#============================================================================== data_global loop_ _journal_name_full 'European Journal of Chemistry' _journal_coden_ASTM EJCUA9 _journal_volume 10 _journal_issue 2 _journal_year 2019 _journal_page_first 125 _journal_page_last 130 #=============================================================================== data_shelx _audit_creation_date 2019-04-15 _audit_creation_method ; Olex2 1.2 (compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381) ; _shelx_SHELXL_version_number '2018/3' _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_id_orcid ? _publ_contact_author_name '' _publ_contact_author_phone ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety '2(C14 H13 N3 O6 Pb)' _chemical_formula_sum 'C28 H26 N6 O12 Pb2' _chemical_formula_weight 1052.93 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pb' 'Pb' -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system 'monoclinic' _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.1786(6) _cell_length_b 9.9706(7) _cell_length_c 21.0908(16) _cell_angle_alpha 90 _cell_angle_beta 99.501(4) _cell_angle_gamma 90 _cell_volume 1488.9(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used ? _cell_measurement_temperature 100 _cell_measurement_theta_max ? _cell_measurement_theta_min ? _shelx_estimated_absorpt_T_max 0.209 _shelx_estimated_absorpt_T_min 0.209 _exptl_absorpt_coefficient_mu 11.371 _exptl_absorpt_correction_T_max 0.2098 _exptl_absorpt_correction_T_min 0.2098 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Blessing 1995' _exptl_absorpt_special_details ? _exptl_crystal_colour 'metallic dark gray' _exptl_crystal_colour_lustre metallic _exptl_crystal_colour_modifier dark _exptl_crystal_colour_primary gray _exptl_crystal_density_diffrn 2.349 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 992 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0413 _diffrn_reflns_av_unetI/netI 0.0405 _diffrn_reflns_Laue_measured_fraction_full 0.970 _diffrn_reflns_Laue_measured_fraction_max 0.972 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_number 12844 _diffrn_reflns_point_group_measured_fraction_full 0.970 _diffrn_reflns_point_group_measured_fraction_max 0.972 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.493 _diffrn_reflns_theta_min 3.529 _diffrn_ambient_temperature 100 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.970 _diffrn_measured_fraction_theta_max 0.972 _diffrn_measurement_device_type 'Rigaku Mercury375R (2x2 bin mode)' _diffrn_measurement_method ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source ? _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 2747 _reflns_number_total 3323 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 1.434 _refine_diff_density_min -1.851 _refine_diff_density_rms 0.204 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 203 _refine_ls_number_reflns 3323 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0424 _refine_ls_R_factor_gt 0.0323 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0441P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0763 _refine_ls_wR_factor_ref 0.0811 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups, All O(H,H) groups 2. Restrained distances C13-C14 1.54 with sigma of 0.02 3. Rigid bond restraints C13, C14 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 4. Uiso/Uaniso restraints and constraints Uanis(O2) = Uanis(O4) = Uanis(O3) Uanis(C13) = Uanis(C14) 5.a Rotating group: O1(H1A,H1B) 5.b Aromatic/amide H refined with riding coordinates: C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8) 5.c Idealised Me refined as rotating group: C14(H14A,H14B,H14C) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary ? 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.16824(3) 0.38596(2) 0.26910(2) 0.03066(9) Uani 1 1 d . . . . . O1 O 0.4922(6) 0.3208(4) 0.3156(2) 0.0490(10) Uani 1 1 d . . . . . H1A H 0.502676 0.233225 0.314676 0.074 Uiso 1 1 d GR . . . . H1B H 0.514055 0.340562 0.356774 0.074 Uiso 1 1 d GR . . . . O2 O -0.1826(6) 0.4478(5) 0.2958(2) 0.0546(7) Uani 1 1 d . . . . . O3 O -0.1109(7) 0.6048(4) 0.2346(2) 0.0546(7) Uani 1 1 d . . . . . O4 O -0.2966(7) 0.6461(5) 0.3030(2) 0.0546(7) Uani 1 1 d . . . . . O5 O 0.3621(7) 0.5449(6) 0.1990(2) 0.0661(14) Uani 1 1 d . . . . . O6 O 0.1564(8) 0.4439(6) 0.1310(2) 0.0657(14) Uani 1 1 d . . . . . N1 N -0.1994(6) 0.5685(5) 0.2776(2) 0.0354(10) Uani 1 1 d . . . . . N2 N 0.2371(6) 0.5788(5) 0.3442(2) 0.0325(10) Uani 1 1 d . . . . . N3 N 0.1645(6) 0.3276(5) 0.3867(2) 0.0327(10) Uani 1 1 d . . . . . C1 C 0.1348(9) 0.2058(6) 0.4084(3) 0.0447(15) Uani 1 1 d . . . . . H1 H 0.104322 0.135588 0.377963 0.054 Uiso 1 1 calc R . . . . C2 C 0.1462(10) 0.1753(7) 0.4740(3) 0.0516(16) Uani 1 1 d . . . . . H2 H 0.124384 