#------------------------------------------------------------------------------ #$Date: 2020-10-06 10:12:07 +0300 (Tue, 06 Oct 2020) $ #$Revision: 257326 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/78/1557872.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_1557872 loop_ _publ_author_name 'Yan, Chenting' 'Takeshita, Masato' 'Nakatsuji, Jun-ya' 'Kurosaki, Akihiro' 'Sato, Kaoko' 'Shang, Rong' 'Nakamoto, Masaaki' 'Yamamoto, Yohsuke' 'Adachi, Yohei' 'Furukawa, Ko' 'Kishi, Ryohei' 'Nakano, Masayoshi' _publ_section_title ; Synthesis and properties of hypervalent electron-rich pentacoordinate nitrogen compounds ; _journal_issue 19 _journal_name_full 'Chemical Science' _journal_page_first 5082 _journal_page_last 5088 _journal_paper_doi 10.1039/D0SC00002G _journal_volume 11 _journal_year 2020 _chemical_formula_sum 'C32 H33 F6 N O4' _chemical_formula_weight 609.59 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2019-08-05 deposited with the CCDC. 2020-04-13 downloaded from the CCDC. ; _cell_angle_alpha 97.5670(10) _cell_angle_beta 107.7540(10) _cell_angle_gamma 95.2740(10) _cell_formula_units_Z 2 _cell_length_a 10.0890(4) _cell_length_b 11.8293(5) _cell_length_c 13.7884(6) _cell_measurement_reflns_used 9969 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 28.34 _cell_measurement_theta_min 2.21 _cell_volume 1538.29(11) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _diffrn_ambient_temperature 173(2) _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.971 _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 0.0452 _diffrn_reflns_av_unetI/netI 0.0459 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.971 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 18837 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.971 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.371 _diffrn_reflns_theta_min 1.754 _exptl_absorpt_coefficient_mu 0.110 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.4319 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.316 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 636 _exptl_crystal_size_max 0.760 _exptl_crystal_size_mid 0.278 _exptl_crystal_size_min 0.163 _exptl_transmission_factor_max 0.00150 _exptl_transmission_factor_min 0.00087 _refine_diff_density_max 0.472 _refine_diff_density_min -0.261 _refine_diff_density_rms 0.046 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 451 _refine_ls_number_reflns 7482 _refine_ls_number_restraints 66 _refine_ls_restrained_S_all 1.035 _refine_ls_R_factor_all 0.0460 _refine_ls_R_factor_gt 0.0406 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0434P)^2^+0.4645P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1065 _refine_ls_wR_factor_ref 0.1114 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6554 _reflns_number_total 7482 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0sc00002g2.cif _cod_data_source_block 2iPr_b _cod_depositor_comments ;Adding full bibliography for 1557869--1557876.cif. Adding full bibliography for 1557869--1557876.cif. ; _cod_database_code 1557872 _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_min 0.4319 _shelx_estimated_absorpt_t_max 0.7457 _shelx_res_file ; exp302_2_1m.res created by SHELXL-2014/7 TITL exp302_2_1m in P-1 CELL 0.71073 10.0890 11.8293 13.7884 97.567 107.754 95.274 ZERR 2.00 0.0004 0.0005 0.0006 0.001 0.001 0.001 LATT 1 SFAC C H N O F UNIT 64 66 2 8 12 LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP -100.000 ACTA L.S. 10 FMAP 2 PLAN 10 0 0.00 