data_payun _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H7 O8 Pb' _chemical_formula_weight 414.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'O' 'O' 0.0106 0.0060 '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' 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.3434(2) _cell_length_b 6.4566(2) _cell_length_c 12.0640(9) _cell_angle_alpha 99.233(7) _cell_angle_beta 102.810(7) _cell_angle_gamma 101.562(7) _cell_volume 461.04(4) _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 ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.984 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 378 _exptl_absorpt_coefficient_mu 18.321 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.1576 _exptl_absorpt_correction_T_max 0.3521 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13939 _diffrn_reflns_av_R_equivalents 0.0335 _diffrn_reflns_av_sigmaI/netI 0.0206 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.30 _diffrn_reflns_theta_max 27.47 _reflns_number_total 2096 _reflns_number_gt 2021 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0160P)^2^+0.5104P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2096 _refine_ls_number_parameters 169 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0180 _refine_ls_R_factor_gt 0.0169 _refine_ls_wR_factor_ref 0.0381 _refine_ls_wR_factor_gt 0.0377 _refine_ls_goodness_of_fit_ref 1.133 _refine_ls_restrained_S_all 1.133 _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 Pb Pb 0.93481(2) 0.726901(19) 0.903731(10) 0.02459(5) Uani 1 1 d . . . O1 O 0.5932(4) 0.4434(4) 0.8325(2) 0.0339(6) Uani 1 1 d . . . O2 O 0.5532(5) 0.6669(5) 0.7144(2) 0.0380(7) Uani 1 1 d . . . O3 O 0.0411(4) 0.5552(4) 0.72680(19) 0.0231(5) Uani 1 1 d D . . O4 O 1.1410(5) 0.1017(4) 0.8412(2) 0.0320(6) Uani 1 1 d . . . O5 O 0.9137(4) 0.5834(4) 0.08364(19) 0.0273(5) Uani 1 1 d . . . O6 O 0.5850(4) 0.2617(5) 0.4907(2) 0.0377(6) Uani 1 1 d D . . O7 O 0.9051(4) 0.2444(4) 0.4477(2) 0.0307(6) Uani 1 1 d . . . OW O 0.3573(6) 0.9253(6) 0.0711(4) 0.0613(10) Uani 1 1 d D . . C1 C 0.4878(6) 0.4916(6) 0.7418(3) 0.0231(7) Uani 1 1 d . . . C2 C 0.2797(6) 0.3266(6) 0.6663(3) 0.0229(7) Uani 1 1 d . . . C3 C 0.0732(5) 0.3405(5) 0.7121(3) 0.0184(6) Uani 1 1 d . . . C4 C 0.1047(5) 0.2794(5) 0.8324(3) 0.0205(6) Uani 1 1 d . . . C5 C 0.8597(6) 0.1779(6) 0.6318(3) 0.0219(7) Uani 1 1 d . . . C6 C 0.7866(6) 0.2323(5) 0.5143(3) 0.0217(7) Uani 1 1 d . . . H1 H 0.252(6) 0.350(6) 0.585(3) 0.025(10) Uiso 1 1 d . . . H2 H 0.304(6) 0.174(6) 0.666(3) 0.026(10) Uiso 1 1 d . . . H3 H 0.756(5) 0.182(5) 0.681(3) 0.006(7) Uiso 1 1 d . . . H4 H 0.883(6) 0.033(6) 0.621(3) 0.017(9) Uiso 1 1 d . . . H5 H 0.065(8) 0.620(7) 0.670(3) 0.049(14) Uiso 1 1 d D . . H6 H 0.542(9) 0.277(8) 0.420(3) 0.053(14) Uiso 1 1 d D . . H7 H 0.407(9) 0.836(8) 0.108(4) 0.061(17) Uiso 1 1 d D . . H8 H 0.443(17) 1.003(15) 0.036(9) 0.06(3) Uiso 0.50 1 d PD . . 