# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Shao-Wu Du' _publ_contact_author_email SWDU@FJIRSM.AC.CN _publ_section_title ; A series of novel Pb(II) or Pb(II)/M(II) (M = Ca and Sr) hybrid inorganic-organic frameworks based on polycarboxylic acids with diverse Pb-O-M (M = Pb, Ca and Sr) inorganic connectivities ; loop_ _publ_author_name 'Shaowu Du.' 'Zhihua Li.' 'Shaowu Du.' 'Shu-Ting Wu.' #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 752040' #TrackingRef 'CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H8 O6 Pb S' _chemical_formula_weight 511.45 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 5.9527(3) _cell_length_b 13.0441(6) _cell_length_c 19.5781(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1520.19(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3435 _cell_measurement_theta_min 3.1214 _cell_measurement_theta_max 27.4835 _exptl_crystal_description needle-shaped _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.235 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 11.260 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.2988 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _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 Monochromator' _diffrn_measurement_device_type 'Mercury70 (2x2 bin mode)' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10709 _diffrn_reflns_av_R_equivalents 0.0365 _diffrn_reflns_av_sigmaI/netI 0.0238 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.49 _diffrn_reflns_theta_max 27.46 _reflns_number_total 1814 _reflns_number_gt 1639 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0413P)^2^+4.5573P] 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 1814 _refine_ls_number_parameters 106 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0292 _refine_ls_R_factor_gt 0.0264 _refine_ls_wR_factor_ref 0.0771 _refine_ls_wR_factor_gt 0.0747 _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 1.74268(3) 0.2500 0.689683(11) 0.01984(11) Uani 1 2 d S . . S1 S 2.1065(3) -0.2500 0.99564(8) 0.0221(3) Uani 1 2 d S . . O1 O 1.8366(6) 0.1376(3) 0.78565(18) 0.0368(8) Uani 1 1 d . . . O2 O 1.5269(6) 0.1310(3) 0.85002(17) 0.0407(9) Uani 1 1 d . . . O3 O 2.3485(8) -0.2500 0.9895(2) 0.0306(10) Uani 1 2 d S . . O4 O 2.0077(8) -0.2500 1.0632(2) 0.0331(11) Uani 1 2 d S . . C1 C 1.7202(8) 0.1029(4) 0.8340(3) 0.0264(10) Uani 1 1 d . . . C2 C 1.8229(7) 0.0173(3) 0.8756(2) 0.0219(8) Uani 1 1 d . . . C3 C 1.7037(8) -0.0229(4) 0.9302(2) 0.0281(9) Uani 1 1 d . . . H3 H 1.5645 0.0047 0.9415 0.034 Uiso 1 1 calc R . . C4 C 1.7903(7) -0.1042(4) 0.9683(2) 0.0270(10) Uani 1 1 d . . . H4 H 1.7105 -0.1315 1.0049 0.032 Uiso 1 1 calc R . . C5 C 1.9985(7) -0.1432(3) 0.9502(2) 0.0221(8) Uani 1 1 d . . . C6 C 2.1184(8) -0.1039(4) 0.8958(2) 0.0316(10) Uani 1 1 d . . . H6 H 2.2572 -0.1316 0.8842 0.038 Uiso 1 1 calc R . . C7 C 2.0314(8) -0.0237(4) 0.8588(2) 0.0315(10) Uani 1 1 d . . . H7 H 2.1125 0.0034 0.8225 0.038 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 0.01738(15) 0.02462(16) 0.01752(16) 0.000 0.00001(7) 0.000 S1 0.0229(7) 0.0201(6) 0.0232(7) 0.000 -0.0050(6) 0.000 O1 0.041(2) 0.0355(19) 0.0341(18) 0.0152(16) -0.0047(17) -0.0033(16) O2 0.0361(19) 0.042(2) 0.044(2) 0.0070(16) -0.0085(16) 0.0128(16) O3 0.023(2) 0.026(2) 0.042(3) 0.000 -0.007(2) 0.000 O4 0.052(3) 0.030(2) 0.017(2) 0.000 -0.0025(19) 0.000 C1 0.035(2) 0.021(2) 0.024(2) 0.0016(19) -0.0074(18) -0.0027(18) C2 0.023(2) 0.0220(19) 0.020(2) 0.0043(16) -0.0028(17) 0.0000(17) C3 0.025(2) 0.031(2) 0.028(2) 0.0059(19) 0.0012(18) 0.008(2) C4 0.026(2) 0.031(2) 0.024(2) 0.0072(19) 0.0060(17) 0.0027(19) C5 0.022(2) 0.0213(19) 0.0233(19) -0.0003(16) -0.0024(15) -0.0002(16) C6 0.022(2) 0.034(2) 0.039(2) 0.009(2) 0.0048(19) 0.0048(19) C7 0.029(2) 0.035(2) 0.031(2) 0.0093(19) 0.0076(18) 0.001(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 O2 2.424(3) 4_556 ? Pb1 O2 2.424(3) 6_657 ? Pb1 O1 2.448(3) 7_565 ? Pb1 O1 2.448(3) . ? S1 O3 1.445(5) . ? S1 O4 1.448(4) . ? S1 C5 1.773(4) 7 ? S1 C5 1.773(4) . ? O1 C1 1.257(7) . ? O2 C1 1.247(6) . ? O2 Pb1 2.424(3) 6_557 ? C1 C2 1.512(6) . ? C2 C3 1.386(6) . ? C2 C7 1.390(6) . ? C3 C4 1.396(6) . ? C3 H3 0.9300 . ? C4 C5 1.386(6) . ? C4 H4 0.9300 . ? C5 C6 1.381(6) . ? C6 C7 1.373(6) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? 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 O2 Pb1 O2 79.65(18) 4_556 6_657 ? O2 Pb1 O1 72.73(13) 4_556 7_565 ? O2 Pb1 O1 118.04(13) 6_657 7_565 ? O2 Pb1 O1 118.04(13) 4_556 . ? O2 Pb1 O1 72.73(12) 6_657 . ? O1 Pb1 O1 73.57(17) 7_565 . ? O3 S1 O4 118.8(3) . . ? O3 S1 C5 108.62(18) . 7 ? O4 S1 C5 108.12(19) . 7 ? O3 S1 C5 108.62(18) . . ? O4 S1 C5 108.12(19) . . ? C5 S1 C5 103.5(3) 7 . ? C1 O1 Pb1 131.8(3) . . ? C1 O2 Pb1 138.7(3) . 6_557 ? O2 C1 O1 126.3(5) . . ? O2 C1 C2 117.0(4) . . ? O1 C1 C2 116.6(4) . . ? C3 C2 C7 119.6(4) . . ? C3 C2 C1 119.2(4) . . ? C7 C2 C1 121.2(4) . . ? C2 C3 C4 120.7(4) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C5 C4 C3 118.2(4) . . ? C5 C4 H4 120.9 . . ? C3 C4 H4 120.9 . . ? C6 C5 C4 121.5(4) . . ? C6 C5 S1 119.4(3) . . ? C4 C5 S1 119.0(3) . . ? C7 C6 C5 119.7(4) . . ? C7 C6 H6 120.2 . . ? C5 C6 H6 120.2 . . ? C6 C7 C2 120.3(4) . . ? C6 C7 H7 119.8 . . ? C2 C7 H7 119.8 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.418 _refine_diff_density_min -2.163 _refine_diff_density_rms 0.160 # Attachment 'CIFs.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 763444' #TrackingRef 'CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H10 O5 Pb S' _chemical_formula_weight 449.43 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 9.4887(7) _cell_length_b 7.4979(5) _cell_length_c 18.1593(12) _cell_angle_alpha 90.00 _cell_angle_beta 91.634(6) _cell_angle_gamma 90.00 _cell_volume 1291.42(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3549 _cell_measurement_theta_min 3.0618 _cell_measurement_theta_max 27.4835 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.312 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 832 _exptl_absorpt_coefficient_mu 13.231 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6019 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _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 Monochromator' _diffrn_measurement_device_type 'Mercury70 (2x2 bin mode)' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9572 _diffrn_reflns_av_R_equivalents 0.0294 _diffrn_reflns_av_sigmaI/netI 0.0285 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 27.49 _reflns_number_total 2958 _reflns_number_gt 2695 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0353P)^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 2958 _refine_ls_number_parameters 154 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0281 _refine_ls_R_factor_gt 0.0247 _refine_ls_wR_factor_ref 0.0603 _refine_ls_wR_factor_gt 0.0585 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _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 0.814577(14) 0.579862(19) 0.247108(7) 0.01962(7) Uani 1 1 d . . . S1 S 0.42716(13) 0.66842(17) 0.21970(9) 0.0455(3) Uani 1 1 d . . . O1 O 0.7984(3) 0.8174(4) 0.34276(15) 0.0292(7) Uani 1 1 d . . . O2 O 1.0049(4) 0.6809(5) 0.34538(18) 0.0403(8) Uani 1 1 d . . . O3 O 0.8568(4) 0.8640(5) 0.17659(19) 0.0469(10) Uani 1 1 d . . . O4 O 0.9874(4) 0.6454(5) 0.1393(2) 0.0528(11) Uani 1 1 d . . . O5 O 0.5758(3) 0.7426(4) 0.2246(2) 0.0425(8) Uani 1 1 d . . . C1 C 0.9203(5) 0.7917(6) 0.3709(2) 0.0261(9) Uani 1 1 d . . . C2 C 0.9614(5) 0.8993(6) 0.4384(2) 0.0280(10) Uani 1 1 d . . . C3 C 0.8689(5) 1.0234(7) 0.4659(2) 0.0338(10) Uani 1 1 d . . . H3 H 0.7805 1.0385 0.4434 0.041 Uiso 1 1 calc R . . C4 C 1.0927(5) 0.8748(7) 0.4733(3) 0.0343(11) Uani 1 1 d . . . H4 H 1.1546 0.7898 0.4556 0.041 Uiso 1 1 calc R . . C5 C 0.9363(5) 0.7966(6) 0.1304(2) 0.0281(9) Uani 1 1 d . . . C6 C 0.9687(5) 0.9020(5) 0.0629(2) 0.0265(9) Uani 1 1 d . . . C7 C 0.9243(6) 1.0781(6) 0.0551(3) 0.0357(12) Uani 1 1 d . . . H7 H 0.8734 1.1316 0.0921 0.043 Uiso 1 1 calc R . . C8 C 0.9558(5) 1.1742(7) -0.0076(3) 0.0376(11) Uani 1 1 d . . . H8 H 0.9255 1.2918 -0.0122 0.045 Uiso 1 1 calc R . . C9 C 0.3380(7) 0.7771(10) 0.2918(5) 0.075(2) Uani 1 1 d . . . H9A H 0.3714 0.7311 0.3385 0.113 Uiso 1 1 calc R . . H9B H 0.2385 0.7559 0.2862 0.113 Uiso 1 1 calc R . . H9C H 0.3559 0.9030 0.2897 0.113 Uiso 1 1 calc R . . C10 C 0.3442(6) 0.7805(8) 0.1439(4) 0.0633(18) Uani 1 1 d . . . H10A H 0.3811 0.7362 0.0988 0.095 Uiso 1 1 calc R . . H10B H 0.3622 0.9062 0.1478 0.095 Uiso 1 1 calc R . . H10C H 0.2444 0.7596 0.1442 0.095 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 0.02283(10) 0.01859(10) 0.01750(9) -0.00032(5) 0.00133(6) -0.00100(5) S1 0.0248(6) 0.0305(7) 0.0807(10) -0.0056(6) -0.0080(6) -0.0035(5) O1 0.0348(18) 0.0332(17) 0.0192(14) -0.0039(12) -0.0084(12) -0.0015(13) O2 0.039(2) 0.043(2) 0.0386(19) -0.0165(16) -0.0103(15) 0.0071(15) O3 0.073(3) 0.0352(19) 0.0340(19) 0.0111(16) 0.0334(19) 0.0116(18) O4 0.065(3) 0.041(2) 0.055(2) 0.0263(19) 0.035(2) 0.0236(19) O5 0.0228(17) 0.0361(19) 0.068(2) -0.0013(17) -0.0088(15) -0.0020(14) C1 0.032(2) 0.026(2) 0.0196(19) -0.0011(16) -0.0036(16) -0.0056(17) C2 0.034(3) 0.032(2) 0.018(2) -0.0040(17) -0.0053(17) -0.0021(17) C3 0.033(2) 0.042(3) 0.025(2) -0.008(2) -0.0124(18) 0.003(2) C4 0.036(3) 0.040(3) 0.026(2) -0.011(2) -0.0081(19) 0.010(2) C5 0.029(2) 0.035(3) 0.021(2) 0.0050(17) 0.0070(17) -0.0036(18) C6 0.029(2) 0.031(2) 0.020(2) 0.0064(17) 0.0106(17) 0.0008(17) C7 0.049(3) 0.032(3) 0.027(2) 0.0049(19) 0.023(2) 0.013(2) C8 0.051(3) 0.030(3) 0.033(3) 0.005(2) 0.019(2) 0.012(2) C9 0.050(4) 0.084(5) 0.092(6) -0.008(4) 0.020(4) -0.002(3) C10 0.041(3) 0.062(4) 0.085(5) -0.008(4) -0.022(3) 0.004(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 2.495(3) . ? Pb1 O3 2.523(3) . ? Pb1 O5 2.596(3) . ? Pb1 O2 2.614(3) . ? Pb1 O4 2.635(3) . ? Pb1 O3 2.704(3) 2_645 ? Pb1 O1 2.754(3) 2_645 ? S1 O5 1.516(3) . ? S1 C9 1.777(7) . ? S1 C10 1.777(6) . ? O1 C1 1.266(5) . ? O1 Pb1 2.754(3) 2_655 ? O2 C1 1.253(5) . ? O3 C5 1.250(5) . ? O3 Pb1 2.704(3) 2_655 ? O4 C5 1.242(5) . ? C1 C2 1.510(6) . ? C2 C3 1.382(6) . ? C2 C4 1.393(6) . ? C3 C4 1.383(6) 3_776 ? C3 H3 0.9300 . ? C4 C3 1.383(6) 3_776 ? C4 H4 0.9300 . ? C5 C6 1.498(6) . ? C6 C8 1.374(6) 3_775 ? C6 C7 1.392(5) . ? C7 C8 1.387(6) . ? C7 H7 0.9300 . ? C8 C6 1.374(6) 3_775 ? C8 H8 0.9300 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 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 O1 Pb1 O3 76.38(11) . . ? O1 Pb1 O5 72.75(10) . . ? O3 Pb1 O5 70.96(12) . . ? O1 Pb1 O2 51.18(10) . . ? O3 Pb1 O2 89.16(13) . . ? O5 Pb1 O2 123.65(11) . . ? O1 Pb1 O4 115.84(12) . . ? O3 Pb1 O4 49.80(11) . . ? O5 Pb1 O4 110.75(12) . . ? O2 Pb1 O4 91.19(13) . . ? O1 Pb1 O3 91.19(10) . 2_645 ? O3 Pb1 O3 150.67(8) . 2_645 ? O5 Pb1 O3 80.04(12) . 2_645 ? O2 Pb1 O3 103.73(12) . 2_645 ? O4 Pb1 O3 152.64(11) . 2_645 ? O1 Pb1 O1 153.09(2) . 2_645 ? O3 Pb1 O1 111.55(11) . 2_645 ? O5 Pb1 O1 85.37(10) . 2_645 ? O2 Pb1 O1 149.43(10) . 2_645 ? O4 Pb1 O1 86.16(12) . 2_645 ? O3 Pb1 O1 69.28(10) 2_645 2_645 ? O5 S1 C9 104.5(3) . . ? O5 S1 C10 105.2(3) . . ? C9 S1 C10 98.3(4) . . ? C1 O1 Pb1 95.7(3) . . ? C1 O1 Pb1 133.1(3) . 2_655 ? Pb1 O1 Pb1 97.36(9) . 2_655 ? C1 O2 Pb1 90.4(2) . . ? C5 O3 Pb1 96.1(3) . . ? C5 O3 Pb1 165.6(3) . 2_655 ? Pb1 O3 Pb1 97.98(10) . 2_655 ? C5 O4 Pb1 91.0(3) . . ? S1 O5 Pb1 130.02(18) . . ? O2 C1 O1 122.6(4) . . ? O2 C1 C2 120.1(4) . . ? O1 C1 C2 117.3(4) . . ? C3 C2 C4 119.6(4) . . ? C3 C2 C1 120.1(4) . . ? C4 C2 C1 120.4(4) . . ? C2 C3 C4 120.3(4) . 3_776 ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 3_776 . ? C3 C4 C2 120.1(4) 3_776 . ? C3 C4 H4 119.9 3_776 . ? C2 C4 H4 119.9 . . ? O4 C5 O3 121.5(4) . . ? O4 C5 C6 119.9(4) . . ? O3 C5 C6 118.6(4) . . ? C8 C6 C7 118.9(4) 3_775 . ? C8 C6 C5 120.2(4) 3_775 . ? C7 C6 C5 120.9(4) . . ? C8 C7 C6 120.3(4) . . ? C8 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? C6 C8 C7 120.8(4) 3_775 . ? C6 C8 H8 119.6 3_775 . ? C7 C8 H8 119.6 . . ? S1 C9 H9A 109.5 . . ? S1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? S1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? S1 C10 H10A 109.5 . . ? S1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? S1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.711 _refine_diff_density_min -1.637 _refine_diff_density_rms 0.164 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 763445' #TrackingRef 'CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H14 Ca O9 Pb S' _chemical_formula_weight 653.62 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ca Ca 0.2262 0.3064 '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 10.143(2) _cell_length_b 