data_salpb25 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H16 O9 Pb' _chemical_formula_weight 475.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pb' 'Pb' -4.0753 8.5060 '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/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.1353(3) _cell_length_b 13.7831(2) _cell_length_c 8.73430(10) _cell_angle_alpha 90.00 _cell_angle_beta 92.0250(10) _cell_angle_gamma 90.00 _cell_volume 2663.11(6) _cell_formula_units_Z 8 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 15092 _cell_measurement_theta_min 6.57 _cell_measurement_theta_max 71.90 _exptl_crystal_description 'parallelepiped' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.371 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1792 _exptl_absorpt_coefficient_mu 25.040 _exptl_absorpt_correction_type 'numerical' _exptl_absorpt_correction_T_min 0.025 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'CrystalClear, Rigaku MSC, 2005' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS SPIDER IPDS' _diffrn_measurement_method '\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16066 _diffrn_reflns_av_R_equivalents 0.0941 _diffrn_reflns_av_sigmaI/netI 0.0688 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 6.81 _diffrn_reflns_theta_max 64.98 _reflns_number_total 2149 _reflns_number_gt 1961 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear, Rigaku MSC, 2005' _computing_cell_refinement 'CrystalClear, Rigaku MSC, 2005' _computing_data_reduction 'CrystalClear, Rigaku MSC, 2005' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2012)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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^)+(0.0349P)^2^+5.8648P] 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 2149 _refine_ls_number_parameters 198 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0418 _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.0864 _refine_ls_wR_factor_gt 0.0831 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _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 Pb Pb 0.259019(12) 0.097003(15) 0.02040(3) 0.02706(16) Uani 1 1 d . . . O1 O 0.2980(2) 0.2588(3) 0.1076(5) 0.0366(12) Uani 1 1 d . . . O2 O 0.3280(3) 0.1409(3) 0.2573(6) 0.0571(17) Uani 1 1 d . . . O3 O 0.3344(2) 0.3587(4) 0.8204(5) 0.0430(13) Uani 1 1 d . . . O4 O 0.2899(2) 0.4860(3) 0.7158(5) 0.0445(13) Uani 1 1 d . . . O5 O 0.5377(3) 0.2322(4) 0.5380(7) 0.0587(17) Uani 1 1 d . . . O6 O 0.5618(3) 0.3870(3) 0.5158(7) 0.0464(14) Uani 1 1 d . . . H6O H 0.5899 0.3728 0.5790 0.060 Uiso 1 1 calc R . . C1 C 0.3631(3) 0.3017(5) 0.3220(7) 0.0312(17) Uani 1 1 d . . . C2 C 0.4249(4) 0.2656(5) 0.3687(8) 0.0331(17) Uani 1 1 d . . . C3 C 0.4601(3) 0.3450(5) 0.4591(8) 0.0314(16) Uani 1 1 d . . . C4 C 0.4258(3) 0.3707(5) 0.6022(7) 