HTAB BOND $H CONF SIMU 0.1 F1 > F7A RIGU 0.1 F1 > F7A SIMU 0.1 F3 > F5A RIGU 0.1 F3 > F5A WGHT 0.043400 0.464500 FVAR 0.18504 0.40605 0.50109 PART 1 21 F1 5 0.168720 0.606092 0.265888 21.00000 0.03733 0.03190 = 0.05935 0.01124 -0.02406 -0.01389 F2 5 0.198073 0.775391 0.243057 21.00000 0.08468 0.03556 = 0.04201 -0.00145 -0.03538 0.02270 F7 5 0.310872 0.658626 0.195000 21.00000 0.04908 0.12939 = 0.01949 -0.01229 0.00622 0.02580 PART 2 -21 F1A 5 0.138170 0.630791 0.283973 -21.00000 0.03849 0.10678 = 0.07409 0.05410 -0.02440 -0.03439 F2A 5 0.197512 0.785118 0.236714 -21.00000 0.03364 0.02580 = 0.02723 0.01166 -0.00426 0.01543 F7A 5 0.287106 0.632817 0.201651 -21.00000 0.09463 0.07272 = 0.03543 -0.03058 -0.03494 0.06236 PART 3 31 F3 5 0.607603 1.151626 1.011922 31.00000 0.04233 0.06802 = 0.04577 -0.02378 0.02165 0.00916 F4 5 0.816504 1.213590 1.026837 31.00000 0.11288 0.03862 = 0.07454 -0.03017 0.05811 -0.01310 F5 5 0.740352 1.063393 1.092058 31.00000 0.09444 0.07008 = 0.02352 0.00488 0.02755 0.02381 PART 4 -31 F3A 5 0.611733 1.165352 0.999556 -31.00000 0.09699 0.08388 = 0.04027 -0.02329 0.00176 0.06851 F4A 5 0.833403 1.200958 1.040217 -31.00000 0.06223 0.08530 = 0.06053 -0.05454 0.02162 -0.02720 F5A 5 0.776920 1.074909 1.098135 -31.00000 0.15357 0.08659 = 0.01572 -0.00112 0.00125 0.06546 PART 0 O1 4 0.848711 0.643892 0.885757 11.00000 0.02186 0.03513 = 0.01492 0.00664 0.00486 0.00688 O2 4 0.650734 0.618030 0.749309 11.00000 0.01859 0.02802 = 0.02046 0.00330 0.00435 0.00425 O3 4 0.825136 0.953892 0.543113 11.00000 0.03994 0.02117 = 0.02939 0.00626 0.01398 0.01387 O4 4 0.875890 0.824494 0.429130 11.00000 0.03120 0.02372 = 0.01706 0.00769 0.00763 0.01191 N1 3 0.703067 0.807631 0.652674 11.00000 0.01716 0.01912 = 0.01602 0.00040 0.00269 0.00768 C1 1 0.255057 0.693367 0.272798 11.00000 0.03032 0.02392 = 0.02923 0.00398 -0.00678 0.00642 C2 1 0.369997 0.723888 0.373833 11.00000 0.02001 0.02009 = 0.01927 0.00372 0.00021 0.00373 C3 1 0.384720 0.829285 0.436961 11.00000 0.01904 0.01875 = 0.02450 0.00554 0.00302 0.00720 AFIX 43 H3 2 0.320069 0.881953 0.416387 11.00000 -1.20000 AFIX 0 C4 1 0.493631 0.857503 0.529840 11.00000 0.02174 0.01607 = 0.02131 0.00211 0.00490 0.00616 AFIX 43 H4 2 0.504231 0.930025 0.572273 11.00000 -1.20000 AFIX 0 C5 1 0.587924 0.779814 0.561378 11.00000 0.01714 0.01847 = 0.01621 0.00306 0.00343 0.00483 C6 1 0.826371 0.755309 0.657187 11.00000 0.01638 0.01733 = 0.01468 -0.00042 0.00176 0.00576 C7 1 0.869104 0.679117 0.726321 11.00000 0.01713 0.01862 = 0.01402 0.00042 0.00264 0.00395 C8 1 0.992033 0.631419 0.733137 11.00000 0.01799 0.01849 = 0.01500 0.00197 0.00215 0.00534 AFIX 43 H8 2 1.023423 0.583710 0.783473 11.00000 -1.20000 AFIX 0 C9 1 1.070654 0.651961 0.667675 11.00000 0.01664 0.01741 = 0.01492 -0.00097 0.00191 0.00454 C10 1 1.202625 0.594135 0.675385 11.00000 0.01762 0.02132 = 0.01790 0.00165 0.00430 0.00730 C11 1 1.266836 0.618455 0.591842 11.00000 0.02708 0.03736 = 0.02947 0.00988 0.01451 0.01477 AFIX 137 H11A 2 1.198968 0.587184 0.523573 11.00000 -1.50000 H11B 2 1.352200 0.581970 0.600953 11.00000 -1.50000 H11C 2 1.290499 0.701800 0.597449 11.00000 -1.50000 AFIX 0 C12 1 0.728987 1.118261 1.011682 11.00000 0.04548 0.03825 = 0.02399 -0.00477 0.00861 0.01374 C13 1 0.721082 1.037472 0.916735 11.00000 0.03523 0.02318 = 0.01744 0.00093 0.00655 0.01142 C14 1 0.593486 0.974699 0.854940 11.00000 0.02885 0.02877 = 0.02246 0.00299 0.00954 0.01306 AFIX 43 H14 2 0.510870 0.983694 0.872890 11.00000 -1.20000 AFIX 0 C15 1 