#============================================================================== data_global loop_ _journal_name_full 'European Journal of Chemistry' _journal_coden_ASTM EJCUA9 _journal_volume 11 _journal_issue 4 _journal_year 2020 _journal_page_first 261 _journal_page_last 275 #=============================================================================== data_5e _audit_creation_method 'SHELXL-2018/3' _shelx_SHELXL_version_number '2018/3' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H18 Cl F O' _chemical_formula_sum 'C20 H18 Cl F O' _chemical_formula_weight 328.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 6.4900(5) _cell_length_b 18.6070(13) _cell_length_c 14.2146(11) _cell_angle_alpha 90 _cell_angle_beta 102.324(2) _cell_angle_gamma 90 _cell_volume 1677.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3283 _cell_measurement_theta_min 3.131 _cell_measurement_theta_max 26.112 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.309 _exptl_crystal_F_000 688 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.25 _exptl_absorpt_coefficient_mu 0.239 _shelx_estimated_absorpt_T_min 0.954 _shelx_estimated_absorpt_T_max 0.965 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source graphite _diffrn_measurement_device_type Bruker _diffrn_measurement_method SAINT _diffrn_standards_number 3283 _diffrn_standards_interval_count 200 _diffrn_standards_decay_% 0 _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 25575 _diffrn_reflns_av_unetI/netI 0.0307 _diffrn_reflns_av_R_equivalents 0.0494 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.131 _diffrn_reflns_theta_max 26.112 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.988 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.988 _diffrn_reflns_point_group_measured_fraction_full 0.996 _reflns_number_total 3283 _reflns_number_gt 2601 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'APEX (Bruker, 2006)' _computing_cell_refinement 'SAINT (Bruker, 2006)' _computing_data_reduction 'SAINT (Bruker, 2006)' _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2015)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2015)' _computing_molecular_graphics 'PLATON(Spek, 2009)' _computing_publication_material 'PLATON(Spek, 2009)' _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0238P)^2^+6.9520P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_extinction_coef 0.051(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3283 _refine_ls_number_parameters 211 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1060 _refine_ls_R_factor_gt 0.0875 _refine_ls_wR_factor_ref 0.2056 _refine_ls_wR_factor_gt 0.1968 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 1.0556(2) 0.51301(7) 0.65003(10) 0.0573(4) Uani 1 1 d . . . . . F1 F 0.9191(4) 0.30875(16) 0.4220(2) 0.0592(8) Uani 1 1 d . . . . . O1 O 1.0725(7) 0.5541(2) 0.8480(3) 0.0795(13) Uani 1 1 d . . . . . C14 C 0.8268(7) 0.3724(2) 0.5487(3) 0.0402(10) Uani 1 1 d . . . . . H14 H 0.965442 0.368326 0.582892 0.048 Uiso 1 1 calc R U . . . C13 C 0.7674(7) 0.3438(2) 0.4568(3) 0.0411(10) Uani 1 1 d . . . . . C11 C 0.4189(7) 0.3835(3) 0.4434(3) 0.0459(11) Uani 1 1 d . . . . . H11 H 0.281150 0.388613 0.408552 0.055 Uiso 1 1 calc R U . . . C9 C 0.6773(7) 0.4070(2) 0.5892(3) 