11 C12 1.360(10) . ? C12 C13 1.397(10) . ? C13 C14 1.370(9) . ? O5 C15 1.261(6) . ? O6 C15 1.244(6) . ? O6 Pb2 2.690(4) 3_557 ? C15 C16 1.516(6) . ? C16 C21 1.379(8) . ? C16 C17 1.396(9) . ? C17 C18 1.351(10) . ? C18 C19 1.371(13) . ? C19 C20 1.365(12) . ? C20 C21 1.387(8) . ? C21 C22 1.498(9) . ? C22 O7 1.213(7) . ? C22 C23 1.496(8) . ? C23 C24 1.381(8) . ? C23 C28 1.386(8) . ? C24 C25 1.371(9) . ? C25 C26 1.388(11) . ? C26 C27 1.362(11) . ? C27 C28 1.361(10) . ? O8 C29 1.265(6) . ? O9 C29 1.266(6) . ? C29 C30 1.480(6) . ? C30 C31 1.385(7) . ? C30 C35 1.397(7) . ? C31 C32 1.388(8) . ? C32 C33 1.377(9) . ? C33 C34 1.378(8) . ? C34 C35 1.403(7) . ? C35 C36 1.514(7) . ? C36 O10 1.213(6) . ? C36 C37 1.488(8) . ? C37 C38 1.388(8) . ? C37 C42 1.389(8) . ? C38 C39 1.401(9) . ? C39 C40 1.378(11) . ? C40 C41 1.370(10) . ? C41 C42 1.414(8) . ? O11 C43 1.265(6) . ? O12 C43 1.268(6) . ? O12 Pb3 2.519(4) 3_557 ? O12 Pb2 2.673(4) 3_557 ? C43 C44 1.482(7) . ? C44 C45 1.397(7) . ? C44 C49 1.399(6) . ? C45 C46 1.391(8) . ? C46 C47 1.374(8) . ? C47 C48 1.380(8) . ? C48 C49 1.403(7) . ? C49 C50 1.501(7) . ? C50 O13 1.213(7) . ? C50 C51 1.466(8) . ? C51 C52 1.386(8) . ? C51 C56 1.387(8) . ? C52 C53 1.393(8) . ? C53 C54 1.353(10) .. ? C54 C55 1.348(10) . ? C55 C56 1.370(10) . ? 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 O1 Pb1 O2 79.71(12) . . ? O1 Pb1 O11 108.83(12) . . ? O2 Pb1 O11 80.30(14) . . ? O1 Pb1 O5 76.69(11) . . ? O2 Pb1 O5 145.27(13) . . ? O11 Pb1 O5 83.62(13) . . ? O1 Pb1 O8 72.09(10) . . ? O2 Pb1 O8 100.97(11) . . ? O11 Pb1 O8 178.59(12) . . ? O5 Pb1 O8 95.61(11) . . ? O1 Pb2 O3 82.19(11) . . ? O1 Pb2 O8 78.81(11) . . ? O3 Pb2 O8 78.77(13) . . ? O1 Pb2 O9 75.91(11) . . ? O3 Pb2 O9 127.42(13) . . ? O8 Pb2 O9 50.52(11) . . ? O1 Pb2 O12 71.86(11) . 3_557 ? O3 Pb2 O12 142.79(12) . 3_557 ? O8 Pb2 O12 120.03(11) . 3_557 ? O9 Pb2 O12 71.86(11) . 3_557 ? O1 Pb2 O6 80.70(10) . 3_557 ? O3 Pb2 O6 78.50(13) . 3_557 ? O8 Pb2 O6 151.14(12) . 3_557 ? O9 Pb2 O6 141.07(11) . 3_557 ? O12 Pb2 O6 71.48(12) 3_557 3_557 ? O1 Pb2 Pb3 36.77(7) . . ? O3 Pb2 Pb3 118.80(9) . . ? O8 Pb2 Pb3 83.88(8) . . ? O9 Pb2 Pb3 51.71(8) . . ? O12 Pb2 Pb3 43.05(8) 3_557 . ? O6 Pb2 Pb3 91.71(8) 3_557 . ? O1 Pb3 O1 75.06(11) . 3_557 ? O1 Pb3 O12 73.78(11) . 3_557 ? O1 Pb3 O12 80.63(12) 3_557 3_557 ? O1 Pb3 O5 74.09(10) . . ? O1 Pb3 O5 107.48(11) 3_557 . ? O12 Pb3 O5 143.32(12) 3_557 . ? O1 Pb3 O6 103.50(11) . . ? O1 Pb3 O6 78.75(10) 3_557 . ? O12 Pb3 O6 159.17(12) 3_557 . ? O5 Pb3 O6 48.74(12) . . ? O1 Pb3 Pb3 37.60(7) . 3_557 ? O1 Pb3 Pb3 37.46(7) 3_557 3_557 ? O12 Pb3 Pb3 73.82(9) 3_557 3_557 ? O5 Pb3 Pb3 90.98(8) . 3_557 ? O6 Pb3 Pb3 91.36(8) . 3_557 ? O1 Pb3 Pb2 35.50(7) . . ? O1 Pb3 Pb2 93.28(7) 3_557 . ? O12 Pb3 Pb2 46.42(9) 3_557 . ? O5 Pb3 Pb2 96.94(8) . . ? O6 Pb3 Pb2 137.81(9) . . ? Pb3 Pb3 Pb2 61.551(6) 3_557 . ? Pb2 O1 Pb1 110.70(12) . . ? Pb2 O1 Pb3 107.73(11) . . ? Pb1 O1 Pb3 112.30(12) . . ? Pb2 O1 Pb3 111.07(12) . 3_557 ? Pb1 O1 Pb3 109.94(11) . 3_557 ? Pb3 O1 Pb3 104.94(11) . 3_557 ? C1 O2 Pb1 116.8(3) . . ? C1 O3 Pb2 139.0(3) . . ? O3 C1 O2 125.3(5) . . ? O3 C1 C2 118.5(5) . . ? O2 C1 C2 116.2(5) . . ? C3 C2 C7 119.2(5) . . ? C3 C2 C1 119.2(5) . . ? C7 C2 C1 121.5(5) . . ? C4 C3 C2 120.1(5) . . ? C5 C4 C3 120.5(6) . . ? C4 C5 C6 119.6(6) . . ? C7 C6 C5 121.2(6) . . ? C6 C7 C2 119.2(6) . . ? C6 C7 C8 116.9(5) . . ? C2 C7 C8 123.9(5) . . ? O4 C8 C9 120.3(6) . . ? O4 C8 C7 120.0(6) . . ? C9 C8 C7 119.6(5) . . ? C10 C9 C14 117.9(6) . . ? C10 C9 C8 123.0(6) . . ? C14 C9 C8 119.0(6) . . ? C9 C10 C11 120.8(7) . . ? C12 C11 C10 120.6(7) . . ? C11 C12 C13 119.1(7) . . ? C14 C13 C12 120.0(6) . . ? C13 C14 C9 121.7(6) . . ? C15 O5 Pb1 136.8(3) . . ? C15 O5 Pb3 94.9(3) . . ? Pb1 O5 Pb3 96.42(12) . . ? C15 O6 Pb2 140.7(3) . 3_557 ? C15 O6 Pb3 90.7(3) . . ? Pb2 O6 Pb3 88.44(10) 3_557 . ? O6 C15 O5 123.4(4) . . ? O6 C15 C16 118.2(5) . . ? O5 C15 C16 118.3(5) . . ? C21 C16 C17 120.0(5) . . ? C21 C16 C15 120.5(5) . . ? C17 C16 C15 119.4(5) . . ? C18 C17 C16 121.5(8) . . ? C17 C18 C19 118.5(8) . . ? C20 C19 C18 121.2(6) . . ? C19 C20 C21 121.1(7) . . ? C16 C21 C20 117.7(6) . . ? C16 C21 C22 124.9(5) . . ? C20 C21 C22 117.5(6) . . ? O7 C22 C23 122.6(6) . . ? O7 C22 C21 119.2(6) . . ? C23 C22 C21 118.0(5) . . ? C24 C23 C28 119.9(6) . . ? C24 C23 C22 120.4(6) . . ? C28 C23 C22 119.5(6) . . ? C25 C24 C23 119.6(6) . . ? C24 C25 C26 120.1(7) . . ? C27 C26 C25 119.7(7) . . ? C28 C27 C26 121.0(7) . . ? C27 C28 C23 119.7(7) . . ? C29 O8 Pb2 95.8(3) . . ? C29 O8 Pb1 108.6(3) . . ? Pb2 O8 Pb1 88.23(10) . . ? C29 O9 Pb2 90.6(3) . . ? O8 C29 O9 121.8(4) . . ? O8 C29 C30 119.1(4) . . ? O9 C29 C30 119.1(4) . . ? C31 C30 C35 118.9(5) . . ? C31 C30 C29 120.2(5) . . ? C35 C30 C29 120.8(4) . . ? C30 C31 C32 121.4(6) . . ? C33 C32 C31 119.4(6) . . ? C32 C33 C34 120.7(5) . . ? C33 C34 C35 119.9(6) . . ? C30 C35 C34 119.7(5) . . ? C30 C35 C36 123.4(4) . . ? C34 C35 C36 116.9(5) . . ? O10 C36 C37 119.8(5) . . ? O10 C36 C35 119.5(5) . . ? C37 C36 C35 120.3(5) . . ? C38 C37 C42 119.9(6) . . ? C38 C37 C36 119.3(6) . . ? C42 C37 C36 120.8(5) . . ? C37 C38 C39 119.7(7) . . ? C40 C39 C38 120.2(7) . . ? C41 C40 C39 120.9(7) . . ? C40 C41 C42 119.5(7) . . ? C37 C42 C41 119.8(6) . . ? C43 O11 Pb1 117.9(3) . . ? C43 O12 Pb3 133.0(3) . 