data_3ba _audit_creation_method 'SHELXL-2018/3' _shelx_SHELXL_version_number '2018/3' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H15 Br N2 O2, C2 H6 O S' _chemical_formula_sum 'C24 H21 Br N2 O3 S' _chemical_formula_weight 497.40 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' 'S' 'S' 0.1246 0.1234 '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 12.066(3) _cell_length_b 10.127(3) _cell_length_c 18.528(5) _cell_angle_alpha 90 _cell_angle_beta 90.135(18) _cell_angle_gamma 90 _cell_volume 2264.0(11) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 402 _cell_measurement_theta_min 4.00 _cell_measurement_theta_max 17.87 _exptl_crystal_description prismatic _exptl_crystal_colour colorless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.459 _exptl_crystal_F_000 1016 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.12 _exptl_absorpt_coefficient_mu 1.936 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.554 _exptl_absorpt_correction_T_max 0.793 _exptl_absorpt_process_details 'SADABS absorption correction - V2.10' _exptl_absorpt_special_details ? _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 22443 _diffrn_reflns_av_unetI/netI 0.0785 _diffrn_reflns_av_R_equivalents 0.0769 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.198 _diffrn_reflns_theta_max 28.098 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.990 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.990 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.990 _diffrn_reflns_point_group_measured_fraction_full 0.996 _reflns_number_total 5461 _reflns_number_gt 3522 _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 APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0684P)^2^] 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 5461 _refine_ls_number_parameters 288 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0861 _refine_ls_R_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.1397 _refine_ls_wR_factor_gt 0.1151 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.983 _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 Br1 Br -0.06597(3) 0.13165(4) 0.35021(2) 0.03642(15) Uani 1 1 d . . . . . S1 S 0.60496(8) 0.18013(9) 0.31482(4) 0.0258(2) Uani 1 1 d . . . . . O2 O 0.43721(19) 0.5797(2) 0.58043(12) 0.0249(5) Uani 1 1 d . . . . . O1 O 0.5345(2) 0.1994(3) 0.64638(12) 0.0306(6) Uani 1 1 d . . . . . O3 O 0.6358(2) 0.1264(2) 0.38800(12) 0.0305(6) Uani 1 1 d . . . . . N2 N 0.3980(2) 0.3826(3) 0.52371(15) 0.0195(6) Uani 1 1 d . . . . . N1 N 0.6270(2) 0.2032(3) 0.54000(15) 0.0234(7) Uani 1 1 d . . . . . C1 C 0.2518(3) 0.2228(3) 0.48653(16) 0.0205(7) Uani 1 1 d . . . . . C4 C 0.0670(3) 0.1665(4) 0.40334(17) 0.0253(8) Uani 1 1 d . . . . . C23 C 0.3904(3) 0.4710(3) 0.57767(16) 0.0208(7) Uani 1 1 d . . . . . C9 C 0.5366(3) 0.1853(4) 0.58071(18) 0.0221(7) Uani 1 1 d . . . . . C22 C 0.3174(3) 0.4125(3) 0.63232(17) 0.0195(7) Uani 1 1 d . . . . . C7 C 0.3461(3) 0.2550(3) 0.53905(16) 0.0194(7) Uani 1 1 d . . . . . C10 C 0.7327(3) 0.2476(4) 0.56300(18) 0.0245(8) Uani 1 1 d . . . . . C3 C 