#============================================================================= data_global loop_ _journal_name_full 'European Journal of Chemistry' _journal_coden_ASTM EJCUA9 _journal_volume 13 _journal_issue 2 _journal_year 2022 _journal_page_first 206 _journal_page_last 213 #============================================================================= data_shelx _audit_creation_date 2022-03-09 _audit_creation_method ; Olex2 1.3-beta (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272) ; _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 ? _chemical_name_common ? _chemical_name_systematic ; 2-aminobenzothiazol 4-fluorobenzoic ; _chemical_formula_moiety 'C7 H6 N2 S, C7 H5 O2 F' _chemical_formula_sum 'C14 H11 F N2 O2 S' _chemical_formula_weight 290.31 _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' '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' 'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0727 0.0534 '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 11.7869(14) _cell_length_b 4.0326(5) _cell_length_c 27.625(3) _cell_angle_alpha 90 _cell_angle_beta 92.731(10) _cell_angle_gamma 90 _cell_volume 1311.6(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 1244 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 66.3820 _cell_measurement_theta_min 3.7480 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 2.345 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.74606 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour orange _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.470 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 600 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0262 _diffrn_reflns_av_unetI/netI 0.0413 _diffrn_reflns_Laue_measured_fraction_full 0.975 _diffrn_reflns_Laue_measured_fraction_max 0.975 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_k_min -3 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 3568 _diffrn_reflns_point_group_measured_fraction_full 0.975 _diffrn_reflns_point_group_measured_fraction_max 0.975 _diffrn_reflns_theta_full 67.101 _diffrn_reflns_theta_max 67.101 _diffrn_reflns_theta_min 3.754 _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 15.9974 _diffrn_measured_fraction_theta_full 0.975 _diffrn_measured_fraction_theta_max 0.975 _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Eos' _diffrn_measurement_method '\w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_source 'micro-focus sealed X-ray tube' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 1748 _reflns_number_total 2280 _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 