#============================================================================== # 1. SUBMISSION DETAILS data_global _publ_contact_author ; Constantin G. Daniliuc Organisch-Chemisches Institut Westf\"alische Wilhelm-Universit\"at M\"unster 48149 M\"unster Germany ; _publ_contact_author_phone '049 251 83-36522' _publ_contact_author_fax '049 251 83-39772' _publ_contact_author_email 'constantin.daniliuc@uni-muenster.de' _publ_requested_journal '.' #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Fluorinative Skeletal Ring Contractions by I(I)/I(III) Catalysis: Stereoselective Synthesis of cis-alfa,alfa-Difluorocyclopropanes ; loop_ _publ_author_name _publ_author_address 'Livingstone, Keith' ; Organisch-Chemisches Institut Westf\"alische Wilhelms-Universit\"at M\"unster Corrensstrasse 36 48149 M\"unster Germany ; 'Siebold, Kathrin' ; Organisch-Chemisches Institut Westf\"alische Wilhelms-Universit\"at M\"unster Corrensstrasse 36 48149 M\"unster Germany ; 'Martin-Heras, Victor' ; Organisch-Chemisches Institut Westf\"alische Wilhelms-Universit\"at M\"unster Corrensstrasse 36 48149 M\"unster Germany ; 'Meyer, Stephanie' ; Organisch-Chemisches Institut Westf\"alische Wilhelms-Universit\"at M\"unster Corrensstrasse 36 48149 M\"unster Germany ; 'Daniliuc, Constantin G.' ; Organisch-Chemisches Institut Westf\"alische Wilhelms-Universit\"at M\"unster Corrensstrasse 36 48149 M\"unster Germany ; 'Gilmour, Ryan' ; Organisch-Chemisches Institut Westf\"alische Wilhelms-Universit\"at M\"unster Corrensstrasse 36 48149 M\"unster Germany ; #============================================================================= # cif data for "gil10360" (compound 5e) #============================================================================= data_gil10360_5e _audit_creation_method 'APEX4 v2021.4-0' _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H9 Br F2 O2' _chemical_formula_iupac ? _chemical_formula_weight 291.09 _chemical_melting_point ? _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.6094(2) _cell_length_b 8.5213(2) _cell_length_c 9.5290(2) _cell_angle_alpha 66.8730(10) _cell_angle_beta 78.2040(10) _cell_angle_gamma 73.9430(10) _cell_volume 542.84(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 7584 _cell_measurement_theta_min 5.0769 _cell_measurement_theta_max 66.6874 _cell_measurement_temperature 100.(2) _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.219 _exptl_crystal_size_mid 0.066 _exptl_crystal_size_min 0.049 _exptl_crystal_density_diffrn 1.781 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 288 _exptl_absorpt_coefficient_mu 5.305 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_process_details ; Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015). "Comparison of silver and molybdenum microfocus X-ray sources for single-crystal structure determination" J. Appl. Cryst. 48, 3-10. doi:10.1107/S1600576714022985 ; _exptl_absorpt_correction_T_min 0.66 _exptl_absorpt_correction_T_max 0.78 _exptl_special_details ; ; _diffrn_ambient_temperature 100.(2) _diffrn_source 'Cu ImS' _diffrn_source_type 'micro focus tube' _diffrn_source_power 0.05 _diffrn_source_current 1.0 _diffrn_source_voltage 50 _diffrn_radiation_probe 'single crystal' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_monochromator 'MX mirror' _diffrn_measurement_device 'Bruker D8 Venture Photon III' _diffrn_measurement_device_type 'single crystal diffractometer' _diffrn_measurement_method 'phi/omega scans' _diffrn_detector_area_resol_mean 7.3910 _diffrn_reflns_number 13022 _diffrn_reflns_av_R_equivalents 0.0601 _diffrn_reflns_av_unetI/netI 0.0334 _diffrn_reflns_theta_min 5.08 _diffrn_reflns_theta_max 66.84 _diffrn_reflns_theta_full 66.84 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _refine_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_number_total 1918 _reflns_number_gt 1703 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0378 _refine_ls_R_factor_gt 0.0304 _refine_ls_wR_factor_gt 0.0601 _refine_ls_wR_factor_ref 0.0636 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_number_reflns 1918 _refine_ls_number_parameters 149 _refine_ls_number_restraints 1 _refine_ls_number_constraints ? _refine_ls_hydrogen_treatment mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0048P)^2^+1.0626P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary ? _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.371 _refine_diff_density_min -0.428 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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' Br Br -0.6763 1.2805 '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' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection 'Bruker APEX4 v2021.4-0 Photon III' _computing_cell_refinement 'SAINT V8.40B (Bruker AXS LLC, 2019)' _computing_data_reduction 'SAINT V8.40B (Bruker AXS LLC, 2019)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_molecular_graphics 'shelXle (C.B. Huebschle, rev 1242)' _computing_publication_material 'SHELXT 2018/2 (Sheldrick, 2018)' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_flags_posn _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Br Br1 0.87183(5) 0.85541(5) -0.08169(4) 0.02914(12) Uani d . . . 1 . . F F1 0.1604(2) 0.4528(2) 0.2597(2) 0.0292(4) Uani d . . . 1 . . F F2 0.3904(2) 0.2258(2) 0.30478(19) 0.0269(4) Uani d . . . 1 . . O O1 0.1960(3) -0.0012(3) 0.5453(2) 0.0237(5) Uani d . . . 1 . . O O2 -0.0668(3) 0.1946(3) 0.5547(3) 0.0278(5) Uani d . . D 1 . . H H02 -0.108(6) 0.128(5) 0.525(5) 0.067(15) Uiso d . . D 1 . . C C1 0.7045(4) 0.7097(4) 0.0347(3) 0.0194(6) Uani d . . . 1 . . C C2 0.5173(4) 0.7745(4) 0.0216(3) 0.0199(6) Uani d . . . 1 . . H H2 0.473452 0.888712 -0.048033 0.024000 Uiso calc U . R 1 . . C C3 0.3959(4) 0.6698(4) 0.1119(3) 0.0190(6) Uani d . . . 1 . . H H3 0.267471 0.712878 0.105053 0.023000 Uiso calc U . R 1 . . C C4 0.4604(4) 0.5027(4) 0.2118(3) 0.0179(6) Uani d . . . 1 . . C C5 0.6485(4) 0.4389(4) 0.2206(3) 0.0206(6) Uani d . . . 1 . . H H5 0.692918 0.323386 0.287842 0.025000 Uiso calc U . R 1 . . C C6 0.7715(4) 0.5424(4) 0.1321(3) 0.0206(6) Uani d . . . 1 . . H H6 0.899959 0.499086 0.138333 0.025000 Uiso calc U . R 1 . . C C7 0.3305(4) 0.3886(4) 0.3146(3) 0.0213(6) Uani d . . . 1 . . C C8 0.3039(4) 0.3752(4) 0.4793(3) 0.0201(6) Uani d . . . 1 . . H H8 0.290313 0.488182 0.493674 0.024000 Uiso calc U . R 1 . . C C9 0.3984(4) 0.2174(4) 0.6002(3) 0.0230(6) Uani d . . . 1 . . H H9A 0.475471 0.119793 0.568739 0.028000 Uiso calc U . R 1 . . H H9B 0.445270 0.236373 0.680558 0.028000 Uiso calc U . R 1 . . C C10 0.1944(4) 0.2493(4) 0.6033(3) 0.0221(6) Uani d . . . 1 . . H H10 0.120408 0.293340 0.685154 0.026000 Uiso calc U . R 1 . . C C11 0.1124(4) 0.1347(4) 0.5644(3) 0.0193(6) Uani d . . . 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Br1 0.02833(19) 0.02650(18) 0.0338(2) -0.01414(13) 0.00551(13) -0.01082(14) F1 0.0236(9) 0.0404(11) 0.0260(10) -0.0157(8) -0.0075(7) -0.0061(8) F2 0.0426(11) 0.0221(9) 0.0228(9) -0.0157(8) -0.0008(8) -0.0106(7) O1 0.0210(11) 0.0221(11) 0.0305(12) -0.0066(9) -0.0032(9) -0.0104(9) O2 0.0202(11) 0.0239(11) 0.0438(14) -0.0053(9) -0.0042(10) -0.0161(10) C1 0.0233(15) 0.0199(15) 0.0200(15) -0.0080(12) -0.0018(12) -0.0104(12) C2 0.0265(16) 0.0169(14) 0.0182(15) -0.0042(12) -0.0054(12) -0.0072(12) C3 0.0179(14) 0.0200(15) 0.0211(15) -0.0030(12) -0.0042(12) -0.0092(12) C4 0.0219(15) 0.0206(15) 0.0161(14) -0.0083(12) -0.0026(11) -0.0089(12) C5 0.0252(16) 0.0188(15) 0.0183(15) -0.0053(12) -0.0063(12) -0.0050(12) C6 0.0187(15) 0.0239(16) 0.0210(15) -0.0033(12) -0.0037(12) -0.0102(13) C7 0.0224(15) 0.0211(15) 0.0254(16) -0.0047(12) -0.0076(12) -0.0110(13) C8 0.0217(15) 0.0221(15) 0.0222(15) -0.0099(12) -0.0016(12) -0.0108(13) C9 0.0272(16) 0.0227(15) 0.0221(15) -0.0060(13) -0.0062(13) -0.0091(13) C10 0.0258(16) 0.0262(16) 0.0177(15) -0.0112(13) 0.0006(12) -0.0092(13) C11 0.0212(15) 0.0185(14) 0.0162(14) -0.0073(12) 0.0006(11) -0.0035(12) _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_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Br1 C1 . 1.900(3) ? F1 C7 . 1.382(3) ? F2 C7 . 1.370(3) ? O1 C11 . 1.221(4) ? O2 C11 . 1.326(4) ? O2 H02 . 0.867(19) ? C1 C6 . 1.381(4) ? C1 C2 . 1.390(4) ? C2 C3 . 1.385(4) ? C2 H2 . 0.950000 ? C3 C4 . 1.383(4) ? C3 H3 . 0.950000 ? C4 C5 . 1.391(4) ? C4 C7 . 1.507(4) ? C5 C6 . 1.383(4) ? C5 H5 . 0.950000 ? C6 H6 . 0.950000 ? C7 C8 . 1.503(4) ? C8 C9 . 1.496(4) ? C8 C10 . 1.528(4) ? C8 H8 . 1.000000 ? C9 C10 . 1.496(4) ? C9 H9A . 0.990000 ? C9 H9B . 0.990000 ? C10 C11 . 1.482(4) ? C10 H10 . 1.000000 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C11 O2 H02 . . 110.(3) ? C6 C1 C2 . . 121.5(3) ? C6 C1 Br1 . . 119.1(2) ? C2 C1 Br1 . . 119.4(2) ? C3 C2 C1 . . 118.9(3) ? C3 C2 H2 . . 120.600000 ? C1 C2 H2 . . 120.600000 ? C4 C3 C2 . . 120.4(3) ? C4 C3 H3 . . 119.800000 ? C2 C3 H3 . . 119.800000 ? C3 C4 C5 . . 119.8(3) ? C3 C4 C7 . . 121.3(3) ? C5 C4 C7 . . 118.9(3) ? C6 C5 C4 . . 120.5(3) ? C6 C5 H5 . . 119.800000 ? C4 C5 H5 . . 119.800000 ? C1 C6 C5 . . 118.9(3) ? C1 C6 H6 . . 120.500000 ? C5 C6 H6 . . 120.500000 ? F2 C7 F1 . . 105.1(2) ? F2 C7 C8 . . 110.4(2) ? F1 C7 C8 . . 108.1(2) ? F2 C7 C4 . . 109.1(2) ? F1 C7 C4 . . 109.4(2) ? C8 C7 C4 . . 114.3(2) ? C9 C8 C7 . . 121.4(3) ? C9 C8 C10 . . 59.27(19) ? C7 C8 C10 . . 121.6(2) ? C9 C8 H8 . . 114.500000 ? C7 C8 H8 . . 114.500000 ? C10 C8 H8 . . 114.500000 ? C10 C9 C8 . . 61.43(19) ? C10 C9 H9A . . 117.600000 ? C8 C9 H9A . . 117.600000 ? C10 C9 H9B . . 117.600000 ? C8 C9 H9B . . 117.600000 ? H9A C9 H9B . . 114.700000 ? C11 C10 C9 . . 120.6(3) ? C11 C10 C8 . . 120.6(2) ? C9 C10 C8 . . 59.29(19) ? C11 C10 H10 . . 115.000000 ? C9 C10 H10 . . 115.000000 ? C8 C10 H10 . . 115.000000 ? O1 C11 O2 . . 122.6(3) ? O1 C11 C10 . . 125.2(3) ? O2 C11 C10 . . 112.3(3) ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C6 C1 C2 C3 . . . . 1.8(4) ? Br1 C1 C2 C3 . . . . -177.3(2) ? C1 C2 C3 C4 . . . . -0.8(4) ? C2 C3 C4 C5 . . . . -0.7(4) ? C2 C3 C4 C7 . . . . 178.1(3) ? C3 C4 C5 C6 . . . . 1.2(4) ? C7 C4 C5 C6 . . . . -177.6(3) ? C2 C1 C6 C5 . . . . -1.3(4) ? Br1 C1 C6 C5 . . . . 177.8(2) ? C4 C5 C6 C1 . . . . -0.2(4) ? C3 C4 C7 F2 . . . . 132.4(3) ? C5 C4 C7 F2 . . . . -48.9(3) ? C3 C4 C7 F1 . . . . 17.9(4) ? C5 C4 C7 F1 . . . . -163.3(2) ? C3 C4 C7 C8 . . . . -103.4(3) ? C5 C4 C7 C8 . . . . 75.4(3) ? F2 C7 C8 C9 . . . . 21.4(4) ? F1 C7 C8 C9 . . . . 135.8(3) ? C4 C7 C8 C9 . . . . -102.1(3) ? F2 C7 C8 C10 . . . . -49.5(4) ? F1 C7 C8 C10 . . . . 64.9(3) ? C4 C7 C8 C10 . . . . -173.0(3) ? C7 C8 C9 C10 . . . . -110.5(3) ? C8 C9 C10 C11 . . . . 109.7(3) ? C9 C8 C10 C11 . . . . -109.6(3) ? C7 C8 C10 C11 . . . . 0.6(4) ? C7 C8 C10 C9 . . . . 110.3(3) ? C9 C10 C11 O1 . . . . 8.9(4) ? C8 C10 C11 O1 . . . . 79.1(4) ? C9 C10 C11 O2 . . . . -172.2(2) ? C8 C10 C11 O2 . . . . -102.1(3) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O2 H02 O1 2_556 0.867(19) 1.80(2) 2.665(3) 177.(5) ? _shelx_res_file ; TITL gil10360.res in P-1 gil10360.res created by SHELXL-2018/3 at 08:28:51 on 29-Jun-2022 CELL 1.54178 7.6094 8.5213 9.5290 66.873 78.204 73.943 ZERR 2.000 0.0002 0.0002 0.0002 0.001 0.001 0.001 LATT 1 SFAC C H Br F O UNIT 22 18 2 4 4 LIST 4 REM Old TITL gil10360 in P-1 REM SHELXT solution in P-1: R1 0.098, Rweak 0.009, Alpha 0.041 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C11 Br F2 O2 SIZE 0.049 0.066 0.219 TEMP -173.150 ACTA CONF L.S. 50 BOND $H FMAP 2 PLAN 10 HTAB EQIV $1 -x, -y, -z+1 HTAB O2 O1_$1 OMIT -1 0 10 DFIX 0.88 O2 H02 WGHT 0.004800 1.062600 FVAR 0.80623 BR1 3 0.871832 0.855414 -0.081687 11.00000 0.02833 0.02650 = 0.03376 -0.01082 0.00551 -0.01414 F1 4 0.160437 0.452758 0.259666 11.00000 0.02363 0.04042 = 0.02602 -0.00607 -0.00750 -0.01570 F2 4 0.390373 0.225789 0.304784 11.00000 0.04262 0.02214 = 0.02278 -0.01060 -0.00077 -0.01574 O1 5 0.196019 -0.001249 0.545335 11.00000 0.02099 0.02214 = 0.03046 -0.01037 -0.00319 -0.00662 O2 5 -0.066814 0.194570 0.554666 11.00000 0.02016 0.02389 = 0.04380 -0.01612 -0.00419 -0.00525 H02 2 -0.108193 0.128362 0.525496 11.00000 0.06657 C1 1 0.704464 0.709724 0.034704 11.00000 0.02331 0.01995 = 0.01995 -0.01038 -0.00177 -0.00799 C2 1 0.517328 0.774511 0.021621 11.00000 0.02647 0.01691 = 0.01824 -0.00717 -0.00541 -0.00417 AFIX 43 H2 2 0.473452 0.888712 -0.048033 11.00000 -1.20000 AFIX 0 C3 1 0.395878 0.669766 0.111851 11.00000 0.01788 0.02000 = 0.02110 -0.00917 -0.00420 -0.00297 AFIX 43 H3 2 0.267471 0.712878 0.105053 11.00000 -1.20000 AFIX 0 C4 1 0.460447 0.502748 0.211808 11.00000 0.02195 0.02064 = 0.01608 -0.00894 -0.00262 -0.00831 C5 1 0.648541 0.438894 0.220611 11.00000 0.02524 0.01880 = 0.01831 -0.00503 -0.00627 -0.00529 AFIX 43 H5 2 0.692918 0.323386 0.287842 11.00000 -1.20000 AFIX 0 C6 1 0.771473 0.542425 0.132139 11.00000 0.01872 0.02393 = 0.02097 -0.01018 -0.00369 -0.00333 AFIX 43 H6 2 0.899959 0.499086 0.138333 11.00000 -1.20000 AFIX 0 C7 1 0.330532 0.388574 0.314622 11.00000 0.02239 0.02114 = 0.02537 -0.01100 -0.00755 -0.00469 C8 1 0.303903 0.375161 0.479271 11.00000 0.02175 0.02205 = 0.02223 -0.01084 -0.00161 -0.00986 AFIX 13 H8 2 0.290313 0.488182 0.493674 11.00000 -1.20000 AFIX 0 C9 1 0.398418 0.217435 0.600194 11.00000 0.02718 0.02273 = 0.02214 -0.00912 -0.00615 -0.00602 AFIX 23 H9A 2 0.475471 0.119793 0.568739 11.00000 -1.20000 H9B 2 0.445270 0.236373 0.680558 11.00000 -1.20000 AFIX 0 C10 1 0.194444 0.249331 0.603277 11.00000 0.02579 0.02622 = 0.01773 -0.00925 0.00060 -0.01118 AFIX 13 H10 2 0.120408 0.293340 0.685154 11.00000 -1.20000 AFIX 0 C11 1 0.112365 0.134714 0.564401 11.00000 0.02116 0.01848 = 0.01624 -0.00352 0.00064 -0.00729 HKLF 4 REM gil10360.res in P-1 REM wR2 = 0.063640, GooF = S = 1.05701, Restrained GooF = 1.05682 for all data REM R1 = 0.030359 for 1703 Fo > 4sig(Fo) and 0.037837 for all 1918 data REM 149 parameters refined using 1 restraints END WGHT 0.0048 1.0625 REM Instructions for potential hydrogen bonds HTAB O2 O1_$1 EQIV $2 x+1, y, z HTAB C6 F1_$2 REM Highest difference peak 0.371, deepest hole -0.428, 1-sigma level 0.083 Q1 1 0.8323 1.0010 -0.2027 11.00000 0.05 0.37 Q2 1 0.3885 0.4461 0.2534 11.00000 0.05 0.33 Q3 1 0.8045 0.7443 -0.1215 11.00000 0.05 0.31 Q4 1 0.8863 0.8558 0.0021 11.00000 0.05 0.30 Q5 1 0.6157 0.7204 0.0270 11.00000 0.05 0.30 Q6 1 0.9987 0.9208 -0.0808 11.00000 0.05 0.30 Q7 1 0.1757 0.2951 0.7950 11.00000 0.05 0.29 Q8 1 -0.1908 0.1116 0.6779 11.00000 0.05 0.29 Q9 1 0.4236 0.9365 0.0387 11.00000 0.05 0.29 Q10 1 0.9942 0.8371 0.0361 11.00000 0.05 0.28 ; _shelx_res_checksum 84395 _shelx_hkl_file ; -1 0 0 124.29 8.70 -1 0 0 130.59 9.00 1 0 0 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215.88 19.80 5 1 9 184.38 18.60 5 1 9 210.48 17.90 5 1 9 210.38 18.80 5 1 9 237.38 20.10 3 -2 -9 58.19 12.60 3 -2 -9 5.40 15.30 3 -2 -9 26.40 11.00 3 -2 -9 48.10 15.60 -3 2 9 31.70 7.10 -3 2 9 34.70 9.40 -3 2 9 36.00 11.90 2 -2 -9 15.40 28.90 2 -2 -9 43.40 17.80 2 -2 -9 10.80 21.40 2 -2 -9 23.90 9.80 -2 2 9 11.60 7.20 -2 2 9 9.70 8.70 -2 2 9 16.50 9.90 1 -2 -9 178.08 22.90 1 -2 -9 124.19 27.10 -1 2 9 151.78 17.30 -1 2 9 152.08 20.80 -1 2 9 200.88 25.70 0 -2 -9 391.36 26.80 0 -2 -9 433.56 30.60 0 2 9 361.46 28.00 0 2 9 416.06 30.10 0 2 9 409.76 29.50 0 2 9 397.56 29.40 -1 -2 -9 -4.90 10.20 -1 -2 -9 -11.30 9.40 1 2 9 -12.60 23.10 1 2 9 -0.30 9.80 1 2 9 41.40 45.30 1 2 9 -10.00 12.80 1 2 9 -16.80 9.80 -2 -2 -9 -10.80 13.50 -2 -2 -9 