#------------------------------------------------------------------------------ #$Date: 2024-11-20 04:49:53 +0200 (Wed, 20 Nov 2024) $ #$Revision: 296005 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/32/1573206.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_1573206 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 2024-08-04 _audit_creation_method ; Olex2 1.5 (compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928) ; _cell_angle_alpha 90 _cell_angle_beta 104.385(7) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.2522(5) _cell_length_b 11.4389(8) _cell_length_c 17.7050(13) _cell_measurement_reflns_used 3034 _cell_measurement_temperature 350.00(10) _cell_measurement_theta_max 79.1690 _cell_measurement_theta_min 4.6270 _cell_volume 1422.71(18) _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 air _diffrn_ambient_temperature 350.00(10) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.9852 _diffrn_measured_fraction_theta_max 0.9687 _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 -0.0485165578 _diffrn_orient_matrix_UB_12 0.0933634007 _diffrn_orient_matrix_UB_13 0.0547165287 _diffrn_orient_matrix_UB_21 0.1932976920 _diffrn_orient_matrix_UB_22 -0.0215031390 _diffrn_orient_matrix_UB_23 0.0584964782 _diffrn_orient_matrix_UB_31 0.0914647225 _diffrn_orient_matrix_UB_32 0.0945475498 _diffrn_orient_matrix_UB_33 -0.0408438935 _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 0.0309 _diffrn_reflns_av_unetI/netI 0.0303 _diffrn_reflns_Laue_measured_fraction_full 0.9852 _diffrn_reflns_Laue_measured_fraction_max 0.9687 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 9254 _diffrn_reflns_point_group_measured_fraction_full 0.9852 _diffrn_reflns_point_group_measured_fraction_max 0.9687 _diffrn_reflns_theta_full 67.6840 _diffrn_reflns_theta_max 79.33 _diffrn_reflns_theta_min 4.65 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 0.679 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.817 _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 1.337 _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 0.1500 _refine_diff_density_min -0.1970 _refine_diff_density_rms 0.0368 _refine_ls_d_res_high 0.7845 _refine_ls_d_res_low 9.5163 _refine_ls_goodness_of_fit_ref 1.0112 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_constraints 0 _refine_ls_number_parameters 305 _refine_ls_number_reflns 3002 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.0112 _refine_ls_R_factor_all 0.0785 _refine_ls_R_factor_gt 0.0418 _refine_ls_shift/su_max 0.0005 _refine_ls_shift/su_mean 0.0001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0447P)^2^+0.1797P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1036 _refine_ls_wR_factor_ref 0.1345 _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 1685 _reflns_number_total 3002 _reflns_threshold_expression I>=2u(I) _iucr_refine_instructions_details ; TITL 2oapb_multit_9_350_00_smart3_abs_a.res in P2(1)/c REM Old TITL 2oAPb_multiT_9_350_00_smart3_abs in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.252, Rweak 0.123, Alpha 0.043 REM 0.287 for 142 systematic absences, Orientation as input REM Formula found by SHELXT: C20 O2 CELL 1.54184 7.2522 11.4389 17.705 90 104.385 90 ZERR 4 0.0005 0.0008 0.0013 0 0.007 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 0.11 0.13 0.18 TEMP 77 CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta WGHT 0.04469 0.179696 FVAR 0.434589 REM REM REM REM > REM REM O1 3 0.44505 0.56090 0.73838 11.00000 0.19384 0.10779 0.06556 = -0.02617 0.00987 -0.00862 O2 3 0.20742 0.12023 0.45530 11.00000 0.35037 0.10019 0.17100 = -0.06590 0.13329 -0.06831 C1 1 0.31838 0.44303 0.62894 11.00000 0.06320 0.07382 0.06330 = -0.00730 0.01791 -0.00031 C2 1 0.29720 0.52874 0.56983 11.00000 0.05743 0.07079 0.06686 = -0.00745 0.01705 -0.00089 C3 1 0.32433 0.65077 0.58606 11.00000 0.08611 0.07261 0.08880 = -0.00867 0.01899 -0.00445 H3 2 0.36017 0.67272 0.64556 11.00000 0.12399 C4 1 0.30606 0.73039 0.52799 11.00000 0.09159 0.07290 0.12533 = 0.00761 0.02536 0.00013 H4 2 0.33468 0.82077 0.54127 11.00000 0.14169 C5 1 0.25953 0.69735 0.44811 11.00000 0.06763 0.10047 0.10462 = 0.02478 0.02054 0.00860 C6 1 0.24729 0.77969 0.38798 11.00000 0.08684 0.13269 0.13710 = 0.05550 0.02878 0.01635 H6 2 0.27586 0.87283 0.40790 11.00000 0.18734 C7 1 0.20243 0.74457 0.31113 11.00000 0.09474 0.19787 0.13370 = 0.08426 0.03127 0.02823 H7 2 0.19114 0.80312 0.26491 11.00000 0.18895 C8 1 0.16816 0.62845 0.29246 11.00000 0.08490 0.21323 0.08253 = 0.05026 0.02023 0.02328 H8 2 0.13507 0.60409 0.23343 11.00000 0.16562 C9 1 0.17938 0.54440 0.35037 11.00000 0.06237 0.15529 0.06706 = 0.01717 0.01411 0.01222 C10 1 0.14546 0.42385 0.33249 11.00000 0.08731 0.17083 0.06623 = -0.01600 0.01245 0.00299 H10 2 0.11028 0.40160 0.27226 11.00000 0.14597 C11 1 0.16113 0.34246 0.38850 11.00000 0.08854 0.12414 