0.585909 0.898853 0.767062 11.00000 0.02142 0.02479 = 0.02050 0.00092 0.00501 0.00670 AFIX 43 H15 2 0.498249 0.855888 0.725189 11.00000 -1.20000 AFIX 0 C16 1 0.706709 0.885496 0.740003 11.00000 0.02240 0.01661 = 0.01671 0.00267 0.00469 0.00770 C17 1 0.905340 0.779306 0.593439 11.00000 0.02025 0.01715 = 0.01465 0.00129 0.00302 0.00523 C18 1 1.024224 0.725623 0.597424 11.00000 0.01833 0.01906 = 0.01600 0.00080 0.00512 0.00419 AFIX 43 H18 2 1.074486 0.739735 0.551124 11.00000 -1.20000 AFIX 0 C19 1 0.776209 0.643881 0.786888 11.00000 0.01975 0.01805 = 0.01594 0.00206 0.00461 0.00716 C20 1 0.764656 0.617002 0.952120 11.00000 0.02947 0.03678 = 0.01932 0.00984 0.01163 0.01073 AFIX 13 H20 2 0.684130 0.555652 0.912800 11.00000 -1.20000 AFIX 0 C21 1 0.709444 0.725265 0.985093 11.00000 0.05370 0.04638 = 0.02757 0.00691 0.02005 0.02131 AFIX 137 H21A 2 0.647541 0.749853 0.924048 11.00000 -1.50000 H21B 2 0.788448 0.786374 1.020586 11.00000 -1.50000 H21C 2 0.656581 0.709689 1.032000 11.00000 -1.50000 AFIX 0 C22 1 0.860962 0.572939 1.041371 11.00000 0.05197 0.08000 = 0.03212 0.03299 0.02167 0.03555 AFIX 137 H22A 2 0.888866 0.500567 1.015961 11.00000 -1.50000 H22B 2 0.811951 0.559535 1.091083 11.00000 -1.50000 H22C 2 0.944807 0.630010 1.075211 11.00000 -1.50000 AFIX 0 C23 1 1.165174 0.463455 0.663237 11.00000 0.02939 0.02238 = 0.03338 0.00232 0.01115 0.00980 AFIX 137 H23A 2 1.094588 0.434503 0.595590 11.00000 -1.50000 H23B 2 1.127236 0.445524 0.717807 11.00000 -1.50000 H23C 2 1.249738 0.426732 0.668544 11.00000 -1.50000 AFIX 0 C24 1 1.312059 0.639585 0.781759 11.00000 0.01898 0.03846 = 0.02467 -0.00121 0.00214 0.00819 AFIX 137 H24A 2 1.397214 0.603604 0.787434 11.00000 -1.50000 H24B 2 1.273644 0.620862 0.835884 11.00000 -1.50000 H24C 2 1.335204 0.723316 0.789889 11.00000 -1.50000 AFIX 0 C25 1 0.863864 0.863468 0.521085 11.00000 0.02023 0.02026 = 0.01919 0.00395 0.00521 0.00572 C26 1 0.829695 0.894010 0.347750 11.00000 0.03457 0.02979 = 0.02289 0.01431 0.00790 0.01190 AFIX 13 H26 2 0.854660 0.977773 0.377928 11.00000 -1.20000 AFIX 0 C27 1 0.672116 0.864019 0.299620 11.00000 0.03416 0.08285 = 0.04343 0.03586 0.00625 0.02044 AFIX 137 H27A 2 0.638738 0.908527 0.243990 11.00000 -1.50000 H27B 2 0.627031 0.882512 0.352304 11.00000 -1.50000 H27C 2 0.648410 0.781572 0.271361 11.00000 -1.50000 AFIX 0 C28 1 0.908395 0.863773 0.273454 11.00000 0.04338 0.04012 = 0.02226 0.01009 0.01209 0.00637 AFIX 137 H28A 2 0.885352 0.781192 0.245681 11.00000 -1.50000 H28B 2 1.009677 0.882673 0.309553 11.00000 -1.50000 H28C 2 0.881463 0.907740 0.216691 11.00000 -1.50000 AFIX 0 C29 1 0.462521 0.645614 0.404863 11.00000 0.02374 0.01788 = 0.02045 -0.00059 0.00237 0.00549 AFIX 43 H29 2 0.451952 0.573398 0.361983 11.00000 -1.20000 AFIX 0 C30 1 0.569919 0.672960 0.498173 11.00000 0.02123 0.01759 = 0.02013 0.00227 0.00252 0.00783 AFIX 43 H30 2 0.632099 0.618783 0.519638 11.00000 -1.20000 AFIX 0 C31 1 0.835297 0.947848 0.803723 11.00000 0.02232 0.02188 = 0.02042 0.00164 0.00530 0.00568 AFIX 43 H31 2 0.918497 0.938444 0.786701 11.00000 -1.20000 AFIX 0 C32 1 0.842006 1.023272 0.891551 11.00000 0.02767 0.02287 = 0.02098 -0.00019 0.00174 0.00468 AFIX 43 H32 2 0.929681 1.065281 0.934529 11.00000 -1.20000 AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM exp302_2_1m in P-1 REM R1 = 0.0406 for 6554 Fo > 4sig(Fo) and 0.0460 for all 7482 data REM 451 parameters refined using 66 restraints END WGHT 0.0434 0.4645 REM Instructions for potential hydrogen bonds EQIV $1 -x+2, -y+2, -z+1 