#------------------------------------------------------------------------------ #$Date: 2024-08-05 20:54:14 +0300 (Mon, 05 Aug 2024) $ #$Revision: 293733 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/18/1571812.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_1571812 loop_ _publ_author_name 'Luo, Zheng' 'Zhang, Xiaoyu' 'Li, Zaiyang' 'Luo, Meiming' 'Zeng, Xiaoming' _publ_section_title ; Mild ketyl radical generation and coupling with alkynes enabled by Cr catalysis: stereoselective access to E-exocyclic allyl alcohols. ; _journal_issue 29 _journal_name_full 'Chemical science' _journal_page_first 11428 _journal_page_last 11434 _journal_paper_doi 10.1039/d4sc02967d _journal_volume 15 _journal_year 2024 _chemical_formula_moiety 'C12 H9 F5 O' _chemical_formula_sum 'C12 H9 F5 O' _chemical_formula_weight 264.19 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_block_doi 10.5517/ccdc.csd.cc2hpmhb _audit_creation_date 2023-08-30 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408) ; _audit_update_record ; 2023-12-15 deposited with the CCDC. 2024-06-09 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 4.915(3) _cell_length_b 11.218(7) _cell_length_c 20.402(14) _cell_measurement_reflns_used 2190 _cell_measurement_temperature 285(2) _cell_measurement_theta_max 22.627 _cell_measurement_theta_min 2.699 _cell_volume 1124.9(12) _computing_cell_refinement 'SAINT V8.40B (?, 2016)' _computing_data_reduction 'SAINT V8.40B (?, 2016)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2014/7 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 285.0 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0865 _diffrn_reflns_av_unetI/netI 0.0815 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.988 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 9067 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.981 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.806 _diffrn_reflns_theta_min 2.072 _diffrn_source_current 1.4 _diffrn_source_power 0.07 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.154 _exptl_absorpt_correction_T_max 0.7455 _exptl_absorpt_correction_T_min 0.4588 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1635 before and 0.0754 after correction. The Ratio of minimum to maximum transmission is 0.6154. The \l/2 correction factor is Not present. ; _exptl_crystal_colour 'clear light colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.560 _exptl_crystal_description needle _exptl_crystal_F_000 536 _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.02 _refine_diff_density_max 0.190 _refine_diff_density_min -0.206 _refine_diff_density_rms 0.045 _refine_ls_abs_structure_details ; Flack x determined using 415 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.8(9) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 164 _refine_ls_number_reflns 2622 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.026 _refine_ls_R_factor_all 0.1124 _refine_ls_R_factor_gt 0.0546 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0583P)^2^+0.1395P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1253 _refine_ls_wR_factor_ref 0.1573 _reflns_Friedel_coverage 0.673 _reflns_Friedel_fraction_full 0.996 _reflns_Friedel_fraction_max 0.970 _reflns_number_gt 1498 _reflns_number_total 2622 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc02967d2.cif _cod_data_source_block mo_zxm_lz_5f_0m_a _cod_depositor_comments 'Adding full bibliography for 1571812.cif.' _cod_original_cell_volume 1124.8(12) _cod_database_code 1571812 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.997 _shelx_estimated_absorpt_t_min 0.930 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All O(H) groups 2.a Ternary CH refined with riding coordinates: C11(H11) 2.b Secondary CH2 refined with riding coordinates: C7(H7A,H7B), C8(H8A,H8B), C12(H12A,H12B) 2.c Aromatic/amide H refined with riding coordinates: C5(H5) 2.d Idealised tetrahedral OH refined as rotating