0.07323 = -0.02861 0.01731 -0.00586 H11 2 0.13966 0.24950 0.37539 11.00000 0.13418 C12 1 0.21387 0.37345 0.46954 11.00000 0.06033 0.09021 0.06650 = -0.01688 0.01662 -0.00194 C13 1 0.23653 0.28952 0.52985 11.00000 0.07228 0.07326 0.08364 = -0.01740 0.02447 -0.00485 C14 1 0.28598 0.32724 0.60713 11.00000 0.07268 0.07289 0.07553 = -0.00539 0.02217 -0.00230 H14 2 0.30495 0.26086 0.65232 11.00000 0.10608 C15 1 0.24478 0.49313 0.49017 11.00000 0.05127 0.08289 0.06244 = -0.00484 0.01452 0.00121 C16 1 0.22679 0.57836 0.42979 11.00000 0.05395 0.10546 0.07164 = 0.01228 0.01506 0.00752 C17 1 0.38052 0.46907 0.71354 11.00000 0.08328 0.09671 0.06192 = -0.01144 0.01750 0.00402 C18 1 0.35901 0.37963 0.77206 11.00000 0.13135 0.14390 0.07210 = 0.01358 0.02176 -0.01410 H18a 2 0.45799 0.32061 0.77694 11.00000 0.21693 H18b 2 0.38068 0.41758 0.82750 11.00000 0.19229 H18c 2 0.23394 0.33724 0.76085 11.00000 0.18504 C19 1 0.21967 0.16067 0.51689 11.00000 0.11670 0.08319 0.11514 = -0.03090 0.04340 -0.01779 C20 1 0.20205 0.08157 0.58198 11.00000 0.16439 0.07429 0.14277 = 0.00571 -0.00357 -0.00484 H20a 2 0.16540 -0.00209 0.56316 11.00000 0.21606 H20b 2 0.34896 0.07763 0.61875 11.00000 0.24790 H20c 2 0.13492 0.11320 0.62395 11.00000 0.34388 HKLF 4 END Q1 1 0.32 0.075 0.55 11 0.05 0.15 Q2 1 0.52 0.925 0.5 11 0.05 0.15 Q4 1 0.2 0.25 0.45 11 0.05 0.12 Q5 1 0.04 0.125 0.6 11 0.05 0.12 Q3 1 0.16 0.05 0.583333 11 0.05 0.13 REM The information below was added by Olex2. REM REM R1 = 0.0418 for 1685 Fo > 4sig(Fo) and 0.0785 for all 3002 data REM 305 parameters refined using 0 restraints REM Highest difference peak 0.1500, deepest hole -0.1970 REM Mean Shift 0.0001, Max Shift 0.0005. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0785 REM R1_gt = 0.0418 REM wR_ref = 0.1345 REM GOOF = 1.0112 REM Shift_max = 0.0005 REM Shift_mean = 0.0001 REM Reflections_all = 3002 REM Reflections_gt = 1685 REM Parameters = 305 REM Hole = -0.1970 REM Peak = 0.1500 REM Flack = n/a ; _cod_data_source_file pen5002.cif _cod_data_source_block 350K _cod_database_code 1573206 _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_16-39-36 ; _iucr_refine_fcf_details ; data_350K _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 7.2522(5) _cell_length_b 11.4389(8) _cell_length_c 17.7050(13) _cell_angle_alpha 90 _cell_angle_beta 104.385(7) _cell_angle_gamma 90 _cell_volume 1422.71(18) 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 0.073 -0.189 0.463 375.557 o -9 0 4 1.507 -0.106 1.324 43.283 o -9 0 8 1.178 0.635 1.165 54.444 o -9 1 1 0.088 -0.318 0.477 352.385 o -9 1 2 0.083 0.059 0.301 806.642 o -9 1 3 0.018 0.128 0.372 564.691 o -9 1 4 0.687 0.613 0.430 274.387 o -9 1 5 1.609 0.389 0.489 182.734 o -9 1 6 2.165 1.260 0.440 156.535 o -9 1 7 0.124 0.230 0.394 454.330 o -9 1 8 0.729 0.511 0.454 257.978 o -9 1 9 0.061 0.094 0.329 689.743 o -9 1 10 0.343 0.424 0.477 285.028 o -9 2 3 1.197 0.688 0.529 179.288 o -9 2 4 0.887 0.151 0.370 331.450 o -9 2 5 0.564 0.530 0.348 378.356 o -9 2 6 3.234 0.988 0.443 127.759 o -9 2 7 0.845 0.336 0.481 236.464 o -9 2 8 0.043 -0.031 0.503 324.298 o -9 3 4 4.259 0.053 0.953 58.233 o -9 3 5 2.174 0.265 0.953 70.408 o -8 0 2 8.194 7.307 1.430 23.342 o -8 0 4 73.199 69.573 3.124 2.534 o -8 0 6 7.505 9.636 2.330 11.897 o -8 0 8 1.559 1.290 0.973 68.901 o -8 0 10 0.005 -0.369 0.884 107.043 o -8 0 12 0.128 0.676 0.577 215.020 o -8 0 14 0.278 0.000 0.524 271.775 o -8 1 1 0.988 1.107 0.634 142.247 o -8 1 2 10.038 10.139 0.904 29.586 o -8 1 3 43.812 43.686 1.522 5.978 o -8 1 4 78.431 80.434 1.836 2.784 o -8 1 5 64.232 62.938 5.745 1.592 o -8 1 6 22.354 24.848 1.959 9.225 o -8 1 7 0.571 0.454 0.717 137.363 o -8 1 8 0.635 0.961 0.679 140.587 o -8 1 9 0.008 0.120 0.703 166.628 o -8 1 10 1.415 1.093 0.535 159.732 o -8 1 11 3.504 3.220 0.605 83.623 o -8 1 12 1.098 0.676 0.463 215.524 o -8 1 13 0.285 0.025 0.410 411.422 o -8 1 14 0.414 0.560 0.357 397.276 o -8 1 15 0.224 0.176 0.336 556.176 o -8 2 1 0.735 0.658 0.666 146.398 o -8 2 2 0.002 -0.065 0.608 226.546 o -8 2 3 10.176 12.311 1.192 23.165 o -8 2 4 61.953 67.979 1.930 3.580 o -8 2 5 60.100 59.980 2.515 3.443 o -8 2 6 23.874 24.218 1.009 12.925 o -8 2 7 4.392 3.683 1.032 45.371 o -8 2 8 0.013 -0.440 0.669 186.323 o -8 2 9 5.114 6.957 0.879 44.828 o -8 2 10 9.790 10.299 0.838 31.132 o -8 2 11 8.480 10.058 0.963 30.917 o -8 2 12 0.581 0.449 0.456 274.107 o -8 2 13 0.682 0.823 0.389 295.711 o -8 2 14 0.169 -0.249 0.376 517.502 o -8 2 15 0.121 -0.012 0.272 947.342 o -8 3 1 0.666 1.501 0.570 168.793 o -8 3 2 7.475 8.313 0.688 42.161 o -8 3 3 1.284 1.348 0.568 149.417 o -8 3 4 0.104 -0.372 0.747 146.849 o -8 3 5 15.901 18.242 0.898 19.209 o -8 3 6 7.735 7.648 0.615 44.512 o -8 3 7 0.116 0.082 0.558 253.192 o -8 3 8 2.938 1.837 0.537 109.613 o -8 3 9 3.860 4.141 0.575 78.084 o -8 3 10 4.898 4.705 0.595 65.982 o -8 3 11 1.340 1.299 0.507 