8.10 9.90 2 2 9 7.30 15.20 2 2 9 32.80 35.10 2 2 9 8.30 7.60 2 2 9 10.20 18.30 2 2 9 -3.50 11.50 2 2 9 -20.10 12.30 -3 -2 -9 373.76 29.70 -3 -2 -9 366.06 26.20 3 2 9 333.67 23.70 3 2 9 333.77 30.20 3 2 9 341.97 38.30 3 2 9 463.35 89.09 3 2 9 396.66 29.60 3 2 9 351.56 33.20 -4 -2 -9 134.29 18.90 -4 -2 -9 140.59 22.00 -4 -2 -9 126.49 25.10 4 2 9 156.18 19.20 4 2 9 110.49 25.10 4 2 9 164.78 21.90 4 2 9 115.19 25.20 -5 -2 -9 14.40 13.60 -5 -2 -9 13.60 10.80 -5 -2 -9 23.20 15.00 5 2 9 34.00 19.10 5 2 9 15.20 13.10 5 2 9 26.30 9.70 5 2 9 20.00 10.30 -6 -2 -9 65.89 11.50 -6 -2 -9 36.90 18.60 -6 -2 -9 78.39 16.10 6 2 9 123.99 19.30 6 2 9 89.29 15.60 6 2 9 83.69 13.90 6 2 9 101.79 17.30 3 -3 -9 -7.50 8.30 3 -3 -9 26.40 18.30 3 -3 -9 4.30 12.50 3 -3 -9 11.90 8.80 -3 3 9 16.30 9.30 -3 3 9 11.90 7.20 -3 3 9 12.50 8.30 2 -3 -9 93.09 22.90 2 -3 -9 46.70 10.70 2 -3 -9 66.09 29.50 -2 3 9 50.49 14.10 -2 3 9 62.79 11.70 1 -3 -9 271.87 25.60 1 -3 -9 345.07 40.20 -1 3 9 289.57 29.90 -1 3 9 281.97 25.50 -1 3 9 298.57 25.30 0 -3 -9 5.10 11.10 0 -3 -9 -5.50 9.90 0 3 9 -1.50 13.70 0 3 9 0.70 9.80 0 3 9 13.00 8.90 0 3 9 16.40 17.40 -1 -3 -9 0.40 12.80 -1 -3 -9 7.90 10.10 1 3 9 28.10 12.90 1 3 9 13.70 8.60 1 3 9 18.50 20.40 -2 -3 -9 317.07 27.30 -2 -3 -9 310.27 27.70 2 3 9 345.27 29.10 2 3 9 287.97 25.70 2 3 9 237.58 28.20 2 3 9 207.88 40.80 2 3 9 337.37 25.70 -3 -3 -9 162.58 24.40 -3 -3 -9 226.98 26.10 3 3 9 242.48 22.00 3 3 9 228.58 21.90 3 3 9 73.19 47.70 3 3 9 218.88 28.20 3 3 9 202.08 31.30 3 3 9 175.78 21.90 4 3 9 31.90 11.40 4 3 9 27.80 10.90 4 3 9 34.10 20.30 4 3 9 23.70 12.90 -5 -3 -9 30.60 14.40 5 3 9 71.99 14.20 5 3 9 84.29 30.10 5 3 9 55.19 14.10 5 3 9 64.89 16.10 -6 -3 -9 49.00 19.70 6 3 9 62.09 17.00 6 3 9 23.60 7.80 6 3 9 41.70 10.80 6 3 9 25.50 13.70 3 -4 -9 170.68 27.50 3 -4 -9 103.29 16.50 -3 4 9 121.49 12.30 -3 4 9 111.29 14.70 -3 4 9 131.49 11.60 2 -4 -9 281.57 25.00 2 -4 -9 274.77 21.50 2 -4 -9 214.28 27.10 -2 4 9 261.97 21.20 -2 4 9 269.57 19.80 -2 4 9 252.77 25.80 1 -4 -9 -10.00 15.20 1 -4 -9 18.00 11.40 1 -4 -9 25.20 12.60 -1 4 9 21.60 10.70 -1 4 9 10.00 7.80 -1 4 9 22.90 8.70 0 -4 -9 42.10 14.60 0 -4 -9 63.09 14.90 0 4 9 58.69 14.10 0 4 9 53.59 13.20 0 4 9 47.80 12.30 0 4 9 10.90 17.40 -1 -4 -9 156.88 21.20 -1 -4 -9 127.29 20.10 1 4 9 134.19 20.00 1 4 9 108.59 25.00 1 4 9 113.39 19.10 1 4 9 129.99 22.80 -2 -4 -9 305.17 27.40 2 4 9 325.67 54.39 2 4 9 365.76 29.10 2 4 9 296.07 29.20 2 4 9 343.67 29.50 2 4 9 367.26 25.30 -3 -4 -9 77.69 16.10 3 4 9 7.60 49.99 3 4 9 79.49 16.40 3 4 9 54.29 16.60 3 4 9 92.99 14.80 3 4 9 87.99 16.20 3 4 9 105.89 22.20 -4 -4 -9 89.49 18.80 -4 -4 -9 50.69 16.40 4 4 9 73.89 16.10 4 4 9 66.79 12.50 4 4 9 90.49 29.70 4 4 9 14.30 23.20 4 4 9 63.59 15.00 4 4 9 74.29 18.20 -5 -4 -9 201.08 23.70 5 4 9 210.58 21.60 5 4 9 201.38 25.60 5 4 9 208.38 22.80 5 4 9 154.98 24.30 5 4 9 208.28 30.00 -6 -4 -9 34.30 10.70 -6 -4 -9 72.59 19.90 6 4 9 83.29 16.90 6 4 9 38.70 17.10 6 4 9 59.29 14.20 6 4 9 19.00 15.90 6 4 9 58.69 20.10 3 -5 -9 83.29 10.90 -3 5 9 75.19 16.00 -3 5 9 91.99 11.10 2 -5 -9 1.30 6.20 2 -5 -9 -3.10 11.30 -2 5 9 14.20 8.70 -2 5 9 -6.80 7.70 -2 5 9 11.20 11.80 1 -5 -9 123.49 17.70 1 -5 -9 61.69 20.70 -1 5 9 105.19 18.40 -1 5 9 98.49 21.20 -1 5 9 110.19 17.30 0 -5 -9 128.19 18.30 0 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-0.60 10.60 2 6 9 475.55 35.70 2 6 9 498.95 32.60 2 6 9 448.96 28.90 3 6 9 49.30 13.90 3 6 9 11.40 16.00 3 6 9 27.70 13.30 3 6 9 42.10 11.50 3 6 9 43.10 12.40 3 6 9 60.59 14.10 4 6 9 30.70 13.60 4 6 9 2.00 7.70 4 6 9 -8.10 7.80 4 6 9 2.80 13.40 4 6 9 3.60 10.60 5 6 9 154.08 32.70 5 6 9 99.39 15.10 5 6 9 104.49 15.90 5 6 9 109.69 15.10 6 6 9 19.80 8.40 6 6 9 12.50 24.00 6 6 9 26.30 8.40 6 6 9 7.60 13.80 1 -7 -9 72.99 18.50 -1 7 9 63.79 10.80 -1 7 9 30.60 15.30 -1 7 9 55.99 10.30 0 7 9 6.20 10.60 0 7 9 3.30 6.60 0 7 9 10.70 10.00 1 7 9 300.47 37.70 1 7 9 212.88 19.20 1 7 9 246.38 18.80 2 7 9 22.60 10.80 2 7 9 21.90 13.70 2 7 9 53.69 19.40 2 7 9 23.60 10.40 3 7 9 70.39 14.50 3 7 9 38.70 14.10 3 7 9 58.49 19.90 3 7 9 83.39 15.60 4 7 9 -2.70 13.40 4 7 9 8.60 14.20 4 7 9 17.40 12.50 4 7 9 6.80 14.70 5 7 9 41.40 11.20 5 7 9 23.90 20.00 5 7 9 45.40 10.60 5 7 9 29.80 8.90 0 8 9 42.50 8.90 1 8 9 100.19 12.20 1 8 9 80.49 13.70 1 8 9 124.19 12.10 2 8 9 27.00 9.40 2 8 9 31.00 18.30 2 8 9 10.30 10.30 3 8 9 23.40 14.80 3 8 9 28.30 16.40 3 8 9 33.20 10.40 4 8 9 150.28 15.50 4 8 9 131.19 16.30 5 8 9 140.09 13.30 5 8 9 156.78 15.10 1 0 -10 122.99 11.90 0 0 -10 56.69 11.80 0 0 10 47.70 10.30 0 0 10 52.79 9.90 -1 0 -10 44.30 9.40 -1 0 -10 17.10 16.80 -1 0 -10 35.50 7.90 1 0 10 17.80 14.20 1 0 10 29.50 7.40 1 0 10 15.00 8.00 -2 0 -10 163.48 29.10 -2 0 -10 154.28 18.40 -2 0 -10 106.49 18.80 2 0 10 133.69 16.30 2 0 10 114.69 20.40 -3 0 -10 7.60 9.00 -3 0 -10 0.10 8.80 3 0 10 4.20 10.80 3 0 10 8.70 6.90 3 0 10 8.90 6.60 2 -1 -10 16.40 8.70 2 -1 -10 15.00 10.40 -2 1 10 6.70 8.20 -2 1 10 35.60 9.50 1 -1 -10 164.98 22.10 1 -1 -10 192.08 26.50 1 -1 -10 169.98 15.10 1 -1 -10 173.78 22.90 -1 1 10 167.78 14.70 0 -1 -10 195.28 18.40 0 -1 -10 178.18 19.30 0 -1 -10 150.18 24.90 0 1 10 173.28 20.70 0 1 10 165.58 18.10 -1 -1 -10 0.90 12.80 -1 -1 -10 17.40 13.90 -1 -1 -10 10.80 9.80 1 1 10 20.20 7.90 1 1 10 -2.00 10.30 1 1 10 21.20 7.10 1 1 10 3.40 9.10 -2 -1 -10 15.60 11.80 -2 -1 -10 -1.30 14.10 -2 -1 -10 -0.10 11.00 2 1 10 18.20 9.40 2 1 10 7.70 9.50 2 1 10 6.10 8.20 2 1 10 2.70 7.00 -3 -1 -10 49.80 17.00 -3 -1 -10 49.20 9.10 -3 -1 -10 47.70 16.00 3 1 10 31.20 12.50 3 1 10 26.00 11.70 3 1 10 38.60 10.00 3 1 10 41.40 9.60 -4 -1 -10 39.10 12.20 -4 -1 -10 31.50 7.70 -4 -1 -10 28.50 24.20 4 1 10 50.49 10.40 4 1 10 21.10 7.30 4 1 10 32.30 8.80 2 -2 -10 64.99 16.10 2 -2 -10 88.89 20.00 2 -2 -10 101.79 12.30 -2 2 10 108.79 11.20 -2 2 10 137.39 19.30 -2 2 10 75.09 13.10 1 -2 -10 172.18 18.80 1 -2 -10 178.98 23.30 -1 2 10 171.58 17.20 -1 2 10 175.68 17.40 0 -2 -10 1.00 12.30 0 -2 -10 25.30 9.90 0 2 10 14.30 7.80 0 2 10 0.40 6.00 0 2 10 -4.20 10.70 0 2 10 2.60 12.20 -1 -2 -10 11.30 13.00 -1 -2 -10 5.40 9.40 1 2 10 8.90 9.60 1 2 10 -5.00 5.60 1 2 10 14.80 7.90 1 2 10 1.50 7.70 -2 -2 -10 -1.50 10.00 -2 -2 -10 4.30 13.20 2 2 10 3.40 8.40 2 2 10 5.00 7.20 2 2 10 2.90 12.80 2 2 10 6.00 9.00 -3 -2 -10 38.80 17.20 -3 -2 -10 50.59 15.60 3 2 10 79.19 21.80 3 2 10 50.49 12.40 3 2 10 85.09 14.90 3 2 10 72.19 11.60 -4 -2 -10 40.00 24.00 -4 -2 -10 15.80 14.00 -4 -2 -10 22.00 14.70 4 2 10 7.70 13.30 4 2 10 17.00 7.40 4 2 10 2.10 7.00 -5 -2 -10 201.88 14.70 5 2 10 159.68 13.90 5 2 10 157.58 20.10 2 -3 -10 124.89 16.70 2 -3 -10 130.69 11.90 -2 3 10 95.39 14.10 -2 3 10 80.39 10.80 -2 3 10 106.29 13.40 1 -3 -10 180.18 18.60 1 -3 -10 173.68 22.00 -1 3 10 173.68 22.60 -1 3 10 165.48 15.40 -1 3 10 243.38 27.60 0 -3 -10 19.70 9.80 0 -3 -10 -7.10 12.00 0 3 10 2.80 6.80 0 3 10 2.00 9.10 0 3 10 6.20 6.30 -1 -3 -10 1.40 11.50 -1 -3 -10 4.80 13.10 1 3 10 1.70 7.20 1 3 10 6.40 13.20 1 3 10 -4.50 10.20 1 3 10 -5.00 5.80 -2 -3 -10 233.18 22.10 -2 -3 -10 307.57 37.10 2 3 10 250.97 22.90 2 3 10 247.78 21.80 2 3 10 230.18 28.60 2 3 10 263.07 24.30 -3 -3 -10 46.50 14.80 3 3 10 38.20 11.00 3 3 10 35.10 14.40 3 3 10 41.10 10.70 3 3 10 14.20 12.80 -4 -3 -10 36.40 14.30 4 3 10 23.50 14.00 4 3 10 25.10 12.90 4 3 10 8.10 15.80 -5 -3 -10 123.09 16.10 -5 -3 -10 67.59 19.60 5 3 10 99.99 14.00 5 3 10 84.49 13.90 5 3 10 55.59 17.10 5 3 10 75.29 11.40 2 -4 -10 204.08 15.20 -2 4 10 234.78 17.60 -2 4 10 192.48 14.50 -2 4 10 192.88 15.60 1 -4 -10 15.40 27.30 1 -4 -10 61.79 15.10 1 -4 -10 53.09 13.00 -1 4 10 91.29 16.10 -1 4 10 31.90 16.30 0 -4 -10 73.29 27.60 0 -4 -10 54.79 11.90 0 -4 -10 57.29 14.10 0 4 10 65.49 11.90 0 4 10 59.19 12.10 0 4 10 54.99 12.20 -1 -4 -10 285.27 24.90 -1 -4 -10 344.57 25.90 1 4 10 336.47 29.10 1 4 10 301.67 24.70 1 4 10 337.37 23.60 1 4 10 328.57 22.50 -2 -4 -10 93.49 17.90 -2 -4 -10 115.69 23.90 2 4 10 123.09 18.00 2 4 10 76.39 21.10 2 4 10 104.89 14.00 2 4 10 92.39 18.90 -3 -4 -10 68.19 18.50 3 4 10 95.39 15.70 3 4 10 80.59 18.00 3 4 10 88.49 21.60 -4 -4 -10 43.10 13.60 -4 -4 -10 37.90 16.10 4 4 10 66.19 25.00 4 4 10 27.10 11.00 4 4 10 49.20 14.40 4 4 10 48.80 11.50 -5 -4 -10 162.48 20.10 5 4 10 172.68 18.40 5 4 10 137.59 25.90 5 4 10 207.28 19.40 5 4 10 160.88 16.10 1 -5 -10 108.19 12.90 -1 5 10 107.59 12.50 -1 5 10 119.29 18.30 -1 5 10 93.69 14.10 0 -5 -10 114.99 19.60 0 5 10 144.69 14.60 0 5 10 132.39 14.80 0 5 10 147.89 16.90 -1 -5 -10 119.59 27.80 1 5 10 153.58 15.30 1 5 10 132.49 18.10 1 5 10 143.69 15.40 2 5 10 10.40 7.60 2 5 10 16.60 9.30 2 5 10 -4.10 9.00 2 5 10 1.70 21.00 3 5 10 115.99 25.70 3 5 10 50.09 13.00 3 5 10 46.60 14.20 3 5 10 29.40 12.00 3 5 10 61.89 11.40 4 5 10 141.09 23.00 4 5 10 113.29 17.90 5 5 10 21.90 12.10 5 5 10 12.20 7.00 5 5 10 44.90 17.60 5 5 10 26.70 9.10 -1 6 10 29.30 8.20 -1 6 10 47.10 9.80 0 6 10 136.59 16.80 0 6 10 134.59 12.90 0 6 10 124.49 15.30 1 6 10 79.19 19.10 1 6 10 42.40 9.50 2 6 10 584.34 34.20 2 6 10 637.54 40.90 2 6 10 595.44 46.10 3 6 10 18.10 11.50 3 6 10 42.20 14.40 3 6 10 -15.50 14.30 4 6 10 58.99 14.10 4 6 10 50.89 13.20 4 6 10 75.69 12.10 4 6 10 63.99 11.80 5 6 10 92.59 19.70 5 6 10 39.30 13.50 5 6 10 61.89 14.00 0 7 10 -6.60 7.40 0 7 10 -1.90 7.50 0 7 10 24.00 16.30 1 7 10 569.64 29.60 2 7 10 5.90 18.30 2 7 10 18.40 6.60 2 7 10 18.70 6.90 3 7 10 19.80 12.60 3 7 10 23.80 8.10 3 7 10 24.40 15.40 3 7 10 30.50 10.10 4 7 10 41.90 15.40 4 7 10 57.39 13.20 4 7 10 49.30 11.60 1 2 11 16.50 9.00 1 2 11 21.50 7.00 1 2 11 18.80 8.40 -2 -2 -11 138.19 16.10 2 2 11 119.49 12.60 2 2 11 137.69 15.50 2 2 11 91.49 12.80 2 2 11 111.99 13.80 0 -3 -11 37.70 7.70 0 3 11 40.40 9.00 0 3 11 51.59 9.20 1 3 11 223.88 17.80 1 3 11 231.78 16.10 1 3 11 180.78 17.00 1 3 11 231.08 18.70 -2 -3 -11 23.00 10.00 2 3 11 38.40 9.60 2 3 11 17.60 7.10 2 3 11 22.80 13.60 2 3 11 35.70 10.10 3 3 11 26.10 8.60 3 3 11 48.00 12.60 3 3 11 23.60 9.80 0 -4 -11 91.29 16.00 0 4 11 102.89 16.90 0 4 11 74.19 10.30 0 4 11 109.49 12.90 -1 -4 -11 21.50 16.80 1 4 11 13.20 8.60 1 4 11 3.30 5.80 1 4 11 6.80 5.90 2 4 11 1.60 6.30 2 4 11 3.60 11.60 2 4 11 0.60 7.70 2 4 11 2.10 6.20 3 4 11 94.29 17.80 3 4 11 54.09 13.10 3 4 11 64.49 12.30 3 4 11 89.29 14.40 4 4 11 68.89 13.60 1 5 11 40.80 8.60 1 5 11 33.10 7.50 1 5 11 17.60 8.40 2 5 11 46.70 10.30 2 5 11 34.40 8.50 2 5 11 25.00 7.20 2 5 11 17.20 10.10 3 5 11 23.00 7.50 3 5 11 19.20 8.20 3 5 11 28.80 11.40 3 5 11 10.30 8.30 2 6 11 77.79 10.10 2 6 11 83.29 13.50 3 6 11 38.80 9.50 3 6 11 22.50 11.30 3 6 11 49.90 9.50 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 6297 #============================================================================= # end of cif data for "gil10360" (compound 5e) #============================================================================= #============================================================================= # cif data for "gil10302" (compound 5k) #============================================================================= data_gil10302_5k _audit_creation_method 'APEX4 v2021.4-0' _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H9 Br F2 O2' _chemical_formula_iupac ? _chemical_formula_weight 291.09 _chemical_melting_point ? _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 5.8059(2) _cell_length_b 26.6422(8) _cell_length_c 6.9652(2) _cell_angle_alpha 90 _cell_angle_beta 101.1680(10) _cell_angle_gamma 90 _cell_volume 1056.99(6) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9866 _cell_measurement_theta_min 6.6884 _cell_measurement_theta_max 66.8173 _cell_measurement_temperature 100.(2) _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.242 _exptl_crystal_size_mid 0.128 _exptl_crystal_size_min 0.086 _exptl_crystal_density_diffrn 1.829 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 576 _exptl_absorpt_coefficient_mu 5.449 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_process_details ; Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015). "Comparison of silver and molybdenum microfocus X-ray sources for single-crystal structure determination" J. Appl. Cryst. 48, 3-10. doi:10.1107/S1600576714022985 ; _exptl_absorpt_correction_T_min 0.49 _exptl_absorpt_correction_T_max 0.65 _exptl_special_details ; ; _diffrn_ambient_temperature 100.(2) _diffrn_source 'Cu ImS' _diffrn_source_type 'micro focus tube' _diffrn_source_power 0.05 _diffrn_source_current 1.0 _diffrn_source_voltage 50 _diffrn_radiation_probe 'single crystal' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_monochromator 'MX mirror' _diffrn_measurement_device 'Bruker D8 Venture Photon III' _diffrn_measurement_device_type 'single crystal diffractometer' _diffrn_measurement_method 'phi/omega scans' _diffrn_detector_area_resol_mean 7.3910 _diffrn_reflns_number 17090 _diffrn_reflns_av_R_equivalents 0.0357 _diffrn_reflns_av_unetI/netI 0.0201 _diffrn_reflns_theta_min 6.69 _diffrn_reflns_theta_max 66.86 _diffrn_reflns_theta_full 66.86 _diffrn_measured_fraction_theta_max 0.975 _diffrn_measured_fraction_theta_full 0.975 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _refine_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_number_total 1822 _reflns_number_gt 1782 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0228 _refine_ls_R_factor_gt 0.0224 _refine_ls_wR_factor_gt 0.0578 _refine_ls_wR_factor_ref 0.0582 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_number_reflns 1822 _refine_ls_number_parameters 149 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_hydrogen_treatment mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0291P)^2^+0.8165P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary ? _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.357 _refine_diff_density_min -0.432 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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' Br Br -0.6763 1.2805 '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' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection 'Bruker APEX4 v2021.4-0 Photon III' _computing_cell_refinement 'SAINT V8.40B (Bruker AXS LLC, 2019)' _computing_data_reduction 'SAINT V8.40B (Bruker AXS LLC, 2019)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_molecular_graphics 'shelXle (C.B. Huebschle, rev 1242)' _computing_publication_material 'SHELXT 2018/2 (Sheldrick, 2018)' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_flags_posn _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Br Br1 0.68609(3) 0.74909(2) 0.00674(3) 0.01911(11) Uani d . . . 1 . . F F1 0.7892(2) 0.63979(4) 0.65494(15) 0.0291(3) Uani d . . . 1 . . F F2 0.70284(17) 0.56933(4) 0.50131(14) 0.0228(3) Uani d . . . 1 . . O O1 0.7649(2) 0.50112(4) 0.81967(18) 0.0200(3) Uani d . . . 1 . . O O2 0.8486(2) 0.55297(5) 1.07642(19) 0.0221(3) Uani d . . . 1 . . H H01 0.971(6) 0.5340(11) 1.097(4) 0.055(8) Uiso d . . . 1 . . C C1 0.2821(3) 0.69077(6) 0.0296(2) 0.0157(3) Uani d . . . 1 . . H H1 0.211808 0.708343 -0.085603 0.019000 Uiso calc U . R 1 . . C C2 0.5121(3) 0.70042(6) 0.1200(2) 0.0149(3) Uani d . . . 1 . . C C3 0.6188(3) 0.67615(6) 0.2902(2) 0.0143(3) Uani d . . . 1 . . H H3 0.776367 0.683574 0.350236 0.017000 Uiso calc U . R 1 . . C C4 0.4896(3) 0.64065(6) 0.3711(2) 0.0140(3) Uani d . . . 1 . . C C5 0.2588(3) 0.62981(6) 0.2814(2) 0.0155(3) Uani d . . . 1 . . H H5 0.171649 0.605383 0.336570 0.019000 Uiso calc U . R 1 . . C C6 0.1566(3) 0.65486(6) 0.1110(2) 0.0164(3) Uani d . . . 