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 Pb 0.03186(9) 0.02008(8) 0.02047(7) 0.00385(5) 0.00858(5) 0.00180(5) O1 0.0293(14) 0.0366(15) 0.0299(13) 0.0157(11) -0.0021(11) -0.0010(11) O2 0.0318(15) 0.0365(15) 0.0372(15) 0.0203(12) -0.0054(12) -0.0044(12) O3 0.0357(14) 0.0198(11) 0.0194(11) 0.0089(9) 0.0122(10) 0.0103(10) O4 0.0408(15) 0.0291(14) 0.0336(14) 0.0172(11) 0.0124(12) 0.0140(12) O5 0.0375(14) 0.0317(13) 0.0180(11) 0.0092(10) 0.0109(10) 0.0135(11) O6 0.0260(14) 0.0617(19) 0.0300(14) 0.0224(13) 0.0051(11) 0.0136(13) O7 0.0350(14) 0.0425(15) 0.0215(12) 0.0129(11) 0.0121(11) 0.0154(12) OW 0.044(2) 0.056(2) 0.103(3) 0.044(2) 0.032(2) 0.0190(17) C1 0.0214(16) 0.0301(18) 0.0204(15) 0.0068(13) 0.0073(13) 0.0086(14) C2 0.0236(17) 0.0254(17) 0.0197(15) 0.0038(13) 0.0078(13) 0.0046(14) C3 0.0191(15) 0.0191(15) 0.0168(14) 0.0048(12) 0.0045(12) 0.0040(12) C4 0.0183(15) 0.0257(17) 0.0185(15) 0.0092(13) 0.0055(12) 0.0035(13) C5 0.0206(16) 0.0248(17) 0.0189(15) 0.0062(13) 0.0042(13) 0.0027(13) C6 0.0259(17) 0.0172(15) 0.0186(15) 0.0027(12) 0.0030(13) 0.0015(13) _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 Pb O5 2.401(2) 2_766 ? Pb O1 2.422(3) . ? Pb O5 2.512(2) 1_556 ? Pb O3 2.533(2) 1_655 ? Pb O4 2.809(3) 1_565 ? Pb O2 2.849(3) . ? Pb OW 2.880(4) 1_656 ? Pb C1 3.005(4) . ? Pb OW 3.204(4) 2_676 ? Pb C4 3.254(3) 2_667 ? Pb O4 3.271(3) 2_767 ? Pb C4 3.334(3) 1_655 ? O1 C1 1.268(4) . ? O1 Pb 4.303(2) 2_767 ? O2 C1 1.248(4) . ? O3 C3 1.430(4) . ? O3 Pb 2.533(2) 1_455 ? O3 H5 0.88(3) . ? O4 C4 1.230(4) 1_655 ? O4 Pb 2.809(3) 1_545 ? O4 Pb 3.271(3) 2_767 ? O5 C4 1.277(4) 2_666 ? O5 Pb 2.401(2) 2_766 ? O5 Pb 2.512(2) 1_554 ? O5 Pb 4.334(2) 2_776 ? O6 C6 1.306(4) . ? O6 H6 0.86(3) . ? O7 C6 1.217(4) . ? O7 Pb 4.596(2) 2_766 ? OW Pb 2.880(4) 1_454 ? OW Pb 3.204(4) 2_676 ? OW Pb 4.335(4) 2_666 ? OW Pb 4.520(4) 2_776 ? OW H7 0.86(3) . ? OW H8 0.89(3) . ? C1 C2 1.516(5) . ? C1 Pb 4.759(3) 1_455 ? C2 C3 1.544(4) . ? C2 Pb 4.727(3) 1_455 ? C2 H1 0.99(4) . ? C2 H2 1.03(4) . ? C3 C4 1.545(4) . ? C3 C5 1.548(4) 1_455 ? C3 Pb 3.502(3) 1_455 ? C3 Pb 4.734(3) 2_667 ? C4 O4 1.230(4) 1_455 ? C4 O5 1.277(4) 2_666 ? C4 Pb 3.254(3) 2_667 ? C4 Pb 3.334(3) 1_455 ? C4 Pb 3.805(3) 1_445 ? C5 C6 1.511(4) . ? C5 C3 1.548(4) 1_655 ? C5 Pb 4.733(3) 1_545 ? C5 H3 0.98(3) . ? C5 H4 0.97(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 O5 Pb O1 80.49(9) 2_766 . ? O5 Pb O5 66.09(9) 2_766 1_556 ? O1 Pb O5 78.65(8) . 