167.799 o -8 3 12 2.732 2.012 0.542 110.981 o -8 3 13 1.445 1.330 0.356 218.506 o -8 3 14 0.003 0.318 0.582 233.490 o -8 4 1 0.392 0.158 0.625 187.465 o -8 4 2 2.389 2.992 1.218 42.683 o -8 4 3 7.151 5.793 0.879 40.526 o -8 4 4 0.588 0.895 0.746 122.868 o -8 4 5 0.325 0.508 0.911 93.107 o -8 4 6 0.510 2.008 0.950 77.125 o -8 4 7 0.026 0.106 0.776 136.803 o -8 4 8 0.008 0.362 0.890 102.808 o -8 4 9 1.411 1.641 1.006 65.228 o -8 4 10 1.140 2.171 1.006 65.263 o -8 4 11 0.020 -0.688 0.953 91.943 o -8 4 12 0.421 0.318 0.847 106.346 o -8 5 1 2.292 2.428 0.784 80.141 o -8 5 2 0.335 -0.320 0.768 132.995 o -8 5 3 0.916 1.535 1.059 63.168 o -8 5 4 2.004 3.283 1.165 46.382 o -8 5 5 2.275 2.171 1.112 50.783 o -8 5 6 1.623 2.171 1.059 57.658 o -8 5 7 0.036 0.318 1.006 80.870 o -8 5 8 0.075 0.661 0.537 248.215 o -8 5 9 0.001 0.477 0.529 271.699 o -8 5 10 0.035 0.477 0.900 99.332 o -8 5 11 0.155 0.688 0.794 121.212 o -8 5 12 0.059 0.424 0.635 191.951 o -8 6 1 0.164 0.675 0.431 340.534 o -8 6 2 0.149 0.310 0.449 351.788 o -8 6 3 0.008 -0.229 0.456 400.162 o -8 6 4 0.836 0.695 0.847 97.285 o -8 6 5 4.319 5.012 0.607 68.207 o -8 6 6 2.356 1.623 0.537 123.716 o -8 6 7 4.011 4.553 0.623 71.148 o -8 6 8 2.351 1.906 0.519 124.069 o -8 6 9 1.862 2.059 0.927 69.068 o -8 6 10 0.995 0.212 0.688 138.009 o -8 6 11 0.165 0.053 0.529 276.133 o -8 7 4 0.122 -0.159 0.424 431.662 o -8 7 5 1.031 1.112 0.477 199.622 o -8 7 6 3.372 2.647 0.529 97.092 o -8 7 7 13.151 6.142 0.688 31.591 o -7 0 2 2.521 3.495 1.588 27.450 o -7 0 4 8.115 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209.338 o 6 7 5 0.406 0.767 0.500 242.411 o 6 7 6 3.103 2.432 0.494 107.645 o 6 7 7 1.243 1.436 0.483 177.383 o 6 7 8 0.066 0.123 0.390 499.194 o 6 7 9 0.904 0.208 0.340 352.495 o 6 8 0 0.741 0.608 0.766 117.450 o 6 8 1 0.501 0.897 0.773 117.662 o 6 8 2 0.402 0.825 0.594 185.488 o 6 8 3 0.077 0.919 0.489 275.797 o 6 8 4 0.281 0.402 0.543 237.210 o 6 8 5 0.007 -0.023 0.442 426.917 o 6 8 6 0.087 0.416 0.432 377.156 o 6 8 7 0.132 0.453 0.496 289.561 o 6 9 0 7.127 6.896 0.668 46.200 o 6 9 1 14.987 14.770 0.784 22.394 o 6 9 2 2.369 0.491 0.509 144.785 o 6 9 3 3.172 2.471 0.477 108.409 o 6 9 4 0.460 -0.183 0.359 454.269 o 6 9 5 0.005 -0.424 0.635 207.104 o 6 10 0 12.138 11.830 8.392 1.149 o 6 10 1 16.557 11.315 7.651 1.359 o 6 10 2 7.285 5.254 4.183 4.461 o 7 0 2 20.258 17.949 2.383 8.427 o 7 0 6 0.674 -0.159 1.006 76.597 o 7 0 8 0.184 1.324 0.900 91.800 o 7 1 0 1.378 0.972 0.559 155.338 o 7 1 1 0.595 1.107 0.507 211.757 o 7 1 2 0.014 -0.351 0.525 302.292 o 7 1 3 43.012 36.013 1.284 6.829 o 7 1 4 5.565 4.375 0.715 56.086 o 7 1 5 16.717 18.002 1.694 12.806 o 7 1 6 2.945 2.313 1.430 32.838 o 7 1 7 0.133 -0.574 0.724 155.193 o 7 1 8 0.002 0.394 0.596 221.262 o 7 1 9 0.216 0.028 0.359 535.389 o 7 2 0 0.007 -0.836 0.497 338.332 o 7 2 1 1.299 0.515 0.504 189.244 o 7 2 2 0.299 0.877 0.453 284.430 o 7 2 3 1.107 0.833 0.441 220.985 o 7 2 4 3.257 1.850 0.659 88.035 o 7 2 5 1.873 1.729 0.606 119.226 o 7 2 6 0.394 0.442 0.559 216.362 o 7 2 7 1.010 0.561 0.528 192.308 o 7 2 8 0.857 0.532 0.449 248.379 o 7 2 9 0.232 -0.430 0.357 540.237 o 7 3 0 0.345 0.350 0.401 375.309 o 7 3 1 0.422 0.129 0.388 400.367 o 7 3 2 0.036 -0.034 0.399 512.729 o 7 3 3 1.214 1.176 0.448 199.694 o 7 3 4 2.225 2.882 0.533 113.832 o 7 3 5 0.024 0.296 0.464 355.133 o 7 3 6 1.085 0.828 0.490 198.785 o 7 3 7 0.038 0.193 0.422 430.742 o 7 3 8 0.491 0.406 0.317 455.825 o 7 3 9 5.216 2.156 0.504 80.244 o 7 4 0 2.708 2.243 0.608 99.554 o 7 4 1 2.539 1.098 0.512 130.794 o 7 4 2 10.039 9.677 1.039 27.375 o 7 4 3 5.536 5.013 0.681 56.391 o 7 4 4 0.160 0.835 0.580 206.160 o 7 4 5 2.666 2.384 0.690 88.049 o 7 4 6 0.688 0.595 0.605 172.547 o 7 4 7 0.032 0.336 0.471 340.570 o 7 4 8 1.794 0.426 0.466 181.603 o 7 5 0 0.631 0.311 0.545 213.652 o 7 5 1 15.277 16.006 0.970 19.890 o 7 5 2 11.548 10.585 0.749 29.592 o 7 5 3 0.830 -0.022 0.510 232.495 o 7 5 4 9.970 9.211 1.098 26.667 o 7 5 5 8.299 8.637 1.012 31.271 o 7 5 6 6.179 5.927 0.591 55.155 o 7 5 7 2.631 2.104 0.945 62.190 o 7 6 0 3.588 3.422 0.874 58.846 o 7 6 1 5.677 4.513 0.865 47.728 o 7 6 2 1.028 1.210 0.636 139.026 o 7 6 3 3.857 2.344 0.721 73.195 o 7 6 4 9.419 8.461 1.158 26.654 o 7 6 5 10.101 6.936 0.786 34.785 o 7 6 6 8.741 1.825 1.191 31.500 o 7 7 0 0.808 0.913 0.595 165.069 o 7 7 1 0.426 0.665 0.566 203.253 o 7 7 2 0.117 -0.258 0.785 132.963 o 7 7 3 1.097 1.254 0.533 169.879 o 7 7 4 0.952 0.027 0.618 168.194 o 7 7 5 2.118 1.212 0.357 182.036 o 7 8 0 0.893 1.203 0.480 203.368 o 7 8 1 0.211 0.241 0.459 333.814 o 7 8 2 0.286 0.426 0.412 363.956 o 7 8 3 0.037 0.212 0.477 342.904 o 8 0 2 1.349 -0.053 1.006 71.253 o 8 0 4 0.615 0.582 0.794 113.153 o 8 1 0 0.048 -0.475 0.711 163.554 o 8 1 1 0.059 0.039 0.653 192.084 o 8 1 2 0.156 -0.201 0.591 227.539 o 8 1 3 0.107 0.193 0.553 253.849 o 8 1 4 0.165 -0.192 0.431 