#------------------------------------------------------------------------------ #$Date: 2024-08-05 21:12:58 +0300 (Mon, 05 Aug 2024) $ #$Revision: 293778 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/20/1572029.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_1572029 loop_ _publ_author_name 'Nascimento, Mitchell A.' 'LaPierre, Etienne A.' 'Patrick, Brian O.' 'Watson, Jade E. T.' 'Watanabe, Lara' 'Rawson, Jeremy' 'Hering-Junghans, Christian' 'Manners, Ian' _publ_section_title ; 1,3-Dipolar cyclisation reactions of nitriles with sterically encumbered cyclic triphosphanes: synthesis and electronic structure of phosphorus-rich heterocycles with tunable colour. ; _journal_issue 30 _journal_name_full 'Chemical science' _journal_page_first 12006 _journal_page_last 12016 _journal_paper_doi 10.1039/d4sc02497d _journal_volume 15 _journal_year 2024 _chemical_formula_moiety 'C53 H77 N O P3, C F3 O3 S' _chemical_formula_sum 'C54 H77 F3 N O4 P3 S' _chemical_formula_weight 986.13 _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-2018/3 _audit_update_record ; 2023-09-05 deposited with the CCDC. 2024-07-01 downloaded from the CCDC. ; _cell_angle_alpha 67.221(2) _cell_angle_beta 80.664(3) _cell_angle_gamma 64.226(2) _cell_formula_units_Z 2 _cell_length_a 13.7735(12) _cell_length_b 14.3310(12) _cell_length_c 16.4614(14) _cell_measurement_reflns_used 9952 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 28.32 _cell_measurement_theta_min 2.50 _cell_volume 2697.7(4) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'LinXTL v. 5.9.9 (Spasyuk, 2009)' _computing_structure_refinement 'SHELXL-2014 (Sheldrick 2014)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type 'Mo k\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0643 _diffrn_reflns_av_unetI/netI 0.0742 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 50897 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.391 _diffrn_reflns_theta_min 1.342 _exptl_absorpt_coefficient_mu 0.203 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.6561 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Sadabs (Sheldrick, 1996)' _exptl_crystal_colour Yellow _exptl_crystal_density_diffrn 1.214 _exptl_crystal_density_method 'not measured' _exptl_crystal_description blade _exptl_crystal_F_000 1056 _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _refine_diff_density_max 0.448 _refine_diff_density_min -0.470 _refine_diff_density_rms 0.064 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 677 _refine_ls_number_reflns 13452 _refine_ls_number_restraints 311 _refine_ls_restrained_S_all 1.008 _refine_ls_R_factor_all 0.0972 _refine_ls_R_factor_gt 0.0517 _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^)+(0.0516P)^2^+1.2931P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1099 _refine_ls_wR_factor_ref 0.1284 _reflns_Friedel_coverage 0.000 _reflns_number_gt 8867 _reflns_number_total 13452 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc02497d4.cif _cod_data_source_block im082 _cod_depositor_comments 'Adding full bibliography for 1572027--1572043.cif.' _cod_database_code 1572029 _shelx_shelxl_version_number 2018/3 _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 0.947 _shelx_estimated_absorpt_t_max 0.994 _shelx_res_file ; TITL im082_a.res in P-1 im082.res created by SHELXL-2018/3 at 12:02:32 on 01-Oct-2021 REM Old TITL im082 in P-1 REM SHELXT solution in P-1: R1 0.167, Rweak 0.009, Alpha 0.062 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C55 O3A F3B S4 CELL 0.71073 13.7735 14.331 16.4614 67.221 80.664 64.226 ZERR 2 0.0012 0.0012 0.0014 0.002 0.003 0.002 LATT 1 SFAC C H F N O P S UNIT 108 154 6 2 8 6 2 DFIX 1.31 C54A F1A DELU C54A O2 S1A S1B O3B O4B C54B O3A O4A F3B F1A F1B F2A F3A F1A SIMU C54A O2 S1A S1B O3B O4B C54B O3A O4A F3B F1A F1B F2A F3A F1A ISOR O2 S1A S1B O3B O4B C54B O3A O4A C54A F3B F1A F2A F3A ISOR C54A O2 S1A S1B O3B O4B C54B O3A O4A F3B F1A F1B F2A F3A F1A L.S. 10 PLAN 50 SIZE 0.03 0.1 0.27 TEMP 23 CONF LIST 4 MORE -1 BOND $H FMAP 2 53 ACTA OMIT 5 5 1 OMIT -2 5 2 REM REM REM WGHT 0.051600 1.293100 FVAR 0.33558 P1 6 0.709058 0.190740 0.200393 11.00000 0.01425 0.01630 = 0.02010 -0.01148 0.00274 -0.00542 P2 6 0.804983 0.150762 0.315149 11.00000 0.01462 0.01369 = 0.01842 -0.00863 0.00204 -0.00441 P3 6 0.826897 0.308815 0.242404 11.00000 0.01755 0.01666 = 0.01728 -0.00981 0.00394 -0.00789 O1 5 0.228770 0.610167 0.027616 11.00000 0.02466 0.03385 = 0.03472 -0.00892 -0.01016 -0.00054 N1 4 0.690722 0.380524 0.206147 11.00000 0.01843 0.01282 = 0.01976 -0.00957 0.00251 -0.00469 AFIX 43 H1 2 0.658451 0.449149 0.201014 11.00000 -1.20000 AFIX 0 C1 1 0.634991 0.336963 0.186424 11.00000 0.01787 0.01608 = 0.01136 -0.00731 0.00429 -0.00571 C40 1 0.746063 0.403717 0.379727 11.00000 0.01924 0.01413 = 0.01605 -0.00650 -0.00004 -0.00456 C2 1 0.530400 0.407179 0.143502 11.00000 0.01872 0.01775 = 0.01296 -0.00555 0.00201 -0.00625 C41 1 0.747278 0.474672 0.418289 11.00000 0.02202 0.01870 = 0.01942 -0.01105 0.00227 -0.00412 AFIX 43 H41 2 0.696195 0.490972 0.460875 11.00000 -1.20000 AFIX 0 C14 1 0.528480 0.143048 0.294172 11.00000 0.01710 0.01664 = 0.01525 -0.00513 -0.00041 -0.00621 C39 1 0.824911 0.378668 0.315890 11.00000 0.01949 0.01490 = 0.01750 -0.00682 0.00047 -0.00699 C3 1 0.484986 0.368323 0.100942 11.00000 0.02038 0.02208 = 0.01898 -0.00974 0.00373 -0.00713 AFIX 43 H3 2 0.522995 0.297317 0.099192 11.00000 -1.20000 AFIX 0 C24 1 0.928179 0.032897 0.302807 11.00000 0.01513 0.01700 = 0.02457 -0.01160 -0.00052 -0.00511 C13 1 0.461266 0.088611 0.306549 11.00000 0.01828 0.02110 = 0.01998 -0.00626 0.00196 -0.00831 AFIX 43 H13 2 0.398980 0.107568 0.339526 11.00000 -1.20000 AFIX 0 C42 1 0.821585 0.521688 0.395577 11.00000 