#------------------------------------------------------------------------------ #$Date: 2019-08-14 03:06:28 +0300 (Wed, 14 Aug 2019) $ #$Revision: 217510 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/39/7123982.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_7123982 loop_ _publ_author_name 'Ho, Luong Phong' 'Zaretzke, Marc-Kevin' 'Bannenberg, Thomas' 'Tamm, Matthias' _publ_section_title ; Heteroleptic diphosphenes and arsaphosphenes bearing neutral and anionic N-heterocyclic carbenes ; _journal_name_full 'Chemical Communications' _journal_paper_doi 10.1039/C9CC05739K _journal_year 2019 _chemical_formula_moiety '2(C72 H71 B F15 N4 P2), C4 H8 O' _chemical_formula_sum 'C74 H75 B F15 N4 O0.5 P2' _chemical_formula_weight 1386.13 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2019-07-23 deposited with the CCDC. 2019-08-13 downloaded from the CCDC. ; _cell_angle_alpha 105.855(2) _cell_angle_beta 90.306(2) _cell_angle_gamma 112.409(2) _cell_formula_units_Z 2 _cell_length_a 12.5253(2) _cell_length_b 15.4459(2) _cell_length_c 20.2657(2) _cell_measurement_reflns_used 82449 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 77.4590 _cell_measurement_theta_min 3.2590 _cell_volume 3460.21(11) _computing_cell_refinement 'CrysAlisPro 1.171.40.21a (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.40.21a (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.40.21a (Rigaku OD, 2018)' _computing_publication_material 'OLEX2 v1.2 (O. V. Dolomanov et al., J. Appl. Cryst., 2009, 42, 339-341)' _computing_structure_refinement 'SHELXL-2018/3 (G. M. Sheldrick, Acta Cryst., 2008, A64, 112-122)' _computing_structure_solution 'SHELXT-2014/5 (G. M. Sheldrick, Acta Cryst., 2015, A71, 3-8)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measurement_device_type 'XtaLAB Synergy, Single source at home/near, HyPix' _diffrn_measurement_method '\w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0416 _diffrn_reflns_av_unetI/netI 0.0164 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.989 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 144778 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.989 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 77.620 _diffrn_reflns_theta_min 2.284 _diffrn_source 'micro-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 1.319 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.399 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.21a (Rigaku Oxford Diffraction, 2018) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'red-green dichroic' _exptl_crystal_density_diffrn 1.330 _exptl_crystal_description irregular _exptl_crystal_F_000 1442 _exptl_crystal_size_max 0.298 _exptl_crystal_size_mid 0.252 _exptl_crystal_size_min 