data_Badjic_TN_ClosedCH3CN _audit_creation_date 2019-05-13 _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. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C24 H15 Br3 O3, C2 H3 N' _chemical_formula_sum 'C26 H18 Br3 N O3' _chemical_formula_weight 632.14 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 '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' _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 11.0228(6) _cell_length_b 9.1224(6) _cell_length_c 22.8268(14) _cell_angle_alpha 90 _cell_angle_beta 95.723(2) _cell_angle_gamma 90 _cell_volume 2283.9(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9056 _cell_measurement_temperature 100 _cell_measurement_theta_max 28.294 _cell_measurement_theta_min 2.905 _shelx_estimated_absorpt_T_max 0.382 _shelx_estimated_absorpt_T_min 0.275 _exptl_absorpt_coefficient_mu 5.329 _exptl_absorpt_correction_T_max 0.0962 _exptl_absorpt_correction_T_min 0.0466 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1099 before and 0.0465 after correction. The Ratio of minimum to maximum transmission is 0.4844. The \l/2 correction factor is Not present.' _exptl_absorpt_special_details ? _exptl_crystal_colour 'Redish Orange' _exptl_crystal_colour_modifier Redish _exptl_crystal_colour_primary Orange _exptl_crystal_density_diffrn 1.838 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description Block _exptl_crystal_F_000 1240 _exptl_crystal_size_max 0.326 _exptl_crystal_size_mid 0.257 _exptl_crystal_size_min 0.224 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0324 _diffrn_reflns_av_unetI/netI 0.0303 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.959 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 25940 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.959 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 28.293 _diffrn_reflns_theta_min 2.864 _diffrn_ambient_temperature 100.0 _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 0.959 _diffrn_measurement_device 'Kappa Four-Circle Diffractometer' _diffrn_measurement_device_type 'Bruker D8 Venture' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator 'Curved-Graphite, Bruker TRIUMPH' _diffrn_radiation_probe X-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'sealed tube' _diffrn_source_type fine-focus _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 4443 _reflns_number_total 5440 _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 v2017.3-0 (Bruker, 2017)' _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 1.931 _refine_diff_density_min -1.298 _refine_diff_density_rms 0.098 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 301 _refine_ls_number_reflns 5440 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0548 _refine_ls_R_factor_gt 0.0394 _refine_ls_restrained_S_all 1.070 _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^)+(0.0306P)^2^+6.0476P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0856 _refine_ls_wR_factor_ref 0.0907 _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), C16(H16), C20(H20), C21(H21), C23(H23) 2.b Idealised Me refined as rotating group: C24(H24A,H24B,H24C), 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 Br1 Br 0.30908(3) -0.03534(4) 0.91593(2) 0.03040(10) Uani 1 1 d . . . . . Br2 Br 1.07292(3) 0.70953(4) 0.96716(2) 0.03346(10) Uani 1 1 d . . . . . Br3 Br 0.73785(5) -0.12890(5) 0.52018(2) 0.04981(14) Uani 1 1 d . . . . . O1 O 0.7333(2) 0.3583(3) 0.88043(10) 0.0254(5) Uani 1 1 d . . . . . O2 O 0.6731(2) 0.0601(3) 0.76788(10) 0.0254(5) Uani 1 1 d . . . . . O3 O 0.8642(2) 0.5227(3) 0.72490(11) 0.0328(6) Uani 1 1 d . . . . . H3 H 0.909303 0.553407 0.699981 0.049 Uiso 1 1 calc GR . . . . C1 C 0.6361(3) 0.2664(4) 0.88531(14) 0.0218(7) Uani 1 1 d . . . . . C2 C 0.6013(3) 0.2502(4) 0.94199(15) 0.0246(7) Uani 1 1 d . . . . . H2 H 0.643661 0.301361 0.974045 0.030 Uiso 1 1 calc R . . . . C3 C 0.5049(3) 0.1592(4) 0.95119(14) 0.0245(7) Uani 1 1 d . . . . . H3A H 0.481312 0.145615 0.989719 0.029 Uiso 1 1 calc R . . . . C4 C 0.4428(3) 0.0877(4) 0.90337(14) 0.0221(7) Uani 1 1 d . . . . . C5 C 0.4767(3) 0.1037(4) 0.84740(14) 0.0228(7) Uani 1 1 d . . . . . H5 H 0.433047 0.054189 0.815270 0.027 Uiso 1 1 calc R . . . . C6 C 0.5757(3) 0.1932(4) 0.83811(14) 0.0199(6) Uani 1 1 d . . . . . C7 C 0.6189(3) 0.2048(4) 0.77765(14) 0.0209(6) Uani 1 1 d . . . . . C8 C 0.7158(3) 0.3212(4) 0.77699(14) 0.0213(7) Uani 1 1 d . . . . . H8 H 0.741513 0.348411 0.739998 0.026 Uiso 1 1 calc R . . . . C9 C 0.7677(3) 0.3884(4) 0.82480(14) 0.0212(6) Uani 1 1 d . . . . . C10 C 0.8650(3) 0.5000(4) 0.82920(15) 0.0221(7) Uani 1 1 d . . . . . C11 C 0.9112(3) 0.5637(4) 0.77948(15) 0.0240(7) Uani 1 1 d . . . . . C12 C 1.0034(3) 0.6687(4) 0.78673(17) 0.0297(8) Uani 1 1 d . . . . . H12 H 1.033336 0.711040 0.752964 0.036 Uiso 1 1 calc R . . . . C13 C 1.0519(3) 0.7122(4) 0.84192(16) 0.0284(7) Uani 1 1 d . . . . . H13 H 1.114836 0.783715 0.846475 0.034 Uiso 1 1 calc R . . . . C14 C 1.0070(3) 0.6495(4) 0.89074(15) 0.0257(7) Uani 1 1 d . . . . . C15 C 0.9161(3) 0.5459(4) 0.88478(15) 0.0238(7) Uani 1 1 d . . . . . H15 H 0.887362 0.504739 0.919037 0.029 Uiso 1 1 calc R . . . . C16 C 0.5157(3) 0.2338(4) 0.73120(14) 0.0231(7) Uani 1 1 d . . . . . H16 H 0.449950 0.293542 0.740888 0.028 Uiso 1 1 calc R . . . . C17 C 0.5122(3) 0.1794(4) 0.67700(15) 0.0263(7) Uani 1 1 d . . . . . C18 C 0.6083(3) 0.0788(4) 0.66381(15) 0.0264(7) Uani 1 1 d . . . . . C19 C 0.6856(3) 0.0211(4) 0.71041(15) 0.0251(7) Uani 1 1 d . . . . . C20 C 0.7724(3) -0.0836(4) 0.70177(17) 0.0324(8) Uani 1 1 d . . . . . H20 H 0.820889 -0.124416 0.734483 0.039 Uiso 1 1 calc R . . . . C21 C 0.7884(4) -0.1290(4) 0.64499(18) 0.0354(9) Uani 1 1 d . . . . . H21 H 0.848856 -0.199571 0.638283 0.042 Uiso 1 1 calc R . . . . C22 C 0.7151(4) -0.0697(4) 0.59854(17) 0.0366(9) Uani 1 1 d . . . . . C23 C 0.6253(4) 0.0306(4) 0.60649(16) 0.0308(8) Uani 1 1 d . . . . . H23 H 0.574915 0.067277 0.573562 0.037 Uiso 1 1 calc R . . . . C24 C 0.4106(4) 0.2173(5) 0.63030(16) 0.0341(8) Uani 1 1 d . . . . . H24A H 0.443830 0.272168 0.598614 0.051 Uiso 1 1 calc GR . . . . H24B H 0.349749 0.277389 0.647631 0.051 Uiso 1 1 calc GR . . . . H24C H 0.372263 0.126975 0.614294 0.051 Uiso 1 1 calc GR . . . . N1S N 1.0209(4) 0.5869(4) 0.63608(17) 0.0460(9) Uani 1 1 d . . . . . C1S C 1.0872(4) 0.5377(5) 0.60712(19) 0.0376(9) Uani 1 1 d . . . . . C2S C 1.1722(4) 0.4730(5) 0.5699(2) 0.0501(11) Uani 1 1 d . . . . . H2SA H 1.155547 0.510810 0.529735 0.075 Uiso 1 1 calc GR . . . . H2SB H 1.162671 0.366198 0.569618 0.075 Uiso 1 1 calc GR . . . . H2SC H 1.255744 0.498374 0.585281 0.075 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 Br1 0.02782(17) 0.0364(2) 0.02725(18) 0.00224(15) 0.00405(14) -0.01251(16) Br2 0.03379(19) 0.0321(2) 0.03289(19) -0.00217(15) -0.00468(15) -0.00815(16) Br3 0.0766(3) 0.0394(2) 0.0386(2) -0.01467(19) 0.0311(2) -0.0145(2) O1 0.0270(12) 0.0290(13) 0.0204(11) -0.0031(10) 0.0037(9) -0.0100(10) O2 0.0311(12) 0.0217(12) 0.0235(11) -0.0024(10) 0.0038(10) 0.0022(10) O3 0.0417(15) 0.0341(15) 0.0235(12) -0.0009(11) 0.0087(11) -0.0134(12) C1 0.0227(15) 0.0206(16) 0.0222(15) 0.0013(13) 0.0022(13) -0.0013(13) C2 0.0275(16) 0.0252(17) 0.0207(15) -0.0032(13) 0.0004(13) -0.0033(14) C3 0.0262(16) 0.0274(18) 0.0203(15) 0.0001(13) 0.0045(13) 0.0009(14) C4 0.0201(15) 0.0220(17) 0.0247(16) 0.0028(13) 0.0042(13) -0.0045(13) C5 0.0250(16) 0.0200(16) 0.0233(16) -0.0010(13) 0.0021(13) -0.0020(13) C6 0.0216(15) 0.0190(16) 0.0192(15) -0.0004(12) 0.0031(12) 0.0009(13) C7 0.0256(15) 0.0185(16) 0.0188(15) -0.0021(12) 0.0034(13) -0.0005(13) C8 0.0220(15) 0.0214(16) 0.0216(15) 0.0002(13) 0.0070(13) -0.0025(13) C9 0.0228(15) 0.0195(16) 0.0223(15) 0.0015(13) 0.0065(13) -0.0001(13) C10 0.0215(15) 0.0176(16) 0.0277(17) -0.0008(13) 0.0050(13) 0.0006(13) C11 0.0275(16) 0.0194(16) 0.0262(16) -0.0024(13) 0.0074(14) 0.0004(14) C12 0.0304(18) 0.0259(18) 0.0343(19) 0.0032(15) 0.0099(15) -0.0026(15) C13 0.0266(16) 0.0225(18) 0.0366(19) 0.0010(15) 0.0051(15) -0.0061(15) C14 0.0253(16) 0.0220(17) 0.0292(17) -0.0030(14) -0.0009(14) 0.0020(14) C15 0.0237(15) 0.0233(17) 0.0248(16) 0.0009(14) 0.0040(13) -0.0018(14) C16 0.0211(15) 0.0245(17) 0.0240(16) 0.0019(13) 0.0028(13) -0.0026(13) C17 0.0298(17) 0.0247(18) 0.0243(16) 0.0038(14) 0.0017(14) -0.0043(15) C18 0.0297(17) 0.0230(17) 0.0271(17) -0.0024(14) 0.0064(14) -0.0077(14) C19 0.0284(16) 0.0189(16) 0.0292(17) -0.0033(14) 0.0082(14) -0.0046(14) C20 0.0316(19) 0.0266(19) 0.039(2) -0.0007(16) 0.0061(16) 0.0007(16) C21 0.038(2) 0.0233(19) 0.047(2) -0.0058(17) 0.0159(18) -0.0012(16) C22 0.049(2) 0.032(2) 0.0313(19) -0.0080(16) 0.0160(18) -0.0100(18) C23 0.040(2) 0.0273(19) 0.0260(17) -0.0024(15) 0.0086(15) -0.0072(17) C24 0.0342(19) 0.040(2) 0.0270(18) 0.0031(16) -0.0023(15) -0.0011(18) N1S 0.049(2) 0.047(2) 0.045(2) -0.0006(17) 0.0166(18) -0.0084(18) C1S 0.039(2) 0.033(2) 0.041(2) 0.0080(18) 0.0079(18) -0.0085(18) C2S 0.044(2) 0.041(3) 0.068(3) 0.001(2) 0.021(2) 0.000(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 1.897(3) . ? Br2 C14 1.902(3) . ? Br3 C22 1.909(4) . ? O1 C1 1.374(4) . ? O1 C9 1.388(4) . ? O2 C7 1.475(4) . ? O2 C19 1.379(4) . ? O3 H3 0.8400 . ? O3 C11 1.353(4) . ? C1 C2 1.393(5) . ? C1 C6 1.381(4) . ? C2 H2 0.9500 . ? C2 C3 1.381(5) . ? C3 H3A 0.9500 . ? C3 C4 1.392(5) . ? C4 C5 1.374(4) . ? C5 H5 0.9500 . ? C5 C6 1.396(5) . ? C6 C7 1.508(4) . ? C7 C8 1.508(4) . ? C7 C16 1.499(4) . ? C8 H8 0.9500 . ? C8 C9 1.330(5) . ? C9 C10 1.475(5) . ? C10 C11 1.414(5) . ? C10 C15 1.400(5) . ? C11 C12 1.395(5) . ? C12 H12 0.9500 . ? C12 C13 1.377(5) . ? C13 H13 0.9500 . ? C13 C14 1.387(5) . ? C14 C15 1.374(5) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C16 C17 1.330(5) . ? C17 C18 1.455(5) . ? C17 C24 1.507(5) . ? C18 C19 1.398(5) . ? C18 C23 1.411(5) . ? C19 C20 1.380(5) . ? C20 H20 0.9500 . ? C20 C21 1.389(5) . ? C21 H21 0.9500 . ? C21 C22 1.378(6) . ? C22 C23 1.373(6) . ? C23 H23 0.9500 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? N1S C1S 1.126(5) . ? C1S C2S 1.451(6) . ? 