# Electronic Supplementary Material (ESI) for Chemical Science. # This journal is © The Royal Society of Chemistry 2021 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_1_a _database_code_depnum_ccdc_archive 'CCDC 2106756' loop_ _audit_author_name _audit_author_address 'Qi Di' 'Jilin University' _audit_update_record ; 2021-09-01 deposited with the CCDC. 2021-10-08 downloaded from the CCDC. ; _audit_creation_date 2021-09-01 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C20 H16 N2 O2' _chemical_formula_sum 'C20 H16 N2 O2' _chemical_formula_weight 316.35 _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' _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_H-M_alt 'C 1 2/c 1' _space_group_name_Hall '-C 2yc' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y, -z+1/2' 3 'x+1/2, y+1/2, z' 4 '-x+1/2, y+1/2, -z+1/2' 5 '-x, -y, -z' 6 'x, -y, z-1/2' 7 '-x+1/2, -y+1/2, -z' 8 'x+1/2, -y+1/2, z-1/2' _cell_length_a 32.003(4) _cell_length_b 4.9042(6) _cell_length_c 20.488(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.159(4) _cell_angle_gamma 90.00 _cell_volume 3174.6(7) _cell_formula_units_Z 8 _cell_measurement_reflns_used 9840 _cell_measurement_temperature 98(2) _cell_measurement_theta_max 31.55 _cell_measurement_theta_min 2.56 _exptl_absorpt_coefficient_mu 0.087 _exptl_absorpt_correction_T_max 0.7462 _exptl_absorpt_correction_T_min 0.7037 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.324 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 1328 _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0482 _diffrn_reflns_av_unetI/netI 0.0341 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_h_min -46 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 30821 _diffrn_reflns_theta_full 31.58 _diffrn_reflns_theta_max 31.58 _diffrn_reflns_theta_min 2.56 _diffrn_ambient_temperature 100 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_current 1.2 _diffrn_source_power 0.06 _diffrn_source_voltage 50.0 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number 0 _reflns_number_gt 4352 _reflns_number_total 5308 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'SAINT V8.38A (Bruker, 2018)' _computing_data_collection ? _computing_data_reduction 'SAINT V8.38A (Bruker, 2018)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _refine_diff_density_max 0.432 _refine_diff_density_min -0.249 _refine_diff_density_rms 0.059 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 219 _refine_ls_number_reflns 5308 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0563 _refine_ls_R_factor_gt 0.0440 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0564P)^2^+2.3841P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1113 _refine_ls_wR_factor_ref 0.1233 _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. ; _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 2.a Aromatic/amide H refined with riding coordinates: C3(H3), C6(H6), C7(H7), C10(H10), C11(H11), C14(H14), C15(H15), C17(H17), C19(H19), C20(H20) 2.b Idealised Me refined as rotating group: C1(H1a,H1b,H1c), C18(H18a,H18b,H18c) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 O1 O 0.40689(3) 1.11398(18) 0.26724(4) 0.02523(18) Uani 1 1 d . . . O2 O 0.33326(2) 0.46109(17) 0.58838(4) 0.02316(17) Uani 1 1 d . . . N1 N 0.51482(3) -0.5102(2) 0.59119(5) 0.0267(2) Uani 1 1 d . . . N2 N 0.26086(3) 1.30806(18) 0.36876(4) 0.01918(18) Uani 1 1 d . . . C1 C 0.43586(4) 0.9150(3) 0.29861(6) 0.0274(2) Uani 1 1 d . . . H1A H 0.4453 0.9674 0.3442 0.041 Uiso 1 1 calc R . . H1B H 0.4601 0.9034 0.2756 0.041 Uiso 1 1 calc R . . H1C H 0.4219 0.7390 0.2973 0.041 Uiso 1 1 calc R . . C2 C 0.37091(3) 1.1582(2) 0.29431(5) 0.0191(2) Uani 1 1 d . . . C3 C 0.36111(3) 1.0178(2) 0.34881(5) 0.01751(19) Uani 1 1 d . . . H3 H 0.3794 0.8838 0.3700 0.021 Uiso 1 1 calc R . . C4 C 0.32305(3) 1.0815(2) 0.37144(5) 0.01642(18) Uani 1 1 d . . . C5 C 0.30263(3) 0.9870(2) 0.42549(5) 0.01681(19) Uani 1 1 d . . . C6 C 0.31474(3) 0.7912(2) 0.47671(5) 0.01684(18) Uani 1 1 d . . . H6 H 0.2967 0.7795 0.5086 0.020 Uiso 1 1 calc R . . C7 C 0.34828(3) 0.6206(2) 0.48596(5) 0.01595(18) Uani 1 1 d . . . H7 H 0.3669 0.6140 0.4548 0.019 Uiso 1 1 calc R . . C8 C 0.35553(3) 0.4461(2) 0.54463(5) 0.01557(18) Uani 1 1 d . . . C9 C 0.39114(3) 0.24265(19) 0.55254(5) 0.01457(17) Uani 1 1 d . . . C10 C 0.39951(3) 0.0988(2) 0.61225(5) 0.01799(19) Uani 1 1 d . . . H10 H 0.3836 0.1365 0.6460 0.022 Uiso 1 1 calc R . . C11 C 0.43091(3) -0.0982(2) 