0.02384 0.01537 = 0.02061 -0.00691 -0.00525 -0.00528 C25 1 0.988846 0.027146 0.225440 11.00000 0.01639 0.02071 = 0.02562 -0.01403 0.00139 -0.00684 C44 1 0.905241 0.421141 0.295551 11.00000 0.02077 0.02164 = 0.01922 -0.00864 0.00106 -0.00961 C21 1 0.499977 0.222843 0.342841 11.00000 0.01809 0.02129 = 0.02147 -0.01179 0.00661 -0.01021 AFIX 13 H21 2 0.547866 0.261657 0.321558 11.00000 -1.20000 AFIX 0 C12 1 0.483526 0.007382 0.271690 11.00000 0.02190 0.01691 = 0.02195 -0.00411 -0.00333 -0.00869 C18 1 0.406024 -0.046078 0.278710 11.00000 0.02454 0.01838 = 0.02803 -0.00506 -0.00259 -0.01142 AFIX 13 H18 2 0.445860 -0.126679 0.304592 11.00000 -1.20000 AFIX 0 C9 1 0.620948 0.116841 0.241660 11.00000 0.01518 0.01503 = 0.02000 -0.00786 -0.00176 -0.00491 C36 1 0.892676 -0.068848 0.467311 11.00000 0.02364 0.01709 = 0.02241 -0.00677 -0.00039 -0.00677 AFIX 13 H36 2 0.852323 0.007389 0.465980 11.00000 -1.20000 AFIX 0 C10 1 0.648944 0.028291 0.210866 11.00000 0.01768 0.01961 = 0.02881 -0.01359 0.00097 -0.00619 C29 1 0.953802 -0.064060 0.380344 11.00000 0.01769 0.01679 = 0.02663 -0.00987 -0.00308 -0.00589 C23 1 0.383193 0.310812 0.326219 11.00000 0.01917 0.02606 = 0.02909 -0.01532 0.00638 -0.00769 AFIX 137 H23A 2 0.334479 0.275692 0.352509 11.00000 -1.50000 H23B 2 0.369631 0.347283 0.263933 11.00000 -1.50000 H23C 2 0.372548 0.364389 0.351835 11.00000 -1.50000 AFIX 0 C30 1 0.976819 0.125688 0.140725 11.00000 0.01445 0.02455 = 0.02332 -0.01460 0.00525 -0.00539 AFIX 13 H30 2 0.911265 0.188673 0.145615 11.00000 -1.20000 AFIX 0 C48 1 0.814493 0.605693 0.433964 11.00000 0.03247 0.02477 = 0.02675 -0.01484 0.00272 -0.01415 AFIX 13 H48 2 0.867121 0.636311 0.403126 11.00000 -1.20000 AFIX 0 C27 1 1.093969 -0.170988 0.301644 11.00000 0.02169 0.01971 = 0.03142 -0.01348 -0.00022 -0.00554 C33 1 1.180236 -0.282337 0.300267 11.00000 0.02985 0.02124 = 0.03121 -0.01295 0.00166 -0.00548 AFIX 13 H33 2 1.193347 -0.334196 0.361386 11.00000 -1.20000 AFIX 0 C4 1 0.384353 0.433350 0.061187 11.00000 0.02389 0.02989 = 0.01776 -0.00743 0.00026 -0.01177 AFIX 43 H4 2 0.354566 0.406363 0.033313 11.00000 -1.20000 AFIX 0 C7 1 0.472582 0.516576 0.142904 11.00000 0.02333 0.02141 = 0.02046 -0.00964 0.00321 -0.00652 AFIX 43 H7 2 0.502220 0.544734 0.169762 11.00000 -1.20000 AFIX 0 C28 1 1.036135 -0.163538 0.377170 11.00000 0.02260 0.01541 = 0.02854 -0.00596 -0.00133 -0.00548 AFIX 43 H28 2 1.052438 -0.226836 0.427732 11.00000 -1.20000 AFIX 0 C45 1 0.659460 0.358777 0.409479 11.00000 0.02147 0.02068 = 0.02014 -0.01246 0.00599 -0.00995 AFIX 13 H45 2 0.669110 0.310677 0.377036 11.00000 -1.20000 AFIX 0 C26 1 1.070225 -0.075545 0.227213 11.00000 0.01967 0.02729 = 0.02740 -0.01671 0.00529 -0.00788 AFIX 43 H26 2 1.109904 -0.079814 0.176377 11.00000 -1.20000 AFIX 0 C43 1 0.900877 0.491789 0.336383 11.00000 0.02384 0.02285 = 0.02321 -0.00832 -0.00015 -0.01269 AFIX 43 H43 2 0.953395 0.519762 0.323192 11.00000 -1.20000 AFIX 0 C11 1 0.579312 -0.023586 0.226841 11.00000 0.02562 0.01900 = 0.02928 -0.01256 -0.00158 -0.00954 AFIX 43 H11 2 0.597833 -0.081387 0.206587 11.00000 -1.20000 AFIX 0 C22 1 0.522109 0.156767 0.441618 11.00000 0.03101 0.03279 = 0.02208 -0.01365 0.00396 -0.01386 AFIX 137 H22A 2 0.505280 0.206893 0.472242 11.00000 -1.50000 H22B 2 0.596789 0.106477 0.450720 11.00000 -1.50000 H22C 2 0.478114 0.115560 0.463737 11.00000 -1.50000 AFIX 0 C5 1 0.328277 0.540229 0.063644 11.00000 0.01910 0.02696 = 0.01872 -0.00274 0.00072 -0.00257 C46 1 0.546091 0.452666 0.388643 11.00000 0.02389 0.03174 = 0.03210 -0.01983 0.00732 -0.00996 AFIX 137 H46A 2 0.533885 0.499499 0.421376 11.00000 -1.50000 H46B 2 0.493422 0.421610 0.404785 11.00000 -1.50000 H46C 2 0.540054 0.495615 0.326734 11.00000 -1.50000 AFIX 0 C34 1 1.138173 -0.328183 0.250035 11.00000 0.03610 0.02193 = 0.04437 -0.02073 0.00225 -0.00593 AFIX 137 H34A 2 1.073544 -0.335612 0.277373 11.00000 -1.50000 H34B 2 1.191871 -0.399417 0.251292 11.00000 -1.50000 H34C 2 1.122809 -0.278180 0.190039 11.00000 -1.50000 AFIX 0 C49 1 0.843826 0.551540 0.531132 11.00000 0.04471 0.03148 = 0.03115 -0.01798 -0.00022 -0.01636 AFIX 137 H49A 2 0.847318 0.604459 0.551399 11.00000 -1.50000 H49B 2 0.912671 0.489586 0.539720 11.00000 -1.50000 H49C 2 0.790056 0.526295 0.563790 11.00000 -1.50000 AFIX 0 C38 1 0.811355 -0.117376 0.474162 11.00000 0.03030 0.02957 = 0.03210 -0.01013 0.00337 -0.01550 AFIX 137 H38A 2 0.761888 -0.071995 0.425296 11.00000 -1.50000 H38B 2 0.772287 -0.119442 0.528266 11.00000 -1.50000 H38C 2 0.848707 -0.191232 0.473235 11.00000 -1.50000 AFIX 0 C19 1 0.369519 -0.018293 0.185901 11.00000 0.02659 0.03132 = 0.03493 -0.01432 0.00064 -0.01472 AFIX 137 H19A 2 0.328856 0.060266 0.159566 11.00000 -1.50000 H19B 2 0.325253 -0.056178 0.189461 11.00000 -1.50000 H19C 2 0.431585 -0.041564 0.150550 11.00000 -1.50000 AFIX 0 C50 1 0.703010 0.701822 0.417391 11.00000 0.03267 0.02148 = 0.04060 -0.01808 0.00026 -0.00938 AFIX 137 H50A 2 0.650114 0.675074 0.449895 11.00000 -1.50000 H50B 2 0.686121 0.733292 0.355629 11.00000 -1.50000 H50C 2 0.702761 0.757488 0.436237 11.00000 -1.50000 AFIX 0 C6 1 0.373653 0.581310 0.103286 11.00000 0.02676 0.02209 = 0.02290 -0.00963 0.00047 -0.00121 AFIX 43 H6 2 0.336595 0.653363 0.102947 11.00000 -1.20000 AFIX 0 C37 1 0.967379 -0.133731 0.547892 11.00000 0.03295 0.02566 = 0.02497 -0.00630 -0.00080 -0.01129 AFIX 137 H37A 2 1.000929 -0.210888 0.555167 11.00000 -1.50000 H37B 2 0.926230 -0.124886 0.599421 11.00000 -1.50000 H37C 2 1.021875 -0.106150 0.539675 11.00000 -1.50000 AFIX 0 C32 1 1.072879 0.156890 0.131907 11.00000 0.02112 0.03029 = 0.03441 -0.01188 0.00229 -0.00969 AFIX 137 H32A 2 1.079906 0.166807 0.184761 11.00000 -1.50000 H32B 2 1.060822 0.224620 0.082626 11.00000 -1.50000 H32C 2 1.137765 