12.709(3) _cell_length_c 16.795(4) _cell_angle_alpha 90.00 _cell_angle_beta 107.036(4) _cell_angle_gamma 90.00 _cell_volume 2070.0(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5676 _cell_measurement_theta_min 3.0004 _cell_measurement_theta_max 27.4758 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.097 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 8.547 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.2498 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _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 Monochromator' _diffrn_measurement_device_type 'Mercury70 (2x2 bin mode)' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14442 _diffrn_reflns_av_R_equivalents 0.0553 _diffrn_reflns_av_sigmaI/netI 0.0664 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4428 _reflns_number_gt 3566 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0460P)^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 4428 _refine_ls_number_parameters 271 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0397 _refine_ls_R_factor_gt 0.0342 _refine_ls_wR_factor_ref 0.0921 _refine_ls_wR_factor_gt 0.0903 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.120 _refine_ls_shift/su_max 0.027 _refine_ls_shift/su_mean 0.001 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 -0.00300(2) 0.984907(16) 0.131074(13) 0.02202(11) Uani 1 1 d . . . Ca1 Ca 0.06862(10) 0.76799(8) 0.28719(6) 0.0154(2) Uani 1 1 d . . . S1 S 0.3897(3) 0.7368(3) 0.45852(16) 0.0819(8) Uani 1 1 d D . . O1 O -0.2693(5) 0.9545(5) 0.1265(5) 0.070(2) Uani 1 1 d . . . O2 O -0.1293(4) 0.8301(4) 0.1908(3) 0.0311(9) Uani 1 1 d . . . O3 O -0.7449(5) 0.9649(4) 0.1506(4) 0.0539(15) Uani 1 1 d . . . O4 O -0.8364(4) 0.8208(3) 0.1848(2) 0.0283(9) Uani 1 1 d . . . O5 O 0.0435(5) 1.1957(3) 0.1251(2) 0.0367(10) Uani 1 1 d . . . O6 O 0.0349(6) 1.1241(4) 0.0037(2) 0.0422(12) Uani 1 1 d . . . O7 O 0.0877(5) 1.5507(4) -0.1908(3) 0.0425(12) Uani 1 1 d . . . O8 O -0.0118(5) 1.3965(3) -0.2269(2) 0.0369(11) Uani 1 1 d . . . O9 O 0.2765(6) 0.7421(6) 0.3805(4) 0.0770(19) Uani 1 1 d . . . C1 C -0.2468(6) 0.8709(5) 0.1659(4) 0.0326(14) Uani 1 1 d . . . C2 C -0.7349(6) 0.8711(5) 0.1724(4) 0.0298(13) Uani 1 1 d . . . C3 C -0.3665(6) 0.8133(5) 0.1824(4) 0.0316(13) Uani 1 1 d . . . C4 C -0.3537(7) 0.7087(5) 0.2084(5) 0.0410(16) Uani 1 1 d . . . H4 H -0.2691 0.6748 0.2189 0.049 Uiso 1 1 calc R . . C5 C -0.4654(7) 0.6552(5) 0.2187(5) 0.0447(17) Uani 1 1 d . . . H5 H -0.4578 0.5845 0.2334 0.054 Uiso 1 1 calc R . . C6 C -0.5909(6) 0.7083(5) 0.2069(4) 0.0345(14) Uani 1 1 d . . . H6 H -0.6664 0.6727 0.2144 0.041 Uiso 1 1 calc R . . C7 C -0.6032(6) 0.8123(4) 0.1844(4) 0.0257(12) Uani 1 1 d . . . C8 C -0.4903(6) 0.8655(5) 0.1718(4) 0.0298(13) Uani 1 1 d . . . H8 H -0.4983 0.9360 0.1564 0.036 Uiso 1 1 calc R . . C9 C 0.0568(6) 1.1992(4) 0.0526(3) 0.0255(12) Uani 1 1 d . . . C10 C 0.0549(6) 1.4607(5) -0.1730(4) 0.0273(13) Uani 1 1 d . . . C11 C 0.1003(6) 1.3052(4) 0.0268(3) 0.0223(11) Uani 1 1 d . . . C12 C 0.1714(7) 1.3761(5) 0.0855(4) 0.0348(14) Uani 1 1 d . . . H12 H 0.1962 1.3585 0.1417 0.042 Uiso 1 1 calc R . . C13 C 0.2063(8) 1.4739(5) 0.0612(4) 0.0392(17) Uani 1 1 d . . . H13 H 0.2543 1.5218 0.1010 0.047 Uiso 1 1 calc R . . C14 C 0.1700(8) 1.5000(5) -0.0219(5) 0.0371(16) Uani 1 1 d . . . H14 H 0.1944 1.5655 -0.0380 0.044 Uiso 1 1 calc R . . C15 C 0.0976(6) 1.4299(4) -0.0818(3) 0.0249(12) Uani 1 1 d . . . C16 C 0.0651(6) 1.3319(4) -0.0578(3) 0.0241(11) Uani 1 1 d . . . H16 H 0.0198 1.2833 -0.0979 0.029 Uiso 1 1 calc R . . C17 C 0.4741(16) 0.8286(15) 0.4325(14) 0.33(3) Uani 1 1 d D . . H17A H 0.4263 0.8940 0.4312 0.499 Uiso 1 1 calc R . . H17B H 0.4834 0.8142 0.3783 0.499 Uiso 1 1 calc R . . H17C H 0.5639 0.8332 0.4722 0.499 Uiso 1 1 calc R . . C18 C 0.4967(12) 0.6463(10) 0.4482(9) 0.110(4) Uani 1 1 d D . . H18A H 0.5719 0.6415 0.4985 0.165 Uiso 1 1 calc R . . H18B H 0.5316 0.6639 0.4026 0.165 Uiso 1 1 calc R . . H18C H 0.4498 0.5798 0.4374 0.165 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 0.02641(15) 0.01482(14) 0.02475(15) 0.00075(7) 0.00735(10) -0.00023(7) Ca1 0.0232(5) 0.0076(4) 0.0165(5) 0.0033(4) 0.0074(4) 0.0015(4) S1 0.0713(17) 0.098(2) 0.0658(15) -0.0033(14) 0.0043(13) 0.0145(15) O1 0.033(3) 0.060(4) 0.117(5) 0.048(4) 0.019(3) 0.003(3) O2 0.018(2) 0.036(2) 0.038(2) 0.0046(19) 0.0053(18) 0.0023(16) O3 0.031(3) 0.029(3) 0.106(5) 0.017(3) 0.026(3) 0.0041(19) O4 0.022(2) 0.032(2) 0.033(2) -0.0022(18) 0.0112(18) -0.0044(16) O5 0.068(3) 0.022(2) 0.027(2) -0.0011(17) 0.025(2) -0.006(2) O6 0.087(4) 0.018(2) 0.023(2) -0.0034(17) 0.019(2) -0.009(2) O7 0.064(3) 0.020(2) 0.041(3) 0.013(2) 0.012(2) -0.008(2) O8 0.069(3) 0.017(2) 0.020(2) 0.0007(16) 0.006(2) -0.005(2) O9 0.055(4) 0.076(5) 0.079(4) 0.011(4) -0.014(3) 0.017(3) C1 0.021(3) 0.033(3) 0.041(3) 0.009(3) 0.004(3) -0.002(2) C2 0.027(3) 0.025(3) 0.038(3) 0.001(2) 0.009(3) 0.000(2) C3 0.023(3) 0.029(3) 0.040(3) 0.004(3) 0.005(3) 0.000(2) C4 0.033(4) 0.029(4) 0.060(4) 0.012(3) 0.013(3) 0.007(3) C5 0.045(4) 0.024(3) 0.073(5) 0.014(3) 0.029(4) 0.007(3) C6 0.033(3) 0.031(3) 0.043(4) 0.005(3) 0.017(3) -0.003(2) C7 0.022(3) 0.022(3) 0.033(3) 0.000(2) 0.008(2) 0.000(2) C8 0.024(3) 0.028(3) 0.039(3) 0.008(3) 0.012(3) 0.003(2) C9 0.046(4) 0.008(2) 0.025(3) 0.002(2) 0.015(3) -0.002(2) C10 0.041(3) 0.020(3) 0.024(3) 0.009(2) 0.014(3) 0.006(2) C11 0.038(3) 0.011(2) 0.021(3) -0.001(2) 0.014(2) -0.007(2) C12 0.049(4) 0.029(3) 0.023(3) 0.000(2) 0.006(3) -0.008(3) C13 0.055(5) 0.025(3) 0.031(3) -0.003(3) 0.001(3) -0.015(3) C14 0.046(4) 0.025(3) 0.035(4) 0.002(3) 0.003(3) -0.014(3) C15 0.042(3) 0.013(3) 0.021(3) 0.000(2) 0.011(2) -0.002(2) C16 0.039(3) 0.014(2) 0.019(3) -0.002(2) 0.009(2) -0.005(2) C17 0.157(18) 0.55(6) 0.36(3) 0.36(4) 0.18(2) 0.22(3) C18 0.087(9) 0.095(10) 0.117(10) 0.008(8) -0.020(7) 0.025(7) _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 2.554(5) 1_655 ? Pb1 O6 2.593(4) 3_575 ? Pb1 O4 2.670(4) 1_655 ? Pb1 O2 2.696(4) . ? Pb1 O1 2.707(5) . ? Pb1 O5 2.727(4) . ? Pb1 Ca1 3.7265(11) . ? Pb1 Ca1 3.9757(12) 2 ? Ca1 O9 2.252(5) . ? Ca1 O5 2.300(4) 2_545 ? Ca1 O4 2.304(4) 1_655 ? Ca1 O2 2.317(4) . ? Ca1 O8 2.320(4) 3_575 ? Ca1 O7 2.333(5) 4_586 ? Ca1 Pb1 3.9757(12) 2_545 ? S1 O9 1.469(6) . ? S1 C17 1.581(15) . ? S1 C18 1.626(11) . ? O1 C1 1.237(8) . ? O2 C1 1.254(7) . ? O3 