####################################################################### # # 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_flnb190404 _database_code_depnum_ccdc_archive 'CCDC 1911671' loop_ _audit_author_name _audit_author_address 'Lydia Karmazin' ;Universite de Strasbourg France ; _audit_update_record ; 2019-04-23 deposited with the CCDC. 2019-06-05 downloaded from the CCDC. ; _audit_creation_method SHELXL-2014/7 _shelx_SHELXL_version_number 2014/7 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H25 F N4 O2' _chemical_formula_sum 'C22 H25 F N4 O2' _chemical_formula_weight 396.46 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' F F 0.0171 0.0103 '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 triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.0215(3) _cell_length_b 10.3318(4) _cell_length_c 12.9525(5) _cell_angle_alpha 73.1910(10) _cell_angle_beta 89.7690(10) _cell_angle_gamma 75.3010(10) _cell_volume 991.17(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9983 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 29.03 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.328 _exptl_crystal_F_000 420 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.140 _exptl_crystal_size_min 0.120 _exptl_absorpt_coefficient_mu 0.094 _shelx_estimated_absorpt_T_min 0.982 _shelx_estimated_absorpt_T_max 0.989 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6929 _exptl_absorpt_correction_T_max 0.7458 _exptl_absorpt_process_details sadabs _exptl_absorpt_special_details ? _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator triumph _diffrn_source 'sealed tube' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 18907 _diffrn_reflns_av_unetI/netI 0.0632 _diffrn_reflns_av_R_equivalents 0.0440 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.647 _diffrn_reflns_theta_max 29.047 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.950 _diffrn_measured_fraction_theta_full 0.990 _diffrn_reflns_Laue_measured_fraction_max 0.950 _diffrn_reflns_Laue_measured_fraction_full 0.990 _diffrn_reflns_point_group_measured_fraction_max 0.950 _diffrn_reflns_point_group_measured_fraction_full 0.990 _reflns_number_total 5016 _reflns_number_gt 3236 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _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. ; _computing_data_collection 'Bruker APEX3' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics 'Mercury (Macrae et al., 2008)' _computing_publication_material 'SHELXL-2014/7 (Sheldrick 2014)' _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+1.5268P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 5016 _refine_ls_number_parameters 269 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1409 _refine_ls_R_factor_gt 0.0962 _refine_ls_wR_factor_ref 0.1450 _refine_ls_wR_factor_gt 0.1272 _refine_ls_goodness_of_fit_ref 1.245 _refine_ls_restrained_S_all 1.245 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_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 C1 C 1.2192(4) -0.0238(3) 0.5831(2) 0.0291(7) Uani 1 1 d . . . . . H1 H 1.2946 -0.1148 0.6128 0.035 Uiso 1 1 calc R U . . . C2 C 1.2417(4) 0.0533(3) 0.4786(2) 0.0259(6) Uani 1 1 d . . . . . C3 C 1.1439(3) 0.1877(3) 0.4274(2) 0.0224(6) Uani 1 1 d . . . . . C4 C 1.0118(3) 0.2404(3) 0.4888(2) 0.0210(6) Uani 1 1 d . . . . . C5 C 0.8707(3) 0.3633(3) 0.4762(2) 0.0223(6) Uani 1 1 d . . . . . C6 C 0.9989(4) 0.1530(3) 0.5931(2) 0.0237(6) Uani 1 1 d . . . . . C7 C 1.1774(3) 0.2673(3) 0.3175(2) 0.0229(6) Uani 1 1 d . . . . . C8 C 1.1746(4) 0.2140(3) 0.2302(2) 0.0273(6) Uani 1 1 d . . . . . H8 H 1.1566 0.1237 0.2412 0.033 Uiso 1 1 calc R U . . . C9 C 1.1981(4) 0.2931(3) 0.1275(2) 0.0331(7) Uani 1 1 d . . . . . H9 H 1.1950 0.2570 0.0681 0.040 Uiso 1 1 calc R U . . . C10 C 1.2260(4) 0.4237(3) 0.1107(2) 0.0339(7) Uani 1 1 d . . . . . H10 H 1.2390 0.4785 0.0398 0.041 Uiso 1 1 calc R U . . . C11 C 1.2348(4) 0.4746(3) 0.1977(2) 0.0320(7) Uani 1 1 d . . . . . H11 H 1.2576 0.5633 0.1867 0.038 Uiso 1 1 calc R U . . . C12 C 1.2109(4) 0.3974(3) 0.3007(2) 0.0263(6) Uani 1 1 d . . . . . H12 H 1.2173 0.4332 0.3599 0.032 Uiso 1 1 calc R U . . . C13 C 0.8110(3) 0.4944(3) 0.3809(2) 0.0206(6) Uani 1 1 d . . . . . H13 H 0.9107 0.5365 0.3627 0.025 Uiso 1 1 calc R U . . . C14 C 0.7529(4) 0.4621(3) 0.2803(2) 0.0267(6) Uani 1 1 d . . . . . H14A H 0.8483 0.3924 0.2617 0.032 Uiso 1 1 calc R U . . . H14B H 0.6533 0.4211 0.2961 0.032 Uiso 1 1 calc R U . . . C15 C 0.7015(4) 0.5951(3) 0.1844(2) 0.0304(7) Uani 1 1 d . . . . . H15A H 0.8038 0.6313 0.1643 0.036 Uiso 1 1 calc R U . . . H15B H 0.6590 0.5732 0.1215 0.036 Uiso 1 1 calc R U . . . C16 C 0.6093(4) 0.7355(3) 0.3093(2) 0.0270(6) Uani 1 1 d . . . . . H16A H 0.5079 0.8021 0.3256 0.032 Uiso 1 1 calc R U . . . H16B H 0.7052 0.7813 0.2962 0.032 Uiso 1 1 calc R U . . . C17 C 0.6623(4) 0.6042(3) 0.4057(2) 0.0245(6) Uani 1 1 d . . . . . H17A H 0.5621 0.5646 0.4242 0.029 Uiso 1 1 calc R U . . . H17B H 0.6983 0.6290 0.4689 0.029 Uiso 1 1 calc R U . . . C18 C 0.4258(4) 0.7830(3) 0.1461(2) 0.0225(6) Uani 1 1 d . . . . . C19 C 0.2865(4) 0.8369(3) -0.0362(2) 0.0254(6) Uani 1 1 d . . . . . C20 C 0.3311(4) 0.7647(3) -0.1238(2) 0.0365(8) Uani 1 1 d . . . . . H20A H 0.4426 0.7760 -0.1505 0.055 Uiso 1 1 calc R U . . . H20B H 0.2411 0.8070 -0.1837 0.055 Uiso 1 1 calc R U . . . H20C H 0.3381 0.6647 -0.0937 0.055 Uiso 1 1 calc R U . . . C21 C 0.3048(4) 0.9856(3) -0.0758(2) 0.0332(7) Uani 1 1 d . . . . . H21A H 0.2803 1.0298 -0.0180 0.050 Uiso 1 1 calc R U . . . H21B H 0.2229 1.0393 -0.1387 0.050 Uiso 1 1 calc R U . . . H21C H 0.4229 0.9836 -0.0964 0.050 Uiso 1 1 calc R U . . . C22 C 0.1088(4) 0.8288(3) -0.0002(2) 0.0318(7) Uani 1 1 d . . . . . H22A H 0.1038 0.7308 0.0215 0.048 Uiso 1 1 calc R U . . . H22B H 0.0217 0.8838 -0.0601 0.048 Uiso 1 1 calc R U . . . H22C H 0.0856 0.8664 0.0612 0.048 Uiso 1 1 calc R U . . . N1 N 1.0980(3) 0.0233(2) 0.64321(19) 0.0291(6) Uani 1 1 d . . . . . N2 N 0.7845(3) 0.3499(2) 0.56448(18) 