1 . . H H6 -0.000425 0.647345 0.049758 0.020000 Uiso calc U . R 1 . . C C7 0.6016(3) 0.61244(6) 0.5544(2) 0.0157(3) Uani d . . . 1 . . C C8 0.4369(3) 0.60129(6) 0.6894(2) 0.0171(4) Uani d . . . 1 . . H H8 0.338917 0.630741 0.712359 0.020000 Uiso calc U . R 1 . . C C9 0.3111(3) 0.55217(7) 0.6862(3) 0.0215(4) Uani d . . . 1 . . H H9A 0.351561 0.525482 0.599501 0.026000 Uiso calc U . R 1 . . H H9B 0.144040 0.552919 0.698367 0.026000 Uiso calc U . R 1 . . C C10 0.4924(3) 0.56580(7) 0.8642(3) 0.0194(4) Uani d . . . 1 . . H H10 0.425650 0.576395 0.979866 0.023000 Uiso calc U . R 1 . . C C11 0.7142(3) 0.53679(6) 0.9139(2) 0.0160(4) Uani d . . . 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Br1 0.01911(15) 0.01944(15) 0.01893(15) -0.00012(6) 0.00408(10) 0.00760(6) F1 0.0274(6) 0.0351(6) 0.0197(5) -0.0143(5) -0.0081(4) 0.0089(5) F2 0.0244(6) 0.0239(6) 0.0224(6) 0.0123(4) 0.0098(4) 0.0067(4) O1 0.0213(6) 0.0185(6) 0.0188(6) 0.0034(5) 0.0002(5) 0.0009(5) O2 0.0234(7) 0.0185(6) 0.0222(7) 0.0034(5) -0.0012(5) -0.0015(5) C1 0.0191(9) 0.0157(8) 0.0119(8) 0.0047(7) 0.0020(6) 0.0006(6) C2 0.0192(8) 0.0124(8) 0.0143(8) 0.0014(6) 0.0058(6) -0.0001(6) C3 0.0145(8) 0.0137(8) 0.0144(8) 0.0013(6) 0.0021(6) -0.0007(6) C4 0.0182(8) 0.0125(8) 0.0114(8) 0.0027(6) 0.0031(6) -0.0016(6) C5 0.0178(8) 0.0137(8) 0.0155(8) -0.0013(6) 0.0043(6) -0.0013(6) C6 0.0156(8) 0.0172(8) 0.0155(8) 0.0004(7) 0.0009(7) -0.0029(7) C7 0.0155(8) 0.0160(8) 0.0143(8) -0.0008(6) -0.0001(6) 0.0001(6) C8 0.0203(9) 0.0175(8) 0.0135(8) 0.0059(7) 0.0035(6) 0.0035(7) C9 0.0160(9) 0.0244(9) 0.0242(9) 0.0013(7) 0.0040(7) 0.0084(7) C10 0.0217(9) 0.0208(9) 0.0176(9) 0.0041(7) 0.0086(7) 0.0064(7) C11 0.0184(8) 0.0154(8) 0.0145(8) -0.0021(7) 0.0042(7) 0.0059(7) _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_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Br1 C2 . 1.9058(17) ? F1 C7 . 1.383(2) ? F2 C7 . 1.373(2) ? O1 C11 . 1.223(2) ? O2 C11 . 1.317(2) ? O2 H01 . 0.86(3) ? C1 C2 . 1.386(2) ? C1 C6 . 1.388(2) ? C1 H1 . 0.950000 ? C2 C3 . 1.387(2) ? C3 C4 . 1.393(2) ? C3 H3 . 0.950000 ? C4 C5 . 1.394(2) ? C4 C7 . 1.515(2) ? C5 C6 . 1.391(2) ? C5 H5 . 0.950000 ? C6 H6 . 0.950000 ? C7 C8 . 1.495(2) ? C8 C9 . 1.497(2) ? C8 C10 . 1.526(2) ? C8 H8 . 1.000000 ? C9 C10 . 1.507(3) ? C9 H9A . 0.990000 ? C9 H9B . 0.990000 ? C10 C11 . 1.484(2) ? C10 H10 . 1.000000 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C11 O2 H01 . . 107.(2) ? C2 C1 C6 . . 118.56(15) ? C2 C1 H1 . . 120.700000 ? C6 C1 H1 . . 120.700000 ? C1 C2 C3 . . 122.24(16) ? C1 C2 Br1 . . 118.66(12) ? C3 C2 Br1 . . 119.09(13) ? C2 C3 C4 . . 118.44(16) ? C2 C3 H3 . . 120.800000 ? C4 C3 H3 . . 120.800000 ? C3 C4 C5 . . 120.37(15) ? C3 C4 C7 . . 120.05(15) ? C5 C4 C7 . . 119.56(15) ? C6 C5 C4 . . 119.82(16) ? C6 C5 H5 . . 120.100000 ? C4 C5 H5 . . 120.100000 ? C1 C6 C5 . . 120.56(16) ? C1 C6 H6 . . 119.700000 ? C5 C6 H6 . . 119.700000 ? F2 C7 F1 . . 103.94(13) ? F2 C7 C8 . . 111.25(14) ? F1 C7 C8 . . 108.85(14) ? F2 C7 C4 . . 108.93(13) ? F1 C7 C4 . . 109.44(13) ? C8 C7 C4 . . 113.95(14) ? C7 C8 C9 . . 122.27(15) ? C7 C8 C10 . . 124.27(15) ? C9 C8 C10 . . 59.81(12) ? C7 C8 H8 . . 113.400000 ? C9 C8 H8 . . 113.400000 ? C10 C8 H8 . . 113.400000 ? C8 C9 C10 . . 61.05(11) ? C8 C9 H9A . . 117.700000 ? C10 C9 H9A . . 117.700000 ? C8 C9 H9B . . 117.700000 ? C10 C9 H9B . . 117.700000 ? H9A C9 H9B . . 114.800000 ? C11 C10 C9 . . 120.17(15) ? C11 C10 C8 . . 123.26(15) ? C9 C10 C8 . . 59.14(11) ? C11 C10 H10 . . 114.400000 ? C9 C10 H10 . . 114.400000 ? C8 C10 H10 . . 114.400000 ? O1 C11 O2 . . 123.47(16) ? O1 C11 C10 . . 124.59(16) ? O2 C11 C10 . . 111.91(15) ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C6 C1 C2 C3 . . . . -1.2(2) ? C6 C1 C2 Br1 . . . . 179.23(12) ? C1 C2 C3 C4 . . . . 0.5(2) ? Br1 C2 C3 C4 . . . . -179.94(12) ? C2 C3 C4 C5 . . . . 0.3(2) ? C2 C3 C4 C7 . . . . 178.57(15) ? C3 C4 C5 C6 . . . . -0.5(2) ? C7 C4 C5 C6 . . . . -178.72(15) ? C2 C1 C6 C5 . . . . 1.1(2) ? C4 C5 C6 C1 . . . . -0.2(2) ? C3 C4 C7 F2 . . . . -90.31(17) ? C5 C4 C7 F2 . . . . 87.94(18) ? C3 C4 C7 F1 . . . . 22.7(2) ? C5 C4 C7 F1 . . . . -159.04(14) ? C3 C4 C7 C8 . . . . 144.83(16) ? C5 C4 C7 C8 . . . . -36.9(2) ? F2 C7 C8 C9 . . . . -28.0(2) ? F1 C7 C8 C9 . . . . -141.94(15) ? C4 C7 C8 C9 . . . . 95.62(19) ? F2 C7 C8 C10 . . . . 45.2(2) ? F1 C7 C8 C10 . . . . -68.8(2) ? C4 C7 C8 C10 . . . . 168.79(15) ? C7 C8 C9 C10 . . . . 113.77(18) ? C8 C9 C10 C11 . . . . -113.06(18) ? C7 C8 C10 C11 . . . . -2.6(3) ? C9 C8 C10 C11 . . . . 107.95(19) ? C7 C8 C10 C9 . . . . -110.56(19) ? C9 C10 C11 O1 . . . . -0.3(3) ? C8 C10 C11 O1 . . . . -71.2(2) ? C9 C10 C11 O2 . . . . -178.26(14) ? C8 C10 C11 O2 . . . . 110.90(19) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O2 H01 O1 3_767 0.86(3) 1.80(3) 2.6468(18) 171.(3) ? C1 H1 Br1 4_575 0.950000 3.030000 3.9183(17) 155.500000 ? C3 H3 Br1 4_676 0.950000 3.010000 3.8942(17) 155.400000 ? _shelx_res_file ; TITL gil10302.res in P2(1)/n gil10302.res created by SHELXL-2018/3 at 08:36:03 on 16-Mar-2022 REM Old TITL cu_gil10302_0m in P2(1)/n REM SHELXT solution in P2(1)/n: R1 0.086, Rweak 0.003, Alpha 0.034 REM 1.991 for 55 systematic absences, Orientation as input REM Formula found by SHELXT: C11 Br F2 O2 CELL 1.54178 5.8059 26.6422 6.9652 90.000 101.168 90.000 ZERR 4.000 0.0002 0.0008 0.0002 0.000 0.001 0.000 LATT 1 SYMM 1/2-X, 1/2+Y, 1/2-Z SFAC C H Br F O UNIT 44 36 4 8 8 LIST 4 SIZE 0.086 0.128 0.242 TEMP -173.150 ACTA CONF L.S. 40 BOND $H FMAP 2 PLAN 10 HTAB EQIV $1 -x+2, -y+1, -z+2 HTAB O2 O1_$1 EQIV $2 x-1/2, -y+3/2, z-1/2 HTAB C1 Br1_$2 EQIV $3 x+1/2, -y+3/2, z+1/2 HTAB C3 Br1_$3 OMIT -3 0 1 OMIT 1 6 3 WGHT 0.029100 0.816500 FVAR 0.81728 BR1 3 0.686091 0.749090 0.006735 11.00000 0.01911 0.01944 = 0.01893 0.00760 0.00408 -0.00012 F1 4 0.789199 0.639793 0.654940 11.00000 0.02742 0.03511 = 0.01970 0.00887 -0.00807 -0.01431 F2 4 0.702844 0.569329 0.501310 11.00000 0.02437 0.02394 = 0.02237 0.00668 0.00984 0.01229 O1 5 0.764890 0.501115 0.819666 11.00000 0.02125 0.01851 = 0.01884 0.00086 0.00020 0.00336 O2 5 0.848644 0.552972 1.076424 11.00000 0.02335 0.01850 = 0.02220 -0.00154 -0.00125 0.00341 H01 2 0.970690 0.534031 1.097393 11.00000 0.05461 C1 1 0.282104 0.690771 0.029575 11.00000 0.01907 0.01572 = 0.01187 0.00062 0.00196 0.00469 AFIX 43 H1 2 0.211808 0.708343 -0.085603 11.00000 -1.20000 AFIX 0 C2 1 0.512111 0.700420 0.119960 11.00000 0.01915 0.01237 = 0.01432 -0.00006 0.00581 0.00135 C3 1 0.618811 0.676152 0.290217 11.00000 0.01455 0.01371 = 0.01436 -0.00073 0.00211 0.00130 AFIX 43 H3 2 0.776367 0.683574 0.350236 11.00000 -1.20000 AFIX 0 C4 1 0.489551 0.640648 0.371117 11.00000 0.01823 0.01250 = 0.01140 -0.00162 0.00308 0.00272 C5 1 0.258796 0.629812 0.281412 11.00000 0.01785 0.01369 = 0.01549 -0.00132 0.00430 -0.00127 AFIX 43 H5 2 0.171649 0.605383 0.336570 11.00000 -1.20000 AFIX 0 C6 1 0.156595 0.654863 0.110995 11.00000 0.01562 0.01717 = 0.01554 -0.00292 0.00091 0.00042 AFIX 43 H6 2 -0.000425 0.647345 0.049758 11.00000 -1.20000 AFIX 0 C7 1 0.601600 0.612441 0.554379 11.00000 0.01550 0.01597 = 0.01434 0.00014 -0.00009 -0.00080 C8 1 0.436882 0.601289 0.689408 11.00000 0.02029 0.01750 = 0.01349 0.00350 0.00345 0.00590 AFIX 13 H8 2 0.338917 0.630741 0.712359 11.00000 -1.20000 AFIX 0 C9 1 0.311085 0.552166 0.686180 11.00000 0.01602 0.02442 = 0.02417 0.00835 0.00397 0.00126 AFIX 23 H9A 2 0.351561 0.525482 0.599501 11.00000 -1.20000 H9B 2 0.144040 0.552919 0.698367 11.00000 -1.20000 AFIX 0 C10 1 0.492376 0.565799 0.864178 11.00000 0.02173 0.02079 = 0.01763 0.00644 0.00865 0.00412 AFIX 13 H10 2 0.425650 0.576395 0.979866 11.00000 -1.20000 AFIX 0 C11 1 0.714176 0.536787 0.913887 11.00000 0.01843 0.01536 = 0.01455 0.00591 0.00422 -0.00212 HKLF 4 REM gil10302.res in P2(1)/n REM wR2 = 0.058163, GooF = S = 1.06328, Restrained GooF = 1.06328 for all data REM R1 = 0.022375 for 1782 Fo > 4sig(Fo) and 0.022814 for all 1822 data REM 149 parameters refined using 0 restraints END WGHT 0.0288 0.8190 REM Instructions for potential hydrogen bonds HTAB O2 O1_$1 HTAB C1 Br1_$2 HTAB C3 Br1_$3 REM Highest difference peak 0.357, deepest hole -0.432, 1-sigma level 0.064 Q1 1 0.6997 0.7961 -0.0014 11.00000 0.05 0.36 Q2 1 0.6982 0.7025 0.0128 11.00000 0.05 0.32 Q3 1 0.5482 0.6263 0.4571 11.00000 0.05 0.32 Q4 1 0.5449 0.6651 0.3458 11.00000 0.05 0.31 Q5 1 0.7144 0.7137 -0.0369 11.00000 0.05 0.30 Q6 1 0.5862 0.7873 0.0611 11.00000 0.05 0.29 Q7 1 0.6447 0.7439 -0.1553 11.00000 0.05 0.28 Q8 1 0.2458 0.6775 0.0941 11.00000 0.05 0.27 Q9 1 0.5779 0.7151 0.0750 11.00000 0.05 0.27 Q10 1 0.1765 0.6495 0.2091 11.00000 0.05 0.25 ; _shelx_res_checksum 19052 _shelx_hkl_file ; -3 0 0 2.50 1.00 3 0 0 0.40 1.10 3 0 0 0.50 1.30 -3 0 0 2.80 1.40 4 0 0 665.23 31.70 4 0 0 638.44 31.60 -4 0 0 627.94 30.30 4 0 0 685.63 31.10 4 0 0 666.23 30.90 -4 0 0 621.14 30.40 -4 0 0 636.24 31.70 4 0 0 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99.59 0 20 -2 2280.37 99.99 0 20 -2 2276.77 100.09 0 20 -2 1984.90 101.89 0 20 2 2194.28 102.49 0 20 2 2207.68 100.79 0 20 -2 2162.58 99.29 0 20 2 2248.48 101.89 0 20 2 2166.28 99.49 1 -20 2 150.08 9.20 1 -20 2 138.89 9.50 -1 -20 -2 135.39 8.50 -1 -20 -2 134.49 8.10 1 -20 2 133.79 8.40 -1 20 -2 131.29 10.30 1 20 2 132.29 8.50 1 20 2 132.39 7.30 1 20 2 126.19 8.40 -1 20 -2 128.29 8.10 1 20 2 129.89 9.90 -1 20 -2 135.49 8.00 1 20 2 137.39 8.30 1 20 2 133.49 7.40 -1 20 -2 135.29 7.40 1 20 2 123.59 10.10 2 -20 2 902.61 40.10 -2 -20 -2 759.42 38.90 2 -20 2 837.92 38.80 -2 -20 -2 853.61 40.30 -2 -20 -2 797.82 38.70 -2 20 -2 784.72 37.60 2 20 2 857.41 38.80 2 20 2 777.72 39.00 2 20 2 828.82 42.10 -2 20 -2 737.93 41.30 -2 20 -2 830.02 38.90 -2 20 -2 836.12 39.00 2 20 2 764.82 37.90 3 -20 2 -1.50 1.90 3 -20 2 -0.50 2.40 3 -20 2 0.30 1.50 -3 -20 -2 1.90 2.30 -3 20 -2 1.60 2.20 -3 20 -2 1.90 1.80 3 20 2 0.00 1.70 3 20 2 -0.30 1.60 -3 20 -2 0.60 1.20 -3 20 -2 -0.10 1.50 3 20 2 0.60 1.20 -4 -20 -2 42.00 4.90 -4 20 -2 35.00 4.20 -4 20 -2 46.50 3.30 -5 -21 2 1.60 1.20 -5 -21 2 0.90 1.70 5 -21 -2 1.50 1.10 5 -21 -2 2.00 1.60 5 21 -2 1.30 0.90 -5 21 2 1.00 1.10 5 21 -2 1.10 1.70 -5 21 2 1.60 0.80 4 -21 -2 921.91 43.00 -4 -21 2 965.80 43.80 4 -21 -2 825.62 44.80 4 -21 -2 892.81 42.80 -4 -21 2 824.52 45.30 -4 -21 2 994.30 43.00 4 21 -2 933.31 42.70 4 21 -2 846.52 43.20 -4 21 2 986.40 42.70 -4 21 2 915.41 42.60 4 21 -2 974.70 42.40 3 -21 -2 4.60 2.30 3 -21 -2 4.00 2.30 3 -21 -2 3.10 2.10 -3 -21 2 7.00 2.10 3 -21 -2 4.70 3.00 -3 -21 2 1.60 2.50 -3 -21 2 -5.70 4.30 -3 -21 2 1.20 2.00 -3 21 2 2.40 2.80 3 21 -2 -1.80 3.10 -3 21 2 2.20 1.50 -3 21 2 3.20 1.50 -3 21 2 1.30 3.10 3 21 -2 2.30 1.50 3 21 -2 2.30 1.60 3 21 -2 0.50 1.40 -2 -21 2 1963.20 90.59 -2 -21 2 2030.30 88.99 2 -21 -2 1785.62 89.49 2 -21 -2 1936.71 89.29 2 -21 -2 1890.71 90.09 -2 -21 2 2049.70 90.19 2 -21 -2 1972.90 90.79 -2 21 2 1927.71 88.69 -2 21 2 2034.20 88.79 2 21 -2 2014.20 89.19 2 21 -2 1840.52 89.19 -2 21 2 1844.72 89.99 2 21 -2 1894.31 88.99 -1 -21 2 87.09 6.90 -1 -21 2 95.09 6.60 -1 -21 2 86.09 5.70 1 -21 -2 89.99 7.00 1 -21 -2 82.29 6.80 -1 -21 2 89.09 6.60 1 21 -2 84.89 5.60 1 21 -2 93.69 5.20 1 21 -2 84.69 7.00 -1 21 2 82.39 7.20 -1 21 2 85.19 5.30 1 21 -2 84.79 5.70 -1 21 2 86.39 8.20 -1 21 2 90.99 5.50 1 21 -2 85.59 5.00 0 -21 -2 723.13 35.00 0 -21 -2 747.13 36.10 0 -21 2 743.63 36.10 0 -21 2 784.82 36.90 0 -21 2 739.53 34.80 0 -21 2 750.52 36.00 0 21 -2 674.93 37.30 0 21 2 757.22 36.00 0 21 2 712.73 35.40 0 21 2 762.82 38.00 0 21 2 747.23 34.80 0 21 -2 747.83 34.60 0 21 2 755.22 34.70 0 21 -2 727.23 35.30 0 21 2 736.93 37.10 -1 -21 -2 0.20 2.50 -1 -21 -2 4.20 1.90 1 -21 2 4.40 2.40 1 -21 2 4.30 1.90 1 -21 2 1.70 1.90 -1 -21 -2 3.10 2.10 1 -21 2 3.20 2.20 1 21 2 5.40 1.50 -1 21 -2 3.60 3.20 -1 21 -2 2.50 1.40 -1 21 -2 5.20 2.00 1 21 2 0.50 3.20 1 21 2 1.80 1.70 1 21 2 5.20 3.10 1 21 2 3.30 1.40 -1 21 -2 2.50 1.90 1 21 2 3.40 2.00 1 21 2 3.60 4.50 -2 -21 -2 1215.88 56.19 2 -21 2 1186.98 57.79 -2 -21 -2 1198.08 56.39 -2 -21 -2 1180.48 56.59 2 -21 2 1190.98 56.09 2 -21 2 1276.07 57.39 -2 21 -2 1120.69 58.89 2 21 2 1207.18 56.39 -2 21 -2 1229.28 56.29 2 21 2 1174.08 59.09 3 -21 2 19.70 2.40 -3 -21 -2 17.70 3.10 -3 -21 -2 14.80 3.10 3 21 2 16.60 2.40 -3 21 -2 25.20 3.10 -3 21 -2 21.90 3.10 3 21 2 18.10 2.20 -3 21 -2 20.80 2.50 3 21 2 23.20 3.20 -3 21 -2 27.70 3.50 -4 21 -2 872.71 43.80 -4 21 -2 965.90 43.40 4 21 2 970.10 43.70 -4 21 -2 953.90 44.00 -4 -22 2 76.59 6.40 4 -22 -2 67.99 5.40 -4 -22 2 76.89 5.70 4 -22 -2 76.49 5.00 -4 -22 2 78.79 4.90 4 -22 -2 71.79 4.90 -4 22 2 79.69 4.70 4 22 -2 74.09 4.60 4 22 -2 67.59 5.50 -4 22 2 75.09 4.60 -3 -22 2 125.19 7.30 -3 -22 2 125.49 8.80 3 -22 -2 120.29 8.10 -3 -22 2 125.19 8.20 3 -22 -2 124.69 7.40 -3 -22 2 91.59 9.70 3 22 -2 106.69 7.20 3 22 -2 131.49 7.00 3 22 -2 121.99 7.10 -3 22 2 126.49 6.90 -3 22 2 122.69 6.90 -2 -22 2 545.45 30.40 2 -22 -2 580.54 29.60 -2 -22 2 641.64 30.50 -2 -22 2 641.94 31.00 2 -22 -2 637.74 30.70 -2 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487.65 23.90 -2 23 2 492.05 26.70 2 23 -2 479.45 25.90 -1 -23 2 53.89 4.40 1 -23 -2 52.79 6.60 -1 -23 2 56.49 5.50 1 -23 -2 63.39 5.40 -1 -23 2 56.59 5.70 -1 -23 2 63.59 5.70 1 23 -2 63.49 4.40 1 23 -2 54.09 3.30 -1 23 2 57.89 6.80 1 23 -2 58.89 4.50 -1 23 2 60.89 5.40 1 23 -2 59.59 5.90 -1 23 2 55.89 4.20 -1 23 2 60.39 4.20 -1 23 2 47.50 6.90 0 -23 2 18.70 2.40 0 -23 -2 10.10 2.20 0 -23 -2 8.90 2.60 0 -23 2 10.30 2.70 0 23 -2 14.50 3.50 0 23 2 13.20 2.10 0 23 -2 22.60 2.50 0 23 -2 19.40 2.30 0 23 -2 15.40 2.60 0 23 2 21.90 3.70 0 23 2 9.90 3.80 0 23 2 17.70 5.10 -1 -23 -2 69.09 5.50 1 -23 2 66.49 6.20 1 -23 2 73.89 6.60 -1 -23 -2 69.69 5.20 1 -23 2 69.99 5.50 -1 -23 -2 68.49 6.30 -1 23 -2 73.99 5.20 1 23 2 80.09 6.10 1 23 2 73.79 5.80 -1 23 -2 78.19 6.00 -1 23 -2 71.09 8.40 1 23 2 74.59 8.40 1 23 2 70.79 4.70 -2 -23 -2 2009.50 93.09 2 -23 2 2028.00 92.79 -2 -23 -2 1904.41 93.59 -2 -23 -2 1954.30 94.19 2 -23 2 2101.99 94.69 2 -23 2 2096.59 94.09 -2 23 -2 1998.60 93.09 2 23 2 1956.30 92.99 -2 23 -2 2017.40 92.99 2 23 2 2039.10 92.89 -2 23 -2 2066.49 92.29 2 23 2 2038.40 92.09 3 -23 2 187.68 11.70 -3 -23 -2 166.28 10.40 3 -23 2 182.28 10.80 -3 23 -2 181.08 10.50 3 23 2 191.88 9.30 -3 23 -2 189.18 10.40 -3 23 -2 203.38 9.60 -4 23 -2 816.32 36.90 4 23 2 775.32 37.60 -4 -24 2 48.20 4.50 4 -24 -2 42.10 3.20 -4 -24 2 46.90 4.60 4 24 -2 41.50 3.30 -4 24 2 55.19 3.30 4 24 -2 47.90 3.80 -3 -24 2 19.80 3.60 3 -24 -2 15.10 3.70 3 -24 -2 17.90 2.80 -3 -24 2 12.60 2.60 -3 -24 2 16.90 2.30 -3 24 2 23.40 2.70 -3 24 2 22.00 2.50 3 24 -2 17.70 2.30 3 24 -2 24.30 2.50 3 24 -2 17.20 2.60 -2 -24 2 187.68 9.90 2 -24 -2 177.38 12.70 -2 -24 2 165.28 11.20 -2 -24 2 183.78 11.40 -2 -24 2 182.78 10.90 2 -24 -2 171.58 9.90 2 24 -2 183.08 9.80 -2 24 2 191.28 9.70 -2 24 2 182.18 9.60 2 24 -2 186.48 9.80 -1 -24 2 2.30 2.20 -1 -24 2 4.80 1.60 -1 -24 2 0.80 2.00 1 -24 -2 1.50 2.20 -1 -24 2 3.60 2.30 1 -24 -2 -3.40 2.80 1 24 -2 0.60 1.40 -1 24 2 3.40 1.40 -1 24 2 1.90 4.40 -1 24 2 1.60 3.90 1 24 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765.22 35.90 5 -2 -3 2084.39 101.39 5 -2 -3 2077.29 101.09 5 -2 -3 2343.57 100.89 5 -2 -3 2202.68 99.59 -5 -2 3 1979.10 98.59 5 -2 -3 2193.28 99.69 5 -2 -3 2273.87 99.99 5 2 -3 2198.48 101.59 5 2 -3 2307.37 99.89 5 2 -3 2217.48 100.49 5 2 -3 2030.80 101.09 -5 2 3 1956.20 98.49 5 2 -3 2231.28 99.49 5 2 -3 2214.78 100.19 4 -2 -3 265.17 