C2 1.244(8) . ? O3 Pb1 2.554(5) 1_455 ? O4 C2 1.278(7) . ? O4 Ca1 2.304(4) 1_455 ? O4 Pb1 2.670(4) 1_455 ? O5 C9 1.264(7) . ? O5 Ca1 2.300(4) 2 ? O6 C9 1.235(7) . ? O6 Pb1 2.593(4) 3_575 ? O7 C10 1.252(8) . ? O7 Ca1 2.333(5) 4_585 ? O8 C10 1.259(7) . ? O8 Ca1 2.320(4) 3_575 ? C1 C3 1.511(8) . ? C2 C7 1.492(8) . ? C3 C8 1.385(8) . ? C3 C4 1.394(9) . ? C4 C5 1.375(9) . ? C4 H4 0.9300 . ? C5 C6 1.402(9) . ? C5 H5 0.9300 . ? C6 C7 1.370(8) . ? C6 H6 0.9300 . ? C7 C8 1.398(8) . ? C8 H8 0.9300 . ? C9 C11 1.520(7) . ? C10 C15 1.515(8) . ? C11 C12 1.374(8) . ? C11 C16 1.402(7) . ? C12 C13 1.386(9) . ? C12 H12 0.9300 . ? C13 C14 1.376(10) . ? C13 H13 0.9300 . ? C14 C15 1.383(8) . ? C14 H14 0.9300 . ? C15 C16 1.378(7) . ? C16 H16 0.9300 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 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 O3 Pb1 O6 85.4(2) 1_655 3_575 ? O3 Pb1 O4 49.86(14) 1_655 1_655 ? O6 Pb1 O4 77.43(14) 3_575 1_655 ? O3 Pb1 O2 117.42(14) 1_655 . ? O6 Pb1 O2 89.04(13) 3_575 . ? O4 Pb1 O2 68.08(12) 1_655 . ? O3 Pb1 O1 165.04(19) 1_655 . ? O6 Pb1 O1 91.8(2) 3_575 . ? O4 Pb1 O1 115.19(15) 1_655 . ? O2 Pb1 O1 47.75(15) . . ? O3 Pb1 O5 85.44(16) 1_655 . ? O6 Pb1 O5 118.14(12) 3_575 . ? O4 Pb1 O5 132.90(13) 1_655 . ? O2 Pb1 O5 146.80(13) . . ? O1 Pb1 O5 108.72(18) . . ? O3 Pb1 Ca1 81.66(13) 1_655 . ? O6 Pb1 Ca1 99.66(10) 3_575 . ? O4 Pb1 Ca1 37.87(8) 1_655 . ? O2 Pb1 Ca1 38.22(8) . . ? O1 Pb1 Ca1 84.35(12) . . ? O5 Pb1 Ca1 138.80(9) . . ? O3 Pb1 Ca1 108.34(13) 1_655 2 ? O6 Pb1 Ca1 142.60(10) 3_575 2 ? O4 Pb1 Ca1 138.05(9) 1_655 2 ? O2 Pb1 Ca1 112.72(9) . 2 ? O1 Pb1 Ca1 82.67(17) . 2 ? O5 Pb1 Ca1 34.10(9) . 2 ? Ca1 Pb1 Ca1 116.381(16) . 2 ? O9 Ca1 O5 91.9(2) . 2_545 ? O9 Ca1 O4 92.9(2) . 1_655 ? O5 Ca1 O4 171.12(16) 2_545 1_655 ? O9 Ca1 O2 168.1(2) . . ? O5 Ca1 O2 95.40(16) 2_545 . ? O4 Ca1 O2 81.10(14) 1_655 . ? O9 Ca1 O8 103.5(2) . 3_575 ? O5 Ca1 O8 79.26(15) 2_545 3_575 ? O4 Ca1 O8 92.36(15) 1_655 3_575 ? O2 Ca1 O8 87.03(16) . 3_575 ? O9 Ca1 O7 90.9(2) . 4_586 ? O5 Ca1 O7 109.07(17) 2_545 4_586 ? O4 Ca1 O7 78.30(17) 1_655 4_586 ? O2 Ca1 O7 77.84(17) . 4_586 ? O8 Ca1 O7 163.22(17) 3_575 4_586 ? O9 Ca1 Pb1 123.18(19) . . ? O5 Ca1 Pb1 135.66(12) 2_545 . ? O4 Ca1 Pb1 45.35(11) 1_655 . ? O2 Ca1 Pb1 46.05(10) . . ? O8 Ca1 Pb1 112.77(10) 3_575 . ? O7 Ca1 Pb1 51.01(12) 4_586 . ? O9 Ca1 Pb1 81.09(19) . 2_545 ? O5 Ca1 Pb1 41.68(11) 2_545 2_545 ? O4 Ca1 Pb1 132.09(11) 1_655 2_545 ? O2 Ca1 Pb1 110.55(11) . 2_545 ? O8 Ca1 Pb1 44.79(10) 3_575 2_545 ? O7 Ca1 Pb1 148.61(13) 4_586 2_545 ? Pb1 Ca1 Pb1 153.45(3) . 2_545 ? O9 S1 C17 93.7(8) . . ? O9 S1 C18 108.0(6) . . ? C17 S1 C18 93.4(7) . . ? C1 O1 Pb1 94.7(4) . . ? C1 O2 Ca1 156.6(4) . . ? C1 O2 Pb1 94.7(4) . . ? Ca1 O2 Pb1 95.73(13) . . ? C2 O3 Pb1 97.2(4) . 1_455 ? C2 O4 Ca1 143.0(4) . 1_455 ? C2 O4 Pb1 90.8(4) . 1_455 ? Ca1 O4 Pb1 96.78(14) 1_455 1_455 ? C9 O5 Ca1 144.6(4) . 2 ? C9 O5 Pb1 97.9(3) . . ? Ca1 O5 Pb1 104.21(15) 2 . ? C9 O6 Pb1 160.9(4) . 3_575 ? C10 O7 Ca1 157.7(5) . 4_585 ? C10 O8 Ca1 155.5(4) . 3_575 ? S1 O9 Ca1 162.7(5) . . ? O1 C1 O2 122.8(6) . . ? O1 C1 C3 118.8(5) . . ? O2 C1 C3 118.3(5) . . ? O3 C2 O4 121.8(6) . . ? O3 C2 C7 120.8(5) . . ? O4 C2 C7 117.4(5) . . ? C8 C3 C4 119.6(6) . . ? C8 C3 C1 119.5(6) . . ? C4 C3 C1 121.0(6) . . ? C5 C4 C3 120.5(6) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C4 C5 C6 119.4(6) . . ? C4 C5 H5 120.3 . . ? C6 C5 H5 120.3 . . ? C7 C6 C5 120.6(6) . . ? C7 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? C6 C7 C8 119.7(5) . . ? C6 C7 C2 121.7(5) . . ? C8 C7 C2 118.6(5) . . ? C3 C8 C7 120.1(6) . . ? C3 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? O6 C9 O5 124.3(5) . . ? O6 C9 C11 120.4(5) . . ? O5 C9 C11 115.3(5) . . ? O7 C10 O8 123.1(5) . . ? O7 C10 C15 117.4(5) . . ? O8 C10 C15 119.6(5) . . ? C12 C11 C16 119.5(5) . . ? C12 C11 C9 120.8(5) . . ? C16 C11 C9 119.6(5) . . ? C11 C12 C13 120.2(6) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C14 C13 C12 120.0(6) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 C15 120.7(6) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? C16 C15 C14 119.4(5) . . ? C16 C15 C10 120.5(5) . . ? C14 C15 C10 120.2(5) . . ? C15 C16 C11 120.2(5) . . ? C15 C16 H16 119.9 . . ? C11 C16 H16 119.9 . . ? S1 C17 H17A 109.5 . . ? S1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? S1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? S1 C18 H18A 109.5 . . ? S1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? S1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.933 _refine_diff_density_max 2.382 _refine_diff_density_min -1.469 _refine_diff_density_rms 0.148 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 763446' #TrackingRef 'CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H16 Ca O12 Pb' _chemical_formula_weight 671.58 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' Ca Ca 0.2262 0.3064 '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 I-42d loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x+1/2, y, -z+3/4' 'x+1/2, -y, -z+3/4' '-y+1/2, -x, z+3/4' 'y+1/2, x, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' '-x+1, y+1/2, -z+5/4' 'x+1, -y+1/2, -z+5/4' '-y+1, -x+1/2, z+5/4' 'y+1, x+1/2, z+5/4' _cell_length_a 21.1180(4) _cell_length_b 21.1180(4) _cell_length_c 9.4092(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4196.22(17) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7425 _cell_measurement_theta_min 2.3697 _cell_measurement_theta_max 27.4785 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.126 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2576 _exptl_absorpt_coefficient_mu 8.350 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7373 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _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 Monochromator' _diffrn_measurement_device_type 'Mercury70 (2x2 bin mode)' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15971 _diffrn_reflns_av_R_equivalents 0.0662 _diffrn_reflns_av_sigmaI/netI 0.0289 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2386 _reflns_number_gt 2374 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0558P)^2^+4.5513P] 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 0.060(9) _refine_ls_number_reflns 2386 _refine_ls_number_parameters 150 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0292 _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.0733 _refine_ls_wR_factor_gt 0.0729 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.059 _refine_ls_shift/su_mean 0.003 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 0.303998(3) 0.2500 0.1250 0.02016(1) Uani 1 2 d S . . Ca1 Ca 0.2500 0.391882(17) -0.1250 0.02340(8) Uani 1 2 d S . . O1 O 0.31996(5) 0.30902(6) -0.16594(12) 0.0324(3) Uani 1 1 d . . . O2 O 0.39197(5) 0.28475(6) -0.00168(12) 0.0326(3) Uani 1 1 d . . . O3 O 0.61617(5) 0.28545(6) -0.10578(11) 0.0337(3) Uani 1 1 d . . . O4 O 0.65325(5) 0.33626(5) -0.29241(12) 0.0279(3) Uani 1 1 d . . . O5 O 0.45493(5) 0.35380(7) -0.60106(11) 0.0368(3) Uani 1 1 d D . . H10 H 0.4140(3) 0.361(2) -0.6525(15) 0.48(9) Uiso 1 1 d D . . O6 O 0.17053(11) 0.46586(9) -0.06908(19) 0.1308(6) Uani 1 1 d D . . H11 H 0.1817 0.4965 -0.0027 0.157 Uiso 1 1 calc R . . C1 C 0.37677(6) 0.30273(6) -0.12520(17) 0.0230(3) Uani 1 1 d . . . C2 C 0.60810(7) 0.31455(7) -0.22126(15) 0.0231(3) Uani 1 1 d . . . C3 C 0.42914(6) 0.31644(7) -0.22664(15) 0.0222(3) Uani 1 1 d . . . C4 C 0.49123(7) 0.31219(7) -0.18054(14) 0.0234(3) Uani 1 1 d . . . H4 H 0.4997 0.3018 -0.0864 0.028 Uiso 1 1 calc R . . C5 C 0.54068(6) 0.32326(7) -0.27341(15) 0.0211(3) Uani 1 1 d . . . C6 C 0.52838(7) 0.33900(7) -0.41450(14) 0.0230(3) Uani 1 1 d . . . H6 H 0.5615 0.3475 -0.4769 0.028 Uiso 1 1 calc R . . C7 C 0.46558(7) 0.34181(7) -0.46090(15) 0.0246(4) Uani 1 1 d . . . C8 C 0.41582(6) 0.33110(6) -0.36705(17) 0.0228(3) Uani 1 1 d . . . H8 H 0.3741 0.3337 -0.3982 0.027 Uiso 1 1 calc R . . C9 C 0.10910(17) 0.47004(19) -0.1217(5) 0.1072(13) Uani 1 1 d D . . H9A H 0.0868 0.5032 -0.0730 0.161 Uiso 1 1 calc R . . H9B H 0.0876 0.4305 -0.1068 0.161 Uiso 1 1 calc R . . H9C H 0.1104 0.4793 -0.2215 0.161 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 0.01803(3) 0.02305(3) 0.01940(3) 0.00486(3) 0.000 0.000 Ca1 0.03588(17) 0.02164(14) 0.01267(13) 0.000 -0.01141(17) 0.000 O1 0.0193(5) 0.0493(6) 0.0285(5) 0.0026(5) 0.0040(4) 0.0002(5) O2 0.0229(5) 0.0527(6) 0.0221(5) 0.0143(4) 0.0026(4) -0.0062(5) O3 0.0252(4) 0.0575(6) 0.0184(5) 0.0199(4) 0.0025(4) 0.0065(4) O4 0.0220(5) 0.0341(5) 0.0276(5) 0.0151(4) 0.0012(4) -0.0018(4) O5 0.0316(5) 0.0625(7) 0.0165(5) 0.0061(5) -0.0010(4) 0.0031(5) O6 0.2254(16) 0.1213(9) 0.0458(8) -0.0448(7) -0.0560(9) 0.1359(8) C1 0.0187(5) 0.0258(5) 0.0245(6) 0.0025(8) 0.0043(5) 0.0000(4) C2 0.0197(6) 0.0299(6) 0.0198(5) 0.0061(5) -0.0026(5) -0.0006(5) C3 0.0219(6) 0.0264(6) 0.0184(5) 0.0057(5) 0.0039(5) -0.0006(5) C4 0.0217(6) 0.0319(7) 0.0167(5) 0.0060(5) -0.0006(5) 0.0039(5) C5 0.0201(6) 0.0254(6) 0.0178(5) 0.0036(5) -0.0009(5) 0.0006(5) C6 0.0284(6) 0.0230(6) 0.0176(6) 0.0032(5) -0.0007(5) -0.0073(5) C7 0.0264(6) 0.0315(7) 0.0158(6) 0.0037(5) -0.0010(5) 0.0029(5) C8 0.0211(5) 0.0271(5) 0.0203(5) 0.0006(6) -0.0031(6) 0.0019(4) C9 0.131(3) 0.105(2) 0.085(2) 0.023(2) 0.004(3) 0.032(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 O2 2.3260(11) . ? Pb1 O2 2.3260(11) 14_454 ? Pb1 O4 2.6684(11) 16_444 ? Pb1 O4 2.6684(11) 3_565 ? Pb1 Ca1 3.9763(3) 10 ? Pb1 Ca1 3.9763(3) . ? Ca1 O3 2.3032(11) 7_564 ? Ca1 O3 2.3032(11) 3_565 ? Ca1 O1 2.3223(12) 5_554 ? Ca1 O1 2.3223(12) . ? Ca1 O6 2.352(2) 5_554 ? Ca1 O6 2.352(2) . ? Ca1 Pb1 3.9763(3) 10_554 ? O1 C1 1.2664(17) . ? O2 C1 1.2642(19) . ? O3 C2 1.2599(18) . ? O3 Ca1 2.3032(11) 4_655 ? O4 C2 1.2520(18) . ? O4 Pb1 2.6684(11) 4_655 ? O5 C7 1.3616(17) . ? O5 H10 1.002(10) . ? O6 C9 1.391(4) . ? O6 H11 0.9300 . ? C1 C3 1.489(2) . ? C2 C5 1.517(2) . ? C3 C4 1.3840(19) . ? C3 C8 1.386(2) . ? C4 C5 1.381(2) . ? C4 H4 0.9300 . ? C5 C6 1.3930(19) . ? C6 C7 1.397(2) . ? C6 H6 0.9300 . ? C7 C8 1.391(2) . ? C8 H8 0.9300 . ? 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 O2 Pb1 O2 73.99(6) . 14_454 ? O2 Pb1 O4 74.64(4) . 16_444 ? O2 Pb1 O4 81.78(4) 14_454 16_444 ? O2 Pb1 O4 81.78(4) . 3_565 ? O2 Pb1 O4 74.64(4) 14_454 3_565 ? O4 Pb1 O4 150.41(5) 16_444 3_565 ? O2 Pb1 Ca1 140.35(3) . 10 ? O2 Pb1 Ca1 71.83(3) 14_454 10 ? O4 Pb1 Ca1 81.11(2) 16_444 10 ? O4 Pb1 Ca1 107.52(2) 3_565 10 ? O2 Pb1 Ca1 71.83(3) . . ? O2 Pb1 Ca1 140.35(3) 14_454 . ? O4 Pb1 Ca1 107.52(2) 16_444 . ? O4 Pb1 Ca1 81.11(2) 3_565 . ? Ca1 Pb1 Ca1 146.669(3) 10 . ? O3 Ca1 O3 171.53(6) 7_564 3_565 ? O3 Ca1 O1 83.91(4) 7_564 5_554 ? O3 Ca1 O1 89.70(4) 3_565 5_554 ? O3 Ca1 O1 89.70(4) 7_564 . ? O3 Ca1 O1 83.91(4) 3_565 . ? O1 Ca1 O1 82.21(6) 5_554 . ? O3 Ca1 O6 94.02(5) 7_564 5_554 ? O3 Ca1 O6 91.61(5) 3_565 5_554 ? O1 Ca1 O6 172.46(6) 5_554 5_554 ? O1 Ca1 O6 90.54(6) . 5_554 ? O3 Ca1 O6 91.61(5) 7_564 . ? O3 Ca1 O6 94.02(5) 3_565 . ? O1 Ca1 O6 90.54(6) 5_554 . ? O1 Ca1 O6 172.46(6) . . ? O6 Ca1 O6 96.78(10) 5_554 . ? O3 Ca1 Pb1 45.04(3) 7_564 10_554 ? O3 Ca1 Pb1 126.53(3) 3_565 10_554 ? O1 Ca1 Pb1 49.30(3) 5_554 10_554 ? O1 Ca1 Pb1 61.09(3) . 10_554 ? O6 Ca1 Pb1 124.94(5) 5_554 10_554 ? O6 Ca1 Pb1 115.35(5) . 10_554 ? O3 Ca1 Pb1 126.53(3) 7_564 . ? O3 Ca1 Pb1 45.04(3) 3_565 . ? O1 Ca1 Pb1 61.09(3) 5_554 . ? O1 Ca1 Pb1 49.30(3) . . ? O6 Ca1 Pb1 115.35(5) 5_554 . ? O6 Ca1 Pb1 124.94(5) . . ? Pb1 Ca1 Pb1 82.207(7) 10_554 . ? C1 O1 Ca1 129.16(10) . . ? C1 O2 Pb1 111.29(9) . . ? C2 O3 Ca1 164.08(10) . 4_655 ? C2 O4 Pb1 100.01(9) . 4_655 ? C7 O5 H10 129.6(8) . . ? C9 O6 Ca1 128.9(2) . . ? C9 O6 H11 115.6 . . ? Ca1 O6 H11 115.6 . . ? O2 C1 O1 123.39(13) . . ? O2 C1 C3 117.33(12) . . ? O1 C1 C3 119.28(13) . . ? O4 C2 O3 122.46(13) . . ? O4 C2 C5 119.82(13) . . ? O3 C2 C5 117.71(13) . . ? C4 C3 C8 120.37(13) . . ? C4 C3 C1 119.34(13) . . ? C8 C3 C1 120.25(12) . . ? C5 C4 C3 120.46(13) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C4 C5 C6 120.15(13) . . ? C4 C5 C2 118.97(12) . . ? C6 C5 C2 120.80(12) . . ? C5 C6 C7 119.00(13) . . ? C5 C6 H6 120.5 . . ? C7 C6 H6 120.5 . . ? O5 C7 C8 121.35(13) . . ? O5 C7 C6 117.86(13) . . ? C8 C7 C6 120.77(13) . . ? C3 C8 C7 119.22(12) . . ? C3 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? O6 C9 H9A 109.5 . . ? O6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? O6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.143 _refine_diff_density_min -1.863 _refine_diff_density_rms 0.156 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 763447' #TrackingRef 'CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H15 N O10 Pb Sr' _chemical_formula_weight 