data_shelx _audit_creation_method 'SHELXL-2017/1' _shelx_SHELXL_version_number '2017/1' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H34 Br2 N4 O3' _chemical_formula_weight 730.49 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' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _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+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.6753(18) _cell_length_b 9.5139(12) _cell_length_c 26.448(4) _cell_angle_alpha 90 _cell_angle_beta 97.271(4) _cell_angle_gamma 90 _cell_volume 3413.4(8) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 2345 _cell_measurement_theta_min 2.018 _cell_measurement_theta_max 27.110 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.421 _exptl_crystal_F_000 1488 _exptl_transmission_factor_min 0.6042 _exptl_transmission_factor_max 0.7071 _exptl_crystal_size_max 0.140 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.040 _exptl_absorpt_coefficient_mu 2.415 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details SADABAS _exptl_absorpt_special_details ? _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'fine-focus sealed tube' _diffrn_measurement_device_type CCD _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 49611 _diffrn_reflns_av_unetI/netI 0.0997 _diffrn_reflns_av_R_equivalents 0.1199 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.018 _diffrn_reflns_theta_max 27.110 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 7514 _reflns_number_gt 2356 _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 ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0782P)^2^+0.8786P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 7514 _refine_ls_number_parameters 432 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2351 _refine_ls_R_factor_gt 0.0675 _refine_ls_wR_factor_ref 0.2194 _refine_ls_wR_factor_gt 0.1484 _refine_ls_goodness_of_fit_ref 0.989 _refine_ls_restrained_S_all 0.989 _refine_ls_shift/su_max 0.003 _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 Br1 Br 0.0607(3) -0.1525(5) 0.7906(3) 0.1249(11) Uani 0.5 1 d . . P A 1 Br2 Br -0.0365(3) 0.3506(6) 0.90559(19) 0.164(2) Uani 0.5 1 d . . P B 1 O3 O 0.2367(3) 0.6528(4) 0.55574(14) 0.0828(11) Uani 1 1 d . . . . . O2 O 0.5731(4) 0.5885(7) 0.7434(2) 0.189(3) Uani 1 1 d . . . . . C34 C -0.0695(9) 0.260(2) 0.5596(5) 0.411(14) Uani 1 1 d . . . C 1 H34A H -0.078710 0.176315 0.578867 0.617 Uiso 1 1 calc R U . C 1 H34B H -0.119955 0.265193 0.530961 0.617 Uiso 1 1 calc R U . C 1 H34C H -0.073347 0.340846 0.580929 0.617 Uiso 1 1 calc R U . C 1 N2 N 0.4416(4) 0.6150(5) 0.68106(19) 0.0859(14) Uani 1 1 d . . . . . N3 N 0.0828(4) 0.2222(7) 0.5856(3) 0.111(2) Uani 1 1 d . . . . . C20 C 0.3231(4) 0.3600(5) 0.63880(18) 0.0666(14) Uani 1 1 d . . . . . H20 H 0.377669 0.331992 0.661110 0.080 Uiso 1 1 calc R U . . . N4 N 0.3528(5) 1.1027(6) 0.5187(2) 0.0971(18) Uani 1 1 d . . . . . C19 C 0.3255(4) 0.4913(5) 0.61592(18) 0.0608(12) Uani 1 1 d . . . . . C18 C 0.4145(4) 0.5859(5) 0.6260(2) 0.0661(13) Uani 1 1 d . . . . . C21 C 0.2446(4) 0.2696(5) 0.63028(19) 0.0681(14) Uani 1 1 d . . . . . C25 C 0.2434(4) 0.5278(5) 0.5828(2) 0.0647(13) Uani 1 1 d . . . . . C26 C 0.3986(4) 0.7213(5) 0.59658(19) 0.0642(13) Uani 1 1 d . . . . . O1 O 0.1199(4) 0.4597(5) 0.84924(19) 0.153(2) Uani 1 1 d . . . . . H1 H 0.079549 0.486040 0.867638 0.229 Uiso 1 1 calc R U . . . C28 C 0.4563(5) 0.9542(6) 0.5768(2) 0.0772(15) Uani 1 1 d . . . . . C31 C 0.3129(4) 0.7482(5) 0.5647(2) 0.0680(14) Uani 1 1 d . . . . . C23 C 0.1615(4) 0.3120(6) 0.5961(2) 0.0749(15) Uani 