0.0272(5) Uani 1 1 d . . . . . N3 N 0.8638(3) 0.2233(3) 0.6357(2) 0.0282(6) Uani 1 1 d . . . . . N4 N 0.5664(3) 0.7022(2) 0.21177(17) 0.0252(5) Uani 1 1 d . . . . . F1 F 1.3704(2) -0.00967(18) 0.42655(14) 0.0371(4) Uani 1 1 d . . . . . O1 O 0.3130(2) 0.8724(2) 0.17027(15) 0.0271(5) Uani 1 1 d . . . . . O2 O 0.4221(2) 0.7522(2) 0.05187(14) 0.0252(4) Uani 1 1 d . . . . . H3N H 0.818(4) 0.191(3) 0.698(3) 0.040(10) Uiso 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0315(16) 0.0197(14) 0.0297(16) -0.0006(12) -0.0059(13) -0.0031(12) C2 0.0255(15) 0.0254(15) 0.0258(15) -0.0088(12) 0.0017(11) -0.0035(12) C3 0.0246(14) 0.0242(14) 0.0174(13) -0.0041(11) -0.0022(11) -0.0068(11) C4 0.0229(14) 0.0206(14) 0.0171(12) -0.0003(11) -0.0022(10) -0.0072(11) C5 0.0230(14) 0.0257(15) 0.0166(13) -0.0039(11) -0.0015(10) -0.0064(11) C6 0.0255(15) 0.0253(15) 0.0181(13) -0.0033(11) -0.0020(11) -0.0063(12) C7 0.0180(13) 0.0269(15) 0.0187(13) -0.0027(11) 0.0014(10) -0.0017(11) C8 0.0294(16) 0.0287(16) 0.0253(15) -0.0095(12) 0.0031(12) -0.0087(12) C9 0.0374(18) 0.0407(19) 0.0232(15) -0.0129(14) 0.0075(13) -0.0101(14) C10 0.0419(19) 0.0364(18) 0.0210(15) -0.0022(13) 0.0090(13) -0.0133(15) C11 0.0380(18) 0.0275(16) 0.0285(16) -0.0030(13) 0.0052(13) -0.0117(14) C12 0.0303(16) 0.0267(15) 0.0206(14) -0.0046(12) 0.0003(11) -0.0082(12) C13 0.0207(13) 0.0225(14) 0.0152(12) -0.0023(11) -0.0004(10) -0.0033(11) C14 0.0264(15) 0.0277(15) 0.0210(14) -0.0088(12) -0.0043(11) 0.0033(12) C15 0.0304(16) 0.0358(17) 0.0158(13) -0.0064(12) -0.0021(11) 0.0059(13) C16 0.0328(16) 0.0254(15) 0.0182(13) -0.0052(12) -0.0051(11) -0.0011(12) C17 0.0285(15) 0.0248(15) 0.0162(13) -0.0032(11) -0.0008(11) -0.0033(12) C18 0.0276(15) 0.0195(14) 0.0150(12) 0.0018(10) 0.0022(11) -0.0051(12) C19 0.0246(14) 0.0247(15) 0.0196(13) 0.0006(11) -0.0073(11) -0.0016(11) C20 0.0412(19) 0.0388(19) 0.0223(15) -0.0060(13) -0.0098(13) -0.0011(15) C21 0.0357(17) 0.0307(17) 0.0264(15) 0.0023(13) -0.0033(13) -0.0091(14) C22 0.0267(16) 0.0281(16) 0.0349(17) -0.0015(13) -0.0047(13) -0.0060(13) N1 0.0334(14) 0.0244(13) 0.0235(12) -0.0004(10) -0.0018(10) -0.0048(11) N2 0.0297(13) 0.0272(13) 0.0177(11) 0.0008(10) -0.0009(10) -0.0040(10) N3 0.0301(14) 0.0288(14) 0.0180(12) 0.0013(10) 0.0035(10) -0.0034(11) N4 0.0288(13) 0.0254(13) 0.0148(11) -0.0040(9) -0.0031(9) 0.0022(10) F1 0.0368(10) 0.0336(10) 0.0328(10) -0.0093(8) 0.0039(8) 0.0044(8) O1 0.0285(11) 0.0252(11) 0.0213(10) -0.0033(8) 0.0014(8) -0.0004(9) O2 0.0247(10) 0.0273(11) 0.0163(9) -0.0021(8) -0.0043(8) 0.0012(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.327(4) . ? C1 C2 1.395(4) . ? C1 H1 0.9500 . ? C2 F1 1.361(3) . ? C2 C3 1.379(4) . ? C3 C4 1.416(4) . ? C3 C7 1.485(4) . ? C4 C6 1.412(4) . ? C4 C5 1.439(4) . ? C5 N2 1.325(3) . ? C5 C13 1.515(4) . ? C6 N1 1.346(4) . ? C6 N3 1.353(4) . ? C7 C12 1.393(4) . ? C7 C8 1.397(4) . ? C8 C9 1.386(4) . ? C8 H8 0.9500 . ? C9 C10 1.379(4) . ? C9 H9 0.9500 . ? C10 C11 1.384(4) . ? C10 H10 0.9500 . ? C11 C12 1.382(4) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C17 1.528(4) . ? C13 C14 1.538(4) . ? C13 H13 1.0000 . ? C14 C15 1.527(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 N4 1.462(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 N4 1.466(3) . ? C16 C17 1.520(4) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 O1 1.229(3) . ? C18 N4 1.346(3) . ? C18 O2 1.350(3) . ? C19 O2 1.483(3) . ? C19 C22 1.513(4) . ? C19 C21 1.517(4) . ? C19 C20 1.524(4) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? N2 N3 1.360(3) . ? N3 H3N 0.89(3) . ? 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 N1 C1 C2 123.5(3) . . ? N1 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? F1 C2 C3 119.3(3) . . ? F1 C2 C1 116.7(2) . . ? C3 C2 C1 124.0(3) . . ? C2 C3 C4 114.0(2) . . ? C2 C3 C7 121.9(3) . . ? C4 C3 C7 124.1(2) . . ? C6 C4 C3 117.4(2) . . ? C6 C4 C5 104.0(2) . . ? C3 C4 C5 138.5(2) . . ? N2 C5 C4 110.2(2) . . ? N2 C5 C13 119.5(2) . . ? C4 C5 C13 130.3(2) . . ? N1 C6 N3 124.9(3) . . ? N1 C6 C4 128.0(3) . . ? N3 C6 C4 107.2(2) . . ? C12 C7 C8 119.2(3) . . ? C12 C7 C3 119.9(2) . . ? C8 C7 C3 120.9(3) . . ? C9 C8 C7 119.9(3) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C10 C9 C8 120.6(3) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C9 C10 C11 119.6(3) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? C12 C11 C10 120.6(3) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C11 C12 C7 120.1(3) . . ? C11 C12 H12 120.0 . . ? C7 C12 H12 120.0 . . ? C5 C13 C17 112.6(2) . . ? C5 C13 C14 112.0(2) . . ? C17 C13 C14 108.0(2) . . ? C5 C13 H13 108.0 . . ? C17 C13 H13 108.0 . . ? C14 C13 H13 108.0 . . ? C15 C14 C13 110.7(2) . . ? C15 C14 H14A 109.5 . . ? C13 C14 H14A 109.5 . . ? C15 C14 H14B 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? N4 C15 C14 110.5(2) . . ? N4 C15 H15A 109.5 . . ? C14 C15 H15A 109.5 . . ? N4 C15 H15B 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 108.1 . . ? N4 C16 C17 111.3(2) . . ? N4 C16 H16A 109.4 . . ? C17 C16 H16A 109.4 . . ? N4 C16 H16B 109.4 . . ? C17 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? C16 C17 C13 111.1(2) . . ? C16 C17 H17A 109.4 . . ? C13 C17 H17A 109.4 . . ? C16 C17 H17B 109.4 . . ? C13 C17 H17B 109.4 . . ? H17A C17 H17B 108.0 . . ? O1 C18 N4 123.8(2) . . ? O1 C18 O2 124.2(2) . . ? N4 C18 O2 112.0(2) . . ? O2 C19 C22 110.9(2) . . ? O2 C19 C21 109.3(2) . . ? C22 C19 C21 113.4(2) . . ? O2 C19 C20 102.8(2) . . ? C22 C19 C20 109.8(2) . . ? C21 C19 C20 110.1(2) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C1 N1 C6 113.1(2) . . ? C5 N2 N3 107.2(2) . . ? C6 N3 N2 111.4(2) . . ? C6 N3 H3N 128(2) . . ? N2 N3 H3N 120(2) . . ? C18 N4 C15 124.5(2) . . ? C18 N4 C16 120.0(2) . . ? C15 N4 C16 114.5(2) . . ? C18 O2 C19 120.9(2) . . ? 