0.086534 0.487388 0.062 Uiso 1 1 calc R . . . . C3 C 0.1889(8) 0.2752(7) 0.5181(3) 0.0450(15) Uani 1 1 d . . . . . H3 H 0.196554 0.256400 0.562652 0.054 Uiso 1 1 calc R . . . . C4 C 0.2696(8) 0.5134(7) 0.5414(3) 0.0453(15) Uani 1 1 d . . . . . H4 H 0.280037 0.497759 0.586281 0.054 Uiso 1 1 calc R . . . . C5 C 0.3005(9) 0.6363(7) 0.5204(3) 0.0463(16) Uani 1 1 d . . . . . H5 H 0.330157 0.706929 0.550621 0.056 Uiso 1 1 calc R . . . . C6 C 0.3219(9) 0.7917(7) 0.4296(3) 0.0473(15) Uani 1 1 d . . . . . H6 H 0.349606 0.865287 0.458242 0.057 Uiso 1 1 calc R . . . . C7 C 0.3133(8) 0.8101(6) 0.3649(3) 0.0451(15) Uani 1 1 d . . . . . H7 H 0.335728 0.895963 0.348110 0.054 Uiso 1 1 calc R . . . . C8 C 0.2715(8) 0.7021(6) 0.3246(3) 0.0393(13) Uani 1 1 d . . . . . H8 H 0.266761 0.716236 0.279835 0.047 Uiso 1 1 calc R . . . . C9 C 0.2458(7) 0.5586(6) 0.4086(2) 0.0296(11) Uani 1 1 d . . . . . C10 C 0.2899(8) 0.6641(6) 0.4537(3) 0.0365(12) Uani 1 1 d . . . . . C11 C 0.2091(7) 0.4272(6) 0.4308(2) 0.0303(11) Uani 1 1 d . . . . . C12 C 0.2216(8) 0.4055(6) 0.4979(3) 0.0357(13) Uani 1 1 d . . . . . C13 C 0.2931(9) 0.5176(6) 0.1427(3) 0.0415(10) Uani 1 1 d D U . . . C14 C 0.3676(9) 0.5619(6) 0.0973(3) 0.0415(10) Uani 1 1 d D U . . . H14A H 0.292695 0.637063 0.076866 0.062 Uiso 1 1 calc GR . . . . H14B H 0.372233 0.490559 0.065594 0.062 Uiso 1 1 calc GR . . . . H14C H 0.496116 0.592556 0.113821 0.062 Uiso 1 1 calc GR . . . . 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 0.03772(14) 0.02663(15) 0.02850(13) -0.00210(7) 0.00799(9) -0.00085(8) O1 0.050(2) 0.037(3) 0.060(3) 0.000(2) 0.007(2) -0.002(2) O2 0.0603(17) 0.0439(17) 0.0645(18) 0.0126(13) 0.0246(14) 0.0071(12) O3 0.0603(17) 0.0439(17) 0.0645(18) 0.0126(13) 0.0246(14) 0.0071(12) O4 0.0603(17) 0.0439(17) 0.0645(18) 0.0126(13) 0.0246(14) 0.0071(12) O5 0.072(3) 0.079(4) 0.051(3) -0.019(3) 0.018(2) -0.026(3) O6 0.091(4) 0.056(3) 0.048(3) -0.008(2) 0.005(3) -0.004(3) N1 0.037(2) 0.033(3) 0.036(2) 0.004(2) 0.007(2) 0.002(2) N2 0.038(2) 0.027(3) 0.034(2) -0.0002(19) 0.008(2) -0.003(2) N3 0.038(2) 0.029(3) 0.032(2) 0.0028(19) 0.0095(19) -0.003(2) C1 0.059(4) 0.034(4) 0.042(3) 0.003(3) 0.010(3) -0.008(3) C2 0.067(4) 0.042(4) 0.048(4) 0.017(3) 0.014(3) 0.001(3) C3 0.047(4) 0.057(4) 0.033(3) 0.013(3) 0.013(3) 0.001(3) C4 0.048(4) 0.060(5) 0.029(3) -0.003(3) 0.007(3) 0.000(3) C5 0.050(4) 0.052(4) 0.035(3) -0.014(3) 0.002(3) 0.008(3) C6 0.049(4) 0.038(4) 0.054(4) -0.014(3) 0.004(3) -0.002(3) C7 0.051(4) 0.021(3) 0.063(4) -0.002(3) 0.011(3) -0.001(3) C8 0.046(3) 0.031(3) 0.041(3) 0.006(2) 0.009(3) -0.003(3) C9 0.024(2) 0.035(3) 0.029(3) -0.002(2) 0.005(2) -0.001(2) C10 0.035(3) 0.035(3) 0.039(3) -0.008(3) 0.004(2) 0.004(3) C11 0.027(3) 0.035(3) 0.030(3) 0.002(2) 0.006(2) 0.001(2) C12 0.033(3) 0.045(4) 0.030(3) 0.004(2) 0.006(2) 0.005(2) C13 0.060(3) 0.024(2) 0.046(2) 0.0085(18) 0.022(2) 0.0051(19) C14 0.060(3) 0.024(2) 0.046(2) 0.0085(18) 0.022(2) 0.0051(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 O1 2.458(4) . ? Pb1 O2 2.740(4) . ? Pb1 O5 2.704(5) . ? Pb1 N2 2.489(5) . ? Pb1 N3 2.553(4) . ? O1 H1A 0.8774 . ? O1 H1B 0.8782 . ? O2 N1 1.263(6) . ? O3 N1 1.244(6) . ? O4 N1 1.223(6) . ? O5 C13 1.238(7) . ? O6 C13 1.218(8) . ? N2 C8 1.333(7) . ? N2 C9 1.362(7) . ? N3 C1 1.327(7) . ? N3 C11 1.362(7) . ? C1 H1 0.9500 . ? C1 C2 1.407(8) . ? C2 H2 0.9500 . ? C2 C3 1.363(9) . ? C3 H3 0.9500 . ? C3 C12 1.399(8) . ? C4 H4 0.9500 . ? C4 C5 1.335(9) . ? C4 C12 1.419(9) . ? C5 H5 0.9500 . ? C5 C10 1.423(8) . ? C6 H6 0.9500 . ? C6 C7 1.369(9) . ? C6 C10 1.403(9) . ? C7 H7 0.9500 . ? C7 C8 1.373(8) . ? C8 H8 0.9500 . ? C9 C10 1.419(8) . ? C9 C11 1.430(8) . ? C11 C12 1.420(7) . ? C13 C14 1.252(7) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Pb1 O2 144.95(14) . . ? O1 Pb1 O5 80.49(15) . . ? O1 Pb1 N2 82.78(15) . . ? O1 Pb1 N3 73.30(14) . . ? O5 Pb1 O2 123.63(15) . . ? N2 Pb1 O2 77.77(15) . . ? N2 Pb1 O5 80.17(14) . . ? N2 Pb1 N3 65.81(15) . . ? N3 Pb1 O2 72.20(14) . . ? N3 Pb1 O5 138.93(14) . . ? Pb1 O1 H1A 109.4 . . ? Pb1 O1 H1B 109.8 . . ? H1A O1 H1B 104.1 . . ? N1 O2 Pb1 101.4(3) . . ? C13 O5 Pb1 103.6(4) . . ? O3 N1 O2 117.7(5) . . ? O4 N1 O2 120.2(5) . . ? O4 N1 O3 122.1(5) . . ? C8 N2 Pb1 122.8(4) . . ? C8 N2 C9 117.7(5) . . ? C9 N2 Pb1 119.4(4) . . ? C1 N3 Pb1 124.8(4) . . ? C1 N3 C11 117.8(5) . . ? C11 N3 Pb1 117.2(3) . . ? N3 C1 H1 118.3 . . ? N3 C1 C2 123.3(6) . . ? C2 C1 H1 118.3 . . ? C1 C2 H2 120.5 . . ? C3 C2 C1 119.0(6) . . ? C3 C2 H2 120.5 . . ? C2 C3 H3 120.0 . . ? C2 C3 C12 120.0(5) . . ? C12 C3 H3 120.0 . . ? C5 C4 H4 119.4 . . ? C5 C4 C12 121.2(6) . . ? C12 C4 H4 119.4 . . ? C4 C5 H5 119.3 . . ? C4 C5 C10 121.5(6) . . ? C10 C5 H5 119.3 . . ? C7 C6 H6 120.0 . . ? C7 C6 C10 120.0(5) . . ? C10 C6 H6 120.0 . . ? C6 C7 H7 120.6 . . ? C6 C7 