#------------------------------------------------------------------------------ #$Date: 2019-05-21 06:25:46 +0300 (Tue, 21 May 2019) $ #$Revision: 215343 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/15/68/7156872.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_7156872 loop_ _publ_author_name 'Warner, Andrew' 'Enright, Kieron M.' 'Cole, John M.' 'Yuan, Kang' 'McGough, John S.' 'Ingleson, Michael James' _publ_section_title ; Borylative Cyclisation of Diynes using BCl3 and Borocations ; _journal_name_full 'Organic & Biomolecular Chemistry' _journal_paper_doi 10.1039/C9OB00991D _journal_year 2019 _chemical_formula_moiety 'C28 H21 B F4 O2' _chemical_formula_sum 'C28 H21 B F4 O2' _chemical_formula_weight 476.30 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_primary iterative _audit_creation_date 2016-11-29 _audit_creation_method ; Olex2 1.2 (compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227) ; _audit_update_record ; 2017-01-26 deposited with the CCDC. 2019-05-20 downloaded from the CCDC. ; _cell_angle_alpha 74.768(7) _cell_angle_beta 73.263(6) _cell_angle_gamma 72.295(6) _cell_formula_units_Z 2 _cell_length_a 8.1811(5) _cell_length_b 12.0413(9) _cell_length_c 12.5311(10) _cell_measurement_reflns_used 2353 _cell_measurement_temperature 150.02(10) _cell_measurement_theta_max 26.6290 _cell_measurement_theta_min 3.7470 _cell_volume 1105.21(15) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'olex2.refine (Bourhis et al., 2015)' _computing_structure_solution ; Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008; Palatinus et al., 2012) ; _diffrn_ambient_temperature 150.02(10) _diffrn_detector_area_resol_mean 8.0714 _diffrn_measured_fraction_theta_full 0.9982 _diffrn_measured_fraction_theta_max 0.8370 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 3.00 83.00 1.0000 3.4400 omega____ theta____ kappa____ phi______ frames - 18.8601 57.0000 -60.0000 80 #__ type_ start__ end____ width___ exp.time_ 2 omega -12.00 45.00 1.0000 3.4400 omega____ theta____ kappa____ phi______ frames - 18.8601 80.0000 21.0000 57 #__ type_ start__ end____ width___ exp.time_ 3 omega -40.00 36.00 1.0000 3.4400 omega____ theta____ kappa____ phi______ frames - 18.8601 -57.0000 60.0000 76 #__ type_ start__ end____ width___ exp.time_ 4 omega -54.00 55.00 1.0000 3.4400 omega____ theta____ kappa____ phi______ frames - 18.8601 -19.0000 120.0000 109 #__ type_ start__ end____ width___ exp.time_ 5 omega 18.00 59.00 1.0000 3.4400 omega____ theta____ kappa____ phi______ frames - 18.8601 -99.0000 -180.0000 41 ; _diffrn_measurement_device_type 'SuperNova, Single source at offset), Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0181825000 _diffrn_orient_matrix_UB_12 -0.0537585000 _diffrn_orient_matrix_UB_13 0.0396588000 _diffrn_orient_matrix_UB_21 -0.0226020000 _diffrn_orient_matrix_UB_22 -0.0301560000 _diffrn_orient_matrix_UB_23 -0.0331613000 _diffrn_orient_matrix_UB_31 0.0888195000 _diffrn_orient_matrix_UB_32 -0.0130568000 _diffrn_orient_matrix_UB_33 -0.0309007000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_unetI/netI 0.0778 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 8344 _diffrn_reflns_theta_full 29.2123 _diffrn_reflns_theta_max 29.21 _diffrn_reflns_theta_min 3.46 _diffrn_source 'SuperNova (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.111 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.80288 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'dark brown' _exptl_crystal_colour_modifier dark _exptl_crystal_colour_primary brown _exptl_crystal_density_diffrn 1.4311 _exptl_crystal_description plate _exptl_crystal_F_000 492.3293 _exptl_crystal_recrystallization_method 'Slow evaporation of a solution in toluene' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.4045 _refine_diff_density_min -0.4577 _refine_diff_density_rms 0.1071 _refine_ls_d_res_high 0.7281 _refine_ls_d_res_low 5.8885 _refine_ls_goodness_of_fit_ref 1.0502 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_constraints 34 _refine_ls_number_parameters 319 _refine_ls_number_reflns 4969 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.0502 _refine_ls_R_factor_all 0.0989 _refine_ls_R_factor_gt 0.0587 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0370P)^2^+0.6160P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1168 _refine_ls_wR_factor_ref 0.1433 _reflns_Friedel_coverage 0.0 _reflns_limit_h_max 10 _reflns_limit_h_min -10 _reflns_limit_k_max 15 _reflns_limit_k_min -14 _reflns_limit_l_max 16 _reflns_limit_l_min 0 _reflns_number_gt 3160 _reflns_number_total 4969 _reflns_threshold_expression I>=2u(I) _iucr_refine_instructions_details ; TITL amji373 in P-1 CELL 0.71073 8.181101 12.04125 12.53114 74.7683 73.2626 72.295 ZERR 2 0.000526 0.000898 0.000945 0.0065 0.0061 0.0062 LATT 1 SFAC C H B O F UNIT 50 0 8 4 8 ACTA WGHT 0.037 0.616 FVAR 5.605266 REM REM REM F2 5 0.24584 1.24364 0.80326 11.00000 0.03705 0.02417 0.02521 = -0.00006 -0.00974 -0.00886 F4 5 0.27802 0.98942 1.23099 11.00000 0.04240 0.02854 0.02216 = -0.00255 -0.01279 -0.00944 F5 5 0.29626 1.33986 0.95921 11.00000 0.04226 0.02261 0.03318 = -0.00512 -0.00643 -0.01322 F8 5 0.31930 1.21197 1.16901 11.00000 0.04483 0.03272 0.03362 = -0.01209 -0.01230 -0.01410 O2 4 0.36116 0.74284 1.22653 11.00000 0.03347 0.02165 0.02496 = 0.00153 -0.01188 -0.00890 O3 4 0.17070 0.67416 1.17341 11.00000 0.03623 0.02724 0.02817 = 0.00298 -0.01301 -0.01518 C1 1 0.17989 0.85196 0.78059 11.00000 0.01755 0.02210 0.02476 = -0.00683 -0.00445 -0.00341 C3 1 0.22452 0.97967 0.87092 11.00000 0.01505 0.02081 0.02423 = -0.00521 -0.00489 -0.00335 C5 1 0.20496 0.87049 0.95368 11.00000 0.01857 0.02218 0.02084 = -0.00328 -0.00485 -0.00443 C8 1 0.25948 0.99167 1.04431 11.00000 0.01772 0.02147 0.02055 = -0.00495 -0.00327 -0.00384 C10 1 0.25102 1.04909 0.65527 11.00000 0.02151 0.02108 0.01995 = -0.00461 -0.00468 -0.00245 C12 1 0.39140 1.10275 0.62492 11.00000 0.02684 0.02718 0.02178 = -0.00557 -0.00550 -0.00642 AFIX 43 H12 2 0.45693 1.09384 0.67753 11.00000 -1.20000 AFIX 0 C13 1 0.17291 0.79096 0.89446 11.00000 0.01865 0.02242 0.02286 = -0.00489 -0.00555 -0.00307 C15 1 0.11400 0.62766 0.84966 11.00000 0.03055 0.02256 0.03062 = -0.00684 -0.00775 -0.00922 AFIX 43 H15 2 0.08924 0.55340 0.87219 11.00000 -1.20000 AFIX 0 C17 1 0.21625 0.97044 0.76574 11.00000 0.01668 0.02342 0.02410 = -0.00498 -0.00480 -0.00173 C20 1 0.27982 1.04516 1.12198 11.00000 0.02248 0.02427 0.01814 = -0.00161 -0.00598 -0.00411 C22 1 0.25430 1.05770 0.93161 11.00000 0.01724 0.02218 0.02163 = -0.00332 -0.00514 -0.00428 C23 1 0.16030 0.79740 0.70185 11.00000 0.02427 0.02779 0.02175 = -0.00318 -0.00591 -0.00728 AFIX 43 H23 2 0.17021 0.83493 0.62608 11.00000 -1.20000 AFIX 0 C26 1 0.23231 0.87220 1.05569 11.00000 0.01995 0.02131 0.02146 = -0.00364 -0.00431 -0.00488 C27 1 0.28837 1.22514 0.98517 11.00000 0.02338 0.01609 0.02906 = -0.00258 -0.00479 -0.00654 C29 1 0.15285 1.06639 0.57428 11.00000 0.02800 0.02552 0.02835 = -0.00361 -0.01029 -0.00452 AFIX 43 H29 2 0.05662 1.03352 0.59344 11.00000 -1.20000 AFIX 0 C32 1 0.26412 1.17443 0.90486 11.00000 0.02131 0.02109 0.02096 = 0.00021 -0.00390 -0.00613 C34 1 0.29720 1.16097 1.09211 11.00000 0.02380 0.02330 0.02702 = -0.00984 -0.00664 -0.00693 C36 1 0.12545 0.68519 0.73834 11.00000 0.02820 0.02858 0.02857 = -0.01094 -0.00637 -0.00902 AFIX 43 H36 2 0.10971 0.64873 0.68644 11.00000 -1.20000 AFIX 0 C38 1 0.33580 0.63567 1.31106 11.00000 0.03198 0.02103 0.02044 = 0.00024 -0.00660 -0.00464 C39 1 0.13926 0.67972 0.92958 11.00000 0.02575 0.02258 0.02514 = -0.00289 -0.00719 -0.00380 AFIX 43 H39 2 0.13348 0.64022 1.00458 11.00000 -1.20000 AFIX 0 C42 1 0.19789 1.13196 0.46607 11.00000 0.03654 0.03008 0.02482 = -0.00234 -0.01348 -0.00145 AFIX 43 H42 2 0.13285 1.14201 0.41288 11.00000 -1.20000 AFIX 0 C44 1 0.25394 0.57376 1.25197 11.00000 0.03635 0.02342 0.02716 = 0.00158 -0.00864 -0.01108 C45 1 0.43372 1.16930 0.51674 11.00000 0.03187 0.03305 0.02788 = -0.00483 -0.00109 -0.01196 AFIX 43 H45 2 0.52660 1.20535 0.49783 11.00000 -1.20000 AFIX 0 C48 1 0.39005 0.48969 1.17896 11.00000 0.06305 0.02653 0.03569 = -0.00716 -0.01226 -0.01356 AFIX 137 H48a 2 0.33224 0.46263 1.13762 11.00000 -1.50000 H48b 2 0.47393 0.53063 1.12650 11.00000 -1.50000 H48c 2 0.44983 0.42279 1.22669 11.00000 -1.50000 AFIX 0 C50 1 0.33980 1.18252 0.43719 11.00000 0.04237 0.02705 0.02119 = -0.00062 -0.00444 -0.00674 AFIX 43 H50 2 0.37144 1.22525 0.36424 11.00000 -1.20000 AFIX 0 C51 1 0.51338 0.56476 1.33639 11.00000 0.03922 0.02886 0.03318 = -0.00137 -0.01257 -0.00344 AFIX 137 H51a 2 0.59720 0.55149 1.26662 11.00000 -1.50000 H51b 2 0.55314 0.60823 1.37390 11.00000 -1.50000 H51c 2 0.50198 0.48977 1.38465 11.00000 -1.50000 AFIX 0 B4 3 0.25278 0.76311 1.15541 11.00000 0.02178 0.02408 0.02226 = -0.00882 -0.00022 -0.00700 C52 1 0.21132 0.67670 1.41715 11.00000 0.04797 0.04165 0.02895 = -0.01101 -0.00545 -0.00489 AFIX 137 H52a 2 0.25992 0.72622 1.44185 11.00000 -1.50000 H52b 2 0.09934 0.72101 1.40050 11.00000 -1.50000 H52c 2 0.19602 0.60881 1.47612 11.00000 -1.50000 AFIX 0 C53 1 0.11152 0.51480 1.32971 11.00000 0.05582 0.04596 0.04218 = 0.01006 -0.01216 -0.03240 AFIX 137 H53a 2 0.01628 0.57319 1.36428 11.00000 -1.50000 H53b 2 0.06874 0.47933 1.28639 11.00000 -1.50000 H53c 2 0.15931 0.45452 1.38769 11.00000 -1.50000 AFIX 0 HKLF 4 END Q1 1 0.266667 1.022222 0.977778 11 0.05 0.4 Q2 1 0.566667 1.266667 1.111111 11 0.05 0.4 Q3 1 0.233333 1.022222 1.088889 11 0.05 0.4 Q4 1 0.1 1.133333 1.111111 11 0.05 0.39 Q5 1 0.166667 0.911111 0.755556 11 0.05 0.39 Q6 1 0.266667 0.666667 1.533333 11 0.05 0.39 Q7 1 0.433333 1.066667 1.111111 11 0.05 0.38 Q8 1 0.266667 0.355556 1.222222 11 0.05 0.37 Q9 1 0 0.555556 1.355556 11 0.05 0.37 Q10 1 0.133333 1.244444 0.711111 11 0.05 0.36 Q11 1 -0.033333 1.044444 0.622222 11 0.05 0.36 Q12 1 0.1 0.733333 1.422222 11 0.05 0.36 Q13 1 0.233333 1.022222 0.6 11 0.05 0.36 Q14 1 0.4 1.288889 0.288889 11 0.05 0.35 Q15 1 0.4 0.333333 1.155556 11 0.05 0.34 Q16 1 0.266667 0.933333 1.044444 11 0.05 0.34 Q17 1 0.3 1.4 1.022222 11 0.05 0.34 Q18 1 0.266667 1.022222 0.888889 11 0.05 0.34 Q19 1 0.266667 1.4 0.888889 11 0.05 0.34 Q20 1 0.4 0.577778 1.355556 11 0.05 0.33 REM The information below was added by Olex2. REM REM R1 = 0.0587 for 3160 Fo > 4sig(Fo) and 0.0989 for all 4969 data REM 319 parameters refined using 0 restraints REM Highest difference peak 0.4045, deepest hole -0.4577 REM Mean Shift 0.0000, Max Shift 0.0000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0989 REM R1_gt = 0.0587 REM wR_ref = 0.1433 REM GOOF = 1.0502 REM Shift_max = 0.0000 REM Shift_mean = 0.0000 REM Reflections_all = 4969 REM Reflections_gt = 3160 REM Parameters = 319 REM Hole = -0.4577 REM Peak = 0.4045 REM Flack = n/a ; _cod_data_source_file c9ob00991d2.cif _cod_data_source_block amji373 _cod_database_code 7156872 _chemical_oxdiff_formula C28H21BF4O2 _chemical_oxdiff_usercomment 'AJW f5-dibenzopentalene(Ph)(BPin)' _reflns_odcompleteness_completeness 99.82 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Aromatic/amide H refined with riding coordinates: C39(H39), C15(H15), C36(H36), C23(H23), C29(H29), C42(H42), C50(H50), C45(H45), C12(H12) 2.b Idealised Me refined as rotating group: C48(H48a,H48b,H48c), C51(H51a,H51b,H51c), C52(H52a,H52b,H52c), C53(H53a,H53b, H53c) ; _iucr_refine_fcf_details ; data_amji373_CCDC1 _computing_structure_refinement 'olex2.refine (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,-z _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 _cell_length_a 8.1811(5) _cell_length_b 12.0413(9) _cell_length_c 