data_Badjic_TN_ChloroClosed _audit_creation_date 2020-03-18 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number '2018/3' _audit_contact_author_address ? _audit_contact_author_email ? _audit_contact_author_name '' _audit_contact_author_phone ? _publ_contact_author_id_orcid ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C24 H15 Cl3 O3, C2 H3 N' _chemical_formula_sum 'C26 H18 Cl3 N O3' _chemical_formula_weight 498.76 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system 'monoclinic' _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' 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 10.7830(2) _cell_length_b 9.0950(2) _cell_length_c 22.4992(4) _cell_angle_alpha 90 _cell_angle_beta 96.6440(10) _cell_angle_gamma 90 _cell_volume 2191.71(7) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9899 _cell_measurement_temperature 100 _cell_measurement_theta_max 74.526 _cell_measurement_theta_min 3.956 _shelx_estimated_absorpt_T_max 0.647 _shelx_estimated_absorpt_T_min 0.503 _exptl_absorpt_coefficient_mu 4.043 _exptl_absorpt_correction_T_max 0.3260 _exptl_absorpt_correction_T_min 0.1942 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0748 before and 0.0456 after correction. The Ratio of minimum to maximum transmission is 0.5957. The \l/2 correction factor is Not present.' _exptl_absorpt_special_details ? _exptl_crystal_colour Colorless _exptl_crystal_colour_primary Colorless _exptl_crystal_density_diffrn 1.512 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description Block _exptl_crystal_F_000 1024 _exptl_crystal_size_max 0.197 _exptl_crystal_size_mid 0.153 _exptl_crystal_size_min 0.118 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0269 _diffrn_reflns_av_unetI/netI 0.0196 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.981 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 20163 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.981 _diffrn_reflns_theta_full 68.000 _diffrn_reflns_theta_max 74.555 _diffrn_reflns_theta_min 3.956 _diffrn_ambient_temperature 100 _diffrn_detector 'Bruker Photon II area detector' _diffrn_detector_area_resol_mean 10.5 _diffrn_detector_type 'CMOS area detector' _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.981 _diffrn_measurement_device 'Kappa Four-Circle Diffractometer' _diffrn_measurement_device_type 'Bruker D8 Venture' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator 'Double Bounce Multilayer Mirrors' _diffrn_radiation_probe X-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_source 'microfocus sealed X-ray tube' _diffrn_source_type 'Incoatec I\mus' _diffrn_special_details ? _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 4146 _reflns_number_total 4420 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT V8.38A (Bruker, 2017)' _computing_data_collection 'APEX3 v2018.7-2 (Bruker, 2018)' _computing_data_reduction 'SAINT V8.38A (Bruker, 2017)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 1.052 _refine_diff_density_min -0.547 _refine_diff_density_rms 0.057 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 301 _refine_ls_number_reflns 4420 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0386 _refine_ls_R_factor_gt 0.0359 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0428P)^2^+1.9865P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0923 _refine_ls_wR_factor_ref 0.0946 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 2.a Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3A), C5(H5), C8(H8), C12(H12), C13(H13), C15(H15), C17(H17), C21(H21), C22(H22), C24(H24) 2.b Idealised Me refined as rotating group: C16(H16A,H16B,H16C), C2S(H2SA,H2SB,H2SC) 2.c Idealised