700.13 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' Sr Sr -1.5307 3.2498 '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 9.8108(5) _cell_length_b 10.4971(4) _cell_length_c 12.3568(5) _cell_angle_alpha 68.336(8) _cell_angle_beta 87.529(9) _cell_angle_gamma 68.261(8) _cell_volume 1092.09(8) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.105 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 644 _exptl_absorpt_coefficient_mu 10.193 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5067 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _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 Monochromator' _diffrn_measurement_device_type 'Mercury70 (2x2 bin mode)' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8406 _diffrn_reflns_av_R_equivalents 0.0323 _diffrn_reflns_av_sigmaI/netI 0.0566 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 27.49 _reflns_number_total 4659 _reflns_number_gt 4083 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0677P)^2^+4.5500P] 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 4659 _refine_ls_number_parameters 300 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0495 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.1163 _refine_ls_wR_factor_gt 0.1106 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.04881(3) 0.38588(3) 0.72176(2) 0.02245(11) Uani 1 1 d . . . Sr1 Sr -0.04515(6) 0.81461(6) 0.49883(5) 0.01327(14) Uani 1 1 d . . . O1 O 0.1177(8) 0.4700(7) 0.8668(6) 0.0440(17) Uani 1 1 d . . . O2 O 0.0641(8) 0.6663(7) 0.7007(5) 0.0417(16) Uani 1 1 d . . . O3 O 0.1073(7) 1.1204(6) 0.7118(5) 0.0362(14) Uani 1 1 d . . . O4 O 0.1766(7) 1.1222(6) 0.8786(5) 0.0323(13) Uani 1 1 d . . . O5 O 0.1317(6) 0.5759(6) 0.4676(5) 0.0279(12) Uani 1 1 d . . . O6 O 0.1725(6) 0.3756(6) 0.4296(5) 0.0294(13) Uani 1 1 d . . . O7 O 0.6942(7) -0.0085(8) 0.5151(8) 0.055(2) Uani 1 1 d . . . O8 O 0.8653(6) 0.0603(6) 0.5548(6) 0.0334(14) Uani 1 1 d . . . O9 O 0.1453(6) 0.6519(6) 1.1829(4) 0.0262(12) Uani 1 1 d . . . O10 O 0.5741(7) 0.4304(8) 0.7432(6) 0.0424(16) Uani 1 1 d . . . H21 H 0.6635 0.3975 0.7604 0.064 Uiso 1 1 calc R . . N1 N 0.5893(10) 0.8095(13) -0.1503(10) 0.077(3) Uani 1 1 d . . . C1 C 0.1008(9) 0.6043(9) 0.8097(8) 0.0285(17) Uani 1 1 d . . . C2 C 0.1432(8) 1.0597(8) 0.8220(7) 0.0235(15) Uani 1 1 d . . . C3 C 0.2141(7) 0.4460(7) 0.4753(6) 0.0198(14) Uani 1 1 d . . . C4 C 0.7313(8) 0.0761(8) 0.5456(7) 0.0272(17) Uani 1 1 d . . . C5 C 0.1179(9) 0.6906(8) 0.8764(7) 0.0240(15) Uani 1 1 d . . . C6 C 0.1224(9) 0.6346(9) 0.9974(7) 0.0265(17) Uani 1 1 d . . . H6 H 0.1148 0.5431 1.0351 0.032 Uiso 1 1 calc R . . C7 C 0.1379(8) 0.7115(8) 1.0645(7) 0.0218(15) Uani 1 1 d . . . C8 C 0.1470(8) 0.8491(8) 1.0055(7) 0.0227(15) Uani 1 1 d . . . H8 H 0.1589 0.9023 1.0476 0.027 Uiso 1 1 calc R . . C9 C 0.1383(8) 0.9076(8) 0.8840(7) 0.0213(15) Uani 1 1 d . . . C10 C 0.1227(8) 0.8309(8) 0.8181(7) 0.0240(15) Uani 1 1 d . . . H10 H 0.1156 0.8719 0.7367 0.029 Uiso 1 1 calc R . . C11 C 0.3644(8) 0.3734(8) 0.5421(7) 0.0217(15) Uani 1 1 d . . . C12 C 0.4013(8) 0.4323(8) 0.6154(7) 0.0239(16) Uani 1 1 d . . . H12 H 0.3305 0.5130 0.6269 0.029 Uiso 1 1 calc R . . C13 C 0.5440(8) 0.3707(9) 0.6715(7) 0.0263(16) Uani 1 1 d . . . C14 C 0.6537(9) 0.2542(8) 0.6470(7) 0.0263(16) Uani 1 1 d . . . H14 H 0.7509 0.2163 0.6798 0.032 Uiso 1 1 calc R . . C15 C 0.6148(8) 0.1980(8) 0.5741(7) 0.0248(16) Uani 1 1 d . . . C16 C 0.4701(8) 0.2544(8) 0.5238(7) 0.0238(16) Uani 1 1 d . . . H16 H 0.4443 0.2122 0.4779 0.029 Uiso 1 1 calc R . . C17 C 0.551(4) 0.950(5) -0.120(4) 0.057(14) Uani 0.28(3) 1 d P A 1 C18 C 0.747(2) 0.792(3) -0.158(2) 0.153(17) Uani 0.72(3) 1 d P A 2 C19 C 0.551(2) 0.707(4) -0.050(2) 0.102(17) Uani 0.47(3) 1 d P A 1 C20 C 0.487(2) 0.902(4) -0.254(2) 0.132(19) Uani 0.53(3) 1 d P A 2 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 0.03059(17) 0.02109(16) 0.01977(18) -0.00881(12) 0.00350(11) -0.01332(12) Sr1 0.0174(3) 0.0121(3) 0.0125(3) -0.0069(2) 0.0016(2) -0.0058(2) O1 0.082(5) 0.036(3) 0.028(3) -0.011(3) 0.002(3) -0.039(3) O2 0.073(5) 0.030(3) 0.019(3) -0.009(2) -0.015(3) -0.014(3) O3 0.062(4) 0.027(3) 0.022(3) -0.008(2) -0.001(3) -0.020(3) O4 0.049(3) 0.024(3) 0.027(3) -0.012(2) -0.002(3) -0.016(3) O5 0.024(3) 0.027(3) 0.035(3) -0.018(2) 0.003(2) -0.006(2) O6 0.028(3) 0.025(3) 0.044(4) -0.020(3) -0.002(2) -0.011(2) O7 0.029(3) 0.051(4) 0.109(7) -0.060(5) 0.006(4) -0.011(3) O8 0.021(3) 0.036(3) 0.053(4) -0.025(3) 0.012(3) -0.014(2) O9 0.033(3) 0.036(3) 0.013(3) -0.007(2) 0.003(2) -0.020(2) O10 0.033(3) 0.055(4) 0.045(4) -0.033(3) -0.007(3) -0.008(3) N1 0.037(5) 0.085(8) 0.068(7) -0.002(6) 0.007(5) -0.009(5) C1 0.032(4) 0.029(4) 0.031(5) -0.013(3) 0.002(3) -0.015(3) C2 0.030(4) 0.018(3) 0.021(4) -0.009(3) 0.003(3) -0.006(3) C3 0.021(3) 0.018(3) 0.018(4) -0.005(3) 0.006(3) -0.007(3) C4 0.026(4) 0.023(4) 0.031(5) -0.013(3) 0.000(3) -0.005(3) C5 0.035(4) 0.024(4) 0.019(4) -0.011(3) 0.004(3) -0.015(3) C6 0.034(4) 0.026(4) 0.025(4) -0.010(3) -0.001(3) -0.016(3) C7 0.023(3) 0.024(4) 0.017(4) -0.011(3) 0.001(3) -0.004(3) C8 0.028(4) 0.020(3) 0.021(4) -0.008(3) -0.001(3) -0.011(3) C9 0.027(4) 0.018(3) 0.020(4) -0.008(3) 0.002(3) -0.010(3) C10 0.036(4) 0.028(4) 0.011(4) -0.006(3) 0.004(3) -0.017(3) C11 0.023(3) 0.019(3) 0.021(4) -0.004(3) 0.001(3) -0.008(3) C12 0.021(3) 0.024(4) 0.027(4) -0.013(3) 0.006(3) -0.007(3) C13 0.023(4) 0.033(4) 0.022(4) -0.012(3) -0.001(3) -0.009(3) C14 0.029(4) 0.024(4) 0.024(4) -0.006(3) 0.003(3) -0.011(3) C15 0.022(3) 0.023(4) 0.029(4) -0.009(3) 0.005(3) -0.009(3) C16 0.028(4) 0.021(3) 0.029(4) -0.011(3) 0.006(3) -0.015(3) C17 0.04(2) 0.09(3) 0.07(3) -0.06(3) -0.003(18) -0.023(19) C18 0.032(9) 0.15(2) 0.13(2) 0.072(18) 0.020(11) -0.001(11) C19 0.031(12) 0.11(3) 0.059(18) 0.062(17) 0.005(11) -0.013(13) C20 0.027(10) 0.20(4) 0.045(14) 0.075(18) -0.014(9) -0.026(15) _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 O9 2.278(5) 2_567 ? Pb1 O1 2.483(6) . ? Pb1 O4 2.582(5) 1_545 ? Pb1 O3 2.678(6) 1_545 ? Pb1 O6 2.711(5) 2_566 ? Pb1 Sr1 4.0199(7) 2_566 ? Pb1 Sr1 4.0847(8) . ? Sr1 O2 2.434(6) . ? Sr1 O3 2.476(6) 2_576 ? Sr1 O8 2.500(5) 2_666 ? Sr1 O7 2.597(6) 1_465 ? Sr1 O6 2.604(5) 2_566 ? Sr1 O5 2.622(5) . ? Sr1 O8 2.736(6) 1_465 ? Sr1 C4 3.047(8) 1_465 ? Sr1 Pb1 4.0199(7) 2_566 ? Sr1 Sr1 4.3099(11) 2_576 ? O1 C1 