12.5311(10) _cell_angle_alpha 74.768(7) _cell_angle_beta 73.263(6) _cell_angle_gamma 72.295(6) _cell_volume 1105.21(15) 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 -10 -5 1 19.591 30.177 13.944 23.245 o -10 -4 1 44.013 34.695 14.058 21.625 o -10 -4 2 66.810 89.407 22.350 8.805 o -10 -3 1 88.590 67.129 19.806 10.781 o -9 -8 1 111.324 114.218 25.081 6.804 o -9 -7 1 153.242 178.201 30.998 4.441 o -9 -7 2 155.900 172.925 30.610 4.540 o -9 -6 1 24.779 40.721 14.908 20.113 o -9 -6 2 10.530 28.842 13.397 25.608 o -9 -6 3 14.400 10.887 9.006 54.389 o -9 -5 1 0.213 4.899 5.297 166.969 o -9 -5 2 84.010 125.083 26.055 6.472 o -9 -5 3 122.295 107.605 23.873 7.363 o -9 -5 4 3.713 16.582 9.383 52.314 o -9 -4 1 25.682 13.861 7.058 76.240 o -9 -4 2 4.688 -1.938 4.308 237.446 o -9 -4 3 6.638 8.416 7.438 81.340 o -9 -4 4 10.255 1.330 4.932 168.567 o -9 -4 5 9.966 7.786 7.943 70.651 o -9 -3 1 0.070 -13.010 8.604 65.727 o -9 -3 2 48.267 23.009 10.897 33.465 o -9 -3 3 0.706 -0.162 4.915 199.155 o -9 -3 4 2.370 -0.125 3.448 378.311 o -9 -2 1 2.634 8.066 7.847 75.669 o -9 -2 2 11.801 8.843 9.179 53.446 o -9 -2 3 2.263 2.191 2.474 648.535 o -9 -2 4 5.643 2.716 4.738 192.029 o -9 -1 1 9.965 4.135 6.405 105.698 o -9 -1 2 19.686 23.516 12.562 28.414 o -9 -1 3 7.646 -3.909 5.284 156.569 o -9 -1 4 4.247 -6.339 8.225 70.138 o -9 0 1 38.215 32.400 13.351 24.051 o -9 0 2 2.590 0.041 7.826 78.117 o -9 0 3 38.469 46.444 16.357 16.491 o -9 0 4 3.342 13.028 9.065 56.416 o -9 1 1 8.655 -3.882 9.663 50.201 o -9 1 2 0.058 -19.367 10.554 43.690 o -9 1 3 19.155 22.051 11.223 35.048 o -9 1 4 5.443 -1.510 6.296 116.198 o -9 1 5 23.850 45.654 14.909 20.051 o -9 2 1 86.332 81.186 20.561 10.044 o -9 2 2 20.098 29.891 13.454 24.819 o -8 -11 1 24.148 27.583 13.339 25.044 o -8 -11 2 48.550 53.237 16.576 15.751 o -8 -10 1 39.585 53.981 18.159 13.530 o -8 -10 2 5.399 2.654 3.217 370.427 o -8 -10 3 1.582 0.540 3.462 381.866 o -8 -9 1 152.384 100.966 22.866 7.712 o -8 -9 2 3.847 3.576 10.960 39.755 o -8 -9 3 10.455 6.124 10.137 44.900 o -8 -8 1 4.562 8.200 8.061 70.972 o -8 -8 2 4.999 -10.522 5.748 138.644 o -8 -8 3 15.561 13.297 9.143 52.335 o -8 -8 4 7.453 25.254 11.778 33.070 o -8 -7 1 205.994 214.382 31.940 4.028 o -8 -7 2 0.244 3.453 2.956 509.735 o -8 -7 3 47.373 59.811 18.470 12.930 o -8 -7 4 25.789 25.697 14.610 21.145 o -8 -6 1 6.313 2.344 6.122 119.937 o -8 -6 2 28.941 3.448 6.261 92.972 o -8 -6 3 34.586 32.187 13.435 23.995 o -8 -6 4 29.049 52.253 18.206 13.676 o -8 -5 1 7.729 10.047 7.394 81.114 o -8 -5 2 7.398 11.579 7.596 77.007 o -8 -5 3 55.844 73.376 13.725 21.020 o -8 -5 4 0.026 5.085 6.027 130.211 o -8 -5 5 7.931 22.464 13.287 26.363 o -8 -4 1 462.334 438.827 43.604 1.976 o -8 -4 2 82.645 84.701 19.666 10.876 o -8 -4 3 8.516 9.345 8.368 64.435 o -8 -4 4 23.663 17.098 10.499 39.228 o -8 -4 5 26.609 6.911 5.614 109.603 o -8 -3 1 119.582 120.697 22.465 8.137 o -8 -3 2 218.694 285.521 34.812 3.381 o -8 -3 3 40.587 28.885 12.155 28.273 o -8 -3 4 8.212 4.771 4.728 181.801 o -8 -3 5 44.806 26.325 14.095 21.683 o -8 -2 1 27.469 26.007 10.802 36.245 o -8 -2 2 0.416 -0.066 3.542 382.802 o -8 -2 3 10.959 16.957 8.102 65.909 o -8 -2 4 1.509 7.941 6.794 100.513 o -8 -2 5 1.523 -0.611 2.464 726.959 o -8 -1 1 45.420 64.990 15.664 17.320 o -8 -1 2 1.406 -3.606 4.679 216.645 o -8 -1 3 11.061 5.107 3.906 232.268 o -8 -1 4 0.012 4.257 4.647 216.598 o -8 -1 5 1.820 1.527 3.553 355.563 o -8 -1 6 4.119 5.893 10.339 44.321 o -8 0 1 16.338 6.884 12.546 29.368 o -8 0 2 12.650 5.062 2.541 379.320 o -8 0 3 2.971 4.013 5.331 159.730 o -8 0 4 69.575 125.461 23.783 7.720 o -8 0 5 31.257 58.797 15.637 17.919 o -8 1 1 387.591 418.371 42.715 2.129 o -8 1 2 455.831 411.299 42.308 2.091 o -8 1 3 82.102 85.612 19.476 11.061 o -8 1 4 4.276 -5.027 6.382 114.544 o -8 1 5 6.579 13.238 8.490 62.729 o -8 2 1 755.828 849.667 60.817 