tetrahedral OH refined as rotating group: O3(H3) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_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 Cl1 Cl 0.25793(6) -0.12611(6) 0.47587(2) 0.04164(15) Uani 1 1 d . . . . . Cl2 Cl 0.69029(4) -0.02915(5) 0.08372(2) 0.02871(12) Uani 1 1 d . . . . . Cl3 Cl -0.07632(4) 0.70219(5) 0.03396(2) 0.02846(12) Uani 1 1 d . . . . . O1 O 0.32876(12) 0.05289(14) 0.23127(5) 0.0223(3) Uani 1 1 d . . . . . O2 O 0.26650(11) 0.35388(14) 0.11697(5) 0.0227(3) Uani 1 1 d . . . . . O3 O 0.13495(13) 0.51777(15) 0.27486(6) 0.0281(3) Uani 1 1 d . . . . . H3 H 0.090510 0.551144 0.300043 0.042 Uiso 1 1 calc GR . . . . C1 C 0.31443(17) 0.0154(2) 0.28929(8) 0.0234(4) Uani 1 1 d . . . . . C2 C 0.22537(18) -0.0900(2) 0.29755(9) 0.0281(4) Uani 1 1 d . . . . . H2 H 0.176196 -0.131578 0.263958 0.034 Uiso 1 1 calc R . . . . C3 C 0.20797(19) -0.1349(2) 0.35516(9) 0.0318(4) Uani 1 1 d . . . . . H3A H 0.146608 -0.206506 0.361374 0.038 Uiso 1 1 calc R . . . . C4 C 0.2818(2) -0.0733(2) 0.40324(9) 0.0316(4) Uani 1 1 d . . . . . C5 C 0.37360(19) 0.0280(2) 0.39567(8) 0.0287(4) Uani 1 1 d . . . . . H5 H 0.424230 0.066541 0.429450 0.034 Uiso 1 1 calc R . . . . C6 C 0.39195(17) 0.0741(2) 0.33779(8) 0.0242(4) Uani 1 1 d . . . . . C7 C 0.49186(17) 0.1745(2) 0.32519(8) 0.0242(4) Uani 1 1 d . . . . . C8 C 0.49011(16) 0.2275(2) 0.26968(8) 0.0219(3) Uani 1 1 d . . . . . H8 H 0.558271 0.285765 0.260241 0.026 Uiso 1 1 calc R . . . . C9 C 0.38380(16) 0.19794(18) 0.22153(7) 0.0195(3) Uani 1 1 d . . . . . C10 C 0.42770(15) 0.18694(19) 0.16068(7) 0.0189(3) Uani 1 1 d . . . . . C11 C 0.36580(15) 0.26190(19) 0.11228(7) 0.0200(3) Uani 1 1 d . . . . . C12 C 0.40163(16) 0.2473(2) 0.05495(8) 0.0226(4) Uani 1 1 d . . . . . H12 H 0.358333 0.299231 0.022275 0.027 Uiso 1 1 calc R . . . . C13 C 0.50057(16) 0.1566(2) 0.04612(8) 0.0225(3) Uani 1 1 d . . . . . H13 H 0.524988 0.144373 0.007179 0.027 Uiso 1 1 calc R . . . . C14 C 0.56432(16) 0.0832(2) 0.09475(8) 0.0216(3) Uani 1 1 d . . . . . C15 C 0.52923(16) 0.09770(19) 0.15154(7) 0.0212(3) Uani 1 1 d . . . . . H15 H 0.573903 0.047246 0.184254 0.025 Uiso 1 1 calc R . . . . C16 C 0.59388(18) 0.2144(2) 0.37376(8) 0.0307(4) Uani 1 1 d . . . . . H16A H 0.657267 0.273288 0.356769 0.046 Uiso 1 1 calc GR . . . . H16B H 0.632281 0.124528 0.391462 0.046 Uiso 1 1 calc GR . . . . H16C H 0.558622 0.271486 0.404718 0.046 Uiso 1 1 calc GR . . . . C17 C 0.28547(15) 0.31471(19) 0.22219(7) 0.0197(3) Uani 1 1 d . . . . . H17 H 0.259611 0.341496 0.259670 0.024 Uiso 1 1 calc R . . . . C18 C 0.23224(15) 0.38310(19) 0.17326(7) 0.0195(3) Uani 1 1 d . . . . . C19 C 0.13270(15) 0.49593(19) 0.16876(8) 0.0202(3) Uani 1 1 d . . . . . C20 C 0.08645(16) 0.5598(2) 0.21901(8) 0.0226(3) Uani 1 1 d . . . . . C21 C -0.00701(17) 0.6662(2) 0.21149(8) 0.0253(4) Uani 1 1 d . . . . . H21 H -0.036391 0.709076 0.245741 0.030 Uiso 1 1 calc R . . . . C22 C -0.05780(17) 0.7106(2) 0.15507(8) 0.0249(4) Uani 1 1 d . . . . . H22 H -0.121955 0.782658 0.150288 0.030 Uiso 1 1 calc R . . . . C23 C -0.01303(16) 0.6476(2) 0.10563(8) 0.0231(4) Uani 1 1 d . . . . . C24 C 0.07998(16) 0.54266(19) 0.11168(8) 0.0220(3) Uani 1 1 d . . . . . H24 H 0.108778 0.501479 0.076978 0.026 Uiso 1 1 calc R . . . . N1S N -0.02194(18) 0.5776(2) 0.36563(8) 0.0378(4) Uani 1 1 d . . . . . C1S C -0.08534(19) 0.5317(2) 0.39816(9) 0.0311(4) Uani 1 1 d . . . . . C2S C -0.1656(2) 0.4715(3) 0.44012(11) 0.0386(5) Uani 1 1 d . . . . . H2SA H -0.252946 0.494716 0.426247 0.058 Uiso 1 1 calc GR . . . . H2SB H -0.142885 0.514861 0.479761 0.058 Uiso 1 1 calc GR . . . . H2SC H -0.154958 0.364615 0.442520 0.058 Uiso 1 1 calc GR . . . . 