0.62212(5) 0.01886(19) Uani 1 1 d . . . H11 H 0.4365 -0.1929 0.6625 0.023 Uiso 1 1 calc R . . C12 C 0.45416(3) -0.1548(2) 0.57147(5) 0.01651(18) Uani 1 1 d . . . C13 C 0.48750(3) -0.3554(2) 0.58206(5) 0.01929(19) Uani 1 1 d . . . C14 C 0.34370(4) 1.3599(2) 0.26171(5) 0.0220(2) Uani 1 1 d . . . H14 H 0.3512 1.4515 0.2250 0.026 Uiso 1 1 calc R . . C15 C 0.30625(4) 1.4232(2) 0.28335(5) 0.0213(2) Uani 1 1 d . . . H15 H 0.2880 1.5573 0.2620 0.026 Uiso 1 1 calc R . . C16 C 0.29623(3) 1.2825(2) 0.33786(5) 0.01813(19) Uani 1 1 d . . . C17 C 0.26501(3) 1.1342(2) 0.42068(5) 0.01871(19) Uani 1 1 d . . . H17 H 0.2452 1.1152 0.4496 0.022 Uiso 1 1 calc R . . C18 C 0.22537(4) 1.4905(2) 0.34797(6) 0.0235(2) Uani 1 1 d . . . H18A H 0.2033 1.4562 0.3744 0.035 Uiso 1 1 calc R . . H18B H 0.2143 1.4587 0.3017 0.035 Uiso 1 1 calc R . . H18C H 0.2348 1.6781 0.3539 0.035 Uiso 1 1 calc R . . C19 C 0.44591(3) -0.0152(2) 0.51140(5) 0.01673(18) Uani 1 1 d . . . H19 H 0.4613 -0.0562 0.4772 0.020 Uiso 1 1 calc R . . C20 C 0.41482(3) 0.1848(2) 0.50256(5) 0.01568(18) Uani 1 1 d . . . H20 H 0.4097 0.2821 0.4626 0.019 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 O1 0.0268(4) 0.0308(4) 0.0190(4) 0.0044(3) 0.0068(3) 0.0021(3) O2 0.0221(4) 0.0270(4) 0.0224(4) 0.0057(3) 0.0095(3) 0.0062(3) N1 0.0267(5) 0.0257(5) 0.0273(5) -0.0004(4) 0.0027(4) 0.0071(4) N2 0.0194(4) 0.0148(4) 0.0218(4) 0.0007(3) -0.0014(3) 0.0021(3) C1 0.0254(5) 0.0327(6) 0.0248(5) 0.0037(5) 0.0066(4) 0.0031(5) C2 0.0225(5) 0.0195(5) 0.0150(4) -0.0012(3) 0.0018(3) -0.0025(4) C3 0.0210(5) 0.0159(4) 0.0148(4) -0.0009(3) 0.0006(3) -0.0006(3) C4 0.0195(4) 0.0130(4) 0.0157(4) -0.0009(3) -0.0004(3) -0.0008(3) C5 0.0173(4) 0.0140(4) 0.0186(4) 0.0001(3) 0.0012(3) -0.0001(3) C6 0.0169(4) 0.0149(4) 0.0185(4) 0.0006(3) 0.0021(3) -0.0011(3) C7 0.0170(4) 0.0145(4) 0.0163(4) 0.0011(3) 0.0024(3) -0.0003(3) C8 0.0149(4) 0.0150(4) 0.0167(4) 0.0009(3) 0.0024(3) -0.0002(3) C9 0.0149(4) 0.0140(4) 0.0147(4) -0.0005(3) 0.0021(3) -0.0009(3) C10 0.0198(4) 0.0185(4) 0.0164(4) 0.0012(3) 0.0051(3) 0.0024(4) C11 0.0218(5) 0.0183(4) 0.0166(4) 0.0025(3) 0.0033(3) 0.0031(4) C12 0.0159(4) 0.0150(4) 0.0182(4) -0.0006(3) 0.0016(3) 0.0004(3) C13 0.0199(5) 0.0186(4) 0.0191(4) -0.0003(4) 0.0025(3) 0.0010(4) C14 0.0285(5) 0.0202(5) 0.0163(4) 0.0023(4) 0.0002(4) -0.0034(4) C15 0.0278(5) 0.0151(4) 0.0185(5) 0.0021(3) -0.0035(4) -0.0008(4) C16 0.0211(5) 0.0138(4) 0.0180(4) -0.0015(3) -0.0015(3) -0.0004(3) C17 0.0187(4) 0.0158(4) 0.0210(4) 0.0000(3) 0.0012(4) 0.0001(3) C18 0.0230(5) 0.0170(5) 0.0281(5) 0.0001(4) -0.0038(4) 0.0055(4) C19 0.0159(4) 0.0178(4) 0.0168(4) -0.0012(3) 0.0035(3) -0.0003(3) C20 0.0159(4) 0.0161(4) 0.0150(4) 0.0008(3) 0.0022(3) -0.0013(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 O1 C1 1.4265(15) . ? O1 C2 1.3726(13) . ? O2 C8 1.2330(12) . ? N1 C13 1.1504(14) . ? N2 C16 1.3879(14) . ? N2 C17 1.3533(13) . ? N2 C18 1.4552(13) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C1 H1C 0.9700 . ? C2 C3 1.3895(14) . ? C2 C14 1.4132(15) . ? C3 H3 0.9400 . ? C3 C4 1.4055(14) . ? C4 C5 1.4486(14) . ? C4 C16 1.4119(14) . ? C5 C6 1.4298(14) . ? C5 C17 1.3939(14) . ? C6 H6 0.9400 . ? C6 C7 1.3502(14) . ? C7 H7 0.9400 . ? C7 C8 1.4638(13) . ? C8 C9 1.5039(13) . ? C9 C10 1.4005(13) . ? C9 C20 1.3967(13) . ? C10 H10 0.9400 . ? C10 C11 1.3856(14) . ? C11 H11 0.9400 . ? C11 C12 1.3976(14) . ? C12 C13 1.4420(14) . ? C12 C19 1.3965(14) . ? C14 H14 0.9400 . ? C14 C15 1.3779(17) . ? C15 H15 0.9400 . ? C15 C16 1.3929(15) . ? C17 H17 0.9400 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C19 H19 0.9400 . ? C19 C20 1.3879(14) . ? C20 H20 0.9400 . ? 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 C2 O1 C1 116.93(9) . . ? C16 N2 C18 125.26(9) . . ? C17 N2 C16 108.45(9) . . ? C17 N2 C18 126.29(10) . . ? O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 123.89(10) . . ? O1 C2 C14 114.39(9) . . ? C3 C2 C14 121.71(10) . . ? C2 C3 H3 120.9 . . ? C2 C3 C4 118.24(9) . . ? C4 C3 H3 120.9 . . ? C3 C4 C5 134.51(9) . . ? C3 C4 C16 119.07(9) . . ? C16 C4 C5 106.42(9) . . ? C6 C5 C4 132.34(9) . . ? C17 C5 C4 105.67(9) . . ? C17 C5 C6 121.99(9) . . ? C5 C6 H6 115.3 . . ? C7 C6 C5 129.47(10) . . ? C7 C6 H6 115.3 . . ? C6 C7 H7 120.1 . . ? C6 C7 C8 119.74(9) . . ? C8 C7 H7 120.1 . . ? O2 C8 C7 121.84(9) . . ? O2 C8 C9 118.50(9) . . ? C7 C8 C9 119.66(8) . . ? C10 C9 C8 117.68(9) . . ? C20 C9 C8 123.10(9) . . ? C20 C9 C10 119.17(9) . . ? C9 C10 H10 