data_ds _audit_creation_date 2019-12-13 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number '2018/3' _audit_contact_author_address ? _audit_contact_author_email ? _audit_contact_author_name '' _audit_contact_author_phone ? _publ_contact_author_id_orcid ? _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 'C23 H20 Cl F2 N O4 S' _chemical_formula_sum 'C23 H20 Cl F2 N O4 S' _chemical_formula_weight 479.91 _chemical_absolute_configuration rm _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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 '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' 'S' 'S' 0.1246 0.1234 '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 4 _space_group_name_H-M_alt 'P 1 21 1' _space_group_name_Hall 'P 2yb' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 5.5826(8) _cell_length_b 16.132(2) _cell_length_c 11.8958(13) _cell_angle_alpha 90 _cell_angle_beta 90.12(5) _cell_angle_gamma 90 _cell_volume 1071.3(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 4059 _cell_measurement_temperature 170 _cell_measurement_theta_max 25.505 _cell_measurement_theta_min 2.525 _shelx_estimated_absorpt_T_max 0.974 _shelx_estimated_absorpt_T_min 0.941 _exptl_absorpt_coefficient_mu 0.325 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.6926 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0905 before and 0.0580 after correction. The Ratio of minimum to maximum transmission is 0.9292. The \l/2 correction factor is Not present.' _exptl_absorpt_special_details ? _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.488 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 496 _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0518 _diffrn_reflns_av_unetI/netI 0.0626 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.991 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 12417 _diffrn_reflns_point_group_measured_fraction_full 0.981 _diffrn_reflns_point_group_measured_fraction_max 0.959 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.564 _diffrn_reflns_theta_min 2.525 _diffrn_ambient_temperature 170.0 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_device_type 'D8 VENTURE' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source ? _diffrn_standards_number 0 _reflns_Friedel_coverage 0.866 _reflns_Friedel_fraction_full 0.962 _reflns_Friedel_fraction_max 0.924 _reflns_number_gt 3351 _reflns_number_total 4273 _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 'SAINT V8.38A (?, 2016)' _computing_data_collection ? _computing_data_reduction 'SAINT V8.38A (?, 2016)' _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 0.247 _refine_diff_density_min -0.317 _refine_diff_density_rms 0.056 _refine_ls_abs_structure_details ; Flack x determined using 1263 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.07(5) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 290 _refine_ls_number_reflns 4273 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0685 _refine_ls_R_factor_gt 0.0434 _refine_ls_restrained_S_all 1.035 _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^)+(0.0405P)^2^+0.1790P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0836 _refine_ls_wR_factor_ref 0.0982 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C8(H8), C9(H9) 2.b Aromatic/amide H refined with riding coordinates: N1(H1), C22(H22), C16(H16), C19(H19), C21(H21), C12(H12), C18(H18), C13(H13), C14(H14), C15(H15), C1(H1A), C4(H4), C5(H5), C3(H3), C2(H2) 2.c Idealised Me refined as rotating group: C23(H23A,H23B,H23C) ; _atom_sites_solution_hydrogens geom _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 S1 S 0.55533(19) 0.46500(8) 0.51198(9) 0.0294(3) Uani 1 1 d . . . . . Cl1 Cl 0.8607(2) 0.46255(8) 0.06600(9) 0.0347(3) Uani 1 1 d . . . . . F2 F 0.9402(5) 0.38823(16) 0.4369(2) 0.0350(7) Uani 1 1 d . . . . . F1 F 0.5991(5) 0.33950(15) 0.3822(2) 0.0373(7) Uani 1 1 d . . . . . O2 O 0.3610(6) 0.5048(2) 0.4549(3) 0.0375(8) Uani 1 1 d . . . . . O3 O 0.3769(6) 0.3789(2) 0.1742(3) 0.0362(8) Uani 1 1 d . . . . . O4 O 0.8605(6) 0.85971(19) 0.2016(3) 0.0394(9) Uani 1 1 d . . . . . O1 O 0.5112(7) 0.4026(2) 0.5950(3) 0.0450(9) Uani 1 1 d . . . . . N1 N 0.9186(7) 0.5241(2) 0.3070(3) 0.0277(9) Uani 1 1 d . . . . . H1 H 1.053982 0.509419 0.339308 0.033 Uiso 1 1 calc R . . . . C17 C 0.8918(8) 0.6074(3) 0.2781(3) 0.0239(10) Uani 1 1 d . . . . . C22 C 1.0712(8) 0.6633(3) 0.3097(4) 0.0281(11) Uani 1 1 d . . . . . H22 H 1.206848 0.643575 0.349951 0.034 Uiso 1 1 calc R . . . . C11 C 0.6120(8) 