HTAB C28 O3_$1 REM Highest difference peak 0.472, deepest hole -0.261, 1-sigma level 0.046 Q1 1 0.8231 0.6573 0.7536 11.00000 0.05 0.47 Q2 1 0.8898 0.8168 0.5596 11.00000 0.05 0.36 Q3 1 0.8351 0.7044 0.6831 11.00000 0.05 0.32 Q4 1 0.3125 0.7088 0.3263 11.00000 0.05 0.31 Q5 1 1.1342 0.6207 0.6683 11.00000 0.05 0.30 Q6 1 0.8585 0.7607 0.6210 11.00000 0.05 0.30 Q7 1 0.5222 0.8064 0.5534 11.00000 0.05 0.29 Q8 1 1.0287 0.6372 0.6947 11.00000 0.05 0.29 Q9 1 0.4384 0.8427 0.4839 11.00000 0.05 0.28 Q10 1 0.9422 0.6726 0.7441 11.00000 0.05 0.28 ; _shelx_res_checksum 26512 loop_ _space_group_symop_operation_xyz 'x, y, z' '-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_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 0.1687(10) 0.6061(5) 0.2659(7) 0.0529(18) Uani 0.41(2) 1 d . U P A 1 F2 F 0.1981(9) 0.7754(8) 0.2431(7) 0.067(3) Uani 0.41(2) 1 d . U P A 1 F7 F 0.3109(9) 0.6586(10) 0.1950(6) 0.069(2) Uani 0.41(2) 1 d . U P A 1 F1A F 0.1382(9) 0.6308(10) 0.2840(7) 0.082(2) Uani 0.59(2) 1 d . U P A 2 F2A F 0.1975(4) 0.7851(5) 0.2367(4) 0.0307(9) Uani 0.59(2) 1 d . U P A 2 F7A F 0.2871(9) 0.6328(7) 0.2017(4) 0.0808(19) Uani 0.59(2) 1 d . U P A 2 F3 F 0.6076(6) 1.1516(7) 1.0119(7) 0.0534(15) Uani 0.50(3) 1 d . U P B 3 F4 F 0.8165(14) 1.2136(9) 1.0268(10) 0.074(2) Uani 0.50(3) 1 d . U P B 3 F5 F 0.7404(12) 1.0634(11) 1.0921(8) 0.0602(18) Uani 0.50(3) 1 d . U P B 3 F3A F 0.6117(8) 1.1654(9) 0.9996(8) 0.078(2) Uani 0.50(3) 1 d . U P B 4 F4A F 0.8334(12) 1.2010(11) 1.0402(10) 0.078(3) Uani 0.50(3) 1 d . U P B 4 F5A F 0.777(2) 1.0749(13) 1.0981(9) 0.089(3) Uani 0.50(3) 1 d . U P B 4 O1 O 0.84871(8) 0.64389(7) 0.88576(6) 0.02379(17) Uani 1 1 d . . . . . O2 O 0.65073(8) 0.61803(7) 0.74931(6) 0.02281(17) Uani 1 1 d . . . . . O3 O 0.82514(10) 0.95389(7) 0.54311(7) 0.02869(19) Uani 1 1 d . . . . . O4 O 0.87589(9) 0.82449(7) 0.42913(6) 0.02308(17) Uani 1 1 d . . . . . N1 N 0.70307(9) 0.80763(8) 0.65267(7) 0.01794(18) Uani 1 1 d . . . . . C1 C 0.25506(13) 0.69337(10) 0.27280(10) 0.0314(3) Uani 1 1 d . . . . . C2 C 0.37000(11) 0.72389(9) 0.37383(8) 0.0211(2) Uani 1 1 d . . . . . C3 C 0.38472(11) 0.82929(9) 0.43696(9) 0.0212(2) Uani 1 1 d . . . . . H3 H 0.3201 0.8820 0.4164 0.025 Uiso 1 1 calc R U . . . C4 C 0.49363(11) 0.85750(9) 0.52984(8) 0.0200(2) Uani 1 1 d . . . . . H4 H 0.5042 0.9300 0.5723 0.024 Uiso 1 1 calc R U . . . C5 C 0.58792(10) 0.77981(9) 0.56138(8) 0.0176(2) Uani 1 1 d . . . . . C6 C 0.82637(10) 0.75531(9) 0.65719(8) 0.0169(2) Uani 1 1 d . . . . . C7 C 0.86910(10) 0.67912(9) 0.72632(8) 0.0173(2) Uani 1 1 d . . . . . C8 C 0.99203(10) 0.63142(9) 0.73314(8) 0.0178(2) Uani 1 1 d . . . . . H8 H 1.0234 0.5837 0.7835 0.021 Uiso 1 1 calc R U . . . C9 C 1.07065(10) 0.65196(9) 0.66767(8) 0.0173(2) Uani 1 1 d . . . . . C10 C 1.20263(11) 0.59413(9) 0.67539(8) 0.0191(2) Uani 1 1 d . . . . . C11 C 1.26684(13) 0.61846(11) 0.59184(10) 0.0290(3) Uani 1 1 d . . . . . H11A H 1.1990 0.5872 0.5236 0.043 Uiso 1 1 calc R U . . . H11B H 1.3522 0.5820 0.6010 0.043 Uiso 1 1 calc R U . . . H11C H 1.2905 0.7018 0.5974 0.043 Uiso 1 1 calc R U . . . C12 C 0.72899(16) 1.11826(12) 1.01168(10) 0.0369(3) Uani 1 1 d . . . . . C13 C 0.72108(13) 1.03747(10) 0.91673(9) 0.0255(2) Uani 1 1 d . . . . . C14 C 0.59349(13) 0.97470(10) 0.85494(9) 0.0259(2) Uani 1 1 d . . . . . H14 H 0.5109 0.9837 0.8729 0.031 Uiso 1 1 calc R U . . . C15 C 0.58591(12) 0.89885(10) 0.76706(8) 0.0227(2) Uani 1 1 d . . . . . H15 H 0.4982 0.8559 0.7252 0.027 Uiso 1 1 calc R U . . . C16 C 