0.147 _refine_diff_density_max 0.638 _refine_diff_density_min -0.603 _refine_diff_density_rms 0.050 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 908 _refine_ls_number_reflns 14569 _refine_ls_number_restraints 66 _refine_ls_restrained_S_all 1.040 _refine_ls_R_factor_all 0.0487 _refine_ls_R_factor_gt 0.0466 _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^)+(0.0641P)^2^+2.1893P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1269 _refine_ls_wR_factor_ref 0.1285 _reflns_Friedel_coverage 0.000 _reflns_number_gt 13627 _reflns_number_total 14569 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9cc05739k3.cif _cod_data_source_block ph40ph _cod_original_cell_volume 3460.20(10) _cod_original_formula_sum 'C74 H75 B F15 N4 O0.50 P2' _cod_database_code 7123982 _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 0.695 _shelx_estimated_absorpt_t_max 0.830 _shelx_res_file ; TITL ph40ph_a.res in P-1 ph40ph.res created by SHELXL-2018/3 at 10:08:28 on 16-Nov-2018 REM Old TITL ph40ph in P-1 REM SHELXT solution in P-1: R1 0.140, Rweak 0.008, 0.040 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C75 B N4 F15 P2 CELL 1.54184 12.5253 15.4459 20.2657 105.855 90.306 112.409 ZERR 2 0.0002 0.0002 0.0002 0.002 0.002 0.002 LATT 1 SFAC C H B F N O P UNIT 148 150 2 30 8 1 4 SADI C101 C102 C102 C103 C103 C104 SADI O100 C101 O100 C104 SADI 0.04 O100 C102 O100 C103 SADI 0.04 C102 C104 C101 C103 SIMU O100 C101 C102 C103 C104 RIGU O100 C101 C102 C103 C104 L.S. 4 0 0 PLAN 20 SIZE 0.252 0.298 0.147 TEMP -173 CONF list 4 fmap 2 53 acta REM REM REM WGHT 0.064100 2.189300 FVAR 3.95891 P1 7 0.249671 0.605810 0.282593 11.00000 0.02530 0.02888 = 0.03947 0.01010 0.00751 0.01191 P2 7 0.412121 0.683171 0.252149 11.00000 0.03136 0.03758 = 0.05074 0.02174 0.01634 0.02022 F1 4 -0.028538 0.201401 0.253309 11.00000 0.02518 0.03544 = 0.03369 0.00593 0.00559 0.01053 F11 4 0.123826 0.023355 0.277359 11.00000 0.03540 0.03071 = 0.03195 0.00648 0.00767 0.01580 F15 4 0.171781 0.344834 0.407694 11.00000 0.04425 0.03037 = 0.02934 0.00629 0.01289 0.01470 F10 4 0.349444 0.167580 0.362670 11.00000 0.02920 0.05906 = 0.02943 0.01657 0.00553 0.01851 F6 4 0.351664 0.258891 0.157781 11.00000 0.03970 0.04918 = 0.03361 0.01809 0.01430 0.02488 F5 4 0.222353 0.060105 0.140386 11.00000 0.03938 0.03771 = 0.03360 -0.00091 0.00544 0.01860 F12 4 0.009764 -0.045047 0.374704 11.00000 0.04570 0.03643 = 0.05110 0.02223 0.01656 0.02107 F14 4 0.060768 0.274419 0.503496 11.00000 0.05764 0.04926 = 0.03122 0.01420 0.02186 0.03159 F7 4 0.558030 0.250010 0.141412 11.00000 0.04165 0.05614 = 0.04591 0.02094 0.02515 0.02569 F3 4 -0.163563 -0.053363 0.046125 11.00000 0.04492 0.03990 = 0.03690 0.00301 -0.01183 -0.00156 F9 4 0.549042 0.151884 