14.00 4 -2 -3 268.37 15.00 4 -2 -3 274.27 14.90 4 2 -3 273.87 15.00 4 2 -3 263.97 14.90 4 2 -3 274.57 14.60 4 2 -3 230.68 14.50 4 2 -3 279.17 14.50 -3 -2 3 5270.37 233.78 3 -2 -3 5233.78 235.68 3 -2 -3 5213.28 234.58 3 2 -3 5421.96 235.18 3 2 -3 4858.51 234.38 -3 2 3 5025.80 233.68 -2 -2 3 1921.21 88.19 2 -2 -3 2004.00 89.29 -2 -2 3 1879.31 88.49 2 -2 -3 2060.79 89.59 2 2 -3 2008.70 89.39 -2 2 3 1844.12 88.39 2 2 -3 1931.41 89.29 -1 -2 3 1264.37 55.69 -1 -2 3 1272.87 55.99 1 -2 -3 1199.88 55.69 -1 2 3 1202.68 55.59 1 2 -3 1175.18 55.79 -1 2 3 1204.98 55.89 1 2 -3 1199.98 55.79 0 -2 3 26.80 2.40 0 -2 3 27.30 2.90 0 -2 3 29.50 2.50 0 2 3 25.40 2.60 0 2 3 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-19 -6 10.70 1.90 3 19 -6 11.00 1.70 3 19 -6 11.30 1.60 -3 19 6 13.10 1.70 2 -19 -6 769.62 36.70 2 -19 -6 753.32 36.20 -2 -19 6 838.22 35.90 -2 19 6 811.02 35.70 -2 19 6 709.13 35.30 2 19 -6 736.13 35.70 1 -19 -6 67.79 5.20 -1 -19 6 72.09 5.90 1 -19 -6 59.09 4.60 -1 19 6 66.09 4.00 1 19 -6 54.69 3.80 0 -19 -6 81.29 6.00 0 -19 6 99.29 5.50 0 19 6 91.29 5.30 0 19 6 89.19 5.10 0 19 -6 93.39 5.20 1 -19 6 3.70 1.40 -1 -19 -6 3.70 1.90 1 19 6 2.60 1.10 -1 19 -6 2.40 1.10 2 -20 -6 465.35 22.20 2 -20 -6 484.35 21.90 2 20 -6 448.46 21.90 -2 20 6 418.56 21.30 -2 20 6 445.66 21.40 1 -20 -6 36.50 3.70 -1 -20 6 35.80 2.90 1 -20 -6 32.00 2.90 -1 20 6 36.30 2.90 0 -20 -6 1050.89 51.19 0 -20 6 1163.98 50.79 0 -20 -6 1013.90 50.99 0 20 6 1150.48 50.69 0 20 -6 1140.19 50.59 2 -21 -6 1061.99 48.20 -2 -21 6 1047.00 47.10 2 -21 -6 955.90 47.30 -2 21 6 1033.70 47.00 1 -21 -6 96.79 6.90 -1 -21 6 96.39 5.10 1 -21 -6 80.79 5.20 -1 21 6 87.09 4.90 0 -21 -6 263.97 13.80 0 -21 -6 264.47 13.80 0 -21 6 282.47 13.50 0 21 -6 289.27 13.20 0 21 6 296.57 13.40 0 21 6 277.37 13.40 4 0 -7 0.30 1.20 4 0 -7 5.80 2.40 3 0 -7 1098.59 48.20 3 0 -7 937.91 49.50 2 0 -7 -1.10 2.10 -2 0 7 1.60 1.50 2 0 -7 0.30 1.50 -2 0 7 0.60 2.20 -1 0 7 1032.40 52.39 1 0 -7 1103.99 51.89 -1 0 7 1104.89 51.79 1 0 -7 1139.59 52.39 0 0 7 0.80 1.90 0 0 -7 -0.40 1.40 0 0 7 4.90 1.50 1 0 7 368.66 18.80 -1 0 -7 353.26 18.40 4 -1 -7 13.40 2.30 4 -1 -7 19.60 2.40 4 1 -7 19.20 2.20 3 -1 -7 375.86 19.50 3 -1 -7 356.86 19.80 3 1 -7 403.36 19.70 3 1 -7 425.16 22.00 2 -1 -7 247.38 12.70 2 -1 -7 226.48 13.10 -2 -1 7 228.88 11.50 -2 -1 7 228.68 12.40 -2 1 7 223.08 12.30 -2 1 7 228.88 11.50 2 1 -7 210.48 12.80 2 1 -7 226.38 12.50 1 -1 -7 680.13 32.40 1 -1 -7 641.04 31.60 -1 -1 7 615.44 32.30 -1 1 7 657.93 31.50 1 1 -7 691.53 32.10 1 1 -7 662.73 31.70 -1 1 7 580.94 32.00 0 -1 7 21.70 3.30 0 -1 -7 22.30 3.30 0 1 7 22.80 3.40 0 1 -7 21.10 3.20 0 1 7 22.10 3.00 1 -1 7 498.65 25.50 -1 -1 -7 510.85 25.30 1 1 7 529.45 25.50 -1 1 -7 505.55 25.20 2 -1 7 41.80 3.80 4 -2 -7 2.80 1.10 4 -2 -7 3.50 2.90 4 2 -7 0.40 1.20 3 -2 -7 1765.72 80.29 3 -2 -7 1706.73 80.69 2 -2 -7 86.29 6.20 2 -2 -7 92.79 7.10 -2 -2 7 89.29 5.50 2 2 -7 88.39 6.50 -2 2 7 88.29 5.50 2 2 -7 96.89 6.40 1 -2 -7 580.24 28.00 1 -2 -7 586.04 28.80 -1 -2 7 539.05 28.70 -1 2 7 555.44 27.80 -1 2 7 549.45 28.60 1 2 -7 548.75 27.90 1 2 -7 608.44 28.30 0 -2 -7 264.57 13.30 0 -2 7 280.47 14.90 0 -2 -7 272.47 14.90 0 2 7 284.27 14.80 0 2 7 278.77 13.80 0 2 -7 274.07 15.00 0 2 -7 261.87 14.70 1 -2 7 12.60 2.80 -1 2 -7 17.30 2.60 1 2 7 12.90 2.90 2 -2 7 21.60 3.10 2 2 7 15.80 3.10 4 -3 -7 15.80 2.50 4 -3 -7 14.20 2.40 4 3 -7 11.10 1.90 3 -3 -7 63.19 4.90 3 -3 -7 71.29 6.00 3 3 -7 65.79 5.10 2 -3 -7 240.28 13.60 2 -3 -7 223.78 12.50 -2 -3 7 228.18 11.60 2 3 -7 221.68 12.60 -2 3 7 237.48 11.70 1 -3 -7 2056.59 92.89 1 -3 -7 1979.20 91.99 1 3 -7 1928.91 91.79 -1 3 7 1965.30 91.69 1 3 -7 2189.98 92.29 -1 3 7 1796.92 92.39 0 -3 7 112.99 7.70 0 -3 -7 111.69 8.00 0 -3 7 121.29 6.70 0 -3 -7 111.49 6.20 0 3 -7 124.99 7.70 0 3 7 119.29 7.60 0 3 7 117.19 6.70 0 3 -7 107.09 7.70 1 -3 7 2627.14 127.19 -1 -3 -7 2811.82 125.99 1 3 7 2710.83 127.09 -1 3 -7 2895.51 126.99 1 3 7 2790.92 126.09 2 -3 7 5.60 3.00 2 3 7 0.50 2.00 4 -4 -7 -0.50 1.80 4 -4 -7 0.20 1.20 4 4 -7 -0.30 1.20 3 -4 -7 874.41 42.40 3 -4 -7 884.91 43.30 3 4 -7 944.31 42.80 2 -4 -7 163.68 9.60 2 -4 -7 171.08 10.80 -2 -4 7 162.88 8.80 2 4 -7 165.38 9.80 -2 4 7 171.58 8.90 1 -4 -7 420.46 21.10 -1 -4 7 412.36 19.10 1 -4 -7 375.26 19.70 -1 -4 7 375.96 20.80 -1 4 7 405.46 19.90 1 4 -7 374.06 19.80 1 4 -7 391.66 20.00 -1 4 7 353.06 20.50 -1 4 7 397.76 19.10 0 -4 -7 0.50 1.90 0 -4 7 2.30 1.90 0 4 7 -2.20 1.70 0 4 7 -0.40 1.10 0 4 -7 0.80 1.50 0 4 -7 -1.40 2.60 1 -4 7 25.00 3.40 -1 -4 -7 34.40 3.40 -1 4 -7 29.20 3.50 1 4 7 31.80 3.80 1 4 7 31.30 3.30 2 -4 7 -1.30 2.00 -2 -4 -7 1.30 1.30 2 4 7 1.60 1.50 2 4 7 1.40 1.90 4 -5 -7 1.10 1.30 4 -5 -7 -0.50 1.90 4 5 -7 0.40 1.20 3 -5 -7 279.47 15.30 3 5 -7 273.57 14.50 2 -5 -7 24.30 3.20 2 -5 -7 33.60 5.00 -2 -5 7 26.80 2.70 2 5 -7 30.10 3.50 -2 5 7 31.80 2.90 -1 -5 7 475.85 24.00 1 -5 -7 516.95 26.00 1 -5 -7 537.55 25.10 1 5 -7 475.45 24.90 -1 5 7 509.15 24.00 0 -5 -7 12.00 3.20 0 -5 7 12.40 2.50 0 -5 7 14.00 2.20 0 -5 -7 6.60 3.00 0 5 -7 12.00 3.80 0 5 7 10.50 1.80 0 5 -7 8.80 2.20 0 5 -7 12.30 1.80 0 5 7 10.00 2.70 1 -5 7 974.70 44.40 -1 -5 -7 922.11 43.40 1 5 7 964.00 43.10 -1 5 -7 858.61 43.70 2 -5 7 -0.80 2.40 -2 -5 -7 -1.50 1.10 2 -5 7 1.60 1.30 2 5 7 1.60 1.40 2 5 7 0.60 2.60 4 -6 -7 10.50 1.90 4 -6 -7 8.30 2.20 4 6 -7 3.20 2.90 4 6 -7 8.30 1.60 3 -6 -7 1036.60 48.60 -3 -6 7 1114.59 48.60 3 -6 -7 1026.80 49.80 -3 6 7 999.30 48.00 2 -6 -7 1.40 2.00 2 -6 -7 2.10 1.60 -2 -6 7 5.10 1.50 2 6 -7 2.40 1.40 -2 6 7 3.10 1.40 1 -6 -7 1234.68 57.89 -1 -6 7 1223.68 55.99 1 -6 -7 1134.19 56.69 1 6 -7 1250.27 56.99 -1 6 7 1213.08 55.99 0 -6 7 67.99 4.50 0 -6 -7 68.59 6.00 0 -6 -7 67.39 6.30 0 -6 7 62.49 5.10 0 6 7 51.49 5.70 0 6 -7 64.79 5.10 0 6 7 70.49 4.60 -1 -6 -7 2.60 1.80 1 -6 7 2.40 1.70 1 -6 7 0.90 1.30 1 6 7 3.30 1.90 1 6 7 3.10 1.30 -1 6 -7 3.20 1.80 -2 -6 -7 11.70 1.70 2 -6 7 15.50 2.60 2 6 7 13.70 2.30 2 6 7 10.00 2.30 4 -7 -7 85.29 5.00 4 -7 -7 93.49 6.30 4 7 -7 82.19 4.90 4 7 -7 96.79 5.70 -3 -7 7 103.89 6.60 3 -7 -7 131.69 8.30 3 -7 -7 118.29 6.70 3 -7 -7 99.29 6.40 -3 7 7 103.89 6.20 3 7 -7 121.59 7.30 2 -7 -7 163.68 10.60 2 -7 -7 162.98 9.30 -2 -7 7 159.18 8.50 2 7 -7 159.28 9.40 -2 7 7 164.58 8.60 -1 -7 7 1496.15 72.99 1 -7 -7 1525.95 73.79 1 7 -7 1694.23 74.09 -1 7 7 1643.04 72.99 0 -7 7 14.30 2.00 0 -7 -7 15.80 3.00 0 -7 7 21.90 3.30 0 -7 -7 14.50 3.10 0 7 7 17.30 2.20 0 7 -7 15.60 2.10 0 7 7 14.90 3.10 0 7 -7 9.40 2.20 1 -7 7 1038.80 46.60 1 7 7 1023.40 45.30 -1 7 -7 873.91 45.60 -2 -7 -7 57.99 3.90 2 -7 7 65.19 4.90 -2 7 -7 64.09 4.00 2 7 7 59.89 4.60 4 -8 -7 -0.30 1.90 4 -8 -7 2.00 1.30 4 8 -7 -2.10 1.40 4 8 -7 0.60 1.20 3 -8 -7 1651.63 75.89 -3 -8 7 1597.64 73.89 3 -8 -7 1632.74 74.09 3 -8 -7 1570.74 74.49 3 8 -7 1697.63 75.09 -3 8 7 1565.84 73.79 2 -8 -7 0.40 2.00 2 -8 -7 2.70 1.80 2 -8 -7 3.30 2.20 -2 -8 7 1.10 1.10 -2 8 7 5.10 1.60 2 8 -7 0.50 1.50 -1 -8 7 161.28 8.80 1 -8 -7 180.98 11.00 1 -8 -7 151.58 9.90 -1 8 7 164.58 8.70 1 8 -7 167.18 9.60 0 -8 7 1.40 1.30 0 -8 7 4.30 2.20 0 -8 -7 2.70 2.00 0 8 -7 2.70 1.60 0 8 7 1.90 1.20 1 -8 7 3.40 2.00 -1 8 -7 5.80 1.50 1 8 7 2.50 1.60 2 -8 7 31.20 3.10 4 -9 -7 17.20 2.10 4 -9 -7 16.30 2.40 4 9 -7 12.30 1.70 3 -9 -7 9.60 2.00 3 9 -7 10.90 3.00 3 9 -7 12.70 2.40 2 -9 -7 131.89 9.50 -2 -9 7 132.89 7.20 2 -9 -7 127.29 7.50 2 -9 -7 137.19 9.30 -2 9 7 141.69 7.60 2 9 -7 136.29 8.00 1 -9 -7 319.67 16.00 -1 -9 7 309.37 15.10 1 9 -7 297.97 15.70 -1 9 7 292.47 14.90 0 -9 -7 140.09 9.20 0 -9 7 136.49 8.40 0 -9 7 137.39 7.50 0 9 -7 126.99 7.90 0 9 7 137.89 7.50 1 -9 7 837.72 39.20 -1 9 -7 882.41 39.00 1 9 7 832.62 39.80 1 9 7 820.62 39.10 4 -10 -7 8.50 1.30 4 10 -7 12.20 1.70 4 10 -7 7.40 1.50 3 -10 -7 2003.60 90.29 -3 -10 7 1904.21 88.59 -3 10 7 1928.91 88.59 -2 -10 7 9.10 1.90 2 -10 -7 9.50 2.10 2 -10 -7 9.70 3.20 2 -10 -7 10.70 2.50 2 10 -7 10.10 2.10 1 -10 -7 900.51 45.60 -1 -10 7 999.40 45.20 1 -10 -7 858.21 44.90 -1 10 7 1058.49 45.20 1 10 -7 1053.39 46.00 0 -10 7 76.19 4.80 0 -10 7 73.69 5.70 0 -10 -7 76.69 6.50 0 10 -7 68.59 5.60 0 10 7 72.89 4.60 0 10 -7 76.59 4.20 1 -10 7 156.28 9.10 -1 -10 -7 141.89 9.20 -1 10 -7 156.38 7.90 1 10 7 155.08 8.00 3 -11 -7 19.10 2.90 3 -11 -7 27.90 3.60 -3 -11 7 25.40 2.60 -3 11 7 24.90 2.50 3 11 -7 24.60 3.10 3 11 -7 29.20 2.70 2 -11 -7 15.20 2.80 2 -11 -7 15.10 2.30 -2 11 7 18.30 2.10 2 11 -7 16.90 2.50 -1 -11 7 153.58 8.60 1 -11 -7 151.88 8.60 1 -11 -7 171.68 10.10 1 11 -7 172.78 9.40 -1 11 7 163.48 8.50 0 -11 7 125.59 7.80 0 -11 -7 126.79 8.40 0 -11 7 114.19 6.70 0 11 -7 117.19 6.90 0 11 -7 119.39 6.10 0 11 7 119.89 6.60 1 -11 7 1284.17 58.89 -1 -11 -7 1229.08 59.99 -1 11 -7 1268.27 58.69 1 11 7 1358.76 59.39 -3 -12 7 335.97 16.80 3 -12 -7 338.57 18.10 3 12 -7 381.56 17.50 -3 12 7 354.66 16.80 -2 -12 7 200.28 9.90 2 -12 -7 189.18 10.00 -2 12 7 192.08 9.80 -1 -12 7 298.37 14.50 1 -12 -7 295.07 14.60 -1 12 7 301.87 14.50 1 12 -7 282.77 14.80 0 -12 -7 131.19 9.90 0 -12 -7 100.99 6.50 0 12 -7 116.79 6.50 1 -12 7 20.10 2.60 1 -12 7 16.20 1.90 1 12 7 18.30 2.20 -3 -13 7 48.70 3.50 3 -13 -7 48.80 3.50 3 13 -7 56.29 3.70 2 -13 -7 28.70 4.20 -2 -13 7 32.30 2.60 2 -13 -7 27.10 2.80 2 13 -7 26.40 2.70 -1 13 7 1581.14 72.59 1 13 -7 1660.43 72.99 -1 13 7 1511.85 72.59 0 -13 -7 22.80 3.00 0 -13 -7 27.50 3.30 0 -13 7 26.60 2.90 0 -13 7 26.50 2.50 0 13 7 27.30 2.20 0 13 -7 25.40 2.50 0 13 7 24.60 2.50 -1 -13 -7 2143.69 94.29 1 -13 7 2061.69 93.29 -1 13 -7 2041.60 93.09 1 13 7 1956.10 93.19 3 -14 -7 1683.13 69.49 -3 -14 7 1481.95 68.69 3 -14 -7 1382.16 69.59 -3 14 7 1477.25 68.59 2 -14 -7 47.60 4.70 2 -14 -7 47.30 4.40 -2 14 7 52.19 3.40 2 14 -7 47.70 3.50 1 -14 -7 1170.98 51.89 -1 -14 7 1137.49 50.99 1 -14 -7 1097.39 52.19 -1 14 7 1074.79 50.59 -1 14 7 1124.69 50.89 1 14 -7 1034.00 50.99 0 -14 7 19.70 2.60 0 -14 7 20.60 3.30 0 -14 -7 23.50 2.80 0 -14 -7 22.00 2.90 0 14 -7 16.30 2.50 2 -15 -7 44.20 3.60 2 -15 -7 45.00 4.40 -2 -15 7 48.60 3.30 2 15 -7 55.99 3.70 -2 15 7 48.70 3.30 1 -15 -7 566.24 28.30 1 -15 -7 575.04 28.80 -1 15 7 632.54 27.50 0 -15 -7 63.19 4.90 0 -15 7 65.49 4.50 0 -15 -7 59.99 3.90 0 -15 7 67.69 4.00 0 15 7 64.19 3.90 0 15 7 56.99 3.60 2 -16 -7 9.10 2.00 -2 -16 7 14.40 1.90 2 -16 -7 10.30 1.80 2 16 -7 15.70 2.30 -2 16 7 15.40 1.90 -1 -16 7 297.37 14.00 1 -16 -7 284.37 14.90 -1 16 7 298.47 14.00 1 16 -7 293.37 14.40 -1 16 7 268.17 13.70 0 -16 7 10.90 1.50 0 -16 -7 8.20 1.60 0 -16 7 9.70 1.80 0 -16 -7 6.10 2.00 0 16 7 14.20 1.80 0 16 7 7.40 1.50 1 -17 -7 207.78 10.60 1 -17 -7 188.08 11.10 -1 -17 7 219.58 10.40 -1 17 7 221.68 10.40 3 0 -8 0.00 0.70 2 0 -8 4.00 1.30 2 0 -8 0.80 2.00 1 0 -8 1.00 1.90 1 0 -8 -0.10 2.50 0 0 -8 626.74 31.10 0 0 -8 692.03 32.00 3 -1 -8 46.60 3.30 3 1 -8 36.50 3.40 2 -1 -8 1535.55 74.59 2 1 -8 1594.24 74.59 -2 1 8 1731.53 73.99 1 -1 -8 13.10 2.30 1 -1 -8 11.50 2.10 1 1 -8 11.90 2.30 1 1 -8 14.60 2.50 0 -1 -8 360.16 17.00 0 -1 8 350.56 17.10 0 -1 -8 336.17 17.70 0 1 8 321.87 17.00 0 1 -8 324.47 16.60 0 1 -8 361.06 17.00 3 -2 -8 13.00 2.10 3 2 -8 10.10 2.00 -2 -2 8 356.66 17.50 2 -2 -8 386.46 18.20 2 -2 -8 344.57 18.40 -2 2 8 367.06 17.50 2 2 -8 385.66 18.20 1 -2 -8 2.50 1.90 1 -2 -8 4.30 1.80 -1 -2 8 4.60 2.70 -1 2 8 4.60 1.30 1 2 -8 4.10 1.40 0 -2 8 1440.76 62.59 0 -2 -8 1415.26 62.59 0 2 -8 1323.27 62.29 0 2 -8 1228.58 61.89 3 -3 -8 233.88 11.70 2 -3 -8 314.47 15.80 2 -3 -8 313.67 15.70 -2 -3 8 314.17 15.00 -2 3 8 327.47 15.10 2 3 -8 297.47 15.60 1 -3 -8 3.50 2.30 -1 -3 8 2.70 2.10 1 -3 -8 1.20 2.70 1 3 -8 1.10 1.60 -1 3 8 2.40 1.20 0 -3 -8 81.39 5.50 0 -3 8 77.19 5.20 0 3 -8 72.49 4.90 0 3 8 90.19 4.70 2 -4 -8 15.00 2.30 -2 -4 8 18.80 1.90 2 -4 -8 11.00 2.60 2 4 -8 17.90 2.40 -2 4 8 10.30 1.70 -1 -4 8 42.70 3.10 1 -4 -8 39.70 4.20 -1 -4 8 46.50 3.90 1 -4 -8 44.90 4.30 1 4 -8 45.70 3.50 -1 4 8 42.10 3.10 0 -4 -8 543.15 27.50 0 -4 8 569.24 27.40 0 4 8 581.04 26.70 0 4 -8 599.04 27.50 -2 -5 8 1005.90 47.20 2 -5 -8 1017.70 48.00 2 -5 -8 1140.79 49.70 2 5 -8 1036.20 47.90 -2 5 8 950.40 47.10 -1 -5 8 2.00 1.30 1 -5 -8 2.30 1.80 -1 -5 8 3.50 1.10 1 -5 -8 2.90 1.60 1 5 -8 4.40 1.30 -1 5 8 4.70 1.20 0 -5 8 5.30 2.00 0 -5 8 6.40 1.30 0 -5 -8 6.10 2.40 0 5 8 5.00 1.30 0 5 -8 3.30 1.10 -2 -6 8 284.67 14.40 2 -6 -8 292.07 14.70 2 6 -8 317.17 15.10 -2 6 8 312.17 14.40 1 -6 -8 4.80 2.20 -1 -6 8 8.70 1.40 -1 -6 8 9.90 2.10 -1 6 8 9.30 1.40 1 6 -8 9.00 1.50 0 -6 -8 730.93 34.60 2 -7 -8 377.66 18.70 1 -7 -8 2.30 1.50 -1 -7 8 2.60 1.80 -1 -7 8 1.80 1.10 -1 7 8 3.30 1.10 1 7 -8 3.10 2.10 -1 -8 8 115.59 7.10 1 -8 -8 132.69 8.00 -1 -8 8 129.79 6.70 1 8 -8 123.79 7.00 -1 8 8 139.09 6.70 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 49762 #============================================================================= # end of cif data for "gil10302" (compound 5k) #============================================================================= #============================================================================= # cif data for "gil10361" (compound 3s) #============================================================================= data_gil10361_3s _audit_creation_method 'APEX4 v2021.4-0' _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H19 Br F2 O4' _chemical_formula_iupac ? _chemical_formula_weight 453.27 _chemical_absolute_configuration ad _chemical_melting_point ? _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_H-M_alt 'P 1 21 1' _space_group_name_Hall 'P 2yb' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.0921(2) _cell_length_b 5.85270(10) _cell_length_c 18.4384(4) _cell_angle_alpha 90 _cell_angle_beta 93.7950(10) _cell_angle_gamma 90 _cell_volume 979.02(3) _cell_formula_units_Z 2 _cell_measurement_reflns_used 9918 _cell_measurement_theta_min 4.8073 _cell_measurement_theta_max 68.4924 _cell_measurement_temperature 100.(2) _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.436 _exptl_crystal_size_mid 0.049 _exptl_crystal_size_min 0.038 _exptl_crystal_density_diffrn 1.538 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 460 _exptl_absorpt_coefficient_mu 3.251 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_process_details ; Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015). "Comparison of silver and molybdenum microfocus X-ray sources for single-crystal structure determination" J. Appl. Cryst. 48, 3-10. doi:10.1107/S1600576714022985 ; _exptl_absorpt_correction_T_min 0.69 _exptl_absorpt_correction_T_max 0.89 _exptl_special_details ; ; _diffrn_ambient_temperature 100.