0.098688 0.122838 11.00000 -1.50000 AFIX 0 C52 1 1.104888 0.371720 0.257812 11.00000 0.02389 0.03662 = 0.03694 -0.01857 0.00831 -0.01535 AFIX 137 H52A 2 1.104966 0.436901 0.261540 11.00000 -1.50000 H52B 2 1.158104 0.348207 0.216176 11.00000 -1.50000 H52C 2 1.121461 0.313592 0.314638 11.00000 -1.50000 AFIX 0 C8 1 0.173244 0.563612 0.001130 11.00000 0.02571 0.04069 = 0.02778 -0.00269 -0.00097 -0.01101 AFIX 137 H8A 2 0.211103 0.539853 -0.046475 11.00000 -1.50000 H8B 2 0.101721 0.618227 -0.018019 11.00000 -1.50000 H8C 2 0.169189 0.501131 0.049894 11.00000 -1.50000 AFIX 0 C20 1 0.307893 -0.012213 0.335663 11.00000 0.03327 0.03634 = 0.02860 -0.00936 0.00445 -0.02403 AFIX 137 H20A 2 0.330937 -0.032451 0.394383 11.00000 -1.50000 H20B 2 0.263666 -0.049362 0.337216 11.00000 -1.50000 H20C 2 0.267120 0.066556 0.311347 11.00000 -1.50000 AFIX 0 C47 1 0.672511 0.288813 0.507420 11.00000 0.03796 0.03368 = 0.02657 -0.00999 0.00589 -0.02130 AFIX 137 H47A 2 0.741739 0.227217 0.517965 11.00000 -1.50000 H47B 2 0.616840 0.261788 0.525620 11.00000 -1.50000 H47C 2 0.667175 0.333360 0.540371 11.00000 -1.50000 AFIX 0 C35 1 1.286845 -0.276569 0.263532 11.00000 0.02606 0.02885 = 0.03783 -0.01939 0.00123 -0.00124 AFIX 137 H35A 2 1.278155 -0.231270 0.202105 11.00000 -1.50000 H35B 2 1.340369 -0.349924 0.270545 11.00000 -1.50000 H35C 2 1.309387 -0.244867 0.294728 11.00000 -1.50000 AFIX 0 C15 1 0.752007 -0.011602 0.160071 11.00000 0.02168 0.03215 = 0.05098 -0.03217 0.01104 -0.01407 AFIX 13 H15 2 0.795527 0.026216 0.162383 11.00000 -1.20000 AFIX 0 C51 1 0.994119 0.397819 0.227817 11.00000 0.03299 0.04660 = 0.03418 -0.02676 0.01314 -0.02688 AFIX 13 H51 2 0.999198 0.332423 0.218327 11.00000 -1.20000 AFIX 0 C31 1 0.965879 0.107506 0.057344 11.00000 0.02730 0.03494 = 0.02502 -0.01776 0.00707 -0.00937 AFIX 137 H31A 2 1.029815 0.047078 0.050174 11.00000 -1.50000 H31B 2 0.956449 0.173667 0.007027 11.00000 -1.50000 H31C 2 0.904526 0.090393 0.062644 11.00000 -1.50000 AFIX 0 C16 1 0.819430 -0.135845 0.201490 11.00000 0.02362 0.03515 = 0.11388 -0.04422 0.01670 -0.00668 AFIX 137 H16A 2 0.781029 -0.175873 0.197165 11.00000 -1.50000 H16B 2 0.832996 -0.154343 0.262374 11.00000 -1.50000 H16C 2 0.886715 -0.155541 0.171010 11.00000 -1.50000 AFIX 0 C17 1 0.726380 0.023228 0.063301 11.00000 0.04225 0.10216 = 0.05238 -0.05614 0.02472 -0.03873 AFIX 137 H17A 2 0.680747 -0.009512 0.058595 11.00000 -1.50000 H17B 2 0.792169 -0.001417 0.032051 11.00000 -1.50000 H17C 2 0.690090 0.102544 0.038329 11.00000 -1.50000 AFIX 0 C53 1 0.961433 0.493995 0.140626 11.00000 0.03918 0.10162 = 0.02560 -0.01691 0.00638 -0.04097 AFIX 137 H53A 2 0.891735 0.507967 0.123206 11.00000 -1.50000 H53B 2 1.013334 0.475907 0.096518 11.00000 -1.50000 H53C 2 0.958544 0.558983 0.146968 11.00000 -1.50000 AFIX 0 O2 5 0.677375 0.588449 0.135112 11.00000 0.03586 0.01871 = 0.03363 -0.00737 -0.00155 -0.01368 PART 2 F2B 3 0.539411 0.776500 -0.006010 10.50000 0.19594 0.03992 = 0.17861 -0.04450 -0.16424 0.03371 PART 0 PART 1 F3A 3 0.571263 0.785774 -0.021908 10.50000 0.11170 0.03627 = 0.02681 -0.00266 -0.02875 -0.03192 PART 0 PART 2 O3B 5 0.521366 0.711680 0.181768 10.50000 0.05896 0.04299 = 0.11768 -0.04749 0.06075 -0.02963 PART 0 PART 1 O3A 5 0.499928 0.725269 0.156847 10.50000 0.05665 0.03623 = 0.12718 -0.03916 0.03880 -0.02487 O4A 5 0.662056 0.720798 0.198963 10.50000 0.13145 0.03385 = 0.02960 -0.00520 -0.02580 -0.04242 PART 0 PART 2 O4B 5 0.690574 0.720987 0.186499 10.50000 0.07578 0.03660 = 0.07890 -0.01624 -0.04396 -0.01843 PART 0 PART 1 S1A 7 0.615507 0.696411 0.147476 10.50000 0.07642 0.02760 = 0.07874 -0.01674 -0.01321 -0.01751 PART 0 PART 2 S1B 7 0.621957 0.693502 0.147006 10.50000 0.03007 0.01006 = 0.00607 -0.00424 0.00795 -0.01301 PART 0 PART 1 F2A 3 0.572997 0.896314 0.031761 10.50000 0.04246 0.00907 = 0.02015 -0.00561 0.00120 -0.00923 PART 0 PART 2 F3B 3 0.567753 0.891384 0.029846 10.50000 0.14188 0.02684 = 0.07933 -0.00596 -0.02624 -0.00146 C54B 1 0.605472 0.787022 0.040785 10.50000 0.08718 0.03494 = 0.03162 -0.01363 -0.00160 -0.01346 PART 0 PART 1 C54A 1 0.621275 0.792430 0.031779 10.50000 0.03465 0.01176 = 0.02399 -0.00412 0.00345 -0.00970 PART 0 PART 2 F1B 3 0.699911 0.765876 -0.003960 10.50000 0.16057 0.03702 = 0.05362 0.00685 0.07015 -0.00909 PART 0 PART 1 F1A 3 0.722367 0.771081 0.008854 10.50000 0.03717 0.03850 = 0.11407 -0.01346 0.02644 -0.01722 HKLF 4 REM im082_a.res in P-1 REM wR2 = 0.1284, GooF = S = 1.013, Restrained GooF = 1.008 for all data REM R1 = 0.0517 for 8867 Fo > 4sig(Fo) and 0.0972 for all 13452 data REM 677 parameters refined using 311 restraints END WGHT 0.0512 1.2979 REM Highest difference peak 0.448, deepest hole -0.470, 1-sigma level 0.064 Q1 1 1.0846 -0.1430 0.2428 11.00000 0.05 0.45 Q2 1 0.4243 -0.1202 0.1194 11.00000 0.05 0.45 Q3 1 0.3241 0.4827 0.0675 11.00000 0.05 0.44 Q4 1 1.0395 -0.1451 0.3200 11.00000 0.05 0.41 Q5 1 0.7782 0.1666 0.2597 11.00000 0.05 0.39 Q6 1 0.8190 0.2220 0.2817 11.00000 0.05 0.37 Q7 1 1.2582 -0.3278 0.3051 11.00000 0.05 0.36 Q8 1 0.7086 0.2262 0.1441 11.00000 0.05 0.35 Q9 1 0.3379 0.5346 0.1140 11.00000 0.05 0.35 Q10 1 0.8218 0.3602 0.2814 11.00000 0.05 0.34 Q11 1 0.6243 0.0829 0.2219 11.00000 0.05 0.34 Q12 1 1.1744 -0.2452 0.2212 11.00000 0.05 0.33 Q13 1 0.8556 0.4987 0.3687 11.00000 0.05 0.32 Q14 1 0.6645 0.2628 0.2009 11.00000 0.05 0.32 Q15 1 0.4648 0.0688 0.2680 11.00000 0.05 0.31 Q16 1 0.9808 0.0713 0.1813 11.00000 0.05 0.31 Q17 1 0.8451 0.3406 0.1812 11.00000 0.05 0.31 Q18 1 0.9401 -0.0803 0.4370 11.00000 0.05 0.31 Q19 1 1.0054 -0.1561 0.4999 11.00000 0.05 0.30 Q20 1 0.7668 0.6019 0.4775 11.00000 0.05 0.30 Q21 1 0.5021 0.3788 0.1386 11.00000 0.05 0.30 Q22 1 0.5643 0.1590 0.2476 11.00000 0.05 0.30 Q23 1 0.7665 0.4209 