#------------------------------------------------------------------------------ #$Date: 2024-08-05 21:03:11 +0300 (Mon, 05 Aug 2024) $ #$Revision: 293758 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/17/1571787.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1571787 loop_ _publ_author_name 'Giri, Rahul' 'Zhilin, Egor' 'Katayev, Dmitry' _publ_section_title ; Divergent functionalization of alkenes enabled by photoredox activation of CDFA and α-halo carboxylic acids. ; _journal_issue 27 _journal_name_full 'Chemical science' _journal_page_first 10659 _journal_page_last 10667 _journal_paper_doi 10.1039/d4sc01084a _journal_volume 15 _journal_year 2024 _chemical_absolute_configuration ad _chemical_formula_sum 'C18 H12 F2 O2' _chemical_formula_weight 298.28 _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _symmetry_cell_setting monoclinic _symmetry_Int_Tables_number 4 _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2023-10-02T14:24:07-00:00 _audit_update_record ; 2023-10-02 deposited with the CCDC. 2024-05-31 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 100.5648(17) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.05628(17) _cell_length_b 5.83820(12) _cell_length_c 23.8712(4) _cell_measurement_reflns_used 17569 _cell_measurement_temperature 173.01(10) _cell_measurement_theta_max 80.116 _cell_measurement_theta_min 3.771 _cell_volume 1377.73(4) _computing_cell_refinement 'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)' _computing_data_collection 'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)' _computing_data_reduction 'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 173.01(10) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 0.988 _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 -25.00 23.00 0.50 1.50 -- -49.99 17.00 88.00 96 2 \w -121.00 -45.00 0.50 1.50 -- -49.99 -17.00 -80.00 152 3 \w -21.00 25.00 0.50 1.50 -- 49.99 -17.00 -80.00 92 4 \w 46.00 122.00 0.50 1.50 -- 49.99 17.00 88.00 152 5 \w -161.00 -85.00 0.50 5.00 -- -90.00 -17.00 -80.00 152 6 \w -121.00 -38.00 0.50 1.50 -- -49.99 -57.00 150.00 166 7 \w -121.00 -38.00 0.50 1.50 -- -49.99 -57.00-180.00 166 8 \w -26.00 22.00 0.50 1.50 -- -49.99 19.00-120.00 96 9 \w -121.00 -30.00 0.50 1.50 -- -49.99 -77.00-150.00 182 10 \w 34.00 66.00 0.50 1.50 -- 49.99 77.00 150.00 64 11 \w 46.00 84.00 0.50 1.50 -- 49.99 38.00-180.00 76 12 \w 49.00 77.00 0.50 1.50 -- 49.99 38.00 150.00 56 13 \w 36.00 90.00 0.50 1.50 -- 49.99-125.00-150.00 108 14 \w 55.00 81.00 0.50 1.50 -- 49.99 19.00-180.00 52 15 \w 38.00 81.00 0.50 1.50 -- 49.99 57.00-120.00 86 16 \w -105.00 -74.00 0.50 5.00 -- -90.00 -77.00 -90.00 62 17 \w -105.00 -79.00 0.50 5.00 -- -90.00 -65.00-173.16 52 18 \w -140.00-114.00 0.50 5.00 -- -90.00 -77.00-150.00 52 19 \w -114.00 -78.00 0.50 5.00 -- -90.00 -61.00-120.00 72 20 \w -98.00 -72.00 0.50 5.00 -- -90.00 -72.00-120.41 52 21 \w -100.00 -74.00 0.50 5.00 -- -90.00 -67.00 175.07 52 22 \w -98.00 -72.00 0.50 5.00 -- -90.00 -77.00-150.00 52 23 \w -98.00 -73.00 0.50 5.00 -- -90.00 -71.00 139.01 50 24 \w -98.00 -72.00 0.50 5.00 -- -90.00 -77.00 150.00 52 25 \w -101.00 -75.00 0.50 5.00 -- -90.00 -66.00 179.51 52 26 \w -96.00 -70.00 0.50 5.00 -- -90.00 -77.00-120.00 52 27 \w -113.00 -79.00 0.50 5.00 -- -90.00 -61.00 150.00 68 28 \w -103.00 -77.00 0.50 5.00 -- -90.00 -61.00-161.40 52 29 \w -99.00 -74.00 0.50 5.00 -- -90.00 -67.00-155.10 50 30 \w -95.00 -70.00 0.50 5.00 -- -90.00 -77.00-180.00 50 31 \w -97.00 -70.00 0.50 5.00 -- -90.00 -77.00 136.45 54 32 \w -161.00-128.00 0.50 5.00 -- -90.00 -77.00 150.00 66 33 \w -101.00 -74.00 0.50 5.00 -- -90.00 -70.00 146.58 54 34 \w -106.00 -77.00 0.50 5.00 -- -90.00 -61.00 120.00 58 35 \w -110.00 -76.00 0.50 5.00 -- -90.00 -64.00-146.48 68 36 \w -108.00 -78.00 0.50 5.00 -- -90.00 -64.00-150.33 60 37 \w -106.00 -73.00 0.50 5.00 -- -90.00 -74.00-110.62 66 38 \w -101.00 -74.00 0.50 5.00 -- -90.00 -69.00 150.48 54 39 \w -100.00 -73.00 0.50 5.00 -- -90.00 -73.00 126.28 54 40 \w -101.00 -74.00 0.50 5.00 -- -90.00 -69.00 153.75 54 41 \w 98.00 178.00 0.50 5.00 -- 111.50 77.00-150.00 160 42 \w 92.00 147.00 0.50 5.00 -- 111.50 77.00 150.00 110 43 \w 120.00 172.00 0.50 5.00 -- 111.50 30.00-180.00 104 44 \w 152.00 177.00 0.50 5.00 -- 111.50 45.00 60.00 50 45 \w 81.00 114.00 0.50 5.00 -- 111.50-131.00 56.96 66 46 \w 44.00 76.00 0.50 5.00 -- 111.50-131.00 56.96 64 47 \w 150.00 177.00 0.50 5.00 -- 111.50 45.00 90.00 54 48 \w 45.00 71.00 0.50 5.00 -- 111.50 -61.00 0.00 52 49 \w 103.00 146.00 0.50 5.00 -- 111.50 61.00-120.00 86 50 \w 41.00 66.00 0.50 5.00 -- 111.50 -61.00-120.00 50 51 \w 45.00 71.00 0.50 5.00 -- 111.50 -61.00 -30.00 52 52 \w 42.00 71.00 0.50 5.00 -- 111.50 -61.00 90.00 58 53 \w 147.00 178.00 0.50 5.00 -- 111.50 61.00-180.00 62 54 \w 98.00 125.00 0.50 5.00 -- 111.50 61.00-180.00 54 55 \w 103.00 148.00 0.50 5.00 -- 111.50 61.00 120.00 90 56 \w 93.00 174.00 0.50 5.00 -- 111.50 77.00 120.00 162 57 \w 79.00 105.00 0.50 5.00 -- 111.50 -77.00 60.00 52 58 \w 43.00 69.00 0.50 5.00 -- 111.50 -61.00 -90.00 52 59 \w 78.00 104.00 0.50 5.00 -- 111.50 -77.00 0.00 52 60 \w 70.00 117.00 0.50 5.00 -- 111.50-132.00-178.80 94 61 \w 41.00 67.00 0.50 5.00 -- 111.50 -77.00 60.00 52 62 \w 75.00 111.00 0.50 5.00 -- 111.50-125.00-150.00 72 63 \w 43.00 70.00 0.50 5.00 -- 111.50 -61.00 120.00 54 64 \w 108.00 136.00 0.50 5.00 -- 111.50 61.00-150.00 56 65 \w 123.00 175.00 0.50 5.00 -- 111.50 45.00 -60.00 104 66 \w 141.00 177.00 0.50 5.00 -- 111.50 77.00-180.00 72 67 \w 81.00 106.00 0.50 5.00 -- 111.50 -94.00-180.00 50 68 \w 51.00 77.00 0.50 5.00 -- 111.50 -94.00-180.00 52 69 \w 92.00 133.00 0.50 5.00 -- 111.50 77.00-180.00 82 70 \w 47.00 73.00 0.50 5.00 -- 