(2) _diffrn_source 'Cu ImS' _diffrn_source_type 'micro focus tube' _diffrn_source_power 0.05 _diffrn_source_current 1.0 _diffrn_source_voltage 50 _diffrn_radiation_probe 'single crystal' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_monochromator 'MX mirror' _diffrn_measurement_device 'Bruker D8 Venture Photon III' _diffrn_measurement_device_type 'single crystal diffractometer' _diffrn_measurement_method 'phi/omega scans' _diffrn_detector_area_resol_mean 7.3910 _diffrn_reflns_number 16410 _diffrn_reflns_av_R_equivalents 0.0474 _diffrn_reflns_av_unetI/netI 0.0372 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 66.58 _diffrn_reflns_theta_full 66.58 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _refine_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_number_total 3403 _reflns_number_gt 3240 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.794 _reflns_Friedel_fraction_max 0.981 _reflns_Friedel_fraction_full 0.981 _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0280 _refine_ls_R_factor_gt 0.0252 _refine_ls_wR_factor_gt 0.0545 _refine_ls_wR_factor_ref 0.0561 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_number_reflns 3403 _refine_ls_number_parameters 254 _refine_ls_number_restraints 1 _refine_ls_number_constraints ? _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0085P)^2^+0.4593P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary ? _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.202 _refine_diff_density_min -0.264 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ; Flack x determined using 1363 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.035(9) 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' Br Br -0.6763 1.2805 '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' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection 'Bruker APEX4 v2021.4-0 Photon III' _computing_cell_refinement 'SAINT V8.40B (Bruker AXS LLC, 2019)' _computing_data_reduction 'SAINT V8.40B (Bruker AXS LLC, 2019)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_molecular_graphics 'shelXle (C.B. Huebschle, rev 1242)' _computing_publication_material 'SHELXT 2018/2 (Sheldrick, 2018)' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_flags_posn _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Br Br1 0.32479(4) 0.05619(7) 0.56918(2) 0.03714(13) Uani d . . . 1 . . F F1 -0.18757(19) 0.1147(3) 0.28449(10) 0.0239(5) Uani d . . . 1 . . F F2 -0.0704(2) 0.4349(3) 0.26681(10) 0.0218(4) Uani d . . . 1 . . O O1 0.1517(2) 0.5921(4) 0.18029(12) 0.0216(5) Uani d . . . 1 . . O O2 0.3637(2) 0.3944(4) 0.19498(12) 0.0169(5) Uani d . . . 1 . . O O3 0.3739(3) 0.6287(4) 0.32370(13) 0.0277(6) Uani d . . . 1 . . O O4 0.4682(3) 0.9357(4) 0.27031(13) 0.0228(5) Uani d . . . 1 . . C C1 0.2009(4) 0.1106(5) 0.48340(18) 0.0218(8) Uani d . . . 1 . . C C2 0.1058(4) -0.0598(6) 0.45828(19) 0.0225(7) Uani d . . . 1 . . H H2 0.097913 -0.198240 0.484645 0.027000 Uiso calc U . R 1 . . C C3 0.0217(4) -0.0243(6) 0.39349(19) 0.0202(7) Uani d . . . 1 . . H H3 -0.043355 -0.140378 0.374800 0.024000 Uiso calc U . R 1 . . C C4 0.0324(3) 0.1805(6) 0.35595(19) 0.0174(7) Uani d . . . 1 . . C C5 0.1269(4) 0.3510(6) 0.38340(18) 0.0191(7) Uani d . . . 1 . . H H5 0.133319 0.491618 0.358044 0.023000 Uiso calc U . R 1 . . C C6 0.2118(4) 0.3163(6) 0.44769(19) 0.0216(7) Uani d . . . 1 . . H H6 0.276386 0.432286 0.466833 0.026000 Uiso calc U . R 1 . . C C7 -0.0481(3) 0.2085(6) 0.28249(19) 0.0188(7) Uani d . . . 1 . . C C8 0.0243(3) 0.0865(6) 0.22228(15) 0.0174(7) Uani d . . . 1 . . H H8 0.030153 -0.082492 0.229988 0.021000 Uiso calc U . R 1 . . C C9 -0.0028(3) 0.1496(6) 0.14398(18) 0.0200(7) Uani d . . . 1 . . H H9A -0.060761 0.289594 0.132390 0.024000 Uiso calc U . R 1 . . H H9B -0.018713 0.023940 0.108378 0.024000 Uiso calc U . R 1 . . C C10 0.1512(3) 0.1785(6) 0.18028(17) 0.0156(7) Uani d . . . 1 . . H H10 0.222817 0.058798 0.166585 0.019000 Uiso calc U . R 1 . . C C11 0.2146(3) 0.4117(6) 0.18600(16) 0.0146(7) Uani d . . . 1 . . C C12 0.4449(3) 0.6049(5) 0.20013(17) 0.0160(7) Uani d . . . 1 . . H H12 0.413562 0.707816 0.158660 0.019000 Uiso calc U . R 1 . . C C13 0.4215(3) 0.7216(6) 0.27208(18) 0.0166(7) Uani d . . . 1 . . C C14 0.4633(4) 1.0623(8) 0.33759(16) 0.0264(7) Uani d . . . 1 . . H H14A 0.377532 1.013456 0.363155 0.040000 Uiso calc U . R 1 . . H H14B 0.455510 1.226027 0.326863 0.040000 Uiso calc U . R 1 . . H H14C 0.553471 1.033122 0.368278 0.040000 Uiso calc U . R 1 . . C C15 0.6085(3) 0.5420(7) 0.19751(15) 0.0178(6) Uani d . . . 1 . . H H15A 0.669209 0.674281 0.214612 0.021000 Uiso calc U . R 1 . . H H15B 0.631170 0.413675 0.231414 0.021000 Uiso calc U . R 1 . . C C16 0.6515(3) 0.4744(5) 0.12248(18) 0.0169(7) Uani d . . . 1 . . C C17 0.6106(4) 0.2647(6) 0.09175(19) 0.0196(7) Uani d . . . 1 . . H H17 0.553098 0.161155 0.117694 0.024000 Uiso calc U . R 1 . . C C18 0.6537(4) 0.2063(6) 0.02311(19) 0.0237(8) Uani d . . . 1 . . H H18 0.624131 0.063998 0.002090 0.028000 Uiso calc U . R 1 . . C C19 0.7389(4) 0.3538(6) -0.01451(18) 0.0244(8) Uani d . . . 1 . . H H19 0.769833 0.311774 -0.060874 0.029000 Uiso calc U . R 1 . . C C20 0.7793(3) 0.5631(8) 0.01535(16) 0.0256(7) Uani d . . . 1 . . H H20 0.836957 0.665935 -0.010752 0.031000 Uiso calc U . R 1 . . C C21 0.7352(4) 0.6230(5) 0.08379(18) 0.0210(7) Uani d . . . 1 . . H H21 0.762802 0.767225 0.104060 0.025000 Uiso calc U . R 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Br1 0.0453(2) 0.0344(2) 0.02954(19) 0.0084(2) -0.01437(14) -0.0010(2) F1 0.0126(8) 0.0308(13) 0.0285(10) -0.0009(8) 0.0035(7) 0.0026(8) F2 0.0231(10) 0.0178(10) 0.0251(10) 0.0068(8) 0.0054(8) 0.0033(8) O1 0.0147(10) 0.0163(14) 0.0340(12) 0.0034(10) 0.0019(9) -0.0002(11) O2 0.0112(11) 0.0123(11) 0.0268(12) -0.0013(9) -0.0008(9) 0.0001(10) O3 0.0358(14) 0.0249(14) 0.0229(12) -0.0126(10) 0.0064(10) -0.0005(10) O4 0.0300(13) 0.0137(12) 0.0257(13) -0.0031(10) 0.0088(10) -0.0009(10) C1 0.0226(17) 0.021(2) 0.0219(16) 0.0064(14) 0.0010(13) -0.0045(13) C2 0.0237(18) 0.0182(17) 0.0260(19) 0.0017(15) 0.0047(14) 0.0027(15) C3 0.0220(17) 0.0150(16) 0.0237(18) -0.0023(13) 0.0024(14) 0.0009(13) C4 0.0141(16) 0.0179(17) 0.0209(17) 0.0038(13) 0.0059(13) -0.0005(14) C5 0.0196(17) 0.0137(17) 0.0246(18) 0.0007(13) 0.0061(13) 0.0031(13) C6 0.0183(17) 0.0197(18) 0.0268(18) -0.0022(14) 0.0019(14) -0.0058(15) C7 0.0139(16) 0.0145(16) 0.0283(18) 0.0019(13) 0.0051(13) 0.0037(14) C8 0.0135(14) 0.0177(18) 0.0209(14) -0.0016(14) 0.0020(11) 0.0007(15) C9 0.0144(15) 0.0264(17) 0.0192(16) -0.0043(13) 0.0005(12) -0.0025(14) C10 0.0133(15) 0.0159(16) 0.0179(16) 0.0000(12) 0.0022(12) -0.0037(13) C11 0.0118(15) 0.0202(18) 0.0120(15) -0.0002(13) 0.0028(12) -0.0005(13) C12 0.0141(14) 0.0128(19) 0.0211(15) -0.0024(12) 0.0014(11) 0.0008(13) C13 0.0105(15) 0.0160(16) 0.0230(18) 0.0000(13) -0.0011(13) 0.0005(14) C14 0.0372(18) 0.0162(15) 0.0265(16) -0.001(2) 0.0072(13) -0.005(2) C15 0.0132(14) 0.0197(16) 0.0203(14) -0.0032(16) 0.0000(11) -0.0004(18) C16 0.0092(14) 0.0184(16) 0.0227(16) 0.0025(12) -0.0022(12) 0.0001(13) C17 0.0177(17) 0.0163(17) 0.0247(18) -0.0005(13) 0.0002(14) 0.0026(14) C18 0.0216(18) 0.0216(18) 0.0272(19) 0.0017(14) -0.0045(14) -0.0036(15) C19 0.0271(19) 0.028(2) 0.0178(17) 0.0048(15) -0.0015(14) -0.0007(15) C20 0.0286(17) 0.0235(17) 0.0252(15) -0.001(2) 0.0060(12) 0.005(2) C21 0.0180(16) 0.0171(18) 0.0278(17) -0.0017(12) 0.0003(13) 0.0002(13) _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_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Br1 C1 . 1.907(3) ? F1 C7 . 1.385(4) ? F2 C7 . 1.368(4) ? O1 C11 . 1.202(4) ? O2 C11 . 1.359(4) ? O2 C12 . 1.436(4) ? O3 C13 . 1.201(4) ? O4 C13 . 1.324(4) ? O4 C14 . 1.448(4) ? C1 C6 . 1.379(5) ? C1 C2 . 1.380(5) ? C2 C3 . 1.391(5) ? C2 H2 . 0.950000 ? C3 C4 . 1.391(4) ? C3 H3 . 0.950000 ? C4 C5 . 1.390(5) ? C4 C7 . 1.505(5) ? C5 C6 . 1.386(5) ? C5 H5 . 0.950000 ? C6 H6 . 0.950000 ? C7 C8 . 1.507(4) ? C8 C9 . 1.495(4) ? C8 C10 . 1.530(4) ? C8 H8 . 1.000000 ? C9 C10 . 1.521(5) ? C9 H9A . 0.990000 ? C9 H9B . 0.990000 ? C10 C11 . 1.482(5) ? C10 H10 . 1.000000 ? C12 C13 . 1.520(5) ? C12 C15 . 1.537(4) ? C12 H12 . 1.000000 ? C14 H14A . 0.980000 ? C14 H14B . 0.980000 ? C14 H14C . 0.980000 ? C15 C16 . 1.515(4) ? C15 H15A . 0.990000 ? C15 H15B . 0.990000 ? C16 C21 . 1.384(4) ? C16 C17 . 1.392(5) ? C17 C18 . 1.392(5) ? C17 H17 . 0.950000 ? C18 C19 . 1.377(5) ? C18 H18 . 0.950000 ? C19 C20 . 1.383(6) ? C19 H19 . 0.950000 ? C20 C21 . 1.394(5) ? C20 H20 . 0.950000 ? C21 H21 . 0.950000 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C11 O2 C12 . . 116.6(2) ? C13 O4 C14 . . 115.8(3) ? C6 C1 C2 . . 122.3(3) ? C6 C1 Br1 . . 119.0(3) ? C2 C1 Br1 . . 118.7(3) ? C1 C2 C3 . . 118.5(3) ? C1 C2 H2 . . 120.700000 ? C3 C2 H2 . . 120.700000 ? C2 C3 C4 . . 120.2(3) ? C2 C3 H3 . . 119.900000 ? C4 C3 H3 . . 119.900000 ? C5 C4 C3 . . 120.0(3) ? C5 C4 C7 . . 120.1(3) ? C3 C4 C7 . . 119.7(3) ? C6 C5 C4 . . 120.1(3) ? C6 C5 H5 . . 119.900000 ? C4 C5 H5 . . 119.900000 ? C1 C6 C5 . . 118.9(3) ? C1 C6 H6 . . 120.600000 ? C5 C6 H6 . . 120.600000 ? F2 C7 F1 . . 105.4(2) ? F2 C7 C4 . . 110.6(3) ? F1 C7 C4 . . 108.9(3) ? F2 C7 C8 . . 111.7(3) ? F1 C7 C8 . . 106.1(3) ? C4 C7 C8 . . 113.7(3) ? C9 C8 C7 . . 122.8(3) ? C9 C8 C10 . . 60.4(2) ? C7 C8 C10 . . 125.9(3) ? C9 C8 H8 . . 112.700000 ? C7 C8 H8 . . 112.700000 ? C10 C8 H8 . . 112.700000 ? C8 C9 C10 . . 60.9(2) ? C8 C9 H9A . . 117.700000 ? C10 C9 H9A . . 117.700000 ? C8 C9 H9B . . 117.700000 ? C10 C9 H9B . . 117.700000 ? H9A C9 H9B . . 114.800000 ? C11 C10 C9 . . 118.4(3) ? C11 C10 C8 . . 126.2(3) ? C9 C10 C8 . . 58.7(2) ? C11 C10 H10 . . 114.000000 ? C9 C10 H10 . . 114.000000 ? C8 C10 H10 . . 114.000000 ? O1 C11 O2 . . 122.8(3) ? O1 C11 C10 . . 128.5(3) ? O2 C11 C10 . . 108.7(3) ? O2 C12 C13 . . 110.0(2) ? O2 C12 C15 . . 106.7(3) ? C13 C12 C15 . . 109.1(2) ? O2 C12 H12 . . 110.300000 ? C13 C12 H12 . . 110.300000 ? C15 C12 H12 . . 110.300000 ? O3 C13 O4 . . 125.5(3) ? O3 C13 C12 . . 124.5(3) ? O4 C13 C12 . . 109.9(3) ? O4 C14 H14A . . 109.500000 ? O4 C14 H14B . . 109.500000 ? H14A C14 H14B . . 109.500000 ? O4 C14 H14C . . 109.500000 ? H14A C14 H14C . . 109.500000 ? H14B C14 H14C . . 109.500000 ? C16 C15 C12 . . 113.6(2) ? C16 C15 H15A . . 108.800000 ? C12 C15 H15A . . 108.800000 ? C16 C15 H15B . . 108.800000 ? C12 C15 H15B . . 108.800000 ? H15A C15 H15B . . 107.700000 ? C21 C16 C17 . . 119.0(3) ? C21 C16 C15 . . 119.4(3) ? C17 C16 C15 . . 121.6(3) ? C18 C17 C16 . . 120.2(3) ? C18 C17 H17 . . 119.900000 ? C16 C17 H17 . . 119.900000 ? C19 C18 C17 . . 120.4(3) ? C19 C18 H18 . . 119.800000 ? C17 C18 H18 . . 119.800000 ? C18 C19 C20 . . 119.9(3) ? C18 C19 H19 . . 120.100000 ? C20 C19 H19 . . 120.100000 ? C19 C20 C21 . . 119.9(3) ? C19 C20 H20 . . 120.000000 ? C21 C20 H20 . . 120.000000 ? C16 C21 C20 . . 120.6(3) ? C16 C21 H21 . . 119.700000 ? C20 C21 H21 . . 119.700000 ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C6 C1 C2 C3 . . . . 2.0(5) ? Br1 C1 C2 C3 . . . . -176.4(3) ? C1 C2 C3 C4 . . . . -1.0(5) ? C2 C3 C4 C5 . . . . -0.3(5) ? C2 C3 C4 C7 . . . . 174.2(3) ? C3 C4 C5 C6 . . . . 0.8(5) ? C7 C4 C5 C6 . . . . -173.8(3) ? C2 C1 C6 C5 . . . . -1.6(5) ? Br1 C1 C6 C5 . . . . 176.8(2) ? C4 C5 C6 C1 . . . . 0.2(5) ? C5 C4 C7 F2 . . . . -28.0(4) ? C3 C4 C7 F2 . . . . 157.5(3) ? C5 C4 C7 F1 . . . . -143.4(3) ? C3 C4 C7 F1 . . . . 42.0(4) ? C5 C4 C7 C8 . . . . 98.5(4) ? C3 C4 C7 C8 . . . . -76.0(4) ? F2 C7 C8 C9 . . . . -32.9(4) ? F1 C7 C8 C9 . . . . 81.5(4) ? C4 C7 C8 C9 . . . . -158.8(3) ? F2 C7 C8 C10 . . . . 42.1(4) ? F1 C7 C8 C10 . . . . 156.5(3) ? C4 C7 C8 C10 . . . . -83.8(4) ? C7 C8 C9 C10 . . . . 115.9(4) ? C8 C9 C10 C11 . . . . -117.2(3) ? C9 C8 C10 C11 . . . . 104.2(4) ? C7 C8 C10 C11 . . . . -6.8(5) ? C7 C8 C10 C9 . . . . -111.0(4) ? C12 O2 C11 O1 . . . . 2.2(4) ? C12 O2 C11 C10 . . . . 178.8(2) ? C9 C10 C11 O1 . . . . 17.8(5) ? C8 C10 C11 O1 . . . . -52.5(5) ? C9 C10 C11 O2 . . . . -158.5(3) ? C8 C10 C11 O2 . . . . 131.2(3) ? C11 O2 C12 C13 . . . . 70.8(3) ? C11 O2 C12 C15 . . . . -171.1(2) ? C14 O4 C13 O3 . . . . 1.5(5) ? C14 O4 C13 C12 . . . . -175.3(3) ? O2 C12 C13 O3 . . . . 17.0(4) ? C15 C12 C13 O3 . . . . -99.7(4) ? O2 C12 C13 O4 . . . . -166.2(2) ? C15 C12 C13 O4 . . . . 77.1(3) ? O2 C12 C15 C16 . . . . 74.4(4) ? C13 C12 C15 C16 . . . . -166.8(3) ? C12 C15 C16 C21 . . . . 107.2(4) ? C12 C15 C16 C17 . . . . -73.7(4) ? C21 C16 C17 C18 . . . . 0.1(5) ? C15 C16 C17 C18 . . . . -179.1(3) ? C16 C17 C18 C19 . . . . 1.0(5) ? C17 C18 C19 C20 . . . . -1.4(5) ? C18 C19 C20 C21 . . . . 0.8(5) ? C17 C16 C21 C20 . . . . -0.7(5) ? C15 C16 C21 C20 . . . . 178.5(3) ? C19 C20 C21 C16 . . . . 0.2(5) ? _shelx_res_file ; TITL gil10361.res in P2(1) gil10361.res created by SHELXL-2018/3 at 08:55:44 on 29-Jun-2022 CELL 1.54178 9.0921 5.8527 18.4384 90.000 93.795 90.000 ZERR 2.000 0.0002 0.0001 0.0004 0.000 0.001 0.000 LATT -1 SYMM -X, 1/2+Y, -Z SFAC C H Br F O UNIT 42 38 2 4 8 LIST 4 REM Old TITL gil10361 in P2(1) REM SHELXT solution in P2(1): R1 0.103, Rweak 0.028, Alpha 0.003 REM 0.276 for 3 systematic absences, Orientation as input REM Flack x= 0.068 ( 0.009 ) from 1377 Parsons' quotients REM Formula found by SHELXT: C21 Br F3 O3 SIZE 0.038 0.049 0.436 TEMP -173.150 ACTA CONF L.S. 40 BOND $H FMAP 2 PLAN 10 HTAB WGHT 0.008500 0.459300 FVAR 0.98912 BR1 3 0.324793 0.056194 0.569176 11.00000 0.04530 0.03435 = 0.02954 -0.00101 -0.01437 0.00835 F1 4 -0.187574 0.114695 0.284491 11.00000 0.01257 0.03084 = 0.02855 0.00264 0.00349 -0.00089 F2 4 -0.070392 0.434881 0.266809 11.00000 0.02306 0.01780 = 0.02507 0.00326 0.00537 0.00679 O1 5 0.151708 0.592079 0.180286 11.00000 0.01465 0.01630 = 0.03401 -0.00015 0.00185 0.00342 O2 5 0.363741 0.394354 0.194983 11.00000 0.01121 0.01230 = 0.02679 0.00010 -0.00081 -0.00127 O3 5 0.373932 0.628714 0.323698 11.00000 0.03583 0.02489 = 0.02293 -0.00053 0.00644 -0.01258 O4 5 0.468188 0.935696 0.270314 11.00000 0.03004 0.01369 = 0.02572 -0.00094 0.00879 -0.00307 C1 1 0.200876 0.110561 0.483400 11.00000 0.02264 0.02084 = 0.02190 -0.00450 0.00095 0.00645 C2 1 0.105770 -0.059808 0.458277 11.00000 0.02366 0.01821 = 0.02604 0.00272 0.00466 0.00172 AFIX 43 H2 2 0.097913 -0.198240 0.484645 11.00000 -1.20000 AFIX 0 C3 1 0.021664 -0.024334 0.393487 11.00000 0.02197 0.01504 = 0.02371 0.00087 0.00239 -0.00230 AFIX 43 H3 2 -0.043355 -0.140378 0.374800 11.00000 -1.20000 AFIX 0 C4 1 0.032441 0.180542 0.355952 11.00000 0.01408 0.01786 = 0.02087 -0.00047 0.00589 0.00377 C5 1 0.126918 0.351041 0.383400 11.00000 0.01959 0.01365 = 0.02461 0.00307 0.00607 0.00069 AFIX 43 H5 2 0.133319 0.491618 0.358044 11.00000 -1.20000 AFIX 0 C6 1 0.211797 0.316340 0.447690 11.00000 0.01826 0.01966 = 0.02683 -0.00580 0.00188 -0.00222 AFIX 43 H6 2 0.276386 0.432286 0.466833 11.00000 -1.20000 AFIX 0 C7 1 -0.048071 0.208505 0.282486 11.00000 0.01394 0.01447 = 0.02833 0.00366 0.00510 0.00193 C8 1 0.024316 0.086477 0.222278 11.00000 0.01352 0.01775 = 0.02090 0.00068 0.00201 -0.00158 AFIX 13 H8 2 0.030153 -0.082492 0.229988 11.00000 -1.20000 AFIX 0 C9 1 -0.002786 0.149584 0.143982 11.00000 0.01439 0.02641 = 0.01917 -0.00251 0.00046 -0.00426 AFIX 23 H9A 2 -0.060761 0.289594 0.132390 11.00000 -1.20000 H9B 2 -0.018713 0.023940 0.108378 11.00000 -1.20000 AFIX 0 C10 1 0.151228 0.178500 0.180280 11.00000 0.01327 0.01589 = 0.01789 -0.00365 0.00224 0.00002 AFIX 13 H10 2 0.222817 0.058798 0.166585 11.00000 -1.20000 AFIX 0 C11 1 0.214578 0.411686 0.185998 11.00000 0.01184 0.02019 = 0.01199 -0.00054 0.00276 -0.00020 C12 1 0.444869 0.604870 0.200133 11.00000 0.01410 0.01284 = 0.02110 0.00076 0.00139 -0.00241 AFIX 13 H12 2 0.413562 0.707816 0.158660 11.00000 -1.20000 AFIX 0 C13 1 0.421471 0.721622 0.272085 11.00000 0.01053 0.01596 = 0.02300 0.00047 -0.00109 0.00000 C14 1 0.463278 1.062308 0.337590 11.00000 0.03725 0.01619 = 0.02650 -0.00514 0.00721 -0.00058 AFIX 137 H14A 2 0.377532 1.013456 0.363155 11.00000 -1.50000 H14B 2 0.455510 1.226027 0.326863 11.00000 -1.50000 H14C 2 0.553471 1.033122 0.368278 11.00000 -1.50000 AFIX 0 C15 1 0.608538 0.541997 0.197512 11.00000 0.01321 0.01970 = 0.02031 -0.00038 -0.00004 -0.00321 AFIX 23 H15A 2 0.669209 0.674281 0.214612 11.00000 -1.20000 H15B 2 0.631170 0.413675 0.231414 11.00000 -1.20000 AFIX 0 C16 1 0.651547 0.474390 0.122485 11.00000 0.00921 0.01842 = 0.02269 0.00015 -0.00218 0.00254 C17 