0.967 o -8 2 2 449.724 440.797 43.574 1.989 o -8 2 3 153.211 167.280 26.530 5.828 o -8 2 4 0.779 -4.015 4.465 240.350 o -8 2 5 15.922 31.576 12.835 27.292 o -8 3 1 131.909 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6.820 8.521 8.354 65.412 o 9 2 4 8.531 11.591 8.972 56.277 o 9 2 5 90.679 120.475 24.146 7.389 o 9 2 6 40.755 54.465 16.652 15.805 o 9 2 7 44.398 42.801 14.149 21.179 o 9 2 8 1.878 -15.278 9.777 50.515 o 9 2 9 76.506 91.354 15.230 16.716 o 9 2 10 133.156 133.727 15.202 14.420 o 9 2 11 4.799 6.824 5.534 143.020 o 9 2 12 19.726 36.908 10.091 41.115 o 9 3 0 12.566 4.228 6.016 114.938 o 9 3 1 3.593 7.817 7.767 76.737 o 9 3 2 29.076 34.202 13.190 25.061 o 9 3 3 13.515 10.102 8.752 57.654 o 9 3 4 13.052 11.162 7.577 74.585 o 9 3 5 28.989 24.164 9.916 41.889 o 9 3 6 13.957 22.509 11.355 34.854 o 9 3 7 43.478 52.318 17.789 13.989 o 9 3 8 110.490 96.309 22.678 8.185 o 9 3 9 23.613 20.490 10.433 39.434 o 9 3 10 118.900 117.581 25.059 6.760 o 9 3 11 1.708 2.100 5.495 155.379 o 9 3 12 24.725 46.623 16.187 17.193 o 9 4 0 41.669 1.283 5.739 94.715 o 9 4 1 37.407 46.370 15.620 17.957 o 9 4 2 40.616 43.304 15.242 18.705 o 9 4 3 0.181 -4.748 6.120 129.728 o 9 4 4 3.390 -0.233 4.574 218.085 o 9 4 5 3.497 -2.365 7.426 86.019 o 9 4 6 0.001 -1.109 5.434 164.878 o 9 4 7 0.215 -6.644 6.632 110.460 o 9 4 8 46.266 60.125 18.079 13.457 o 9 4 9 1.025 2.155 4.182 265.198 o 9 4 10 17.188 5.892 6.781 89.326 o 9 4 11 3.119 15.143 11.829 33.718 o 9 5 0 34.149 47.587 15.769 17.734 o 9 5 1 34.307 59.753 18.255 13.444 o 9 5 2 4.238 5.736 8.127 70.549 o 9 5 3 121.505 98.575 22.139 8.422 o 9 5 4 9.442 1.579 4.644 188.468 o 9 5 5 0.470 1.847 6.730 106.135 o 9 5 6 31.302 40.435 15.344 18.854 o 9 5 7 136.253 90.959 21.573 8.691 o 9 5 8 83.208 121.851 25.760 6.619 o 9 5 9 36.615 46.522 16.373 16.511 o 9 5 10 42.649 32.488 14.011 21.869 o 9 5 11 3.408 11.011 8.950 58.086 o 9 6 0 0.074 6.471 7.109 93.787 o 9 6 1 15.601 18.925 10.641 39.287 o 9 6 2 0.962 -12.716 8.522 66.672 o 9 6 3 1.269 5.151 4.841 194.567 o 9 6 4 26.543 22.417 11.029 35.271 o 9 6 5 11.626 15.516 8.823 56.585 o 9 6 6 13.320 26.412 11.486 33.980 o 9 6 7 0.084 -6.882 6.991 99.522 o 9 6 8 1.414 1.547 3.729 328.794 o 9 6 9 8.715 17.759 10.497 41.393 o 9 6 10 56.281 63.690 19.261 11.819 o 9 6 11 1.263 -19.393 11.680 35.545 o 9 7 0 1.070 13.887 10.155 45.733 o 9 7 1 4.016 12.103 10.292 44.204 o 9 7 2 24.508 21.923 11.397 33.522 o 9 7 3 45.528 34.388 14.009 21.692 o 9 7 4 18.093 27.188 12.873 27.146 o 9 7 5 204.037 300.345 40.047 2.667 o 9 7 6 149.237 176.917 31.254 4.390 o 9 7 7 0.660 2.102 7.910 76.938 o 9 7 8 6.744 -12.399 10.411 43.785 o 9 7 9 35.937 39.028 15.549 18.273 o 9 7 10 12.578 35.009 14.497 21.823 o 9 8 0 13.191 11.554 7.790 70.870 o 9 8 1 46.713 42.433 14.985 19.072 o 9 8 2 4.144 -2.480 7.943 75.116 o 9 8 3 37.999 40.153 15.011 19.376 o 9 8 4 426.369 370.798 44.386 1.988 o 9 8 5 287.112 254.570 37.236 2.930 o 9 8 6 3.694 -22.227 11.450 36.702 o 9 8 7 23.633 43.688 16.130 17.380 o 9 8 8 0.755 -3.622 10.500 44.030 o 9 8 9 37.156 0.230 8.254 57.763 o 9 8 10 8.153 7.413 6.927 91.950 o 9 9 0 11.787 25.471 11.957 31.735 o 9 9 1 4.741 5.318 7.117 90.606 o 9 9 2 2.924 12.413 11.250 37.343 o 9 9 3 192.473 157.388 29.486 4.747 o 9 9 4 295.265 286.772 39.632 2.606 o 9 9 5 74.291 94.820 23.414 8.017 o 9 9 6 49.537 55.417 17.980 13.573 o 9 9 7 41.259 51.078 17.660 14.233 o 9 9 8 30.433 13.281 9.007 50.088 o 9 9 9 17.919 29.974 15.270 19.681 o 9 10 2 21.467 30.171 13.727 23.832 o 9 10 3 1.541 5.551 9.496 52.941 o 9 10 4 20.349 32.288 14.355 21.940 o 9 10 5 2.514 14.689 10.635 41.534 o 9 10 6 33.641 21.688 10.275 38.930 o 9 10 7 0.009 6.327 7.190 91.839 o 9 10 8 8.248 21.826 11.969 32.163 o 10 0 6 3.478 7.604 7.586 80.364 o 10 0 7 2.846 3.040 5.352 159.881 o 10 0 8 60.303 35.606 14.768 19.173 o 10 1 3 10.345 11.270 9.017 55.303 o 