111.50-125.00-150.00 52 71 \w 130.00 156.00 0.50 5.00 -- 111.50 77.00-120.00 52 72 \w 97.00 123.00 0.50 5.00 -- 111.50 77.00 90.00 52 73 \w 92.00 123.00 0.50 5.00 -- 111.50 77.00-120.00 62 74 \w 43.00 71.00 0.50 5.00 -- 111.50 -61.00-180.00 56 75 \w 41.00 71.00 0.50 5.00 -- 111.50 -61.00 -60.00 60 76 \w 70.00 108.00 0.50 5.00 -- 111.50-125.00 120.00 76 77 \w 147.00 173.00 0.50 5.00 -- 111.50 17.00 88.00 52 78 \w 113.00 139.00 0.50 5.00 -- 111.50 17.00 88.00 52 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.126752 _diffrn_orient_matrix_UB_12 -0.0592391 _diffrn_orient_matrix_UB_13 -0.0248744 _diffrn_orient_matrix_UB_21 -0.0864794 _diffrn_orient_matrix_UB_22 -0.0053985 _diffrn_orient_matrix_UB_23 -0.060367 _diffrn_orient_matrix_UB_31 0.0272812 _diffrn_orient_matrix_UB_32 0.2570798 _diffrn_orient_matrix_UB_33 -0.0068588 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_unetI/netI 0.0381 _diffrn_reflns_Laue_measured_fraction_full 1 _diffrn_reflns_Laue_measured_fraction_max 0.988 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 28713 _diffrn_reflns_point_group_measured_fraction_full 0.986 _diffrn_reflns_point_group_measured_fraction_max 0.949 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 80.686 _diffrn_reflns_theta_min 3.767 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 0.938 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_correction_T_min 0.898 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.42.89a (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 colourless _exptl_crystal_density_diffrn 1.438 _exptl_crystal_description block _exptl_crystal_F_000 616 _exptl_crystal_size_max 0.118 _exptl_crystal_size_mid 0.084 _exptl_crystal_size_min 0.056 _refine_diff_density_max 0.201 _refine_diff_density_min -0.17 _refine_diff_density_rms 0.045 _refine_ls_abs_structure_details ; Flack x determined using 2145 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.01(11) _refine_ls_extinction_coef 0.0043(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 597 _refine_ls_number_reflns 5747 _refine_ls_number_restraints 497 _refine_ls_restrained_S_all 1.039 _refine_ls_R_factor_all 0.0412 _refine_ls_R_factor_gt 0.0386 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0592P)^2^+0.2780P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1097 _refine_ls_wR_factor_ref 0.1114 _reflns_Friedel_coverage 0.747 _reflns_Friedel_fraction_full 0.969 _reflns_Friedel_fraction_max 0.902 _reflns_number_gt 5224 _reflns_number_total 5747 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc01084a2.cif _cod_data_source_block 23DK001_RG-41 _cod_depositor_comments 'Adding full bibliography for 1571787.cif.' _cod_original_cell_volume 1377.74(4) _cod_original_sg_symbol_H-M 'P 21' _cod_database_code 1571787 _shelx_estimated_absorpt_t_min 0.897 _shelx_estimated_absorpt_t_max 0.949 _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling - B-factor correction ; _oxdiff_exptl_absorpt_empirical_full_max 1.199 _oxdiff_exptl_absorpt_empirical_full_min 0.826 _shelx_shelxl_version_number 2018/3 _shelx_res_file ; TITL 23dk001_rg-41_a.res in P2(1) shelx.res created by SHELXL-2018/3 at 14:23:21 on 02-Oct-2023 REM Old TITL 23DK001_RG-41 in P2(1) REM SHELXT solution in P2(1): R1 0.159, Rweak 0.005, Alpha 0.001 REM 8.816 for 4 systematic absences, Orientation as input REM Flack x = -0.030 ( 0.086 ) from 2123 Parsons' quotients REM Formula found by SHELXT: C36 O1A F5 CELL 1.54184 10.056279 5.838205 23.871214 90 100.5648 90 ZERR 4 0.000166 0.000117 0.000419 0 0.0017 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H F O UNIT 72 48 8 8 RIGU 0.001 0.001 C1B > O2B RIGU 0.001 0.001 C1A > O2A ISOR 0.01 0.02 C2A C7A C6A C5A C4A C3A C1A C8A C9A C10A C11A C12A C13A C14A = C15A C16A C17A C18A O1A O2A F2A F1A ISOR 0.01 0.02 C16B C18B O2B O1B C17B F1B F2B ISOR 0.002 0.02 C1B L.S. 40 0 0 PLAN 20 SIZE 0.056 0.084 0.118 TEMP -100 CONF list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.059200 0.278000 EXTI 0.004308 FVAR 5.74930 0.85150 C2B 1 0.991198 0.800472 0.140799 11.00000 0.02725 0.04201 = 0.02792 0.00418 0.00649 0.00172 C3B 1 1.047120 0.984030 0.174115 11.00000 0.03142 0.04910 = 0.03082 -0.00039 0.00351 -0.00022 AFIX 43 H3B 2 0.989218 1.095183 0.186067 11.00000 -1.20000 AFIX 0 C4B 1 1.186472 1.007383 0.190200 11.00000 0.03361 0.05678 = 0.03549 0.00272 0.00286 -0.00738 AFIX 43 H4B 2 1.223225 1.136906 0.211711 11.00000 -1.20000 AFIX 0 C5B 1 1.271473 0.842341 0.174915 11.00000 0.02652 0.07073 = 0.03705 0.01042 0.00506 -0.00256 AFIX 43 H5B 2 1.366662 0.855915 0.186602 11.00000 -1.20000 AFIX 0 C6B 1 1.216946 0.656689 0.142394 11.00000 0.02997 0.05808 = 0.03721 0.00950 0.01136 0.00812 AFIX 43 H6B 2 1.275762 0.542137 0.132599 11.00000 -1.20000 AFIX 0 C7B 1 1.076580 0.633866 0.123549 11.00000 0.02965 0.04447 = 0.03055 0.00849 0.01041 0.00640 C8B 1 1.031171 0.437549 0.087159 11.00000 0.03788 0.04347 = 0.04136 0.00398 0.01789 0.00951 AFIX 43 H8B 2 1.090519 0.309569 0.091889 11.00000 -1.20000 AFIX 0 C9B 1 0.918450 0.411061 0.048151 11.00000 0.04307 0.03847 = 0.03653 -0.00216 0.01534 0.00254 AFIX 43 H9B 2 0.907343 0.266174 0.029772 11.00000 -1.20000 AFIX 0 C10B 1 0.810064 0.577327 0.030232 11.00000 0.03243 0.04119 = 0.03092 -0.00184 0.01026 -0.00225 C11B 1 0.736833 0.557506 -0.025420 11.00000 0.04271 0.04803 = 0.03097 -0.00494 0.01199 -0.00721 AFIX 43 H11B 2 0.753916 0.430955 -0.048096 11.00000 -1.20000 AFIX 0 C12B 1 0.640539 0.716739 -0.048228 11.00000 0.03879 0.06142 = 0.02867 0.00014 0.00331 -0.01228 AFIX 43 H12B 2 0.592489 0.699826 -0.086155 11.00000 -1.20000 AFIX 0 C13B 1 0.614562 0.900487 -0.015598 11.00000 0.03663 0.05378 = 0.03401 0.00579 0.00125 0.00064 AFIX 43 H13B 2 0.550263 