0.2663(3) 0.1116(4) 0.0240(10) Uani 1 1 d . . . . . C16 C 0.4355(9) 0.2072(3) 0.1290(4) 0.0287(11) Uani 1 1 d . . . . . H16 H 0.296956 0.221123 0.171227 0.034 Uiso 1 1 calc R . . . . C10 C 0.5757(8) 0.3502(3) 0.1587(4) 0.0252(10) Uani 1 1 d . . . . . C19 C 0.6786(9) 0.7227(3) 0.1953(4) 0.0305(11) Uani 1 1 d . . . . . H19 H 0.542044 0.742970 0.156198 0.037 Uiso 1 1 calc R . . . . C21 C 1.0557(9) 0.7458(3) 0.2838(4) 0.0313(11) Uani 1 1 d . . . . . H21 H 1.180834 0.782339 0.305672 0.038 Uiso 1 1 calc R . . . . C20 C 0.8580(9) 0.7767(3) 0.2257(4) 0.0283(11) Uani 1 1 d . . . . . C12 C 0.8146(9) 0.2452(3) 0.0483(4) 0.0293(11) Uani 1 1 d . . . . . H12 H 0.938681 0.284651 0.037496 0.035 Uiso 1 1 calc R . . . . C8 C 0.7448(7) 0.4610(3) 0.2885(3) 0.0239(9) Uani 1 1 d . . . . . H8 H 0.587365 0.488613 0.274037 0.029 Uiso 1 1 calc R . . . . C18 C 0.6947(8) 0.6385(3) 0.2214(4) 0.0262(10) Uani 1 1 d . . . . . H18 H 0.568854 0.602143 0.199869 0.031 Uiso 1 1 calc R . . . . C13 C 0.8340(8) 0.1669(3) 0.0017(4) 0.0302(11) Uani 1 1 d . . . . . H13 H 0.968886 0.153355 -0.043291 0.036 Uiso 1 1 calc R . . . . C7 C 0.7226(8) 0.4113(3) 0.3978(4) 0.0280(10) Uani 1 1 d . . . . . C14 C 0.6580(9) 0.1085(3) 0.0203(4) 0.0299(11) Uani 1 1 d . . . . . H14 H 0.672567 0.054736 -0.011483 0.036 Uiso 1 1 calc R . . . . C15 C 0.4594(9) 0.1282(3) 0.0854(4) 0.0317(11) Uani 1 1 d . . . . . H15 H 0.340543 0.087429 0.099863 0.038 Uiso 1 1 calc R . . . . C9 C 0.7958(8) 0.4021(3) 0.1893(3) 0.0249(10) Uani 1 1 d . . . . . H9 H 0.934113 0.365036 0.207599 0.030 Uiso 1 1 calc R . . . . C6 C 0.7432(8) 0.5412(3) 0.5677(4) 0.0294(11) Uani 1 1 d . . . . . C1 C 0.7098(10) 0.6229(3) 0.5362(4) 0.0377(12) Uani 1 1 d . . . . . H1A H 0.587114 0.637212 0.484264 0.045 Uiso 1 1 calc R . . . . C4 C 1.0679(10) 0.5796(4) 0.6845(5) 0.0499(15) Uani 1 1 d . . . . . H4 H 1.192915 0.565560 0.735358 0.060 Uiso 1 1 calc R . . . . C5 C 0.9216(9) 0.5175(3) 0.6428(4) 0.0399(13) Uani 1 1 d . . . . . H5 H 0.942191 0.461215 0.664419 0.048 Uiso 1 1 calc R . . . . C23 C 0.6608(10) 0.8917(3) 0.1423(4) 0.0433(13) Uani 1 1 d . . . . . H23A H 0.648465 0.864344 0.068985 0.065 Uiso 1 1 calc GR . . . . H23B H 0.681275 0.951501 0.131403 0.065 Uiso 1 1 calc GR . . . . H23C H 0.514540 0.881430 0.185521 0.065 Uiso 1 1 calc GR . . . . C3 C 1.0368(11) 0.6613(4) 0.6540(5) 0.0512(16) Uani 1 1 d . . . . . H3 H 1.140701 0.702540 0.683766 0.061 Uiso 1 1 calc R . . . . C2 C 0.8573(11) 0.6839(3) 0.5813(5) 0.0483(15) Uani 1 1 d . . . . . H2 H 0.834158 0.740424 0.561904 0.058 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 S1 0.0268(6) 0.0347(6) 0.0267(5) 0.0013(6) -0.0002(4) -0.0036(6) Cl1 0.0417(7) 0.0325(6) 0.0299(6) 0.0030(6) 0.0052(5) -0.0008(7) F2 0.0342(16) 0.0339(16) 0.0369(15) 0.0047(12) -0.0076(12) 0.0068(13) F1 0.0483(18) 0.0245(15) 0.0390(16) 0.0026(12) -0.0053(13) -0.0116(13) O2 0.0239(19) 0.054(2) 0.0349(18) -0.0033(16) -0.0062(15) 0.0059(16) O3 0.0210(18) 0.041(2) 0.046(2) -0.0110(16) -0.0030(15) 0.0057(15) O4 0.051(2) 0.0226(18) 0.045(2) 0.0032(15) -0.0026(17) -0.0022(16) O1 0.056(2) 0.046(2) 0.0338(19) 0.0092(17) 0.0048(17) -0.014(2) N1 0.025(2) 0.023(2) 0.035(2) 0.0023(17) -0.0105(17) -0.0025(17) C17 0.026(2) 0.024(2) 0.021(2) -0.0017(18) 0.0025(18) 0.000(2) C22 0.023(3) 0.031(3) 0.030(3) 0.000(2) -0.003(2) 0.001(2) C11 0.021(2) 0.028(2) 0.023(2) -0.0005(19) -0.0028(18) 0.002(2) C16 0.021(3) 0.036(3) 0.028(3) -0.001(2) 0.001(2) -0.003(2) C10 0.026(3) 0.029(2) 0.021(2) -0.0028(19) -0.0021(19) 0.001(2) C19 0.032(3) 0.031(3) 0.028(3) 0.001(2) 0.000(2) 0.004(2) C21 0.030(3) 0.029(3) 0.035(3) -0.003(2) 0.001(2) -0.004(2) C20 0.034(3) 0.020(2) 0.030(3) 0.0011(19) 0.006(2) 0.001(2) C12 0.026(3) 0.029(3) 0.033(3) 0.000(2) 0.003(2) 0.000(2) C8 0.022(2) 0.022(2) 0.028(2) 0.003(2) -0.0011(16) 0.000(2) C18 0.024(2) 0.025(2) 0.029(2) -0.0031(19) -0.0017(19) 0.001(2) C13 0.030(3) 0.034(3) 0.026(2) 0.001(2) -0.001(2) 0.004(2) C7 0.028(3) 0.022(2) 0.034(3) 0.0035(19) -0.007(2) -0.003(2) C14 0.038(3) 0.024(2) 0.028(2) -0.0018(19) -0.010(2) 0.000(2) C15 0.030(3) 0.028(3) 0.037(3) 0.002(2) -0.005(2) -0.009(2) C9 0.023(2) 0.023(2) 0.028(2) 0.0009(18) -0.0032(19) 0.000(2) C6 0.024(3) 0.040(3) 0.024(2) -0.003(2) -0.0008(19) -0.002(2) C1 0.044(3) 0.036(3) 0.032(3) -0.001(2) 0.000(2) 0.001(3) C4 0.034(3) 0.077(5) 0.039(3) -0.018(3) -0.009(2) -0.003(3) C5 0.037(3) 0.048(3) 0.035(3) -0.006(2) -0.005(2) 0.004(3) C23 0.063(4) 0.025(3) 0.042(3) 0.006(2) 0.000(3) 0.007(3) C3 0.046(4) 0.064(4) 0.044(3) -0.027(3) 0.005(3) -0.012(3) C2 