0.3253 11.00000 0.05 0.30 Q24 1 0.6156 0.6178 0.1590 11.00000 0.05 0.30 Q25 1 0.9013 -0.0686 0.4139 11.00000 0.05 0.30 Q26 1 0.9412 0.4621 0.2233 11.00000 0.05 0.30 Q27 1 0.1619 0.4948 0.0153 11.00000 0.05 0.29 Q28 1 1.0689 -0.0282 0.1642 11.00000 0.05 0.29 Q29 1 0.7374 0.3379 0.2012 11.00000 0.05 0.29 Q30 1 0.7347 0.4608 0.3833 11.00000 0.05 0.28 Q31 1 0.5135 0.1817 0.3868 11.00000 0.05 0.28 Q32 1 0.8225 0.5600 0.4080 11.00000 0.05 0.28 Q33 1 0.2266 0.5430 0.0398 11.00000 0.05 0.28 Q34 1 0.9794 0.0363 0.2716 11.00000 0.05 0.27 Q35 1 0.5101 0.6503 0.2546 11.00000 0.05 0.27 Q36 1 0.7931 0.3754 0.3600 11.00000 0.05 0.27 Q37 1 0.4424 0.7648 0.0754 11.00000 0.05 0.26 Q38 1 0.6812 0.3461 0.1802 11.00000 0.05 0.26 Q39 1 0.6508 0.1745 0.2571 11.00000 0.05 0.26 Q40 1 0.4608 -0.0814 0.0989 11.00000 0.05 0.26 Q41 1 0.4802 0.7997 0.0808 11.00000 0.05 0.26 Q42 1 0.4841 0.4608 0.1449 11.00000 0.05 0.26 Q43 1 0.8663 0.1037 0.2988 11.00000 0.05 0.26 Q44 1 0.4966 0.1954 0.3131 11.00000 0.05 0.25 Q45 1 0.9467 0.0396 0.2520 11.00000 0.05 0.25 Q46 1 0.7615 0.7277 0.1209 11.00000 0.05 0.25 Q47 1 0.6025 0.0210 0.2163 11.00000 0.05 0.25 Q48 1 0.4419 0.2793 0.3215 11.00000 0.05 0.24 Q49 1 0.5563 0.3740 0.1750 11.00000 0.05 0.24 Q50 1 0.7627 0.1748 0.1743 11.00000 0.05 0.24 ; _shelx_res_checksum 68039 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 P1 P 0.70906(4) 0.19074(4) 0.20039(4) 0.01587(12) Uani 1 1 d . . . . . P2 P 0.80498(4) 0.15076(4) 0.31515(4) 0.01538(12) Uani 1 1 d . . . . . P3 P 0.82690(5) 0.30882(4) 0.24240(4) 0.01607(12) Uani 1 1 d . . . . . O1 O 0.22877(14) 0.61017(14) 0.02762(12) 0.0352(4) Uani 1 1 d . . . . . N1 N 0.69072(14) 0.38052(14) 0.20615(11) 0.0167(4) Uani 1 1 d . . . . . H1 H 0.658451 0.449149 0.201014 0.020 Uiso 1 1 calc R U . . . C1 C 0.63499(17) 0.33696(17) 0.18642(13) 0.0153(4) Uani 1 1 d . . . . . C40 C 0.74606(17) 0.40372(17) 0.37973(14) 0.0169(4) Uani 1 1 d . . . . . C2 C 0.53040(17) 0.40718(17) 0.14350(13) 0.0172(4) Uani 1 1 d . . . . . C41 C 0.74728(18) 0.47467(17) 0.41829(15) 0.0205(5) Uani 1 1 d . . . . . H41 H 0.696195 0.490972 0.460875 0.025 Uiso 1 1 calc R U . . . C14 C 0.52848(17) 0.14305(17) 0.29417(14) 0.0167(4) Uani 1 1 d . . . . . C39 C 0.82491(17) 0.37867(17) 0.31589(14) 0.0170(4) Uani 1 1 d . . . . . C3 C 0.48499(18) 0.36832(18) 0.10094(14) 0.0207(5) Uani 1 1 d . . . . . H3 H 0.522995 0.297317 0.099192 0.025 Uiso 1 1 calc R U . . . C24 C 0.92818(17) 0.03290(17) 0.30281(15) 0.0180(4) Uani 1 1 d . . . . . C13 C 0.46127(18) 0.08861(18) 0.30655(14) 0.0203(5) Uani 1 1 d . . . . . H13 H 0.398980 0.107568 0.339526 0.024 Uiso 1 1 calc R U . . . C42 C 0.82159(18) 0.52169(17) 0.39558(15) 0.0201(5) Uani 1 1 d . . . . . C25 C 0.98885(17) 0.02715(18) 0.22544(15) 0.0194(5) Uani 1 1 d . . . . . C44 C 0.90524(18) 0.42114(18) 0.29555(15) 0.0199(5) Uani 1 1 d . . . . . C21 C 0.49998(17) 0.22284(18) 0.34284(14) 0.0189(5) Uani 1 1 d . . . . . H21 H 0.547866 0.261657 0.321558 0.023 Uiso 1 1 calc R U . . . C12 C 0.48353(18) 0.00738(17) 0.27169(15) 0.0204(5) Uani 1 1 d . . . . . C18 C 0.40602(19) -0.04608(18) 0.27871(16) 0.0233(5) Uani 1 1 d . . . . . H18 H 0.445860 -0.126679 0.304592 0.028 Uiso 1 1 calc R U . . . C9 C 0.62095(17) 0.11684(17) 0.24166(14) 0.0164(4) Uani 1 1 d . . . . . C36 C 0.89268(18) -0.06885(18) 0.46731(15) 0.0217(5) Uani 1 1 d . . . . . H36 H 0.852323 0.007389 0.465980 0.026 Uiso 1 1 calc R U . . . C10 C 0.64894(18) 0.02829(18) 0.21087(15) 0.0210(5) Uani 1 1 d . . . . . C29 C 0.95380(18) -0.06406(17) 0.38034(15) 0.0197(5) Uani 1 1 d . . . . . C23 C 0.38319(18) 0.31081(19) 0.32622(16) 0.0243(5) Uani 1 1 d . . . . . H23A H 0.334479 0.275692 0.352509 0.037 Uiso 1 1 calc R U . . . H23B H 0.369631 0.347283 0.263933 0.037 Uiso 1 1 calc R U . . . H23C H 0.372548 0.364389 0.351835 0.037 Uiso 1 1 calc R U . . . C30 C 0.97682(17) 0.12569(18) 0.14073(14) 0.0204(5) Uani 1 1 d . . . . . H30 H 0.911265 0.188673 0.145615 0.024 Uiso 1 1 calc R U . . . C48 C 0.8145(2) 0.60569(19) 0.43396(16) 0.0255(5) Uani 1 1 d . . . . . H48 H 0.867121 0.636311 0.403126 0.031 Uiso 1 1 calc R U . . . C27 C 1.09397(18) -0.17099(18) 0.30164(16) 0.0239(5) Uani 1 1 d . . . . . C33 C 1.1802(2) -0.28234(19) 0.30027(17) 0.0283(5) Uani 1 1 d . . . . . H33 H 1.193347 -0.334196 0.361386 0.034 Uiso 1 1 calc R U . . . C4 C 0.38435(19) 0.43335(19) 0.06119(15) 0.0239(5) Uani 1 1 d . . . . . H4 H 0.354566 0.406363 0.033313 0.029 Uiso 1 1 calc R U . . . C7 C 0.47258(18) 0.51658(18) 0.14290(15) 0.0224(5) Uani 1 1 d . . . . . H7 H 0.502220 0.544734 0.169762 0.027 Uiso 1 1 calc R U . . . C28 C 1.03613(18) -0.16354(18) 0.37717(16) 0.0235(5) Uani 1 1 d . . . . . H28 H 1.052438 -0.226836 0.427732 0.028 Uiso 1 1 calc R U . . . C45 C 0.65946(18) 0.35878(18) 0.40948(14) 0.0193(5) Uani 1 1 d . . . . . H45 H 0.669110 0.310677 0.377036 0.023 Uiso 1 1 calc R U . . . C26 C 1.07022(18) -0.07554(19) 0.22721(16) 0.0238(5) Uani 1 1 d . . . . . H26 H 1.109904 -0.079814 0.176377 0.029 Uiso 1 1 calc R U . . . C43 C 0.90088(19) 0.49179(18) 0.33638(15) 0.0220(5) Uani 1 1 d . . . . . H43 H 0.953395 0.519762 0.323192 0.026 Uiso 1 1 calc R U . . . C11 C 0.57931(19) -0.02359(18) 0.22684(15) 0.0229(5) Uani 1 1 d . . . . . H11 H 0.597833 -0.081387 0.206587 0.028 Uiso 1 1 calc R U . . . C22 C 0.5221(2) 0.1568(2) 0.44162(15) 0.0275(5) Uani 1 1 d . . . . . H22A H 0.505280 0.206893 0.472242 0.041 Uiso 1 1 calc R U . . . H22B H 0.596789 0.106477 0.450720 0.041 Uiso 1 1 calc R U . . . H22C H 0.478114 0.115560 0.463737 0.041 Uiso 1 1 calc R U . . . C5 C 0.32828(19) 0.54023(19) 0.06364(15) 0.0261(5) Uani 1 1 d . . . . . C46 C 0.54609(19) 0.4527(2) 0.38864(17) 0.0279(5) Uani 1 1 d . . . . . H46A H 0.533885 0.499499 0.421376 0.042 Uiso 1 1 calc