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 N1 C1 C2 F1 -179.3(3) . . . . ? N1 C1 C2 C3 1.7(5) . . . . ? F1 C2 C3 C4 178.7(2) . . . . ? C1 C2 C3 C4 -2.3(4) . . . . ? F1 C2 C3 C7 -1.3(4) . . . . ? C1 C2 C3 C7 177.6(3) . . . . ? C2 C3 C4 C6 1.4(4) . . . . ? C7 C3 C4 C6 -178.6(2) . . . . ? C2 C3 C4 C5 -175.4(3) . . . . ? C7 C3 C4 C5 4.6(5) . . . . ? C6 C4 C5 N2 0.5(3) . . . . ? C3 C4 C5 N2 177.6(3) . . . . ? C6 C4 C5 C13 -178.2(3) . . . . ? C3 C4 C5 C13 -1.1(5) . . . . ? C3 C4 C6 N1 0.2(4) . . . . ? C5 C4 C6 N1 178.0(3) . . . . ? C3 C4 C6 N3 -179.1(2) . . . . ? C5 C4 C6 N3 -1.3(3) . . . . ? C2 C3 C7 C12 -123.3(3) . . . . ? C4 C3 C7 C12 56.7(4) . . . . ? C2 C3 C7 C8 57.1(4) . . . . ? C4 C3 C7 C8 -122.9(3) . . . . ? C12 C7 C8 C9 -2.6(4) . . . . ? C3 C7 C8 C9 177.0(3) . . . . ? C7 C8 C9 C10 0.6(5) . . . . ? C8 C9 C10 C11 1.6(5) . . . . ? C9 C10 C11 C12 -1.9(5) . . . . ? C10 C11 C12 C7 0.0(5) . . . . ? C8 C7 C12 C11 2.3(4) . . . . ? C3 C7 C12 C11 -177.3(3) . . . . ? N2 C5 C13 C17 5.7(4) . . . . ? C4 C5 C13 C17 -175.7(3) . . . . ? N2 C5 C13 C14 -116.3(3) . . . . ? C4 C5 C13 C14 62.3(4) . . . . ? C5 C13 C14 C15 -177.4(2) . . . . ? C17 C13 C14 C15 58.0(3) . . . . ? C13 C14 C15 N4 -56.4(3) . . . . ? N4 C16 C17 C13 55.2(3) . . . . ? C5 C13 C17 C16 178.5(2) . . . . ? C14 C13 C17 C16 -57.3(3) . . . . ? C2 C1 N1 C6 0.0(4) . . . . ? N3 C6 N1 C1 178.3(3) . . . . ? C4 C6 N1 C1 -1.0(4) . . . . ? C4 C5 N2 N3 0.5(3) . . . . ? C13 C5 N2 N3 179.3(2) . . . . ? N1 C6 N3 N2 -177.7(3) . . . . ? C4 C6 N3 N2 1.7(3) . . . . ? C5 N2 N3 C6 -1.4(3) . . . . ? O1 C18 N4 C15 179.8(3) . . . . ? O2 C18 N4 C15 1.1(4) . . . . ? O1 C18 N4 C16 -11.8(4) . . . . ? O2 C18 N4 C16 169.4(2) . . . . ? C14 C15 N4 C18 -136.5(3) . . . . ? C14 C15 N4 C16 54.6(3) . . . . ? C17 C16 N4 C18 136.5(3) . . . . ? C17 C16 N4 C15 -54.1(3) . . . . ? O1 C18 O2 C19 6.6(4) . . . . ? N4 C18 O2 C19 -174.6(2) . . . . ? C22 C19 O2 C18 -62.1(3) . . . . ? C21 C19 O2 C18 63.7(3) . . . . ? C20 C19 O2 C18 -179.4(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3N O1 0.89(3) 2.04(3) 2.924(3) 174(3) 2_666 _refine_diff_density_max 0.343 _refine_diff_density_min -0.392 _refine_diff_density_rms 0.071 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL mo_flnb190404_0m_a.res in P-1 CELL 0.71073 8.0215 10.3318 12.9525 73.191 89.769 75.301 ZERR 2.00 0.0003 0.0004 0.0005 0.001 0.001 0.001 LATT 1 SFAC C H N F O UNIT 44 50 8 2 4 MERG 2 EQIV $1 -x+1, -y+1, -z+1 HTAB N3 O1_$1 FMAP 2 PLAN 10 SIZE 0.120 0.140 0.200 ACTA BOND $H CONF LIST 4 L.S. 8 TEMP -100.00 WGHT 0.000000 1.526800 FVAR 0.78830 C1 1 1.219161 -0.023773 0.583075 11.00000 0.03150 0.01973 = 0.02970 -0.00057 -0.00593 -0.00311 AFIX 43 H1 2 1.294591 -0.114810 0.612754 11.00000 -1.20000 AFIX 0 C2 1 1.241654 0.053316 0.478567 11.00000 0.02549 0.02543 = 0.02584 -0.00876 0.00171 -0.00355 C3 1 1.143921 0.187662 0.427360 11.00000 0.02459 0.02416 = 0.01736 -0.00405 -0.00216 -0.00682 C4 1 1.011779 0.240448 0.488817 11.00000 0.02288 0.02055 = 0.01706 -0.00025 -0.00221 -0.00723 C5 1 0.870680 0.363298 0.476152 11.00000 0.02301 0.02569 = 0.01663 -0.00388 -0.00149 -0.00635 C6 1 0.998851 0.153033 0.593133 11.00000 0.02548 0.02529 = 0.01808 -0.00328 -0.00204 -0.00634 C7 1 1.177385 0.267323 0.317538 11.00000 0.01804 0.02685 = 0.01867 -0.00265 0.00143 -0.00172 C8 1 1.174594 0.214007 0.230196 11.00000 0.02940 0.02875 = 0.02534 -0.00948 0.00309 -0.00874 AFIX 43 H8 2 1.156626 0.123721 0.241171 11.00000 -1.20000 AFIX 0 C9 1 1.198096 0.293105 0.127479 11.00000 0.03742 0.04072 = 0.02325 -0.01293 0.00752 -0.01009 AFIX 43 H9 2 1.194969 0.257003 0.068082 11.00000 -1.20000 AFIX 0 C10 1 1.225976 0.423726 0.110696 11.00000 0.04192 0.03639 = 0.02100 -0.00219 0.00902 -0.01331 AFIX 43 H10 2 1.239021 0.478454 0.039818 11.00000 -1.20000 AFIX 0 C11 1 1.234828 0.474561 0.197742 11.00000 0.03802 0.02750 = 0.02853 -0.00296 0.00517 -0.01166 AFIX 43 H11 2 1.257562 0.563272 0.186680 11.00000 -1.20000 AFIX 0 C12 1 1.210884 0.397405 0.300652 11.00000 0.03034 0.02675 = 0.02061 -0.00457 0.00030 -0.00822 AFIX 43 H12 2 1.217285 0.433151 0.359930 11.00000 -1.20000 AFIX 0 C13 1 0.811039 0.494417 0.380917 11.00000 0.02073 0.02251 = 0.01518 -0.00229 -0.00037 -0.00333 AFIX 13 H13 2 0.910737 0.536515 0.362721 11.00000 -1.20000 AFIX 0 C14 1 0.752888 0.462068 0.280285 11.00000 0.02644 0.02769 = 0.02104 -0.00877 -0.00430 0.00334 AFIX 23 H14A 2 0.848266 0.392435 0.261710 11.00000 -1.20000 H14B 2 0.653285 0.421064 0.296132 11.00000 -1.20000 AFIX 0 C15 1 0.701460 0.595129 0.184447 11.00000 0.03044 0.03577 = 0.01582 -0.00643 -0.00208 0.00591 AFIX 23 H15A 2 0.803823 0.631334 0.164254 11.00000 -1.20000 H15B 2 0.658994 0.573158 0.121532 11.00000 -1.20000 AFIX 0 C16 1 0.609349 0.735475 0.309301 11.00000 0.03277 0.02542 = 0.01817 -0.00521 -0.00510 -0.00109 AFIX 23 H16A 2 0.507860 0.802119 0.325645 11.00000 -1.20000 H16B 2 0.705150 0.781260 0.296201 11.00000 -1.20000 AFIX 0 C17 1 0.662315 0.604237 0.405653 11.00000 0.02852 0.02477 = 0.01622 -0.00317 -0.00085 -0.00332 AFIX 23 H17A 2 0.562097 0.564622 0.424219 11.00000 -1.20000 H17B 2 0.698285 0.628988 0.468893 11.00000 -1.20000 AFIX 0 C18 1 0.425810 0.783016 0.146108 11.00000 0.02762 0.01953 = 0.01503 0.00181 0.00215 -0.00514 C19 1 0.286512 0.836883 -0.036209 11.00000 0.02462 0.02468 = 0.01964 0.00055 -0.00731 -0.00165 C20 1 0.331067 0.764706 -0.123827 11.00000 0.04119 0.03880 = 0.02230 -0.00600 -0.00978 -0.00109 AFIX 137 H20A 2 0.442577 0.776010 -0.150515 11.00000 -1.50000 H20B 2 0.241147 0.806993 -0.183655 11.00000 -1.50000 H20C 2 0.338125 0.664704 -0.093653 11.00000 -1.50000 AFIX 0 C21 1 0.304768 0.985551 -0.075811 11.00000 0.03566 0.03072 = 0.02644 0.00225 -0.00335 -0.00905 AFIX 137 H21A 2 0.280299 1.029808 -0.017964 11.00000 -1.50000 H21B 2 0.222909 1.039270 -0.138687 11.00000 -1.50000 H21C 2 0.422887 0.983607 -0.096361 11.00000 -1.50000 AFIX 0 C22 1 0.108765 0.828778 -0.000249 11.00000 0.02668 0.02811 = 0.03491 -0.00151 -0.00472 -0.00600 AFIX 137 H22A 2 0.103840 0.730827 0.021476 11.00000 -1.50000 H22B 2 0.021714 0.883837 -0.060132 11.00000 -1.50000 H22C 2 0.085620 0.866420 0.061200 11.00000 -1.50000 AFIX 0 N1 3 1.098048 0.023280 0.643215 11.00000 0.03341 0.02444 = 0.02347 -0.00043 -0.00179 -0.00477 N2 3 0.784509 0.349905 0.564479 11.00000 0.02969 0.02720 = 0.01767 0.00081 -0.00093 -0.00399 N3 3 0.863842 0.223321 0.635692 11.00000 0.03005 0.02879 = 0.01795 0.00127 0.00349 -0.00340 N4 3 0.566354 0.702177 0.211766 11.00000 0.02882 0.02538 = 0.01478 -0.00400 -0.00309 0.00219 F1 4 1.370446 -0.009670 0.426548 11.00000 0.03676 0.03364 = 0.03281 -0.00925 0.00390 0.00438 O1 5 0.313007 0.872379 0.170266 11.00000 0.02851 0.02521 = 0.02128 -0.00329 0.00139 -0.00040 O2 5 0.422067 0.752190 0.051868 11.00000 0.02466 0.02728 = 0.01634 -0.00211 -0.00426 0.00124 H3N 2 0.817718 0.191292 0.697676 11.00000 0.03979 HKLF 4 1.0 1.00 0.00 0.00 0.00 1.00 0.00 0.00 0.00 1.00 REM mo_flnb190404_0m_a.res in P-1 REM R1 = 0.0962 for 3236 Fo > 4sig(Fo) and 0.1409 for all 5016 data REM 269 parameters refined using 0 restraints END WGHT 0.0000 1.4972 REM Highest difference peak 0.343, deepest hole -0.392, 1-sigma level 0.071 Q1 1 1.1505 0.2808 0.1784 11.00000 0.05 0.34 Q2 1 0.7279 0.5552 0.3735 11.00000 0.05 0.33 Q3 1 0.7744 0.4735 0.3309 11.00000 0.05 0.32 Q4 1 0.5933 0.7180 0.2455 11.00000 0.05 0.31 Q5 1 1.1595 0.2399 0.3784 11.00000 0.05 0.31 Q6 1 1.2881 0.4241 0.2626 11.00000 0.05 0.30 Q7 1 0.8435 0.4324 0.4309 11.00000 0.05 0.29 Q8 1 0.1061 0.9038 -0.0750 11.00000 0.05 0.29 Q9 1 0.2713 0.8106 -0.0840 11.00000 0.05 0.28 Q10 1 0.9731 0.3213 0.4753 11.00000 0.05 0.27 ; _shelx_res_checksum 10821 _shelx_hkl_file ; -1 0 0 66.39 1.80 -1 0 0 69.49 2.50 -1 0 0 70.79 2.00 -1 0 0 71.69 3.10 -1 0 0 60.89 2.20 -1 0 0 70.99 3.30 1 0 0 67.29 2.30 1 0 0 69.99 2.00 1 0 0 67.19 2.80 1 0 0 68.69 1.80 1 0 0 68.79 2.50 -2 0 0 5676.13 93.19 -2 0 0 5617.44 101.19 -2 0 0 5638.04 95.19 -2 0 0 5678.43 104.89 2 0 0 5476.25 94.39 2 0 0 5447.16 98.09 2 0 0 5634.24 104.99 2 0 0 5439.96 99.09 2 0 0 5527.65 93.19 -3 0 0 81.29 3.20 -3 0 0 70.69 6.10 -3 0 0 71.09 5.00 3 0 0 75.09 5.10 3 0 0 77.89 6.90 3 0 0 73.89 5.30 3 0 0 81.99 4.20 3 0 0 74.79 3.50 -4 0 0 11.60 2.80 -4 0 0 11.90 4.80 4 0 0 12.90 3.20 4 0 0 6.90 1.60 4 0 0 17.50 5.20 -5 0 0 253.77 12.20 -5 0 0 256.17 9.70 5 0 0 262.77 8.20 5 0 0 257.67 9.60 5 0 0 258.57 7.00 -6 0 0 -0.10 3.30 -6 0 0 -4.10 6.30 6 0 0 0.20 1.70 6 0 0 0.00 1.60 6 0 0 3.10 2.10 6 0 0 2.20 2.90 -7 0 0 39.30 10.40 7 0 0 36.80 5.10 7 0 0 41.10 8.20 7 0 0 40.60 6.50 -8 0 0 10.40 8.50 8 0 0 -2.00 2.50 8 0 0 0.40 1.90 8 0 0 4.90 3.20 9 0 0 66.89 9.00 9 0 0 75.39 10.10 -10 1 0 42.00 14.20 9 -1 0 -0.40 2.20 -9 1 0 21.90 11.00 8 -1 0 18.40 4.10 -8 1 0 33.10 12.00 7 -1 0 96.69 7.60 7 -1 0 94.59 9.90 7 -1 0 95.79 6.50 -7 1 0 103.59 11.70 6 -1 0 169.48 8.30 6 -1 0 178.68 10.60 6 -1 0 174.08 7.30 -6 1 0 157.38 12.20 -6 1 0 173.68 9.20 5 -1 0 125.79 6.00 5 -1 0 135.79 8.40 5 -1 0 141.69 7.30 -5 1 0 130.89 7.30 -5 1 0 133.29 10.00 4 -1 0 689.23 13.80 4 -1 0 721.23 15.50 4 -1 0 702.63 14.20 4 -1 0 693.03 15.10 -4 1 0 689.63 14.70 -4 1 0 698.43 17.80 3 -1 0 100.79 5.30 3 -1 0 104.19 4.60 3 -1 0 102.19 5.20 3 -1 0 101.19 4.60 -3 1 0 97.99 5.00 -3 1 0 91.19 8.10 -3 1 0 101.09 7.30 -3 1 0 98.59 2.50 2 -1 0 1146.69 20.40 2 -1 0 1168.38 19.50 2 -1 0 1113.69 22.90 2 -1 0 1097.59 20.10 2 -1 0 1158.68 19.50 -2 1 0 1129.59 19.30 -2 1 0 1078.69 22.70 -2 1 0 1131.79 21.70 -2 1 0 1138.39 19.90 -2 1 0 1122.89 21.50 1 -1 0 -0.20 1.30 1 -1 0 -1.40 1.40 1 -1 0 0.90 0.70 1 -1 0 1.10 0.80 1 -1 0 0.00 0.70 1 -1 0 2.80 1.40 -1 1 0 0.90 1.40 -1 1 0 1.30 1.00 -1 1 0 0.90 0.70 -1 1 0 -0.90 1.40 -1 1 0 -0.30 0.70 0 -1 0 26.80 1.60 0 -1 0 27.40 2.00 0 -1 0 26.40 1.20 0 -1 0 25.00 1.50 0 1 0 27.90 1.50 0 1 0 26.70 2.00 0 1 0 26.90 2.30 0 1 0 27.80 1.20 0 1 0 26.20 1.50 -1 -1 0 6.80 1.60 -1 -1 0 8.40 1.20 -1 -1 0 9.30 1.80 -1 -1 0 5.80 2.30 -1 -1 0 6.90 2.00 -1 -1 0 8.60 1.80 1 1 0 6.20 2.10 1 1 0 9.30 2.00 1 1 0 6.90 1.50 1 1 0 8.20 1.30 1 1 0 7.20 2.10 -2 -1 0 116.69 3.60 -2 -1 0 103.29 3.30 -2 -1 0 108.99 2.10 -2 -1 0 111.59 2.60 -2 -1 0 89.89 5.50 -2 -1 0 96.69 5.80 2 1 0 109.49 2.60 2 1 0 117.79 3.90 2 1 0 94.69 5.80 2 1 0 114.89 5.20 2 1 0 110.89 3.40 2 1 0 88.19 6.40 -3 -1 0 1276.97 23.20 -3 -1 0 1327.37 21.60 -3 -1 0 1254.17 22.70 -3 -1 0 1306.37 24.60 -3 -1 0 1268.17 24.20 3 1 0 1335.77 22.30 3 1 0 1286.37 22.50 3 1 0 1285.27 22.80 3 1 0 1297.67 23.40 3 1 0 1272.17 24.00 -4 -1 0 0.40 2.70 -4 -1 0 5.00 1.60 -4 -1 0 1.20 4.40 4 1 0 1.40 1.20 4 1 0 3.40 1.60 4 1 0 3.10 1.40 4 1 0 3.50 1.10 -5 -1 0 91.79 7.10 -5 -1 0 91.69 8.20 -5 -1 0 92.79 3.80 5 1 0 98.59 5.50 5 1 0 94.79 7.00 5 1 0 93.99 4.10 -6 -1 0 136.69 10.00 -6 -1 0 142.79 11.90 6 1 0 146.19 5.40 6 1 0 155.38 9.30 6 1 0 149.49 7.20 -7 -1 0 -3.40 7.20 7 1 0 -0.40 1.70 7 1 0 1.30 2.60 7 1 0 4.10 2.20 -8 -1 0 8.80 8.40 8 1 0 1.10 2.40 8 1 0 7.20 2.90 -9 -1 0 21.40 9.50 9 1 0 -0.70 2.40 9 1 0 1.50 2.30 10 1 0 39.10 8.30 10 1 0 43.40 11.00 -10 2 0 52.09 17.60 9 -2 0 50.29 7.20 9 -2 0 39.40 8.40 9 -2 0 44.50 11.10 -9 2 0 78.29 14.40 8 -2 0 34.60 9.90 8 -2 0 35.10 6.70 8 -2 0 29.70 7.20 -8 2 0 55.09 12.30 7 -2 0 458.65 12.50 7 -2 0 449.46 13.20 7 -2 0 470.25 15.70 -7 2 0 466.15 18.70 6 -2 0 5.90 2.30 6 -2 0 5.80 1.90 6 -2 0 13.00 4.20 -6 2 0 12.50 7.70 5 -2 0 81.59 6.90 5 -2 0 88.49 8.20 5 -2 0 90.49 6.50 5 -2 0 87.49 6.20 -5 2 0 81.29 11.20 -5 2 0 86.69 6.10 4 -2 0 14.80 4.10 4 -2 0 18.30 4.50 4 -2 0 12.40 4.70 -4 2 0 14.00 4.10 -4 2 0 13.70 2.30 -4 2 0 21.30 7.60 3 -2 0 250.87 7.30 3 -2 0 240.98 6.90 3 -2 0 246.38 6.70 3 -2 0 238.78 5.60 -3 2 0 235.28 11.80 -3 2 0 244.78 5.60 -3 2 0 241.68 6.40 -3 2 0 249.38 10.30 2 -2 0 60.89 2.90 2 -2 0 67.39 4.10 2 -2 0 60.89 3.20 2 -2 0 76.59 8.80 2 -2 0 59.99 4.00 -2 2 0 62.49 3.20 -2 2 0 61.09 3.20 -2 2 0 49.99 7.40 -2 2 0 59.19 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92.99 4.70 3 2 0 85.79 6.00 -4 -2 0 876.31 19.10 -4 -2 0 874.71 15.50 -4 -2 0 891.51 14.60 -4 -2 0 876.01 19.60 4 2 0 876.21 15.50 4 2 0 855.91 16.20 4 2 0 876.81 18.20 -5 -2 0 51.89 7.10 -5 -2 0 56.89 2.70 -5 -2 0 52.49 7.10 5 2 0 65.19 5.40 5 2 0 59.09 3.10 5 2 0 67.09 6.70 5 2 0 62.99 2.80 -6 -2 0 128.99 4.20 -6 -2 