0.70671(11) 0.88550(9) 0.74000(8) 0.0186(2) Uani 1 1 d . . . . . C17 C 0.90534(11) 0.77931(9) 0.59344(8) 0.0179(2) Uani 1 1 d . . . . . C18 C 1.02422(11) 0.72562(9) 0.59742(8) 0.0180(2) Uani 1 1 d . . . . . H18 H 1.0745 0.7397 0.5511 0.022 Uiso 1 1 calc R U . . . C19 C 0.77621(11) 0.64388(9) 0.78689(8) 0.0179(2) Uani 1 1 d . . . . . C20 C 0.76466(13) 0.61700(11) 0.95212(9) 0.0268(2) Uani 1 1 d . . . . . H20 H 0.6841 0.5557 0.9128 0.032 Uiso 1 1 calc R U . . . C21 C 0.70944(17) 0.72527(13) 0.98509(11) 0.0399(3) Uani 1 1 d . . . . . H21A H 0.6475 0.7499 0.9240 0.060 Uiso 1 1 calc R U . . . H21B H 0.7884 0.7864 1.0206 0.060 Uiso 1 1 calc R U . . . H21C H 0.6566 0.7097 1.0320 0.060 Uiso 1 1 calc R U . . . C22 C 0.86096(18) 0.57294(17) 1.04137(12) 0.0488(4) Uani 1 1 d . . . . . H22A H 0.8889 0.5006 1.0160 0.073 Uiso 1 1 calc R U . . . H22B H 0.8120 0.5595 1.0911 0.073 Uiso 1 1 calc R U . . . H22C H 0.9448 0.6300 1.0752 0.073 Uiso 1 1 calc R U . . . C23 C 1.16517(13) 0.46346(10) 0.66324(10) 0.0280(2) Uani 1 1 d . . . . . H23A H 1.0946 0.4345 0.5956 0.042 Uiso 1 1 calc R U . . . H23B H 1.1272 0.4455 0.7178 0.042 Uiso 1 1 calc R U . . . H23C H 1.2497 0.4267 0.6685 0.042 Uiso 1 1 calc R U . . . C24 C 1.31206(12) 0.63959(11) 0.78176(9) 0.0288(3) Uani 1 1 d . . . . . H24A H 1.3972 0.6036 0.7874 0.043 Uiso 1 1 calc R U . . . H24B H 1.2736 0.6209 0.8359 0.043 Uiso 1 1 calc R U . . . H24C H 1.3352 0.7233 0.7899 0.043 Uiso 1 1 calc R U . . . C25 C 0.86386(11) 0.86347(9) 0.52109(8) 0.0199(2) Uani 1 1 d . . . . . C26 C 0.82969(13) 0.89401(11) 0.34775(9) 0.0280(2) Uani 1 1 d . . . . . H26 H 0.8547 0.9778 0.3779 0.034 Uiso 1 1 calc R U . . . C27 C 0.67212(16) 0.86402(18) 0.29962(13) 0.0517(4) Uani 1 1 d . . . . . H27A H 0.6387 0.9085 0.2440 0.078 Uiso 1 1 calc R U . . . H27B H 0.6270 0.8825 0.3523 0.078 Uiso 1 1 calc R U . . . H27C H 0.6484 0.7816 0.2714 0.078 Uiso 1 1 calc R U . . . C28 C 0.90839(15) 0.86377(12) 0.27345(10) 0.0344(3) Uani 1 1 d . . . . . H28A H 0.8854 0.7812 0.2457 0.052 Uiso 1 1 calc R U . . . H28B H 1.0097 0.8827 0.3096 0.052 Uiso 1 1 calc R U . . . H28C H 0.8815 0.9077 0.2167 0.052 Uiso 1 1 calc R U . . . C29 C 0.46252(11) 0.64561(9) 0.40486(8) 0.0220(2) Uani 1 1 d . . . . . H29 H 0.4520 0.5734 0.3620 0.026 Uiso 1 1 calc R U . . . C30 C 0.56992(11) 0.67296(9) 0.49817(8) 0.0203(2) Uani 1 1 d . . . . . H30 H 0.6321 0.6188 0.5196 0.024 Uiso 1 1 calc R U . . . C31 C 0.83530(12) 0.94785(9) 0.80372(8) 0.0219(2) Uani 1 1 d . . . . . H31 H 0.9185 0.9384 0.7867 0.026 Uiso 1 1 calc R U . . . C32 C 0.84201(12) 1.02327(10) 0.89155(9) 0.0255(2) Uani 1 1 d . . . . . H32 H 0.9297 1.0653 0.9345 0.031 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 0.037(3) 0.032(2) 0.059(3) 0.0112(16) -0.024(2) -0.0139(15) F2 0.085(4) 0.036(3) 0.042(3) -0.001(2) -0.035(3) 0.023(2) F7 0.049(2) 0.129(6) 0.0195(17) -0.012(2) 0.0062(18) 0.026(3) F1A 0.038(2) 0.107(4) 0.074(3) 0.054(3) -0.0244(19) -0.034(2) F2A 0.0336(14) 0.0258(13) 0.0272(14) 0.0117(10) -0.0043(12) 0.0154(10) F7A 0.095(3) 0.073(2) 0.035(2) -0.0306(14) -0.0349(19) 0.062(2) F3 0.042(2) 0.068(2) 0.046(2) -0.0238(18) 0.022(2) 0.009(3) F4 0.113(6) 0.039(2) 0.075(4) -0.030(2) 0.058(4) -0.013(3) F5 0.094(4) 0.070(2) 0.024(3) 0.005(2) 0.028(3) 0.024(3) F3A 0.097(5) 0.084(3) 0.040(2) -0.023(2) 0.002(2) 0.069(4) F4A 0.062(3) 0.085(6) 0.061(3) -0.055(4) 0.022(2) -0.027(3) F5A 0.154(8) 0.087(5) 0.0157(18) -0.001(2) 0.001(4) 0.065(5) O1 0.0219(4) 0.0351(4) 0.0149(4) 0.0066(3) 0.0049(3) 0.0069(3) O2 