3_557 ? C43 O12 Pb2 134.3(3) . 3_557 ? Pb3 O12 Pb2 90.53(11) 3_557 3_557 ? O11 C43 O12 121.2(5) . . ? O11 C43 C44 118.6(5) . . ? O12 C43 C44 120.0(5) . . ? C45 C44 C49 120.3(4) . . ? C45 C44 C43 118.8(4) . . ? C49 C44 C43 120.8(4) . . ? C46 C45 C44 120.8(5) . . ? C47 C46 C45 119.0(6) . . ? C46 C47 C48 120.7(5) . . ? C47 C48 C49 121.5(5) . . ? C44 C49 C48 117.7(5) . . ? C44 C49 C50 122.6(4) . . ? C48 C49 C50 119.5(4) . . ? O13 C50 C51 122.3(5) . . ? O13 C50 C49 118.4(5) . . ? C51 C50 C49 119.2(5) . . ? C52 C51 C56 118.4(6) . . ? C52 C51 C50 121.6(5) . . ? C56 C51 C50 120.0(5) . . ? C51 C52 C53 120.1(6) . . ? C54 C53 C52 119.7(7) . . ? C55 C54 C53 120.7(7) . . ? C54 C55 C56 120.9(7) . . ? C55 C56 C51 120.1(7) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 32.52 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.946 _refine_diff_density_min -1.145 _refine_diff_density_rms 0.201 data_cent _database_code_CSD 158367 _publ_requested_journal test _audit_creation_method SHELXL-97 _chemical_name_systematic 'C12 Cl18 O15 Pb3' _chemical_name_common 'C12 Cl18 O15 Pb3' _chemical_formula_moiety 'C12 Cl18 O15 Pb3' _chemical_formula_sum 'C12 Cl18 O15 Pb3' _chemical_formula_weight 1643.79 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' 'Cl' 'Cl' 0.1484 0.1585 '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' '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 11.2919(12) _cell_length_b 11.9710(14) _cell_length_c 16.0512(16) _cell_angle_alpha 70.171(4) _cell_angle_beta 75.406(5) _cell_angle_gamma 74.713(2) _cell_volume 1937.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 17154 _cell_measurement_theta_min 1.95 _cell_measurement_theta_max 30.10 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.818 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1488 _exptl_absorpt_coefficient_mu 14.303 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_process_details '(SADABS; Sheldrick, 1997)' _exptl_absorpt_correction_T_min 0.507 _exptl_absorpt_correction_T_max 0.928 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'SMART area CCD' _diffrn_measurement_method /f-/w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 17154 _diffrn_reflns_av_R_equivalents 0.0556 _diffrn_reflns_av_sigmaI/netI 0.1310 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 30.10 _reflns_number_total 11077 _reflns_number_gt 5489 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortex in OSCAIL (McArdle, 1995)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0899P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11077 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1409 _refine_ls_R_factor_gt 0.0657 _refine_ls_wR_factor_ref 0.1734 _refine_ls_wR_factor_gt 0.1474 _refine_ls_goodness_of_fit_ref 0.882 _refine_ls_restrained_S_all 0.882 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.21042(5) 0.44007(5) 0.47807(3) 0.03693(15) Uani 1 d . . . O1 O 0.3791(10) 0.4304(12) 0.3436(8) 0.071(4) Uani 1 d . . . C1 C 0.4852(14) 0.4507(13) 0.3085(11) 0.049(4) Uani 1 d . . . O2 O 0.5452(12) 0.5106(11) 0.3291(8) 0.068(3) Uani 1 d . . . C2 C 0.5507(15) 0.4004(14) 0.2301(11) 0.051(4) Uani 1 d . . . Cl1A Cl 0.7090(4) 0.3760(6) 0.2155(4) 0.094(2) Uani 1 d . . . Cl1B Cl 0.5063(5) 0.2671(5) 0.2392(4) 0.0874(16) Uani 1 d . . . Cl1C Cl 0.5006(7) 0.5108(5) 0.1311(4) 0.111(2) Uani 1 d . . . O3 O 0.0129(9) 0.5852(9) 0.5435(6) 0.044(2) Uani 1 d . . . C3 C 0.0627(14) 0.5954(11) 0.6001(8) 0.033(3) Uani 1 d . . . O4 O 0.1697(10) 0.5488(9) 0.6117(7) 0.047(2) Uani 1 d . . . C4 C -0.0143(14) 0.6849(13) 0.6546(11) 0.046(4) Uani 1 d . . . Cl2A Cl 0.0143(5) 0.6238(5) 0.7666(3) 0.0763(14) Uani 1 d . . . Cl2B Cl 0.0372(6) 0.8220(4) 0.6050(4) 0.0955(19) Uani 1 d . . . Cl2C Cl -0.1752(4) 0.7061(5) 0.6603(3) 0.0734(14) Uani 1 d . . . O1W O 0.1526(10) 0.6146(10) 0.3587(7) 0.063(3) Uani 1 d . . . O2W O 0.3699(13) 0.5600(13) 0.4684(9) 0.087(4) Uani 1 d . . . Pb2 Pb 0.27632(5) 0.37174(5) 0.73623(3) 0.03706(15) Uani 1 d . . . O5 O 0.4756(9) 0.2248(8) 0.7132(6) 0.040(2) Uani 1 d . . . C5 C 0.4697(13) 0.2342(12) 0.6324(8) 0.032(3) Uani 1 d . . . O6 O 0.3884(9) 0.3092(8) 0.5938(6) 0.043(2) Uani 1 d . . . C6 C 0.5655(16) 0.1547(15) 