####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_eds_071903_0m _database_code_depnum_ccdc_archive 'CCDC 1978089' loop_ _audit_author_name _audit_author_address 'Eric Sylvester' ;University at Buffalo United States of America ; _audit_update_record ; 2020-01-15 deposited with the CCDC. 2020-12-07 downloaded from the CCDC. ; _audit_creation_date 2019-07-25 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number 2016/6 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C23 H18 Cl2 O2' _chemical_formula_sum 'C23 H18 Cl2 O2' _chemical_formula_weight 397.27 _chemical_absolute_configuration ad _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_H-M_alt 'P 21 21 21' _space_group_name_Hall 'P 2ac 2ab' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 5.4867(5) _cell_length_b 12.1391(11) _cell_length_c 28.047(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1868.0(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 6905 _cell_measurement_temperature 90 _cell_measurement_theta_max 26.266 _cell_measurement_theta_min 2.750 _shelx_estimated_absorpt_T_max 0.996 _shelx_estimated_absorpt_T_min 0.931 _exptl_absorpt_coefficient_mu 0.363 _exptl_absorpt_correction_T_max 0.7138 _exptl_absorpt_correction_T_min 0.6053 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1111 before and 0.0614 after correction. The Ratio of minimum to maximum transmission is 0.8480. The \l/2 correction factor is Not present.' _exptl_absorpt_special_details ? _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.413 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description prism _exptl_crystal_F_000 824 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0573 _diffrn_reflns_av_unetI/netI 0.0421 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_number 19753 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.387 _diffrn_reflns_theta_min 1.828 _diffrn_ambient_temperature 90 _diffrn_detector 'Bruker APEX2 area detector' _diffrn_detector_area_resol_mean 7.9 _diffrn_detector_type 'CCD area detector' _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker SMART APEX2 area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator 'mirror optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'microfocus rotating anode' _diffrn_source_type 'Incoatec I\ms' _diffrn_standards_number 0 _reflns_Friedel_coverage 0.704 _reflns_Friedel_fraction_full 0.996 _reflns_Friedel_fraction_max 0.995 _reflns_number_gt 3428 _reflns_number_total 3809 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT V8.38A (?, 2016)' _computing_data_collection ? _computing_data_reduction 'SAINT V8.38A (?, 2016)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'XT (Sheldrick, 2015)' _refine_diff_density_max 0.215 _refine_diff_density_min -0.203 _refine_diff_density_rms 0.044 _refine_ls_abs_structure_details ; Flack x determined using 1297 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.03(3) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 244 _refine_ls_number_reflns 3809 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0371 _refine_ls_R_factor_gt 0.0304 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0340P)^2^+0.1270P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0685 _refine_ls_wR_factor_ref 0.0704 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups 2.a Secondary CH2 refined with riding coordinates: C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B) 2.b Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C5(H5), C6(H6), C19(H19), C20(H20), C22(H22), C23(H23) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary ? 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 1.07708(12) 1.14965(5) 0.50934(2) 0.01760(15) Uani 1 1 d . . . . . Cl2 Cl -0.55140(14) -0.20685(5) 0.73185(2) 0.02686(18) Uani 1 1 d . . . . . O1 O 0.3772(3) 0.50809(13) 0.61631(6) 0.0148(4) Uani 1 1 d . . . . . O2 O 0.1287(3) 0.63316(13) 0.65693(6) 0.0200(4) Uani 1 1 d . . . . . C1 C 0.8999(5) 1.03961(18) 0.52917(8) 0.0134(5) Uani 1 1 d . . . . . C2 C 0.9767(5) 0.93238(19) 0.52019(8) 0.0152(5) Uani 1 1 d . . . . . H2 H 1.122527 0.919034 0.502864 0.018 Uiso 1 1 calc R . . . . C3 C 0.8373(5) 0.8452(2) 0.53692(8) 0.0154(5) Uani 1 1 d . . . . . H3 H 0.889420 0.771784 0.531232 0.019 Uiso 1 1 calc R . . . . C4 C 0.6207(5) 0.86399(19) 0.56207(8) 0.0137(5) Uani 1 1 d . . . . . C5 C 0.5478(5) 0.97303(18) 0.57017(8) 0.0145(5) Uani 1 1 d . . . . . H5 H 0.401243 0.987151 0.587155 0.017 Uiso 1 1 calc R . . . . C6 C 0.6862(5) 1.0603(2) 0.55379(9) 0.0155(5) Uani 1 1 d . . . . . H6 H 0.635016 1.133970 0.559400 0.019 Uiso 1 1 calc R . . . . C7 C 0.4796(4) 0.77251(19) 0.57974(8) 0.0134(5) Uani 1 1 d . . . . . C8 C 0.3642(5) 0.69565(19) 0.59401(9) 0.0149(5) Uani 1 1 d . . . . . C9 C 0.2202(5) 0.60158(19) 0.61153(9) 0.0134(5) Uani 1 1 d . . . . . C10 C 0.2078(4) 0.41840(19) 0.62619(9) 0.0142(5) Uani 1 1 d . . . . . C11 C 0.1091(5) 0.4374(2) 0.67619(9) 0.0192(6) Uani 1 1 d . . . . . H11A H 0.244521 0.435091 0.699486 0.023 Uiso 1 1 calc R . . . . H11B H -0.007915 0.378294 0.684441 0.023 Uiso 1 1 calc R . . . . C12 C -0.0181(5) 0.5492(2) 0.67874(9) 0.0224(6) Uani 1 1 d . . . . . H12A H -0.177318 0.544908 0.662235 0.027 Uiso 1 1 calc R . . . . H12B H -0.048696 0.568666 0.712493 0.027 Uiso 1 1 calc R . . . . C13 C 0.0181(5) 0.55984(19) 0.57787(9) 0.0161(5) Uani 1 1 d . . . . . H13A H 0.058935 0.575390 0.544157 0.019 Uiso 1 1 calc R . . . . H13B H -0.140499 0.594468 0.585559 0.019 Uiso 1 1 calc R . . . . C14 C 0.0113(4) 0.43427(19) 0.58747(8) 0.0150(5) Uani 1 1 d . . . . . H14A H -0.150947 0.410965 0.599142 0.018 Uiso 1 1 calc R . . . . H14B H 0.051783 0.392087 0.558319 0.018 Uiso 1 1 calc R . . . . C15 C 0.3542(5) 0.31215(19) 0.62149(10) 0.0179(6) Uani 1 1 d . . . . . H15A H 0.411139 0.304129 0.588173 0.022 Uiso 1 1 calc R . . . . H15B H 0.499486 0.316192 0.642347 0.022 Uiso 1 1 calc R . . . . C16 C 0.2073(5) 0.2150(2) 0.63471(8) 0.0157(6) Uani 1 1 d . . . . . C17 C 0.0842(5) 0.14019(19) 0.64784(8) 0.0160(5) Uani 1 1 d . . . . . C18 C -0.0703(5) 0.05402(18) 0.66662(8) 0.0136(5) Uani 1 1 d . . . . . C19 C -0.0099(5) -0.05741(19) 0.66298(8) 0.0163(6) Uani 1 1 d . . . . . H19 H 0.135077 -0.078474 0.646870 0.020 Uiso 1 1 calc R . . . . C20 C -0.1591(5) -0.1376(2) 0.68260(9) 0.0175(6) Uani 1 1 d . . . . . H20 H -0.117144 -0.213355 0.680096 0.021 Uiso 1 1 calc R . . . . C21 C -0.3689(5) -0.10600(19) 0.70575(9) 0.0168(6) Uani 1 1 d . . . . . C22 C -0.4352(5) 0.00389(19) 0.70983(8) 0.0177(5) Uani 1 1 d . . . . . H22 H -0.580512 0.024267 0.726000 0.021 Uiso 1 1 calc R . . . . C23 C -0.2857(5) 0.08314(19) 0.68991(9) 0.0163(6) Uani 1 1 d . . . . . H23 H -0.330203 0.158601 0.692115 0.020 Uiso 1 1 calc R . . . . 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 0.0171(3) 0.0148(3) 0.0209(3) 0.0040(2) 0.0013(3) -0.0048(3) Cl2 0.0255(4) 0.0252(3) 0.0299(4) 0.0100(3) -0.0006(3) -0.0116(3) O1 0.0102(9) 0.0085(8) 0.0257(9) 0.0029(7) -0.0013(8) -0.0011(7) O2 0.0256(11) 0.0135(9) 0.0209(9) -0.0027(7) 0.0066(8) -0.0035(8) C1 0.0135(14) 0.0133(11) 0.0134(11) 0.0032(9) -0.0026(11) -0.0045(11) C2 0.0135(14) 0.0160(12) 0.0161(12) -0.0008(9) 0.0016(11) 0.0004(10) C3 0.0168(14) 0.0102(11) 0.0192(13) 0.0005(10) -0.0015(10) 0.0013(10) C4 0.0145(14) 0.0134(12) 0.0133(12) 0.0013(9) -0.0038(10) -0.0011(10) C5 0.0119(13) 0.0146(12) 0.0170(12) 0.0005(9) 0.0011(11) 0.0006(11) C6 0.0169(14) 0.0128(12) 0.0169(13) -0.0004(10) -0.0006(11) 0.0027(11) C7 0.0120(13) 0.0114(12) 0.0169(12) -0.0008(9) -0.0006(11) 0.0021(10) C8 0.0151(14) 0.0113(11) 0.0183(13) -0.0008(10) -0.0023(11) 0.0023(10) C9 0.0155(13) 0.0091(11) 0.0154(12) 0.0000(9) 0.0003(11) 0.0019(10) C10 0.0106(13) 0.0099(12) 0.0222(14) 0.0026(9) 0.0011(11) -0.0029(10) C11 0.0264(16) 0.0135(12) 0.0177(12) 0.0024(9) 0.0007(12) -0.0024(12) C12 0.0285(17) 0.0180(13) 0.0208(13) -0.0013(10) 0.0084(12) -0.0047(12) C13 0.0125(14) 0.0164(12) 0.0195(12) 0.0036(10) -0.0010(11) -0.0013(10) C14 0.0124(14) 0.0139(12) 0.0186(12) -0.0002(10) 0.0013(10) -0.0018(10) C15 0.0149(14) 0.0123(12) 0.0267(14) 0.0024(10) 0.0018(12) -0.0003(10) C16 0.0173(14) 0.0119(12) 0.0179(13) 0.0021(10) 0.0001(11) 0.0032(11) C17 0.0170(14) 0.0131(11) 0.0178(12) 0.0004(9) -0.0014(11) 0.0040(12) C18 0.0171(14) 0.0117(11) 0.0119(11) 0.0008(9) -0.0022(11) -0.0008(11) C19 0.0190(15) 0.0153(12) 0.0147(12) -0.0016(10) 0.0043(11) 0.0016(10) C20 0.0222(15) 0.0103(12) 0.0198(13) 0.0005(10) -0.0004(11) -0.0008(11) C21 0.0182(15) 0.0179(12) 0.0144(13) 0.0049(10) -0.0035(11) -0.0062(11) C22 0.0146(14) 0.0218(12) 0.0166(12) 0.0006(10) 0.0026(12) 0.0017(12) C23 0.0200(15) 0.0116(12) 0.0173(13) 0.0003(10) -0.0020(11) 0.0037(11) _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 C1 1.743(2) . ? Cl2 C21 1.743(2) . ? O1 C9 1.431(3) . ? O1 C10 1.458(3) . ? O2 C9 1.421(3) . ? O2 C12 1.435(3) . ? C1 C2 1.391(3) . ? C1 C6 1.384(4) . ? C2 H2 0.9500 . ? C2 C3 1.387(3) . ? C3 H3 0.9500 . ? C3 C4 1.401(4) . ? C4 C5 1.401(3) . ? C4 C7 1.442(3) . ? C5 H5 0.9500 . ? C5 C6 1.382(3) . ? C6 H6 0.9500 . ? C7 C8 1.197(3) . ? C8 C9 1.473(3) . ? C9 C13 1.542(3) . ? C10 C11 1.521(4) . ? C10 C14 1.542(3) . ? C10 C15 1.525(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C11 C12 1.528(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C13 C14 1.548(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C15 C16 1.476(3) . ? C16 C17 1.190(4) . ? C17 C18 1.446(3) . ? C18 C19 1.396(3) . ? C18 C23 1.396(4) . ? C19 H19 0.9500 . ? C19 C20 1.386(3) . ? C20 H20 0.9500 . ? C20 C21 1.377(4) . ? C21 C22 1.387(3) . ? C22 H22 0.9500 . ? C22 C23 1.382(3) . ? C23 H23 0.9500 . ? 