#------------------------------------------------------------------------------ #$Date: 2024-11-20 04:49:53 +0200 (Wed, 20 Nov 2024) $ #$Revision: 296005 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/32/1573203.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_1573203 loop_ _publ_author_name 'Zwolenik, A.' 'Makal, A.' _publ_section_title ; Tracking anharmonic oscillations in the structure of β-1,3-diacetylpyrene. ; _journal_issue 1 _journal_name_full IUCrJ _journal_paper_doi 10.1107/S2052252524010443 _journal_volume 12 _journal_year 2025 _chemical_formula_moiety 'C20 H14 O2' _chemical_formula_sum 'C20 H14 O2' _chemical_formula_weight 286.333 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_Int_Tables_number 14 _atom_sites_solution_primary dual _audit_creation_date 2024-08-02 _audit_creation_method ; Olex2 1.5 (compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928) ; _cell_angle_alpha 90 _cell_angle_beta 102.926(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.1945(2) _cell_length_b 10.9948(3) _cell_length_c 17.7698(5) _cell_measurement_reflns_used 5292 _cell_measurement_temperature 190.00(10) _cell_measurement_theta_max 79.0470 _cell_measurement_theta_min 4.7510 _cell_volume 1370.01(7) _computing_cell_refinement 'CrysAlisPro 1.171.43.104a (Rigaku OD, 2023)' _computing_data_collection 'CrysAlisPro system (CCD 42.70a 64-bit (release 22-09-2022))' _computing_data_reduction 'CrysAlisPro 1.171.43.104a (Rigaku OD, 2023)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'olex2.refine 1.5 (Bourhis et al., 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 190.00(10) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 1.0000 _diffrn_measured_fraction_theta_max 0.9919 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames -------------------------------------------------------------------------- 1 \w -96.00 3.00 0.50 0.40 -- -38.96 -60.00 100.00 198 2 \w 84.00 141.00 0.50 1.60 -- 84.48 60.00-120.00 114 3 \w 7.00 124.00 0.50 1.60 -- 84.48 -60.00 100.00 234 4 \w 126.00 168.00 0.50 3.20 -- 130.00 -60.00 100.00 84 5 \w 42.00 109.00 0.50 3.20 -- 130.00 -60.00 100.00 134 6 \w 149.00 178.00 0.50 3.20 -- 130.00 60.00-120.00 58 7 \w -129.00 -88.00 0.50 0.40 -- -38.96 -99.00-120.00 82 8 \w -103.00 -74.00 0.50 0.40 -- -38.96-125.00-180.00 58 9 \w -39.00 42.00 0.50 0.40 -- -38.96 60.00-120.00 162 10 \w 41.00 111.00 0.50 0.40 -- 38.96-125.00 0.00 140 11 \w 110.00 169.00 0.50 1.60 -- 84.48 111.00 30.00 118 12 \w 103.00 132.00 0.50 1.60 -- 84.48 63.00-180.00 58 13 \w 108.00 148.00 0.50 1.60 -- 84.48 111.00-150.00 80 14 \w 145.00 171.00 0.50 1.60 -- 84.48 63.00-180.00 52 15 \w 120.00 145.00 0.50 1.60 -- 84.48 178.00 30.00 50 16 \w 63.00 118.00 0.50 1.60 -- 84.48 178.00 90.00 110 17 \w 75.00 108.00 0.50 1.60 -- 84.48 178.00 150.00 66 18 \w 24.00 107.00 0.50 1.60 -- 84.48-111.00 120.00 166 19 \w 24.00 108.00 0.50 1.60 -- 84.48-111.00 60.00 168 20 \w 54.00 101.00 0.50 3.20 -- 130.00-104.00-180.00 94 21 \w 142.00 177.00 0.50 3.20 -- 130.00 104.00 120.00 70 22 \w 151.00 176.00 0.50 3.20 -- 130.00 63.00-180.00 50 23 \w 63.00 102.00 0.50 3.20 -- 130.00 -50.00 -30.00 78 24 \w 117.00 165.00 0.50 3.20 -- 130.00 50.00-150.00 96 25 \w 102.00 134.00 0.50 3.20 -- 130.00 63.00-180.00 64 26 \w 37.00 107.00 0.50 3.20 -- 130.00-104.00 90.00 140 27 \w 136.00 173.00 0.50 3.20 -- 130.00 0.00 90.00 74 28 \w 36.00 105.00 0.50 3.20 -- 130.00 0.00 90.00 138 29 \w 31.00 77.00 0.50 3.20 -- 130.00 -91.00 30.00 92 30 \w 36.00 87.00 0.50 3.20 -- 130.00-104.00-150.00 102 31 \w 33.00 104.00 0.50 3.20 -- 130.00 -91.00 90.00 142 32 \w 130.00 155.00 0.50 3.20 -- 130.00 -50.00 -30.00 50 33 \w 91.00 167.00 0.50 3.20 -- 130.00 138.00 -30.00 152 34 \w 89.00 122.00 0.50 3.20 -- 130.00 77.00 -60.00 66 35 \w 121.00 173.00 0.50 3.20 -- 130.00 104.00 -60.00 104 36 \w 48.00 73.00 0.50 3.20 -- 130.00 -91.00 0.00 50 37 \w 42.00 72.00 0.50 3.20 -- 130.00-104.00 150.00 60 38 \w 36.00 67.00 0.50 3.20 -- 130.00-104.00 30.00 62 39 \w 107.00 163.00 0.50 3.20 -- 130.00 104.00-180.00 112 40 \w 153.00 178.00 0.50 3.20 -- 130.00 38.00 30.00 50 41 \w 95.00 120.00 0.50 3.20 -- 130.00 -38.00 120.00 50 42 \w 149.00 178.00 0.50 3.20 -- 130.00 -38.00 120.00 58 43 \w 67.00 97.00 0.50 3.20 -- 130.00 38.00 30.00 60 44 \w 129.00 154.00 0.50 3.20 -- 130.00 63.00 -90.00 50 45 \w 119.00 144.00 0.50 3.20 -- 130.00 104.00 150.00 50 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0603041017 _diffrn_orient_matrix_UB_12 0.0977049854 _diffrn_orient_matrix_UB_13 -0.0520328607 _diffrn_orient_matrix_UB_21 -0.1903567036 _diffrn_orient_matrix_UB_22 -0.0167100690 _diffrn_orient_matrix_UB_23 -0.0592618887 _diffrn_orient_matrix_UB_31 -0.0916679939 _diffrn_orient_matrix_UB_32 0.0990083514 _diffrn_orient_matrix_UB_33 0.0411463626 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0287 _diffrn_reflns_av_unetI/netI 0.0283 _diffrn_reflns_Laue_measured_fraction_full 1.0000 _diffrn_reflns_Laue_measured_fraction_max 0.9919 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 9160 _diffrn_reflns_point_group_measured_fraction_full 1.0000 _diffrn_reflns_point_group_measured_fraction_max 0.9919 _diffrn_reflns_theta_full 67.6840 _diffrn_reflns_theta_max 79.33 _diffrn_reflns_theta_min 4.76 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 0.705 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.838 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.43.104a (Rigaku Oxford Diffraction, 2023) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.388 _exptl_crystal_description irregular _exptl_crystal_F_000 601.956 _exptl_crystal_size_max 0.183 _exptl_crystal_size_mid 0.129 _exptl_crystal_size_min 0.107 _refine_diff_density_max 0.0950 _refine_diff_density_min -0.1003 _refine_diff_density_rms 0.0247 _refine_ls_d_res_high 0.7845 _refine_ls_d_res_low 9.2824 _refine_ls_goodness_of_fit_ref 1.0974 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_constraints 0 _refine_ls_number_parameters 375 _refine_ls_number_reflns 2945 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.0974 _refine_ls_R_factor_all 0.0277 _refine_ls_R_factor_gt 0.0221 _refine_ls_shift/su_max -0.0003 _refine_ls_shift/su_mean 0.0000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0170P)^2^+0.0352P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0532 _refine_ls_wR_factor_ref 0.0555 _reflns_Friedel_coverage 0.0 _reflns_limit_h_max 8 _reflns_limit_h_min -9 _reflns_limit_k_max 14 _reflns_limit_k_min 0 _reflns_limit_l_max 22 _reflns_limit_l_min 0 _reflns_number_gt 2514 _reflns_number_total 2945 _reflns_threshold_expression I>=2u(I) _iucr_refine_instructions_details ; TITL 2oapb_multit_1_190_00_smart3_abs_a.res in P2(1)/c REM Old TITL 2oAPb_multiT_1_190_00_smart3_abs in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.149, Rweak 0.011, Alpha 0.016 REM 0.353 for 155 systematic absences, Orientation as input REM Formula found by SHELXT: C20 O2 CELL 1.54184 7.1945 10.9948 17.7698 90 102.926 90 ZERR 4 0.0002 0.0003 0.0005 0 0.003 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H O UNIT 80 56 8 L.S. 10 PLAN 5 SIZE 0.107 0.129 0.183 TEMP -83 CONF BOND list 4 MORE -1 BOND $H fmap 2 acta WGHT 0.017012 0.035215 FVAR 0.403313 REM REM REM REM > REM REM O1 3 0.46757 0.57169 0.73605 11.00000 0.06489 0.04869 0.03355 = -0.01022 0.00620 -0.00783 O2 3 0.25184 0.09183 0.47094 11.00000 0.09329 0.03978 0.05915 = -0.01764 0.03242 -0.00601 C1 1 0.31963 0.44395 0.63164 11.00000 0.03141 0.03421 0.02877 = -0.00454 0.00762 0.00070 C2 1 0.29987 0.52925 0.57036 11.00000 0.02882 0.03369 0.03103 = -0.00454 0.00739 0.00054 C3 1 0.33103 0.65734 0.58274 11.00000 0.04191 0.03466 0.03918 = -0.00556 0.01012 -0.00191 H3 2 0.37067 0.68830 0.64222 11.00000 0.10581 0.05917 0.04377 = -0.01176 0.01719 -0.01449 C4 1 0.31642 0.73644 0.52291 11.00000 0.04376 0.03527 0.04927 = 0.00027 0.01252 -0.00006 H4 2 0.34432 0.83522 0.53364 11.00000 0.10424 0.03983 0.10343 = 0.00011 0.01364 -0.00834 C5 1 0.26705 0.69585 0.44472 11.00000 0.03220 0.04130 0.04399 = 0.00610 0.01042 0.00412 C6 1 0.25903 0.77616 0.38289 11.00000 0.04124 0.05146 0.05579 = 0.01810 0.01350 0.00641 H6 2 0.28927 0.87312 0.39551 11.00000 0.08664 0.06050 0.11892 = 0.01525 0.02535 -0.00338 C7 1 0.21221 0.73466 0.30716 11.00000 0.04223 0.06842 0.04995 = 0.02294 0.01268 0.01111 H7 2 0.20944 0.79654 0.25955 11.00000 0.09669 0.09942 0.07496 = 0.06594 0.01872 0.01520 C8 1 0.17167 0.61230 0.29212 11.00000 0.03935 0.07437 0.03603 = 0.01268 0.00845 0.00930 H8 2 0.13344 0.57949 0.23198 11.00000 0.08309 0.13599 0.03505 = 0.00320 0.01029 0.00044 C9 1 0.17909 0.52924 0.35258 11.00000 0.03128 0.05649 0.03120 = 0.00356 0.00619 0.00540 C10 1 0.14071 0.40312 0.33838 11.00000 0.04098 0.06197 0.02874 = -0.00602 0.00456 0.00018 H10 2 0.10080 0.37272 0.27847 11.00000 0.09534 0.10437 0.03764 = -0.01862 0.00004 -0.00785 C11 1 0.15532 0.32214 0.39700 11.00000 0.04100 0.04885 0.03238 = -0.01011 0.00592 -0.00216 H11 2 0.12695 0.22586 0.38461 11.00000 0.09122 0.05152 0.05861 = -0.02350 0.01722 -0.01106 C12 1 0.21263 0.35956 0.47621 11.00000 0.02993 0.03747 0.02982 = -0.00631 0.00690 -0.00017 C13 1 0.23580 0.27688 0.53853 11.00000 0.03414 0.03389 0.03265 = -0.00620 0.00804 -0.00015 C14 1 0.28426 0.32138 0.61387 11.00000 0.03529 0.03472 0.03128 = -0.00290 0.00816 0.00050 H14 2 0.30254 0.25785 0.66138 11.00000 0.08680 0.05655 0.04658 = 0.01750 0.00997 0.00016 C15 1 0.24523 0.48613 0.49273 11.00000 0.02673 0.03631 0.02932 = -0.00274 0.00687 0.00143 C16 1 0.22862 0.57047 0.43017 11.00000 0.02708 0.04278 0.03296 = 0.00267 0.00733 0.00450 C17 1 0.38565 0.47680 0.71490 11.00000 0.03666 0.04097 0.03036 = -0.00655 0.00778 0.00125 C18 1 0.35051 0.38854 0.77491 11.00000 0.05391 0.05792 0.03119 = 0.00052 0.00863 -0.00331 H18a 2 0.44030 0.30795 0.77663 11.00000 0.11966 0.09077 0.08974 = 0.03284 0.02917 0.05508 H18b 2 0.38462 0.42936 0.83114 11.00000 0.13731 0.10262 0.04001 = -0.01655 0.02295 -0.02959 H18c 2 0.20760 0.35557 0.76401 11.00000 0.08142 0.12314 0.07549 = 0.01908 0.01999 -0.04180 C19 1 0.22400 0.14156 0.52843 11.00000 0.04303 0.03538 0.04351 = -0.00834 0.01041 -0.00166 C20 1 0.17979 0.06570 0.59286 11.00000 0.05501 0.03603 0.05170 = -0.00040 0.01055 0.00051 H20a 2 0.14663 -0.02693 0.57141 11.00000 0.14729 0.04302 0.10086 = -0.01385 0.02623 -0.01747 H20b 2 0.30318 0.06069 0.64172 11.00000 0.09092 0.09630 0.08546 = 0.02749 -0.02681 0.00002 H20c 2 0.06859 0.10425 0.61503 11.00000 0.12315 0.07370 0.13136 = 0.02480 0.07570 0.03010 HKLF 4 END Q1 1 0.541667 0.475 0.783333 11 0.05 0.1 Q2 1 0.083333 0.4 0.5 11 0.05 0.09 Q3 1 0.166667 0.225 0.483333 11 0.05 0.09 Q4 1 0.416667 0.6 0.466667 11 0.05 0.08 Q5 1 0.083333 0.2 0.333333 11 0.05 0.08 REM The information below was added by Olex2. REM REM R1 = 0.0221 for 2514 Fo > 4sig(Fo) and 0.0277 for all 2945 data REM 375 parameters refined using 0 restraints REM Highest difference peak 0.0950, deepest hole -0.1003 REM Mean Shift 0.0000, Max Shift -0.0003. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0277 REM R1_gt = 0.0221 REM wR_ref = 0.0555 REM GOOF = 1.0974 REM Shift_max = -0.0003 REM Shift_mean = 0.0000 REM Reflections_all = 2945 REM Reflections_gt = 2514 REM Parameters = 375 REM Hole = -0.1003 REM Peak = 0.0950 REM Flack = n/a ; _cod_data_source_file pen5002.cif _cod_data_source_block 190K _cod_database_code 1573203 _chemical_oxdiff_formula 'C20 H14 O2' _olex2_refinement_description ; ; _olex2_refine_details ; Refinement using NoSpherA2, an implementation of NOn-SPHERical Atom-form-factors in Olex2. Please cite: F. Kleemiss et al. Chem. Sci. DOI 10.1039/D0SC05526C - 2021 NoSpherA2 implementation of HAR makes use of tailor-made aspherical atomic form factors calculated on-the-fly from a Hirshfeld-partitioned electron density (ED) - not from spherical-atom form factors. The ED is calculated from a gaussian basis set single determinant SCF wavefunction - either Hartree-Fock or DFT using selected funtionals - for a fragment of the crystal. This fragment can be embedded in an electrostatic crystal field by employing cluster charges or modelled using implicit solvation models, depending on the software used. The following options were used: SOFTWARE: ORCA 5.0 PARTITIONING: NoSpherA2 INT ACCURACY: Normal METHOD: B3LYP BASIS SET: 6-31G(d,p) CHARGE: 0 MULTIPLICITY: 1 DATE: 2024-03-29_16-24-53 ; _iucr_refine_fcf_details ; data_190K _computing_structure_refinement 'olex2.refine 1.5 (Bourhis et al., 2015)' _shelx_refln_list_code 4 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x,y+1/2,-z+1/2 3 -x,-y,-z 4 x,-y-1/2,z-1/2 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 _cell_length_a 7.1945(2) _cell_length_b 10.9948(3) _cell_length_c 17.7698(5) _cell_angle_alpha 90 _cell_angle_beta 102.926(3) _cell_angle_gamma 90 _cell_volume 1370.01(7) loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_calc _refln_F_squared_meas _refln_F_squared_sigma _refln_F_squared_weight _refln_observed_status -9 0 2 0.032 0.492 0.304 861.061 o -9 0 4 0.007 0.369 0.553 274.800 o -9 0 6 49.841 48.977 1.414 19.161 o -9 0 8 0.324 0.516 0.369 569.917 o -9 1 2 3.266 2.309 0.348 375.646 o -9 1 3 1.391 0.922 0.290 667.371 o -9 1 4 19.533 16.650 0.506 84.545 o -9 1 5 12.838 12.127 0.448 123.648 o -9 1 6 6.480 5.100 0.377 233.899 o -9 1 7 1.256 1.230 0.284 682.878 o -9 1 8 23.142 20.052 0.635 64.486 o -9 2 3 6.988 6.517 0.615 135.064 o -9 2 4 45.537 37.563 1.475 20.232 o -9 2 5 4.612 2.828 0.492 219.988 o -9 2 6 53.160 41.682 1.537 17.769 o -8 0 2 0.001 -0.246 0.739 156.290 o -8 0 4 65.688 62.485 2.021 11.278 o -8 0 6 15.514 15.592 1.598 26.910 o -8 0 8 33.628 34.682 1.456 23.386 o -8 0 10 10.740 13.005 1.045 55.599 o -8 0 12 0.143 -0.270 0.423 468.365 o -8 0 14 24.565 24.229 0.953 43.950 o -8 1 1 24.178 24.216 0.844 49.240 o -8 1 2 62.619 60.372 1.230 17.781 o -8 1 3 110.536 107.758 1.836 7.971 o -8 1 4 370.628 374.247 4.992 1.094 o -8 1 5 114.371 111.654 2.976 5.150 o -8 1 6 80.373 81.184 1.988 9.842 o -8 1 7 5.339 6.879 0.583 153.616 o -8 1 8 9.876 9.382 0.710 97.755 o -8 1 9 3.249 3.043 0.419 293.428 o -8 1 10 24.567 23.117 0.695 56.925 o -8 1 11 81.379 81.814 1.396 12.661 o -8 1 12 23.953 23.374 0.730 55.700 o -8 1 13 9.541 8.681 0.460 151.927 o -8 1 14 0.234 0.861 0.319 725.181 o -8 1 15 1.970 1.414 0.430 342.856 o -8 2 1 25.053 26.017 0.752 51.888 o -8 2 2 6.430 7.015 0.515 167.098 o -8 2 3 92.008 91.509 1.611 10.321 o -8 2 4 565.771 585.185 11.867 0.334 o -8 2 5 261.926 268.376 4.195 1.813 o -8 2 6 118.541 122.501 2.603 5.633 o -8 2 7 21.982 21.528 0.798 55.285 o -8 2 8 0.718 0.862 0.484 326.311 o -8 2 9 49.759 49.506 1.159 22.425 o -8 2 10 38.975 40.797 0.996 30.071 o -8 2 11 15.960 16.473 0.614 83.697 o -8 2 12 4.901 4.926 0.461 217.325 o -8 2 13 0.888 0.736 0.330 615.756 o -8 2 14 3.530 3.144 0.283 419.491 o -8 3 1 11.641 11.474 0.612 103.851 o -8 3 2 104.478 106.977 1.935 8.007 o -8 3 3 17.409 16.540 0.691 73.251 o -8 3 4 3.277 4.704 0.445 255.367 o -8 3 5 156.892 159.343 2.659 4.307 o -8 3 6 48.004 49.392 1.039 24.626 o -8 3 7 4.826 4.215 0.423 245.503 o -8 3 8 17.788 19.364 0.691 69.991 o -8 3 9 1.976 2.022 0.449 313.192 o -8 3 10 7.763 9.022 0.543 141.580 o -8 3 11 0.926 0.972 0.366 510.754 o -8 3 12 38.326 32.951 0.847 35.715 o -8 3 13 17.699 16.046 1.045 47.922 o -8 3 14 0.294 -0.246 0.369 597.028 o -8 4 1 1.387 2.090 0.738 141.768 o -8 4 2 5.567 4.656 0.648 139.265 o -8 4 3 30.363 31.968 1.783 18.790 o -8 4 4 0.478 0.804 0.542 271.315 o -8 4 5 9.711 10.882 0.782 85.571 o -8 4 6 3.800 4.517 0.629 157.242 o -8 4 7 0.057 0.612 0.542 282.282 o -8 4 8 3.407 2.561 0.565 197.488 o -8 4 9 0.038 0.369 0.676 184.543 o -8 4 10 3.447 3.935 0.738 126.435 o -8 4 11 37.154 35.718 1.598 20.152 o -8 4 12 4.586 2.582 0.553 190.301 o -8 4 13 9.226 7.193 0.615 121.921 o -8 5 1 33.381 35.541 1.195 28.788 o -8 5 2 0.653 0.922 0.676 176.502 o -8 5 3 1.250 1.168 0.738 145.235 o -8 5 4 