0.0397(10) Uani 1 1 d . . . . . C12 C 0.5642(7) 0.3479(2) 0.4006(3) 0.0409(10) Uani 1 1 d . . . . . C5 C 0.7291(7) 0.4367(2) 0.6880(3) 0.0400(10) Uani 1 1 d . . . . . C6 C 0.8855(7) 0.4832(3) 0.7207(3) 0.0430(10) Uani 1 1 d . . . . . C10 C 0.4711(7) 0.4114(3) 0.5357(3) 0.0476(11) Uani 1 1 d . . . . . H10 H 0.367762 0.433342 0.562129 0.057 Uiso 1 1 calc R U . . . C1 C 0.9230(8) 0.5161(3) 0.8178(4) 0.0507(12) Uani 1 1 d . . . . . C15 C 0.4977(8) 0.3184(3) 0.3010(3) 0.0467(11) Uani 1 1 d . . . . . C2 C 0.7580(9) 0.5004(3) 0.8747(4) 0.0558(13) Uani 1 1 d . . . . . H2A H 0.643044 0.534351 0.856551 0.067 Uiso 1 1 calc R U . . . H2B H 0.818750 0.507269 0.942640 0.067 Uiso 1 1 calc R U . . . C4 C 0.5828(8) 0.4135(3) 0.7524(3) 0.0518(12) Uani 1 1 d . . . . . H4A H 0.549483 0.363041 0.740660 0.062 Uiso 1 1 calc R U . . . H4B H 0.452052 0.440278 0.734192 0.062 Uiso 1 1 calc R U . . . C3 C 0.6700(8) 0.4240(3) 0.8594(3) 0.0489(12) Uani 1 1 d . . . . . C20 C 0.6284(9) 0.3220(3) 0.2345(4) 0.0577(13) Uani 1 1 d . . . . . H20 H 0.764430 0.340265 0.253176 0.069 Uiso 1 1 calc R U . . . C7 C 0.8466(10) 0.3698(3) 0.8977(4) 0.0688(16) Uani 1 1 d . . . . . H7A H 0.955833 0.374340 0.861936 0.103 Uiso 1 1 calc R U . . . H7B H 0.790305 0.321898 0.890517 0.103 Uiso 1 1 calc R U . . . H7C H 0.904117 0.379185 0.964557 0.103 Uiso 1 1 calc R U . . . C8 C 0.4911(10) 0.4141(4) 0.9138(4) 0.0722(17) Uani 1 1 d . . . . . H8A H 0.545865 0.420122 0.981575 0.108 Uiso 1 1 calc R U . . . H8B H 0.432497 0.366807 0.901714 0.108 Uiso 1 1 calc R U . . . H8C H 0.383196 0.449280 0.891957 0.108 Uiso 1 1 calc R U . . . C16 C 0.2959(9) 0.2907(3) 0.2713(4) 0.0686(17) Uani 1 1 d . . . . . H16 H 0.207318 0.287041 0.314560 0.082 Uiso 1 1 calc R U . . . C19 C 0.5554(12) 0.2985(3) 0.1411(4) 0.0759(18) Uani 1 1 d . . . . . H19 H 0.642984 0.300362 0.097182 0.091 Uiso 1 1 calc R U . . . C18 C 0.3528(13) 0.2723(4) 0.1129(5) 0.089(2) Uani 1 1 d . . . . . H18 H 0.302992 0.257110 0.049841 0.106 Uiso 1 1 calc R U . . . C17 C 0.2271(11) 0.2687(4) 0.1769(5) 0.088(2) Uani 1 1 d . . . . . H17 H 0.090733 0.250891 0.157149 0.106 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0514(7) 0.0565(8) 0.0664(9) -0.0006(6) 0.0177(6) -0.0062(6) F1 0.0429(15) 0.0660(19) 0.069(2) -0.0162(15) 0.0132(14) 0.0066(14) O1 0.088(3) 0.082(3) 0.067(3) -0.022(2) 0.014(2) -0.035(3) C14 0.033(2) 0.041(2) 0.045(2) 0.0026(19) 0.0046(18) 0.0018(18) C13 0.036(2) 0.039(2) 0.049(3) -0.001(2) 0.0124(19) 0.0023(18) C11 0.036(2) 0.052(3) 0.048(3) -0.001(2) 0.0037(19) 0.005(2) C9 0.040(2) 0.041(2) 0.037(2) 0.0026(19) 0.0067(18) 0.0013(19) C12 0.040(2) 0.040(2) 0.044(2) 0.0005(19) 0.0101(19) -0.0024(19) C5 0.038(2) 0.046(2) 0.035(2) 0.0020(19) 0.0078(18) 0.0035(19) C6 0.041(2) 0.046(2) 0.042(2) 0.002(2) 0.0085(19) 0.002(2) C10 0.035(2) 0.057(3) 0.051(3) -0.005(2) 0.010(2) 0.004(2) C1 0.061(3) 0.042(3) 0.046(3) -0.001(2) 0.005(2) -0.003(2) C15 0.049(3) 0.043(3) 0.046(3) -0.004(2) 0.005(2) -0.001(2) C2 0.070(3) 0.053(3) 0.044(3) -0.004(2) 0.011(2) 0.002(3) C4 0.050(3) 0.066(3) 0.039(2) -0.005(2) 0.008(2) -0.010(2) C3 0.054(3) 0.055(3) 0.039(2) -0.002(2) 0.012(2) 0.000(2) C20 0.066(3) 0.056(3) 0.052(3) -0.005(2) 0.013(3) -0.002(3) C7 0.086(4) 0.054(3) 0.061(3) 0.010(3) 0.004(3) 