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 Cl1 0.0604(3) 0.0376(3) 0.0313(3) 0.0130(2) 0.0240(2) 0.0137(2) Cl2 0.0260(2) 0.0380(3) 0.0225(2) -0.00251(17) 0.00430(16) 0.01096(17) Cl3 0.0293(2) 0.0279(2) 0.0266(2) 0.00234(16) -0.00373(16) 0.00424(17) O1 0.0277(6) 0.0203(6) 0.0193(6) 0.0013(5) 0.0042(5) -0.0022(5) O2 0.0251(6) 0.0265(7) 0.0168(6) 0.0019(5) 0.0039(4) 0.0070(5) O3 0.0358(7) 0.0312(7) 0.0186(6) 0.0008(5) 0.0082(5) 0.0098(6) C1 0.0263(8) 0.0209(9) 0.0242(8) 0.0045(7) 0.0080(7) 0.0063(7) C2 0.0301(9) 0.0234(9) 0.0318(10) 0.0015(7) 0.0074(7) 0.0021(7) C3 0.0359(10) 0.0238(10) 0.0385(11) 0.0066(8) 0.0161(8) 0.0027(8) C4 0.0419(11) 0.0293(10) 0.0262(9) 0.0083(8) 0.0153(8) 0.0110(8) C5 0.0350(10) 0.0292(10) 0.0229(9) 0.0029(7) 0.0077(7) 0.0091(8) C6 0.0273(9) 0.0243(9) 0.0214(8) 0.0023(7) 0.0050(7) 0.0080(7) C7 0.0263(9) 0.0258(9) 0.0206(8) -0.0016(7) 0.0028(7) 0.0053(7) C8 0.0214(8) 0.0242(9) 0.0204(8) -0.0019(7) 0.0034(6) 0.0017(7) C9 0.0231(8) 0.0177(8) 0.0179(8) 0.0011(6) 0.0035(6) -0.0004(6) C10 0.0210(8) 0.0187(8) 0.0171(8) -0.0013(6) 0.0029(6) -0.0024(6) C11 0.0197(8) 0.0203(8) 0.0201(8) -0.0005(6) 0.0032(6) 0.0001(6) C12 0.0250(8) 0.0246(9) 0.0180(8) 0.0011(7) 0.0016(6) 0.0007(7) C13 0.0246(8) 0.0263(9) 0.0174(8) -0.0020(7) 0.0058(6) -0.0007(7) C14 0.0196(8) 0.0234(9) 0.0221(8) -0.0029(7) 0.0039(6) 0.0018(6) C15 0.0229(8) 0.0215(9) 0.0188(8) 0.0005(6) 0.0012(6) 0.0002(7) C16 0.0312(10) 0.0372(11) 0.0227(9) -0.0033(8) -0.0013(7) 0.0032(8) C17 0.0210(8) 0.0205(8) 0.0182(8) -0.0004(6) 0.0048(6) -0.0007(6) C18 0.0199(8) 0.0200(8) 0.0194(8) -0.0020(6) 0.0054(6) -0.0021(6) C19 0.0204(8) 0.0182(8) 0.0223(8) 0.0001(6) 0.0034(6) -0.0013(6) C20 0.0249(8) 0.0209(9) 0.0227(8) 0.0018(7) 0.0055(7) -0.0008(7) C21 0.0260(9) 0.0237(9) 0.0273(9) -0.0018(7) 0.0081(7) 0.0009(7) C22 0.0230(8) 0.0206(9) 0.0312(9) 0.0016(7) 0.0033(7) 0.0020(7) C23 0.0225(8) 0.0219(9) 0.0241(8) 0.0020(7) -0.0003(6) -0.0015(7) C24 0.0226(8) 0.0214(9) 0.0223(8) -0.0009(7) 0.0037(6) -0.0018(7) N1S 0.0418(10) 0.0378(10) 0.0358(9) 0.0003(8) 0.0127(8) 0.0061(8) C1S 0.0337(10) 0.0279(10) 0.0324(10) -0.0043(8) 0.0072(8) 0.0047(8) C2S 0.0375(11) 0.0350(12) 0.0461(12) -0.0020(9) 0.0165(9) -0.0016(9) _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 Cl1 C4 1.7506(19) . ? Cl2 C14 1.7403(17) . ? Cl3 C23 1.7487(18) . ? O1 C1 1.375(2) . ? O1 C9 1.473(2) . ? O2 C11 1.372(2) . ? O2 C18 1.386(2) . ? O3 H3 0.8400 . ? O3 C20 1.359(2) . ? C1 C2 1.384(3) . ? C1 C6 1.401(3) . ? C2 H2 0.9500 . ? C2 C3 1.392(3) . ? C3 H3A 0.9500 . ? C3 C4 1.385(3) . ? C4 C5 1.377(3) . ? C5 H5 0.9500 . ? C5 C6 1.404(3) . ? C6 C7 1.465(3) . ? C7 C8 1.337(3) . ? C7 C16 1.503(3) . ? C8 H8 0.9500 . ? C8 C9 1.508(2) . ? C9 C10 1.503(2) . ? C9 C17 1.502(2) . ? C10 C11 1.389(2) . ? C10 C15 1.397(2) . ? C11 C12 1.395(2) . ? C12 H12 0.9500 . ? C12 C13 1.381(2) . ? C13 H13 0.9500 . ? C13 C14 1.394(2) . ? C14 C15 1.380(2) . ? C15 H15 0.9500 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17 0.9500 . ? C17 C18 1.335(2) . ? C18 C19 1.480(2) . ? C19 C20 1.412(2) . ? C19 C24 1.409(2) . ? C20 C21 1.393(3) . ? C21 H21 0.9500 . ? C21 C22 1.383(3) . ? C22 H22 0.9500 . ? C22 C23 1.387(3) . ? C23 C24 1.380(3) . ? C24 H24 0.9500 . ? N1S C1S 1.137(3) . ? C1S C2S 1.459(3) . ? C2S H2SA 0.9800 . ? C2S H2SB 0.9800 . ? C2S H2SC 0.9800 . ? 