1 0.610596 0.264698 0.091749 11.00000 0.01768 0.01625 = 0.02475 0.00261 0.00016 -0.00046 AFIX 43 H17 2 0.553098 0.161155 0.117694 11.00000 -1.20000 AFIX 0 C18 1 0.653666 0.206332 0.023110 11.00000 0.02156 0.02156 = 0.02725 -0.00362 -0.00453 0.00165 AFIX 43 H18 2 0.624131 0.063998 0.002090 11.00000 -1.20000 AFIX 0 C19 1 0.738872 0.353798 -0.014507 11.00000 0.02715 0.02797 = 0.01778 -0.00067 -0.00148 0.00482 AFIX 43 H19 2 0.769833 0.311774 -0.060874 11.00000 -1.20000 AFIX 0 C20 1 0.779251 0.563100 0.015347 11.00000 0.02860 0.02346 = 0.02523 0.00547 0.00600 -0.00135 AFIX 43 H20 2 0.836957 0.665935 -0.010752 11.00000 -1.20000 AFIX 0 C21 1 0.735183 0.623037 0.083788 11.00000 0.01800 0.01709 = 0.02784 0.00016 0.00026 -0.00172 AFIX 43 H21 2 0.762802 0.767225 0.104060 11.00000 -1.20000 AFIX 0 HKLF 4 REM gil10361.res in P2(1) REM wR2 = 0.056116, GooF = S = 1.06700, Restrained GooF = 1.06683 for all data REM R1 = 0.025232 for 3240 Fo > 4sig(Fo) and 0.028022 for all 3403 data REM 254 parameters refined using 1 restraints END WGHT 0.0085 0.4593 REM Instructions for potential hydrogen bonds EQIV $1 x, y-1, z HTAB C8 O1_$1 EQIV $2 x, y+1, z HTAB C14 O3_$2 EQIV $3 x+1, y, z HTAB C15 F1_$3 REM Highest difference peak 0.202, deepest hole -0.264, 1-sigma level 0.047 Q1 1 0.4173 0.2409 0.5758 11.00000 0.05 0.20 Q2 1 0.2482 0.0536 0.5211 11.00000 0.05 0.20 Q3 1 -0.0138 0.2156 0.3229 11.00000 0.05 0.19 Q4 1 0.4796 0.9808 0.3792 11.00000 0.05 0.19 Q5 1 -0.0208 0.0965 0.1824 11.00000 0.05 0.19 Q6 1 0.1003 0.1433 0.2141 11.00000 0.05 0.18 Q7 1 0.3801 -0.1155 0.6114 11.00000 0.05 0.18 Q8 1 0.2328 -0.1146 0.5638 11.00000 0.05 0.18 Q9 1 0.0089 0.1337 0.3870 11.00000 0.05 0.18 Q10 1 0.2014 0.3074 0.4058 11.00000 0.05 0.17 ; _shelx_res_checksum 33425 _shelx_hkl_file ; 1 0 0 71.19 4.10 1 0 0 85.29 4.10 -1 0 0 72.19 4.70 2 0 0 354.76 17.30 -2 0 0 326.97 18.60 -3 0 0 2739.93 133.39 4 0 0 518.15 31.10 5 0 0 392.26 26.00 -5 0 0 343.97 28.00 -5 0 0 347.57 21.70 6 0 0 1201.18 69.59 6 0 0 1303.67 67.49 6 0 0 1214.18 67.39 6 0 0 1330.17 67.89 -6 0 0 1302.67 65.39 -7 0 0 197.68 18.50 7 0 0 224.58 21.40 7 0 0 219.98 21.70 -7 0 0 177.38 32.80 8 0 0 66.59 17.20 -8 0 0 96.89 16.30 -8 0 0 91.09 17.40 8 0 0 116.69 19.60 8 0 0 86.59 17.40 8 0 0 91.09 13.00 -9 0 0 208.08 20.30 9 0 0 202.18 29.40 9 0 0 199.98 33.50 9 0 0 226.08 24.40 -9 0 0 146.49 31.00 -9 0 0 255.87 30.00 -10 0 0 36.10 13.00 -10 0 0 65.19 19.70 10 0 0 50.59 13.30 10 0 0 45.90 40.40 10 0 0 20.90 11.70 0 -1 0 -0.10 3.40 0 1 0 2.90 2.40 0 1 0 0.20 2.70 1 -1 0 3683.23 177.28 1 -1 0 3791.92 178.38 -1 1 0 3635.04 177.48 -1 1 0 3650.83 177.68 2 -1 0 1649.54 74.99 2 -1 0 1503.15 75.99 -2 1 0 1359.96 75.69 -2 1 0 1481.95 75.79 3 -1 0 1602.24 77.89 3 -1 0 1516.35 78.99 3 -1 0 1542.45 77.09 -3 1 0 1560.24 80.69 -3 1 0 1551.24 80.19 4 -1 0 4382.06 202.58 4 -1 0 4114.49 205.28 4 -1 0 4192.08 201.58 -4 1 0 4130.59 207.48 5 -1 0 229.18 16.30 5 -1 0 230.38 19.20 5 -1 0 255.67 21.00 -5 1 0 311.97 25.20 6 -1 0 107.09 15.70 6 -1 0 96.29 18.00 6 -1 0 125.09 21.70 -6 -1 0 95.79 14.00 6 -1 0 120.79 15.90 6 -1 0 90.09 16.90 -6 1 0 126.29 27.40 -6 1 0 95.99 21.20 -6 1 0 95.99 19.40 6 1 0 95.69 24.20 6 1 0 113.59 14.90 6 1 0 94.09 16.00 -6 1 0 128.79 13.40 6 1 0 120.59 19.80 6 1 0 136.99 20.80 7 -1 0 495.25 34.40 7 -1 0 553.14 35.50 -7 -1 0 528.45 31.80 7 -1 0 535.55 39.10 7 -1 0 527.45 37.60 7 -1 0 525.75 41.50 7 1 0 557.74 35.10 -7 1 0 521.25 34.50 7 1 0 568.04 35.80 -7 1 0 477.15 52.59 7 1 0 472.65 39.00 7 1 0 550.14 37.00 -7 1 0 515.95 54.09 7 1 0 550.34 40.00 -8 -1 0 191.48 19.20 8 -1 0 186.38 35.10 8 -1 0 186.68 18.70 8 -1 0 164.38 34.40 8 1 0 189.48 24.60 8 1 0 130.49 29.20 8 1 0 207.68 21.60 -8 1 0 162.98 21.30 -8 1 0 204.88 24.30 -8 1 0 206.08 24.50 -8 1 0 222.88 47.10 8 1 0 187.58 21.60 9 -1 0 2.00 11.40 9 -1 0 7.50 8.20 9 -1 0 28.30 9.80 9 -1 0 4.70 22.00 9 1 0 13.50 11.20 -9 1 0 21.20 10.60 9 1 0 4.10 10.20 -9 1 0 -4.40 25.70 -9 1 0 29.90 12.60 9 1 0 26.80 15.50 -10 -1 0 138.19 30.10 -10 -1 0 145.19 20.90 10 -1 0 174.18 19.20 -10 1 0 219.48 27.20 10 1 0 210.08 18.90 10 1 0 180.68 36.80 -10 1 0 223.48 29.00 -10 1 0 198.28 19.60 0 2 0 9999.00 474.45 1 -2 0 375.76 25.40 1 -2 0 401.16 25.20 1 -2 0 390.26 24.70 -1 2 0 392.86 23.80 -1 2 0 389.26 24.60 2 -2 0 411.26 27.70 2 -2 0 346.67 24.30 -2 2 0 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27.50 7 2 0 249.48 26.40 7 2 0 264.67 30.40 7 2 0 262.47 28.20 -7 2 0 251.17 36.60 7 2 0 256.47 23.70 -7 2 0 247.18 22.70 7 2 0 262.87 23.70 -7 2 0 284.27 31.60 -7 2 0 283.47 27.10 -7 2 0 250.57 47.40 8 -2 0 288.77 30.50 8 -2 0 270.27 26.50 -8 -2 0 259.07 22.60 8 2 0 282.07 27.50 -8 2 0 320.37 25.40 -8 2 0 350.66 35.20 8 2 0 246.28 29.10 9 -2 0 157.08 20.60 9 -2 0 188.58 16.80 -9 2 0 158.68 18.50 9 2 0 167.08 19.40 -9 2 0 151.58 27.60 9 2 0 157.48 23.40 9 2 0 146.39 16.10 -9 2 0 152.48 20.80 10 -2 0 12.10 6.10 10 2 0 1.80 7.70 10 2 0 20.50 26.80 -10 2 0 12.40 8.90 10 2 0 12.50 8.80 -10 2 0 30.00 12.70 0 -3 0 -4.70 5.80 0 -3 0 -3.30 6.40 0 -3 0 -1.60 8.20 0 -3 0 -12.10 10.90 1 -3 0 2760.72 137.49 1 -3 0 2612.34 131.09 1 -3 0 2698.33 135.59 1 -3 0 2667.13 135.99 -1 3 0 2893.61 132.79 -1 3 0 2466.25 135.29 2 -3 0 3416.66 167.58 2 -3 0 3611.44 173.08 2 -3 0 3446.56 172.28 2 -3 0 3249.77 168.98 2 -3 0 3564.14 174.58 -2 3 0 3231.98 172.38 -2 3 0 3601.74 170.58 -2 3 0 3494.05 171.68 3 -3 0 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-18 109.39 17.40 1 2 18 75.69 16.10 -2 -2 -18 244.68 20.80 2 -2 18 250.87 22.60 -2 -2 -18 238.08 22.90 2 2 18 203.78 17.50 2 2 18 213.98 22.50 -2 2 -18 268.47 52.99 -2 2 -18 221.98 20.60 -3 -2 -18 3.80 8.90 3 -2 18 7.20 9.90 -3 -2 -18 4.70 9.30 -3 2 -18 -21.60 10.80 3 2 18 -2.70 15.40 -3 2 -18 1.90 9.40 -4 -2 -18 379.46 32.40 4 -2 18 399.76 25.30 4 2 18 385.06 26.40 -4 2 -18 467.25 26.20 4 2 18 422.76 31.40 -4 -3 18 22.50 7.70 4 -3 -18 27.20 7.90 -4 -3 18 16.80 5.50 4 -3 -18 20.20 10.00 -4 3 18 27.10 6.50 4 3 -18 24.50 6.00 -3 -3 18 97.19 14.10 3 -3 -18 60.29 20.20 3 -3 -18 77.19 14.10 3 3 -18 53.69 12.80 3 3 -18 67.19 11.30 -3 3 18 75.09 13.90 -2 -3 18 85.49 15.80 2 -3 -18 88.89 16.40 2 3 -18 91.99 13.30 2 3 -18 70.19 14.40 1 -3 -18 140.09 16.00 1 -3 -18 127.49 15.60 1 3 -18 109.99 15.80 1 3 -18 112.09 15.00 -1 3 18 88.89 22.50 0 -3 -18 147.19 26.10 0 -3 -18 99.69 19.80 0 3 18 105.99 15.70 0 3 18 91.09 12.60 1 -3 18 634.04 40.50 1 3 18 715.63 36.10 -1 3 -18 649.24 36.70 -2 -3 -18 38.20 12.90 2 -3 18 27.30 8.40 -2 -3 -18 18.40 8.80 -2 3 -18 40.50 8.20 3 -3 18 315.87 25.20 -3 -3 -18 359.76 22.50 -3 -3 -18 378.76 26.60 3 3 18 346.07 25.80 6 0 -19 100.19 18.50 -6 0 19 100.79 18.30 -5 0 19 2.90 6.90 5 0 -19 5.00 5.50 -4 0 19 436.16 32.30 4 0 -19 437.06 34.30 -4 0 19 480.85 28.70 -3 0 19 199.88 40.20 -3 0 19 103.99 20.70 3 0 -19 159.18 17.00 -3 0 19 143.89 16.70 3 0 -19 150.78 19.00 -2 0 19 186.88 22.20 2 0 -19 230.18 20.80 2 0 -19 206.38 27.50 -2 0 19 149.69 25.40 2 0 -19 226.48 23.20 -2 0 19 191.48 18.50 -1 0 19 409.96 27.00 -1 0 19 411.96 29.40 -1 0 19 389.66 30.80 1 0 -19 424.96 30.00 1 0 -19 438.16 32.10 1 0 -19 412.46 37.70 0 0 19 9.80 9.30 0 0 19 19.30 9.70 0 0 -19 22.20 9.90 0 0 -19 38.70 18.60 0 0 -19 42.10 13.40 0 0 -19 8.50 15.50 1 0 19 23.40 9.70 -1 0 -19 2.70 9.70 -1 0 -19 18.80 9.80 -1 0 -19 32.10 25.30 -1 0 -19 24.70 16.90 -2 0 -19 31.40 10.20 -2 0 -19 4.90 21.10 2 0 19 23.90 8.90 -3 0 -19 40.30 10.50 -3 0 -19 54.89 13.70 -4 0 -19 417.76 25.90 4 0 19 390.36 24.30 -4 0 -19 381.96 25.00 5 -1 -19 148.49 14.70 -5 -1 19 134.19 15.30 5 1 -19 163.58 15.60 -5 1 19 143.99 15.40 4 -1 -19 75.89 13.70 4 -1 -19 98.29 17.60 -4 -1 19 84.89 21.00 -4 -1 19 129.79 22.70 -4 1 19 91.29 17.60 -4 1 19 90.89 13.80 4 1 -19 126.59 25.70 3 -1 -19 275.17 25.80 -3 -1 19 313.37 26.20 3 -1 -19 202.68 36.40 -3 -1 19 243.28 19.70 -3 -1 19 187.48 34.50 3 1 -19 271.37 21.80 -3 1 19 316.17 24.80 -3 1 19 294.87 24.00 3 1 -19 281.47 21.30 2 -1 -19 39.90 14.00 -2 -1 19 29.10 8.50 -2 -1 19 43.60 20.20 -2 -1 19 22.30 12.00 2 -1 -19 44.20 10.80 2 -1 -19 20.00 12.10 -2 1 19 20.60 9.50 2 1 -19 28.70 10.10 2 1 -19 32.90 9.40 -2 1 19 27.10 9.80 1 -1 -19 191.08 20.60 -1 -1 19 175.68 17.50 1 -1 -19 156.78 31.90 -1 -1 19 178.38 26.90 -1 -1 19 191.58 23.00 1 1 -19 164.68 18.70 1 1 -19 135.59 26.10 -1 1 19 196.68 20.90 1 1 -19 201.68 21.10 0 -1 19 175.38 16.70 0 -1 19 169.78 25.90 0 -1 19 178.88 21.00 0 -1 -19 180.48 21.10 0 -1 -19 130.79 31.00 0 -1 -19 163.18 20.10 0 -1 -19 148.39 29.10 0 1 -19 213.58 20.70 0 1 -19 220.38 20.20 0 1 -19 124.39 22.50 0 1 19 203.58 20.20 1 -1 19 139.89 18.70 1 -1 19 174.58 22.90 -1 -1 -19 148.59 19.30 -1 -1 -19 154.18 17.30 -1 1 -19 154.08 29.60 1 1 19 139.19 17.00 -1 1 -19 171.28 18.30 -2 -1 -19 114.19 14.30 2 -1 19 116.99 16.30 -2 -1 -19 148.99 16.40 -2 1 -19 120.49 16.90 2 1 19 96.69 13.90 -3 -1 -19 611.64 36.00 -3 -1 -19 518.85 35.70 -3 1 -19 605.44 40.80 3 1 19 554.94 32.00 -4 -1 -19 155.48 20.00 4 -1 19 211.88 15.90 -4 -1 -19 212.98 15.90 -4 1 -19 204.38 16.00 -5 -2 19 7.00 6.20 5 -2 -19 15.20 6.30 5 -2 -19 14.70 7.50 -5 2 19 2.30 5.20 -5 2 19 0.90 11.90 5 2 -19 8.80 6.80 4 -2 -19 62.69 12.30 -4 -2 19 65.89 9.80 4 -2 -19 44.40 15.60 4 2 -19 61.49 9.20 -4 2 19 64.99 10.70 3 -2 -19 107.09 23.60 3 -2 -19 161.78 15.30 -3 -2 19 124.59 21.60 -3 2 19 145.59 22.30 3 2 -19 148.99 25.20 2 -2 -19 47.70 10.70 2 -2 -19 18.10 16.00 -2 -2 19 -5.20 13.50 -2 2 19 31.00 8.90 2 2 -19 23.20 7.00 1 -2 -19 313.97 26.10 1 -2 -19 330.27 23.80 -1 -2 19 237.48 35.00 -1 -2 19 361.46 29.90 -1 2 19 319.97 24.30 1 2 -19 303.07 23.30 1 2 -19 329.67 24.30 0 -2 19 34.70 22.80 0 -2 19 11.20 12.90 0 -2 -19 32.30 10.30 0 2 -19 14.10 10.20 0 2 -19 18.40 10.30 0 2 19 20.60 7.60 1 -2 19 238.58 18.30 -1 -2 -19 242.38 20.80 -1 -2 -19 220.58 25.50 -1 2 -19 193.58 17.70 -2 -2 -19 277.37 23.10 -2 -2 -19 309.17 22.20 2 -2 19 295.47 21.10 -2 2 -19 303.67 23.50 2 2 19 261.57 18.40 -2 2 -19 277.57 21.50 -3 -2 -19 15.80 9.10 3 -2 19 18.30 6.30 -3 -2 -19 5.90 8.70 -3 2 -19 14.80 6.00 -3 2 -19 32.40 8.50 -3 -3 19 42.30 10.50 3 -3 -19 48.30 8.80 3 3 -19 51.39 7.70 -3 3 19 40.60 8.60 -2 -3 19 279.37 18.80 2 -3 -19 304.57 22.00 -2 3 19 275.67 20.20 2 3 -19 277.17 19.80 -1 -3 19 -0.50 9.70 1 -3 -19 8.10 11.10 -1 3 19 7.70 6.20 1 3 -19 16.20 7.30 0 -3 -19 103.79 13.50 0 -3 19 116.59 15.00 0 -3 -19 104.69 12.60 0 3 -19 104.49 11.20 0 3 19 76.49 10.70 -1 -3 -19 101.29 13.20 -1 3 -19 91.79 13.10 -2 -3 -19 159.88 15.60 -2 -3 -19 186.28 16.30 2 -3 19 173.78 14.50 2 3 19 155.18 21.30 -2 3 -19 149.29 13.60 -2 3 -19 159.28 14.90 5 0 -20 118.99 20.30 -5 0 20 61.29 15.40 -5 0 20 95.59 18.80 -4 0 20 258.77 19.80 -4 0 20 276.67 22.90 4 0 -20 276.77 22.20 -3 0 20 27.50 6.50 -3 0 20 33.00 8.60 3 0 -20 28.60 9.90 3 0 -20 19.10 9.20 -2 0 20 8.80 14.40 2 0 -20 3.00 9.50 2 0 -20 11.70 6.40 -2 0 20 21.50 9.10 -1 0 20 123.09 13.60 -1 0 20 132.99 17.80 1 0 -20 166.08 17.30 1 0 -20 105.69 18.20 1 0 -20 71.69 21.20 0 0 -20 432.26 49.20 0 0 -20 505.65 32.30 0 0 20 503.85 33.10 0 0 -20 484.75 35.60 -1 0 -20 -13.30 17.30 -1 0 -20 -1.40 8.10 1 0 20 2.20 5.50 -2 0 -20 606.04 35.20 -2 0 -20 551.24 36.60 2 0 20 588.14 38.40 -3 0 -20 55.19 12.80 -3 0 -20 44.70 12.50 3 0 20 49.00 10.30 -4 -1 20 4.30 6.70 4 -1 -20 6.50 6.40 -4 -1 20 -11.60 8.90 4 -1 -20 -8.10 11.80 -4 1 20 0.10 6.10 -4 1 20 -0.40 9.70 4 1 -20 4.40 7.30 3 -1 -20 15.60 9.80 -3 -1 20 47.80 11.50 3 -1 -20 22.30 8.10 3 1 -20 23.10 8.20 -3 1 20 23.20 9.00 -2 -1 20 327.87 22.70 2 -1 -20 316.17 26.60 -2 1 20 290.17 28.20 2 1 -20 256.47 21.70 2 1 -20 231.38 27.50 -1 -1 20 25.30 12.20 -1 -1 20 13.40 12.90 1 -1 -20 20.20 7.40 1 -1 -20 -8.30 20.50 1 1 -20 24.30 10.20 -1 1 20 7.20 8.40 1 1 -20 7.40 9.60 0 -1 -20 181.78 18.80 0 -1 -20 154.48 20.30 0 -1 20 217.98 29.30 0 -1 20 168.28 16.30 0 1 -20 204.78 25.20 0 1 20 124.39 16.70 0 1 -20 120.19 18.10 1 -1 20 349.96 28.00 -1 -1 -20 255.97 24.40 2 -1 20 10.70 5.80 -2 -1 -20 2.40 8.30 -2 -1 -20 4.20 13.50 2 1 20 -5.50 5.60 -2 1 -20 2.00 13.50 -2 1 -20 -3.50 7.20 -3 -1 -20 338.77 24.40 -3 -1 -20 314.47 21.70 3 -1 20 293.57 21.40 3 1 20 319.07 22.40 -3 1 -20 345.57 22.80 -3 -2 20 100.29 25.90 3 -2 -20 83.89 10.10 3 -2 -20 48.10 10.30 -3 -2 20 69.29 9.30 -3 2 20 65.39 10.90 3 2 -20 80.19 12.20 2 -2 -20 27.20 8.80 2 -2 -20 37.40 15.70 -2 -2 20 38.70 21.40 -2 2 20 55.29 12.80 2 2 -20 45.60 9.20 1 -2 -20 98.29 15.50 -1 -2 20 113.19 12.70 1 2 -20 94.79 12.00 -1 2 20 108.79 14.10 0 -2 -20 200.28 17.30 0 -2 20 226.28 18.70 0 -2 -20 198.28 18.10 0 -2 20 208.68 15.90 0 2 -20 242.88 19.40 0 2 20 215.18 17.50 1 -2 20 29.10 9.90 1 -2 20 51.79 10.50 -1 -2 -20 44.50 10.20 -1 -2 -20 55.59 12.30 -1 2 -20 56.49 11.60 -1 2 -20 40.50 14.50 1 2 20 39.60 9.20 -2 -2 -20 362.16 24.00 2 -2 20 373.86 23.60 -2 2 -20 340.77 23.50 -2 2 -20 431.36 26.00 -3 0 21 16.00 9.70 3 0 -21 0.00 9.60 3 0 -21 -10.70 9.40 -3 0 21 -2.80 7.60 2 0 -21 19.40 7.80 2 0 -21 10.20 11.00 -2 0 21 20.30 9.40 -2 0 21 27.10 12.60 1 0 -21 139.69 13.40 -1 0 21 144.99 17.30 0 0 -21 351.36 23.20 -1 0 -21 21.60 6.50 1 0 21 18.90 7.70 2 0 21 147.59 12.60 -2 0 -21 178.48 16.00 -3 -1 21 28.40 8.30 3 -1 -21 15.70 6.40 -3 -1 21 20.50 6.30 3 -1 -21 3.30 10.50 -3 1 21 12.00 9.20 3 1 -21 22.00 6.30 -2 -1 21 172.88 16.30 2 -1 -21 152.08 16.70 2 -1 -21 134.79 14.80 -2 -1 21 151.18 16.10 -2 1 21 138.99 13.80 2 1 -21 149.19 14.40 -1 -1 21 36.70 8.60 1 -1 -21 40.90 10.50 -1 -1 21 26.80 9.60 0 -1 -21 11.70 8.20 0 -1 21 3.10 5.90 0 1 21 11.10 5.10 0 1 -21 5.40 7.00 0 1 -21 14.70 7.10 -1 -1 -21 115.59 15.20 1 -1 21 102.99 14.60 -1 1 -21 83.59 14.40 -1 1 -21 132.79 11.90 1 1 21 117.49 12.80 2 -1 21 226.48 18.30 2 1 21 243.78 17.60 -1 -2 21 181.78 16.70 1 2 -21 155.18 16.20 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 78257 #============================================================================= # end of cif data for "gil10361" (compound 3s) #============================================================================= #============================================================================= # cif data for "gil10346" (compound 4e-OH) #============================================================================= data_gil10346_4e-OH _audit_creation_method 'APEX4 v2021.4-0' _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H9 Br O3' _chemical_formula_iupac ? _chemical_formula_weight 269.09 _chemical_melting_point ? _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 6.2312(2) _cell_length_b 10.6655(3) _cell_length_c 15.3509(5) _cell_angle_alpha 90 _cell_angle_beta 93.7740(10) _cell_angle_gamma 90 _cell_volume 1017.99(5) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9944 _cell_measurement_theta_min 8.6842 _cell_measurement_theta_max 68.2157 _cell_measurement_temperature 100.(2) _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.219 _exptl_crystal_size_mid 0.098 _exptl_crystal_size_min 0.055 _exptl_crystal_density_diffrn 1.756 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 536 _exptl_absorpt_coefficient_mu 5.386 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_process_details ; Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015). "Comparison of silver and molybdenum microfocus X-ray sources for single-crystal structure determination" J. Appl. Cryst. 48, 3-10. doi:10.1107/S1600576714022985 ; _exptl_absorpt_correction_T_min 0.65 _exptl_absorpt_correction_T_max 0.76 _exptl_special_details ; ; _diffrn_ambient_temperature 100.