R U . . . H46B H 0.493422 0.421610 0.404785 0.042 Uiso 1 1 calc R U . . . H46C H 0.540054 0.495615 0.326734 0.042 Uiso 1 1 calc R U . . . C34 C 1.1382(2) -0.3282(2) 0.25004(18) 0.0337(6) Uani 1 1 d . . . . . H34A H 1.073544 -0.335612 0.277373 0.051 Uiso 1 1 calc R U . . . H34B H 1.191871 -0.399417 0.251292 0.051 Uiso 1 1 calc R U . . . H34C H 1.122809 -0.278180 0.190039 0.051 Uiso 1 1 calc R U . . . C49 C 0.8438(2) 0.5515(2) 0.53113(17) 0.0331(6) Uani 1 1 d . . . . . H49A H 0.847318 0.604459 0.551399 0.050 Uiso 1 1 calc R U . . . H49B H 0.912671 0.489586 0.539720 0.050 Uiso 1 1 calc R U . . . H49C H 0.790056 0.526295 0.563790 0.050 Uiso 1 1 calc R U . . . C38 C 0.8114(2) -0.1174(2) 0.47416(17) 0.0301(6) Uani 1 1 d . . . . . H38A H 0.761888 -0.071995 0.425296 0.045 Uiso 1 1 calc R U . . . H38B H 0.772287 -0.119442 0.528266 0.045 Uiso 1 1 calc R U . . . H38C H 0.848707 -0.191232 0.473235 0.045 Uiso 1 1 calc R U . . . C19 C 0.3695(2) -0.0183(2) 0.18590(17) 0.0291(5) Uani 1 1 d . . . . . H19A H 0.328856 0.060266 0.159566 0.044 Uiso 1 1 calc R U . . . H19B H 0.325253 -0.056178 0.189461 0.044 Uiso 1 1 calc R U . . . H19C H 0.431585 -0.041564 0.150550 0.044 Uiso 1 1 calc R U . . . C50 C 0.7030(2) 0.70182(19) 0.41739(18) 0.0299(6) Uani 1 1 d . . . . . H50A H 0.650114 0.675074 0.449895 0.045 Uiso 1 1 calc R U . . . H50B H 0.686121 0.733292 0.355629 0.045 Uiso 1 1 calc R U . . . H50C H 0.702761 0.757488 0.436237 0.045 Uiso 1 1 calc R U . . . C6 C 0.37365(19) 0.58131(19) 0.10329(15) 0.0268(5) Uani 1 1 d . . . . . H6 H 0.336595 0.653363 0.102947 0.032 Uiso 1 1 calc R U . . . C37 C 0.9674(2) -0.1337(2) 0.54789(16) 0.0289(5) Uani 1 1 d . . . . . H37A H 1.000929 -0.210888 0.555167 0.043 Uiso 1 1 calc R U . . . H37B H 0.926230 -0.124886 0.599421 0.043 Uiso 1 1 calc R U . . . H37C H 1.021875 -0.106150 0.539675 0.043 Uiso 1 1 calc R U . . . C32 C 1.07288(19) 0.1569(2) 0.13191(17) 0.0291(5) Uani 1 1 d . . . . . H32A H 1.079906 0.166807 0.184761 0.044 Uiso 1 1 calc R U . . . H32B H 1.060822 0.224620 0.082626 0.044 Uiso 1 1 calc R U . . . H32C H 1.137765 0.098688 0.122838 0.044 Uiso 1 1 calc R U . . . C52 C 1.10489(19) 0.3717(2) 0.25781(17) 0.0306(6) Uani 1 1 d . . . . . H52A H 1.104966 0.436901 0.261540 0.046 Uiso 1 1 calc R U . . . H52B H 1.158104 0.348207 0.216176 0.046 Uiso 1 1 calc R U . . . H52C H 1.121461 0.313592 0.314638 0.046 Uiso 1 1 calc R U . . . C8 C 0.1732(2) 0.5636(2) 0.00113(17) 0.0354(6) Uani 1 1 d . . . . . H8A H 0.211103 0.539853 -0.046475 0.053 Uiso 1 1 calc R U . . . H8B H 0.101721 0.618227 -0.018019 0.053 Uiso 1 1 calc R U . . . H8C H 0.169189 0.501131 0.049894 0.053 Uiso 1 1 calc R U . . . C20 C 0.3079(2) -0.0122(2) 0.33566(17) 0.0303(6) Uani 1 1 d . . . . . H20A H 0.330937 -0.032451 0.394383 0.045 Uiso 1 1 calc R U . . . H20B H 0.263666 -0.049362 0.337216 0.045 Uiso 1 1 calc R U . . . H20C H 0.267120 0.066556 0.311347 0.045 Uiso 1 1 calc R U . . . C47 C 0.6725(2) 0.2888(2) 0.50742(16) 0.0312(6) Uani 1 1 d . . . . . H47A H 0.741739 0.227217 0.517965 0.047 Uiso 1 1 calc R U . . . H47B H 0.616840 0.261788 0.525620 0.047 Uiso 1 1 calc R U . . . H47C H 0.667175 0.333360 0.540371 0.047 Uiso 1 1 calc R U . . . C35 C 1.2868(2) -0.2766(2) 0.26353(18) 0.0324(6) Uani 1 1 d . . . . . H35A H 1.278155 -0.231270 0.202105 0.049 Uiso 1 1 calc R U . . . H35B H 1.340369 -0.349924 0.270545 0.049 Uiso 1 1 calc R U . . . H35C H 1.309387 -0.244867 0.294728 0.049 Uiso 1 1 calc R U . . . C15 C 0.75201(19) -0.0116(2) 0.16007(18) 0.0294(6) Uani 1 1 d . . . . . H15 H 0.795527 0.026216 0.162383 0.035 Uiso 1 1 calc R U . . . C51 C 0.9941(2) 0.3978(2) 0.22782(17) 0.0314(6) Uani 1 1 d . . . . . H51 H 0.999198 0.332423 0.218327 0.038 Uiso 1 1 calc R U . . . C31 C 0.9659(2) 0.1075(2) 0.05734(16) 0.0289(6) Uani 1 1 d . . . . . H31A H 1.029815 0.047078 0.050174 0.043 Uiso 1 1 calc R U . . . H31B H 0.956449 0.173667 0.007027 0.043 Uiso 1 1 calc R U . . . H31C H 0.904526 0.090393 0.062644 0.043 Uiso 1 1 calc R U . . . C16 C 0.8194(2) -0.1358(2) 0.2015(3) 0.0558(10) Uani 1 1 d . . . . . H16A H 0.781029 -0.175873 0.197165 0.084 Uiso 1 1 calc R U . . . H16B H 0.832996 -0.154343 0.262374 0.084 Uiso 1 1 calc R U . . . H16C H 0.886715 -0.155541 0.171010 0.084 Uiso 1 1 calc R U . . . C17 C 0.7264(3) 0.0232(3) 0.0633(2) 0.0557(9) Uani 1 1 d . . . . . H17A H 0.680747 -0.009512 0.058595 0.084 Uiso 1 1 calc R U . . . H17B H 0.792169 -0.001417 0.032051 0.084 Uiso 1 1 calc R U . . . H17C H 0.690090 0.102544 0.038329 0.084 Uiso 1 1 calc R U . . . C53 C 0.9614(2) 0.4940(3) 0.14063(18) 0.0535(9) Uani 1 1 d . . . . . H53A H 0.891735 0.507967 0.123206 0.080 Uiso 1 1 calc R U . . . H53B H 1.013334 0.475907 0.096518 0.080 Uiso 1 1 calc R U . . . H53C H 0.958544 0.558983 0.146968 0.080 Uiso 1 1 calc R U . . . O2 O 0.67738(14) 0.58845(13) 0.13511(11) 0.0288(4) Uani 1 1 d . U . . . F2B F 0.5394(11) 0.7765(8) -0.0060(8) 0.146(6) Uani 0.5 1 d . . P A 2 F3A F 0.5713(9) 0.7858(8) -0.0219(5) 0.0567(19) Uani 0.5 1 d . U P B 1 O3B O 0.5214(14) 0.712(2) 0.1818(16) 0.071(5) Uani 0.5 1 d . U P A 2 O3A O 0.4999(15) 0.725(2) 0.1568(17) 0.073(5) Uani 0.5 1 d . U P B 1 O4A O 0.6621(15) 0.7208(19) 0.1990(12) 0.060(4) Uani 0.5 1 d . U P B 1 O4B O 0.6906(15) 0.721(2) 0.1865(13) 0.061(4) Uani 0.5 1 d . U P A 2 S1A S 0.6155(5) 0.6964(4) 0.1475(3) 0.0613(14) Uani 0.5 1 d . U P B 1 S1B S 0.6220(3) 0.6935(3) 0.14701(16) 0.0141(6) Uani 0.5 1 d . U P A 2 F2A F 0.5730(6) 0.8963(6) 0.0318(4) 0.0244(12) Uani 0.5 1 d . U P B 1 F3B F 0.5678(10) 0.8914(9) 0.0298(8) 0.096(3) Uani 0.5 1 d . U P A 2 C54B C 0.6055(16) 0.787(2) 0.0408(15) 0.055(4) Uani 0.5 1 d . U P A 2 C54A C 0.6213(12) 0.7924(15) 0.0318(13) 0.025(2) Uani 0.5 1 d D U P B 1 F1B F 0.6999(9) 0.7659(9) -0.0040(6) 