0.1144(3) 0.0679(4) 0.44396(17) 0.0256(8) Uani 1 1 d . . . . . H3 H 0.084605 -0.016835 0.443623 0.031 Uiso 1 1 calc R U . . . C17 C 0.2950(3) 0.2839(3) 0.61272(16) 0.0199(7) Uani 1 1 d . . . . . C8 C 0.4342(3) 0.1447(3) 0.53810(17) 0.0218(7) Uani 1 1 d . . . . . C21 C 0.2732(3) 0.4683(4) 0.69454(17) 0.0252(8) Uani 1 1 d . . . . . H21 H 0.288653 0.555272 0.707188 0.030 Uiso 1 1 calc R U . . . C18 C 0.2282(3) 0.2046(4) 0.65499(17) 0.0247(8) Uani 1 1 d . . . . . H18 H 0.213449 0.117537 0.642309 0.030 Uiso 1 1 calc R U . . . C6 C 0.2041(3) 0.3202(4) 0.44356(17) 0.0245(8) Uani 1 1 d . . . . . H6 H 0.234416 0.404660 0.442822 0.029 Uiso 1 1 calc R U . . . C2 C 0.2076(3) 0.0962(4) 0.48560(17) 0.0231(7) Uani 1 1 d . . . . . H2 H 0.240435 0.029939 0.513002 0.028 Uiso 1 1 calc R U . . . C5 C 0.1117(3) 0.2920(4) 0.40188(18) 0.0284(8) Uani 1 1 d . . . . . H5 H 0.079946 0.357088 0.373093 0.034 Uiso 1 1 calc R U . . . C20 C 0.2058(3) 0.3906(4) 0.73678(19) 0.0301(9) Uani 1 1 d . . . . . H20 H 0.174623 0.425059 0.778598 0.036 Uiso 1 1 calc R U . . . C19 C 0.1840(3) 0.2598(4) 0.71686(18) 0.0288(8) Uani 1 1 d . . . . . H19 H 0.138614 0.208454 0.746081 0.035 Uiso 1 1 calc R U . . . C16 C 0.7997(3) 0.3023(4) 0.51105(19) 0.0284(8) Uani 1 1 d . . . . . H16 H 0.774388 0.309646 0.463762 0.034 Uiso 1 1 calc R U . . . C11 C 0.7716(3) 0.2330(4) 0.6334(2) 0.0368(10) Uani 1 1 d . . . . . H11 H 0.727500 0.194177 0.668620 0.044 Uiso 1 1 calc R U . . . C25 C 0.4589(3) 0.1994(4) 0.3144(2) 0.0332(9) Uani 1 1 d . . . . . H25A H 0.435536 0.233588 0.268462 0.050 Uiso 1 1 calc R U . . . H25B H 0.424361 0.115278 0.322522 0.050 Uiso 1 1 calc R U . . . H25C H 0.437637 0.259620 0.351862 0.050 Uiso 1 1 calc R U . . . C24 C 0.6106(4) 0.0434(4) 0.25424(19) 0.0377(10) Uani 1 1 d . . . . . H24A H 0.591469 0.072333 0.206472 0.057 Uiso 1 1 calc R U . . . H24B H 0.684148 0.007328 0.254090 0.057 Uiso 1 1 calc R U . . . H24C H 0.559066 -0.023180 0.269576 0.057 Uiso 1 1 calc R U . . . C15 C 0.9048(3) 0.3465(4) 0.5291(2) 0.0405(10) Uani 1 1 d . . . . . H15 H 0.949365 0.385608 0.494226 0.049 Uiso 1 1 calc R U . . . C14 C 0.9435(3) 0.3324(5) 0.5990(3) 0.0484(12) Uani 1 1 d . . . . . H14 H 1.014598 0.360400 0.610990 0.058 Uiso 1 1 calc R U . . . C13 C 0.8771(3) 0.2774(5) 0.6500(2) 0.0493(13) Uani 1 1 d . . . . . H13 H 0.903205 0.269522 0.697123 0.059 Uiso 1 1 calc R U . . . H1N H 0.615(3) 0.202(4) 0.495(2) 0.024(10) Uiso 1 1 d . . . . . H2N H 0.448(3) 0.391(4) 0.488(2) 0.040(12) 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 0.0287(2) 0.0488(3) 0.0317(2) -0.00064(18) -0.00804(15) -0.01060(19) S1 0.0332(5) 0.0231(5) 0.0211(4) 0.0019(4) -0.0023(3) -0.0026(4) O2 0.0308(13) 0.0173(13) 0.0267(12) -0.0043(10) 0.0059(10) -0.0072(11) O1 0.0325(13) 0.0404(17) 0.0191(12) -0.0035(11) 0.0016(10) -0.0013(13) O3 0.0392(14) 0.0283(15) 0.0239(13) 0.0015(11) -0.0080(11) -0.0009(12) N2 0.0223(14) 0.0170(15) 0.0192(14) -0.0009(12) 0.0033(11) -0.0025(12) N1 0.0246(14) 0.0292(18) 0.0163(14) -0.0023(13) -0.0011(11) -0.0002(14) C1 0.0210(15) 0.0246(19) 0.0161(15) -0.0017(14) 