407.994 o 8 1 5 0.005 -0.291 0.351 677.075 o 8 1 6 0.007 -0.212 0.529 297.803 o 8 2 0 0.405 -0.682 0.586 213.298 o 8 2 1 0.012 0.501 0.536 262.366 o 8 2 2 0.208 0.439 0.505 273.447 o 8 2 3 0.054 0.153 0.455 375.879 o 8 2 4 0.103 0.006 0.450 388.403 o 8 2 5 0.394 0.026 0.353 481.702 o 8 3 0 0.008 -0.303 0.478 364.966 o 8 3 1 0.002 0.521 0.450 357.347 o 8 3 2 0.835 0.500 0.421 271.590 o 8 3 3 0.065 0.425 0.345 548.482 o 8 3 4 0.056 0.424 0.487 311.211 o 8 3 5 0.438 -0.212 0.477 299.341 o 8 4 0 1.607 1.235 0.602 132.327 o 8 4 1 0.402 1.007 0.539 209.249 o 8 4 2 0.337 -1.200 0.662 175.142 o 8 4 3 0.102 0.064 0.558 255.856 o 8 5 0 0.036 0.659 1.032 75.450 o 8 5 1 0.472 -0.265 0.847 108.123 o 8 5 2 1.489 1.377 0.741 102.814 o 8 6 0 0.597 0.053 0.741 134.075 o 8 6 1 1.561 0.953 0.635 128.539 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 1.621 _oxdiff_exptl_absorpt_empirical_full_min 0.650 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 0.4450(6) 0.5609(3) 0.73838(18) 0.1263(15) Uani 1.000000 . O2 O 0.2074(8) 0.1202(4) 0.4553(3) 0.195(2) Uani 1.000000 . C1 C 0.3184(2) 0.44303(16) 0.62894(10) 0.0664(4) Uani 1.000000 . C2 C 0.2972(2) 0.52874(15) 0.56983(10) 0.0647(4) Uani 1.000000 . C3 C 0.3243(3) 0.65077(18) 0.58606(14) 0.0830(6) Uani 1.000000 . H3 H 0.360(3) 0.673(2) 0.6456(15) 0.124(8) Uiso 1.000000 . C4 C 0.3061(3) 0.7304(2) 0.52799(17) 0.0969(7) Uani 1.000000 . H4 H 0.335(4) 0.821(3) 0.5413(15) 0.142(9) Uiso 1.000000 . C5 C 0.2595(3) 0.6974(2) 0.44811(15) 0.0911(6) Uani 1.000000 . C6 C 0.2473(4) 0.7797(3) 0.3880(2) 0.1187(10) Uani 1.000000 . H6 H 0.276(5) 0.873(3) 0.408(2) 0.187(15) Uiso 1.000000 . C7 C 0.2024(4) 0.7446(4) 0.3111(3) 0.1416(15) Uani 1.000000 . H7 H 0.191(5) 0.803(3) 0.265(2) 0.189(13) Uiso 1.000000 . C8 C 0.1682(4) 0.6285(5) 0.29246(18) 0.1270(12) Uani 1.000000 . H8 H 0.135(4) 0.604(3) 0.233(2) 0.166(11) Uiso 1.000000 . C9 C 0.1794(3) 0.5444(3) 0.35037(12) 0.0953(7) Uani 1.000000 . C10 C 0.1455(3) 0.4239(3) 0.33249(15) 0.1093(9) Uani 1.000000 . H10 H 0.110(4) 0.402(2) 0.2723(18) 0.146(9) Uiso 1.000000 . C11 C 0.1611(3) 0.3425(3) 0.38850(14) 0.0958(7) Uani 1.000000 . H11 H 0.140(4) 0.249(3) 0.3754(16) 0.134(9) Uiso 1.000000 . C12 C 0.2139(2) 0.37345(18) 0.46954(10) 0.0722(5) Uani 1.000000 . C13 C 0.2365(3) 0.28952(18) 0.52985(12) 0.0755(5) Uani 1.000000 . C14 C 0.2860(3) 0.32724(17) 0.60713(12) 0.0730(5) Uani 1.000000 . H14 H 0.305(3) 0.2609(19) 0.6523(12) 0.106(6) Uiso 1.000000 . C15 C 0.2448(2) 0.49313(16) 0.49017(10) 0.0655(4) Uani 1.000000 . C16 C 0.2268(2) 0.5784(2) 0.42979(11) 0.0771(5) Uani 1.000000 . C17 C 0.3805(3) 0.4691(2) 0.71354(13) 0.0807(6) Uani 1.000000 . C18 C 0.3590(6) 0.3796(3) 0.77206(16) 0.1164(9) Uani 1.000000 . H18a H 0.458(6) 0.321(4) 0.777(2) 0.22(2) Uiso 1.000000 . H18b H 0.381(5) 0.418(3) 0.827(2) 0.192(14) Uiso 1.000000 . H18c H 0.234(5) 0.337(3) 0.761(2) 0.185(15) Uiso 1.000000 . C19 C 0.2197(4) 0.1607(3) 0.51689(19) 0.1024(8) Uani 1.000000 . C20 C 0.2021(7) 0.0816(3) 0.5820(2) 0.1345(12) Uani 1.000000 . H20a H 0.165(5) -0.002(4) 0.563(2) 0.216(16) Uiso 1.000000 . H20b H 0.349(7) 0.078(4) 0.619(3) 0.25(2) Uiso 1.000000 . H20c H 0.135(10) 0.113(6) 0.624(4) 0.34(4) Uiso 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 0.194(4) 0.108(3) 0.066(2) -0.009(3) 0.010(2) -0.0262(19) O2 0.350(6) 0.100(3) 0.171(4) -0.068(3) 0.133(4) -0.066(3) C1 0.0632(9) 0.0738(11) 0.0633(10) -0.0003(8) 0.0179(7) -0.0073(9) C2 0.0574(9) 0.0708(11) 0.0669(10) -0.0009(7) 0.0170(7) -0.0075(9) C3 0.0861(13) 0.0726(13) 0.0888(15) -0.0044(10) 0.0190(11) -0.0087(12) C4 0.0916(15) 0.0729(15) 0.125(2) 0.0001(11) 0.0254(14) 0.0076(14) C5 0.0676(11) 0.1005(17) 0.1046(17) 0.0086(11) 0.0205(11) 0.0248(14) C6 0.0868(15) 0.133(3) 0.137(3) 0.0163(15) 0.0288(16) 0.055(2) C7 0.0947(19) 0.198(4) 0.134(3) 0.028(2) 0.0313(19) 0.084(3) C8 0.0849(16) 0.213(4) 0.0825(18) 0.023(2) 0.0202(13) 0.050(2) C9 0.0624(11) 0.155(2) 0.0671(12) 0.0122(12) 0.0141(9) 0.0172(15) C10 0.0873(15) 0.171(3) 0.0662(14) 0.0030(16) 0.0124(11) -0.0160(17) C11 0.0885(14) 0.124(2) 0.0732(14) -0.0059(13) 0.0173(10) -0.0286(14) C12 0.0603(9) 0.0902(14) 0.0665(10) -0.0019(8) 0.0166(8) -0.0169(10) C13 0.0723(11) 0.0733(12) 0.0836(13) -0.0048(9) 0.0245(9) -0.0174(10) C14 0.0727(11) 0.0729(13) 0.0755(12) -0.0023(9) 0.0222(9) -0.0054(10) C15 0.0513(8) 0.0829(12) 0.0624(10) 0.0012(8) 0.0145(7) -0.0048(9) C16 0.0539(9) 0.1055(17) 0.0716(12) 0.0075(9) 0.0151(8) 0.0123(11) C17 0.0833(13) 0.0967(18) 0.0619(13) 0.0040(12) 0.0175(10) -0.0114(13) C18 0.131(3) 0.144(3) 0.0721(15) -0.014(2) 0.0218(15) 0.0136(16) C19 0.1167(18) 0.0832(19) 0.115(2) -0.0178(14) 0.0434(16) -0.0309(17) C20 0.164(3) 0.0743(17) 0.143(3) -0.0048(18) -0.004(3) 0.0057(18) 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 -2 967.89 22.35 0 0 -3 -0.06 0.17 0 0 -4 201.93 5.33 0 0 -5 -0.06 0.11 0 0 -5 -0.06 0.25 0 