0.112(5) Uani 0.5 1 d . U P A 2 F1A F 0.7224(7) 0.7711(10) 0.0089(8) 0.071(2) Uani 0.5 1 d D U P B 1 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 P1 0.0143(3) 0.0163(3) 0.0201(3) -0.0115(2) 0.0027(2) -0.0054(2) P2 0.0146(3) 0.0137(3) 0.0184(3) -0.0086(2) 0.0020(2) -0.0044(2) P3 0.0176(3) 0.0167(3) 0.0173(3) -0.0098(2) 0.0039(2) -0.0079(2) O1 0.0247(10) 0.0339(10) 0.0347(11) -0.0089(8) -0.0102(8) -0.0005(8) N1 0.0184(9) 0.0128(8) 0.0198(10) -0.0096(8) 0.0025(7) -0.0047(7) C1 0.0179(11) 0.0161(10) 0.0114(10) -0.0073(8) 0.0043(8) -0.0057(8) C40 0.0192(11) 0.0141(10) 0.0161(11) -0.0065(9) 0.0000(8) -0.0046(8) C2 0.0187(11) 0.0178(10) 0.0130(11) -0.0056(9) 0.0020(8) -0.0062(9) C41 0.0220(12) 0.0187(11) 0.0194(12) -0.0110(9) 0.0023(9) -0.0041(9) C14 0.0171(11) 0.0166(10) 0.0152(11) -0.0051(9) -0.0004(8) -0.0062(9) C39 0.0195(11) 0.0149(10) 0.0175(11) -0.0068(9) 0.0005(9) -0.0070(9) C3 0.0204(12) 0.0221(11) 0.0190(12) -0.0097(10) 0.0037(9) -0.0071(9) C24 0.0151(11) 0.0170(10) 0.0246(12) -0.0116(9) -0.0005(9) -0.0051(9) C13 0.0183(11) 0.0211(11) 0.0200(12) -0.0063(9) 0.0020(9) -0.0083(9) C42 0.0238(12) 0.0154(10) 0.0206(12) -0.0069(9) -0.0052(9) -0.0053(9) C25 0.0164(11) 0.0207(11) 0.0256(12) -0.0140(10) 0.0014(9) -0.0068(9) C44 0.0208(12) 0.0216(11) 0.0192(12) -0.0086(9) 0.0011(9) -0.0096(9) C21 0.0181(11) 0.0213(11) 0.0215(12) -0.0118(9) 0.0066(9) -0.0102(9) C12 0.0219(12) 0.0169(10) 0.0219(12) -0.0041(9) -0.0033(9) -0.0087(9) C18 0.0245(12) 0.0184(11) 0.0280(13) -0.0051(10) -0.0026(10) -0.0114(10) C9 0.0152(10) 0.0150(10) 0.0200(11) -0.0079(9) -0.0018(8) -0.0049(8) C36 0.0236(12) 0.0171(11) 0.0224(12) -0.0068(9) -0.0004(9) -0.0068(9) C10 0.0177(11) 0.0196(11) 0.0288(13) -0.0136(10) 0.0010(9) -0.0062(9) C29 0.0177(11) 0.0168(10) 0.0266(12) -0.0099(10) -0.0031(9) -0.0059(9) C23 0.0192(12) 0.0261(12) 0.0291(13) -0.0153(11) 0.0064(10) -0.0077(10) C30 0.0144(11) 0.0245(11) 0.0233(12) -0.0146(10) 0.0052(9) -0.0054(9) C48 0.0325(14) 0.0248(12) 0.0267(13) -0.0148(11) 0.0027(10) -0.0141(11) C27 0.0217(12) 0.0197(11) 0.0314(13) -0.0135(10) -0.0002(10) -0.0055(9) C33 0.0298(14) 0.0212(12) 0.0312(14) -0.0130(11) 0.0017(11) -0.0055(10) C4 0.0239(12) 0.0299(12) 0.0178(12) -0.0074(10) 0.0003(9) -0.0118(10) C7 0.0233(12) 0.0214(11) 0.0205(12) -0.0096(10) 0.0032(9) -0.0065(10) C28 0.0226(12) 0.0154(10) 0.0285(13) -0.0060(10) -0.0013(10) -0.0055(9) C45 0.0215(11) 0.0207(11) 0.0201(12) -0.0125(9) 0.0060(9) -0.0099(9) C26 0.0197(12) 0.0273(12) 0.0274(13) -0.0167(11) 0.0053(9) -0.0079(10) C43 0.0238(12) 0.0228(11) 0.0232(12) -0.0083(10) -0.0001(9) -0.0127(10) C11 0.0256(12) 0.0190(11) 0.0293(13) -0.0126(10) -0.0016(10) -0.0095(10) C22 0.0310(14) 0.0328(13) 0.0221(13) -0.0137(11) 0.0040(10) -0.0139(11) C5 0.0191(12) 0.0270(12) 0.0187(12) -0.0027(10) 0.0007(9) -0.0026(10) C46 0.0239(13) 0.0317(13) 0.0321(14) -0.0198(11) 0.0073(10) -0.0100(11) C34 0.0361(15) 0.0219(12) 0.0444(16) -0.0207(12) 0.0022(12) -0.0059(11) C49 0.0447(17) 0.0315(14) 0.0312(14) -0.0180(12) -0.0002(12) -0.0164(12) C38 0.0303(14) 0.0296(13) 0.0321(14) -0.0101(11) 0.0034(11) -0.0155(11) C19 0.0266(13) 0.0313(13) 0.0349(15) -0.0143(12) 0.0006(11) -0.0147(11) C50 0.0327(14) 0.0215(12) 0.0406(15) -0.0181(11) 0.0003(11) -0.0094(11) C6 0.0268(13) 0.0221(12) 0.0229(13) -0.0096(10) 0.0005(10) -0.0012(10) C37 0.0329(14) 0.0257(12) 0.0250(13) -0.0063(11) -0.0008(11) -0.0113(11) C32 0.0211(12) 0.0303(13) 0.0344(14) -0.0119(11) 0.0023(10) -0.0097(10) C52 0.0239(13) 0.0366(14) 0.0369(15) -0.0186(12) 0.0083(11) -0.0153(11) C8 0.0257(14) 0.0407(15) 0.0278(14) -0.0027(12) -0.0010(11) -0.0110(12) C20 0.0333(14) 0.0363(14) 0.0286(14) -0.0094(11) 0.0045(11) -0.0240(12) C47 0.0380(15) 0.0337(14) 0.0266(14) -0.0100(11) 0.0059(11) -0.0213(12) C35 0.0261(14) 0.0289(13) 0.0378(15) -0.0194(12) 0.0012(11) -0.0012(11) C15 0.0217(12) 0.0322(13) 0.0510(17) -0.0322(13) 0.0110(11) -0.0141(11) C51 0.0330(14) 0.0466(15) 0.0342(15) -0.0268(13) 0.0131(11) -0.0269(13) C31 0.0273(13) 0.0349(14) 0.0250(13) -0.0178(11) 0.0071(10) -0.0094(11) C16 0.0236(15) 0.0352(16) 0.114(3) -0.0442(19) 0.0167(17) -0.0067(13) C17 0.0422(18) 0.102(3) 0.052(2) -0.056(2) 0.0247(15) -0.0387(19) C53 0.0392(18) 0.102(3) 0.0256(15) -0.0169(17) 0.0064(13) -0.0410(19) O2 0.0359(10) 0.0187(8) 0.0336(10) -0.0074(7) -0.0015(8) -0.0137(7) F2B 0.196(12) 0.040(5) 0.179(10) -0.045(6) -0.164(9) 0.034(5) F3A 0.112(5) 0.036(3) 0.027(2) -0.003(2) -0.029(3) -0.032(3) O3B 0.059(7) 0.043(7) 0.118(11) -0.047(8) 0.061(8) -0.030(7) O3A 0.057(6) 0.036(5) 0.127(13) -0.039(7) 0.039(6) -0.025(5) O4A 0.131(12) 0.034(5) 0.030(3) -0.005(3) -0.026(6) -0.042(8) O4B 0.076(6) 0.037(5) 0.079(10) -0.016(7) -0.044(6) -0.018(4) S1A 0.076(3) 0.028(2) 0.079(3) -0.0167(19) -0.013(2) -0.018(2) S1B 0.0301(14) 0.0101(13) 0.0061(9) -0.0042(9) 0.0079(9) -0.0130(11) F2A 0.042(3) 0.009(3) 0.020(3) -0.006(2) 0.001(2) -0.009(2) F3B 0.142(8) 0.027(4) 0.079(6) -0.006(4) -0.026(6) -0.001(5) C54B 0.087(9) 0.035(5) 0.032(5) -0.014(4) -0.002(5) -0.013(7) C54A 0.035(4) 0.012(3) 0.024(4) -0.004(3) 0.003(3) -0.010(3) F1B 0.161(10) 0.037(4) 0.054(4) 0.007(3) 0.070(6) -0.009(6) F1A 0.037(3) 0.039(3) 0.114(6) -0.013(3) 0.026(3) -0.017(2) 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' 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 C1 P1 C9 110.97(10) . . ? C1 P1 P2 94.28(7) . . ? C9 P1 P2 106.71(7) . . ? C24 P2 P1 100.03(7) . . ? C24 P2 P3 109.03(7) . . ? P1 P2 P3 87.97(3) . . ? N1 P3 C39 100.38(9) . . ? N1 P3 P2 91.43(6) . . ? C39 P3 P2 112.51(7) . . ? C5 O1 C8 116.5(2) . . ? C1 N1 P3 125.17(14) . . ? C1 N1 H1 117.4 . . ? P3 N1 H1 117.4 . . ? N1 C1 C2 120.47(18) . . ? N1 C1 P1 114.52(15) . . ? C2 C1 P1 124.23(15) . . ? C41 C40 C39 118.1(2) . . ? C41 