1 1 d . . . . . C27 C 0.4683(4) 0.8270(5) 0.60136(19) 0.0730(14) Uani 1 1 d . . . . . H27 H 0.526929 0.811030 0.622490 0.088 Uiso 1 1 calc R U . . . C29 C 0.3679(5) 0.9773(6) 0.5439(2) 0.0800(16) Uani 1 1 d . . . . . C30 C 0.2966(4) 0.8737(6) 0.5383(2) 0.0795(15) Uani 1 1 d . . . . . H30 H 0.237997 0.888083 0.517021 0.095 Uiso 1 1 calc R U . . . C17 C 0.5065(5) 0.5094(6) 0.6145(3) 0.0816(16) Uani 1 1 d . . . . . C24 C 0.1634(4) 0.4416(6) 0.5731(2) 0.0788(16) Uani 1 1 d . . . . . H24 H 0.109420 0.470911 0.550629 0.095 Uiso 1 1 calc R U . . . N1 N 0.2623(4) 0.4602(6) 0.7964(2) 0.1148(18) Uani 1 1 d . . . . . C22 C 0.2482(4) 0.1259(5) 0.6544(2) 0.0918(18) Uani 1 1 d . . . . . H22A H 0.252535 0.055606 0.628764 0.138 Uiso 1 1 calc R U . . . H22B H 0.189586 0.110962 0.670190 0.138 Uiso 1 1 calc R U . . . H22C H 0.304928 0.119491 0.679765 0.138 Uiso 1 1 calc R U . . . C1 C 0.1604(5) 0.2584(8) 0.8041(2) 0.0878(17) Uani 1 1 d . . . . . C7 C 0.2421(5) 0.3336(7) 0.7853(2) 0.0970(19) Uani 1 1 d . . . . . H7 H 0.280702 0.285998 0.764326 0.116 Uiso 1 1 calc R U . . . C9 C 0.3016(5) 0.6289(6) 0.7335(2) 0.106(2) Uani 1 1 d . . . . . H9A H 0.261867 0.698166 0.748460 0.127 Uiso 1 1 calc R U . . . H9B H 0.258882 0.579104 0.707320 0.127 Uiso 1 1 calc R U . . . C6 C 0.1421(5) 0.1227(8) 0.7904(2) 0.104(2) Uani 1 1 d . . . . . H6 H 0.181881 0.078931 0.769054 0.124 Uiso 1 1 calc R U . . . C12 C 0.5724(6) 0.4994(9) 0.6575(5) 0.122(3) Uani 1 1 d . . . . . C16 C 0.5269(5) 0.4544(6) 0.5687(3) 0.115(2) Uani 1 1 d . . . . . H16 H 0.480997 0.460870 0.539734 0.138 Uiso 1 1 calc R U . . . C32 C 0.5353(5) 1.0657(6) 0.5833(2) 0.103(2) Uani 1 1 d . . . . . H32A H 0.582499 1.043148 0.612250 0.155 Uiso 1 1 calc R U . . . H32B H 0.505931 1.155252 0.588669 0.155 Uiso 1 1 calc R U . . . H32C H 0.567901 1.069701 0.553277 0.155 Uiso 1 1 calc R U . . . C4 C 0.0066(5) 0.1126(9) 0.8375(3) 0.113(2) Uani 1 1 d . . . . . H4A H -0.045787 0.063328 0.848235 0.135 Uiso 1 1 calc R U . . . C35 C 0.2647(5) 1.1371(6) 0.4852(3) 0.107(2) Uani 1 1 d . . . . . H35A H 0.208802 1.137069 0.504460 0.129 Uiso 1 1 calc R U . . . H35B H 0.253079 1.065839 0.458902 0.129 Uiso 1 1 calc R U . . . C2 C 0.1019(5) 0.3251(7) 0.8358(3) 0.105(2) Uani 1 1 d . . . . . C11 C 0.5340(7) 0.5686(9) 0.6999(4) 0.119(3) Uani 1 1 d . . . . . C10 C 0.3827(5) 0.7050(7) 0.7086(2) 0.111(2) Uani 1 1 d . . . . . H10A H 0.352055 0.775809 0.685358 0.133 Uiso 1 1 calc R U . . . H10B H 0.425800 0.753256 0.734971 0.133 Uiso 1 1 calc R U . . . C3 C 0.0235(5) 0.2498(9) 0.8523(3) 0.114(2) Uani 1 1 d . . . . . C5 C 0.0668(6) 0.0485(8) 0.8071(3) 0.108(2) Uani 1 1 d . . . . . C8 C 0.3419(5) 0.5277(8) 0.7734(3) 0.128(3) Uani 1 1 d . . . . . H8A H 0.380346 0.456743 0.758475 0.153 Uiso 1 1 calc R U . . . H8B H 0.385173 0.576661 0.799512 0.153 Uiso 1 1 calc R U . . . C13 C 0.6643(10) 0.4257(14) 0.6572(7) 0.193(8) Uani 1 1 d . . . . . H13 H 0.708256 0.410668 0.686480 0.231 Uiso 1 1 calc R U . . . C36 C 0.2727(5) 1.2790(7) 0.4607(3) 0.133(3) Uani 1 1 d . . . . . H36A H 0.212993 1.298751 0.438663 0.199 Uiso 1 1 calc R U . . . H36B H 0.283051 1.349878 0.486652 0.199 Uiso 1 1 calc R U . . . H36C H 0.327285 1.278717 0.441139 0.199 Uiso 1 1 calc R U . . . C33 C -0.0016(6) 0.2567(10) 0.5470(5) 0.183(5) Uani 1 1 d . . . C 1 C15 C 0.6193(9) 0.3877(9) 0.5667(6) 0.174(5) Uani 1 1 d . . . . . H15 H 0.637452 0.350310 0.536731 0.208 Uiso 1 1 calc R U . . . C14 C 0.6807(15) 0.3825(17) 0.6129(9) 0.223(12) Uani 1 1 d . . . . . H14 H 0.742237 0.342077 0.611515 0.268 Uiso 1 1 calc R U . . . Br1A Br 0.0210(4) -0.1251(6) 