0.0310(16) Uani 1 1 d . . . H4A H 0.4472 0.4240 0.6574 0.040 Uiso 1 1 calc R . . H4B H 0.4254 0.3137 0.6710 0.040 Uiso 1 1 calc R . . C5 C 0.3604(4) 0.4022(4) 0.5641(8) 0.0307(19) Uani 1 1 d . . . H5 H 0.3614 0.4647 0.5061 0.040 Uiso 1 1 calc R . . C6 C 0.3264(3) 0.3264(4) 0.4644(7) 0.0313(15) Uani 1 1 d . . . H6A H 0.2863 0.3522 0.4314 0.041 Uiso 1 1 calc R . . H6B H 0.3201 0.2668 0.5250 0.041 Uiso 1 1 calc R . . C7 C 0.3274(3) 0.2303(5) 0.2256(8) 0.0330(17) Uani 1 1 d . . . C8 C 0.3255(4) 0.4180(4) 0.7076(8) 0.0291(17) Uani 1 1 d . . . C9 C 0.5225(3) 0.3145(5) 0.5066(7) 0.0354(17) Uani 1 1 d . . . O1W O 0.3305(3) 0.1486(4) -0.1882(6) 0.0652(19) Uani 1 1 d . . . H1WA H 0.3326 0.2135 -0.1894 0.085 Uiso 1 1 d . . . H1WB H 0.3689 0.1282 -0.1969 0.085 Uiso 1 1 d . . . O2W O 0.3441(2) -0.0482(3) 0.0348(5) 0.0449(13) Uani 1 1 d . . . H2WA H 0.3199 -0.0935 0.0693 0.058 Uiso 1 1 d . . . H2WB H 0.3727 -0.0739 -0.0197 0.058 Uiso 1 1 d . . . O3W O 0.4566(5) 0.0383(6) 0.0947(13) 0.078(3) Uani 0.60 1 d P . . O4W O 0.4516(7) 0.0263(9) -0.0860(18) 0.067(4) Uani 0.40 1 d P . . H1 H 0.369(3) 0.353(4) 0.261(7) 0.026(17) Uiso 1 1 d . . . H2A H 0.446(3) 0.247(3) 0.276(8) 0.025(18) Uiso 1 1 d . . . H2B H 0.424(3) 0.216(4) 0.436(7) 0.018(17) Uiso 1 1 d . . . H3 H 0.460(4) 0.406(4) 0.398(9) 0.05(3) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb 0.0372(3) 0.0230(2) 0.0208(2) -0.00247(8) -0.00359(17) -0.00168(9) O1 0.046(3) 0.034(2) 0.029(2) -0.0013(19) -0.016(2) 0.003(2) O2 0.086(5) 0.035(3) 0.047(3) 0.008(2) -0.031(3) -0.018(3) O3 0.050(4) 0.043(3) 0.036(3) 0.011(2) 0.003(2) 0.010(3) O4 0.053(4) 0.044(3) 0.036(3) 0.007(2) 0.001(2) 0.016(3) O5 0.058(4) 0.040(3) 0.077(4) -0.008(3) -0.024(3) 0.000(3) O6 0.048(4) 0.048(3) 0.043(3) 0.006(2) -0.009(3) -0.009(3) C1 0.046(5) 0.030(3) 0.017(3) -0.001(3) -0.003(3) -0.006(3) C2 0.044(5) 0.032(3) 0.022(3) 0.000(3) -0.010(3) -0.006(3) C3 0.035(5) 0.026(3) 0.032(4) 0.003(3) -0.007(3) 0.004(3) C4 0.038(5) 0.032(3) 0.022(3) -0.004(3) -0.006(3) -0.003(3) C5 0.043(6) 0.023(3) 0.026(4) 0.001(2) -0.007(3) -0.002(3) C6 0.025(4) 0.033(3) 0.035(4) 0.005(3) -0.007(3) -0.008(3) C7 0.036(5) 0.033(3) 0.030(4) 0.001(3) -0.002(3) -0.009(3) C8 0.036(5) 0.021(3) 0.031(4) 0.002(3) -0.004(3) -0.002(3) C9 0.049(5) 0.030(4) 0.027(3) -0.007(3) -0.001(3) 0.003(4) O1W 0.103(6) 0.035(3) 0.059(4) 0.000(3) 0.024(4) -0.006(3) O2W 0.059(4) 0.035(3) 0.042(3) -0.003(2) 0.007(3) 0.008(3) O3W 0.076(8) 0.047(6) 0.110(9) -0.009(6) 0.008(7) 0.005(5) O4W 0.076(13) 0.047(8) 0.075(11) 0.001(7) -0.011(8) 0.004(8) _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 O1 2.500(4) . ? Pb O1W 2.556(6) . ? Pb O1 2.587(4) 7 ? Pb O2 2.598(5) . ? Pb O3 2.604(5) 7_556 ? Pb O2W 2.748(5) . ? Pb O4 2.759(4) 4_545 ? O1 C7 1.262(8) . ? O1 Pb 2.587(4) 7 ? O2 C7 1.263(8) . ? O3 C8 