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 O1 C10 103.09(18) . . ? C9 O2 C12 112.86(18) . . ? C2 C1 Cl1 119.3(2) . . ? C6 C1 Cl1 119.50(18) . . ? C6 C1 C2 121.1(2) . . ? C1 C2 H2 120.5 . . ? C3 C2 C1 119.0(2) . . ? C3 C2 H2 120.5 . . ? C2 C3 H3 119.5 . . ? C2 C3 C4 121.0(2) . . ? C4 C3 H3 119.5 . . ? C3 C4 C5 118.5(2) . . ? C3 C4 C7 120.2(2) . . ? C5 C4 C7 121.2(2) . . ? C4 C5 H5 119.6 . . ? C6 C5 C4 120.9(2) . . ? C6 C5 H5 119.6 . . ? C1 C6 H6 120.3 . . ? C5 C6 C1 119.5(2) . . ? C5 C6 H6 120.3 . . ? C8 C7 C4 179.1(3) . . ? C7 C8 C9 179.5(3) . . ? O1 C9 C8 108.9(2) . . ? O1 C9 C13 103.28(19) . . ? O2 C9 O1 110.03(19) . . ? O2 C9 C8 106.21(19) . . ? O2 C9 C13 112.5(2) . . ? C8 C9 C13 115.9(2) . . ? O1 C10 C11 106.8(2) . . ? O1 C10 C14 102.61(18) . . ? O1 C10 C15 106.24(19) . . ? C11 C10 C14 112.4(2) . . ? C11 C10 C15 113.3(2) . . ? C15 C10 C14 114.4(2) . . ? C10 C11 H11A 109.7 . . ? C10 C11 H11B 109.7 . . ? C10 C11 C12 109.9(2) . . ? H11A C11 H11B 108.2 . . ? C12 C11 H11A 109.7 . . ? C12 C11 H11B 109.7 . . ? O2 C12 C11 110.8(2) . . ? O2 C12 H12A 109.5 . . ? O2 C12 H12B 109.5 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 108.1 . . ? C9 C13 H13A 111.1 . . ? C9 C13 H13B 111.1 . . ? C9 C13 C14 103.54(19) . . ? H13A C13 H13B 109.0 . . ? C14 C13 H13A 111.1 . . ? C14 C13 H13B 111.1 . . ? C10 C14 C13 103.23(19) . . ? C10 C14 H14A 111.1 . . ? C10 C14 H14B 111.1 . . ? C13 C14 H14A 111.1 . . ? C13 C14 H14B 111.1 . . ? H14A C14 H14B 109.1 . . ? C10 C15 H15A 109.3 . . ? C10 C15 H15B 109.3 . . ? H15A C15 H15B 108.0 . . ? C16 C15 C10 111.5(2) . . ? C16 C15 H15A 109.3 . . ? C16 C15 H15B 109.3 . . ? C17 C16 C15 175.9(3) . . ? C16 C17 C18 176.0(3) . . ? C19 C18 C17 122.4(2) . . ? C23 C18 C17 118.9(2) . . ? C23 C18 C19 118.7(2) . . ? C18 C19 H19 119.6 . . ? C20 C19 C18 120.8(2) . . ? C20 C19 H19 119.6 . . ? C19 C20 H20 120.5 . . ? C21 C20 C19 119.0(2) . . ? C21 C20 H20 120.5 . . ? C20 C21 Cl2 118.85(19) . . ? C20 C21 C22 121.8(2) . . ? C22 C21 Cl2 119.4(2) . . ? C21 C22 H22 120.6 . . ? C23 C22 C21 118.7(2) . . ? C23 C22 H22 120.6 . . ? C18 C23 H23 119.5 . . ? C22 C23 C18 121.0(2) . . ? C22 C23 H23 119.5 . . ? _shelx_res_file ; TITL eds_071903_0m_a.res in P2(1)2(1)2(1) eds_071903_0m.res created by SHELXL-2016/6 at 13:28:39 on 25-Jul-2019 REM Old TITL EDS_071903_0m in P2(1)2(1)2(1) REM SHELXT solution in P2(1)2(1)2(1) REM R1 0.084, Rweak 0.021, Alpha 0.001, Orientation as input REM Flack x = 0.028 ( 0.028 ) from Parsons' quotients REM Formula found by SHELXT: C23 O2 Cl2 CELL 0.71073 5.4867 12.1391 28.0466 90 90 90 ZERR 4 0.0005 0.0011 0.0026 0 0 0 LATT -1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H Cl O UNIT 92 72 8 8 L.S. 4 PLAN 20 SIZE 0.2 0.02 0.01 TEMP -183.15 BOND $H list 4 fmap 2 acta REM REM REM WGHT 0.034000 0.127000 FVAR 0.52274 CL1 3 1.077079 1.149646 0.509336 11.00000 0.01706 0.01481 = 0.02091 0.00405 0.00129 -0.00479 CL2 3 -0.551397 -0.206847 0.731851 11.00000 0.02546 0.02524 = 0.02986 0.01000 -0.00062 -0.01156 O1 4 0.377157 0.508090 0.616312 11.00000 0.01019 0.00854 = 0.02568 0.00286 -0.00129 -0.00111 O2 4 0.128704 0.633158 0.656928 11.00000 0.02564 0.01346 = 0.02086 -0.00272 0.00657 -0.00346 C1 1 0.899852 1.039607 0.529165 11.00000 0.01353 0.01331 = 0.01338 0.00317 -0.00260 -0.00448 C2 1 0.976710 0.932383 0.520191 11.00000 0.01354 0.01599 = 0.01606 -0.00082 0.00160 0.00040 AFIX 43 H2 2 1.122527 0.919034 0.502864 11.00000 -1.20000 AFIX 0 C3 1 0.837250 0.845240 0.536920 11.00000 0.01684 0.01024 = 0.01919 0.00052 -0.00150 0.00134 AFIX 43 H3 2 0.889420 0.771784 0.531232 11.00000 -1.20000 AFIX 0 C4 1 0.620659 0.863987 0.562073 11.00000 0.01451 0.01339 = 0.01330 0.00129 -0.00385 -0.00109 C5 1 0.547768 0.973033 0.570175 11.00000 0.01187 0.01458 = 0.01704 0.00052 0.00114 0.00063 AFIX 43 H5 2 0.401243 0.987151 0.587155 11.00000 -1.20000 AFIX 0 C6 1 0.686176 1.060335 0.553794 11.00000 0.01693 0.01276 = 0.01689 -0.00041 -0.00056 0.00270 AFIX 43 H6 2 0.635016 1.133970 0.559400 11.00000 -1.20000 AFIX 0 C7 1 0.479559 0.772509 0.579743 11.00000 0.01198 0.01138 = 0.01692 -0.00080 -0.00056 0.00211 C8 1 0.364155 0.695645 0.594011 11.00000 0.01508 0.01128 = 0.01834 -0.00084 -0.00226 0.00231 C9 1 0.220178 0.601578 0.611529 11.00000 0.01554 0.00912 = 0.01543 0.00000 0.00027 0.00187 C10 1 0.207835 0.418402 0.626191 11.00000 0.01064 0.00986 = 0.02219 0.00262 0.00107 -0.00285 C11 1 0.109069 0.437385 0.676187 11.00000 0.02641 0.01354 = 0.01769 0.00236 0.00072 -0.00239 AFIX 23 H11A 2 0.244521 0.435091 0.699486 11.00000 -1.20000 H11B 2 -0.007915 0.378294 0.684441 11.00000 -1.20000 AFIX 0 C12 1 -0.018102 0.549248 0.678737 11.00000 0.02851 0.01803 = 0.02079 -0.00131 0.00839 -0.00473 AFIX 23 H12A 2 -0.177318 0.544908 0.662235 11.00000 -1.20000 H12B 2 -0.048696 0.568666 0.712493 11.00000 -1.20000 AFIX 0 C13 1 0.018070 0.559840 0.577873 11.00000 0.01255 0.01638 = 0.01947 0.00358 -0.00104 -0.00129 AFIX 23 H13A 2 0.058935 0.575390 0.544157 11.00000 -1.20000 H13B 2 -0.140499 0.594468 0.585559 11.00000 -1.20000 AFIX 0 C14 1 0.011349 0.434274 0.587473 11.00000 0.01241 0.01393 = 0.01858 -0.00024 0.00131 -0.00184 AFIX 23 H14A 2 -0.150947 0.410965 0.599142 11.00000 -1.20000 H14B 2 0.051783 0.392087 0.558319 11.00000 -1.20000 AFIX 0 C15 1 0.354201 0.312147 0.621488 11.00000 0.01486 0.01225 = 0.02672 0.00240 0.00182 -0.00028 AFIX 23 H15A 2 0.411139 0.304129 0.588173 11.00000 -1.20000 H15B 2 0.499486 0.316192 0.642347 11.00000 -1.20000 AFIX 0 C16 1 0.207310 0.215009 0.634707 11.00000 0.01725 0.01194 = 0.01789 0.00207 0.00012 0.00322 C17 1 0.084227 0.140187 0.647841 11.00000 0.01704 0.01311 = 0.01777 0.00042 -0.00138 0.00402 C18 1 -0.070271 0.054019 0.666616 11.00000 0.01710 0.01171 = 0.01190 0.00083 -0.00221 -0.00081 C19 1 -0.009928 -0.057408 0.662979 11.00000 0.01898 0.01534 = 0.01473 -0.00161 0.00429 0.00164 AFIX 43 H19 2 0.135077 -0.078474 0.646870 11.00000 -1.20000 AFIX 0 C20 1 -0.159095 -0.137647 0.682595 11.00000 0.02225 0.01032 = 0.01981 0.00052 -0.00044 -0.00082 AFIX 43 H20 2 -0.117144 -0.213355 0.680096 11.00000 -1.20000 AFIX 0 C21 1 -0.368940 -0.105997 0.705753 11.00000 0.01815 0.01786 = 0.01435 0.00489 -0.00348 -0.00623 C22 1 -0.435199 0.003886 0.709832 11.00000 0.01461 0.02177 = 0.01664 0.00064 0.00261 0.00173 AFIX 43 H22 2 -0.580512 0.024267 0.726000 11.00000 -1.20000 AFIX 0 C23 1 -0.285684 0.083144 0.689915 11.00000 0.01996 0.01156 = 0.01728 0.00026 -0.00198 0.00369 AFIX 43 H23 2 -0.330203 0.158601 0.692115 11.00000 -1.20000 AFIX 0 HKLF 4 REM eds_071903_0m_a.res in P2(1)2(1)2(1) REM R1 = 0.0304 for 3428 Fo > 4sig(Fo) and 0.0371 for all 3809 data REM 244 parameters refined using 0 restraints END WGHT 0.0340 0.1270 REM Highest difference peak 0.215, deepest hole -0.203, 1-sigma level 0.044 Q1 1 0.0904 0.5960 0.5961 11.00000 0.05 0.22 Q2 1 -0.3392 -0.1405 0.6812 11.00000 0.05 0.21 Q3 1 0.3685 0.7590 0.5979 11.00000 0.05 0.21 Q4 1 0.1194 0.4237 0.6106 11.00000 0.05 0.19 Q5 1 0.7343 0.8548 0.5632 11.00000 0.05 0.19 Q6 1 0.5927 1.0026 0.5466 11.00000 0.05 0.19 Q7 1 0.7621 1.0424 0.5293 11.00000 0.05 0.19 Q8 1 -0.2386 -0.1146 0.7082 11.00000 0.05 0.19 Q9 1 0.1662 0.4149 0.6513 11.00000 0.05 0.18 Q10 1 0.5829 0.9059 0.5543 11.00000 0.05 0.17 Q11 1 -0.1358 0.0715 0.6880 11.00000 0.05 0.17 Q12 1 -0.1777 0.0655 0.6760 11.00000 0.05 0.17 Q13 1 0.0060 0.0945 0.6631 11.00000 0.05 0.17 Q14 1 0.8749 0.8961 0.5269 11.00000 0.05 0.16 Q15 1 0.4176 0.4955 0.5816 11.00000 0.05 0.16 Q16 1 1.0239 1.1936 0.4808 11.00000 0.05 0.16 Q17 1 0.2305 0.4013 0.6583 11.00000 0.05 0.16 Q18 1 -0.4046 -0.0497 0.6996 11.00000 0.05 0.15 Q19 1 0.6052 0.9144 0.5778 11.00000 0.05 0.15 Q20 1 -0.5151 -0.1802 0.6971 11.00000 0.05 0.15 ; _shelx_res_checksum 64564 _shelx_hkl_file ; -1 0 0 -0.30 1.40 -1 0 0 -0.50 1.60 -2 0 0 4143.69 198.98 -2 0 0 4123.79 198.28 -2 0 0 3994.00 197.78 -4 0 0 178.48 14.00 -5 0 0 1.00 4.00 -5 0 0 5.10 16.00 -5 0 0 -0.50 6.30 -6 0 0 28.40 9.40 -6 0 0 31.00 8.60 -6 0 0 24.70 5.90 -6 0 0 55.89 27.40 0 -1 0 0.30 0.80 0 1 0 -1.00 0.60 0 -1 0 0.00 0.70 0 -1 0 -0.20 0.60 -1 -1 0 6772.12 357.06 1 -1 0 7346.56 359.46 -1 1 0 7274.57 358.86 1 -1 0 7289.67 357.26 -1 1 0 7994.50 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-2 30 3.30 7.10 -3 2 -30 -50.99 42.00 3 2 30 15.00 7.50 0 3 -30 294.97 25.90 0 -3 30 221.38 21.10 0 3 30 277.67 22.10 0 -3 -30 265.67 27.30 -1 3 30 12.80 9.30 -1 -3 -30 18.80 11.80 -1 -3 -30 6.00 15.20 1 3 -30 20.00 10.60 1 -3 30 11.90 12.00 -1 -3 30 21.40 5.50 -1 -3 30 21.10 10.50 1 -3 -30 18.80 13.10 1 3 30 21.50 9.50 -1 3 -30 25.10 11.10 2 3 -30 178.28 22.40 -2 -3 -30 176.28 34.00 2 -3 30 162.18 15.10 -2 -3 -30 156.98 20.70 -2 3 30 152.68 17.10 -2 -3 30 147.99 17.30 2 3 30 171.38 16.60 2 -3 -30 182.68 21.60 -2 3 -30 141.69 19.80 -2 -3 30 167.88 13.20 -2 3 -30 272.47 49.90 3 -3 30 10.20 8.50 -3 3 30 16.10 10.50 -3 -3 -30 48.20 31.80 3 3 -30 8.90 14.50 -3 -3 -30 8.30 13.30 3 -3 -30 7.80 12.70 -3 -3 30 10.40 11.40 -3 -3 30 23.00 7.70 -3 3 -30 4.40 12.10 -3 3 -30 66.09 35.50 0 -4 30 20.90 13.20 0 4 -30 32.80 12.70 0 4 30 26.50 10.60 0 -4 -30 39.80 14.40 1 -4 30 1.90 10.50 -1 4 30 7.80 10.20 1 4 -30 14.40 12.60 -1 -4 -30 16.30 12.90 -1 -4 -30 13.90 15.40 -1 -4 30 18.80 10.30 1 4 30 23.30 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2.10 12.30 0 6 -30 -11.80 16.40 0 -6 -30 0.10 10.40 1 6 -30 102.89 21.80 -1 6 30 79.29 13.00 -1 -6 -30 103.19 19.00 1 -6 30 77.99 11.60 -1 -6 30 77.59 8.60 -1 6 -30 81.89 14.80 1 6 30 69.69 11.80 -1 -6 30 63.09 16.30 1 -6 -30 81.39 16.40 -2 6 30 40.80 12.60 -2 -6 -30 19.90 14.00 2 6 -30 49.30 18.80 2 -6 30 29.10 9.60 -2 -6 -30 -11.30 28.30 -2 6 -30 22.70 12.80 -2 -6 30 16.30 11.70 2 -6 -30 23.30 13.20 -2 -6 30 20.90 7.20 0 -7 30 351.06 26.00 0 -7 -30 315.77 22.20 0 -7 -30 327.57 31.00 0 7 -30 329.87 34.90 0 7 30 325.67 24.40 1 7 -30 31.90 18.90 -1 7 30 16.70 10.70 1 -7 30 27.50 9.10 -1 -7 -30 29.80 14.50 1 -7 -30 18.00 14.00 -1 -7 30 27.80 6.80 -1 -7 30 22.40 12.70 1 -7 -30 22.00 7.30 -1 7 -30 11.20 18.60 0 0 31 0.30 9.40 0 0 -31 -2.80 11.20 1 0 31 -0.90 10.70 -1 0 31 0.00 8.70 -1 0 31 -1.40 5.30 1 0 -31 -6.60 10.60 -1 0 -31 1.30 11.40 -2 0 31 47.90 12.40 -2 0 -31 20.70 32.60 2 0 31 