0.0186(4) 0.0280(4) 0.0205(4) 0.0033(3) 0.0044(3) 0.0043(3) O3 0.0399(5) 0.0212(4) 0.0294(4) 0.0063(3) 0.0140(4) 0.0139(3) O4 0.0312(4) 0.0237(4) 0.0171(4) 0.0077(3) 0.0076(3) 0.0119(3) N1 0.0172(4) 0.0191(4) 0.0160(4) 0.0004(3) 0.0027(3) 0.0077(3) C1 0.0303(6) 0.0239(6) 0.0292(6) 0.0040(5) -0.0068(5) 0.0064(5) C2 0.0200(5) 0.0201(5) 0.0193(5) 0.0037(4) 0.0002(4) 0.0037(4) C3 0.0190(5) 0.0187(5) 0.0245(5) 0.0055(4) 0.0030(4) 0.0072(4) C4 0.0217(5) 0.0161(4) 0.0213(5) 0.0021(4) 0.0049(4) 0.0062(4) C5 0.0171(5) 0.0185(5) 0.0162(5) 0.0031(4) 0.0034(4) 0.0048(4) C6 0.0164(4) 0.0173(4) 0.0147(4) -0.0004(4) 0.0018(4) 0.0058(4) C7 0.0171(4) 0.0186(5) 0.0140(4) 0.0004(4) 0.0026(4) 0.0039(4) C8 0.0180(5) 0.0185(5) 0.0150(5) 0.0020(4) 0.0021(4) 0.0053(4) C9 0.0166(4) 0.0174(4) 0.0149(5) -0.0010(4) 0.0019(4) 0.0045(4) C10 0.0176(5) 0.0213(5) 0.0179(5) 0.0017(4) 0.0043(4) 0.0073(4) C11 0.0271(6) 0.0374(6) 0.0295(6) 0.0099(5) 0.0145(5) 0.0148(5) C12 0.0455(8) 0.0382(7) 0.0240(6) -0.0048(5) 0.0086(6) 0.0137(6) C13 0.0352(6) 0.0232(5) 0.0174(5) 0.0009(4) 0.0066(4) 0.0114(5) C14 0.0289(6) 0.0288(6) 0.0225(5) 0.0030(4) 0.0095(5) 0.0131(5) C15 0.0214(5) 0.0248(5) 0.0205(5) 0.0009(4) 0.0050(4) 0.0067(4) C16 0.0224(5) 0.0166(4) 0.0167(5) 0.0027(4) 0.0047(4) 0.0077(4) C17 0.0202(5) 0.0171(4) 0.0146(4) 0.0013(4) 0.0030(4) 0.0052(4) C18 0.0183(5) 0.0191(5) 0.0160(5) 0.0008(4) 0.0051(4) 0.0042(4) C19 0.0197(5) 0.0181(5) 0.0159(5) 0.0021(4) 0.0046(4) 0.0072(4) C20 0.0295(6) 0.0368(6) 0.0193(5) 0.0098(5) 0.0116(5) 0.0107(5) C21 0.0537(9) 0.0464(8) 0.0276(6) 0.0069(6) 0.0201(6) 0.0213(7) C22 0.0520(9) 0.0800(12) 0.0321(7) 0.0330(8) 0.0217(7) 0.0355(8) C23 0.0294(6) 0.0224(5) 0.0334(6) 0.0023(5) 0.0112(5) 0.0098(4) C24 0.0190(5) 0.0385(7) 0.0247(6) -0.0012(5) 0.0021(4) 0.0082(5) C25 0.0202(5) 0.0203(5) 0.0192(5) 0.0039(4) 0.0052(4) 0.0057(4) C26 0.0346(6) 0.0298(6) 0.0229(5) 0.0143(5) 0.0079(5) 0.0119(5) C27 0.0342(7) 0.0829(12) 0.0434(9) 0.0359(9) 0.0062(6) 0.0204(8) C28 0.0434(7) 0.0401(7) 0.0223(6) 0.0101(5) 0.0121(5) 0.0064(6) C29 0.0237(5) 0.0179(5) 0.0205(5) -0.0006(4) 0.0024(4) 0.0055(4) C30 0.0212(5) 0.0176(5) 0.0201(5) 0.0023(4) 0.0025(4) 0.0078(4) C31 0.0223(5) 0.0219(5) 0.0204(5) 0.0016(4) 0.0053(4) 0.0057(4) C32 0.0277(6) 0.0229(5) 0.0210(5) -0.0002(4) 0.0017(4) 0.0047(4) 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' N N 0.0061 0.0033 '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' F F 0.0171 0.0103 '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 C19 O1 C20 115.79(8) . . ? C25 O4 C26 117.00(8) . . ? C5 N1 C16 124.47(8) . . ? C5 N1 C6 118.24(8) . . ? C16 N1 C6 117.28(8) . . ? F2 C1 F1 113.1(5) . . ? F7A C1 F2A 109.5(4) . . ? F2 C1 F7 102.1(5) . . ? F1 C1 F7 101.9(5) . . ? F7A C1 F1A 106.5(4) . . ? F2A C1 F1A 100.3(5) . . ? F2 C1 C2 113.9(4) . . ? F1 C1 C2 114.5(4) . . ? F7A C1 C2 114.8(3) . . ? F2A C1 C2 114.0(2) . . ? F7 C1 C2 109.7(4) . . ? F1A C1 C2 110.5(3) . . ? C29 C2 C3 120.08(10) . . ? C29 C2 C1 119.30(10) . . ? C3 C2 C1 120.62(10) . . ? C4 C3 C2 120.05(10) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 120.33(10) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C4 C5 C30 119.00(10) . . ? C4 C5 N1 121.80(9) . . ? C30 C5 N1 119.15(9) . . ? C17 C6 C7 119.26(9) . . ? C17 C6 N1 120.79(9) . . ? C7 C6 N1 119.95(9) . . ? C8 C7 C6 119.81(9) . . ? C8 C7 C19 120.91(9) . . ? C6 C7 C19 119.15(9) . . ? C7 C8 C9 121.68(9) . . ? C7 C8 H8 119.2 . . ? C9 C8 H8 119.2 . . ? C18 C9 C8 117.54(9) . . ? C18 C9 C10 