1.270(10) . ? O2 C1 1.260(10) . ? O3 C2 1.272(10) . ? O3 Sr1 2.476(6) 2_576 ? O3 Pb1 2.678(6) 1_565 ? O4 C2 1.244(9) . ? O4 Pb1 2.582(5) 1_565 ? O5 C3 1.272(9) . ? O6 C3 1.257(9) . ? O6 Sr1 2.604(5) 2_566 ? O6 Pb1 2.711(5) 2_566 ? O7 C4 1.250(10) . ? O7 Sr1 2.597(6) 1_645 ? O8 C4 1.267(9) . ? O8 Sr1 2.500(5) 2_666 ? O8 Sr1 2.736(6) 1_645 ? O9 C7 1.355(9) . ? O9 Pb1 2.278(5) 2_567 ? O10 C13 1.354(10) . ? O10 H21 0.8200 . ? N1 C20 1.43(2) . ? N1 C19 1.46(2) . ? N1 C18 1.50(2) . ? N1 C17 1.56(4) . ? C1 C5 1.485(11) . ? C2 C9 1.512(10) . ? C3 C11 1.498(9) . ? C4 C15 1.511(11) . ? C4 Sr1 3.047(8) 1_645 ? C5 C6 1.386(11) . ? C5 C10 1.398(10) . ? C6 C7 1.400(11) . ? C6 H6 0.9300 . ? C7 C8 1.392(10) . ? C8 C9 1.389(11) . ? C8 H8 0.9300 . ? C9 C10 1.386(10) . ? C10 H10 0.9300 . ? C11 C16 1.384(11) . ? C11 C12 1.394(11) . ? C12 C13 1.393(10) . ? C12 H12 0.9300 . ? C13 C14 1.420(11) . ? C14 C15 1.376(11) . ? C14 H14 0.9300 . ? C15 C16 1.391(10) . ? C16 H16 0.9300 . ? 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 O9 Pb1 O1 92.4(2) 2_567 . ? O9 Pb1 O4 78.44(19) 2_567 1_545 ? O1 Pb1 O4 85.10(19) . 1_545 ? O9 Pb1 O3 84.4(2) 2_567 1_545 ? O1 Pb1 O3 134.3(2) . 1_545 ? O4 Pb1 O3 49.57(17) 1_545 1_545 ? O9 Pb1 O6 81.63(18) 2_567 2_566 ? O1 Pb1 O6 106.11(19) . 2_566 ? O4 Pb1 O6 157.54(18) 1_545 2_566 ? O3 Pb1 O6 118.33(17) 1_545 2_566 ? O9 Pb1 Sr1 96.97(14) 2_567 2_566 ? O1 Pb1 Sr1 165.67(18) . 2_566 ? O4 Pb1 Sr1 86.22(12) 1_545 2_566 ? O3 Pb1 Sr1 36.98(12) 1_545 2_566 ? O6 Pb1 Sr1 86.01(12) 2_566 2_566 ? O9 Pb1 Sr1 113.91(14) 2_567 . ? O1 Pb1 Sr1 83.38(14) . . ? O4 Pb1 Sr1 163.40(13) 1_545 . ? O3 Pb1 Sr1 139.02(13) 1_545 . ? O6 Pb1 Sr1 38.82(11) 2_566 . ? Sr1 Pb1 Sr1 102.472(13) 2_566 . ? O2 Sr1 O3 159.6(2) . 2_576 ? O2 Sr1 O8 95.2(2) . 2_666 ? O3 Sr1 O8 89.2(2) 2_576 2_666 ? O2 Sr1 O7 104.6(3) . 1_465 ? O3 Sr1 O7 91.9(2) 2_576 1_465 ? O8 Sr1 O7 112.7(2) 2_666 1_465 ? O2 Sr1 O6 76.6(2) . 2_566 ? O3 Sr1 O6 94.53(19) 2_576 2_566 ? O8 Sr1 O6 165.62(18) 2_666 2_566 ? O7 Sr1 O6 81.1(2) 1_465 2_566 ? O2 Sr1 O5 82.0(2) . . ? O3 Sr1 O5 77.84(19) 2_576 . ? O8 Sr1 O5 93.68(17) 2_666 . ? O7 Sr1 O5 151.70(18) 1_465 . ? O6 Sr1 O5 73.62(17) 2_566 . ? O2 Sr1 O8 88.1(2) . 1_465 ? O3 Sr1 O8 111.97(19) 2_576 1_465 ? O8 Sr1 O8 69.3(2) 2_666 1_465 ? O7 Sr1 O8 48.47(17) 1_465 1_465 ? O6 Sr1 O8 121.48(17) 2_566 1_465 ? O5 Sr1 O8 159.55(16) . 1_465 ? O2 Sr1 C4 96.5(2) . 1_465 ? O3 Sr1 C4 103.3(2) 2_576 1_465 ? O8 Sr1 C4 91.5(2) 2_666 1_465 ? O7 Sr1 C4 23.93(19) 1_465 1_465 ? O6 Sr1 C4 101.07(19) 2_566 1_465 ? O5 Sr1 C4 174.68(19) . 1_465 ? O8 Sr1 C4 24.56(18) 1_465 1_465 ? O2 Sr1 Pb1 119.91(14) . 2_566 ? O3 Sr1 Pb1 40.58(13) 2_576 2_566 ? O8 Sr1 Pb1 109.92(14) 2_666 2_566 ? O7 Sr1 Pb1 113.25(15) 1_465 2_566 ? O6 Sr1 Pb1 65.72(13) 2_566 2_566 ? O5 Sr1 Pb1 44.16(12) . 2_566 ? O8 Sr1 Pb1 151.44(13) 1_465 2_566 ? C4 Sr1 Pb1 134.32(15) 1_465 2_566 ? O2 Sr1 Pb1 44.85(14) . . ? O3 Sr1 Pb1 117.76(13) 2_576 . ? O8 Sr1 Pb1 125.86(14) 2_666 . ? O7 Sr1 Pb1 112.19(19) 1_465 . ? O6 Sr1 Pb1 40.74(12) 2_566 . ? O5 Sr1 Pb1 53.63(13) . . ? O8 Sr1 Pb1 127.26(14) 1_465 . ? C4 Sr1 Pb1 122.01(16) 1_465 . ? Pb1 Sr1 Pb1 77.528(13) 2_566 . ? O2 Sr1 Sr1 91.86(14) . 2_576 ? O3 Sr1 Sr1 103.27(13) 2_576 2_576 ? O8 Sr1 Sr1 36.44(13) 2_666 2_576 ? O7 Sr1 Sr1 78.64(14) 1_465 2_576 ? O6 Sr1 Sr1 153.33(13) 2_566 2_576 ? O5 Sr1 Sr1 129.21(12) . 2_576 ? O8 Sr1 Sr1 32.87(11) 1_465 2_576 ? C4 Sr1 Sr1 55.81(15) 1_465 2_576 ? Pb1 Sr1 Sr1 139.06(2) 2_566 2_576 ? Pb1 Sr1 Sr1 136.41(2) . 2_576 ? C1 O1 Pb1 105.4(5) . . ? C1 O2 Sr1 170.0(6) . . ? C2 O3 Sr1 167.9(5) . 2_576 ? C2 O3 Pb1 89.6(4) . 1_565 ? Sr1 O3 Pb1 102.44(19) 2_576 1_565 ? C2 O4 Pb1 94.7(4) . 1_565 ? C3 O5 Sr1 167.7(5) . . ? C3 O6 Sr1 135.1(5) . 2_566 ? C3 O6 Pb1 96.4(4) . 2_566 ? Sr1 O6 Pb1 100.44(17) 2_566 2_566 ? C4 O7 Sr1 98.7(5) . 1_645 ? C4 O8 Sr1 145.9(5) . 2_666 ? C4 O8 Sr1 91.6(5) . 1_645 ? Sr1 O8 Sr1 110.7(2) 2_666 1_645 ? C7 O9 Pb1 122.5(4) . 2_567 ? C13 O10 H21 109.5 . . ? C20 N1 C19 120.4(16) . . ? C20 N1 C18 118.4(15) . . ? C19 N1 C18 119.4(14) . . ? C20 N1 C17 88(2) . . ? C19 N1 C17 104(3) . . ? C18 N1 C17 92(2) . . ? O2 C1 O1 122.1(7) . . ? O2 C1 C5 120.0(7) . . ? O1 C1 C5 117.9(7) . . ? O4 C2 O3 122.6(7) . . ? O4 C2 C9 120.4(7) . . ? O3 C2 C9 117.0(7) . . ? O6 C3 O5 122.0(6) . . ? O6 C3 C11 118.9(6) . . ? O5 C3 C11 119.2(7) . . ? O7 C4 O8 121.2(7) . . ? O7 C4 C15 119.5(7) . . ? O8 C4 C15 119.3(7) . . ? O7 C4 Sr1 57.4(4) . 1_645 ? O8 C4 Sr1 63.9(4) . 1_645 ? C15 C4 Sr1 175.6(5) . 1_645 ? C6 C5 C10 119.6(7) . . ? C6 C5 C1 119.7(7) . . ? C10 C5 C1 120.7(7) . . ? C5 C6 C7 122.1(7) . . ? C5 C6 H6 119.0 . . ? C7 C6 H6 119.0 . . ? O9 C7 C8 121.8(7) . . ? O9 C7 C6 120.5(7) . . ? C8 C7 C6 117.7(7) . . ? C9 C8 C7 120.5(7) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C10 C9 C8 121.5(7) . . ? C10 C9 C2 119.2(7) . . ? C8 C9 C2 119.3(7) . . ? C9 C10 C5 118.7(7) . . ? C9 C10 H10 120.7 . . ? C5 C10 H10 120.7 . . ? C16 C11 C12 120.0(7) . . ? C16 C11 C3 119.6(7) . . ? C12 C11 C3 120.2(7) . . ? C13 C12 C11 120.2(7) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? O10 C13 C12 118.0(7) . . ? O10 C13 C14 122.5(7) . . ? C12 C13 C14 119.4(7) . . ? C15 C14 C13 119.3(7) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C14 C15 C16 120.9(7) . . ? C14 C15 C4 119.7(7) . . ? C16 C15 C4 119.4(7) . . ? C11 C16 C15 120.1(7) . . ? C11 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? _diffrn_measured_fraction_theta_max 0.931 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.931 _refine_diff_density_max 2.342 _refine_diff_density_min -1.818 _refine_diff_density_rms 0.222 #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 763448' #TrackingRef 'CIFs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H28 Ca O14 Pb S4' _chemical_formula_weight 1012.05 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' Ca Ca 0.2262 0.3064 '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' S S 0.1246 0.1234 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 11.4429(14) _cell_length_b 23.6717(14) _cell_length_c 8.1660(9) _cell_angle_alpha 90.00 _cell_angle_beta 128.596(4) _cell_angle_gamma 90.00 _cell_volume 1728.