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_molecular_graphics 'Olex2 1.3-beta (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3-beta (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _refine_diff_density_max 0.221 _refine_diff_density_min -0.276 _refine_diff_density_rms 0.047 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 189 _refine_ls_number_reflns 2280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0615 _refine_ls_R_factor_gt 0.0446 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0592P)^2^+0.3717P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1139 _refine_ls_wR_factor_ref 0.1274 _refine_special_details ? _olex2_refinement_description ; 1.a Aromatic/amide H refined with riding coordinates: C35(H35), C36(H36), C8(H8), C7(H7), C32(H32), C6(H6), C5(H5), C33(H33) 1.b Tetrahedral OH refined with riding coordinates: O40(H401) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _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 S3 S 0.49188(6) 0.41868(18) 0.65657(2) 0.0537(2) Uani 1 1 d . . . . . F37 F 0.02693(17) 1.6111(5) 0.33605(7) 0.0796(6) Uani 1 1 d . . . . . O40 O 0.21030(17) 0.9921(6) 0.53259(7) 0.0633(6) Uani 1 1 d . . . . . H401 H 0.250340 0.895214 0.553153 0.095 Uiso 1 1 calc R U . . . C4 C 0.3774(2) 0.5705(6) 0.68740(9) 0.0462(6) Uani 1 1 d . . . . . O39 O 0.34807(17) 0.8432(6) 0.48512(7) 0.0664(6) Uani 1 1 d . . . . . C2 C 0.4273(2) 0.5636(7) 0.60208(9) 0.0502(6) Uani 1 1 d . . . . . C31 C 0.1936(2) 1.1470(6) 0.45023(9) 0.0440(6) Uani 1 1 d . . . . . C35 C 0.0284(2) 1.4310(7) 0.41680(11) 0.0563(7) Uani 1 1 d . . . . . H35 H -0.044046 1.517298 0.420027 0.068 Uiso 1 1 calc R U . . . N10 N 0.4763(3) 0.5227(9) 0.56064(10) 0.0717(8) Uani 1 1 d . . . . . C34 C 0.0809(3) 1.4535(7) 0.37384(10) 0.0553(7) Uani 1 1 d . . . . . N1 N 0.32992(18) 0.7177(6) 0.60639(7) 0.0486(5) Uani 1 1 d . . . . . C36 C 0.0856(2) 1.2772(7) 0.45514(10) 0.0504(6) Uani 1 1 d . . . . . H36 H 0.051605 1.260158 0.484725 0.060 Uiso 1 1 calc R U . . . C38 C 0.2576(2) 0.9795(7) 0.49137(9) 0.0496(6) Uani 1 1 d . . . . . C8 C 0.2022(2) 0.8654(7) 0.67128(10) 0.0546(7) Uani 1 1 d . . . . . H8 H 0.150444 0.971997 0.650090 0.065 Uiso 1 1 calc R U . . . C9 C 0.3002(2) 0.7248(6) 0.65428(9) 0.0445(6) Uani 1 1 d . . . . . C7 C 0.1826(3) 0.8449(8) 0.71983(12) 0.0646(8) Uani 1 1 d . . . . . H7 H 0.116683 0.936458 0.731361 0.078 Uiso 1 1 calc R U . . . C32 C 0.2428(2) 1.1699(7) 0.40589(10) 0.0522(6) Uani 1 1 d . . . . . H32 H 0.314362 1.079127 0.402085 0.063 Uiso 1 1 calc R U . . . C6 C 0.2598(3) 0.6895(8) 0.75201(11) 0.0656(8) Uani 