group: O1(H1) ; _shelx_res_file ; mo_zxm_lz_5f_0m_a.res created by SHELXL-2014/7 TITL mo_ZXM_LZ_5F_0m_a.res in P2(1)2(1)2(1) CELL 0.71073 4.9147 11.2178 20.4024 90 90 90 ZERR 4 0.0028 0.0069 0.0138 0 0 0 LATT -1 SYMM 0.5+X,0.5-Y,-Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5-X,-Y,0.5+Z SFAC C H F O UNIT 48 36 20 4 L.S. 9 PLAN 5 0 0 SIZE 0.02 0.12 0.48 TEMP 11.85 CONF HTAB BOND $H fmap 2 acta MORE -1 OMIT 0 0 2 OMIT 0 0 8 OMIT 3 6 3 REM REM REM WGHT 0.058300 0.139500 FVAR 0.94777 F1 3 1.079556 0.316734 0.864655 11.00000 0.11751 0.10614 = 0.07570 0.00983 -0.02985 -0.01683 F2 3 0.854961 0.171338 0.657431 11.00000 0.07598 0.05482 = 0.07644 -0.00852 0.00808 0.00686 F3 3 1.162089 0.160953 0.765802 11.00000 0.08738 0.07464 = 0.10382 0.01684 -0.01298 0.01457 F4 3 0.365818 0.492576 0.747936 11.00000 0.07683 0.06709 = 0.08117 -0.01776 0.01238 0.01046 F5 3 0.677797 0.483660 0.854753 11.00000 0.12248 0.09427 = 0.06417 -0.02749 0.00804 -0.01195 O1 4 0.204442 0.292337 0.514029 11.00000 0.05290 0.09721 = 0.09627 -0.04330 -0.00467 0.00526 AFIX 147 H1 2 0.356312 0.284064 0.498020 11.00000 -1.50000 AFIX 0 C1 1 0.925493 0.322068 0.810781 11.00000 0.07809 0.07321 = 0.05581 0.01103 -0.00371 -0.01918 C2 1 0.723473 0.407170 0.805491 11.00000 0.07943 0.06038 = 0.05309 -0.00684 0.00816 -0.01631 C3 1 0.569292 0.411119 0.749471 11.00000 0.06222 0.04926 = 0.06014 -0.00090 0.01038 -0.00341 C4 1 0.604247 0.335078 0.697165 11.00000 0.05400 0.04352 = 0.05606 0.00164 0.00433 -0.00743 C5 1 0.432764 0.332146 0.638471 11.00000 0.05391 0.05008 = 0.06154 -0.01086 0.00973 -0.00914 AFIX 43 H5 2 0.374135 0.257154 0.625121 11.00000 -1.20000 AFIX 0 C6 1 0.350793 0.423123 0.602029 11.00000 0.05102 0.05254 = 0.05767 -0.00965 0.00250 0.00053 C7 1 0.429424 0.552171 0.607037 11.00000 0.09226 0.05257 = 0.07824 -0.00347 -0.00204 -0.00312 AFIX 23 H7A 2 0.622741 0.560203 0.615540 11.00000 -1.20000 H7B 2 0.329513 0.591100 0.642008 11.00000 -1.20000 AFIX 0 C8 1 0.356809 0.605475 0.541547 11.00000 0.17769 0.07669 = 0.10102 0.01851 -0.03998 -0.01051 AFIX 23 H8A 2 0.204945 0.660046 0.546219 11.00000 -1.20000 H8B 2 0.510559 0.649135 0.523872 11.00000 -1.20000 AFIX 0 C9 1 0.810121 0.250356 0.705634 11.00000 0.05770 0.04794 = 0.05691 -0.00131 0.00994 -0.00575 C10 1 0.966497 0.243687 0.760192 11.00000 0.06363 0.05553 = 0.06638 0.00789 0.00211 -0.00586 C11 1 0.182193 0.407435 0.541813 11.00000 0.05721 0.07336 = 0.07151 -0.02105 -0.00916 0.00734 AFIX 13 H11 2 -0.008847 0.422535 0.552791 11.00000 -1.20000 AFIX 0 C12 1 0.282153 0.505555 0.497052 11.00000 0.14893 0.10229 = 0.07894 0.01425 -0.03483 -0.01548 AFIX 23 H12A 2 0.438936 0.479238 0.472059 11.00000 -1.20000 H12B 2 0.140163 0.529780 0.466836 11.00000 -1.20000 AFIX 0 HKLF 4 REM mo_ZXM_LZ_5F_0m_a.res in P2(1)2(1)2(1) REM R1 = 0.0546 for 1498 Fo > 4sig(Fo) and 0.1124 for all 2622 data REM 164 parameters refined using 0 restraints END WGHT 0.0581 0.1411 REM Instructions for potential hydrogen bonds EQIV $1 x+1/2, -y+1/2, -z+1 HTAB O1 O1_$1 REM Highest difference peak 0.190, deepest hole -0.206, 1-sigma level 0.045 Q1 1 0.0216 0.2737 0.5072 11.00000 0.05 0.19 Q2 1 0.0206 0.4156 0.5975 11.00000 0.05 0.15 Q3 1 1.0753 0.1916 0.7106 11.00000 0.05 0.14 Q4 1 1.1421 0.3539 0.9153 11.00000 0.05 0.14 Q5 1 0.1083 0.6114 0.6054 11.00000 0.05 0.14 ; _shelx_res_checksum 35758 _shelx_hkl_file ; 1 0 0 0.50 0.80 -1 0 0 -0.30 0.70 -1 0 0 0.30 0.80 1 0 0 0.40 0.80 -2 0 0 760.92 51.59 -2 0 0 607.94 51.39 2 0 0 750.52 51.99 2 0 0 784.82 52.29 -3 0 0 -1.80 1.30 -3 0 0 1.20 1.80 -4 0 0 242.88 19.40 4 0 0 276.67 22.90 -4 0 0 249.18 21.80 5 0 0 -2.60 2.90 6 0 0 2.00 3.80 1 -1 0 1656.33 133.39 1 -1 0 2067.89 133.39 -1 -1 0 2022.60 134.69 -1 -1 0 1913.51 134.49 1 1 0 2071.89 134.79 1 1 0 1930.91 134.49 2 -1 0 151.38 13.70 -2 -1 0 180.08 14.40 2 -1 0 183.08 13.60 -2 -1 0 161.38 14.30 2 1 0 174.18 14.50 2 1 0 182.18 14.70 3 -1 0 91.49 9.40 -3 -1 0 77.29 8.70 -3 -1 0 73.79 8.90 3 1 0 96.19 9.90 -4 -1 0 23.80 5.30 4 -1 0 35.20 7.20 -4 -1 0 28.80 6.10 4 1 0 54.49 7.50 -5 -1 0 21.60 4.10 -5 -1 0 19.30 4.20 5 -1 0 20.00 6.00 5 1 0 17.40 6.20 6 -1 0 11.20 4.40 6 1 0 -0.70 3.50 0 -2 0 36.70 3.50 0 -2 0 42.40 3.90 -1 -2 0 418.86 30.70 -1 -2 0 405.26 30.80 1 2 0 421.56 31.00 1 2 0 426.26 30.60 -2 -2 0 251.17 19.80 -2 -2 0 223.48 19.40 2 -2 0 212.58 18.10 2 2 0 265.47 20.20 2 2 0 255.27 19.60 3 -2 0 247.18 20.10 -3 -2 0 226.08 20.10 -3 -2 0 228.88 20.70 3 2 0 253.27 20.90 -4 -2 0 15.10 4.70 4 -2 0 12.40 4.50 -4 -2 0 17.30 4.80 4 2 0 24.10 5.90 -5 -2 0 11.90 4.00 -5 -2 0 17.50 5.70 5 -2 0 14.70 5.10 6 -2 0 5.20 4.20 6 2 0 6.80 5.70 0 -3 0 0.20 0.80 0 -3 0 -0.80 0.70 -1 -3 0 7.90 2.50 -1 -3 0 10.10 3.00 1 -3 0 11.30 1.40 1 3 0 11.60 3.10 1 3 0 11.30 2.80 -2 -3 0 522.05 40.40 -2 -3 0 531.75 40.50 2 -3 0 470.75 37.70 2 3 0 572.84 40.30 2 3 0 605.34 41.30 -3 -3 0 35.30 7.40 3 -3 0 44.10 6.10 -3 -3 0 38.20 7.30 3 3 0 47.20 8.10 4 -3 0 26.50 5.90 -4 -3 0 5.20 4.30 -4 -3 0 14.80 4.80 4 3 0 24.30 6.20 -5 -3 0 -2.60 3.40 5 -3 0 5.90 4.10 5 3 0 1.40 4.10 -6 -3 0 4.60 4.40 -6 -3 0 4.60 5.80 6 -3 0 3.20 4.50 6 3 0 18.20 6.70 0 -4 0 91.69 8.70 0 -4 0 95.69 8.20 -1 -4 0 40.00 5.20 -1 -4 0 39.40 5.40 1 -4 0 36.30 3.90 1 4 0 39.50 5.00 -2 -4 0 57.29 8.00 2 -4 0 60.59 5.50 -2 -4 0 70.89 8.40 2 4 0 83.59 8.40 -3 -4 0 10.20 4.10 3 -4 0 7.40 3.00 -3 -4 0 10.70 4.30 3 4 0 11.80 4.20 4 -4 0 23.60 6.60 -4 -4 0 19.70 5.50 -4 -4 0 9.50 4.90 4 4 0 20.00 5.50 -5 -4 0 9.80 4.70 5 -4 0 3.40 3.60 -5 -4 0 6.70 5.40 5 4 0 -0.10 3.80 -6 -4 0 7.30 5.20 6 -4 0 3.40 3.70 -6 -4 0 5.10 6.50 6 4 0 9.80 5.90 0 -5 0 0.40 1.10 0 -5 0 0.10 1.30 -1 -5 0 370.66 28.40 1 -5 0 342.97 26.10 -1 -5 0 339.57 27.50 1 5 0 362.36 27.30 -2 -5 0 34.10 6.80 -2 -5 0 26.60 6.20 2 -5 0 32.60 3.70 2 5 0 43.10 6.00 -3 -5 0 19.60 6.10 -3 -5 0 23.20 6.20 3 -5 0 17.00 3.80 3 5 0 26.10 6.00 4 -5 0 19.30 5.30 -4 -5 0 6.80 5.40 -4 -5 0 18.20 5.50 4 5 0 17.90 5.90 -5 -5 0 16.70 6.00 -5 -5 0 9.30 6.20 5 -5 0 10.10 4.90 5 5 0 23.10 7.70 6 -5 0 4.00 4.00 -6 -5 0 -2.90 6.30 -6 -5 0 -8.60 8.80 6 5 0 -5.10 5.20 0 -6 0 1248.98 89.89 0 -6 0 1233.48 87.79 -1 -6 0 40.70 6.00 -1 -6 0 39.30 7.30 1 -6 0 43.10 5.20 1 6 0 40.80 5.60 2 -6 0 0.00 1.10 -2 -6 0 1.70 2.60 -2 -6 0 0.10 2.00 2 6 0 1.60 2.30 -3 -6 0 18.30 6.20 -3 -6 0 25.60 6.70 3 6 0 20.00 5.80 4 -6 0 84.29 10.60 -4 -6 0 99.49 12.60 -4 -6 0 91.49 12.90 4 6 0 85.29 11.80 -5 -6 0 1.60 3.80 5 -6 0 3.50 3.50 5 6 0 3.50 4.50 0 -7 0 -1.30 1.30 0 -7 0 -1.50 1.00 1 -7 0 89.39 10.00 -1 -7 0 107.49 11.60 -1 -7 0 100.89 10.80 -2 -7 0 3.30 2.60 -2 -7 0 -0.50 1.70 2 -7 0 1.40 1.70 2 7 0 -2.20 1.70 -3 -7 0 -0.80 2.30 -3 -7 0 4.70 3.40 3 -7 0 3.10 2.00 3 7 0 4.10 3.40 -4 -7 0 9.00 4.80 4 -7 0 4.90 3.80 4 7 0 6.00 3.80 -5 -7 0 -1.10 6.20 5 -7 0 -8.20 3.60 -5 -7 0 -1.50 4.90 5 7 0 7.00 5.00 0 -8 0 59.49 8.50 0 -8 0 61.59 7.60 -1 -8 0 90.09 11.60 1 -8 0 96.59 10.40 -1 -8 0 99.69 11.20 1 -8 0 99.89 9.50 -2 -8 0 34.60 8.20 -2 -8 0 34.80 8.20 2 8 0 42.10 7.70 -3 -8 0 118.99 15.20 -3 -8 0 115.09 17.10 3 -8 0 118.09 12.20 3 8 0 165.98 17.30 -4 -8 0 11.00 4.60 4 -8 0 6.50 4.80 -4 -8 0 1.20 4.50 4 8 0 4.00 3.80 5 -8 0 0.40 4.30 -5 -8 0 0.00 4.90 0 -9 0 -1.20 2.50 0 -9 0 0.90 2.10 -1 -9 0 34.90 8.10 -1 -9 0 25.70 6.40 1 -9 0 20.20 5.40 1 -9 0 21.50 4.70 -2 -9 0 21.90 6.70 2 -9 0 18.40 5.20 -2 -9 0 10.70 5.60 2 9 0 28.30 6.20 -3 -9 0 0.10 2.90 3 -9 0 -0.10 2.70 3 9 0 3.90 3.30 -4 -9 0 3.00 3.90 -4 -9 0 2.10 5.00 4 -9 0 5.00 3.40 4 9 0 2.00 3.40 -5 -9 0 10.90 7.10 5 -9 0 -6.30 4.20 5 9 0 4.90 6.10 0 -10 0 15.70 5.40 1 -10 0 27.30 7.00 -1 -10 0 26.20 7.60 -1 -10 0 42.80 8.90 -2 -10 0 22.10 7.30 2 -10 0 23.20 4.70 -2 -10 0 21.10 6.70 2 -10 0 21.30 5.80 -3 -10 0 8.80 5.70 3 -10 0 4.90 4.30 -3 -10 0 10.50 6.70 3 10 0 30.10 7.40 -4 -10 0 3.60 4.70 4 -10 0 -7.60 3.20 4 10 0 0.60 3.50 0 -11 0 1.30 3.20 0 -11 0 -2.60 2.60 1 -11 0 8.20 4.00 1 -11 0 1.40 3.70 -1 -11 0 12.90 5.60 -1 -11 0 4.90 4.20 -2 -11 0 13.00 6.30 2 -11 