0.7879(3) 0.188(2) Uani 0.5 1 d . . P A 2 Br2A Br -0.0779(3) 0.3266(5) 0.8829(2) 0.1559(18) Uani 0.5 1 d . . P B 2 H3 H 0.081(4) 0.157(5) 0.604(2) 0.07(2) Uiso 1 1 d . . . . . H4 H 0.397(4) 1.155(5) 0.525(2) 0.08(2) 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 Br1 0.114(2) 0.1036(13) 0.156(2) -0.0380(12) 0.0112(17) -0.0071(14) Br2 0.176(4) 0.155(3) 0.187(4) 0.053(3) 0.119(3) 0.045(3) O3 0.077(3) 0.078(2) 0.090(3) 0.014(2) -0.001(2) -0.002(2) O2 0.177(5) 0.244(7) 0.122(5) 0.071(4) -0.077(4) -0.122(5) C34 0.134(11) 0.91(4) 0.179(12) 0.16(2) -0.037(10) 0.046(18) N2 0.097(4) 0.088(3) 0.071(4) 0.004(3) 0.005(3) -0.026(3) N3 0.090(5) 0.104(5) 0.132(5) 0.019(4) -0.011(4) -0.029(4) C20 0.065(3) 0.072(4) 0.063(3) 0.003(3) 0.007(3) -0.010(3) N4 0.117(5) 0.078(4) 0.096(4) 0.007(3) 0.009(4) -0.008(4) C19 0.066(3) 0.064(3) 0.053(3) -0.005(3) 0.012(3) -0.009(3) C18 0.069(4) 0.068(3) 0.063(4) 0.001(3) 0.013(3) -0.005(3) C21 0.075(4) 0.069(3) 0.062(4) -0.001(3) 0.015(3) -0.004(3) C25 0.066(4) 0.068(3) 0.061(3) 0.002(3) 0.011(3) 0.002(3) C26 0.078(4) 0.058(3) 0.058(3) 0.002(3) 0.017(3) 0.000(3) O1 0.228(6) 0.096(4) 0.157(4) 0.003(3) 0.116(4) 0.006(4) C28 0.106(5) 0.064(4) 0.065(4) -0.007(3) 0.021(4) -0.013(3) C31 0.081(4) 0.064(4) 0.061(4) -0.002(3) 0.021(3) -0.002(3) C23 0.068(4) 0.082(4) 0.075(4) -0.008(3) 0.007(3) -0.015(3) C27 0.090(4) 0.064(4) 0.067(4) 0.002(3) 0.017(3) -0.005(3) C29 0.112(5) 0.062(4) 0.070(4) 0.006(3) 0.027(4) 0.008(4) C30 0.089(4) 0.072(4) 0.079(4) 0.006(3) 0.014(3) 0.007(3) C17 0.073(4) 0.068(4) 0.108(5) 0.023(4) 0.024(4) -0.006(3) C24 0.067(4) 0.078(4) 0.088(4) 0.007(3) -0.003(3) -0.007(3) N1 0.151(5) 0.113(4) 0.088(4) 0.010(4) 0.042(3) -0.023(4) C22 0.106(5) 0.083(4) 0.084(4) 0.000(3) 0.005(3) -0.026(3) C1 0.100(5) 0.097(5) 0.070(4) 0.014(4) 0.027(4) 0.009(4) C7 0.107(5) 0.112(5) 0.075(4) 0.019(4) 0.025(4) 0.011(4) C9 0.156(6) 0.095(5) 0.073(4) -0.008(4) 0.038(4) -0.017(4) C6 0.118(6) 0.118(6) 0.075(5) -0.005(4) 0.016(4) -0.003(5) C12 0.070(6) 0.106(6) 0.188(10) 0.062(6) 0.009(6) -0.025(4) C16 0.119(6) 0.074(4) 0.168(7) 0.009(4) 0.081(5) -0.003(4) C32 0.129(5) 0.079(4) 0.104(5) 0.008(3) 0.019(4) -0.028(4) C4 0.098(5) 0.115(6) 0.125(6) 0.041(5) 0.011(5) 0.013(5) C35 0.130(6) 0.079(4) 0.114(5) 0.024(4) 0.023(5) 0.007(4) C2 0.131(6) 0.088(5) 0.103(5) 0.028(4) 0.041(5) 0.012(5) C11 0.104(7) 0.134(7) 0.107(7) 0.051(6) -0.029(6) -0.062(5) C10 0.170(7) 0.097(5) 0.067(4) -0.006(4) 0.020(4) -0.042(5) C3 0.117(6) 0.110(6) 0.126(6) 0.045(5) 0.056(5) 0.042(5) C5 0.113(6) 0.120(6) 0.091(5) 0.000(4) 0.005(4) -0.019(5) C8 0.146(6) 0.153(6) 0.085(5) 0.029(5) 0.017(5) -0.050(5) C13 0.078(8) 0.147(11) 0.35(2) 0.129(13) 0.016(10) -0.012(7) C36 0.155(6) 0.096(5) 0.147(6) 0.034(5) 0.017(5) 0.009(4) C33 0.057(5) 0.174(8) 0.304(14) 0.055(8) -0.029(7) -0.049(5) C15 0.177(11) 0.073(5) 0.305(17) -0.002(8) 0.168(11) -0.005(7) C14 0.120(11) 0.121(10) 0.44(4) 0.101(16) 0.086(16) -0.018(8) Br1A 0.223(6) 0.202(5) 0.139(2) -0.032(3) 0.020(4) -0.102(4) Br2A 0.150(3) 0.1050(15) 0.234(5) 0.013(2) 0.107(3) 0.0301(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 C5 1.961(9) . ? Br2 C3 1.968(9) . ? O3 C31 1.379(6) . ? O3 C25 1.385(5) . ? O2 C11 1.219(8) . ? C34 C33 1.026(14) . ? N2 C11 1.371(9) . ? N2 C10 1.435(7) . ? N2 C18 1.483(6) . ? N3 C23 1.375(7) . ? N3 C33 1.478(10) . ? C20 C21 1.372(6) . ? C20 C19 1.390(6) . ? N4 C29 1.370(7) . ? N4 C35 1.440(8) . ? C19 C25 1.379(6) . ? C19 C18 1.510(6) . ? C18 C26 1.506(7) . ? C18 C17 1.518(7) . ? C21 C23 1.419(7) . ? C21 C22 1.508(7) . ? C25 C24 