(2) _diffrn_source 'Cu ImS' _diffrn_source_type 'micro focus tube' _diffrn_source_power 0.05 _diffrn_source_current 1.0 _diffrn_source_voltage 50 _diffrn_radiation_probe 'single crystal' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_monochromator 'MX mirror' _diffrn_measurement_device 'Bruker D8 Venture Photon III' _diffrn_measurement_device_type 'single crystal diffractometer' _diffrn_measurement_method 'phi/omega scans' _diffrn_detector_area_resol_mean 7.3910 _diffrn_reflns_number 19006 _diffrn_reflns_av_R_equivalents 0.0372 _diffrn_reflns_av_unetI/netI 0.0189 _diffrn_reflns_theta_min 8.90 _diffrn_reflns_theta_max 66.59 _diffrn_reflns_theta_full 66.59 _diffrn_measured_fraction_theta_max 0.977 _diffrn_measured_fraction_theta_full 0.977 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _refine_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_number_total 1758 _reflns_number_gt 1736 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0193 _refine_ls_R_factor_gt 0.0190 _refine_ls_wR_factor_gt 0.0513 _refine_ls_wR_factor_ref 0.0514 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _refine_ls_number_reflns 1758 _refine_ls_number_parameters 140 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_hydrogen_treatment mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0260P)^2^+0.6546P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary ? _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.307 _refine_diff_density_min -0.302 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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' Br Br -0.6763 1.2805 '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' _computing_data_collection 'Bruker APEX4 v2021.4-0 Photon III' _computing_cell_refinement 'SAINT V8.40B (Bruker AXS LLC, 2019)' _computing_data_reduction 'SAINT V8.40B (Bruker AXS LLC, 2019)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_molecular_graphics 'shelXle (C.B. Huebschle, rev 1242)' _computing_publication_material 'SHELXT 2018/2 (Sheldrick, 2018)' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_flags_posn _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Br Br1 0.88924(3) 0.34124(2) 0.04477(2) 0.02003(10) Uani d . . . 1 . . O O1 0.0853(2) 0.64886(10) 0.24253(8) 0.0187(3) Uani d . . . 1 . . O O2 0.32344(18) 0.54407(10) 0.42429(7) 0.0178(2) Uani d . . . 1 . . O O3 0.3584(2) 0.34748(11) 0.47470(9) 0.0192(3) Uani d . . . 1 . . H H3A 0.444(4) 0.374(2) 0.4994(15) 0.017(6) Uiso d . . . 1 . . C C1 0.6567(3) 0.40236(15) 0.10651(10) 0.0154(3) Uani d . . . 1 . . C C2 0.6109(3) 0.53005(16) 0.10530(10) 0.0176(3) Uani d . . . 1 . . H H2 0.693278 0.586632 0.073282 0.021000 Uiso calc U . R 1 . . C C3 0.4427(3) 0.57270(15) 0.15175(10) 0.0158(3) Uani d . . . 1 . . H H3 0.409986 0.659695 0.151856 0.019000 Uiso calc U . R 1 . . C C4 0.3202(3) 0.48979(14) 0.19853(10) 0.0135(3) Uani d . . . 1 . . C C5 0.3707(3) 0.36166(15) 0.19855(10) 0.0146(3) Uani d . . . 1 . . H H5 0.288097 0.304618 0.230124 0.017000 Uiso calc U . R 1 . . C C6 0.5396(3) 0.31751(15) 0.15300(10) 0.0154(3) Uani d . . . 1 . . H H6 0.574768 0.230835 0.153529 0.018000 Uiso calc U . R 1 . . C C7 0.1334(2) 0.53806(14) 0.24416(10) 0.0136(3) Uani d . . . 1 . . C C8 -0.0024(2) 0.44334(14) 0.28831(10) 0.0142(3) Uani d . . . 1 . . H H8 -0.078890 0.382486 0.247580 0.017000 Uiso calc U . R 1 . . C C9 -0.1253(3) 0.48076(16) 0.36345(11) 0.0193(3) Uani d . . . 1 . . H H9A -0.272402 0.446698 0.366379 0.023000 Uiso calc U . R 1 . . H H9B -0.105837 0.567350 0.385841 0.023000 Uiso calc U . R 1 . . C C10 0.0625(3) 0.39008(15) 0.37852(10) 0.0152(3) Uani d . . . 1 . . H H10 0.023928 0.300392 0.388294 0.018000 Uiso calc U . R 1 . . C C11 0.2590(2) 0.43590(14) 0.42734(10) 0.0137(3) Uani d . . . 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Br1 0.01915(13) 0.02346(13) 0.01782(13) 0.00087(6) 0.00386(8) -0.00094(6) O1 0.0242(6) 0.0121(6) 0.0193(6) 0.0034(4) -0.0013(5) 0.0007(4) O2 0.0206(6) 0.0139(6) 0.0178(6) -0.0037(4) -0.0056(5) 0.0031(4) O3 0.0229(7) 0.0141(6) 0.0191(6) -0.0021(5) -0.0092(6) 0.0019(4) C1 0.0147(7) 0.0201(8) 0.0108(7) 0.0009(6) -0.0027(6) -0.0027(6) C2 0.0202(8) 0.0171(8) 0.0153(8) -0.0049(6) -0.0004(6) 0.0020(6) C3 0.0212(8) 0.0109(7) 0.0147(8) -0.0012(6) -0.0036(6) -0.0001(6) C4 0.0163(7) 0.0127(7) 0.0107(7) -0.0005(6) -0.0047(6) -0.0003(6) C5 0.0177(8) 0.0121(7) 0.0135(8) -0.0015(6) -0.0015(6) 0.0007(6) C6 0.0188(8) 0.0121(7) 0.0145(8) 0.0012(6) -0.0042(6) -0.0010(6) C7 0.0175(8) 0.0123(7) 0.0101(7) -0.0004(6) -0.0058(6) -0.0012(6) C8 0.0137(7) 0.0145(7) 0.0137(7) -0.0004(6) -0.0034(6) -0.0018(6) C9 0.0142(8) 0.0227(8) 0.0212(8) 0.0003(6) 0.0014(6) -0.0019(7) C10 0.0171(8) 0.0146(8) 0.0139(8) -0.0028(6) 0.0006(6) 0.0009(6) C11 0.0165(7) 0.0150(8) 0.0099(7) 0.0004(6) 0.0022(6) 0.0001(6) _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_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Br1 C1 . 1.8983(16) ? O1 C7 . 1.2190(19) ? O2 C11 . 1.2235(19) ? O3 C11 . 1.320(2) ? O3 H3A . 0.69(2) ? C1 C6 . 1.389(2) ? C1 C2 . 1.391(2) ? C2 C3 . 1.383(2) ? C2 H2 . 0.950000 ? C3 C4 . 1.398(2) ? C3 H3 . 0.950000 ? C4 C5 . 1.402(2) ? C4 C7 . 1.489(2) ? C5 C6 . 1.384(2) ? C5 H5 . 0.950000 ? C6 H6 . 0.950000 ? C7 C8 . 1.507(2) ? C8 C9 . 1.481(2) ? C8 C10 . 1.527(2) ? C8 H8 . 1.000000 ? C9 C10 . 1.524(2) ? C9 H9A . 0.990000 ? C9 H9B . 0.990000 ? C10 C11 . 1.476(2) ? C10 H10 . 1.000000 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C11 O3 H3A . . 109.4(18) ? C6 C1 C2 . . 122.03(15) ? C6 C1 Br1 . . 118.48(12) ? C2 C1 Br1 . . 119.48(12) ? C3 C2 C1 . . 118.48(15) ? C3 C2 H2 . . 120.800000 ? C1 C2 H2 . . 120.800000 ? C2 C3 C4 . . 121.00(15) ? C2 C3 H3 . . 119.500000 ? C4 C3 H3 . . 119.500000 ? C3 C4 C5 . . 119.12(15) ? C3 C4 C7 . . 119.56(14) ? C5 C4 C7 . . 121.27(15) ? C6 C5 C4 . . 120.63(15) ? C6 C5 H5 . . 119.700000 ? C4 C5 H5 . . 119.700000 ? C5 C6 C1 . . 118.73(15) ? C5 C6 H6 . . 120.600000 ? C1 C6 H6 . . 120.600000 ? O1 C7 C4 . . 121.61(15) ? O1 C7 C8 . . 120.97(15) ? C4 C7 C8 . . 117.33(13) ? C9 C8 C7 . . 120.27(14) ? C9 C8 C10 . . 60.87(11) ? C7 C8 C10 . . 122.29(13) ? C9 C8 H8 . . 114.400000 ? C7 C8 H8 . . 114.400000 ? C10 C8 H8 . . 114.400000 ? C8 C9 C10 . . 61.05(10) ? C8 C9 H9A . . 117.700000 ? C10 C9 H9A . . 117.700000 ? C8 C9 H9B . . 117.700000 ? C10 C9 H9B . . 117.700000 ? H9A C9 H9B . . 114.800000 ? C11 C10 C9 . . 118.02(14) ? C11 C10 C8 . . 119.92(13) ? C9 C10 C8 . . 58.07(10) ? C11 C10 H10 . . 116.100000 ? C9 C10 H10 . . 116.100000 ? C8 C10 H10 . . 116.100000 ? O2 C11 O3 . . 123.46(14) ? O2 C11 C10 . . 123.79(14) ? O3 C11 C10 . . 112.75(13) ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C6 C1 C2 C3 . . . . -0.3(2) ? Br1 C1 C2 C3 . . . . -179.09(11) ? C1 C2 C3 C4 . . . . -0.4(2) ? C2 C3 C4 C5 . . . . 0.5(2) ? C2 C3 C4 C7 . . . . -176.94(14) ? C3 C4 C5 C6 . . . . 0.1(2) ? C7 C4 C5 C6 . . . . 177.44(14) ? C4 C5 C6 C1 . . . . -0.7(2) ? C2 C1 C6 C5 . . . . 0.8(2) ? Br1 C1 C6 C5 . . . . 179.63(12) ? C3 C4 C7 O1 . . . . -0.7(2) ? C5 C4 C7 O1 . . . . -178.09(14) ? C3 C4 C7 C8 . . . . 175.81(13) ? C5 C4 C7 C8 . . . . -1.5(2) ? O1 C7 C8 C9 . . . . -29.6(2) ? C4 C7 C8 C9 . . . . 153.79(14) ? O1 C7 C8 C10 . . . . -102.31(18) ? C4 C7 C8 C10 . . . . 81.12(18) ? C7 C8 C9 C10 . . . . -112.51(15) ? C8 C9 C10 C11 . . . . 109.52(15) ? C9 C8 C10 C11 . . . . -106.26(16) ? C7 C8 C10 C11 . . . . 3.0(2) ? C7 C8 C10 C9 . . . . 109.30(17) ? C9 C10 C11 O2 . . . . -33.0(2) ? C8 C10 C11 O2 . . . . 34.3(2) ? C9 C10 C11 O3 . . . . 147.06(14) ? C8 C10 C11 O3 . . . . -145.58(14) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O3 H3A O2 3_666 0.69(2) 2.00(2) 2.6958(17) 176.(2) ? _shelx_res_file ; TITL gil10346.res in P2(1)/c gil10346.res created by SHELXL-2018/3 at 10:16:06 on 09-Jun-2022 CELL 1.54178 6.2312 10.6655 15.3509 90.000 93.774 90.000 ZERR 4.000 0.0002 0.0003 0.0005 0.000 0.001 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H Br O UNIT 44 36 4 12 LIST 4 REM Old TITL gil10346 in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.053, Rweak 0.003, Alpha 0.040 REM 1.487 for 112 systematic absences, Orientation as input REM Formula found by SHELXT: C11 Br O3 SIZE 0.055 0.098 0.219 TEMP -173.150 ACTA CONF L.S. 30 BOND $H FMAP 2 PLAN 10 HTAB EQIV $1 -x+1, -y+1, -z+1 HTAB O3 O2_$1 OMIT 1 0 6 WGHT 0.026000 0.654600 FVAR 0.87217 BR1 3 0.889241 0.341236 0.044773 11.00000 0.01915 0.02346 = 0.01782 -0.00094 0.00386 0.00087 O1 4 0.085342 0.648865 0.242531 11.00000 0.02422 0.01213 = 0.01931 0.00067 -0.00134 0.00336 O2 4 0.323438 0.544071 0.424291 11.00000 0.02063 0.01391 = 0.01783 0.00315 -0.00559 -0.00372 O3 4 0.358435 0.347481 0.474699 11.00000 0.02288 0.01412 = 0.01915 0.00187 -0.00923 -0.00212 H3A 2 0.444494 0.373641 0.499433 11.00000 0.01682 C1 1 0.656697 0.402361 0.106511 11.00000 0.01469 0.02013 = 0.01077 -0.00267 -0.00273 0.00088 C2 1 0.610893 0.530046 0.105296 11.00000 0.02025 0.01707 = 0.01534 0.00203 -0.00043 -0.00488 AFIX 43 H2 2 0.693278 0.586632 0.073282 11.00000 -1.20000 AFIX 0 C3 1 0.442726 0.572703 0.151746 11.00000 0.02120 0.01092 = 0.01467 -0.00014 -0.00358 -0.00124 AFIX 43 H3 2 0.409986 0.659695 0.151856 11.00000 -1.20000 AFIX 0 C4 1 0.320188 0.489793 0.198534 11.00000 0.01630 0.01268 = 0.01069 -0.00028 -0.00472 -0.00055 C5 1 0.370651 0.361660 0.198550 11.00000 0.01770 0.01213 = 0.01354 0.00070 -0.00150 -0.00153 AFIX 43 H5 2 0.288097 0.304618 0.230124 11.00000 -1.20000 AFIX 0 C6 1 0.539582 0.317511 0.153005 11.00000 0.01885 0.01212 = 0.01453 -0.00103 -0.00422 0.00119 AFIX 43 H6 2 0.574768 0.230835 0.153529 11.00000 -1.20000 AFIX 0 C7 1 0.133407 0.538062 0.244159 11.00000 0.01753 0.01233 = 0.01015 -0.00117 -0.00577 -0.00037 C8 1 -0.002414 0.443342 0.288306 11.00000 0.01370 0.01452 = 0.01374 -0.00181 -0.00339 -0.00040 AFIX 13 H8 2 -0.078890 0.382486 0.247580 11.00000 -1.20000 AFIX 0 C9 1 -0.125261 0.480765 0.363452 11.00000 0.01416 0.02274 = 0.02116 -0.00195 0.00144 0.00026 AFIX 23 H9A 2 -0.272402 0.446698 0.366379 11.00000 -1.20000 H9B 2 -0.105837 0.567350 0.385841 11.00000 -1.20000 AFIX 0 C10 1 0.062510 0.390076 0.378519 11.00000 0.01707 0.01463 = 0.01389 0.00087 0.00056 -0.00283 AFIX 13 H10 2 0.023928 0.300392 0.388294 11.00000 -1.20000 AFIX 0 C11 1 0.258998 0.435902 0.427337 11.00000 0.01648 0.01498 = 0.00991 0.00014 0.00216 0.00036 HKLF 4 REM gil10346.res in P2(1)/c REM wR2 = 0.051429, GooF = S = 1.09231, Restrained GooF = 1.09231 for all data REM R1 = 0.019039 for 1736 Fo > 4sig(Fo) and 0.019263 for all 1758 data REM 140 parameters refined using 0 restraints END WGHT 0.0260 0.6545 REM Instructions for potential hydrogen bonds HTAB O3 O2_$1 EQIV $2 -x+1, y-1/2, -z+1/2 HTAB C6 O2_$2 EQIV $3 x-1, y, z HTAB C8 Br1_$3 EQIV $4 -x, y-1/2, -z+1/2 HTAB C8 O1_$4 EQIV $5 x-1, -y+1/2, z+1/2 HTAB C10 Br1_$5 HTAB C10 O1_$4 REM Highest difference peak 0.307, deepest hole -0.302, 1-sigma level 0.056 Q1 1 0.1574 0.4135 0.4028 11.00000 0.05 0.31 Q2 1 0.2353 0.5076 0.2155 11.00000 0.05 0.29 Q3 1 -0.0191 0.4365 0.3941 11.00000 0.05 0.26 Q4 1 0.7334 0.3783 0.0845 11.00000 0.05 0.26 Q5 1 0.5751 0.3576 0.1190 11.00000 0.05 0.24 Q6 1 -0.0082 0.3602 0.2522 11.00000 0.05 0.23 Q7 1 0.0563 0.4923 0.2663 11.00000 0.05 0.22 Q8 1 0.4616 0.3426 0.1742 11.00000 0.05 0.21 Q9 1 -0.0820 0.4761 0.3070 11.00000 0.05 0.20 Q10 1 0.4874 0.5403 0.1111 11.00000 0.05 0.20 ; _shelx_res_checksum 61192 _shelx_hkl_file ; 2 0 0 1039.50 47.80 2 0 0 1003.30 48.20 2 0 0 1070.39 49.50 -2 0 0 1020.20 47.80 3 0 0 224.88 14.50 3 0 0 220.98 11.60 -3 0 0 207.08 12.60 3 0 0 209.48 12.70 4 0 0 9999.00 406.26 4 0 0 8797.82 405.36 4 0 0 8264.47 409.06 5 0 0 4321.77 200.08 -5 0 0 4581.34 205.08 -5 0 0 4422.96 200.38 -5 0 0 4491.65 203.78 -5 0 0 4537.05 200.68 5 0 0 4608.44 209.48 5 0 0 4066.59 200.18 -6 0 0 293.27 15.40 -6 0 0 258.97 19.70 6 0 0 272.07 23.20 6 0 0 258.07 14.60 -6 0 0 312.67 20.10 6 0 0 283.27 14.80 7 0 0 14.30 2.10 7 0 0 8.70 2.00 -7 0 0 11.50 2.20 -7 0 0 17.30 5.30 0 -1 0 1.10 0.50 0 -1 0 1.30 0.40 -3 -1 0 5401.76 226.18 -3 -1 0 4570.54 224.38 3 1 0 4907.11 224.28 3 1 0 5113.59 226.08 4 -1 0 132.19 11.00 4 -1 0 141.19 8.90 4 -1 0 145.39 9.30 4 -1 0 140.99 8.40 -4 -1 0 150.08 10.80 -4 -1 0 129.99 9.20 -4 -1 0 145.09 8.30 4 -1 0 140.49 12.90 4 1 0 150.58 8.20 4 1 0 132.59 12.30 4 1 0 122.09 9.20 -4 1 0 141.79 8.80 -4 1 0 154.08 11.20 4 1 0 152.68 9.40 -4 1 0 153.88 10.40 -4 1 0 152.18 8.40 5 -1 0 46.80 4.40 5 -1 0 52.09 5.70 -5 -1 0 60.59 5.20 -5 -1 0 44.50 7.40 -5 -1 0 61.59 8.30 -5 -1 0 61.19 5.80 5 -1 0 46.70 9.50 5 1 0 56.19 6.40 5 1 0 40.50 8.50 -5 1 0 49.30 6.30 -5 1 0 46.30 6.70 5 1 0 40.10 5.30 -5 1 0 47.60 6.70 5 1 0 41.70 4.30 -5 1 0 51.09 5.50 -6 -1 0 1999.60 106.29 6 -1 0 2172.38 102.09 6 -1 0 2315.07 101.89 -6 -1 0 2348.76 102.69 -6 -1 0 2223.18 107.19 -6 -1 0 2335.87 102.89 -6 1 0 2340.07 102.59 -6 1 0 2196.28 106.29 -6 1 0 2222.18 102.59 -6 1 0 2197.18 107.19 6 1 0 2233.48 101.79 6 1 0 2193.18 102.19 7 -1 0 526.05 24.40 -7 -1 0 506.25 24.60 7 -1 0 491.55 23.90 -7 -1 0 517.45 24.70 -7 -1 0 517.55 28.40 7 1 0 507.25 23.80 -7 1 0 473.95 28.30 7 1 0 497.25 24.20 -7 1 0 533.95 24.60 -7 1 0 505.45 24.40 1 -2 0 622.74 29.30 1 -2 0 658.33 30.00 -1 2 0 595.94 28.60 1 2 0 596.54 30.50 2 -2 0 866.01 40.40 2 -2 0 823.82 41.00 2 2 0 828.92 42.10 -2 2 0 898.21 40.90 -2 2 0 860.61 40.20 3 -2 0 1390.16 67.49 -3 -2 0 1559.44 69.39 3 -2 0 1506.95 68.59 3 -2 0 1347.57 69.59 3 2 0 1585.54 72.19 -3 2 0 1591.34 69.69 -3 2 0 1465.95 68.59 -3 2 0 1335.47 67.09 4 -2 0 203.38 11.40 4 -2 0 220.68 13.00 4 -2 0 225.58 12.10 -4 -2 0 211.88 11.30 4 -2 0 186.48 10.90 4 -2 0 225.08 15.10 4 -2 0 242.88 16.80 -4 2 0 220.48 13.40 -4 2 0 220.28 11.80 4 2 0 235.38 17.20 -4 2 0 184.48 11.80 4 2 0 175.98 11.70 -4 2 0 218.78 14.40 4 2 0 204.68 10.80 4 2 0 181.38 12.20 5 -2 0 190.38 12.10 -5 -2 0 171.28 11.10 5 -2 0 184.38 11.60 5 -2 0 202.78 18.00 5 -2 0 198.68 11.10 5 -2 0 165.38 15.90 -5 2 0 172.08 13.70 5 2 0 176.48 11.50 5 2 0 195.58 12.20 -5 2 0 185.18 11.80 -5 2 0 197.68 11.10 -5 2 0 208.08 12.00 5 2 0 177.28 17.60 5 2 0 182.28 10.30 -5 2 0 195.98 15.00 -6 -2 0 305.47 16.10 -6 -2 0 302.67 19.90 6 -2 0 291.57 15.80 -6 -2 0 321.37 16.20 6 -2 0 321.07 26.40 -6 2 0 282.77 19.70 6 2 0 284.17 15.90 -6 2 0 284.17 19.00 6 2 0 299.77 15.70 -6 2 0 290.07 15.70 6 2 0 283.47 14.90 6 2 0 310.97 25.90 -6 2 0 280.07 16.50 7 -2 0 64.09 4.70 -7 -2 0 77.29 5.70 -7 -2 0 72.09 5.00 -7 -2 0 65.39 7.80 7 2 0 66.89 6.00 7 2 0 65.99 4.80 -7 2 0 62.89 4.60 -7 2 0 82.49 13.40 0 -3 0 1.10 1.40 0 3 0 2.70 2.30 1 -3 0 314.97 16.50 1 -3 0 318.17 16.10 1 3 0 332.07 17.60 -1 3 0 301.17 16.50 -1 3 0 329.17 15.50 2 -3 0 291.27 16.00 2 -3 0 264.17 14.90 -2 3 0 288.77 14.50 -2 3 0 266.07 15.30 2 3 0 287.57 17.10 3 -3 0 227.78 14.60 3 -3 0 254.17 13.00 3 -3 0 239.28 13.50 3 -3 0 249.78 16.00 -3 3 0 290.67 15.90 3 3 0 286.57 18.10 -3 3 0 273.87 13.30 4 -3 0 35.90 4.30 -4 -3 0 33.40 3.70 4 -3 0 34.40 4.00 4 -3 0 27.80 3.50 4 -3 0 30.10 4.80 4 -3 0 33.70 4.10 4 -3 0 34.00 6.40 4 3 0 39.10 4.60 -4 3 0 34.60 3.90 -4 3 0 38.80 6.20 -4 3 0 34.40 4.30 -4 3 0 34.30 4.50 4 3 0 36.90 4.80 -4 3 0 34.00 5.30 4 3 0 26.40 3.10 4 3 0 31.60 6.80 5 -3 0 177.78 16.40 5 -3 0 180.28 12.10 -5 -3 0 177.88 10.40 5 -3 0 166.98 10.50 -5 -3 0 164.08 10.00 5 -3 0 184.28 17.60 5 -3 0 154.18 10.90 5 3 0 179.58 11.00 -5 3 0 169.98 10.50 -5 3 0 159.48 10.90 5 3 0 153.08 10.80 -5 3 0 173.28 13.00 5 3 0 151.68 16.80 -5 3 0 181.08 10.50 5 3 0 174.28 10.60 5 3 0 162.08 9.20 -5 3 0 187.28 