0 11.00 5.00 2 -11 0 16.30 4.50 -2 -11 0 10.10 5.70 -3 -11 0 8.50 5.70 3 -11 0 4.10 3.70 -4 -11 0 5.00 5.90 4 -11 0 6.10 4.60 4 11 0 17.10 7.00 0 -12 0 424.26 36.00 -1 -12 0 -1.80 4.30 -1 -12 0 3.60 4.10 1 -12 0 -1.40 2.80 1 -12 0 2.90 4.90 2 -12 0 1.30 2.80 2 -12 0 -6.40 3.80 -2 -12 0 -7.90 4.50 -3 -12 0 2.80 6.80 3 -12 0 5.70 2.90 0 -13 0 1.10 4.00 0 -13 0 -6.90 3.60 1 -13 0 4.10 4.50 1 -13 0 -6.60 3.10 -1 -13 0 -5.30 4.00 2 -13 0 9.20 4.10 -2 -13 0 7.50 6.40 2 -13 0 9.70 5.80 -3 -13 0 6.50 8.60 3 -13 0 -4.10 4.70 0 -14 0 10.00 8.50 1 -14 0 25.60 9.20 -1 -14 0 38.00 10.20 1 -14 0 43.50 9.20 -2 -14 0 0.80 6.20 2 -14 0 -0.70 5.30 6 0 -1 4.80 4.80 5 0 -1 53.89 10.30 -4 0 1 21.10 4.10 -4 0 1 21.60 4.60 4 0 -1 31.30 7.10 -3 0 1 -0.70 1.30 -3 0 1 0.20 1.90 3 0 -1 4.30 2.60 -2 0 1 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1955.10 131.59 1 1 1 1882.61 131.09 -2 -1 -1 506.25 39.00 2 -1 1 537.75 38.30 -2 -1 -1 557.94 39.40 2 -1 1 559.04 38.30 2 1 1 496.25 38.90 2 1 1 538.95 39.50 3 -1 1 33.30 5.30 -3 -1 -1 21.70 4.70 -3 -1 -1 32.40 5.60 3 -1 1 20.70 4.70 3 1 1 30.30 5.60 3 1 1 32.70 6.20 -4 -1 -1 -0.10 2.10 4 -1 1 -1.20 2.00 -4 -1 -1 0.70 2.10 4 1 1 -4.00 1.90 5 -1 1 18.60 5.60 -5 -1 -1 20.40 3.40 5 1 1 24.00 6.10 6 -1 1 1.40 3.70 6 1 1 9.10 5.10 6 -2 -1 1.40 4.90 -6 -2 1 7.00 3.30 -6 -2 1 8.40 3.60 6 2 -1 13.60 6.10 -5 -2 1 18.80 5.90 5 -2 -1 8.50 4.80 -5 -2 1 9.50 4.40 -4 -2 1 15.30 5.30 -4 -2 1 13.40 4.20 4 -2 -1 31.90 7.00 4 2 -1 12.50 4.70 -3 -2 1 511.35 45.10 3 -2 -1 698.53 45.80 -3 -2 1 582.04 44.90 3 2 -1 600.14 45.60 2 -2 -1 334.67 26.20 -2 -2 1 329.87 27.20 -2 -2 1 364.36 27.00 2 2 -1 358.06 27.30 -1 -2 1 8291.17 648.94 -1 2 1 9999.00 635.24 -1 2 1 8091.29 614.84 0 -2 -1 2307.67 182.38 0 -2 1 2334.37 183.08 -1 -2 -1 8391.76 601.54 1 2 1 7786.12 600.14 2 -2 1 382.96 25.60 -2 -2 -1 391.66 28.30 2 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-10 -19 -4.60 8.00 4 0 -20 18.10 8.60 3 0 -20 2.70 5.90 -3 0 20 -0.40 6.40 -2 0 20 18.10 8.60 2 0 -20 12.20 7.70 1 0 -20 31.20 9.80 0 0 -20 479.35 40.40 0 0 20 365.86 39.70 -1 0 -20 34.10 10.20 1 0 20 29.80 10.70 2 0 20 8.10 9.20 -2 0 -20 10.10 4.10 -2 0 -20 8.80 6.20 3 0 20 8.70 10.80 4 0 20 -15.40 11.20 4 1 -20 13.10 7.90 3 -1 -20 -5.70 5.30 -3 1 20 18.10 8.00 3 1 -20 0.60 5.50 2 -1 -20 -6.90 5.10 -2 -1 20 3.70 5.60 2 1 -20 -0.50 4.80 -2 1 20 3.90 6.10 1 -1 -20 84.29 16.60 1 1 -20 82.09 15.40 0 -1 20 3.70 6.40 0 -1 -20 19.80 8.80 0 1 -20 13.90 6.80 0 1 20 0.90 5.90 -1 -1 -20 88.89 16.90 1 -1 20 112.39 22.00 -1 1 -20 101.09 16.50 1 1 20 101.59 19.40 -2 -1 -20 -0.20 2.80 -2 -1 -20 3.50 5.00 -2 1 -20 -2.40 2.10 -2 1 -20 5.30 4.10 2 1 20 14.90 9.00 -3 -1 -20 -0.20 4.80 3 -1 20 15.20 9.90 3 1 20 8.20 9.90 4 -1 20 10.20 8.50 4 -2 -20 0.90 8.10 4 2 -20 2.40 6.90 3 -2 -20 6.10 6.30 -3 2 20 2.70 7.80 3 2 -20 -0.90 5.00 2 -2 -20 -1.70 4.60 -2 -2 20 -3.00 7.10 2 2 -20 1.40 4.30 -2 2 20 8.70 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-1.40 5.20 -2 -4 20 13.10 11.10 2 -4 -20 6.00 7.10 2 4 -20 5.20 4.20 -2 4 20 5.30 7.10 -1 -4 20 8.30 6.90 1 -4 -20 11.60 6.40 -1 4 20 2.80 6.10 0 -4 -20 -4.70 4.90 0 4 -20 12.90 5.80 0 4 20 0.10 6.50 -1 -4 -20 0.90 5.00 1 -4 20 4.80 6.00 -1 4 -20 -0.50 3.00 1 4 20 -9.30 5.50 -2 -4 -20 8.40 6.90 2 -4 20 12.60 8.60 2 4 20 -2.20 6.20 -3 -4 -20 -6.60 5.90 3 -4 20 0.40 8.30 3 -5 -20 10.50 8.90 -3 5 20 13.60 9.30 3 5 -20 5.90 6.30 2 -5 -20 -7.30 5.70 2 5 -20 6.20 5.00 -2 5 20 14.00 8.40 1 -5 -20 4.10 7.40 -1 -5 20 16.10 9.40 -1 5 20 5.40 5.30 0 -5 -20 -4.10 4.40 0 -5 20 2.90 7.90 0 5 -20 4.30 4.10 0 5 20 -4.90 5.40 1 -5 20 -3.10 6.10 -1 -5 -20 19.20 8.20 1 5 20 9.40 7.30 -2 -5 -20 -0.60 6.50 2 -5 20 -5.80 7.60 -2 -5 -20 4.60 3.30 3 -5 20 -7.20 8.30 -3 -5 -20 2.50 7.50 -3 -5 -20 -0.40 4.10 3 -6 -20 6.90 8.60 3 6 -20 2.10 6.00 -3 6 20 15.90 10.30 2 -6 -20 10.70 6.80 2 6 -20 1.10 4.80 -2 6 20 12.70 8.50 -1 -6 20 8.40 7.10 -1 6 20 -4.70 5.30 0 -6 20 -1.60 6.00 0 -6 -20 1.20 6.50 0 6 -20 -3.50 3.30 0 6 20 4.80 5.50 -1 -6 -20 3.60 7.20 1 -6 20 -8.80 7.30 -1 6 -20 3.00 1.30 -2 -6 -20 3.90 4.70 2 -6 20 10.80 8.90 -2 -6 -20 13.70 9.00 -3 -6 -20 17.70 9.00 3 -6 20 -14.20 8.30 2 -7 -20 -3.60 8.40 2 7 -20 2.80 5.40 -2 7 20 -0.20 8.60 1 -7 -20 19.60 11.20 -1 7 20 15.40 8.90 0 -7 20 22.00 10.40 0 -7 -20 4.30 8.30 0 7 -20 8.80 4.20 -1 -7 -20 7.10 7.60 -2 -7 -20 9.80 8.90 2 -7 20 1.00 7.40 2 -8 -20 -1.60 7.40 -2 8 20 -0.30 8.40 2 8 -20 10.70 6.40 1 -8 -20 14.10 8.40 0 -8 20 4.50 9.40 0 -8 -20 1.20 7.00 0 8 -20 1.50 2.90 1 -8 20 12.60 8.60 -1 -8 -20 0.80 8.20 -2 -8 -20 0.60 8.60 1 -9 -20 -4.30 7.20 1 9 -20 -0.80 7.30 0 -9 -20 -6.30 8.50 1 -9 20 10.90 8.70 -1 -9 -20 -3.90 8.10 3 0 -21 4.50 6.10 2 0 -21 -1.30 4.50 -2 0 21 7.10 7.20 1 0 -21 24.20 9.30 -1 0 -21 42.20 11.20 -2 0 -21 -2.70 5.20 2 0 21 15.20 11.00 -2 0 -21 5.40 3.70 3 0 21 -13.80 9.90 -3 0 -21 -2.20 2.20 3 -1 -21 -6.40 5.90 3 1 -21 12.90 7.30 2 -1 -21 11.20 6.30 -2 -1 21 15.00 7.80 2 1 -21 -3.40 4.80 -2 1 21 -6.70 6.80 1 -1 -21 19.30 8.30 -1 -1 21 19.40 11.30 1 1 -21 14.30 7.90 0 -1 -21 16.90 7.50 0 1 -21 44.80 10.60 0 1 21 19.20 8.80 1 -1 21 25.80 12.60 -1 -1 -21 33.50 10.00 -1 1 -21 41.20 9.50 1 1 21 29.40 11.30 -2 -1 -21 -1.20 2.50 -2 -1 -21 1.70 4.70 2 1 21 12.20 8.00 -2 1 -21 2.00 4.20 -2 1 -21 1.30 2.80 3 -1 21 -0.20 8.50 -3 -1 -21 9.40 6.00 3 1 21 11.50 10.20 3 -2 -21 9.10 7.60 3 2 -21 15.60 7.40 2 -2 -21 11.10 7.30 2 2 -21 -3.10 5.40 -2 2 21 -13.20 5.60 1 -2 -21 27.00 10.20 -1 -2 21 29.30 10.00 -1 2 21 33.00 10.50 1 2 -21 28.60 9.20 0 -2 -21 -1.90 4.60 0 2 -21 -0.10 4.10 1 -2 21 27.90 11.70 -1 -2 -21 32.20 10.40 1 2 21 26.90 11.20 -1 2 -21 35.10 8.80 -2 -2 -21 3.00 3.40 2 -2 21 -1.20 9.40 -2 -2 -21 11.70 7.40 -2 2 -21 9.00 3.00 2 2 21 12.90 9.10 -3 -2 -21 0.20 4.00 3 -2 21 4.30 12.30 -3 -2 -21 7.90 7.00 3 -3 -21 13.70 8.60 3 3 -21 0.10 5.00 2 -3 -21 22.10 8.90 -2 3 21 39.50 11.10 2 3 -21 13.80 7.90 1 -3 -21 6.00 5.80 -1 -3 21 5.40 7.30 1 3 -21 19.50 7.00 -1 3 21 5.10 6.60 0 -3 -21 -1.20 5.00 0 -3 21 -0.60 8.80 0 3 -21 2.00 4.30 1 -3 21 18.80 10.10 -1 -3 -21 8.00 7.30 1 3 21 -1.00 7.10 -1 3 -21 16.40 5.40 2 -3 21 24.10 13.10 -2 -3 -21 21.90 8.80 2 3 21 26.10 11.30 -3 -3 -21 -4.60 6.10 -3 -3 -21 -2.40 3.70 3 4 -21 2.30 5.20 2 -4 -21 20.90 9.50 -2 4 21 10.40 7.50 -1 -4 21 -0.10 5.70 1 -4 -21 8.50 6.70 1 4 -21 6.10 5.20 -1 4 21 17.70 8.40 0 -4 -21 10.00 8.20 0 -4 21 8.90 8.70 0 4 -21 5.30 5.40 0 4 21 1.60 6.20 -1 -4 -21 5.00 5.20 1 -4 21 12.70 8.60 1 4 21 18.50 9.50 -1 4 -21 2.40 3.70 -2 -4 -21 2.90 6.10 2 -4 21 5.90 11.10 -3 -4 -21 -5.50 6.30 3 -4 21 -15.00 12.20 3 -5 -21 14.80 10.20 2 -5 -21 3.80 7.40 -2 5 21 11.50 9.10 2 5 -21 -4.30 3.80 -1 -5 21 6.20 9.40 1 -5 -21 15.20 7.90 1 5 -21 6.10 4.90 -1 5 21 18.00 8.30 0 -5 -21 16.90 9.10 0 -5 21 16.70 9.20 0 5 -21 5.40 5.00 0 5 21 -0.20 6.70 -1 -5 -21 2.50 5.60 -1 5 -21 -0.70 2.90 -2 -5 -21 6.00 6.10 2 -5 21 10.60 9.40 -2 -5 -21 5.10 4.10 -3 -5 -21 1.00 4.40 -3 -5 -21 16.80 9.00 3 -5 21 17.00 10.80 2 -6 -21 5.00 8.40 2 6 -21 7.80 6.30 1 -6 -21 8.70 7.90 1 6 -21 3.00 5.10 0 -6 21 -13.50 7.50 0 -6 -21 4.90 7.90 0 6 -21 -5.30 3.10 1 -6 21 -6.20 6.70 -1 -6 -21 -8.90 5.20 -1 6 -21 0.70 1.30 -2 -6 -21 5.40 6.40 2 -7 -21 -13.10 7.00 2 7 -21 2.60 5.30 1 -7 -21 -5.10 6.70 1 7 -21 3.10 4.40 0 -7 21 -1.60 8.10 0 -7 -21 -6.90 5.90 0 7 -21 -1.40 3.30 -1 -7 -21 3.00 7.30 1 -7 21 -3.10 8.30 2 -7 21 3.90 9.80 -2 -7 -21 21.60 9.90 1 -8 -21 6.00 9.50 1 8 -21 2.90 5.40 0 -8 -21 9.40 11.00 0 8 -21 8.90 4.20 -1 -8 -21 8.40 9.40 1 -8 21 -1.30 7.70 0 -9 -21 13.10 9.60 2 0 -22 -0.60 5.00 -1 0 22 0.00 6.70 1 0 -22 15.80 6.80 0 0 -22 4.60 5.70 0 0 22 14.30 9.90 -1 0 -22 24.90 8.90 1 0 22 0.60 8.10 -2 0 -22 -1.10 3.10 2 0 22 -18.00 7.70 -2 0 -22 -4.70 4.50 -3 0 -22 4.60 2.80 2 -1 -22 12.80 7.50 2 1 -22 11.30 7.90 1 -1 -22 -2.80 5.80 -1 -1 22 21.40 10.80 -1 1 22 8.00 7.40 1 1 -22 -0.20 4.70 0 -1 -22 -4.30 4.40 0 -1 22 4.40 7.40 0 1 -22 3.50 5.70 0 1 22 -6.00 6.30 -1 -1 -22 29.20 10.80 1 -1 22 26.40 11.60 -1 1 -22 6.60 6.40 1 1 22 3.70 9.70 -2 -1 -22 13.00 6.90 -2 -1 -22 8.00 4.00 2 -1 22 -1.80 7.70 2 1 22 24.00 13.10 -2 1 -22 7.10 5.00 3 -1 22 -8.40 10.00 -3 -1 -22 5.10 5.10 3 -2 -22 3.60 8.70 2 -2 -22 17.90 10.60 2 2 -22 22.90 9.40 1 -2 -22 14.00 8.70 -1 -2 22 21.40 11.00 -1 2 22 23.20 8.80 1 2 -22 17.30 7.60 0 -2 22 4.80 6.00 0 -2 -22 3.80 4.80 0 2 -22 -5.20 5.10 0 2 22 -1.10 6.20 -1 -2 -22 17.50 9.10 1 -2 22 7.40 10.30 -1 2 -22 33.80 9.10 1 2 22 29.40 11.00 2 -2 22 25.30 12.50 -2 -2 -22 19.50 5.20 -2 2 -22 10.40 4.70 -2 2 -22 21.60 4.60 3 -2 22 8.80 12.40 -3 -2 -22 -3.10 5.60 -3 -2 -22 -4.20 4.30 3 -3 -22 5.10 9.10 2 -3 -22 14.10 8.80 2 3 -22 1.80 5.50 1 -3 -22 6.20 7.10 1 3 -22 2.30 5.30 -1 3 22 5.30 8.20 0 -3 22 3.60 9.20 0 -3 -22 17.80 7.90 0 3 22 10.30 7.00 0 3 -22 14.20 6.20 1 -3 22 1.00 8.50 -1 -3 -22 3.70 5.00 -1 3 -22 2.00 4.00 -2 -3 -22 5.10 7.50 2 -3 22 -1.20 10.00 3 -3 22 -3.60 11.30 -3 -3 -22 5.80 4.70 3 -4 -22 -0.40 7.90 3 4 -22 1.70 7.00 2 -4 -22 8.80 8.10 2 4 -22 10.20 6.70 1 -4 -22 0.30 6.40 1 4 -22 7.60 6.80 0 -4 -22 12.20 8.10 0 -4 22 15.50 10.00 0 4 -22 6.80 5.90 1 -4 22 -0.20 9.80 -1 -4 -22 13.90 7.80 -1 4 -22 -3.60 3.60 2 -4 22 11.00 11.10 -2 -4 -22 14.40 5.10 -2 -4 -22 14.30 8.10 3 -4 22 -22.00 9.80 -3 -4 -22 -2.50 5.40 -3 -4 -22 -2.30 7.00 1 -5 -22 0.00 7.20 1 5 -22 15.20 6.60 0 -5 -22 1.80 6.70 0 -5 22 1.70 9.20 0 5 -22 -3.90 4.00 1 -5 22 -9.40 8.70 -1 -5 -22 2.90 8.30 -2 -5 -22 2.90 7.20 2 -5 22 12.10 10.90 2 -6 -22 12.20 9.50 2 6 -22 3.90 6.50 1 -6 -22 -1.10 8.10 1 6 -22 -4.50 4.20 0 -6 -22 5.40 7.40 0 6 -22 8.30 5.00 -1 -6 -22 -1.60 6.40 1 -6 22 -10.20 8.00 -1 6 -22 1.00 1.50 2 -6 22 1.80 9.20 -2 -6 -22 3.40 9.60 1 -7 -22 10.50 9.20 1 7 -22 -7.70 4.50 0 7 -22 0.50 3.70 -1 -7 -22 0.40 7.00 0 -8 -22 -1.90 7.90 0 8 -22 0.30 3.70 3 0 -23 13.10 7.80 2 0 -23 10.00 7.00 1 0 -23 10.20 7.20 0 0 23 9.60 9.00 0 0 -23 9.70 7.50 1 0 23 11.40 9.40 -2 0 -23 -7.90 4.50 -2 0 -23 2.40 3.70 -3 0 -23 -1.20 2.50 3 -1 -23 -8.80 7.30 3 1 -23 1.20 6.90 2 -1 -23 7.50 7.40 2 1 -23 -8.30 4.80 1 -1 -23 19.80 7.80 1 1 -23 -0.60 6.80 0 -1 23 1.80 8.70 0 -1 -23 2.70 5.10 0 1 -23 7.00 6.20 -1 -1 -23 11.10 6.90 1 -1 23 21.40 12.20 -1 1 -23 15.20 8.00 2 -1 23 -7.90 8.50 -2 -1 -23 -0.50 6.20 -2 -1 -23 2.70 3.60 -2 1 -23 0.50 4.70 -2 1 -23 1.00 3.80 -3 -1 -23 -2.90 5.40 3 -2 -23 4.80 7.60 3 2 -23 4.50 6.60 2 -2 -23 2.10 8.60 2 2 -23 15.20 7.70 1 -2 -23 -5.10 6.40 1 2 -23 1.10 6.10 0 -2 -23 12.20 7.80 0 -2 23 8.60 10.60 0 2 -23 29.80 9.90 1 -2 23 15.70 10.80 -1 -2 -23 10.10 6.90 -1 2 -23 -0.80 4.40 -2 -2 -23 -0.10 7.70 2 -2 23 26.90 12.70 -2 2 -23 4.00 3.60 -2 2 -23 4.10 3.40 -3 -2 -23 -2.40 5.00 -3 -2 -23 3.60 6.30 2 -3 -23 4.10 7.20 2 3 -23 20.60 9.60 1 -3 -23 6.30 6.70 0 -3 -23 16.50 8.40 1 -3 23 3.50 10.20 -1 -3 -23 -9.40 5.00 -1 3 -23 8.50 4.90 2 -3 23 22.40 13.20 -2 -3 -23 24.20 6.30 -2 -3 -23 9.90 7.90 2 -4 -23 5.60 8.50 2 4 -23 5.20 6.40 1 -4 -23 -2.10 6.90 1 4 -23 6.20 5.80 0 -4 -23 3.40 8.10 0 4 -23 6.00 5.50 -1 -4 -23 4.60 6.50 1 -4 23 5.10 9.10 -1 4 -23 2.90 4.40 -2 -4 -23 8.40 4.20 2 -4 23 1.60 11.20 -2 -4 -23 5.30 7.20 2 -5 -23 -3.10 9.10 2 5 -23 -8.40 6.20 1 -5 -23 3.40 7.60 1 5 -23 2.00 5.30 0 -5 -23 6.20 7.40 0 5 -23 8.90 5.10 -1 -5 -23 11.60 7.50 -1 5 -23 -0.60 4.10 -2 -5 -23 -12.20 8.80 2 -5 23 -1.10 12.30 1 -6 -23 -16.40 6.90 1 6 -23 4.00 5.40 0 6 -23 7.00 4.70 -1 -6 -23 -1.20 8.00 1 -7 -23 -2.10 8.90 1 7 -23 -7.20 4.80 0 -7 -23 -8.60 8.50 0 7 -23 1.70 4.50 -1 -7 -23 3.10 10.30 2 0 -24 -12.90 6.10 1 0 -24 -6.30 5.30 0 0 -24 -0.10 6.80 -1 0 -24 -1.40 5.80 -2 0 -24 5.40 5.80 -2 0 -24 8.20 4.50 2 -1 -24 -9.40 6.90 2 1 -24 5.20 7.30 1 -1 -24 10.00 8.20 1 1 -24 16.00 7.60 0 -1 -24 6.10 7.50 0 1 -24 2.30 6.20 -1 -1 -24 1.80 7.40 -1 1 -24 1.00 7.00 -2 -1 -24 2.80 3.70 -2 1 -24 -6.00 3.60 -2 1 -24 -4.80 4.40 2 -2 -24 -4.20 7.50 2 2 -24 -0.20 6.90 1 -2 -24 12.30 9.10 1 2 -24 18.00 8.80 0 -2 -24 19.20 8.00 0 2 -24 -1.60 6.10 -1 -2 -24 12.80 8.10 -1 2 -24 4.20 5.90 -2 -2 -24 10.30 8.40 -2 2 -24 14.50 4.90 -2 2 -24 14.90 4.30 2 -3 -24 18.70 8.90 2 3 -24 1.40 6.20 1 -3 -24 22.70 9.50 1 3 -24 -6.30 6.60 0 -3 -24 -16.70 6.30 0 3 -24 -4.80 5.70 -1 -3 -24 1.40 7.40 -1 3 -24 7.50 5.20 -2 -3 -24 9.70 5.00 -2 -3 -24 14.40 8.90 2 -4 -24 12.60 8.70 2 4 -24 -4.00 7.60 1 -4 -24 3.60 7.40 1 4 -24 -2.30 6.50 0 -4 -24 0.70 8.00 0 4 -24 5.70 9.40 -1 -4 -24 -2.30 7.20 -1 4 -24 5.30 4.60 -2 -4 -24 28.80 10.90 1 -5 -24 2.60 7.90 1 5 -24 7.70 7.50 0 -5 -24 11.60 9.60 0 5 -24 4.80 5.70 -1 -5 -24 4.50 7.40 -1 5 -24 3.10 5.00 0 -6 -24 -13.10 7.90 0 6 -24 10.90 5.20 2 0 -25 4.40 8.80 1 0 -25 -0.20 7.10 0 0 -25 2.70 7.50 -1 0 -25 -1.70 6.80 -2 0 -25 0.70 4.20 -2 0 -25 2.80 6.00 2 -1 -25 12.30 8.50 2 1 -25 -0.90 6.30 1 -1 -25 -12.00 6.50 1 1 -25 5.60 6.50 0 -1 -25 -6.60 7.30 0 1 -25 -1.00 6.70 -1 -1 -25 -7.90 6.80 -1 1 -25 1.70 5.80 -2 -1 -25 -0.80 7.40 -2 1 -25 3.10 4.60 -2 1 -25 1.70 5.30 2 -2 -25 -5.40 7.60 2 2 -25 -2.50 6.50 1 -2 -25 -5.70 7.50 1 2 -25 2.20 7.70 0 -2 -25 9.40 8.10 0 2 -25 -1.90 5.70 -1 -2 -25 -3.00 6.50 -1 2 -25 1.20 6.10 -2 -2 -25 -0.60 4.70 -2 -2 -25 -9.40 7.20 -2 2 -25 0.90 4.20 -2 2 -25 2.30 3.50 1 -3 -25 4.00 8.30 1 3 -25 0.00 6.00 0 -3 -25 10.80 7.30 0 3 -25 -0.20 6.00 -1 -3 -25 -0.20 8.80 -1 3 -25 -8.00 4.80 1 -4 -25 2.20 8.00 1 4 -25 4.50 7.40 0 4 -25 -4.10 5.50 -1 -4 -25 7.20 8.90 -1 4 -25 -5.30 4.20 0 -5 -25 -0.90 8.70 1 0 -26 10.40 8.50 0 0 -26 11.00 9.60 -1 0 -26 7.80 8.10 1 1 -26 8.50 7.00 0 -1 -26 11.80 8.80 0 1 -26 -3.30 5.50 -1 -1 -26 2.90 8.70 -1 1 -26 0.00 7.10 1 -2 -26 2.20 8.00 1 2 -26 16.70 9.10 0 -2 -26 7.10 9.10 0 2 -26 2.10 6.40 -1 -2 -26 -0.20 8.70 0 3 -26 0.40 6.80 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 94902 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, 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_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 F1 F 1.0796(8) 0.3167(3) 0.86465(16) 0.0998(11) Uani 1 1 d . . . . . F2 F 0.8550(5) 0.1713(2) 0.65743(14) 0.0691(8) Uani 1 1 d . . . . . F3 F 1.1621(6) 0.1610(3) 0.76580(18) 0.0886(10) Uani 1 1 d . . . . . F4 F 0.3658(6) 0.4926(2) 0.74794(15) 0.0750(8) Uani 1 1 d . . . . . F5 F 0.6778(8) 0.4837(3) 0.85475(16) 0.0936(11) Uani 1 1 d . . . . . O1 O 0.2044(7) 0.2923(3) 0.5140(2) 0.0821(12) Uani 1 1 d . . . . . H1 H 0.3563 0.2841 0.4980 0.123 Uiso 1 1 calc R U . . . C1 C 0.9255(11) 0.3221(5) 0.8108(3) 0.0690(13) Uani 1 1 d . . . . . C2 C 0.7235(11) 0.4072(4) 0.8055(3) 0.0643(13) Uani 1 1 d . . . . . C3 C 0.5693(9) 0.4111(4) 0.7495(2) 0.0572(11) Uani 1 1 d . . . . . C4 C 0.6042(9) 0.3351(3) 0.6972(2) 0.0512(10) Uani 1 1 d . . . . . C5 C 0.4328(9) 0.3321(4) 0.6385(2) 0.0552(11) Uani 1 1 d . . . . . H5 H 0.3741 0.2572 0.6251 0.066 Uiso 1 1 calc R U . . . C6 C 0.3508(9) 0.4231(4) 0.6020(2) 0.0537(11) Uani 1 1 d . . . . . C7 C 0.4294(13) 0.5522(4) 0.6070(3) 0.0744(15) Uani 1 1 d . . . . . H7A H 0.6227 0.5602 0.6155 0.089 Uiso 1 1 calc R U . . . H7B H 0.3295 0.5911 0.6420 0.089 Uiso 1 1 calc R U . . . C8 C 0.3568(19) 0.6055(5) 0.5415(3) 0.118(3) Uani 1 1 d . . . . . H8A H 0.2049 0.6600 0.5462 0.142 Uiso 1 1 calc R U . . . H8B H 0.5106 0.6491 0.5239 0.142 Uiso 1 1 calc R U . . . C9 C 0.8101(9) 0.2504(4) 0.7056(2) 0.0542(11) Uani 1 1 d . . . . . C10 C 0.9665(10) 0.2437(4) 0.7602(3) 0.0618(12) Uani 1 1 d . . . . . C11 C 0.1822(10) 0.4074(4) 0.5418(3) 0.0674(13) Uani 1 1 d . . . . . H11 H -0.0088 0.4225 0.5528 0.081 Uiso 1 1 calc R U . . . C12 C 0.282(2) 0.5056(6) 0.4971(3) 0.110(2) Uani 1 1 d . . . . . H12A H 0.4389 0.4792 0.4721 0.132 Uiso 1 1 calc R U . . . H12B H 0.1402 0.5298 0.4668 0.132 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 F1 0.118(3) 0.106(2) 0.076(2) 0.0098(19) -0.030(2) -0.017(2) F2 0.0760(17) 0.0548(13) 0.0764(19) -0.0085(14) 0.0081(15) 0.0069(13) F3 0.0874(19) 0.0746(18) 0.104(2) 0.0168(17) -0.0130(19) 0.0146(18) F4 0.0768(17) 0.0671(16) 0.081(2) -0.0178(15) 0.0124(18) 