0.342325 11.00000 0.03322 0.06368 = 0.04996 0.02214 0.00384 0.02533 F2 4 -0.199938 0.079952 0.153823 11.00000 0.02581 0.04938 = 0.04932 0.01041 -0.00340 0.00668 F4 4 0.050724 -0.061188 0.044286 11.00000 0.05981 0.03473 = 0.03077 -0.00445 0.00188 0.01310 F13 4 -0.025093 0.078766 0.488988 11.00000 0.06031 0.05510 = 0.04842 0.03291 0.03255 0.03533 F8 4 0.657608 0.191001 0.230843 11.00000 0.02987 0.05753 = 0.06280 0.01959 0.01692 0.02567 N1 5 0.205337 0.406829 0.265931 11.00000 0.01926 0.02658 = 0.02258 0.00407 0.00403 0.00873 N2 5 0.374878 0.500861 0.324225 11.00000 0.02066 0.02692 = 0.02398 0.00385 0.00197 0.00824 N3 5 0.485136 0.847143 0.206380 11.00000 0.03361 0.03510 = 0.03253 0.01205 0.01070 0.01701 N4 5 0.314248 0.824176 0.238412 11.00000 0.02988 0.03705 = 0.02951 0.00934 0.00543 0.01873 C2 1 0.251216 0.342778 0.281075 11.00000 0.02285 0.02924 = 0.02009 0.00488 0.00611 0.01075 C40 1 0.149718 0.187646 0.334305 11.00000 0.02185 0.03124 = 0.02616 0.00756 0.00375 0.01124 C1 1 0.282025 0.502909 0.291268 11.00000 0.02086 0.02845 = 0.02467 0.00489 0.00512 0.01015 C3 1 0.356994 0.405174 0.317368 11.00000 0.02339 0.02945 = 0.02401 0.00586 0.00356 0.01134 AFIX 43 H3 2 0.410976 0.385313 0.335452 11.00000 -1.20000 AFIX 0 C28 1 0.111016 0.146852 0.200140 11.00000 0.02865 0.02707 = 0.02478 0.00701 0.00353 0.00806 C41 1 0.107016 0.089153 0.331646 11.00000 0.02456 0.03394 = 0.02761 0.00774 0.00541 0.01479 C4 1 0.093283 0.382979 0.228547 11.00000 0.01985 0.02793 = 0.02887 0.00615 0.00150 0.00808 C42 1 0.049606 0.051089 0.381988 11.00000 0.02909 0.03417 = 0.03929 0.01701 0.00759 0.01627 C61 1 0.207453 0.790498 0.268574 11.00000 0.02600 0.03516 = 0.03429 0.00884 0.00538 0.01879 C16 1 0.471419 0.583220 0.369648 11.00000 0.02360 0.02625 = 0.02893 0.00555 -0.00265 0.00757 C29 1 -0.001869 0.142498 0.199649 11.00000 0.02950 0.02881 = 0.02654 0.00618 0.00317 0.00806 C39 1 0.393456 0.185639 0.304728 11.00000 0.02604 0.03206 = 0.02740 0.00531 0.00534 0.01039 C5 1 0.081092 0.352129 0.156258 11.00000 0.02510 0.02915 = 0.02902 0.00501 0.00182 0.00905 C45 1 0.132496 0.246889 0.395038 11.00000 0.02830 0.03191 = 0.02734 0.00903 0.00655 0.01356 C44 1 0.075357 0.212072 0.446833 11.00000 0.03472 0.04212 = 0.02685 0.01072 0.01063 0.02254 C33 1 0.121956 0.073916 0.145813 11.00000 0.03384 0.03131 = 0.02644 0.00606 0.00373 0.01088 C34 1 0.335007 0.210223 0.259575 11.00000 0.02560 0.02537 = 0.02581 0.00226 0.00458 0.00979 C62 1 0.211615 0.829061 0.339653 11.00000 0.03001 0.03492 = 0.03521 0.00738 0.00577 0.01817 C9 1 0.003273 0.394435 0.266535 11.00000 0.02343 0.03282 = 0.03378 0.00921 0.00598 0.01108 C17 1 0.451476 0.622793 0.436892 11.00000 0.03660 0.03203 = 0.02931 0.00469 -0.00032 0.01233 C46 1 0.397285 