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 C1 O1 C9 117.06(13) . . ? C11 O2 C18 118.69(13) . . ? C20 O3 H3 109.5 . . ? O1 C1 C2 117.08(17) . . ? O1 C1 C6 121.48(16) . . ? C2 C1 C6 121.32(17) . . ? C1 C2 H2 120.1 . . ? C1 C2 C3 119.90(19) . . ? C3 C2 H2 120.1 . . ? C2 C3 H3A 120.6 . . ? C4 C3 C2 118.76(19) . . ? C4 C3 H3A 120.6 . . ? C3 C4 Cl1 119.00(16) . . ? C5 C4 Cl1 118.97(16) . . ? C5 C4 C3 122.03(17) . . ? C4 C5 H5 120.2 . . ? C4 C5 C6 119.66(19) . . ? C6 C5 H5 120.2 . . ? C1 C6 C5 118.26(18) . . ? C1 C6 C7 118.21(16) . . ? C5 C6 C7 123.46(17) . . ? C6 C7 C16 120.19(16) . . ? C8 C7 C6 118.31(16) . . ? C8 C7 C16 121.49(18) . . ? C7 C8 H8 118.8 . . ? C7 C8 C9 122.32(16) . . ? C9 C8 H8 118.8 . . ? O1 C9 C8 109.78(13) . . ? O1 C9 C10 104.52(13) . . ? O1 C9 C17 109.55(13) . . ? C10 C9 C8 111.90(14) . . ? C17 C9 C8 110.24(14) . . ? C17 C9 C10 110.69(14) . . ? C11 C10 C9 120.55(15) . . ? C11 C10 C15 118.92(15) . . ? C15 C10 C9 120.51(15) . . ? O2 C11 C10 123.20(15) . . ? O2 C11 C12 115.55(15) . . ? C10 C11 C12 121.26(16) . . ? C11 C12 H12 120.3 . . ? C13 C12 C11 119.43(16) . . ? C13 C12 H12 120.3 . . ? C12 C13 H13 120.3 . . ? C12 C13 C14 119.49(16) . . ? C14 C13 H13 120.3 . . ? C13 C14 Cl2 119.44(13) . . ? C15 C14 Cl2 119.37(14) . . ? C15 C14 C13 121.19(16) . . ? C10 C15 H15 120.2 . . ? C14 C15 C10 119.70(16) . . ? C14 C15 H15 120.2 . . ? C7 C16 H16A 109.5 . . ? C7 C16 H16B 109.5 . . ? C7 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C9 C17 H17 118.0 . . ? C18 C17 C9 123.91(15) . . ? C18 C17 H17 118.0 . . ? O2 C18 C19 109.78(14) . . ? C17 C18 O2 121.99(15) . . ? C17 C18 C19 128.23(15) . . ? C20 C19 C18 123.44(15) . . ? C24 C19 C18 118.98(15) . . ? C24 C19 C20 117.57(16) . . ? O3 C20 C19 119.36(16) . . ? O3 C20 C21 120.22(16) . . ? C21 C20 C19 120.41(16) . . ? C20 C21 H21 119.4 . . ? C22 C21 C20 121.20(17) . . ? C22 C21 H21 119.4 . . ? C21 C22 H22 120.7 . . ? C21 C22 C23 118.56(17) . . ? C23 C22 H22 120.7 . . ? C22 C23 Cl3 119.17(14) . . ? C24 C23 Cl3 119.28(14) . . ? C24 C23 C22 121.55(16) . . ? C19 C24 H24 119.6 . . ? C23 C24 C19 120.71(16) . . ? C23 C24 H24 119.6 . . ? N1S C1S C2S 179.3(2) . . ? C1S C2S H2SA 109.5 . . ? C1S C2S H2SB 109.5 . . ? C1S C2S H2SC 109.5 . . ? H2SA C2S H2SB 109.5 . . ? H2SA C2S H2SC 109.5 . . ? H2SB C2S H2SC 109.5 . . ? 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 _geom_hbond_publ_flag O3 H3 N1S 0.84 2.03 2.851(2) 165.6 . yes _shelx_res_file ; TITL Badjic_TN_ChloroClosed in P2(1)/c badjic_tn_chloroclosed.res created by SHELXL-2018/3 at 17:38:04 on 18-Mar-2020 REM SHELXT solution in P2(1)/c: R1 0.128, Rweak 0.005, Alpha 0.019 REM 0.724 for 283 systematic absences, Orientation as input REM Formula found by SHELXT: C26 N O3 Cl3 CELL 1.54178 10.783 9.095 22.4992 90 96.644 90 ZERR 4 0.0002 0.0002 0.0004 0 0.001 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Cl N O UNIT 104 72 12 4 12 L.S. 10 PLAN 20 SIZE 0.197 0.153 0.118 TEMP -173.15 HTAB O3 N1S BOND $H list 4 fmap 2 acta 136 REM REM REM WGHT 0.042800 1.986500 FVAR 0.48537 CL1 3 0.257929 -0.126109 0.475875 11.00000 0.06042 0.03758 = 0.03130 0.01299 0.02398 0.01374 CL2 3 0.690294 -0.029153 0.083720 11.00000 0.02603 0.03797 = 0.02249 -0.00251 0.00430 0.01096 CL3 3 -0.076316 0.702194 0.033957 11.00000 0.02930 0.02787 = 0.02658 0.00234 -0.00373 0.00424 O1 5 0.328762 0.052888 0.231270 11.00000 0.02770 0.02031 = 0.01931 0.00125 0.00421 -0.00216 O2 5 0.266498 0.353878 0.116967 11.00000 0.02506 0.02646 = 0.01681 0.00192 0.00394 0.00700 O3 5 0.134952 0.517769 0.274861 11.00000 0.03575 0.03119 = 0.01860 0.00083 0.00817 0.00982 AFIX 147 H3 2 0.090510 0.551144 0.300043 11.00000 -1.50000 AFIX 0 C1 1 0.314430 0.015355 0.289285 11.00000 0.02628 0.02095 = 0.02424 0.00454 0.00797 0.00632 C2 1 0.225368 -0.089998 0.297546 11.00000 0.03006 0.02340 = 0.03177 0.00153 0.00736 0.00210 AFIX 43 H2 2 0.176196 -0.131578 0.263958 11.00000 -1.20000 AFIX 0 C3 1 0.207967 -0.134931 0.355158 11.00000 0.03592 0.02384 = 0.03848 0.00664 0.01606 0.00275 AFIX 