C40 C45 117.54(19) . . ? C39 C40 C45 124.39(18) . . ? C3 C2 C7 118.3(2) . . ? C3 C2 C1 120.50(19) . . ? C7 C2 C1 121.2(2) . . ? C42 C41 C40 122.6(2) . . ? C42 C41 H41 118.7 . . ? C40 C41 H41 118.7 . . ? C13 C14 C9 118.49(19) . . ? C13 C14 C21 117.35(19) . . ? C9 C14 C21 124.06(19) . . ? C40 C39 C44 119.95(19) . . ? C40 C39 P3 126.46(16) . . ? C44 C39 P3 113.10(16) . . ? C4 C3 C2 121.3(2) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C25 C24 C29 119.37(19) . . ? C25 C24 P2 127.66(17) . . ? C29 C24 P2 112.63(16) . . ? C12 C13 C14 122.8(2) . . ? C12 C13 H13 118.6 . . ? C14 C13 H13 118.6 . . ? C43 C42 C41 118.21(19) . . ? C43 C42 C48 120.9(2) . . ? C41 C42 C48 120.8(2) . . ? C26 C25 C24 118.4(2) . . ? C26 C25 C30 116.58(19) . . ? C24 C25 C30 124.97(19) . . ? C43 C44 C39 118.6(2) . . ? C43 C44 C51 117.8(2) . . ? C39 C44 C51 123.57(19) . . ? C14 C21 C22 109.39(18) . . ? C14 C21 C23 113.05(18) . . ? C22 C21 C23 110.96(18) . . ? C14 C21 H21 107.7 . . ? C22 C21 H21 107.7 . . ? C23 C21 H21 107.7 . . ? C11 C12 C13 117.6(2) . . ? C11 C12 C18 119.30(19) . . ? C13 C12 C18 123.1(2) . . ? C20 C18 C12 114.37(19) . . ? C20 C18 C19 109.6(2) . . ? C12 C18 C19 109.00(19) . . ? C20 C18 H18 107.9 . . ? C12 C18 H18 107.9 . . ? C19 C18 H18 107.9 . . ? C14 C9 C10 119.22(19) . . ? C14 C9 P1 127.12(15) . . ? C10 C9 P1 113.54(16) . . ? C38 C36 C37 110.96(19) . . ? C38 C36 C29 109.40(19) . . ? C37 C36 C29 112.95(19) . . ? C38 C36 H36 107.8 . . ? C37 C36 H36 107.8 . . ? C29 C36 H36 107.8 . . ? C11 C10 C9 119.0(2) . . ? C11 C10 C15 118.32(19) . . ? C9 C10 C15 122.72(19) . . ? C28 C29 C24 119.0(2) . . ? C28 C29 C36 116.7(2) . . ? C24 C29 C36 124.21(19) . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C30 C31 114.26(19) . . ? C25 C30 C32 109.41(19) . . ? C31 C30 C32 110.04(19) . . ? C25 C30 H30 107.6 . . ? C31 C30 H30 107.6 . . ? C32 C30 H30 107.6 . . ? C49 C48 C42 111.65(19) . . ? C49 C48 C50 111.4(2) . . ? C42 C48 C50 110.88(19) . . ? C49 C48 H48 107.5 . . ? C42 C48 H48 107.5 . . ? C50 C48 H48 107.5 . . ? C28 C27 C26 118.3(2) . . ? C28 C27 C33 120.4(2) . . ? C26 C27 C33 121.3(2) . . ? C35 C33 C27 112.9(2) . . ? C35 C33 C34 111.6(2) . . ? C27 C33 C34 110.0(2) . . ? C35 C33 H33 107.4 . . ? C27 C33 H33 107.4 . . ? C34 C33 H33 107.4 . . ? C3 C4 C5 118.9(2) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? C6 C7 C2 120.6(2) . . ? C6 C7 H7 119.7 . . ? C2 C7 H7 119.7 . . ? C27 C28 C29 122.2(2) . . ? C27 C28 H28 118.9 . . ? C29 C28 H28 118.9 . . ? C40 C45 C47 110.22(19) . . ? C40 C45 C46 111.37(18) . . ? C47 C45 C46 111.10(19) . . ? C40 C45 H45 108.0 . . ? C47 C45 H45 108.0 . . ? C46 C45 H45 108.0 . . ? C27 C26 C25 122.7(2) . . ? C27 C26 H26 118.7 . . ? C25 C26 H26 118.7 . . ? C42 C43 C44 122.4(2) . . ? C42 C43 H43 118.8 . . ? C44 C43 H43 118.8 . . ? C12 C11 C10 122.5(2) . . ? C12 C11 H11 118.7 . . ? C10 C11 H11 118.7 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O1 C5 C6 115.9(2) . . ? O1 C5 C4 123.6(2) . . ? C6 C5 C4 120.5(2) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C48 C50 H50A 109.5 . . ? C48 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C48 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C7 C6 C5 120.3(2) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? O1 C8 H8A 109.5 . . ? O1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C10 C15 C17 110.5(2) . . ? C10 C15 C16 112.6(2) . . ? C17 C15 C16 112.2(2) . . ? C10 C15 H15 107.1 . . ? C17 C15 H15 107.1 . . ? C16 C15 H15 107.1 . . ? C53 C51 C52 111.4(2) . . ? C53 C51 C44 109.5(2) . . ? C52 C51 C44 113.8(2) . . ? C53 C51 H51 107.3 . . ? C52 C51 H51 107.3 . . ? C44 C51 H51 107.3 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? O4A S1A O3A 117.6(13) . . ? O4A S1A O2 116.7(10) . . ? O3A S1A O2 113.3(12) . . ? O4A S1A C54A 105.4(11) . . ? O3A S1A C54A 100.9(12) . . ? O2 S1A C54A 99.3(7) . . ? O3B S1B O2 114.3(12) . . ? O3B S1B O4B 115.5(13) . . ? O2 S1B O4B 113.4(9) . . ? O3B S1B C54B 106.8(12) . . ? O2 S1B C54B 102.8(9) . . ? O4B S1B C54B 102.1(12) . . ? F3B C54B F1B 105.2(16) . . ? F3B C54B F2B 106.8(18) . . ? F1B C54B F2B 104(2) . . ? F3B C54B S1B 117.6(19) . . ? F1B C54B S1B 111.5(15) . . ? F2B C54B S1B 110.5(14) . . ? F3A C54A F1A 111.3(16) . . ? F3A C54A F2A 107.8(13) . . ? F1A C54A F2A 108.8(14) . . ? F3A C54A S1A 111.9(11) . . ? F1A C54A S1A 109.4(12) . . ? F2A C54A S1A 107.5(12) . . ? 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 P1 C1 1.824(2) . ? P1 C9 1.830(2) . ? P1 P2 2.2262(8) . ? P2 C24 1.853(2) . ? P2 P3 2.2433(8) . ? P3 N1 1.7726(19) . ? P3 C39 1.836(2) . ? O1 C5 1.358(3) . ? O1 C8 1.413(3) . ? N1 C1 1.319(3) . ? N1 H1 0.8600 . ? C1 C2 1.451(3) . ? C40 C41 1.398(3) . ? C40 C39 1.413(3) . ? C40 C45 1.520(3) . ? C2 C3 1.393(3) . ? C2 C7 1.413(3) . ? C41 C42 1.386(3) . ? C41 H41 0.9300 . ? C14 C13 1.397(3) . ? C14 C9 1.410(3) . ? C14 C21 1.523(3) . ? C39 C44 1.419(3) . ? C3 C4 1.384(3) . ? C3 H3 0.9300 . ? C24 C25 1.415(3) . ? C24 C29 1.425(3) . ? C13 C12 1.389(3) . ? C13 H13 0.9300 . ? C42 C43 1.377(3) . ? C42 C48 1.525(3) . ? C25 C26 1.402(3) . ? C25 C30 1.521(3) . ? C44 C43 1.393(3) . ? C44 C51 1.531(3) . ? C21 C22 1.533(3) . ? C21 C23 1.537(3) . ? C21 H21 0.9800 . ? C12 C11 1.382(3) . ? C12 C18 1.531(3) . ? C18 C20 1.521(3) . ? C18 C19 1.533(3) . ? C18 H18 0.9800 . ? C9 C10 1.423(3) . ? C36 C38 1.525(3) . ? C36 C37 1.529(3) . ? C36 C29 1.532(3) . ? C36 H36 0.9800 . ? C10 C11 1.389(3) . ? C10 C15 1.523(3) . ? C29 C28 1.398(3) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C30 C31 1.534(3) . ? C30 C32 1.541(3) . ? C30 H30 0.9800 . ? C48 C49 1.516(3) . ? C48 C50 1.528(3) . ? C48 H48 0.9800 . ? C27 C28 1.378(3) . ? C27 C26 1.386(3) . ? C27 C33 1.526(3) . ? C33 C35 1.519(4) . ? C33 C34 1.536(3) . ? C33 H33 0.9800 . ? C4 C5 1.398(3) . ? C4 H4 0.9300 . ? C7 C6 1.365(3) . ? C7 H7 0.9300 . ? C28 H28 0.9300 . ? C45 C47 1.524(3) . ? C45 C46 1.535(3) . ? C45 H45 0.9800 . ? C26 H26 0.9300 . ? C43 H43 0.9300 . ? C11 H11 0.9300 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C5 C6 1.383(3) . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C6 H6 0.9300 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C52 C51 1.522(3) . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C15 C17 1.525(4) . ? C15 C16 1.525(4) . ? C15 H15 0.9800 . ? C51 C53 1.517(4) . ? C51 H51 0.9800 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? O2 S1B 1.438(3) . ? O2 S1A 1.484(5) . ? F2B C54B 1.37(3) . ? F3A C54A 1.26(3) . ? O3B S1B 1.364(17) . ? O3A S1A 1.458(19) . ? O4A S1A 1.361(16) . ? O4B S1B 1.481(17) . ? S1A C54A 1.882(17) . ? S1B C54B 1.72(2) . ? F2A C54A 1.34(2) . ? F3B C54B 1.30(3) . ? C54B F1B 1.358(18) . ? C54A F1A 1.313(13) . ? 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 C39 P3 N1 C1 -147.40(18) . . . . ? P2 P3 N1 C1 -34.20(17) . . . . ? P3 N1 C1 C2 -169.61(15) . . . . ? P3 N1 C1 P1 0.7(2) . . . . ? C9 P1 C1 N1 143.35(15) . . . . ? P2 P1 C1 N1 33.63(15) . . . . ? C9 P1 C1 C2 -46.8(2) . . . . ? P2 P1 C1 C2 -156.48(17) . . . . ? N1 C1 C2 C3 162.1(2) . . . . ? P1 C1 C2 C3 -7.2(3) . . . . ? N1 C1 C2 C7 -17.2(3) . . . . ? P1 C1 C2 C7 173.43(16) . . . . ? C39 C40 C41 C42 0.7(3) . . . . ? C45 C40 C41 C42 -179.2(2) . . . . ? C41 C40 C39 C44 2.8(3) . . . . ? C45 C40 C39 C44 -177.2(2) . . . . ? C41 C40 C39 P3 -168.60(17) . . . . ? C45 C40 C39 P3 11.3(3) . . . . ? N1 P3 C39 C40 45.5(2) . . . . ? P2 P3 C39 C40 -50.5(2) . . . . ? N1 P3 C39 C44 -126.48(16) . . . . ? P2 P3 C39 C44 137.59(14) . . . . ? C7 C2 C3 C4 -1.9(3) . . . . ? C1 C2 C3 C4 178.7(2) . . . . ? P1 P2 C24 C25 48.1(2) . . . . ? P3 P2 C24 C25 -43.2(2) . . . . ? P1 P2 C24 C29 -125.08(15) . . . . ? P3 P2 C24 C29 143.61(14) . . . . ? C9 C14 C13 C12 2.1(3) . . . . ? C21 C14 C13 C12 -174.6(2) . . . . ? C40 C41 C42 C43 -3.9(3) . . . . ? C40 C41 C42 C48 175.1(2) . . . . ? C29 C24 C25 C26 2.1(3) . . . . ? P2 C24 C25 C26 -170.66(17) . . . . ? C29 C24 C25 C30 -174.5(2) . . . . ? P2 C24 C25 C30 12.7(3) . . . . ? C40 C39 C44 C43 -3.2(3) . . . . ? P3 C39 C44 C43 169.32(17) . . . . ? C40 C39 C44 C51 179.6(2) . . . . ? P3 C39 C44 C51 -7.8(3) . . . . ? C13 C14 C21 C22 70.7(2) . . . . ? C9 C14 C21 C22 -105.8(2) . . . . ? C13 C14 C21 C23 -53.5(3) . . . . ? C9 C14 C21 C23 130.0(2) . . . . ? C14 C13 C12 C11 3.3(3) . . . . ? C14 C13 C12 C18 -175.0(2) . . . . ? C11 C12 C18 C20 175.4(2) . . . . ? C13 C12 C18 C20 -6.4(3) . . . . ? C11 C12 C18 C19 -61.5(3) . . . . ? C13 C12 C18 C19 116.8(2) . . . . ? C13 C14 C9 C10 -6.6(3) . . . . ? C21 C14 C9 C10 169.9(2) . . . . ? C13 C14 C9 P1 169.15(17) . . . . ? C21 C14 C9 P1 -14.4(3) . . . . ? C1 P1 C9 C14 -28.2(2) . . . . ? P2 P1 C9 C14 73.3(2) . . . . ? C1 P1 C9 C10 147.73(16) . . . . ? P2 P1 C9 C10 -110.82(16) . . . . ? C14 C9 C10 C11 5.6(3) . . . . ? P1 C9 C10 C11 -170.67(18) . . . . ? C14 C9 C10 C15 -175.0(2) . . . . ? P1 C9 C10 C15 8.7(3) . . . . ? C25 C24 C29 C28 -2.1(3) . . . . ? P2 C24 C29 C28 171.72(17) . . . . ? C25 C24 C29 C36 -178.7(2) . . . . ? P2 C24 C29 C36 -4.9(3) . . . . ? C38 C36 C29 C28 -78.2(2) . . . . ? C37 C36 C29 C28 45.9(3) . . . . ? C38 C36 C29 C24 98.5(2) . . . . ? C37 C36 C29 C24 -137.4(2) . . . . ? C26 C25 C30 C31 52.5(3) . . . . ? C24 C25 C30 C31 -130.8(2) . . . . ? C26 C25 C30 C32 -71.4(2) . . . . ? C24 C25 C30 C32 105.3(2) . . . . ? C43 C42 C48 C49 -110.6(3) . . . . ? C41 C42 C48 C49 70.5(3) . . . . ? C43 C42 C48 C50 124.5(2) . . . . ? C41 C42 C48 C50 -54.5(3) . . . . ? C28 C27 C33 C35 -130.1(2) . . . . ? C26 C27 C33 C35 51.1(3) . . . . ? C28 C27 C33 C34 104.5(3) . . . . ? C26 C27 C33 C34 -74.3(3) . . . . ? C2 C3 C4 C5 0.5(3) . . . . ? C3 C2 C7 C6 1.5(3) . . . . ? C1 C2 C7 C6 -179.2(2) . . . . ? C26 C27 C28 C29 1.2(4) . . . . ? C33 C27 C28 C29 -177.6(2) . . . . ? C24 C29 C28 C27 0.4(3) . . . . ? C36 C29 C28 C27 177.2(2) . . . . ? C41 C40 C45 C47 -62.1(3) . . . . ? C39 C40 C45 C47 118.0(2) . . . . ? C41 C40 C45 C46 61.7(3) . . . . ? C39 C40 C45 C46 -118.2(2) . . . . ? C28 C27 C26 C25 -1.2(4) . . . . ? C33 C27 C26 C25 177.7(2) . . . . ? C24 C25 C26 C27 -0.5(3) . . . . ? C30 C25 C26 C27 176.4(2) . . . . ? C41 C42 C43 C44 3.5(3) . . . . ? C48 C42 C43 C44 -175.5(2) . . . . ? C39 C44 C43 C42 0.0(3) . . . . ? C51 C44 C43 C42 177.3(2) . . . . ? C13 C12 C11 C10 -4.4(3) . . . . ? C18 C12 C11 C10 174.0(2) . . . . ? C9 C10 C11 C12 0.0(4) . . . . ? C15 C10 C11 C12 -179.5(2) . . . . ? C8 O1 C5 C6 -169.0(2) . . . . ? C8 O1 C5 C4 11.8(3) . . . . ? C3 C4 C5 O1 -179.2(2) . . . . ? C3 C4 C5 C6 1.5(3) . . . . ? C2 C7 C6 C5 0.5(3) . . . . ? O1 C5 C6 C7 178.7(2) . . . . ? C4 C5 C6 C7 -2.0(4) . . . . ? C11 C10 C15 C17 71.7(3) . . . . ? C9 C10 C15 C17 -107.7(3) . . . . ? C11 C10 C15 C16 -54.6(3) . . . . ? C9 C10 C15 C16 126.0(3) . . . . ? C43 C44 C51 C53 -79.8(3) . . . . ? C39 C44 C51 C53 97.4(3) . . . . ? C43 C44 C51 C52 45.7(3) . . . . ? C39 C44 C51 C52 -137.1(2) . . . . ? O3B S1B C54B F3B 67(2) . . . . ? O2 S1B C54B F3B -172.5(15) . . . . ? O4B S1B C54B F3B -54.8(19) . . . . ? O3B S1B C54B F1B -171(2) . . . . ? O2 S1B C54B F1B -51(2) . . . . ? O4B S1B C54B F1B 67(2) . . . . ? O3B S1B C54B F2B -56(2) . . . . ? O2 S1B C54B F2B 64.5(15) . . . . ? O4B S1B C54B F2B -177.8(16) . . . . ? O4A S1A C54A F3A -173.7(14) . . . . ? O3A S1A C54A F3A -50.9(17) . . . . ? O2 S1A C54A F3A 65.2(12) . . . . ? O4A S1A C54A F1A 62.5(18) . . . . ? O3A S1A C54A F1A -174.7(18) . . . . ? O2 S1A C54A F1A -58.7(16) . . . . ? O4A S1A C54A F2A -55.5(14) . . . . ? O3A S1A C54A F2A 67.3(16) . . . . ? O2 S1A C54A F2A -176.7(10) . . . . ?