0.786656 0.233477 11.00000 0.02802 0.03532 = 0.02864 0.00877 0.00607 0.01520 C30 1 -0.093770 0.078116 0.149378 11.00000 0.02749 0.03552 = 0.03644 0.01123 -0.00047 0.00520 C36 1 0.503619 0.226839 0.194958 11.00000 0.03218 0.03516 = 0.03582 0.00886 0.01408 0.01509 C43 1 0.032688 0.113764 0.440103 11.00000 0.03393 0.04682 = 0.03444 0.02238 0.01490 0.02315 C35 1 0.397055 0.231829 0.205025 11.00000 0.03161 0.03177 = 0.02996 0.00736 0.00808 0.01491 C13 1 0.013796 0.428773 0.345087 11.00000 0.02618 0.03711 = 0.03339 0.00751 0.00978 0.01455 AFIX 13 H13 2 0.095450 0.444657 0.363499 11.00000 -1.20000 AFIX 0 C21 1 0.579855 0.614115 0.345472 11.00000 0.02407 0.03046 = 0.03965 0.01171 0.00032 0.01191 C38 1 0.499921 0.178031 0.296047 11.00000 0.02814 0.03560 = 0.03655 0.00802 0.00164 0.01448 C10 1 0.181931 0.350640 0.115511 11.00000 0.02893 0.03917 = 0.02532 0.00244 0.00243 0.01402 AFIX 13 H10 2 0.246731 0.356492 0.147754 11.00000 -1.20000 AFIX 0 C31 1 -0.075913 0.010437 0.095525 11.00000 0.03771 0.03180 = 0.02905 0.00565 -0.00563 0.00073 C32 1 0.032338 0.007468 0.094558 11.00000 0.04535 0.02844 = 0.02610 0.00313 0.00226 0.00866 C66 1 0.106288 0.723011 0.224869 11.00000 0.03236 0.03695 = 0.03769 0.00321 -0.00143 0.02184 C47 1 0.456096 0.919986 0.195235 11.00000 0.04460 0.03688 = 0.03377 0.01285 0.01092 0.01978 AFIX 43 H47 2 0.502447 0.970763 0.176989 11.00000 -1.20000 AFIX 0 C63 1 0.108512 0.794875 0.368161 11.00000 0.03571 0.04035 = 0.03967 0.00844 0.01189 0.02155 AFIX 43 H63 2 0.108006 0.817730 0.416650 11.00000 -1.20000 AFIX 0 C37 1 0.554986 0.198122 0.240600 11.00000 0.02493 0.03471 = 0.04575 0.00618 0.00993 0.01451 C54 1 0.689165 0.903551 0.249743 11.00000 0.03092 0.03820 = 0.05388 0.02323 0.01431 0.01292 C6 1 -0.027987 0.326522 0.121536 11.00000 0.02982 0.04378 = 0.03123 0.00810 -0.00217 0.01122 AFIX 43 H6 2 -0.040002 0.302885 0.072479 11.00000 -1.20000 AFIX 0 C48 1 0.349769 0.905779 0.215029 11.00000 0.04365 0.04099 = 0.03348 0.01102 0.00729 0.02471 AFIX 43 H48 2 0.307097 0.944604 0.213257 11.00000 -1.20000 AFIX 0 C49 1 0.598282 0.843085 0.197103 11.00000 0.03588 0.03913 = 0.04339 0.02064 0.01937 0.01971 C25 1 0.601556 0.562723 0.275135 11.00000 0.02414 0.03939 = 0.04326 0.01473 0.00815 0.01460 AFIX 13 H25 2 0.524652 0.522820 0.245928 11.00000 -1.20000 AFIX 0 C19 1 0.651589 0.737670 0.457196 11.00000 0.03680 0.03419 = 0.04815 0.00255 -0.01321 0.00918 AFIX 43 H19 2 0.713505 0.792884 0.486978 11.00000 -1.20000 AFIX 0 C64 1 0.006770 0.727935 0.326560 11.00000 0.02867 0.04137 = 0.05707 0.01269 0.01289 0.01863 AFIX 43 H64 2 -0.063002 0.705762 0.346842 11.00000 -1.20000 AFIX 0 C8 1 -0.102849 0.369971 0.228519 11.00000 0.02333 0.04759 = 0.04473 0.01522 0.00765 0.01533 AFIX 43 H8 2 -0.165326 