10 1 4 41.702 11.710 9.060 47.263 o 10 1 5 7.927 13.913 11.047 37.947 o 10 1 6 61.491 57.794 17.001 14.701 o 10 1 7 3.700 -8.817 9.778 50.114 o 10 1 8 70.982 71.928 19.390 11.405 o 10 2 1 18.361 17.094 9.595 47.013 o 10 2 2 4.957 -1.050 8.308 68.489 o 10 2 3 122.321 132.000 26.311 6.153 o 10 2 4 58.367 51.010 16.693 15.338 o 10 2 5 36.986 18.459 9.908 41.098 o 10 2 6 35.173 19.536 11.860 30.362 o 10 2 7 78.207 91.123 22.409 8.657 o 10 2 8 27.900 25.217 11.049 34.842 o 10 3 0 22.470 10.777 9.755 45.463 o 10 3 1 98.699 100.947 23.268 7.900 o 10 3 2 29.416 42.090 16.360 16.791 o 10 3 3 109.045 103.360 23.871 7.471 o 10 3 4 98.510 96.846 23.510 7.774 o 10 3 5 65.028 111.340 25.153 7.044 o 10 3 6 6.854 11.175 8.635 61.031 o 10 3 7 0.293 11.200 9.423 53.353 o 10 3 8 0.007 7.453 10.154 46.516 o 10 4 0 1.845 0.442 5.069 183.366 o 10 4 1 1.703 -4.094 7.166 93.512 o 10 4 2 16.742 0.087 7.928 69.624 o 10 4 3 6.863 19.261 10.967 38.263 o 10 4 4 0.019 1.107 4.343 254.954 o 10 4 5 0.424 17.504 10.875 39.873 o 10 4 6 2.262 -3.296 5.706 145.360 o 10 4 7 4.416 -4.864 9.530 52.539 o 10 4 8 1.036 -6.792 8.818 62.261 o 10 5 0 12.888 13.125 8.983 54.749 o 10 5 1 23.956 4.563 8.091 63.504 o 10 5 2 5.532 20.701 11.271 36.407 o 10 5 3 14.819 17.246 10.781 38.575 o 10 5 4 3.519 2.104 5.192 168.753 o 10 5 5 8.176 -8.629 9.339 53.724 o 10 5 6 0.865 -18.902 10.133 47.248 o 10 5 7 0.097 -6.923 9.409 54.961 o 10 5 8 4.066 22.277 13.642 25.289 o 10 6 0 21.777 6.906 4.968 137.380 o 10 6 1 1.706 2.848 6.661 106.614 o 10 6 2 12.483 -7.610 7.218 84.934 o 10 6 3 57.678 61.121 18.774 12.373 o 10 6 4 2.699 -22.586 12.456 31.153 o 10 6 5 126.305 150.274 29.548 4.965 o 10 6 6 3.495 1.169 7.184 91.351 o 10 6 7 15.198 32.644 14.211 22.590 o 10 6 8 61.374 79.466 21.310 9.700 o 10 7 2 3.688 7.402 9.437 52.837 o 10 7 3 6.651 3.507 7.943 73.110 o 10 7 4 14.554 22.841 11.096 36.276 o 10 7 5 4.912 14.665 10.862 39.542 o 10 7 6 109.668 144.086 29.322 5.100 o 10 7 7 10.297 26.947 11.618 33.553 o ; _olex2_exptl_crystal_mounting_method 'Mounted in a Oxford cryosystems cold stream at 150 K' _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x,-y,-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_refinement_flags_posn F1 F 0.24584(19) 1.24364(13) 0.80326(12) 0.0288(4) Uani 1.000000 . F2 F 0.27802(19) 0.98942(13) 1.23099(12) 0.0301(4) Uani 1.000000 . F3 F 0.2963(2) 1.33986(13) 0.95921(13) 0.0320(4) Uani 1.000000 . F4 F 0.3193(2) 1.21197(14) 1.16901(13) 0.0341(4) Uani 1.000000 . O1 O 0.3612(2) 0.74284(15) 1.22653(15) 0.0262(4) Uani 1.000000 . O2 O 0.1707(2) 0.67416(16) 1.17341(15) 0.0292(4) Uani 1.000000 . C1 C 0.1799(3) 0.8520(2) 0.7806(2) 0.0214(6) Uani 1.000000 . H53a C 0.2245(3) 0.9797(2) 0.8709(2) 0.0200(5) Uani 1.000000 . H53b C 0.2050(3) 0.8705(2) 0.9537(2) 0.0208(5) Uani 1.000000 . H53c C 0.2595(3) 0.9917(2) 1.0443(2) 0.0202(5) Uani 1.000000 . C2 C 0.2510(3) 1.0491(2) 0.6553(2) 0.0214(5) Uani 1.000000 . H48a C 0.3914(3) 1.1028(2) 0.6249(2) 0.0252(6) Uani 1.000000 . H48b C 0.1729(3) 0.7910(2) 0.8945(2) 0.0215(6) Uani 1.000000 . H48c C 0.1140(3) 0.6277(2) 0.8497(2) 0.0268(6) Uani 1.000000 . C3 C 0.2162(3) 0.9704(2) 0.7657(2) 0.0220(6) Uani 1.000000 . C4 C 0.2798(3) 1.0452(2) 1.1220(2) 0.0222(6) Uani 1.000000 . C5 C 0.2543(3) 1.0577(2) 0.9316(2) 0.0205(5) Uani 1.000000 . H52a C 0.1603(3) 0.7974(2) 0.7019(2) 0.0246(6) Uani 1.000000 . H52b C 0.2323(3) 0.8722(2) 1.0557(2) 0.0211(5) Uani 1.000000 . H52c C 0.2884(3) 1.2251(2) 0.9852(2) 0.0231(6) Uani 1.000000 . C6 C 0.1529(3) 1.0664(2) 0.5743(2) 0.0272(6) Uani 1.000000 . H51a C 0.2641(3) 1.1744(2) 0.9049(2) 0.0220(6) Uani 1.000000 . H51b C 0.2972(3) 1.1610(2) 1.0921(2) 0.0233(6) Uani 1.000000 . H51c C 0.1254(3) 0.6852(2) 0.7383(2) 0.0269(6) Uani 1.000000 . C7 C 0.3358(3) 0.6357(2) 1.3111(2) 0.0256(6) Uani 1.000000 . C8 C 0.1393(3) 0.6797(2) 0.9296(2) 0.0250(6) Uani 