43 H3A 2 0.146608 -0.206506 0.361374 11.00000 -1.20000 AFIX 0 C4 1 0.281799 -0.073315 0.403243 11.00000 0.04188 0.02934 = 0.02623 0.00832 0.01533 0.01097 C5 1 0.373596 0.028013 0.395670 11.00000 0.03502 0.02918 = 0.02295 0.00286 0.00769 0.00907 AFIX 43 H5 2 0.424230 0.066541 0.429450 11.00000 -1.20000 AFIX 0 C6 1 0.391950 0.074058 0.337787 11.00000 0.02734 0.02435 = 0.02139 0.00234 0.00499 0.00804 C7 1 0.491864 0.174493 0.325190 11.00000 0.02627 0.02584 = 0.02059 -0.00165 0.00283 0.00532 C8 1 0.490115 0.227463 0.269680 11.00000 0.02136 0.02419 = 0.02044 -0.00186 0.00340 0.00174 AFIX 43 H8 2 0.558271 0.285765 0.260241 11.00000 -1.20000 AFIX 0 C9 1 0.383803 0.197945 0.221527 11.00000 0.02306 0.01768 = 0.01793 0.00115 0.00347 -0.00036 C10 1 0.427704 0.186944 0.160680 11.00000 0.02097 0.01873 = 0.01715 -0.00128 0.00286 -0.00241 C11 1 0.365797 0.261896 0.112278 11.00000 0.01966 0.02028 = 0.02014 -0.00046 0.00317 0.00013 C12 1 0.401627 0.247266 0.054955 11.00000 0.02502 0.02460 = 0.01802 0.00113 0.00156 0.00067 AFIX 43 H12 2 0.358333 0.299231 0.022275 11.00000 -1.20000 AFIX 0 C13 1 0.500571 0.156600 0.046115 11.00000 0.02462 0.02626 = 0.01742 -0.00200 0.00584 -0.00065 AFIX 43 H13 2 0.524988 0.144373 0.007179 11.00000 -1.20000 AFIX 0 C14 1 0.564323 0.083180 0.094753 11.00000 0.01964 0.02339 = 0.02206 -0.00287 0.00387 0.00181 C15 1 0.529228 0.097703 0.151536 11.00000 0.02295 0.02151 = 0.01884 0.00047 0.00115 0.00016 AFIX 43 H15 2 0.573903 0.047246 0.184254 11.00000 -1.20000 AFIX 0 C16 1 0.593879 0.214420 0.373758 11.00000 0.03120 0.03719 = 0.02271 -0.00332 -0.00126 0.00317 AFIX 137 H16A 2 0.657267 0.273288 0.356769 11.00000 -1.50000 H16B 2 0.632281 0.124528 0.391462 11.00000 -1.50000 H16C 2 0.558622 0.271486 0.404718 11.00000 -1.50000 AFIX 0 C17 1 0.285468 0.314714 0.222192 11.00000 0.02105 0.02052 = 0.01820 -0.00040 0.00479 -0.00073 AFIX 43 H17 2 0.259611 0.341496 0.259670 11.00000 -1.20000 AFIX 0 C18 1 0.232239 0.383102 0.173265 11.00000 0.01993 0.01997 = 0.01937 -0.00198 0.00545 -0.00208 C19 1 0.132704 0.495935 0.168765 11.00000 0.02038 0.01821 = 0.02230 0.00014 0.00344 -0.00125 C20 1 0.086448 0.559849 0.219008 11.00000 0.02486 0.02087 = 0.02269 0.00183 0.00547 -0.00077 C21 1 -0.007007 0.666226 0.211494 11.00000 0.02600 0.02370 = 0.02728 -0.00176 0.00815 0.00087 AFIX 43 H21 2 -0.036391 0.709076 0.245741 11.00000 -1.20000 AFIX 0 C22 1 -0.057799 0.710595 0.155065 11.00000 0.02304 0.02059 = 0.03119 0.00165 0.00328 0.00200 AFIX 43 H22 2 -0.121955 0.782658 0.150288 11.00000 -1.20000 AFIX 0 C23 1 -0.013028 0.647595 0.105629 11.00000 0.02247 0.02193 = 0.02415 0.00204 -0.00031 -0.00148 C24 1 0.079981 0.542663 0.111682 11.00000 0.02263 0.02138 = 0.02230 -0.00087 0.00374 -0.00176 AFIX 43 H24 2 0.108778 0.501479 0.076978 11.00000 -1.20000 AFIX 0 N1S 4 -0.021943 0.577600 0.365628 11.00000 0.04176 0.03775 = 0.03579 0.00026 0.01268 0.00611 C1S 1 -0.085343 0.531729 0.398155 11.00000 0.03373 0.02793 = 0.03235 -0.00434 0.00717 0.00474 C2S 1 -0.165625 0.471538 0.440116 11.00000 0.03746 0.03495 = 0.04610 -0.00199 0.01646 -0.00162 AFIX 137 H2SA 2 -0.252946 0.494716 0.426247 11.00000 -1.50000 H2SB 2 -0.142885 0.514861 0.479761 11.00000 -1.50000 H2SC 2 -0.154958 0.364615 0.442520 11.00000 -1.50000 AFIX 0 HKLF 4 REM Badjic_TN_ChloroClosed in P2(1)/c REM wR2 = 0.0946, GooF = S = 1.053, Restrained GooF = 1.053 for all data REM R1 = 0.0359 for 4146 Fo > 4sig(Fo) and 0.0386 for all 4420 data REM 301 parameters refined using 0 restraints END WGHT 0.0428 1.9865 REM Highest difference peak 1.052, deepest hole -0.547, 1-sigma level 0.057 Q1 1 0.3601 -0.0576 0.4973 11.00000 0.05 1.05 Q2 1 0.2062 -0.1751 0.4478 11.00000 0.05 