119.6 . . ? C11 C10 C9 120.81(9) . . ? C11 C10 H10 119.6 . . ? C10 C11 H11 120.3 . . ? C10 C11 C12 119.31(9) . . ? C12 C11 H11 120.3 . . ? C11 C12 C13 119.50(9) . . ? C19 C12 C11 120.57(9) . . ? C19 C12 C13 119.92(9) . . ? N1 C13 C12 178.22(12) . . ? C2 C14 H14 119.7 . . ? C15 C14 C2 120.51(10) . . ? C15 C14 H14 119.7 . . ? C14 C15 H15 121.0 . . ? C14 C15 C16 117.99(10) . . ? C16 C15 H15 121.0 . . ? N2 C16 C4 108.52(9) . . ? N2 C16 C15 129.01(10) . . ? C15 C16 C4 122.47(10) . . ? N2 C17 C5 110.95(9) . . ? N2 C17 H17 124.5 . . ? C5 C17 H17 124.5 . . ? N2 C18 H18A 109.5 . . ? N2 C18 H18B 109.5 . . ? N2 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C12 C19 H19 120.2 . . ? C20 C19 C12 119.51(9) . . ? C20 C19 H19 120.2 . . ? C9 C20 H20 119.7 . . ? C19 C20 C9 120.61(9) . . ? C19 C20 H20 119.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C2 C3 C4 -179.61(9) . . . . ? O1 C2 C14 C15 179.43(9) . . . . ? O2 C8 C9 C10 -5.86(14) . . . . ? O2 C8 C9 C20 171.70(10) . . . . ? C1 O1 C2 C3 -1.33(15) . . . . ? C1 O1 C2 C14 179.20(10) . . . . ? C2 C3 C4 C5 -178.79(10) . . . . ? C2 C3 C4 C16 0.55(14) . . . . ? C2 C14 C15 C16 -0.11(16) . . . . ? C3 C2 C14 C15 -0.05(16) . . . . ? C3 C4 C5 C6 0.71(19) . . . . ? C3 C4 C5 C17 179.89(11) . . . . ? C3 C4 C16 N2 179.61(9) . . . . ? C3 C4 C16 C15 -0.74(15) . . . . ? C4 C5 C6 C7 -5.68(19) . . . . ? C4 C5 C17 N2 0.07(11) . . . . ? C5 C4 C16 N2 -0.88(11) . . . . ? C5 C4 C16 C15 178.77(9) . . . . ? C5 C6 C7 C8 176.72(10) . . . . ? C6 C5 C17 N2 179.36(9) . . . . ? C6 C7 C8 O2 -4.39(15) . . . . ? C6 C7 C8 C9 175.83(9) . . . . ? C7 C8 C9 C10 173.92(9) . . . . ? C7 C8 C9 C20 -8.52(14) . . . . ? C8 C9 C10 C11 177.82(9) . . . . ? C8 C9 C20 C19 -176.66(9) . . . . ? C9 C10 C11 C12 -0.53(16) . . . . ? C10 C9 C20 C19 0.86(14) . . . . ? C10 C11 C12 C13 178.61(10) . . . . ? C10 C11 C12 C19 -0.12(15) . . . . ? C11 C12 C13 N1 -87(4) . . . . ? C11 C12 C19 C20 1.13(15) . . . . ? C12 C19 C20 C9 -1.50(15) . . . . ? C13 C12 C19 C20 -177.60(9) . . . . ? C14 C2 C3 C4 -0.17(15) . . . . ? C14 C15 C16 N2 -179.92(10) . . . . ? C14 C15 C16 C4 0.51(15) . . . . ? C16 N2 C17 C5 -0.63(12) . . . . ? C16 C4 C5 C6 -178.68(10) . . . . ? C16 C4 C5 C17 0.49(11) . . . . ? C17 N2 C16 C4 0.94(11) . . . . ? C17 N2 C16 C15 -178.67(10) . . . . ? C17 C5 C6 C7 175.25(10) . . . . ? C18 N2 C16 C4 -178.63(9) . . . . ? C18 N2 C16 C15 1.75(17) . . . . ? C18 N2 C17 C5 178.94(9) . . . . ? C19 C12 C13 N1 91(4) . . . . ? C20 C9 C10 C11 0.17(15) . . . . ? loop_ _diffrn_refln_index_h _diffrn_refln_index_k _diffrn_refln_index_l _diffrn_refln_intensity_net _diffrn_refln_intensity_u 4 0 0 801.22 31.2 -6 0 0 7.2 1.2 6 0 0 8 0.7 8 0 0 349.67 15.9 -8 0 0 359.76 15.8 -8 0 0 403.16 15 -10 0 0 12.4 1.1 -10 0 0 12.7 1.7 10 0 0 12.1 1.1 10 0 0 14.3 2.2 -12 0 0 325.47 12.8 12 0 0 298.37 14.7 -12 0 0 336.37 14.7 12 0 0 308.27 13.1 -14 0 0 54.39 3.2 14 0 0 45 2.9 -14 0 0 49.3 4 -14 0 0 49.1 2.7 14 0 0 53.39 4.4 16 0 0 7.2 1.3 16 0 0 5.4 1 16 0 0 5.7 1.8 -16 0 0 4 1.2 -16 0 0 4.2 0.9 18 0 0 12.8 1.4 -18 0 0 18.2 3.2 -18 0 0 15.4 1.4 18 0 0 9.2 2.2 -18 0 0 19.7 2 18 0 0 14 1.7 -20 0 0 346.17 17.5 20 0 0 346.27 15.3 -20 0 0 376.06 15.7 -20 0 0 371.66 14.8 20 0 0 317.87 15.5 20 0 0 377.86 18.4 -22 0 0 44.6 4.6 22 0 0 46.5 3.3 -22 0 0 45.7 2.9 22 0 0 47.5 3.6 22 0 0 44.1 5 -24 0 0 231.68 11.3 -24 0 0 230.88 13.8 24 0 0 289.27 12.6 -24 0 0 267.07 12.6 24 0 0 250.37 14.8 24 0 0 237.18 11.6 -26 0 0 9 1.9 26 0 0 9.8 2 26 0 0 5.1 2 28 0 0 192.28 10.4 28 0 0 182.38 12.8 -28 0 0 189.98 10.3 -30 0 0 11.9 2.2 30 0 0 22.8 5.1 30 0 0 20.6 2.7 32 0 0 109.69 7.4 -32 0 0 114.99 7.5 32 0 0 112.69 10.1 34 0 0 2 2 -34 0 0 4.6 1.5 34 0 0 1.3 0.8 -34 0 0 2 1.2 -36 0 0 46.8 4.6 -36 0 0 47 4.8 36 0 0 41.8 7.6 -38 0 0 13.9 3.2 -38 0 0 13.7 2.7 38 0 0 16 5.1 38 0 0 14.5 3.1 40 0 0 4.5 1.6 -40 0 0 7.8 2.5 -40 0 0 4.7 1.6 40 0 0 12.9 4.2 42 0 0 5.1 2 42 0 0 6 2.8 -42 0 0 6.5 2.4 44 0 0 1.9 1.3 44 0 0 1.1 2.8 -44 0 0 2.4 1.6 46 0 0 12.8 4.7 46 0 0 18.4 3.3 -1 -1 0 1216.68 46.9 1 -1 0 1309.57 47.3 1 1 0 1031.4 46.6 -1 1 0 1187.58 46.7 -1 1 0 1148.79 46.9 1 1 0 1360.66 46.7 3 -1 0 4.6 0.9 3 -1 0 2.3 0.4 -3 -1 0 3.8 0.7 3 -1 0 3.5 0.7 3 -1 0 3.6 0.9 -3 -1 0 3.7 0.7 -3 1 0 4 0.7 3 1 0 3.2 0.6 3 1 0 2 0.4 -3 1 0 3.1 0.6 5 -1 0 1857.51 74.79 -5 -1 0 1944.51 74.29 5 1 0 2034.9 74.49 5 1 0 1997.6 74.59 -5 1 0 1896.51 74.79 -5 1 0 1915.41 74.69 -5 1 0 1963.2 74.99 -7 -1 0 5892.81 277.07 -7 1 0 5845.32 287.17 7 1 0 5986.3 278.47 -9 -1 0 35.1 1.9 9 -1 0 39.6 2.3 9 -1 0 32.3 3 9 -1 0 37.5 2.9 9 -1 0 35.3 2.5 9 1 0 36.8 2.9 -9 1 0 37 2.5 -9 1 0 40.4 3.3 -11 -1 0 230.38 8.9 11 -1 0 221.18 9.5 11 -1 0 222.98 11 11 -1 0 215.88 9.7 -11 -1 0 213.88 10.3 11 -1 0 222.18 10.5 11 1 0 220.28 9.5 11 1 0 216.88 10.7 -11 1 0 220.38 10.8 -11 1 0 208.68 9.5 -13 -1 0 390.06 17.1 13 -1 0 365.86 15.9 13 -1 0 368.56 17.6 13 -1 0 361.76 16.8 -13 1 0 406.66 17.6 13 1 0 384.26 15.9 13 1 0 370.86 17.4 -13 1 0 412.06 16.2 -13 1 0 389.56 16.2 15 -1 0 27 2.7 15 -1 0 27.2 3.2 15 -1 0 27.6 2.2 -15 -1 0 20.2 2.5 15 1 0 29 3.2 -15 1 0 26 2.2 -15 1 0 30 2.4 -15 1 0 25.8 3 15 1 0 27.6 2.1 17 -1 0 212.98 10.6 17 -1 0 206.08 9.5 -17 -1 0 211.48 11 17 -1 0 218.58 11.8 -17 1 0 205.18 9.5 17 1 0 198.48 9.3 -17 1 0 200.18 11.2 17 1 0 209.18 11.5 -17 1 0 190.88 9.5 19 -1 0 68.59 4.9 19 -1 0 59.09 3.9 -19 -1 0 71.79 5.3 19 1 0 60.59 5.5 19 1 0 60.69 3.9 -19 1 0 56.19 5.1 -19 1 0 62.09 4 -19 1 0 62.79 4 -21 -1 0 181.88 10.5 21 -1 0 165.68 8.7 21 -1 0 161.98 9.6 21 -1 0 188.98 11.5 21 1 0 177.08 8.7 21 1 0 179.68 11.1 -21 1 0 195.78 9.4 -21 1 0 186.38 8.9 -23 -1 0 144.09 9.3 23 -1 0 140.09 7.6 -23 -1 0 145.29 6.6 23 -1 0 151.58 8.8 23 -1 0 144.49 10.2 -23 1 0 141.09 9.9 23 1 0 141.69 7.5 -23 1 0 147.99 7.7 23 1 0 136.59 9.9 -23 1 0 169.08 8.3 -25 -1 0 117.19 6.7 25 -1 0 145.69 8.9 -25 -1 0 150.68 6.5 25 -1 0 144.89 10.4 -25 1 0 149.49 8.1 25 1 0 142.29 10.3 -25 1 0 140.39 7.6 -25 1 0 140.39 9.8 27 -1 0 1.4 0.9 -27 -1 0 1.5 0.7 27 1 0 -0.7 1.3 27 1 0 2.9 1 -27 1 0 0.1 0.4 -27 1 0 1.3 0.7 -29 -1 0 25.9 2.4 29 -1 0 29.9 5.4 29 -1 0 24.5 3.3 -29 -1 0 28.7 2.1 -29 1 0 26.6 2.7 29 1 0 26.9 2.6 -29 1 0 30.7 3.2 29 1 0 30.6 5.6 31 -1 0 85.09 8.4 -31 -1 0 70.49 4.3 -31 -1 0 82.59 4.9 31 -1 0 83.69 6.8 31 1 0 90.29 5.6 -31 1 0 81.89 6 31 1 0 83.09 8.3 -31 1 0 86.09 5.4 33 -1 0 -0.4 1 33 -1 0 1 1.8 -33 1 0 1.7 0.9 33 1 0 0.2 0.7 -33 1 0 0.4 0.8 33 1 0 0.6 1.4 35 -1 0 14.8 3.2 35 -1 0 14.1 4.7 35 1 0 17.3 1.9 -35 1 0 13.6 2.3 -35 1 0 13 2.7 35 1 0 17.1 4.9 37 -1 0 0.3 0.7 37 -1 0 0.8 1.8 37 1 0 1.4 0.9 -37 1 0 1.9 1.3 37 1 0 0.4 1.5 -37 1 0 -0.7 0.6 39 -1 0 45.6 5 39 -1 0 35.6 6.7 -39 1 0 40.6 5.1 39 1 0 43.2 4 39 1 0 30.8 8 41 -1 0 -0.6 1.7 41 -1 0 1.5 1.5 41 1 0 0 0.9 -41 1 0 -0.7 0.9 -41 1 0 -2.7 1.1 41 1 0 0.7 1.7 43 -1 0 9.8 3.3 43 -1 0 8.1 2.6 -43 1 0 4.9 1.7 43 1 0 5.4 2.9 -43 1 0 9.9 3.2 43 1 0 8.8 2.2 45 -1 0 39.4 7.8 45 -1 0 40.2 5.4 -45 1 0 40.8 5.4 -45 1 0 42.1 5.1 45 1 0 35.7 7.5 45 1 0 35.1 4.1 0 -2 0 922.11 37.9 0 -2 0 992.8 37.5 0 2 0 898.01 37.3 0 2 0 933.71 37.8 2 -2 0 12 1.6 -2 -2 0 14 1.8 2 -2 0 14.8 2.4 -2 -2 0 14 1.6 -2 2 0 12.4 1.3 2 2 0 14.2 2.1 2 2 0 13.7 1.5 -2 2 0 14.6 2.2 -4 -2 0 0.1 0.4 4 -2 0 0.5 0.4 -4 -2 0 0.2 0.5 4 -2 0 0.8 0.6 -4 2 0 0.2 0.3 -4 2 0 0.2 0.4 -4 2 0 0.5 0.4 -4 2 0 0.2 0.3 4 2 0 0.6 0.5 4 2 0 0.6 0.3 6 -2 0 807.62 33.6 -6 -2 0 829.82 32.2 -6 -2 0 772.62 32.5 6 -2 0 775.12 31.9 6 -2 0 766.12 32.1 6 -2 0 804.62 32.7 6 2 0 844.62 32.5 -6 2 0 745.13 32.9 -6 2 0 818.92 31.9 6 2 0 845.42 32 -6 2 0 830.82 32.2 8 -2 0 138.59 7.1 8 -2 0 130.69 7.1 8 -2 0 134.19 6.6 -8 -2 0 127.19 6.5 8 -2 0 141.69 8 -8 2 0 134.39 7.2 8 2 0 139.59 6.9 -8 2 0 133.19 6.4 -8 2 0 129.39 7.4 8 2 0 125.39 6.5 -8 2 0 136.99 7.1 10 -2 0 199.38 10.5 10 -2 0 228.28 11.8 10 -2 0 214.08 10.1 -10 -2 0 229.18 10 -10 -2 0 223.08 9.9 10 2 0 226.18 10.6 10 2 0 237.68 10.4 10 2 0 234.38 9.6 -10 2 0 216.98 11.1 -10 2 0 211.28 10.7 -10 2 0 223.48 10 12 -2 0 0.7 0.7 -12 -2 0 1.4 0.6 -12 -2 0 0.6 0.4 12 -2 0 0.8 0.6 12 -2 0 -0.4 0.5 12 -2 0 0.1 0.5 -12 2 0 0.8 0.4 -12 2 0 0.2 0.5 12 2 0 -0.2 0.4 12 2 0 1.3 0.8 -12 2 0 -0.9 0.5 -12 2 0 0.3 0.5 14 -2 0 238.98 11.7 14 -2 0 260.27 13.3 14 -2 0 246.68 11.3 14 -2 0 258.77 12.9 -14 -2 0 244.38 10.7 -14 -2 0 241.78 11.6 -14 2 0 224.98 12 -14 2 0 241.38 11.1 -14 2 0 247.38 12.5 14 2 0 266.27 11.3 14 2 0 249.08 11.2 14 2 0 244.58 12.3 -14 2 0 241.48 11.9 -16 -2 0 7 1.6 16 -2 0 5.7 1.2 16 -2 0 3.9 1.3 16 -2 0 12.1 2.8 -16 -2 0 8 1.2 -16 2 0 6.5 1.8 -16 2 0 5.9 1.5 16 2 0 8.7 2 -16 2 0 7.6 1.4 16 2 0 9.8 1.6 16 2 0 6.7 1.2 18 -2 0 57.99 5.2 -18 -2 0 46.8 2.8 18 -2 0 39.2 3.5 -18 -2 0 45.1 3.9 18 -2 0 43.4 4.4 -18 2 0 42.5 3.3 -18 2 0 43.2 4.3 -18 2 0 42 3.6 18 2 0 42.8 3.2 18 2 0 41.9 4.3 18 2 0 46.2 3.3 -20 -2 0 0.3 0.7 20 -2 0 0 0.4 20 -2 0 0.2 0.5 20 -2 0 -0.1 0.8 -20 2 0 -0.4 0.5 20 2 0 0.1 0.5 -20 2 0 0.6 0.9 -20 2 0 0.5 0.4 20 2 0 -0.3 0.7 22 -2 0 5.2 1.8 -22 -2 0 4.3 1.6 22 -2 0 6.4 2.3 22 2 0 