0.377661 0.252308 11.00000 -1.20000 AFIX 0 C18 1 0.544590 0.703019 0.479725 11.00000 0.04595 0.03587 = 0.03338 0.00076 -0.00637 0.01279 AFIX 43 H18 2 0.533761 0.734041 0.525063 11.00000 -1.20000 AFIX 0 C20 1 0.670607 0.693529 0.391941 11.00000 0.02311 0.03601 = 0.05853 0.01332 -0.00308 0.00862 AFIX 43 H20 2 0.746214 0.717171 0.378194 11.00000 -1.20000 AFIX 0 C58 1 0.673628 0.967905 0.317255 11.00000 0.03094 0.04297 = 0.04824 0.01617 0.00613 0.01067 AFIX 13 H58 2 0.593220 0.966111 0.312686 11.00000 -1.20000 AFIX 0 C15 1 -0.068435 0.349043 0.374137 11.00000 0.03466 0.04671 = 0.03565 0.01077 0.01522 0.01424 AFIX 137 H15A 2 -0.149310 0.335714 0.359556 11.00000 -1.50000 H15B 2 -0.053761 0.371635 0.424731 11.00000 -1.50000 H15C 2 -0.054695 0.288915 0.356658 11.00000 -1.50000 AFIX 0 C65 1 0.004997 0.692953 0.256290 11.00000 0.02641 0.03841 = 0.05756 0.00483 -0.00201 0.01650 AFIX 43 H65 2 -0.066183 0.647659 0.228688 11.00000 -1.20000 AFIX 0 C50 1 0.610393 0.781561 0.135377 11.00000 0.04770 0.04243 = 0.04539 0.02164 0.02417 0.02237 C12 1 0.150343 0.255928 0.056293 11.00000 0.05133 0.03763 = 0.02587 0.00571 0.00629 0.01898 AFIX 137 H12A 2 0.113241 0.199486 0.073661 11.00000 -1.50000 H12B 2 0.221078 0.253448 0.037018 11.00000 -1.50000 H12C 2 0.096434 0.254060 0.020190 11.00000 -1.50000 AFIX 0 C7 1 -0.119259 0.334986 0.157433 11.00000 0.02444 0.05466 = 0.04405 0.01481 -0.00130 0.01344 AFIX 43 H7 2 -0.193204 0.316619 0.132940 11.00000 -1.20000 AFIX 0 C67 1 0.321701 0.906757 0.385389 11.00000 0.03408 0.04618 = 0.03266 0.00261 0.00401 0.01568 AFIX 13 H67 2 0.382373 0.928420 0.354740 11.00000 -1.20000 AFIX 0 C14 1 -0.010383 0.521807 0.371488 11.00000 0.03803 0.04521 = 0.04844 0.00819 0.01414 0.02331 AFIX 137 H14A 2 0.042774 0.573426 0.353845 11.00000 -1.50000 H14B 2 0.001585 0.543976 0.422135 11.00000 -1.50000 H14C 2 -0.090944 0.507413 0.355338 11.00000 -1.50000 AFIX 0 C22 1 0.338292 0.578583 0.465550 11.00000 0.04533 0.04306 = 0.02864 0.00364 0.00837 0.01252 AFIX 13 H22 2 0.284657 0.521092 0.427497 11.00000 -1.20000 AFIX 0 C60 1 0.759607 1.074840 0.332944 11.00000 0.03221 0.04194 = 0.06285 0.01775 0.00132 0.01248 AFIX 137 H60A 2 0.839194 1.078999 0.339457 11.00000 -1.50000 H60B 2 0.743398 1.114625 0.375157 11.00000 -1.50000 H60C 2 0.751285 1.099372 0.294265 11.00000 -1.50000 AFIX 0 C51 1 0.723011 0.783785 0.127876 11.00000 0.05900 0.05179 = 0.05988 0.03020 0.03903 0.03424 AFIX 43 H51 2 0.736261 0.744151 0.086551 11.00000 -1.20000 AFIX 0 C26 1 0.677137 0.634630 0.238573 11.00000 0.03451 0.05430 = 0.05823 0.02668 0.01911 0.02349 AFIX 137 H26A 2 0.641587 0.680251 0.235616 11.00000 -1.50000 H26B 2 0.683426 0.598261 0.191907 11.00000 -1.50000 H26C 2 0.754878 0.671503 0.264743 11.00000 -1.50000 