1.364(6) . ? C26 C31 1.377(6) . ? C26 C27 1.380(6) . ? O1 C2 1.343(7) . ? C28 C27 1.374(7) . ? C28 C29 1.414(7) . ? C28 C32 1.508(7) . ? C31 C30 1.387(7) . ? C23 C24 1.376(7) . ? C29 C30 1.381(7) . ? C17 C12 1.361(9) . ? C17 C16 1.379(9) . ? N1 C7 1.262(7) . ? N1 C8 1.462(8) . ? C1 C6 1.356(8) . ? C1 C2 1.385(8) . ? C1 C7 1.465(8) . ? C9 C8 1.483(8) . ? C9 C10 1.541(8) . ? C6 C5 1.367(8) . ? C12 C13 1.441(15) . ? C12 C11 1.456(10) . ? C16 C15 1.421(11) . ? C4 C5 1.366(9) . ? C4 C3 1.374(9) . ? C35 C36 1.508(7) . ? C2 C3 1.404(9) . ? C3 Br2A 1.842(8) . ? C5 Br1A 1.816(9) . ? C13 C14 1.29(2) . ? C15 C14 1.39(2) . ? 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 C31 O3 C25 118.5(4) . . ? C11 N2 C10 123.9(7) . . ? C11 N2 C18 113.7(6) . . ? C10 N2 C18 121.5(5) . . ? C23 N3 C33 121.6(6) . . ? C21 C20 C19 123.6(5) . . ? C29 N4 C35 124.0(6) . . ? C25 C19 C20 116.2(4) . . ? C25 C19 C18 122.3(5) . . ? C20 C19 C18 121.4(5) . . ? N2 C18 C26 110.4(4) . . ? N2 C18 C19 112.3(4) . . ? C26 C18 C19 111.0(4) . . ? N2 C18 C17 100.1(5) . . ? C26 C18 C17 112.1(4) . . ? C19 C18 C17 110.5(4) . . ? C20 C21 C23 118.3(5) . . ? C20 C21 C22 121.1(5) . . ? C23 C21 C22 120.6(5) . . ? C24 C25 C19 122.4(5) . . ? C24 C25 O3 114.9(5) . . ? C19 C25 O3 122.7(5) . . ? C31 C26 C27 116.5(5) . . ? C31 C26 C18 122.0(5) . . ? C27 C26 C18 121.5(5) . . ? C27 C28 C29 118.0(5) . . ? C27 C28 C32 121.6(6) . . ? C29 C28 C32 120.4(5) . . ? O3 C31 C26 123.3(5) . . ? O3 C31 C30 114.2(5) . . ? C26 C31 C30 122.5(5) . . ? N3 C23 C24 121.8(6) . . ? N3 C23 C21 119.7(6) . . ? C24 C23 C21 118.5(5) . . ? C28 C27 C26 124.0(5) . . ? N4 C29 C30 120.6(7) . . ? N4 C29 C28 119.9(6) . . ? C30 C29 C28 119.5(5) . . ? C29 C30 C31 119.7(6) . . ? C12 C17 C16 121.4(8) . . ? C12 C17 C18 110.1(7) . . ? C16 C17 C18 128.5(7) . . ? C25 C24 C23 121.0(5) . . ? C7 N1 C8 118.4(6) . . ? C6 C1 C2 119.8(6) . . ? C6 C1 C7 119.8(7) . . ? C2 C1 C7 120.4(7) . . ? N1 C7 C1 122.7(6) . . ? C8 C9 C10 112.7(6) . . ? C1 C6 C5 121.8(7) . . ? C17 C12 C13 120.9(12) . . ? C17 C12 C11 110.3(8) . . ? C13 C12 C11 128.7(12) . . ? C17 C16 C15 118.9(9) . . ? C5 C4 C3 120.0(7) . . ? N4 C35 C36 111.5(6) . . ? O1 C2 C1 119.7(7) . . ? O1 C2 C3 121.8(7) . . ? C1 C2 C3 118.5(7) . . ? O2 C11 N2 124.6(11) . . ? O2 C11 C12 129.7(11) . . ? N2 C11 C12 105.7(7) . . ? N2 C10 C9 114.6(5) . . ? C4 C3 C2 120.3(7) . . ? C4 C3 Br2A 113.1(7) . . ? C2 C3 Br2A 125.5(7) . . ? C4 C3 Br2 126.6(6) . . ? C2 C3 Br2 112.2(6) . . ? C4 C5 C6 119.7(7) . . ? C4 C5 Br1A 111.0(7) . . ? C6 C5 Br1A 128.8(7) . . ? C4 C5 Br1 123.7(7) . . ? C6 C5 Br1 116.4(7) . . ? N1 C8 C9 110.7(6) . . ? C14 C13 C12 114(2) . . ? C34 C33 N3 116.2(14) . . ? C14 C15 C16 115.0(14) . . ? C13 C14 C15 129(2) . . ? _refine_diff_density_max 0.363 _refine_diff_density_min -0.288 _refine_diff_density_rms 0.047 _shelx_res_file ; TITL AS_SC2L_0m_a.res in P2(1)/c shelx.res created by SHELXL-2017/1 at 20:24:21 on 20-Aug-2019 CELL 0.71073 13.6753 9.5139 26.4482 90.000 97.271 90.000 ZERR 4.00 0.0018 0.0012 0.0035 0.000 0.004 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O BR UNIT 144 136 16 12 8 MERG 2 FMAP 2 PLAN 20 ACTA L.S. 10 TEMP 0.00 WGHT 0.078200 0.878600 FVAR 0.37356 PART 1 BR1 5 0.060728 -0.152493 0.790592 10.50000 0.11396 0.10358 = 0.15581 -0.03801 0.01124 -0.00711 BR2 5 -0.036477 0.350605 0.905595 10.50000 0.17591 0.15486 = 0.18704 0.05342 0.11853 0.04473 PART 0 O3 4 0.236683 0.652840 0.555745 11.00000 0.07749 0.07755 = 0.09035 0.01360 -0.00089 -0.00206 O2 4 0.573131 0.588541 0.743371 11.00000 0.17668 0.24356 = 0.12174 0.07148 -0.07716 -0.12168 PART 1 C34 1 -0.069503 0.259810 0.559643 11.00000 0.13356 0.90646 = 0.17930 0.15937 -0.03706 0.04640 AFIX 133 H34A 2 -0.078710 0.176315 0.578867 11.00000 -1.50000 H34B 2 -0.119955 0.265193 0.530961 11.00000 -1.50000 H34C 2 -0.073347 0.340846 0.580929 11.00000 -1.50000 AFIX 0 PART 0 N2 3 0.441584 0.614960 0.681056 11.00000 0.09715 0.08841 = 0.07067 0.00409 0.00515 -0.02597 N3 3 0.082770 0.222151 0.585600 11.00000 0.09023 0.10404 = 0.13160 0.01935 -0.01079 -0.02871 C20 1 0.323088 0.360032 0.638803 11.00000 0.06482 0.07164 = 0.06297 0.00298 0.00651 -0.00966 AFIX 43 H20 2 0.377669 0.331992 0.661110 11.00000 -1.20000 AFIX 0 N4 3 0.352831 1.102747 0.518712 11.00000 0.11670 0.07779 = 0.09559 0.00710 0.00856 -0.00753 C19 1 0.325469 0.491255 0.615919 11.00000 0.06596 0.06401 = 0.05339 -0.00450 0.01159 -0.00904 C18 1 0.414470 0.585906 0.625979 11.00000 0.06854 0.06755 = 0.06331 0.00121 0.01261 -0.00474 C21 1 0.244616 0.269623 0.630277 11.00000 0.07495 0.06861 = 0.06235 -0.00061 0.01477 -0.00421 C25 1 0.243364 0.527815 0.582751 11.00000 0.06617 0.06764 = 0.06115 0.00237 0.01122 0.00191 C26 1 0.398556 0.721346 0.596585 11.00000 0.07842 0.05789 = 0.05826 0.00226 0.01678 -0.00035 O1 4 0.119920 0.459681 0.849243 11.00000 0.22788 0.09582 = 0.15749 0.00327 0.11622 0.00628 AFIX 83 H1 2 0.079549 0.486040 0.867638 11.00000 -1.50000 AFIX 0 C28 1 0.456328 0.954237 0.576802 11.00000 0.10596 0.06360 = 0.06484 -0.00664 0.02124 -0.01286 C31 1 0.312876 0.748151 0.564744 11.00000 0.08120 0.06432 = 0.06145 -0.00178 0.02090 -0.00236 C23 1 0.161518 0.312014 0.596053 11.00000 0.06753 0.08220 = 0.07465 -0.00777 0.00743 -0.01514 C27 1 0.468286 0.826963 0.601364 11.00000 0.08952 0.06414 = 0.06713 0.00229 0.01733 -0.00471 AFIX 43 H27 2 0.526929 0.811030 0.622490 11.00000 -1.20000 AFIX 0 C29 1 0.367931 0.977288 0.543905 11.00000 0.11185 0.06207 = 0.06987 0.00645 0.02663 0.00782 C30 1 0.296614 0.873724 0.538346 11.00000 0.08873 0.07164 = 0.07879 0.00599 0.01372 0.00696 AFIX 43 H30 2 0.237997 0.888083 0.517021 11.00000 -1.20000 AFIX 0 C17 1 0.506544 0.509434 0.614511 11.00000 0.07252 0.06775 = 0.10773 0.02348 0.02420 -0.00561 C24 1 0.163434 0.441626 0.573084 11.00000 0.06705 0.07791 = 0.08812 0.00743 -0.00342 -0.00709 AFIX 43 H24 2 0.109420 0.470911 0.550629 11.00000 -1.20000 AFIX 0 N1 3 0.262267 0.460166 0.796409 11.00000 0.15072 0.11281 = 0.08755 0.01047 0.04154 -0.02316 C22 1 0.248246 0.125862 0.654444 11.00000 0.10610 0.08330 = 0.08440 -0.00030 0.00543 -0.02573 AFIX 133 H22A 2 0.252535 0.055606 0.628764 11.00000 -1.50000 H22B 2 0.189586 0.110962 0.670190 11.00000 -1.50000 H22C 2 0.304928 0.119491 0.679765 11.00000 -1.50000 AFIX 0 C1 1 0.160446 0.258444 0.804115 11.00000 0.09966 0.09729 = 0.07049 0.01444 0.02695 0.00879 C7 1 0.242128 0.333557 0.785303 11.00000 0.10704 0.11220 = 0.07529 0.01934 0.02537 0.01136 AFIX 43 H7 2 0.280702 0.285998 0.764326 11.00000 -1.20000 AFIX 0 C9 1 0.301567 0.628917 0.733452 11.00000 0.15608 0.09504 = 0.07333 -0.00809 0.03812 -0.01660 AFIX 23 H9A 2 0.261867 0.698166 0.748460 11.00000 -1.20000 H9B 2 0.258882 0.579104 0.707320 11.00000 -1.20000 AFIX 0 C6 1 0.142148 0.122705 0.790395 11.00000 0.11838 0.11808 = 0.07517 -0.00466 0.01642 -0.00257 AFIX 43 H6 2 0.181881 0.078931 0.769054 11.00000 -1.20000 AFIX 0 C12 1 0.572373 0.499390 0.657509 11.00000 0.07001 0.10566 = 0.18843 0.06210 0.00853 -0.02547 C16 1 0.526924 0.454421 0.568743 11.00000 0.11887 0.07375 = 0.16773 0.00922 0.08134 -0.00288 AFIX 43 H16 2 0.480997 0.460870 0.539734 11.00000 -1.20000 AFIX 0 C32 1 0.535347 1.065717 0.583344 