1.289(8) . ? O3 Pb 2.604(5) 7_556 ? O4 C8 1.228(7) . ? O4 Pb 2.759(4) 4 ? O5 C9 1.212(7) . ? O6 C9 1.326(8) . ? O6 H6O 0.8400 . ? C1 C2 1.498(10) . ? C1 C7 1.502(9) . ? C1 C6 1.547(9) . ? C1 H1 0.90(6) . ? C2 C3 1.543(9) . ? C2 H2A 0.98(7) . ? C2 H2B 0.90(6) . ? C3 C9 1.489(10) . ? C3 C4 1.527(9) . ? C3 H3 1.00(7) . ? C4 C5 1.535(10) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C8 1.512(10) . ? C5 C6 1.539(8) . ? C5 H5 1.0000 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? O1W H1WA 0.8957 . ? O1W H1WB 0.8994 . ? O2W H2WA 0.8834 . ? O2W H2WB 0.8795 . ? O3W O4W 1.587(17) . ? 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 Pb O1W 75.71(17) . . ? O1 Pb O1 66.69(16) . 7 ? O1W Pb O1 77.47(19) . 7 ? O1 Pb O2 50.45(14) . . ? O1W Pb O2 98.13(19) . . ? O1 Pb O2 115.41(14) 7 . ? O1 Pb O3 84.26(18) . 7_556 ? O1W Pb O3 146.99(19) . 7_556 ? O1 Pb O3 70.53(16) 7 7_556 ? O2 Pb O3 88.58(19) . 7_556 ? O1 Pb O2W 114.02(15) . . ? O1W Pb O2W 78.14(16) . . ? O1 Pb O2W 154.45(16) 7 . ? O2 Pb O2W 75.57(16) . . ? O3 Pb O2W 134.58(14) 7_556 . ? O1 Pb O4 147.63(14) . 4_545 ? O1W Pb O4 81.85(16) . 4_545 ? O1 Pb O4 86.00(13) 7 4_545 ? O2 Pb O4 158.19(15) . 4_545 ? O3 Pb O4 103.37(15) 7_556 4_545 ? O2W Pb O4 83.15(15) . 4_545 ? C7 O1 Pb 97.7(4) . . ? C7 O1 Pb 145.3(4) . 7 ? Pb O1 Pb 113.31(16) . 7 ? C7 O2 Pb 93.0(4) . . ? C8 O3 Pb 99.0(4) . 7_556 ? C8 O4 Pb 128.0(4) . 4 ? C9 O6 H6O 109.5 . . ? C2 C1 C7 113.1(5) . . ? C2 C1 C6 110.7(5) . . ? C7 C1 C6 108.3(6) . . ? C2 C1 H1 106(4) . . ? C7 C1 H1 106(4) . . ? C6 C1 H1 113(4) . . ? C1 C2 C3 110.1(6) . . ? C1 C2 H2A 109(4) . . ? C3 C2 H2A 111(4) . . ? C1 C2 H2B 113(4) . . ? C3 C2 H2B 103(4) . . ? H2A C2 H2B 111(5) . . ? C9 C3 C4 108.7(5) . . ? C9 C3 C2 112.9(5) . . ? C4 C3 C2 109.1(6) . . ? C9 C3 H3 112(5) . . ? C4 C3 H3 104(4) . . ? C2 C3 H3 110(5) . . ? C3 C4 C5 112.4(5) . . ? C3 C4 H4A 109.1 . . ? C5 C4 H4A 109.1 . . ? C3 C4 H4B 109.1 . . ? C5 C4 H4B 109.1 . . ? H4A C4 H4B 107.9 . . ? C8 C5 C4 111.5(6) . . ? C8 C5 C6 108.3(6) . . ? C4 C5 C6 111.7(5) . . ? C8 C5 H5 108.4 . . ? C4 C5 H5 108.4 . . ? C6 C5 H5 108.4 . . ? C5 C6 C1 110.1(5) . . ? C5 C6 H6A 109.6 . . ? C1 C6 H6A 109.6 . . ? C5 C6 H6B 109.6 . . ? C1 C6 H6B 109.6 . . ? H6A C6 H6B 108.1 . . ? O1 C7 O2 118.9(6) . . ? O1 C7 C1 120.0(6) . . ? O2 C7 C1 121.1(6) . . ? O4 C8 O3 121.4(7) . . ? O4 C8 C5 120.4(6) . . ? O3 C8 C5 118.3(6) . . ? O5 C9 O6 121.0(7) . . ? O5 C9 C3 125.0(6) . . ? O6 C9 C3 113.9(6) . . ? Pb O1W H1WA 108.7 . . ? Pb O1W H1WB 125.7 . . ? H1WA O1W H1WB 105.2 . . ? Pb O2W H2WA 96.2 . . ? Pb O2W H2WB 140.7 . . ? H2WA O2W H2WB 110.8 . . ? _diffrn_measured_fraction_theta_max 0.946 _diffrn_reflns_theta_full 64.98 _diffrn_measured_fraction_theta_full 0.946 _refine_diff_density_max 2.106 _refine_diff_density_min -1.666 _refine_diff_density_rms 0.234