0.010(3) C8 0.078(4) 0.093(5) 0.052(3) -0.005(3) 0.027(3) -0.012(3) C16 0.053(3) 0.082(4) 0.068(4) -0.025(3) 0.004(3) -0.007(3) C19 0.109(5) 0.075(4) 0.046(3) -0.003(3) 0.023(3) 0.018(4) C18 0.113(6) 0.078(5) 0.059(4) -0.023(3) -0.016(4) 0.019(4) C17 0.073(4) 0.101(5) 0.079(5) -0.040(4) -0.010(4) -0.004(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl1 C6 1.735(5) . ? F1 C13 1.359(5) . ? O1 C1 1.203(6) . ? C14 C9 1.389(6) . ? C14 C13 1.387(6) . ? C14 H14 0.9300 . ? C13 C12 1.390(6) . ? C11 C12 1.394(6) . ? C11 C10 1.384(6) . ? C11 H11 0.9300 . ? C9 C10 1.393(6) . ? C9 C5 1.480(6) . ? C12 C15 1.494(6) . ? C5 C6 1.339(6) . ? C5 C4 1.515(6) . ? C6 C1 1.481(6) . ? C10 H10 0.9300 . ? C1 C2 1.503(7) . ? C15 C16 1.387(7) . ? C15 C20 1.400(7) . ? C2 C3 1.529(7) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C4 C3 1.519(6) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C3 C7 1.537(7) . ? C3 C8 1.537(7) . ? C20 C19 1.382(8) . ? C20 H20 0.9300 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C16 C17 1.383(8) . ? C16 H16 0.9300 . ? C19 C18 1.380(10) . ? C19 H19 0.9300 . ? C18 C17 1.347(10) . ? C18 H18 0.9300 . ? C17 H17 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C9 C14 C13 119.4(4) . . ? C9 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? F1 C13 C12 119.3(4) . . ? F1 C13 C14 116.7(4) . . ? C12 C13 C14 124.0(4) . . ? C12 C11 C10 122.7(4) . . ? C12 C11 H11 118.6 . . ? C10 C11 H11 118.6 . . ? C14 C9 C10 118.4(4) . . ? C14 C9 C5 122.0(4) . . ? C10 C9 C5 119.6(4) . . ? C11 C12 C13 115.0(4) . . ? C11 C12 C15 120.2(4) . . ? C13 C12 C15 124.8(4) . . ? C6 C5 C9 125.0(4) . . ? C6 C5 C4 120.1(4) . . ? C9 C5 C4 114.9(4) . . ? C5 C6 C1 123.5(4) . . ? C5 C6 Cl1 122.2(4) . . ? C1 C6 Cl1 114.2(3) . . ? C11 C10 C9 120.5(4) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? O1 C1 C2 122.4(5) . . ? O1 C1 C6 122.3(5) . . ? C2 C1 C6 115.3(4) . . ? C16 C15 C20 118.8(5) . . ? C16 C15 C12 119.2(5) . . ? C20 C15 C12 121.9(4) . . ? C1 C2 C3 113.1(4) . . ? C1 C2 H2A 109.0 . . ? C3 C2 H2A 109.0 . . ? C1 C2 H2B 109.0 . . ? C3 C2 H2B 109.0 . . ? H2A C2 H2B 107.8 . . ? C5 C4 C3 114.9(4) . . ? C5 C4 H4A 108.6 . . ? C3 C4 H4A 108.6 . . ? C5 C4 H4B 108.6 . . ? C3 C4 H4B 108.6 . . ? H4A C4 H4B 107.5 . . ? C2 C3 C4 108.1(4) . . ? C2 C3 C7 109.4(4) . . ? C4 C3 C7 111.1(4) . . ? C2 C3 C8 109.8(4) . . ? C4 C3 C8 109.2(4) . . ? C7 C3 C8 109.2(5) . . ? C19 C20 C15 120.0(6) . . ? C19 C20 H20 120.0 . . ? C15 C20 H20 120.0 . . ? C3 C7 H7A 109.5 . . ? C3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C15 C16 C17 119.6(6) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C20 C19 C18 120.0(6) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C17 C18 C19 120.0(6) . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C18 C17 C16 121.6(7) . . ? C18 C17 H17 119.2 . . ? C16 C17 H17 119.