76.89 9.80 -2 0 -31 32.40 13.70 -2 0 31 63.59 8.50 2 0 -31 53.09 14.10 -3 0 31 90.39 15.20 3 0 -31 60.99 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31 -7.80 10.20 -2 3 -31 -3.00 12.70 0 -4 31 -4.60 12.40 0 4 31 -3.40 9.90 0 -4 -31 -2.60 12.30 0 4 -31 6.40 11.40 1 -4 31 47.00 13.90 -1 -4 -31 48.10 13.30 1 4 -31 46.50 14.60 -1 4 31 45.20 12.40 -1 -4 31 55.99 13.30 1 4 31 78.09 12.00 1 -4 -31 64.69 16.00 -1 -4 31 61.29 7.60 -1 4 -31 71.69 14.70 2 4 -31 48.10 17.10 2 -4 31 51.39 9.80 -2 4 31 36.50 11.20 -2 -4 -31 39.20 14.70 -2 -4 -31 43.60 30.40 -2 -4 31 60.59 13.30 -2 -4 31 50.99 8.10 -2 4 -31 51.99 13.50 -2 4 -31 122.59 42.50 2 -4 -31 47.80 13.60 2 4 31 15.50 11.20 0 5 31 95.09 14.10 0 -5 -31 97.79 17.40 0 -5 31 122.79 16.20 0 5 -31 129.59 17.60 1 -5 31 17.00 8.10 1 5 -31 9.30 13.90 -1 -5 -31 0.60 12.50 -1 5 31 0.90 10.80 -1 -5 31 4.60 11.80 1 -5 -31 -8.20 13.60 1 5 31 -9.90 9.40 -1 -5 31 6.80 5.40 -1 5 -31 -1.90 11.70 2 -5 31 71.69 11.30 -2 -5 -31 45.90 29.60 -2 -5 -31 81.69 17.70 2 5 -31 53.69 19.80 -2 5 31 65.29 13.90 -2 5 -31 68.89 14.90 -2 -5 31 55.99 15.00 -2 -5 31 82.49 9.10 2 -5 -31 39.70 13.60 0 6 31 60.09 13.40 0 -6 31 81.99 17.40 0 6 -31 89.99 21.10 0 -6 -31 83.19 18.30 1 -6 31 49.00 10.40 -1 -6 -31 37.40 14.10 -1 6 31 48.50 12.10 1 6 -31 18.50 19.20 -1 -6 31 35.90 7.40 -1 6 -31 50.39 13.30 1 -6 -31 35.90 14.50 -1 -6 31 49.60 16.40 1 6 31 25.90 10.90 0 -7 -31 28.00 14.10 0 7 -31 24.50 19.90 0 -7 31 50.89 14.00 0 7 31 13.60 11.30 0 0 32 21.80 11.50 0 0 -32 31.60 11.40 -1 0 32 22.20 9.90 1 0 32 2.80 10.30 -1 0 -32 3.10 12.80 -1 0 32 16.50 5.90 1 0 -32 23.10 13.00 2 0 -32 152.48 20.90 -2 0 -32 169.98 45.10 -2 0 32 149.99 17.60 -2 0 32 150.78 13.20 -2 0 -32 155.68 21.20 2 0 32 216.18 16.30 0 1 -32 133.99 17.90 0 1 32 114.49 15.40 0 -1 32 126.79 14.50 0 -1 -32 113.09 19.10 -1 -1 -32 76.19 16.40 1 1 -32 82.19 15.10 -1 1 32 66.89 12.30 1 -1 32 74.19 14.20 -1 1 32 86.09 8.60 -1 1 -32 76.39 17.60 -1 -1 32 92.09 13.10 -1 1 -32 209.88 42.80 -1 -1 32 82.19 8.60 1 -1 -32 98.89 17.00 1 1 32 85.49 14.70 -2 -1 -32 92.69 33.90 2 1 -32 98.39 17.60 -2 1 32 77.09 13.80 -2 -1 -32 108.29 18.00 2 -1 32 88.39 11.10 -2 -1 32 93.29 14.80 -2 1 -32 229.18 40.60 -2 -1 32 90.39 10.10 2 -1 -32 82.29 17.50 2 1 32 153.98 14.60 -2 1 -32 92.89 17.60 0 2 32 11.30 9.40 0 -2 -32 5.80 13.70 0 2 -32 15.80 12.70 0 -2 32 20.10 11.40 -1 -2 -32 76.69 16.80 1 -2 32 69.69 15.00 1 2 -32 44.80 13.50 -1 2 -32 134.49 40.80 1 2 32 56.19 13.00 -1 -2 32 71.79 13.30 -1 -2 32 70.79 7.80 1 -2 -32 51.09 15.00 -1 2 -32 62.19 14.40 -2 2 32 49.40 12.10 2 2 -32 38.70 14.60 -2 -2 -32 34.90 29.90 2 -2 32 60.79 9.90 -2 -2 -32 50.49 15.40 -2 2 -32 37.20 15.50 -2 -2 32 44.10 13.10 -2 -2 32 45.80 8.50 2 2 32 47.90 12.20 -2 2 -32 154.38 43.40 2 -2 -32 44.80 15.70 0 -3 32 21.10 13.30 0 3 32 19.50 10.70 0 -3 -32 8.00 13.70 0 3 -32 29.10 12.90 -1 3 32 69.29 13.20 1 3 -32 86.39 16.80 1 -3 32 71.89 15.50 -1 -3 -32 68.09 16.90 1 3 32 71.29 12.70 -1 3 -32 71.09 15.30 -1 -3 32 63.09 13.10 1 -3 -32 82.59 16.30 -1 -3 32 72.99 8.00 2 3 -32 11.90 13.40 2 -3 32 10.60 8.70 -2 -3 -32 22.10 28.50 -2 3 32 13.70 11.60 -2 -3 -32 -6.40 12.80 -2 3 -32 -8.90 12.60 -2 -3 32 -2.20 9.80 -2 3 -32 34.60 41.40 -2 -3 32 6.00 6.80 2 -3 -32 11.20 13.10 2 3 32 -28.40 9.90 0 4 32 45.40 11.20 0 -4 -32 49.99 15.80 0 -4 32 57.89 15.00 0 4 -32 41.20 12.80 -1 4 32 37.70 11.40 1 -4 32 41.50 12.40 1 4 -32 36.90 17.10 -1 -4 -32 41.50 14.70 1 4 32 34.60 11.40 -1 -4 32 31.80 6.70 -1 -4 32 34.20 13.00 -1 4 -32 36.60 13.20 1 -4 -32 29.80 15.80 -2 -4 -32 13.20 14.70 -2 4 32 14.90 10.50 2 -4 32 25.60 8.60 2 4 -32 20.70 15.30 -2 -4 -32 -1.10 28.70 2 -4 -32 11.50 13.00 -2 -4 32 0.10 11.40 -2 4 -32 100.39 43.60 -2 -4 32 15.80 7.00 -2 4 -32 12.70 12.50 2 4 32 -21.60 11.10 0 -5 -32 33.90 15.60 0 5 -32 43.50 13.60 0 5 32 42.60 12.50 0 -5 32 45.00 14.30 1 -5 32 40.80 10.00 -1 -5 -32 19.00 14.60 -1 5 32 -3.90 11.70 1 5 -32 12.60 17.20 -1 -5 32 18.00 6.20 1 5 32 14.70 10.30 1 -5 -32 8.70 15.90 -1 5 -32 18.50 13.20 -1 -5 32 10.70 15.10 0 -6 -32 14.60 14.90 0 6 -32 28.00 18.60 0 -6 32 -8.50 13.30 0 6 32 7.10 11.90 0 0 -33 8.10 11.70 0 0 33 -0.80 10.90 -1 0 -33 90.79 19.10 1 0 -33 116.79 18.80 -1 0 33 107.09 9.50 -1 0 33 102.29 14.70 1 0 33 96.59 14.00 -2 0 -33 98.99 33.40 -2 0 33 -7.20 7.10 -2 0 -33 -3.40 13.30 -2 0 33 5.00 10.00 2 0 -33 6.60 13.40 0 -1 33 -4.90 10.50 0 1 -33 10.60 12.20 0 -1 -33 -4.40 13.90 0 1 33 -18.00 10.90 -1 -1 33 46.00 11.60 -1 1 -33 127.69 41.70 1 -1 -33 46.60 14.80 -1 1 -33 43.20 16.00 -1 -1 33 44.50 7.20 1 1 33 44.40 12.50 2 -1 33 45.70 9.60 2 1 -33 33.40 14.10 -2 1 33 31.90 8.00 -2 1 33 4.20 12.30 -2 -1 -33 7.70 34.30 -2 -1 -33 25.40 14.40 -2 -1 33 30.60 7.80 -2 1 -33 144.19 39.20 2 1 33 56.49 9.30 -2 -1 33 28.10 12.70 -2 1 -33 25.10 14.20 2 -1 -33 26.10 15.20 0 2 33 91.69 13.70 0 -2 -33 68.49 18.00 0 -2 33 85.99 14.80 0 2 -33 86.09 15.80 1 -2 33 91.99 16.60 1 2 -33 91.29 17.30 -1 -2 -33 65.99 15.90 -1 2 33 83.19 14.20 -1 2 -33 82.29 14.80 1 -2 -33 86.09 16.10 1 2 33 78.69 13.80 -1 -2 33 76.79 15.40 -1 -2 33 96.79 9.50 -2 -2 -33 84.79 17.40 2 2 -33 68.89 18.70 2 -2 33 83.69 12.10 -2 -2 -33 44.20 34.00 -2 2 33 47.20 14.40 2 2 33 86.59 12.60 -2 -2 33 71.09 13.70 2 -2 -33 66.49 17.60 -2 -2 33 64.49 9.30 -2 2 -33 167.78 50.69 -2 2 -33 40.90 17.10 0 3 33 -8.70 9.20 0 3 -33 -8.90 11.70 0 -3 -33 2.30 14.10 0 -3 33 -3.50 13.70 1 -3 33 24.00 14.30 -1 3 33 22.10 11.50 -1 -3 -33 14.70 14.40 1 3 -33 12.20 11.20 -1 3 -33 8.30 12.30 1 3 33 -3.10 11.30 1 -3 -33 19.10 11.70 -1 -3 33 3.30 12.20 0 4 33 127.49 16.00 0 -4 33 139.19 18.70 0 4 -33 136.89 19.10 0 -4 -33 135.69 20.90 1 4 -33 5.20 16.80 -1 4 33 26.90 12.20 1 -4 33 30.60 10.60 -1 -4 -33 29.70 13.30 1 4 33 0.30 11.50 1 -4 -33 8.20 14.10 -1 -4 33 25.40 11.40 -1 4 -33 23.40 13.20 0 5 -33 158.18 20.90 0 5 33 156.98 18.20 0 -5 33 169.98 21.40 0 -5 -33 179.18 23.90 0 0 -34 110.49 18.10 0 0 34 81.59 13.80 1 0 34 -13.70 11.60 -1 0 -34 124.19 40.00 -1 0 -34 -9.00 15.10 1 0 -34 11.90 13.20 -1 0 34 -9.50 11.00 0 1 34 -3.20 12.00 0 -1 34 7.90 10.30 0 1 -34 9.00 11.10 0 -1 -34 3.80 13.30 1 -1 34 35.20 14.40 1 1 -34 7.00 12.40 -1 1 34 -6.40 11.90 -1 -1 -34 21.10 13.60 -1 1 -34 21.00 14.80 1 1 34 14.90 12.80 -1 -1 34 7.60 12.90 -1 1 -34 115.79 41.20 1 -1 -34 21.20 12.40 0 2 -34 8.10 12.90 0 -2 34 4.00 13.90 0 2 34 -4.90 10.50 0 -2 -34 -6.90 14.60 1 -2 34 -5.60 14.00 -1 -2 -34 -2.40 13.70 -1 2 34 11.10 12.30 1 2 -34 11.60 13.90 1 2 34 -8.80 12.40 -1 -2 34 -6.20 12.90 -1 2 -34 23.70 13.00 1 -2 -34 7.60 13.90 0 3 34 -1.60 11.70 0 3 -34 5.80 13.70 0 -3 34 6.30 13.30 0 -3 -34 12.10 16.20 -1 -3 -34 55.99 15.60 0 0 -35 8.30 11.60 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 97750 _olex2_submission_special_instructions 'No special instructions were received' ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_asb-achiralketal-biphenyl _database_code_depnum_ccdc_archive 'CCDC 2020673' loop_ _audit_author_name _audit_author_address 'Eric Sylvester' ;State University of New York, Buffalo United States of America ; _audit_update_record ; 2020-07-31 deposited with the CCDC. 2020-12-07 downloaded from the CCDC. ; _audit_creation_date 2020-07-31 _audit_creation_method ; Olex2 1.3 (compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938) ; _shelx_SHELXL_version_number 2018/3 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C31 H28 O2' _chemical_formula_sum 'C31 H28 O2' _chemical_formula_weight 432.53 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/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 14.015(2) _cell_length_b 9.4761(9) _cell_length_c 17.0238(18) _cell_angle_alpha 90 _cell_angle_beta 95.826(6) _cell_angle_gamma 90 _cell_volume 2249.2(5) _cell_formula_units_Z 4 _cell_measurement_reflns_used 6747 _cell_measurement_temperature 90 _cell_measurement_theta_max 26.398 _cell_measurement_theta_min 2.405 _shelx_estimated_absorpt_T_max 0.999 _shelx_estimated_absorpt_T_min 0.997 _exptl_absorpt_coefficient_mu 0.078 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.7058 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2014/2 (Bruker,2014/2) was used for absorption correction. wR2(int) was 0.1751 before and 0.0450 after correction. The Ratio of minimum to maximum transmission is 0.9469. The \l/2 correction factor is 0.00150.' _exptl_absorpt_special_details ? _exptl_crystal_colour colourless _exptl_crystal_colour_lustre ? _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.277 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description plate _exptl_crystal_F_000 920 _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.01 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.1985 _diffrn_reflns_av_unetI/netI 0.1030 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 21398 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.403 _diffrn_reflns_theta_min 1.795 _diffrn_ambient_temperature 90.0 _diffrn_detector_area_resol_mean 7.9 _diffrn_detector_type 'CCD area detector' _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker SMART APEX2 area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source ? _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 3661 _reflns_number_total 4604 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)' _computing_data_collection ? _computing_data_reduction 'SAINT v8.34A (Bruker, 2013)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL n/a (Sheldrick, 2008)' _computing_structure_solution 'olex2.solve 1.3 (Bourhis et al., 2015)' _refine_diff_density_max 0.324 _refine_diff_density_min -0.364 _refine_diff_density_rms 0.066 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 317 _refine_ls_number_reflns 4604 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0726 _refine_ls_R_factor_gt 0.0593 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0181P)^2^+1.2055P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1589 _refine_ls_wR_factor_ref 0.1662 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups 2. Rigid bond restraints C6B, C6 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 3. Uiso/Uaniso restraints and constraints C6B \\sim C5B \\sim C5 \\sim C6: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.08 within 1.7A Uanis(C6B) = Uanis(C6) Uanis(C2) = Uanis(C2B) Uanis(O2) = Uanis(O2B) Uanis(C6B) = Uanis(C2B) = Uanis(C3B) = Uanis(C5B) Uanis(C6B) = Uanis(C5B) = Uanis(C2B) = Uanis(C3B) 4. Others Sof(O1B)=Sof(O2B)=Sof(C2B)=Sof(H2BA)=Sof(H2BB)=Sof(C3B)=Sof(H3BA)=Sof(H3BB)= Sof(C6B)=Sof(H7BA)=Sof(H7BB)=Sof(C5B)=Sof(H8BA)=Sof(H8BB)=1-FVAR(1) Sof(O1)=Sof(O2)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C5)= Sof(H5A)=Sof(H5B)=Sof(C6)=Sof(H6A)=Sof(H6B)=FVAR(1) 5.a Secondary CH2 refined with riding coordinates: C7(H7A,H7B), C2B(H2BA,H2BB), C3B(H3BA,H3BB), C6B(H7BA,H7BB), C5B(H8BA,H8BB), C2(H2A,H2B), C3(H3A,H3B), C5(H5A,H5B), C6(H6A,H6B) 5.b Aromatic/amide H refined with riding coordinates: C9(H9), C10(H10), C12(H12), C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22), C24(H24), C25(H25), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _atom_sites_solution_secondary ? 