0 -6 270.75 6.59 0 0 -6 285.52 7.44 0 0 -7 -0.17 0.34 0 0 -8 21.88 1.49 0 0 -9 0.12 0.36 0 0 -10 2.35 0.63 0 0 -11 -0.16 0.41 0 0 -11 0.27 0.21 0 0 -12 3.93 0.45 0 0 -12 6.18 1.06 0 0 -13 -0.34 0.24 0 0 -14 0.11 0.24 0 0 -15 -0.06 0.25 0 0 -16 2.75 0.44 0 0 -17 0.11 0.23 0 0 -18 -0.05 0.22 0 0 -19 -0.04 0.18 0 0 -20 2.67 0.26 0 0 -21 0.01 0.13 0 1 -1 1756.96 40.3 0 -1 -2 286.4 7.01 0 1 -2 299.41 7.04 0 1 -3 513.67 11.99 0 -1 -3 490.79 11.96 0 -1 -4 14.09 0.82 0 1 -4 15.14 0.84 0 1 -5 24.19 1.23 0 -1 -5 22.81 1.21 0 1 -5 23.31 0.99 0 1 -6 16.79 0.85 0 -1 -6 17.75 1.12 0 1 -6 16.35 1.1 0 1 -7 -0.08 0.32 0 -1 -7 0.17 0.28 0 1 -7 0.04 0.18 0 -1 -8 1.62 0.5 0 1 -8 2.03 0.57 0 1 -9 18.69 1.48 0 -1 -9 19.78 1.53 0 1 -10 2.22 0.63 0 -1 -10 2.36 0.59 0 1 -11 5.83 0.46 0 1 -11 6.3 0.51 0 -1 -11 5.41 0.49 0 -1 -11 6.56 0.99 0 1 -11 5.6 0.96 0 1 -12 7.3 0.59 0 -1 -12 7.51 0.6 0 1 -12 5.64 1.07 0 -1 -12 8.19 1.22 0 1 -12 6.81 0.52 0 1 -13 14.79 0.88 0 1 -13 15.12 0.81 0 -1 -13 13.51 0.85 0 -1 -14 19.41 1.05 0 1 -14 18.57 0.95 0 -1 -15 3.13 0.46 0 -1 -16 3.21 0.49 0 -1 -17 0.21 0.24 0 -1 -17 -0.02 0.29 0 -1 -18 0.19 0.26 0 -1 -19 0.19 0.2 0 -1 -19 0.35 0.25 0 1 -19 -0.1 0.21 0 -1 -20 0.22 0.2 0 -1 -20 0.3 0.16 0 1 -20 0.17 0.18 0 -1 -20 0.03 0.18 0 -1 -21 1.25 0.16 0 -1 -21 1.52 0.17 0 2 0 26.61 1.06 0 2 0 27.74 1.07 0 2 1 54.47 1.66 0 2 1 54.86 1.74 0 2 -2 428.89 9.96 0 -2 -2 412.94 9.92 0 2 -3 163.96 4.23 0 -2 -3 156.72 4.19 0 2 -4 13.52 0.81 0 -2 -4 15.15 0.84 0 2 -5 24.3 1.25 0 -2 -5 25.19 1.26 0 2 -6 24.43 1.24 0 -2 -6 27.32 1.42 0 2 -6 26.36 1.43 0 -2 -7 31.49 1.7 0 2 -7 34.21 1.52 0 2 -7 29.01 1.66 0 -2 -8 2.25 0.5 0 2 -8 1.85 0.5 0 2 -9 0.12 0.36 0 -2 -9 -0.24 0.34 0 -2 -10 21.26 1.71 0 2 -10 24.32 1.03 0 2 -10 26.41 1.88 0 2 -11 2.16 0.31 0 -2 -11 2.9 0.71 0 2 -11 1.93 0.64 0 -2 -11 1.87 0.31 0 2 -11 1.8 0.32 0 2 -12 35.5 1.35 0 2 -12 35.51 1.43 0 -2 -12 34.54 1.39 0 -2 -12 29.95 2.37 0 2 -12 33.05 2.45 0 2 12 33.65 1.36 0 2 -13 79.95 2.56 0 2 -13 73.83 2.4 0 -2 -13 77.85 2.51 0 2 -14 47.43 1.78 0 2 -14 50.27 1.9 0 -2 -14 50.98 1.9 0 2 -15 0.5 0.25 0 -2 -15 -0.21 0.28 0 2 -15 0.05 0.25 0 2 -16 1.2 0.37 0 2 -16 1.05 0.29 0 -2 -16 0.43 0.28 0 2 -17 0.31 0.27 0 -2 -17 -0.12 0.3 0 -2 -17 0.4 0.26 0 2 18 -0.09 0.23 0 2 -18 0.59 0.24 0 -2 -18 0.3 0.27 0 2 -19 0.3 0.19 0 -2 -19 0.05 0.23 0 2 19 0.09 0.23 0 2 -19 -0.05 0.2 0 -2 -19 0.34 0.18 0 2 -20 0.78 0.17 0 -2 -20 0.26 0.18 0 -2 -20 0.66 0.17 0 -2 -20 0.45 0.2 0 2 20 0.23 0.19 0 2 -20 0.41 0.17 0 -2 -21 -0.05 0.14 0 -2 -21 -0.1 0.11 0 -2 -21 0.13 0.13 0 2 -21 -0.03 0.11 0 2 -21 -0.07 0.13 0 3 0 0.14 0.27 0 3 0 0.19 0.25 0 3 1 0.1 0.25 0 3 1 0.08 0.18 0 3 2 25.63 1.07 0 3 -2 25.8 0.91 0 3 2 24.91 1.23 0 3 -3 0.24 0.17 0 3 3 0.63 0.35 0 -3 -3 0.31 0.17 0 3 -4 16.8 0.9 0 -3 -4 14.94 0.86 0 3 -5 206.84 5.68 0 -3 -5 204.69 5.64 0 3 -6 207.99 6.04 0 3 -6 218.61 6.07 0 -3 -6 212.26 6.02 0 3 -7 6.72 0.73 0 -3 -7 7.09 0.8 0 3 -7 6.89 0.78 0 3 -8 21.82 1.37 0 3 -8 20.16 1.45 0 -3 -8 20 1.46 0 3 -9 0.62 0.39 0 -3 -9 0.24 0.33 0 3 -10 8.31 0.56 0 -3 -10 8.87 1.1 0 3 -10 7.73 0.54 0 3 -10 7.82 1.04 0 3 -11 5.85 0.97 0 3 -11 5.91 0.49 0 -3 -11 4.52 0.9 0 -3 -11 5.33 0.48 0 3 -11 6.48 0.51 0 -3 -12 3.47 0.41 0 3 -12 3.11 0.83 0 3 -12 3.66 0.44 0 3 12 3.38 0.44 0 3 -12 4.1 0.43 0 3 -13 57.09 1.98 0 3 13 55.69 2.03 0 -3 -13 54.62 1.97 0 3 -13 57.12 2.02 0 3 -14 6.84 0.59 0 3 -14 7.13 0.64 0 -3 -14 7.36 0.62 0 3 14 7.5 0.65 0 3 -15 4.21 0.49 0 -3 -15 3.65 0.46 0 3 -15 4.29 0.49 0 -3 -16 18.07 1.02 0 3 -16 17.57 0.95 0 3 -16 18.4 1.03 0 3 -17 1.46 0.28 0 -3 -17 1.9 0.34 0 -3 -17 1.8 0.38 0 3 -17 1.34 0.3 0 -3 -18 1.04 0.33 0 3 -18 0.89 0.23 0 -3 -18 1.05 0.29 0 3 -18 0.5 0.21 0 -3 -18 0.92 0.22 0 -3 -19 0.08 0.21 0 3 -19 0.2 0.16 0 3 -19 -0.01 0.18 0 3 19 0.33 0.23 0 -3 -19 0.19 0.16 0 3 20 0.33 0.19 0 -3 -20 0.1 0.18 0 -3 -20 0.41 0.15 0 3 -20 0.47 0.15 0 -3 -20 0.28 0.16 0 3 -20 0.26 0.14 0 -3 -20 0.2 0.18 0 3 21 0.01 0.13 0 -3 -21 0.03 0.1 0 3 -21 0.08 0.08 0 -3 -21 0.05 0.12 0 3 21 0.04 0.12 0 4 0 96.1 3.21 0 4 1 6.13 0.66 0 4 2 -0.07 0.24 0 4 3 45.45 2.02 0 4 -4 0.55 0.22 0 4 4 0.66 0.36 0 4 5 199.39 5.97 0 4 -5 196.31 5.49 0 4 -6 128.82 4.43 0 4 -6 139.9 4.27 0 4 -7 5.91 0.76 0 4 -7 5.38 0.71 0 4 -8 2.39 0.58 0 4 -8 3.84 0.67 0 4 -9 1.33 0.43 0 4 -9 2.36 0.58 0 4 -10 0.04 0.18 0 4 10 0.04 0.22 0 4 -10 -0.14 0.29 0 4 -11 21.81 1.86 0 4 11 22.3 1.09 0 4 -11 22.2 1.03 0 4 -11 20.41 1 0 4 -12 2.12 0.36 0 4 -12 1.38 0.31 0 4 12 1.82 0.36 0 4 -13 7.88 0.63 0 4 13 7.39 0.65 0 4 -13 7.73 0.62 0 4 -14 1.26 0.31 0 4 14 1.65 0.36 0 4 -14 1.96 0.36 0 4 -15 7.44 0.63 0 4 -15 7.12 0.61 0 4 15 6.78 0.64 0 -4 -16 3.61 0.5 0 4 -16 4.21 0.46 0 4 16 2.99 0.45 0 4 -17 0.51 0.21 0 4 -17 0.28 0.21 0 -4 -17 0.02 0.31 0 4 -17 0.07 0.2 0 -4 -17 0.04 0.25 0 -4 -18 0.32 0.31 0 -4 -18 0.23 0.23 0 4 -18 -0.01 0.19 0 4 -18 0.21 0.18 0 -4 -19 0.05 0.16 