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C9 C14 C13 F1 -178.2(4) . . . . ? C9 C14 C13 C12 0.5(7) . . . . ? C13 C14 C9 C10 0.4(7) . . . . ? C13 C14 C9 C5 178.1(4) . . . . ? C10 C11 C12 C13 -1.2(7) . . . . ? C10 C11 C12 C15 179.5(5) . . . . ? F1 C13 C12 C11 178.6(4) . . . . ? C14 C13 C12 C11 -0.1(7) . . . . ? F1 C13 C12 C15 -2.2(7) . . . . ? C14 C13 C12 C15 179.1(4) . . . . ? C14 C9 C5 C6 54.5(7) . . . . ? C10 C9 C5 C6 -127.8(5) . . . . ? C14 C9 C5 C4 -128.4(5) . . . . ? C10 C9 C5 C4 49.3(6) . . . . ? C9 C5 C6 C1 175.2(4) . . . . ? C4 C5 C6 C1 -1.8(7) . . . . ? C9 C5 C6 Cl1 -2.0(7) . . . . ? C4 C5 C6 Cl1 -178.9(4) . . . . ? C12 C11 C10 C9 2.2(8) . . . . ? C14 C9 C10 C11 -1.7(7) . . . . ? C5 C9 C10 C11 -179.5(4) . . . . ? C5 C6 C1 O1 175.0(5) . . . . ? Cl1 C6 C1 O1 -7.6(7) . . . . ? C5 C6 C1 C2 -6.6(7) . . . . ? Cl1 C6 C1 C2 170.8(4) . . . . ? C11 C12 C15 C16 -34.8(7) . . . . ? C13 C12 C15 C16 146.0(5) . . . . ? C11 C12 C15 C20 141.0(5) . . . . ? C13 C12 C15 C20 -38.2(7) . . . . ? O1 C1 C2 C3 -144.8(5) . . . . ? C6 C1 C2 C3 36.8(6) . . . . ? C6 C5 C4 C3 -20.7(7) . . . . ? C9 C5 C4 C3 162.0(4) . . . . ? C1 C2 C3 C4 -56.7(6) . . . . ? C1 C2 C3 C7 64.4(6) . . . . ? C1 C2 C3 C8 -175.7(4) . . . . ? C5 C4 C3 C2 48.4(6) . . . . ? C5 C4 C3 C7 -71.6(6) . . . . ? C5 C4 C3 C8 167.8(5) . . . . ? C16 C15 C20 C19 0.2(8) . . . . ? C12 C15 C20 C19 -175.6(5) . . . . ? C20 C15 C16 C17 -1.1(9) . . . . ? C12 C15 C16 C17 174.8(6) . . . . ? C15 C20 C19 C18 0.8(9) . . . . ? C20 C19 C18 C17 -0.9(10) . . . . ? C19 C18 C17 C16 0.0(12) . . . . ? C15 C16 C17 C18 1.0(11) . . . . ? _refine_diff_density_max 0.292 _refine_diff_density_min -0.367 _refine_diff_density_rms 0.073 _shelx_res_file ; TITL d3_a.res in P2(1)/c 5e.res created by SHELXL-2018/3 at 18:01:14 on 12-Aug-2020 CELL 0.71073 6.4900 18.6070 14.2146 90.000 102.324 90.000 ZERR 4.00 0.0005 0.0013 0.0011 0.000 0.002 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H O CL F UNIT 80 72 8 4 1 MERG 2 FMAP 2 PLAN 20 SIZE 0.15 0.20 0.20 ACTA BOND $H OMIT 0 0 -2 OMIT 0 0 2 HTAB ACTA CONF L.S. 10 TEMP 23.00 WGHT 0.023800 6.952000 EXTI 0.051266 FVAR 1.08367 CL1 4 1.055556 0.513006 0.650027 11.00000 0.05138 0.05650 = 0.06641 -0.00061 0.01765 -0.00616 F1 5 0.919085 0.308746 0.422041 11.00000 0.04288 0.06596 = 0.06941 -0.01615 0.01323 0.00661 O1 3 1.072489 0.554093 0.848004 11.00000 0.08770 0.08247 = 0.06721 -0.02225 0.01377 -0.03486 C14 1 0.826779 0.372355 0.548711 11.00000 0.03284 0.04145 = 0.04471 0.00257 0.00464 0.00181 AFIX 43 H14 2 0.965442 0.368326 0.582892 11.00000 -1.20000 AFIX 0 C13 1 0.767372 0.343776 0.456797 11.00000 0.03637 0.03886 = 0.04942 -0.00122 0.01239 0.00233 C11 1 0.418902 0.383466 0.443417 11.00000 0.03560 0.05190 = 0.04776 -0.00082 0.00368 0.00527 AFIX 43 H11 2 0.281150 0.388613 0.408552 11.00000 -1.20000 AFIX 0 C9 1 0.677256 0.407045 0.589225 11.00000 0.04036 0.04084 = 0.03726 0.00260 0.00674 0.00132 C12 1 0.564225 0.347898 0.400587 11.00000 0.03981 0.03972 = 0.04376 0.00047 0.01011 -0.00241 C5 1 0.729138 0.436748 0.688014 11.00000 0.03831 0.04612 = 0.03541 0.00197 0.00784 0.00346 C6 1 0.885520 0.483247 0.720747 11.00000 0.04086 0.04553 = 0.04248 0.00218 0.00849 0.00190 C10 1 0.471099 0.411441 0.535676 11.00000 0.03541 0.05708 = 0.05094 -0.00462 0.01039 0.00443 AFIX 43 H10 2 0.367762 0.433342 0.562129 11.00000 -1.20000 AFIX 0 C1 1 0.922989 0.516103 0.817776 11.00000 0.06091 0.04164 = 0.04633 -0.00129 0.00454 -0.00295 C15 1 0.497706 0.318382 0.301008 11.00000 0.04909 0.04254 = 0.04608 -0.00382 0.00452 -0.00125 C2 1 0.757976 0.500362 0.874750 11.00000 0.07018 0.05321 = 0.04350 -0.00420 0.01077 0.00199 AFIX 23 H2A 2 0.643044 0.534351 0.856551 