11.00000 0.12893 0.07880 = 0.10357 0.00814 0.01853 -0.02793 AFIX 133 H32A 2 0.582499 1.043148 0.612250 11.00000 -1.50000 H32B 2 0.505931 1.155252 0.588669 11.00000 -1.50000 H32C 2 0.567901 1.069701 0.553277 11.00000 -1.50000 AFIX 0 C4 1 0.006614 0.112575 0.837513 11.00000 0.09793 0.11453 = 0.12477 0.04063 0.01147 0.01270 AFIX 43 H4A 2 -0.045787 0.063328 0.848235 11.00000 -1.20000 AFIX 0 C35 1 0.264664 1.137063 0.485221 11.00000 0.13046 0.07891 = 0.11417 0.02359 0.02286 0.00675 AFIX 23 H35A 2 0.208802 1.137069 0.504460 11.00000 -1.20000 H35B 2 0.253079 1.065839 0.458902 11.00000 -1.20000 AFIX 0 C2 1 0.101879 0.325135 0.835827 11.00000 0.13062 0.08812 = 0.10253 0.02772 0.04066 0.01162 C11 1 0.533956 0.568645 0.699937 11.00000 0.10378 0.13438 = 0.10729 0.05074 -0.02881 -0.06198 C10 1 0.382739 0.705039 0.708564 11.00000 0.16958 0.09729 = 0.06749 -0.00623 0.02002 -0.04185 AFIX 23 H10A 2 0.352055 0.775809 0.685358 11.00000 -1.20000 H10B 2 0.425800 0.753256 0.734971 11.00000 -1.20000 AFIX 0 C3 1 0.023460 0.249847 0.852270 11.00000 0.11709 0.11016 = 0.12590 0.04473 0.05579 0.04187 C5 1 0.066847 0.048493 0.807099 11.00000 0.11277 0.11964 = 0.09062 0.00017 0.00453 -0.01887 C8 1 0.341884 0.527725 0.773393 11.00000 0.14618 0.15285 = 0.08477 0.02867 0.01674 -0.05024 AFIX 23 H8A 2 0.380346 0.456743 0.758475 11.00000 -1.20000 H8B 2 0.385173 0.576661 0.799512 11.00000 -1.20000 AFIX 0 C13 1 0.664348 0.425735 0.657152 11.00000 0.07779 0.14749 = 0.35028 0.12896 0.01561 -0.01228 AFIX 43 H13 2 0.708256 0.410668 0.686480 11.00000 -1.20000 AFIX 0 C36 1 0.272732 1.279001 0.460689 11.00000 0.15479 0.09630 = 0.14666 0.03364 0.01730 0.00927 AFIX 33 H36A 2 0.212993 1.298751 0.438663 11.00000 -1.50000 H36B 2 0.283051 1.349878 0.486652 11.00000 -1.50000 H36C 2 0.327285 1.278717 0.441139 11.00000 -1.50000 AFIX 0 PART 1 C33 1 -0.001631 0.256685 0.546999 11.00000 0.05746 0.17423 = 0.30445 0.05536 -0.02920 -0.04950 PART 0 C15 1 0.619336 0.387696 0.566678 11.00000 0.17733 0.07323 = 0.30534 -0.00190 0.16812 -0.00548 AFIX 43 H15 2 0.637452 0.350310 0.536731 11.00000 -1.20000 AFIX 0 C14 1 0.680702 0.382506 0.612856 11.00000 0.11968 0.12106 = 0.44181 0.10146 0.08570 -0.01830 AFIX 43 H14 2 0.742237 0.342077 0.611515 11.00000 -1.20000 AFIX 0 PART 2 BR1A 5 0.021045 -0.125063 0.787863 10.50000 0.22331 0.20232 = 0.13876 -0.03236 0.01983 -0.10225 BR2A 5 -0.077888 0.326552 0.882870 10.50000 0.15032 0.10496 = 0.23367 0.01272 0.10665 0.03012 PART 0 H3 2 0.080791 0.157197 0.603889 11.00000 0.07118 H4 2 0.396668 1.155309 0.524683 11.00000 0.08067 HKLF 4 REM AS_SC2L_0m_a.res in P2(1)/c REM R1 = 0.0675 for 2356 Fo > 4sig(Fo) and 0.2351 for all 7514 data REM 432 parameters refined using 0 restraints END WGHT 0.0742 0.9836 REM Highest difference peak 0.363, deepest hole -0.288, 1-sigma level 0.047 Q1 1 -0.0863 0.3425 0.5642 11.00000 0.05 0.36 Q2 1 -0.0340 0.1132 0.5303 11.00000 0.05 0.24 Q3 1 0.1963 0.5133 0.8247 11.00000 0.05 0.24 Q4 1 -0.0347 0.2251 0.5004 11.00000 0.05 0.22 Q5 1 0.0383 0.3023 0.4909 11.00000 0.05 0.22 Q6 1 0.0541 -0.0608 0.7595 11.00000 0.05 0.21 Q7 1 -0.1011 0.1628 0.5588 11.00000 0.05 0.21 Q8 1 0.0195 0.2124 0.5504 11.00000 0.05 0.17 Q9 1 0.5365 0.6474 0.7695 11.00000 0.05 0.16 Q10 1 0.5157 1.1353 0.6142 11.00000 0.05 0.16 Q11 1 0.1781 0.6885 0.7486 11.00000 0.05 0.15 Q12 1 0.5846 0.5482 0.7304 11.00000 0.05 0.15 Q13 1 -0.0330 0.1499 0.4832 11.00000 0.05 0.14 Q14 1 -0.0492 0.2685 0.9595 11.00000 0.05 0.14 Q15 1 0.0234 -0.3111 0.7585 11.00000 0.05 0.14 Q16 1 0.4129 0.7110 0.7955 11.00000 0.05 0.13 Q17 1 0.6723 0.3418 