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 C1 C 0.65709(13) 0.6843(2) 0.75318(11) 0.0204(5) Uani 1 1 d . . . . . C4 C 0.77154(14) 0.6700(2) 0.66845(11) 0.0215(5) Uani 1 1 d . . . . . C7 C 0.64250(13) 0.7073(2) 0.83978(10) 0.0153(4) Uani 1 1 d . . . . . H7A H 0.677731 0.633121 0.871785 0.018 Uiso 1 1 calc R U . . . H7B H 0.670586 0.799516 0.856891 0.018 Uiso 1 1 calc R U . . . C8 C 0.53825(13) 0.7046(2) 0.85629(10) 0.0147(4) Uani 1 1 d . . . . . C9 C 0.47980(13) 0.8221(2) 0.84154(10) 0.0159(4) Uani 1 1 d . . . . . H9 H 0.505908 0.905922 0.821842 0.019 Uiso 1 1 calc R U . . . C10 C 0.38346(13) 0.8187(2) 0.85520(11) 0.0163(4) Uani 1 1 d . . . . . H10 H 0.344688 0.899796 0.843728 0.020 Uiso 1 1 calc R U . . . C11 C 0.34302(13) 0.6988(2) 0.88535(10) 0.0144(4) Uani 1 1 d . . . . . C12 C 0.40205(13) 0.5815(2) 0.90167(11) 0.0176(4) Uani 1 1 d . . . . . H12 H 0.376440 0.498730 0.923036 0.021 Uiso 1 1 calc R U . . . C13 C 0.49831(13) 0.5843(2) 0.88696(11) 0.0186(4) Uani 1 1 d . . . . . H13 H 0.537120 0.503156 0.898018 0.022 Uiso 1 1 calc R U . . . C14 C 0.23933(13) 0.6961(2) 0.90008(10) 0.0148(4) Uani 1 1 d . . . . . C15 C 0.19128(13) 0.8196(2) 0.91644(10) 0.0161(4) Uani 1 1 d . . . . . H15 H 0.224833 0.906854 0.919098 0.019 Uiso 1 1 calc R U . . . C16 C 0.09415(14) 0.8168(2) 0.92903(11) 0.0185(4) Uani 1 1 d . . . . . H16 H 0.061957 0.902022 0.939299 0.022 Uiso 1 1 calc R U . . . C17 C 0.04503(14) 0.6902(2) 0.92655(11) 0.0210(4) Uani 1 1 d . . . . . H17 H -0.020617 0.688042 0.935963 0.025 Uiso 1 1 calc R U . . . C18 C 0.09163(14) 0.5666(2) 0.91033(12) 0.0234(5) Uani 1 1 d . . . . . H18 H 0.057794 0.479637 0.908392 0.028 Uiso 1 1 calc R U . . . C19 C 0.18813(13) 0.5691(2) 0.89679(11) 0.0194(4) Uani 1 1 d . . . . . H19 H 0.219389 0.483773 0.885220 0.023 Uiso 1 1 calc R U . . . C20 C 0.87641(13) 0.6771(2) 0.65639(11) 0.0159(4) Uani 1 1 d . . . . . C21 C 0.90413(13) 0.6552(2) 0.58127(10) 0.0178(4) Uani 1 1 d . . . . . H21 H 0.856924 0.635804 0.538561 0.021 Uiso 1 1 calc R U . . . C22 C 0.99989(13) 0.6614(2) 0.56809(10) 0.0159(4) Uani 1 1 d . . . . . H22 H 1.017602 0.645584 0.516413 0.019 Uiso 1 1 calc R U . . . C23 C 1.07124(13) 0.69076(19) 0.62989(10) 0.0142(4) Uani 1 1 d . . . . . C24 C 1.04266(13) 0.7135(2) 0.70496(10) 0.0159(4) Uani 1 1 d . . . . . H24 H 1.089464 0.734563 0.747699 0.019 Uiso 1 1 calc R U . . . C25 C 0.94643(13) 0.7058(2) 0.71798(10) 0.0163(4) Uani 1 1 d . . . . . H25 H 0.928375 0.720410 0.769664 0.020 Uiso 1 1 calc R U . . . C26 C 1.17436(13) 0.69399(19) 0.61546(11) 0.0144(4) Uani 1 1 d . . . . . C27 C 1.20133(13) 0.7155(2) 0.53973(11) 0.0174(4) Uani 1 1 d . . . . . H27 H 1.153242 0.730244 0.497045 0.021 Uiso 1 1 calc R U . . . C28 C 1.29719(13) 0.7156(2) 0.52557(11) 0.0186(4) Uani 1 1 d . . . . . H28 H 1.313913 0.730321 0.473490 0.022 Uiso 1 1 calc R U . . . C29 C 1.36865(14) 0.6944(2) 0.58694(12) 0.0194(4) Uani 1 1 d . . . . . H29 H 1.434196 0.693785 0.577182 0.023 Uiso 1 1 calc R U . . . C30 C 1.34325(13) 0.6743(2) 0.66257(11) 0.0194(4) Uani 1 1 d . . . . . H30 H 1.391711 0.660633 0.705106 0.023 Uiso 1 1 calc R U . . . C31 C 1.24720(13) 0.6738(2) 0.67676(11) 0.0171(4) Uani 1 1 d . . . . . H31 H 1.230891 0.659487 0.728991 0.021 Uiso 1 1 calc R U . . . O1B O 0.7611(9) 0.7347(14) 0.7475(7) 0.017(3) Uani 0.142(2) 1 d . . P A 2 O2B O 0.7463(7) 0.8363(11) 0.6238(6) 0.0157(4) Uani 0.142(2) 1 d . . P A 2 C2B C 0.6132(10) 0.8562(16) 0.7086(8) 0.0151(4) Uani 0.142(2) 1 d . . P A 2 H2BA H 0.542462 0.861288 0.706639 0.018 Uiso 0.142(2) 1 calc R U P A 2 H2BB H 0.640813 0.935762 0.741109 0.018 Uiso 0.142(2) 1 calc R U P A 2 C3B C 0.6439(9) 0.8659(14) 0.6256(7) 0.0151(4) Uani 0.142(2) 1 d . . P A 2 H3BA H 0.606136 0.797695 0.591065 0.018 Uiso 0.142(2) 1 calc R U P A 2 H3BB H 0.629731 0.961724 0.604434 0.018 Uiso 0.142(2) 1 calc R U P A 2 C6B C 0.6314(10) 0.5890(16) 0.6991(8) 0.0151(4) Uani 0.142(2) 1 d . U P A 2 H7BA H 0.568855 0.614666 0.670387 0.018 Uiso 0.142(2) 1 calc R U P A 2 H7BB H 0.624798 0.495703 0.724178 0.018 Uiso 0.142(2) 1 calc R U P A 2 C5B C 0.7060(11) 0.5826(17) 0.6436(8) 0.0151(4) Uani 0.142(2) 1 d . U P A 2 H8BA H 0.732630 0.485978 0.642097 0.018 Uiso 0.142(2) 1 calc R U P A 2 H8BB H 0.678337 0.608429 0.589669 0.018 Uiso 0.142(2) 1 calc R U P A 2 O1 O 0.76024(13) 0.6631(2) 0.75071(11) 0.0132(4) Uani 0.858(2) 1 d . . P A 1 O2 O 0.73779(11) 0.53640(18) 0.63339(9) 0.0157(4) Uani 0.858(2) 1 d . . P A 1 C2 C 0.61180(16) 0.5416(3) 0.72261(13) 0.0151(4) Uani 0.858(2) 1 d . . P A 1 H2A H 0.635968 0.464040 0.758171 0.018 Uiso 0.858(2) 1 calc R U P A 1 H2B H 0.541208 0.545983 0.722462 0.018 Uiso 0.858(2) 1 calc R U P A 1 C3 C 0.63759(15) 0.5129(2) 0.63959(13) 0.0175(5) Uani 0.858(2) 1 d . . P A 1 H3A H 0.621300 0.414030 0.625105 0.021 Uiso 0.858(2) 1 calc R U P A 1 H3B H 0.599228 0.575398 0.601942 0.021 Uiso 0.858(2) 1 calc R U P A 1 C5 C 0.70903(17) 0.7923(3) 0.63801(12) 0.0154(5) Uani 0.858(2) 1 d . U P A 1 H5A H 0.678363 0.772943 0.584114 0.019 Uiso 0.858(2) 1 calc R U P A 1 H5B H 0.746966 0.880297 0.637109 0.019 Uiso 0.858(2) 1 calc R U P A 1 C6 C 0.63317(16) 0.8037(3) 0.69746(13) 0.0151(4) Uani 0.858(2) 1 d . U P A 1 H6A H 0.638122 0.895390 0.725506 0.018 Uiso 0.858(2) 1 calc R U P A 1 H6B H 0.567539 0.793541 0.670517 0.018 Uiso 0.858(2) 1 calc R U P A 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0068(9) 0.0396(12) 0.0145(9) -0.0043(8) -0.0009(7) 0.0003(8) C4 0.0131(10) 0.0399(13) 0.0110(9) -0.0039(8) -0.0007(7) -0.0010(9) C7 0.0116(9) 0.0215(9) 0.0123(9) -0.0019(7) -0.0003(7) 0.0000(7) C8 0.0125(9) 0.0232(10) 0.0083(8) -0.0052(7) 0.0005(6) -0.0013(7) C9 0.0155(9) 0.0185(9) 0.0137(9) -0.0007(7) 0.0017(7) -0.0029(7) C10 0.0148(10) 0.0190(9) 0.0148(9) -0.0018(7) -0.0006(7) 0.0025(7) C11 0.0131(9) 0.0212(9) 0.0088(8) -0.0022(7) 0.0008(6) -0.0006(7) C12 0.0157(9) 0.0187(9) 0.0186(9) 0.0017(8) 0.0026(7) -0.0007(8) C13 0.0151(9) 0.0203(10) 0.0204(9) 0.0002(8) 0.0021(7) 0.0023(8) C14 0.0127(9) 0.0222(10) 0.0093(8) 0.0007(7) 0.0003(6) 0.0011(7) C15 0.0142(9) 0.0227(10) 0.0109(8) 0.0000(7) -0.0015(7) -0.0007(7) C16 0.0163(10) 0.0268(10) 0.0122(9) 0.0001(8) 0.0006(7) 0.0055(8) C17 0.0122(9) 0.0325(11) 0.0182(9) 0.0030(8) 0.0015(7) 0.0018(8) C18 0.0165(10) 0.0251(10) 0.0282(11) 0.0033(9) 0.0010(8) -0.0026(8) C19 0.0157(10) 0.0204(10) 0.0222(10) 0.0020(8) 0.0025(7) 0.0025(8) C20 0.0112(9) 0.0217(10) 0.0147(9) 0.0022(7) 0.0007(7) 0.0025(7) C21 0.0132(9) 0.0278(10) 0.0113(8) 0.0009(8) -0.0034(7) -0.0012(8) C22 0.0154(9) 0.0226(10) 0.0098(8) 0.0011(7) 0.0015(7) -0.0007(8) C23 0.0127(9) 0.0164(9) 0.0131(9) 0.0008(7) -0.0003(7) 0.0002(7) C24 0.0131(9) 0.0212(9) 0.0126(8) -0.0015(7) -0.0024(7) -0.0007(7) C25 0.0158(9) 0.0239(10) 0.0092(8) -0.0013(7) 0.0006(7) 0.0003(8) C26 0.0132(9) 0.0144(9) 0.0155(9) -0.0031(7) 0.0012(7) -0.0001(7) C27 0.0138(9) 0.0239(10) 0.0139(9) -0.0009(7) -0.0009(7) -0.0002(8) C28 0.0166(10) 0.0249(10) 0.0150(9) -0.0009(8) 0.0054(7) -0.0005(8) C29 0.0124(9) 0.0217(10) 0.0242(10) -0.0064(8) 0.0026(7) -0.0011(8) C30 0.0123(9) 0.0266(11) 0.0182(9) -0.0048(8) -0.0035(7) 0.0006(8) C31 0.0138(9) 0.0237(10) 0.0137(9) -0.0027(8) 0.0010(7) -0.0012(8) O1B 0.021(6) 0.015(6) 0.013(5) 0.000(5) -0.008(4) -0.009(6) O2B 0.0110(8) 0.0193(8) 0.0168(8) -0.0058(6) 0.0016(6) -0.0012(6) C2B 0.0117(8) 0.0190(9) 0.0145(8) -0.0002(6) 0.0005(6) 0.0014(6) C3B 0.0117(8) 0.0190(9) 0.0145(8) -0.0002(6) 0.0005(6) 0.0014(6) C6B 0.0117(8) 0.0190(9) 0.0145(8) -0.0002(6) 0.0005(6) 0.0014(6) C5B 0.0117(8) 0.0190(9) 0.0145(8) -0.0002(6) 0.0005(6) 0.0014(6) O1 0.0070(8) 0.0233(11) 0.0090(8) 0.0001(9) -0.0006(5) 0.0007(9) O2 0.0110(8) 0.0193(8) 0.0168(8) -0.0058(6) 0.0016(6) -0.0012(6) C2 0.0117(8) 0.0190(9) 0.0145(8) -0.0002(6) 0.0005(6) 0.0014(6) C3 0.0129(11) 0.0214(11) 0.0179(11) -0.0070(9) 0.0003(8) -0.0026(9) C5 0.0117(11) 0.0225(12) 0.0115(10) -0.0001(9) -0.0017(8) 0.0013(9) C6 0.0117(8) 0.0190(9) 0.0145(8) -0.0002(6) 0.0005(6) 0.0014(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_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C7 1.525(2) . ? C1 O1B 1.547(12) . ? C1 C2B 1.874(15) . ? C1 C6B 1.314(14) . ? C1 O1 1.464(3) . ? C1 C2 1.560(3) . ? C1 C6 1.493(3) . ? C4 C20 1.506(3) . ? C4 O1B 1.499(12) . ? C4 O2B 1.770(11) . ? C4 C5B 1.277(15) . ? C4 O1 1.427(3) . ? C4 O2 1.458(3) . ? C4 C5 1.512(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7 C8 1.516(2) . ? C8 C9 1.390(3) . ? C8 C13 1.394(3) . ? C9 H9 0.9500 . ? C9 C10 1.393(3) . ? C10 H10 0.9500 . ? C10 C11 1.391(3) . ? C11 C12 1.396(3) . ? C11 C14 1.500(2) . ? C12 H12 0.9500 . ? C12 C13 1.397(3) . ? C13 H13 0.9500 . ? C14 C15 1.392(3) . ? C14 C19 1.400(3) . ? C15 H15 0.9500 . ? C15 C16 1.400(3) . ? C16 H16 0.9500 . ? C16 C17 1.382(3) . ? C17 H17 0.9500 . ? C17 C18 1.382(3) . ? C18 H18 0.9500 . ? C18 C19 1.395(3) . ? C19 H19 0.9500 . ? C20 C21 1.389(3) . ? C20 C25 1.388(2) . ? C21 H21 0.9500 . ? C21 C22 1.384(3) . ? C22 H22 0.9500 . ? C22 C23 1.404(2) . ? C23 C24 1.394(3) . ? C23 C26 1.491(2) . ? C24 H24 0.9500 . ? C24 C25 1.391(3) . ? C25 H25 0.9500 . ? C26 C27 1.395(3) . ? C26 C31 1.397(2) . ? C27 H27 0.9500 . ? C27 C28 1.389(3) . ? C28 H28 0.9500 . ? C28 C29 1.386(3) . ? C29 H29 0.9500 . ? C29 C30 1.383(3) . ? C30 H30 0.9500 . ? C30 C31 1.392(3) . ? C31 H31 0.9500 . ? O2B C3B 1.466(15) . ? C2B H2BA 0.9900 . ? C2B H2BB 0.9900 . ? C2B C3B 1.521(18) . ? C3B H3BA 0.9900 . ? C3B H3BB 0.9900 . ? C6B H7BA 0.9900 . ? C6B H7BB 0.9900 . ? C6B C5B 1.48(2) . ? C5B H8BA 0.9900 . ? C5B H8BB 0.9900 . ? O2 C3 1.436(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C2 C3 1.518(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C5 C6 1.544(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? 