11.00000 -1.20000 H2B 2 0.818750 0.507269 0.942640 11.00000 -1.20000 AFIX 0 C4 1 0.582768 0.413512 0.752352 11.00000 0.04990 0.06636 = 0.03863 -0.00454 0.00841 -0.01035 AFIX 23 H4A 2 0.549483 0.363041 0.740660 11.00000 -1.20000 H4B 2 0.452052 0.440278 0.734192 11.00000 -1.20000 AFIX 0 C3 1 0.669987 0.424033 0.859418 11.00000 0.05410 0.05459 = 0.03886 -0.00229 0.01152 0.00017 C20 1 0.628421 0.322018 0.234491 11.00000 0.06571 0.05580 = 0.05192 -0.00456 0.01319 -0.00235 AFIX 43 H20 2 0.764430 0.340265 0.253176 11.00000 -1.20000 AFIX 0 C7 1 0.846649 0.369769 0.897702 11.00000 0.08587 0.05420 = 0.06110 0.00986 0.00410 0.01018 AFIX 137 H7A 2 0.955833 0.374340 0.861936 11.00000 -1.50000 H7B 2 0.790305 0.321898 0.890517 11.00000 -1.50000 H7C 2 0.904117 0.379185 0.964557 11.00000 -1.50000 AFIX 0 C8 1 0.491103 0.414132 0.913765 11.00000 0.07773 0.09266 = 0.05199 -0.00516 0.02682 -0.01204 AFIX 137 H8A 2 0.545865 0.420122 0.981575 11.00000 -1.50000 H8B 2 0.432497 0.366807 0.901714 11.00000 -1.50000 H8C 2 0.383196 0.449280 0.891957 11.00000 -1.50000 AFIX 0 C16 1 0.295895 0.290725 0.271267 11.00000 0.05254 0.08164 = 0.06786 -0.02527 0.00425 -0.00664 AFIX 43 H16 2 0.207318 0.287041 0.314560 11.00000 -1.20000 AFIX 0 C19 1 0.555439 0.298505 0.141089 11.00000 0.10870 0.07542 = 0.04626 -0.00253 0.02258 0.01822 AFIX 43 H19 2 0.642984 0.300362 0.097182 11.00000 -1.20000 AFIX 0 C18 1 0.352760 0.272277 0.112945 11.00000 0.11285 0.07814 = 0.05942 -0.02342 -0.01649 0.01891 AFIX 43 H18 2 0.302992 0.257110 0.049841 11.00000 -1.20000 AFIX 0 C17 1 0.227061 0.268656 0.176912 11.00000 0.07308 0.10054 = 0.07892 -0.04023 -0.01034 -0.00423 AFIX 43 H17 2 0.090733 0.250891 0.157149 11.00000 -1.20000 AFIX 0 HKLF 4 REM d3_a.res in P2(1)/c REM wR2 = 0.2056, GooF = S = 1.055, Restrained GooF = 1.055 for all data REM R1 = 0.0875 for 2601 Fo > 4sig(Fo) and 0.1060 for all 3283 data REM 211 parameters refined using 0 restraints END WGHT 0.0377 5.1453 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 0.292, deepest hole -0.367, 1-sigma level 0.073 Q1 1 1.0989 0.5411 0.7484 11.00000 0.05 0.29 Q2 1 0.9756 0.5776 0.7939 11.00000 0.05 0.28 Q3 1 1.0017 0.4871 0.5588 11.00000 0.05 0.28 Q4 1 0.1874 0.5052 0.4917 11.00000 0.05 0.27 Q5 1 1.0168 0.3417 0.7148 11.00000 0.05 0.26 Q6 1 0.1727 0.4605 0.5372 11.00000 0.05 0.25 Q7 1 0.7784 0.3114 0.1007 11.00000 0.05 0.25 Q8 1 1.2033 0.5122 0.6828 11.00000 0.05 0.25 Q9 1 0.9930 0.4466 0.6615 11.00000 0.05 0.25 Q10 1 0.8176 0.3290 0.7250 11.00000 0.05 0.25 Q11 1 1.2257 0.5504 0.6925 11.00000 0.05 0.24 Q12 1 0.3285 0.3851 0.6032 11.00000 0.05 0.23 Q13 1 0.0812 0.2805 0.1117 11.00000 0.05 0.23 Q14 1 0.4628 0.2566 0.1193 11.00000 0.05 0.23 Q15 1 0.6084 0.4108 0.8967 11.00000 0.05 0.23 Q16 1 0.1800 0.2546 0.3431 11.00000 0.05 0.23 Q17 1 0.3311 0.2443 0.1576 11.00000 0.05 0.22 Q18 1 1.1600 0.4142 0.5988 11.00000 0.05 0.22 Q19 1 0.7367 0.4101 0.2199 11.00000 0.05 0.22 Q20 1 1.1572 0.5125 0.8207 11.00000 0.05 0.22 ; _shelx_res_checksum 5246 _shelx_hkl_file ; 1 0 0 370.96 16.80 2 0 0 2529.55 114.69 -2 0 0 2651.63 114.29 2 0 0 2542.35 112.99 2 0 0 2582.24 114.09 2 0 0 2593.54 114.79 -2 0 0 2575.44 113.09 2 0 0 2645.84 113.59 -3 0 0 -6.80 5.60 3 0 0 -1.70 1.50 3 0 0 4.20 2.70 3 0 0 -1.50 2.40 3 0 0 -1.30 