6.6 1.4 -22 2 0 12.8 2.1 -22 2 0 3.8 1.4 22 2 0 6.9 2.4 -22 2 0 9.2 2.2 24 -2 0 99.19 7.5 24 -2 0 93.99 8 24 2 0 91.89 7.7 -24 2 0 82.69 5.6 -24 2 0 92.49 7.5 -24 2 0 90.99 6.1 26 -2 0 62.59 6.8 26 -2 0 71.89 6.4 -26 2 0 71.29 5 26 2 0 67.19 6.8 -26 2 0 63.89 6.2 -26 2 0 61.89 4.9 28 -2 0 9.5 2.9 28 -2 0 16 3.8 28 2 0 9.5 2.9 -28 2 0 12.2 2.3 -28 2 0 8.8 1.8 30 -2 0 18.6 3.9 30 -2 0 22.3 5.3 30 2 0 21.4 4.4 -30 2 0 25.4 3 32 -2 0 3.3 1.8 32 -2 0 4.1 1.9 -32 2 0 3.6 1.3 32 2 0 2.4 0.8 32 2 0 1.7 1.3 34 -2 0 17.1 4.1 34 -2 0 14.2 4.2 -34 2 0 10.3 2.3 34 2 0 15 1.9 34 2 0 18.1 4.9 36 -2 0 61.59 6.8 36 -2 0 55.19 7.4 -36 2 0 55.29 5.2 36 2 0 61.19 4.2 36 2 0 66.79 7.8 38 -2 0 163.28 13.9 38 -2 0 166.18 12.2 -38 2 0 162.98 10.5 38 2 0 162.78 8.4 38 2 0 171.08 13.8 40 -2 0 30.3 7.2 40 -2 0 27.9 5.3 -40 2 0 26.9 4.2 40 2 0 28.1 5.8 40 2 0 27.9 2.6 42 -2 0 12.5 3.5 42 2 0 13 4.3 -42 2 0 10.2 2.4 -42 2 0 15 4.5 44 -2 0 17.5 4 44 -2 0 9.1 2.8 44 2 0 12.3 4.1 -44 2 0 10.4 2.6 -44 2 0 11.8 3.9 1 -3 0 101.29 7.1 -1 -3 0 108.19 7.2 1 -3 0 106.29 6.7 -1 -3 0 109.79 6.7 -1 3 0 115.49 7.1 -1 3 0 126.19 6.9 1 3 0 108.09 6.9 -1 3 0 112.49 6.1 1 3 0 116.79 6.6 1 3 0 112.19 6.1 3 -3 0 22.6 3 -3 -3 0 24.8 2.6 3 -3 0 21.3 2.5 -3 -3 0 27.7 3 -3 3 0 25.6 2.3 -3 3 0 22.3 2.5 3 3 0 23.5 2.4 -3 3 0 22.1 2.7 3 3 0 24.8 2.8 -5 -3 0 298.97 13.1 5 -3 0 257.57 14.1 5 -3 0 253.77 13 -5 -3 0 281.37 13.6 -5 3 0 254.07 13 -5 3 0 278.97 11.8 -5 3 0 271.97 13.6 5 3 0 259.57 12.5 5 3 0 279.17 13.3 -5 3 0 255.77 12.1 7 -3 0 3.2 1.6 -7 -3 0 4 1.3 -7 -3 0 2 1 7 -3 0 2.8 1 -7 3 0 4.1 1.1 -7 3 0 3.1 0.9 7 3 0 2.6 0.9 -7 3 0 2.2 0.9 -7 3 0 2.8 1.2 7 3 0 2.7 1 9 -3 0 4.2 1.1 9 -3 0 5.5 1.3 9 -3 0 3.6 1.3 -9 -3 0 4.2 1.2 9 -3 0 3.6 1.6 9 3 0 3.8 1.1 -9 3 0 5.5 1.3 -9 3 0 3.7 1.2 -9 3 0 5.7 2.9 -9 3 0 5.2 1.9 9 3 0 4.8 1.3 11 -3 0 214.08 11.5 11 -3 0 216.58 11.1 11 -3 0 217.08 10.7 -11 -3 0 217.88 10.8 11 -3 0 258.97 14.4 -11 3 0 221.08 10.5 -11 3 0 217.98 11.6 -11 3 0 205.48 11.8 11 3 0 228.08 10.6 11 3 0 231.58 10.4 -11 3 0 219.38 11.2 11 3 0 239.58 11.3 13 -3 0 28.9 3.1 -13 -3 0 23.6 2.4 13 -3 0 31.2 5 -13 3 0 21.6 2.7 13 3 0 25.9 2.1 13 3 0 25.1 2.6 -13 3 0 25.4 3 13 3 0 21.9 2.6 -13 3 0 30.3 3.1 -13 3 0 26.8 2.4 15 -3 0 66.19 4.6 -15 -3 0 68.59 4.4 15 -3 0 72.39 8 15 -3 0 67.39 5.3 15 -3 0 64.29 5.1 -15 3 0 62.89 5.7 15 3 0 66.69 4.9 15 3 0 68.49 4.7 -15 3 0 60.89 5.1 -15 3 0 64.19 5.1 -15 3 0 62.59 4.3 17 -3 0 3.9 1.5 17 -3 0 4.5 2.3 17 -3 0 3.7 1.2 -17 -3 0 3.9 1.1 17 -3 0 5 2 -17 -3 0 6.2 1.3 -17 3 0 5 1.6 17 3 0 4.8 1.2 17 3 0 4.8 1.2 -17 3 0 9.7 2.7 -17 3 0 4.9 1.3 17 3 0 6.2 1.8 19 -3 0 62.49 6.4 19 -3 0 70.19 6.1 -19 -3 0 72.19 4.3 -19 -3 0 62.79 4.5 -19 3 0 65.49 5.7 19 3 0 67.19 4.6 -19 3 0 66.89 4.6 21 -3 0 10.2 2.9 21 -3 0 11.4 2.8 -21 -3 0 13.4 1.7 -21 -3 0 7.7 1.9 -21 3 0 11.2 2 21 3 0 16.4 3.2 21 3 0 10 1.8 -21 3 0 9.5 2.4 23 -3 0 117.79 9.1 23 -3 0 111.89 9.1 -23 3 0 117.09 8.6 23 3 0 116.69 8.6 23 3 0 113.09 6.5 -23 3 0 122.69 7.1 25 -3 0 0.7 1.2 25 -3 0 0.4 1.1 -25 3 0 3 1.3 25 3 0 -0.7 0.6 25 3 0 0.3 0.8 -25 3 0 0.2 0.5 27 -3 0 -0.3 1.5 27 -3 0 0.8 1.3 -27 3 0 0.8 0.6 27 3 0 -1.4 1.1 27 3 0 1.4 0.7 29 -3 0 -0.2 0.8 29 -3 0 -0.7 0.8 29 3 0 -0.8 1.1 -29 3 0 0.3 0.8 29 3 0 1.2 0.7 31 -3 0 0.2 1.1 31 -3 0 1.9 1.9 -31 3 0 1.1 0.9 31 3 0 -0.8 0.9 31 3 0 0.5 0.9 33 -3 0 0.6 1.2 33 -3 0 -1.6 1.3 -33 3 0 0.1 0.8 33 3 0 -0.6 1.2 35 -3 0 36.4 6.4 35 -3 0 21.5 5.2 -35 3 0 33 5.2 37 -3 0 0 1.2 37 -3 0 -2.6 1.7 37 3 0 1.4 1.7 -37 3 0 -0.5 0.9 39 -3 0 7 3.2 39 -3 0 6.3 3.4 39 3 0 4.5 2.7 -39 3 0 5.6 1.9 41 -3 0 -3.6 2.4 41 -3 0 -2.4 1 -41 3 0 1.2 1.1 41 3 0 0.2 1.8 0 -4 0 20.9 3.9 0 4 0 20.9 3.5 0 4 0 12.9 2.1 -2 -4 0 52.89 5.1 2 -4 0 49.8 5.2 2 -4 0 47.6 4.5 -2 -4 0 55.09 4.8 2 4 0 41.5 3.9 2 4 0 52.49 4.8 -2 4 0 50.59 3.9 -2 4 0 53.89 5 2 4 0 50.09 4 -4 -4 0 57.29 5.2 4 -4 0 53.49 4.7 4 -4 0 59.29 7.1 -4 -4 0 47.5 4.3 4 4 0 49.5 4.6 -4 4 0 48.6 3.8 4 4 0 39 3.9 6 -4 0 36.5 4.5 -6 -4 0 46.3 4.7 6 -4 0 36.6 4 -6 -4 0 48.8 4.2 6 4 0 42 3.8 6 4 0 49.4 6.2 -6 4 0 41.6 3.5 8 -4 0 5 1.5 -8 -4 0 6.6 1.9 -8 -4 0 3.5 1.5 8 -4 0 3.2 1.7 8 4 0 9.4 2.1 -8 4 0 6 1.3 -8 4 0 8.9 1.8 8 4 0 5.2 1.4 10 -4 0 48.8 4.7 -10 -4 0 43 4 10 -4 0 38.3 5 -10 4 0 45.2 4 10 4 0 50.49 3.9 10 4 0 46.4 3.5 -10 4 0 48.3 3.7 10 4 0 48 4.3 12 -4 0 119.89 8.5 -12 -4 0 126.89 7.8 12 -4 0 139.59 10.4 -12 4 0 141.39 7.6 -12 4 0 140.09 7.8 12 4 0 136.29 8.3 12 4 0 131.39 7.4 12 4 0 127.09 6.6 -14 -4 0 1 0.8 14 -4 0 2.9 1.6 14 -4 0 