0.5864(10) 0.054(4) Uani 1 d . . . Cl3A Cl 0.5244(8) 0.0075(6) 0.6316(6) 0.149(3) Uani 1 d . . . Cl3B Cl 0.7136(6) 0.1246(9) 0.6157(5) 0.146(3) Uani 1 d . . . Cl3C Cl 0.5785(8) 0.1926(6) 0.4730(3) 0.128(3) Uani 1 d . . . O7 O 0.2233(9) 0.1680(9) 0.7605(7) 0.050(3) Uani 1 d . . . C7 C 0.1513(14) 0.1928(13) 0.7076(9) 0.040(3) Uani 1 d . . . O8 O 0.1038(9) 0.2973(8) 0.6632(7) 0.047(2) Uani 1 d . . . C8 C 0.1250(14) 0.0839(12) 0.6855(10) 0.045(4) Uani 1 d . . . Cl4A Cl 0.1820(7) -0.0546(4) 0.7572(6) 0.143(4) Uani 1 d . . . Cl4B Cl 0.1912(9) 0.0877(8) 0.5767(5) 0.152(3) Uani 1 d . . . Cl4C Cl -0.0350(5) 0.0966(5) 0.6993(5) 0.107(2) Uani 1 d . . . O9 O 0.3643(10) 0.2513(9) 0.8862(6) 0.050(3) Uani 1 d . . . C9 C 0.3452(13) 0.1969(12) 0.9679(9) 0.038(3) Uani 1 d . . . O10 O 0.4128(10) 0.1001(9) 1.0031(7) 0.052(3) Uani 1 d . . . C10 C 0.2369(16) 0.2515(14) 1.0289(10) 0.053(4) Uani 1 d . . . Cl5A Cl 0.1281(5) 0.3659(5) 0.9705(4) 0.103(2) Uani 1 d . . . Cl5B Cl 0.1554(5) 0.1417(5) 1.1064(4) 0.0918(17) Uani 1 d . . . Cl5C Cl 0.3017(6) 0.3139(7) 1.0866(4) 0.114(2) Uani 1 d . . . Pb3 Pb 0.56282(5) 0.08272(5) 0.85836(3) 0.04018(15) Uani 1 d . . . O11 O 0.6615(13) 0.1513(12) 0.9463(7) 0.078(4) Uani 1 d . . . C11 C 0.7261(15) 0.2203(13) 0.8874(10) 0.048(4) Uani 1 d . . . O12 O 0.7192(11) 0.2534(10) 0.8084(7) 0.059(3) Uani 1 d . . . C12 C 0.8207(15) 0.2613(14) 0.9219(10) 0.051(4) Uani 1 d . . . Cl6A Cl 0.8727(7) 0.3869(6) 0.8441(4) 0.111(2) Uani 1 d . . . Cl6B Cl 0.7538(8) 0.2959(7) 1.0212(4) 0.129(3) Uani 1 d . . . Cl6C Cl 0.9452(7) 0.1404(7) 0.9374(7) 0.141(3) Uani 1 d . . . O3W O 0.3847(10) -0.0167(11) 0.8715(7) 0.062(3) Uani 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 0.0443(3) 0.0335(3) 0.0330(3) -0.0128(2) -0.0100(2) -0.0005(2) O1 0.037(7) 0.097(10) 0.082(9) -0.039(8) 0.008(6) -0.017(6) C1 0.041(9) 0.035(8) 0.063(10) -0.011(7) -0.002(8) -0.003(7) O2 0.084(9) 0.063(8) 0.059(7) -0.035(6) 0.020(6) -0.028(7) C2 0.053(10) 0.042(9) 0.070(10) -0.030(8) -0.004(8) -0.016(7) Cl1A 0.049(3) 0.125(5) 0.151(5) -0.109(4) 0.005(3) -0.017(3) Cl1B 0.100(4) 0.063(3) 0.118(4) -0.041(3) -0.010(3) -0.036(3) Cl1C 0.160(6) 0.068(4) 0.078(4) -0.006(3) -0.033(4) 0.015(4) O3 0.050(6) 0.044(6) 0.047(6) -0.025(5) -0.010(5) -0.005(5) C3 0.051(9) 0.024(6) 0.034(7) -0.015(5) -0.007(6) -0.014(6) O4 0.051(7) 0.032(5) 0.058(6) -0.013(5) -0.019(5) 0.002(5) C4 0.046(9) 0.044(9) 0.065(10) -0.033(8) -0.022(8) -0.003(7) Cl2A 0.072(3) 0.117(4) 0.049(2) -0.042(3) -0.010(2) -0.012(3) Cl2B 0.121(5) 0.047(3) 0.127(5) -0.044(3) 0.007(4) -0.031(3) Cl2C 0.044(2) 0.103(4) 0.095(3) -0.068(3) -0.015(2) 0.003(2) O1W 0.062(8) 0.041(6) 0.057(7) 0.012(5) -0.015(6) 0.008(5) O2W 0.098(11) 0.086(10) 0.093(10) -0.036(8) -0.002(8) -0.050(9) Pb2 0.0502(3) 0.0289(3) 0.0331(3) -0.0114(2) -0.0123(2) -0.0017(2) O5 0.058(6) 0.031(5) 0.030(5) -0.008(4) -0.019(4) 0.002(4) C5 0.042(8) 0.031(7) 0.022(6) -0.003(5) -0.010(6) -0.010(6) O6 0.059(7) 0.038(6) 0.036(5) -0.010(4) -0.023(5) -0.002(5) C6 0.068(11) 0.054(10) 0.039(8) -0.011(7) -0.014(8) -0.009(8) Cl3A 0.190(8) 0.060(4) 0.182(8) -0.053(4) 0.040(6) -0.043(4) Cl3B 0.070(4) 0.240(10) 0.149(6) -0.123(7) -0.032(4) 0.035(5) Cl3C 0.207(8) 0.102(5) 0.050(3) -0.042(3) -0.037(4) 0.050(5) O7 0.045(6) 0.041(6) 0.075(7) -0.018(5) -0.028(6) -0.012(5) C7 0.051(9) 0.037(8) 0.041(8) -0.012(6) -0.013(7) -0.018(7) O8 0.047(6) 0.022(5) 0.068(7) -0.014(5) -0.013(5) 0.006(4) C8 0.064(10) 0.022(7) 0.059(9) -0.014(6) -0.030(8) -0.003(6) Cl4A 0.189(7) 0.027(2) 0.251(9) -0.003(4) -0.169(7) -0.007(3) Cl4B 0.224(9) 0.148(7) 0.125(6) -0.104(6) 0.028(6) -0.076(7) Cl4C 0.061(3) 0.058(3) 0.220(8) -0.045(4) -0.049(4) -0.013(2) O9 0.078(8) 0.036(6) 0.025(5) -0.008(4) -0.008(5) 0.006(5) C9 0.038(8) 0.033(7) 0.036(7) -0.006(6) -0.011(6) 0.001(6) O10 0.057(7) 0.046(6) 0.041(6) -0.005(5) -0.009(5) -0.001(5) C10 0.073(11) 0.043(9) 0.050(9) -0.018(7) 0.004(8) -0.033(8) Cl5A 0.078(4) 0.076(4) 0.107(4) -0.008(3) -0.011(3) 0.035(3) Cl5B 0.080(4) 0.069(3) 0.097(4) -0.007(3) 0.018(3) -0.020(3) Cl5C 0.111(5) 0.168(7) 0.118(5) -0.115(5) 0.005(4) -0.045(4) Pb3 0.0467(3) 0.0403(3) 0.0294(3) -0.0072(2) -0.0098(2) -0.0026(2) O11 0.104(11) 0.093(10) 0.043(6) -0.004(6) -0.009(7) -0.055(9) C11 0.057(10) 0.036(8) 0.044(9) -0.013(7) 0.003(8) -0.006(7) O12 0.076(8) 0.063(8) 0.042(6) -0.017(5) -0.003(6) -0.027(6) C12 0.062(11) 0.049(9) 0.049(9) -0.018(7) -0.002(8) -0.026(8) Cl6A 0.155(6) 0.112(5) 0.087(4) -0.006(3) -0.026(4) -0.087(5) Cl6B 0.196(8) 0.157(7) 0.075(4) -0.074(4) 0.016(4) -0.090(6) Cl6C 0.111(5) 0.112(6) 0.229(9) -0.070(6) -0.107(6) 0.027(4) O3W 0.040(6) 0.082(9) 0.053(7) 0.008(6) -0.021(5) -0.019(6) _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 2.379(9) . ? Pb1 O1 