6.30 3 0 0 -0.40 4.30 4 0 0 18.80 3.00 4 0 0 18.40 5.20 -4 0 0 32.80 8.70 4 0 0 28.60 9.30 4 0 0 20.30 6.20 5 0 0 516.65 26.90 5 0 0 453.25 30.30 5 0 0 448.56 26.20 5 0 0 470.35 22.80 5 0 0 479.15 23.20 5 0 0 481.75 25.30 6 0 0 295.17 16.80 6 0 0 343.87 20.40 6 0 0 316.57 27.50 6 0 0 290.67 20.50 6 0 0 310.17 16.40 6 0 0 367.26 24.60 7 0 0 68.39 16.10 7 0 0 74.19 8.40 7 0 0 90.49 9.20 1 -1 0 1465.55 72.09 1 -1 0 1822.12 71.69 1 1 0 1748.33 71.69 1 1 0 1516.35 72.09 2 -1 0 1133.79 51.39 2 -1 0 1120.69 50.09 -2 -1 0 1141.29 50.99 -2 -1 0 1114.89 50.59 2 -1 0 1107.49 51.99 -2 1 0 1148.19 51.69 2 1 0 1129.69 50.69 2 1 0 1104.69 49.90 2 1 0 1131.89 50.69 -2 1 0 1117.69 50.29 2 1 0 1149.58 51.69 3 -1 0 1563.84 75.39 3 -1 0 1628.54 74.49 3 -1 0 1640.64 75.39 3 -1 0 1627.44 73.29 3 -1 0 1612.14 72.59 -3 -1 0 1668.43 74.39 3 1 0 1637.84 73.59 -3 1 0 1697.73 72.99 3 1 0 1583.64 75.29 3 1 0 1617.04 72.39 3 1 0 1640.34 73.89 3 1 0 1673.13 75.29 -3 1 0 1678.73 75.09 4 -1 0 12.90 3.10 4 -1 0 17.20 3.20 4 -1 0 17.60 5.90 4 -1 0 25.00 5.60 4 -1 0 9.00 7.70 -4 -1 0 17.50 7.40 4 -1 0 14.20 2.40 -4 1 0 11.10 7.60 4 1 0 8.50 9.00 4 1 0 22.20 4.70 -4 1 0 20.00 4.90 4 1 0 20.40 5.60 4 1 0 13.90 5.80 5 -1 0 40.30 4.90 5 -1 0 48.60 14.10 5 -1 0 45.50 4.70 5 1 0 55.09 7.70 5 1 0 52.49 15.40 5 1 0 37.10 4.70 6 -1 0 39.00 10.80 6 -1 0 50.19 6.60 6 -1 0 29.70 15.00 6 1 0 45.10 7.30 6 1 0 67.99 19.60 6 1 0 27.90 6.20 7 -1 0 63.99 15.80 7 -1 0 78.99 23.10 7 -1 0 19.10 8.40 7 -1 0 37.70 8.60 7 1 0 31.30 16.60 7 1 0 14.70 11.70 -1 -2 0 4853.51 210.88 -2 -2 0 2254.57 99.59 -2 -2 0 2262.37 99.29 2 -2 0 2237.48 100.39 2 -2 0 2198.58 100.69 -2 -2 0 2285.67 100.59 2 -2 0 2191.48 98.99 2 2 0 2248.38 99.19 -2 2 0 2336.27 100.69 -2 2 0 2294.07 99.29 2 2 0 2270.67 99.69 2 2 0 2244.68 100.29 3 -2 0 304.57 16.80 -3 -2 0 331.67 17.70 3 -2 0 313.47 17.40 3 -2 0 300.97 14.70 3 -2 0 316.37 20.10 -3 -2 0 337.87 16.40 3 -2 0 305.97 15.50 3 2 0 320.17 17.50 3 2 0 321.27 16.20 -3 2 0 326.07 19.40 3 2 0 304.17 17.40 3 2 0 294.07 15.10 -3 2 0 298.07 16.80 4 -2 0 11.20 4.00 4 -2 0 3.70 4.90 4 -2 0 3.10 8.30 -4 2 0 10.10 7.40 -4 2 0 2.30 4.30 4 2 0 4.90 7.60 4 2 0 18.20 4.20 5 -2 0 135.49 11.90 5 -2 0 154.08 8.50 5 -2 0 153.38 10.90 5 -2 0 111.49 12.10 5 -2 0 124.69 17.20 5 2 0 152.78 9.40 5 2 0 147.09 10.00 5 2 0 121.19 21.60 5 2 0 119.29 8.20 -5 2 0 106.39 11.50 5 2 0 107.89 13.50 5 2 0 146.69 10.90 6 -2 0 58.29 10.90 6 -2 0 58.39 11.80 6 2 0 48.20 12.20 6 2 0 54.09 11.00 6 2 0 59.89 6.40 7 -2 0 29.10 12.10 7 -2 0 35.30 8.60 7 -2 0 6.20 8.20 7 -2 0 7.80 9.50 7 -2 0 54.49 19.10 7 2 0 13.60 8.60 7 2 0 4.20 5.30 7 2 0 19.60 11.10 7 2 0 40.40 18.10 7 2 0 19.60 9.70 7 2 0 16.70 5.90 0 -3 0 0.90 1.50 0 -3 0 -0.50 1.60 0 -3 0 -2.00 1.70 0 3 0 2.60 2.60 0 3 0 3.80 1.80 0 3 0 0.20 2.00 -2 -3 0 37.20 4.40 2 -3 0 46.10 5.60 -2 -3 0 39.80 7.30 2 -3 0 51.39 4.10 -2 -3 0 36.90 5.20 -2 3 0 52.29 8.40 2 3 0 42.10 3.50 -2 3 0 32.20 6.30 2 3 0 42.20 4.00 2 3 0 31.10 5.80 3 -3 0 452.05 26.30 -3 -3 0 481.55 23.20 3 -3 0 467.05 22.40 -3 -3 0 465.65 25.60 3 -3 0 487.85 24.40 3 3 0 461.85 23.90 3 3 0 451.25 23.90 3 3 0 432.36 21.60 -3 3 0 493.35 26.10 3 3 0 455.95 22.40 -3 3 0 464.75 23.50 4 -3 0 581.44 33.20 4 -3 0 606.84 28.50 4 -3 0 599.54 29.70 4 -3 0 