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 118.8(3) . . ? C19 O2 C7 117.0(3) . . ? C11 O3 H3 109.5 . . ? O1 C1 C2 115.4(3) . . ? O1 C1 C6 123.4(3) . . ? C6 C1 C2 121.2(3) . . ? C1 C2 H2 120.3 . . ? C3 C2 C1 119.5(3) . . ? C3 C2 H2 120.3 . . ? C2 C3 H3A 120.4 . . ? C2 C3 C4 119.2(3) . . ? C4 C3 H3A 120.4 . . ? C3 C4 Br1 119.2(2) . . ? C5 C4 Br1 119.4(2) . . ? C5 C4 C3 121.4(3) . . ? C4 C5 H5 120.3 . . ? C4 C5 C6 119.5(3) . . ? C6 C5 H5 120.3 . . ? C1 C6 C5 119.2(3) . . ? C1 C6 C7 120.6(3) . . ? C5 C6 C7 120.2(3) . . ? O2 C7 C6 104.2(3) . . ? O2 C7 C8 109.3(3) . . ? O2 C7 C16 110.0(3) . . ? C8 C7 C6 110.3(3) . . ? C16 C7 C6 111.9(3) . . ? C16 C7 C8 110.9(3) . . ? C7 C8 H8 117.9 . . ? C9 C8 C7 124.3(3) . . ? C9 C8 H8 117.9 . . ? O1 C9 C10 109.7(3) . . ? C8 C9 O1 121.7(3) . . ? C8 C9 C10 128.6(3) . . ? C11 C10 C9 123.1(3) . . ? C15 C10 C9 119.5(3) . . ? C15 C10 C11 117.4(3) . . ? O3 C11 C10 119.3(3) . . ? O3 C11 C12 120.4(3) . . ? C12 C11 C10 120.2(3) . . ? C11 C12 H12 119.4 . . ? C13 C12 C11 121.2(3) . . ? C13 C12 H12 119.4 . . ? C12 C13 H13 120.7 . . ? C12 C13 C14 118.6(3) . . ? C14 C13 H13 120.7 . . ? C13 C14 Br2 118.9(3) . . ? C15 C14 Br2 119.8(3) . . ? C15 C14 C13 121.3(3) . . ? C10 C15 H15 119.4 . . ? C14 C15 C10 121.3(3) . . ? C14 C15 H15 119.4 . . ? C7 C16 H16 118.6 . . ? C17 C16 C7 122.7(3) . . ? C17 C16 H16 118.6 . . ? C16 C17 C18 118.3(3) . . ? C16 C17 C24 121.5(3) . . ? C18 C17 C24 120.2(3) . . ? C19 C18 C17 118.7(3) . . ? C19 C18 C23 117.4(3) . . ? C23 C18 C17 123.8(3) . . ? O2 C19 C18 121.1(3) . . ? O2 C19 C20 116.8(3) . . ? C20 C19 C18 122.0(3) . . ? C19 C20 H20 120.2 . . ? C19 C20 C21 119.6(4) . . ? C21 C20 H20 120.2 . . ? C20 C21 H21 120.6 . . ? C22 C21 C20 118.8(4) . . ? C22 C21 H21 120.6 . . ? C21 C22 Br3 119.2(3) . . ? C23 C22 Br3 118.5(3) . . ? C23 C22 C21 122.3(3) . . ? C18 C23 H23 120.2 . . ? C22 C23 C18 119.7(4) . . ? C22 C23 H23 120.2 . . ? C17 C24 H24A 109.5 . . ? C17 C24 H24B 109.5 . . ? C17 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N1S C1S C2S 179.5(5) . . ? 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 2.02 2.852(4) 169.2 . yes C8 H8 O3 0.95 2.14 2.803(4) 125.9 . yes _shelx_res_file ; TITL Badjic_TN_ClosedCH3CN in P2(1)/c badjic_tn_closedch3cn.res created by SHELXL-2018/3 at 12:57:59 on 13-May-2019 REM SHELXT solution in P2(1)/c: R1 0.146, Rweak 0.011, Alpha 0.029 REM 0.898 for 306 systematic absences, Orientation as input REM Formula found by SHELXT: C26 N O3 Br3 CELL 0.71073 11.0228 9.1224 22.8268 90 95.723 90 ZERR 4 0.0006 0.0006 0.0014 0 0.002 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Br N O UNIT 104 72 12 4 12 L.S. 10 PLAN 20 SIZE 0.326 0.257 0.224 TEMP -173.15 HTAB O3 N1S HTAB C8 O3 BOND $H list 4 fmap 2 acta 50 REM REM REM WGHT 0.030600 6.047600 FVAR 0.33494 BR1 3 0.309083 -0.035345 0.915932 11.00000 0.02782 0.03638 = 0.02725 0.00224 0.00405 -0.01251 BR2 3 1.072915 0.709529 0.967160 11.00000 0.03379 0.03208 = 0.03289 -0.00217 -0.00468 -0.00815 BR3 3 0.737847 -0.128903 0.520180 11.00000 0.07655 0.03943 = 0.03856 -0.01467 0.03113 -0.01453 O1 5 0.733341 0.358251 0.880428 11.00000 0.02700 0.02905 = 0.02040 -0.00307 0.00375 -0.01000 O2 5 0.673136 0.060074 0.767877 11.00000 0.03109 0.02174 = 0.02346 -0.00236 0.00381 0.00216 O3 5 0.864182 0.522728 0.724897 11.00000 0.04173 0.03414 = 0.02353 -0.00087 0.00875 -0.01337 AFIX 147 H3 2 0.909303 0.553407 0.699981 11.00000 -1.50000 AFIX 0 C1 1 0.636055 0.266440 0.885310 11.00000 0.02265 0.02056 = 0.02223 0.00135 0.00217 -0.00128 C2 1 0.601349 0.250233 0.941987 11.00000 0.02751 0.02525 = 0.02068 -0.00325 0.00042 -0.00331 AFIX 43 H2 2 0.643661 0.301361 0.974045 11.00000 -1.20000 AFIX 0 C3 1 0.504940 0.159243 0.951189 11.00000 0.02620 0.02745 = 0.02029 0.00006 0.00454 0.00093 AFIX 43 H3A 2 0.481312 0.145615 0.989719 11.00000 -1.20000 AFIX 0 C4 1 0.442770 0.087717 0.903368 11.00000 0.02008 0.02202 = 0.02468 0.00283 0.00419 -0.00455 C5 1 0.476662 0.103679 0.847399 11.00000 0.02504 0.02000 = 0.02333 -0.00097 0.00205 -0.00198 AFIX 43 H5 2 0.433047 0.054189 0.815270 11.00000 -1.20000 AFIX 0 C6 1 0.575687 0.193188 0.838111 11.00000 0.02164 0.01897 = 0.01924 -0.00036 0.00312 0.00093 C7 