C8 118.7(6) . . ? C8 C7 H7 120.6 . . ? N2 C8 C7 124.3(6) . . ? N2 C8 H8 117.8 . . ? C7 C8 H8 117.8 . . ? N2 C9 C10 121.8(5) . . ? N2 C9 C11 118.8(5) . . ? C10 C9 C11 119.4(5) . . ? C6 C10 C5 123.3(6) . . ? C6 C10 C9 117.5(5) . . ? C9 C10 C5 119.3(6) . . ? N3 C11 C9 118.7(5) . . ? N3 C11 C12 122.5(5) . . ? C12 C11 C9 118.8(5) . . ? C3 C12 C4 122.8(5) . . ? C3 C12 C11 117.4(5) . . ? C4 C12 C11 119.8(6) . . ? O5 C13 C14 120.2(7) . . ? O6 C13 O5 120.6(6) . . ? O6 C13 C14 119.2(7) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma 0 0 -4 2222.93 46.73 0 0 4 2617.11 52.54 0 0 4 2337.2 47.29 0 0 -5 0.72 1.27 0 0 5 13.85 1.77 0 0 5 -0.12 0.71 0 0 -6 1454.92 33.94 0 0 6 1543.69 33.08 0 0 6 1448.19 31.47 0 0 -7 1.65 2.27 0 0 7 1.87 1.03 0 0 7 -0.6 0.97 0 0 -8 873.15 24.25 0 0 8 842.76 20.65 0 0 8 825.15 20.43 0 0 -9 0.83 2.13 0 0 9 2.23 1.22 0 0 9 0.08 1.24 0 0 -10 84.89 7.2 0 0 10 84.88 5.86 0 0 10 82.78 5.73 0 0 -11 1.16 2.19 0 0 11 1.53 1.54 0 0 11 0.21 1.29 0 0 -12 2.23 2.55 0 0 12 4.52 1.92 0 0 12 4.78 2.22 0 0 -13 3.27 2.92 0 0 13 0.1 1.87 0 0 13 0.93 1.69 0 0 -14 41.1 6.45 0 0 14 39.92 4.54 0 0 14 38.48 4.89 0 0 -15 -0.87 2.88 0 0 15 1.05 1.96 0 0 -16 160.29 13.17 0 0 16 176.72 10.76 0 0 16 157.51 10.04 0 0 -17 1.09 3.98 0 0 17 -0.72 2.08 0 0 17 0.31 1.97 0 0 -18 203.46 15.7 0 0 18 202.28 11.38 0 0 18 190.5 10.82 0 0 -19 0.65 4.45 0 0 19 9.01 5.22 0 0 20 6.2 4.88 0 0 -21 -1.46 5.08 0 0 21 2.14 2.25 0 0 21 0.26 2.54 0 0 22 0.22 1.37 0 0 -23 0.37 4.92 0 0 23 1.06 2.3 0 0 23 1.28 2.95 0 0 24 2.51 2.69 0 0 -25 -0.18 5.1 0 0 -26 228.82 20.84 0 0 -27 1.63 5.39 0 1 -3 94.02 5.36 0 -1 -3 90.95 5.53 0 -1 3 84.35 4.99 0 -1 -3 86.02 4.67 0 1 3 89.55 4.8 0 1 3 79.74 4.67 0 1 -4 296.24 14.53 0 -1 -4 286.03 14.3 0 -1 4 275.71 13.38 0 1 4 290.77 13.61 0 1 4 265 12.75 0 1 -5 1701.59 37.59 0 -1 -5 1769.75 39.26 0 -1 5 1791.49 38.26 0 1 5 1647.52 34.58 0 1 5 1745.1 37.1 0 1 -6 704.57 19.07 0 -1 -6 645.91 18.01 0 -1 6 678.11 17.15 0 1 6 736.84 17.58 0 1 6 662.37 16.66 0 1 -7 1682.08 39.21 0 -1 -7 1662.21 39.05 0 -1 7 1724.07 38.05 0 1 7 1640.15 35.79 0 1 7 1664.87 36.62 0 1 -8 1414.65 34.94 0 -1 -8 1356.58 33.91 0 -1 8 1461.99 33.6 0 1 8 1469.33 32.85 0 -1 8 1379.22 32.38 0 1 8 1383.29 31.72 0 1 -9 860.48 24.97 0 -1 -9 834.96 24.63 0 -1 9 884.73 22.89 0 1 9 892.63 22.15 0 -1 9 888.47 23.19 0 1 9 823.31 21.21 0 1 -10 1144.05 34.88 0 -1 -10 1160.36 35.67 0 -1 10 1204.03 33.75 0 1 10 1120.77 30.86 0 -1 10 1098.03 32.04 0 1 10 1056.21 29.85 0 1 -11 853.04 28.59 0 -1 -11 873.73 29.63 0 -1 11 841.7 25.62 0 1 11 793.8 23.62 0 -1 11 821.68 25.94 0 1 11 761.42 23.23 0 1 -12 455.18 22.66 0 -1 12 456.44 20.24 0 1 12 462.54 11.87 0 -1 12 466.62 13.25 0 1 12 422.67 18.81 0 1 -13 985.53 37.09 0 -1 -13 1049.81 39.43 0 -1 13 1041.13 35.59 0 1 13 1050.69 35.14 0 -1 13 1028.43 37.61 0 1 13 972.98 33.3 0 1 -14 778.38 35.36 0 -1 14 815.06 33.73 0 1 14 824.93 33.4 0 -1 14 811.72 34.1 0 1 14 787.48 32.72 0 1 -15 863.98 38 0 -1 -15 871.32 38.4 0 -1 15 857.33 34.43 0 1 15 870.2 34.48 0 -1 15 829.23 35.26 0 1 15 839.14 34.18 0 -1 16 600.09 26.45 0 1 16 601.99 26.38 0 -1 16 554.01 24.45 0 1 16 536.64 24.2 0 1 -17 485.45 26.97 0 -1 17 499.26 24.45 0 1 17 602.19 27.71 0 -1 17 496.94 23.73 0 1 17 495.01 24.07 0 1 19 0.37 1.07 0 1 20 0.32 1.24 0 1 -21 75.73 11.86 0 -1 -21 86.04 13.55 0 1 21 0.58 1.33 0 1 21 87.05 11.66 0 1 -22 51.32 9.88 0 -1 -22 44.9 9.77 0 -1 22 49.56 6.94 0 1 22 0.08 1.36 0 -1 22 50.66 7.25 0 1 22 53.43 7.85 0 1 -23 26.3 8.8 0 -1 -23 24.57 8.78 0 -1 23 -1.17 2.27 0 1 23 0.42 1.41 0 -1 23 21.14 5.35 0 1 23 21.13 6.43 0 -1 -24 25.52 10.37 0 1 -24 22.99 8.5 0 -1 24 0.72 1.64 0 -1 24 15.59 4.87 0 1 -25 6.88 5.33 0 -1 -25 2.68 4.52 0 1 25 6.62 5.39 0 1 -26 2.54 4.84 0 -1 -26 1.25 4.65 0 2 0 317.29 14.4 0 -2 0 337.09 8.2 0 -2 0 347.68 10 0 2 -1 1790.92 36.58 0 -2 -1 1751.24 35.9 0 2 -1 1664.81 33.63 0 -2 1 1737.96 35.53 0 -2 -1 1775.41 37.53 0 -2 1 2055.85 43.64 0 -2 2 390.44 10.09 0 2 -2 432.37 10.63 0 -2 -2 396.88 10.57 0 2 -2 400.58 10.53 0 -2 -2 405.72 10.78 0 -2 2 418.96 12.17 0 2 2 395.93 11.78 0 2 -3 1703.34 35.68 0 -2 -3 1701.61 36.69 0 -2 -3 1711.47 36.22 0 2 3 1670.93 35.25 0 2 -4 19.88 2.19 0 -2 -4 24.32 2.74 0 -2 4 23.45 2.9 0 2 4 21.19 2.19 0 2 4 18.63 2.47 0 2 -5 1482.19 33.35 0 -2 -5 1574.12 36.1 0 -2 5 1624.04 36.73 0 2 5 1448.58 31.36 0 2 5 1597 35.75 0 2 -6 116.93 7.59 0 -2 -6 121.75 8.15 0 -2 6 112.03 7.35 0 2 6 123.84 7.08 0 2 6 109.43 7.04 0 2 -7 1231.85 30.25 0 -2 -7 1257.19 31.6 0 -2 7 1242.85 30.06 0 2 7 1292.19 29.14 0 2 7 1273.37 30.3 0 2 -8 55.27 5.7 0 -2 -8 53.84 5.29 0 -2 8 54.95 4.99 0 2 8 55.16 4.37 0 2 8 54.08 5.05 0 2 -9 660.72 22.72 0 -2 -9 670.11 23.07 0 -2 9 673.93 21.61 0 2 9 701.83 20.75 0 2 9 659.14 20.97 0 2 -10 12.7 3.62 0 -2 -10 8.83 4.33 0 -2 10 11.1 2.51 0 2 10 9.39 