598.74 30.70 -4 -3 0 589.04 29.70 4 3 0 635.44 31.20 -4 3 0 610.24 33.10 4 3 0 598.14 29.20 -4 3 0 615.94 30.00 4 3 0 585.74 28.00 4 3 0 619.24 30.80 4 3 0 577.34 32.60 5 -3 0 19.60 4.70 5 -3 0 31.50 7.50 5 -3 0 45.50 13.70 -5 3 0 25.50 21.60 5 3 0 32.80 4.50 5 3 0 20.10 8.60 -5 3 0 44.90 9.00 6 -3 0 9.90 6.90 6 -3 0 19.80 7.70 6 -3 0 13.60 8.30 6 3 0 8.90 4.50 6 3 0 19.10 9.00 6 3 0 32.50 10.70 6 3 0 31.20 14.00 6 3 0 14.70 4.00 7 -3 0 44.60 11.60 7 -3 0 53.69 9.30 7 -3 0 81.19 16.60 7 3 0 28.20 10.10 7 3 0 54.39 15.00 0 -4 0 176.78 10.40 0 -4 0 165.78 9.80 0 -4 0 174.88 9.20 0 4 0 165.88 10.20 0 4 0 171.38 9.50 0 4 0 179.38 8.90 -2 -4 0 9.20 3.90 2 -4 0 2.80 3.20 -2 -4 0 5.60 2.40 2 -4 0 0.90 2.60 2 -4 0 8.30 6.50 2 4 0 7.40 4.60 -2 4 0 4.10 4.00 -2 4 0 10.80 6.90 -2 4 0 2.10 4.40 2 4 0 7.50 2.50 3 -4 0 1188.58 56.09 -3 -4 0 1247.08 58.69 -3 -4 0 1280.87 57.09 3 -4 0 1248.58 58.39 3 -4 0 1214.68 59.29 -3 4 0 1285.67 59.19 3 4 0 1236.38 55.79 -3 4 0 1240.08 56.89 3 4 0 1231.48 57.69 3 4 0 1240.68 57.49 -4 -4 0 44.80 5.20 4 -4 0 49.40 11.60 4 4 0 37.40 8.90 4 4 0 28.30 3.50 4 4 0 39.20 11.50 -4 4 0 36.00 8.40 4 4 0 36.80 4.20 -4 4 0 44.80 11.90 5 -4 0 315.67 19.40 5 -4 0 315.17 16.20 5 -4 0 296.57 18.50 5 -4 0 280.87 23.80 -5 4 0 244.18 23.30 5 4 0 286.67 20.70 5 4 0 328.47 18.60 5 4 0 314.97 15.40 -5 4 0 321.37 18.60 5 4 0 252.37 32.30 5 4 0 316.37 17.10 6 -4 0 154.38 14.50 6 -4 0 185.58 14.40 6 -4 0 155.58 15.50 6 -4 0 189.68 11.30 6 4 0 167.98 23.20 6 4 0 167.88 14.10 6 4 0 205.28 12.80 6 4 0 155.38 10.40 6 4 0 170.88 18.10 -6 4 0 182.18 14.90 6 4 0 199.08 13.10 7 -4 0 166.28 18.10 7 -4 0 168.58 11.70 7 -4 0 136.39 14.00 7 4 0 158.18 28.50 7 4 0 130.29 10.20 7 4 0 126.59 17.20 7 4 0 147.39 17.00 7 4 0 155.98 16.30 0 -5 0 -3.70 3.00 0 -5 0 -0.10 2.80 0 -5 0 0.90 3.00 0 5 0 2.60 2.70 0 5 0 2.00 4.00 0 5 0 -4.80 4.10 1 -5 0 2012.90 89.49 1 -5 0 1993.60 89.09 -1 -5 0 1943.51 89.29 1 -5 0 2119.09 89.49 -1 -5 0 2013.10 89.29 -1 5 0 2002.70 89.29 -1 5 0 2048.50 89.19 -1 5 0 2042.20 89.79 1 5 0 1912.81 88.99 2 -5 0 26.30 4.60 -2 -5 0 39.40 4.60 2 -5 0 33.90 5.30 -2 -5 0 41.00 8.00 2 -5 0 32.00 9.00 -2 5 0 28.10 7.40 2 5 0 36.70 7.20 -2 5 0 30.10 9.20 2 5 0 43.10 4.20 3 -5 0 182.68 12.30 3 -5 0 166.98 15.40 -3 -5 0 196.88 11.10 -3 -5 0 179.18 14.40 3 -5 0 176.98 10.30 3 5 0 169.58 10.80 3 5 0 169.08 13.20 3 5 0 180.98 9.50 -3 5 0 180.68 13.00 -3 5 0 174.08 15.20 -4 -5 0 908.61 46.30 -4 -5 0 930.31 43.80 4 -5 0 905.01 44.90 4 -5 0 894.21 47.00 4 -5 0 903.51 42.60 4 5 0 920.71 44.60 4 5 0 910.41 42.20 4 5 0 898.11 41.70 -4 5 0 958.40 44.10 4 5 0 896.31 44.80 -4 5 0 925.61 47.30 -5 -5 0 24.40 6.90 5 -5 0 26.70 7.60 5 -5 0 39.90 8.50 5 -5 0 27.00 11.90 5 5 0 26.80 4.80 -5 5 0 35.40 9.10 5 5 0 16.20 9.20 5 5 0 39.90 6.30 5 5 0 31.70 15.20 6 -5 0 63.49 12.00 -6 5 0 62.29 11.10 6 5 0 49.90 12.70 6 5 0 41.40 10.80 6 5 0 43.10 6.20 6 5 0 33.50 9.80 6 5 0 67.39 20.50 7 -5 0 46.10 11.20 7 5 0 64.09 15.50 7 5 0 15.10 11.10 7 5 0 31.70 7.90 7 5 0 32.20 10.90 7 5 0 77.19 24.90 0 -6 0 1802.42 79.69 0 -6 0 1744.93 80.09 0 -6 0 1851.51 79.19 0 6 0 1814.12 79.19 0 6 0 1798.32 79.89 0 6 0 1725.43 78.59 -1 -6 0 8389.86 355.16 1 -6 0 8283.47 355.16 1 -6 0 8228.78 354.96 -1 -6 0 7944.60 354.96 1 6 0 7770.92 