1_556 ? O5 Pb O3 62.58(7) 2_766 1_655 ? O1 Pb O3 85.40(9) . 1_655 ? O5 Pb O3 128.00(7) 1_556 1_655 ? O5 Pb O4 124.62(8) 2_766 1_565 ? O1 Pb O4 138.38(8) . 1_565 ? O5 Pb O4 139.35(8) 1_556 1_565 ? O3 Pb O4 80.31(8) 1_655 1_565 ? O5 Pb O2 115.56(9) 2_766 . ? O1 Pb O2 48.42(8) . . ? O5 Pb O2 122.47(8) 1_556 . ? O3 Pb O2 75.19(9) 1_655 . ? O4 Pb O2 90.05(8) 1_565 . ? O5 Pb OW 79.64(10) 2_766 1_656 ? O1 Pb OW 150.97(9) . 1_656 ? O5 Pb OW 74.02(10) 1_556 1_656 ? O3 Pb OW 103.76(10) 1_655 1_656 ? O4 Pb OW 70.65(9) 1_565 1_656 ? O2 Pb OW 160.42(9) . 1_656 ? O5 Pb C1 97.19(9) 2_766 . ? O1 Pb C1 24.09(9) . . ? O5 Pb C1 101.25(9) 1_556 . ? O3 Pb C1 77.88(9) 1_655 . ? O4 Pb C1 114.29(8) 1_565 . ? O2 Pb C1 24.42(8) . . ? OW Pb C1 175.05(9) 1_656 . ? O5 Pb OW 163.30(9) 2_766 2_676 ? O1 Pb OW 89.03(10) . 2_676 ? O5 Pb OW 99.24(9) 1_556 2_676 ? O3 Pb OW 129.86(9) 1_655 2_676 ? O4 Pb OW 71.56(8) 1_565 2_676 ? O2 Pb OW 64.48(11) . 2_676 ? OW Pb OW 104.74(8) 1_656 2_676 ? C1 Pb OW 77.23(10) . 2_676 ? O5 Pb C4 85.70(8) 2_766 2_667 ? O1 Pb C4 88.66(9) . 2_667 ? O5 Pb C4 20.95(8) 1_556 2_667 ? O3 Pb C4 148.26(8) 1_655 2_667 ? O4 Pb C4 122.42(8) 1_565 2_667 ? O2 Pb C4 122.08(8) . 2_667 ? OW Pb C4 68.94(10) 1_656 2_667 ? C1 Pb C4 107.17(9) . 2_667 ? OW Pb C4 81.07(10) 2_676 2_667 ? O5 Pb O4 106.98(7) 2_766 2_767 ? O1 Pb O4 96.38(8) . 2_767 ? O5 Pb O4 42.56(7) 1_556 2_767 ? O3 Pb O4 169.05(7) 1_655 2_767 ? O4 Pb O4 104.90(6) 1_565 2_767 ? O2 Pb O4 114.00(8) . 2_767 ? OW Pb O4 69.71(10) 1_656 2_767 ? C1 Pb O4 107.90(8) . 2_767 ? OW Pb O4 61.06(9) 2_676 2_767 ? C4 Pb O4 21.73(7) 2_667 2_767 ? O5 Pb C4 17.73(7) 2_766 1_655 ? O1 Pb C4 75.85(9) . 1_655 ? O5 Pb C4 82.29(8) 1_556 1_655 ? O3 Pb C4 45.75(7) 1_655 1_655 ? O4 Pb C4 117.24(8) 1_565 1_655 ? O2 Pb C4 101.36(8) . 1_655 ? OW Pb C4 90.79(10) 1_656 1_655 ? C1 Pb C4 87.08(9) . 1_655 ? OW Pb C4 164.25(10) 2_676 1_655 ? C4 Pb C4 102.60(7) 2_667 1_655 ? O4 Pb C4 124.18(7) 2_767 1_655 ? C1 O1 Pb 104.7(2) . . ? C1 O1 Pb 166.8(2) . 2_767 ? Pb O1 Pb 69.16(6) . 2_767 ? C1 O2 Pb 84.8(2) . . ? C3 O3 Pb 121.65(17) . 1_455 ? C3 O3 H5 114(3) . . ? Pb O3 H5 124(3) 1_455 . ? C4 O4 Pb 137.3(2) 1_655 1_545 ? C4 O4 Pb 78.33(19) 1_655 2_767 ? Pb O4 Pb 75.10(6) 1_545 2_767 ? C4 O4 Pb 17.22(17) 1_655 . ? Pb O4 Pb 122.76(8) 1_545 . ? Pb O4 Pb 61.79(4) 2_767 . ? C4 O5 Pb 127.3(2) 2_666 2_766 ? C4 O5 Pb 114.34(19) 2_666 1_554 ? Pb O5 Pb 113.91(9) 2_766 1_554 ? C4 O5 Pb 57.59(17) 2_666 2_776 ? Pb O5 Pb 145.46(9) 2_766 2_776 ? Pb O5 Pb 58.97(5) 1_554 2_776 ? C6 O6 H6 112(3) . . ? C6 O7 Pb 155.9(2) . 