0.36 Q3 1 0.4083 0.1960 0.1892 11.00000 0.05 0.35 Q4 1 0.4364 0.1992 0.2502 11.00000 0.05 0.33 Q5 1 0.3339 0.2640 0.2219 11.00000 0.05 0.32 Q6 1 0.4977 0.1107 0.4222 11.00000 0.05 0.30 Q7 1 0.4371 0.1203 0.3273 11.00000 0.05 0.29 Q8 1 0.4045 0.2335 0.1402 11.00000 0.05 0.28 Q9 1 0.3448 0.0505 0.3181 11.00000 0.05 0.26 Q10 1 0.1817 0.4395 0.1732 11.00000 0.05 0.26 Q11 1 0.3796 0.2463 0.0829 11.00000 0.05 0.25 Q12 1 0.1100 0.5224 0.1933 11.00000 0.05 0.25 Q13 1 0.4748 0.2374 0.3000 11.00000 0.05 0.24 Q14 1 0.2602 0.0397 0.2104 11.00000 0.05 0.23 Q15 1 0.5471 0.1020 0.1224 11.00000 0.05 0.23 Q16 1 0.1061 0.5229 0.1421 11.00000 0.05 0.23 Q17 1 0.5114 0.1651 0.3702 11.00000 0.05 0.23 Q18 1 0.4349 0.1825 0.0514 11.00000 0.05 0.22 Q19 1 0.5095 0.1696 0.2891 11.00000 0.05 0.22 Q20 1 0.4694 0.1288 0.1560 11.00000 0.05 0.21 ; _shelx_res_checksum 26655 _shelx_hkl_file ; 1 0 0 316.57 7.30 1 0 0 326.47 7.50 1 0 0 315.07 8.50 1 0 0 323.97 9.30 -1 0 0 321.17 9.20 2 0 0 16.90 1.60 2 0 0 17.80 2.60 2 0 0 16.20 2.00 -2 0 0 17.10 2.50 3 0 0 1630.54 39.30 -3 0 0 1737.33 42.00 4 0 0 257.57 12.20 -4 0 0 258.47 14.10 4 0 0 261.67 9.10 5 0 0 1614.64 36.40 -5 0 0 1630.24 48.20 5 0 0 1582.44 43.00 -6 0 0 435.46 11.70 6 0 0 467.85 21.10 6 0 0 508.55 15.60 -6 0 0 468.95 24.80 -7 0 0 15.00 2.10 -7 0 0 23.60 5.20 8 0 0 14.80 3.70 -8 0 0 12.70 2.00 9 0 0 128.69 6.10 -9 0 0 131.89 6.00 9 0 0 137.29 5.90 -10 0 0 249.08 8.80 10 0 0 251.07 8.50 10 0 0 260.57 9.10 11 0 0 28.00 2.60 -11 0 0 26.10 2.50 12 0 0 184.88 6.50 -12 0 0 208.38 7.50 -13 0 0 230.88 6.40 13 0 0 241.38 6.60 0 -1 0 1.50 0.70 0 1 0 2.20 0.60 0 1 0 1.50 0.50 1 -1 0 1065.29 24.70 1 -1 0 1050.39 25.50 -1 -1 0 1012.50 23.90 -1 1 0 1043.90 20.30 1 1 0 1079.59 21.80 1 1 0 1022.40 24.90 1 1 0 1053.09 22.90 -1 1 0 1026.70 20.90 -1 1 0 1072.09 21.80 1 1 0 1075.49 23.20 2 -1 0 258.27 11.40 -2 -1 0 252.57 10.50 -2 1 0 253.87 10.80 2 1 0 264.17 9.20 2 1 0 269.77 9.00 2 1 0 262.67 11.10 2 1 0 264.47 8.00 2 1 0 264.37 6.00 3 -1 0 2709.83 51.09 -3 -1 0 2719.83 61.99 3 -1 0 2611.54 62.59 3 1 0 2796.32 57.09 3 1 0 2826.02 54.59 3 1 0 2793.92 57.49 -3 1 0 2882.81 63.49 -4 -1 0 2218.18 56.19 4 -1 0 2370.16 73.69 4 -1 0 2108.79 41.90 -4 1 0 2199.68 56.59 4 1 0 2238.78 51.59 4 1 0 2196.68 47.10 4 1 0 2216.18 49.30 -5 -1 0 76.79 3.60 5 -1 0 75.19 8.40 -5 -1 0 78.49 8.60 5 1 0 69.29 5.20 -5 1 0 71.69 8.30 5 1 0 79.29 6.30 5 1 0 84.39 5.90 -6 -1 0 253.57 8.00 6 -1 0 264.27 8.20 -6 -1 0 253.57 17.80 6 -1 0 262.27 16.80 6 1 0 259.87 12.50 -6 1 0 272.47 18.80 6 1 0 251.97 12.40 -7 -1 0 7.80 3.80 7 -1 0 3.60 5.20 7 -1 0 3.10 1.20 -7 -1 0 2.70 1.20 7 1 0 3.20 1.80 -8 -1 0 7.30 1.50 -8 -1 0 6.70 1.30 8 -1 0 4.10 2.10 8 -1 0 10.40 2.40 9 -1 0 39.80 3.40 9 -1 0 45.30 3.50 -9 -1 0 43.60 3.50 -9 1 0 33.30 3.10 9 1 0 40.30 3.30 9 1 0 39.80 5.40 10 -1 0 99.49 5.00 10 -1 0 93.99 5.40 -10 -1 0 88.79 4.40 10 1 0 92.39 5.00 -10 1 0 95.89 5.00 -11 -1 0 0.60 0.80 11 -1 0 3.90 1.30 11 -1 0 0.80 0.70 11 1 0 1.80 0.90 -11 1 0 1.90 0.80 12 -1 0 35.00 3.50 -12 -1 0 34.90 2.30 12 -1 0 26.30 2.90 12 1 0 33.30 2.30 -12 1 0 33.40 2.40 13 -1 0 0.00 0.40 -13 1 0 -0.50 0.40 13 1 0 0.00 0.50 0 -2 0 806.22 21.80 0 2 0 797.32 19.00 0 2 0 805.32 19.40 0 2 0 835.62 20.00 -1 -2 0 682.93 20.60 -1 -2 0 675.53 16.70 1 -2 0 676.03 21.50 -1 2 0 722.43 16.90 1 2 0 639.84 21.20 -1 2 0 690.73 16.20 1 2 0 680.33 16.90 1 2 0 683.23 18.40 1 2 0 699.73 18.40 -1 2 0 741.43 18.00 2 -2 0 3918.91 84.39 -2 -2 0 3623.64 80.29 -2 2 0 3998.40 73.99 2 2 0 3797.32 77.79 2 2 0 3938.61 75.89 -3 -2 0 109.39 8.20 3 -2 0 116.49 9.30 3 2 0 113.49 6.30 3 2 0 111.19 6.80 3 2 0 117.49 7.20 -3 2 0 108.19 4.50 -4 -2 0 569.94 22.80 4 -2 0 568.34 