0.0029(12) -0.0033(15) C4 0.0259(17) 0.032(2) 0.0177(16) -0.0034(15) 0.0028(13) -0.0028(16) C23 0.0211(16) 0.0238(19) 0.0176(15) -0.0018(14) -0.0025(12) 0.0002(15) C9 0.0232(16) 0.0223(18) 0.0208(17) -0.0004(14) 0.0014(13) 0.0014(15) C22 0.0210(15) 0.0169(17) 0.0206(16) -0.0008(14) 0.0015(13) 0.0002(14) C7 0.0240(16) 0.0179(18) 0.0162(15) 0.0019(13) 0.0020(12) -0.0030(15) C10 0.0193(16) 0.029(2) 0.0257(17) -0.0091(15) -0.0027(13) 0.0025(16) C3 0.0263(17) 0.025(2) 0.0250(17) -0.0064(15) 0.0040(14) -0.0065(16) C17 0.0208(15) 0.0207(18) 0.0181(16) -0.0005(14) 0.0011(12) -0.0003(15) C8 0.0219(16) 0.0215(19) 0.0220(16) -0.0044(14) -0.0003(13) 0.0003(15) C21 0.0291(18) 0.0246(19) 0.0220(17) -0.0032(15) 0.0020(14) -0.0022(16) C18 0.0254(17) 0.026(2) 0.0223(17) 0.0000(15) 0.0018(14) -0.0083(16) C6 0.0250(17) 0.027(2) 0.0216(17) 0.0002(15) 0.0037(13) -0.0030(16) C2 0.0241(16) 0.0222(19) 0.0228(17) -0.0026(14) -0.0005(13) -0.0002(15) C5 0.0319(19) 0.032(2) 0.0215(17) 0.0041(16) 0.0019(14) 0.0033(18) C20 0.0304(18) 0.040(2) 0.0199(17) -0.0005(16) 0.0057(14) -0.0018(18) C19 0.0251(17) 0.037(2) 0.0247(18) 0.0076(17) 0.0066(14) -0.0075(18) C16 0.0232(17) 0.032(2) 0.0305(19) -0.0036(17) 0.0015(14) 0.0010(17) C11 0.0288(18) 0.056(3) 0.0258(19) -0.0084(19) -0.0035(15) 0.002(2) C25 0.033(2) 0.035(2) 0.031(2) -0.0002(17) -0.0052(16) 0.0005(19) C24 0.057(3) 0.029(2) 0.0262(19) -0.0015(17) -0.0032(18) 0.003(2) C15 0.0258(19) 0.037(3) 0.059(3) -0.011(2) 0.0096(18) -0.0007(19) C14 0.0219(19) 0.058(3) 0.066(3) -0.027(3) -0.012(2) -0.001(2) C13 0.034(2) 0.079(4) 0.035(2) -0.022(2) -0.0125(18) 0.009(2) _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 C4 1.913(3) . ? S1 O3 1.507(2) . ? S1 C25 1.773(4) . ? S1 C24 1.784(4) . ? O2 C23 1.238(4) . ? O1 C9 1.225(4) . ? N2 C23 1.345(4) . ? N2 C7 1.464(4) . ? N2 H2N 0.91(4) . ? N1 C9 1.340(4) . ? N1 C10 1.416(4) . ? N1 H1N 0.85(4) . ? C1 C2 1.389(5) . ? C1 C6 1.392(5) . ? C1 C7 1.530(4) . ? C4 C3 1.375(5) . ? C4 C5 1.381(5) . ? C23 C22 1.469(5) . ? C9 C8 1.521(4) . ? C22 C17 1.379(5) . ? C22 C21 1.392(5) . ? C7 C17 1.527(4) . ? C7 C8 1.542(5) . ? C10 C16 1.375(5) . ? C10 C11 1.394(5) . ? C3 C2 1.392(4) . ? C3 H3 0.9300 . ? C17 C18 1.382(5) . ? C21 C20 1.377(5) . ? C21 H21 0.9300 . ? C18 C19 1.383(5) . ? C18 H18 0.9300 . ? C6 C5 1.385(5) . ? C6 H6 0.9300 . ? C2 H2 0.9300 . ? C5 H5 0.9300 . ? C20 C19 1.400(5) . ? C20 H20 0.9300 . ? C19 H19 0.9300 . ? C16 C15 1.386(5) . ? C16 H16 0.9300 . ? C11 C13 1.384(5) . ? C11 H11 0.9300 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C15 C14 1.382(6) . ? C15 H15 0.9300 . ? C14 C13 1.360(7) . ? C14 H14 0.9300 . ? C13 H13 0.9300 . ? 