0.063(4) 0.039(3) 0.044(3) -0.013(3) 0.010(3) -0.012(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 S1 O2 1.430(3) . ? S1 O1 1.432(3) . ? S1 C7 1.863(5) . ? S1 C6 1.745(5) . ? Cl1 C9 1.799(4) . ? F2 C7 1.352(5) . ? F1 C7 1.360(5) . ? O3 C10 1.217(5) . ? O4 C20 1.370(5) . ? O4 C23 1.415(6) . ? N1 C17 1.394(6) . ? N1 C8 1.423(6) . ? C17 C22 1.399(6) . ? C17 C18 1.384(6) . ? C22 C21 1.369(6) . ? C11 C16 1.388(6) . ? C11 C10 1.479(6) . ? C11 C12 1.402(6) . ? C16 C15 1.383(7) . ? C10 C9 1.530(6) . ? C19 C20 1.375(7) . ? C19 C18 1.396(6) . ? C21 C20 1.393(7) . ? C12 C13 1.384(6) . ? C8 C7 1.534(6) . ? C8 C9 1.543(6) . ? C13 C14 1.379(7) . ? C14 C15 1.390(7) . ? C6 C1 1.383(7) . ? C6 C5 1.390(7) . ? C1 C2 1.389(7) . ? C4 C5 1.385(8) . ? C4 C3 1.378(9) . ? C3 C2 1.372(8) . ? 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 S1 O1 120.7(2) . . ? O2 S1 C7 104.11(19) . . ? O2 S1 C6 108.6(2) . . ? O1 S1 C7 105.2(2) . . ? O1 S1 C6 109.7(2) . . ? C6 S1 C7 107.6(2) . . ? C20 O4 C23 116.9(4) . . ? C17 N1 C8 125.4(4) . . ? N1 C17 C22 118.6(4) . . ? C18 C17 N1 123.7(4) . . ? C18 C17 C22 117.7(4) . . ? C21 C22 C17 121.5(4) . . ? C16 C11 C10 118.3(4) . . ? C16 C11 C12 119.1(4) . . ? C12 C11 C10 122.5(4) . . ? C15 C16 C11 120.6(4) . . ? O3 C10 C11 122.1(4) . . ? O3 C10 C9 119.2(4) . . ? C11 C10 C9 118.7(4) . . ? C20 C19 C18 120.7(5) . . ? C22 C21 C20 120.6(4) . . ? O4 C20 C19 124.9(5) . . ? O4 C20 C21 116.4(4) . . ? C19 C20 C21 118.7(4) . . ? C13 C12 C11 120.1(4) . . ? N1 C8 C7 107.4(3) . . ? N1 C8 C9 115.6(3) . . ? C7 C8 C9 110.0(4) . . ? C17 C18 C19 120.8(4) . . ? C14 C13 C12 120.1(4) . . ? F2 C7 S1 109.2(3) . . ? F2 C7 F1 105.5(3) . . ? F2 C7 C8 111.2(4) . . ? F1 C7 S1 103.9(3) . . ? F1 C7 C8 111.8(4) . . ? C8 C7 S1 114.6(3) . . ? C13 C14 C15 120.2(4) . . ? C16 C15 C14 119.8(4) . . ? C10 C9 Cl1 105.4(3) . . ? C10 C9 C8 111.7(3) . . ? C8 C9 Cl1 109.1(3) . . ? C1 C6 S1 119.2(4) . . ? C1 C6 C5 122.2(5) . . ? C5 C6 S1 118.6(4) . . ? C6 C1 C2 119.4(5) . . ? C3 C4 C5 121.6(5) . . ? C4 C5 C6 116.9(5) . . ? C2 C3 C4 120.7(5) . . ? C3 C2 C1 119.2(6) . . ? loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma 1 0 0 4.9 2 1 0 0 0.2 1.1 -1 0 0 0.1 1.2 -1 0 0 1.6 1.3 2 0 0 409.56 22.6 2 0 0 392.66 19.5 -2 0 0 363.46 20.6 -2 0 0 388.36 19.8 3 0 0 74.89 9.7 3 0 0 77.49 14 -3 0 0 70.89 13.2 -3 0 0 65.39 12.5 4 0 0 731.83 43.9 4 0 0 773.22 39.2 -4 0 0 759.72 40 -4 0 0 734.73 42.4 5 0 0 30.3 11.2 5 0 0 34.7 15.5 -5 0 0 26 11.8 -5 0 0 42.5 12.4 -6 0 0 46.6 16.7 -6 0 -1 59.09 17.9 -5 0 -1 -6.8 9.8 -5 0 -1 3.8 6.8 -4 0 -1 278.67 26.3 -4 0 -1 287.37 24.1 4 0 1 303.27 27.6 4 0 1 275.27 22.9 -3 0 -1 109.09 14.3 -3 0 -1 110.69 13 3 0 1 149.99 16.4 3 0 1 141.69 14.6 -2 0 -1 118.09 10.6 -2 0 -1 117.49 11.8 2 0 1 120.19 12.2 2 0 1 131.99 11.2 -1 0 -1 4995.1 97.69 -1 0 -1 5064.89 101.49 1 0 1 5196.08 102.29 1 0 -1 4114.59 81.29 1 0 -1 4076.79 82.59 -1 0 1 4075.19 82.89 -1 0 1 4277.67 81.69 2 0 -1 2877.61 72.59 2 0 -1 2954.2 70.79 -2 0 1 2903.11 72.09 -2 0 1 2714.63 69.59 3 0 -1 419.06 27.7 3 0 -1 406.86 24.3 -3 0 1 437.46 25.6 -3 0 1 301.37 37.7 4 0 -1 525.05 36 4 0 -1 537.25 32.4 -4 0 1 546.95 35 -4 0 1 506.55 32.7 5 0 -1 158.58 19.1 5 0 -1 115.89 23.9 -5 0 1 187.08 27.2 -5 0 1 171.38 22.4 6 0 -1 413.56 35.9 -6 0 1 311.97 34.1 -6 0 -2 -1.4 9.7 -5 0 -2 40.8 15.1 -4 0 -2 45.5 12 -4 0 -2 29.2 11.4 4 0 2 35.1 12.2 -3 0 -2 352.26 23.3 -3 0 -2 353.16 25.6 3 0 2 315.97 25.2 -2 0 -2 588.24 28.6 -2 0 -2 550.34 25.2 2 0 2 577.74 29.4 -1 0 -2 25.7 5.5 1 0 2 22.6 2.9 1 0 2 28 5.6 0 0 -2 158.58 6.3 0 0 -2 174.98 7.8 0 0 -2 177.48 10.4 0 0 2 176.68 6.7 1 0 -2 8540.65 159.38 1 0 -2 8297.27 150.18 -1 0 2 8199.58 149.88 -1 0 2 8650.63 160.18 2 0 -2 309.87 18.2 2 0 -2 337.87 19.4 -2 0 2 335.37 18.4 -2 0 2 313.67 19.5 3 0 -2 97.59 15.2 -3 0 2 110.09 12.5 -3 0 2 96.09 13.3 4 0 -2 41.9 10.8 4 0 -2 69.59 14.9 -4 0 2 40.6 12.3 -4 0 2 52.29 12.8 5 0 -2 365.36 35.5 5 0 -2 387.06 31 -5 0 2 362.86 33.4 -5 0 2 401.96 34.1 6 0 -2 45.8 15.9 -6 0 2 60.79 18.8 -6 0 -3 40.7 19.1 6 0 3 30.8 14.5 -5 0 -3 246.28 27.2 -5 0 -3 246.48 29.3 -4 0 -3 19.7 9.8 -4 0 -3 19.1 8.1 4 0 3 13 15.5 -3 0 -3 47.5 10.9 -3 0 -3 37.8 10.2 3 0 3 60.89 12.6 -2 0 -3 164.28 14.9 2 0 3 174.38 11.5 2 0 3 182.88 20 -1 0 -3 4950.2 103.99 1 0 3 5046.7 105.19 1 0 3 4795.22 89.09 0 0 -3 261.77 11.8 0 0 -3 278.07 16.4 0 0 -3 271.67 10 0 0 3 265.97 10.1 1 0 -3 9631.14 188.48 1 0 -3 9722.23 171.08 -1 0 3 9999 189.38 2 0 -3 7.3 3.9 2 0 -3 10.5 4.1 -2 0 3 9.6 4.5 -2 0 3 10.9 3.5 3 0 -3 167.98 16.8 3 0 -3 177.58 