24.60 4 2 0 528.45 17.20 4 2 0 521.65 18.20 4 2 0 556.04 19.30 -5 -2 0 936.91 34.40 -5 -2 0 940.61 20.40 5 -2 0 905.21 34.70 5 -2 0 990.20 21.60 5 2 0 921.51 28.60 -5 2 0 913.51 21.70 5 2 0 955.50 30.10 5 2 0 923.31 28.30 -6 -2 0 654.83 15.80 -6 -2 0 648.34 29.80 6 -2 0 641.24 15.90 6 -2 0 606.74 30.00 6 2 0 633.34 22.30 6 2 0 651.03 23.80 7 -2 0 465.45 14.30 -7 -2 0 525.55 13.90 -7 -2 0 559.14 30.70 7 -2 0 500.15 13.70 -7 -2 0 528.45 12.80 7 -2 0 512.35 29.10 7 2 0 495.85 21.40 7 2 0 504.15 21.20 -8 -2 0 154.18 6.60 -8 -2 0 151.18 5.70 8 -2 0 150.98 5.80 8 -2 0 152.48 6.60 9 -2 0 392.66 10.80 9 -2 0 385.86 12.40 9 -2 0 409.26 12.00 -9 -2 0 385.66 10.60 -9 -2 0 384.06 12.00 9 2 0 381.66 11.40 -9 2 0 390.66 11.60 -10 -2 0 0.90 1.50 -10 -2 0 0.50 1.50 -10 2 0 0.40 1.30 -11 -2 0 61.19 3.20 11 -2 0 60.79 3.60 11 -2 0 59.39 3.80 11 2 0 56.89 3.40 -11 2 0 55.69 3.80 12 -2 0 55.39 2.80 -12 2 0 52.99 2.80 12 2 0 50.79 2.90 -13 2 0 63.79 2.50 13 2 0 66.49 2.50 0 -3 0 -0.60 1.10 0 -3 0 -1.00 1.00 0 3 0 0.40 0.80 0 3 0 -1.20 0.60 -1 -3 0 867.01 28.10 1 -3 0 971.90 29.80 -1 -3 0 963.20 24.70 -1 3 0 953.60 23.50 -1 3 0 953.70 23.20 1 3 0 933.41 25.50 1 3 0 874.81 27.30 1 3 0 953.90 24.10 -1 3 0 975.90 23.20 -2 -3 0 831.22 17.20 -2 -3 0 777.42 17.60 -2 -3 0 813.72 26.50 2 -3 0 865.51 29.60 2 3 0 843.92 24.00 2 3 0 830.82 24.70 2 3 0 816.82 22.00 -2 3 0 829.92 19.20 -2 3 0 841.12 20.80 -3 -3 0 443.46 19.00 3 -3 0 440.66 21.80 3 3 0 426.26 15.10 -3 3 0 449.66 12.90 3 3 0 447.06 17.40 3 3 0 460.35 17.20 -4 -3 0 140.99 4.80 -4 -3 0 132.39 11.00 4 -3 0 141.19 12.70 4 -3 0 133.19 4.80 -4 3 0 128.59 5.70 4 3 0 124.49 9.20 4 3 0 134.69 8.10 4 3 0 121.69 8.70 5 -3 0 975.40 21.20 -5 -3 0 898.91 35.00 5 -3 0 954.00 39.20 -5 -3 0 961.00 20.70 5 3 0 955.70 31.00 5 3 0 936.11 28.40 5 3 0 897.01 29.70 -6 -3 0 11.40 3.20 6 -3 0 5.50 3.40 6 3 0 6.90 2.00 6 3 0 2.60 2.00 -7 -3 0 218.18 7.30 -7 -3 0 213.88 7.80 7 -3 0 208.58 6.90 7 -3 0 210.78 7.90 7 3 0 219.18 13.90 7 3 0 210.48 14.30 8 -3 0 49.80 3.30 8 -3 0 51.59 3.80 -8 -3 0 51.79 3.70 -8 -3 0 48.80 3.20 8 3 0 60.19 6.90 9 -3 0 2.10 1.00 -9 -3 0 0.80 1.00 9 -3 0 0.70 0.80 9 -3 0 2.80 1.10 -9 -3 0 3.20 1.00 9 3 0 2.30 1.00 -9 3 0 4.00 1.20 -10 -3 0 465.15 11.90 -10 -3 0 463.55 13.40 10 -3 0 466.55 12.90 10 -3 0 479.95 12.10 10 3 0 464.35 12.70 -10 3 0 471.95 12.60 -11 -3 0 61.19 5.30 -11 -3 0 63.49 3.10 11 -3 0 65.79 3.60 11 3 0 65.29 3.50 -11 3 0 60.99 3.30 12 -3 0 4.50 0.90 12 3 0 3.90 0.70 -12 3 0 5.80 1.00 0 -4 0 263.87 15.80 0 -4 0 287.97 14.30 0 4 0 259.47 10.70 0 4 0 278.27 12.30 0 4 0 269.47 12.00 1 -4 0 16.50 3.80 -1 -4 0 9.70 3.60 1 4 0 8.10 2.60 1 4 0 9.80 2.60 -1 4 0 11.60 2.30 1 4 0 10.20 2.60 -1 4 0 9.90 2.10 -1 4 0 15.30 2.60 -2 -4 0 300.67 10.50 -2 -4 0 310.17 15.70 2 -4 0 290.87 17.70 -2 -4 0 283.37 9.40 -2 4 0 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80.69 4.60 7 -3 9 75.49 4.70 -7 -3 -9 81.89 4.80 -7 -3 -9 82.49 4.20 7 -3 9 78.89 4.30 7 3 9 77.69 4.70 -7 3 -9 78.79 4.40 -8 -3 -9 12.70 1.80 -8 -3 -9 8.40 1.60 8 -3 9 8.60 1.70 8 -3 9 8.00 1.80 8 -3 9 7.60 1.40 -8 3 -9 10.70 2.00 8 3 9 10.20 1.80 -9 -3 -9 20.20 3.00 9 -3 9 18.00 2.30 9 -3 9 17.20 2.10 9 -3 9 19.80 2.20 -9 -3 -9 14.10 2.00 9 3 9 21.20 2.30 -9 3 -9 24.60 2.40 10 -3 9 95.49 4.40 -10 -3 -9 95.99 4.70 10 3 9 96.49 4.30 -10 3 -9 92.99 4.20 11 -3 9 127.69 4.20 -11 3 -9 127.39 4.20 11 3 9 129.09 4.60 11 3 9 131.79 4.20 12 -4 -9 105.99 3.70 -12 4 9 116.49 4.40 -11 -4 9 53.49 3.60 11 -4 -9 50.79 3.00 -11 4 9 57.19 2.90 10 -4 -9 11.60 1.70 -10 -4 9 16.90 2.10 10 4 -9 14.40 1.70 -10 4 9 18.10 3.20 -9 -4 9 118.69 6.10 9 -4 -9 114.49 5.20 -9 -4 9 120.79 5.20 9 -4 -9 110.69 5.60 9 -4 -9 125.89 