1.000000 . C9 C 0.1979(4) 1.1320(2) 0.4661(2) 0.0312(7) Uani 1.000000 . C10 C 0.2539(4) 0.5738(2) 1.2520(2) 0.0291(6) Uani 1.000000 . C11 C 0.4337(4) 1.1693(2) 0.5167(2) 0.0315(7) Uani 1.000000 . C12 C 0.3900(4) 0.4897(3) 1.1790(3) 0.0407(8) Uani 1.000000 . C13 C 0.3398(4) 1.1825(2) 0.4372(2) 0.0320(7) Uani 1.000000 . C14 C 0.5134(4) 0.5648(3) 1.3364(2) 0.0349(7) Uani 1.000000 . C15 B 0.2528(4) 0.7631(3) 1.1554(2) 0.0226(6) Uani 1.000000 . C16 C 0.2113(4) 0.6767(3) 1.4171(2) 0.0408(8) Uani 1.000000 . C17 C 0.1115(4) 0.5148(3) 1.3297(3) 0.0468(9) Uani 1.000000 . H39 H 0.1335(3) 0.6402(2) 1.0046(2) 0.0300(7) Uiso 1.000000 R C18 H 0.0892(3) 0.5534(2) 0.8722(2) 0.0321(7) Uiso 1.000000 R H15 H 0.1097(3) 0.6487(2) 0.6864(2) 0.0323(7) Uiso 1.000000 R C19 H 0.1702(3) 0.8349(2) 0.6261(2) 0.0295(7) Uiso 1.000000 R H36 H 0.0566(3) 1.0335(2) 0.5934(2) 0.0327(7) Uiso 1.000000 R C20 H 0.1328(4) 1.1420(2) 0.4129(2) 0.0375(8) Uiso 1.000000 R H23 H 0.3714(4) 1.2253(2) 0.3642(2) 0.0385(8) Uiso 1.000000 R C21 H 0.5266(4) 1.2053(2) 0.4978(2) 0.0378(8) Uiso 1.000000 R C22 H 0.4569(3) 1.0938(2) 0.6775(2) 0.0302(7) Uiso 1.000000 R C23 H 0.3322(5) 0.4626(15) 1.1376(14) 0.0610(12) Uiso 1.000000 GR C24 H 0.4739(16) 0.5306(6) 1.1265(12) 0.0610(12) Uiso 1.000000 GR H12 H 0.450(2) 0.4228(9) 1.2267(3) 0.0610(12) Uiso 1.000000 GR C25 H 0.5972(7) 0.5515(15) 1.2666(3) 0.0523(11) Uiso 1.000000 GR H45 H 0.5531(12) 0.6082(8) 1.3739(15) 0.0523(11) Uiso 1.000000 GR C26 H 0.5020(7) 0.4898(7) 1.3847(13) 0.0523(11) Uiso 1.000000 GR H50 H 0.2599(13) 0.7262(15) 1.4419(10) 0.0613(12) Uiso 1.000000 GR C27 H 0.0993(9) 0.7210(16) 1.4005(5) 0.0613(12) Uiso 1.000000 GR H42 H 0.196(2) 0.6088(3) 1.4761(6) 0.0613(12) Uiso 1.000000 GR C28 H 0.0163(13) 0.5732(4) 1.3643(13) 0.0702(13) Uiso 1.000000 GR H29 H 0.0687(19) 0.4793(16) 1.2864(4) 0.0702(13) Uiso 1.000000 GR B1 H 0.1593(8) 0.4545(13) 1.3877(10) 0.0702(13) Uiso 1.000000 GR 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 F1 0.0370(9) 0.0242(8) 0.0252(9) -0.0089(6) -0.0097(6) -0.0001(7) F2 0.0424(9) 0.0285(9) 0.0222(9) -0.0094(7) -0.0128(7) -0.0025(7) F3 0.0423(9) 0.0226(8) 0.0332(10) -0.0132(7) -0.0064(7) -0.0051(7) F4 0.0448(10) 0.0327(9) 0.0336(10) -0.0141(7) -0.0123(7) -0.0121(7) O1 0.0335(10) 0.0216(10) 0.0250(10) -0.0089(8) -0.0119(8) 0.0015(8) O2 0.0362(11) 0.0272(11) 0.0282(11) -0.0152(8) -0.0130(8) 0.0030(8) C1 0.0175(12) 0.0221(14) 0.0248(14) -0.0034(10) -0.0044(10) -0.0068(11) H53a 0.0150(12) 0.0208(13) 0.0242(14) -0.0034(9) -0.0049(9) -0.0052(11) H53b 0.0186(12) 0.0222(14) 0.0208(14) -0.0044(10) -0.0049(10) -0.0033(11) H53c 0.0177(12) 0.0215(13) 0.0206(14) -0.0038(10) -0.0033(9) -0.0050(11) C2 0.0215(13) 0.0211(13) 0.0200(14) -0.0025(10) -0.0047(10) -0.0046(11) H48a 0.0268(14) 0.0272(15) 0.0218(14) -0.0064(11) -0.0055(10) -0.0056(11) H48b 0.0186(12) 0.0224(14) 0.0229(14) -0.0031(10) -0.0055(10) -0.0049(11) H48c 0.0306(15) 0.0226(14) 0.0306(16) -0.0092(11) -0.0078(11) -0.0068(12) C3 0.0167(12) 0.0234(14) 0.0241(14) -0.0017(10) -0.0048(10) -0.0050(11) C4 0.0225(13) 0.0243(14) 0.0181(13) -0.0041(10) -0.0060(10) -0.0016(11) C5 0.0172(12) 0.0222(14) 0.0216(14) -0.0043(10) -0.0051(9) -0.0033(11) H52a 0.0243(13) 0.0278(15) 0.0217(14) -0.0073(11) -0.0059(10) -0.0032(11) H52b 0.0200(13) 0.0213(13) 0.0215(14) -0.0049(10) -0.0043(10) -0.0036(11) H52c 0.0234(13) 0.0161(13) 0.0291(15) -0.0065(10) -0.0048(10) -0.0026(11) C6 0.0280(14) 0.0255(15) 0.0283(16) -0.0045(11) -0.0103(11) -0.0036(12) H51a 0.0213(13) 0.0211(14) 0.0210(14) -0.0061(10) -0.0039(10) 0.0002(11) H51b 0.0238(13) 0.0233(14) 0.0270(15) -0.0069(10) -0.0066(10) -0.0098(12) H51c 0.0282(14) 0.0286(15) 0.0286(16) -0.0090(11) -0.0064(11) -0.0109(12) C7 0.0320(15) 0.0210(14) 0.0204(14) -0.0046(11) -0.0066(11) 0.0002(11) C8 0.0258(14) 0.0226(14) 0.0251(15) -0.0038(10) -0.0072(11) -0.0029(11) C9 0.0365(16) 