17.1 -3 0 3 154.78 14.9 -3 0 3 165.88 16.6 4 0 -3 -3.3 3.3 4 0 -3 10.3 7.6 -4 0 3 0.4 6.3 -4 0 3 12.9 7.4 5 0 -3 -0.9 9.4 5 0 -3 12.9 9.2 -5 0 3 15.1 8.6 -5 0 3 9.4 12.1 6 0 -3 68.69 18.5 -6 0 -4 -18.7 10.3 -5 0 -4 203.88 27.8 5 0 4 211.38 22.6 -4 0 -4 37.9 11.9 -4 0 -4 39.4 13.1 4 0 4 39.2 10.4 4 0 4 13.8 8.1 -3 0 -4 29.1 9.2 -3 0 -4 23.1 7.9 3 0 4 9.1 5.1 3 0 4 30.4 9.6 -2 0 -4 210.78 17.3 2 0 4 212.58 18.6 2 0 4 213.08 12.2 -1 0 -4 2087.59 41.1 -1 0 -4 2051.99 55.09 1 0 4 2050.49 41.9 1 0 4 1994.1 55.09 0 0 -4 0.9 2.5 0 0 -4 3.9 1.7 0 0 -4 2.2 1.6 0 0 4 -1.4 1.1 1 0 -4 65.69 10.9 1 0 -4 54.49 3.8 -1 0 4 54.49 10 2 0 -4 265.37 15 2 0 -4 277.17 20.6 -2 0 4 246.68 19.6 3 0 -4 121.39 15.3 3 0 -4 112.09 14 -3 0 4 144.69 16.3 4 0 -4 47.9 12.7 4 0 -4 34.1 11.1 -4 0 4 56.99 15.8 5 0 -4 2 9.2 5 0 -4 20.2 12.6 -5 0 4 16.2 12.1 6 0 -4 47.2 15.4 -6 0 -5 104.79 26 6 0 5 112.79 20.3 -5 0 -5 22.3 13.7 5 0 5 44.5 11.3 -4 0 -5 3.5 6.8 -4 0 -5 7.8 6.3 4 0 5 9.9 8.4 4 0 5 10.2 4.7 -3 0 -5 89.69 15.6 -3 0 -5 92.29 16.6 3 0 5 87.39 17.1 3 0 5 81.29 9.7 -2 0 -5 92.59 12.2 2 0 5 83.69 14.5 2 0 5 94.59 7.4 -1 0 -5 2.5 1.2 -1 0 -5 3.2 2.8 1 0 5 5.1 3.9 1 0 5 2.7 1.5 0 0 -5 21.6 7.3 0 0 -5 9.2 3.1 0 0 -5 21.7 3.9 0 0 5 11.2 3 1 0 -5 170.18 16.4 1 0 -5 208.08 17.1 1 0 -5 200.68 6.1 1 0 -5 213.48 6.5 -1 0 5 193.28 17.3 2 0 -5 4280.67 89.69 2 0 -5 4275.17 110.39 -2 0 5 4372.96 112.59 3 0 -5 -2.9 3.6 3 0 -5 1.1 4.4 -3 0 5 3.3 6 4 0 -5 12.5 7.9 4 0 -5 -4.6 5.4 -4 0 5 0.6 7.1 5 0 -5 177.48 20.4 6 0 -5 217.78 27 -6 0 -6 94.59 22.3 6 0 6 73.69 16.8 -5 0 -6 4.4 10.8 5 0 6 0.9 6.6 -4 0 -6 173.88 21.3 -4 0 -6 161.38 22.3 4 0 6 125.59 24.4 4 0 6 170.58 17.7 -3 0 -6 138.89 17.7 3 0 6 141.19 23.4 3 0 6 143.59 11.5 -2 0 -6 8.8 4.9 2 0 6 0.3 5.4 2 0 6 9.7 3.1 -1 0 -6 574.64 16 -1 0 -6 577.94 26.4 1 0 6 553.54 17.5 1 0 6 585.24 27.5 0 0 -6 38.7 6.8 0 0 -6 31.2 4.2 0 0 -6 44.9 10.9 0 0 6 29.8 4.9 1 0 -6 2523.35 73.99 1 0 -6 2567.34 79.89 -1 0 6 2674.43 82.19 2 0 -6 277.67 23.6 2 0 -6 250.67 12.8 2 0 -6 236.28 22.7 -2 0 6 268.27 23.2 3 0 -6 85.59 16.9 3 0 -6 83.39 10.5 -3 0 6 92.89 17.3 4 0 -6 102.99 19.7 4 0 -6 106.19 17.1 -4 0 6 84.59 18.9 5 0 -6 124.69 23.1 5 0 -6 178.88 22.9 6 0 -6 20.7 13.1 -6 0 -7 15.1 23.5 6 0 7 53.79 22.7 6 0 7 18.2 10.9 -5 0 -7 13.9 12.4 5 0 7 0.9 6.3 -4 0 -7 27.8 12.7 4 0 7 -0.5 4.7 -3 0 -7 234.28 23.8 3 0 7 230.88 13.7 3 0 7 232.58 25.7 -2 0 -7 629.84 34.5 2 0 7 634.44 36 2 0 7 599.24 18.2 -1 0 -7 3.2 3.6 1 0 7 -2.9 2.5 0 0 -7 6.6 5.1 0 0 -7 7.1 2.6 0 0 -7 3.1 3.6 0 0 7 3.7 2.5 1 0 -7 35 14.1 1 0 -7 56.79 13.1 -1 0 7 39.8 11.3 2 0 -7 773.32 43.1 2 0 -7 782.52 20.7 2 0 -7 814.72 21 2 0 -7 821.72 45.1 -2 0 7 797.82 44.1 3 0 -7 346.27 19.9 3 0 -7 334.37 29 3 0 -7 312.87 35.5 -3 0 7 318.57 28.7 4 0 -7 53.39 15 4 0 -7 61.19 12.4 -4 0 7 48.9 15.4 5 0 -7 3.2 9.1 5 0 -7 -2 10.7 6 0 -7 41.2 18.1 -5 0 -8 146.09 27.9 5 0 8 219.18 23.9 5 0 8 211.98 19 -4 0 -8 12.8 12.3 4 0 8 1.5 4.9 -3 0 -8 23.2 10.3 3 0 8 16.6 4.1 3 0 8 19.8 11.4 -2 0 -8 25.4 8.6 2 0 8 25.8 9.7 -1 0 -8 748.33 21 -1 0 -8 772.32 46.5 -1 0 -8 797.62 33.6 1 0 8 778.82 35.3 0 0 -8 565.04 20.4 0 0 -8 506.15 36 0 0 -8 538.55 25.8 0 0 8 549.74 21.1 1 0 -8 2127.59 78.69 1 0 -8 1946.81 68.59 -1 0 8 2014.9 79.39 2 0 -8 675.03 41.8 2 0 -8 649.04 41.8 -2 0 8 630.84 42.1 3 0 -8 -3.7 5.1 3 0 -8 7.4 10.6 3 0 -8 -4.6 2.6 -3 0 8 0.4 6.5 4 0 -8 118.59 15.6 5 0 -8 12.6 12.2 5 0 -8 -24.1 9.5 -5 0 -9 4 11.4 5 0 9 37.8 19.4 5 0 9 31.8 10.2 -4 0 -9 -12.8 8.5 4 0 9 6.3 5.9 4 0 9 -4.1 3.5 -3 0 -9 72.79 15.7 3 0 9 75.89 18.7 -2 0 -9 219.08 21.4 2 0 9 232.18 22.8 -1 0 -9 8.4 8.4 -1 0 -9 4.7 4.4 1 0 9 7 5 0 0 -9 158.38 14.2 0 0 -9 144.09 10 0 0 -9 187.38 22.5 0 0 9 159.58 10.8 1 0 -9 581.34 41.1 1 0 -9 579.14 34.4 2 0 -9 -9 7.9 2 0 -9 -6.4 5.4 -2 0 9 5.1 7.2 3 0 -9 379.36 35.4 3 0 -9 364.66 37.4 4 0 -9 -10.7 6.2 5 0 -9 12.6 10.9 5 0 -9 14.5 13.8 -5 0 -10 -24.5 10.8 5 0 10 10 5.8 5 0 10 1.2 7.2 -4 0 -10 79.79 18.2 -3 0 -10 9.3 9.9 3 0 10 0.6 12.5 -2 0 -10 62.89 13.5 2 0 10 42.6 14.4 -1 0 -10 120.69 6.6 -1 0 -10 159.48 15.1 -1 0 -10 147.69 26.6 1 0 10 86.69 21.5 0 0 -10 178.68 15.7 0 0 -10 152.18 26.9 0 0 10 163.38 10.5 1 0 -10 72.39 14.5 1 0 -10 89.19 20.3 2 0 -10 246.78 29.9 2 0 -10 235.68 27.8 3 0 -10 122.69 25.2 4 0 -10 -2.7 2.9 4 0 -10 10.6 3.5 4 0 -10 -15.1 7.3 5 0 -10 45.5 17.1 5 0 -10 28.6 15.6 -4 0 -11 9 12.8 -3 0 -11 11 10.4 3 0 11 4 15.9 -2 0 -11 171.58 21.1 -2 0 -11 144.29 29 2 0 11 214.38 23.2 -1 0 -11 50.39 17.1 -1 0 -11 65.39 12.1 1 0 11 76.19 13.5 0 0 -11 6.9 6.8 0 0 -11 3.8 7.2 1 0 -11 4.3 