56.381 57.973 2.336 10.163 o -8 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6 14 33.666 32.437 2.551 10.669 o 0 6 15 2.101 2.158 0.667 163.725 o 0 6 16 2.853 4.443 1.518 35.194 o 0 6 17 0.005 0.364 0.760 146.743 o 0 6 18 19.865 20.682 0.758 60.933 o 0 6 19 16.089 15.870 0.784 68.090 o 0 7 1 9.161 9.264 1.086 55.886 o 0 7 2 86.638 90.522 3.549 4.761 o 0 7 3 2.100 1.410 0.612 193.214 o 0 7 4 62.294 64.342 2.318 9.770 o 0 7 5 71.013 65.832 3.227 5.994 o 0 7 6 5.872 6.448 1.072 62.175 o 0 7 7 61.016 63.822 2.715 8.006 o 0 7 8 175.485 184.291 4.448 2.419 o 0 7 9 236.886 238.880 6.715 1.223 o 0 7 10 441.343 446.847 14.416 0.305 o 0 7 11 391.626 408.179 10.170 0.524 o 0 7 12 39.269 33.259 3.135 7.394 o 0 7 13 1.612 2.167 1.844 24.630 o 0 7 14 36.359 38.049 1.392 23.507 o 0 7 15 3.232 4.473 0.626 163.047 o 0 7 16 18.471 19.209 0.923 52.948 o 0 7 17 32.718 34.477 0.959 35.371 o 0 7 18 3.125 2.890 0.454 270.013 o 0 7 19 22.695 23.361 1.107 39.092 o 0 8 0 44.700 46.374 5.594 2.549 o 0 8 1 7.112 8.301 0.889 79.648 o 0 8 2 5.427 5.615 1.019 68.788 o 0 8 3 341.510 364.263 8.977 0.666 o 0 8 4 592.562 609.056 13.693 0.274 o 0 8 5 1001.580 1032.060 17.675 0.132 o 0 8 6 731.707 735.343 11.396 0.274 o 0 8 7 346.737 352.714 6.262 0.985 o 0 8 8 24.205 23.138 1.599 23.964 o 0 8 9 9.009 10.612 1.412 36.215 o 0 8 10 16.267 17.419 1.713 23.696 o 0 8 11 22.076 24.456 1.931 18.215 o 0 8 12 39.979 39.051 1.418 22.089 o 0 8 13 18.736 18.709 1.379 32.056 o 0 8 14 4.536 4.437 0.790 108.306 o 0 8 15 10.992 11.744 0.780 81.963 o 0 8 16 61.223 64.576 1.498 15.339 o 0 8 17 39.474 37.896 1.151 27.218 o 0 8 18 10.418 8.819 0.522 131.628 o 0 9 1 13.996 14.348 1.239 40.840 o 0 9 2 4.880 6.297 1.146 56.488 o 0 9 3 116.722 125.978 3.770 3.779 o 0 9 4 554.919 569.918 10.790 0.376 o 0 9 5 509.614 525.446 10.092 0.434 o 0 9 6 3.321 4.313 1.087 64.985 o 0 9 7 7.501 7.928 1.005 65.834 o 0 9 8 21.888 22.604 1.781 20.861 o 0 9 9 47.861 54.100 3.689 5.306 o 0 9 10 93.238 98.431 2.614 6.675 o 0 9 11 43.605 48.541 2.859 8.241 o 0 9 12 0.471 0.357 0.633 205.488 o 0 9 13 2.649 2.566 0.752 129.257 o 0 9 14 8.628 9.071 0.847 81.414 o 0 9 15 0.144 -0.118 0.560 269.180 o 0 9 16 22.857 26.656 0.977 43.261 o 0 10 0 14.155 15.062 2.336 14.163 o 0 10 1 114.410 123.177 4.478 3.031 o 0 10 2 15.620 13.032 1.499 30.157 o 0 10 3 276.751 287.535 6.363 1.168 o 0 10 4 43.590 45.785 2.082 13.210 o 0 10 5 0.196 0.625 0.747 149.772 o 0 10 6 3.128 3.400 0.834 105.171 o 0 10 7 39.120 41.404 1.757 17.239 o 0 10 8 13.987 14.410 1.018 53.611 o 0 10 9 48.750 49.120 3.627 5.483 o 0 10 10 0.778 1.045 0.826 119.729 o 0 10 11 6.848 7.070 1.291 44.358 o 0 10 12 8.611 8.967 0.840 82.442 o 0 10 13 3.024 3.321 1.383 42.129 o 0 10 14 0.484 0.816 0.472 349.687 o 0 10 15 3.029 2.927 0.455 270.981 o 0 11 1 6.705 7.563 0.599 137.862 o 0 11 2 4.570 4.863 0.554 178.660 o 0 11 3 59.463 59.260 1.343 17.366 o 0 11 4 14.836 14.250 0.770 72.936 o 0 11 5 83.887 82.295 1.740 10.706 o 0 11 6 29.762 30.255 0.913 39.778 o 0 11 7 1.427 1.454 0.658 176.333 o 0 11 8 0.083 0.564 0.735 155.463 o 0 11 9 35.529 36.865 1.476 22.344 o 0 11 10 42.408 43.550 1.496 19.976 o 0 11 11 23.426 25.209 1.128 37.362 o 0 11 12 0.589 0.455 0.346 613.746 o 0 11 13 5.887 4.980 0.615 146.260 o 0 12 0 18.585 17.868 1.151 41.254 o 0 12 1 54.630 56.236 1.423 17.611 o 0 12 2 4.381 4.850 0.427 245.432 o 0 12 3 0.063 0.027 0.458 402.859 o 0 12 4 0.173 0.169 0.382 562.092 o 0 12 5 60.834 62.441 1.024 19.848 o 0 12 6 0.111 0.420 0.683 179.814 o 0 12 7 2.714 2.951 0.922 89.760 o 0 12 8 7.909 7.819 1.445 35.826 o 0 12 9 33.838 33.775 1.783 18.160 o 0 12 10 30.997 33.812 1.537 22.571 o 0 12 11 66.815 61.231 2.090 10.836 o 0 13 1 0.001 -0.445 0.324 814.841 o 0 13 2 71.770 76.022 1.540 13.136 o 0 13 3 18.232 18.314 0.509 85.507 o 0 13 4 99.978 101.700 1.947 8.321 o 0 13 5 34.247 33.312 0.967 34.645 o 0 13 6 6.093 5.935 0.434 207.531 o 0 13 7 5.612 4.307 0.478 203.860 o 0 13 8 11.953 10.451 0.738 86.615 o 0 14 1 3.894 2.459 0.430 276.386 o 1 0 0 761.434 744.060 21.394 0.131 o 1 0 2 3075.680 3156.240 86.253 0.008 o 1 0 4 8931.770 8258.080 398.680 0.000 o 1 0 6 3783.570 3857.820 107.954 0.005 o 1 0 8 11.551 9.467 2.889 9.738 o 1 0 10 99.061 97.589 4.672 3.036 o 1 0 12 5.566 8.484 1.721 26.627 o 1 0 14 12.916 13.402 2.213 15.783 o 1 0 16 13.334 12.553 2.705 10.906 o 1 0 18 6.583 7.298 0.674 120.491 o 1 0 20 348.808 357.741 6.803 0.903 o 1 1 0 287.867 280.125 4.492 1.587 o 1 1 1 68.295 70.661 1.890 11.557 o 1 1 2 914.968 931.181 19.258 0.132 o 1 1 3 206.701 202.516 4.658 2.076 o 1 1 4 24.857 26.005 2.521 11.494 o 1 1 5 14.299 13.909 1.511 30.068 o 1 1 6 2087.440 2077.530 42.906 0.027 o 1 1 7 1970.940 1874.420 39.754 0.031 o 1 1 8 572.788 548.469 14.976 0.254 o 1 1 9 335.404 326.130 10.976 0.520 o 1 1 10 0.000 0.319 0.721 163.226 o 1 1 11 0.401 0.366 0.703 168.167 o 1 1 12 144.009 146.714 4.716 2.554 o 1 1 13 38.238 37.723 2.223 12.740 o 1 1 14 162.744 167.795 4.351 2.623 o 1 1 15 67.526 69.039 4.365 3.746 o 1 1 16 165.725 171.966 6.278 1.597 o 1 1 17 19.180 19.607 0.793 60.257 o 1 1 18 26.639 28.654 0.764 48.469 o 1 1 19 4.002 3.410 0.568 185.154 o 1 1 20 47.289 44.026 0.957 27.015 o 1 1 21 83.134 76.386 1.826 10.571 o 1 2 0 261.513 260.406 3.979 1.907 o 1 2 1 1984.740 1934.130 29.541 0.041 o 1 2 2 80.500 78.115 2.229 8.878 o 1 2 3 2295.300 2070.700 35.059 0.031 o 1 2 4 23.795 25.803 1.690 21.937 o 1 2 5 1.161 1.757 0.857 109.024 o 1 2 6 1131.970 1142.120 25.300 0.081 o 1 2 7 2157.060 2072.000 43.558 0.026 o 1 2 8 1926.750 1822.270 39.537 0.032 o 1 2 9 109.197 95.925 5.299 2.443 o 1 2 10 81.287 79.362 2.899 6.502 o 1 2 11 6.171 5.634 0.885 85.021 o 1 2 12 92.925 86.319 2.756 6.481 o 1 2 13 204.231 204.985 4.921 1.961 o 1 2 14 241.288 240.551 5.618 1.501 o 1 2 15 35.781 34.612 3.074 7.720 o 1 2 16 3.212 4.549 0.941 83.839 o 1 2 17 189.987 190.132 2.316 3.792 o 1 2 18 14.005 13.684 0.576 97.385 o 1 2 19 4.065 4.957 0.403 265.336 o 1 2 20 5.343 5.451 0.391 243.188 o 1 3 0 6334.880 5910.810 306.743 0.001 o 1 3 1 26.761 20.954 1.304 31.002 o 1 3 2 693.385 632.895 39.015 0.051 o 1 3 3 552.901 537.796 12.236 0.334 o 1 3 4 341.355 330.354 6.392 0.995 o 1 3 5 1217.860 1174.110 20.885 0.095 o 1 3 6 1853.940 1772.490 37.255 0.035 o 1 3 7 81.213 80.325 4.369 3.582 o 1 3 8 4.513 6.927 3.135 8.514 o 1 3 9 70.377 67.479 2.638 7.907 o 1 3 10 140.754 137.429 3.465 3.783 o 1 3 11 1.051 1.449 0.627 195.860 o 1 3 12 249.230 251.846 4.825 1.701 o 1 3 13 37.157 36.731 2.630 9.909 o 1 3 14 20.736 20.726 1.760 21.595 o 1 3 15 4.556 5.153 0.930 82.165 o 1 3 16 96.117 97.558 1.870 8.893 o 1 3 17 3.011 3.135 0.370 345.542 o 1 3 18 0.868 0.910 0.421 409.886 o 1 3 19 6.000 6.081 0.436 206.770 o 1 3 20 62.895 56.874 0.912 21.084 o 1 4 0 163.740 166.691 4.169 2.750 o 1 4 1 1071.400 1054.790 18.944 0.118 o 1 4 2 181.190 191.932 9.406 0.814 o 1 4 3 261.309 257.085 8.294 0.875 o 1 4 4 168.956 170.509 6.581 1.482 o 1 4 5 2163.820 2103.080 62.645 0.016 o 1 4 6 2594.850 2437.020 72.236 0.012 o 1 4 7 6.647 10.697 3.012 9.105 o 1 4 8 1.986 2.570 0.890 98.011 o 1 4 9 17.736 17.677 1.456 30.120 o 1 4 10 259.846 260.519 6.890 1.120 o 1 4 11 53.599 51.421 3.473 5.793 o 1 4 12 90.131 92.708 5.164 2.645 o 1 4 13 49.452 52.379 3.812 5.009 o 1 4 14 38.427 37.106 2.304 12.085 o 1 4 15 28.243 29.571 2.828 9.232 o 1 4 16 6.272 5.645 0.600 146.196 o 1 4 17 0.630 0.983 0.524 283.460 o 1 4 18 6.558 6.316 0.823 93.109 o 1 4 19 0.076 0.296 0.586 245.114 o 1 4 20 11.656 10.026 0.469 131.836 o 1 5 0 875.463 887.256 17.078 0.156 o 1 5 1 429.100 423.322 9.700 0.527 o 1 5 2 35.087 32.927 2.947 8.337 o 1 5 3 80.726 76.539 6.271 1.943 o 1 5 4 6.463 8.361 2.521 12.899 o 1 5 5 21.531 24.468 3.996 5.049 o 1 5 6 0.449 0.449 1.414 42.358 o 1 5 7 148.548 157.500 7.777 1.178 o 1 5 8 1.683 1.481 0.746 138.840 o 1 5 9 188.739 188.410 5.715 1.721 o 1 5 10 24.834 26.559 1.869 18.655 o 1 5 11 0.003 -0.246 0.884 109.216 o 1 5 12 15.483 16.403 2.152 