2.507(11) . ? Pb1 O2W 2.529(12) . ? Pb1 O3 2.667(10) . ? Pb1 O3 2.735(10) 2_566 ? Pb1 O4 2.755(10) . ? O1 C1 1.237(17) . ? C1 O2 1.269(19) . ? C1 C2 1.52(2) . ? O2 Pb2 2.564(12) 2_666 ? C2 Cl1A 1.702(16) . ? C2 Cl1B 1.745(14) . ? C2 Cl1C 1.796(18) . ? O3 C3 1.236(15) . ? O3 Pb1 2.735(10) 2_566 ? C3 O4 1.222(16) . ? C3 C4 1.559(18) . ? O4 Pb2 2.632(10) . ? C4 Cl2B 1.746(15) . ? C4 Cl2C 1.751(15) . ? C4 Cl2A 1.773(16) . ? Pb2 O5 2.496(9) . ? Pb2 O7 2.543(9) . ? Pb2 O2 2.564(12) 2_666 ? Pb2 O6 2.568(9) . ? Pb2 O9 2.638(9) . ? O5 C5 1.280(14) . ? O5 Pb3 2.622(8) . ? C5 O6 1.228(15) . ? C5 C6 1.47(2) . ? C6 Cl3C 1.697(15) . ? C6 Cl3B 1.764(18) . ? C6 Cl3A 1.800(17) . ? O7 C7 1.233(16) . ? C7 O8 1.263(17) . ? C7 C8 1.575(18) . ? C8 Cl4B 1.708(16) . ? C8 Cl4A 1.733(14) . ? C8 Cl4C 1.736(16) . ? O9 C9 1.242(15) . ? O9 Pb3 2.649(10) . ? C9 O10 1.245(16) . ? C9 C10 1.51(2) . ? O10 Pb3 2.543(10) . ? O10 Pb3 2.550(10) 2_657 ? C10 Cl5C 1.747(15) . ? C10 Cl5B 1.753(14) . ? C10 Cl5A 1.756(19) . ? Pb3 O11 2.443(12) . ? Pb3 O3W 2.527(10) . ? Pb3 O10 2.550(10) 2_657 ? O11 C11 1.244(17) . ? C11 O12 1.209(17) . ? C11 C12 1.56(2) . ? C12 Cl6B 1.719(16) . ? C12 Cl6A 1.729(15) . ? C12 Cl6C 1.730(18) . ? 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 O1 73.4(4) . . ? O1W Pb1 O2W 80.6(5) . . ? O1 Pb1 O2W 70.0(4) . . ? O1W Pb1 O3 71.0(3) . . ? O1 Pb1 O3 143.5(4) . . ? O2W Pb1 O3 96.1(4) . . ? O1W Pb1 O3 76.1(4) . 2_566 ? O1 Pb1 O3 112.8(3) . 2_566 ? O2W Pb1 O3 154.2(4) . 2_566 ? O3 Pb1 O3 66.0(3) . 2_566 ? O1W Pb1 O4 99.0(4) . . ? O1 Pb1 O4 133.4(4) . . ? O2W Pb1 O4 63.4(4) . . ? O3 Pb1 O4 47.5(3) . . ? O3 Pb1 O4 109.4(3) 2_566 . ? C1 O1 Pb1 143.0(11) . . ? O1 C1 O2 127.8(16) . . ? O1 C1 C2 116.3(14) . . ? O2 C1 C2 115.9(13) . . ? C1 O2 Pb2 141.7(10) . 2_666 ? C1 C2 Cl1A 113.1(11) . . ? C1 C2 Cl1B 112.4(11) . . ? Cl1A C2 Cl1B 109.1(9) . . ? C1 C2 Cl1C 106.6(11) . . ? Cl1A C2 Cl1C 108.9(9) . . ? Cl1B C2 Cl1C 106.5(9) . . ? C3 O3 Pb1 95.5(8) . . ? C3 O3 Pb1 141.1(9) . 2_566 ? Pb1 O3 Pb1 114.0(3) . 2_566 ? O4 C3 O3 125.5(13) . . ? O4 C3 C4 117.8(11) . . ? O3 C3 C4 116.5(13) . . ? C3 O4 Pb2 135.9(9) . . ? C3 O4 Pb1 91.6(8) . . ? Pb2 O4 Pb1 101.2(3) . . ? C3 C4 Cl2B 108.1(10) . . ? C3 C4 Cl2C 112.6(9) . . ? Cl2B C4 Cl2C 111.1(9) . . ? C3 C4 Cl2A 108.6(10) . . ? Cl2B C4 Cl2A 109.2(7) . . ? Cl2C C4 Cl2A 107.2(9) . . ? O5 Pb2 O7 71.8(3) . . ? O5 Pb2 O2 71.6(3) . 2_666 ? O7 Pb2 O2 142.3(3) . 2_666 ? O5 Pb2 O6 51.1(3) . . ? O7 Pb2 O6 74.5(3) . . ? O2 Pb2 O6 75.5(3) 2_666 . ? O5 Pb2 O4 127.3(3) . . ? O7 Pb2 O4 113.5(3) . . ? O2 Pb2 O4 82.1(4) 2_666 . ? O6 Pb2 O4 78.7(3) . . ? O5 Pb2 O9 66.9(3) . . ? O7 Pb2 O9 81.4(3) . . ? O2 Pb2 O9 92.8(4) 2_666 . ? O6 Pb2 O9 117.6(3) . . ? O4 Pb2 O9 161.2(3) . . ? C5 O5 Pb2 94.6(8) . . ? C5 O5 Pb3 144.8(8) . . ? Pb2 O5 Pb3 116.6(3) . . ? O6 C5 O5 121.3(13) . . ? O6 C5 C6 120.9(12) . . ? O5 C5 C6 117.8(12) . . ? C5 O6 Pb2 92.6(7) . . ? C5 C6 Cl3C 116.6(12) . . ? C5 C6 Cl3B 113.6(11) . . ? Cl3C C6 Cl3B 110.4(10) . . ? C5 C6 Cl3A 106.3(11) . . ? Cl3C C6 Cl3A 106.6(9) . . ? Cl3B C6 Cl3A 101.8(9) . . ? C7 O7 Pb2 102.9(8) . . ? O7 C7 O8 126.7(13) . . ? O7 C7 C8 117.2(13) . . ? O8 C7 C8 115.8(12) . . ? C7 C8 Cl4B 109.8(10) . . ? C7 C8 Cl4A 111.9(10) . . ? Cl4B C8 Cl4A 109.5(9) . . ? C7 C8 Cl4C 109.2(10) . . ? Cl4B C8 Cl4C 109.1(9) . . ? Cl4A C8 Cl4C 107.3(8) . . ? C9 O9 Pb2 149.3(10) . . ? C9 O9 Pb3 91.1(8) . . ? Pb2 O9 Pb3 110.9(3) . . ? O9 C9 O10 123.2(13) . . ? O9 C9 C10 119.0(13) . . ? O10 C9 C10 117.8(13) . . ? C9 O10 Pb3 96.0(8) . . ? C9 O10 Pb3 146.6(9) . 2_657 ? Pb3 O10 Pb3 116.4(4) . 2_657 ? C9 C10 Cl5C 106.1(11) . . ? C9 C10 Cl5B 111.7(11) . . ? Cl5C C10 Cl5B 109.5(9) . . ? C9 C10 Cl5A 113.5(11) . . ? Cl5C C10 Cl5A 108.7(9) . . ? Cl5B C10 Cl5A 107.3(9) . . ? O11 Pb3 O3W 142.1(4) . . ? O11 Pb3 O10 70.7(4) . . ? O3W Pb3 O10 73.0(4) . . ? O11 Pb3 O10 77.4(4) . 2_657 ? O3W Pb3 O10 77.2(3) . 2_657 ? O10 Pb3 O10 63.6(4) . 2_657 ? O11 Pb3 O5 123.6(4) . . ? O3W Pb3 O5 80.8(3) . . ? O10 Pb3 O5 113.0(3) . . ? O10 Pb3 O5 157.7(3) 2_657 . ? O11 Pb3 O9 87.2(4) . . ? O3W Pb3 O9 77.5(4) . . ? O10 Pb3 O9 49.8(3) . . ? O10 Pb3 O9 112.9(3) 2_657 . ? O5 Pb3 O9 65.0(3) . . ? C11 O11 Pb3 103.0(10) . . ? O12 C11 O11 123.5(16) . . ? O12 C11 C12 121.2(14) . . ? O11 C11 C12 115.3(14) . . ? C11 C12 Cl6B 111.0(11) . . ? C11 C12 Cl6A 111.5(11) . . ? Cl6B C12 Cl6A 108.4(9) . . ? C11 C12 Cl6C 105.8(10) . . ? Cl6B C12 Cl6C 110.8(10) . . ? Cl6A C12 Cl6C 109.4(9) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 30.10 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 4.827 _refine_diff_density_min -3.830 _refine_diff_density_rms 0.344 data_js070 _database_code_CSD 158368 _publ_requested_journal test _audit_creation_method SHELXL-97 _chemical_name_systematic 'C14 H10 N2 O9 Pb' _chemical_name_common 'C14 H10 N2 O9 Pb' _chemical_formula_moiety 'C14 H10 N2 O9 Pb' _chemical_formula_sum 'C14 H10 N2 O9 Pb' _chemical_formula_weight 557.43 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' 'O' 'O' 0.0106 0.0060 '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' '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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, -z-1/2' _cell_length_a 12.5336(8) _cell_length_b 7.1979(5) _cell_length_c 18.7487(12) _cell_angle_alpha 90.00 _cell_angle_beta 102.7720(10) _cell_angle_gamma 90.00 _cell_volume 1649.57(19) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2885 _cell_measurement_theta_min 3.041 _cell_measurement_theta_max 25.449 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.245 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 10.281 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_process_details '(SADABS; Bruker, 1999)' _exptl_absorpt_correction_T_min 0.3483 _exptl_absorpt_correction_T_max 0.6839 _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 SMART area CCD detector' _diffrn_measurement_method /f-/w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 16278 _diffrn_reflns_av_R_equivalents 0.0691 _diffrn_reflns_av_sigmaI/netI 0.1143 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 32.51 _reflns_number_total 5907 _reflns_number_gt 3177 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortex in OSCAIL (McArdle, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0217P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patterson _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 5907 _refine_ls_number_parameters 243 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1113 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.0738 _refine_ls_wR_factor_gt 0.0623 _refine_ls_goodness_of_fit_ref 0.848 _refine_ls_restrained_S_all 0.848 _refine_ls_shift/su_max 0.000 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.22383(2) 0.01973(2) 0.182647(12) 0.03278(7) Uani 1 d . . . O1 O 0.2230(4) -0.1214(5) 0.2997(2) 0.0404(12) Uani 1 d . . . O2 O 0.2214(4) 0.1775(5) 0.3182(2) 0.0497(14) Uani 1 d . . . C1 C 0.2284(4) 0.0169(7) 0.3420(3) 0.0301(12) Uani 1 d . . . C2 C 0.2553(5) -0.0186(6) 0.4231(3) 0.0296(12) Uani 1 d . . . C3 C 0.1861(5) 0.0284(7) 0.4691(3) 0.0332(13) Uani 1 d . . . N1 N 0.0762(5) 0.0992(7) 0.4384(3) 0.0413(13) Uani 1 d . . . O3 O 0.0324(4) 0.0521(8) 0.3769(3) 0.0740(16) Uani 1 d . . . O4 O 0.0320(4) 0.1940(6) 0.4774(3) 0.0610(14) Uani 1 d . . . C4 C 0.2177(5) 0.0038(8) 0.5450(3) 0.0432(15) Uani 1 d . . . H4 H 0.1716 0.0376 0.5754 0.052 Uiso 1 calc R . . C5 C 0.3186(6) -0.0715(8) 0.5728(3) 0.0428(17) Uani 1 d . . . H5 H 0.3404 -0.0902 0.6230 0.051 Uiso 1 calc R . . C6 C 0.3886(6) -0.1203(8) 0.5291(4) 0.0429(17) Uani 1 d . . . H6 H 0.4569 -0.1703 0.5497 0.051 Uiso 1 calc R . . C7 C 0.3573(5) -0.0947(7) 0.4543(3) 0.0356(14) Uani 1 d . . . H7 H 0.4045 -0.1285 0.4245 0.043 Uiso 1 calc R . . O5 O 0.0357(4) -0.1262(5) 0.1616(3) 0.0491(13) Uani 1 d . . . O6 O 0.0325(4) 0.1769(5) 0.1764(3) 0.0570(15) Uani 1 d . . . C8 C -0.0148(5) 0.0238(8) 0.1648(3) 0.0415(15) Uani 1 d . . . C9 C -0.1354(5) 0.0105(7) 0.1598(3) 0.0396(14) Uani 1 d . . . C10 C -0.2173(5) 0.0228(7) 0.0960(3) 0.0383(14) Uani 1 d . . . N2 N -0.1877(6) 0.0549(7) 0.0263(3) 0.0515(16) Uani 1 d . . . O7 O -0.0945(5) 0.0943(8) 0.0250(3) 0.0708(16) Uani 1 d . . . O8 O -0.2612(5) 0.0346(8) -0.0294(3) 0.0742(16) Uani 1 d . . . C11 C -0.3267(6) 0.0008(9) 0.0978(4) 0.0547(17) Uani 1 d . . . H11 H -0.3803 0.0112 0.0549 0.066 Uiso 1 calc R . . C12 C -0.3557(7) -0.0358(11) 0.1620(5) 0.071(2) Uani 1 d . . . H12 H -0.4291 -0.0505 0.1629 0.085 Uiso 1 calc R . . C13 C -0.2779(8) -0.0510(12) 0.2250(5) 0.079(3) Uani 1 d . . . H13 H -0.2983 -0.0782 0.2686 0.095 Uiso 1 calc R . . C14 C -0.1704(7) -0.0266(10) 0.2246(4) 0.063(2) Uani 1 d . . . H14 H -0.1186 -0.0347 0.2684 0.075 Uiso 1 calc R . . O9 O 0.4339(4) 0.0268(7) 0.2538(3) 0.0516(12) Uani 1 d . . . H9WA H 0.448(6) 0.122(8) 0.274(4) 0.04(2) Uiso 1 d . . . H9WB H 0.445(8) -0.066(12) 0.284(5) 0.12(4) Uiso 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 0.04030(14) 0.02666(9) 0.03170(11) 0.00075(11) 0.00864(9) -0.00062(12) O1 0.060(4) 0.0324(18) 0.026(2) -0.0023(16) 0.003(2) 0.0035(19) O2 0.082(4) 0.0293(18) 0.036(3) 0.0078(17) 0.010(3) -0.005(2) C1 0.027(3) 0.031(2) 0.033(3) -0.001(2) 0.008(2) -0.003(2) C2 0.033(3) 0.026(2) 0.032(3) -0.001(2) 0.011(2) -0.011(3) C3 0.031(3) 0.037(3) 0.031(3) 0.003(2) 0.005(3) 0.001(3) N1 0.033(4) 0.053(3) 0.037(3) 0.002(2) 0.007(3) -0.002(3) O3 0.044(3) 0.126(4) 0.046(3) -0.013(3) -0.003(3) 0.017(3) O4 0.051(4) 0.071(3) 0.065(4) -0.010(3) 0.021(3) 