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2785 _cell_measurement_theta_min 3.1917 _cell_measurement_theta_max 27.4797 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.944 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 996 _exptl_absorpt_coefficient_mu 5.340 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7357 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _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 Monochromator' _diffrn_measurement_device_type 'Mercury70 (2x2 bin mode)' _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6567 _diffrn_reflns_av_R_equivalents 0.0203 _diffrn_reflns_av_sigmaI/netI 0.0213 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 27.47 _reflns_number_total 2022 _reflns_number_gt 2005 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_data_reduction 'CrystalClear (Rigaku/MSC Inc., 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0555P)^2^+10.1280P] 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 2022 _refine_ls_number_parameters 125 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0354 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_ref 0.0934 _refine_ls_wR_factor_gt 0.0928 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.097 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.5000 0.0000 1.0000 0.02554(13) Uani 1 4 d S . . Ca1 Ca 0.5000 0.0000 0.5000 0.0094(3) Uani 1 4 d S . . S1 S 0.0000 0.26920(6) 0.0000 0.0210(3) Uani 1 2 d S . . S2 S 0.20760(17) 0.0000 -0.0154(2) 0.0277(3) Uani 1 2 d S . . O1 O 0.3100(6) 0.07354(19) 0.7557(8) 0.0533(12) Uani 1 1 d . . . O2 O 0.4592(4) 0.06456(13) 0.6712(5) 0.0271(7) Uani 1 1 d . . . O3 O -0.0909(4) 0.29970(14) 0.0363(6) 0.0306(7) Uani 1 1 d . . . O4 O 0.2451(5) 0.0000 0.1984(7) 0.0291(10) Uani 1 2 d S . . C1 C 0.3520(6) 0.08764(19) 0.6532(8) 0.0283(9) Uani 1 1 d . . . C2 C 0.2718(5) 0.13567(18) 0.5003(7) 0.0211(8) Uani 1 1 d . . . C3 C 0.3010(5) 0.14900(19) 0.3627(7) 0.0236(9) Uani 1 1 d . . . H3 H 0.3737 0.1291 0.3688 0.028 Uiso 1 1 calc R . . C4 C 0.2225(5) 0.19175(19) 0.2171(7) 0.0235(8) Uani 1 1 d . . . H4 H 0.2430 0.2010 0.1266 0.028 Uiso 1 1 calc R . . C5 C 0.1127(4) 0.22074(17) 0.2071(6) 0.0197(8) Uani 1 1 d . . . C6 C 0.0836(5) 0.20900(19) 0.3454(7) 0.0240(9) Uani 1 1 d . . . H6 H 0.0114 0.2292 0.3395 0.029 Uiso 1 1 calc R . . C7 C 0.1642(5) 0.16658(19) 0.4920(7) 0.0241(9) Uani 1 1 d . . . H7 H 0.1465 0.1585 0.5863 0.029 Uiso 1 1 calc R . . C8 C 0.0824(9) 0.0575(4) -0.1546(11) 0.065(2) Uani 1 1 d . . . H8A H 0.0085 0.0473 -0.2992 0.098 Uiso 1 1 calc R . . H8B H 0.1371 0.0899 -0.1444 0.098 Uiso 1 1 calc R . . H8C H 0.0339 0.0664 -0.0952 0.098 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 0.03027(19) 0.02369(18) 0.02261(18) 0.000 0.01647(15) 0.000 Ca1 0.0167(6) 0.0075(6) 0.0080(6) 0.000 0.0097(5) 0.000 S1 0.0224(6) 0.0184(6) 0.0247(7) 0.000 0.0159(6) 0.000 S2 0.0236(7) 0.0402(9) 0.0218(7) 0.000 0.0154(6) 0.000 O1 0.075(3) 0.047(2) 0.078(3) 0.031(2) 0.068(3) 0.022(2) O2 0.0383(17) 0.0210(15) 0.0255(15) 0.0001(12) 0.0216(14) 0.0081(13) O3 0.0347(17) 0.0265(16) 0.0384(19) 0.0002(14) 0.0266(16) 0.0084(13) O4 0.026(2) 0.043(3) 0.019(2) 0.000 0.0143(19) 0.000 C1 0.038(2) 0.0171(19) 0.034(2) 0.0012(17) 0.024(2) 0.0017(17) C2 0.025(2) 0.0180(19) 0.024(2) -0.0023(16) 0.0168(17) -0.0023(15) C3 0.0216(19) 0.027(2) 0.026(2) -0.0003(17) 0.0169(18) 0.0033(16) C4 0.0242(19) 0.029(2) 0.026(2) 0.0035(17) 0.0198(18) 0.0025(16) C5 0.0173(17) 0.0212(19) 0.0197(18) -0.0021(15) 0.0111(15) -0.0016(14) C6 0.0235(19) 0.026(2) 0.027(2) -0.0012(17) 0.0183(18) 0.0021(16) C7 0.029(2) 0.026(2) 0.028(2) -0.0005(17) 0.0232(19) 0.0010(17) C8 0.067(4) 0.094(6) 0.052(4) 0.039(4) 0.045(4) 0.047(4) _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 2.515(4) 6 ? Pb1 O1 2.515(4) 2_657 ? Pb1 O1 2.515(4) . ? Pb1 O1 2.515(4) 5_657 ? Ca1 O2 2.307(3) . ? Ca1 O2 2.307(3) 6 ? Ca1 O2 2.307(3) 5_656 ? Ca1 O2 2.307(3) 2_656 ? Ca1 O4 2.369(5) . ? Ca1 O4 2.369(5) 5_656 ? Ca1 S2 3.3674(16) . ? Ca1 S2 3.3674(16) 5_656 ? S1 O3 1.440(3) . ? S1 O3 1.440(3) 2 ? S1 C5 1.766(4) 2 ? S1 C5 1.766(4) . ? S2 O4 1.516(5) . ? S2 C8 1.780(7) 6 ? S2 C8 1.780(7) . ? O1 C1 1.243(6) . ? O2 C1 1.265(6) . ? C1 C2 1.505(6) . ? C2 C3 1.394(6) . ? C2 C7 1.398(6) . ? C3 C4 1.383(6) . ? C3 H3 0.9300 . ? C4 C5 1.389(6) . ? C4 H4 0.9300 . ? C5 C6 1.391(6) . ? C6 C7 1.384(6) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 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 O1 Pb1 O1 180.00 6 2_657 ? O1 Pb1 O1 87.6(3) 6 . ? O1 Pb1 O1 92.4(3) 2_657 . ? O1 Pb1 O1 92.4(3) 6 5_657 ? O1 Pb1 O1 87.6(3) 2_657 5_657 ? O1 Pb1 O1 180.00 . 5_657 ? O2 Ca1 O2 82.97(17) . 6 ? O2 Ca1 O2 180.0 . 5_656 ? O2 Ca1 O2 97.03(17) 6 5_656 ? O2 Ca1 O2 97.03(17) . 2_656 ? O2 Ca1 O2 180.00 6 2_656 ? O2 Ca1 O2 82.97(17) 5_656 2_656 ? O2 Ca1 O4 92.68(12) . . ? O2 Ca1 O4 92.68(12) 6 . ? O2 Ca1 O4 87.32(12) 5_656 . ? O2 Ca1 O4 87.32(12) 2_656 . ? O2 Ca1 O4 87.32(12) . 5_656 ? O2 Ca1 O4 87.32(12) 6 5_656 ? O2 Ca1 O4 92.68(12) 5_656 5_656 ? O2 Ca1 O4 92.68(12) 2_656 5_656 ? O4 Ca1 O4 180.0 . 5_656 ? O2 Ca1 S2 109.79(8) . . ? O2 Ca1 S2 109.79(8) 6 . ? O2 Ca1 S2 70.21(8) 5_656 . ? O2 Ca1 S2 70.21(8) 2_656 . ? O4 Ca1 S2 23.29(12) . . ? O4 Ca1 S2 156.71(12) 5_656 . ? O2 Ca1 S2 70.21(8) . 5_656 ? O2 Ca1 S2 70.21(8) 6 5_656 ? O2 Ca1 S2 109.79(8) 5_656 5_656 ? O2 Ca1 S2 109.79(8) 2_656 5_656 ? O4 Ca1 S2 156.71(12) . 5_656 ? O4 Ca1 S2 23.29(12) 5_656 5_656 ? S2 Ca1 S2 180.00 . 5_656 ? O3 S1 O3 119.8(3) . 2 ? O3 S1 C5 109.44(19) . 2 ? O3 S1 C5 108.6(2) 2 2 ? O3 S1 C5 108.6(2) . . ? O3 S1 C5 109.44(19) 2 . ? C5 S1 C5 99.0(3) 2 . ? O4 S2 C8 105.8(3) . 6 ? O4 S2 C8 105.8(3) . . ? C8 S2 C8 99.8(7) 6 . ? O4 S2 Ca1 38.16(18) . . ? C8 S2 Ca1 125.1(3) 6 . ? C8 S2 Ca1 125.1(3) . . ? C1 O1 Pb1 102.3(3) . . ? C1 O2 Ca1 139.8(3) . . ? S2 O4 Ca1 118.6(3) . . ? O1 C1 O2 124.1(4) . . ? O1 C1 C2 118.0(4) . . ? O2 C1 C2 117.9(4) . . ? C3 C2 C7 119.3(4) . . ? C3 C2 C1 120.8(4) . . ? C7 C2 C1 119.9(4) . . ? C4 C3 C2 120.3(4) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 119.4(4) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? C4 C5 C6 121.3(4) . . ? C4 C5 S1 118.1(3) . . ? C6 C5 S1 120.4(3) . . ? C7 C6 C5 118.7(4) . . ? C7 C6 H6 120.7 . . ? C5 C6 H6 120.7 . . ? C6 C7 C2 120.9(4) . . ? C6 C7 H7 119.6 . . ? C2 C7 H7 119.6 . . ? S2 C8 H8A 109.5 . . ? S2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? S2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 3.044 _refine_diff_density_min -0.687 _refine_diff_density_rms 0.175 #===END