16.234 o 1 5 13 0.274 0.523 1.000 84.325 o 1 5 14 115.353 117.360 6.148 1.865 o 1 5 15 6.212 6.332 1.414 38.264 o 1 5 16 27.076 33.874 2.889 8.863 o 1 5 17 11.015 12.385 0.828 75.732 o 1 5 18 10.899 10.204 0.697 95.374 o 1 5 19 33.640 35.891 0.957 34.569 o 1 6 0 3.787 5.164 2.275 16.018 o 1 6 1 45.290 53.670 5.902 2.295 o 1 6 2 481.455 457.391 19.673 0.182 o 1 6 3 60.087 55.330 5.902 2.253 o 1 6 4 250.855 241.695 7.271 1.076 o 1 6 5 158.695 145.730 4.732 2.458 o 1 6 6 144.777 140.547 3.739 3.418 o 1 6 7 37.670 43.462 2.041 14.194 o 1 6 8 462.185 474.575 16.937 0.233 o 1 6 9 991.294 1015.240 30.185 0.069 o 1 6 10 0.472 -0.658 0.975 88.835 o 1 6 11 199.763 208.594 6.212 1.481 o 1 6 12 3.204 2.126 1.041 72.013 o 1 6 13 49.983 51.801 3.289 6.399 o 1 6 14 1.098 1.367 0.708 157.014 o 1 6 15 31.213 31.378 1.347 26.679 o 1 6 16 0.005 0.000 0.708 170.044 o 1 6 17 6.766 8.497 0.697 112.228 o 1 6 18 15.357 16.106 0.598 87.362 o 1 6 19 3.374 3.443 0.615 170.413 o 1 7 0 3.550 2.540 0.606 176.801 o 1 7 1 3.283 2.985 0.625 168.971 o 1 7 2 209.403 209.356 3.817 2.465 o 1 7 3 1.051 0.761 0.637 194.366 o 1 7 4 1.884 0.930 0.540 245.689 o 1 7 5 11.365 10.911 0.966 62.536 o 1 7 6 4.073 4.645 0.812 104.769 o 1 7 7 322.346 332.952 7.537 0.862 o 1 7 8 757.289 780.015 17.038 0.175 o 1 7 9 1845.650 1914.480 38.515 0.033 o 1 7 10 206.111 196.665 5.995 1.552 o 1 7 11 255.211 258.328 10.021 0.665 o 1 7 12 79.994 85.453 4.857 3.005 o 1 7 13 109.115 107.127 2.831 5.603 o 1 7 14 7.853 7.915 0.711 106.580 o 1 7 15 10.507 9.108 1.128 51.572 o 1 7 16 54.728 53.481 1.420 17.850 o 1 7 17 40.244 42.149 0.983 29.544 o 1 7 18 9.496 8.717 0.736 95.655 o 1 8 0 42.130 43.419 1.536 19.482 o 1 8 1 4.532 5.382 0.775 109.900 o 1 8 2 6.224 6.877 1.038 64.828 o 1 8 3 266.182 267.018 4.994 1.556 o 1 8 4 121.028 127.285 3.017 4.789 o 1 8 5 150.577 145.444 4.611 2.593 o 1 8 6 120.344 114.630 3.934 3.601 o 1 8 7 0.183 -0.246 0.910 102.593 o 1 8 8 0.450 -0.246 1.414 42.469 o 1 8 9 173.939 182.895 7.808 1.119 o 1 8 10 3.154 2.398 1.414 40.571 o 1 8 11 107.440 111.256 2.809 5.638 o 1 8 12 3.711 3.298 0.630 162.312 o 1 8 13 9.175 10.086 0.764 90.414 o 1 8 14 2.970 2.311 0.566 203.701 o 1 8 15 4.830 4.264 0.539 185.464 o 1 8 16 31.881 32.015 1.260 28.388 o 1 8 17 11.491 9.127 0.459 137.577 o 1 9 0 39.977 40.105 2.019 14.345 o 1 9 1 10.203 10.111 1.086 54.475 o 1 9 2 19.334 21.324 1.235 36.411 o 1 9 3 213.823 212.653 5.063 1.842 o 1 9 4 469.915 475.495 9.286 0.510 o 1 9 5 150.448 143.364 4.820 2.453 o 1 9 6 19.742 18.812 2.336 13.655 o 1 9 7 26.482 33.628 2.828 9.223 o 1 9 8 36.804 37.194 3.320 6.713 o 1 9 9 3.668 3.960 1.021 72.407 o 1 9 10 73.430 78.276 2.520 8.035 o 1 9 11 34.498 34.449 1.246 27.434 o 1 9 12 2.395 2.192 1.045 72.599 o 1 9 13 0.828 0.661 0.505 302.000 o 1 9 14 1.251 1.967 0.565 229.175 o 1 9 15 0.388 0.676 0.615 216.065 o 1 9 16 7.837 6.494 0.646 123.225 o 1 10 0 9.194 7.336 1.343 40.148 o 1 10 1 3.619 3.223 0.882 94.346 o 1 10 2 121.185 116.190 3.441 4.229 o 1 10 3 440.892 438.118 8.731 0.578 o 1 10 4 47.845 49.581 2.115 12.446 o 1 10 5 19.262 20.306 1.739 22.314 o 1 10 6 43.853 44.909 1.877 15.125 o 1 10 7 0.033 0.238 0.603 232.415 o 1 10 8 6.040 7.774 1.168 53.014 o 1 10 9 5.401 6.640 0.827 95.053 o 1 10 10 5.119 5.863 0.890 86.217 o 1 10 11 9.812 10.852 0.910 70.237 o 1 10 12 1.786 2.929 0.652 169.749 o 1 10 13 15.163 20.841 1.353 33.953 o 1 10 14 15.105 15.800 1.045 50.199 o 1 11 0 0.004 0.127 0.418 484.676 o 1 11 1 18.201 17.189 0.706 69.996 o 1 11 2 11.137 10.290 0.567 115.718 o 1 11 3 16.758 16.598 0.653 77.940 o 1 11 4 62.572 63.841 1.347 16.476 o 1 11 5 7.985 7.484 0.650 119.377 o 1 11 6 4.743 4.388 0.852 95.406 o 1 11 7 3.754 3.434 0.803 109.767 o 1 11 8 3.211 3.523 0.631 164.769 o 1 11 9 4.481 5.088 0.830 99.248 o 1 11 10 1.831 2.940 0.592 199.051 o 1 11 11 19.555 20.488 0.697 65.650 o 1 11 12 8.371 7.131 0.676 112.929 o 1 12 0 1.283 1.280 0.391 430.580 o 1 12 1 6.690 6.762 0.521 163.987 o 1 12 2 0.029 0.165 0.436 443.506 o 1 12 3 15.266 16.169 0.588 88.507 o 1 12 4 2.215 2.206 0.419 334.370 o 1 12 5 10.785 10.676 0.984 61.878 o 1 12 6 6.973 6.200 0.760 103.235 o 1 12 7 0.832 0.401 0.586 232.357 o 1 12 8 17.136 17.968 0.866 58.819 o 1 12 9 48.120 49.071 1.445 19.088 o 1 12 10 0.041 -0.221 0.324 806.355 o 1 13 0 1.667 1.676 0.282 614.321 o 1 13 1 2.068 2.074 0.321 482.289 o 1 13 2 13.129 12.808 0.466 117.709 o 1 13 3 1.183 0.774 0.274 761.271 o 1 13 4 0.924 0.839 0.259 862.375 o 1 13 5 0.344 0.388 0.305 807.275 o 1 13 7 0.321 0.461 0.304 808.440 o 2 0 0 62980.400 61471.100 1631.980 0.000 o 2 0 2 1474.470 1503.430 44.202 0.032 o 2 0 4 96.792 103.835 6.455 1.778 o 2 0 6 199.765 194.330 10.636 0.649 o 2 0 8 28.275 25.206 4.242 4.453 o 2 0 10 1.020 2.302 1.230 54.600 o 2 0 12 152.333 154.369 7.070 1.374 o 2 0 14 9.477 9.222 2.152 17.120 o 2 0 16 132.229 137.381 3.773 3.536 o 2 0 18 8.944 8.597 0.686 106.232 o 2 0 20 101.319 96.028 3.135 5.268 o 2 1 0 1358.440 1387.010 23.319 0.075 o 2 1 1 3801.920 3769.170 79.921 0.008 o 2 1 2 7.611 7.321 1.291 43.830 o 2 1 3 378.424 387.163 15.308 0.295 o 2 1 4 29.208 29.118 1.939 16.961 o 2 1 5 573.681 574.836 14.367 0.265 o 2 1 6 59.529 58.144 4.887 3.164 o 2 1 7 338.197 326.228 10.846 0.528 o 2 1 8 139.590 140.693 4.623 2.670 o 2 1 9 104.768 110.433 3.178 4.978 o 2 1 10 40.857 43.117 1.982 14.480 o 2 1 11 65.018 63.459 2.825 7.453 o 2 1 12 215.005 225.981 7.162 1.172 o 2 1 13 121.156 131.297 4.651 2.798 o 2 1 14 53.649 55.354 2.329 10.427 o 2 1 15 26.021 33.370 1.794 19.150 o 2 1 16 2.073 2.202 0.417 341.619 o 2 1 17 19.263 20.355 0.651 69.618 o 2 1 18 2.809 2.425 0.391 342.102 o 2 1 19 0.209 0.340 0.338 694.886 o 2 1 20 1.408 1.173 0.326 556.345 o 2 2 0 951.815 944.383 16.587 0.150 o 2 2 1 490.935 480.629 8.243 0.555 o 2 2 2 121.332 115.260 3.491 4.163 o 2 2 3 426.486 434.887 9.654 0.528 o 2 2 4 73.528 74.813 2.760 7.232 o 2 2 5 118.814 115.528 5.151 2.461 o 2 2 6 32.296 31.773 2.395 11.910 o 2 2 7 1.563 0.615 1.476 38.395 o 2 2 8 43.955 44.208 1.890 15.017 o 2 2 9 81.846 78.386 2.587 7.475 o 2 2 10 3.930 5.148 0.971 77.593 o 2 2 11 40.083 44.559 2.391 11.114 o 2 2 12 1376.440 1410.310 29.017 0.059 o 2 2 13 741.409 760.846 13.783 0.226 o 2 2 14 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9 10.306 10.328 1.844 22.490 o 3 4 10 0.139 -0.130 1.260 53.632 o 3 4 11 1.935 2.334 1.137 62.417 o 3 4 12 33.087 31.661 3.074 7.828 o 3 4 13 0.000 0.257 0.703 171.781 o 3 4 14 0.000 0.680 0.660 192.342 o 3 4 15 1.006 0.758 0.716 156.385 o 3 4 16 6.259 6.193 0.735 110.657 o 3 4 17 0.769 0.715 0.516 291.212 o 3 4 18 0.208 -0.004 0.324 777.657 o 3 5 0 399.366 395.277 5.483 0.949 o 3 5 1 161.598 159.861 2.875 3.981 o 3 5 2 3.424 3.148 0.583 185.472 o 3 5 3 15.134 16.511 1.060 48.966 o 3 5 4 366.902 378.093 8.097 0.721 o 3 5 5 266.932 269.440 6.438 1.192 o 3 5 6 1.247 2.213 1.230 54.448 o 3 5 7 757.307 761.704 23.300 0.116 o 3 5 8 143.535 153.140 6.885 1.452 o 3 5 9 1.854 2.565 1.063 70.785 o 3 5 10 66.612 69.529 3.151 6.261 o 3 5 11 48.449 45.694 2.543 9.707 o 3 5 12 150.415 152.562 2.740 4.391 o 3 5 13 87.397 89.763 3.013 5.914 o 3 5 14 0.326 0.061 0.984 87.465 o 3 5 15 27.400 27.035 1.238 31.504 o 3 5 16 1.393 0.902 0.576 227.275 o 3 5 17 9.527 10.428 0.629 110.869 o 3 6 0 195.186 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379.813 5.646 0.969 o 4 3 3 25.406 25.225 1.203 33.782 o 4 3 4 1.899 1.220 0.629 187.346 o 4 3 5 1.747 2.035 0.695 155.398 o 4 3 6 105.619 115.417 3.239 4.807 o 4 3 7 10.462 10.730 1.345 38.552 o 4 3 8 109.160 112.873 3.265 4.722 o 4 3 9 1.069 1.288 0.934 93.525 o 4 3 10 500.368 519.056 9.914 0.448 o 4 3 11 771.987 776.629 13.877 0.217 o 4 3 12 206.625 211.107 2.680 3.156 o 4 3 13 166.373 159.620 2.593 4.205 o 4 3 14 72.834 71.768 1.356 14.438 o 4 3 15 0.750 0.972 0.472 338.233 o 4 3 16 3.021 2.645 0.499 241.886 o 4 4 0 164.434 170.113 4.866 2.273 o 4 4 1 1.153 1.904 0.670 171.130 o 4 4 2 43.752 42.886 2.341 11.295 o 4 