0.0301(16) 0.0248(16) -0.0014(12) -0.0135(12) -0.0023(12) C10 0.0363(16) 0.0234(15) 0.0272(16) -0.0111(12) -0.0086(12) 0.0016(12) C11 0.0319(15) 0.0330(16) 0.0279(16) -0.0120(12) -0.0011(12) -0.0048(13) C12 0.063(2) 0.0265(17) 0.0357(18) -0.0136(14) -0.0123(15) -0.0072(14) C13 0.0424(17) 0.0271(16) 0.0212(15) -0.0067(12) -0.0044(12) -0.0006(12) C14 0.0392(17) 0.0289(16) 0.0332(17) -0.0034(12) -0.0126(13) -0.0014(13) C15 0.0218(15) 0.0241(16) 0.0223(16) -0.0070(12) -0.0002(11) -0.0088(13) C16 0.0480(19) 0.0417(19) 0.0289(17) -0.0049(14) -0.0055(13) -0.0110(14) C17 0.056(2) 0.046(2) 0.042(2) -0.0324(16) -0.0122(15) 0.0101(16) loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source _atom_type_scat_dispersion_source H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236 57.79970 0.0030380000826 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' 'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2' C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870 51.65120 0.215599998832 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' 'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2' B 0.00141 0.00067 2.05450 1.33260 1.09790 0.70680 23.21850 1.02100 60.34980 0.14030 -0.193200007081 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' 'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2' O 0.01158 0.00611 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390 32.90890 0.250800013542 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' 'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2' F 0.01794 0.01033 3.53920 2.64120 1.51700 1.02430 10.28250 4.29440 0.26150 26.14760 0.277599990368 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' 'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C15 O1 C7 107.2(2) C15 O2 C10 107.1(2) C3 C1 H48b 110.0(2) H52a C1 H48b 119.7(2) H52a C1 C3 130.3(2) C3 H53a H53b 110.7(2) C5 H53a H53b 106.2(2) C5 H53a C3 143.0(2) H48b H53b H53a 107.1(2) H52b H53b H53a 111.8(2) H52b H53b H48b 140.9(2) C5 H53c C4 119.0(2) H52b H53c C4 131.2(2) H52b H53c C5 109.7(2) C3 C2 H48a 120.3(2) C6 C2 H48a 118.2(2) C6 C2 C3 121.3(2) C11 H48a C2 120.4(3) H53b H48b C1 106.0(2) C8 H48b C1 120.9(2) C8 H48b H53b 133.1(2) C8 H48c H51c 120.7(3) H53a C3 C1 106.1(2) C2 C3 C1 123.3(2) C2 C3 H53a 130.4(2) H53c C4 F2 121.9(2) H51b C4 F2 117.3(2) H51b C4 H53c 120.8(2) H53c C5 H53a 106.3(2) H51a C5 H53a 134.1(2) H51a C5 H53c 119.4(2) H51c H52a C1 118.9(2) H53c H52b H53b 105.8(2) C15 H52b H53b 125.1(2) C15 H52b H53c 128.7(2) H51a H52c F3 119.9(2) H51b H52c F3 119.6(2) H51b H52c H51a 120.5(2) C9 C6 C2 120.7(3) C5 H51a F1 122.0(2) H52c H51a F1 118.0(2) H52c H51a C5 120.0(2) C4 H51b F4 120.1(2) H52c H51b F4 119.6(2) H52c H51b C4 120.3(2) H52a H51c H48c 121.2(3) C10 C7 O1 102.89(19) C14 C7 O1 108.3(2) C14 C7 C10 114.8(2) C16 C7 O1 106.9(2) C16 C7 C10 113.3(2) C16 C7 C14 110.0(2) H48c C8 H48b 118.5(2) C13 C9 C6 120.0(3) C7 C10 O2 102.2(2) C12 C10 O2 106.3(2) C12 C10 C7 113.7(2) C17 C10 O2 107.6(2) C17 C10 C7 115.2(2) C17 C10 C12 110.8(2) C13 C11 H48a 120.8(3) C11 C13 C9 119.8(3) O2 C15 O1 113.8(2) H52b C15 O1 124.1(2) H52b C15 O2 121.9(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance F1 H51a 1.347(3) F2 C4 1.352(3) F3 H52c 1.351(3) F4 H51b 1.348(3) O1 C7 1.466(3) O1 C15 1.360(3) O2 C10 1.468(3) O2 C15 1.368(3) C1 H48b 1.417(3) C1 C3 1.498(4) C1 H52a 1.388(3) H53a H53b 1.465(3) H53a C3 1.374(3) H53a C5 1.464(3) H53b H48b 1.475(3) H53b H52b 1.366(3) H53c C4 1.370(3) H53c C5 1.433(3) H53c H52b 1.486(3) C2 H48a 1.397(4) C2 C3 1.464(3) C2 C6 1.405(3) H48a C11 1.388(4) H48b C8 1.381(4) H48c H51c 1.375(4) H48c C8 1.402(4) C4 H51b 1.386(4) C5 H51a 1.378(3) H52a H51c 1.397(4) H52b C15 1.562(4) H52c H51a 1.392(4) H52c H51b 1.370(4) C6 C9 1.387(4) C7 C10 1.559(4) C7 C14 1.520(3) C7 C16 1.519(3) C9 C13 1.386(4) C10 C12 1.522(4) C10 C17 1.516(4) C11 C13 1.376(4)