0.9 0.9 14 -4 0 0.1 0.6 14 4 0 1.2 0.8 14 4 0 1.8 0.5 -14 4 0 0.9 0.7 -14 4 0 0.4 0.7 16 -4 0 10.8 2.3 16 -4 0 12.4 3 -16 -4 0 13.2 2.3 16 -4 0 8.3 2.8 -16 4 0 13.5 2.3 16 4 0 14.2 2.5 -16 4 0 13.2 2.7 16 4 0 13.1 2.4 18 -4 0 -0.4 0.8 -18 -4 0 0.2 0.7 18 -4 0 -0.1 0.9 -18 4 0 0.8 0.8 -18 4 0 0.6 1 18 4 0 -0.9 1 18 4 0 0 0.7 -20 -4 0 0.7 0.7 20 -4 0 0.7 1.3 20 -4 0 1.7 1.1 -20 4 0 0.8 0.8 20 4 0 3.1 1.2 -20 4 0 2.3 1.4 20 4 0 -0.1 0.8 22 -4 0 3.3 2 22 -4 0 4.5 2.3 -22 -4 0 2.2 1.1 22 4 0 1.9 1.3 -22 4 0 3.8 1.3 -22 4 0 5.1 1.9 22 4 0 2.8 1.2 -24 -4 0 2.9 1 24 -4 0 1.5 1.3 24 -4 0 1 1.6 24 4 0 5.4 2 -24 4 0 3.9 1.6 -24 4 0 3.4 1.3 24 4 0 3 1.1 26 -4 0 3.9 2.1 26 -4 0 4.2 2.1 26 4 0 7.2 1.6 26 4 0 7.4 2.6 -26 4 0 8.5 1.9 -26 4 0 3.7 2.1 28 -4 0 2.7 1.9 28 -4 0 4.2 1.9 28 4 0 4.1 0.8 28 4 0 1.6 1.2 -28 4 0 0.4 0.8 30 -4 0 0.9 1.3 30 -4 0 3.8 2 30 4 0 -0.3 1.3 -30 4 0 1.2 0.8 32 -4 0 58.49 7.5 -32 4 0 66.99 6.1 32 4 0 48.9 8.1 34 -4 0 -0.5 1.5 34 -4 0 1 2.4 34 4 0 -2 1.1 -34 4 0 -1.3 0.9 36 -4 0 250.67 17.9 36 -4 0 236.68 17 -36 4 0 259.57 14.3 36 4 0 279.07 17.3 38 -4 0 0 1.2 38 -4 0 -1.6 2.5 38 4 0 3.4 2.1 -38 4 0 -0.3 0.9 1 -5 0 1.7 1 1 -5 0 0.9 1.1 -1 -5 0 0.2 0.8 -1 -5 0 0.5 1.3 -1 5 0 -0.7 0.7 3 -5 0 73.89 6.3 3 -5 0 67.59 6.8 -3 -5 0 56.59 6.1 -3 -5 0 65.19 5.8 -3 5 0 65.59 5 3 5 0 68.49 5.2 5 -5 0 16.6 3.2 5 -5 0 15.7 3.9 -5 -5 0 14 2.8 -5 -5 0 13.6 3.2 -5 5 0 20.3 3.1 5 5 0 17 2.9 -7 -5 0 14.7 3.3 7 -5 0 13.5 3.1 7 -5 0 15.3 3.9 -7 -5 0 18.3 3.7 7 5 0 14 2.7 -7 5 0 13.5 2.6 7 5 0 19.9 3.2 9 -5 0 13 3.1 -9 -5 0 17.3 3.4 9 -5 0 16.1 3.8 9 5 0 22.9 2.7 -9 5 0 19 3 11 -5 0 39.1 5.8 11 -5 0 24.3 5.1 -11 -5 0 29.7 3.6 11 5 0 30.1 2.6 -11 5 0 27.3 3 11 5 0 29.3 2.9 -13 -5 0 22.1 2.9 13 -5 0 22.4 4.4 13 -5 0 19.4 4.2 -13 5 0 21.1 2.6 -13 5 0 22.3 2.7 13 5 0 24.8 2.3 15 -5 0 51.59 5.4 -15 -5 0 56.89 5.1 15 -5 0 61.89 7.1 -15 5 0 52.89 4.5 -17 -5 0 38.1 4 17 -5 0 36.1 6.3 -17 5 0 36.4 3.6 17 5 0 32.5 3.7 -17 5 0 35.5 4 19 -5 0 0.9 1.1 -19 -5 0 -1.3 0.7 19 5 0 1.4 1.2 -19 5 0 -0.9 0.9 -21 -5 0 50.09 4.3 21 -5 0 48.6 7.9 -21 5 0 40.9 4 -21 5 0 46.3 4.9 21 5 0 44.1 4.2 23 -5 0 8.2 4.3 -23 -5 0 9.8 2.2 -23 5 0 9.1 2.8 -23 5 0 7.1 2 -25 -5 0 1.5 0.9 25 -5 0 1.3 1.7 25 -5 0 -1.2 1.4 25 5 0 3.2 1.5 -25 5 0 0.6 0.9 27 -5 0 54.49 7.4 -27 5 0 60.19 5.7 27 5 0 61.39 5.6 29 -5 0 176.48 14.6 29 5 0 193.58 14.2 -29 5 0 192.28 11.1 31 -5 0 -2.1 1 31 -5 0 3.7 2.2 -31 5 0 2.4 1.3 31 5 0 1 1.5 33 -5 0 7.2 3.1 33 -5 0 8.9 3.6 33 5 0 10.3 3.3 -33 5 0 8.5 2 0 -6 0 25 4.4 0 -6 0 26.6 5.2 0 6 0 26.1 3.3 -2 -6 0 -0.4 1.3 2 -6 0 0.9 1.2 -2 -6 0 1.7 1.3 2 -6 0 1.2 1.6 2 6 0 0.3 0.9 2 6 0 1.2 1.2 -2 6 0 2 1.2 -4 -6 0 73.29 6.7 -4 -6 0 69.59 7.3 4 -6 0 67.99 7.8 4 -6 0 60.49 6.4 -4 6 0 70.59 5.7 4 6 0 69.89 5.7 4 6 0 74.99 6.5 -6 -6 0 3 1.6 6 -6 0 0.2 1.1 -6 -6 0 0.5 1.5 6 -6 0 1.2 1.2 6 6 0 1 1.4 -6 6 0 1 0.9 6 6 0 -0.6 0.6 -8 -6 0 37.9 4.8 8 -6 0 63.29 6.4 8 -6 0 50.59 6.5 8 6 0 55.89 5.1 -8 6 0 39.9 4.1 8 6 0 51.69 4.8 10 -6 0 54.29 7 10 -6 0 50.09 8.4 -10 -6 0 44.9 5.1 10 6 0 54.29 4.5 10 6 0 52.19 5 10 6 0 48.6 3.7 -10 6 0 49 4.6 -12 -6 0 7.7 2.5 12 -6 0 10.4 5.1 12 6 0 8 1.5 -12 6 0 8.1 2 12 6 0 11.2 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2.4 18 2 -27 12.3 3.2 18 2 -27 5.6 2.3 -18 2 27 6.4 3.1 -16 -2 27 2.2 1.8 -16 -2 27 -2 0.8 -16 2 27 0.3 1.1 16 2 -27 0.1 1.2 -14 -2 27 35.7 4.5 -14 -2 27 34.6 4.7 -14 2 27 32.3 6.3 14 2 -27 29.4 4.5 -12 -2 27 25.1 4.9 -12 -2 27 23.2 4 12 2 -27 25.7 4.2 -12 2 27 29.7 6 -10 -2 27 -1.8 1 -10 -2 27 -0.6 1 -10 2 27 -0.9 1.2 10 2 -27 -0.1 1.2 -8 -2 27 9.7 2.8 -8 -2 27 7.9 2.9 -8 2 27 6.8 2.2 8 2 -27 9.1 2.5 -6 -2 27 9.3 3.1 -6 -2 27 9.4 2.8 6 2 -27 11 2.5 -6 2 27 6.9 2.5 -4 -2 27 24.7 5 -4 -2 27 28.3 5.5 -4 -2 27 25.5 4.9 -4 2 27 25.5 4.8 4 2 -27 25.6 4 -2 -2 27 22.9 4.9 -2 -2 27 15.2 3.3 -2 -2 27 17 4.3 -2 2 27 17.1 3.4 2 2 -27 17.5 3.3 0 -2 27 14.1 3.7 0 -2 27 16.2 3.7 0 2 -27 19.3 3.3 0 2 27 22.4 4.7 0 2 27 23.7 4.8 2 -2 27 7.3 2.5 2 -2 27 8 2.3 2 2 27 6.2 2.3 2 2 27 6.5 2.7 -2 2 -27 7.1 2.1 4 -2 27 3.1 2 4 -2 27 0.4 1.2 4 2 27 -0.3 0.9 4 2 27 -2.3 1.6 6 -2 27 1.4 2.2 6 -2 27 -1.6 0.9 6 2 27 -2.3 1.1 6 2 27 -1.1 1.4 8 -2 27 50.89 5.7 8 -2 27 37.2 6.5 -8 2 -27 50.79 4.6 8 2 27 49.5 6.7 8 2 27 48.8 5.5 -13 -3 27 32.6 5 -13 -3 27 29.7 5.3 13 3 -27 33.3 5.2 -13 3 27 33.5 6.9 -11 -3 27 -0.7 1.5 -11 -3 27 -0.2 1.7 -11 3 27 2.2 2.6 11 3 -27 0.8 1.3 -9 -3 27 -1.2 1.1 9 3 -27 0.8 1.3 -9 3 27 3.9 2.4 -7 3 27 7.5 2.8 7 3 -27 10 2.6 -5 -3 27 56.69 