2.02 0 2 10 7.67 2.27 0 2 -11 100.97 8.32 0 -2 -11 110 9.43 0 -2 11 104.53 7.33 0 2 11 113 7.4 0 2 11 104.59 7.68 0 2 -12 11.37 3.97 0 -2 -12 9.98 3.64 0 -2 12 11.05 2.98 0 2 12 11.14 2.39 0 -2 12 11.24 6.42 0 2 12 11.07 3.1 0 2 -13 14.75 4.82 0 -2 -13 15.56 4.81 0 -2 13 14.78 3.3 0 2 13 18.03 3.27 0 -2 13 15.31 8.39 0 2 13 14.59 3.71 0 2 -14 41.08 6.4 0 -2 -14 46.12 7.21 0 -2 14 38.29 4.85 0 2 14 35.55 4.04 0 -2 14 42.97 6.85 0 2 14 36.35 4.68 0 2 -15 33.11 6.49 0 -2 -15 37.42 6.84 0 -2 15 33.08 5.29 0 2 15 33.55 4.11 0 -2 15 36.35 9.54 0 2 15 33.98 4.97 0 2 -16 15.08 5.09 0 -2 -16 19.13 6.28 0 -2 16 15.59 4.26 0 2 16 16.81 3.52 0 -2 16 14.23 8.66 0 2 16 15.26 3.59 0 2 -17 85.87 9.48 0 -2 -17 86.23 10.19 0 -2 17 84.58 8.2 0 2 17 87.9 7.11 0 -2 17 84.52 12.07 0 2 17 89.5 8.27 0 2 -18 0.78 3.74 0 -2 -18 2.61 4.4 0 2 18 -0.42 0.95 0 2 18 0.25 2.62 0 2 19 0.28 0.93 0 2 -20 4.14 5.88 0 -2 -20 1.75 4.83 0 -2 20 2.49 3.99 0 2 20 0.54 1.51 0 -2 20 -0.35 2.42 0 2 21 0.12 1.22 0 2 -22 10.92 6.27 0 -2 -22 13.23 6.99 0 -2 22 16.72 5.69 0 2 22 2.07 2.09 0 -2 22 17.24 5.76 0 2 22 11.93 5.75 0 2 -23 294.74 27.46 0 -2 -23 284.66 26.83 0 -2 23 294.24 23.57 0 2 23 279.05 22.72 0 2 -24 2.02 4.73 0 -2 -24 0.36 4.82 0 -2 24 1.87 3.37 0 -2 24 1 3.12 0 2 -25 266.97 24.96 0 -2 -25 278 22.7 0 2 -26 12.67 9.06 0 -2 -26 5.32 5.33 0 -3 0 4.84 1.12 0 -3 0 2.1 1.52 0 -3 -1 103.99 5.94 0 -3 1 95.87 5.45 0 -3 -1 101.21 6.61 0 -3 1 102.63 6.85 0 3 -2 230.74 11.58 0 -3 -2 230.68 11.7 0 -3 -2 227.23 12.09 0 -3 2 217.79 12.18 0 3 2 215.32 12.44 0 3 -3 626.82 15.34 0 -3 -3 614.54 16.14 0 -3 -3 619.22 16.46 0 -3 3 640.03 18.59 0 3 3 628.86 18.3 0 3 -4 325.03 7.4 0 -3 -4 346.68 11.45 0 -3 -4 339.78 11.47 0 -3 4 333.26 10.67 0 3 4 327.73 10.14 0 3 -5 738.98 18.77 0 -3 -5 782.21 21.02 0 -3 -5 763.24 20.1 0 -3 5 748.78 21.43 0 3 5 729.76 18.6 0 3 5 758.33 21.22 0 3 -6 1565.3 35.85 0 -3 -6 1655.75 39.1 0 -3 -6 1623.76 36.38 0 -3 6 1667.77 39.87 0 3 6 1609.48 35.88 0 3 6 1674.48 39.45 0 3 -7 264.37 12.54 0 -3 -7 286.27 14.27 0 -3 7 263.24 13.06 0 3 7 284.06 12.27 0 3 7 249.06 12.24 0 3 -8 1342.93 38.16 0 -3 -8 1349.43 39.23 0 -3 8 1329.5 38.29 0 3 8 1357.91 36.34 0 3 8 1336.22 38.06 0 3 -9 539.08 22.66 0 -3 -9 575.02 24.57 0 -3 9 542.96 22.77 0 3 9 589.64 22.58 0 3 9 545.07 22.9 0 3 -10 1371.75 40.13 0 -3 -10 1289.69 39.24 0 -3 10 1332.34 39.16 0 3 10 1382.25 37.7 0 3 10 1341.71 38.92 0 3 -11 358.43 18.79 0 -3 -11 359.19 18.85 0 -3 11 350.72 17.71 0 3 11 381.23 17.25 0 3 11 349.33 17.51 0 3 -12 1017.51 37.28 0 -3 -12 1055.05 39.47 0 -3 12 1065.64 37.88 0 3 12 1052.79 35.21 0 3 12 1072.03 37.75 0 3 -13 223.73 14.08 0 -3 -13 218.14 13.93 0 -3 13 223.79 12.88 0 3 13 240.82 11.86 0 3 13 222.71 12.56 0 3 -14 877.17 37.61 0 -3 -14 872.32 38.07 0 -3 14 889.54 36.9 0 3 14 932.15 35.85 0 3 14 861.22 35.35 0 3 -15 219.66 13.27 0 -3 -15 240.56 14.6 0 -3 15 240.06 12.71 0 3 15 223.6 9.91 0 -3 15 217.08 14.32 0 3 15 212.93 11.11 0 3 -16 603.87 30.55 0 -3 -16 569.33 30.12 0 -3 16 607.49 29.52 0 3 16 560.19 25.07 0 -3 16 538.12 27.2 0 3 16 557.47 26.92 0 3 -17 273.15 19.77 0 -3 -17 284 20.98 0 -3 17 273.57 18.29 0 3 17 274.53 16.27 0 -3 17 250.23 31.25 0 3 17 246.8 12.65 0 3 18 -0.75 0.9 0 3 19 -0.06 0.88 0 3 20 1.01 1.46 0 -3 20 149.53 25.96 0 3 -21 44.92 9.68 0 -3 -21 42.16 9.72 0 -3 21 36.99 7.16 0 -3 21 34.23 9.28 0 3 21 39.32 7.51 0 3 -22 89.8 12.02 0 -3 -22 99.93 14.67 0 -3 22 93.39 11.75 0 -3 22 85.73 15.03 0 3 22 90.98 10.62 0 3 -23 15.44 7.18 0 -3 -23 14.91 6.99 0 -3 23 19.02 6.1 0 3 23 14.62 5.75 0 3 -24 19.61 7.51 0 -3 -24 33.29 10.64 0 -3 24 28.99 7.96 0 3 24 23.13 6.88 0 3 -25 -3.09 4.4 0 -3 -25 1.48 5.01 0 -3 25 -0.31 3.21 0 3 -26 1.62 4.58 0 -3 -26 4.05 7.34 0 -3 26 -0.04 3.04 0 -4 0 2391 49.63 0 -4 0 2597.71 57.38 0 -4 -1 22.89 2.65 0 -4 1 23.13 2.66 0 -4 -1 24.09 3.65 0 -4 1 22.65 3.5 0 4 -2 2628.92 54.65 0 -4 -2 2188.49 46.7 0 -4 -2 2313.3 51.36 0 -4 2 2513.65 56.65 0 4 -3 192.24 10.12 0 -4 -3 191.57 10.9 0 -4 -3 192.78 11.52 0 -4 3 181.99 11.85 0 4 3 179.37 11.9 0 4 -4 2383.97 50.05 0 -4 -4 2180.6 48.09 0 -4 -4 2266.07 50.25 0 -4 4 2543.99 58.32 0 4 4 2613.88 59.65 0 4 -5 363.63 14.62 0 -4 -5 350.89 15.51 0 -4 -5 362.52 15.68 0 -4 5 350.14 16.9 0 4 5 338.2 16.32 0 4 -6 1209.49 33.64 0 -4 -6 1201.74 34.63 0 -4 -6 1231.75 34.65 0 -4 6 1208.31 36.45 0 4 6 1209.35 36.26 0 4 -7 1.96 1.95 0 -4 -7 5.24 2.59 0 -4 -7 6.29 2.95 0 -4 7 1.95 1.66 0 4 7 3.13 2.19 0 4 -8 843.51 25.82 0 -4 -8 876.63 28.33 0 -4 -8 884 27.09 0 -4 8 843.33 28.08 0 4 8 853.68 25.54 0 4 8 842.46 27.72 0 4 -9 78.49 6.59 0 -4 -9 79.21 6.8 0 -4 -9 84.3 11.9 0 -4 9 77.43 7.48 0 4 9 81.08 5.4 0 4 9 70.98 6.38 0 4 -10 187.05 11.52 0 -4 -10 193.64 12.72 0 -4 -10 198.38 10.99 0 -4 10 192.86 12.67 0 4 10 192.27 10.85 0 4 10 180.87 11.63 0 4 -11 3.73 2.6 0 -4 -11 