0 4 -19 0.17 0.14 0 4 -19 0.27 0.15 0 -4 -19 0.15 0.24 0 -4 -19 0.17 0.2 0 4 19 0.29 0.21 0 4 20 0.38 0.18 0 -4 -20 0.33 0.18 0 4 -20 -0.04 0.08 0 4 21 -0.11 0.11 0 5 0 -0.09 0.3 0 5 1 369.14 9.91 0 5 2 287.89 8.13 0 5 3 123.94 4.28 0 5 4 6.02 0.8 0 5 -5 11.78 1.13 0 5 5 9.08 1.02 0 5 -6 19.84 1.5 0 5 6 19.94 1.56 0 5 -7 7.26 0.95 0 5 -7 7.11 0.5 0 5 -8 2.02 0.53 0 5 -8 1.69 0.28 0 5 8 1.92 0.6 0 5 8 1.63 0.29 0 5 -9 0.85 0.24 0 5 -9 0.67 0.5 0 5 10 3.15 0.42 0 5 11 0.2 0.22 0 5 -12 2.22 0.38 0 5 12 1.63 0.36 0 5 -13 0.9 0.31 0 5 13 0.73 0.32 0 5 14 1.76 0.4 0 5 -14 2.6 0.42 0 5 15 -0.05 0.25 0 5 -15 -0.19 0.25 0 -5 -16 0.42 0.36 0 5 16 0.86 0.3 0 5 16 0.91 0.46 0 5 -16 0.79 0.27 0 5 17 0.31 0.4 0 -5 -17 0.14 0.32 0 -5 -17 0.42 0.26 0 -5 -18 0.2 0.29 0 -5 -18 0.24 0.24 0 -5 -19 -0.01 0.23 0 -5 -19 0.26 0.21 0 5 19 0.14 0.2 0 -5 -20 0.18 0.15 0 5 20 0.18 0.15 0 6 1 0.11 0.27 0 6 2 77.09 3.34 0 6 3 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7 7 -7 0.18 0.23 7 7 -7 0.3 0.17 7 7 -6 0.99 0.25 7 7 -6 1.14 0.21 7 7 -5 0.06 0.23 7 7 -5 0.21 0.18 7 7 -4 -0.09 0.23 7 7 -4 0.02 0.18 7 -7 -4 -0.06 0.26 7 7 -3 0.17 0.22 7 7 -3 0.09 0.18 7 -7 -3 0.57 0.25 7 7 -2 0.08 0.23 7 7 -2 -0.09 0.17 7 -7 -2 -0.06 0.25 7 7 -1 0.13 0.22 7 7 -1 0.07 0.16 7 -7 -1 0.11 0.24 7 7 0 0.23 0.21 7 7 0 0.31 0.16 7 -7 0 -0.1 0.24 7 7 1 0.11 0.19 7 7 1 0.15 0.16 7 -7 1 0.11 0.22 7 7 2 0.01 0.19 7 7 2 0.14 0.14 7 -7 2 -0.43 0.23 7 7 3 0.16 0.17 7 7 3 0.13 0.14 7 -7 3 0.48 0.2 7 7 4 0.02 0.15 7 7 4 0.19 0.12 7 -7 4 -0.29 0.18 7 7 5 0.11 0.12 7 7 5 0.27 0.1 7 -7 5 0.31 0.14 7 8 -11 0.75 0.13 7 8 -11 0.65 0.12 7 8 -10 -0.21 0.15 7 -8 -10 -0.02 0.18 7 8 -10 -0.03 0.12 7 -8 -10 -0.15 0.17 7 8 -9 -0.06 0.17 7 -8 -9 0.14 0.2 7 8 -9 -0.15 0.13 7 -8 -9 0.09 0.18 7 8 -8 0.24 0.17 7 8 -8 0.18 0.15 7 -8 -8 0.06 0.18 7 8 -7 0.36 0.2 7 8 -7 0.33 0.16 7 8 -6 -0.07 0.19 7 8 -6 -0.02 0.15 7 8 -5 -0.25 0.2 7 8 -5 0.17 0.16 7 8 -4 -0.1 0.19 7 8 -4 -0.13 0.16 7 8 -3 -0.2 0.2 7 8 -3 -0.13 0.16 7 8 -2 0.15 0.19 7 8 -2 0.4 0.15 7 8 -1 -0.12 0.18 7 8 -1 -0.02 0.15 7 -8 -1 0.07 0.2 7 8 0 0.17 0.17 7 8 0 0.18 0.13 7 -8 0 0.36 0.19 7 8 1 0.14 0.16 7 8 1 0.08 0.13 7 -8 1 -0.1 0.17 7 8 2 0.07 0.14 7 8 2 0.05 0.12 7 -8 2 0.13 0.15 7 8 3 0.04 0.09 7 -9 -8 0.03 0.13 7 9 -8 0.15 0.09 7 9 -7 0.09 0.1 7 9 -6 0.15 0.12 7 9 -4 -0.09 0.11 8 0 -15 0.05 0.12 8 0 -15 0.02 0.11 8 0 -14 0.01 0.14 8 0 -14 -0.01 0.14 8 0 -13 -0.02 0.15 8 0 -13 0.01 0.14 8 0 -12 0.06 0.17 8 0 -12 0.19 0.16 8 0 -12 0.13 0.31 8 0 -11 0.02 0.18 8 0 -11 -0.06 0.16 8 0 -11 -0.11 0.33 8 0 -10 -0.14 0.19 8 0 -10 0.06 0.35 8 0 -9 0.04 0.19 8 0 -9 0.11 0.36 8 0 -8 0.24 0.21 8 0 -8 0.25 0.38 8 0 -7 -0.02 0.37 8 0 -6 1.82 0.44 8 0 -5 -0.07 0.21 8 0 -4 13.14 0.59 8 0 -3 0.16 0.22 8 0 -2 1.38 0.27 8 0 1 0.01 0.2 8 0 2 -0.01 0.19 8 0 3 0.14 0.17 8 0 4 0.11 0.15 8 0 5 0.03 0.12 8 1 -15 0.09 0.11 8 -1 -15 0.04 0.11 8 1 -15 -0.03 0.11 8 1 -14 0.2 0.14 8 -1 -14 0.25 0.14 8 1 -14 0.01 0.13 8 -1 -14 -0.02 0.13 8 1 -13 0.01 0.15 8 -1 -13 -0.12 0.16 8 1 -13 -0.02 0.15 8 -1 -13 0.15 0.16 8 1 -12 0.16 0.17 8 -1 -12 0.15 0.17 8 1 -12 0.2 0.16 8 1 -12 0.11 0.31 8 -1 -12 -0.08 0.29 8 1 -11 0.72 0.2 8 -1 -11 0.8 0.21 8 1 -11 0.31 0.19 8 1 -11 0.84 0.36 8 -1 -11 0.3 0.34 8 1 -10 0.28 0.19 8 -1 -10 0.28 0.21 8 1 -10 0.13 0.18 8 1 -10 0.35 0.35 8 -1 -10 -0.04 0.34 8 1 -9 -0.17 0.22 8 -1 -9 0.05 0.2 8 1 -9 -0.2 0.38 8 -1 -9 0.5 0.36 8 1 -8 0.14 0.21 8 -1 -8 0.2 0.21 8 1 -8 0.34 0.37 8 -1 -8 0.07 0.35 8 1 -7 0.09 0.21 8 -1 -7 0.09 0.2 8 -1 -7 0.07 0.38 8 -1 -6 4.89 0.34 8 1 -6 4.15 0.52 8 -1 -5 11.07 0.54 8 1 -5 13.24 0.76 8 1 -4 14.83 0.67 8 -1 -4 15.22 0.68 8 -1 -4 15.4 0.64 8 1 -4 15.33 0.82 8 1 -3 7.62 0.49 8 -1 -3 8.82 0.51 8 -1 -3 8.27 0.47 8 1 -2 1.62 0.3 8 -1 -2 2 0.31 8 -1 -2 2.05 0.28 8 1 -1 0.26 0.24 8 -1 -1 0.14 0.27 8 -1 -1 0.31 0.21 8 -1 -1 0.1 0.25 8 1 0 -0.06 0.24 8 -1 0 0.03 0.22 8 -1 0 -0.25 0.24 8 1 1 -0.16 0.24 8 -1 1 0.1 0.22 8 -1 1 0.06 0.19 8 1 2 -0.05 0.2 8 -1 2 -0.19 0.22 8 -1 2 0.09 0.17 8 1 3 0.01 0.2 8 -1 3 0.01 0.19 8 -1 3 0.08 0.16 8 1 4 -0.03 0.17 8 -1 4 -0.11 0.19 8 -1 4 -0.12 0.15 8 1 4 0.1 0.15 8 1 5 -0.05 0.15 8 -1 5 -0.06 0.15 8 -1 5 -0.12 0.12 8 1 5 0.01 0.12 8 -1 6 -0.04 0.1 8 -2 -15 0.05 0.08 8 2 -15 -0.09 0.09 8 -2 -15 0.03 0.1 8 2 -14 0.02 0.12 8 -2 -14 -0.16 0.13 8 2 -14 -0.01 0.12 8 2 -13 0.26 0.14 8 -2 -13 0.05 0.15 8 2 -13 0.18 0.14 8 -2 -13 0.12 0.16 8 2 -12 0.1 0.15 8 -2 -12 -0.04 0.16 8 2 -12 0.18 0.14 8 2 -11 1.97 0.22 8 -2 -11 2.22 0.24 8 2 -11 1.3 0.2 8 2 -11 2.17 0.37 8 2 -10 2.1 0.24 8 -2 -10 1.84 0.25 8 2 -10 1.72 0.39 8 2 -9 1.41 0.23 8 -2 -9 1.19 0.24 8 2 -8 -0.03 0.19 8 -2 -8 -0.24 0.22 8 2 -8 0.24 0.37 8 -2 -8 -0.25 0.38 8 2 -7 0.75 0.22 8 -2 -7 1.04 0.24 8 2 -7 0.31 0.41 8 -2 -7 0.13 0.4 8 -2 -6 4.91 0.34 8 2 -6 4.35 0.36 8 -2 -6 4.26 0.37 8 2 -6 4.74 0.51 8 -2 -5 10.97 0.53 8 2 -5 11.92 0.71 8 -2 -4 12.68 0.6 8 -2 -4 13.26 0.59 8 2 -4 12.39 0.73 8 2 -3 2.26 0.3 8 -2 -3 1.81 0.31 8 -2 -3 2.83 0.3 8 2 -3 1.85 0.44 8 2 -2 0.19 0.24 8 -2 -2 0.05 0.25 8 -2 -2 -0.18 0.22 8 -2 -2 0.02 0.27 8 2 -2 -0.17 0.35 8 2 -1 0.14 0.22 8 -2 -1 0.19 0.24 8 -2 -1 -0.08 0.25 8 2 -1 0.28 0.33 8 2 0 -0.23 0.23 8 -2 0 0.03 0.23 8 -2 0 0.03 0.19 8 -2 0 -0.4 0.25 8 2 1 0.04 0.2 8 -2 1 0.06 0.21 8 -2 1 -0.05 0.18 8 -2 1 0.38 0.23 8 2 2 0.22 0.19 8 -2 2 0.14 0.21 8 -2 2 0.01 0.17 8 -2 2 -0.03 0.2 8 2 3 0.02 0.17 8 -2 3 -0.04 0.18 8 -2 3 -0.16 0.16 8 -2 3 0.32 0.18 8 2 4 0.1 0.15 8 -2 4 -0.07 0.17 8 -2 4 -0.03 0.13 8 2 5 -0.03 0.11 8 -2 5 0.04 0.13 8 2 5 0.01 0.11 8 -3 -14 0.06 0.11 8 3 -13 0.29 0.12 8 -3 -13 0.17 0.12 8 3 -13 0.29 0.11 8 3 -12 0.49 0.17 8 3 -12 0.53 0.15 8 -3 -12 0.53 0.15 8 3 -12 0.08 0.1 8 3 -11 0.37 0.18 8 3 -11 0.21 0.16 8 -3 -11 0.17 0.16 8 3 -10 0.99 0.22 8 3 -10 0.78 0.18 8 -3 -10 0.91 0.19 8 3 -9 0.94 0.23 8 3 -9 0.74 0.18 8 -3 -9 0.66 0.19 8 3 -9 0.83 0.37 8 3 -8 0.29 0.22 8 3 -8 0.39 0.17 8 -3 -8 0.51 0.2 8 3 -8 0.38 0.35 8 -3 -8 0.04 0.34 8 3 -7 0.13 0.21 8 3 -7 -0.01 0.18 8 -3 -7 -0.03 0.19 8 3 -7 -0.04 0.34 8 -3 -6 1.5 0.23 8 3 -6 1.62 0.28 8 3 -6 1.58 0.24 8 -3 -6 0.95 0.23 8 3 -6 1.44 0.4 8 -3 -5 3.45 0.32 8 3 -5 3.27 0.33 8 3 -5 3.5 0.3 8 3 -5 3.62 0.46 8 -3 -4 0.02 0.21 8 3 -4 -0.13 0.22 8 3 -4 -0.13 0.38 8 -3 -3 0.14 0.23 8 -3 -3 0.14 0.2 8 3 -3 0.43 0.22 8 -3 -3 0.42 0.27 8 3 -3 0.14 0.34 8 3 -2 1.54 0.25 8 -3 -2 1.49 0.27 8 -3 -2 1.81 0.26 8 3 -2 1.37 0.26 8 3 -1 0.32 0.21 8 -3 -1 0.26 0.21 8 3 -1 0.21 0.2 8 -3 -1 0.36 0.25 8 3 0 -0.01 0.19 8 -3 0 -0.18 0.22 8 -3 0 0.01 0.19 8 3 0 -0.22 0.19 8 -3 0 0.13 0.23 8 3 1 -0.06 0.18 8 -3 1 -0.01 0.2 8 -3 1 0.04 0.18 8 3 1 0.06 0.18 8 -3 1 0.53 0.22 8 3 2 0.06 0.17 8 -3 2 0.16 0.18 8 -3 2 0.19 0.16 8 3 2 0.27 0.18 8 -3 2 -0.27 0.21 8 3 3 0.07 0.13 8 -3 3 0.02 0.16 8 -3 3 0.04 0.14 8 3 3 0.16 0.14 8 -3 3 0.11 0.17 8 -3 4 0.08 0.13 8 -3 4 0.08 0.13 8 3 5 -0.04 0.09 8 4 -12 0.06 0.16 8 4 -11 -0.13 0.18 8 4 -10 0.41 0.19 8 4 -9 0.31 0.19 8 4 -8 -0.01 0.2 8 4 -8 0.19 0.31 8 4 -7 0.01 0.2 8 4 -7 0.17 0.31 8 -4 -7 -0.11 0.3 8 4 -6 0.4 0.22 8 4 -6 0.35 0.31 8 4 -5 -0.04 0.21 8 4 -5 0.29 0.3 8 -4 -4 0.15 0.19 8 4 -4 0.19 0.21 8 -4 -3 1.21 0.23 8 4 -3 0.93 0.24 8 4 -2 0.35 0.22 8 -4 -2 0.81 0.26 8 -4 -1 0.06 0.18 8 4 -1 0.22 0.2 8 -4 -1 -0.25 0.25 8 -4 0 0.14 0.18 8 4 0 0.26 0.19 8 -4 0 0.32 0.23 8 -4 1 0.18 0.16 8 4 1 0.08 0.17 8 -4 1 0.34 0.21 8 4 2 -0.12 0.16 8 -4 2 -0.36 0.2 8 4 3 0.04 0.14 8 -4 3 -0.02 0.16 8 5 -12 0.08 0.12 8 5 -11 0.13 0.15 8 5 -10 0.09 0.17 8 5 -9 0.12 0.18 8 5 -9 0.07 0.12 8 5 -8 0.18 0.19 8 5 -8 0.09 0.12 8 5 -7 0.06 0.19 8 5 -6 0.41 0.2 8 5 -5 0.41 0.21 8 5 -4 0.62 0.22 8 5 -3 0.29 0.2 8 5 -2 0.07 0.18 8 -5 -2 -0.22 0.22 8 5 -1 0.43 0.2 8 -5 -1 0.49 0.22 8 5 0 -0.05 0.17 8 -5 0 0.34 0.21 8 5 1 -0.05 0.16 8 5 2 0.26 0.14 8 6 -11 0.01 0.1 8 6 -10 0.04 0.13 8 6 -9 0.58 0.16 8 6 -9 0.23 0.11 8 6 -8 0.36 0.17 8 6 -8 0.36 0.12 8 6 -7 0.74 0.19 8 6 -7 0.92 0.15 8 6 -6 0.38 0.19 8 6 -6 0.26 0.12 8 6 -5 0.96 0.2 8 6 -5 0.94 0.14 8 6 -4 -0.05 0.17 8 6 -4 0.27 0.13 8 6 -3 -0.1 0.17 8 6 -3 -0.01 0.1 8 6 -2 0.04 0.16 8 6 -2 0.07 0.1 8 6 -1 0.04 0.14 8 6 -1 0.19 0.1 8 6 0 0.01 0.14 8 6 1 0.18 0.12 8 7 -7 1.16 0.13 8 7 -6 0.5 0.1 8 7 -5 0.21 0.09 8 7 -4 -0.03 0.08 9 0 -9 -0.03 0.2 9 0 -8 0.12 0.22 9 0 -7 0.06 0.22 9 0 -5 0.01 0.24 9 0 -4 -0.02 0.25 9 0 -3 -0.04 0.1 9 0 -3 -0.11 0.22 9 0 -2 -0.05 0.1 9 0 -2 -0.01 0.18 9 0 -1 -0.02 0.09 9 -1 -10 0.08 0.09 9 1 -9 -0.01 0.1 9 -1 -9 0.01 0.1 9 1 -9 0.02 0.19 9 -1 -9 0.08 0.18 9 1 -8 0.12 0.11 9 -1 -8 0.2 0.12 9 -1 -8 -0.14 0.22 9 1 -7 -0.05 0.12 9 -1 -7 0.13 0.12 9 1 -7 0.11 0.22 9 -1 -7 -0.01 0.22 9 1 -6 0.4 0.13 9 -1 -6 0.24 0.14 9 1 -6 0.15 0.23 9 -1 -6 0.01 0.25 9 1 -5 0.11 0.12 9 -1 -5 0.26 0.13 9 1 -5 -0.19 0.24 9 -1 -5 -0.08 0.24 9 1 -4 0.13 0.12 9 -1 -4 0.11 0.13 9 1 -4 0.1 0.21 9 1 -3 0.04 0.11 9 -1 -3 0.11 0.12 9 1 -3 -0.09 0.19 9 -1 -3 -0.03 0.21 9 -1 -2 0.03 0.1 9 1 -2 -0.07 0.1 9 -1 -2 -0.03 0.11 9 -1 -2 0.2 0.19 9 -1 -1 -0.06 0.09 9 -2 -8 0.06 0.09 9 -2 -8 -0.13 0.17 9 2 -7 0.07 0.09 9 -2 -7 0.28 0.12 9 2 -7 -0.06 0.21 9 -2 -7 -0.22 0.22 9 2 -6 0.22 0.1 9 -2 -6 0.36 0.12 9 2 -6 -0.01 0.21 9 -2 -6 0.01 0.21 9 2 -5 0.06 0.1 9 -2 -5 0.13 0.11 9 2 -5 0.22 0.19 9 -2 -5 -0.01 0.22 9 2 -4 -0.01 0.1 9 -2 -4 0.07 0.11 9 -2 -4 0.03 0.21 9 -2 -3 0.13 0.1 9 -3 -5 0.05 0.18 9 -3 -4 0.01 0.18 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 118.53(16) . . ? C17 C1 C2 123.91(18) . . ? C17 C1 C14 117.53(19) . . ? C3 C2 C1 122.97(17) . . ? C15 C2 C1 119.15(16) . . ? C15 C2 C3 117.88(18) . . ? H3 C3 C2 115.0(13) . . ? C4 C3 C2 121.4(2) . . ? C4 C3 H3 123.6(13) . . ? H4 C4 C3 120.4(15) . . ? C5 C4 C3 122.1(2) . . ? C5 C4 H4 117.5(15) . . ? C6 C5 C4 122.0(3) . . ? C16 C5 C4 118.1(2) . . ? C16 C5 C6 119.9(3) . . ? H6 C6 C5 115.1(19) . . ? C7 C6 C5 120.5(4) . . ? C7 