8.8 1 0 -11 -3.9 6.3 2 0 -11 5.9 13.8 2 0 -11 -11.9 7.4 3 0 -11 328.17 36.5 4 0 -11 38.3 16.4 -4 0 -12 17.8 12.9 -3 0 -12 9.1 12.8 -3 0 -12 37.2 15.4 -2 0 -12 -4 9 -2 0 -12 18.8 10.2 2 0 12 -17.6 9.6 -1 0 -12 69.89 22.1 1 0 12 87.29 13.7 0 0 -12 2.4 6.5 0 0 -12 0.5 9.1 1 0 -12 32.5 12.7 1 0 -12 11.3 8.7 2 0 -12 278.07 34.2 2 0 -12 287.27 31.8 3 0 -12 114.99 25.1 4 0 -12 1.8 12.9 -3 0 -13 -8.3 13.4 -2 0 -13 24.2 16 -2 0 -13 5 11.6 2 0 13 40.6 16.4 -1 0 -13 28 15.3 0 0 -13 6.4 9.2 0 0 -13 2.6 12.5 1 0 -13 96.99 21.9 1 0 -13 80.09 15.6 2 0 -13 -6.2 10.4 2 0 -13 -2.9 14.2 3 0 -13 38.5 16.9 -2 0 -14 6.4 13.9 2 0 14 20.5 16.5 -1 0 -14 39.7 15.1 1 0 14 31.5 10.3 0 0 -14 110.09 14.5 0 0 -14 94.39 28 1 0 -14 80.09 24.8 1 0 -14 54.69 16.2 2 0 -14 0.5 22 2 1 -14 144.99 28.5 1 1 -14 27.9 14.4 1 1 -14 46.6 21.4 0 1 -14 36.5 11.2 0 1 -14 50.39 20.3 1 -1 14 175.98 16.1 -1 1 -14 186.78 37.6 2 -1 14 29.1 17.7 -2 1 -14 4.9 18.5 3 1 -13 35.6 17.6 2 1 -13 20.9 14.7 1 1 -13 -11.2 11.9 1 1 -13 1.4 10.6 0 1 -13 193.38 34.3 1 -1 13 10.8 8 -1 1 -13 27.9 12.5 2 -1 13 61.29 17.2 -2 1 -13 77.49 23.3 4 1 -12 -25.5 11 3 1 -12 28.4 17.5 2 1 -12 32.4 17.5 2 1 -12 15.8 12.8 1 1 -12 113.69 25.2 1 1 -12 68.99 16.2 0 1 -12 24.7 9.1 0 1 -12 8 11.2 -1 1 -12 147.79 28.4 -1 1 -12 113.09 8.1 2 -1 12 78.89 17.1 -2 1 -12 85.59 21.4 -3 1 -12 31.5 15.8 -3 1 -12 11.1 11.7 -4 1 -12 60.39 20.8 4 1 -11 211.78 29.3 3 1 -11 40 17.7 2 1 -11 -12.3 11.1 2 1 -11 29.4 12.1 1 1 -11 41.4 13.2 1 1 -11 72.09 19.8 0 1 -11 186.18 19.1 0 1 -11 128.69 26.4 -1 1 -11 83.89 8.2 -1 1 -11 92.79 23 2 -1 11 332.37 30.3 -2 1 -11 280.77 34.9 -2 1 -11 315.07 26.2 3 -1 11 129.79 27 -3 1 -11 95.39 24.4 -3 1 -11 119.99 21.5 -4 1 -11 20.3 10.7 5 1 -10 51.09 18.7 4 1 -10 26.5 14.7 3 1 -10 18.7 13.2 2 1 -10 55.89 14.7 2 1 -10 27.1 13.4 1 1 -10 55.49 17 1 1 -10 61.39 12 0 -1 10 159.28 8.5 0 1 -10 122.69 14.3 0 1 -10 153.48 27.7 1 -1 10 98.29 12.6 -1 1 -10 106.39 12.3 -1 1 -10 82.09 20.3 -1 1 -10 89.49 7.7 2 -1 10 773.32 43.8 -2 1 -10 878.21 44.4 3 -1 10 10.9 11.6 -3 1 -10 -2.3 8.7 4 -1 10 137.99 10.2 -4 1 -10 91.49 20.1 5 -1 10 31.1 13.6 5 -1 10 33.9 9.5 -5 1 -10 40.1 17.2 5 1 -9 32 12.2 5 1 -9 -3.8 8.4 4 1 -9 203.48 14.9 4 1 -9 207.88 26.9 3 1 -9 157.28 29.9 3 1 -9 125.29 25.5 -2 -1 9 41.4 13.3 2 1 -9 15.1 7.5 2 1 -9 26.6 10.6 1 1 -9 565.44 42 1 1 -9 502.35 32.5 0 -1 9 432.16 16.6 0 1 -9 432.66 25.2 0 1 -9 421.16 34.9 1 -1 9 121.69 13.2 -1 1 -9 135.69 9.7 -1 1 -9 102.99 20.6 -1 1 -9 106.79 11.9 2 -1 9 11.4 3 2 -1 9 22.6 8.6 -2 1 -9 3.9 5.8 3 -1 9 116.59 9.6 3 -1 9 121.99 23.2 -3 1 -9 102.99 18.9 4 -1 9 118.79 11.7 -4 1 -9 98.19 21.5 5 -1 9 3.3 8.9 -5 1 -9 -4.9 9.2 5 1 -8 64.19 17.9 5 1 -8 38.6 15.2 4 1 -8 40.8 15 -3 -1 8 41.7 12.5 3 1 -8 64.29 6.6 3 1 -8 72.29 20 3 1 -8 57.09 15.2 -2 -1 8 914.11 53.79 2 1 -8 854.21 48.5 2 1 -8 880.61 49.6 -1 -1 8 50.09 14.6 1 1 -8 63.59 15.6 1 1 -8 62.19 12.6 0 -1 8 227.78 11.7 0 1 -8 217.68 23.6 0 1 -8 247.78 17.8 1 -1 8 237.18 18.1 -1 1 -8 225.18 12.5 -1 1 -8 254.97 17.8 -1 1 -8 252.37 26.4 2 -1 8 864.21 27.8 2 -1 8 895.01 44.9 -2 1 -8 930.11 43.6 3 -1 8 220.18 25.4 3 -1 8 197.38 13.9 -3 1 -8 201.38 23.4 4 -1 8 51.69 9.8 -4 1 -8 -2.6 10 5 -1 8 104.29 16.1 -5 1 -8 81.79 20.9 6 1 -7 57.59 18.8 5 1 -7 59.09 16.8 5 1 -7 42 14.8 4 1 -7 95.39 15.7 4 1 -7 115.29 22 -3 -1 7 199.28 33.5 3 1 -7 226.18 24.4 3 1 -7 245.58 15.7 -2 -1 7 74.69 16.5 2 1 -7 86.79 17.4 2 1 -7 96.69 17.4 -1 -1 7 253.97 24.1 1 1 -7 280.17 22.6 1 1 -7 262.47 24.8 0 -1 7 55.19 5.4 0 1 -7 47.5 12.5 0 1 -7 31.1 7.3 1 -1 7 254.67 17.9 1 -1 7 215.68 13.2 -1 1 -7 226.08 22.8 -1 1 -7 222.18 11.8 -1 1 -7 225.78 16.7 2 -1 7 101.19 8.6 2 -1 7 117.89 18.1 -2 1 -7 107.29 13.8 3 -1 7 110.99 20.2 3 -1 7 111.59 10.9 -3 1 -7 123.59 17 4 -1 7 255.77 19.6 -4 1 -7 258.67 29.1 5 -1 7 2.5 7.9 -5 1 -7 24.6 12 6 -1 7 12.2 10 -6 1 -7 29.7 16.5 6 1 -6 -11.4 8.4 5 1 -6 160.18 24.6 5 1 -6 213.28 26.3 -4 -1 6 127.99 22.1 4 1 -6 113.29 15.1 4 1 -6 107.09 19.6 -3 -1 6 19.1 11.3 3 1 -6 26.5 9.8 3 1 -6 23.5 11.8 3 1 -6 27.2 7 -2 -1 6 746.53 41.4 2 1 -6 760.62 41.9 2 1 -6 779.02 41.5 2 1 -6 782.42 23 -1 -1 6 1539.65 59.09 1 1 -6 1562.24 59.19 1 1 -6 1439.36 54.09 0 -1 6 6.1 2.6 0 1 -6 5.1 4.4 0 1 -6 15 4.4 1 -1 6 75.29 9.6 1 -1 6 73.59 7.2 -1 1 -6 76.49 6.3 -1 1 -6 82.29 9.2 2 -1 6 51.69 11.2 2 -1 6 34.2 6.1 -2 1 -6 74.29 13.5 3 -1 6 43.5 8.2 3 -1 6 48.7 13 -3 1 -6 55.29 13.6 4 -1 6 229.98 18.8 4 -1 6 258.87 29.1 -4 1 -6 198.28 25.3 -4 1 -6 193.38 22 5 -1 6 38.1 12.4 -5 1 -6 11.6 13.7 6 -1 6 12.1 9.3 -6 1 -6 18.6 11.8 6 1 -5 