0 133.79 10.20 -6 -2 0 119.89 10.60 6 2 0 145.39 9.00 6 2 0 136.19 4.40 6 2 0 134.99 6.70 -7 -2 0 171.78 13.30 7 2 0 162.58 5.30 7 2 0 165.68 8.60 7 2 0 168.08 11.50 -8 -2 0 16.20 8.10 8 2 0 3.70 2.00 8 2 0 4.60 2.30 9 2 0 28.30 6.90 -10 -2 0 19.40 10.30 10 2 0 -3.80 2.40 10 2 0 -6.30 2.80 9 -3 0 0.20 4.70 -9 3 0 47.40 16.20 8 -3 0 24.90 7.10 -8 3 0 45.90 13.60 7 -3 0 161.68 9.00 7 -3 0 158.58 10.20 7 -3 0 168.98 8.90 -7 3 0 160.48 13.50 6 -3 0 75.19 7.30 6 -3 0 71.89 7.00 6 -3 0 67.79 9.00 -6 3 0 68.99 10.80 5 -3 0 111.19 7.50 5 -3 0 103.69 5.90 5 -3 0 113.89 7.20 -5 3 0 104.39 4.20 -5 3 0 116.49 11.50 -5 3 0 110.79 5.70 -5 3 0 96.59 14.10 4 -3 0 19.60 5.00 4 -3 0 26.00 4.90 4 -3 0 20.80 3.80 -4 3 0 23.70 3.80 -4 3 0 33.80 9.10 -4 3 0 22.40 3.40 3 -3 0 2.80 2.90 3 -3 0 2.60 2.40 3 -3 0 2.70 1.50 -3 3 0 1.70 1.30 -3 3 0 3.70 2.50 -3 3 0 0.20 1.40 2 -3 0 120.69 10.60 2 -3 0 120.49 4.60 2 -3 0 113.59 4.80 2 -3 0 118.49 5.90 -2 3 0 116.89 3.90 -2 3 0 100.79 8.90 -2 3 0 117.19 4.60 -2 3 0 112.09 9.70 1 -3 0 106.29 4.70 1 -3 0 102.99 3.70 1 -3 0 103.79 4.90 1 -3 0 110.89 8.10 -1 3 0 109.69 8.90 -1 3 0 108.09 4.70 -1 3 0 95.79 8.40 0 -3 0 0.80 2.20 0 -3 0 3.60 2.40 0 -3 0 -4.20 3.20 0 3 0 -0.40 2.80 0 3 0 17.10 6.60 0 3 0 -0.40 2.00 0 3 0 3.60 3.10 -1 -3 0 718.93 14.00 -1 -3 0 729.93 13.80 -1 -3 0 724.13 15.30 -1 -3 0 723.43 12.70 1 3 0 719.13 12.60 1 3 0 712.83 14.20 1 3 0 719.03 15.40 1 3 0 696.43 14.50 1 3 0 736.53 15.80 1 3 0 669.13 13.70 -2 -3 0 55.29 5.50 -2 -3 0 61.19 2.60 -2 -3 0 52.59 4.40 -2 -3 0 46.40 4.00 -2 -3 0 58.49 2.20 2 3 0 55.09 4.00 2 3 0 58.19 4.10 2 3 0 55.49 2.10 2 3 0 56.09 2.80 2 3 0 63.79 5.20 2 3 0 60.59 6.50 -3 -3 0 3.30 3.00 -3 -3 0 2.50 2.70 -3 -3 0 5.30 3.40 -3 -3 0 2.20 0.90 3 3 0 2.70 1.20 3 3 0 3.40 2.20 3 3 0 4.50 2.60 3 3 0 7.90 2.40 3 3 0 3.30 1.00 -4 -3 0 151.68 5.50 -4 -3 0 154.28 3.70 -4 -3 0 138.49 8.30 -4 -3 0 145.19 7.70 4 3 0 158.88 5.50 4 3 0 156.48 8.50 4 3 0 159.18 7.50 4 3 0 155.38 5.50 -5 -3 0 4.10 2.70 -5 -3 0 3.10 4.80 -5 -3 0 0.40 3.70 5 3 0 2.00 1.40 5 3 0 3.60 1.60 5 3 0 5.90 2.70 5 3 0 1.30 2.50 -6 -3 0 3.90 1.10 -6 -3 0 1.10 5.90 6 3 0 2.50 1.90 6 3 0 0.90 3.10 6 3 0 2.70 1.90 6 3 0 2.30 2.70 -7 -3 0 30.80 8.20 7 3 0 13.20 2.50 7 3 0 13.60 4.00 7 3 0 28.50 8.50 -8 -3 0 29.40 10.30 8 3 0 8.80 2.50 8 3 0 5.10 2.10 8 3 0 12.60 4.10 -9 -3 0 14.50 8.90 9 3 0 33.20 13.00 -10 -3 0 61.79 15.40 10 3 0 61.79 13.60 9 -4 0 -0.10 3.30 9 -4 0 10.40 5.40 9 -4 0 4.20 2.30 8 -4 0 0.60 1.90 8 -4 0 2.70 5.00 8 -4 0 -4.40 2.60 -8 4 0 11.90 9.40 7 -4 0 9.10 2.60 7 -4 0 12.90 4.60 7 -4 0 25.00 7.90 -7 4 0 22.10 8.60 6 -4 0 106.79 9.60 6 -4 0 113.89 7.70 6 -4 0 100.49 7.40 -6 4 0 106.39 11.90 5 -4 0 402.26 11.90 5 -4 0 406.76 11.80 -5 4 0 421.86 21.80 -5 4 0 407.86 17.30 4 -4 0 98.29 7.50 4 -4 0 105.99 7.00 -4 4 0 105.79 6.20 -4 4 0 104.09 3.80 -4 4 0 78.09 13.90 -4 4 0 108.29 11.10 3 -4 0 -1.50 3.00 3 -4 0 0.20 3.30 3 -4 0 1.60 1.40 -3 4 0 1.10 1.20 -3 4 0 -1.40 1.60 2 -4 0 8.90 3.40 2 -4 0 4.10 1.30 2 -4 0 10.00 3.50 -2 4 0 0.90 1.40 -2 4 0 2.70 3.00 1 -4 0 53.59 8.00 1 -4 0 57.59 4.70 1 -4 0 60.39 3.40 1 -4 0 61.79 5.30 -1 4 0 51.19 9.30 -1 4 0 64.39 9.30 0 -4 0 1378.36 23.30 0 -4 0 1437.36 24.30 0 -4 0 1374.96 26.60 0 4 0 1427.36 24.30 0 4 0 1369.86 24.80 0 4 0 1368.06 27.50 0 4 0 1408.06 28.50 -1 -4 0 161.38 6.80 -1 -4 0 171.28 5.00 1 4 0 166.88 7.90 1 4 0 166.58 6.80 1 4 0 164.38 4.80 1 4 0 156.48 6.10 1 4 0 177.98 9.10 -2 -4 0 69.29 2.90 -2 -4 0 70.69 3.10 -2 -4 0 64.59 5.00 2 4 0 72.79 7.70 2 4 0 69.19 4.30 2 4 0 77.39 5.80 2 4 0 68.79 2.90 -3 -4 0 628.04 10.60 -3 -4 0 615.74 13.40 -3 -4 0 639.04 11.40 3 4 0 621.84 15.60 3 4 0 628.44 11.50 3 4 0 626.64 14.30 -4 -4 0 89.89 7.00 -4 -4 0 82.69 5.30 -4 -4 0 78.99 4.30 4 4 0 87.69 4.30 4 4 0 103.69 7.70 4 4 0 90.39 8.80 -5 -4 0 150.68 4.10 -5 -4 0 148.79 9.20 -5 -4 0 155.08 6.50 5 4 0 150.68 8.80 5 4 0 155.28 10.90 5 4 0 149.69 6.00 -6 -4 0 -0.60 3.50 -6 -4 0 1.50 5.70 6 4 0 0.60 1.70 6 4 0 0.40 1.70 6 4 0 -1.60 3.50 -7 -4 0 31.30 10.00 7 4 0 31.20 8.70 7 4 0 34.10 6.40 -8 -4 0 12.60 8.30 8 4 0 1.50 2.00 8 4 0 8.60 4.50 8 4 0 4.50 2.30 -9 -4 0 -0.90 8.70 9 4 0 -0.60 2.40 9 4 0 5.50 5.00 9 4 0 -2.80 2.00 -10 -4 0 11.40 10.40 10 4 0 -2.10 2.40 10 4 0 9.80 5.90 8 -5 0 9.10 5.50 -8 5 0 12.00 9.30 7 -5 0 -2.10 2.40 7 -5 0 -2.10 4.40 7 -5 0 1.10 1.90 -7 5 0 7.80 8.80 -6 5 0 12.90 8.90 5 -5 0 18.10 5.00 -5 5 0 39.50 13.40 -5 5 0 21.30 8.20 4 -5 0 39.30 6.90 4 -5 0 27.90 5.90 -4 5 0 42.90 13.10 3 -5 0 12.20 4.20 3 -5 0 4.90 1.70 3 -5 0 8.10 4.00 -3 5 0 2.10 2.10 2 -5 0 50.99 4.30 2 -5 0 44.50 5.60 2 -5 0 45.90 5.60 -2 5 0 37.10 11.60 -2 5 0 44.80 11.00 -2 5 0 47.90 3.90 1 -5 0 391.56 10.20 1 -5 0 368.46 10.30 1 -5 0 379.36 8.60 -1 5 0 388.66 16.20 -1 5 0 385.46 15.10 0 -5 0 1106.59 19.20 0 -5 0 1162.88 20.70 0 -5 0 1100.89 21.80 0 -5 0 1086.99 23.30 0 5 0 1111.19 24.80 0 5 0 1101.89 21.10 0 5 0 1107.69 26.00 -1 -5 0 250.97 8.60 -1 -5 0 257.37 7.00 1 5 0 257.47 12.20 1 5 0 251.77 10.80 1 5 0 245.18 8.90 -2 -5 0 593.84 10.70 -2 -5 0 600.04 11.40 -2 -5 0 594.24 13.80 2 5 0 594.84 16.00 2 5 0 579.04 11.20 2 5 0 595.84 16.20 2 5 0 588.94 14.10 -3 -5 0 223.88 5.50 -3 -5 0 218.38 8.00 -3 -5 0 226.78 5.20 3 5 0 223.58 5.10 3 5 0 226.88 9.00 3 5 0 224.88 10.40 -4 -5 0 282.97 5.10 -4 -5 0 281.07 9.20 4 5 0 281.17 6.90 4 5 0 282.27 10.50 4 5 0 287.77 11.80 -5 -5 0 98.49 4.60 -5 -5 0 95.59 8.60 -5 -5 0 96.59 7.00 5 5 0 107.49 10.00 5 5 0 108.29 9.70 5 5 0 101.49 5.50 -6 -5 0 0.40 4.30 -6 -5 0 1.40 1.60 -6 -5 0 4.90 6.00 6 5 0 2.50 2.00 6 5 0 1.10 1.80 6 5 0 2.00 3.60 7 5 0 6.80 2.00 7 5 0 9.90 4.00 7 5 0 4.50 2.00 -8 -5 0 40.60 11.30 8 5 0 32.20 9.40 8 5 0 30.40 6.40 8 5 0 39.50 13.50 -9 -5 0 18.70 8.20 9 5 0 11.10 5.30 -10 -5 0 7.20 9.10 10 5 0 1.40 5.40 10 5 0 -5.00 2.60 10 5 0 -4.40 2.60 8 -6 0 -3.20 2.90 8 -6 0 4.50 6.00 8 -6 0 -0.10 2.20 -8 6 0 10.70 9.60 7 -6 0 -3.30 2.50 7 -6 0 2.40 1.90 7 -6 0 0.00 5.50 -7 6 0 6.80 8.70 5 -6 0 23.80 6.30 5 -6 0 17.50 5.40 -5 6 0 15.70 8.60 4 -6 0 113.39 7.70 4 -6 0 126.79 8.20 -4 6 0 139.89 16.50 3 -6 0 114.99 7.30 3 -6 0 120.99 8.00 3 -6 0 125.19 8.10 -3 6 0 108.49 15.30 2 -6 0 1.60 1.60 2 -6 0 7.20 4.00 2 -6 0 3.60 4.90 -2 6 0 0.20 2.00 -2 6 0 -3.50 4.50 -2 6 0 4.30 2.10 1 -6 0 39.70 4.40 1 -6 0 44.40 6.50 1 -6 0 30.90 5.90 -1 6 0 47.00 11.70 -1 6 0 40.60 12.20 -1 6 0 48.80 4.70 0 -6 0 15.30 3.40 0 -6 0 12.10 5.20 0 -6 0 17.90 4.60 0 6 0 8.30 4.30 0 6 0 24.50 9.80 -1 -6 0 142.99 7.70 -1 -6 0 151.58 5.80 1 6 0 137.49 8.70 1 6 0 161.78 13.90 1 6 0 144.69 9.90 -2 -6 0 41.40 3.90 -2 -6 0 41.60 3.00 -2 -6 0 39.40 6.10 2 6 0 41.30 8.50 2 6 0 56.69 10.10 2 6 0 42.90 7.20 -3 -6 0 65.09 7.20 -3 -6 0 58.39 3.40 -3 -6 0 59.79 3.60 3 6 0 60.69 3.40 3 6 0 68.59 7.80 3 6 0 79.29 10.50 -4 -6 0 308.37 6.40 -4 -6 0 305.07 10.80 4 6 0 325.87 14.40 4 6 0 313.37 11.70 -5 -6 0 32.50 6.90 5 6 0 30.80 10.90 5 6 0 32.20 4.80 5 6 0 43.60 8.90 -6 -6 0 3.20 2.40 -6 -6 0 2.60 4.80 6 6 0 0.70 1.70 6 6 0 1.00 3.80 6 6 0 2.00 2.20 -7 -6 0 17.00 6.80 -7 -6 0 30.80 6.70 7 6 0 11.70 4.40 7 6 0 21.50 5.50 -8 -6 0 16.20 7.10 8 6 0 4.90 4.20 8 6 0 3.20 2.20 8 6 0 5.20 2.10 -9 -6 0 -2.90 7.60 9 6 0 -3.50 2.10 9 6 0 -2.90 4.30 9 6 0 -1.10 2.10 10 6 0 16.40 6.10 10 6 0 6.40 2.70 10 6 0 9.90 2.70 7 -7 0 5.60 6.10 7 -7 0 -1.90 3.00 7 -7 0 1.40 2.00 -7 7 0 13.10 10.00 6 -7 0 39.80 8.00 6 -7 0 15.20 3.00 -6 7 0 24.30 9.60 5 -7 0 1.20 5.20 4 -7 0 -0.90 4.50 -4 7 0 39.30 14.90 3 -7 0 409.26 11.50 3 -7 0 404.66 12.70 3 -7 0 415.66 12.90 -3 7 0 414.86 19.50 2 -7 0 -1.80 5.50 2 -7 0 -1.30 4.80 2 -7 0 -0.40 1.80 -2 7 0 -4.20 5.30 -2 7 0 1.50 2.30 -2 7 0 0.10 2.10 1 -7 0 175.98 6.60 1 -7 0 167.68 9.20 1 -7 0 176.68 9.00 -1 7 0 173.58 15.30 -1 7 0 164.78 15.70 0 -7 0 54.69 4.20 0 -7 0 57.59 6.00 0 -7 0 40.40 7.20 0 7 0 59.09 13.90 0 7 0 54.79 12.70 -1 -7 0 -1.40 5.30 -1 -7 0 3.50 3.40 1 7 0 5.80 4.80 1 7 0 1.50 1.60 1 7 0 -0.50 1.70 -2 -7 0 7.20 3.00 -2 -7 0 0.70 5.50 2 7 0 3.20 1.80 2 7 0 34.80 13.40 -3 -7 0 28.30 6.20 -3 -7 0 28.10 4.10 3 7 0 46.80 11.20 3 7 0 33.10 8.60 -4 -7 0 19.30 3.30 -4 -7 0 14.10 6.10 -4 -7 0 8.50 1.40 4 7 0 7.10 2.20 4 7 0 8.60 4.00 -5 -7 0 8.70 6.40 -5 -7 0 12.40 1.80 5 7 0 6.00 2.40 5 7 0 9.30 4.20 -6 -7 0 55.39 7.70 -6 -7 0 53.59 5.10 6 7 0 53.69 5.30 6 7 0 59.09 12.40 6 7 0 59.69 9.40 -7 -7 0 3.50 5.40 7 7 0 -0.10 4.10 7 7 0 -0.10 1.70 7 7 0 -0.90 2.20 8 7 0 5.70 4.50 8 7 0 5.70 2.00 8 7 0 1.00 2.40 -9 -7 0 -0.30 7.90 9 7 0 -3.20 4.20 9 7 0 -0.80 2.10 9 7 0 -2.70 2.50 -10 -7 0 -6.70 8.50 10 7 0 -1.00 4.70 10 7 0 -4.10 2.50 4 -8 0 91.59 8.60 4 -8 0 87.99 7.90 3 -8 0 84.49 8.20 3 -8 0 98.79 8.80 3 -8 0 91.79 6.50 -3 8 0 122.19 15.30 2 -8 0 3.10 5.70 2 -8 0 3.70 4.90 2 -8 0 0.20 1.70 -2 8 0 2.20 5.00 -2 8 0 1.40 2.30 -2 8 0 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367.06 15.20 4 6 -3 376.66 14.40 -4 -6 3 370.26 8.80 -4 -6 3 357.56 13.00 -4 -6 3 365.16 16.20 3 6 -3 83.09 10.20 3 6 -3 82.09 10.40 -3 -6 3 77.79 5.20 -3 -6 3 71.29 7.90 -3 -6 3 62.89 9.00 2 6 -3 2.90 1.10 2 6 -3 4.60 2.20 2 6 -3 8.60 4.60 -2 -6 3 4.50 3.90 -2 -6 3 11.50 6.10 -2 -6 3 10.90 3.30 1 6 -3 33.20 11.60 1 6 -3 41.70 8.10 -1 -6 3 37.50 5.80 -1 -6 3 39.80 7.50 0 6 -3 1.10 1.20 0 6 -3 -2.20 4.30 0 -6 3 2.10 4.00 0 -6 3 -0.10 5.60 -1 6 -3 168.08 14.30 -1 6 -3 183.68 10.00 -1 6 -3 171.28 7.30 1 -6 3 164.38 9.00 1 -6 3 190.78 8.40 1 -6 3 181.78 7.70 1 -6 3 173.68 9.40 -2 6 -3 0.80 1.50 -2 6 -3 2.70 7.20 2 -6 3 1.20 4.30 2 -6 3 2.00 1.90 2 -6 3 1.30 6.10 -3 6 -3 75.59 11.70 3 -6 3 75.69 6.60 3 -6 3 83.79 8.40 3 -6 3 79.09 7.70 -4 6 -3 14.40 8.10 4 -6 3 5.90 2.40 4 -6 3 17.00 5.20 4 -6 3 11.60 5.10 -5 6 -3 1.50 7.10 5 -6 3 7.40 6.10 5 -6 3 0.10 2.20 5 -6 3 -3.10 4.90 -6 6 -3 9.30 8.10 6 -6 3 3.30 2.50 6 -6 3 -0.10 4.90 -7 6 -3 30.10 12.40 7 -6 3 -0.60 5.30 10 5 -3 56.79 8.60 10 5 -3 54.69 15.20 10 5 -3 40.20 11.70 9 5 -3 255.87 11.00 9 5 -3 246.28 15.20 9 5 -3 260.27 16.50 -9 -5 3 265.77 14.30 8 5 -3 5.60 2.40 8 5 -3 3.30 3.60 8 5 -3 1.00 2.40 -8 -5 3 8.80 6.10 -8 -5 3 31.00 12.10 7 5 -3 128.99 11.80 7 5 -3 127.99 7.80 7 5 -3 137.59 12.00 -7 -5 3 131.99 9.40 -7 -5 3 142.49 8.30 -7 -5 3 148.59 14.00 6 5 -3 6.00 2.30 6 5 -3 6.30 3.20 6 5 -3 4.30 2.10 -6 -5 3 5.90 5.80 -6 -5 3 12.00 2.50 -6 -5 3 19.20 5.40 -6 -5 3 8.80 4.80 5 5 -3 1.20 2.00 5 5 -3 0.00 1.80 5 5 -3 1.10 3.20 -5 -5 3 1.10 1.90 -5 -5 3 0.00 5.30 -5 -5 3 -4.10 5.20 4 5 -3 43.30 8.70 4 5 -3 49.20 9.00 -4 -5 3 35.20 7.30 -4 -5 3 41.40 3.70 -4 -5 3 26.40 5.50 3 5 -3 4.40 3.10 3 5 -3 2.30 2.50 3 5 -3 2.20 1.90 -3 -5 3 2.40 2.40 -3 -5 3 2.00 3.90 -3 -5 3 5.40 5.00 2 5 -3 0.80 1.70 2 5 -3 0.30 0.80 2 5 -3 3.30 3.10 -2 -5 3 -1.00 3.20 -2 -5 3 2.50 4.90 -2 -5 3 2.40 2.50 1 5 -3 113.69 12.30 1 5 -3 111.59 6.70 1 5 -3 112.69 9.70 -1 -5 3 109.99 7.50 -1 -5 3 117.09 5.50 -1 -5 3 110.79 7.20 0 5 -3 4.70 3.70 0 -5 3 9.10 5.50 0 -5 3 7.10 3.20 -1 5 -3 21.70 6.60 -1 5 -3 14.90 4.90 1 -5 3 19.00 6.00 1 -5 3 19.50 4.30 -2 5 -3 54.29 9.90 -2 5 -3 42.60 9.30 2 -5 3 45.40 6.20 2 -5 3 45.20 6.00 2 -5 3 38.10 7.10 -3 5 -3 29.00 9.40 -3 5 -3 23.40 10.30 3 -5 3 23.00 4.90 3 -5 3 23.40 5.90 3 -5 3 22.50 6.90 -4 5 -3 94.49 10.80 4 -5 3 96.49 7.10 4 -5 3 101.09 7.30 4 -5 3 99.29 7.60 -5 5 -3 6.10 7.20 5 -5 3 0.50 2.20 5 -5 3 1.60 4.60 5 -5 3 4.60 4.10 -6 5 -3 4.40 7.70 6 -5 3 -5.30 4.30 6 -5 3 -0.40 2.50 -7 5 -3 39.60 12.10 7 -5 3 15.00 5.90 7 -5 3 5.70 2.70 8 -5 3 0.10 5.70 10 4 -3 0.70 2.80 10 4 -3 7.40 5.30 -10 -4 3 30.80 12.30 9 4 -3 0.10 4.40 9 4 -3 0.60 2.30 -9 -4 3 6.90 7.10 8 4 -3 1.20 4.00 8 4 -3 0.80 2.10 -8 -4 3 6.50 6.20 -8 -4 3 16.10 7.80 7 4 -3 0.80 2.00 7 4 -3 1.50 3.50 7 4 -3 1.70 2.20 -7 -4 3 5.80 6.60 -7 -4 3 2.40 5.20 -7 -4 3 4.00 4.00 6 4 -3 2.60 2.10 6 4 -3 4.00 3.10 6 4 -3 3.00 2.10 -6 -4 3 -0.60 5.30 -6 -4 3 6.80 1.80 -6 -4 3 6.20 4.50 -6 -4 3 5.20 4.90 -6 -4 3 6.70 1.80 5 4 -3 1.90 2.80 5 4 -3 2.70 1.90 5 4 -3 2.10 1.90 -5 -4 3 2.00 2.00 -5 -4 3 1.40 4.50 -5 -4 3 2.20 3.90 -5 -4 3 1.10 4.90 4 4 -3 241.28 10.40 4 4 -3 234.58 7.60 4 4 -3 254.97 7.10 4 4 -3 224.98 10.10 -4 -4 