AFIX 0 C27 1 0.658379 0.492611 0.281599 11.00000 0.03653 0.04265 = 0.05784 0.01605 0.01264 0.02214 AFIX 137 H27A 2 0.733995 0.530214 0.310159 11.00000 -1.50000 H27B 2 0.669440 0.458095 0.235543 11.00000 -1.50000 H27C 2 0.607946 0.444803 0.303220 11.00000 -1.50000 AFIX 0 C70 1 0.105661 0.684493 0.147477 11.00000 0.04455 0.05753 = 0.03662 -0.00038 -0.00594 0.03079 AFIX 13 H70 2 0.186736 0.691970 0.138693 11.00000 -1.20000 AFIX 0 B1 3 0.208745 0.222423 0.267643 11.00000 0.02419 0.02779 = 0.02326 0.00506 0.00507 0.01006 C52 1 0.814098 0.842202 0.179204 11.00000 0.03762 0.05477 = 0.07885 0.03643 0.02956 0.02306 AFIX 43 H52 2 0.889058 0.841794 0.173039 11.00000 -1.20000 AFIX 0 C55 1 0.509739 0.718932 0.079529 11.00000 0.06271 0.05070 = 0.04052 0.01439 0.02330 0.02871 AFIX 13 H55 2 0.436237 0.709622 0.101250 11.00000 -1.20000 AFIX 0 C11 1 0.226057 0.438753 0.086804 11.00000 0.05092 0.03933 = 0.04772 0.00639 0.02410 0.01221 AFIX 137 H11A 2 0.164042 0.434152 0.054643 11.00000 -1.50000 H11B 2 0.293427 0.438680 0.062456 11.00000 -1.50000 H11C 2 0.248857 0.499651 0.124995 11.00000 -1.50000 AFIX 0 C53 1 0.798322 0.901108 0.239227 11.00000 0.03167 0.04801 = 0.07023 0.02809 0.01634 0.01495 AFIX 43 H53 2 0.862439 0.940779 0.274123 11.00000 -1.20000 AFIX 0 C69 1 0.299993 0.995682 0.426077 11.00000 0.04998 0.03299 = 0.06162 0.00648 -0.00575 0.01609 AFIX 137 H69A 2 0.265414 1.018417 0.394359 11.00000 -1.50000 H69B 2 0.373897 1.048242 0.450211 11.00000 -1.50000 H69C 2 0.246667 0.977740 0.459902 11.00000 -1.50000 AFIX 0 C59 1 0.684048 0.926829 0.376539 11.00000 0.07377 0.05467 = 0.05555 0.02453 0.00960 0.01973 AFIX 137 H59A 2 0.628125 0.858469 0.365304 11.00000 -1.50000 H59B 2 0.667565 0.965764 0.419066 11.00000 -1.50000 H59C 2 0.763128 0.929945 0.383221 11.00000 -1.50000 AFIX 0 C24 1 0.356998 0.539958 0.524376 11.00000 0.06761 0.07274 = 0.04280 0.02484 0.00842 0.01398 AFIX 137 H24A 2 0.392996 0.492889 0.508239 11.00000 -1.50000 H24B 2 0.281887 0.507423 0.539613 11.00000 -1.50000 H24C 2 0.408137 0.594734 0.563091 11.00000 -1.50000 AFIX 0 C23 1 0.278045 0.650154 0.487933 11.00000 0.05601 0.06482 = 0.05703 0.00590 0.02165 0.02654 AFIX 137 H23A 2 0.328867 0.708096 0.524841 11.00000 -1.50000 H23B 2 0.204637 0.617769 0.504892 11.00000 -1.50000 H23C 2 0.262223 0.670226 0.448337 11.00000 -1.50000 AFIX 0 C68 1 0.368866 0.866860 0.434581 11.00000 0.07208 0.04561 = 0.07672 -0.01077 -0.03352 0.03290 AFIX 137 H68A 2 0.311175 0.845919 0.465624 11.00000 -1.50000 H68B 2 0.440978 0.918305 0.461869 11.00000 -1.50000 H68C 2 0.384729 0.810740 0.407835 11.00000 -1.50000 AFIX 0 C71 1 0.026297 0.575783 0.118453 11.00000 0.06319 0.06223 = 0.05457 -0.01387 -0.01137 0.03057 AFIX 137 H71A 2 0.045799 0.538708 0.145347 