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 C7 C1 O1B 103.7(5) . . ? C7 C1 C2B 101.3(5) . . ? C7 C1 C2 110.89(17) . . ? O1B C1 C2B 88.8(7) . . ? C6B C1 C7 136.2(7) . . ? C6B C1 O1B 111.2(8) . . ? C6B C1 C2B 105.0(8) . . ? O1 C1 C7 106.09(15) . . ? O1 C1 C2 103.93(16) . . ? O1 C1 C6 104.16(17) . . ? C6 C1 C7 117.55(18) . . ? C6 C1 C2 112.80(17) . . ? C20 C4 O2B 93.2(4) . . ? C20 C4 C5 117.28(18) . . ? O1B C4 C20 106.8(5) . . ? O1B C4 O2B 89.3(6) . . ? C5B C4 C20 131.6(8) . . ? C5B C4 O1B 115.5(8) . . ? C5B C4 O2B 109.2(7) . . ? O1 C4 C20 110.06(15) . . ? O1 C4 O2 107.35(17) . . ? O1 C4 C5 104.68(17) . . ? O2 C4 C20 105.29(16) . . ? O2 C4 C5 111.88(16) . . ? C1 C7 H7A 108.8 . . ? C1 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? C8 C7 C1 113.79(14) . . ? C8 C7 H7A 108.8 . . ? C8 C7 H7B 108.8 . . ? C9 C8 C7 120.96(17) . . ? C9 C8 C13 118.08(17) . . ? C13 C8 C7 120.96(17) . . ? C8 C9 H9 119.5 . . ? C8 C9 C10 120.98(17) . . ? C10 C9 H9 119.5 . . ? C9 C10 H10 119.4 . . ? C11 C10 C9 121.22(17) . . ? C11 C10 H10 119.4 . . ? C10 C11 C12 117.92(17) . . ? C10 C11 C14 120.87(16) . . ? C12 C11 C14 121.21(17) . . ? C11 C12 H12 119.6 . . ? C11 C12 C13 120.81(18) . . ? C13 C12 H12 119.6 . . ? C8 C13 C12 120.98(17) . . ? C8 C13 H13 119.5 . . ? C12 C13 H13 119.5 . . ? C15 C14 C11 121.08(17) . . ? C15 C14 C19 118.31(17) . . ? C19 C14 C11 120.60(16) . . ? C14 C15 H15 119.6 . . ? C14 C15 C16 120.83(18) . . ? C16 C15 H15 119.6 . . ? C15 C16 H16 120.0 . . ? C17 C16 C15 120.07(18) . . ? C17 C16 H16 120.0 . . ? C16 C17 H17 120.1 . . ? C16 C17 C18 119.84(19) . . ? C18 C17 H17 120.1 . . ? C17 C18 H18 119.9 . . ? C17 C18 C19 120.30(19) . . ? C19 C18 H18 119.9 . . ? C14 C19 H19 119.7 . . ? C18 C19 C14 120.64(18) . . ? C18 C19 H19 119.7 . . ? C21 C20 C4 119.13(16) . . ? C25 C20 C4 122.04(17) . . ? C25 C20 C21 118.83(17) . . ? C20 C21 H21 119.7 . . ? C22 C21 C20 120.61(16) . . ? C22 C21 H21 119.7 . . ? C21 C22 H22 119.5 . . ? C21 C22 C23 121.03(17) . . ? C23 C22 H22 119.5 . . ? C22 C23 C26 120.62(16) . . ? C24 C23 C22 117.94(17) . . ? C24 C23 C26 121.42(16) . . ? C23 C24 H24 119.6 . . ? C25 C24 C23 120.76(16) . . ? C25 C24 H24 119.6 . . ? C20 C25 C24 120.83(17) . . ? C20 C25 H25 119.6 . . ? C24 C25 H25 119.6 . . ? C27 C26 C23 120.90(16) . . ? C27 C26 C31 117.67(17) . . ? C31 C26 C23 121.42(17) . . ? C26 C27 H27 119.4 . . ? C28 C27 C26 121.22(17) . . ? C28 C27 H27 119.4 . . ? C27 C28 H28 119.8 . . ? C29 C28 C27 120.43(17) . . ? C29 C28 H28 119.8 . . ? C28 C29 H29 120.4 . . ? C30 C29 C28 119.14(18) . . ? C30 C29 H29 120.4 . . ? C29 C30 H30 119.8 . . ? C29 C30 C31 120.45(17) . . ? C31 C30 H30 119.8 . . ? C26 C31 H31 119.5 . . ? C30 C31 C26 121.08(17) . . ? C30 C31 H31 119.5 . . ? C4 O1B C1 96.2(6) . . ? C3B O2B C4 108.3(8) . . ? C1 C2B H2BA 110.0 . . ? C1 C2B H2BB 110.0 . . ? H2BA C2B H2BB 108.4 . . ? C3B C2B C1 108.4(10) . . ? C3B C2B H2BA 110.0 . . ? C3B C2B H2BB 110.0 . . ? O2B C3B C2B 112.2(10) . . ? O2B C3B H3BA 109.2 . . ? O2B C3B H3BB 109.2 . . ? C2B C3B H3BA 109.2 . . ? C2B C3B H3BB 109.2 . . ? H3BA C3B H3BB 107.9 . . ? C1 C6B H7BA 110.0 . . ? C1 C6B H7BB 110.0 . . ? C1 C6B C5B 108.4(11) . . ? H7BA C6B H7BB 108.4 . . ? C5B C6B H7BA 110.0 . . ? C5B C6B H7BB 110.0 . . ? C4 C5B C6B 107.0(12) . . ? C4 C5B H8BA 110.3 . . ? C4 C5B H8BB 110.3 . . ? C6B C5B H8BA 110.3 . . ? C6B C5B H8BB 110.3 . . ? H8BA C5B H8BB 108.6 . . ? C4 O1 C1 103.30(15) . . ? C3 O2 C4 112.54(16) . . ? C1 C2 H2A 109.7 . . ? C1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? C3 C2 C1 109.78(19) . . ? C3 C2 H2A 109.7 . . ? C3 C2 H2B 109.7 . . ? O2 C3 C2 111.56(17) . . ? O2 C3 H3A 109.3 . . ? O2 C3 H3B 109.3 . . ? C2 C3 H3A 109.3 . . ? C2 C3 H3B 109.3 . . ? H3A C3 H3B 108.0 . . ? C4 C5 H5A 110.9 . . ? C4 C5 H5B 110.9 . . ? C4 C5 C6 104.05(18) . . ? H5A C5 H5B 109.0 . . ? C6 C5 H5A 110.9 . . ? C6 C5 H5B 110.9 . . ? C1 C6 C5 103.77(18) . . ? C1 C6 H6A 111.0 . . ? C1 C6 H6B 111.0 . . ? C5 C6 H6A 111.0 . . ? C5 C6 H6B 111.0 . . ? H6A C6 H6B 109.0 . . ? 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 C1 C7 C8 C9 -80.2(2) . . . . ? C1 C7 C8 C13 100.0(2) . . . . ? C1 C2B C3B O2B -50.5(13) . . . . ? C1 C6B C5B C4 1.6(15) . . . . ? C1 C2 C3 O2 46.6(2) . . . . ? C4 C20 C21 C22 179.82(18) . . . . ? C4 C20 C25 C24 -179.19(18) . . . . ? C4 O2B C3B C2B 54.6(12) . . . . ? C4 O2 C3 C2 -47.6(2) . . . . ? C4 C5 C6 C1 -2.4(2) . . . . ? C7 C1 O1B C4 165.6(5) . . . . ? C7 C1 C2B C3B 166.9(8) . . . . ? C7 C1 C6B C5B -150.0(8) . . . . ? C7 C1 O1 C4 -169.06(17) . . . . ? C7 C1 C2 C3 -173.23(16) . . . . ? C7 C1 C6 C5 144.68(17) . . . . ? C7 C8 C9 C10 178.69(16) . . . . ? C7 C8 C13 C12 -179.55(16) . . . . ? C8 C9 C10 C11 1.2(3) . . . . ? C9 C8 C13 C12 0.7(3) . . . . ? C9 C10 C11 C12 0.1(3) . . . . ? C9 C10 C11 C14 179.83(16) . . . . ? C10 C11 C12 C13 -0.9(3) . . . . ? C10 C11 C14 C15 -27.1(3) . . . . ? C10 C11 C14 C19 152.13(18) . . . . ? C11 C12 C13 C8 0.6(3) . . . . ? C11 C14 C15 C16 179.08(16) . . . . ? C11 C14 C19 C18 -179.87(16) . . . . ? C12 C11 C14 C15 152.61(17) . . . . ? C12 C11 C14 C19 -28.1(3) . . . . ? C13 C8 C9 C10 -1.5(3) . . . . ? C14 C11 C12 C13 179.31(16) . . . . ? C14 C15 C16 C17 1.0(3) . . . . ? C15 C14 C19 C18 -0.6(3) . . . . ? C15 C16 C17 C18 -1.1(3) . . . . ? C16 C17 C18 C19 0.3(3) . . . . ? C17 C18 C19 C14 0.6(3) . . . . ? C19 C14 C15 C16 -0.2(3) . . . . ? C20 C4 O1B C1 -167.9(4) . . . . ? C20 C4 O2B C3B -179.7(7) . . . . ? C20 C4 C5B C6B 155.9(7) . . . . ? C20 C4 O1 C1 169.47(17) . . . . ? C20 C4 O2 C3 -179.75(15) . . . . ? C20 C4 C5 C6 -146.77(18) . . . . ? C20 C21 C22 C23 -0.4(3) . . . . ? C21 C20 C25 C24 0.4(3) . . . . ? C21 C22 C23 C24 0.0(3) . . . . ? C21 C22 C23 C26 178.60(17) . . . . ? C22 C23 C24 C25 0.7(3) . . . . ? C22 C23 C26 C27 21.7(3) . . . . ? C22 C23 C26 C31 -157.43(18) . . . . ? C23 C24 C25 C20 -0.8(3) . . . . ? C23 C26 C27 C28 -178.62(17) . . . . ? C23 C26 C31 C30 178.76(17) . . . . ? C24 C23 C26 C27 -159.74(19) . . . . ? C24 C23 C26 C31 21.2(3) . . . . ? C25 C20 C21 C22 0.2(3) . . . . ? C26 C23 C24 C25 -177.97(17) . . . . ? C26 C27 C28 C29 -0.1(3) . . . . ? C27 C26 C31 C30 -0.4(3) . . . . ? C27 C28 C29 C30 -0.5(3) . . . . ? C28 C29 C30 C31 0.6(3) . . . . ? C29 C30 C31 C26 -0.2(3) . . . . ? C31 C26 C27 C28 0.5(3) . . . . ? O1B C1 C7 C8 163.8(5) . . . . ? O1B C1 C2B C3B 63.2(10) . . . . ? O1B C1 C6B C5B -9.6(13) . . . . ? O1B C4 C20 C21 -165.1(5) . . . . ? O1B C4 C20 C25 14.5(6) . . . . ? O1B C4 O2B C3B -73.0(8) . . . . ? O1B C4 C5B C6B 7.6(14) . . . . ? O2B C4 C20 C21 -74.9(4) . . . . ? O2B C4 C20 C25 104.7(3) . . . . ? O2B C4 O1B C1 99.0(7) . . . . ? O2B C4 C5B C6B -91.2(11) . . . . ? C2B C1 C7 C8 72.3(5) . . . . ? C2B C1 O1B C4 -93.0(7) . . . . ? C2B C1 C6B C5B 85.0(11) . . . . ? C6B C1 C7 C8 -53.9(9) . . . . ? C6B C1 O1B C4 12.6(11) . . . . ? C6B C1 C2B C3B -48.4(11) . . . . ? C5B C4 C20 C21 44.6(9) . . . . ? C5B C4 C20 C25 -135.9(9) . . . . ? C5B C4 O1B C1 -12.1(12) . . . . ? C5B C4 O2B C3B 43.9(11) . . . . ? O1 C1 C7 C8 -169.38(16) . . . . ? O1 C1 C2 C3 -59.6(2) . . . . ? O1 C1 C6 C5 27.7(2) . . . . ? O1 C4 C20 C21 166.82(19) . . . . ? O1 C4 C20 C25 -13.6(3) . . . . ? O1 C4 O2 C3 63.0(2) . . . . ? O1 C4 C5 C6 -24.5(2) . . . . ? O2 C4 C20 C21 51.4(2) . . . . ? O2 C4 C20 C25 -129.00(18) . . . . ? O2 C4 O1 C1 -76.4(2) . . . . ? O2 C4 C5 C6 91.44(19) . . . . ? C2 C1 C7 C8 -57.2(2) . . . . ? C2 C1 O1 C4 74.0(2) . . . . ? C2 C1 C6 C5 -84.4(2) . . . . ? C5 C4 C20 C21 -73.7(2) . . . . ? C5 C4 C20 C25 105.9(2) . . . . ? C5 C4 O1 C1 42.6(2) . . . . ? C5 C4 O2 C3 -51.3(2) . . . . ? C6 C1 C7 C8 74.7(2) . . . . ? C6 C1 O1 C4 -44.4(2) . . . . ? C6 C1 C2 C3 52.5(2) . . . . ? _shelx_res_file ; TITL eds_111703_0m_a.res in P2(1)/n asb-achiralketal-biphenyl.res created by SHELXL-2018/3 at 18:46:52 on 31-Jul-2020 REM Old TITL eds_111703_0m_a.res in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.144, Rweak 0.005, Alpha 0.037, Orientation as input REM Formula found by SHELXT: C30 O2 CELL 0.71073 14.0147 9.4761 17.0238 90 95.826 90 ZERR 4 0.0021 0.0009 0.0018 0 0.006 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H O UNIT 124 112 8 DELU C6B C6 SIMU 0.02 0.08 1.7 C6B C5B C5 C6 EADP C6B C6 EADP C2 C2B EADP O2 O2B EADP C6B C2B C3B C5B EADP C6B C5B C2B C3B L.S. 20 0 0 PLAN 5 SIZE 0.04 0.03 0.01 TEMP -183.15 CONF BOND $H list 4 MORE -1 fmap 2 53 acta REM REM REM WGHT 0.018100 1.205500 FVAR 0.12569 0.85791 C1 1 0.657086 0.684302 0.753181 11.00000 0.00675 0.03956 = 0.01447 -0.00428 -0.00085 0.00028 C4 1 0.771537 0.669988 0.668450 11.00000 0.01313 0.03993 = 0.01103 -0.00389 -0.00074 -0.00103 C7 1 0.642498 0.707300 0.839785 11.00000 0.01163 0.02152 = 0.01235 -0.00192 -0.00028 0.00003 AFIX 23 H7A 2 0.677731 0.633121 0.871785 11.00000 -1.20000 H7B 2 0.670586 0.799516 0.856891 11.00000 -1.20000 AFIX 0 C8 1 0.538246 0.704604 0.856295 11.00000 0.01251 0.02320 = 0.00833 -0.00520 0.00049 -0.00129 C9 1 0.479797 0.822078 0.841538 11.00000 0.01549 0.01847 = 0.01366 -0.00073 0.00173 -0.00290 AFIX 43 H9 2 0.505908 0.905922 0.821842 11.00000 -1.20000 AFIX 0 C10 1 0.383464 0.818699 0.855204 11.00000 0.01479 0.01904 = 0.01476 -0.00177 -0.00065 0.00246 AFIX 43 H10 2 0.344688 0.899796 0.843728 11.00000 -1.20000 AFIX 0 C11 1 0.343021 0.698750 0.885345 11.00000 0.01310 0.02123 = 0.00877 -0.00216 0.00078 -0.00062 C12 1 0.402048 0.581479 0.901668 11.00000 0.01575 0.01865 = 0.01862 0.00171 0.00259 -0.00068 AFIX 43 H12 2 0.376440 0.498730 0.923036 11.00000 -1.20000 AFIX 0 C13 1 0.498307 0.584348 0.886960 11.00000 0.01512 0.02025 = 0.02038 0.00024 0.00207 0.00229 AFIX 43 H13 2 0.537120 0.503156 0.898018 11.00000 -1.20000 AFIX 0 C14 1 0.239332 0.696144 0.900084 11.00000 0.01266 0.02224 = 0.00932 0.00073 0.00033 0.00109 C15 1 0.191278 0.819601 0.916444 11.00000 0.01420 0.02271 = 0.01087 0.00003 -0.00151 -0.00074 AFIX 43 H15 2 0.224833 0.906854 0.919098 11.00000 -1.20000 AFIX 0 C16 1 0.094152 0.816787 0.929033 11.00000 0.01630 0.02683 = 0.01224 0.00008 0.00057 0.00554 AFIX 43 H16 2 0.061957 0.902022 0.939299 11.00000 -1.20000 AFIX 0 C17 1 0.045031 0.690165 0.926546 11.00000 0.01216 0.03248 = 0.01824 0.00299 0.00149 0.00184 AFIX 43 H17 2 -0.020617 0.688042 0.935963 11.00000 -1.20000 AFIX 0 C18 1 0.091627 0.566643 0.910329 11.00000 0.01650 0.02511 = 0.02820 0.00334 0.00101 -0.00264 AFIX 43 H18 2 0.057794 0.479637 0.908392 11.00000 -1.20000 AFIX 0 C19 1 0.188126 0.569129 0.896790 11.00000 0.01571 0.02039 = 0.02218 0.00196 0.00250 0.00246 AFIX 43 H19 2 0.219389 0.483773 0.885220 11.00000 -1.20000 AFIX 0 C20 1 0.876409 0.677117 0.656387 11.00000 0.01117 0.02174 = 0.01470 0.00217 0.00068 0.00250 C21 1 0.904125 0.655218 0.581273 11.00000 0.01325 0.02779 = 0.01132 0.00093 -0.00342 -0.00119 AFIX 43 H21 2 0.856924 0.635804 0.538561 11.00000 -1.20000 AFIX 0 C22 1 0.999891 0.661427 0.568093 11.00000 0.01538 0.02262 = 0.00976 0.00113 0.00147 -0.00073 AFIX 43 H22 2 1.017602 0.645584 0.516413 11.00000 -1.20000 AFIX 0 C23 1 1.071236 0.690762 0.629886 11.00000 0.01270 0.01645 = 0.01311 0.00076 -0.00030 0.00023 C24 1 1.042661 0.713540 0.704956 11.00000 0.01307 0.02119 = 0.01259 -0.00148 -0.00238 -0.00070 AFIX 43 H24 2 1.089464 0.734563 0.747699 11.00000 -1.20000 AFIX 0 C25 1 0.946427 0.705837 0.717977 11.00000 0.01575 0.02393 = 0.00919 -0.00125 0.00059 0.00034 AFIX 43 H25 2 0.928375 0.720410 0.769664 11.00000 -1.20000 AFIX 0 C26 1 1.174357 0.693988 0.615459 11.00000 0.01319 0.01438 = 0.01550 -0.00307 0.00125 -0.00012 C27 1 1.201332 0.715454 0.539730 11.00000 0.01378 0.02394 = 0.01389 -0.00086 -0.00085 -0.00018 AFIX 43 H27 2 1.153242 0.730244 0.497045 11.00000 -1.20000 AFIX 0 C28 1 1.297193 0.715609 0.525568 11.00000 0.01664 0.02488 = 0.01503 -0.00093 0.00538 -0.00049 AFIX 43 H28 2 1.313913 0.730321 0.473490 11.00000 -1.20000 AFIX 0 C29 1 1.368647 0.694433 0.586937 11.00000 0.01235 0.02172 = 0.02417 -0.00635 0.00255 -0.00111 AFIX 43 H29 2 1.434196 0.693785 0.577182 11.00000 -1.20000 AFIX 0 C30 1 1.343249 0.674257 0.662569 11.00000 0.01235 0.02656 = 0.01822 -0.00482 -0.00345 0.00063 AFIX 43 H30 2 1.391711 0.660633 0.705106 11.00000 -1.20000 AFIX 0 C31 1 1.247197 0.673784 0.676759 11.00000 0.01381 0.02366 = 0.01372 -0.00267 0.00101 -0.00124 AFIX 43 H31 2 1.230891 0.659487 0.728991 11.00000 -1.20000 AFIX 0 PART 2 O1B 3 0.761137 0.734711 0.747480 -21.00000 0.02078 0.01517 = 0.01316 -0.00020 -0.00772 -0.00876 O2B 3 0.746330 0.836301 0.623762 -21.00000 0.01098 0.01929 = 0.01678 -0.00579 0.00155 -0.00120 C2B 1 0.613223 0.856225 0.708618 -21.00000 0.01166 0.01904 = 0.01445 -0.00025 0.00048 0.00141 AFIX 23 H2BA 2 0.542462 0.861288 0.706639 -21.00000 -1.20000 H2BB 2 0.640813 0.935762 0.741109 -21.00000 -1.20000 AFIX 0 C3B 1 0.643905 0.865861 0.625611 -21.00000 0.01166 0.01904 = 0.01445 -0.00025 0.00048 0.00141 AFIX 23 H3BA 2 0.606136 0.797695 0.591065 -21.00000 -1.20000 H3BB 2 0.629731 0.961724 0.604434 -21.00000 -1.20000 AFIX 0 C6B 1 0.631429 0.588959 0.699086 -21.00000 0.01166 0.01904 = 0.01445 -0.00025 0.00048 0.00141 AFIX 23 H7BA 2 0.568855 0.614666 0.670387 -21.00000 -1.20000 H7BB 2 0.624798 0.495703 0.724178 -21.00000 -1.20000 AFIX 0 C5B 1 0.705952 0.582567 0.643582 -21.00000 0.01166 0.01904 = 0.01445 -0.00025 0.00048 0.00141 AFIX 23 H8BA 2 0.732630 0.485978 0.642097 -21.00000 -1.20000 H8BB 2 0.678337 0.608429 0.589669 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 O1 3 0.760236 0.663070 0.750712 21.00000 0.00696 0.02326 = 0.00896 0.00014 -0.00059 0.00071 O2 3 0.737792 0.536402 0.633392 21.00000 0.01098 0.01929 = 0.01678 -0.00579 0.00155 -0.00120 C2 1 0.611805 0.541628 0.722611 21.00000 0.01166 0.01904 = 0.01445 -0.00025 0.00048 0.00141 AFIX 23 H2A 2 0.635968 0.464040 0.758171 21.00000 -1.20000 H2B 2 0.541208 0.545983 0.722462 21.00000 -1.20000 AFIX 0 C3 1 0.637589 0.512946 0.639591 21.00000 0.01291 0.02139 = 0.01785 -0.00697 0.00031 -0.00255 AFIX 23 H3A 2 0.621300 0.414030 0.625105 21.00000 -1.20000 H3B 2 0.599228 0.575398 0.601942 21.00000 -1.20000 AFIX 0 C5 1 0.709026 0.792291 0.638011 21.00000 0.01174 0.02247 = 0.01153 -0.00007 -0.00171 0.00135 AFIX 23 H5A 2 0.678363 0.772943 0.584114 21.00000 -1.20000 H5B 2 0.746966 0.880297 0.637109 21.00000 -1.20000 AFIX 0 C6 1 0.633168 0.803749 0.697464 21.00000 0.01166 0.01904 = 0.01445 -0.00025 0.00048 0.00141 AFIX 23 H6A 2 0.638122 0.895390 0.725506 21.00000 -1.20000 H6B 2 0.567539 0.793541 0.670517 21.00000 -1.20000 AFIX 0 HKLF 4 REM eds_111703_0m_a.res in P2(1)/n REM wR2 = 0.166175, GooF = S = 1.07923, Restrained GooF = 1.07773 for all data REM R1 = 0.059259 for 3661 Fo > 4sig(Fo) and 0.072597 for all 4604 data REM 317 parameters refined using 12 restraints END WGHT 0.0181 1.2054 REM Highest difference peak 0.324, deepest hole -0.364, 1-sigma level 0.066 Q1 1 0.6462 0.7595 0.7395 11.00000 0.05 0.32 Q2 1 0.8388 0.7008 0.7626 11.00000 0.05 0.26 Q3 1 1.0544 0.6507 0.6677 11.00000 0.05 0.26 Q4 1 1.0044 0.6587 0.7165 11.00000 0.05 0.26 Q5 1 1.2403 0.6735 0.5231 11.00000 0.05 0.24 ; _shelx_res_checksum 83697 _shelx_hkl_file ; 0 0 -2 73.33 0.86 1 0 0 -2 48.27 0.38 2 0 0 -2 53.35 0.42 3 0 0 2 42.46 0.36 2 0 0 2 50.46 0.44 3 0 0 -3 0.04 0.05 1 0 0 -3 0.08 0.07 2 0 0 -3 0.02 0.05 3 0 0 3 -0.02 0.05 1 0 0 3 -0.02 0.07 2 0 0 3 0.03 0.05 3 0 0 -4 990.45 15.78 1 0 0 -4 629.22 4.55 2 0 0 -4 670.47 4.02 3 0 0 4 919.47 13.33 1 0 0 4 554.66 4.23 2 0 0 4 655.66 3.90 3 0 0 -5 0.11 0.07 1 0 0 -5 0.14 0.11 2 0 0 -5 0.18 0.07 3 0 0 5 0.08 0.07 1 0 0 5 0.14 0.10 2 0 0 5 0.13 0.08 3 0 0 -6 102.28 0.79 1 0 0 -6 65.87 0.78 2 0 0 -6 71.12 0.63 3 0 0 6 89.55 0.74 1 0 0 6 53.80 0.72 2 0 0 6 64.87 0.61 3 0 0 -7 0.31 0.09 1 0 0 -7 0.20 0.13 2 0 0 7 0.17 0.09 1 0 0 7 0.11 0.12 2 0 0 7 0.13 0.08 3 0 0 -8 40.80 0.58 1 0 0 -8 27.08 0.60 2 0 0 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0.38 2 0 -1 -3 30.36 0.39 3 0 -1 3 48.67 0.50 1 0 -1 3 41.60 0.47 2 0 -1 3 40.86 0.29 3 0 1 -3 49.29 0.50 1 0 1 -3 40.93 0.47 2 0 1 -3 43.82 0.30 3 0 1 3 30.15 0.20 1 0 1 3 24.94 0.36 2 0 -1 -4 112.96 0.84 1 0 -1 -4 62.87 0.64 2 0 -1 -4 76.55 0.66 3 0 -1 4 115.70 0.84 1 0 -1 4 83.52 0.75 2 0 -1 4 91.32 0.49 3 0 1 -4 122.41 1.43 1 0 1 -4 93.29 0.79 2 0 1 -4 98.64 0.51 3 0 1 4 80.24 0.42 1 0 1 4 60.84 0.63 2 0 -1 -5 83.77 0.51 1 0 -1 -5 43.63 0.60 2 0 -1 -5 53.65 0.60 3 0 -1 5 81.76 0.76 1 0 -1 5 53.55 0.66 2 0 -1 5 62.21 0.46 3 0 1 -5 88.33 0.79 1 0 1 -5 66.97 0.74 2 0 1 -5 72.37 0.49 3 0 1 5 66.38 0.46 1 0 1 5 42.00 0.58 2 0 1 5 55.76 0.61 3 0 -1 -6 145.34 1.31 1 0 -1 -6 77.09 0.86 2 0 -1 -6 93.11 0.84 3 0 -1 6 141.01 1.07 1 0 -1 6 93.70 0.95 2 0 -1 6 101.60 0.65 3 0 1 -6 148.17 1.09 1 0 1 -6 121.37 1.08 2 0 1 -6 132.50 0.74 3 0 1 6 114.69 0.69 1 0 1 6 81.72 0.88 2 0 1 6 91.63 0.83 3 0 -1 -7 8.51 0.22 1 0 -1 -7 4.89 0.28 2 0 -1 -7 6.47 0.26 3 0 -1 7 8.16 0.31 1 0 -1 7 6.32 0.20 3 0 1 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18.64 0.57 1 0 1 -13 15.02 0.62 2 0 1 -13 16.08 0.44 3 0 -1 -14 7.45 0.34 1 0 -1 -14 4.09 0.42 2 0 -1 -14 5.46 0.35 3 0 1 -14 7.39 0.41 1 0 1 -14 4.98 0.43 2 0 1 -14 5.63 0.31 3 0 -1 -15 6.89 0.34 1 0 -1 -15 4.22 0.45 2 0 -1 -15 5.19 0.36 3 0 1 -15 6.77 0.40 1 0 1 -15 4.76 0.44 2 0 1 -15 5.05 0.30 3 0 -1 -16 0.69 0.16 1 0 -1 -16 0.69 0.27 2 0 -1 -16 0.52 0.19 3 0 1 -16 0.63 0.20 1 0 1 -16 0.50 0.24 2 0 1 -16 0.49 0.16 3 0 -1 -17 0.41 0.26 2 0 -1 -17 0.28 0.19 3 0 1 -17 0.48 0.19 1 0 1 -17 0.37 0.24 2 0 1 -17 0.57 0.25 3 0 -1 -18 1.23 0.34 2 0 -1 -18 1.24 0.26 3 0 1 -18 1.67 0.28 1 0 1 -18 1.12 0.31 2 0 -1 -19 2.75 0.43 2 0 1 -19 4.05 0.50 2 0 -1 -20 0.14 0.27 2 0 1 -20 0.23 0.24 2 0 -1 -21 2.65 0.46 2 0 1 -21 2.88 0.47 2 0 -2 0 1356.84 19.28 1 0 -2 0 1245.47 16.72 2 0 2 0 1428.18 20.38 1 0 2 0 1192.45 14.53 2 0 -2 -1 657.08 11.03 1 0 -2 -1 344.76 2.99 2 0 -2 1 698.09 4.92 1 0 -2 1 619.10 4.12 2 0 2 -1 687.07 4.81 1 0 2 -1 602.97 4.14 2 0 -2 -2 6.59 0.14 1 0 -2 -2 12.22 0.18 1 0 -2 -2 5.43 0.20 2 0 -2 2 11.94 0.29 1 0 -2 2 10.59 0.26 2 0 2 -2 12.07 0.29 1 0 2 -2 10.96 0.27 2 0 2 2 6.13 0.20 2 0 -2 -3 57.73 0.31 1 0 -2 -3 57.10 0.61 2 0 -2 -3 68.29 0.69 3 0 -2 3 113.44 0.90 1 0 -2 3 96.91 0.80 2 0 -2 3 108.65 0.61 3 0 2 -3 115.55 1.78 1 0 2 -3 100.08 0.81 2 0 2 3 54.63 0.59 2 0 -2 -4 1.75 0.07 1 0 -2 -4 1.34 0.16 2 0 -2 -4 1.61 0.17 3 0 -2 4 2.41 0.20 1 0 -2 4 1.95 0.17 2 0 -2 4 2.11 0.11 3 0 2 -4 2.49 0.19 1 0 2 -4 1.95 0.18 2 0 2 4 1.55 0.06 1 0 2 4 1.40 0.15 2 0 -2 -5 6.84 0.11 1 0 -2 -5 3.76 0.22 2 0 -2 -5 4.62 0.24 3 0 -2 5 8.56 0.31 1 0 -2 5 7.23 0.29 2 0 -2 5 7.28 0.18 3 0 2 -5 7.95 0.29 1 0 2 -5 7.83 0.30 2 0 2 -5 8.24 0.19 3 0 2 5 4.44 0.09 1 0 2 5 4.17 0.22 2 0 -2 -6 7.80 0.14 1 0 -2 -6 4.81 0.26 2 0 -2 -6 5.17 0.26 3 0 -2 6 7.11 0.31 1 0 -2 6 5.17 0.28 2 0 -2 6 5.54 0.17 3 0 2 -6 7.59 0.31 1 0 2 -6 6.47 0.30 2 0 2 6 4.89 0.12 1 0 2 6 4.34 0.24 2 0 -2 -7 61.68 0.44 1 0 -2 -7 31.51 0.62 2 