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 O3 S1 C25 106.70(17) . . ? O3 S1 C24 106.02(17) . . ? C25 S1 C24 97.0(2) . . ? C23 N2 C7 114.4(3) . . ? C23 N2 H2N 122(3) . . ? C7 N2 H2N 121(3) . . ? C9 N1 C10 127.4(3) . . ? C9 N1 H1N 114(2) . . ? C10 N1 H1N 117(2) . . ? C2 C1 C6 119.2(3) . . ? C2 C1 C7 119.3(3) . . ? C6 C1 C7 121.3(3) . . ? C3 C4 C5 121.2(3) . . ? C3 C4 Br1 119.7(3) . . ? C5 C4 Br1 119.1(3) . . ? O2 C23 N2 126.2(3) . . ? O2 C23 C22 127.2(3) . . ? N2 C23 C22 106.6(3) . . ? O1 C9 N1 124.1(3) . . ? O1 C9 C8 121.9(3) . . ? N1 C9 C8 114.0(3) . . ? C17 C22 C21 121.8(3) . . ? C17 C22 C23 108.5(3) . . ? C21 C22 C23 129.7(3) . . ? N2 C7 C17 100.3(3) . . ? N2 C7 C1 112.5(3) . . ? C17 C7 C1 108.0(3) . . ? N2 C7 C8 110.0(3) . . ? C17 C7 C8 115.4(3) . . ? C1 C7 C8 110.5(3) . . ? C16 C10 C11 120.1(3) . . ? C16 C10 N1 116.6(3) . . ? C11 C10 N1 123.3(3) . . ? C4 C3 C2 119.2(3) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C22 C17 C18 120.9(3) . . ? C22 C17 C7 109.7(3) . . ? C18 C17 C7 129.2(3) . . ? C9 C8 C7 111.0(3) . . ? C20 C21 C22 117.8(3) . . ? C20 C21 H21 121.1 . . ? C22 C21 H21 121.1 . . ? C17 C18 C19 117.5(3) . . ? C17 C18 H18 121.2 . . ? C19 C18 H18 121.2 . . ? C5 C6 C1 120.3(3) . . ? C5 C6 H6 119.9 . . ? C1 C6 H6 119.9 . . ? C1 C2 C3 120.5(3) . . ? C1 C2 H2 119.7 . . ? C3 C2 H2 119.7 . . ? C4 C5 C6 119.6(3) . . ? C4 C5 H5 120.2 . . ? C6 C5 H5 120.2 . . ? C21 C20 C19 120.1(3) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C18 C19 C20 121.9(3) . . ? C18 C19 H19 119.1 . . ? C20 C19 H19 119.1 . . ? C10 C16 C15 120.0(4) . . ? C10 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C13 C11 C10 118.8(4) . . ? C13 C11 H11 120.6 . . ? C10 C11 H11 120.6 . . ? S1 C25 H25A 109.5 . . ? S1 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? S1 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? S1 C24 H24A 109.5 . . ? S1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? S1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C14 C15 C16 120.0(4) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C13 C14 C15 119.7(4) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C14 C13 C11 121.4(4) . . ? C14 C13 H13 119.3 . . ? C11 C13 H13 119.3 . . ? _refine_diff_density_max 0.856 _refine_diff_density_min -0.593 _refine_diff_density_rms 0.099 _shelx_res_file ; TITL F1_a.res in P2(1)/c shelx.res created by SHELXL-2018/3 at 10:11:37 on 30-Mar-2019 CELL 0.71073 12.0659 10.1273 18.5276 90.000 90.135 90.000 ZERR 4.00 0.0034 0.0028 0.0049 0.000 0.018 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O BR S UNIT 96 84 8 12 4 4 MERG 2 FMAP 2 PLAN 5 ACTA BOND $H L.S. 20 TEMP 23.00 WGHT 0.068400 FVAR 0.38952 BR1 5 -0.065971 0.131651 0.350211 11.00000 0.02867 0.04885 = 0.03171 -0.00064 -0.00804 -0.01060 S1 6 0.604963 0.180127 0.314821 11.00000 0.03319 0.02309 = 0.02113 0.00190 -0.00229 -0.00256 O2 4 0.437205 0.579661 0.580433 11.00000 0.03080 0.01730 = 0.02667 -0.00430 0.00590 -0.00724 O1 4 0.534542 0.199378 0.646382 11.00000 0.03248 0.04040 = 0.01905 -0.00350 0.00157 -0.00133 O3 4 0.635812 0.126380 0.388001 11.00000 0.03921 0.02833 = 0.02391 0.00152 -0.00799 -0.00085 N2 3 0.397970 0.382625 0.523714 11.00000 0.02230 0.01699 = 0.01916 -0.00087 0.00329 -0.00245 N1 3 0.627048 0.203242 0.540003 11.00000 0.02458 0.02925 = 0.01634 -0.00229 -0.00110 -0.00019 C1 1 0.251844 0.222822 0.486530 11.00000 0.02095 0.02455 = 0.01607 -0.00166 0.00293 -0.00326 C4 1 0.066966 0.166519 0.403341 11.00000 0.02592 