C6 H6 124.4(19) . . ? H7 C7 C6 123(2) . . ? C8 C7 C6 120.2(3) . . ? C8 C7 H7 117(2) . . ? H8 C8 C7 118.6(18) . . ? C9 C8 C7 121.0(3) . . ? C9 C8 H8 120.4(18) . . ? C10 C9 C8 122.0(3) . . ? C16 C9 C8 119.8(3) . . ? C16 C9 C10 118.2(2) . . ? H10 C10 C9 116.1(15) . . ? C11 C10 C9 121.9(2) . . ? C11 C10 H10 121.9(15) . . ? H11 C11 C10 122.4(15) . . ? C12 C11 C10 121.3(3) . . ? C12 C11 H11 116.2(15) . . ? C13 C12 C11 122.6(2) . . ? C15 C12 C11 118.8(2) . . ? C15 C12 C13 118.60(16) . . ? C14 C13 C12 118.95(18) . . ? C19 C13 C12 124.4(2) . . ? C19 C13 C14 116.6(2) . . ? C13 C14 C1 123.70(19) . . ? H14 C14 C1 118.8(11) . . ? H14 C14 C13 117.5(11) . . ? C12 C15 C2 121.07(16) . . ? C16 C15 C2 119.84(18) . . ? C16 C15 C12 119.09(17) . . ? C9 C16 C5 118.7(2) . . ? C15 C16 C5 120.62(19) . . ? C15 C16 C9 120.7(2) . . ? C1 C17 O1 123.0(3) . . ? C18 C17 O1 116.6(3) . . ? C18 C17 C1 120.4(2) . . ? H18a C18 C17 110(3) . . ? H18b C18 C17 110.4(19) . . ? H18b C18 H18a 106(3) . . ? H18c C18 C17 116(2) . . ? H18c C18 H18a 107(3) . . ? H18c C18 H18b 108(3) . . ? C13 C19 O2 121.3(4) . . ? C20 C19 O2 118.6(4) . . ? C20 C19 C13 119.9(3) . . ? H20a C20 C19 112(2) . . ? H20b C20 C19 103(2) . . ? H20b C20 H20a 107(3) . . ? H20c C20 C19 119(4) . . ? H20c C20 H20a 115(4) . . ? H20c C20 H20b 98(4) . . ? 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 1.189(4) . ? O2 C19 1.167(4) . ? C1 C2 1.414(2) . ? C1 C14 1.383(3) . ? C1 C17 1.483(3) . ? C2 C3 1.429(3) . ? C2 C15 1.426(2) . ? C3 H3 1.05(2) . ? C3 C4 1.355(3) . ? C4 H4 1.07(3) . ? C4 C5 1.421(3) . ? C5 C6 1.408(3) . ? C5 C16 1.406(3) . ? C6 H6 1.13(4) . ? C6 C7 1.378(5) . ? C7 H7 1.04(4) . ? C7 C8 1.376(5) . ? C8 H8 1.05(3) . ? C8 C9 1.393(4) . ? C9 C10 1.422(4) . ? C9 C16 1.416(3) . ? C10 H10 1.06(3) . ? C10 C11 1.344(4) . ? C11 H11 1.09(3) . ? C11 C12 1.435(3) . ? C12 C13 1.415(3) . ? C12 C15 1.420(3) . ? C13 C14 1.394(3) . ? C13 C19 1.492(3) . ? C14 H14 1.09(2) . ? C15 C16 1.429(3) . ? C17 C18 1.492(4) . ? C18 H18a 0.97(4) . ? C18 H18b 1.05(4) . ? C18 H18c 1.00(4) . ? C19 C20 1.495(5) . ? C20 H20a 1.03(4) . ? C20 H20b 1.10(5) . ? C20 H20c 1.05(7) . ? 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 -11.7(4) . . . . ? O1 C17 C1 C14 165.9(3) . . . . ? O2 C19 C13 C12 8.8(5) . . . . ? O2 C19 C13 C14 -168.3(4) . . . . ? C1 C2 C3 C4 178.85(19) . . . . ? C1 C2 C15 C12 -0.04(18) . . . . ? C1 C2 C15 C16 -178.66(15) . . . . ? C1 C14 C13 C12 -1.3(2) . . . . ? C1 C14 C13 C19 176.0(2) . . . . ? C2 C3 C4 C5 -0.1(2) . . . . ? C2 C15 C12 C11 179.92(17) . . . . ? C2 C15 C12 C13 -0.13(18) . . . . ? C2 C15 C16 C5 -0.26(18) . . . . ? C2 C15 C16 C9 178.46(15) . . . . ? C3 C4 C5 C6 -177.7(2) . . . . ? C3 C4 C5 C16 1.8(3) . . . . ? C4 C5 C6 C7 179.8(2) . . . . ? C4 C5 C16 C9 179.69(18) . . . . ? C4 C5 C16 C15 -1.6(2) . . . . ? C5 C6 C7 C8 0.3(3) . . . . ? C5 C16 C9 C8 0.7(2) . . . . ? C5 C16 C9 C10 -179.64(19) . . . . ? C5 C16 C15 C12 -178.92(16) . . . . ? C6 C7 C8 C9 -0.5(3) . . . . ? C7 C8 C9 C10 -179.7(3) . . . . ? C7 C8 C9 C16 -0.0(3) . . . . ? C8 C9 C10 C11 178.3(2) . . . . ? C8 C9 C16 C15 -178.07(18) . . . . ? C9 C10 C11 C12 -0.2(3) . . . . ? C9 C16 C15 C12 -0.2(2) . . . . ? C10 C11 C12 C13 -178.3(2) . . . . ? C10 C11 C12 C15 1.7(3) . . . . ? C11 C12 C13 C14 -179.29(18) . . . . ? C11 C12 C13 C19 3.6(2) . . . . ? C11 C12 C15 C16 -1.4(2) . . . . ? C12 C13 C19 C20 -166.1(3) . . . . ? 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 -5.0550 0.2631 1.4648 0.3500 -0.8971 -0.4973 -1.0956 -6.3033 6.8153 -0.1624 0.3224 -0.9745 5.0550 -0.2631 -1.4648 -0.3500 0.8971 0.4973 3.1052 5.1340 -6.0508 -0.0024 0.1359 1.0166 -0.8622 5.1282 7.1683 0.9128 0.1424 0.1132 1.8981 -3.0527 -10.1620 -0.9331 -0.1619 0.3000 -1.1671 -7.2007 -1.1167 -0.6768 -0.1361 -0.7419 -3.0470 1.2963 -4.6189 0.0161 -0.8870 0.0325 4.0804 -0.3133 4.5555 0.0220 1.0620 0.1575 2.9708 -4.3785 2.5477 -0.4135 0.8174 -0.2463 -3.9540 3.2537 5.4155 0.7919 -0.5175 -0.2752 2.8930 -5.2582 -6.3717 -0.9799 0.2996 0.0277 -1.1026 -0.7881 -10.7989 -0.6110 -0.8279 0.2657 -0.1650 -6.1290 -6.1174 -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 -0.00016(3) -0.000015(9) 0.000004(7) -0.000000(3) 0.000001(2) -0.000001(2) -0.000002(2) -0.0000005(11) 0.0000006(8) -0.0000000(9) O2 -0.000303(17) 0.000071(4) -0.000031(3) -0.0000125(16) 0.0000077(10) -0.0000038(10) 0.0000038(10) -0.0000009(5) 0.0000008(4) -0.0000001(5) 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 0.000004(6) 0.0000009(15) -0.0000003(11) 0.0000000(5) -0.0000001(3) 0.0000001(3) 0.0000001(2) 0.00000001(13) -0.00000003(10) -0.00000002(10) -0.00000001(18) 0.00000005(9) -0.00000007(6) -0.00000002(5) -0.00000002(6) O2 -0.000048(3) 0.0000080(7) -0.0000092(6) -0.0000017(3) 0.00000143(16) -0.00000139(15) 0.00000027(11) -0.00000023(6) 0.00000012(5) -0.00000009(5) -0.00000019(8) -0.00000004(4) 0.00000000(3) -0.00000004(2) 0.00000005(3)