6.4 -5 3 27 51.69 6.3 5 3 -27 49.3 5 -3 -3 27 0.9 2.1 -3 -3 27 4.5 1.9 3 3 -27 7.6 2.2 -3 3 27 3.9 2.3 -1 -3 27 1.4 2 -1 -3 27 2.3 2 -1 3 27 0.2 1.6 1 3 -27 2.4 1.4 -1 3 27 1.8 1.7 1 -3 27 10.4 2.6 1 3 27 8.2 2.6 -24 0 28 0.7 2.1 24 0 -28 3.5 2.1 22 0 -28 13.2 2.6 -22 0 28 21.5 4.4 22 0 -28 14.3 3.4 20 0 -28 3.3 1.9 20 0 -28 1.5 1.1 -20 0 28 12 3.5 18 0 -28 105.49 9 -18 0 28 98.79 8.6 18 0 -28 104.89 6.5 16 0 -28 4.4 1.4 -16 0 28 5.3 2.3 -14 0 28 3.9 1.4 14 0 -28 4.2 1.3 -12 0 28 40.4 5 12 0 -28 28.5 2.8 -10 0 28 6.4 2.5 -8 0 28 1 1 8 0 -28 -0.8 0.7 -6 0 28 18 3.7 4 0 -28 -0.7 0.7 -4 0 28 -1.2 1.1 0 0 28 85.69 8.6 0 0 28 96.89 8.4 2 0 28 88.79 8.1 2 0 28 94.69 9.1 4 0 28 31.1 3.8 4 0 28 24.6 4.3 4 0 28 22 4.8 6 0 28 2.3 2.4 6 0 28 -0.3 1 -6 0 -28 -0.7 0.7 6 0 28 1.6 1.7 8 0 28 1 2 8 0 28 -0.1 1 8 0 28 -0.5 1.4 -8 0 -28 -0.6 0.7 10 0 28 1.7 1.7 10 0 28 0 1.5 10 0 28 -0.3 1.2 -10 0 -28 -1.9 0.7 23 -1 -28 1.5 1.6 23 1 -28 1.1 1.7 -21 -1 28 -0.3 1.6 21 -1 -28 -1.7 1.1 21 1 -28 2.3 1.4 21 1 -28 1.3 1.6 -21 1 28 5.5 2.2 19 -1 -28 -2.6 1.4 19 -1 -28 -0.5 0.9 -19 -1 28 1.6 1.1 19 1 -28 0 1.2 -19 1 28 -1 1 19 1 -28 1.8 1.9 -17 -1 28 1.6 1.4 -17 1 28 3.7 2.1 17 1 -28 0.8 1 -15 -1 28 2.2 1.3 -15 1 28 2.5 2.1 15 1 -28 2.3 1.3 -13 -1 28 4.5 2.4 13 1 -28 3.7 1.9 -13 1 28 5.9 2.4 -11 -1 28 2.4 1.5 -11 1 28 1.8 1.5 11 1 -28 0 1 -9 -1 28 57.39 6.2 -9 1 28 71.79 6.9 9 1 -28 55.49 4.6 -7 -1 28 27.8 5 7 1 -28 28.5 3.2 -7 1 28 29.2 5.3 -5 -1 28 1 1.1 -5 1 28 3.1 1.5 5 1 -28 4.4 1.2 -3 -1 28 20.8 4.5 -3 -1 28 32.2 4.1 -3 -1 28 21.1 4.7 3 1 -28 31.1 3.2 -3 1 28 24.2 4.6 -1 -1 28 3.4 1.9 -1 -1 28 -0.7 1 -1 -1 28 1.1 1.1 -1 1 28 0.6 1.2 1 1 -28 2.1 1.1 -1 1 28 1.8 1.5 1 -1 28 2.8 1.6 1 -1 28 1.2 1.8 1 -1 28 -0.8 1 1 1 28 1.9 1.6 1 1 28 2.7 1.8 -1 1 -28 2.9 1.2 3 -1 28 4.9 2.6 3 -1 28 3 2.2 3 -1 28 3.2 1.7 3 1 28 6.5 2.8 3 1 28 2 1.4 -3 1 -28 4.4 1.6 5 -1 28 38 4.9 5 -1 28 38.1 7 5 -1 28 38.5 6.6 5 1 28 40.6 5.2 5 1 28 45.1 6.1 -5 1 -28 40.6 3.7 7 -1 28 19.7 4.5 7 -1 28 17.7 3.5 -7 1 -28 21.9 2.6 7 1 28 17.1 4.7 7 1 28 28.9 5.5 9 -1 28 19.1 5.3 9 1 28 20.7 4.8 -18 -2 28 1.5 1.6 -18 2 28 1.4 2.5 18 2 -28 0.8 1.6 -16 -2 28 32.8 5.9 -16 -2 28 22.4 4.5 -16 2 28 24.6 5.2 16 2 -28 28.2 4.4 -14 -2 28 9 2.6 -14 -2 28 8.3 2.8 14 2 -28 9.8 2.3 -14 2 28 12 4 -12 -2 28 6 2.5 -12 -2 28 10 3.1 -12 2 28 3.1 2.2 12 2 -28 5.5 2.4 -10 -2 28 65.69 6.4 -10 -2 28 49.5 5.7 -10 2 28 56.59 6.6 10 2 -28 42.7 4.9 -8 -2 28 1.3 1.4 -8 -2 28 -2.6 1.3 8 2 -28 0.3 1.1 -8 2 28 0.6 1.2 -6 -2 28 6.2 1.9 -6 -2 28 2.2 2 -6 2 28 5.4 2.4 6 2 -28 6.7 2 -4 -2 28 16.8 3.6 -4 -2 28 15 4.3 -4 -2 28 9.3 2.6 4 2 -28 18 3.3 -4 2 28 14.7 3.4 -2 -2 28 15.9 3.8 -2 -2 28 17.2 4.3 -2 -2 28 18.1 3.9 2 2 -28 16 3 -2 2 28 19.7 4.1 0 -2 28 1.2 1.2 0 -2 28 0.5 1.5 0 2 28 -1 1.4 0 2 28 -1.2 1.5 0 2 -28 -1.7 1 2 -2 28 34.7 6.4 2 -2 28 46.1 5.6 -2 2 -28 44.9 7.3 2 2 28 43.8 5.3 2 2 28 44 6.1 4 -2 28 9.4 2.8 4 -2 28 11.7 4.2 4 2 28 6.2 2.3 -4 2 -28 12 2.6 4 2 28 11.9 3.8 20 0 -29 0.8 1.6 -18 0 29 -2.2 1.5 18 0 -29 3.9 0.9 -16 0 29 1.7 1.2 16 0 -29 1.6 1.1 14 0 -29 -0.6 0.9 -14 0 29 1.2 1.4 12 0 -29 -1 0.9 -12 0 29 -1.1 1.2 10 0 -29 -1.4 1.6 -10 0 29 0.5 1.7 -8 0 29 -0.6 1.1 8 0 -29 0.5 0.9 -6 0 29 0.4 1.2 6 0 -29 0.2 0.7 4 0 -29 -0.7 0.6 -4 0 29 -0.3 1.3 2 0 -29 -1.1 0.6 -2 0 29 0.3 1.4 -2 0 29 2.5 1.8 0 0 29 0.6 1.6 0 0 -29 -0.7 1 0 0 29 0.8 1.7 2 0 29 3.1 1.9 2 0 29 -1.3 1.2 -4 0 -29 -0.7 0.7 4 0 29 -0.4 1.3 4 0 29 -0.9 1.3 4 0 29 -1.3 1.1 -17 -1 29 -2.1 1.4 -17 1 29 -0.5 1.4 17 1 -29 -1.9 1 -15 -1 29 7.4 2.5 -15 1 29 4.4 1.8 15 1 -29 11.9 2.4 -13 -1 29 7.7 2.4 -13 1 29 5.3 2.5 13 1 -29 9.2 2.1 -11 -1 29 8.1 2.8 11 1 -29 7.6 2.1 -11 1 29 7.7 2.2 -9 -1 29 7.1 2.4 -9 1 29 4.2 2 9 1 -29 2.4 1.9 -7 -1 29 1.7 1.6 -7 1 29 -2.3 1.5 7 1 -29 0.1 1.1 -5 -1 29 17.8 3.7 -5 -1 29 24 4.1 5 1 -29 22.9 2.8 -5 1 29 17.2 3.6 -3 -1 29 4.8 2.4 -3 -1 29 12.2 3.2 -3 -1 29 6.7 2.9 3 1 -29 10.1 2 -3 1 29 9.4 3 -1 -1 29 9.3 3.1 -1 -1 29 11.4 3 -1 -1 29 5.7 2.4 -1 1 29 11.9 3.5 -1 1 29 7.4 2.8 1 1 -29 13.7 2.2 1 -1 29 -1 1.6 1 -1 29 -1.1 1.2 1 -1 29 0.7 1.5 1 1 29 -0.8 0.9 -1 1 -29 -1.6 0.8 3 -1 29 18.2 4.2 3 -1 29 24.1 5 3 -1 29 19.6 3.9 3 1 29 20.2 5.2 -3 1 -29 22.1 2.7 3 1 29 18.6 4.6 -6 -2 29 6.6 2.8 -10 0 30 3.1 2 -8 0 30 25.5 5.4 4 0 -30 -1.6 0.9 -4 0 30 0 1.2 _iucr_refine_instructions_details ; TITL 1_a.res in C2/c CELL 0.71073 32.003 4.9042 20.4881 90 99.159 90 ZERR 8 0.0038 0.0006 0.0024 0 0.004 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H N