4.2 2.87 0 -4 11 2.76 3.16 0 4 11 4.26 2.23 0 4 11 2.32 2.44 0 4 -12 34.81 5.07 0 -4 -12 31.04 5.05 0 -4 12 33.41 5.2 0 4 12 30.48 3.92 0 4 12 30.21 5.03 0 4 -13 1.92 2.72 0 -4 -13 1.38 3 0 -4 13 0.07 2.59 0 4 13 0.54 1.65 0 4 13 0.9 2.7 0 4 -14 7.19 3.98 0 -4 -14 10.34 4.65 0 -4 14 3.76 3.63 0 4 14 5.15 2.25 0 4 14 6.12 3.78 0 4 -15 -0.78 2.29 0 -4 -15 0.34 3.39 0 -4 15 0.54 2.88 0 4 15 0.01 1.55 0 4 15 1.6 2.96 0 4 -16 89.73 9.44 0 -4 -16 95.15 10.71 0 -4 16 89.19 9.82 0 4 16 94.73 7.7 0 4 16 91.56 9.24 0 4 -17 0.28 2.6 0 -4 -17 0.41 4.16 0 -4 17 0.58 3.31 0 4 17 -0.08 1.82 0 -4 17 0.06 2 0 4 17 0.09 2.56 0 4 -18 249.15 18.47 0 -4 -18 261.17 20.19 0 -4 18 268.88 19.32 0 4 18 181.26 10.86 0 4 18 264.87 18.55 0 4 -19 11.62 5.1 0 -4 -19 14.25 7.23 0 -4 19 16.13 5.42 0 4 19 0.48 1.1 0 -4 19 11.05 5.86 0 4 19 12.31 4.86 0 4 -20 267.29 24.37 0 -4 -20 268.6 25.19 0 -4 20 279.11 23.79 0 -4 20 241.93 22.22 0 4 20 282.73 24.51 0 4 -21 22.45 7.27 0 -4 -21 20.4 8.24 0 -4 21 22.65 7.03 0 -4 21 17.51 11.79 0 -4 -22 248.69 24.41 0 -4 22 243.3 21.9 0 4 22 230.44 20.74 0 -4 -23 7.38 6.13 0 -4 23 7.76 6.62 0 -4 23 7.15 4.16 0 4 23 11.65 6.81 0 -4 -24 248.91 24.31 0 -4 24 260.92 22.82 0 4 24 236.81 20.71 0 4 -25 3.45 7.26 0 -4 -25 8.47 5.5 0 -4 25 9.62 5.92 0 -5 0 0.89 1 0 -5 0 0.48 2.06 0 -5 -1 95.06 5.64 0 -5 1 87.28 5.46 0 -5 -1 97.44 7.38 0 -5 1 98.63 7.83 0 5 -2 28.42 6.81 0 -5 -2 31.14 3.19 0 -5 -2 27.87 4.04 0 -5 2 30.76 4.5 0 5 -3 181.85 8.71 0 -5 -3 169.92 8.99 0 -5 -3 182.91 10.52 0 -5 3 179.16 11.4 0 5 -4 43.62 3.48 0 -5 -4 44.01 3.95 0 -5 -4 47.85 5.21 0 -5 4 40.35 5.3 0 5 4 37.54 5.2 0 5 -5 416.16 16.41 0 -5 -5 418.72 18.2 0 -5 -5 417 18.47 0 -5 5 411.75 19.76 0 5 5 390.74 19.13 0 5 -6 32.45 3.37 0 -5 -6 34.64 4.47 0 -5 -6 29.79 3.84 0 -5 6 28.72 4.8 0 5 6 24.92 4.27 0 5 -7 746.09 25.73 0 -5 -7 746.95 27.99 0 -5 -7 746.73 27.68 0 -5 7 735.74 29.1 0 5 7 731.02 28.86 0 5 -8 129.92 8.37 0 -5 -8 141.54 10.16 0 -5 -8 140.42 9.31 0 -5 8 130.73 10.47 0 5 8 122.41 10.35 0 5 -9 1122.24 43.7 0 -5 -9 1149.77 46.62 0 -5 -9 1152.07 46.48 0 -5 9 1099.36 45.88 0 5 9 1155.66 47.83 0 5 -10 448.61 21.04 0 -5 -10 454.53 23.24 0 -5 -10 464.46 21.7 0 -5 10 434.05 22.42 0 5 10 435.46 22.72 0 5 -11 1055.36 41.19 0 -5 -11 1072.14 43.84 0 -5 -11 1164.61 45.3 0 -5 11 1078.49 44.62 0 5 11 1108.36 42.03 0 5 11 1112.77 45.64 0 5 -12 216.05 13.02 0 -5 -12 201.15 13.49 0 -5 12 207.57 14.02 0 5 12 212.14 11.73 0 5 12 208.83 14.67 0 -5 -13 1445.57 60.29 0 -5 13 1413.46 59.47 0 5 13 1457.07 57.47 0 5 13 1443.57 60.18 0 -5 -14 358.74 23.06 0 -5 -14 387.11 22.43 0 -5 14 359.87 22.79 0 5 14 384.42 21.68 0 5 14 371.99 24.06 0 -5 -15 471.39 29.3 0 -5 -15 490.95 28.42 0 -5 15 472.95 28.97 0 5 15 497.99 27.33 0 5 15 492.39 29.88 0 -5 -16 147.39 12.4 0 -5 -16 153.47 21.49 0 -5 16 147.89 11.61 0 5 16 152.03 9.75 0 5 16 147.12 12.12 0 -5 -17 295.18 21.47 0 -5 17 295.24 20.83 0 5 17 297.3 18.25 0 5 17 287.48 20.19 0 5 -18 126.69 14.86 0 -5 -18 133.38 15.98 0 -5 -18 116.77 12.4 0 -5 18 126.94 15.41 0 5 18 169.7 14.95 0 5 18 121.61 14.19 0 5 -19 198.7 19.79 0 -5 -19 214.69 21.7 0 -5 19 215.07 21.21 0 -5 19 167.85 32.35 0 5 19 214.89 19.96 0 5 -20 12.5 5.51 0 -5 -20 13 8.05 0 -5 20 13.37 6.28 0 -5 20 9.26 5.3 0 5 20 12.33 5.88 0 5 -21 81.92 11.68 0 -5 -21 98.26 14.57 0 -5 21 95.15 12.34 0 -5 21 69.1 22.31 0 5 -22 2.41 5.21 0 -5 -22 4.15 7.25 0 -5 22 5.4 4.93 0 5 22 2.54 4.91 0 5 -23 30.18 8.09 0 -5 -23 33.41 10.74 0 -5 23 24.98 7.79 0 5 23 36.3 8.53 0 5 -24 1.7 5.55 0 -5 -24 -1.81 4.32 0 -5 24 0.82 3.77 0 5 24 -2.19 3.88 0 -6 0 316.97 14.39 0 -6 0 321.65 17.42 0 -6 -1 1280.34 40.45 0 -6 1 1245.01 39.23 0 -6 -1 1358.98 46.28 0 -6 1 1345.79 46.47 0 -6 -2 367.85 16.32 0 -6 -2 368.78 18.79 0 -6 2 375.19 19.48 0 -6 -3 1106.1 36.3 0 -6 -3 1133.51 39.53 0 -6 3 1148.49 41.48 0 -6 -4 334.59 16.02 0 -6 -4 329.17 17.57 0 -6 4 336.08 18.7 0 -6 -5 1026.24 35.14 0 -6 -5 995.44 35.54 0 -6 5 992.85 37.43 0 6 5 978.46 37.59 0 -6 -6 271.07 13.92 0 -6 -6 301.63 15.49 0 -6 6 303.39 14.5 0 6 6 275.9 16.21 0 6 -7 514.25 21.63 0 -6 -7 511.09 23.76 0 -6 -7 545.14 25 0 -6 7 511.88 25.71 0 6 7 488.81 25.23 0 6 -8 153.12 8.95 0 -6 -8 153.99 10.83 0 -6 -8 171.1 10.81 0 -6 8 145.31 11.73 0 6 8 150.94 12.24 0 6 -9 212.5 11.18 0 -6 -9 227.19 13.73 0 -6 -9 227.9 12.59 0 -6 9 215.43 14.06 0 6 9 210.17 14.2 0 6 -10 21.38 3.99 0 -6 -10 24.43 4.88 0 -6 -10 23.47 10.81 0 -6 10 22.07 5.36 0 6 10 24.65 6.3 0 6 -11 38.12 5.46 0 -6 -11 35.93 6.7 0 -6 -11 41.43 6.76 0 -6 11 35.21 6.27 0 6 11 38.03 7 0 6 -12 55.17 6.19 0 -6 -12 56.98 7.8 0 -6 12 53.81 7.66 0 6 12 57.57 7.85 0 6 -13 38.12 5.96 0 -6 -13 38.41 6.81 0 -6 -13 39.54 9.88 0 -6 13 34.64 6.04 0 6 13 37.1 7.45 0 6 -14 28.8 5.38 0 -6 -14 33.49 6.87 0 -6 -14 32.93 7.07 0 -6 14 35.3 6.71 0 6 14 29.59 6.98 0 6 -15 