0.03214 = 0.01771 -0.00341 0.00284 -0.00279 C23 1 0.390370 0.471020 0.577665 11.00000 0.02111 0.02379 = 0.01758 -0.00175 -0.00247 0.00021 C9 1 0.536611 0.185254 0.580711 11.00000 0.02319 0.02226 = 0.02083 -0.00043 0.00138 0.00143 C22 1 0.317369 0.412457 0.632315 11.00000 0.02099 0.01692 = 0.02059 -0.00083 0.00147 0.00018 C7 1 0.346075 0.254981 0.539048 11.00000 0.02397 0.01793 = 0.01622 0.00191 0.00203 -0.00301 C10 1 0.732697 0.247642 0.563002 11.00000 0.01927 0.02858 = 0.02569 -0.00908 -0.00272 0.00248 C3 1 0.114408 0.067851 0.443963 11.00000 0.02634 0.02535 = 0.02504 -0.00641 0.00401 -0.00653 AFIX 43 H3 2 0.084605 -0.016835 0.443623 11.00000 -1.20000 AFIX 0 C17 1 0.294979 0.283861 0.612717 11.00000 0.02078 0.02069 = 0.01813 -0.00051 0.00107 -0.00031 C8 1 0.434191 0.144734 0.538100 11.00000 0.02186 0.02148 = 0.02200 -0.00435 -0.00035 0.00032 C21 1 0.273178 0.468326 0.694542 11.00000 0.02909 0.02463 = 0.02204 -0.00317 0.00201 -0.00225 AFIX 43 H21 2 0.288653 0.555272 0.707188 11.00000 -1.20000 AFIX 0 C18 1 0.228171 0.204650 0.654994 11.00000 0.02541 0.02632 = 0.02227 0.00000 0.00178 -0.00832 AFIX 43 H18 2 0.213449 0.117537 0.642309 11.00000 -1.20000 AFIX 0 C6 1 0.204115 0.320235 0.443555 11.00000 0.02500 0.02711 = 0.02156 0.00021 0.00366 -0.00297 AFIX 43 H6 2 0.234416 0.404660 0.442822 11.00000 -1.20000 AFIX 0 C2 1 0.207576 0.096240 0.485597 11.00000 0.02415 0.02220 = 0.02280 -0.00257 -0.00052 -0.00021 AFIX 43 H2 2 0.240435 0.029939 0.513002 11.00000 -1.20000 AFIX 0 C5 1 0.111687 0.291981 0.401878 11.00000 0.03190 0.03187 = 0.02148 0.00410 0.00186 0.00334 AFIX 43 H5 2 0.079946 0.357088 0.373093 11.00000 -1.20000 AFIX 0 C20 1 0.205765 0.390585 0.736775 11.00000 0.03036 0.04007 = 0.01992 -0.00050 0.00572 -0.00183 AFIX 43 H20 2 0.174623 0.425059 0.778598 11.00000 -1.20000 AFIX 0 C19 1 0.184037 0.259766 0.716861 11.00000 0.02506 0.03657 = 0.02474 0.00756 0.00664 -0.00753 AFIX 43 H19 2 0.138614 0.208454 0.746081 11.00000 -1.20000 AFIX 0 C16 1 0.799670 0.302312 0.511049 11.00000 0.02315 0.03172 = 0.03049 -0.00362 0.00152 0.00104 AFIX 43 H16 2 0.774388 0.309646 0.463762 11.00000 -1.20000 AFIX 0 C11 1 0.771612 0.233038 0.633430 11.00000 0.02879 0.05570 = 0.02575 -0.00844 -0.00348 0.00248 AFIX 43 H11 2 0.727500 0.194177 0.668620 11.00000 -1.20000 AFIX 0 C25 1 0.458872 0.199359 0.314364 11.00000 0.03343 0.03545 = 0.03069 -0.00019 -0.00522 0.00046 AFIX 33 H25A 2 0.435536 0.233588 0.268462 11.00000 -1.50000 H25B 2 0.424361 0.115278 0.322522 11.00000 -1.50000 H25C 2 0.437637 0.259620 0.351862 11.00000 -1.50000 AFIX 0 C24 1 0.610557 0.043358 0.254244 11.00000 0.05749 0.02937 = 0.02621 -0.00155 -0.00319 0.00266 AFIX 33 H24A 2 0.591469 0.072333 0.206472 11.00000 -1.50000 H24B 2 0.684148 0.007328 0.254090 11.00000 -1.50000 H24C 2 0.559066 -0.023180 0.269576 11.00000 -1.50000 AFIX 0 C15 1 0.904825 0.346492 0.529102 11.00000 0.02581 0.03730 = 0.05852 -0.01143 0.00961 -0.00070 AFIX 43 H15 2 0.949365 0.385608 0.494226 11.00000 -1.20000 AFIX 0 C14 1 0.943506 0.332412 0.598962 11.00000 0.02195 0.05762 = 0.06566 -0.02656 -0.01223 -0.00135 AFIX 43 H14 2 1.014598 0.360400 0.610990 11.00000 -1.20000 AFIX 0 C13 1 0.877135 0.277440 0.650045 11.00000 0.03352 0.07907 = 0.03515 -0.02164 -0.01251 0.00941 AFIX 43 H13 2 0.903205 0.269522 0.697123 11.00000 -1.20000 AFIX 0 H1N 2 0.615041 0.201594 0.494941 11.00000 0.02422 H2N 2 0.448328 0.391447 0.487562 11.00000 0.04006 HKLF 4 REM F1_a.res in P2(1)/c REM wR2 = 0.1397, GooF = S = 0.983, Restrained GooF = 0.983 for all data REM R1 = 0.0499 for 3522 Fo > 4sig(Fo) and 0.0861 for all 5461 data REM 288 parameters refined using 0 restraints END WGHT 0.0687 0.0000 REM Highest difference peak 0.856, deepest hole -0.593, 1-sigma level 0.099 Q1 1 0.3989 0.0610 0.5538 11.00000 0.05 0.86 Q2 1 0.4625 0.1275 0.4890 11.00000 0.05 0.84 Q3 1 -0.0980 0.1374 0.3817 11.00000 0.05 0.36 Q4 1 0.4622 0.1696 0.5509 11.00000 0.05 0.36 Q5 1 0.4597 0.3017 0.3427 11.00000 0.05 0.36 ; _shelx_res_checksum 17245 _shelx_hkl_file ; 3 0 0 -6.60 3.60 -3 0 0 10.30 4.30 3 0 0 11.20 5.50 -3 0 0 11.30 5.50 -3 0 0 15.50 5.80 -4 0 0 672.53 30.90 -4 0 0 719.93 27.50 4 0 0 713.83 32.40 -4 0 0 741.33 32.90 -5 0 0 165.08 19.40 -5 0 0 164.58 15.40 5 0 0 152.48 19.00 6 0 0 4636.14 135.59 6 0 0 4793.42 121.39 -6 0 0 4864.11 134.59 -6 0 0 4534.05 123.29 -7 0 0 1912.51 63.19 7 0 0 1947.71 60.89 7 0 0 1835.42 73.39 -7 0 0 1952.20 72.89 -8 0 0 615.24 38.80 -8 0 0 694.13 33.80 8 0 0 634.04 41.60 8 0 0 594.84 30.40 -9 0 0 367.46 25.60 9 0 0 365.46 24.20 9 0 0 399.16 35.30 -9 0 0 332.67 37.30 -10 0 0 -0.80 8.40 -10 0 0 -0.40 6.00 10 0 0 -1.90 5.20 -11 0 0 -0.40 7.50 11 0 0 -5.70 5.20 -11 0 0 -5.50 6.10 -12 0 0 138.19 29.40 -12 0 0 118.39 20.10 12 0 0 145.29 20.70 13 0 0 137.19 20.50 -13 0 0 140.49 29.70 -13 0 0 145.19 22.40 -14 0 0 15.80 12.00 14 0 0 11.70 10.00 -14 0 0 11.10 14.20 -15 0 0 299.17 46.70 15 0 0 353.56 33.10 0 -1 0 -8.10 1.70 0 -1 0 -0.80 3.00 0 1 0 -2.20 2.70 0 1 0 -6.10 2.00 -1 -1 0 1.00 2.90 -1 -1 0 15.10 4.40 1 1 0 10.60 3.70 -2 -1 0 6.50 4.00 2 -1 0 1.30 1.70 -2 -1 0 7.20 3.30 -2 -1 0 -0.50 3.80 -2 1 0 3.00 2.70 -2 1 0 4.80 1.90 2 1 0 1.90 3.80 -2 1 0 -1.40 1.50 2 1 0 7.00 4.20 -2 1 0 3.90 1.50 -3 -1 0 5006.70 131.69 3 -1 0 4870.01 112.19 -3 -1 0 4543.05 116.39 -3 -1 0 4445.46 112.59 -3 1 0 4500.45 117.59 3 1 0 4433.06 122.79 -3 1 0 4579.44 109.19 -3 1 0 4527.45 111.39 -4 -1 0 895.21 33.20 4 -1 0 960.70 33.80 -4 -1 0 903.11 36.30 -4 1 0 902.31 37.10 4 1 0 860.61 40.60 -4 1 0 873.71 32.80 -4 1 0 907.11 30.00 -5 -1 0 521.05 28.70 -5 -1 0 503.85 25.00 5 -1 0 499.55 25.80 -5 1 0 494.35 25.60 -5 1 0 483.45 28.00 5 1 0 497.35 31.60 -5 1 0 521.85 22.50 5 1 0 488.45 20.40 -6 -1 0 436.06 24.70 6 -1 0 421.96 26.40 -6 -1 0 473.65 29.40 6 1 0 457.85 20.70 -6 1 0 443.06 28.80 6 1 0 438.16 31.90 -6 1 0 425.96 22.20 -7 -1 0 107.59 18.60 -7 -1 0 110.49 16.20 -7 1 0 74.19 16.20 7 1 0 92.09 12.00 -7 1 0 100.99 13.20 7 1 0 105.89 20.20 -8 -1 0 8.30 9.00 -8 -1 0 3.30 5.30 -8 -1 0 -1.30 4.80 -8 -1 0 3.10 5.50 -8 1 0 0.40 4.10 8 1 0 2.20 8.40 -8 1 0 -8.80 4.80 8 1 0 1.40 3.90 -8 1 0 0.70 6.20 -9 -1 0 -0.60 9.30 -9 -1 0 6.30 8.70 -9 -1 0 5.20 