1 1 d . . . . . H6 H 0.244706 0.678285 0.784703 0.079 Uiso 1 1 calc R U . . . C5 C 0.3583(3) 0.5518(7) 0.73612(10) 0.0568(7) Uani 1 1 d . . . . . H5 H 0.410320 0.449358 0.757627 0.068 Uiso 1 1 calc R U . . . C33 C 0.1870(3) 1.3258(7) 0.36730(10) 0.0572(7) Uani 1 1 d . . . . . H33 H 0.220341 1.344119 0.337580 0.069 Uiso 1 1 calc R U . . . H101 H 0.533(3) 0.401(9) 0.5581(13) 0.076(11) Uiso 1 1 d . . . . . H102 H 0.441(3) 0.603(10) 0.5392(14) 0.077(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 S3 0.0563(4) 0.0569(4) 0.0473(4) 0.0031(3) -0.0029(3) 0.0089(3) F37 0.0825(12) 0.0886(14) 0.0661(11) 0.0205(10) -0.0142(9) 0.0078(11) O40 0.0577(11) 0.0912(15) 0.0414(9) 0.0046(10) 0.0061(8) 0.0184(11) C4 0.0538(14) 0.0405(13) 0.0439(13) -0.0019(11) 0.0000(10) -0.0040(11) O39 0.0580(12) 0.0918(16) 0.0498(11) 0.0028(11) 0.0065(9) 0.0237(11) C2 0.0489(14) 0.0594(16) 0.0418(13) 0.0022(12) -0.0017(10) 0.0034(12) C31 0.0475(13) 0.0434(13) 0.0413(12) -0.0058(10) 0.0023(10) -0.0036(11) C35 0.0501(15) 0.0543(16) 0.0640(17) -0.0013(14) -0.0016(12) 0.0038(12) N10 0.0643(16) 0.105(2) 0.0456(13) 0.0034(15) 0.0054(12) 0.0325(17) C34 0.0637(17) 0.0505(15) 0.0506(15) 0.0042(12) -0.0089(12) -0.0022(13) N1 0.0462(11) 0.0591(13) 0.0402(11) -0.0021(10) -0.0008(8) 0.0033(10) C36 0.0511(14) 0.0529(15) 0.0475(14) -0.0026(12) 0.0067(11) 0.0000(12) C38 0.0506(15) 0.0519(15) 0.0461(13) -0.0027(12) 0.0018(11) 0.0007(12) C8 0.0530(15) 0.0572(16) 0.0534(15) -0.0059(13) 0.0020(12) 0.0041(13) C9 0.0487(13) 0.0431(13) 0.0418(12) -0.0037(10) 0.0018(10) -0.0037(11) C7 0.0714(19) 0.0647(19) 0.0590(17) -0.0140(15) 0.0160(14) -0.0040(15) C32 0.0518(14) 0.0538(15) 0.0516(15) 0.0005(12) 0.0081(11) 0.0024(12) C6 0.095(2) 0.0588(17) 0.0444(14) -0.0049(13) 0.0140(15) -0.0082(17) C5 0.080(2) 0.0486(14) 0.0420(13) 0.0002(12) 0.0002(13) -0.0037(14) C33 0.0684(18) 0.0579(16) 0.0456(14) 0.0027(12) 0.0055(12) -0.0028(14) _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 S3 C4 1.741(3) . ? S3 C2 1.755(3) . ? F37 C34 1.354(3) . ? O40 H401 0.8200 . ? O40 C38 1.292(3) . ? C4 C9 1.404(4) . ? C4 C5 1.377(4) . ? O39 C38 1.219(3) . ? C2 N10 1.317(4) . ? C2 N1 1.315(3) . ? C31 C36 1.389(4) . ? C31 C38 1.495(4) . ? C31 C32 1.383(4) . ? C35 H35 0.9300 . ? C35 C34 1.367(4) . ? C35 C36 1.376(4) . ? N10 H101 0.83(4) . ? N10 H102 0.78(4) . ? C34 C33 1.373(4) . ? N1 C9 1.385(3) . ? C36 H36 0.9300 . ? C8 H8 0.9300 . ? C8 C9 1.389(4) . ? C8 C7 1.374(4) . ? C7 H7 0.9300 . ? C7 C6 1.391(5) . ? C32 H32 0.9300 . ? C32 C33 1.378(4) . ? C6 H6 0.9300 . ? C6 C5 1.378(4) . ? C5 H5 0.9300 . ? C33 H33 