0 -2 -7 37.50 0.64 3 0 -2 7 49.00 0.47 3 0 2 -7 64.37 0.86 1 0 2 -7 51.49 0.80 2 0 2 -7 57.66 0.51 3 0 2 7 33.52 0.33 1 0 -2 -8 11.45 0.23 1 0 -2 -8 5.75 0.32 2 0 -2 -8 7.00 0.32 3 0 -2 8 7.76 0.22 3 0 2 -8 10.80 0.39 1 0 2 -8 9.42 0.40 2 0 2 -8 10.14 0.24 3 0 2 8 6.07 0.17 1 0 -2 -9 0.89 0.10 1 0 -2 -9 0.46 0.16 2 0 -2 -9 0.71 0.17 3 0 -2 9 0.32 0.09 3 0 2 -9 0.58 0.15 1 0 2 -9 0.52 0.16 2 0 2 -9 0.47 0.09 3 0 2 9 0.53 0.08 1 0 -2 -10 22.61 0.37 1 0 -2 -10 12.44 0.49 2 0 -2 -10 15.92 0.49 3 0 -2 10 14.88 0.33 3 0 2 -10 21.32 0.58 1 0 2 -10 16.66 0.55 2 0 2 -10 20.28 0.37 3 0 2 10 13.50 0.29 1 0 -2 -11 0.19 0.08 1 0 -2 -11 0.08 0.16 2 0 -2 -11 0.18 0.13 3 0 -2 11 0.11 0.08 3 0 2 -11 0.03 0.13 1 0 2 -11 0.14 0.16 2 0 2 -11 0.05 0.09 3 0 2 11 0.11 0.08 1 0 -2 -12 13.59 0.34 1 0 -2 -12 8.08 0.47 2 0 -2 -12 8.28 0.41 3 0 -2 12 7.87 0.28 3 0 2 -12 14.02 0.53 1 0 2 -12 10.05 0.51 2 0 2 -12 11.67 0.32 3 0 2 12 7.70 0.27 1 0 -2 -13 29.74 0.52 1 0 -2 -13 17.17 0.67 2 0 -2 -13 18.21 0.58 3 0 -2 13 16.58 0.40 3 0 2 -13 27.11 0.74 1 0 2 -13 22.39 0.75 2 0 2 -13 24.14 0.47 3 0 2 13 16.31 0.39 1 0 -2 -14 0.40 0.11 1 0 -2 -14 0.00 0.20 2 0 -2 -14 0.22 0.17 3 0 2 -14 0.28 0.17 1 0 2 -14 0.31 0.20 2 0 2 -14 0.21 0.12 3 0 -2 -15 2.22 0.20 1 0 -2 -15 1.21 0.29 2 0 -2 -15 1.71 0.27 3 0 2 -15 2.35 0.32 1 0 2 -15 1.96 0.33 2 0 2 -15 2.17 0.21 3 0 -2 -16 0.58 0.26 2 0 -2 -16 0.64 0.22 3 0 2 -16 0.86 0.23 1 0 2 -16 0.90 0.27 2 0 -2 -17 1.40 0.35 2 0 -2 -17 2.03 0.31 3 0 2 -17 3.14 0.36 1 0 2 -17 2.31 0.39 2 0 -2 -18 1.60 0.36 2 0 -2 -18 1.54 0.30 3 0 2 -18 1.76 0.30 1 0 2 -18 1.48 0.34 2 0 -2 -19 0.75 0.32 2 0 -2 -19 0.35 0.23 3 0 2 -19 0.91 0.26 1 0 2 -19 0.76 0.31 2 0 -2 -20 0.05 0.27 2 0 2 -20 0.26 0.27 2 0 -3 0 0.04 0.07 1 0 -3 0 0.11 0.08 2 0 3 0 0.03 0.08 1 0 3 0 0.05 0.08 2 0 -3 -1 198.07 1.75 1 0 -3 -1 99.73 0.84 2 0 -3 -1 170.51 1.09 2 0 -3 1 202.55 2.27 1 0 -3 1 171.71 1.10 2 0 3 -1 201.58 5.28 1 0 3 -1 174.42 1.11 2 0 -3 -2 22.26 0.32 1 0 -3 -2 32.52 0.38 1 0 -3 -2 15.69 0.36 2 0 -3 2 32.74 0.53 1 0 -3 2 29.05 0.48 2 0 3 -2 33.34 0.54 1 0 3 -2 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136.58 1.31 2 -1 1 -3 144.77 0.95 3 1 -1 3 153.23 1.49 1 1 -1 3 125.55 0.85 2 1 -1 3 130.41 0.70 3 1 1 3 84.89 0.32 1 1 1 3 159.91 0.89 1 1 1 3 100.10 0.74 3 -1 -1 -4 3.81 0.19 2 -1 -1 -4 4.58 0.20 3 -1 1 -4 7.98 0.25 1 -1 1 -4 6.31 0.25 2 -1 1 -4 6.10 0.19 3 1 -1 4 7.10 0.24 1 1 -1 4 5.81 0.24 2 1 -1 4 5.66 0.18 3 1 1 4 4.61 0.11 1 1 1 4 7.22 0.14 1 1 1 4 4.17 0.19 2 1 1 4 4.62 0.21 3 -1 -1 -5 307.81 2.61 2 -1 -1 -5 364.06 3.50 3 -1 1 -5 617.83 5.07 1 -1 1 -5 449.80 3.82 2 -1 1 -5 457.33 2.99 3 1 -1 5 559.31 4.69 1 1 -1 5 380.09 7.97 2 1 -1 5 426.41 3.17 3 1 1 5 526.87 2.89 1 1 1 5 286.08 1.49 2 1 1 5 351.63 2.41 3 -1 -1 -6 17.14 0.27 1 -1 -1 -6 10.59 0.35 2 -1 -1 -6 10.61 0.32 3 -1 1 -6 17.57 0.40 1 -1 1 -6 13.00 0.39 2 -1 1 -6 13.53 0.30 3 1 -1 6 16.21 0.38 1 1 -1 6 10.69 0.36 2 1 -1 6 13.05 0.30 3 1 1 6 15.77 0.26 1 1 1 6 8.77 0.32 2 1 1 6 10.44 0.32 3 -1 -1 -7 5.80 0.19 1 -1 -1 -7 3.52 0.25 2 -1 -1 -7 3.32 0.22 3 -1 1 -7 6.51 0.28 1 -1 1 -7 5.29 0.30 2 -1 1 -7 5.49 0.22 3 1 -1 7 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0.61 0.11 2 -1 2 3 0.41 0.07 1 -1 2 3 0.39 0.10 2 1 -2 -3 0.46 0.07 1 1 -2 -3 0.30 0.10 2 1 2 -3 0.77 0.13 1 1 2 -3 0.78 0.11 2 -1 -2 2 5.56 0.22 1 -1 -2 2 5.06 0.18 2 -1 2 2 2.70 0.12 1 -1 2 2 2.37 0.16 2 1 -2 -2 2.58 0.13 1 1 -2 -2 2.29 0.16 2 1 2 -2 5.57 0.22 1 1 2 -2 5.00 0.18 2 -1 -2 1 64.55 0.58 1 -1 -2 1 60.20 0.49 2 -1 -2 1 41.95 0.41 3 -1 2 1 47.63 0.54 1 1 -2 -1 38.71 0.41 1 1 -2 -1 32.66 0.44 2 1 -2 -1 58.39 0.58 2 1 2 -1 62.62 0.57 1 1 2 -1 57.17 0.48 2 -1 -2 0 7.88 0.20 1 -1 -2 0 7.53 0.18 2 -1 -2 0 5.34 0.19 3 -1 2 0 5.87 0.19 1 -1 2 0 7.09 0.23 2 1 -2 0 5.25 0.19 1 1 -2 0 7.45 0.22 2 1 2 0 8.15 0.21 1 1 2 0 7.11 0.18 2 -1 -2 -1 6.71 0.16 1 -1 -2 -1 3.89 0.15 2 -1 -2 -1 5.01 0.19 3 -1 2 -1 6.41 0.22 2 1 -2 1 4.74 0.19 1 1 -2 1 7.96 0.24 1 1 -2 1 6.19 0.22 2 1 2 1 7.94 0.18 1 1 2 1 3.82 0.15 2 -1 -2 -2 184.88 1.17 1 -1 -2 -2 129.31 1.07 2 -1 -2 -2 140.40 1.36 3 -1 2 -2 207.53 1.15 2 1 -2 2 239.84 2.74 1 1 -2 2 201.57 1.14 2 1 -2 2 221.70 1.68 3 1 2 2 240.09 1.60 1 1 2 2 113.80 0.73 2 1 2 2 148.76 0.98 3 -1 -2 -3 241.36 2.22 2 -1 -2 -3 314.05 3.00 3 -1 2 -3 505.04 4.38 1 -1 2 -3 429.88 3.94 2 1 -2 3 481.97 13.79 1 1 -2 3 438.84 3.24 2 1 -2 3 474.95 3.16 3 1 2 3 327.91 2.64 3 -1 -2 -4 5.92 0.23 2 -1 -2 -4 6.79 0.26 3 -1 2 -4 12.63 0.35 1 -1 2 -4 9.95 0.31 2 -1 2 -4 11.01 0.25 3 1 -2 4 9.75 0.32 2 1 -2 4 11.44 0.26 3 1 2 4 5.65 0.25 2 1 2 4 7.46 0.28 3 -1 -2 -5 6.49 0.27 2 -1 -2 -5 8.01 0.30 3 -1 2 -5 14.24 0.39 1 -1 2 -5 12.16 0.36 2 -1 2 -5 12.60 0.27 3 1 -2 5 10.55 0.34 2 1 -2 5 11.33 0.27 3 1 2 5 6.25 0.25 2 1 2 5 8.57 0.30 3 -1 -2 -6 0.17 0.11 2 -1 -2 -6 0.23 0.11 3 -1 2 -6 0.44 0.14 1 -1 2 -6 0.25 0.12 2 -1 2 -6 0.17 0.08 3 1 -2 6 0.25 0.12 1 1 -2 6 0.33 0.09 3 1 2 6 0.05 0.09 2 1 2 6 0.22 0.12 3 -1 -2 -7 10.24 0.38 2 -1 -2 -7 13.11 0.41 3 -1 2 -7 20.53 0.51 1 -1 2 -7 16.51 0.48 2 -1 2 -7 16.71 0.34 3 1 -2 7 14.55 0.32 3 1 2 7 11.86 0.17 1 1 2 7 12.09 0.17 1 -1 -2 -8 6.51 0.34 2 -1 -2 -8 7.64 0.34 3 -1 2 -8 11.90 0.42 1 -1 2 -8 9.63 0.40 2 -1 2 -8 10.19 0.29 3 1 -2 8 8.66 0.27 3 1 2 8 7.87 0.17 1 1 2 8 8.16 0.18 1 -1 -2 -9 0.52 0.17 2 -1 -2 -9 0.67 0.16 3 -1 2 -9 0.97 0.19 1 -1 2 -9 0.67 0.18 2 -1 2 -9 0.74 0.12 3 1 -2 9 0.61 0.12 3 1 2 9 0.65 0.08 1 1 2 9 0.59 0.08 1 -1 -2 -10 54.13 0.96 2 -1 -2 -10 52.89 0.89 3 -1 2 -10 87.80 1.15 1 -1 2 -10 66.97 1.09 2 -1 2 -10 73.90 0.79 3 1 -2 10 52.09 0.67 3 1 2 10 52.52 0.52 1 1 2 10 53.32 0.53 1 -1 -2 -11 49.81 0.97 2 -1 -2 -11 52.13 0.91 3 -1 2 -11 87.68 1.19 1 -1 2 -11 67.18 1.15 2 -1 2 -11 72.67 0.82 3 1 -2 11 54.46 0.72 3 1 2 11 52.60 0.57 1 1 2 11 51.57 0.57 1 -1 -2 -12 10.50 0.52 2 -1 -2 -12 11.22 0.47 3 -1 2 -12 18.39 0.60 1 -1 2 -12 14.34 0.59 2 -1 2 -12 15.70 0.42 3 1 -2 12 12.02 0.38 3 1 2 12 11.44 0.30 1 1 2 12 11.19 0.30 1 -1 -2 -13 6.74 0.47 2 -1 -2 -13 7.83 0.42 3 -1 2 -13 12.92 0.53 1 -1 2 -13 9.31 0.52 2 -1 2 -13 10.73 0.37 3 1 -2 13 7.13 0.36 3 1 2 13 7.34 0.27 1 1 2 13 7.38 0.27 1 -1 -2 -14 17.08 0.70 2 -1 -2 -14 19.68 0.65 3 -1 2 -14 27.99 0.77 1 -1 2 -14 21.15 0.77 2 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1.03 0.18 1 1 -3 -15 0.72 0.27 2 1 -3 -15 0.82 0.22 3 1 3 -15 1.11 0.27 1 1 3 -15 0.98 0.27 2 1 -3 -14 9.65 0.29 1 1 -3 -14 5.49 0.47 2 1 -3 -14 6.50 0.42 3 1 3 -14 9.35 0.51 1 1 3 -14 7.07 0.49 2 -1 3 13 0.84 0.11 1 1 -3 -13 1.79 0.15 1 1 -3 -13 0.78 0.23 2 1 -3 -13 1.20 0.24 3 1 3 -13 1.66 0.28 1 1 3 -13 1.53 0.28 2 -1 3 12 9.88 0.26 1 1 -3 -12 19.65 0.37 1 1 -3 -12 10.21 0.52 2 1 -3 -12 12.78 0.51 3 1 3 -12 18.83 0.64 1 1 3 -12 15.48 0.61 2 -1 -3 11 10.39 0.20 3 -1 3 11 8.04 0.23 1 1 -3 -11 16.37 0.32 1 1 -3 -11 8.30 0.46 2 1 -3 -11 10.69 0.46 3 1 3 -11 17.51 0.60 1 1 3 -11 14.64 0.57 2 -1 -3 10 1.47 0.10 3 -1 3 10 1.51 0.11 1 1 -3 -10 2.76 0.15 1 1 -3 -10 1.68 0.26 2 1 -3 -10 2.02 0.24 3 1 3 -10 2.55 0.28 1 1 3 -10 2.28 0.28 2 -1 -3 9 4.54 0.13 3 -1 3 9 3.62 0.14 1 1 -3 -9 6.20 0.19 1 1 -3 -9 3.44 0.29 2 1 -3 -9 4.31 0.30 3 1 3 -9 6.50 0.36 1 1 3 -9 5.38 0.34 2 -1 -3 8 1.55 0.10 3 -1 3 8 0.86 0.09 1 1 -3 -8 1.17 0.11 1 1 -3 -8 0.83 0.17 2 1 -3 -8 0.86 0.17 3 1 3 -8 1.65 0.22 1 1 3 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5 1.26 0.15 2 -1 -3 -6 4.03 0.25 2 -1 -3 -6 4.37 0.27 3 -1 3 -6 8.95 0.36 1 -1 3 -6 7.65 0.35 2 1 -3 6 7.38 0.24 3 -1 -3 -7 1.01 0.17 2 -1 -3 -7 1.46 0.21 3 -1 3 -7 2.07 0.25 1 -1 3 -7 1.55 0.21 2 -1 3 -7 1.88 0.15 3 1 -3 7 1.72 0.16 3 -1 -3 -8 6.31 0.34 2 -1 -3 -8 8.10 0.38 3 -1 3 -8 14.58 0.50 1 -1 3 -8 11.43 0.45 2 -1 3 -8 12.24 0.32 3 1 -3 8 9.83 0.29 3 -1 -3 -9 0.28 0.15 2 -1 -3 -9 0.15 0.14 3 -1 3 -9 0.12 0.15 1 -1 3 -9 0.01 0.13 2 -1 3 -9 0.02 0.08 3 1 -3 9 0.02 0.09 3 -1 -3 -10 5.80 0.37 2 -1 -3 -10 7.59 0.40 3 -1 3 -10 12.07 0.50 1 -1 3 -10 9.61 0.47 2 -1 3 -10 11.02 0.32 3 1 -3 10 8.91 0.30 3 -1 -3 -11 3.71 0.35 2 -1 -3 -11 4.86 0.35 3 -1 3 -11 7.42 0.42 1 -1 3 -11 6.20 0.42 2 -1 3 -11 6.77 0.27 3 1 -3 11 4.93 0.25 3 -1 -3 -12 0.16 0.19 2 -1 -3 -12 -0.01 0.14 3 -1 3 -12 0.11 0.16 1 -1 3 -12 0.21 0.18 2 -1 3 -12 0.23 0.11 3 1 -3 12 0.07 0.11 3 -1 -3 -13 4.21 0.42 2 -1 -3 -13 4.98 0.38 3 -1 3 -13 7.27 0.46 1 -1 3 -13 6.66 0.47 2 -1 3 -13 6.97 0.29 3 1 -3 13 5.37 0.29 3 1 3 13 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0.76 0.27 2 1 -4 -15 1.18 0.27 3 1 4 -15 1.48 0.31 1 1 4 -15 1.29 0.29 2 1 -4 -14 0.80 0.26 2 1 -4 -14 1.20 0.26 3 1 4 -14 1.32 0.28 1 1 4 -14 1.34 0.29 2 1 -4 -13 0.80 0.25 2 1 -4 -13 0.52 0.20 3 1 4 -13 1.20 0.26 1 1 4 -13 0.93 0.24 2 1 -4 -12 16.15 0.65 2 1 -4 -12 19.57 0.66 3 1 4 -12 33.71 0.89 1 1 4 -12 31.24 0.86 2 1 -4 -11 0.22 0.17 2 1 -4 -11 0.44 0.18 3 1 4 -11 0.85 0.21 1 1 4 -11 0.72 0.21 2 -1 -4 10 1.69 0.11 3 -1 4 10 1.21 0.08 1 1 -4 -10 1.32 0.24 2 1 -4 -10 1.66 0.25 3 1 4 -10 2.29 0.28 1 1 4 -10 2.12 0.28 2 -1 -4 9 0.18 0.07 3 -1 4 9 0.28 0.05 1 1 -4 -9 0.25 0.06 1 1 -4 -9 0.36 0.16 2 1 -4 -9 0.25 0.15 3 1 4 -9 0.40 0.17 1 1 4 -9 0.28 0.15 2 -1 -4 8 13.03 0.25 3 -1 4 8 9.56 0.19 1 1 -4 -8 10.20 0.21 1 1 -4 -8 7.35 0.38 2 1 -4 -8 9.72 0.43 3 1 4 -8 15.39 0.54 1 1 4 -8 13.44 0.49 2 -1 -4 7 0.09 0.06 3 -1 4 7 0.11 0.05 1 1 -4 -7 0.06 0.05 1 1 -4 -7 0.05 0.11 2 1 -4 -7 0.09 0.13 3 1 4 -7 0.09 0.12 1 1 4 -7 0.07 0.12 2 -1 -4 6 4.94 0.18 3 -1 4 6 2.97 0.14 1 1 -4 -6 2.57 0.13 1 1 -4 -6 2.24 0.23 2 1 4 -6 4.52 0.31 1 1 4 -6 4.16 0.27 2 1 -4 -5 32.59 0.41 1 1 -4 -5 32.05 0.65 2 1 4 -5 58.05 0.89 1 1 4 -5 53.95 0.80 2 -1 -4 4 3.25 0.23 2 1 -4 -4 1.45 0.13 1 1 -4 -4 3.22 0.16 1 1 -4 -4 1.45 0.19 2 1 4 -4 3.45 0.26 1 1 4 -4 3.46 0.24 2 -1 -4 3 0.09 0.09 2 1 -4 -3 0.13 0.07 1 1 -4 -3 0.27 0.08 1 1 -4 -3 0.16 0.10 2 1 4 -3 0.08 0.09 1 1 4 -3 0.04 0.09 2 -1 -4 2 12.21 0.38 1 -1 -4 2 11.92 0.34 2 1 -4 -2 7.49 0.25 1 1 -4 -2 14.17 0.34 1 1 -4 -2 7.40 0.31 2 1 -4 -2 