164.88 28.3 5 1 -5 19.7 10.3 5 1 -5 23.5 12.5 -4 -1 5 35 12.8 4 1 -5 19.9 7.9 4 1 -5 18.4 8.7 4 1 -5 3.4 12.1 -3 -1 5 329.97 27.1 3 1 -5 307.27 25.5 3 1 -5 264.07 27.6 3 1 -5 307.07 20.5 -2 -1 5 515.35 31.5 2 1 -5 514.95 20.3 2 1 -5 538.35 32.2 2 1 -5 565.94 34.5 -1 -1 5 377.76 25.3 1 1 -5 434.46 26.5 1 1 -5 413.96 25.4 0 -1 5 378.46 14 0 -1 5 364.16 18.9 0 1 -5 379.16 13.3 0 1 -5 376.76 18.8 0 1 -5 383.56 24.2 1 -1 5 2451.85 56.09 1 -1 5 2493.55 65.19 -1 1 -5 2561.94 64.79 -1 1 -5 2488.85 53.69 2 -1 5 35 6.2 2 -1 5 41.6 9.6 -2 1 -5 31.9 9.8 3 -1 5 382.46 21.5 3 -1 5 362.56 29.2 -3 1 -5 319.47 26.7 4 -1 5 704.03 35.5 4 -1 5 747.43 47.8 -4 1 -5 752.12 47.5 5 -1 5 79.59 15.1 -5 1 -5 95.19 21.4 6 -1 5 51.69 17.9 -6 1 -5 55.89 17.1 6 1 -4 60.19 18.3 -5 -1 4 7.9 8.3 5 1 -4 15.8 9.1 5 1 -4 13.3 10.2 -4 -1 4 62.09 12.8 -4 -1 4 89.19 18.1 4 1 -4 53.39 12.9 4 1 -4 37.9 11 -3 -1 4 778.62 41.3 -3 -1 4 816.52 34.7 3 1 -4 841.52 41.8 3 1 -4 797.52 36 -2 -1 4 178.08 17.5 -2 -1 4 194.18 12.4 2 1 -4 202.18 17.8 2 1 -4 199.58 19.4 2 1 -4 185.48 12.5 -1 -1 4 506.15 26.8 1 1 -4 507.25 26.5 1 1 -4 521.05 11.9 1 1 -4 509.55 26.5 0 -1 4 240.78 9.8 0 -1 4 225.38 13.5 0 1 -4 235.38 13.5 0 1 -4 252.47 17.7 0 1 -4 238.18 9.4 1 -1 4 546.05 18.8 1 -1 4 545.25 24.1 -1 1 -4 535.95 17.7 -1 1 -4 550.54 23.8 2 -1 4 101.49 12.9 2 -1 4 102.59 9 -2 1 -4 115.09 12.7 3 -1 4 855.31 35.4 3 -1 4 892.61 46 -3 1 -4 916.01 45.1 -3 1 -4 837.02 39.1 4 -1 4 21.4 7 4 -1 4 30.9 10.5 -4 1 -4 17.4 11.1 -4 1 -4 24.9 10 5 -1 4 334.27 28.2 -5 1 -4 338.57 31.2 -5 1 -4 260.37 31.2 6 -1 4 101.59 18.4 -6 1 -4 15 14.5 -6 -1 3 107.69 22.8 6 1 -3 91.99 18.4 -5 -1 3 246.28 24.6 -5 -1 3 206.18 28.4 5 1 -3 161.18 28 5 1 -3 178.78 20.9 -4 -1 3 70.19 15.7 -4 -1 3 66.19 14 4 1 -3 77.59 15.4 4 1 -3 78.09 15.5 -3 -1 3 25.2 8.2 -3 -1 3 26 7.3 3 1 -3 37.1 8.5 3 1 -3 31.4 8.9 -2 -1 3 80.99 13.5 -2 -1 3 69.79 7.9 2 1 -3 86.49 10.9 2 1 -3 77.19 8.3 -1 -1 3 5439.46 116.49 -1 -1 3 5364.46 96.59 1 1 -3 5246.77 116.49 1 1 -3 5360.96 97.49 1 1 -3 5417.36 115.49 0 -1 3 7911.21 146.69 0 -1 3 7909.31 137.39 0 -1 3 7837.42 153.78 0 1 -3 7799.42 153.58 0 1 -3 7657.93 145.09 1 -1 3 1579.34 37.7 1 -1 3 1606.34 45.4 -1 1 -3 1590.74 37.3 -1 1 -3 1816.32 46.9 2 -1 3 164.68 19.1 2 -1 3 167.48 11.9 -2 1 -3 174.58 15.8 3 -1 3 66.09 14.4 3 -1 3 55.29 10.5 -3 1 -3 44.8 9.5 -3 1 -3 73.49 14.7 4 -1 3 1302.97 51.79 4 -1 3 1243.18 82.39 -4 1 -3 1143.99 49.8 -4 1 -3 1068.79 56.39 5 -1 3 383.96 31.4 -5 1 -3 350.26 31.9 -5 1 -3 396.56 36.7 6 -1 3 1.7 8.2 -6 1 -3 15.7 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6 313.67 21.5 -3 -6 6 292.07 30.7 3 6 -6 282.37 32.3 3 6 -6 323.57 30.2 -2 -6 6 457.85 36.3 -2 -6 6 435.86 33.2 -2 -6 6 396.76 21.5 2 6 -6 401.96 33.9 2 6 -6 426.46 32.8 -1 -6 6 202.28 21.3 -1 -6 6 169.68 20.8 -1 -6 6 237.88 14.9 1 6 -6 185.38 19.9 1 6 -6 207.98 21.7 0 -6 6 265.17 23.8 0 -6 6 337.67 26.9 0 6 -6 287.87 22.9 0 6 -6 324.87 26 1 -6 6 78.89 14.9 1 -6 6 88.79 13.7 -1 6 -6 78.39 10.5 -1 6 -6 82.29 15.8 2 -6 6 190.08 19.5 2 -6 6 168.38 17.1 -2 6 -6 162.48 16.5 -2 6 -6 155.78 18.3 3 -6 6 218.68 21.8 3 -6 6 258.47 45.2 -3 6 -6 212.48 21.4 4 -6 6 293.47 26.7 -4 6 -6 318.17 25.8 5 -6 6 14.3 9.3 -5 6 -6 0.7 11.7 6 -6 6 42.4 17.4 -6 -6 5 84.19 20 6 6 -5 55.79 18.9 -5 -6 5 83.09 17.7 5 6 -5 108.69 21.6 5 6 -5 117.09 24.5 -4 -6 5 219.28 22.3 4 6 -5 230.58 24.5 4 6 -5 191.68 36.4 -3 -6 5 424.86 26.5 -3 -6 5 410.06 33.4 3 6 -5 415.06 36.5 3 6 -5 329.77 24.4 3 6 -5 305.37 28.9 -2 -6 5 392.86 22.3 -2 -6 5 429.96 34.6 -2 -6 5 396.86 31.1 2 6 -5 437.16 31.9 2 6 -5 399.36 22.8 2 6 -5 378.86 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106.59 25.7 -2 -18 -1 75.79 23.9 -1 -18 -1 275.57 44.4 -1 -18 -1 321.47 28.8 -1 -18 -1 263.87 36.5 0 -18 -1 24.1 14.4 0 -18 -1 26.9 9.3 0 -18 -1 10.9 9.9 1 -18 -1 30.4 14.9 1 -18 -1 54.29 22.7 2 -18 -1 -8 11 2 -18 -1 5.8 14.3 3 -18 -1 9.4 15.4 3 -18 -1 9.3 13.1 -3 -18 -2 2.6 15 -2 -18 -2 85.89 23.3 -2 -18 -2 83.09 28.2 -1 -18 -2 -19.7 10.5 -1 -18 -2 8.5 11.7 -1 -18 -2 -8.7 10.8 0 -18 -2 84.09 13.7 0 -18 -2 39.4 17.6 0 -18 -2 48.6 17.9 1 -18 -2 62.29 20.3 1 -18 -2 80.19 23.6 2 -18 -2 18.5 9.9 2 -18 -2 20.5 13.4 3 -18 -2 145.99 29 -2 -18 -3 15.1 21.3 -2 -18 -3 2.5 12.1 -1 -18 -3 33.9 15.4 -1 -18 -3 37.4 21.4 0 -18 -3 0.2 11.3 0 -18 -3 6.3 8.5 0 -18 -3 -5.6 12.7 1 -18 -3 8.9 10.9 2 -18 -3 112.49 26.7 2 -18 -3 108.49 25.7 -2 -18 -4 72.69 25.5 -2 -18 -4 124.29 30.1 -1 -18 -4 25.7 14.5 -1 -18 -4 10.7 12.8 -1 -18 -4 -6.1 12.6 0 -18 -4 -21 11.9 0 -18 -4 16.4 16.3 0 -18 -4 13.9 