0.0105(15) F5 0.122(3) 0.094(2) 0.064(2) -0.0275(17) 0.0080(19) -0.012(2) O1 0.0529(17) 0.097(3) 0.096(3) -0.043(2) -0.0047(19) 0.0053(18) C1 0.078(3) 0.073(3) 0.056(3) 0.011(3) -0.004(3) -0.019(3) C2 0.079(3) 0.060(3) 0.053(3) -0.007(3) 0.008(3) -0.016(3) C3 0.062(3) 0.049(2) 0.060(3) -0.001(2) 0.010(3) -0.003(2) C4 0.054(2) 0.044(2) 0.056(3) 0.002(2) 0.004(2) -0.0074(19) C5 0.054(2) 0.050(2) 0.062(3) -0.011(2) 0.010(2) -0.009(2) C6 0.051(2) 0.053(2) 0.058(3) -0.010(2) 0.002(2) 0.001(2) C7 0.092(3) 0.053(2) 0.078(4) -0.003(3) -0.002(3) -0.003(3) C8 0.178(8) 0.077(4) 0.101(5) 0.019(4) -0.040(6) -0.011(5) C9 0.058(2) 0.048(2) 0.057(3) -0.001(2) 0.010(2) -0.006(2) C10 0.064(3) 0.056(2) 0.066(3) 0.008(2) 0.002(3) -0.006(2) C11 0.057(3) 0.073(3) 0.072(3) -0.021(3) -0.009(3) 0.007(2) C12 0.149(7) 0.102(5) 0.079(5) 0.014(4) -0.035(4) -0.015(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C11 O1 H1 109.5 . . ? F1 C1 C2 120.2(5) . . ? F1 C1 C10 120.5(5) . . ? C10 C1 C2 119.3(5) . . ? F5 C2 C1 120.3(5) . . ? F5 C2 C3 120.8(5) . . ? C3 C2 C1 119.0(5) . . ? F4 C3 C2 116.7(4) . . ? F4 C3 C4 119.5(4) . . ? C2 C3 C4 123.8(4) . . ? C3 C4 C5 125.2(4) . . ? C3 C4 C9 114.5(4) . . ? C9 C4 C5 120.1(4) . . ? C4 C5 H5 116.0 . . ? C6 C5 C4 128.0(4) . . ? C6 C5 H5 116.0 . . ? C5 C6 C7 128.7(4) . . ? C5 C6 C11 122.7(4) . . ? C11 C6 C7 108.2(4) . . ? C6 C7 H7A 110.7 . . ? C6 C7 H7B 110.7 . . ? C6 C7 C8 105.1(5) . . ? H7A C7 H7B 108.8 . . ? C8 C7 H7A 110.7 . . ? C8 C7 H7B 110.7 . . ? C7 C8 H8A 110.2 . . ? C7 C8 H8B 110.2 . . ? H8A C8 H8B 108.5 . . ? C12 C8 C7 107.5(5) . . ? C12 C8 H8A 110.2 . . ? C12 C8 H8B 110.2 . . ? F2 C9 C4 118.5(4) . . ? F2 C9 C10 118.2(4) . . ? C10 C9 C4 123.3(4) . . ? F3 C10 C1 119.0(5) . . ? F3 C10 C9 121.0(5) . . ? C9 C10 C1 120.0(5) . . ? O1 C11 C6 113.2(4) . . ? O1 C11 H11 108.9 . . ? O1 C11 C12 113.4(5) . . ? C6 C11 H11 108.9 . . ? C6 C11 C12 103.4(4) . . ? C12 C11 H11 108.9 . . ? C8 C12 C11 105.1(5) . . ? C8 C12 H12A 110.7 . . ? C8 C12 H12B 110.7 . . ? C11 C12 H12A 110.7 . . ? C11 C12 H12B 110.7 . . ? H12A C12 H12B 108.8 . . ? 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 F1 C1 1.336(6) . ? F2 C9 1.342(5) . ? F3 C10 1.341(5) . ? F4 C3 1.355(5) . ? F5 C2 1.340(5) . ? O1 H1 0.8200 . ? O1 C11 1.414(5) . ? C1 C2 1.382(7) . ? C1 C10 1.371(7) . ? C2 C3 1.372(7) . ? C3 C4 1.377(6) . ? C4 C5 1.465(6) . ? C4 C9 1.399(6) . ? C5 H5 0.9300 . ? C5 C6 1.325(6) . ? C6 C7 1.502(6) . ? C6 C11 1.492(7) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 C8 1.507(8) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 C12 1.488(8) . ? C9 C10 1.355(7) . ? C11 H11 0.9800 . ? C11 C12 1.512(8) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? 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 F1 C1 C2 F5 -1.1(7) . . . . ? F1 C1 C2 C3 179.6(5) . . . . ? F1 C1 C10 F3 0.5(7) . . . . ? F1 C1 C10 C9 -179.6(4) . . . . ? F2 C9 C10 F3 0.4(6) . . . . ? F2 C9 C10 C1 -179.4(4) . . . . ? F4 C3 C4 C5 -1.4(6) . . . . ? F4 C3 C4 C9 -176.5(4) . . . . ? F5 C2 C3 F4 -2.2(6) . . . . ? F5 C2 C3 C4 -179.7(4) . . . . ? O1 C11 C12 C8 -156.0(6) . . . . ? C1 C2 C3 F4 177.1(4) . . . . ? C1 C2 C3 C4 -0.4(7) . . . . ? C2 C1 C10 F3 -179.7(4) . . . . ? C2 C1 C10 C9 0.2(7) . . . . ? C2 C3 C4 C5 176.0(4) . . . . ? C2 C3 C4 C9 0.9(6) . . . . ? C3 C4 C5 C6 47.5(7) . . . . ? C3 C4 C9 F2 178.9(4) . . . . ? C3 C4 C9 C10 -0.9(6) . . . . ? C4 C5 C6 C7 5.9(8) . . . . ? C4 C5 C6 C11 178.0(4) . . . . ? C4 C9 C10 F3 -179.8(4) . . . . ? C4 C9 C10 C1 0.4(7) . . . . ? C5 C4 C9 F2 3.5(6) . . . . ? C5 C4 C9 C10 -176.3(4) . . . . ? C5 C6 C7 C8 160.9(6) . . . . ? C5 C6 C11 O1 -22.5(7) . . . . ? C5 C6 C11 C12 -145.6(5) . . . . ? C6 C7 C8 C12 -9.0(9) . . . . ? C6 C11 C12 C8 -33.0(8) . . . . ? C7 C6 C11 O1 151.1(4) . . . . ? C7 C6 C11 C12 28.0(6) . . . . ? C7 C8 C12 C11 26.3(9) . . . . ? C9 C4 C5 C6 -137.6(5) . . . . ? C10 C1 C2 F5 179.1(5) . . . . ? C10 C1 C2 C3 -0.2(7) . . . . ? C11 C6 C7 C8 -12.1(6) . . . . ?