102.3 9.07 0 -6 -15 114.7 11.93 0 -6 -15 114.98 12.37 0 -6 15 107.66 11.58 0 6 15 115.13 12.93 0 6 -16 16.73 5.1 0 -6 -16 10.69 4.73 0 -6 16 18.49 5.66 0 6 16 17.93 6.4 0 6 -17 129.98 14.35 0 -6 -17 148.4 16.63 0 -6 17 136.14 15.92 0 6 17 150.85 17.25 0 6 -18 31.23 7.3 0 -6 -18 36.1 8.01 0 -6 18 34.1 7.58 0 6 18 34.2 8.76 0 -6 -19 150.94 16.81 0 -6 19 143.29 15.21 0 6 19 160.6 16.7 0 -6 -20 20.27 6.97 0 -6 20 24.32 7.7 0 -6 20 18.59 5.38 0 6 20 22.23 7.91 0 -6 -21 189.19 20.97 0 -6 21 168.29 17.46 0 -6 21 128.08 20.98 0 6 -22 23.59 7.22 0 -6 -22 30.39 9.75 0 -6 22 22.25 7.41 0 6 22 26.52 8.72 0 -6 -23 232.64 21.03 0 -6 23 207.66 17.03 0 6 23 227.83 19.44 0 -7 0 0.45 1.32 0 -7 0 0.86 2.85 0 7 -1 7.07 3.87 0 -7 -1 10.66 3.13 0 -7 1 8.33 2.49 0 -7 -1 11.01 4.16 0 -7 1 8.69 3.59 0 7 -2 29.83 3.73 0 -7 -2 27.48 3.45 0 -7 -2 26.58 4.97 0 -7 2 30.09 6 0 -7 -3 6.53 2.45 0 -7 -3 5.57 3.26 0 -7 3 5.79 3.39 0 -7 -4 185.1 10.3 0 -7 -4 182.42 11.91 0 -7 4 175.38 12.76 0 -7 -5 8.59 3.01 0 -7 -5 9.28 3.25 0 -7 5 6.66 3.75 0 -7 -6 410.9 18.1 0 -7 -6 427.31 21.3 0 -7 6 425.53 18.21 0 -7 -7 94.6 8.6 0 -7 -7 88.35 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3.21 8 -2 -3 0.39 2.43 8 2 -3 3.27 4.64 8 2 -2 13.32 7.38 8 -2 -2 11.26 9.99 8 -2 -2 7.11 5.47 -8 2 2 9.49 6.38 8 -2 -2 7.54 5.22 8 2 -2 10.23 5.62 8 2 -1 74.9 42.44 8 -2 -1 71.26 26.09 -8 -2 1 111.81 21.8 8 -2 -1 64.88 10.01 -8 2 1 74.99 12.03 8 -2 -1 60.78 29.81 8 2 -1 83.57 11.65 8 2 0 0.8 3.68 8 -2 0 0.43 3.59 -8 -2 0 6.53 9.96 8 -2 0 0.19 1.72 -8 2 0 -1.11 3.31 8 -2 0 0.75 2.69 8 2 0 2.19 3.27 8 2 1 85.72 17.72 8 -2 1 68.57 46.45 -8 -2 -1 64.81 16.12 8 -2 1 40.65 22.33 8 -2 1 51.16 17.35 8 2 1 80.97 11.79 8 -2 2 1.94 2.85 -8 -2 -2 0.07 6.27 -8 2 -2 0.45 4.94 8 -2 2 -0.15 2.86 8 -2 2 1.17 2.66 8 2 2 3.44 4.09 -8 -2 -3 134.05 23.5 -8 2 -3 133.91 21 8 -2 3 103.59 13.78 8 2 3 127.27 16.04 8 -2 4 10.81 9.07 -8 -2 -4 26.96 14.67 -8 2 -4 7 7.89 8 -2 4 7.19 4 8 2 4 1.98 4.11 -8 -2 -5 126.75 20.36 -8 2 -5 112.51 19.12 8 -2 5 100.48 11.61 8 2 5 113.27 13.79 -8 -2 -6 2.45 6.44 -8 2 -6 6.87 8.94 8 2 6 0.6 3.78 -8 -2 -7 152.62 23.65 -8 2 -7 152.44 20.7 8 -2 7 127.89 15.25 8 2 7 149.69 16.96 -8 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28.75 12.65 8 -3 4 19.17 12.58 8 3 4 21.72 7.77 -8 -3 -5 14.81 11.23 8 -3 5 9.43 7.76 8 3 5 7.82 5.45 -8 -3 -6 5.94 8.79 8 -3 6 3.68 4.09 8 3 6 6.86 5.78 -8 -3 -7 0.72 5.77 8 -3 7 0.72 4.1 8 3 7 2.11 4.3 -8 -3 -8 -1.71 5.66 8 -3 8 0.57 2.5 8 3 8 -0.5 4.17 8 4 -14 98.81 17.77 8 -4 -14 85.4 14.6 -8 -4 14 86.17 14.51 -8 4 14 72.42 12.02 8 4 -13 2.3 5.87 8 -4 -13 4.41 7.1 -8 -4 13 4.39 6.57 -8 4 13 6.58 6.23 8 4 -12 114.5 18.23 8 -4 -12 103.78 16.07 -8 -4 12 96.67 13.57 -8 4 12 95.77 13.77 8 4 -11 2.58 5.85 8 -4 -11 4.75 6.34 -8 -4 11 5.25 5.09 -8 4 11 6.07 6.69 8 4 -10 80.13 17.55 8 -4 -10 71.2 12.8 -8 4 10 67.77 13.12 8 4 -9 -3.41 5.26 8 -4 -9 3.47 6.56 8 -4 -9 5.75 5.51 -8 -4 9 1.33 4.01 -8 4 9 4.01 4.31 8 4 -8 28.17 12.41 8 -4 -8 24.14 8.95 8 -4 -8 18.56 9.11 -8 -4 8 26.32 7.15 -8 4 8 24.63 8.36 8 4 -7 3.24 7.58 8 -4 -7 2.51 5.97 8 -4 -7 1.67 2.15 -8 -4 7 -0.42 3.35 -8 4 7 5 5.58 8 4 -6 0.54 4.17 8 -4 -6 -0.29 4.41 8 -4 -6 1.02 3.35 -8 4 6 1.7 4.16 8 4 -5 1.06 2.63 8 -4 -5 -0.02 4.63 8 -4 -5 -1.29 4.16 -8 -4 5 -1.34 3.04 -8 4 5 3.01 4.33 8 4 -4 7.9 5.26 8 -4 -4 0.44 4.82 -8 -4 4 12.21 12.13 -8 4 4 3.09 4.57 8 -4 -4 2.35 2.92 8 4 -3 -0.02 3.84 8 -4 -3 -1.72 4.78 -8 -4 3 -0.35 6.35 8 -4 -3 1.17 2.59 -8 4 3 -0.08 4.07 8 -4 -3 0.9 3.56 8 4 -2 21.12 11.83 -8 -4 2 19.02 9.81 8 -4 -2 11.78 10.69 8 -4 -2 9.53 9.38 8 4 -2 17.83 7.28 8 4 -1 3.56 3.91 -8 -4 1 1.3 6.28 8 -4 -1 1.84 3.47 8 -4 -1 4.88 3.98 8 4 -1 7.4 6.39 8 4 0 54.7 15.8 -8 -4 0 51.32 15.16 8 -4 0 36.92 17.8 8 -4 0 32.24 25.57 8 4 0 50.13 9.91 -8 -4 -1 -0.92 5.99 8 -4 1 4.3 3.61 8 -4 1 5.93 5.51 8 4 1 4.14 5.06 -8 -4 -2 104.32 19.53 8 -4 2 68.99 10.7 8 -4 2 63.72 28.67 8 4 2 89.69 12.75 -8 -4 -3 26.01 13.58 8 -4 3 0.41 3.37 8 -4 3 5.05 4.43 8 4 3 2.92 4.32 -8 -4 -4 93.76 17.98 8 -4 4 59.1 34.81 8 4 4 88.9 13.36 -8 -4 -5 16.95 12.66 8 -4 5 9.6 6.99 8 4 5 2.1 4.53 -8 -4 -6 125.15 20.16 8 -4 6 87.11 28.26 8 4 6 109.87 13.79 -8 -4 -7 8.75 10.38 8 -4 7 3.51 4.59 8 4 7 4.3 4.49 8 5 -12 18.37 11.29 8 -5 -12 8.37 7.55 8 -5 -12 10.91 7.94 -8 5 12 9.3 6.15 8 5 -11 79.71 17.5 8 -5 -11 70.41 12.55 8 -5 -11 58.36 22.99 -8 -5 11 69.39 11.42 -8 5 11 63.75 11.77 8 5 -10 47.23 16.67 8 -5 -10 30.25 10.42 8 -5 -10 18.99 14.62 -8 -5 10 24.14 8.77 -8 5 10 19.81 8.45 8 5 -9 129.61 21.21 8 -5 -9 85.19 30.34 -8 -5 9 84.97 11.45 -8 5 9 92.47 14.65 8 5 -8 46.65 14.88 8 -5 -8 19.6 14.7 -8 -5 8 21.53 7.05 -8 5 8 33.9 10.49 8 5 -7 188.95 25.34 8 -5 -7 140.08 17.38 -8 5 7 145.41 17.4 8 5 -6 38.66 29.83 8 -5 -6 36.42 17.48 -8 5 6 35.85 10.87 8 5 -5 186.89 45.3 8 -5 -5 149.67 40.95 -8 5 5 165.73 19.33 8 5 -4 32.34 19.61 -8 -5 4 52.37 16.3 8 -5 -4 25.87 17.1 8 -5 -4 14.01 8.41 8 5 -3 165.62 46.91 -8 -5 3 223.75 28.93 8 -5 -3 144.87 29.41 8 -5 -3 132.97 17.83 8 5 -2 15 13.95 -8 -5 2 33.1 14.5 8 -5 -2 11.14 6.25 8 -5 -2 8.32 5.93 8 5 -1 96.4 31.2 -8 -5 1 109.77 22.15 8 -5 -1 72.13 26.04 8 -5 -1 68.12 22.75 8 5 -1 101.04 14.27 8 5 0 26.85 12.56 -8 -5 0 29.86 14.89 8 -5 0 17.89 8.46 8 -5 0 14.31 10.1 8 5 0 16.17 6.7 -8 -5 -1 85.26 18.66 8 -5 1 53.6 11.41 8 -5 1 41.93 23.74 8 5 1 52.56 10.72 -8 -5 -2 24.63 13.34 8 -5 2 17.85 8.11 8 -5 2 9.46 8.53 8 5 2 18.77 8.34 -8 -5 -3 55.44 14.33 8 -5 3 26.44 7.57 8 -5 3 27.63 15.47 8 5 3 33.91 9.82 -8 -5 -4 10.52 11.62 8 -5 4 4.73 5.55 8 -5 4 5.53 4.78 8 5 4 7.78 8.13 -8 -5 -5 19.53 11.87 8 -5 5 11.71 6.02 8 5 5 12.45 7.94 8 6 -9 12.03 10.7 8 -6 -9 7.44 6.18 -8 -6 9 8.44 6.77 -8 6 9 12.88 8.57 8 6 -8 9.45 8.69 8 -6 -8 9.5 8.6 -8 6 8 7.06 7.66 8 6 -7 15.37 10.82 8 -6 -7 11.47 7.89 8 6 -6 3.26 5.17 8 -6 -6 -1.46 4.47 8 6 -5 2.37 3.11 8 -6 -5 -2.48 4.74 8 6 -4 5.74 5.85 -8 -6 4 -1.05 6.16 8 -6 -4 1.71 3.57 8 6 -3 8.43 5.56 -8 -6 3 3.38 6.38 8 -6 -3 2.96 4.28 8 6 -2 5.52 10.03 -8 -6 2 16.99 11.16 8 -6 -2 5.39 3.67 8 6 -1 16.47 9.05 -8 -6 1 20.24 12.44 8 -6 -1 18.44 8.79 8 6 0 2.77 4.18 -8 -6 0 3.66 6.23 8 -6 0 2.8 4.61 8 -6 0 3.67 3.66 8 6 0 4.93 6.7 8 6 1 48.41 14.78 -8 -6 -1 43.54 14.12 8 -6 1 39.55 11 8 -6 1 23.99 15.6 8 6 1 39.17 10.09 8 -6 2 2.22 4.98 8 -6 2 2.7 3.78 8 6 2 2.72 4.29 9 0 -11 3.48 8.21 -9 0 11 0.94 3.92 9 0 -10 16.42 9.96 -9 0 10 12.71 6.1 9 0 -9 0.36 6.15 9 0 -8 48.27 17.12 -9 0 8 29.48 8.32 -9 0 7 0.23 3.94 9 0 -6 75.59 19.15 -9 0 6 47.71 9.84 9 0 -3 3.95 7.32 9 0 -2 112.64 37.07 9 0 -1 5.74 6.55 -9 0 1 1.56 6.86 9 0 0 115.75 42.17 9 0 1 -0.18 3.32 9 0 2 109.45 41.85 -9 0 -2 132.92 22.2 9 0 2 103.7 12.54 9 1 -11 59.1 16.78 9 -1 -11 52.2 14.94 -9 -1 11 50.56 11.62 -9 1 11 46.48 11.53 9 1 -10 52.88 14.84 9 -1 -10 64.62 16.44 -9 1 10 40.09 10.16 9 1 -9 55.47 17.25 9 -1 -9 40.64 13.34 -9 -1 9 31.4 8.51 -9 1 9 35.22 9.88 9 1 -8 53.63 17.09 9 -1 -8 49.58 15.88 -9 -1 8 26.4 7.52 9 -1 -7 51.06 15.1 -9 -1 7 40.46 8.98 -9 1 7 36.2 9.75 9 1 -6 23.64 13.18 9 -1 -6 16.31 10.18 9 1 -5 26.01 13.19 9 -1 -5 14.7 10.12 -9 1 5 16.64 7.71 9 1 -4 7.35 9.48 9 -1 -4 6.79 7.44 9 -1 -4 8.85 5.88 -9 1 4 5.3 5.56 9 1 -3 9.47 7.89 9 -1 -3 11.49 9.59 9 -1 -3 6.09 5.17 9 1 -2 0.79 5.23 9 -1 -2 2.5 5.96 -9 -1 2 -3.44 6.4 9 1 -1 -1.9 6.4 9 -1 -1 2.5 5.32 -9 -1 1 -1.52 6.3 9 1 0 0.48 3.43 -9 -1 0 -0.07 6.11 9 1 1 2.55 4.18 9 -1 1 0.77 4.35 -9 -1 -1 -0.45 6 9 -1 1 1.6 3.44 9 1 1 0.27 3.46 9 1 2 8.11 6.15 9 -1 2 1.33 3.73 9 -1 2 4.77 4.03 9 1 2 4.89 5.91 9 2 -9 47.65 15.09 9 -2 -9 39.23 12.76 -9 -2 9 22.88 7.29 -9 2 9 32.11 8.74 9 -2 -8 5.73 10.33 -9 -2 8 1.12 3.83 -9 2 8 4.37 4.68 9 2 -7 108.89 22.11 9 -2 -7 90.8 18.47 9 2 -6 6.76 9.46 9 -2 -6 7.14 5.77 -9 2 6 7.03 6.31 9 2 -5 76.22 40.28 9 -2 -5 89.84 17.73 9 -2 -5 42.22 31.23 -9 2 5 50.36 9.55 9 2 -4 3.82 7.64 9 -2 -4 1.33 2.21 -9 2 4 4.04 5.89 9 2 -3 134.31 68.81 -9 -2 3 172.23 24.94 9 -2 -3 77.09 43.77 9 2 -2 10.65 12 9 -2 -2 -0.02 6.56 -9 -2 2 1.21 7.57 9 -2 -2 1.92 4.93 9 2 -1 146.13 57.73 -9 -2 1 165.97 26.96 9 2 0 2.37 5.17 9 -2 0 2.2 3.92 -9 -2 0 5.5 10.99 9 2 1 91.74 42.86 -9 2 -1 105.86 20.53 9 -2 1 89.39 12.27 9 3 -7 20.71 12.96 9 -3 -7 17.85 12.33 9 -3 -7 6.5 8.13 -9 3 7 13.86 8.03 9 3 -6 13.27 9.56 9 -3 -6 21.2 10.07 9 -3 -6 9.82 6.97 9 3 -5 7.26 5.84 9 -3 -5 15.65 11.08 9 -3 -5 3.7 5.77 -9 3 5 -0.47 4.05 9 3 -4 28.12 14.7 9 -3 -4 31.1 13.76 9 -3 -4 12.29 9.03 -9 3 4 18.33 8.98 9 3 -3 18.33 13.16 9 -3 -3 2.19 5.56 9 3 -2 1.96 2.27 -9 -3 2 4.57 6.9 9 -3 -2 0.3 2.04 _iucr_refine_instructions_details ; TITL shelx in P2(1)/c shelx.res created by SHELXL-2018/3 at 01:04:32 on 15-Apr-2019 CELL 0.71073 7.1786 9.9706 21.0908 90 99.501 90 ZERR 2 0.0006 0.0007 0.0016 0 0.004 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O Pb UNIT 56 52 12 24 4 DFIX 1.54 C13 C14 DELU C13 C14 EADP O2 O4 O3 EADP C13 C14 L.S. 10 PLAN -10 0 0 SIZE 0.2 0.2 0.2 TEMP -173.15 BOND $H fmap 2 acta OMIT 0 9 11 OMIT -1 7 4 OMIT -1 3 20 OMIT 0 3 18 OMIT 0 8 4 OMIT -1 8 8 OMIT 1 0 18 OMIT -2 6 21 OMIT 1 9 9 OMIT 1 9 3 OMIT 0 8 6 OMIT 1 0 20 OMIT -2 7 4 OMIT 2 1 13 OMIT 2 0 16 OMIT 1 2 17 OMIT -1 5 21 OMIT -1 8 4 OMIT 0 9 9 OMIT 2 1 19 OMIT 1 9 7 OMIT 0 2 21 OMIT 0 2 19 OMIT 0 0 22 OMIT -1 8 6 OMIT -1 8 5 OMIT 3 10 1 OMIT -1 3 22 OMIT -3 4 24 OMIT 1 9 5 OMIT -2 4 22 OMIT -2 2 23 OMIT 3 10 3 OMIT 0 3 19 OMIT 2 10 8 OMIT 0 8 7 OMIT 2 10 5 OMIT 2 1 18 OMIT 2 10 6 OMIT 0 1 19 OMIT -1 1 25 OMIT -1 3 21 OMIT 0 9 5 OMIT -1 1 23 OMIT -1 1 24 OMIT 2 10 10 OMIT 0 1 20 OMIT 2 10 12 OMIT 1 2 23 OMIT -1 8 7 OMIT -2 4 24 OMIT -3 6 23 OMIT 0 0 24 OMIT -1 1 21 OMIT 0 9 7 OMIT 0 8 3 OMIT 4 11 6 OMIT 2 10 9 OMIT -1 1 22 OMIT 2 