4 3 7.746 6.754 1.044 62.397 o 4 4 4 16.191 15.840 1.558 27.829 o 4 4 5 272.268 273.965 7.345 1.003 o 4 4 6 0.177 1.322 1.000 83.733 o 4 4 7 58.722 58.688 2.859 7.596 o 4 4 8 26.849 29.263 2.828 9.286 o 4 4 9 3.229 7.070 1.844 23.936 o 4 4 10 4.768 5.409 1.130 58.463 o 4 4 11 36.289 37.031 1.324 24.913 o 4 4 12 63.704 63.402 1.685 13.656 o 4 4 13 76.257 78.629 3.443 5.242 o 4 4 14 0.176 0.013 0.603 232.246 o 4 4 15 2.504 2.459 0.545 220.666 o 4 4 16 6.634 5.562 0.615 139.844 o 4 5 0 243.603 242.152 4.107 2.007 o 4 5 1 219.351 223.390 3.885 2.309 o 4 5 2 48.739 51.076 2.021 13.054 o 4 5 3 85.676 84.542 2.816 6.547 o 4 5 4 12.594 11.417 1.133 48.622 o 4 5 5 214.007 226.378 5.240 1.745 o 4 5 6 15.165 13.145 1.514 29.810 o 4 5 7 315.587 324.933 8.517 0.754 o 4 5 8 174.504 186.176 5.736 1.764 o 4 5 9 107.478 105.446 4.180 3.479 o 4 5 10 123.518 128.096 2.403 5.805 o 4 5 11 5.515 7.068 0.667 127.742 o 4 5 12 5.886 6.763 1.291 45.036 o 4 5 13 52.934 54.100 2.459 9.758 o 4 5 14 19.359 20.626 1.475 28.579 o 4 5 15 9.376 8.914 0.984 64.818 o 4 5 16 1.632 0.615 0.430 369.200 o 4 6 0 46.565 49.039 2.383 10.671 o 4 6 1 0.073 0.734 0.571 253.454 o 4 6 2 17.931 16.164 1.273 36.821 o 4 6 3 29.875 30.749 1.491 24.059 o 4 6 4 54.045 56.768 2.234 10.941 o 4 6 5 22.320 22.600 1.289 32.882 o 4 6 6 267.964 278.856 6.078 1.258 o 4 6 7 302.272 315.077 6.764 1.019 o 4 6 8 229.417 232.591 6.577 1.279 o 4 6 9 32.885 34.719 1.093 31.627 o 4 6 10 1.587 1.603 0.559 230.920 o 4 6 11 3.545 3.205 0.673 148.056 o 4 6 12 9.969 9.399 0.744 92.272 o 4 6 13 4.258 3.990 0.476 225.736 o 4 6 14 15.760 15.140 0.735 73.700 o 4 6 15 4.402 3.566 0.615 161.645 o 4 7 0 20.971 20.601 1.190 37.492 o 4 7 1 8.537 9.331 0.806 86.884 o 4 7 2 7.684 7.508 0.765 98.031 o 4 7 3 7.816 7.082 0.958 71.036 o 4 7 4 26.764 30.849 1.917 17.445 o 4 7 5 63.621 64.593 5.103 2.896 o 4 7 6 56.977 58.588 3.996 4.504 o 4 7 7 104.023 99.904 2.083 7.758 o 4 7 8 78.541 79.208 1.893 10.469 o 4 7 9 1.134 1.276 0.522 271.633 o 4 7 10 62.805 66.187 1.504 14.986 o 4 7 11 47.953 49.689 1.395 19.685 o 4 7 12 2.677 1.571 0.629 178.305 o 4 7 13 10.442 9.464 0.555 122.962 o 4 7 14 35.913 31.094 1.045 32.321 o 4 8 0 7.755 6.849 1.238 47.107 o 4 8 1 17.717 16.894 1.630 25.418 o 4 8 2 111.725 113.040 3.384 4.483 o 4 8 3 21.128 22.383 1.501 27.141 o 4 8 4 0.067 1.345 0.798 130.532 o 4 8 5 31.191 30.773 1.178 30.928 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14.258 0.258 o 5 1 7 22.984 19.904 1.804 20.490 o 5 1 8 1.588 1.227 2.152 18.231 o 5 1 9 0.049 0.492 0.956 92.626 o 5 1 10 11.369 11.700 0.755 84.281 o 5 1 11 0.128 -0.370 0.471 380.226 o 5 1 12 11.699 13.527 0.989 58.687 o 5 1 13 16.264 16.784 1.414 32.134 o 5 1 14 1.928 2.682 0.676 159.424 o 5 1 15 12.368 11.619 0.922 64.685 o 5 2 0 35.541 34.656 1.829 17.253 o 5 2 1 1.211 1.347 0.686 165.818 o 5 2 2 9.717 9.048 1.016 61.301 o 5 2 3 191.357 192.145 4.601 2.215 o 5 2 4 45.697 44.200 1.976 14.026 o 5 2 5 7.836 9.126 1.121 54.432 o 5 2 6 2.779 3.903 0.911 90.517 o 5 2 7 20.686 17.733 1.695 23.193 o 5 2 8 6.694 4.514 1.120 57.855 o 5 2 9 1.016 0.011 0.997 83.841 o 5 2 10 30.514 31.966 0.932 38.125 o 5 2 11 46.316 45.575 1.870 14.892 o 5 2 12 24.092 21.956 1.217 34.656 o 5 2 13 35.060 34.827 1.348 25.090 o 5 2 14 7.261 7.326 0.691 113.823 o 5 2 15 22.076 18.290 2.705 10.441 o 5 3 0 51.583 52.480 3.320 6.264 o 5 3 1 38.815 43.199 2.369 11.382 o 5 3 2 263.007 264.357 6.222 1.254 o 5 3 3 11.315 10.153 1.061 55.237 o 5 3 4 6.419 6.832 1.147 54.794 o 5 3 5 46.288 47.303 2.054 13.150 o 5 3 6 54.753 52.903 3.195 6.586 o 5 3 7 15.330 17.715 1.673 24.794 o 5 3 8 103.008 101.875 5.779 2.131 o 5 3 9 0.147 0.484 0.644 201.119 o 5 3 10 4.487 4.562 0.642 148.107 o 5 3 11 38.835 40.096 1.673 18.444 o 5 3 12 154.396 151.909 3.673 3.318 o 5 3 13 5.868 5.495 0.716 117.757 o 5 3 14 3.810 3.980 0.799 109.545 o 5 3 15 16.740 10.205 0.738 76.324 o 5 4 0 19.127 21.087 2.459 12.449 o 5 4 1 1.441 0.738 1.230 54.905 o 5 4 2 86.304 82.257 4.795 3.040 o 5 4 3 17.615 20.410 2.459 12.553 o 5 4 4 345.671 361.621 9.126 0.650 o 5 4 5 58.347 61.285 2.697 8.222 o 5 4 6 15.388 14.585 2.859 9.732 o 5 4 7 0.221 -0.021 0.989 86.887 o 5 4 8 35.697 40.623 1.963 15.322 o 5 4 9 4.677 4.938 1.783 25.459 o 5 4 10 67.258 71.477 2.001 10.961 o 5 4 11 0.246 0.248 0.716 163.602 o 5 4 12 5.840 4.751 0.735 115.032 o 5 4 13 6.843 5.723 0.648 129.432 o 5 4 14 8.672 8.240 0.443 164.990 o 5 5 0 188.163 195.285 7.020 1.284 o 5 5 1 8.006 8.453 1.025 62.855 o 5 5 2 241.417 245.915 6.882 1.170 o 5 5 3 219.458 227.770 5.321 1.693 o 5 5 4 91.411 93.244 3.028 5.744 o 5 5 5 79.367 76.645 2.351 8.474 o 5 5 6 263.632 267.398 5.185 1.510 o 5 5 7 135.332 141.183 2.078 5.845 o 5 5 8 0.042 0.471 0.449 409.365 o 5 5 9 5.899 6.917 0.577 151.533 o 5 5 10 2.151 1.574 0.612 191.794 o 5 5 11 15.475 14.408 0.910 59.847 o 5 5 12 0.009 -0.288 0.676 186.570 o 5 5 13 1.515 1.084 0.366 467.620 o 5 6 0 0.852 0.518 0.682 173.685 o 5 6 1 73.909 73.759 2.613 7.756 o 5 6 2 51.814 53.855 2.666 8.750 o 5 6 3 31.710 33.968 1.786 18.401 o 5 6 4 12.852 11.735 1.158 46.756 o 5 6 5 78.084 74.625 1.778 11.257 o 5 6 6 374.797 377.967 4.020 1.215 o 5 6 7 372.281 377.045 3.983 1.229 o 5 6 8 68.057 67.191 1.251 16.168 o 5 6 9 1.638 1.907 0.413 367.487 o 5 6 10 15.790 15.402 0.653 81.401 o 5 6 11 3.507 3.031 0.484 240.044 o 5 6 12 58.521 55.137 1.937 12.694 o 5 6 13 1.496 1.260 0.304 596.532 o 5 7 0 0.113 -0.331 0.614 224.600 o 5 7 1 60.268 61.510 2.341 9.831 o 5 7 2 54.578 51.814 2.140 11.689 o 5 7 3 0.561 0.620 0.429 417.697 o 5 7 4 1.377 2.174 0.623 191.184 o 5 7 5 100.170 104.728 2.360 7.030 o 5 7 6 34.658 35.657 1.037 32.077 o 5 7 7 21.644 20.201 0.690 63.162 o 5 7 8 1.194 0.449 0.393 453.300 o 5 7 9 82.335 80.259 1.562 11.786 o 5 7 10 31.298 31.784 1.151 31.383 o 5 7 11 7.419 6.777 0.459 178.155 o 5 7 12 0.744 1.414 0.430 388.833 o 5 8 0 91.737 91.342 1.567 10.525 o 5 8 1 11.624 10.473 0.547 116.687 o 5 8 2 41.764 44.359 0.979 28.591 o 5 8 3 3.615 3.848 0.500 222.416 o 5 8 4 0.837 0.957 0.435 386.967 o 5 8 5 0.075 0.145 0.433 447.102 o 5 8 6 0.982 0.785 0.406 431.759 o 5 8 7 1.554 1.710 0.393 403.124 o 5 8 8 5.166 5.251 0.445 219.491 o 5 8 9 109.151 101.820 3.595 4.273 o 5 8 10 5.045 3.911 0.527 190.299 o 5 9 0 151.395 150.937 2.658 4.490 o 5 9 1 7.888 8.167 0.721 104.157 o 5 9 2 199.173 201.160 3.821 2.571 o 5 9 3 121.612 124.070 2.235 6.255 o 5 9 4 5.970 6.724 0.544 162.252 o 5 9 5 1.139 1.410 0.520 271.960 o 5 9 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44.858 o 6 1 7 12.374 13.372 1.134 47.934 o 6 1 8 1.221 0.890 0.553 247.480 o 6 1 9 0.050 0.393 0.760 146.388 o 6 1 10 41.018 42.764 1.586 19.045 o 6 1 11 36.733 36.882 1.099 29.485 o 6 1 12 9.465 8.783 0.673 106.354 o 6 1 13 0.216 -0.307 0.615 222.864 o 6 2 0 84.868 90.316 2.581 7.180 o 6 2 1 30.732 31.069 1.520 23.256 o 6 2 2 4.995 3.873 1.000 73.046 o 6 2 3 8.562 8.027 1.325 41.196 o 6 2 4 0.426 0.344 0.672 183.399 o 6 2 5 0.067 0.820 0.648 198.047 o 6 2 6 14.202 15.035 1.018 53.143 o 6 2 7 0.131 1.200 0.672 182.056 o 6 2 8 4.415 5.101 0.625 152.279 o 6 2 9 18.925 20.664 1.174 39.254 o 6 2 10 149.772 151.114 3.565 3.480 o 6 2 11 25.239 26.033 1.087 37.646 o 6 2 12 184.045 177.963 3.100 3.334 o 6 3 0 8.873 10.537 0.999 62.995 o 6 3 1 52.225 51.873 2.427 10.032 o 6 3 2 4.517 3.603 0.903 88.052 o 6 3 3 0.411 0.659 0.945 93.837 o 6 3 4 145.990 157.810 5.194 2.202 o 6 3 5 2.312 2.348 0.609 187.751 o 6 3 6 45.221 45.512 1.571 18.329 o 6 3 7 0.196 1.811 1.383 44.014 o 6 3 8 34.785 38.669 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5.549 5.991 0.456 204.347 o 6 6 1 1.024 1.514 0.419 391.622 o 6 6 2 10.648 10.725 0.853 75.067 o 6 6 3 20.208 20.029 0.766 60.367 o 6 6 4 28.738 26.395 1.008 38.350 o 6 6 5 71.879 69.830 1.529 13.526 o 6 6 6 137.974 136.354 2.768 4.751 o 6 6 7 104.497 106.063 2.797 5.801 o 6 6 8 2.710 2.580 0.615 180.114 o 6 6 9 0.272 0.034 0.472 371.407 o 6 6 10 9.040 7.131 0.615 