3 226.78 5.80 -4 -4 3 222.58 12.50 -4 -4 3 233.98 8.90 3 4 -3 81.89 7.70 3 4 -3 79.19 7.60 3 4 -3 83.09 4.40 -3 -4 3 73.29 3.90 -3 -4 3 76.09 6.10 -3 -4 3 74.59 7.90 2 4 -3 1199.78 25.00 2 4 -3 1233.98 21.70 2 4 -3 1231.68 24.50 -2 -4 3 1208.48 21.60 -2 -4 3 1238.68 23.90 -2 -4 3 1220.48 25.20 1 4 -3 131.19 9.60 1 4 -3 118.99 5.40 1 4 -3 115.19 8.10 -1 -4 3 124.29 5.10 -1 -4 3 114.79 6.90 -1 -4 3 120.49 6.90 0 4 -3 549.15 11.80 0 4 -3 562.44 16.70 0 4 -3 558.04 12.70 0 -4 3 553.24 12.50 0 -4 3 551.44 12.10 0 -4 3 564.64 13.50 -1 4 -3 31.90 4.00 -1 4 -3 28.10 8.50 -1 4 -3 39.20 5.40 1 -4 3 44.50 5.60 1 -4 3 33.70 6.00 1 -4 3 35.60 6.10 -2 4 -3 406.76 12.70 -2 4 -3 402.46 13.70 2 -4 3 370.96 13.90 2 -4 3 395.36 10.00 2 -4 3 420.26 10.90 2 -4 3 397.66 11.10 -3 4 -3 330.97 14.10 3 -4 3 316.47 10.10 3 -4 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4 8.30 5.80 3 -9 4 8.80 2.80 -4 9 -4 35.40 12.60 4 -9 4 8.10 2.90 4 -9 4 16.40 6.40 9 8 -4 -3.40 2.80 -8 -8 4 47.00 9.90 7 8 -4 36.50 12.20 6 8 -4 2.40 2.40 6 8 -4 -4.00 4.10 -6 -8 4 12.30 7.80 5 8 -4 0.90 2.40 5 8 -4 -3.90 4.10 -5 -8 4 10.20 6.80 -5 -8 4 0.40 2.80 4 8 -4 1.90 4.90 4 8 -4 3.60 2.30 4 8 -4 3.40 1.50 -4 -8 4 13.00 7.00 -4 -8 4 15.30 3.50 3 8 -4 6.30 2.40 3 8 -4 12.70 4.90 -3 -8 4 34.40 8.50 -3 -8 4 25.00 5.90 2 8 -4 134.79 10.10 2 8 -4 169.78 16.20 -2 -8 4 171.88 8.20 -2 -8 4 169.78 10.80 1 8 -4 96.69 15.40 -1 -8 4 86.49 6.90 -1 -8 4 91.59 9.60 0 8 -4 9.20 5.10 0 -8 4 10.10 6.90 0 -8 4 5.80 4.40 -1 8 -4 58.89 17.60 1 -8 4 31.90 9.40 1 -8 4 15.10 5.00 -2 8 -4 32.90 8.70 2 -8 4 58.99 9.80 2 -8 4 51.89 7.20 2 -8 4 34.80 7.30 -3 8 -4 -0.70 7.30 3 -8 4 0.30 4.90 3 -8 4 -0.40 2.30 3 -8 4 9.50 6.70 -4 8 -4 22.10 8.80 4 -8 4 40.60 8.50 4 -8 4 11.50 5.70 -5 8 -4 35.20 13.20 5 -8 4 2.60 5.80 9 7 -4 29.80 7.90 9 7 -4 0.80 2.90 -8 -7 4 35.00 8.70 -7 -7 4 92.39 13.50 -7 -7 4 73.69 9.40 -6 -7 4 41.50 9.10 -6 -7 4 47.50 12.50 -5 -7 4 21.10 4.30 -5 -7 4 27.00 8.90 -5 -7 4 28.20 11.20 4 7 -4 149.29 11.80 4 7 -4 135.59 13.20 -4 -7 4 166.28 12.70 -4 -7 4 159.68 6.60 -4 -7 4 154.88 10.90 3 7 -4 0.40 2.20 3 7 -4 3.60 4.40 3 7 -4 0.90 1.20 -3 -7 4 2.50 3.30 -3 -7 4 2.60 4.80 -3 -7 4 7.70 6.60 2 7 -4 577.14 18.40 2 7 -4 584.94 22.30 2 7 -4 555.04 14.90 -2 -7 4 577.64 17.00 -2 -7 4 618.44 14.20 1 7 -4 63.79 15.30 1 7 -4 59.39 7.70 -1 -7 4 62.39 6.50 -1 -7 4 66.69 10.10 0 7 -4 36.70 14.40 0 -7 4 34.20 8.10 0 -7 4 40.30 7.30 -1 7 -4 209.58 15.90 -1 7 -4 240.68 9.90 1 -7 4 200.08 8.10 1 -7 4 191.38 10.50 1 -7 4 184.98 9.10 -2 7 -4 -3.10 6.50 2 -7 4 0.70 2.10 2 -7 4 2.30 4.50 2 -7 4 4.30 5.90 -3 7 -4 12.50 7.60 3 -7 4 25.20 8.10 3 -7 4 12.70 5.30 3 -7 4 5.60 2.30 -4 7 -4 0.20 7.30 4 -7 4 9.70 5.70 4 -7 4 -0.60 5.10 4 -7 4 -1.30 2.20 -5 7 -4 10.40 8.30 5 -7 4 4.20 5.40 5 -7 4 2.20 2.50 6 -7 4 10.90 3.10 6 -7 4 15.50 6.20 10 6 -4 -7.30 4.40 10 6 -4 2.00 3.00 9 6 -4 5.00 2.70 8 6 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17.80 3 5 -4 600.24 17.70 -3 -5 4 615.94 15.90 -3 -5 4 614.14 17.80 -3 -5 4 613.74 12.90 2 5 -4 3.50 2.00 2 5 -4 6.70 3.70 -2 -5 4 3.00 3.70 -2 -5 4 5.40 3.00 -2 -5 4 3.80 5.50 1 5 -4 19.20 4.80 1 5 -4 27.30 9.70 -1 -5 4 17.90 6.40 -1 -5 4 30.70 5.40 -1 -5 4 20.00 6.80 0 5 -4 456.25 16.90 0 5 -4 404.56 12.00 0 5 -4 455.85 9.50 0 -5 4 458.45 13.30 0 -5 4 449.06 11.40 0 -5 4 444.26 11.80 -1 5 -4 153.38 6.90 -1 5 -4 172.18 7.50 -1 5 -4 148.59 12.80 -1 5 -4 157.18 9.50 1 -5 4 167.18 8.40 1 -5 4 164.18 9.50 1 -5 4 157.38 7.30 -2 5 -4 2.00 6.20 2 -5 4 0.80 1.90 2 -5 4 -1.30 4.10 2 -5 4 -1.10 5.30 -3 5 -4 18.70 6.70 3 -5 4 14.40 5.70 3 -5 4 6.80 2.20 3 -5 4 9.00 4.60 -4 5 -4 16.20 6.90 4 -5 4 9.40 2.30 4 -5 4 18.50 5.20 4 -5 4 20.00 6.30 -5 5 -4 62.99 12.00 5 -5 4 65.09 6.60 5 -5 4 46.30 7.20 5 -5 4 47.10 7.30 -6 5 -4 35.40 12.50 6 -5 4 3.10 2.70 6 -5 4 8.50 4.90 -7 5 -4 15.40 9.50 7 -5 4 -4.90 5.40 7 -5 4 -0.50 2.60 9 4 -4 44.50 8.00 9 4 -4 43.40 13.30 -9 -4 4 56.89 10.90 -8 -4 4 33.30 7.50 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30.60 5.00 1 -4 4 33.10 3.90 1 -4 4 34.30 5.80 -2 4 -4 -0.40 5.30 2 -4 4 0.80 1.80 2 -4 4 3.80 5.00 2 -4 4 -0.20 1.30 2 -4 4 3.60 3.60 -3 4 -4 2.20 6.50 3 -4 4 0.20 1.90 3 -4 4 -1.10 4.00 3 -4 4 0.10 4.80 -4 4 -4 176.58 11.80 4 -4 4 183.98 9.20 4 -4 4 178.08 8.40 4 -4 4 181.48 8.80 -5 4 -4 66.39 11.70 5 -4 4 64.49 7.00 5 -4 4 63.89 6.10 5 -4 4 59.29 7.80 -6 4 -4 37.10 11.10 6 -4 4 26.70 7.10 6 -4 4 18.60 5.10 -7 4 -4 50.89 13.10 7 -4 4 28.60 7.60 7 -4 4 21.80 5.30 8 -4 4 2.90 5.40 10 3 -4 45.90 14.50 -10 -3 4 76.39 13.90 -9 -3 4 39.30 10.40 8 3 -4 -0.50 2.10 8 3 -4 2.60 2.20 8 3 -4 3.80 3.80 -8 -3 4 15.10 7.20 -8 -3 4 11.40 6.40 7 3 -4 109.99 8.00 7 3 -4 102.39 10.60 7 3 -4 118.39 10.80 -7 -3 4 131.49 14.90 -7 -3 4 122.09 9.90 -7 -3 4 120.09 6.60 6 3 -4 10.00 3.20 6 3 -4 6.50 2.10 6 3 -4 8.00 2.30 -6 -3 4 19.40 6.60 -6 -3 4 15.70 4.70 -6 -3 4 8.60 5.80 5 3 -4 18.90 7.00 5 3 -4 35.10 8.20 -5 -3 4 20.40 6.00 -5 -3 4 12.50 5.30 -5 -3 4 19.80 5.60 -5 -3 4 24.90 3.90 -5 -3 4 23.60 3.00 4 3 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2.50 3.90 -5 3 -4 25.70 9.60 5 -3 4 28.90 5.10 5 -3 4 22.10 6.10 -6 3 -4 182.98 13.90 6 -3 4 161.98 9.00 6 -3 4 176.18 9.70 -7 3 -4 15.20 9.40 7 -3 4 5.80 4.80 7 -3 4 3.70 2.10 7 -3 4 3.70 2.50 8 -3 4 16.80 5.30 8 -3 4 10.30 3.00 8 -3 4 7.30 2.40 9 -3 4 -0.70 2.80 10 2 -4 71.49 14.20 -10 -2 4 82.49 14.70 -10 -2 4 113.99 15.50 9 2 -4 50.59 12.00 -9 -2 4 67.19 14.40 -9 -2 4 46.20 11.50 8 2 -4 36.60 10.40 -8 -2 4 40.10 10.30 -8 -2 4 44.00 11.80 7 2 -4 59.99 9.40 7 2 -4 55.79 7.40 7 2 -4 52.39 9.50 -7 -2 4 60.19 5.00 -7 -2 4 68.19 13.60 -7 -2 4 62.59 9.00 6 2 -4 -0.60 2.70 6 2 -4 3.40 2.00 6 2 -4 1.50 2.10 -6 -2 4 -1.60 5.10 -6 -2 4 4.10 3.90 -6 -2 4 -3.40 6.00 5 2 -4 73.29 6.00 5 2 -4 73.39 7.70 5 2 -4 69.79 7.70 -5 -2 4 71.89 3.20 -5 -2 4 68.59 5.60 -5 -2 4 65.79 6.90 -5 -2 4 67.29 10.20 4 2 -4 14.20 5.30 -4 -2 4 7.40 4.10 -4 -2 4 13.90 4.20 -4 -2 4 14.40 2.80 -4 -2 4 16.10 4.40 3 2 -4 190.48 6.40 3 2 -4 201.38 8.80 3 2 -4 189.58 6.90 -3 -2 4 196.38 7.50 -3 -2 4 183.88 5.30 -3 -2 4 185.38 5.60 -3 -2 4 185.38 10.60 2 2 -4 275.57 7.80 2 2 -4 280.97 9.10 2 2 -4 270.17 8.70 -2 -2 4 284.27 8.50 -2 -2 4 276.47 7.30 -2 -2 4 268.67 10.10 1 2 -4 1503.25 27.00 1 2 -4 1495.75 27.30 1 2 -4 1473.75 30.30 -1 -2 4 1480.35 27.60 -1 -2 4 1487.25 28.20 -1 -2 4 1490.35 27.10 0 2 -4 862.81 15.90 0 2 -4 875.71 17.50 0 2 -4 865.61 17.70 0 -2 4 839.62 18.10 0 -2 4 879.51 17.40 0 -2 4 851.91 16.20 0 -2 4 859.21 17.40 -1 2 -4 415.06 10.60 -1 2 -4 423.86 9.60 1 -2 4 413.66 9.80 1 -2 4 418.96 9.70 1 -2 4 425.46 12.70 1 -2 4 430.56 10.80 1 -2 4 409.96 9.50 -2 2 -4 10.70 4.50 2 -2 4 10.00 3.90 2 -2 4 9.00 3.40 2 -2 4 10.40 3.20 2 -2 4 14.40 5.30 -3 2 -4 225.18 10.20 3 -2 4 231.58 5.00 3 -2 4 241.28 7.70 3 -2 4 238.98 8.10 3 -2 4 225.38 7.40 3 -2 4 233.88 5.40 -4 2 -4 10.10 6.20 4 -2 4 11.00 2.10 4 -2 4 13.90 4.70 4 -2 4 6.80 3.80 4 -2 4 5.10 1.90 4 -2 4 9.40 2.30 -5 2 -4 43.90 11.90 5 -2 4 51.59 4.90 5 -2 4 54.49 7.30 5 -2 4 49.20 2.80 5 -2 4 49.90 4.90 5 -2 4 45.00 6.90 -6 2 -4 9.60 7.70 6 -2 4 1.00 2.10 6 -2 4 0.50 3.60 -7 2 -4 48.10 12.20 7 -2 4 18.70 4.70 7 -2 4 29.50 6.80 7 -2 4 33.90 8.70 -8 2 -4 47.50 15.50 8 -2 4 4.10 2.80 8 -2 4 1.80 4.50 -9 2 -4 37.70 14.50 9 -2 4 0.40 2.30 9 -2 4 -7.30 4.60 -10 -1 4 52.39 13.90 -9 -1 4 43.80 12.00 -9 -1 4 54.89 13.20 8 1 -4 208.78 12.60 8 1 -4 221.88 10.00 -8 -1 4 246.58 14.30 -8 -1 4 268.17 16.40 7 1 -4 212.38 11.70 7 1 -4 201.28 9.00 -7 -1 4 206.98 6.30 -7 -1 4 231.78 14.40 -7 -1 4 206.08 12.20 6 1 -4 167.58 8.20 6 1 -4 167.08 10.30 -6 -1 4 155.28 12.70 -6 -1 4 161.28 6.40 -6 -1 4 150.78 10.20 5 1 -4 189.68 7.60 5 1 -4 189.78 9.20 -5 -1 4 184.68 6.80 -5 -1 4 176.48 11.30 -5 -1 4 181.78 8.90 4 1 -4 100.09 5.60 4 1 -4 98.69 6.90 -4 -1 4 92.09 9.60 -4 -1 4 95.99 3.80 -4 -1 4 93.49 5.90 -4 -1 4 96.39 5.50 3 1 -4 81.89 5.00 3 1 -4 76.69 4.70 3 1 -4 77.59 4.60 3 1 -4 86.09 5.90 -3 -1 4 80.99 3.80 -3 -1 4 82.09 5.40 -3 -1 4 76.09 4.60 -3 -1 4 68.29 8.30 -3 -1 4 73.49 7.80 2 1 -4 1.20 1.10 2 1 -4 1.00 1.00 2 1 -4 1.10 1.20 2 1 -4 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5 34.80 12.60 3 8 -5 5.80 5.20 -3 -8 5 21.30 7.50 -3 -8 5 16.20 4.20 2 8 -5 91.79 13.20 -2 -8 5 104.59 11.30 -2 -8 5 96.59 7.00 1 8 -5 53.29 14.20 -1 -8 5 27.60 6.40 -1 -8 5 41.50 9.20 0 8 -5 38.20 15.20 0 -8 5 2.60 4.90 0 -8 5 6.20 7.70 -1 8 -5 69.99 10.70 1 -8 5 88.29 10.80 1 -8 5 86.29 8.10 1 -8 5 90.39 7.80 -2 8 -5 91.49 10.70 2 -8 5 100.79 10.70 2 -8 5 79.59 8.40 2 -8 5 86.49 8.20 -3 8 -5 30.30 10.80 3 -8 5 9.30 2.80 3 -8 5 14.20 5.90 3 -8 5 34.50 9.20 -4 8 -5 188.58 15.00 4 -8 5 167.98 10.80 4 -8 5 171.08 10.00 4 -8 5 194.58 11.60 5 -8 5 50.39 9.90 5 -8 5 49.40 10.40 9 7 -5 2.10 2.80 -8 -7 5 12.50 6.70 -7 -7 5 7.70 6.60 -7 -7 5 42.60 15.20 6 7 -5 74.09 12.60 -6 -7 5 112.89 14.10 -6 -7 5 104.79 9.40 5 7 -5 116.59 11.60 5 7 -5 99.29 12.10 -5 -7 5 141.89 10.90 -5 -7 5 146.49 15.30 -5 -7 5 133.89 6.20 4 7 -5 34.60 10.00 -4 -7 5 56.29 12.90 -4 -7 5 41.00 9.40 -4 -7 5 37.30 5.10 3 7 -5 372.36 16.10 3 7 -5 374.36 17.50 3 7 -5 371.06 11.70 -3 -7 5 422.76 16.70 -3 -7 5 405.86 11.20 -3 -7 5 398.76 14.30 2 7 -5 3.60 4.80 -2 -7 5 8.10 4.30 -2 -7 5 8.70 6.90 -2 -7 5 5.50 3.60 1 7 -5 132.69 14.40 -1 -7 5 123.49 8.00 -1 -7 5 120.49 10.80 0 7 -5 80.69 14.20 0 7 -5 40.40 8.40 0 -7 5 61.79 8.60 0 -7 5 60.99 7.70 -1 7 -5 23.00 6.70 1 -7 5 23.90 5.70 1 -7 5 20.10 5.00 1 -7 5 31.80 8.00 -2 7 -5 42.40 9.30 2 -7 5 36.30 8.00 2 -7 5 42.70 8.30 2 -7 5 39.10 6.50 -3 7 -5 10.20 7.00 3 -7 5 7.60 2.40 3 -7 5 6.90 5.10 3 -7 5 15.50 6.60 -4 7 -5 36.80 9.80 4 -7 5 28.40 7.30 4 -7 5 34.10 7.80 4 -7 5 55.09 8.70 -5 7 -5 16.60 9.00 5 -7 5 0.20 2.80 5 -7 5 -8.70 5.00 6 -7 5 -1.70 5.70 9 6 -5 82.39 9.30 9 6 -5 48.50 12.10 -8 -6 5 59.99 16.10 -8 -6 5 24.40 8.10 -7 -6 5 35.70 8.10 -7 -6 5 61.19 13.80 6 6 -5 37.60 9.70 -6 -6 5 55.89 12.50 -6 -6 5 53.89 8.60 -6 -6 5 47.40 4.50 5 6 -5 388.96 15.80 5 6 -5 420.16 15.80 -5 -6 5 434.76 14.70 -5 -6 5 448.66 10.50 -5 -6 5 460.75 18.70 4 6 -5 105.79 11.10 4 6 -5 97.29 11.60 -4 -6 5 103.29 12.20 -4 -6 5 95.39 9.00 -4 -6 5 107.49 6.20 3 6 -5 259.17 10.20 3 6 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15.50 9.40 6 -3 7 -1.40 2.40 6 -3 7 3.20 4.60 -7 3 -7 54.79 13.40 7 -3 7 9.60 5.10 8 -3 7 -3.80 5.00 8 -3 7 0.20 2.50 8 -3 7 -1.00 3.10 -9 -2 7 80.69 16.90 8 2 -7 2.60 4.50 -8 -2 7 43.50 13.60 7 2 -7 -1.70 2.50 7 2 -7 -0.40 2.40 -7 -2 7 18.00 7.30 -7 -2 7 7.70 7.10 -7 -2 7 3.70 5.00 6 2 -7 1.50 2.20 6 2 -7 -1.30 2.10 6 2 -7 -0.40 1.90 -6 -2 7 -0.60 5.40 -6 -2 7 -0.40 5.00 -6 -2 7 5.40 3.80 5 2 -7 75.39 6.70 5 2 -7 79.69 8.40 5 2 -7 85.39 10.30 -5 -2 7 79.29 8.20 -5 -2 7 82.49 5.70 -5 -2 7 74.59 12.30 4 2 -7 67.09 9.50 4 2 -7 58.69 5.90 -4 -2 7 60.29 3.40 -4 -2 7 62.59 11.40 -4 -2 7 63.99 8.00 3 2 -7 -0.30 1.70 3 2 -7 -1.10 1.80 3 2 -7 0.70 1.80 -3 -2 7 -4.10 4.60 -3 -2 7 0.80 5.30 2 2 -7 98.29 7.50 2 2 -7 97.79 8.40 2 2 -7 123.59 5.60 -2 -2 7 111.59 9.70 -2 -2 7 126.29 8.20 -2 -2 7 110.09 4.60 -1 -2 7 74.39 7.30 -1 -2 7 71.79 9.30 -1 -2 7 68.69 5.80 0 2 -7 1.20 2.40 0 -2 7 1.50 3.20 0 -2 7 0.60 2.50 0 -2 7 4.30 3.70 0 -2 7 9.00 5.30 -1 2 -7 165.48 7.60 1 -2 7 176.08 7.50 1 -2 7 168.88 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1 -5 -17 -2.80 6.30 -1 5 17 -13.40 7.60 -1 5 17 -1.00 9.10 0 -5 -17 52.19 10.50 0 5 17 65.49 13.90 -1 -5 -17 19.10 7.40 1 5 17 3.70 8.40 1 5 17 22.40 10.60 -2 -5 -17 19.40 7.60 2 5 17 26.10 10.10 2 5 17 1.70 8.70 -3 -5 -17 62.79 11.30 3 5 17 76.79 13.20 3 5 17 39.00 15.10 1 -6 -17 108.49 12.90 -1 6 17 80.39 20.10 -1 6 17 126.29 13.20 0 -6 -17 14.40 7.30 0 6 17 18.80 10.00 0 6 17 4.90 8.70 -1 -6 -17 9.80 7.60 1 6 17 19.40 9.80 1 6 17 -1.10 8.90 -2 -6 -17 181.48 13.50 2 6 17 146.59 20.30 2 6 17 197.18 14.00 0 -7 -17 11.70 7.30 0 7 17 -3.90 8.50 0 7 17 28.20 9.50 -1 -7 -17 -3.70 7.20 1 7 17 9.80 9.20 1 7 17 -10.50 7.70 -2 -7 -17 -3.30 7.00 2 7 17 -7.80 7.70 2 7 17 13.30 8.70 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 3199