11.88 0.38 2 1 4 -2 12.96 0.39 1 1 4 -2 11.55 0.35 2 -1 -4 1 17.98 0.43 1 -1 -4 1 16.63 0.39 2 1 -4 -1 11.87 0.33 1 1 -4 -1 19.66 0.41 1 1 -4 -1 9.43 0.33 2 1 -4 -1 15.99 0.43 2 1 4 -1 19.47 0.44 1 1 4 -1 16.38 0.39 2 -1 -4 0 20.10 0.42 1 -1 -4 0 18.20 0.40 2 -1 4 0 18.11 0.45 2 1 -4 0 14.57 0.38 1 1 -4 0 21.19 0.45 1 1 -4 0 17.93 0.45 2 1 4 0 20.40 0.43 1 -1 -4 -1 1.93 0.16 1 -1 -4 -1 0.99 0.14 2 -1 -4 -1 1.68 0.16 2 -1 -4 -1 1.20 0.18 3 -1 4 -1 1.60 0.19 2 1 -4 1 1.19 0.16 1 1 -4 1 1.88 0.18 1 1 -4 1 1.68 0.18 2 1 4 1 1.93 0.17 1 -1 -4 -2 107.67 0.81 1 -1 -4 -2 52.89 0.68 2 -1 -4 -2 99.11 0.94 2 -1 -4 -2 72.27 0.90 3 -1 4 -2 101.21 1.05 2 1 -4 2 121.81 1.34 1 1 4 2 120.82 0.86 1 -1 -4 -3 3.21 0.16 1 -1 -4 -3 1.39 0.17 2 -1 -4 -3 1.81 0.20 3 -1 4 -3 3.46 0.26 1 -1 4 -3 2.86 0.23 2 -1 -4 -4 31.79 0.35 1 -1 -4 -4 44.82 0.42 1 -1 -4 -4 27.82 0.55 2 -1 -4 -4 31.80 0.66 3 -1 4 -4 53.96 0.85 1 -1 4 -4 46.81 0.77 2 1 -4 4 50.75 0.66 3 -1 -4 -5 2.32 0.09 1 -1 -4 -5 3.63 0.11 1 -1 -4 -5 2.15 0.20 2 -1 -4 -5 2.45 0.24 3 -1 4 -5 4.51 0.29 1 -1 4 -5 3.77 0.28 2 1 -4 5 4.11 0.22 3 -1 -4 -6 23.02 0.55 2 -1 -4 -6 29.96 0.69 3 -1 4 -6 47.89 0.86 1 -1 4 -6 41.24 0.79 2 1 -4 6 42.52 0.60 3 -1 -4 -7 0.12 0.11 2 -1 -4 -7 0.04 0.13 3 -1 4 -7 -0.01 0.13 1 -1 4 -7 0.08 0.13 2 1 -4 7 0.09 0.09 3 -1 -4 -8 1.93 0.24 2 -1 -4 -8 2.31 0.27 3 -1 4 -8 3.59 0.32 1 -1 4 -8 2.99 0.29 2 1 -4 8 2.95 0.20 3 -1 -4 -9 0.21 0.15 2 -1 -4 -9 0.25 0.16 3 -1 4 -9 0.35 0.17 1 -1 4 -9 0.10 0.15 2 1 -4 9 0.31 0.11 3 -1 -4 -10 14.15 0.55 2 -1 -4 -10 19.65 0.64 3 -1 4 -10 28.22 0.78 1 -1 4 -10 23.91 0.72 2 1 -4 10 20.46 0.44 3 -1 -4 -11 1.45 0.27 2 -1 -4 -11 2.23 0.30 3 -1 4 -11 3.64 0.36 1 -1 4 -11 2.75 0.31 2 1 -4 11 2.79 0.22 3 -1 -4 -12 47.84 1.06 2 -1 -4 -12 59.56 1.15 3 -1 4 -12 93.31 1.46 1 -1 4 -12 80.69 1.39 2 1 -4 12 61.46 0.77 3 -1 -4 -13 4.81 0.44 2 -1 -4 -13 4.77 0.42 3 -1 4 -13 7.73 0.48 1 -1 4 -13 8.12 0.52 2 -1 -4 -14 3.21 0.41 2 -1 -4 -14 3.33 0.38 3 -1 4 -14 5.62 0.45 1 -1 4 -14 5.13 0.46 2 -1 -4 -15 1.04 0.30 2 -1 -4 -15 1.12 0.27 3 -1 4 -15 2.16 0.35 1 -1 4 -15 1.89 0.35 2 -1 -4 -16 5.90 0.56 2 -1 -4 -16 6.64 0.50 3 -1 4 -16 9.57 0.62 2 -1 -4 -17 0.13 0.26 2 -1 -4 -17 0.12 0.23 3 -1 4 -17 0.07 0.22 2 1 -4 17 0.06 0.23 1 -1 -4 -18 0.78 0.32 2 -1 -4 -18 0.85 0.30 3 -1 4 -18 1.59 0.36 2 1 -4 18 0.50 0.27 1 -1 -4 -19 0.89 0.34 2 -1 -4 -19 0.90 0.32 3 -1 4 -19 1.39 0.35 2 1 -4 19 0.80 0.30 1 1 -5 -19 2.34 0.48 2 1 -5 -19 1.99 0.39 3 1 5 -19 2.93 0.45 1 1 5 -19 3.21 0.48 2 1 -5 -18 0.05 0.30 2 1 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6 36.30 0.59 2 2 0 -6 53.23 0.64 1 2 0 -6 34.44 0.58 2 -2 0 5 0.06 0.08 2 2 0 -5 0.01 0.08 1 2 0 -5 -0.02 0.09 2 -2 0 4 58.28 0.59 1 -2 0 4 45.06 0.53 2 2 0 -4 69.25 0.64 1 2 0 -4 47.50 0.55 2 -2 0 3 0.06 0.07 1 -2 0 3 0.01 0.07 2 2 0 -3 0.02 0.07 1 2 0 -3 0.03 0.07 2 -2 0 2 0.16 0.07 1 -2 0 2 0.15 0.06 2 -2 0 2 0.28 0.06 3 2 0 -2 0.25 0.08 1 2 0 -2 0.17 0.06 2 2 0 -2 0.30 0.06 3 -2 0 1 0.03 0.06 1 -2 0 1 0.00 0.04 2 -2 0 1 -0.01 0.05 3 2 0 -1 0.04 0.06 1 2 0 -1 -0.01 0.04 2 -2 0 0 47.14 0.41 1 -2 0 0 76.30 0.83 2 -2 0 0 80.94 0.75 3 2 0 0 46.36 0.41 1 2 0 0 81.75 0.70 2 2 0 0 77.72 0.77 3 -2 0 -1 0.00 0.05 1 -2 0 -1 0.00 0.04 2 -2 0 -1 0.01 0.05 3 2 0 1 0.03 0.05 1 2 0 1 -0.01 0.04 2 2 0 1 0.00 0.06 3 -2 0 -2 12.81 0.23 1 -2 0 -2 19.32 0.28 2 -2 0 -2 19.86 0.32 3 2 0 2 12.30 0.23 1 2 0 2 17.95 0.31 3 -2 0 -3 0.09 0.06 1 -2 0 -3 0.11 0.08 2 -2 0 -3 0.20 0.10 3 2 0 3 0.06 0.06 1 2 0 3 0.06 0.13 2 2 0 3 0.03 0.08 3 -2 0 -4 96.89 0.80 2 -2 0 -4 90.18 0.76 3 2 0 4 71.04 0.59 1 2 0 4 78.61 0.73 2 2 0 4 101.96 0.81 3 -2 0 -5 0.14 0.11 2 -2 0 -5 0.25 0.11 3 2 0 5 0.18 0.08 1 2 0 5 0.32 0.09 1 2 0 5 0.15 0.11 2 2 0 5 0.20 0.10 3 -2 0 -6 0.68 0.14 2 -2 0 -6 0.63 0.13 3 2 0 6 0.63 0.10 1 2 0 6 0.77 0.11 1 2 0 6 0.72 0.14 2 2 0 6 0.68 0.13 3 -2 0 -7 0.06 0.12 2 -2 0 -7 0.05 0.10 3 2 0 7 0.05 0.08 1 2 0 7 0.16 0.09 1 2 0 7 0.09 0.10 3 -2 0 -8 54.95 0.85 2 -2 0 -8 51.73 0.73 3 2 0 8 45.30 0.62 1 2 0 8 69.35 0.77 1 2 0 8 47.08 0.70 3 -2 0 -9 0.54 0.17 2 -2 0 -9 0.65 0.15 3 2 0 9 0.53 0.12 1 2 0 9 0.60 0.13 1 -2 0 -10 56.40 0.97 2 -2 0 -10 51.87 0.81 3 2 0 10 41.93 0.67 1 2 0 10 65.15 0.83 1 -2 0 -11 0.09 0.17 2 -2 0 -11 0.06 0.13 3 2 0 11 0.09 0.10 1 -2 0 -12 7.59 0.45 2 -2 0 -12 7.50 0.38 3 2 0 12 6.03 0.31 1 -2 0 -13 0.01 0.18 2 -2 0 -13 0.20 0.16 3 2 0 13 0.15 0.12 1 -2 0 -14 206.97 2.24 2 -2 0 -14 208.01 1.85 3 2 0 14 167.74 1.57 1 -2 0 -15 0.27 0.22 2 -2 0 -15 0.28 0.19 3 2 0 15 0.34 0.16 1 -2 0 -16 0.10 0.20 2 -2 0 -16 -0.01 0.18 3 2 0 16 0.19 0.15 1 -2 0 -17 -0.26 0.19 2 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0.64 0.12 3 2 -1 -12 10.36 0.38 1 2 -1 -12 6.63 0.44 2 2 -1 -12 7.69 0.34 3 2 1 -12 10.56 0.44 1 2 1 -12 7.19 0.44 2 2 1 -12 7.90 0.26 3 2 -1 -11 0.80 0.15 1 2 -1 -11 0.64 0.21 2 2 -1 -11 0.60 0.14 3 2 1 -11 0.75 0.18 1 2 1 -11 0.35 0.18 2 2 1 -11 0.64 0.10 3 -2 1 10 0.17 0.10 1 2 -1 -10 0.29 0.11 1 2 -1 -10 0.11 0.15 2 2 -1 -10 0.21 0.10 3 2 1 -10 0.28 0.14 1 2 1 -10 0.23 0.16 2 2 1 -10 0.15 0.07 3 -2 1 9 16.78 0.40 1 2 -1 -9 22.50 0.46 1 2 -1 -9 13.64 0.48 2 2 -1 -9 15.52 0.40 3 2 1 -9 24.18 0.56 1 2 1 -9 16.83 0.52 2 2 1 -9 20.47 0.30 3 -2 1 8 90.56 0.86 1 2 -1 -8 119.85 0.98 1 2 -1 -8 69.98 0.96 2 2 -1 -8 88.38 0.87 3 2 1 -8 132.77 1.22 1 2 1 -8 89.26 1.05 2 2 1 -8 100.24 0.59 3 -2 -1 7 33.93 0.59 1 -2 -1 7 22.63 0.52 2 -2 1 7 29.03 0.47 1 2 -1 -7 36.36 0.52 1 2 -1 -7 22.52 0.52 2 2 1 -7 41.34 0.66 1 2 1 -7 28.42 0.57 2 2 1 -7 28.40 0.28 3 -2 -1 6 31.52 0.55 1 -2 -1 6 21.87 0.47 2 -2 1 6 21.43 0.38 1 -2 1 6 20.03 0.46 2 2 -1 -6 32.43 0.46 1 2 -1 -6 20.70 0.47 2 2 1 -6 38.46 0.60 1 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47.28 0.47 3 2 1 0 27.58 0.33 1 -2 -1 -1 40.26 0.36 1 -2 -1 -1 45.80 0.28 2 -2 1 -1 41.24 0.46 1 -2 1 -1 61.55 0.53 2 -2 1 -1 65.86 0.56 3 2 -1 1 64.95 0.55 2 2 -1 1 65.04 0.56 3 2 1 1 37.75 0.35 1 2 1 1 36.54 0.25 2 2 1 1 46.33 0.48 3 -2 -1 -2 56.55 0.40 1 -2 -1 -2 70.30 0.48 2 -2 -1 -2 81.63 0.68 3 -2 1 -2 72.53 0.63 1 -2 1 -2 100.61 0.74 2 -2 1 -2 101.80 0.72 3 2 -1 2 95.53 0.72 2 2 -1 2 99.17 0.71 3 2 1 2 62.71 0.42 1 2 1 2 55.39 0.42 2 2 1 2 72.79 0.65 3 -2 -1 -3 13.81 0.20 1 -2 -1 -3 14.29 0.28 2 -2 -1 -3 16.30 0.35 3 -2 1 -3 14.29 0.31 1 -2 1 -3 19.56 0.37 2 -2 1 -3 20.99 0.35 3 2 -1 3 14.01 0.31 1 2 -1 3 18.54 0.36 2 2 -1 3 19.02 0.34 3 2 1 3 11.78 0.19 1 2 1 3 11.70 0.25 2 -2 -1 -4 16.74 0.23 1 -2 -1 -4 15.04 0.33 2 -2 -1 -4 17.06 0.38 3 -2 1 -4 21.83 0.43 2 -2 1 -4 21.01 0.38 3 2 -1 4 16.99 0.36 1 2 -1 4 24.33 0.42 1 2 -1 4 19.48 0.41 2 2 -1 4 21.61 0.38 3 2 1 4 12.46 0.21 1 -2 -1 -5 14.92 0.36 2 -2 -1 -5 16.53 0.40 3 -2 1 -5 20.36 0.45 2 -2 1 -5 19.45 0.38 3 2 -1 5 15.81 0.37 1 2 -1 5 23.32 0.44 1 2 -1 5 19.65 0.44 2 2 -1 5 17.98 0.37 3 2 1 5 14.55 0.24 1 2 1 5 25.03 0.31 1 2 1 5 12.66 0.34 2 2 1 5 17.75 0.41 3 -2 -1 -6 1.05 0.16 2 -2 -1 -6 1.02 0.16 3 -2 1 -6 1.72 0.20 2 -2 1 -6 1.45 0.17 3 2 -1 6 0.88 0.13 1 2 -1 6 1.69 0.16 1 2 -1 6 1.30 0.17 2 2 -1 6 1.25 0.16 3 2 1 6 0.84 0.10 1 2 1 6 1.48 0.12 1 2 1 6 0.72 0.14 2 2 1 6 0.83 0.14 3 -2 -1 -7 0.21 0.13 2 -2 -1 -7 0.26 0.12 3 -2 1 -7 0.06 0.12 2 -2 1 -7 0.17 0.11 3 2 -1 7 0.17 0.10 1 2 -1 7 0.19 0.10 3 2 1 7 0.24 0.07 1 2 1 7 0.28 0.08 1 2 1 7 0.29 0.12 3 -2 -1 -8 80.32 1.02 2 -2 -1 -8 95.64 1.05 3 -2 1 -8 98.77 1.16 2 -2 1 -8 102.82 0.97 3 2 -1 8 77.48 0.91 1 2 -1 8 85.03 0.89 3 2 1 8 76.31 0.68 1 2 1 8 118.13 0.85 1 -2 -1 -9 8.64 0.40 2 -2 -1 -9 10.27 0.40 3 -2 1 -9 9.56 0.42 2 -2 1 -9 9.30 0.34 3 2 -1 9 7.72 0.33 1 2 -1 9 7.48 0.31 3 2 1 9 8.21 0.26 1 2 1 9 11.76 0.31 1 -2 -1 -10 0.53 0.19 2 -2 -1 -10 0.40 0.15 3 -2 1 -10 0.52 0.18 2 -2 1 -10 0.47 0.14 3 2 -1 10 0.42 0.14 1 2 1 10 0.34 0.10 1 2 1 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2.84 0.29 1 2 2 -12 2.34 0.30 2 2 2 -12 2.61 0.12 3 -2 2 11 5.96 0.25 1 2 -2 -11 10.15 0.33 1 2 -2 -11 5.66 0.39 2 2 -2 -11 6.65 0.34 3 2 2 -11 11.09 0.46 1 2 2 -11 8.82 0.45 2 -2 2 10 4.56 0.22 1 2 -2 -10 7.88 0.28 1 2 -2 -10 4.33 0.33 2 2 -2 -10 5.69 0.30 3 2 2 -10 9.02 0.41 1 2 2 -10 7.42 0.40 2 -2 2 9 46.44 0.60 1 2 -2 -9 71.93 0.74 1 2 -2 -9 44.00 0.84 2 2 -2 -9 53.44 0.81 3 2 2 -9 85.16 1.11 1 2 2 -9 68.19 1.00 2 -2 2 8 5.18 0.21 1 2 -2 -8 7.70 0.26 1 2 -2 -8 5.16 0.31 2 2 -2 -8 6.76 0.30 3 2 2 -8 10.24 0.40 1 2 2 -8 7.90 0.36 2 -2 2 7 0.38 0.09 1 2 -2 -7 0.40 0.09 1 2 -2 -7 0.41 0.14 2 2 2 -7 0.50 0.13 1 2 2 -7 0.50 0.15 2 -2 -2 6 0.85 0.16 1 -2 -2 6 0.73 0.15 2 -2 2 6 0.85 0.11 1 2 -2 -6 0.90 0.11 1 2 -2 -6 0.64 0.13 2 2 2 -6 1.38 0.19 1 2 2 -6 1.02 0.16 2 -2 -2 5 27.15 0.53 1 -2 -2 5 22.51 0.45 2 -2 2 5 18.60 0.32 1 -2 2 5 17.79 0.43 2 2 -2 -5 20.30 0.34 1 2 -2 -5 17.82 0.44 2 2 2 -5 33.43 0.59 1 2 2 -5 27.88 0.49 2 -2 -2 4 6.23 0.26 1 -2 -2 4 5.01 0.22 2 -2 -2 4 5.94 0.11 3 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22.28 0.48 1 2 -5 -3 10.73 0.42 2 2 5 -3 21.00 0.56 1 2 5 -3 18.83 0.47 2 -2 -5 2 0.17 0.10 2 -2 -5 2 0.08 0.10 3 2 -5 -2 -0.03 0.09 1 2 -5 -2 0.18 0.10 1 2 -5 -2 0.11 0.11 2 2 5 -2 0.08 0.11 1 2 5 -2 0.09 0.10 2 -2 -5 1 0.39 0.11 2 -2 -5 1 0.24 0.11 3 2 -5 -1 0.21 0.11 1 2 -5 -1 0.19 0.12 2 2 5 -1 0.43 0.13 1 2 5 -1 0.24 0.11 2 -2 -5 0 31.51 0.59 1 -2 -5 0 18.44 0.43 2 -2 -5 0 32.37 0.57 2 -2 -5 0 21.95 0.53 3 -2 5 0 33.79 0.70 2 2 -5 0 21.60 0.53 1 2 5 0 36.67 0.63 1 -2 -5 -1 1.67 0.18 1 -2 -5 -1 1.11 0.15 2 -2 -5 -1 1.80 0.18 2 -2 -5 -1 1.16 0.19 3 -2 5 -1 2.04 0.23 2 2 -5 1 1.65 0.21 1 2 5 1 2.03 0.19 1 -2 -5 -2 7.05 0.27 1 -2 -5 -2 3.94 0.23 2 -2 -5 -2 7.02 0.29 2 -2 -5 -2 4.57 0.30 3 -2 5 -2 7.00 0.36 2 2 -5 2 5.43 0.31 1 2 5 2 7.86 0.28 1 -2 -5 -3 1.45 0.15 1 -2 -5 -3 0.99 0.15 2 -2 -5 -3 1.67 0.19 2 -2 -5 -3 1.51 0.22 3 -2 5 -3 1.18 0.20 2 2 -5 3 0.74 0.17 1 2 5 3 1.83 0.16 1 -2 -5 -4 50.63 0.54 1 -2 -5 -4 34.03 0.63 2 -2 -5 -4 40.93 0.82 3 -2 5 -4 57.59 0.96 2 2 -5 4 41.40 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