122.942 o 6 7 0 0.830 0.723 0.505 301.061 o 6 7 1 5.974 5.429 0.543 167.773 o 6 7 2 1.946 1.802 0.397 378.513 o 6 7 3 36.548 34.483 0.768 38.364 o 6 7 4 1.759 1.966 0.426 345.767 o 6 7 5 9.858 9.417 0.517 134.203 o 6 7 6 9.076 7.584 0.456 160.712 o 6 7 7 0.070 -0.385 0.352 677.970 o 6 7 8 0.043 -0.137 0.288 1018.110 o 6 7 9 8.277 5.902 0.391 197.190 o 6 8 0 15.010 14.583 0.804 69.177 o 6 8 1 0.043 0.636 0.505 323.642 o 6 8 2 7.086 6.365 0.612 135.573 o 6 8 3 0.049 0.397 0.407 498.616 o 6 8 4 6.331 5.284 0.460 197.512 o 6 8 5 7.033 6.892 0.494 169.187 o 6 8 6 6.816 7.538 1.107 57.387 o 6 8 7 17.759 15.168 2.244 14.942 o 6 9 0 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7 2 4 12.821 13.680 0.610 96.576 o 7 2 5 0.056 0.657 0.418 464.936 o 7 2 6 15.558 14.929 0.563 92.199 o 7 2 7 49.585 51.424 1.712 15.723 o 7 2 8 21.352 20.472 0.695 63.111 o 7 2 9 0.832 0.477 0.305 721.324 o 7 3 0 12.415 11.733 0.562 108.360 o 7 3 1 2.022 1.723 0.391 385.066 o 7 3 2 8.915 9.278 0.470 151.793 o 7 3 3 5.631 5.308 0.429 220.324 o 7 3 4 55.069 53.979 0.984 22.692 o 7 3 5 3.747 3.751 0.435 262.187 o 7 3 6 16.980 15.862 0.542 89.045 o 7 3 7 1.055 0.991 0.320 614.138 o 7 3 8 5.356 5.082 0.351 269.447 o 7 3 9 20.103 15.774 1.598 25.767 o 7 4 0 11.059 10.809 0.644 102.068 o 7 4 1 11.936 12.095 0.648 96.558 o 7 4 2 56.049 59.573 2.217 10.838 o 7 4 3 31.990 33.212 1.022 34.299 o 7 4 4 4.867 5.030 0.558 173.557 o 7 4 5 37.513 36.751 0.983 31.851 o 7 4 6 16.560 17.136 0.668 76.381 o 7 4 7 1.365 1.390 0.443 348.537 o 7 4 8 0.294 0.428 0.351 630.313 o 7 5 0 4.269 4.202 0.575 175.983 o 7 5 1 71.093 72.741 1.589 13.064 o 7 5 2 51.868 56.338 1.525 16.971 o 7 5 3 4.863 4.289 0.735 120.002 o 7 5 4 146.832 158.169 3.004 4.085 o 7 5 5 120.215 118.197 3.483 4.168 o 7 5 6 71.030 75.560 1.978 10.686 o 7 5 7 25.700 24.416 1.353 29.394 o 7 6 0 13.929 13.888 1.204 42.769 o 7 6 1 51.665 50.950 1.752 15.118 o 7 6 2 18.880 19.686 0.840 57.472 o 7 6 3 64.728 67.158 2.168 10.346 o 7 6 4 39.757 41.157 0.944 30.747 o 7 6 5 57.279 53.540 1.682 14.943 o 7 6 6 83.174 74.320 1.717 11.181 o 7 7 0 0.089 0.754 0.449 402.217 o 7 7 1 12.608 14.364 0.650 91.041 o 7 7 2 13.023 13.011 0.730 82.081 o 7 7 3 28.618 29.915 0.840 43.285 o 7 7 4 0.052 0.172 0.306 880.004 o 7 7 5 6.090 4.672 0.553 166.367 o 7 8 0 43.174 44.092 1.282 22.938 o 7 8 1 0.308 0.184 0.861 113.785 o 7 8 2 6.209 5.061 0.411 222.211 o 8 0 0 0.205 0.861 0.696 171.155 o 8 0 2 23.760 23.669 1.130 37.504 o 8 0 4 57.241 57.792 1.652 14.961 o 8 0 6 0.476 0.369 0.492 331.578 o 8 1 0 0.106 0.563 0.468 373.813 o 8 1 1 7.144 7.756 0.552 147.398 o 8 1 2 7.158 8.142 0.487 165.105 o 8 1 3 0.038 0.099 0.339 731.358 o 8 1 4 0.745 0.803 0.360 543.793 o 8 1 5 0.155 -0.127 0.312 846.234 o 8 1 6 0.156 -0.338 0.348 685.061 o 8 2 0 5.210 5.218 0.487 199.114 o 8 2 1 1.021 1.076 0.430 384.320 o 8 2 2 9.381 9.153 0.575 124.995 o 8 2 3 0.237 0.261 0.360 616.195 o 8 2 4 0.190 -0.145 0.283 1008.410 o 8 2 5 11.560 9.723 0.449 137.350 o 8 3 0 0.000 0.445 0.420 468.996 o 8 3 1 0.093 0.331 0.396 523.884 o 8 3 2 21.034 20.708 1.189 37.481 o 8 3 3 2.140 2.971 0.476 272.198 o 8 3 4 0.226 -0.307 0.615 222.718 o 8 3 5 1.954 1.045 0.492 283.755 o 8 4 0 2.922 2.951 0.799 114.661 o 8 4 1 9.562 9.283 0.922 70.559 o 8 4 2 1.374 1.235 0.472 315.775 o 8 4 3 8.653 7.090 0.799 90.401 o 8 4 4 44.484 38.239 1.475 20.370 o 8 5 0 5.889 6.861 0.586 148.984 o 8 5 1 12.105 12.144 0.673 92.598 o 8 5 2 4.220 4.019 0.428 255.103 o 8 6 0 0.047 0.369 0.430 447.746 o ; _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.115 _oxdiff_exptl_absorpt_empirical_full_min 0.870 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x,y+1/2,-z+1/2 3 -x,-y,-z 4 x,-y-1/2,z-1/2 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_refinement_flags_posn O1 O 0.46757(19) 0.57169(13) 0.73605(7) 0.0498(4) Uani 1.000000 . O2 O 0.2518(2) 0.09183(12) 0.47094(9) 0.0617(5) Uani 1.000000 . C1 C 0.31963(9) 0.44395(6) 0.63164(4) 0.03132(14) Uani 1.000000 . C2 C 0.29987(9) 0.52925(6) 0.57036(4) 0.03107(14) Uani 1.000000 . C3 C 0.33103(10) 0.65734(7) 0.58274(5) 0.03842(16) Uani 1.000000 . H3 H 0.3707(17) 0.6883(9) 0.6422(6) 0.070(3) Uani 1.000000 . C4 C 0.31642(11) 0.73644(7) 0.52291(5) 0.04244(17) Uani 1.000000 . H4 H 0.3443(18) 0.8352(9) 0.5336(7) 0.084(4) Uani 1.000000 . C5 C 0.26705(10) 0.69585(7) 0.44472(4) 0.03886(16) Uani 1.000000 . C6 C 0.25903(11) 0.77616(9) 0.38289(5) 0.0491(2) Uani 1.000000 . H6 H 0.2893(18) 0.8731(11) 0.3955(8) 0.088(4) Uani 1.000000 . C7 C 0.21221(12) 0.73466(9) 0.30716(5) 0.0532(2) Uani 1.000000 . H7 H 0.2094(17) 0.7965(11) 0.2595(6) 0.090(4) Uani 1.000000 . C8 C 0.17167(11) 0.61230(10) 0.29212(5) 0.0499(2) Uani 1.000000 . H8 H 0.1334(17) 0.5795(12) 0.2320(6) 0.085(4) Uani 1.000000 . C9 C 0.17909(10) 0.52924(8) 0.35258(4) 0.03978(17) Uani 1.000000 . C10 C 0.14071(11) 0.40312(8) 0.33838(4) 0.04441(18) Uani 1.000000 . H10 H 0.1008(18) 0.3727(11) 0.2785(6) 0.081(3) Uani 1.000000 . C11 C 0.15532(10) 0.32214(8) 0.39700(4) 0.04110(17) Uani 1.000000 . H11 H 0.1269(16) 0.2259(9) 0.3846(6) 0.067(3) Uani 1.000000 . C12 C 0.21263(9) 0.35956(6) 0.47621(4) 0.03237(14) Uani 1.000000 . C13 C 0.23580(9) 0.27688(6) 0.53853(4) 0.03347(14) Uani 1.000000 . C14 C 0.28426(9) 0.32138(7) 0.61387(4) 0.03365(15) Uani 1.000000 . H14 H 0.3025(15) 0.2578(9) 0.6614(5) 0.064(3) Uani 1.000000 . C15 C 0.24523(8) 0.48613(6) 0.49273(4) 0.03069(14) Uani 1.000000 . C16 C 0.22862(9) 0.57047(7) 0.43017(4) 0.03418(15) Uani 1.000000 . C17 C 0.38565(10) 0.47680(8) 0.71490(4) 0.03595(16) Uani 1.000000 . C18 C 0.35051(14) 0.38854(9) 0.77491(5) 0.04781(19) Uani 1.000000 . H18a H 0.440(2) 0.3079(12) 0.7766(8) 0.099(5) Uani 1.000000 . H18b H 0.385(2) 0.4294(12) 0.8311(6) 0.093(4) Uani 1.000000 . H18c H 0.2076(19) 0.3556(13) 0.7640(7) 0.093(4) Uani 1.000000 . C19 C 0.22400(11) 0.14156(7) 0.52843(5) 0.04053(17) Uani 1.000000 . C20 C 0.17979(14) 0.06570(8) 0.59286(5) 0.04780(19) Uani 1.000000 . H20a H 0.147(2) -0.0269(10) 0.5714(8) 0.097(4) Uani 1.000000 . H20b H 0.3032(19) 0.0607(12) 0.6417(8) 0.098(4) Uani 1.000000 . H20c H 0.069(2) 0.1042(11) 0.6150(9) 0.102(5) Uani 1.000000 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O1 0.0649(10) 0.0487(10) 0.0336(8) -0.0078(8) 0.0062(7) -0.0102(7) O2 0.0933(13) 0.0398(9) 0.0592(10) -0.0060(8) 0.0324(9) -0.0176(8) C1 0.0314(3) 0.0342(3) 0.0288(3) 0.0007(2) 0.0076(2) -0.0045(3) C2 0.0288(3) 0.0337(3) 0.0310(3) 0.0005(2) 0.0074(2) -0.0045(2) C3 0.0419(3) 0.0347(4) 0.0392(4) -0.0019(3) 0.0101(3) -0.0056(3) H3 0.106(9) 0.059(6) 0.044(6) -0.014(6) 0.017(6) -0.012(5) C4 0.0438(4) 0.0353(4) 0.0493(4) -0.0001(3) 0.0125(3) 0.0003(3) H4 0.104(9) 0.040(6) 0.103(9) -0.008(6) 0.014(7) 0.000(6) C5 0.0322(3) 0.0413(4) 0.0440(4) 0.0041(3) 0.0104(3) 0.0061(3) C6 0.0412(4) 0.0515(5) 0.0558(5) 0.0064(3) 0.0135(3) 0.0181(4) H6 0.087(9) 0.060(8) 0.119(11) -0.003(6) 0.025(8) 0.015(7) C7 0.0422(4) 0.0684(6) 0.0500(5) 0.0111(4) 0.0127(3) 0.0229(4) H7 0.097(9) 0.099(9) 0.075(8) 0.015(7) 0.019(6) 0.066(7) C8 0.0393(4) 0.0744(6) 0.0360(4) 0.0093(4) 0.0085(3) 0.0127(4) H8 0.083(8) 0.136(11) 0.035(6) 0.000(7) 0.010(5) 0.003(7) C9 0.0313(3) 0.0565(5) 0.0312(3) 0.0054(3) 0.0062(2) 0.0036(3) C10 0.0410(4) 0.0620(5) 0.0287(3) 0.0002(3) 0.0046(3) -0.0060(3) H10 0.095(9) 0.104(9) 0.038(6) -0.008(7) 0.000(5) -0.019(6) C11 0.0410(4) 0.0489(4) 0.0324(3) -0.0022(3) 0.0059(3) -0.0101(3) H11 0.091(8) 0.052(6) 0.059(6) -0.011(5) 0.017(6) -0.023(5) C12 0.0299(3) 0.0375(3) 0.0298(3) -0.0002(2) 0.0069(2) -0.0063(3) C13 0.0341(3) 0.0339(3) 0.0327(3) -0.0001(3) 0.0080(2) -0.0062(3) C14 0.0353(3) 0.0347(3) 0.0313(3) 0.0005(3) 0.0082(2) -0.0029(3) H14 0.087(8) 0.057(6) 0.047(6) 0.000(5) 0.010(5) 0.017(5) C15 0.0267(3) 0.0363(3) 0.0293(3) 0.0014(2) 0.0069(2) -0.0027(3) C16 0.0271(3) 0.0428(4) 0.0330(3) 0.0045(2) 0.0073(2) 0.0027(3) C17 0.0367(3) 0.0410(4) 0.0304(3) 0.0012(3) 0.0078(3) -0.0065(3) C18 0.0539(5) 0.0579(5) 0.0312(4) -0.0033(4) 