354.76 -1 6 0 8342.96 355.26 -1 6 0 8187.68 354.96 -1 6 0 8269.87 354.66 1 6 0 8019.10 354.36 -2 -6 0 860.11 39.20 2 -6 0 795.72 38.60 2 -6 0 850.11 40.50 -2 -6 0 824.12 39.70 2 -6 0 812.22 39.70 2 6 0 807.92 39.70 2 6 0 838.82 39.10 -2 6 0 799.52 39.50 -2 6 0 838.52 39.50 -2 6 0 826.22 40.50 3 -6 0 182.78 16.70 3 -6 0 198.28 11.00 3 -6 0 209.58 13.00 -3 -6 0 192.88 15.10 -3 -6 0 191.98 11.80 3 6 0 171.58 9.50 3 6 0 202.78 11.40 -3 6 0 194.48 16.50 -3 6 0 184.48 13.90 3 6 0 188.38 14.10 4 -6 0 41.90 13.00 4 -6 0 49.10 5.40 -4 -6 0 36.90 5.60 4 6 0 38.40 10.70 5 -6 0 27.30 12.50 5 -6 0 31.90 8.80 -5 6 0 -4.80 11.00 -5 6 0 15.10 6.60 5 6 0 14.30 13.80 5 6 0 10.80 8.70 5 6 0 17.10 4.60 5 6 0 12.60 4.40 6 -6 0 249.68 19.10 6 -6 0 287.17 18.30 6 -6 0 260.27 18.20 6 -6 0 312.77 16.10 6 6 0 284.97 16.20 6 6 0 241.68 22.80 6 6 0 267.67 18.40 6 6 0 264.07 26.60 -6 6 0 300.27 19.50 6 6 0 285.27 14.60 6 6 0 263.77 21.30 7 -6 0 131.89 13.20 7 -6 0 110.29 12.80 7 -6 0 106.29 18.50 7 6 0 134.49 14.30 7 6 0 107.59 16.60 -7 6 0 118.19 14.20 7 6 0 109.69 9.40 7 6 0 104.29 18.10 0 -7 0 -0.50 3.70 0 -7 0 -3.80 2.30 0 7 0 -6.70 4.30 0 7 0 3.80 2.40 1 -7 0 1805.52 80.99 1 -7 0 1825.02 81.19 -1 -7 0 1715.43 78.69 -1 -7 0 1868.91 81.39 1 -7 0 1873.81 81.49 -1 -7 0 1756.12 81.39 -1 7 0 1839.62 80.79 1 7 0 1766.82 80.79 1 7 0 1745.93 80.99 -1 7 0 1835.02 81.69 -1 7 0 1850.61 81.49 -2 -7 0 138.39 11.60 -2 -7 0 140.59 9.10 2 -7 0 135.09 8.90 2 -7 0 122.79 9.60 -2 7 0 106.99 9.40 -2 7 0 129.69 12.80 -2 7 0 109.09 11.90 3 -7 0 1362.76 64.09 3 -7 0 1313.07 62.89 3 -7 0 1320.57 61.39 -3 -7 0 1315.47 63.09 -3 -7 0 1370.36 62.19 -3 7 0 1349.96 62.19 3 7 0 1359.06 62.29 3 7 0 1267.87 58.59 -3 7 0 1373.56 64.39 3 7 0 1336.67 62.79 4 -7 0 115.09 15.70 4 -7 0 109.19 9.10 -4 -7 0 90.69 8.30 4 -7 0 101.79 8.00 -4 -7 0 109.29 13.80 -4 7 0 91.59 15.20 -4 7 0 100.19 11.80 4 7 0 112.09 8.80 4 7 0 94.99 13.00 4 7 0 94.29 6.20 -5 -7 0 606.74 31.20 5 -7 0 636.34 30.20 5 -7 0 599.54 32.10 5 -7 0 629.94 38.00 5 7 0 670.63 32.40 5 7 0 590.64 28.90 5 7 0 644.34 37.90 5 7 0 576.14 28.90 -5 7 0 609.64 32.50 5 7 0 591.54 36.30 -5 7 0 580.24 37.60 6 -7 0 45.20 9.60 6 -7 0 25.70 7.60 6 -7 0 36.10 10.10 6 -7 0 6.50 13.90 6 7 0 28.20 8.60 6 7 0 27.50 10.60 6 7 0 55.59 12.20 -6 7 0 43.30 11.50 6 7 0 45.40 6.90 7 -7 0 85.99 37.50 7 -7 0 12.60 9.20 7 -7 0 35.60 13.60 7 -7 0 21.30 8.10 7 7 0 12.90 6.20 7 7 0 26.10 10.10 -7 7 0 7.80 9.00 7 7 0 -1.50 11.60 7 7 0 19.30 17.50 7 7 0 -2.50 8.30 7 7 0 16.20 10.10 0 -8 0 51.59 4.60 0 -8 0 68.29 9.40 0 8 0 42.00 7.30 0 8 0 57.89 4.50 0 8 0 49.00 8.30 1 -8 0 3156.78 143.19 -1 -8 0 3167.78 144.09 1 -8 0 3302.37 143.99 -1 -8 0 3173.88 141.19 -1 -8 0 3404.26 144.19 1 -8 0 3312.77 143.89 -1 8 0 3335.37 144.09 -1 8 0 3331.47 143.29 -1 8 0 3310.97 144.19 1 8 0 3210.58 143.49 1 8 0 3059.39 143.69 -2 -8 0 137.39 9.60 2 -8 0 121.69 10.10 2 -8 0 127.99 9.50 2 -8 0 111.79 12.70 -2 -8 0 129.49 11.60 -2 8 0 115.99 13.10 -2 8 0 132.99 9.20 -2 8 0 115.49 12.30 -3 -8 0 123.19 13.00 3 -8 0 127.29 9.30 3 -8 0 134.49 9.80 3 -8 0 118.29 14.30 -3 -8 0 139.49 9.80 -3 8 0 127.99 14.40 -3 8 0 129.49 12.40 3 8 0 119.99 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'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 95120