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 C4 S3 C2 89.29(12) . . ? C38 O40 H401 109.5 . . ? C9 C4 S3 109.27(19) . . ? C5 C4 S3 128.7(2) . . ? C5 C4 C9 122.0(3) . . ? N10 C2 S3 120.9(2) . . ? N1 C2 S3 115.12(19) . . ? N1 C2 N10 124.0(3) . . ? C36 C31 C38 121.9(2) . . ? C32 C31 C36 119.1(3) . . ? C32 C31 C38 119.0(2) . . ? C34 C35 H35 120.9 . . ? C34 C35 C36 118.2(3) . . ? C36 C35 H35 120.9 . . ? C2 N10 H101 122(3) . . ? C2 N10 H102 112(3) . . ? H101 N10 H102 126(4) . . ? F37 C34 C35 119.0(3) . . ? F37 C34 C33 118.2(3) . . ? C35 C34 C33 122.8(3) . . ? C2 N1 C9 111.0(2) . . ? C31 C36 H36 119.6 . . ? C35 C36 C31 120.9(3) . . ? C35 C36 H36 119.6 . . ? O40 C38 C31 115.4(2) . . ? O39 C38 O40 124.0(3) . . ? O39 C38 C31 120.6(2) . . ? C9 C8 H8 120.5 . . ? C7 C8 H8 120.5 . . ? C7 C8 C9 119.1(3) . . ? N1 C9 C4 115.3(2) . . ? N1 C9 C8 125.7(2) . . ? C8 C9 C4 119.0(2) . . ? C8 C7 H7 119.5 . . ? C8 C7 C6 121.1(3) . . ? C6 C7 H7 119.5 . . ? C31 C32 H32 119.6 . . ? C33 C32 C31 120.7(3) . . ? C33 C32 H32 119.6 . . ? C7 C6 H6 119.5 . . ? C5 C6 C7 120.9(3) . . ? C5 C6 H6 119.5 . . ? C4 C5 C6 117.9(3) . . ? C4 C5 H5 121.0 . . ? C6 C5 H5 121.0 . . ? C34 C33 C32 118.3(3) . . ? C34 C33 H33 120.8 . . ? C32 C33 H33 120.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S3 C4 C9 N1 1.0(3) . . . . ? S3 C4 C9 C8 -179.8(2) . . . . ? S3 C4 C5 C6 -179.4(2) . . . . ? S3 C2 N1 C9 -0.8(3) . . . . ? F37 C34 C33 C32 179.0(3) . . . . ? C4 S3 C2 N10 179.8(3) . . . . ? C4 S3 C2 N1 1.2(2) . . . . ? C2 S3 C4 C9 -1.2(2) . . . . ? C2 S3 C4 C5 178.5(3) . . . . ? C2 N1 C9 C4 -0.1(3) . . . . ? C2 N1 C9 C8 -179.3(3) . . . . ? C31 C32 C33 C34 -0.9(4) . . . . ? C35 C34 C33 C32 -0.3(5) . . . . ? N10 C2 N1 C9 -179.4(3) . . . . ? C34 C35 C36 C31 -0.3(4) . . . . ? C36 C31 C38 O40 -6.2(4) . . . . ? C36 C31 C38 O39 173.9(3) . . . . ? C36 C31 C32 C33 1.4(4) . . . . ? C36 C35 C34 F37 -178.4(3) . . . . ? C36 C35 C34 C33 0.9(5) . . . . ? C38 C31 C36 C35 179.9(3) . . . . ? C38 C31 C32 C33 -179.2(3) . . . . ? C8 C7 C6 C5 0.1(5) . . . . ? C9 C4 C5 C6 0.2(4) . . . . ? C9 C8 C7 C6 0.7(5) . . . . ? C7 C8 C9 C4 -1.0(4) . . . . ? C7 C8 C9 N1 178.1(3) . . . . ? C7 C6 C5 C4 -0.5(4) . . . . ? C32 C31 C36 C35 -0.8(4) . . . . ? C32 C31 C38 O40 174.5(3) . . . . ? C32 C31 C38 O39 -5.4(4) . . . . ? C5 C4 C9 N1 -178.7(2) . . . . ? C5 C4 C9 C8 0.6(4) . . . . ? _shelx_res_file ; TITL BB_S4_5_Rt_Cu in P21/c #14 shelx.res created by SHELXL-2018/3 at 12:43:40 on 25-Nov-2019 CELL 1.54184 11.7869 4.0326 27.6252 90.000 92.731 90.000 ZERR 4.00 0.0014 0.0005 0.0026 0.000 0.010 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O