1 0.618885 0.204788 0.777652 11.00000 0.02559 0.01847 = 0.01877 -0.00209 0.00338 -0.00047 C8 1 0.715821 0.321226 0.776991 11.00000 0.02198 0.02139 = 0.02161 0.00020 0.00704 -0.00246 AFIX 43 H8 2 0.741513 0.348411 0.739998 11.00000 -1.20000 AFIX 0 C9 1 0.767718 0.388371 0.824796 11.00000 0.02276 0.01950 = 0.02228 0.00147 0.00654 -0.00012 C10 1 0.865002 0.499964 0.829196 11.00000 0.02155 0.01760 = 0.02766 -0.00084 0.00499 0.00062 C11 1 0.911173 0.563666 0.779479 11.00000 0.02753 0.01935 = 0.02616 -0.00238 0.00743 0.00038 C12 1 1.003422 0.668728 0.786731 11.00000 0.03041 0.02590 = 0.03428 0.00323 0.00991 -0.00261 AFIX 43 H12 2 1.033336 0.711040 0.752964 11.00000 -1.20000 AFIX 0 C13 1 1.051922 0.712239 0.841922 11.00000 0.02660 0.02248 = 0.03655 0.00103 0.00513 -0.00612 AFIX 43 H13 2 1.114836 0.783715 0.846475 11.00000 -1.20000 AFIX 0 C14 1 1.006985 0.649511 0.890737 11.00000 0.02531 0.02195 = 0.02917 -0.00304 -0.00087 0.00196 C15 1 0.916097 0.545947 0.884781 11.00000 0.02369 0.02327 = 0.02477 0.00094 0.00402 -0.00184 AFIX 43 H15 2 0.887362 0.504739 0.919037 11.00000 -1.20000 AFIX 0 C16 1 0.515661 0.233797 0.731202 11.00000 0.02107 0.02451 = 0.02398 0.00195 0.00279 -0.00263 AFIX 43 H16 2 0.449950 0.293542 0.740888 11.00000 -1.20000 AFIX 0 C17 1 0.512248 0.179376 0.677000 11.00000 0.02980 0.02472 = 0.02428 0.00383 0.00168 -0.00433 C18 1 0.608254 0.078772 0.663812 11.00000 0.02971 0.02304 = 0.02712 -0.00237 0.00639 -0.00773 C19 1 0.685605 0.021126 0.710408 11.00000 0.02835 0.01887 = 0.02921 -0.00328 0.00819 -0.00460 C20 1 0.772387 -0.083594 0.701770 11.00000 0.03157 0.02664 = 0.03939 -0.00070 0.00611 0.00071 AFIX 43 H20 2 0.820889 -0.124416 0.734483 11.00000 -1.20000 AFIX 0 C21 1 0.788417 -0.128964 0.644990 11.00000 0.03774 0.02326 = 0.04743 -0.00583 0.01592 -0.00119 AFIX 43 H21 2 0.848856 -0.199571 0.638283 11.00000 -1.20000 AFIX 0 C22 1 0.715052 -0.069701 0.598539 11.00000 0.04886 0.03210 = 0.03126 -0.00797 0.01598 -0.01004 C23 1 0.625300 0.030551 0.606493 11.00000 0.04000 0.02734 = 0.02600 -0.00243 0.00864 -0.00719 AFIX 43 H23 2 0.574915 0.067277 0.573562 11.00000 -1.20000 AFIX 0 C24 1 0.410634 0.217294 0.630300 11.00000 0.03423 0.03985 = 0.02703 0.00309 -0.00226 -0.00110 AFIX 137 H24A 2 0.443830 0.272168 0.598614 11.00000 -1.50000 H24B 2 0.349749 0.277389 0.647631 11.00000 -1.50000 H24C 2 0.372263 0.126975 0.614294 11.00000 -1.50000 AFIX 0 N1S 4 1.020916 0.586874 0.636080 11.00000 0.04891 0.04661 = 0.04475 -0.00060 0.01663 -0.00838 C1S 1 1.087189 0.537657 0.607121 11.00000 0.03939 0.03338 = 0.04069 0.00796 0.00791 -0.00848 C2S 1 1.172185 0.473014 0.569920 11.00000 0.04418 0.04123 = 0.06804 0.00074 0.02051 -0.00006 AFIX 137 H2SA 2 1.155547 0.510810 0.529735 11.00000 -1.50000 H2SB 2 1.162671 0.366198 0.569618 11.00000 -1.50000 H2SC 2 1.255744 0.498374 0.585281 11.00000 -1.50000 AFIX 0 HKLF 4 REM Badjic_TN_ClosedCH3CN in P2(1)/c REM wR2 = 0.0907, GooF = S = 1.070, Restrained GooF = 1.070 for all data REM R1 = 0.0394 for 4443 Fo > 4sig(Fo) and 0.0548 for all 5440 data REM 301 parameters refined using 0 restraints END WGHT 0.0306 6.0477 REM Highest difference peak 1.931, deepest hole -1.298, 1-sigma level 0.098 Q1 1 0.6507 -0.0692 0.5005 11.00000 0.05 1.93 Q2 1 0.7961 -0.1608 0.5514 11.00000 0.05 0.98 Q3 1 1.0052 0.7091 0.9804 11.00000 0.05 0.78 Q4 1 1.1333 0.6324 0.9613 11.00000 0.05 0.54 Q5 1 0.6459 -0.1579 0.5224 11.00000 0.05 0.48 Q6 1 0.5994 0.1978 0.8090 11.00000 0.05 0.46 Q7 1 0.8753 0.5424 0.8034 11.00000 0.05 0.41 Q8 1 1.0631 0.6984 0.9314 11.00000 0.05 0.40 Q9 1 0.3260 -0.0675 0.8897 11.00000 0.05 0.40 Q10 1 1.0140 0.5731 0.6001 11.00000 0.05 0.39 Q11 1 0.2400 -0.0498 0.9199 11.00000 0.05 0.39 Q12 1 1.0362 0.6577 0.8179 11.00000 0.05 0.38 Q13 1 1.0012 0.6724 0.8603 11.00000 0.05 0.37 Q14 1 0.7449 -0.0313 0.7400 11.00000 0.05 0.37 Q15 1 0.3389 -0.0628 0.9392 11.00000 0.05 0.36 Q16 1 0.5835 0.3905 0.9865 11.00000 0.05 0.36 Q17 1 1.2050 0.5441 0.5518 11.00000 0.05 0.35 Q18 1 0.4711 0.1111 0.8786 11.00000 0.05 0.35 Q19 1 0.3057 0.0437 0.9139 11.00000 0.05 0.35 Q20 1 0.5690 0.2032 0.7478 11.00000 0.05 0.35 ; _shelx_res_checksum 27485 _shelx_hkl_file ; -2 0 0 482.55 13.30 -4 0 0 748.83 21.00 -4 0 0 753.12 21.10 -4 0 0 761.02 21.50 -5 0 0 3768.42 101.89 -6 0 0 638.54 18.80 -6 0 0 624.54 18.80 -6 0 0 674.93 20.00 -6 0 0 664.73 19.10 -7 0 0 -2.80 6.10 -7 0 0 4.30 4.00 -7 0 0 4.50 3.70 -7 0 0 4.20 3.40 -8 0 0 223.28 9.20 -8 0 0 218.68 9.70 -8 0 0 214.88 11.50 -8 0 0 229.38 9.70 -9 0 0 213.28 9.90 -9 0 0 228.98 12.50 -9 0 0 250.07 10.90 -9 0 0 232.58 10.50 -10 0 0 218.38 9.60 -10 0 0 217.48 10.20 -10 0 0 217.98 10.90 -10 0 0 187.88 13.00 -11 0 0 15.20 7.10 -11 0 0 8.20 7.70 -11 0 0 24.50 6.00 -11 0 0 24.30 6.20 -12 0 0 129.89 15.20 -12 0 0 106.29 9.90 -12 0 0 125.49 10.10 -13 0 0 373.36 14.50 -13 0 0 351.56 15.60 -13 0 0 337.77 17.30 -14 0 0 39.60 9.50 -14 0 0 26.50 8.10 -14 0 0 49.30 7.10 -1 -1 0 529.15 13.60 -1 -1 0 466.15 13.90 -2 -1 0 13.90 1.40 -2 -1 0 12.80 1.60 2 -1 0 8.30 1.70 -2 1 0 10.50 1.80 2 1 0 3.80 1.00 -2 1 0 7.40 0.70 2 1 0 9.10 2.00 3 -1 0 4518.35 122.89 -3 -1 0 4801.72 122.79 -3 -1 0 4439.66 122.39 3 -1 0 4506.35 122.79 3 1 0 4783.72 122.69 -3 1 0 4280.87 122.49 3 1 0 4432.06 122.59 -3 1 0 4386.56 122.69 -4 -1 0 2538.75 68.59 4 -1 0 2563.84 68.29 -4 -1 0 2528.45 68.09 4 1 0 2479.45 68.59 -4 1 0 2519.25 68.19 5 -1 0 68.19 5.10 -5 -1 0 66.49 4.50 -5 -1 0 66.29 5.00 -5 1 0 65.19 4.90 -5 1 0 65.89 3.90 -5 1 0 79.39 5.40 -6 -1 0 350.86 11.60 -6 -1 0 354.36 13.00 -6 -1 0 362.76 11.60 -6 1 0 387.96 11.80 -6 1 0 367.46 11.20 -6 1 0 360.96 11.50 -7 -1 0 134.69 9.00 -7 -1 0 138.19 10.40 -7 -1 0 122.99 6.50 -7 -1 0 127.99 6.80 -7 1 0 128.89 7.60 -7 1 0 116.79 5.60 -7 1 0 118.09 6.80 -8 -1 0 57.19 5.90 -8 -1 0 54.39 6.70 -8 -1 0 68.09 6.00 -8 -1 0 55.39 5.90 -8 1 0 69.39 6.20 -8 1 0 62.89 8.50 -8 1 0 83.79 7.60 -8 1 0 53.49 6.70 -9 -1 0 277.17 11.00 -9 -1 0 258.97 10.10 -9 -1 0 266.77 11.60 -9 -1 0 278.97 13.10 -9 1 0 280.87 13.30 -9 1 0 254.67 9.80 -9 1 0 255.17 11.70 -9 1 0 258.87 10.60 -10 -1 0 152.98 10.20 -10 -1 0 166.08 9.40 -10 -1 0 158.98 11.90 -10 -1 0 150.28 9.60 -10 1 0 157.28 12.20 -10 1 0 161.28 10.40 -10 1 0 167.68 9.00 -10 1 0 145.39 8.90 -11 -1 0 18.50 6.90 -11 -1 0 0.00 7.70 -11 -1 0 10.10 4.80 -11 -1 0 16.00 6.00 -11 1 0 14.50 5.50 -11 1 0 12.60 8.00 -11 1 0 16.10 5.00 -11 1 0 7.80 6.80 -12 -1 0 207.48 13.30 -12 -1 0 173.98 11.10 -12 -1 0 172.68 9.20 -12 1 0 168.98 9.20 -12 1 0 172.68 14.10 -12 1 0 185.38 11.50 -13 -1 0 3.50 6.00 -13 -1 0 8.20 7.10 -13 -1 0 2.80 8.50 -13 1 0 -5.50 8.80 -13 1 0 -3.60 7.70 -13 1 0 2.10 5.80 -14 -1 0 3.70 8.10 -14 -1 0 17.20 7.40 -14 -1 0 7.90 8.90 -14 1 0 14.40 8.40 -14 1 0 3.50 11.10 -14 1 0 0.40 9.30 0 -2 0 263.27 8.20 0 -2 0 258.77 8.20 0 2 0 277.17 8.20 0 2 0 269.87 8.30 -1 -2 0 56.09 2.80 1 -2 0 58.09 3.00 -1 -2 0 54.89 2.90 1 2 0 62.99 3.50 1 2 0 61.69 2.50 1 2 0 66.29 3.50 -1 2 0 55.99 2.80 -1 2 0 58.89 3.10 -2 -2 0 5331.57 149.88 -2 -2 0 5420.96 150.18 2 -2 0 5560.74 150.38 -2 2 0 5569.84 150.38 2 2 0 5588.74 150.28 -2 2 0 5384.06 150.18 -3 -2 0 235.98 7.50 3 -2 0 236.18 8.10 -3 -2 0 237.48 7.40 -3 -2 0 232.48 8.20 -3 2 0 229.38 8.00 3 2 0 238.18 7.10 3 2 0 229.18 8.30 4 -2 0 153.78 5.90 -4 -2 0 153.58 6.40 -4 -2 0 155.88 7.20 4 2 0 160.58 7.50 -4 2 0 152.08 6.70 -4 2 0 144.19 4.30 4 2 0 149.19 5.20 -5 -2 0 829.22 23.60 5 -2 0 851.11 24.10 -5 -2 0 827.12 24.40 -5 2 0 823.92 24.00 5 2 0 845.62 24.80 5 2 0 849.81 25.00 6 -2 0 1373.26 37.80 -6 -2 0 1399.66 38.10 -6 -2 0 1352.76 37.30 6 2 0 1303.67 38.40 -6 2 0 1316.17 37.50 6 2 0 1435.66 37.10 -6 2 0 1304.67 36.50 -6 2 0 1304.57 37.40 -7 -2 0 1124.49 31.70 7 -2 0 1136.29 32.30 -7 -2 0 1155.88 32.60 -7 -2 0 1190.08 32.80 -7 2 0 1133.79 35.30 7 2 0 1122.39 33.00 -7 2 0 1092.69 30.90 -7 2 0 1080.09 31.90 -8 -2 0 113.79 8.10 -8 -2 0 99.69 7.00 -8 -2 0 113.89 8.90 8 -2 0 104.09 7.80 -8 -2 0 110.79 9.60 -8 2 0 107.59 8.40 -8 2 0 105.69 5.50 -8 2 0 107.89 7.90 -9 -2 0 375.56 15.00 -9 -2 0 378.56 15.50 -9 -2 0 384.76 14.60 -9 -2 0 389.06 13.10 -9 2 0 399.66 12.30 -9 2 0 400.76 14.80 -9 2 0 399.96 14.00 -10 -2 0 156.08 8.40 -10 -2 0 151.98 10.70 -10 -2 0 168.18 9.50 -10 -2 0 151.98 11.10 -10 2 0 158.78 11.00 -10 2 0 166.88 9.60 -10 2 0 175.18 12.50 -10 2 0 158.88 7.50 -11 -2 0 118.09 9.50 -11 -2 0 127.19 9.70 -11 -2 0 132.59 8.20 -11 2 0 137.69 7.40 -11 2 0 140.09 9.70 -12 -2 0 90.19 7.70 -12 -2 0 97.59 8.90 -12 -2 0 93.19 9.10 -12 -2 0 99.69 9.50 -12 2 0 103.09 10.20 -12 2 0 114.09 9.20 -12 2 0 99.99 9.50 -13 -2 0 28.00 8.70 -13 -2 0 27.20 6.90 -13 -2 0 47.50 6.30 -13 2 0 34.90 7.20 -13 2 0 22.70 14.90 -14 -2 0 125.29 10.50 -14 -2 0 114.89 10.20 -14 -2 0 105.19 10.30 -14 2 0 98.69 11.30 -14 2 0 118.39 10.20 0 -3 0 4.20 2.00 0 -3 0 -0.10 2.80 0 3 0 0.10 3.00 0 3 0 1.40 1.80 -1 -3 0 706.13 20.10 1 -3 0 727.13 19.80 -1 -3 0 719.73 20.30 1 -3 0 710.63 20.20 1 3 0 718.33 20.20 -1 3 0 708.23 20.10 -1 3 0 710.13 20.30 1 3 0 708.33 20.20 2 -3 0 1674.83 44.80 -2 -3 0 1611.14 44.60 -2 -3 0 1633.94 44.50 -2 3 0 1622.54 44.40 2 3 0 1593.44 44.50 2 3 0 1628.54 44.10 2 3 0 1572.04 44.60 -2 3 0 1695.73 44.80 -3 -3 0 678.93 19.30 -3 -3 0 658.93 18.60 3 -3 0 687.83 19.80 -3 -3 0 658.03 19.30 3 3 0 680.43 19.40 3 3 0 664.73 19.30 -3 3 0 686.33 19.80 -4 -3 0 22.50 2.90 -4 -3 0 22.40 3.30 -4 -3 0 19.10 4.20 4 -3 0 18.60 3.10 -4 3 0 17.50 3.20 4 3 0 21.80 4.30 4 3 0 28.00 3.00 -5 -3 0 1557.84 43.50 -5 -3 0 1535.45 43.50 -5 -3 0 1595.74 44.10 5 -3 0 1592.94 44.10 5 3 0 