0.0086(3) 0.0005(3) H18a 0.120(11) 0.091(10) 0.090(10) 0.055(9) 0.029(8) 0.033(8) H18b 0.137(12) 0.103(10) 0.040(7) -0.030(9) 0.023(7) -0.017(7) H18c 0.081(9) 0.123(11) 0.075(9) -0.042(8) 0.020(7) 0.019(8) C19 0.0430(4) 0.0354(4) 0.0435(4) -0.0017(3) 0.0104(3) -0.0083(4) C20 0.0550(5) 0.0360(4) 0.0517(5) 0.0005(3) 0.0105(4) -0.0004(3) H20a 0.147(13) 0.043(7) 0.101(10) -0.017(7) 0.026(9) -0.014(7) H20b 0.091(9) 0.096(10) 0.085(9) 0.000(8) -0.027(8) 0.027(8) H20c 0.123(12) 0.074(9) 0.131(13) 0.030(8) 0.076(10) 0.025(8) loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source _atom_type_scat_dispersion_source C 0.01788 0.00908 'NoSpherA2: Chem.Sci. 2021, DOI:10.1039/D0SC05526C' 'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850' H 0.00000 0.00000 'NoSpherA2: Chem.Sci. 2021, DOI:10.1039/D0SC05526C' 'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850' O 0.04960 0.03234 'NoSpherA2: Chem.Sci. 2021, DOI:10.1039/D0SC05526C' 'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850' loop_ _diffrn_refln_index_h _diffrn_refln_index_k _diffrn_refln_index_l _diffrn_refln_intensity_net _diffrn_refln_intensity_u 0 0 2 843.39 22.58 0 0 3 -0.12 0.17 0 0 4 158.24 4.66 0 0 5 0.02 0.11 0 0 5 0.33 0.25 0 0 6 162.68 4.2 0 0 6 116.12 3.56 0 0 7 -0.06 0.27 0 0 8 91.6 3.36 0 0 9 0.17 0.28 0 0 10 1.77 0.46 0 0 11 0.06 0.16 0 0 12 36.86 2.22 0 0 12 36.05 1.41 0 0 13 0.15 0.17 0 0 13 0.23 0.21 0 0 14 1.41 0.29 0 0 15 0.4 0.25 0 0 16 40.11 1.64 0 0 17 -0.04 0.24 0 0 18 0.4 0.24 0 0 19 0.12 0.17 0 0 20 13.39 0.53 0 0 21 0.01 0.13 0 0 22 7.97 0.28 0 1 1 1272.73 33.95 0 -1 2 304.92 8.32 0 1 2 305.3 8.31 0 1 3 494.71 13.3 0 -1 3 482.38 13.29 0 1 4 2.09 0.32 0 -1 4 1.87 0.3 0 1 5 12.48 0.66 0 -1 5 12.86 0.77 0 1 5 13.02 0.76 0 1 6 21.25 0.96 0 -1 6 22.17 1.13 0 1 6 21.29 1.12 0 1 7 11.23 0.68 0 -1 7 12.83 0.9 0 1 8 0.65 0.36 0 -1 8 0.79 0.33 0 1 9 2.53 0.5 0 -1 9 3.98 0.61 0 1 10 5.21 0.73 0 -1 10 5.23 0.7 0 1 11 14.28 0.73 0 -1 11 15.04 0.74 0 -1 11 14.12 1.25 0 1 11 14.73 0.7 0 1 11 14.28 1.24 0 1 12 0.33 0.19 0 1 12 0.03 0.18 0 -1 12 0.65 0.44 0 1 12 0.13 0.34 0 -1 12 0.24 0.2 0 -1 13 105.57 3.31 0 1 13 104.47 3.29 0 1 13 101.65 3.21 0 -1 14 210.66 6.11 0 1 14 202.51 6 0 1 14 210.51 6.11 0 1 15 58.21 2.1 0 1 15 54.06 1.98 0 -1 15 59.51 2.12 0 -1 16 0.8 0.29 0 1 16 0.67 0.26 0 1 17 3.67 0.44 0 -1 17 3.29 0.42 0 -1 18 2.74 0.29 0 1 18 2.95 0.29 0 1 19 1.94 0.24 0 -1 19 2.34 0.24 0 1 19 2.02 0.23 0 -1 19 2.06 0.24 0 1 20 0.23 0.16 0 -1 20 0.07 0.15 0 -1 20 -0.15 0.15 0 1 20 -0.02 0.13 0 -1 21 3.59 0.22 0 1 21 3.64 0.21 0 -1 21 3.38 0.21 0 1 21 3.3 0.21 0 -1 22 0.4 0.07 0 2 0 72.01 2.29 0 2 0 74.05 2.26 0 2 -1 19.42 0.81 0 2 -1 16.69 0.7 0 -2 2 251.92 7.02 0 2 2 261.3 7.03 0 -2 3 186.57 5.25 0 2 3 183.17 5.24 0 2 4 33.7 1.29 0 -2 4 33.18 1.3 0 -2 5 8.02 0.59 0 2 5 8.41 0.6 0 -2 6 7.06 0.62 0 2 6 6.15 0.58 0 2 6 7.66 0.6 0 2 7 67.38 2.52 0 2 7 62.51 2.37 0 -2 7 65.87 2.51 0 2 8 14.8 1.05 0 2 8 14.14 0.92 0 2 9 -0.09 0.28 0 -2 9 0.26 0.32 0 2 10 19.63 1.38 0 -2 10 20.4 1.42 0 2 11 16.65 1.35 0 -2 11 17.17 0.82 0 2 11 17.48 0.79 0 -2 11 14.15 1.3 0 2 11 17.08 0.8 0 -2 12 83.17 3.77 0 -2 12 84.79 2.79 0 2 12 87.34 2.8 0 2 12 89.46 3.85 0 2 12 88.39 2.76 0 -2 13 201.81 5.82 0 2 13 198.88 5.8 0 2 13 193.29 5.74 0 -2 14 165.69 5.04 0 2 14 166.32 4.98 0 2 14 170.07 5.05 0 2 15 7.41 0.55 0 -2 15 8.25 0.62 0 2 15 8.49 0.62 0 2 16 0.13 0.19 0 2 16 0.04 0.21 0 -2 16 -0.3 0.25 0 -2 17 0.02 0.18 0 -2 17 0.21 0.22 0 2 17 0.04 0.19 0 2 17 -0.08 0.17 0 2 17 -0.07 0.21 0 -2 17 -0.02 0.21 0 -2 18 0.29 0.2 0 2 18 0.05 0.17 0 2 19 1.45 0.2 0 2 19 1.04 0.18 0 -2 19 1.12 0.2 0 -2 19 1.53 0.2 0 2 -19 1.35 0.2 0 -2 19 1.49 0.2 0 2 -20 0.98 0.16 0 -2 20 1.14 0.17 0 -2 20 0.7 0.15 0 -2 20 1.04 0.17 0 2 20 0.99 0.17 0 -2 20 0.98 0.14 0 2 20 1.02 0.16 0 -2 21 0.49 0.12 0 2 21 0.33 0.11 0 -2 21 0.36 0.11 0 2 21 0.38 0.1 0 3 0 0.12 0.24 0 3 -1 35.92 1.46 0 3 -2 21.99 1.07 0 -3 3 -0.02 0.14 0 3 -3 0.09 0.22 0 3 3 -0.05 0.13 0 -3 4 20.96 0.95 0 3 4 21.74 0.95 0 3 5 223.07 6.51 0 -3 5 223.89 6.52 0 3 6 332.07 9.79 0 3 6 350.56 9.98 0 -3 6 345.99 9.82 0 -3 7 33.74 1.61 0 3 7 34.97 1.67 0 3 7 34.66 1.62 0 3 8 46.03 2.05 0 3 8 45.12 2.04 0 -3 8 44.22 2.04 0 -3 9 6.73 0.76 0 3 9 6.74 0.76 0 -3 10 24.45 1.62 0 3 10 23.59 0.99 0 3 10 26.86 1.64 0 3 10 27.06 1.05 0 3 11 49.71 1.72 0 -3 11 44.74 2.45 0 3 -11 49 1.71 0 3 11 45.67 1.67 0 -3 11 49.14 1.7 0 3 11 48.55 2.5 0 3 -12 0.91 0.26 0 3 12 1.28 0.26 0 -3 12 0.96 0.23 0 3 12 0.75 0.22 0 3 12 0.39 0.39 0 3 13 61.77 2.12 0 -3 13 63.53 2.14 0 3 -13 61.23 2.13 0 3 13 57.43 2.1 0 3 14 14.49 0.81 0 -3 14 14.85 0.83 0 3 14 13.71 0.78 0 3 -14 14 0.8 0 3 15 10.67 0.67 0 -3 15 10.21 0.69 0 3 15 9.31 0.65 0 3 16 58.34 2.07 0 3 16 54.23 2 0 -3 16 57.93 2.07 0 3 17 1.42 0.27 0 -3 17 1.16 0.22 0 -3 17 2.02 0.28 0 3 17 1.74 0.23 0 -3 18 5.53 0.37 0 3 18 4.99 0.32 0 3 18 5.26 0.34 0 -3 18 4.97 0.33 0 -3 18 5.81 0.34 0 3 19 1.8 0.2 0 -3 19 1.9 0.2 0 -3 19 2 0.21 0 -3 19 2.02 0.24 0 3 -19 2.15 0.23 0 3 19 2.01 0.21 0 -3 20 0.91 0.14 0 3 20 0.93 0.14 0 -3 20 0.62 0.12 0 3 -20 0.94 0.16 0 -3 20 0.69 0.14 0 -3 20 0.77 0.17 0 3 20 0.46 0.11 0 -3 21 -0.05 0.09 0 3 -21 -0.02 0.09 0 -3 21 0.12 0.08 0 3 -21 0.14 0.09 0 3 21 0 0.07 0 -3 21 0.11 0.08 0 4 0 3.85 0.5 0 4 -1 2.68 0.42 0 4 -2 27.73 1.4 0 4 -3 77.19 2.85 0 4 -4 43.79 1.95 0 4 -5 31.34 1.62 0 4 6 46.13 2.11 0 4 7 5.38 0.65 0 4 8 -0.09 0.26 0 4 -9 11.96 0.65 0 4 9 11.72 1.05 0 4 -10 0.26 0.2 0 4 11 51.86 1.84 0 4 -11 52.09 1.86 0 4 -12 0.12 0.23 0 4 12 0.11 0.18 0 4 13 2.71 0.36 0 4 -13 1.93 0.34 0 4 14 8.35 0.61 0 4 -14 8.64 0.63 0 4 -15 35.73 1.48 0 4 15 36.37 1.47 0 4 16 35.14 1.4 0 -4 16 33.69 1.19 0 4 17 5.22 0.44 0 -4 17 5.08 0.35 0 -4 17 4.25 0.37 0 -4 18 -0.16 0.2 0 -4 18 -0.06 0.17 0 4 -19 0.02 0.16 0 -4 19 0.08 0.12 0 -4 19 0.13 0.16 0 -4 19 0.04 0.13 0 -4 20 6.7 0.32 0 4 -20 6.79 0.31 0 -4 20 6.2 0.28 0 4 -21 2.63 0.14 0 4 -21 2.61 0.15 0 5 0 0.15 0.27 0 5 -1 680.73 19.16 0 5 -2 381.04 11.21 0 5 -3 177.93 5.83 0 5 -4 0.34 0.3 0 5 5 5.9 0.73 0 5 -5 4.26 0.66 0 5 -6 47 2.36 0 5 6 49.98 2.37 0 5 -7 1.49 0.25 0 5 7 1.45 0.46 0 5 -7 0.66 0.38 0 5 7 1.46 0.23 0 5 8 20.77 1.51 0 5 8 21.76 0.93 0 5 9 8.12 0.53 0 5 9 6.19 0.87 0 5 10 3.13 0.35 0 5 -10 3.08 0.38 0 5 -11 0.36 0.24 0 5 -12 3.54 0.43 0 5 13 9.34 0.64 0 5 -13 8.73 0.63 0 5 -14 2.28 0.4 0 5 14 4.1 0.44 0 5 -15 1.02 0.29 0 5 15 0.95 0.27 0 5 16 4.9 0.43 0 -5 16 4.76 0.35 0 5 -16 4.28 0.45 0 5 -16 5.16 0.37 0 5 -17 2.47 0.27 0 -5 17 3.06 0.27 0 -5 17 2.24 0.28 0 5 -18 7.05 0.38 0 -5 18 7.36 0.38 0 -5 18 7.08 0.4 0 -5 19 1.69 0.18 0 5 -19 1.74 0.19 0 -5 19 1.67 0.2 0 -5 20 5.59 0.25 0 5 -20 5.2 0.24 0 6 0 96.89 3.65 0 6 1 7.48 0.83 0 6 -1 7.87 0.8 0 6 -1 6.78 0.79 0 6 2 75.68 3.19 0 6 -2 81.83 3.33 0 6 3 72.23 3.01 0 6 -3 62.17 2.93 0 6 4 33.91 1.96 0 6 -4 36.06 2.01 0 6 5 13.92 0.69 0 6 -5 12.93 1.19 0 6 5 13.72 0.66 0 6 -6 3.86 0.36 0 6 6 4 0.36 0 6 6 3.4 0.34 0 6 -6 2.8 0.6 0 6 7 94.8 2.97 0 6 -7 97.19 3.01 0 6 -7 87.8 4.04 0 6 7 99.37 3 0 6 7 96.53 4.07 0 6 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0.16 -8 3 4 0.75 0.16 -8 3 4 0.54 0.16 -8 -3 3 2.71 0.23 -8 3 3 2.88 0.22 -8 -3 3 2.5 0.23 -8 3 3 2.63 0.22 -8 -3 2 17.97 0.65 -8 3 2 17.53 0.62 -8 -3 2 17.65 0.64 -8 3 2 16.48 0.61 -8 3 1 1.72 0.19 -8 -3 1 1.79 0.19 -8 -3 1 1.94 0.21 -8 -3 1 2.03 0.21 -8 3 0 0.15 0.13 -8 -3 0 0.15 0.13 -8 -3 0 0.01 0.14 -8 -3 0 -0.04 0.15 -8 3 -1 0.13 0.12 -8 -3 -1 0.01 0.12 -8 -3 -1 0.18 0.14 -8 -3 -1 -0.11 0.14 -8 3 -2 2.97 0.19 -8 -3 -2 3.13 0.2 -8 -3 -2 3.8 0.23 -8 -3 -2 3.64 0.22 -8 3 -3 0.66 0.11 -8 -3 -3 0.33 0.11 -8 -3 -3 0.38 0.12 -8 -3 -3 0.38 0.12 -8 -3 -4 -0.05 0.1 -8 3 -5 0.17 0.08 -8 -4 13 1.17 0.1 -8 4 12 0.42 0.09 -8 4 11 5.81 0.26 -8 4 10 0.64 0.12 -8 4 9 0.06 0.11 -8 4 8 0.44 0.13 -8 4 8 0.39 0.13 -8 4 7 0.09 0.12 -8 4 7 0.11 0.13 -8 4 6 0.73 0.14 -8 4 6 0.74 0.15 -8 4 5 1.76 0.18 -8 4 5 1.78 0.18 -8 4 4 0.11 0.13 -8 4 4 0.15 0.12 -8 4 3 5.2 0.29 -8 4 2 0.79 0.14 -8 -4 2 0.71 0.16 -8 4 1 0.34 0.12 -8 4 0 0.48 0.13 -8 4 -1 1.51 0.15 -8 4 -2 0.16 0.1 -8 -4 -2 0.25 0.12 -8 4 -3 1.04 0.11 -8 -4 -3 1.3 0.14 -8 -4 -4 6.22 0.24 -8 5 11 -0.04 0.08 -8 5 10 0.04 0.09 -8 5 9 0.34 0.11 -8 5 8 0.14 0.11 -8 5 7 4.62 0.25 -8 5 6 1.31 0.15 -8 5 5 2.94 0.21 -8 5 4 9.43 0.38 -8 5 3 0.19 0.12 -8 5 2 0.15 0.11 -8 5 1 5.94 0.27 -8 -5 1 5.6 0.28 -8 5 0 1.02 0.13 -8 -5 0 1.21 0.14 -8 5 -1 1.98 0.15 -8 -5 -1 1.97 0.16 -8 5 -2 0.61 0.09 -8 -5 -2 0.71 0.11 -8 6 9 11.79 0.39 -8 6 8 5.33 0.23 -8 6 7 3.4 0.18 -8 6 7 2.68 0.15 -8 6 6 1.52 0.14 -8 6 6 1.39 0.11 -8 6 5 9.17 0.33 -8 6 5 7.27 0.29 -8 6 4 0.55 0.11 -8 6 4 0.44 0.09 -8 6 3 1.32 0.13 -8 6 3 0.99 0.1 -8 6 2 0.08 0.08 -8 6 1 0.63 0.1 -8 6 0 0.06 0.07 -9 0 9 -0.01 0.06 -9 0 8 0.02 0.08 -9 0 8 0.14 0.07 -9 0 7 -0.01 0.08 -9 0 7 -0.01 0.08 -9 0 6 8.19 0.31 -9 0 6 7.73 0.31 -9 0 5 -0.01 0.09 -9 0 4 0.06 0.09 -9 0 3 -0.01 0.08 -9 0 3 -0.05 0.08 -9 0 2 0.05 0.07 -9 0 2 0.11 0.07 -9 0 1 0.01 0.06 -9 -1 8 3.04 0.16 -9 1 8 3.32 0.16 -9 1 8 3.42 0.17 -9 -1 7 0.22 0.08 -9 1 7 0.15 0.08 -9 -1 7 0.23 0.08 -9 -1 6 0.9 0.11 -9 1 6 0.75 0.1 -9 -1 6 0.84 0.11 -9 -1 5 1.98 0.14 -9 1 5 1.69 0.14 -9 1 5 2.17 0.14 -9 -1 5 1.99 0.14 -9 -1 4 2.71 0.16 -9 1 4 2.57 0.16 -9 1 4 2.55 0.15 -9 -1 4 2.98 0.16 -9 -1 3 0.05 0.08 -9 1 3 0.23 0.08 -9 1 3 0.17 0.08 -9 -1 2 0.39 0.08 -9 1 2 0.36 0.08 -9 2 6 6.78 0.25 -9 -2 5 0.46 0.08 -9 -2 4 6.11 0.24 -9 -2 3 1.06 0.1 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 5 0 -1 0.0615 1 -6 -7 0.0631 -5 0 1 0.0532 -3 5 6 0.0610 1 5 -7 0.0418 -2 -3 10 0.0486 1 -7 1 0.0784 3 1 5 0.0843 -4 0 -5 0.0655 -3 -4 -3 0.0684 4 3 -5 0.0524 -3 -5 6 0.0506 1 -1 11 0.0735 0 -6 6 0.0694 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 C14 C1 C2 118.86(6) . . ? C17 C1 C2 123.72(6) . . ? C17 C1 C14 117.35(6) . . ? C3 C2 C1 123.03(6) . . ? C15 C2 C1 118.70(6) . . ? C15 C2 C3 118.27(6) . . ? H3 C3 C2 117.1(6) . . ? C4 C3 C2 121.72(7) . . ? C4 C3 H3 121.2(5) . . ? H4 C4 C3 120.7(7) . . ? C5 C4 C3 121.37(7) . . ? C5 C4 H4 117.9(7) . . ? C6 C5 C4 121.63(8) . . ? C16 C5 C4 118.52(7) . . ? C16 C5 C6 119.84(8) . . ? H6 C6 C5 118.6(7) . . ? C7 C6 C5 120.75(9) . . ? C7 C6 H6 120.6(7) . . ? H7 C7 C6 120.6(7) . . ? C8 C7 C6 119.95(8) . . ? C8 C7 H7 119.4(7) . . ? H8 C8 C7 119.9(7) . . ? C9 C8 C7 120.84(8) . . ? C9 C8 H8 119.2(7) . . ? C10 C9 C8 121.69(8) . . ? C16 C9 C8 119.66(8) . . ? C16 C9 C10 118.65(7) . . ? H10 C10 C9 118.0(7) . . ? C11 C10 C9 121.59(7) . . ? C11 C10 H10 120.4(7) . . ? H11 C11 C10 120.2(6) . . ? C12 C11 C10 121.39(8) . . ? C12 C11 H11 118.4(6) . . ? C13 C12 C11 122.78(7) . . ? C15 C12 C11 118.55(7) . . ? C15 C12 C13 118.66(6) . . ? C14 C13 C12 119.13(6) . . ? C19 C13 C12 123.45(6) . . ? C19 C13 C14 117.29(7) . . ? C13 C14 C1 123.39(7) . . ? H14 C14 C1 117.6(5) . . ? H14 C14 C13 118.9(5) . . ? C12 C15 C2 121.21(6) . . ? C16 C15 C2 119.48(6) . . ? C16 C15 C12 119.28(6) . . ? C9 C16 C5 118.94(7) . . ? C15 C16 C5 120.59(6) . . ? C15 C16 C9 120.44(7) . . ? C1 C17 O1 122.58(9) . . ? C18 C17 O1 118.75(9) . . ? C18 C17 C1 118.66(7) . . ? H18a C18 C17 110.5(7) . . ? H18b C18 C17 110.5(7) . . ? H18b C18 H18a 107.6(11) . . ? H18c C18 C17 113.5(7) . . ? H18c C18 H18a 105.6(11) . . ? H18c C18 H18b 108.8(10) . . ? C13 C19 O2 122.14(10) . . ? C20 C19 O2 119.52(10) . . ? C20 C19 C13 118.33(7) . . ? H20a C20 C19 108.5(7) . . ? H20b C20 C19 111.0(7) . . ? H20b C20 H20a 107.7(10) . . ? H20c C20 C19 111.6(7) . . ? H20c C20 H20a 112.3(11) . . ? H20c C20 H20b 105.8(12) . . ? 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 O1 C17 1.2158(15) . ? O2 C19 1.2143(15) . ? C1 C2 1.4199(9) . ? C1 C14 1.3945(10) . ? C1 C17 1.4935(10) . ? C2 C3 1.4353(10) . ? C2 C15 1.4281(9) . ? C3 H3 1.086(9) . ? C3 C4 1.3594(11) . ? C4 H4 1.113(10) . ? C4 C5 1.4266(11) . ? C5 C6 1.4006(11) . ? C5 C16 1.4183(11) . ? C6 H6 1.101(12) . ? C6 C7 1.3891(14) . ? C7 H7 1.082(9) . ? C7 C8 1.3898(15) . ? C8 H8 1.103(10) . ? C8 C9 1.4020(11) . ? C9 C10 1.4253(12) . ? C9 C16 1.4190(10) . ? C10 H10 1.091(10) . ? C10 C11 1.3565(12) . ? C11 H11 1.091(10) . ? C11 C12 1.4356(9) . ? C12 C13 1.4134(10) . ? C12 C15 1.4307(10) . ? C13 C14 1.3944(9) . ? C13 C19 1.4987(10) . ? C14 H14 1.081(9) . ? C15 C16 1.4321(9) . ? C17 C18 1.5044(11) . ? C18 H18a 1.093(12) . ? C18 H18b 1.072(11) . ? C18 H18c 1.066(12) . ? C19 C20 1.5068(12) . ? C20 H20a 1.095(11) . ? C20 H20b 1.096(12) . ? C20 H20c 1.056(12) . ? 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 O1 C17 C1 C2 -17.03(11) . . . . ? O1 C17 C1 C14 159.98(10) . . . . ? O2 C19 C13 C12 23.05(12) . . . . ? O2 C19 C13 C14 -152.76(11) . . . . ? C1 C2 C3 C4 178.06(7) . . . . ? C1 C2 C15 C12 -0.67(7) . . . . ? C1 C2 C15 C16 -178.65(5) . . . . ? C1 C14 C13 C12 -2.85(8) . . . . ? C1 C14 C13 C19 173.14(7) . . . . ? C2 C3 C4 C5 0.75(8) . . . . ? C2 C15 C12 C11 179.11(6) . . . . ? C2 C15 C12 C13 -0.09(7) . . . . ? C2 C15 C16 C5 0.39(7) . . . . ? C2 C15 C16 C9 178.45(6) . . . . ? C3 C4 C5 C6 -177.47(7) . . . . ? C3 C4 C5 C16 1.46(9) . . . . ? C4 C5 C6 C7 179.46(7) . . . . ? C4 C5 C16 C9 179.90(6) . . . . ? C4 C5 C16 C15 -2.01(7) . . . . ? C5 C6 C7 C8 0.35(9) . . . . ? C5 C16 C9 C8 0.88(7) . . . . ? C5 C16 C9 C10 179.98(6) . . . . ? C5 C16 C15 C12 -177.62(6) . . . . ? C6 C7 C8 C9 -0.62(9) . . . . ? C7 C8 C9 C10 -179.08(7) . . . . ? C7 C8 C9 C16 -0.01(9) . . . . ? C8 C9 C10 C11 177.35(7) . . . . ? C8 C9 C16 C15 -177.20(6) . . . . ? C9 C10 C11 C12 -0.82(9) . . . . ? C9 C16 C15 C12 0.43(7) . . . . ? C10 C11 C12 C13 -177.68(7) . . . . ? C10 C11 C12 C15 3.15(8) . . . . ? C11 C12 C13 C14 -177.39(6) . . . . ? C11 C12 C13 C19 6.89(8) . . . . ? C11 C12 C15 C16 -2.90(7) . . . . ? C12 C13 C19 C20 -158.16(7) . . . . ? loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 5.0033 -0.0030 -0.9327 0.3500 -0.8971 -0.4973 1.0085 -6.0057 -6.9867 -0.1624 0.3224 -0.9745 -5.0033 0.0030 0.9327 -0.3500 0.8971 0.4973 -3.0084 5.0056 5.9590 -0.0024 0.1359 1.0166 0.9999 4.9869 -7.0205 0.9128 0.1424 0.1132 -2.0034 -2.9839 10.0086 -0.9331 -0.1619 0.3000 1.0056 -6.9942 1.0383 -0.6768 -0.1361 -0.7419 2.9986 1.0051 5.0526 0.0161 -0.8870 0.0325 -4.0000 -0.0054 -5.0697 0.0220 1.0620 0.1575 -2.9972 -4.0003 -3.0379 -0.4135 0.8174 -0.2463 4.0023 2.9900 -4.9669 0.7919 -0.5175 -0.2752 -3.0006 -4.9876 5.9898 -0.9799 0.2996 0.0277 0.9963 -0.9849 11.0472 -0.6110 -0.8279 0.2657 0.0019 -5.9879 6.0349 -0.8989 -0.2579 -0.3447 loop_ _atom_site_anharm_gc_c_label _atom_site_anharm_gc_c_111 _atom_site_anharm_gc_c_112 _atom_site_anharm_gc_c_113 _atom_site_anharm_gc_c_122 _atom_site_anharm_gc_c_123 _atom_site_anharm_gc_c_133 _atom_site_anharm_gc_c_222 _atom_site_anharm_gc_c_223 _atom_site_anharm_gc_c_233 _atom_site_anharm_gc_c_333 O1 -0.000010(3) -0.0000005(9) 0.0000002(7) -0.0000004(5) 0.0000000(2) 0.0000000(2) -0.0000004(5) -0.00000020(18) 0.00000000(12) 0.00000005(14) O2 -0.0000136(14) 0.0000019(4) -0.0000008(3) -0.0000003(2) 0.00000043(11) -0.00000020(11) -0.0000001(2) 0.00000006(8) -0.00000003(6) -0.00000012(6) loop_ _atom_site_anharm_gc_d_label _atom_site_anharm_gc_d_1111 _atom_site_anharm_gc_d_1112 _atom_site_anharm_gc_d_1113 _atom_site_anharm_gc_d_1122 _atom_site_anharm_gc_d_1123 _atom_site_anharm_gc_d_1133 _atom_site_anharm_gc_d_1222 _atom_site_anharm_gc_d_1223 _atom_site_anharm_gc_d_1233 _atom_site_anharm_gc_d_1333 _atom_site_anharm_gc_d_2222 _atom_site_anharm_gc_d_2223 _atom_site_anharm_gc_d_2233 _atom_site_anharm_gc_d_2333 _atom_site_anharm_gc_d_3333 O1 0.0000003(4) -0.00000003(12) 0.00000001(8) 0.00000002(5) -0.00000000(3) -0.00000001(2) 0.00000003(4) 0.000000018(14) -0.000000002(10) -0.000000001(11) 0.00000001(4) 0.000000015(14) 0.000000002(7) -0.000000002(6) -0.000000000(8) O2 0.00000030(19) -0.00000011(5) 0.00000008(4) 0.00000004(2) -0.000000031(13) 0.000000025(12) -0.000000007(16) 0.000000012(6) -0.000000009(5) 0.000000009(5) -0.000000025(17) 0.000000004(6) 0.000000003(3) -0.000000003(3) 0.000000005(4)