S F UNIT 56 44 8 8 4 4 MERG 2 MORE -1 FMAP 2 PLAN 5 OMIT 4 4 13 OMIT 4 4 14 ACTA BOND $H CONF LIST 4 L.S. 4 WGHT 0.059200 0.371700 FVAR 0.48039 S3 5 0.491882 0.418683 0.656567 11.00000 0.05632 0.05691 = 0.04726 0.00315 -0.00287 0.00895 F37 6 0.026932 1.611092 0.336053 11.00000 0.08253 0.08861 = 0.06605 0.02053 -0.01424 0.00779 O40 4 0.210301 0.992085 0.532592 11.00000 0.05773 0.09120 = 0.04143 0.00462 0.00615 0.01836 AFIX 83 H401 2 0.250340 0.895214 0.553153 11.00000 -1.50000 AFIX 0 C4 1 0.377386 0.570514 0.687403 11.00000 0.05385 0.04053 = 0.04386 -0.00189 0.00003 -0.00398 O39 4 0.348068 0.843242 0.485118 11.00000 0.05796 0.09179 = 0.04985 0.00283 0.00648 0.02373 C2 1 0.427253 0.563605 0.602078 11.00000 0.04895 0.05936 = 0.04180 0.00215 -0.00171 0.00341 C31 1 0.193567 1.146973 0.450230 11.00000 0.04750 0.04335 = 0.04127 -0.00576 0.00228 -0.00362 C35 1 0.028371 1.430997 0.416800 11.00000 0.05009 0.05432 = 0.06402 -0.00131 -0.00161 0.00378 AFIX 43 H35 2 -0.044046 1.517298 0.420027 11.00000 -1.20000 AFIX 0 N10 3 0.476275 0.522716 0.560644 11.00000 0.06426 0.10550 = 0.04557 0.00344 0.00535 0.03251 C34 1 0.080853 1.453491 0.373836 11.00000 0.06372 0.05046 = 0.05064 0.00425 -0.00888 -0.00216 N1 3 0.329918 0.717726 0.606394 11.00000 0.04620 0.05908 = 0.04022 -0.00213 -0.00077 0.00329 C36 1 0.085634 1.277164 0.455137 11.00000 0.05112 0.05293 = 0.04755 -0.00260 0.00670 -0.00005 AFIX 43 H36 2 0.051605 1.260158 0.484725 11.00000 -1.20000 AFIX 0 C38 1 0.257596 0.979450 0.491372 11.00000 0.05060 0.05193 = 0.04609 -0.00268 0.00176 0.00074 C8 1 0.202157 0.865436 0.671282 11.00000 0.05300 0.05721 = 0.05340 -0.00591 0.00203 0.00411 AFIX 43 H8 2 0.150444 0.971997 0.650090 11.00000 -1.20000 AFIX 0 C9 1 0.300236 0.724822 0.654284 11.00000 0.04871 0.04308 = 0.04180 -0.00367 0.00182 -0.00371 C7 1 0.182600 0.844915 0.719835 11.00000 0.07136 0.06473 = 0.05902 -0.01402 0.01602 -0.00396 AFIX 43 H7 2 0.116683 0.936458 0.731361 11.00000 -1.20000 AFIX 0 C32 1 0.242805 1.169923 0.405886 11.00000 0.05183 0.05381 = 0.05161 0.00053 0.00809 0.00243 AFIX 43 H32 2 0.314362 1.079127 0.402085 11.00000 -1.20000 AFIX 0 C6 1 0.259793 0.689464 0.752005 11.00000 0.09457 0.05877 = 0.04444 -0.00485 0.01401 -0.00817 AFIX 43 H6 2 0.244706 0.678285 0.784703 11.00000 -1.20000 AFIX 0 C5 1 0.358306 0.551789 0.736116 11.00000 0.07963 0.04858 = 0.04205 0.00023 0.00021 -0.00373 AFIX 43 H5 2 0.410320 0.449358 0.757627 11.00000 -1.20000 AFIX 0 C33 1 0.186976 1.325833 0.367299 11.00000 0.06835 0.05790 = 0.04559 0.00270 0.00550 -0.00281 AFIX 43 H33 2 0.220341 1.344119 0.337580 11.00000 -1.20000 AFIX 0 