0.5907 11.00000 0.05 0.13 Q18 1 0.3733 1.3202 0.4531 11.00000 0.05 0.13 Q19 1 0.4891 0.7354 0.7475 11.00000 0.05 0.13 Q20 1 0.3609 0.3405 0.7283 11.00000 0.05 0.13 ; _shelx_res_checksum 40346 _shelx_hkl_file ; 2 0 0 2987.60 77.79 2 0 0 2998.00 79.19 2 0 0 2961.10 78.69 -2 0 0 3025.20 79.19 -2 0 0 3006.10 78.69 -3 0 0 4555.24 118.49 -3 0 0 4612.74 118.39 3 0 0 4528.45 118.79 3 0 0 4442.46 119.09 3 0 0 4443.36 116.89 -3 0 0 4510.85 119.29 -4 0 0 1204.58 41.70 4 0 0 1214.68 41.10 4 0 0 1203.98 41.30 -4 0 0 1200.48 40.50 -4 0 0 1231.98 40.80 4 0 0 1215.98 39.20 5 0 0 286.87 16.00 -5 0 0 275.97 17.90 5 0 0 283.67 17.20 -5 0 0 289.57 17.50 5 0 0 292.07 18.00 5 0 0 280.77 17.70 -5 0 0 286.87 17.20 -6 0 0 330.17 20.40 6 0 0 268.37 21.10 6 0 0 314.87 18.30 -6 0 0 292.87 19.70 6 0 0 294.87 19.50 -6 0 0 298.87 20.90 6 0 0 313.07 20.40 7 0 0 36.90 8.30 7 0 0 32.00 12.00 -7 0 0 44.00 9.90 7 0 0 33.40 8.70 -7 0 0 41.50 10.50 -7 0 0 49.50 9.50 -8 0 0 65.99 13.20 8 0 0 72.29 14.10 8 0 0 79.69 12.70 8 0 0 49.60 9.80 -8 0 0 71.79 12.20 9 0 0 19.50 8.40 9 0 0 16.60 10.70 -9 0 0 11.30 7.40 -9 0 0 9.00 7.60 9 0 0 17.60 8.40 10 0 0 152.28 17.10 -10 0 0 143.99 18.20 10 0 0 147.29 17.50 -10 0 0 107.79 17.60 11 0 0 5.20 8.10 11 0 0 2.60 7.80 -11 0 0 17.40 8.30 -11 0 0 9.60 9.60 12 0 0 99.39 17.40 -12 0 0 138.59 20.60 12 0 0 113.89 18.70 -13 0 0 9.40 12.40 13 0 0 74.19 16.70 13 0 0 16.00 11.60 14 0 0 2.70 9.20 14 0 0 5.50 9.40 -14 0 0 11.50 12.20 -14 0 0 -7.00 9.00 -15 0 0 -1.20 8.00 15 0 0 -3.70 8.60 16 0 0 -0.40 11.60 -16 0 0 27.10 17.10 16 0 0 -15.70 10.90 -17 0 0 22.00 19.10 17 0 0 -31.10 10.50 17 0 0 3.80 13.40 0 -1 0 1.10 1.00 0 -1 0 -0.20 1.00 0 -1 0 0.50 0.90 1 -1 0 9.90 1.90 -1 -1 0 3.40 1.50 -1 -1 0 10.00 2.50 1 -1 0 8.80 1.80 -1 -1 0 9.40 2.80 -1 -1 0 9.70 2.60 -1 1 0 6.80 1.70 1 1 0 12.10 2.90 2 -1 0 621.04 21.30 -2 -1 0 704.03 25.60 -2 -1 0 684.03 26.00 2 -1 0 641.14 21.40 -2 -1 0 646.74 24.80 2 1 0 673.63 24.70 2 1 0 704.43 26.50 2 1 0 623.04 24.50 2 1 0 673.93 24.60 -2 1 0 655.23 21.60 3 -1 0 4050.59 111.29 3 -1 0 4120.09 111.39 -3 -1 0 4313.97 116.49 3 -1 0 4175.28 106.69 -3 -1 0 4327.17 117.09 -3 -1 0 4240.48 115.89 3 -1 0 4196.68 107.49 3 1 0 4252.87 117.19 -3 1 0 4314.27 110.69 -3 1 0 4369.16 112.29 3 1 0 4406.16 116.19 -3 1 0 4284.87 106.99 3 1 0 4251.37 114.99 -4 -1 0 1790.02 57.99 4 -1 0 1740.23 54.19 -4 -1 0 1741.23 58.49 -4 -1 0 1676.33 62.39 4 -1 0 1773.62 50.89 4 -1 0 1749.53 49.80 4 -1 0 1818.42 53.49 4 1 0 1759.22 57.49 4 1 0 1729.93 58.69 -4 1 0 1810.22 53.19 -4 1 0 1767.62 54.59 4 1 0 1813.42 70.79 -4 1 0 1784.32 50.09 5 -1 0 1261.07 41.30 5 -1 0 1233.08 39.70 -5 -1 0 1270.47 47.70 -5 -1 0 1208.28 53.09 5 -1 0 1258.87 42.50 -5 -1 0 1264.97 47.70 5 -1 0 1255.97 44.30 5 1 0 1171.28 44.60 -5 1 0 1274.57 40.20 -5 1 0 1284.27 43.10 -5 1 0 1257.07 45.50 5 1 0 1241.28 48.30 5 1 0 1305.77 48.40 -6 -1 0 498.15 28.10 -6 -1 0 522.05 28.80 6 -1 0 485.55 23.50 6 -1 0 509.05 24.50 6 -1 0 485.75 25.90 6 -1 0 489.15 22.30 -6 1 0 514.25 25.50 6 1 0 499.45 28.90 6 1 0 536.45 29.10 -6 1 0 503.85 22.60 -6 1 0 496.65 26.50 6 1 0 505.75 30.50 7 -1 0 218.58 16.60 7 -1 0 213.08 17.90 7 -1 0 211.28 14.80 -7 -1 0 231.58 20.80 7 -1 0 228.18 17.30 -7 1 0 207.98 20.50 -7 1 0 214.58 15.60 7 1 0 213.28 19.50 -7 1 0 223.18 17.10 7 1 0 207.28 17.20 -8 -1 0 -3.60 6.80 8 -1 0 2.50 4.90 -8 -1 0 5.40 7.60 8 -1 0 3.80 4.60 8 -1 0 -4.40 5.40 8 1 0 2.10 5.40 8 1 0 -0.10 4.70 -8 1 0 6.20 6.60 -8 1 0 -1.30 4.60 -9 -1 0 67.19 14.60 9 -1 0 74.39 12.80 9 -1 0 63.49 10.80 -9 -1 0 82.19 16.60 9 -1 0 53.29 11.00 9 1 0 53.19 11.40 -9 1 0 45.70 11.20 -9 1 0 60.49 10.60 9 1 0 62.19 13.20 10 -1 0 -3.50 5.80 10 -1 0 9.80 7.70 -10 -1 0 6.20 10.70 -10 -1 0 -2.20 8.30 10 1 0 -8.00 5.40 -10 1 0 14.20 7.30 10 1 0 -2.50 8.10 -10 1 0 -1.10 5.70 11 -1 0 2.40 6.80 11 -1 0 11.40 8.60 -11 -1 0 16.20 10.10 -11 -1 0 5.00 9.70 -11 1 0 5.80 7.20 11 1 0 8.00 8.80 11 1 0 16.20 9.50 -11 1 0 -4.50 5.80 12 -1 0 12.10 11.00 -12 -1 0 15.20 12.80 -12 -1 0 25.70 13.40 12 -1 0 1.70 7.90 -12 1 0 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11.50 8.60 -9 -2 3 6.40 7.80 9 -2 -3 1.50 6.30 9 -2 -3 1.40 5.10 -9 -2 3 3.60 8.10 9 -2 -3 0.10 6.10 -9 2 3 -1.50 4.40 9 2 -3 -7.20 6.10 9 2 -3 9.20 6.80 8 -2 -3 333.77 23.90 8 -2 -3 307.17 21.20 8 -2 -3 299.47 18.10 -8 -2 3 306.97 26.80 8 -2 -3 307.37 19.30 -8 -2 3 319.77 26.60 8 2 -3 331.37 26.30 8 2 -3 302.67 23.10 -7 -2 3 38.80 11.10 -7 -2 3 42.10 11.40 7 -2 -3 33.90 7.30 7 -2 -3 37.10 9.40 7 -2 -3 33.60 7.10 7 2 -3 42.90 9.20 7 2 -3 36.20 10.60 -7 2 3 29.90 7.60 6 -2 -3 337.77 17.30 6 -2 -3 369.36 23.90 -6 -2 3 439.36 27.30 -6 -2 3 374.66 26.60 6 -2 -3 364.46 19.80 6 -2 -3 353.46 17.40 -6 2 3 368.66 17.50 6 2 -3 400.96 23.60 6 2 -3 378.56 25.30 6 2 -3 298.47 24.10 -6 2 3 388.16 21.90 5 -2 -3 733.73 33.80 -5 -2 3 801.42 37.10 -5 -2 3 804.02 37.50 5 -2 -3 720.73 27.20 5 -2 -3 800.92 29.70 -5 -2 3 832.02 39.40 5 -2 -3 829.02 27.70 -5 2 3 841.02 30.50 -5 2 3 834.12 27.80 5 2 -3 848.42 35.30 5 2 -3 827.52 37.70 5 2 -3 787.72 38.40 -5 2 3 833.32 33.30 5 2 -3 879.71 39.70 -4 -2 3 445.86 26.90 -4 -2 3 463.55 25.10 4 -2 -3 491.15 19.10 4 -2 -3 541.15 24.90 -4 -2 3 485.55 26.20 4 -2 -3 534.35 18.60 4 2 -3 490.35 26.20 4 2 -3 467.45 23.80 -4 2 3 501.25 19.30 -4 2 3 505.95 23.00 -4 2 3 476.55 18.20 3 -2 -3 6.50 2.30 -3 -2 3 3.20 4.30 3 -2 -3 9.10 4.20 -3 -2 3 0.60 4.20 3 -2 -3 4.00 2.30 -3 -2 3 8.50 4.50 -3 -2 3 11.20 4.10 3 2 -3 5.80 4.20 3 2 -3 6.60 4.60 -3 2 3 9.60 2.60 -3 2 3 5.00 2.70 3 2 -3 9.50 3.70 3 2 -3 3.50 3.50 -3 2 3 6.80 2.30 -2 -2 3 62.29 7.70 2 -2 -3 50.59 5.20 -2 -2 3 44.60 9.50 -2 -2 3 64.19 7.90 2 -2 -3 63.69 7.40 -2 -2 3 61.69 7.10 2 2 -3 71.29 7.40 2 2 -3 55.89 7.10 -2 2 3 55.09 3.20 -2 2 3 61.09 5.10 2 2 -3 54.09 9.50 2 2 -3 52.69 8.10 2 2 -3 53.49 7.90 -2 2 3 53.69 6.20 1 -2 -3 875.81 25.20 -1 -2 3 865.01 31.70 -1 -2 3 872.81 35.00 1 -2 -3 874.81 30.70 -1 -2 3 895.01 30.60 1 -2 -3 847.72 32.60 -1 2 3 862.71 24.70 1 2 -3 923.31 31.90 -1 2 3 893.31 26.00 1 2 -3 881.21 34.90 1 2 -3 861.51 33.40 1 2 -3 897.81 29.80 1 2 -3 881.41 32.00 1 2 -3 898.91 30.50 -1 2 3 914.91 30.40 -1 2 3 903.61 32.20 0 -2 3 1934.71 57.59 0 -2 -3 1913.61 59.99 0 -2 3 1869.01 52.29 0 -2 -3 1909.71 53.19 0 -2 -3 1965.40 58.99 0 -2 3 1875.31 54.79 0 2 -3 1850.91 54.69 0 2 3 1872.41 51.89 0 2 -3 1863.81 56.89 0 2 -3 1870.91 58.59 0 2 3 1934.81 59.29 0 2 -3 1870.41 54.69 0 2 3 1887.51 57.69 0 2 -3 1922.71 52.59 0 2 -3 1897.31 52.99 -1 -2 -3 2.20 3.50 1 -2 3 3.70 1.60 -1 -2 -3 5.20 3.20 1 -2 3 2.70 2.00 1 -2 3 4.80 2.70 -1 -2 -3 1.60 2.80 -1 2 -3 1.00 2.00 1 2 3 3.50 2.90 -1 2 -3 2.20 1.30 1 2 3 5.60 2.90 1 2 3 9.90 4.30 -1 2 -3 7.30 3.40 -2 -2 -3 64.99 10.50 2 -2 3 88.29 8.20 2 -2 3 71.79 4.90 2 -2 3 85.19 6.10 -2 -2 -3 83.39 8.50 -2 -2 -3 66.99 10.40 2 2 3 95.09 10.70 -2 2 -3 77.19 7.90 2 2 3 82.19 8.10 2 2 3 79.69 9.60 -2 2 -3 76.49 4.70 -2 2 -3 82.79 5.30 -3 -2 -3 -0.30 3.20 3 -2 3 -2.40 2.70 -3 -2 -3 2.50 3.90 3 -2 3 3.70 2.10 3 -2 3 4.60 2.10 -3 -2 -3 1.80 3.40 -3 2 -3 3.20 1.80 -3 2 -3 2.20 1.60 3 2 3 3.20 3.30 3 2 3 -1.10 3.00 3 2 3 7.70 4.70 3 2 3 -1.30 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