6.60 9 -1 0 13.20 8.00 -9 -1 0 7.00 5.90 -9 1 0 1.10 5.40 -9 1 0 -0.50 7.20 9 1 0 -1.50 9.50 9 1 0 0.50 4.70 -9 1 0 3.40 8.40 -10 -1 0 582.84 43.20 -10 -1 0 623.44 36.60 10 -1 0 631.54 35.40 -10 1 0 627.54 45.00 10 1 0 605.54 30.70 10 1 0 626.44 50.09 -10 1 0 657.13 34.80 11 -1 0 73.19 15.40 -11 -1 0 27.50 13.20 -11 -1 0 51.89 13.70 -11 -1 0 -0.10 10.90 -11 1 0 36.80 15.40 -11 1 0 48.00 12.80 11 1 0 65.19 13.00 -12 -1 0 318.57 43.10 -12 -1 0 328.67 33.50 12 -1 0 298.17 30.50 -12 1 0 333.57 43.30 12 1 0 290.67 26.90 -12 1 0 307.17 30.30 13 -1 0 27.30 11.90 -13 -1 0 26.50 13.00 -13 -1 0 29.00 17.20 -13 1 0 56.29 19.70 13 1 0 50.59 12.30 -14 -1 0 20.10 16.00 14 -1 0 2.90 9.50 -14 -1 0 26.30 13.20 -14 1 0 14.70 15.10 14 1 0 5.80 7.90 -15 -1 0 14.80 14.70 15 -1 0 -0.10 9.10 -15 -1 0 7.20 13.00 -15 1 0 -7.90 10.30 0 -2 0 8140.09 194.08 0 -2 0 8209.38 192.88 0 2 0 8458.75 194.68 0 2 0 8267.57 190.48 0 2 0 8033.70 192.88 -1 -2 0 5.60 4.70 1 -2 0 -0.70 2.50 -1 -2 0 2.10 3.00 1 -2 0 2.60 2.40 -1 -2 0 2.90 5.00 -1 2 0 -0.20 2.20 1 2 0 -0.70 3.80 1 2 0 2.50 4.80 -1 2 0 -2.60 2.00 1 2 0 -3.70 1.80 2 -2 0 72.69 6.40 -2 -2 0 121.29 11.40 -2 2 0 135.09 12.50 2 2 0 120.79 15.70 2 2 0 99.19 10.00 -2 2 0 130.29 12.30 -3 -2 0 314.97 17.60 3 2 0 319.27 23.40 -3 2 0 295.37 9.70 -3 2 0 303.07 9.50 -3 2 0 314.77 18.40 -4 -2 0 51.39 9.70 -4 2 0 47.90 5.70 -4 2 0 49.80 6.30 4 2 0 59.59 14.20 -4 2 0 37.00 8.70 -5 -2 0 2.00 3.80 -5 -2 0 -5.30 4.90 5 -2 0 -1.60 4.20 -5 -2 0 1.20 3.60 -5 2 0 1.70 2.60 -5 2 0 6.80 6.10 5 2 0 1.20 5.70 -5 2 0 4.80 3.30 -5 2 0 1.30 4.10 -6 -2 0 84.09 15.30 -6 -2 0 70.49 12.00 6 2 0 73.99 7.30 6 2 0 58.89 15.80 -6 2 0 80.99 10.20 -6 2 0 63.19 13.40 -6 2 0 63.69 10.40 -7 -2 0 264.07 24.90 -7 -2 0 238.68 27.20 -7 2 0 240.48 16.30 7 2 0 260.67 34.30 7 2 0 243.98 13.10 -7 2 0 287.67 30.80 -8 -2 0 11.00 7.00 -8 -2 0 2.10 6.30 -8 -2 0 -1.20 7.60 8 2 0 4.30 3.70 -8 2 0 -1.30 4.20 -8 2 0 6.70 7.10 -8 2 0 -0.30 5.50 8 2 0 2.00 8.60 -9 -2 0 5.40 6.50 -9 -2 0 -1.60 6.20 -9 -2 0 -3.20 4.80 -9 2 0 4.30 5.20 9 2 0 4.10 4.10 9 2 0 -0.40 10.40 -9 2 0 -2.50 6.20 -10 -2 0 -11.50 9.20 -10 -2 0 -0.90 7.50 -10 -2 0 13.90 8.70 10 -2 0 5.40 7.40 10 2 0 4.80 4.60 10 2 0 6.30 13.20 -10 2 0 6.30 6.30 -10 2 0 3.80 8.60 -11 -2 0 21.10 10.60 -11 -2 0 -7.90 11.80 11 -2 0 14.20 9.20 -11 -2 0 18.80 12.50 11 2 0 28.60 7.70 11 2 0 8.50 15.70 -11 2 0 26.60 13.50 -12 -2 0 21.00 13.90 -12 -2 0 -4.20 13.40 -12 -2 0 10.80 9.90 12 -2 0 7.20 8.90 12 2 0 1.80 5.00 -12 2 0 -2.40 8.50 -13 -2 0 18.10 14.80 13 -2 0 14.80 10.60 -13 -2 0 17.90 12.50 -13 2 0 17.60 15.30 13 2 0 16.80 6.60 -14 -2 0 2.50 11.30 -14 -2 0 9.30 13.70 14 -2 0 -4.90 8.00 -14 2 0 2.00 13.10 15 -2 0 11.60 11.80 -15 -2 0 -10.60 12.10 -15 -2 0 22.50 15.00 -15 2 0 4.00 15.60 0 -3 0 0.00 3.40 0 -3 0 -2.40 4.10 0 3 0 2.60 3.70 0 3 0 0.00 2.80 0 3 0 -1.40 2.90 0 3 0 -0.40 5.50 -1 -3 0 87.79 10.60 -1 -3 0 71.49 13.10 1 -3 0 70.59 8.80 1 -3 0 56.79 8.30 1 3 0 64.29 8.70 -1 3 0 63.39 8.70 -1 3 0 98.59 11.60 -1 3 0 60.89 8.80 -2 -3 0 89.29 15.90 -2 -3 0 122.19 12.50 2 -3 0 141.49 