1.013083 -0.031353 11.00000 -1.20000 AFIX 0 C14B 1 0.682706 0.920898 0.040513 11.00000 0.03128 0.04272 = 0.03508 0.00034 0.00361 0.00168 AFIX 43 H14B 2 0.664050 1.047649 0.062802 11.00000 -1.20000 AFIX 0 C15B 1 0.778018 0.757910 0.064501 11.00000 0.02760 0.04088 = 0.02809 -0.00083 0.00645 -0.00090 C1B 1 0.838586 0.765832 0.128077 11.00000 0.02717 0.03878 = 0.02922 -0.00433 0.00696 0.00302 C16B 1 0.794471 0.557415 0.160806 11.00000 0.03018 0.05177 = 0.02858 0.00071 0.00921 0.00008 AFIX 23 H16A 2 0.782950 0.418321 0.136679 11.00000 -1.20000 H16B 2 0.860797 0.525639 0.196014 11.00000 -1.20000 AFIX 0 C17B 1 0.661736 0.636849 0.174226 11.00000 0.02521 0.07030 = 0.02539 -0.00653 0.00566 -0.00606 C18B 1 0.672489 0.897602 0.176072 11.00000 0.02287 0.07019 = 0.03573 -0.01787 0.00237 0.00093 F1B 3 0.632635 0.555570 0.223593 11.00000 0.03620 0.10848 = 0.03035 0.00149 0.01340 -0.00766 F2B 3 0.554396 0.578605 0.132627 11.00000 0.02995 0.07292 = 0.03676 -0.00990 -0.00008 -0.01044 O1B 4 0.777946 0.961656 0.152470 11.00000 0.02826 0.04934 = 0.03591 -0.01205 0.00492 0.00493 O2B 4 0.600851 1.029852 0.194525 11.00000 0.03026 0.08855 = 0.06660 -0.03494 0.01168 0.00477 PART 1 C1 1 0.660884 0.324580 0.374086 21.00000 0.02564 0.03388 = 0.02688 0.00052 0.00733 -0.00380 C2 1 0.507716 0.353589 0.360811 21.00000 0.02658 0.03922 = 0.02724 -0.00494 0.00843 -0.00083 C3 1 0.449634 0.535015 0.327671 21.00000 0.03105 0.04926 = 0.02821 0.00210 0.00403 0.00122 AFIX 43 H3 2 0.506176 0.650735 0.316725 21.00000 -1.20000 AFIX 0 C4 1 0.310400 0.551164 0.310122 21.00000 0.03249 0.05759 = 0.03253 0.00314 0.00347 0.00839 AFIX 43 H4 2 0.272390 0.678981 0.288244 21.00000 -1.20000 AFIX 0 C5 1 0.227490 0.381453 0.324502 21.00000 0.02519 0.06661 = 0.03721 -0.00583 0.00463 0.00132 AFIX 43 H5 2 0.132343 0.390496 0.312027 21.00000 -1.20000 AFIX 0 C6 1 0.283579 0.197662 0.357230 21.00000 0.02943 0.05610 = 0.03806 -0.00560 0.01246 -0.00807 AFIX 43 H6 2 0.226103 0.079395 0.366229 21.00000 -1.20000 AFIX 0 C7 1 0.423809 0.182217 0.377448 21.00000 0.02943 0.04478 = 0.03080 -0.00871 0.01117 -0.00382 C8 1 0.471104 -0.012470 0.413552 21.00000 0.03849 0.04407 = 0.04489 -0.00264 0.01914 -0.00930 AFIX 43 H8 2 0.413218 -0.142338 0.408523 21.00000 -1.20000 AFIX 0 C9 1 0.583872 -0.037052 0.452873 21.00000 0.04414 0.03794 = 0.03994 0.00497 0.01750 0.00119 AFIX 43 H9 2 0.595402 -0.182080 0.471168 21.00000 -1.20000 AFIX 0 C10 1 0.691189 0.129249 0.471295 21.00000 0.03269 0.03780 = 0.03279 0.00066 0.01169 0.00337 C11 1 0.766596 0.107305 0.526631 21.00000 0.04195 0.05157 = 0.02951 0.00774 0.01187 0.00832 AFIX 43 H11 2 0.751196 -0.021628 0.548867 21.00000 -1.20000 AFIX 0 C12 1 0.862243 0.266444 0.549818 21.00000 0.03911 0.06037 = 0.02739 -0.00135 0.00219 0.01299 AFIX 43 H12 2 0.910928 0.248062 0.587595 21.00000 -1.20000 AFIX 0 C13 1 0.886540 0.452780 0.517575 21.00000 0.03570 0.05768 = 0.03047 -0.00466 0.00158 0.00117 AFIX 43 H13 2 0.950691 0.565470 0.533412 21.00000 -1.20000 AFIX 0 C14 1 0.817225 0.475271 0.462064 21.00000 0.03131 0.04246 = 0.03130 -0.00347 0.00328 -0.00031 AFIX 43 H14 2 0.834946 0.604000 0.440222 21.00000 -1.20000 AFIX 0 C15 1 0.722234 0.313821 0.437509 21.00000 0.02914 0.04047 = 0.02565 0.00131 0.00729 0.00300 C16 1 0.707586 0.122784 0.339867 21.00000 0.02795 0.04118 = 0.02957 -0.00080 0.00893 -0.00173 AFIX 23 H16C 2 0.721536 -0.018600 0.363101 21.00000 -1.20000 H16D 2 0.641199 0.091909 0.304621 21.00000 -1.20000 AFIX 0 C17 1 0.839055 0.210548 0.326468 21.00000 0.02470 0.04806 = 0.02338 0.00171 0.00532 0.00089 C18 1 0.825088 0.470373 0.327041 21.00000 0.02288 0.04776 = 0.02813 0.00340 0.00284 -0.00413 F1 3 0.866432 0.139795 0.275909 21.00000 0.03681 0.06196 = 0.03177 -0.00163 0.01565 -0.00020 F2 3 0.947910 0.149622 0.366862 21.00000 0.02670 0.06097 = 0.03756 0.00701 0.00063 0.00575 O1 4 0.718728 0.527043 0.350899 21.00000 0.02835 0.03805 = 0.03085 0.00400 0.00680 -0.00418 O2 4 0.895065 0.609221 0.309419 21.00000 0.03288 0.05441 = 0.05056 0.00807 0.01200 -0.01087 SAME C1 > O2 PART 2 C1A 1 0.660533 0.232288 0.371211 -21.00000 0.03171 0.03305 = 0.02782 -0.00088 0.00318 -0.00166 C2A 1 0.508038 0.266726 0.359332 -21.00000 0.03192 0.02725 = 0.02111 -0.00470 0.00089 -0.00332 C3A 1 0.451868 0.444129 0.324973 -21.00000 0.03344 0.03682 = 0.03626 0.00700 0.00558 0.00040 AFIX 43 H3A 2 0.508635 0.549093 0.310067 -21.00000 -1.20000 AFIX 0 C4A 1 0.311114 0.470072 0.311962 -21.00000 0.03344 0.03956 = 0.04406 0.00785 0.00545 0.00201 AFIX 43 H4A 2 0.273740 0.605076 0.293136 -21.00000 -1.20000 AFIX 0 C5A 1 0.226383 0.304488 0.325870 -21.00000 0.03259 0.03598 = 0.02580 -0.00265 0.00887 0.00233 AFIX 43 H5A 2 0.131318 0.315826 0.313411 -21.00000 -1.20000 AFIX 0 C6A 1 0.282497 0.118762 0.358711 -21.00000 0.03296 0.03648 = 0.03340 0.00033 0.00424 -0.00215 AFIX 43 H6A 2 0.225242 0.004452 0.369780 -21.00000 -1.20000 AFIX 0 C7A 1 0.424384 0.100308 0.375554 -21.00000 0.03270 0.02340 = 0.01923 -0.00933 0.00470 -0.00262 C8A 1 0.467926 -0.086067 0.414204 -21.00000 0.03270 0.03197 = 0.02869 0.00009 0.00941 -0.00097 AFIX 43 H8A 2 0.403898 -0.206590 0.412698 -21.00000 -1.20000 AFIX 0 C9A 1 0.582551 -0.119696 0.451869 -21.00000 0.03110 0.03008 = 0.02647 0.00155 0.01161 -0.00024 AFIX 43 H9A 2 0.594308 -0.266696 0.469133 -21.00000 -1.20000 AFIX 0 C10A 1 0.689477 0.042768 0.468908 -21.00000 0.02988 0.02960 = 0.02742 -0.00249 0.01078 0.00172 C11A 1 0.758102 0.023919 0.525608 -21.00000 0.03601 0.03925 = 0.03006 0.00225 0.00706 -0.00297 AFIX 43 H11A 2 0.735184 -0.095882 0.549042 -21.00000 -1.20000 AFIX 0 C12A 1 0.857342 0.176113 0.547306 -21.00000 0.03248 0.03623 = 0.03295 -0.00193 0.00523 0.00215 AFIX 43 H12A 2 0.907704 0.152888 0.584611 -21.00000 -1.20000 