O UNIT 160 128 16 16 L.S. 4 PLAN 5 0 0 TEMP -28.18 CONF HTAB BOND $H fmap 2 acta MORE -1 REM REM REM WGHT 0.056400 2.384100 FVAR 0.27861 O1 4 0.406887 1.113980 0.267240 11.00000 0.02682 0.03084 = 0.01904 0.00437 0.00677 0.00212 O2 4 0.333256 0.461086 0.588375 11.00000 0.02208 0.02699 = 0.02236 0.00574 0.00951 0.00621 N1 3 0.514818 -0.510170 0.591188 11.00000 0.02668 0.02567 = 0.02726 -0.00043 0.00265 0.00713 N2 3 0.260856 1.308065 0.368757 11.00000 0.01939 0.01484 = 0.02179 0.00069 -0.00141 0.00209 C1 1 0.435857 0.915033 0.298609 11.00000 0.02540 0.03271 = 0.02481 0.00372 0.00662 0.00307 AFIX 137 H1A 2 0.445283 0.967365 0.344234 11.00000 -1.50000 H1B 2 0.460060 0.903449 0.275631 11.00000 -1.50000 H1C 2 0.421927 0.739003 0.297292 11.00000 -1.50000 AFIX 0 C2 1 0.370907 1.158201 0.294314 11.00000 0.02246 0.01945 = 0.01503 -0.00123 0.00178 -0.00247 C3 1 0.361105 1.017793 0.348811 11.00000 0.02104 0.01595 = 0.01481 -0.00088 0.00063 -0.00062 AFIX 43 H3 2 0.379440 0.883751 0.369985 11.00000 -1.20000 AFIX 0 C4 1 0.323049 1.081496 0.371439 11.00000 0.01952 0.01298 = 0.01571 -0.00093 -0.00040 -0.00079 C5 1 0.302634 0.987019 0.425492 11.00000 0.01734 0.01396 = 0.01859 0.00008 0.00121 -0.00013 C6 1 0.314740 0.791197 0.476712 11.00000 0.01689 0.01488 = 0.01850 0.00061 0.00206 -0.00115 AFIX 43 H6 2 0.296711 0.779496 0.508619 11.00000 -1.20000 AFIX 0 C7 1 0.348279 0.620618 0.485959 11.00000 0.01701 0.01450 = 0.01626 0.00110 0.00240 -0.00027 AFIX 43 H7 2 0.366898 0.613957 0.454839 11.00000 -1.20000 AFIX 0 C8 1 0.355534 0.446101 0.544634 11.00000 0.01491 0.01504 = 0.01672 0.00094 0.00242 -0.00016 C9 1 0.391142 0.242648 0.552540 11.00000 0.01491 0.01398 = 0.01473 -0.00048 0.00206 -0.00092 C10 1 0.399513 0.098844 0.612253 11.00000 0.01980 0.01846 = 0.01644 0.00120 0.00512 0.00244 AFIX 43 H10 2 0.383638 0.136484 0.646049 11.00000 -1.20000 AFIX 0 C11 1 0.430910 -0.098238 0.622121 11.00000 0.02177 0.01831 = 0.01659 0.00246 0.00330 0.00313 AFIX 43 H11 2 0.436514 -0.192896 0.662462 11.00000 -1.20000 AFIX 0 C12 1 0.454160 -0.154819 0.571469 11.00000 0.01589 0.01502 = 0.01825 -0.00058 0.00161 0.00043 C13 1 0.487502 -0.355389 0.582057 11.00000 0.01990 0.01861 = 0.01914 -0.00034 0.00250 0.00100 C14 1 0.343700 1.359853 0.261713 11.00000 0.02847 0.02015 = 0.01627 0.00232 0.00019 -0.00336 AFIX 43 H14 2 0.351210 1.451489 0.224983 11.00000 -1.20000 AFIX 0 C15 1 0.306251 1.423181 0.283350 11.00000 0.02783 0.01512 = 0.01854 0.00212 -0.00349 -0.00078 AFIX 43 H15 2 0.288014 1.557277 0.261970 11.00000 -1.20000 AFIX 0 C16 1 0.296233 1.282491 0.337862 11.00000 0.02111 0.01380 = 0.01796 -0.00146 -0.00155 -0.00041 C17 1 0.265008 1.134186 0.420681 11.00000 0.01871 0.01582 = 0.02099 -0.00001 0.00125 0.00006 AFIX 43 H17 2 0.245167 1.115197 0.449633 11.00000 -1.20000 AFIX 0 C18 1 0.225370 1.490479 0.347966 11.00000 0.02299 0.01696 = 0.02807 0.00011 -0.00376 0.00549 AFIX 137 H18A 2 0.203320 1.456227 0.374391 11.00000 -1.50000 H18B 2 0.214327 1.458729 0.301703 11.00000 -1.50000 H18C 2 0.234808 1.678080 0.353945 11.00000 -1.50000 AFIX 0 C19 1 0.445907 -0.015151 0.511399 11.00000 0.01593 0.01777 = 0.01679 -0.00118 0.00347 -0.00028 AFIX 43 H19 2 0.461291 -0.056237 0.477205 11.00000 -1.20000 AFIX 0 C20 1 0.414824 0.184765 0.502555 11.00000 0.01590 0.01608 = 0.01498 0.00080 0.00223 -0.00130 AFIX 43 H20 2 0.409662 0.282105 0.462558 11.00000 -1.20000 HKLF 4 REM 1_a.res in C2/c REM R1 = 0.0440 for 4352 Fo > 4sig(Fo) and 0.0563 for all 5308 data REM 219 parameters refined using 0 restraints END WGHT 0.0564 2.3841 REM Highest difference peak 0.432, deepest hole -0.249, 1-sigma level 0.059 Q1 1 0.4379 -0.1354 0.5910 11.00000 0.05 0.43 Q2 1 0.3729 0.3380 0.5465 11.00000 0.05 0.43 Q3 1 0.3925 0.1540 0.5785 11.00000 0.05 0.42 Q4 1 0.4500 -0.0775 0.5429 11.00000 0.05 0.41 Q5 1 0.2999 1.3494 0.3081 11.00000 0.05 0.39 REM The information below was added by Olex2. REM REM R1 = 0.0440 for 4352 Fo > 4sig(Fo) and 0.0563 for all 32690 data REM 219 parameters refined using n/a restraints REM Highest difference peak 0.43, deepest hole -0.25 REM Mean Shift 0, Max Shift -0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0563 REM R1_gt = 0.0440 REM wR_ref = 0.1233 REM GOOF = 1.037 REM Shift_max = -0.001 REM Shift_mean = 0 REM Reflections_all = 32690 REM Reflections_gt = 4352 REM Parameters = 219 REM Hole = -0.25 REM Peak = 0.43 REM Flack = n/a ; _olex2_submission_special_instructions 'No special instructions were received'