0.014(3) C4 0.052(4) 0.050(3) 0.029(3) 0.004(3) 0.012(3) -0.002(3) C5 0.054(5) 0.044(3) 0.025(3) 0.006(3) -0.002(3) -0.002(3) C6 0.038(5) 0.041(3) 0.042(4) 0.008(3) -0.007(3) 0.003(3) C7 0.032(4) 0.035(3) 0.040(4) -0.001(3) 0.007(3) 0.011(3) O5 0.043(3) 0.042(2) 0.059(3) -0.002(2) 0.003(3) -0.001(2) O6 0.055(4) 0.038(2) 0.078(4) -0.011(2) 0.013(3) -0.011(2) C8 0.048(4) 0.041(3) 0.034(3) -0.001(3) 0.006(3) -0.009(3) C9 0.039(4) 0.036(3) 0.045(3) -0.007(3) 0.009(3) -0.012(3) C10 0.045(4) 0.037(3) 0.035(3) -0.001(3) 0.013(3) 0.000(3) N2 0.071(5) 0.044(3) 0.045(4) 0.009(3) 0.023(4) 0.023(3) O7 0.053(4) 0.104(4) 0.061(4) 0.023(3) 0.027(3) 0.006(3) O8 0.077(4) 0.104(4) 0.038(3) 0.009(3) 0.004(3) 0.022(4) C11 0.037(4) 0.064(4) 0.060(4) -0.008(4) 0.004(3) -0.003(4) C12 0.057(6) 0.094(6) 0.069(6) -0.014(5) 0.033(5) -0.019(5) C13 0.080(7) 0.116(7) 0.050(5) -0.023(5) 0.035(5) -0.025(6) C14 0.065(6) 0.083(5) 0.041(4) -0.010(4) 0.013(4) -0.020(5) O9 0.045(3) 0.043(2) 0.069(3) 0.001(3) 0.016(2) -0.002(2) _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 O1 2.421(4) . ? Pb1 O5 2.531(5) . ? Pb1 O2 2.558(4) 4_656 ? Pb1 O6 2.631(5) . ? Pb1 O1 2.670(3) 4_666 ? Pb1 O9 2.676(5) . ? O1 C1 1.265(6) . ? O1 Pb1 2.670(3) 4_656 ? O2 C1 1.236(6) . ? O2 Pb1 2.558(3) 4_666 ? C1 C2 1.505(7) . ? C2 C3 1.393(8) . ? C2 C7 1.394(8) . ? C3 C4 1.400(7) . ? C3 N1 1.463(8) . ? N1 O3 1.210(6) . ? N1 O4 1.219(7) . ? C4 C5 1..369(9) . ? C4 H4 0.9300 . ? C5 C6 1.372(9) . ? C5 H5 0.9300 . ? C6 C7 1.384(8) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? O5 C8 1.260(7) . ? O6 C8 1.248(6) . ? C8 C9 1.497(9) . ? C9 C10 1.396(8) . ? C9 C14 1.405(9) . ? C10 C11 1.388(9) . ? C10 N2 1.454(8) . ? N2 O7 1.208(7) . ? N2 O8 1.238(7) . ? C11 C12 1.359(10) . ? C11 H11 0.9300 . ? C12 C13 1.360(11) . ? C12 H12 0.9300 . ? C13 C14 1.361(11) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? O9 H9WA 0.78(6) . ? O9 H9WB 0.87(9) . ? 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 O1 Pb1 O5 77.10(15) . . ? O1 Pb1 O2 69.90(13) . 4_656 ? O5 Pb1 O2 80.87(15) . 4_656 ? O1 Pb1 O6 91.97(16) . . ? O5 Pb1 O6 50.43(12) . . ? O2 Pb1 O6 131.07(15) 4_656 . ? O1 Pb1 O1 110.17(9) . 4_666 ? O5 Pb1 O1 128.27(14) . 4_666 ? O2 Pb1 O1 150.74(15) 4_656 4_666 ? O6 Pb1 O1 77.86(13) . 4_666 ? O1 Pb1 O9 75.92(16) . . ? O5 Pb1 O9 149.94(15) . . ? O2 Pb1 O9 77.62(15) 4_656 . ? O6 Pb1 O9 143.20(15) . . ? O1 Pb1 O9 74.26(14) 4_666 . ? C1 O1 Pb1 103.2(3) . . ? C1 O1 Pb1 134.9(3) . 4_656 ? Pb1 O1 Pb1 117.86(15) . 4_656 ? C1 O2 Pb1 154.9(4) . 4_666 ? O2 C1 O1 121.3(5) . . ? O2 C1 C2 120.4(5) . . ? O1 C1 C2 118.0(4) . . ? C3 C2 C7 118.3(5) . . ? C3 C2 C1 123.6(5) . . ? C7 C2 C1 118.0(5) . . ? C2 C3 C4 121.5(5) . . ? C2 C3 N1 120.1(5) . . ? C4 C3 N1 118.3(5) . . ? O3 N1 O4 123.8(6) . . ? O3 N1 C3 117.8(5) . . ? O4 N1 C3 118.2(5) . . ? C5 C4 C3 117.8(6) . . ? C5 C4 H4 121.1 . . ? C3 C4 H4 121.1 . . ? C4 C5 C6 122.2(6) . . ? C4 C5 H5 118.9 . . ? C6 C5 H5 118.9 . . ? C5 C6 C7 119.8(6) . . ? C5 C6 H6 120.1 . . ? C7 C6 H6 120.1 . . ? C6 C7 C2 120.3(6) . . ? C6 C7 H7 119.8 . . ? C2 C7 H7 119.8 . . ? C8 O5 Pb1 95.6(4) . . ? C8 O6 Pb1 91.2(4) . . ? O6 C8 O5 122.7(6) . . ? O6 C8 C9 120.1(6) . . ? O5 C8 C9 117.0(5) .. . ? C10 C9 C14 116.2(6) . . ? C10 C9 C8 126.2(6) . . ? C14 C9 C8 117.5(6) . . ? C11 C10 C9 121.0(6) . . ? C11 C10 N2 119.3(6) . . ? C9 C10 N2 119.7(6) . . ? O7 N2 O8 123.6(7) . . ? O7 N2 C10 119.7(6) . . ? O8 N2 C10 116.6(7) . . ? C12 C11 C10 120.2(7) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C11 C12 C13 120.3(8) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C12 C13 C14 120.4(8) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C13 C14 C9 121.9(7) . . ? C13 C14 H14 119.1 . . ? C9 C14 H14 119.1 . . ? Pb1 O9 H9WA 110(5) . . ? Pb1 O9 H9WB 108(7) . . ? H9WA O9 H9WB 112(8) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O9 H9WA O5 0.78(6) 2.16(6) 2.938(7) 170(7) 4_666 O9 H9WB O6 0.87(9) 1.99(9) 2.827(6) 162(9) 4_656 _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 32.51 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 2.129 _refine_diff_density_min -1.989 _refine_diff_density_rms 0.172 data_js075 _database_code_CSD 158369 _publ_requested_journal test _audit_creation_method SHELXL-97 _chemical_name_systematic 'C14 H8 N4 O13 Pb' _chemical_name_common 'C14 H8 N4 O13 Pb' _chemical_formula_moiety 'C14 H8 N4 O13 Pb' _chemical_formula_sum 'C14 H8 N4 O13 Pb' _chemical_formula_weight 647.43 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' 'Pb' 'Pb' -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 7.2864(3) _cell_length_b 11.0392(5) _cell_length_c 23.2010(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1866.20(14) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4469 _cell_measurement_theta_min 2.547 _cell_measurement_theta_max 31.440 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.304 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 9.124 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_process_details '(SADABS; Bruker, 1999)' _exptl_absorpt_correction_T_min 0.6095 _exptl_absorpt_correction_T_max 0.9281 _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 SMART area CCD detector' _diffrn_measurement_method /f-/w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 19078 _diffrn_reflns_av_R_equivalents 0.0331 _diffrn_reflns_av_sigmaI/netI 0.0399 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 32.48 _reflns_number_total 6692 _reflns_number_gt 5695 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortex in OSCAIL (McArdle, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0178P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.008(5) _refine_ls_number_reflns 6692 _refine_ls_number_parameters 297 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0347 _refine_ls_R_factor_gt 0.0251 _refine_ls_wR_factor_ref 0.0434 _refine_ls_wR_factor_gt 0.0418 _refine_ls_goodness_of_fit_ref 0.929 _refine_ls_restrained_S_all 0.929 _refine_ls_shift/su_max 0.002 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.656098(16) 0.189528(11) -0.037893(5) 0.03207(3) Uani 1 d . . . C1 C 0.6195(5) 0.5358(3) 0.05708(15) 0.0348(8) Uani 1 d . . . C2 C 0.4495(5) 0.5901(3) 0.04678(16) 0.0383(8) Uani 1 d . . . H2 H 0.3591 0.5507 0.0256 0.046 Uiso 1 calc R . . C3 C 0.4202(5) 0.7052(4) 0.06921(17) 0.0439(9) Uani 1 d . . . C4 C 0.5506(7) 0.7677(4) 0.09911(17) 0.0523(11) Uani 1 d . . . H4 H 0.5287 0.8457 0.1126 0.063 Uiso 1 calc R . . C5 C 0.7132(6) 0.7117(3) 0.10835(18) 0.0486(10) Uani 1 d . . . C6 C 0.7523(6) 0.5961(3) 0.08830(16) 0.0409(8) Uani 1 d . . . H6 H 0.8652 0.5601 0.0957 0.049 Uiso 1 calc R . . O1 O 0.5219(3) 0.3575(2) 0.00869(11) 0.0363(5) Uani 1 d . . . O2 O 0.8160(3) 0.3723(2) 0.03021(12) 0.0448(6) Uani 1 d . . . C7 C 0.6577(5) 0.4133(2) 0.03066(13) 0.0320(6) Uani 1 d . . . N1 N 0.2405(6) 0.7627(4) 0.05789(17) 0.0599(11) Uani 1 d . . . O3 O 0.1199(4) 0.6996(3) 0.03606(15) 0.0740(9) Uani 1 d . . . O4 O 0.2230(6) 0.8694(3) 0.07168(17) 0.0850(12) Uani 1 d . . . N2 N 0.8566(7) 0.7783(3) 0.14088(16) 0.0648(10) Uani 1 d . . . O5 O 0.9877(6) 0.7232(3) 0.15948(15) 0.0788(11) Uani 1 d . . . O6 O 0.8335(8) 0.8862(3) 0.1464(2) 0.1102(16) Uani 1 d . . . C8 C 0.6339(5) 0.4273(3) -0.18873(14) 0.0341(7) Uani 1 d . . . C9 C 0.4777(5) 0.4240(3) -0.22232(14) 0.0357(7) Uani 1 d . . . H9 H 0.3798 0.3742 -0.2122 0.043 Uiso 1 calc R . . C10 C 0.4687(5) 0.4955(3) -0.27116(15) 0.0393(8) Uani 1 d . . . C11 C 0.6069(5) 0.5722(4) -0.28757(17) 0.0452(9) Uani 1 d . . . H11 H 0.5968 0.6208 -0.3202 0.054 Uiso 1 calc R . . C12 C 0.7623(5) 0.5738(4) -0.25327(17) 0.0425(8) Uani 1 d . . . C13 C 0.7792(5) 0.5013(4) -0.20463(16) 0.0390(8) Uani 1 d . . . H13 H 0.8866 0.5024 -0.1830 0.047 Uiso 1 calc R . . O7 O 0.4978(3) 0.2970(3) -0.11983(10) 0.0429(6) Uani 1 d . . . O8 O 0.7885(3) 0.3470(2) -0.10623(11) 0.0447(7) Uani 1 d . . . C14 C 0.6422(6) 0.3517(3) -0.13433(14) 0.0361(7) Uani 1 d . . . N3 N 0.3024(5) 0.4874(3) -0.30725(16) 0.0525(9) Uani 1 d . . . O9 O 0.1748(5) 0.4255(3) -0.29116(14) 0.0702(9) Uani 1 d . . . O10 O 0.3032(5) 0.5434(3) -0.35325(15) 0.0836(13) Uani 1 d . . . N4 N 0.9132(5) 0.6561(4) -0.2687(2) 0.0633(11) Uani 1 d . . . O11 O 0.9014(5) 0.7090(4) -0.31461(19) 0.1018(15) Uani 1 d . . . O12 O 1.0418(5) 0.6656(3) -0.23624(16) 0.0788(11) Uani 1 d . . . O1W O 0.6516(6) 0.1084(3) 0.07004(14) 0.0562(8) Uani 1 d . . . H1WA H 0.749(9) 0.100(6) 0.086(3) 0.12(3) Uiso 1 d . . . H1WB H 0.562(6) 0.126(4) 0.079(2) 0.049(15) Uiso 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 0.03643(5) 0.03041(5) 0.02936(5) -0.00399(6) -0.00410(6) 0.00480(6) C1 0.0430(19) 0.0272(15) 0.0340(17) -0.0046(12) 0.0035(14) -0.0023(13) C2 0.0483(18) 0.0276(15) 0.039(2) 0.0012(15) 0.0060(17) -0.0001(13) C3 0.059(2) 0.035(2) 0.0380(19) 0.0003(16) 0.0118(17) 0.0091(17) C4 0.085(3) 0.0337(19) 0.038(2) -0.0092(16) 0.007(2) 0.0033(19) C5 0.069(2) 0.040(2) 0.038(2) -0.0083(17) -0.0044(19) -0.0105(18) C6 0.052(2) 0.0356(18) 0.0349(19) -0.0019(15) 0.0002(17) -0.0007(16) O1 0.0360(12) 0.0349(12) 0.0379(13) -0.0088(10) 0.0042(11) -0.0007(10) O2 0.0373(13) 0.0424(13) 0.0546(17) -0.0066(12) -0.0045(14) 0.0100(10) C7 0.0436(15) 0.0264(12) 0.0262(15) -0.0004(12) 0.0043(18) -0.0039(14) N1 0.079(3) 0.056(2) 0.045(2) 0.0019(17) -0.002(2) 0.028(2) O3 0.0718(19) 0.084(2) 0.066(2) 0.002(2) -0.0127(19) 0.034(2) O4 0.118(3) 0.0510(19) 0.087(3) -0.0079(18) -0.004(2) 0.0432(19) N2 0.087(3) 0.055(2) 0.053(2) -0.0141(17) -0.013(2) -0.019(2) O5 