10.1 1 -18 -4 66.69 19.3 1 -18 -4 59.79 20.5 2 -18 -4 22 15.8 -2 -18 -5 136.69 31.4 -2 -18 -5 129.19 27.2 -1 -18 -5 8.7 19.4 -1 -18 -5 65.19 15.5 -1 -18 -5 27 16.9 0 -18 -5 93.09 22.9 0 -18 -5 67.99 13.9 1 -18 -5 25.1 12.2 2 -18 -5 21.3 20.3 -1 -18 -6 14.4 18.6 -1 -18 -6 11.4 17.5 0 -18 -6 -7.4 9.8 0 -18 -6 21.8 17.3 1 -18 -6 79.69 9 1 -18 -6 46.7 19 1 -18 -6 82.99 10.3 0 -19 5 25.7 17.3 -1 -19 4 0.2 13.8 -1 -19 4 69.99 26.2 1 19 -4 45.5 18.8 0 -19 4 79.29 19.2 0 -19 4 34.1 17.6 0 -19 4 87.69 26.1 0 19 -4 37.8 12.9 1 -19 4 0.8 16.3 1 -19 4 14.7 14.6 -1 -19 3 3.8 12.7 -1 -19 3 28.9 21 1 19 -3 -5.8 8.7 0 -19 3 -2.8 12 0 -19 3 26.6 25.5 1 -19 3 8.6 18.5 1 -19 3 38 16.7 -2 -19 2 -18.1 11.7 -2 -19 2 27.8 12.9 2 19 -2 -4.4 8.1 -1 -19 2 3.4 13.4 -1 -19 2 30.3 18.9 -1 -19 2 4.7 16.5 1 19 -2 7.3 10 0 -19 2 60.29 20.3 0 -19 2 60.59 14.8 0 -19 2 52.79 19.3 0 19 -2 61.29 13.3 1 -19 2 27.1 27 1 -19 2 36.5 19.9 2 -19 2 -4.4 15 2 -19 2 -6.7 14.7 -2 -19 1 31.9 18.9 -2 -19 1 18.3 17.6 2 19 -1 15.8 13 -1 -19 1 -10.4 13.2 -1 -19 1 1.9 11.5 -1 -19 1 4.8 15.5 1 19 -1 23.1 11 0 -19 1 28.2 10.2 0 -19 1 21.4 16.6 0 -19 1 35.7 13.4 1 -19 1 -0.3 11.7 1 -19 1 -11.3 14.8 2 -19 1 38.8 19 2 -19 1 100.89 25.3 -2 -19 0 -3.4 14.9 -1 -19 0 88.09 22.5 -1 -19 0 148.39 33.9 -1 -19 0 81.19 18.4 0 -19 0 7.7 8.9 0 -19 0 32.3 13.8 0 -19 0 9.8 10.4 1 -19 0 88.19 25.3 1 -19 0 161.08 32.5 2 -19 0 5.1 14.8 2 -19 0 15.3 14.1 -2 -19 -1 101.79 29.1 -2 -19 -1 169.98 32.5 -1 -19 -1 -2.4 12.1 -1 -19 -1 -5.9 15.8 -1 -19 -1 7.7 14.2 0 -19 -1 24.8 10.1 0 -19 -1 22.9 16.3 0 -19 -1 -3 10.1 1 -19 -1 0.6 13.1 1 -19 -1 12.5 16.9 2 -19 -1 58.09 20.1 -2 -19 -2 -24.2 13.5 -2 -19 -2 -3.6 15 -1 -19 -2 31.1 15.5 -1 -19 -2 3.1 14.3 -1 -19 -2 2.9 26.3 0 -19 -2 61.39 22.8 0 -19 -2 44.6 20.1 0 -19 -2 46.1 13.1 1 -19 -2 22.8 14.3 2 -19 -2 30.7 13.4 2 -19 -2 7.4 11.3 -1 -19 -3 -8 14.4 -1 -19 -3 -25.6 13.9 -1 -19 -3 17.3 16.6 0 -19 -3 8.8 9.3 1 -19 -3 8.1 10.9 1 -19 -3 24.7 17.1 -1 -19 -4 8.5 13.6 -1 -19 -4 -18.6 11.9 -1 -19 -4 57.59 17.1 0 -19 -4 12.5 12.7 0 -19 -4 -7.3 16.2 0 -19 -4 64.99 23 1 -19 -4 45.5 18.2 1 -19 -4 16.5 14.4 0 -19 -5 20.8 18.2 0 -20 2 55.09 17.3 0 -20 1 -14.1 14.1 0 -20 1 6.9 14 0 -20 1 16.9 16.4 0 -20 0 120.89 40.3 0 -20 0 128.69 22.7 0 -20 0 120.09 30.8 0 -20 -1 29.1 17.4 0 -20 -1 -9.9 22.8 0 -20 -2 23.5 15.3 _iucr_refine_instructions_details ; TITL ds_a.res in P2(1) ds.res created by SHELXL-2018/3 at 10:27:10 on 13-Dec-2019 REM Old TITL DS in P2(1) REM SHELXT solution in P2(1) REM R1 0.099, Rweak 0.023, Alpha 0.000, Orientation as input REM Flack x = -0.109 ( 0.054 ) from Parsons' quotients REM Formula found by SHELXT: C23 N2 O5 S2 CELL 0.71073 5.5826 16.1315 11.8958 90 90.12 90 ZERR 2 0.0008 0.002 0.0013 0 0.05 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H Cl F N O S UNIT 46 40 2 4 2 8 2 L.S. 4 PLAN 20 SIZE 0.19 0.12 0.08 TEMP -103.15 list 4 fmap 2 acta REM REM REM WGHT 0.040500 0.179000 FVAR 0.91564 S1 7 0.555331 0.465002 0.511976 11.00000 0.02676 0.03474 = 0.02668 0.00129 -0.00021 -0.00356 CL1 3 0.860748 0.462548 0.066000 11.00000 0.04175 0.03249 = 0.02990 0.00301 0.00518 -0.00083 F2 4 0.940206 0.388232 0.436888 11.00000 0.03416 0.03388 = 0.03695 0.00471 -0.00763 0.00675 F1 4 0.599083 0.339502 0.382187 11.00000 0.04829 0.02450 = 0.03896 0.00259 -0.00534 -0.01156 O2 6 0.360995 0.504759 0.454927 11.00000 0.02387 0.05378 = 0.03485 -0.00331 -0.00620 0.00589 O3 6 0.376939 0.378926 0.174189 11.00000 0.02104 0.04119 = 0.04623 -0.01097 -0.00305 0.00568 O4 6 0.860469 0.859707 0.201603 11.00000 0.05095 0.02262 = 0.04451 0.00322 -0.00259 -0.00220 O1 6 0.511222 0.402622 0.594989 11.00000 0.05552 0.04577 = 0.03384 0.00924 0.00480 -0.01391 N1 5 0.918572 0.524138 0.306991 11.00000 0.02501 0.02332 = 0.03462 0.00228 -0.01045 -0.00248 AFIX 43 H1 2 1.053982 0.509419 0.339308 11.00000 -1.20000 AFIX 0 C17 1 0.891847 0.607354 0.278120 11.00000 0.02627 0.02421 = 0.02111 -0.00173 0.00252 -0.00050 C22 1 1.071216 0.663285 0.309670 11.00000 0.02342 0.03074 = 0.03025 -0.00005 -0.00253 0.00073 AFIX 43 H22 2 1.206848 0.643575 0.349951 11.00000 -1.20000 AFIX 0 C11 1 0.612039 0.266335 0.111590 11.00000 0.02120 0.02795 = 0.02281 -0.00048 -0.00280 0.00211 C16 1 0.435479 0.207202 0.128993 11.00000 0.02138 0.03630 = 0.02832 -0.00114 0.00071 -0.00296 AFIX 43 H16 2 0.296956 0.221123 0.171227 11.00000 -1.20000 AFIX 0 C10 1 0.575694 0.350213 0.158708 11.00000 0.02586 0.02918 = 0.02050 -0.00280 -0.00208 0.00129 C19 1 0.678551 0.722729 0.195325 11.00000 0.03236 0.03096 = 0.02824 0.00063 0.00000 