AFIX 0 C13A 1 0.885754 0.361397 0.516429 -21.00000 0.03665 0.03777 = 0.03368 -0.00260 -0.00084 -0.00621 AFIX 43 H13A 2 0.950146 0.472231 0.533145 -21.00000 -1.20000 AFIX 0 C14A 1 0.817539 0.386222 0.458824 -21.00000 0.02461 0.03124 = 0.03179 -0.00329 0.00443 -0.00042 AFIX 43 H14A 2 0.836938 0.512136 0.436428 -21.00000 -1.20000 AFIX 0 C15A 1 0.721806 0.222231 0.435964 -21.00000 0.02124 0.03027 = 0.02766 -0.00199 0.00555 0.00061 C16A 1 0.703583 0.016854 0.339565 -21.00000 0.03496 0.03930 = 0.02346 -0.00030 0.00686 0.00135 AFIX 23 H16E 2 0.714674 -0.119668 0.364588 -21.00000 -1.20000 H16F 2 0.637127 -0.017454 0.304563 -21.00000 -1.20000 AFIX 0 C17A 1 0.836572 0.093497 0.325777 -21.00000 0.03334 0.04790 = 0.02959 0.00626 0.00681 0.00268 C18A 1 0.826732 0.354000 0.322933 -21.00000 0.02547 0.04771 = 0.03538 0.00802 0.00007 -0.00118 F1A 3 0.864098 0.007537 0.276745 -21.00000 0.04094 0.06929 = 0.03355 0.00181 0.01207 0.00840 F2A 3 0.942722 0.030604 0.367522 -21.00000 0.03987 0.05531 = 0.04206 0.00623 -0.00143 0.00787 O1A 4 0.720566 0.426976 0.346929 -21.00000 0.02920 0.04040 = 0.03602 0.00831 0.00176 -0.00011 O2A 4 0.899072 0.485927 0.304282 -21.00000 0.03586 0.05629 = 0.06469 0.01839 0.01170 -0.00304 HKLF 4 REM 23dk001_rg-41_a.res in P2(1) REM wR2 = 0.1114, GooF = S = 1.065, Restrained GooF = 1.039 for all data REM R1 = 0.0386 for 5224 Fo > 4sig(Fo) and 0.0412 for all 5747 data REM 597 parameters refined using 497 restraints END WGHT 0.0752 0.1166 REM Highest difference peak 0.201, deepest hole -0.170, 1-sigma level 0.045 Q1 1 0.6571 1.2557 0.1798 11.00000 0.05 0.20 Q2 1 0.6823 0.7721 0.1809 11.00000 0.05 0.19 Q3 1 0.9286 0.7950 0.1395 11.00000 0.05 0.18 Q4 1 0.8886 0.2541 0.0029 11.00000 0.05 0.17 Q5 1 0.5749 0.3075 0.3596 11.00000 0.05 0.17 Q6 1 0.6046 0.7647 0.1386 11.00000 0.05 0.16 Q7 1 0.4770 0.5041 0.3600 11.00000 0.05 0.16 Q8 1 0.8367 0.8075 0.3192 11.00000 0.05 0.16 Q9 1 1.0153 0.8302 0.1586 11.00000 0.05 0.15 Q10 1 1.0015 1.1712 0.1429 11.00000 0.05 0.15 Q11 1 0.9009 0.3014 0.3590 11.00000 0.05 0.15 Q12 1 0.6150 -0.1747 0.4980 11.00000 0.05 0.15 Q13 1 0.7747 0.1810 0.3255 11.00000 0.05 0.15 Q14 1 0.8565 0.4797 0.0369 11.00000 0.05 0.15 Q15 1 0.7919 0.5914 0.0039 11.00000 0.05 0.15 Q16 1 0.4767 0.3186 0.3434 11.00000 0.05 0.14 Q17 1 0.0208 0.3174 0.3418 11.00000 0.05 0.14 Q18 1 0.9018 0.3872 0.3448 11.00000 0.05 0.14 Q19 1 0.7158 0.5767 0.1663 11.00000 0.05 0.14 Q20 1 1.4810 0.7809 0.1591 11.00000 0.05 0.14 ; _shelx_res_checksum 7451 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C2B C 0.9912(2) 0.8005(5) 0.14080(9) 0.0322(5) Uani 1 1 d . . . . . C3B C 1.0471(2) 0.9840(6) 0.17411(10) 0.0374(6) Uani 1 1 d . . . . . H3B H 0.989218 1.095183 0.186067 0.045 Uiso 1 1 calc R U . . . C4B C 1.1865(2) 1.0074(6) 0.19020(11) 0.0424(6) Uani 1 1 d . . . . . H4B H 1.223225 1.136906 0.211711 0.051 Uiso 1 1 calc R U . . . C5B C 1.2715(2) 0.8423(7) 0.17491(11) 0.0449(7) Uani 1 1 d . . . . . H5B H 1.366662 0.855915 0.186602 0.054 Uiso 1 1 calc R U . . . C6B C 1.2169(2) 0.6567(6) 0.14239(10) 0.0411(6) Uani 1 1 d . . . . . H6B H 1.275762 0.542137 0.132599 0.049 Uiso 1 1 calc R U . . . C7B C 1.0766(2) 0.6339(5) 0.12355(10) 0.0343(5) Uani 1 1 d . . . . . C8B C 1.0312(2) 0.4375(6) 0.08716(11) 0.0396(6) Uani 1 1 d . . . . . H8B H 1.090519 0.309569 0.091889 0.047 Uiso 1 1 calc R U . . . C9B C 0.9184(3) 0.4111(5) 0.04815(10) 0.0383(6) Uani 1 1 d . . . . . H9B H 0.907343 0.266174 0.029772 0.046 Uiso 1 1 calc R U . . . C10B C 0.8101(2) 0.5773(5) 0.03023(10) 0.0343(6) Uani 1 1 d . . . . . C11B C 0.7368(3) 0.5575(6) -0.02542(10) 0.0399(6) Uani 1 1 d . . . . . H11B H 0.753916 0.430955 -0.048096 0.048 Uiso 1 1 calc R U . . . C12B C 0.6405(3) 0.7167(6) -0.04823(10) 0.0433(7) Uani 1 1 d . . . . . H12B H 0.592489 0.699826 -0.086155 0.052 Uiso 1 1 calc R U . . . C13B C 0.6146(3) 0.9005(6) -0.01560(11) 0.0421(6) Uani 1 1 d . . . . . H13B H 0.550263 1.013083 -0.031353 0.051 Uiso 1 1 calc R U . . . C14B C 0.6827(2) 0.9209(6) 0.04051(10) 0.0367(6) Uani 1 1 d . . . . . H14B H 0.66405 1.047649 0.062802 0.044 Uiso 1 1 calc R U . . . C15B C 0.7780(2) 0.7579(5) 0.06450(9) 0.0320(5) Uani 1 1 d . . . . . C1B C 0.8386(2) 0.7658(5) 0.12808(9) 0.0315(5) Uani 1 1 d . U . . . C16B C 0.7945(2) 0.5574(6) 0.16081(10) 0.0364(6) Uani 1 1 d . U . . . H16A H 0.78295 0.418321 0.136679 0.044 Uiso 1 1 calc R U . . . H16B H 0.860797 0.525639 0.196014 0.044 Uiso 1 1 calc R U . . . C17B C 0.6617(2) 0.6368(6) 0.17423(10) 0.0402(6) Uani 1 1 d . U . . . C18B C 0.6725(2) 0.8976(7) 0.17607(11) 0.0433(6) Uani 1 1 d . U . . . F1B F 0.63264(15) 0.5556(6) 0.22359(6) 0.0574(6) Uani 1 1 d . U . . . F2B F 0.55440(14) 0.5786(5) 0.13263(6) 0.0473(5) Uani 1 1 d . U . . . O1B O 0.77795(16) 0.9617(4) 0.15247(7) 0.0380(5) Uani 1 1 d . U . . . O2B O 0.60085(18) 1.0299(6) 0.19452(10) 0.0614(7) Uani 1 1 d . U . . . C1 C 0.6609(3) 0.3246(6) 0.37409(12) 0.0285(7) Uani 0.851(9) 1 d D . P A 1 C2 C 0.5077(3) 0.3536(7) 0.36081(16) 0.0306(8) Uani 0.851(9) 1 d D . P A 1 C3 C 0.4496(3) 0.5350(8) 0.32767(17) 0.0363(9) Uani 0.851(9) 1 d D . P A 1 H3 H 0.506176 0.650735 0.316725 0.044 Uiso 0.851(9) 1 calc R U P A 1 C4 C 0.3104(4) 0.5512(9) 0.3101(2) 0.0412(11) Uani 0.851(9) 1 d D . P A 1 H4 H 0.27239 0.678981 0.288244 0.049 Uiso 0.851(9) 1 calc R U P A 1 C5 C 0.2275(4) 0.3815(9) 0.3245(3) 0.0431(12) Uani 0.851(9) 1 d D . P A 1 H5 H 0.132343 0.390496 0.312027 0.052 Uiso 0.851(9) 1 calc R U P A 1 C6 C 0.2836(4) 0.1977(9) 0.3572(2) 0.0404(12) Uani 0.851(9) 1 d D . P A 1 H6 H 0.226103 0.079395 0.366229 0.048 Uiso 0.851(9) 1 calc R U P A 1 C7 C 0.4238(4) 0.1822(7) 0.37745(18) 0.0343(10) Uani 0.851(9) 1 d D . P A 1 C8 C 0.4711(4) -0.0125(8) 0.4136(2) 