2_766 ? Pb OW Pb 75.26(8) 1_454 2_676 ? Pb OW Pb 66.09(7) 1_454 2_666 ? Pb OW Pb 117.04(9) 2_676 2_666 ? Pb OW Pb 141.48(13) 1_454 2_776 ? Pb OW Pb 109.23(10) 2_676 2_776 ? Pb OW Pb 132.12(8) 2_666 2_776 ? Pb OW H7 112(4) 1_454 . ? Pb OW H7 139(4) 2_676 . ? Pb OW H7 47(4) 2_666 . ? Pb OW H7 90(4) 2_776 . ? Pb OW H8 107(8) 1_454 . ? Pb OW H8 93(7) 2_676 . ? Pb OW H8 144(7) 2_666 . ? Pb OW H8 36(8) 2_776 . ? H7 OW H8 120(9) . . ? O2 C1 O1 121.6(3) . . ? O2 C1 C2 120.8(3) . . ? O1 C1 C2 117.6(3) . . ? O2 C1 Pb 70.76(19) . . ? O1 C1 Pb 51.23(18) . . ? C2 C1 Pb 166.7(2) . . ? O2 C1 Pb 94.1(2) . 1_455 ? O1 C1 Pb 96.8(2) . 1_455 ? C2 C1 Pb 79.61(18) . 1_455 ? Pb C1 Pb 107.42(9) . 1_455 ? C1 C2 C3 112.0(3) . . ? C1 C2 Pb 8.86(15) . . ? C3 C2 Pb 115.36(19) . . ? C1 C2 Pb 82.00(18) . 1_455 ? C3 C2 Pb 31.36(15) . 1_455 ? Pb C2 Pb 86.90(6) . 1_455 ? C1 C2 H1 109(2) . . ? C3 C2 H1 110(2) . . ? Pb C2 H1 114(2) . . ? Pb C2 H1 114(2) 1_455 . ? C1 C2 H2 109(2) . . ? C3 C2 H2 108(2) . . ? Pb C2 H2 100(2) . . ? Pb C2 H2 129(2) 1_455 . ? H1 C2 H2 109(3) . . ? O3 C3 C2 111.5(3) . . ? O3 C3 C4 107.3(2) . . ? C2 C3 C4 109.8(3) . . ? O3 C3 C5 110.1(3) . 1_455 ? C2 C3 C5 111.7(3) . 1_455 ? C4 C3 C5 106.2(3) . 1_455 ? O3 C3 Pb 38.01(13) . 1_455 ? C2 C3 Pb 135.4(2) . 1_455 ? C4 C3 Pb 70.92(16) . 1_455 ? C5 C3 Pb 110.47(19) 1_455 1_455 ? O3 C3 Pb 94.95(16) . 2_667 ? C2 C3 Pb 121.35(18) . 2_667 ? C4 C3 Pb 13.78(14) . 2_667 ? C5 C3 Pb 105.86(18) 1_455 2_667 ? Pb C3 Pb 57.72(4) 1_455 2_667 ? O4 C4 O5 124.1(3) 1_455 2_666 ? O4 C4 C3 118.6(3) 1_455 . ? O5 C4 C3 117.2(3) 2_666 . ? O4 C4 Pb 79.93(18) 1_455 2_667 ? O5 C4 Pb 44.71(15) 2_666 2_667 ? C3 C4 Pb 159.7(2) . 2_667 ? O4 C4 Pb 156.5(2) 1_455 1_455 ? O5 C4 Pb 34.94(14) 2_666 1_455 ? C3 C4 Pb 83.10(17) . 1_455 ? Pb C4 Pb 77.40(7) 2_667 1_455 ? O4 C4 Pb 30.07(17) 1_455 1_445 ? O5 C4 Pb 105.95(19) 2_666 1_445 ? C3 C4 Pb 128.9(2) . 1_445 ? Pb C4 Pb 63.11(5) 2_667 1_445 ? Pb C4 Pb 129.37(9) 1_455 1_445 ? C6 C5 C3 113.2(3) . 1_655 ? C6 C5 Pb 110.0(2) . . ? C3 C5 Pb 49.80(16) 1_655 . ? C6 C5 Pb 156.6(2) . 1_545 ? C3 C5 Pb 87.87(17) 1_655 1_545 ? Pb C5 Pb 91.18(6) . 1_545 ? C6 C5 H3 116.0(18) . . ? C3 C5 H3 101.4(19) 1_655 . ? Pb C5 H3 57.7(19) . . ? Pb C5 H3 66.5(18) 1_545 . ? C6 C5 H4 109(2) . . ? C3 C5 H4 110(2) 1_655 . ? Pb C5 H4 141(2) . . ? Pb C5 H4 51(2) 1_545 . ? H3 C5 H4 107(3) . . ? O7 C6 O6 123.6(3) . . ? O7 C6 C5 122.6(3) . . ? O6 C6 C5 113.8(3) . . ? 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 O3 H5 O7 0.88(3) 1.81(3) 2.690(3) 176(5) 2_666 O6 H6 O2 0.86(3) 1.72(3) 2.583(4) 174(5) 2_666 OW H7 O1 0.86(3) 2.04(3) 2.854(4) 158(5) 2_666 OW H8 OW 0.89(3) 2.04(5) 2.891(8) 160(10) 2_675 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.169 _refine_diff_density_min -0.466 _refine_diff_density_rms 0.144