H101 2 0.533010 0.401402 0.558093 11.00000 0.07627 H102 2 0.440840 0.602879 0.539200 11.00000 0.07709 HKLF 4 REM BB_S4_5_Rt_Cu in P21/c #14 REM wR2 = 0.1274, GooF = S = 1.009, Restrained GooF = 1.009 for all data REM R1 = 0.0446 for 1748 Fo > 4sig(Fo) and 0.0615 for all 2280 data REM 189 parameters refined using 0 restraints END WGHT 0.0630 0.2067 REM Highest difference peak 0.221, deepest hole -0.276, 1-sigma level 0.047 Q1 1 0.4988 -0.0614 0.6588 11.00000 0.05 0.22 Q2 1 0.4654 0.4527 0.6912 11.00000 0.05 0.19 Q3 1 0.1345 1.1516 0.4482 11.00000 0.05 0.17 Q4 1 0.1241 1.3119 0.3668 11.00000 0.05 0.17 Q5 1 0.2580 0.8659 0.6608 11.00000 0.05 0.16 ; _shelx_res_checksum 33387 _shelx_hkl_file ; 0 0 -4 456.78 8.74 0 0 -5 -0.14 0.71 0 0 -6 516.01 11.48 0 0 -7 0.95 0.87 0 0 -8 102.76 5.78 0 0 -9 0.11 0.94 0 0 -10 1123.11 22.83 0 0 -11 0.73 1.30 0 0 -12 739.82 20.29 0 0 -13 -0.08 0.86 0 0 -14 179.93 7.36 0 0 -15 0.17 0.98 0 0 -16 390.35 12.05 0 0 -17 -0.74 1.28 0 0 -18 187.28 9.04 0 0 -19 -0.21 0.78 0 0 -20 122.09 7.81 0 0 -21 0.95 1.12 0 0 -22 49.28 5.37 0 0 -23 -0.72 1.17 0 0 24 2.58 0.95 0 0 -24 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-11 1 20 0.28 0.47 -11 1 19 20.51 1.63 11 1 -19 24.96 1.61 -11 1 18 0.63 0.58 11 1 -18 1.24 0.54 -11 1 17 1.26 0.68 11 1 -17 1.79 0.63 -11 1 16 0.13 0.62 -11 1 15 -0.73 0.67 -11 1 14 0.65 0.63 -11 1 13 92.80 4.04 -11 1 12 14.28 1.69 -11 1 11 22.24 2.03 11 1 -10 1.21 0.69 -11 1 10 1.70 0.67 11 1 -9 5.19 1.17 -11 1 9 4.91 1.06 11 1 -8 41.06 3.01 11 1 -7 1.19 0.76 11 1 -6 0.27 0.71 11 1 -5 13.38 1.76 11 1 -4 -1.16 0.99 11 1 -3 -0.36 0.85 11 1 -2 18.82 2.11 11 1 -1 6.74 1.46 11 1 0 0.40 0.74 -11 1 0 1.17 0.83 11 1 1 7.82 1.51 -11 1 -1 8.65 1.63 11 1 2 -0.30 0.74 -11 1 -2 -0.67 0.81 11 1 3 14.81 1.97 -11 1 -3 14.68 1.92 11 1 4 10.11 1.63 -11 1 -4 9.13 1.63 11 1 5 2.11 1.05 -11 1 -5 0.62 0.75 11 1 6 14.34 1.88 -11 1 -6 11.97 1.75 11 1 7 25.60 2.46 -11 1 -7 21.65 2.30 11 1 8 2.77 1.06 -11 1 -8 0.50 0.79 11 1 9 4.74 1.15 -11 1 -9 5.16 1.20 -11 1 -10 0.87 0.62 -11 1 -11 2.92 0.93 -11 1 -12 7.03 1.27 -11 1 -13 -0.20 0.62 -11 1 -14 0.34 0.50 -11 1 -15 14.61 1.48 -11 1 -16 0.65 0.47 -11 1 -17 1.86 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0 -3 0.34 0.67 12 0 -2 16.14 1.96 12 0 -1 0.02 0.66 12 0 0 19.33 2.12 12 0 1 -0.07 0.70 12 0 2 52.39 3.44 12 0 3 -0.18 0.79 12 0 4 8.43 1.46 12 0 5 0.06 0.71 12 0 6 0.08 0.72 12 0 7 0.83 0.79 12 0 8 150.35 5.53 12 0 9 -0.56 0.77 12 0 10 0.46 0.64 12 0 11 0.85 0.67 12 0 12 2.53 0.77 12 0 13 0.99 0.55 12 0 14 4.27 0.85 12 0 15 -0.02 0.42 -12 1 16 0.12 0.43 12 1 -16 -0.15 0.37 -12 1 15 19.99 1.60 12 1 -15 23.62 1.66 -12 1 14 1.26 0.60 -12 1 13 -0.10 0.46 -12 1 12 0.57 0.55 -12 1 11 -0.27 0.43 -12 1 10 0.07 0.52 12 1 -9 0.98 0.76 -12 1 9 1.77 0.69 -12 1 8 24.36 2.05 12 1 -8 27.37 2.26 12 1 -7 2.42 0.87 -12 1 7 1.96 0.72 12 1 -6 4.22 1.02 12 1 -5 3.41 0.96 12 1 -4 3.10 0.95 12 1 -3 12.72 1.66 12 1 -2 0.68 0.63 12 1 -1 -0.36 0.74 12 1 0 2.80 0.93 12 1 1 22.35 2.21 12 1 2 1.23 0.71 12 1 3 3.22 0.97 12 1 4 23.10 2.21 12 1 5 18.88 1.96 -12 1 -5 15.10 1.80 12 1 6 2.22 0.84 -12 1 -6 1.37 0.66 12 1 7 24.09 2.15 -12 1 -7 21.09 2.04 12 1 8 8.41 1.34 -12 1 -8 8.91 1.36 12 1 9 13.80 1.64 -12 1 -9 13.31 1.53 12 1 10 3.53 0.95 -12 1 -10 3.78 0.91 12 1 11 40.11 2.49 -12 1 -11 47.58 2.63 12 1 12 16.14 1.54 -12 1 -12 18.50 1.59 12 1 13 -0.24 0.55 -12 1 -13 0.35 0.53 12 1 14 4.44 0.82 -12 1 -14 4.86 0.81 -12 2 11 7.73 0.97 12 2 -11 6.70 0.83 12 2 -10 -0.09 0.37 12 2 -9 9.54 1.02 12 2 -8 3.16 0.66 -12 2 8 2.94 0.72 -12 2 7 0.41 0.48 -12 2 6 4.30 0.87 -12 2 5 8.37 1.15 -12 2 4 9.17 1.22 -12 2 3 8.37 1.22 -12 2 2 5.54 1.01 -12 2 1 0.27 0.55 -12 2 0 -0.16 0.51 -12 2 -1 4.20 0.92 -12 2 -2 3.30 0.87 -12 2 -3 0.82 0.59 -12 2 -4 5.75 0.98 -12 2 -5 6.17 1.00 -12 2 -6 22.94 1.63 -13 0 13 1.54 0.66 -13 0 12 27.33 1.93 -13 0 11 -0.79 0.57 -13 0 10 0.88 0.63 -13 0 9 -0.43 0.58 13 0 -8 4.21 0.90 -13 0 8 4.08 0.93 13 0 -7 -0.02 0.58 13 0 -6 16.68 1.68 13 0 -5 -0.48 0.70 13 0 -4 0.44 0.56 13 0 -3 -0.34 0.69 13 0 -2 1.07 0.67 13 0 -1 -0.28 0.58 13 0 0 42.70 2.73 13 0 1 -0.02 0.52 13 0 2 0.06 0.63 13 0 3 0.42 0.58 13 0 4 2.29 0.85 13 0 5 0.15 0.65 13 0 6 0.65 0.59 13 0 7 -0.97 0.64 13 0 8 0.79 0.52 13 0 9 0.27 0.46 13 0 10 2.09 0.65 13 1 -12 1.71 0.51 -13 1 11 1.11 0.47 -13 1 10 2.60 0.68 -13 1 9 4.10 0.79 -13 1 8 0.79 0.47 13 1 -7 0.79 0.59 -13 1 7 0.80 0.46 -13 -1 7 1.01 0.58 13 1 -6 0.46 0.50 -13 1 6 1.56 0.64 13 1 -5 2.09 0.72 -13 1 5 2.14 0.66 13 1 -4 6.20 1.06 -13 1 4 3.67 0.75 13 1 -3 16.83 1.67 13 1 -2 -0.25 0.68 13 1 -1 0.01 0.70 13 1 0 4.58 0.93 13 1 1 -0.54 0.68 13 1 2 0.59 0.57 13 1 3 3.21 0.87 13 1 4 -0.59 0.58 13 1 5 7.09 1.05 13 1 6 3.78 0.85 13 1 7 9.68 1.20 13 1 8 10.97 1.20 14 0 -2 11.43 1.20 14 0 -1 -0.87 0.57 0 0 0 0.00 0.00 TITL BB_S4_5_Rt_Cu in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 1.54184 11.786917 4.032645 27.625210 90.0000 92.7312 90.0000 ZERR 1.00 0.001432 0.000456 0.002621 0.0000 0.0102 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H N O Cl UNIT 56.00 48.00 8.00 12.00 4.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 22061 _olex2_submission_special_instructions 'No special instructions were received'