6.50 -9 4 9 122.49 5.40 9 4 -9 123.59 5.20 -9 4 9 116.39 5.80 8 -4 -9 44.60 3.70 8 -4 -9 34.90 3.10 -8 -4 9 40.30 3.20 -8 4 9 39.60 3.20 -8 4 9 41.40 3.60 8 4 -9 41.50 3.10 -7 -4 9 106.09 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9 -4 9 35.80 2.60 9 4 9 37.80 3.30 -9 4 -9 39.20 3.60 -10 -4 -9 19.10 1.50 10 -4 9 13.80 1.70 -10 4 -9 15.90 1.60 10 4 9 16.10 1.70 10 4 9 13.80 1.80 11 -4 9 38.70 2.50 11 4 9 32.50 2.20 11 4 9 32.60 1.40 -11 4 -9 31.30 1.60 11 -5 -9 2.20 0.70 -11 -5 9 1.30 0.60 -11 5 9 2.00 0.50 10 -5 -9 98.69 4.40 -10 -5 9 96.49 4.70 10 -5 -9 99.09 3.90 -10 -5 9 101.49 4.10 -10 5 9 95.59 3.90 -9 -5 9 247.18 8.90 9 -5 -9 247.98 9.50 9 -5 -9 249.48 8.50 9 -5 -9 243.68 7.90 -9 5 9 246.48 7.70 -9 5 9 261.77 9.70 8 -5 -9 10.30 1.70 8 -5 -9 13.60 2.20 -8 -5 9 8.90 1.70 8 -5 -9 8.20 1.80 -8 -5 9 9.60 1.70 8 5 -9 10.40 1.70 -8 5 9 8.10 1.80 -8 5 9 11.10 1.70 -7 -5 9 8.00 1.40 -7 -5 9 6.50 2.70 7 -5 -9 7.40 1.70 7 -5 -9 6.00 2.60 7 -5 -9 7.40 1.80 -7 5 9 7.90 1.60 -7 5 9 7.10 1.80 7 5 -9 8.10 1.30 6 -5 -9 61.39 3.80 -6 -5 9 61.79 3.80 6 -5 -9 58.99 4.40 -6 -5 9 62.29 4.10 6 -5 -9 51.29 4.20 6 5 -9 62.69 3.50 -6 5 9 57.29 4.30 6 5 -9 62.39 3.60 -6 5 9 58.09 3.50 -5 -5 9 110.49 5.00 -5 -5 9 116.89 5.60 5 -5 -9 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1 26 119.09 4.50 -2 1 -26 120.89 4.00 -3 -1 -26 1.90 0.40 -3 1 -26 1.20 0.40 3 1 26 1.10 0.50 5 -2 -26 31.90 2.00 5 2 -26 30.50 2.00 -5 2 26 30.50 1.70 4 -2 -26 69.99 2.90 4 -2 -26 72.09 2.50 -4 2 26 69.69 2.90 4 2 -26 68.59 2.90 3 -2 -26 1.00 0.50 3 -2 -26 0.60 0.80 3 2 -26 0.30 0.40 -3 2 26 0.60 0.40 2 -2 -26 3.00 0.60 2 -2 -26 3.10 0.60 -2 2 26 2.00 0.70 2 2 -26 3.30 0.80 1 -2 -26 139.79 4.40 1 -2 -26 139.29 4.70 1 2 -26 135.39 4.60 -1 2 26 141.99 4.80 0 -2 -26 47.40 3.10 0 -2 -26 54.69 2.50 0 2 -26 53.99 2.60 0 2 26 50.99 2.60 -1 -2 -26 2.40 0.50 -1 -2 -26 3.50 0.90 -1 2 -26 3.80 0.70 1 2 26 3.30 0.60 -2 2 -26 12.80 1.10 2 2 26 14.10 1.70 3 2 26 25.50 1.40 -3 2 -26 30.00 1.40 5 3 -26 23.40 1.20 -5 3 26 23.60 1.40 5 3 -26 23.90 1.40 4 -3 -26 1.80 0.40 4 3 -26 2.00 0.40 -4 3 26 1.10 0.70 3 -3 -26 73.99 3.40 3 3 -26 76.29 2.70 -3 3 26 77.99 3.00 2 -3 -26 109.99 4.40 -2 3 26 121.39 4.00 2 3 -26 113.49 3.60 1 -3 -26 14.50 1.50 1 3 -26 14.00 1.10 -1 3 26 17.00 1.40 0 3 -26 13.00 1.10 0 3 26 12.50 1.30 -1 -3 -26 12.40 1.00 1 3 26 13.70 1.60 -1 3 -26 13.20 1.30 -2 -3 -26 24.20 1.80 2 3 26 26.90 1.40 -2 3 -26 28.90 1.30 3 -4 -26 186.58 4.80 -3 4 26 187.68 4.70 2 -4 -26 0.30 0.30 -2 4 26 0.60 0.30 1 -4 -26 15.20 1.10 -1 4 26 15.20 1.00 0 -4 -26 77.09 2.60 0 4 26 81.19 2.60 5 0 -27 0.00 0.20 4 0 -27 -0.10 0.30 3 0 -27 -0.40 0.30 -3 0 27 0.00 0.60 -2 0 27 -0.40 0.50 1 0 -27 0.50 0.40 0 0 -27 -0.90 0.50 0 0 27 -0.70 0.40 1 0 27 -0.20 0.40 -1 0 -27 -0.20 0.30 -2 0 -27 -0.30 0.20 5 -1 -27 11.50 0.90 5 1 -27 11.70 0.90 4 -1 -27 72.59 2.90 -4 1 27 76.19 2.80 4 1 -27 91.39 3.60 3 -1 -27 7.60 1.00 -3 1 27 6.90 1.10 3 1 -27 6.80 0.90 2 -1 -27 14.30 1.30 -2 1 27 17.40 1.40 2 1 -27 16.30 1.40 1 -1 -27 250.07 6.80 1 1 -27 257.97 6.80 -1 1 27 259.57 6.80 0 -1 -27 2.80 0.50 0 1 -27 1.40 0.60 -1 -1 -27 50.59 2.40 1 1 27 54.09 2.30 -1 1 -27 56.69 2.40 -2 1 -27 68.29 2.50 2 1 27 63.89 2.40 -4 2 27 96.29 3.10 4 2 -27 93.99 2.90 3 2 -27 169.38 5.40 -3 2 27 172.38 4.90 -2 2 27 37.90 1.90 2 2 -27 39.80 2.20 -1 2 27 0.00 0.40 1 2 -27 0.30 0.30 0 2 -27 3.90 0.70 0 2 27 2.70 0.60 1 2 27 158.38 4.40 -1 2 -27 156.18 4.20 2 3 -27 22.30 1.10 -2 3 27 21.10 1.30 1 3 -27 16.80 0.90 -1 3 27 16.30 1.10 2 0 -28 2.20 0.50 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 54734 _olex2_submission_special_instructions 'No special instructions were received'