0.00351 AFIX 43 H19 2 0.542044 0.742970 0.156198 11.00000 -1.20000 AFIX 0 C21 1 1.055683 0.745800 0.283799 11.00000 0.02980 0.02882 = 0.03516 -0.00292 0.00110 -0.00407 AFIX 43 H21 2 1.180834 0.782339 0.305672 11.00000 -1.20000 AFIX 0 C20 1 0.857981 0.776674 0.225677 11.00000 0.03424 0.02008 = 0.03049 0.00112 0.00648 0.00149 C12 1 0.814560 0.245184 0.048342 11.00000 0.02635 0.02871 = 0.03291 0.00012 0.00278 -0.00006 AFIX 43 H12 2 0.938681 0.284651 0.037496 11.00000 -1.20000 AFIX 0 C8 1 0.744820 0.461001 0.288495 11.00000 0.02198 0.02184 = 0.02786 0.00256 -0.00107 -0.00036 AFIX 13 H8 2 0.587365 0.488613 0.274037 11.00000 -1.20000 AFIX 0 C18 1 0.694709 0.638513 0.221365 11.00000 0.02442 0.02500 = 0.02929 -0.00315 -0.00171 0.00068 AFIX 43 H18 2 0.568854 0.602143 0.199869 11.00000 -1.20000 AFIX 0 C13 1 0.834011 0.166910 0.001670 11.00000 0.02998 0.03421 = 0.02644 0.00057 -0.00081 0.00376 AFIX 43 H13 2 0.968886 0.153355 -0.043291 11.00000 -1.20000 AFIX 0 C7 1 0.722637 0.411275 0.397849 11.00000 0.02797 0.02198 = 0.03397 0.00347 -0.00736 -0.00336 C14 1 0.658039 0.108531 0.020277 11.00000 0.03751 0.02394 = 0.02828 -0.00176 -0.01003 -0.00049 AFIX 43 H14 2 0.672567 0.054736 -0.011483 11.00000 -1.20000 AFIX 0 C15 1 0.459423 0.128169 0.085382 11.00000 0.03016 0.02825 = 0.03661 0.00241 -0.00547 -0.00860 AFIX 43 H15 2 0.340543 0.087429 0.099863 11.00000 -1.20000 AFIX 0 C9 1 0.795779 0.402062 0.189265 11.00000 0.02297 0.02347 = 0.02818 0.00089 -0.00323 -0.00040 AFIX 13 H9 2 0.934113 0.365036 0.207599 11.00000 -1.20000 AFIX 0 C6 1 0.743187 0.541176 0.567723 11.00000 0.02373 0.04031 = 0.02409 -0.00284 -0.00081 -0.00155 C1 1 0.709779 0.622891 0.536219 11.00000 0.04447 0.03632 = 0.03227 -0.00064 -0.00006 0.00098 AFIX 43 H1A 2 0.587114 0.637212 0.484264 11.00000 -1.20000 AFIX 0 C4 1 1.067942 0.579602 0.684488 11.00000 0.03386 0.07741 = 0.03852 -0.01779 -0.00875 -0.00310 AFIX 43 H4 2 1.192915 0.565560 0.735358 11.00000 -1.20000 AFIX 0 C5 1 0.921601 0.517454 0.642762 11.00000 0.03668 0.04773 = 0.03536 -0.00573 -0.00459 0.00421 AFIX 43 H5 2 0.942191 0.461215 0.664419 11.00000 -1.20000 AFIX 0 C23 1 0.660843 0.891705 0.142321 11.00000 0.06313 0.02518 = 0.04174 0.00608 0.00007 0.00670 AFIX 137 H23A 2 0.648465 0.864344 0.068985 11.00000 -1.50000 H23B 2 0.681275 0.951501 0.131403 11.00000 -1.50000 H23C 2 0.514540 0.881430 0.185521 11.00000 -1.50000 AFIX 0 C3 1 1.036764 0.661347 0.654032 11.00000 0.04561 0.06380 = 0.04434 -0.02703 0.00488 -0.01210 AFIX 43 H3 2 1.140701 0.702540 0.683766 11.00000 -1.20000 AFIX 0 C2 1 0.857309 0.683851 0.581268 11.00000 0.06284 0.03859 = 0.04360 -0.01292 0.01039 -0.01196 AFIX 43 H2 2 0.834158 0.740424 0.561904 11.00000 -1.20000 AFIX 0 HKLF 4 REM ds_a.res in P2(1) REM wR2 = 0.0982, GooF = S = 1.035, Restrained GooF = 1.035 for all data REM R1 = 0.0434 for 3351 Fo > 4sig(Fo) and 0.0685 for all 4273 data REM 290 parameters refined using 1 restraints END WGHT 0.0316 0.2303 REM Highest difference peak 0.247, deepest hole -0.317, 1-sigma level 0.056 Q1 1 0.8330 0.7384 0.0820 11.00000 0.05 0.25 Q2 1 0.7734 0.9575 0.0379 11.00000 0.05 0.22 Q3 1 0.3324 0.2208 0.1405 11.00000 0.05 0.22 Q4 1 0.7996 0.9616 0.1418 11.00000 0.05 0.22 Q5 1 0.5293 0.2380 0.1119 11.00000 0.05 0.20 Q6 1 0.7058 0.7782 0.4357 11.00000 0.05 0.20 Q7 1 0.6816 0.7621 0.5586 11.00000 0.05 0.20 Q8 1 0.5710 0.5781 0.1532 11.00000 0.05 0.19 Q9 1 0.5415 0.5024 0.1166 11.00000 0.05 0.19 Q10 1 0.7422 0.4438 0.3429 11.00000 0.05 0.19 Q11 1 0.9188 0.5223 0.5196 11.00000 0.05 0.19 Q12 1 0.4109 0.4480 0.0912 11.00000 0.05 0.18 Q13 1 0.7050 0.3625 0.4778 11.00000 0.05 0.18 Q14 1 0.8809 0.3362 0.3760 11.00000 0.05 0.18 Q15 1 0.7083 0.8385 -0.0036 11.00000 0.05 0.17 Q16 1 0.5327 0.4667 0.2966 11.00000 0.05 0.17 Q17 1 0.6672 0.4984 -0.0032 11.00000 0.05 0.17 Q18 1 0.6862 0.4745 0.2780 11.00000 0.05 0.17 Q19 1 0.3295 0.2195 0.2264 11.00000 0.05 0.17 Q20 1 0.4816 0.1799 0.1579 11.00000 0.05 0.17 REM The information below was added by Olex2. REM REM R1 = 0.0434 for 3351 Fo > 4sig(Fo) and 0.0685 for all 12455 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.25, deepest hole -0.32 REM Mean Shift 0, Max Shift 0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0685 REM R1_gt = 0.0434 REM wR_ref = 0.0982 REM GOOF = 1.035 REM Shift_max = 0.001 REM Shift_mean = 0 REM Reflections_all = 12455 REM Reflections_gt = 3351 REM Parameters = n/a REM Hole = -0.32 REM Peak = 0.25 REM Flack = -0.07(5) ; _olex2_submission_special_instructions 'No special instructions were received'