122.59(9) . . ? C8 C9 C10 119.88(9) . . ? C11 C10 C23 107.96(9) . . ? C11 C10 C9 112.25(9) . . ? C23 C10 C9 109.62(9) . . ? C11 C10 C24 108.82(9) . . ? C23 C10 C24 109.45(9) . . ? C9 C10 C24 108.71(8) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? F4 C12 F3 105.8(6) . . ? F4A C12 F3A 107.8(7) . . ? F4A C12 F5A 92.8(15) . . ? F3A C12 F5A 116.2(13) . . ? F4 C12 F5 117.4(9) . . ? F3 C12 F5 93.7(7) . . ? F4A C12 C13 114.0(6) . . ? F4 C12 C13 112.7(6) . . ? F3 C12 C13 114.2(3) . . ? F3A C12 C13 111.3(4) . . ? F5A C12 C13 113.3(6) . . ? F5 C12 C13 111.6(5) . . ? C32 C13 C14 119.94(10) . . ? C32 C13 C12 119.89(12) . . ? C14 C13 C12 120.15(11) . . ? C13 C14 C15 120.32(11) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C14 C15 C16 120.17(11) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C15 C16 C31 119.07(10) . . ? C15 C16 N1 121.55(10) . . ? C31 C16 N1 119.33(9) . . ? C6 C17 C18 120.05(9) . . ? C6 C17 C25 120.11(9) . . ? C18 C17 C25 119.83(9) . . ? C9 C18 C17 121.51(9) . . ? C9 C18 H18 119.2 . . ? C17 C18 H18 119.2 . . ? O2 C19 O1 124.64(10) . . ? O2 C19 C7 123.08(9) . . ? O1 C19 C7 112.27(9) . . ? O1 C20 C22 106.22(10) . . ? O1 C20 C21 108.42(10) . . ? C22 C20 C21 113.08(12) . . ? O1 C20 H20 109.7 . . ? C22 C20 H20 109.7 . . ? C21 C20 H20 109.7 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C10 C23 H23A 109.5 . . ? C10 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C10 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C10 C24 H24A 109.5 . . ? C10 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C10 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O3 C25 O4 124.82(10) . . ? O3 C25 C17 124.50(10) . . ? O4 C25 C17 110.68(9) . . ? O4 C26 C28 105.65(9) . . ? O4 C26 C27 107.88(10) . . ? C28 C26 C27 113.25(12) . . ? O4 C26 H26 110.0 . . ? C28 C26 H26 110.0 . . ? C27 C26 H26 110.0 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 C2 119.92(10) . . ? C30 C29 H29 120.0 . . ? C2 C29 H29 120.0 . . ? C29 C30 C5 120.60(9) . . ? C29 C30 H30 119.7 . . ? C5 C30 H30 119.7 . . ? C32 C31 C16 120.38(10) . . ? C32 C31 H31 119.8 . . ? C16 C31 H31 119.8 . . ? C13 C32 C31 120.09(11) . . ? C13 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? 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 1.262(8) . ? F2 C1 1.226(10) . ? F7 C1 1.390(6) . ? F1A C1 1.394(7) . ? F2A C1 1.358(5) . ? F7A C1 1.277(6) . ? F3 C12 1.322(6) . ? F4 C12 1.318(10) . ? F5 C12 1.337(10) . ? F3A C12 1.328(7) . ? F4A C12 1.295(9) . ? F5A C12 1.331(11) . ? O1 C19 1.3361(12) . ? O1 C20 1.4690(13) . ? O2 C19 1.2048(13) . ? O3 C25 1.2053(13) . ? O4 C25 1.3360(13) . ? O4 C26 1.4653(13) . ? N1 C5 1.4040(13) . ? N1 C16 1.4051(13) . ? N1 C6 1.4279(12) . ? C1 C2 1.4904(15) . ? C2 C29 1.3898(15) . ? C2 C3 1.3912(15) . ? C3 C4 1.3859(15) . ? C3 H3 0.9500 . ? C4 C5 1.3973(14) . ? C4 H4 0.9500 . ? C5 C30 1.4005(14) . ? C6 C17 1.3925(15) . ? C6 C7 1.3978(14) . ? C7 C8 1.3917(14) . ? C7 C19 1.4989(14) . ? C8 C9 1.4007(15) . ? C8 H8 0.9500 . ? C9 C18 1.3920(14) . ? C9 C10 1.5337(14) . ? C10 C11 1.5289(15) . ? C10 C23 1.5318(16) . ? C10 C24 1.5346(15) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.4921(16) . ? C13 C32 1.3849(17) . ? C13 C14 1.3868(18) . ? C14 C15 1.3869(15) . ? C14 H14 0.9500 . ? C15 C16 1.3953(15) . ? C15 H15 0.9500 . ? C16 C31 1.3990(15) . ? C17 C18 1.3978(14) . ? C17 C25 1.4984(14) . ? C18 H18 0.9500 . ? C20 C22 1.5043(17) . ? C20 C21 1.5131(18) . ? C20 H20 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C26 C28 1.5032(18) . ? C26 C27 1.512(2) . ? C26 H26 1.0000 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.3819(15) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.3862(15) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? 