0.0410(11) Uani 0.851(9) 1 d D . P A 1 H8 H 0.413218 -0.142338 0.408523 0.049 Uiso 0.851(9) 1 calc R U P A 1 C9 C 0.5839(4) -0.0371(8) 0.4529(2) 0.0394(10) Uani 0.851(9) 1 d D . P A 1 H9 H 0.595402 -0.18208 0.471168 0.047 Uiso 0.851(9) 1 calc R U P A 1 C10 C 0.6912(4) 0.1292(7) 0.47130(15) 0.0337(8) Uani 0.851(9) 1 d D . P A 1 C11 C 0.7666(5) 0.1073(8) 0.52663(16) 0.0403(11) Uani 0.851(9) 1 d D . P A 1 H11 H 0.751196 -0.021628 0.548867 0.048 Uiso 0.851(9) 1 calc R U P A 1 C12 C 0.8622(5) 0.2664(9) 0.54982(17) 0.0428(11) Uani 0.851(9) 1 d D . P A 1 H12 H 0.910928 0.248062 0.587595 0.051 Uiso 0.851(9) 1 calc R U P A 1 C13 C 0.8865(4) 0.4528(9) 0.51758(16) 0.0419(10) Uani 0.851(9) 1 d D . P A 1 H13 H 0.950691 0.56547 0.533412 0.05 Uiso 0.851(9) 1 calc R U P A 1 C14 C 0.8172(4) 0.4753(7) 0.46206(15) 0.0353(9) Uani 0.851(9) 1 d D . P A 1 H14 H 0.834946 0.604 0.440222 0.042 Uiso 0.851(9) 1 calc R U P A 1 C15 C 0.7222(4) 0.3138(7) 0.43751(12) 0.0315(8) Uani 0.851(9) 1 d D . P A 1 C16 C 0.7076(3) 0.1228(7) 0.33987(13) 0.0324(8) Uani 0.851(9) 1 d D . P A 1 H16C H 0.721536 -0.0186 0.363101 0.039 Uiso 0.851(9) 1 calc R U P A 1 H16D H 0.641199 0.091909 0.304621 0.039 Uiso 0.851(9) 1 calc R U P A 1 C17 C 0.8391(3) 0.2105(8) 0.32647(11) 0.0319(8) Uani 0.851(9) 1 d D . P A 1 C18 C 0.8251(3) 0.4704(7) 0.32704(12) 0.0332(8) Uani 0.851(9) 1 d D . P A 1 F1 F 0.8664(2) 0.1398(5) 0.27591(8) 0.0423(8) Uani 0.851(9) 1 d D . P A 1 F2 F 0.94791(19) 0.1496(5) 0.36686(9) 0.0424(8) Uani 0.851(9) 1 d D . P A 1 O1 O 0.7187(2) 0.5270(5) 0.35090(11) 0.0322(6) Uani 0.851(9) 1 d D . P A 1 O2 O 0.8951(2) 0.6092(6) 0.30942(12) 0.0454(8) Uani 0.851(9) 1 d D . P A 1 C1A C 0.6605(16) 0.232(4) 0.3712(7) 0.031(3) Uani 0.149(9) 1 d D U P A 2 C2A C 0.5080(16) 0.267(4) 0.3593(9) 0.027(3) Uani 0.149(9) 1 d D U P A 2 C3A C 0.452(2) 0.444(4) 0.3250(11) 0.036(5) Uani 0.149(9) 1 d D U P A 2 H3A H 0.508635 0.549093 0.310067 0.043 Uiso 0.149(9) 1 calc R U P A 2 C4A C 0.311(2) 0.470(5) 0.3120(15) 0.039(5) Uani 0.149(9) 1 d D U P A 2 H4A H 0.27374 0.605076 0.293136 0.047 Uiso 0.149(9) 1 calc R U P A 2 C5A C 0.226(3) 0.304(4) 0.3259(15) 0.031(4) Uani 0.149(9) 1 d D U P A 2 H5A H 0.131318 0.315826 0.313411 0.037 Uiso 0.149(9) 1 calc R U P A 2 C6A C 0.282(2) 0.119(4) 0.3587(15) 0.035(5) Uani 0.149(9) 1 d D U P A 2 H6A H 0.225242 0.004452 0.36978 0.041 Uiso 0.149(9) 1 calc R U P A 2 C7A C 0.4244(19) 0.100(3) 0.3756(9) 0.025(4) Uani 0.149(9) 1 d D U P A 2 C8A C 0.468(2) -0.086(4) 0.4142(12) 0.031(4) Uani 0.149(9) 1 d D U P A 2 H8A H 0.403898 -0.20659 0.412698 0.037 Uiso 0.149(9) 1 calc R U P A 2 C9A C 0.583(2) -0.120(4) 0.4519(10) 0.028(4) Uani 0.149(9) 1 d D U P A 2 H9A H 0.594308 -0.266696 0.469133 0.034 Uiso 0.149(9) 1 calc R U P A 2 C10A C 0.689(2) 0.043(4) 0.4689(8) 0.028(4) Uani 0.149(9) 1 d D U P A 2 C11A C 0.758(3) 0.024(4) 0.5256(9) 0.035(5) Uani 0.149(9) 1 d D U P A 2 H11A H 0.735184 -0.095882 0.549042 0.042 Uiso 0.149(9) 1 calc R U P A 2 C12A C 0.857(3) 0.176(4) 0.5473(10) 0.034(5) Uani 0.149(9) 1 d D U P A 2 H12A H 0.907704 0.152888 0.584611 0.041 Uiso 0.149(9) 1 calc R U P A 2 C13A C 0.886(3) 0.361(4) 0.5164(10) 0.037(5) Uani 0.149(9) 1 d D U P A 2 H13A H 0.950146 0.472231 0.533145 0.044 Uiso 0.149(9) 1 calc R U P A 2 C14A C 0.818(2) 0.386(4) 0.4588(8) 0.029(4) Uani 0.149(9) 1 d D U P A 2 H14A H 0.836938 0.512136 0.436428 0.035 Uiso 0.149(9) 1 calc R U P A 2 C15A C 0.7218(19) 0.222(4) 0.4360(7) 0.026(3) Uani 0.149(9) 1 d D U P A 2 C16A C 0.7036(17) 0.017(4) 0.3396(7) 0.032(3) Uani 0.149(9) 1 d D U P A 2 H16E H 0.714674 -0.119668 0.364588 0.039 Uiso 0.149(9) 1 calc R U P A 2 H16F H 0.637127 -0.017454 0.304563 0.039 Uiso 0.149(9) 1 calc R U P A 2 C17A C 0.8366(16) 0.093(5) 0.3258(7) 0.037(3) Uani 0.149(9) 1 d D U P A 2 C18A C 0.8267(16) 0.354(5) 0.3229(8) 0.037(3) Uani 0.149(9) 1 d D U P A 2 F1A F 0.8641(13) 0.008(5) 0.2767(5) 0.047(4) Uani 0.149(9) 1 d D U P A 2 F2A F 0.9427(13) 0.031(4) 0.3675(6) 0.047(4) Uani 0.149(9) 1 d D U P A 2 O1A O 0.7206(14) 0.427(4) 0.3469(7) 0.036(3) Uani 0.149(9) 1 d D U P A 2 O2A O 0.8991(15) 0.486(5) 0.3043(8) 0.052(4) Uani 0.149(9) 1 d D U P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C2B 0.0272(10) 0.0420(15) 0.0279(10) 0.0042(9) 0.0065(8) 0.0017(9) C3B 0.0314(11) 0.0491(16) 0.0308(11) -0.0004(10) 0.0035(9) -0.0002(10) C4B 0.0336(12) 0.0568(18) 0.0355(12) 0.0027(11) 0.0029(9) -0.0074(11) C5B 0.0265(11) 0.071(2) 0.0370(12) 0.0104(13) 0.0051(9) -0.0026(11) C6B 0.0300(12) 0.0581(18) 0.0372(12) 0.0095(12) 0.0114(9) 0.0081(11) C7B 0.0297(11) 0.0445(15) 0.0305(11) 0.0085(10) 0.0104(9) 0.0064(9) C8B 0.0379(12) 0.0435(15) 0.0414(12) 0.0040(11) 0.0179(10) 0.0095(10) C9B 0.0431(13) 0.0385(15) 0.0365(12) -0.0022(10) 0.0153(10) 0.0025(10) C10B 0.0324(11) 0.0412(15) 0.0309(11) -0.0018(9) 0.0103(9) -0.0023(9) C11B 0.0427(13) 0.0480(16) 0.0310(11) -0.0049(10) 0.0120(10) -0.0072(11) C12B 0.0388(13) 0.0614(19) 0.0287(11) 0.0001(11) 0.0033(9) -0.0123(12) C13B 0.0366(12) 0.0538(17) 0.0340(12) 0.0058(11) 0.0012(10) 0.0006(11) C14B 0.0313(11) 0.0427(15) 0.0351(11) 0.0003(10) 0.0036(9) 0.0017(10) C15B 0.0276(10) 0.0409(14) 0.0281(10) -0.0008(9) 0.0064(8) -0.0009(9) C1B 0.0272(10) 0.0388(13) 0.0292(10) -0.0043(8) 0.0070(8) 0.0030(8) C16B 0.0302(10) 0.0518(15) 0.0286(10) 0.0007(10) 0.0092(8) 0.0001(10) C17B 0.0252(10) 0.0703(16) 0.0254(10) -0.0065(10) 0.0057(8) -0.0061(10) C18B 0.0229(10) 0.0702(16) 0.0357(11) -0.0179(11) 0.0024(8) 0.0009(10) F1B 0.0362(8) 0.1085(16) 0.0304(7) 0.0015(8) 0.0134(6) -0.0077(9) F2B 0.0300(7) 0.0729(13) 0.0368(7) -0.0099(7) -0.0001(6) -0.0104(7) O1B 0.0283(8) 0.0493(12) 0.0359(8) -0.0120(7) 0.0049(6) 0.0049(7) O2B 0.0303(9) 0.0885(18) 0.0666(13) -0.0349(13) 0.0117(9) 