1609.04 43.10 -5 3 0 1627.74 44.10 5 3 0 1582.14 44.30 -6 -3 0 88.39 6.60 6 -3 0 87.49 7.20 6 3 0 90.39 4.50 -6 3 0 95.99 5.80 6 3 0 87.29 6.70 -7 -3 0 389.96 14.40 -7 -3 0 383.46 13.50 7 -3 0 384.46 13.90 -7 -3 0 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1 13 191.98 16.00 -11 1 13 171.78 5.60 -11 1 13 204.48 14.00 -10 -1 13 130.09 7.90 -10 -1 13 135.89 12.00 -10 1 13 123.39 4.00 -10 1 13 118.29 11.20 -10 1 13 123.49 11.00 -9 -1 13 163.78 9.60 -9 -1 13 163.38 12.10 -9 -1 13 161.18 8.50 -9 1 13 156.98 14.40 -9 1 13 167.68 11.20 -8 -1 13 64.79 8.30 -8 -1 13 60.89 5.90 -8 1 13 72.19 7.80 -8 1 13 71.69 18.10 -8 1 13 59.99 6.80 -7 -1 13 307.47 14.10 -7 -1 13 300.77 10.70 7 -1 -13 315.27 12.60 -7 1 13 312.67 13.60 -7 1 13 317.27 15.70 -7 1 13 315.37 11.90 6 -1 -13 145.49 9.40 -6 -1 13 148.39 8.20 -6 -1 13 144.39 10.70 -6 1 13 142.89 8.30 -6 1 13 148.19 10.40 -6 1 13 146.39 4.40 -6 1 13 140.09 12.10 -5 -1 13 24.20 5.10 5 -1 -13 14.50 5.80 -5 -1 13 22.10 6.80 -5 1 13 27.90 5.10 -5 1 13 28.40 2.10 -5 1 13 31.00 7.20 4 -1 -13 -6.10 5.70 -4 -1 13 10.50 4.40 -4 -1 13 5.20 4.60 4 -1 -13 6.70 2.00 -4 1 13 -3.00 4.50 -4 1 13 2.60 2.40 4 1 -13 17.30 6.00 -4 1 13 6.10 6.60 -4 1 13 4.40 4.80 -3 -1 13 375.06 13.10 3 -1 -13 374.96 13.40 -3 -1 13 362.16 14.50 3 -1 -13 374.06 11.30 3 -1 -13 384.16 14.50 3 1 -13 362.06 12.90 -3 1 13 367.66 13.20 -3 1 13 367.86 14.90 3 1 -13 379.36 14.30 3 1 -13 361.76 11.00 -3 1 13 371.66 13.30 2 -1 -13 167.78 10.20 2 -1 -13 162.48 8.30 -2 -1 13 169.08 9.00 -2 -1 13 184.68 10.60 2 -1 -13 161.58 7.20 -2 1 13 172.38 11.00 2 1 -13 174.28 9.90 -2 1 13 171.18 9.80 2 1 -13 163.88 10.00 -2 1 13 165.58 9.20 -2 1 13 167.58 7.40 2 1 -13 181.18 6.60 -1 -1 13 3.10 6.40 -1 -1 13 -2.20 4.90 1 -1 -13 3.70 4.10 1 -1 -13 1.80 4.50 1 -1 -13 0.40 6.40 -1 1 13 21.40 5.90 1 1 -13 6.00 6.20 1 1 -13 0.30 3.90 -1 1 13 1.50 4.80 -1 1 13 0.40 6.80 1 1 -13 -0.20 5.90 -1 1 13 -1.80 3.40 0 -1 13 1956.90 55.89 0 -1 -13 1971.70 56.39 0 -1 13 2033.60 56.49 0 -1 -13 2074.39 56.89 0 -1 -13 2003.60 55.49 0 1 -13 1951.50 54.99 0 1 -13 2136.49 61.79 0 1 13 1920.21 57.19 0 1 13 2068.09 56.79 0 1 13 2007.70 55.19 0 1 13 2002.90 55.19 0 1 -13 1935.01 56.39 -1 -1 -13 47.80 5.50 -1 -1 -13 48.10 7.10 -1 -1 -13 41.80 8.00 1 -1 13 46.40 5.70 -1 1 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-13 429.96 25.00 -7 -1 -13 409.86 18.90 -7 1 -13 434.86 18.10 -7 1 -13 416.56 18.60 -8 -1 -13 230.48 16.10 -8 -1 -13 208.08 15.80 -8 1 -13 204.88 14.70 -8 1 -13 171.58 15.30 -9 -1 -13 31.40 10.00 -9 -1 -13 23.00 7.60 -9 1 -13 0.60 9.10 -9 1 -13 16.80 7.20 -10 -1 -13 274.67 18.70 -10 -1 -13 276.47 17.80 -10 1 -13 276.87 15.10 -10 1 -13 275.97 17.40 -11 -1 -13 8.00 10.70 -11 -1 -13 -3.20 11.40 -11 1 -13 2.70 8.40 -11 1 -13 2.20 8.10 -12 -1 -13 33.20 11.50 -12 1 -13 41.60 11.30 -13 -2 13 2.90 10.50 -13 2 13 8.30 8.30 -13 2 13 2.30 10.60 -12 -2 13 0.60 10.20 -12 -2 13 17.50 9.30 -12 2 13 16.50 6.90 -11 -2 13 -2.80 10.00 -11 -2 13 -0.90 3.60 -11 2 13 9.60 6.70 -11 2 13 5.60 3.90 -11 2 13 2.90 7.00 -10 -2 13 -3.80 3.80 -10 -2 13 -3.40 3.00 -10 -2 13 6.70 8.50 -10 2 13 5.70 6.60 -10 2 13 0.30 2.70 -10 2 13 1.00 3.80 -10 2 13 -1.40 6.70 -9 -2 13 200.28 8.00 -9 -2 13 226.78 13.50 -9 2 13 216.48 13.20 -9 2 13 193.28 12.10 -9 2 13 208.48 7.30 -8 -2 13 138.49 11.60 8 -2 -13 108.09 9.90 -8 -2 13 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541.95 20.70 2 1 -23 530.85 17.60 -2 1 23 581.14 22.60 -1 -1 23 14.10 7.90 1 -1 -23 -1.00 8.20 1 -1 -23 0.40 10.50 -1 1 23 -3.10 10.90 1 1 -23 1.90 5.80 -1 1 23 8.10 7.40 1 1 -23 0.20 9.60 0 -1 23 261.67 14.90 0 -1 -23 273.57 14.10 0 -1 -23 270.27 17.90 0 1 -23 265.47 17.00 0 1 -23 294.47 13.40 0 1 23 283.37 18.50 0 1 23 276.07 13.40 -1 -1 -23 111.19 9.60 1 -1 23 116.09 12.20 -1 -1 -23 122.99 12.60 -1 1 -23 123.19 11.30 1 1 23 125.09 9.80 -1 1 -23 114.19 12.00 -2 -1 -23 30.50 8.20 -2 -1 -23 35.50 8.70 2 -1 23 45.50 8.80 -2 1 -23 31.30 8.30 -2 1 -23 29.10 10.90 2 1 23 47.40 6.80 -3 -1 -23 492.55 21.70 -3 -1 -23 463.95 19.60 -3 1 -23 418.26 21.50 3 1 23 458.65 15.60 -3 1 -23 437.46 19.00 -4 -1 -23 -2.60 9.50 -4 -1 -23 0.50 11.00 4 -1 23 -2.70 4.80 4 1 23 1.70 4.20 -4 1 -23 7.10 8.80 -4 1 -23 -11.60 10.90 4 1 23 2.00 3.90 -5 -1 -23 23.00 7.50 -5 1 -23 19.70 9.70 -6 -1 -23 43.30 12.10 -6 -1 -23 35.40 13.10 -6 1 -23 17.00 12.20 -7 -1 -23 -6.40 10.90 -7 1 -23 -3.20 10.50 -10 2 23 48.70 11.40 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11.10 -1 2 -23 184.18 16.00 2 -2 23 19.50 11.50 -2 -2 -23 39.10 9.20 -2 -2 -23 15.40 11.20 -2 2 -23 24.70 6.00 2 2 23 32.90 5.60 -2 2 -23 18.80 10.70 -3 -2 -23 75.19 10.30 -3 -2 -23 61.59 9.10 3 -2 23 71.79 12.30 -3 2 -23 75.49 12.00 3 2 23 66.49 6.90 -3 2 -23 55.09 9.30 -4 -2 -23 13.70 10.00 -4 -2 -23 8.90 11.30 -4 2 -23 28.00 11.80 4 2 23 14.10 3.70 -4 2 -23 17.90 9.30 -5 -2 -23 23.80 7.70 -5 -2 -23 8.50 13.00 -5 2 -23 26.80 10.00 -6 -2 -23 53.79 9.10 -6 -2 -23 82.89 11.70 -6 2 -23 60.79 8.50 -6 2 -23 52.59 9.60 -7 2 -23 46.60 11.60 -9 3 23 46.80 10.80 -8 -3 23 160.38 13.10 -8 3 23 166.18 14.10 -8 3 23 172.88 15.90 -7 -3 23 27.40 11.50 -7 3 23 6.50 12.90 -7 3 23 39.50 10.90 -6 -3 23 138.99 15.50 -6 3 23 109.79 9.90 -6 3 23 102.39 12.20 -5 -3 23 5.80 11.10 -5 3 23 -4.00 9.90 -5 3 23 0.40 7.10 -5 3 23 0.70 7.60 5 3 -23 -8.20 7.10 4 -3 -23 26.00 6.50 -4 -3 23 19.30 11.20 -4 3 23 21.90 4.80 -4 3 23 42.40 9.80 -4 3 23 33.60 8.40 4 3 -23 25.00 3.60 4 3 -23 22.40 7.50 4 3 -23 26.80 3.80 3 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-27 86.29 9.60 1 -1 27 104.89 11.00 -1 1 -27 87.39 9.10 1 1 27 92.79 10.60 -2 -1 -27 109.89 10.50 -2 -1 -27 102.39 13.20 2 1 27 116.79 9.30 -2 1 -27 103.79 10.00 -2 1 -27 100.59 12.80 3 -1 27 30.80 6.10 -3 -1 -27 22.90 8.80 -3 -1 -27 42.30 9.90 -3 1 -27 31.40 7.10 -3 1 -27 33.90 12.20 3 1 27 30.20 6.30 -4 -1 -27 167.08 16.10 -4 1 -27 172.48 15.40 -5 1 -27 -7.10 10.20 -7 2 27 69.89 12.90 -6 2 27 102.09 13.50 -6 2 27 102.19 12.60 -5 -2 27 220.38 18.50 -5 2 27 204.78 14.60 -5 2 27 177.78 16.90 -4 -2 27 42.60 12.80 4 -2 -27 56.09 6.10 4 2 -27 47.60 9.50 -4 2 27 53.99 10.80 -4 2 27 65.99 9.90 -3 -2 27 249.88 15.60 3 -2 -27 240.28 11.70 3 2 -27 223.08 15.80 -3 2 27 242.88 16.00 -3 2 27 246.48 19.60 2 -2 -27 5.30 6.80 -2 -2 27 -5.70 12.10 -2 2 27 21.90 8.90 2 2 -27 -3.80 9.70 2 2 -27 1.50 5.30 -2 2 27 20.40 12.60 -1 -2 27 51.99 9.80 1 -2 -27 56.79 11.00 1 -2 -27 26.00 9.30 1 2 -27 57.79 7.00 -1 2 27 62.19 8.80 1 2 -27 33.30 10.70 0 -2 -27 24.40 8.50 0 -2 -27 0.60 11.90 0 -2 27 12.70 12.60 0 2 27 15.80 9.00 0 2 -27 14.30 8.90 0 2 -27 12.60 10.70 -1 -2 -27 139.09 14.20 -1 -2 -27 139.19 11.00 1 -2 27 157.68 15.00 1 2 27 159.38 10.70 -1 2 -27 159.48 15.40 -1 2 -27 135.09 12.40 -2 -2 -27 -1.40 9.00 -2 -2 -27 -15.10 11.40 2 -2 27 -14.10 12.20 -2 2 -27 -11.70 8.20 -2 2 -27 4.70 8.20 2 2 27 6.10 5.70 -3 -2 -27 -1.00 11.00 -3 2 -27 -6.10 8.80 -3 2 -27 12.60 11.90 -4 -2 -27 7.50 10.20 -4 2 -27 23.50 7.10 -5 2 -27 8.30 8.20 -7 3 27 95.19 13.30 -6 3 27 91.09 13.40 -5 3 27 35.10 11.20 -5 3 27 32.30 12.60 4 -3 -27 66.19 6.40 4 3 -27 58.49 9.10 3 -3 -27 -12.00 7.90 -3 -3 27 15.00 12.50 3 3 -27 -10.40 10.70 -3 3 27 4.20 9.50 2 -3 -27 194.98 18.90 -2 -3 27 196.38 14.70 2 3 -27 202.68 15.00 2 3 -27 217.08 10.40 -2 3 27 192.08 14.60 1 -3 -27 -6.50 12.10 -1 -3 27 9.50 12.30 1 -3 -27 -5.80 8.10 -1 3 27 -0.60 8.20 1 3 -27 2.40 10.10 1 3 -27 9.30 6.20 0 -3 27 10.60 8.80 0 -3 -27 24.90 9.10 0 -3 -27 3.70 8.80 0 3 27 4.20 7.40 0 3 -27 -20.80 10.20 0 3 -27 5.70 7.00 1 -3 27 89.79 10.50 -1 -3 -27 77.99 10.30 -1 -3 -27 85.99 13.40 1 3 27 66.99 8.80 -1 3 -27 83.59 8.70 2 -3 27 21.10 12.50 -2 -3 -27 4.70 9.50 2 3 27 -3.00 6.90 -2 3 -27 11.10 8.40 -2 3 -27 -15.30 11.10 3 -3 27 32.50 9.40 -3 -3 -27 18.10 7.50 -3 3 -27 32.90 9.60 -3 3 -27 8.40 11.90 -4 -3 -27 -13.70 10.40 -4 3 -27 7.50 9.80 -5 4 27 3.30 10.80 4 -4 -27 17.30 7.90 -4 4 27 46.50 10.70 4 4 -27 23.40 8.00 3 -4 -27 142.79 12.80 -3 4 27 149.09 12.00 3 4 -27 145.89 12.20 2 -4 -27 7.20 8.30 -2 -4 27 7.60 14.30 2 4 -27 6.50 6.60 -2 4 27 10.20 9.10 2 4 -27 2.90 8.90 -1 -4 27 29.80 9.40 1 -4 -27 16.40 9.00 -1 4 27 25.00 8.50 1 4 -27 16.10 9.80 1 4 -27 14.40 9.30 0 -4 27 3.70 12.20 0 -4 -27 2.80 9.50 0 4 27 -4.50 7.40 0 4 -27 -1.00 7.20 0 4 -27 1.90 10.20 1 -4 27 102.59 13.90 -1 -4 -27 84.59 11.10 1 4 27 85.59 10.80 -1 4 -27 83.09 9.10 2 -4 27 92.79 13.70 -2 -4 -27 87.99 9.00 -2 4 -27 81.39 9.70 -2 4 -27 82.59 12.40 -3 -4 -27 13.30 10.50 3 -4 27 9.10 12.30 -3 4 -27 22.10 9.40 4 -5 -27 194.88 12.80 -4 5 27 202.58 16.90 3 -5 -27 -8.40 8.30 3 5 -27 2.50 7.70 -3 5 27 7.40 10.00 2 -5 -27 -0.10 9.30 -2 5 27 5.10 9.10 2 5 -27 16.40 8.80 1 -5 -27 57.49 10.50 -1 5 27 52.39 9.40 1 5 -27 73.89 10.30 1 5 -27 61.79 8.80 0 -5 -27 62.89 11.00 0 5 -27 79.49 8.40 0 5 27 53.79 10.30 0 5 -27 78.29 11.10 -1 -5 -27 15.10 10.70 -1 5 -27 18.40 11.00 -1 5 -27 33.70 8.40 1 5 27 10.50 8.60 -5 0 28 239.38 17.60 -4 0 28 73.19 13.80 -4 0 28 79.69 11.30 3 0 -28 -2.10 5.90 -3 0 28 9.80 9.60 3 0 -28 -5.70 10.60 -3 0 28 -0.90 12.70 -2 0 28 350.96 17.20 2 0 -28 302.47 16.10 -2 0 28 366.16 21.40 -1 0 28 245.58 14.90 -1 0 28 256.67 15.90 0 0 -28 46.40 8.80 0 0 -28 35.10 7.90 0 0 28 28.50 8.00 0 0 28 57.29 13.70 -1 0 -28 201.18 18.00 1 0 28 204.18 12.30 -1 0 -28 198.38 13.90 2 0 28 70.69 8.30 -2 0 -28 66.79 9.60 -2 0 -28 76.19 9.80 -3 0 -28 59.59 11.50 -4 0 -28 33.40 10.10 -5 -1 28 100.39 12.30 -5 1 28 102.39 12.10 -4 -1 28 111.09 11.80 4 1 -28 92.19 11.30 -4 1 28 119.99 14.20 -4 1 28 128.09 13.60 3 -1 -28 2.70 6.50 -3 -1 28 16.20 12.60 -3 1 28 1.70 12.50 -3 1 28 5.60 9.40 3 1 -28 -9.60 10.10 -2 -1 28 4.80 12.70 2 -1 -28 -14.00 7.60 -2 1 28 8.80 12.80 2 1 -28 -5.30 10.50 2 1 -28 -1.10 5.40 -2 1 28 -2.80 8.80 1 -1 -28 46.10 12.00 -1 -1 28 47.00 13.10 1 -1 -28 17.30 13.10 1 1 -28 21.40 11.00 -1 1 28 25.30 9.50 1 1 -28 23.40 6.70 -1 1 28 40.60 8.80 0 -1 -28 -8.90 7.60 0 -1 -28 15.80 11.90 0 -1 28 37.50 13.10 0 1 28 12.70 7.60 0 1 -28 15.40 7.30 1 -1 28 9.50 13.10 -1 -1 -28 6.60 8.40 -1 -1 -28 14.80 11.80 1 1 28 12.30 6.80 -1 1 -28 15.30 8.10 -1 1 -28 13.90 11.40 -2 -1 -28 91.39 10.40 2 -1 28 125.09 10.60 -2 1 -28 89.09 13.10 -2 1 -28 120.29 10.30 2 1 28 130.49 11.30 3 -1 28 13.20 5.90 -3 1 -28 17.10 9.50 -4 -1 -28 11.80 10.10 -4 1 -28 32.50 10.00 -5 2 28 111.09 12.30 -5 2 28 127.29 16.80 -4 2 28 95.29 11.70 4 2 -28 73.39 10.20 -4 2 28 108.69 14.10 3 -2 -28 12.40 7.20 -3 2 28 15.00 9.60 -3 2 28 15.40 13.00 3 2 -28 -2.30 9.70 -2 -2 28 15.10 10.70 2 -2 -28 12.10 11.90 2 -2 -28 9.90 8.40 2 2 -28 4.00 6.30 2 2 -28 -16.70 9.80 -2 2 28 11.60 9.00 -1 -2 28 195.58 18.70 1 -2 -28 175.98 14.90 1 2 -28 178.08 16.10 -1 2 28 206.98 13.80 1 2 -28 179.38 13.00 0 -2 -28 57.69 12.80 0 -2 -28 37.90 8.80 0 -2 28 43.30 13.40 0 2 -28 50.69 9.10 0 2 28 55.39 8.10 1 -2 28 9.50 9.10 -1 -2 -28 -3.30 8.70 -1 -2 -28 -1.80 9.70 1 2 28 17.40 8.30 -1 2 -28 5.40 7.90 -1 2 -28 21.10 11.10 -2 -2 -28 1.20 6.50 2 2 28 11.10 7.10 -2 2 -28 -25.10 11.30 -2 2 -28 7.30 8.60 -3 -2 -28 32.80 10.10 -5 3 28 -0.10 10.80 4 3 -28 24.00 8.70 -4 3 28 39.20 10.60 3 -3 -28 -14.20 8.00 3 3 -28 -14.10 9.00 -3 3 28 9.00 9.80 2 -3 -28 4.80 7.60 -2 3 28 16.70 9.10 2 3 -28 1.10 9.50 2 3 -28 17.50 7.90 1 -3 -28 8.30 8.30 1 -3 -28 2.50 10.10 1 3 -28 7.00 6.40 1 3 -28 0.80 10.00 -1 3 28 -4.40 8.10 0 -3 -28 96.29 10.20 0 3 -28 94.09 9.80 0 3 28 103.29 9.00 -1 -3 -28 7.80 9.20 -1 3 -28 10.80 7.90 1 3 28 5.60 6.60 -1 3 -28 -11.10 10.80 -2 3 -28 -7.90 8.20 -2 3 -28 -9.60 11.20 -3 -3 -28 117.19 11.70 -3 3 -28 107.49 10.90 4 4 -28 -26.90 9.60 -4 4 28 2.10 10.30 3 -4 -28 26.80 7.70 3 4 -28 27.90 8.90 -3 4 28 13.10 10.00 2 -4 -28 -4.10 8.30 -2 4 28 -3.20 9.00 2 4 -28 10.40 9.30 1 -4 -28 10.50 9.10 -1 4 28 16.00 8.60 1 4 -28 19.50 6.60 1 4 -28 15.90 9.90 0 -4 -28 15.90 9.60 0 4 28 30.00 7.90 0 4 -28 27.60 9.20 0 4 -28 19.60 20.10 -1 4 -28 48.20 11.60 -1 4 -28 74.39 9.00 1 4 28 62.69 7.70 -4 0 29 1.50 7.10 2 0 -29 -4.00 5.80 2 0 -29 -14.30 10.90 -2 0 29 -2.70 8.90 1 0 -29 -0.50 13.00 -1 0 29 8.00 8.20 1 0 -29 -4.00 11.20 0 0 29 -7.00 7.60 0 0 -29 -5.90 7.30 0 0 -29 -1.30 11.30 1 0 29 5.80 7.00 -1 0 -29 2.40 8.10 -1 0 -29 -14.40 9.10 -2 0 -29 -6.10 8.50 2 0 29 -4.20 6.20 -3 0 -29 0.70 9.20 -4 -1 29 -10.70 10.20 -4 1 29 16.70 10.40 4 1 -29 -4.00 9.80 3 -1 -29 -3.80 8.20 -3 -1 29 -8.40 6.80 3 1 -29 -7.20 10.20 -2 -1 29 -1.80 9.20 2 -1 -29 3.10 6.40 2 -1 -29 7.00 11.90 2 1 -29 4.70 6.40 -2 1 29 2.90 8.70 1 -1 -29 -0.90 7.10 -1 -1 29 5.60 8.60 1 -1 -29 3.40 8.20 1 1 -29 -2.40 10.80 -1 1 29 1.00 8.20 1 1 -29 21.70 7.60 0 -1 -29 68.09 8.70 0 -1 29 82.69 9.30 0 -1 -29 86.49 15.00 0 1 29 90.79 8.80 0 1 -29 67.69 8.40 0 1 -29 79.19 9.40 1 -1 29 90.19 8.80 -1 -1 -29 83.09 9.50 -1 1 -29 82.09 12.90 1 1 29 87.49 8.10 -1 1 -29 98.79 9.40 -2 -1 -29 2.40 8.90 2 -1 29 9.90 6.70 -2 1 -29 9.30 8.70 -4 2 29 165.38 16.00 4 2 -29 143.69 11.60 -3 2 29 12.80 8.00 3 2 -29 -9.40 9.60 2 -2 -29 4.90 12.10 2 -2 -29 2.30 12.60 -2 2 29 19.60 9.00 2 2 -29 3.90 10.30 1 -2 -29 136.29 12.40 1 2 -29 130.49 14.60 -1 2 29 131.19 12.80 0 -2 -29 -17.20 8.30 0 2 29 -2.00 9.10 0 2 -29 -11.70 8.70 0 2 -29 -8.90 10.80 -1 -2 -29 41.50 9.20 -1 2 -29 31.00 8.60 1 2 29 47.50 7.30 -1 2 -29 30.90 8.30 -2 2 -29 -1.70 8.80 4 3 -29 9.60 8.70 -4 3 29 26.40 10.50 -3 3 29 80.49 10.80 3 3 -29 38.80 9.80 2 -3 -29 274.27 16.40 2 3 -29 274.17 16.60 1 -3 -29 44.80 10.60 -1 3 29 30.40 8.80 0 -3 -29 38.00 9.30 0 3 -29 29.70 7.60 0 3 29 15.30 9.40 0 3 -29 22.80 11.10 -1 -3 -29 19.50 9.60 -1 3 -29 10.70 9.60 -1 3 -29 7.10 11.20 1 3 29 11.20 6.90 -3 0 30 128.49 11.70 3 0 -30 110.99 10.10 2 0 -30 338.47 20.00 1 0 -30 111.49 10.70 -1 0 30 85.99 9.90 1 0 -30 93.39 13.10 0 0 -30 39.00 9.60 0 0 30 31.90 8.20 1 0 30 22.90 8.90 -1 0 -30 10.20 8.40 3 -1 -30 14.30 11.60 -3 -1 30 19.50 10.30 -3 1 30 32.10 9.90 3 1 -30 6.20 10.60 -2 -1 30 31.60 9.90 -2 1 30 15.40 17.40 2 1 -30 12.70 11.10 1 -1 -30 5.80 7.10 -1 -1 30 12.90 9.10 1 1 -30 -9.30 10.80 1 1 -30 -5.70 6.50 -1 1 30 -1.50 8.10 0 -1 -30 28.10 8.10 0 -1 30 19.10 8.50 0 1 -30 25.50 9.10 0 1 30 25.30 7.90 2 2 -30 -12.20 10.00 1 -2 -30 9.60 9.40 -1 2 30 -17.60 8.20 1 2 -30 -2.30 10.40 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 77057 _olex2_submission_special_instructions 'No special instructions were received'