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 F2 C1 C2 C29 -165.9(5) . . . . ? F1 C1 C2 C29 61.7(5) . . . . ? F7A C1 C2 C29 -34.7(6) . . . . ? F2A C1 C2 C29 -162.11(19) . . . . ? F7 C1 C2 C29 -52.1(5) . . . . ? F1A C1 C2 C29 85.8(7) . . . . ? F2 C1 C2 C3 14.4(5) . . . . ? F1 C1 C2 C3 -118.0(5) . . . . ? F7A C1 C2 C3 145.6(6) . . . . ? F2A C1 C2 C3 18.2(2) . . . . ? F7 C1 C2 C3 128.1(5) . . . . ? F1A C1 C2 C3 -93.9(7) . . . . ? C29 C2 C3 C4 1.47(17) . . . . ? C1 C2 C3 C4 -178.79(11) . . . . ? C2 C3 C4 C5 -0.95(17) . . . . ? C3 C4 C5 C30 -0.51(16) . . . . ? C3 C4 C5 N1 177.08(10) . . . . ? C16 N1 C5 C4 28.22(16) . . . . ? C6 N1 C5 C4 -150.56(10) . . . . ? C16 N1 C5 C30 -154.19(10) . . . . ? C6 N1 C5 C30 27.02(14) . . . . ? C5 N1 C6 C17 65.27(13) . . . . ? C16 N1 C6 C17 -113.60(11) . . . . ? C5 N1 C6 C7 -114.82(11) . . . . ? C16 N1 C6 C7 66.31(13) . . . . ? C17 C6 C7 C8 2.18(15) . . . . ? N1 C6 C7 C8 -177.73(9) . . . . ? C17 C6 C7 C19 -173.69(9) . . . . ? N1 C6 C7 C19 6.40(14) . . . . ? C6 C7 C8 C9 -4.06(15) . . . . ? C19 C7 C8 C9 171.73(9) . . . . ? C7 C8 C9 C18 2.28(15) . . . . ? C7 C8 C9 C10 -177.83(9) . . . . ? C18 C9 C10 C11 -5.09(14) . . . . ? C8 C9 C10 C11 175.03(10) . . . . ? C18 C9 C10 C23 -125.06(11) . . . . ? C8 C9 C10 C23 55.06(12) . . . . ? C18 C9 C10 C24 115.34(11) . . . . ? C8 C9 C10 C24 -64.54(12) . . . . ? F4A C12 C13 C32 26.4(8) . . . . ? F4 C12 C13 C32 39.6(7) . . . . ? F3 C12 C13 C32 160.4(5) . . . . ? F3A C12 C13 C32 148.6(7) . . . . ? F5A C12 C13 C32 -78.1(11) . . . . ? F5 C12 C13 C32 -94.9(5) . . . . ? F4A C12 C13 C14 -155.1(8) . . . . ? F4 C12 C13 C14 -141.8(7) . . . . ? F3 C12 C13 C14 -21.0(5) . . . . ? F3A C12 C13 C14 -32.8(7) . . . . ? F5A C12 C13 C14 100.4(11) . . . . ? F5 C12 C13 C14 83.7(5) . . . . ? C32 C13 C14 C15 -0.93(18) . . . . ? C12 C13 C14 C15 -179.50(11) . . . . ? C13 C14 C15 C16 -0.23(17) . . . . ? C14 C15 C16 C31 1.23(16) . . . . ? C14 C15 C16 N1 178.66(10) . . . . ? C5 N1 C16 C15 32.49(15) . . . . ? C6 N1 C16 C15 -148.72(10) . . . . ? C5 N1 C16 C31 -150.08(10) . . . . ? C6 N1 C16 C31 28.71(14) . . . . ? C7 C6 C17 C18 1.33(15) . . . . ? N1 C6 C17 C18 -178.76(9) . . . . ? C7 C6 C17 C25 -178.13(9) . . . . ? N1 C6 C17 C25 1.78(15) . . . . ? C8 C9 C18 C17 1.33(15) . . . . ? C10 C9 C18 C17 -178.56(9) . . . . ? C6 C17 C18 C9 -3.14(15) . . . . ? C25 C17 C18 C9 176.33(9) . . . . ? C20 O1 C19 O2 -3.97(15) . . . . ? C20 O1 C19 C7 176.50(9) . . . . ? C8 C7 C19 O2 -132.17(11) . . . . ? C6 C7 C19 O2 43.65(15) . . . . ? C8 C7 C19 O1 47.37(13) . . . . ? C6 C7 C19 O1 -136.81(10) . . . . ? C19 O1 C20 C22 156.55(12) . . . . ? C19 O1 C20 C21 -81.63(13) . . . . ? C26 O4 C25 O3 -4.14(16) . . . . ? C26 O4 C25 C17 175.92(9) . . . . ? C6 C17 C25 O3 42.24(16) . . . . ? C18 C17 C25 O3 -137.23(12) . . . . ? C6 C17 C25 O4 -137.82(10) . . . . ? C18 C17 C25 O4 42.71(13) . . . . ? C25 O4 C26 C28 156.05(10) . . . . ? C25 O4 C26 C27 -82.54(14) . . . . ? C3 C2 C29 C30 -0.51(17) . . . . ? C1 C2 C29 C30 179.75(11) . . . . ? C2 C29 C30 C5 -0.96(17) . . . . ? C4 C5 C30 C29 1.47(16) . . . . ? N1 C5 C30 C29 -176.18(10) . . . . ? C15 C16 C31 C32 -1.08(16) . . . . ? N1 C16 C31 C32 -178.57(10) . . . . ? C14 C13 C32 C31 1.09(18) . . . . ? C12 C13 C32 C31 179.65(11) . . . . ? C16 C31 C32 C13 -0.07(17) . . . . ?