0.0048(10) C1 0.0256(12) 0.034(2) 0.0269(12) 0.0005(13) 0.0073(10) -0.0038(12) C2 0.0266(12) 0.039(2) 0.0272(14) -0.0049(16) 0.0084(10) -0.0008(13) C3 0.0310(14) 0.049(3) 0.0282(14) 0.0021(18) 0.0040(10) 0.0012(16) C4 0.0325(15) 0.058(3) 0.0325(17) 0.003(2) 0.0035(12) 0.0084(17) C5 0.0252(14) 0.067(4) 0.0372(19) -0.006(3) 0.0046(12) 0.0013(19) C6 0.0294(14) 0.056(3) 0.038(2) -0.006(2) 0.0125(13) -0.0081(17) C7 0.0294(14) 0.045(3) 0.0308(15) -0.0087(18) 0.0112(11) -0.0038(15) C8 0.0385(17) 0.044(3) 0.045(2) -0.003(2) 0.0191(13) -0.0093(18) C9 0.0441(18) 0.038(3) 0.0399(17) 0.0050(18) 0.0175(13) 0.0012(17) C10 0.0327(15) 0.038(2) 0.0328(15) 0.0007(15) 0.0117(11) 0.0034(16) C11 0.042(2) 0.052(3) 0.0295(14) 0.0077(17) 0.0119(13) 0.008(2) C12 0.0391(18) 0.060(3) 0.0274(15) -0.0013(19) 0.0022(12) 0.013(2) C13 0.0357(17) 0.058(3) 0.0305(14) -0.0047(17) 0.0016(11) 0.001(2) C14 0.0313(15) 0.042(3) 0.0313(14) -0.0035(15) 0.0033(11) -0.0003(16) C15 0.0291(15) 0.040(2) 0.0256(12) 0.0013(13) 0.0073(10) 0.0030(15) C16 0.0280(13) 0.041(2) 0.0296(14) -0.0008(14) 0.0089(10) -0.0017(13) C17 0.0247(12) 0.048(2) 0.0234(12) 0.0017(14) 0.0053(9) 0.0009(13) C18 0.0229(13) 0.048(2) 0.0281(13) 0.0034(13) 0.0028(10) -0.0041(13) F1 0.0368(10) 0.062(2) 0.0318(9) -0.0016(10) 0.0157(7) -0.0002(10) F2 0.0267(9) 0.061(2) 0.0376(9) 0.0070(11) 0.0006(7) 0.0058(10) O1 0.0284(10) 0.0381(17) 0.0309(10) 0.0040(11) 0.0068(8) -0.0042(10) O2 0.0329(12) 0.054(2) 0.0506(13) 0.0081(14) 0.0120(9) -0.0109(12) C1A 0.032(4) 0.033(6) 0.028(4) -0.001(4) 0.003(3) -0.002(4) C2A 0.032(4) 0.027(6) 0.021(6) -0.005(5) 0.001(3) -0.003(4) C3A 0.033(5) 0.037(8) 0.036(8) 0.007(7) 0.006(5) 0.000(5) C4A 0.033(5) 0.040(9) 0.044(10) 0.008(8) 0.005(5) 0.002(5) C5A 0.033(5) 0.036(8) 0.026(8) -0.003(6) 0.009(5) 0.002(5) C6A 0.033(4) 0.036(9) 0.033(8) 0.000(7) 0.004(5) -0.002(5) C7A 0.033(4) 0.023(7) 0.019(6) -0.009(5) 0.005(4) -0.003(4) C8A 0.033(5) 0.032(8) 0.029(6) 0.000(6) 0.009(4) -0.001(5) C9A 0.031(5) 0.030(7) 0.026(6) 0.002(6) 0.012(4) 0.000(5) C10A 0.030(6) 0.030(7) 0.027(4) -0.002(4) 0.011(4) 0.002(5) C11A 0.036(7) 0.039(9) 0.030(5) 0.002(5) 0.007(4) -0.003(7) C12A 0.032(7) 0.036(8) 0.033(6) -0.002(5) 0.005(5) 0.002(6) C13A 0.037(8) 0.038(8) 0.034(5) -0.003(6) -0.001(4) -0.006(7) C14A 0.025(6) 0.031(7) 0.032(5) -0.003(5) 0.004(4) 0.000(6) C15A 0.021(5) 0.030(6) 0.028(4) -0.002(4) 0.006(3) 0.001(5) C16A 0.035(4) 0.039(6) 0.023(5) 0.000(5) 0.007(4) 0.001(4) C17A 0.033(4) 0.048(6) 0.030(4) 0.006(4) 0.007(3) 0.003(4) C18A 0.025(5) 0.048(6) 0.035(7) 0.008(5) 0.000(4) -0.001(4) F1A 0.041(5) 0.069(9) 0.034(4) 0.002(5) 0.012(3) 0.008(6) F2A 0.040(4) 0.055(9) 0.042(4) 0.006(6) -0.001(4) 0.008(5) O1A 0.029(4) 0.040(6) 0.036(5) 0.008(5) 0.002(4) 0.000(4) O2A 0.036(6) 0.056(8) 0.065(9) 0.018(8) 0.012(6) -0.003(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -1 -1 -1 0.0513 0 1 -1 0.0358 1 0 1 0.0408 -1 0 -1 0.0149 -1 1 -1 0.0262 -1 0 0 0.0206 -1 1 0 0.0301 1 -1 0 0.0759 1 1 -1 0.045 1 0 -1 0.0489 1 -1 -1 0.0705 0 1 0 0.0395 0 0 -1 0.0279 0 0 1 0.0279 5 2 4 0.0374 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 C3B C2B C7B 119.7(2) . . ? C3B C2B C1B 120.2(2) . . ? C7B C2B C1B 119.8(2) . . ? C4B C3B C2B 121.0(2) . . ? C4B C3B H3B 119.5 . . ? C2B C3B H3B 119.5 . . ? C5B C4B C3B 120.0(3) . . ? C5B C4B H4B 120 . . ? C3B C4B H4B 120 . . ? C4B C5B C6B 119.5(2) . . ? C4B C5B H5B 120.2 . . ? C6B C5B H5B 120.2 . . ? C5B C6B C7B 121.6(2) . . ? C5B C6B H6B 119.2 . . ? C7B C6B H6B 119.2 . . ? C6B C7B C2B 118.1(2) . . ? C6B C7B C8B 116.8(2) . . ? C2B C7B C8B 125.1(2) . . ? C9B C8B C7B 129.6(2) . . ? C9B C8B H8B 115.2 . . ? C7B C8B H8B 115.2 . . ? C8B C9B C10B 128.1(2) . . ? C8B C9B H9B 115.9 . . ? C10B C9B H9B 115.9 . . ? C11B C10B C15B 118.5(2) . . ? C11B C10B C9B 117.1(2) . . ? C15B C10B C9B 124.4(2) . . ? C12B C11B C10B 121.8(2) . . ? C12B C11B H11B 119.1 . . ? C10B C11B H11B 119.1 . . ? C13B C12B C11B 119.5(2) . . ? C13B C12B H12B 120.2 . . ? C11B C12B H12B 120.2 . . ? C12B C13B C14B 119.9(2) . . ? C12B C13B H13B 120 . . ? C14B C13B H13B 120 . . ? C13B C14B C15B 121.0(2) . . ? C13B C14B H14B 119.5 . . ? C15B C14B H14B 119.5 . . ? C14B C15B C10B 119.0(2) . . ? C14B C15B C1B 120.3(2) . . ? C10B C15B C1B 120.5(2) . . ? O1B C1B C2B 107.14(19) . . ? O1B C1B C15B 107.39(18) . . ? C2B C1B C15B 113.93(18) . . ? O1B C1B C16B 103.48(17) . . ? C2B C1B C16B 111.96(19) . . ? C15B C1B C16B 112.1(2) . . ? C17B C16B C1B 102.3(2) . . ? C17B C16B H16A 111.3 . . ? C1B C16B H16A 111.3 . . ? C17B C16B H16B 111.3 . . ? C1B C16B H16B 111.3 . . ? H16A C16B H16B 109.2 . . ? F1B C17B F2B 106.1(2) . . ? F1B C17B C16B 114.9(2) . . ? F2B C17B C16B 112.5(2) . . ? F1B C17B C18B 110.5(2) . . ? F2B C17B C18B 108.1(2) . . ? C16B C17B C18B 104.7(2) . . ? O2B C18B O1B 123.5(3) . . ? O2B C18B C17B 127.7(3) . . ? O1B C18B C17B 108.8(2) . . ? C18B O1B C1B 111.6(2) . . ? O1 C1 C2 106.7(2) . . ? O1 C1 C15 106.9(2) . . ? C2 C1 C15 114.8(2) . . ? O1 C1 C16 103.5(2) . . ? C2 C1 C16 111.5(2) . . ? C15 C1 C16 112.6(3) . . ? C3 C2 C7 119.4(3) . . ? C3 C2 C1 120.5(3) . . ? C7 C2 C1 119.7(3) . . ? C2 C3 C4 121.3(3) . . ? C2 C3 H3 119.3 . . ? C4 C3 H3 119.3 . . ? C5 C4 C3 119.9(4) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 119.7(3) . . ? C4 C5 H5 120.2 . . ? C6 C5 H5 120.2 . . ? C5 C6 C7 121.5(3) . . ? C5 C6 H6 119.3 . . ? C7 C6 H6 119.3 . . ? C6 C7 C2 118.1(3) . . ? C6 C7 C8 116.9(3) . . ? C2 C7 C8 125.0(3) . . ? C9 C8 C7 129.9(4) . . ? C9 C8 H8 115 . . ? C7 C8 H8 115 . . ? C8 C9 C10 128.6(4) . . ? C8 C9 H9 115.7 . . ? C10 C9 H9 115.7 . . ? C11 C10 C15 117.9(3) . . ? C11 C10 C9 117.7(3) . . ? C15 C10 C9 124.3(3) . . ? C12 C11 C10 122.2(4) . . ? C12 C11 H11 118.9 . . ? C10 