0.103(3) 0.068(2) 0.065(2) 0.0014(18) -0.034(2) -0.021(2) O6 0.129(4) 0.052(2) 0.150(4) -0.044(2) -0.029(4) -0.010(3) C8 0.0406(18) 0.0354(16) 0.0261(15) -0.0026(13) 0.0016(15) 0.0065(15) C9 0.0409(18) 0.0397(18) 0.0264(17) -0.0008(14) 0.0027(15) 0.0021(15) C10 0.048(2) 0.044(2) 0.0260(17) 0.0010(15) -0.0051(16) 0.0020(16) C11 0.057(2) 0.044(2) 0.0346(19) 0.0055(17) 0.0028(17) 0.0033(17) C12 0.0423(19) 0.044(2) 0.041(2) 0.0015(17) 0.0040(17) -0.0009(16) C13 0.041(2) 0.0457(19) 0.0305(19) -0.0027(16) -0.0042(16) 0.0039(16) O7 0.0437(13) 0.0485(15) 0.0365(13) 0.0071(13) -0.0012(11) -0.0040(12) O8 0.0395(13) 0.0594(18) 0.0351(14) 0.0032(12) -0.0056(11) 0.0015(11) C14 0.0469(19) 0.0391(16) 0.0222(15) -0.0049(12) -0.0029(17) 0.0123(17) N3 0.063(2) 0.054(2) 0.0409(19) 0.0077(16) -0.0116(17) -0.0001(17) O9 0.0552(18) 0.091(2) 0.064(2) 0.0263(18) -0.0124(18) -0.019(2) O10 0.097(3) 0.099(3) 0.054(2) 0.0362(19) -0.036(2) -0.034(2) N4 0.055(2) 0.067(3) 0.068(3) 0.009(2) 0.006(2) -0.0035(18) O11 0.071(2) 0.132(4) 0.102(3) 0.072(3) -0.001(2) -0.026(2) O12 0.0623(19) 0.095(3) 0.079(2) 0.010(2) -0.0108(19) -0.0278(19) O1W 0.0447(17) 0.073(2) 0.0504(18) 0.0062(15) -0.0014(19) 0.0079(19) _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 O1 2.358(2) . ? Pb1 O7 2.520(3) . ? Pb1 O8 2.543(3) . ? Pb1 O2 2.577(2) 4_455 ? Pb1 O1W 2.660(3) . ? Pb1 O1 2.799(2) 4 ? Pb1 O2 2.815(3) . ? C1 C6 1.380(5) . ? C1 C2 1.397(5) . ? C1 C7 1.511(4) . ? C2 C3 1.389(5) . ? C2 H2 0.9300 . ? C3 C4 1.364(6) . ? C3 N1 1.479(5) . ? C4 C5 1.353(6) . ? C4 H4 0.9300 . ? C5 C6 1.388(5) . ? C5 N2 1.484(5) . ? C6 H6 0.9300 . ? O1 C7 1.272(4) . ? O1 Pb1 2.799(2) 4_455 ? O2 C7 1.239(4) . ? O2 Pb1 2.577(2) 4 ? N1 O4 1.227(5) . ? N1 O3 1.231(5) . ? N2 O6 1.210(5) . ? N2 O5 1.212(5) . ? C8 C9 1.380(5) . ? C8 C13 1.387(5) . ? C8 C14 1.515(5) . ? C9 C10 1.383(5) . ? C9 H9 0.9300 . ? C10 C11 1.369(5) . ? C10 N3 1.476(5) . ? C11 C12 1.384(5) . ? C11 H11 0.9300 . ? C12 C13 1.389(5) . ? C12 N4 1.470(5) . ? C13 H13 0.9300 . ? O7 C14 1.259(5) . ? O8 C14 1.251(4) . ? N3 O9 1.212(4) . ? N3 O10 1.234(4) . ? N4 O12 1.207(5) . ? N4 O11 1.218(5) . ? O1W H1WA 0.80(7) . ? O1W H1WB 0.72(4) . ? 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 O1 Pb1 O7 77.62(9) . . ? O1 Pb1 O8 84.57(9) . . ? O7 Pb1 O8 51.79(8) . . ? O1 Pb1 O2 77.16(8) . 4_455 ? O7 Pb1 O2 74.74(8) . 4_455 ? O8 Pb1 O2 126.09(8) . 4_455 ? O1 Pb1 O1W 80.11(10) . . ? O7 Pb1 O1W 149.67(11) . . ? O8 Pb1 O1W 145.27(10) . . ? O2 Pb1 O1W 80.44(11) 4_455 . ? O1 Pb1 O1 115.45(6) . 4 ? O7 Pb1 O1 134..89(7) . 4 ? O8 Pb1 O1 85.21(7) . 4 ? O2 Pb1 O1 148.22(7) 4_455 4 ? O1W Pb1 O1 73.81(10) . 4 ? O1 Pb1 O2 49.53(7) . . ? O7 Pb1 O2 105.97(8) . . ? O8 Pb1 O2 72.71(8) . . ? O2 Pb1 O2 123.30(6) 4_455 . ? O1W Pb1 O2 73.62(9) . . ? O1 Pb1 O2 66.61(6) 4 . ? C6 C1 C2 120.3(3) . . ? C6 C1 C7 121.1(3) . . ? C2 C1 C7 118.6(3) . . ? C3 C2 C1 117.7(3) . . ? C3 C2 H2 121.1 . . ? C1 C2 H2 121.1 . . ? C4 C3 C2 123.1(4) . . ? C4 C3 N1 119.3(4) . . ? C2 C3 N1 117.5(4) . . ? C5 C4 C3 117.3(3) . . ? C5 C4 H4 121.3 . . ? C3 C4 H4 121.3 . . ? C4 C5 C6 123.1(4) . . ? C4 C5 N2 118.1(4) . . ? C6 C5 N2 118.8(4) . . ? C1 C6 C5 118.4(4) . . ? C1 C6 H6 120.8 . . ? C5 C6 H6 120.8 . . ? C7 O1 Pb1 103.98(19) . . ? C7 O1 Pb1 137.2(2) . 4_455 ? Pb1 O1 Pb1 111.10(9) . 4_455 ? C7 O2 Pb1 172.5(2) . 4 ? C7 O2 Pb1 83.17(19) . . ? Pb1 O2 Pb1 104.29(8) 4 . ? O2 C7 O1 123.0(3) . . ? O2 C7 C1 120.1(3) . . ? O1 C7 C1 116.9(3) . . ? O4 N1 O3 125.2(4) . . ? O4 N1 C3 117.3(5) . . ? O3 N1 C3 117.6(3) . . ? O6 N2 O5 124.5(5) . . ? O6 N2 C5 116.3(5) . . ? O5 N2 C5 119.2(4) . . ? C9 C8 C13 119.7(3) . . ? C9 C8 C14 119.2(3) . . ? C13 C8 C14 121.1(3) . . ? C8 C9 C10 119.1(3) . . ? C8 C9 H9 120.4 . . ? C10 C9 H9 120.4 . . ? C11 C10 C9 123.1(3) . . ? C11 C10 N3 118.9(3) . . ? C9 C10 N3 118.0(3) . . ? C10 C11 C12 116.7(3) . . ? C10 C11 H11 121.6 . . ? C12 C11 H11 121.6 . . ? C11 C12 C13 122.1(4) . . ? C11 C12 N4 118.7(4) . . ? C13 C12 N4 119.2(4) . . ? C8 C13 C12 119.2(3) . . ? C8 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? C14 O7 Pb1 92.6(2) . . ? C14 O8 Pb1 91.7(2) . . ? O8 C14 O7 123.6(3) . . ? O8 C14 C8 119.4(4) . . ? O7 C14 C8 117.0(3) . . ? O9 N3 O10 123.6(4) . . ? O9 N3 C10 119.3(3) . . ? O10 N3 C10 117.1(4) . . ? O12 N4 O11 124.0(4) . . ? O12 N4 C12 118.8(4) . . ? O11 N4 C12 117.1(4) . . ? Pb1 O1W H1WA 117(5) . . ? Pb1 O1W H1WB 102(4) . . ? H1WA O1W H1WB 135(6) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1WA O7 0.80(7) 2.29(7) 2.964(5) 143(6) 4 O1W H1WB O8 0.72(4) 2.11(5) 2.819(5) 173(5) 4_455 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 32.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.255 _refine_diff_density_min -0.782 _refine_diff_density_rms 0.092