10 4 OMIT 4 11 2 OMIT 1 10 11 OMIT 2 10 11 OMIT 3 10 0 OMIT -2 8 8 OMIT 2 10 1 OMIT -2 9 11 OMIT 3 10 2 OMIT 4 11 4 OMIT 2 10 7 OMIT 0 0 20 OMIT 2 10 3 OMIT 3 11 8 OMIT 1 10 13 OMIT -1 0 2 OMIT 0 2 1 OMIT 2 0 0 OMIT -1 1 7 OMIT -1 2 2 OMIT -1 2 6 OMIT 0 2 3 OMIT -2 4 3 OMIT -1 0 4 OMIT 0 2 4 OMIT 1 1 1 REM REM REM WGHT 0.044100 SWAT 0.020007 178.8756 FVAR 0.22456 PB1 5 0.168240 0.385960 0.269099 11.00000 0.03772 0.02663 = 0.02850 -0.00210 0.00799 -0.00085 O1 4 0.492211 0.320845 0.315632 11.00000 0.04953 0.03663 = 0.06022 0.00008 0.00697 -0.00228 AFIX 7 H1A 2 0.502676 0.233225 0.314676 11.00000 -1.50000 H1B 2 0.514055 0.340562 0.356774 11.00000 -1.50000 AFIX 0 O2 4 -0.182584 0.447762 0.295789 11.00000 0.06027 0.04388 = 0.06448 0.01257 0.02457 0.00715 O3 4 -0.110867 0.604845 0.234627 11.00000 0.06027 0.04388 = 0.06448 0.01257 0.02457 0.00715 O4 4 -0.296637 0.646074 0.303005 11.00000 0.06027 0.04388 = 0.06448 0.01257 0.02457 0.00715 O5 4 0.362060 0.544915 0.198992 11.00000 0.07173 0.07868 = 0.05055 -0.01943 0.01826 -0.02603 O6 4 0.156383 0.443910 0.131001 11.00000 0.09139 0.05551 = 0.04816 -0.00839 0.00524 -0.00372 N1 3 -0.199384 0.568480 0.277633 11.00000 0.03745 0.03299 = 0.03626 0.00440 0.00720 0.00194 N2 3 0.237132 0.578825 0.344239 11.00000 0.03786 0.02662 = 0.03351 -0.00025 0.00760 -0.00302 N3 3 0.164544 0.327561 0.386734 11.00000 0.03833 0.02916 = 0.03192 0.00282 0.00951 -0.00324 C1 1 0.134824 0.205791 0.408358 11.00000 0.05856 0.03394 = 0.04218 0.00336 0.01023 -0.00811 AFIX 43 H1 2 0.104322 0.135588 0.377963 11.00000 -1.20000 AFIX 0 C2 1 0.146179 0.175332 0.474014 11.00000 0.06658 0.04161 = 0.04831 0.01715 0.01448 0.00090 AFIX 43 H2 2 0.124384 0.086534 0.487388 11.00000 -1.20000 AFIX 0 C3 1 0.188946 0.275233 0.518144 11.00000 0.04716 0.05679 = 0.03310 0.01293 0.01277 0.00083 AFIX 43 H3 2 0.196554 0.256400 0.562652 11.00000 -1.20000 AFIX 0 C4 1 0.269645 0.513354 0.541399 11.00000 0.04768 0.05983 = 0.02877 -0.00290 0.00708 0.00004 AFIX 43 H4 2 0.280037 0.497759 0.586281 11.00000 -1.20000 AFIX 0 C5 1 0.300472 0.636345 0.520385 11.00000 0.05028 0.05248 = 0.03458 -0.01418 0.00212 0.00826 AFIX 43 H5 2 0.330157 0.706929 0.550621 11.00000 -1.20000 AFIX 0 C6 1 0.321913 0.791694 0.429629 11.00000 0.04865 0.03751 = 0.05420 -0.01444 0.00355 -0.00246 AFIX 43 H6 2 0.349606 0.865287 0.458242 11.00000 -1.20000 AFIX 0 C7 1 0.313260 0.810114 0.364873 11.00000 0.05107 0.02128 = 0.06335 -0.00181 0.01094 -0.00137 AFIX 43 H7 2 0.335728 0.895963 0.348110 11.00000 -1.20000 AFIX 0 C8 1 0.271489 0.702136 0.324620 11.00000 0.04610 0.03116 = 0.04130 0.00572 0.00914 -0.00331 AFIX 43 H8 2 0.266761 0.716236 0.279835 11.00000 -1.20000 AFIX 0 C9 1 0.245801 0.558623 0.408551 11.00000 0.02438 0.03543 = 0.02902 -0.00214 0.00458 -0.00103 C10 1 0.289864 0.664105 0.453693 11.00000 0.03535 0.03463 = 0.03869 -0.00776 0.00411 0.00445 C11 1 0.209128 0.427246 0.430796 11.00000 0.02722 0.03482 = 0.02959 0.00170 0.00648 0.00114 C12 1 0.221637 0.405509 0.497892 11.00000 0.03280 0.04459 = 0.03005 0.00446 0.00643 0.00541 C13 1 0.293122 0.517604 0.142733 11.00000 0.05953 0.02384 = 0.04587 0.00845 0.02248 0.00506 C14 1 0.367591 0.561851 0.097282 11.00000 0.05953 0.02384 = 0.04587 0.00845 0.02248 0.00506 AFIX 137 H14A 2 0.292695 0.637063 0.076866 11.00000 -1.50000 H14B 2 0.372233 0.490559 0.065594 11.00000 -1.50000 H14C 2 0.496116 0.592556 0.113821 11.00000 -1.50000 AFIX 0 HKLF 4 REM shelx in P2(1)/c REM wR2 = 0.0811, GooF = S = 1.029, Restrained GooF = 1.060 for all data REM R1 = 0.0323 for 2747 Fo > 4sig(Fo) and 0.0424 for all 3323 data REM 203 parameters refined using 2 restraints END WGHT 0.0441 0.0000 REM Highest difference peak 1.434, deepest hole -1.851, 1-sigma level 0.204 Q1 1 0.4014 0.6058 0.1175 11.00000 0.05 1.43 Q2 1 0.5081 0.8870 0.3064 11.00000 0.05 1.14 Q3 1 -0.1591 0.3475 0.2307 11.00000 0.05 1.05 Q4 1 -0.1634 0.4247 0.2679 11.00000 0.05 0.98 Q5 1 0.3168 0.5390 0.1326 11.00000 0.05 0.88 Q6 1 0.3203 0.5221 0.0794 11.00000 0.05 0.74 Q7 1 0.4940 0.9380 0.2578 11.00000 0.05 0.66 Q8 1 0.0145 0.4544 0.2867 11.00000 0.05 0.65 Q9 1 0.1150 0.2870 0.2142 11.00000 0.05 0.64 Q10 1 0.2633 0.4638 0.2261 11.00000 0.05 0.64 REM The information below was added by Olex2. REM REM R1 = 0.0323 for 2747 Fo > 4sig(Fo) and 0.0424 for all 13453 data REM n/a parameters refined using n/a restraints REM Highest difference peak 1.43, deepest hole -1.85 REM Mean Shift 0, Max Shift -0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0424 REM R1_gt = 0.0323 REM wR_ref = 0.0811 REM GOOF = 1.029 REM Shift_max = -0.001 REM Shift_mean = 0 REM Reflections_all = 13453 REM Reflections_gt = 2747 REM Parameters = n/a REM Hole = -1.85 REM Peak = 1.43 REM Flack = n/a ; _olex2_submission_special_instructions 'No special instructions were received'