C11 H11 118.9 . . ? C11 C12 C13 119.3(3) . . ? C11 C12 H12 120.4 . . ? C13 C12 H12 120.4 . . ? C12 C13 C14 119.9(4) . . ? C12 C13 H13 120 . . ? C14 C13 H13 120 . . ? C13 C14 C15 121.6(3) . . ? C13 C14 H14 119.2 . . ? C15 C14 H14 119.2 . . ? C14 C15 C10 118.8(3) . . ? C14 C15 C1 120.7(3) . . ? C10 C15 C1 120.3(3) . . ? C17 C16 C1 102.4(3) . . ? C17 C16 H16C 111.3 . . ? C1 C16 H16C 111.3 . . ? C17 C16 H16D 111.3 . . ? C1 C16 H16D 111.3 . . ? H16C C16 H16D 109.2 . . ? F1 C17 F2 106.4(2) . . ? F1 C17 C16 114.6(3) . . ? F2 C17 C16 112.5(3) . . ? F1 C17 C18 110.3(3) . . ? F2 C17 C18 108.4(3) . . ? C16 C17 C18 104.5(3) . . ? O2 C18 O1 123.2(4) . . ? O2 C18 C17 127.5(3) . . ? O1 C18 C17 109.3(3) . . ? C18 O1 C1 111.3(3) . . ? O1A C1A C2A 107.5(14) . . ? O1A C1A C15A 107.9(13) . . ? C2A C1A C15A 113.1(14) . . ? O1A C1A C16A 105.2(12) . . ? C2A C1A C16A 112.0(13) . . ? C15A C1A C16A 110.7(13) . . ? C3A C2A C7A 119.4(15) . . ? C3A C2A C1A 120.0(16) . . ? C7A C2A C1A 119.9(15) . . ? C2A C3A C4A 120.1(18) . . ? C2A C3A H3A 120 . . ? C4A C3A H3A 120 . . ? C5A C4A C3A 121(2) . . ? C5A C4A H4A 119.4 . . ? C3A C4A H4A 119.4 . . ? C4A C5A C6A 119(2) . . ? C4A C5A H5A 120.7 . . ? C6A C5A H5A 120.7 . . ? C5A C6A C7A 120(2) . . ? C5A C6A H6A 119.9 . . ? C7A C6A H6A 119.9 . . ? C2A C7A C6A 120.0(16) . . ? C2A C7A C8A 125.4(17) . . ? C6A C7A C8A 114.3(18) . . ? C9A C8A C7A 132(2) . . ? C9A C8A H8A 114.2 . . ? C7A C8A H8A 114.2 . . ? C8A C9A C10A 126.9(19) . . ? C8A C9A H9A 116.5 . . ? C10A C9A H9A 116.5 . . ? C15A C10A C11A 118.8(16) . . ? C15A C10A C9A 125.5(16) . . ? C11A C10A C9A 115.5(17) . . ? C12A C11A C10A 120.6(19) . . ? C12A C11A H11A 119.7 . . ? C10A C11A H11A 119.7 . . ? C11A C12A C13A 121.4(19) . . ? C11A C12A H12A 119.3 . . ? C13A C12A H12A 119.3 . . ? C12A C13A C14A 119.2(18) . . ? C12A C13A H13A 120.4 . . ? C14A C13A H13A 120.4 . . ? C15A C14A C13A 118.8(17) . . ? C15A C14A H14A 120.6 . . ? C13A C14A H14A 120.6 . . ? C10A C15A C14A 120.9(15) . . ? C10A C15A C1A 120.1(14) . . ? C14A C15A C1A 118.8(15) . . ? C17A C16A C1A 101.7(13) . . ? C17A C16A H16E 111.4 . . ? C1A C16A H16E 111.4 . . ? C17A C16A H16F 111.4 . . ? C1A C16A H16F 111.4 . . ? H16E C16A H16F 109.3 . . ? F1A C17A F2A 106.0(13) . . ? F1A C17A C16A 114.3(15) . . ? F2A C17A C16A 111.5(14) . . ? F1A C17A C18A 110.8(15) . . ? F2A C17A C18A 109.6(15) . . ? C16A C17A C18A 104.7(13) . . ? O2A C18A O1A 122(2) . . ? O2A C18A C17A 128.2(18) . . ? O1A C18A C17A 109.9(13) . . ? C18A O1A C1A 109.6(14) . . ? 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 C2B C3B 1.390(4) . ? C2B C7B 1.408(3) . ? C2B C1B 1.522(3) . ? C3B C4B 1.390(3) . ? C3B H3B 0.95 . ? C4B C5B 1.381(4) . ? C4B H4B 0.95 . ? C5B C6B 1.386(4) . ? C5B H5B 0.95 . ? C6B C7B 1.407(3) . ? C6B H6B 0.95 . ? C7B C8B 1.460(4) . ? C8B C9B 1.337(4) . ? C8B H8B 0.95 . ? C9B C10B 1.464(3) . ? C9B H9B 0.95 . ? C10B C11B 1.401(3) . ? C10B C15B 1.408(3) . ? C11B C12B 1.380(4) . ? C11B H11B 0.95 . ? C12B C13B 1.379(4) . ? C12B H12B 0.95 . ? C13B C14B 1.393(3) . ? C13B H13B 0.95 . ? C14B C15B 1.397(3) . ? C14B H14B 0.95 . ? C15B C1B 1.529(3) . ? C1B O1B 1.466(3) . ? C1B C16B 1.554(4) . ? C16B C17B 1.502(3) . ? C16B H16A 0.99 . ? C16B H16B 0.99 . ? C17B F1B 1.351(3) . ? C17B F2B 1.369(3) . ? C17B C18B 1.526(5) . ? C18B O2B 1.194(3) . ? C18B O1B 1.342(3) . ? C1 O1 1.470(3) . ? C1 C2 1.524(4) . ? C1 C15 1.528(4) . ? C1 C16 1.555(4) . ? C2 C3 1.385(5) . ? C2 C7 1.412(4) . ? C3 C4 1.389(4) . ? C3 H3 0.95 . ? C4 C5 1.378(6) . ? C4 H4 0.95 . ? C5 C6 1.385(6) . ? C5 H5 0.95 . ? C6 C7 1.407(4) . ? C6 H6 0.95 . ? C7 C8 1.453(5) . ? C8 C9 1.341(5) . ? C8 H8 0.95 . ? C9 C10 1.458(5) . ? C9 H9 0.95 . ? C10 C11 1.403(4) . ? C10 C15 1.415(4) . ? C11 C12 1.378(6) . ? C11 H11 0.95 . ? C12 C13 1.380(6) . ? C12 H12 0.95 . ? C13 C14 1.386(4) . ? C13 H13 0.95 . ? C14 C15 1.393(5) . ? C14 H14 0.95 . ? C16 C17 1.506(4) . ? C16 H16C 0.99 . ? C16 H16D 0.99 . ? C17 F1 1.351(3) . ? C17 F2 1.367(3) . ? C17 C18 1.524(5) . ? C18 O2 1.199(4) . ? C18 O1 1.342(3) . ? C1A O1A 1.456(18) . ? C1A C2A 1.521(18) . ? C1A C15A 1.557(18) . ? C1A C16A 1.57(2) . ? C2A C3A 1.38(2) . ? C2A C7A 1.386(19) . ? C3A C4A 1.40(2) . ? C3A H3A 0.95 . ? C4A C5A 1.37(2) . ? C4A H4A 0.95 . ? C5A C6A 1.40(2) . ? C5A H5A 0.95 . ? C6A C7A 1.41(2) . ? C6A H6A 0.95 . ? C7A C8A 1.44(2) . ? C8A C9A 1.340(19) . ? C8A H8A 0.95 . ? C9A C10A 1.44(2) . ? C9A H9A 0.95 . ? C10A C15A 1.384(19) . ? C10A C11A 1.406(19) . ? C11A C12A 1.37(2) . ? C11A H11A 0.95 . ? C12A C13A 1.37(2) . ? C12A H12A 0.95 . ? C13A C14A 1.43(2) . ? C13A H13A 0.95 . ? C14A C15A 1.396(19) . ? C14A H14A 0.95 . ? C16A C17A 1.503(18) . ? C16A H16E 0.99 . ? C16A H16F 0.99 . ? C17A F1A 1.348(17) . ? C17A F2A 1.370(17) . ? C17A C18A 1.52(2) . ? C18A O2A 1.200(19) . ? C18A O1A 1.369(18) . ? 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 C7B C2B C3B C4B 0.7(4) . . . . ? C1B C2B C3B C4B 174.5(2) . . . . ? C2B C3B C4B C5B -2.5(4) . . . . ? C3B C4B C5B C6B 1.5(4) . . . . ? C4B C5B C6B C7B 1.2(4) . . . . ? C5B C6B C7B C2B -2.8(4) . . . . ? C5B C6B C7B C8B 177.0(2) . . . . ? C3B C2B C7B C6B 1.8(3) . . . . ? C1B C2B C7B C6B -171.9(2) . . . . ? C3B C2B C7B C8B -177.9(2) . . . . ? C1B C2B C7B C8B 8.3(3) . . . . ? C6B C7B C8B C9B -154.1(3) . . . . ? C2B C7B C8B C9B 25.7(4) . . . . ? C7B C8B C9B C10B 1.7(4) . . . . ? C8B C9B C10B C11B 152.2(3) . . . . ? C8B C9B C10B C15B -25.8(4) . . . . ? C15B C10B C11B C12B 3.8(4) . . . . ? C9B C10B C11B C12B -174.3(2) . . . . ? C10B C11B C12B C13B -0.3(4) . . . . ? C11B C12B C13B C14B -1.8(4) . . . . ? C12B C13B C14B C15B 0.2(4) . . . . ? C13B C14B C15B C10B 3.3(4) . . . . ? C13B C14B C15B C1B -172.2(2) . . . . ? C11B C10B C15B C14B -5.2(3) . . . . ? C9B C10B C15B C14B 172.8(2) . . . . ? C11B C10B C15B C1B 170.3(2) . . . . ? C9B C10B C15B C1B -11.7(3) . . . . ? C3B C2B C1B O1B 4.6(3) . . . . ? C7B C2B C1B O1B 178.29(19) . . . . ? C3B C2B C1B C15B 123.2(2) . . . . ? C7B C2B C1B C15B -63.1(3) . . . . ? C3B C2B C1B C16B -108.2(3) . . . . ? C7B C2B C1B C16B 65.5(3) . . . . ? C14B C15B C1B O1B -0.1(3) . . . . ? C10B C15B C1B O1B -175.5(2) . . . . ? C14B C15B C1B C2B -118.6(2) . . . . ? C10B C15B C1B C2B 66.0(3) . . . . ? C14B C15B C1B C16B 112.9(3) . . . . ? C10B C15B C1B C16B -62.5(3) . . . . ? O1B C1B C16B C17B 29.7(2) . . . . ? C2B C1B C16B C17B 144.72(19) . . . . ? C15B C1B C16B C17B -85.8(2) . . . . ? C1B C16B C17B F1B -148.0(2) . . . . ? C1B C16B C17B F2B 90.5(3) . . . . ? C1B C16B C17B C18B -26.6(2) . . . . ? F1B C17B C18B O2B -42.0(4) . . . . ? F2B C17B C18B O2B 73.7(3) . . . . ? C16B C17B C18B O2B -166.2(3) . . . . ? F1B C17B C18B O1B 138.60(19) . . . . ? F2B C17B C18B O1B -105.7(2) . . . . ? C16B C17B C18B O1B 14.4(3) . . . . ? O2B C18B O1B C1B -173.9(2) . . . . ? C17B C18B O1B C1B 5.6(3) . . . . ? C2B C1B O1B C18B -140.96(19) . . . . ? C15B C1B O1B C18B 96.3(2) . . . . ? C16B C1B O1B C18B -22.5(2) . . . . ? O1 C1 C2 C3 5.6(4) . . . . ? C15 C1 C2 C3 123.8(4) . . . . ? C16 C1 C2 C3 -106.7(4) . . . . ? O1 C1 C2 C7 179.2(3) . . . . ? C15 C1 C2 C7 -62.6(4) . . . . ? C16 C1 C2 C7 66.9(4) . . . . ? C7 C2 C3 C4 -0.4(6) . . . . ? C1 C2 C3 C4 173.1(4) . . . . ? C2 C3 C4 C5 -1.6(7) . . . . ? C3 C4 C5 C6 1.1(8) . . . . ? C4 C5 C6 C7 1.5(8) . . . . ? C5 C6 C7 C2 -3.5(7) . . . . ? C5 C6 C7 C8 177.3(5) . . . . ? C3 C2 C7 C6 2.9(6) . . . . ? C1 C2 C7 C6 -170.7(4) . . . . ? C3 C2 C7 C8 -177.9(4) . . . . ? C1 C2 C7 C8 8.5(6) . . . . ? C6 C7 C8 C9 -155.6(6) . . . . ? C2 C7 C8 C9 25.3(8) . . . . ? C7 C8 C9 C10 1.1(9) . . . . ? C8 C9 C10 C11 153.7(5) . . . . ? C8 C9 C10 C15 -24.8(7) . . . . ? C15 C10 C11 C12 4.3(6) . . . . ? C9 C10 C11 C12 -174.4(4) . . . . ? C10 C11 C12 C13 -0.8(7) . . . . ? C11 C12 C13 C14 -1.5(7) . . . . ? C12 C13 C14 C15 0.2(6) . . . . ? C13 C14 C15 C10 3.4(6) . . . . ? C13 C14 C15 C1 -171.8(4) . . . . ? C11 C10 C15 C14 -5.4(5) . . . . ? C9 C10 C15 C14 173.1(4) . . . . ? C11 C10 C15 C1 169.7(4) . . . . ? C9 C10 C15 C1 -11.7(5) . . . . ? O1 C1 C15 C14 -1.7(4) . . . . ? C2 C1 C15 C14 -119.7(4) . . . . ? C16 C1 C15 C14 111.3(4) . . . . ? O1 C1 C15 C10 -176.7(3) . . . . ? C2 C1 C15 C10 65.2(4) . . . . ? C16 C1 C15 C10 -63.8(4) . . . . ? O1 C1 C16 C17 29.4(3) . . . . ? C2 C1 C16 C17 143.7(3) . . . . ? C15 C1 C16 C17 -85.6(3) . . . . ? C1 C16 C17 F1 -146.7(3) . . . . ? C1 C16 C17 F2 91.5(3) . . . . ? C1 C16 C17 C18 -25.9(3) . . . . ? F1 C17 C18 O2 -42.7(4) . . . . ? F2 C17 C18 O2 73.4(4) . . . . ? C16 C17 C18 O2 -166.4(3) . . . . ? F1 C17 C18 O1 137.1(2) . . . . ? F2 C17 C18 O1 -106.7(3) . . . . ? C16 C17 C18 O1 13.5(3) . . . . ? O2 C18 O1 C1 -173.8(3) . . . . ? C17 C18 O1 C1 6.3(3) . . . . ? C2 C1 O1 C18 -140.5(3) . . . . ? C15 C1 O1 C18 96.2(3) . . . . ? C16 C1 O1 C18 -22.8(3) . . . . ? O1A C1A C2A C3A 7(2) . . . . ? C15A C1A C2A C3A 126(2) . . . . ? C16A C1A C2A C3A -108(2) . . . . ? O1A C1A C2A C7A 177.0(17) . . . . ? C15A C1A C2A C7A -64(2) . . . . ? C16A C1A C2A C7A 62(2) . . . . ? C7A C2A C3A C4A 7(4) . . . . ? C1A C2A C3A C4A 177(2) . . . . ? C2A C3A C4A C5A -9(5) . . . . ? C3A C4A C5A C6A 7(5) . . . . ? C4A C5A C6A C7A -2(5) . . . . ? C3A C2A C7A C6A -3(3) . . . . ? C1A C2A C7A C6A -173(2) . . . . ? C3A C2A C7A C8A -176(2) . . . . ? C1A C2A C7A C8A 14(3) . . . . ? C5A C6A C7A C2A 0(4) . . . . ? C5A C6A C7A C8A 174(3) . . . . ? C2A C7A C8A C9A 17(5) . . . . ? C6A C7A C8A C9A -157(3) . . . . ? C7A C8A C9A C10A 9(5) . . . . ? C8A C9A C10A C15A -27(4) . . . . ? C8A C9A C10A C11A 147(3) . . . . ? C15A C10A C11A C12A -2(4) . . . . ? C9A C10A C11A C12A -177(2) . . . . ? C10A C11A C12A C13A 5(4) . . . . ? C11A C12A C13A C14A -5(4) . . . . ? C12A C13A C14A C15A 1(3) . . . . ? C11A C10A C15A C14A -2(3) . . . . ? C9A C10A C15A C14A 173(2) . . . . ? C11A C10A C15A C1A 173(2) . . . . ? C9A C10A C15A C1A -13(3) . . . . ? C13A C14A C15A C10A 2(3) . . . . ? C13A C14A C15A C1A -173(2) . . . . ? O1A C1A C15A C10A -175.3(16) . . . . ? C2A C1A C15A C10A 66(2) . . . . ? C16A C1A C15A C10A -61(2) . . . . ? O1A C1A C15A C14A 0(2) . . . . ? C2A C1A C15A C14A -119.2(19) . . . . ? C16A C1A C15A C14A 114.2(18) . . . . ? O1A C1A C16A C17A 29.4(15) . . . . ? C2A C1A C16A C17A 145.8(14) . . . . ? C15A C1A C16A C17A -86.9(15) . . . . ? C1A C16A C17A F1A -147.5(15) . . . . ? C1A C16A C17A F2A 92.4(16) . . . . ? C1A C16A C17A C18A -26.1(16) . . . . ? F1A C17A C18A O2A -43(3) . . . . ? F2A C17A C18A O2A 74(3) . . . . ? C16A C17A C18A O2A -167(2) . . . . ? F1A C17A C18A O1A 138.5(15) . . . . ? F2A C17A C18A O1A -104.9(16) . . . . ? C16A C17A C18A O1A 15(2) . . . . ? O2A C18A O1A C1A -173.8(18) . . . . ? C17A C18A O1A C1A 5(2) . . . . ? C2A C1A O1A C18A -141.1(16) . . . . ? C15A C1A O1A C18A 96.6(17) . . . . ? C16A C1A O1A C18A -21.6(17) . . . . ? 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 -1.0011 -1.0003 -1.0022 -0.0427 0.1525 -0.2776 0.0009 1.0002 -0.9976 -0.0343 0.0547 0.264 1.0002 -0.0001 1 0.1019 -0.1469 0.0204 -1.0002 0.0001 -1 -0.1019 0.1469 -0.0204 -0.9992 1.0005 -0.9978 -0.1611 0.1412 0.2368 -1.0001 0.0002 -0.0002 -0.1268 0.0865 -0.0272 -0.9991 1.0006 0.002 -0.186 0.0809 0.23 0.9991 -1.0006 -0.002 0.186 -0.0809 -0.23 1.001 1 -0.9973 0.0924 -0.0318 0.2912 1 -0.0004 -0.9996 0.1516 -0.0261 0.034 0.999 -1.0008 -1.0017 0.2108 -0.0205 -0.2232 0.001 1.0004 0.0022 -0.0592 -0.0056 0.2572 -0.0001 -0.0002 -0.9998 0.0249 0.0604 0.0068 0.0001 0.0002 0.9998 -0.0249 -0.0604 -0.0068 5.0026 2.0002 4.0046 0.416 -0.6852 0.6232