14.80 -6 -3 0 275.47 14.80 -6 -3 0 280.27 15.20 6 -3 0 267.37 14.60 6 -3 0 270.77 15.50 -6 -3 0 299.57 19.10 6 3 0 272.07 15.10 -6 3 0 242.58 19.00 6 3 0 264.67 14.60 -6 3 0 261.07 14.40 -6 3 0 306.87 15.70 -6 3 0 264.97 18.00 -6 3 0 261.27 14.30 6 3 0 267.07 13.40 7 -3 0 7.00 2.20 -7 -3 0 4.90 3.40 -7 -3 0 8.50 2.30 -7 -3 0 4.90 1.70 -7 3 0 9.10 3.00 7 3 0 2.90 2.10 7 3 0 2.80 1.80 1 -4 0 1907.81 87.39 1 -4 0 1895.51 86.89 -1 4 0 1837.02 87.49 1 4 0 1933.01 89.29 2 -4 0 856.61 42.80 2 -4 0 867.91 43.30 2 -4 0 815.22 40.40 2 4 0 977.10 45.50 -2 4 0 887.21 41.30 3 -4 0 101.99 8.30 3 -4 0 108.49 6.80 3 -4 0 91.99 8.80 3 -4 0 98.09 6.20 3 -4 0 104.59 6.90 -3 4 0 82.99 6.40 3 4 0 101.49 7.80 -3 4 0 100.69 7.60 -3 4 0 101.09 6.60 -3 4 0 98.09 8.70 3 4 0 103.79 10.50 -3 4 0 89.39 6.30 3 4 0 110.89 7.30 4 -4 0 1698.13 81.39 4 -4 0 1683.53 78.69 4 -4 0 1751.12 76.89 4 -4 0 1602.64 75.39 -4 -4 0 1624.34 75.49 4 -4 0 1515.85 75.89 4 -4 0 1647.44 75.59 -4 4 0 1600.84 77.89 -4 4 0 1742.93 76.19 -4 4 0 1696.73 75.69 4 4 0 1537.95 74.59 4 4 0 1656.73 83.89 -4 4 0 1569.64 75.39 4 4 0 1619.04 76.59 -4 4 0 1807.72 80.49 4 4 0 1635.24 76.89 -5 -4 0 736.13 35.50 5 -4 0 861.91 46.40 5 -4 0 802.12 38.60 -5 -4 0 728.13 35.90 5 -4 0 754.32 44.40 5 -4 0 759.42 35.90 5 -4 0 739.13 36.60 -5 4 0 698.13 35.20 -5 4 0 732.13 38.30 5 4 0 694.33 36.40 5 4 0 746.43 44.80 -5 4 0 786.22 36.30 5 4 0 776.92 36.00 -5 4 0 720.93 35.30 5 4 0 763.72 36.60 -5 4 0 677.73 39.70 5 4 0 693.43 34.10 6 -4 0 435.36 23.30 -6 -4 0 460.65 23.30 -6 -4 0 449.46 26.80 6 -4 0 443.16 23.20 -6 -4 0 471.25 23.10 6 -4 0 464.85 23.80 6 4 0 483.55 23.10 -6 4 0 462.45 27.60 -6 4 0 450.55 23.20 6 4 0 467.95 23.70 -6 4 0 439.06 25.50 6 4 0 493.95 23.70 -7 -4 0 175.38 8.50 -7 -4 0 141.49 8.30 7 4 0 154.38 8.80 7 4 0 130.19 8.80 -7 4 0 152.28 8.60 0 -5 0 0.80 1.50 0 5 0 0.20 1.80 1 -5 0 605.04 30.00 -1 -5 0 657.33 30.90 1 -5 0 650.03 31.90 1 -5 0 654.33 32.40 1 5 0 679.73 35.00 3 -5 0 2026.70 90.39 3 -5 0 1970.40 94.09 3 -5 0 2002.00 89.49 3 -5 0 1961.40 89.69 3 -5 0 1830.02 91.99 3 -5 0 1777.42 89.79 3 5 0 1798.82 90.09 3 5 0 1842.12 98.59 -3 5 0 2025.20 89.89 -3 5 0 2111.09 93.59 -3 5 0 1827.92 89.59 -3 5 0 2181.68 91.09 3 5 0 2052.89 89.69 3 5 0 2037.90 90.39 3 5 0 1831.02 89.69 3 5 0 2076.09 90.79 4 -5 0 245.78 13.30 4 -5 0 262.27 18.90 -4 -5 0 256.47 13.30 4 -5 0 265.97 13.70 4 -5 0 272.67 14.80 -4 5 0 252.67 13.10 4 5 0 229.08 14.30 4 5 0 225.58 14.00 -4 5 0 234.28 17.40 4 5 0 269.67 13.80 4 5 0 256.97 16.00 4 5 0 259.97 20.70 -4 5 0 248.78 14.00 4 5 0 228.58 14.80 5 -5 0 59.79 6.30 5 -5 0 43.80 5.50 5 -5 0 45.00 10.10 5 -5 0 51.19 6.90 5 -5 0 42.80 10.00 -5 -5 0 58.89 5.30 -5 5 0 48.30 6.00 -5 5 0 54.89 8.40 -5 5 0 39.20 5.80 5 5 0 47.60 5.80 5 5 0 53.29 5.40 5 5 0 52.29 10.90 -6 -5 0 1029.70 46.00 6 -5 0 943.51 46.60 6 -5 0 982.00 46.10 6 -5 0 866.61 46.70 -6 -5 0 1032.90 50.29 -6 5 0 927.81 49.80 6 5 0 986.30 45.90 6 5 0 1027.70 46.60 6 5 0 979.30 45.90 -6 5 0 992.60 46.20 -1 -6 0 1860.71 87.19 1 -6 0 1982.00 89.19 1 -6 0 1915.81 88.59 1 -6 0 1893.31 86.19 1 6 0 1909.61 87.19 1 6 0 1698.73 87.19 1 6 0 1921.81 92.39 -1 6 0 2001.70 89.39 2 -6 0 148.29 11.00 2 -6 0 133.19 10.00 2 -6 0 126.39 8.50 2 -6 0 132.19 7.80 -2 6 0 133.79 7.40 2 6 0 150.58 13.30 2 6 0 146.49 9.00 2 6 0 135.49 9.20 -2 6 0 138.99 8.20 -2 6 0 134.39 8.70 2 6 0 121.29 8.90 -2 6 0 132.69 10.20 -2 6 0 126.99 7.90 3 -6 0 773.72 36.10 3 -6 0 817.62 37.30 3 -6 0 732.33 36.60 3 -6 0 726.73 39.10 3 -6 0 793.32 36.40 3 -6 0 736.73 40.90 3 6 0 730.83 37.30 -3 6 0 804.52 36.80 -3 6 0 731.73 36.30 3 6 0 794.32 44.10 3 6 0 741.43 36.90 -3 6 0 744.83 36.20 3 6 0 772.72 36.70 3 6 0 779.32 36.60 3 6 0 713.83 36.00 -3 6 0 731.23 39.90 -3 6 0 771.92 36.50 4 -6 0 4111.69 201.48 4 -6 0 4425.96 204.98 4 -6 0 4441.26 202.48 4 -6 0 4354.66 201.18 4 -6 0 4212.88 200.88 4 -6 0 4340.17 207.78 4 6 0 4458.95 211.88 -4 6 0 4719.03 201.68 4 6 0 4107.69 201.08 4 6 0 4763.52 202.88 4 6 0 4737.83 202.48 4 6 0 4500.25 201.58 4 6 0 4403.96 201.28 -4 6 0 4718.43 206.68 5 -6 0 1959.10 93.69 5 -6 0 1903.01 89.59 -5 -6 0 2060.29 90.29 -5 -6 0 1903.61 90.49 5 -6 0 1894.21 100.09 5 -6 0 2002.10 91.69 5 -6 0 1998.30 90.99 -5 6 0 2028.20 90.89 5 6 0 1804.72 90.29 5 6 0 1949.80 91.39 5 6 0 2166.18 91.79 -5 6 0 1894.11 95.09 5 6 0 2030.50 90.69 6 -6 0 204.38 11.80 -6 -6 0 206.58 11.30 -6 -6 0 200.98 11.20 6 -6 0 199.28 11.30 -6 -6 0 188.28 14.10 -6 6 0 228.48 11.80 6 6 0 208.78 11.70 6 6 0 200.68 11.30 6 6 0 208.58 12.00 0 -7 0 -0.70 1.80 0 -7 0 2.60 2.40 0 7 0 -0.70 2.40 0 7 0 0.80 1.50 0 7 0 1.30 1.90 0 7 0 0.90 2.10 1 -7 0 1214.58 55.29 1 -7 0 1083.29 51.49 -1 -7 0 1118.49 52.89 -1 7 0 1138.69 52.09 1 7 0 1122.29 52.29 -1 7 0 1093.29 54.79 -1 7 0 1152.18 52.29 -1 7 0 1170.78 52.49 1 7 0 1079.49 51.79 -1 7 0 1068.39 51.39 1 7 0 1018.00 52.09 -1 7 0 1192.98 53.09 1 7 0 1072.39 52.19 -2 -7 0 3460.85 160.48 2 -7 0 3543.15 164.58 2 -7 0 3522.55 160.08 2 -7 0 3558.84 160.98 2 -7 0 3386.76 160.28 2 -7 0 3488.35 163.58 -2 7 0 3830.22 166.18 -2 7 0 3467.45 160.18 2 7 0 3728.63 160.78 -2 7 0 3409.56 159.98 -2 7 0 3685.83 160.58 2 7 0 3512.85 160.78 2 7 0 3440.76 159.88 2 7 0 3622.64 161.48 -2 7 0 3366.86 160.08 -2 7 0 3483.45 160.58 2 7 0 3447.95 160.38 2 7 0 3740.53 169.28 3 -7 0 1495.65 74.89 3 -7 0 1546.85 71.39 3 -7 0 1518.75 76.79 -3 7 0 1450.75 71.09 3 7 0 1600.14 72.19 3 7 0 1551.04 71.09 -3 7 0 1555.14 71.39 3 7 0 1595.74 81.19 3 7 0 1663.73 72.89 3 7 0 1441.26 71.09 3 7 0 1441.16 71.39 -3 7 0 1572.54 75.49 -3 7 0 1585.04 71.69 4 -7 0 127.49 12.90 -4 -7 0 147.49 8.90 4 -7 0 159.38 10.80 4 -7 0 163.58 9.30 4 -7 0 146.49 10.00 4 -7 0 150.68 14.20 4 -7 0 155.68 9.40 -4 7 0 152.28 9.20 4 7 0 147.79 9.90 -4 7 0 128.19 12.90 4 7 0 149.19 9.60 4 7 0 150.48 17.80 -4 7 0 133.09 8.30 4 7 0 148.29 10.80 4 7 0 138.69 9.80 5 -7 0 20.10 6.10 5 -7 0 16.20 3.40 5 -7 0 18.20 4.00 5 -7 0 18.50 2.70 -5 -7 0 23.30 3.70 -5 -7 0 23.20 3.20 5 7 0 17.50 3.40 -5 7 0 14.10 6.40 5 7 0 15.10 3.40 5 7 0 19.30 3.40 -5 7 0 21.30 3.80 -5 7 0 18.90 3.40 6 -7 0 806.02 41.20 -6 -7 0 876.21 40.70 -6 -7 0 857.41 40.50 6 7 0 842.22 40.50 6 7 0 936.31 41.30 -6 7 0 926.31 41.00 0 -8 0 213.98 12.30 0 -8 0 223.18 14.50 0 -8 0 214.18 11.80 0 8 0 226.58 12.90 0 8 0 214.88 12.40 0 8 0 230.48 12.80 0 8 0 230.78 13.30 1 -8 0 5.90 3.40 1 -8 0 4.50 3.30 1 -8 0 5.00 2.00 -1 -8 0 4.00 2.50 1 -8 0 10.90 2.60 1 8 0 4.30 3.20 -1 8 0 9.40 4.10 1 8 0 2.50 2.70 1 8 0 7.20 3.40 1 8 0 8.60 2.60 -1 8 0 5.80 2.10 -1 8 0 5.80 2.40 2 -8 0 26.10 4.10 2 -8 0 20.40 5.70 2 -8 0 23.50 5.70 2 -8 0 17.90 3.60 -2 8 0 35.40 6.00 2 8 0 16.60 3.40 2 8 0 33.60 4.40 2 8 0 21.10 4.10 -2 8 0 25.70 3.80 2 8 0 33.00 4.60 -2 8 0 28.80 4.20 2 8 0 23.30 3.70 -2 8 0 26.50 3.90 -2 8 0 31.90 4.50 2 8 0 27.70 4.70 -2 8 0 27.50 3.60 3 -8 0 88.89 10.20 3 -8 0 100.99 7.10 3 -8 0 98.19 8.00 3 -8 0 90.89 7.20 3 -8 0 93.79 11.90 3 8 0 104.49 8.70 3 8 0 103.69 7.90 3 8 0 90.59 14.10 -3 8 0 86.79 7.30 -3 8 0 96.39 6.60 -3 8 0 89.49 10.20 3 8 0 103.49 7.50 3 8 0 99.69 7.80 -3 8 0 90.89 7.30 3 8 0 98.29 7.90 -4 -8 0 203.98 11.40 4 -8 0 223.08 16.60 4 -8 0 220.18 11.80 4 -8 0 215.48 11.90 4 -8 0 212.28 12.80 -4 8 0 203.38 11.90 -4 8 0 170.68 16.00 4 8 0 197.18 11.80 4 8 0 210.18 12.50 4 8 0 196.78 12.70 4 8 0 198.28 12.10 -4 8 0 217.88 12.00 -5 -8 0 -2.30 2.00 5 -8 0 1.20 2.80 5 -8 0 0.60 1.70 -5 8 0 4.80 6.80 -5 8 0 0.20 1.50 -5 8 0 9.70 5.30 5 8 0 1.90 1.80 5 8 0 0.90 1.70 0 -9 0 3.90 3.90 0 -9 0 3.40 3.20 0 9 0 -0.80 2.10 0 9 0 4.20 2.10 0 9 0 2.70 2.00 0 9 0 -0.30 2.90 1 -9 0 156.78 9.00 1 -9 0 137.39 12.20 1 -9 0 150.08 9.80 1 -9 0 143.99 9.60 1 9 0 140.69 9.00 -1 9 0 150.98 9.10 1 9 0 144.19 9.50 -1 9 0 141.59 10.30 1 9 0 148.09 10.10 1 9 0 135.29 9.90 -1 9 0 149.69 9.60 -1 9 0 142.79 9.10 -1 9 0 146.89 8.30 2 -9 0 2711.33 137.09 2 -9 0 2961.40 133.19 2 -9 0 2843.22 132.39 2 -9 0 2997.20 132.29 -2 -9 0 2707.93 131.49 -2 9 0 2754.52 131.99 -2 9 0 3181.78 133.49 -2 9 0 2866.41 132.69 -2 9 0 2983.80 131.79 2 9 0 2784.72 132.39 -2 9 0 2937.01 132.59 2 9 0 3080.39 133.89 2 9 0 3018.00 132.89 2 9 0 2794.12 132.39 3 -9 0 89.19 6.50 3 -9 0 81.19 6.80 3 -9 0 73.49 11.00 3 -9 0 87.59 7.00 3 9 0 85.99 6.60 -3 9 0 84.69 6.70 3 9 0 81.49 7.30 3 9 0 80.59 7.10 -3 9 0 83.09 5.90 -3 9 0 82.39 6.60 -3 9 0 76.19 6.50 4 -9 0 202.48 16.20 4 -9 0 237.48 13.10 4 -9 0 219.48 12.10 -4 9 0 226.78 12.00 4 9 0 220.68 12.80 4 9 0 208.38 11.80 4 9 0 216.28 13.30 -4 9 0 183.28 15.40 5 -9 0 1.10 1.50 5 -9 0 2.90 2.70 -5 9 0 3.20 1.50 5 9 0 4.10 2.30 5 9 0 2.20 1.60 0 -10 0 3073.79 143.29 0 -10 0 2886.41 141.69 0 -10 0 3314.77 140.49 -1 -10 0 853.31 40.20 1 -10 0 844.62 40.40 1 -10 0 815.02 44.90 1 -10 0 838.32 41.00 1 -10 0 819.62 40.60 -1 10 0 900.31 41.80 1 10 0 886.41 42.10 1 10 0 893.71 41.30 1 10 0 854.01 41.10 -1 10 0 839.62 40.80 1 10 0 784.72 40.00 -1 10 0 859.81 41.30 -1 10 0 868.21 40.60 2 -10 0 34.50 4.90 -2 -10 0 36.30 4.20 2 -10 0 50.89 5.30 2 -10 0 40.90 4.00 2 10 0 27.60 4.80 -2 10 0 40.50 4.70 2 10 0 41.50 4.70 -2 10 0 39.70 5.10 2 10 0 26.60 4.20 -2 10 0 37.50 4.00 -2 10 0 37.60 4.70 -2 10 0 39.50 4.00 2 10 0 40.70 5.20 3 -10 0 58.79 5.00 3 -10 0 56.09 5.50 3 -10 0 59.69 5.20 3 10 0 54.99 5.70 -3 10 0 52.49 4.70 -3 10 0 60.49 4.60 -3 10 0 52.99 5.10 3 10 0 54.49 6.40 3 10 0 53.99 5.10 4 -10 0 997.30 46.80 4 -10 0 1041.20 46.90 4 10 0 1056.09 47.80 4 10 0 964.40 46.70 -4 10 0 1032.00 46.60 4 10 0 967.60 47.10 0 -11 0 3.30 2.10 0 -11 0 2.50 3.10 0 11 0 -0.70 2.10 0 11 0 0.10 1.90 0 11 0 -1.60 1.50 0 11 0 -0.30 1.70 1 -11 0 354.76 18.80 1 -11 0 358.66 18.60 -1 -11 0 353.26 18.50 -1 11 0 373.96 19.50 1 11 0 387.16 19.80 1 11 0 389.76 19.40 -1 11 0 350.06 18.50 -1 11 0 368.06 19.10 1 11 0 350.66 19.10 -1 11 0 369.06 18.90 2 -11 0 1241.08 56.99 2 -11 0 1287.07 56.99 -2 -11 0 1117.69 56.19 2 11 0 1304.67 57.29 -2 11 0 1195.48 56.39 -2 11 0 1289.67 57.49 2 11 0 1151.48 57.69 -2 11 0 1231.98 57.09 -2 11 0 1189.68 56.79 3 -11 0 1346.27 62.29 3 -11 0 1466.85 62.59 3 -11 0 1331.67 62.89 -3 11 0 1229.98 62.39 3 11 0 1398.36 62.59 0 -12 0 510.85 25.10 0 -12 0 542.15 25.10 0 12 0 514.45 25.40 0 12 0 530.35 25.40 0 12 0 496.95 25.60 -1 -12 0 168.38 9.70 1 -12 0 192.08 10.30 -1 12 0 183.98 10.30 1 12 0 181.98 10.10 1 12 0 179.68 10.60 1 12 0 172.58 10.30 -1 12 0 177.68 10.10 -1 12 0 175.08 9.70 2 -12 0 21.60 2.90 2 -12 0 24.80 2.80 2 12 0 17.70 2.90 -2 12 0 19.00 2.70 2 12 0 20.10 2.70 -7 0 1 -1.00 2.20 -7 0 1 3.00 4.70 -7 0 1 5.70 1.70 7 0 -1 -1.00 2.10 7 0 -1 2.50 1.30 -6 0 1 1.50 3.10 -6 0 1 5.50 5.60 6 0 -1 1.50 1.70 6 0 -1 8.00 9.20 -6 0 1 -0.80 2.30 6 0 -1 -0.70 1.70 -5 0 1 5.30 2.80 -5 0 1 6.90 3.90 5 0 -1 0.70 1.80 5 0 -1 8.10 5.70 5 0 -1 -1.30 3.90 -5 0 1 0.40 3.60 -5 0 1 0.60 1.80 -4 0 1 0.30 1.60 4 0 -1 -1.30 1.60 -4 0 1 9.50 2.80 4 0 -1 1.80 3.20 4 0 -1 1.90 1.70 4 0 -1 4.00 3.20 4 0 -1 -0.30 3.10 4 0 -1 -0.90 2.30 3 0 -1 1.00 1.60 3 0 -1 1.70 2.60 -3 0 1 -0.30 1.60 3 0 -1 3.10 2.20 -3 0 1 0.60 1.40 2 0 -1 0.30 1.20 2 0 -1 -1.20 1.60 2 0 -1 6.60 2.00 -2 0 1 2.10 1.50 -1 0 1 -0.80 0.80 1 0 -1 2.50 1.20 1 0 -1 0.10 1.00 1 0 -1 0.40 0.90 0 0 -1 2.60 0.60 -1 0 -1 0.40 1.00 1 0 1 1.40 1.10 1 0 1 1.10 0.80 2 0 1 0.20 1.40 2 0 1 2.10 2.30 2 0 1 0.60 1.10 -2 0 -1 1.80 1.50 3 0 1 -0.30 2.60 3 0 1 0.40 1.80 -3 0 -1 4.40 2.30 3 0 1 1.70 1.40 4 0 1 1.10 3.20 4 0 1 1.40 1.60 -4 0 -1 0.90 2.80 -4 0 -1 -1.30 1.90 -4 0 -1 3.00 1.60 4 0 1 2.20 2.80 4 0 1 5.70 2.80 5 0 1 3.00 3.10 -5 0 -1 0.10 2.90 -5 0 -1 2.60 2.10 5 0 1 1.20 1.80 -5 0 -1 1.20 1.80 5 0 1 3.10 3.80 -5 0 -1 1.20 3.50 5 0 1 2.20 4.90 -6 0 -1 1.60 2.40 -6 0 -1 -1.20 2.60 6 0 1 1.80 2.40 -6 0 -1 -4.30 4.80 6 0 1 19.10 10.40 -6 0 -1 0.40 2.00 6 0 1 2.30 1.50 7 0 1 1.70 2.30 -7 0 -1 0.10 1.90 -7 0 -1 1.70 2.20 -7 0 -1 -1.90 2.90 7 0 1 4.80 1.30 7 -1 -1 96.09 7.40 -7 -1 1 123.99 7.30 7 -1 -1 117.69 7.10 -7 -1 1 123.59 7.50 -7 -1 1 105.39 11.10 -7 1 1 119.19 7.20 7 1 -1 111.49 6.80 -7 1 1 116.19 6.80 -7 1 1 121.39 10.40 7 1 -1 114.99 6.60 -6 -1 1 114.39 7.90 -6 -1 1 112.29 10.80 6 -1 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171.98 9.60 -2 6 9 176.28 10.20 2 6 -9 164.18 11.20 2 6 -9 172.88 10.70 -2 6 9 173.38 10.50 -1 -6 9 202.88 17.10 -1 -6 9 212.88 12.20 1 -6 -9 221.28 12.20 1 -6 -9 229.28 15.40 -1 6 9 214.48 13.10 -1 6 9 209.88 12.60 -1 6 9 202.18 12.20 1 6 -9 223.28 11.60 1 6 -9 223.38 13.00 -1 6 9 230.18 14.10 -1 6 9 206.78 12.70 1 6 -9 226.38 13.40 -1 6 9 196.78 10.90 0 -6 9 54.39 5.30 0 -6 9 52.09 5.50 0 -6 -9 45.70 4.50 0 -6 9 56.49 9.00 0 -6 -9 54.89 7.10 0 6 -9 40.30 5.00 0 6 -9 55.79 5.20 0 6 9 45.30 5.60 0 6 -9 36.30 8.60 0 6 9 46.40 4.80 0 6 9 56.89 6.10 0 6 9 51.49 6.50 0 6 9 49.30 7.60 0 6 9 42.30 5.50 0 6 9 49.20 5.30 1 -6 9 213.08 13.30 -1 -6 -9 232.08 12.80 1 -6 9 244.98 13.00 1 -6 9 241.68 19.00 1 -6 9 217.08 15.70 1 -6 9 250.87 13.30 1 6 9 248.38 13.10 -1 6 -9 246.78 17.60 1 6 9 257.27 14.00 -1 6 -9 227.78 14.40 1 6 9 244.58 14.10 1 6 9 246.58 14.00 1 6 9 244.88 14.00 1 6 9 246.28 14.10 1 6 9 204.98 13.50 -1 6 -9 225.38 13.30 2 -6 9 286.77 15.80 2 -6 9 305.57 15.90 2 -6 9 314.67 19.50 2 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5.10 3 -7 -9 38.50 10.60 -3 -7 9 49.40 6.30 -3 -7 9 52.69 5.60 3 -7 -9 42.80 5.00 -3 7 9 45.70 5.60 -3 7 9 43.60 4.10 3 7 -9 41.90 4.40 -3 7 9 49.80 5.50 -3 7 9 42.20 5.00 3 7 -9 44.30 5.00 -3 7 9 47.60 5.40 3 7 -9 40.20 5.10 -2 -7 9 114.19 13.10 -2 -7 9 105.49 7.90 2 -7 -9 94.59 7.70 -2 -7 9 90.99 12.30 2 -7 -9 104.99 7.40 -2 -7 9 116.19 7.70 2 -7 -9 99.19 11.70 -2 -7 9 118.49 10.20 -2 7 9 83.29 7.40 -2 7 9 93.99 7.90 2 7 -9 96.49 8.40 -2 7 9 106.39 7.70 -2 7 9 101.99 7.60 -2 7 9 106.39 6.50 -2 7 9 108.69 7.80 2 7 -9 116.09 8.50 -1 -7 9 945.31 50.69 -1 -7 9 1001.60 47.00 -1 -7 9 935.11 52.69 1 -7 -9 939.41 46.90 1 -7 -9 1014.60 50.29 -1 -7 9 1028.30 46.90 1 -7 -9 1000.40 46.60 -1 7 9 1033.10 47.30 -1 7 9 1050.19 47.70 1 7 -9 1019.60 47.30 -1 7 9 998.30 47.60 -1 7 9 959.60 47.30 1 7 -9 887.41 46.70 -1 7 9 998.90 47.70 -1 7 9 978.80 46.60 0 -7 9 608.74 33.00 0 -7 9 643.54 36.20 0 -7 -9 570.14 32.20 0 -7 9 600.24 29.20 0 -7 9 549.74 30.40 0 -7 9 589.14 29.40 0 -7 -9 604.04 28.80 0 7 -9 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1.70 0 -3 -17 0.00 1.30 0 -3 17 -0.30 1.30 0 3 17 3.40 1.90 0 3 17 3.00 2.40 0 3 17 -0.30 2.00 -1 -3 -17 356.66 16.90 -1 -3 -17 345.67 16.70 1 -3 17 351.46 16.60 1 3 17 302.07 16.10 1 3 17 332.77 16.40 1 3 17 340.37 17.00 1 -4 -17 347.67 17.80 1 -4 -17 372.16 18.00 -1 4 17 390.66 18.30 -1 4 17 350.16 17.80 1 4 -17 374.36 18.00 0 -4 17 670.93 32.10 0 -4 -17 690.93 32.20 0 -4 -17 672.53 32.10 0 4 17 694.33 32.40 0 4 17 713.73 32.00 0 4 17 659.03 31.60 -1 0 18 518.65 24.70 0 0 18 8.00 1.80 0 0 -18 10.20 2.30 0 0 18 8.50 2.00 -1 -1 18 124.49 6.60 1 -1 -18 108.89 6.30 -1 -1 18 120.09 7.60 -1 1 18 112.39 6.90 0 -1 -18 1167.68 50.39 0 1 18 992.10 51.29 0 1 18 1145.29 49.80 0 1 -18 1078.39 49.70 1 -2 -18 270.07 14.90 -1 2 18 311.87 14.20 -1 2 18 317.97 14.80 0 -2 18 89.49 6.30 0 -2 -18 93.09 5.80 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 40161 #============================================================================= # end of cif data for "gil10346" (compound 4e-OH) #============================================================================= #============================================================================= # end of cif file #=============================================================================