7.90 2 3 0 166.78 12.30 2 3 0 156.78 19.70 -2 3 0 102.49 12.00 -2 3 0 128.29 13.60 -2 3 0 147.19 8.40 -3 -3 0 633.64 28.30 -3 3 0 634.54 29.50 3 3 0 720.83 38.70 3 3 0 609.24 27.20 3 3 0 630.24 25.80 -4 -3 0 921.11 38.00 4 3 0 880.41 34.40 -4 3 0 892.41 39.30 4 3 0 952.80 49.20 -5 -3 0 234.48 23.20 -5 3 0 244.08 24.70 5 3 0 222.38 29.50 -5 3 0 219.68 8.20 5 3 0 230.58 17.10 -6 -3 0 83.59 15.10 6 3 0 56.29 10.70 6 3 0 43.50 15.30 -6 3 0 74.49 8.10 -6 3 0 51.29 12.10 -6 3 0 83.59 8.10 -7 -3 0 239.98 24.10 -7 -3 0 237.88 27.40 7 3 0 194.38 31.20 -7 3 0 225.28 27.70 -7 3 0 199.18 13.90 -8 -3 0 7.50 6.50 -8 -3 0 15.60 9.40 -8 -3 0 2.10 10.40 8 3 0 -3.20 9.40 -8 3 0 1.70 7.50 -9 -3 0 23.60 10.30 -9 -3 0 2.40 11.60 -9 -3 0 29.80 12.30 9 3 0 21.10 15.50 -9 3 0 4.80 10.00 -10 -3 0 94.89 18.10 -10 -3 0 95.59 21.50 10 3 0 98.29 26.90 -10 3 0 130.89 25.20 -11 -3 0 458.85 41.00 -11 -3 0 429.46 46.30 11 3 0 500.95 60.79 -11 3 0 464.25 50.59 -12 -3 0 -3.30 9.30 12 -3 0 15.10 11.10 -12 -3 0 6.80 9.70 -12 -3 0 -3.10 10.00 -12 3 0 9.40 12.80 -13 -3 0 55.09 20.40 -13 -3 0 35.00 14.90 -13 -3 0 8.40 16.60 13 -3 0 55.49 16.90 -13 3 0 36.70 17.70 14 -3 0 -1.00 9.50 -14 -3 0 -1.10 11.00 -14 -3 0 10.10 11.00 -14 3 0 -4.40 10.10 -15 -3 0 -1.40 13.20 15 -3 0 9.00 11.50 -15 3 0 -3.70 11.60 0 -4 0 1126.19 45.20 0 4 0 1045.80 43.20 0 4 0 1071.79 39.80 0 4 0 1027.70 38.10 1 -4 0 940.01 36.90 -1 -4 0 959.00 44.40 1 -4 0 900.81 35.40 -1 -4 0 843.62 35.30 -1 4 0 947.81 36.00 -1 4 0 935.11 37.00 1 4 0 853.11 41.40 1 4 0 904.71 35.50 -1 4 0 879.31 35.60 1 4 0 882.61 33.20 -2 -4 0 2382.76 71.39 2 -4 0 2424.46 64.69 2 4 0 2340.07 67.39 -2 4 0 2350.36 72.79 2 4 0 2383.46 83.59 2 4 0 2472.75 71.79 -2 4 0 2292.77 65.19 -2 4 0 2321.17 71.89 -3 -4 0 209.98 20.00 3 -4 0 179.08 8.50 3 4 0 158.38 16.70 3 4 0 169.78 15.80 -3 4 0 182.28 19.50 -3 4 0 150.98 17.60 3 4 0 189.68 25.80 -4 -4 0 296.77 20.90 -4 -4 0 202.98 29.30 4 4 0 246.48 17.10 4 4 0 225.88 29.60 4 4 0 275.47 19.70 -4 4 0 236.78 23.20 -5 -4 0 -3.00 7.00 -5 -4 0 1.70 4.70 5 4 0 -1.20 7.10 -5 4 0 2.40 4.90 5 4 0 1.70 4.80 -6 -4 0 534.35 33.30 6 4 0 526.45 29.50 -6 4 0 563.44 35.20 6 4 0 560.64 43.90 -7 -4 0 889.81 46.30 -7 4 0 848.92 47.40 7 4 0 778.02 40.20 7 4 0 909.61 59.59 -8 -4 0 1014.00 53.69 -8 -4 0 1144.59 50.19 8 4 0 1093.99 50.79 8 4 0 1036.00 67.99 -9 -4 0 186.68 28.20 -9 -4 0 191.98 25.30 9 4 0 204.08 27.00 9 4 0 274.17 42.80 -9 4 0 187.18 28.00 -10 -4 0 31.60 12.30 -10 -4 0 3.30 14.50 -10 -4 0 3.50 9.20 -10 4 0 27.40 13.10 10 4 0 11.80 10.30 10 4 0 14.90 14.80 -11 -4 0 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4.50 12.00 2 4 23 16.80 18.20 -3 0 24 -14.30 8.70 -2 0 24 31.40 13.80 -1 0 24 382.86 37.80 0 0 24 195.48 27.50 1 0 24 23.60 12.30 2 0 24 4.80 9.30 -2 -1 24 23.90 13.20 -2 1 24 17.10 11.20 -1 -1 24 1.00 11.30 -1 1 24 22.50 11.20 0 -1 24 41.30 16.10 0 1 24 19.30 9.90 1 -1 24 40.10 15.50 1 1 24 36.90 12.10 2 -1 24 -1.90 9.80 2 1 24 -9.90 7.30 -1 -2 24 -1.80 10.20 0 -2 24 32.40 16.10 1 -2 24 39.00 15.40 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 85294