11.00000 -1.50000 H71B 2 0.037185 0.551621 0.070047 11.00000 -1.50000 H71C 2 -0.054991 0.567300 0.121353 11.00000 -1.50000 AFIX 0 C57 1 0.508969 0.616986 0.044518 11.00000 0.07585 0.04594 = 0.07805 0.01126 0.02914 0.02432 AFIX 137 H57A 2 0.576931 0.623862 0.019394 11.00000 -1.50000 H57B 2 0.437761 0.577092 0.012096 11.00000 -1.50000 H57C 2 0.511722 0.584983 0.079735 11.00000 -1.50000 AFIX 0 C72 1 0.071257 0.745085 0.110101 11.00000 0.12006 0.08589 = 0.04156 0.00681 -0.01384 0.06235 AFIX 137 H72A 2 -0.009503 0.736314 0.115828 11.00000 -1.50000 H72B 2 0.078604 0.723323 0.060809 11.00000 -1.50000 H72C 2 0.122565 0.814547 0.129651 11.00000 -1.50000 AFIX 0 C56 1 0.510746 0.771427 0.025823 11.00000 0.12680 0.06299 = 0.05315 0.02038 -0.00405 0.02915 AFIX 137 H56A 2 0.515988 0.837779 0.048970 11.00000 -1.50000 H56B 2 0.438955 0.734951 -0.006477 11.00000 -1.50000 H56C 2 0.577942 0.775349 0.000396 11.00000 -1.50000 AFIX 0 PART -1 O100 6 0.515496 1.026816 0.078934 10.50000 0.06704 0.06291 = 0.04744 0.02357 0.01222 0.02861 C101 1 0.407132 0.997778 0.035181 10.50000 0.06694 0.07306 = 0.06543 0.02072 0.00467 0.02617 AFIX 23 H10A 2 0.385217 1.054453 0.041565 10.50000 -1.20000 H10B 2 0.343478 0.945091 0.047572 10.50000 -1.20000 AFIX 0 C102 1 0.426719 0.961940 -0.038301 10.50000 0.07019 0.07647 = 0.05584 0.01685 0.01861 0.03802 AFIX 23 H10C 2 0.397681 0.991980 -0.067705 10.50000 -1.20000 H10D 2 0.385549 0.889735 -0.056327 10.50000 -1.20000 AFIX 0 C103 1 0.559409 0.992521 -0.038124 10.50000 0.06692 0.05724 = 0.03932 0.01712 -0.00312 0.02385 AFIX 23 H10E 2 0.580455 0.935025 -0.048035 10.50000 -1.20000 H10F 2 0.589633 1.028967 -0.071915 10.50000 -1.20000 AFIX 0 C104 1 0.603178 1.057678 0.035275 10.50000 0.05718 0.07782 = 0.04758 0.02470 0.01603 0.03499 AFIX 23 H10G 2 0.675322 1.053383 0.051252 10.50000 -1.20000 H10H 2 0.621254 1.126724 0.037509 10.50000 -1.20000 AFIX 0 HKLF 4 REM ph40ph_a.res in P-1 REM wR2 = 0.1285, GooF = S = 1.042, Restrained GooF = 1.040 for all data REM R1 = 0.0466 for 13627 Fo > 4sig(Fo) and 0.0487 for all 14569 data REM 908 parameters refined using 66 restraints END WGHT 0.0641 2.1893 REM Highest difference peak 0.638, deepest hole -0.603, 1-sigma level 0.050 Q1 1 0.4152 0.7220 0.3048 11.00000 0.05 0.64 Q2 1 0.3348 0.6096 0.2308 11.00000 0.05 0.59 Q3 1 0.2741 0.6594 0.3636 11.00000 0.05 0.52 Q4 1 0.4348 0.6343 0.2007 11.00000 0.05 0.44 Q5 1 0.4120 0.8941 0.4010 11.00000 0.05 0.42 Q6 1 0.4348 0.6451 0.0758 11.00000 0.05 0.39 Q7 1 0.2844 0.5790 0.3017 11.00000 0.05 0.38 Q8 1 0.2796 0.8922 0.0162 11.00000 0.05 0.36 Q9 1 0.7743 0.8778 0.1962 11.00000 0.05 0.34 Q10 1 0.5416 1.0809 -0.0702 11.00000 0.05 0.34 Q11 1 0.4968 0.7430 0.3142 11.00000 0.05 0.32 Q12 1 0.3409 0.6609 0.5261 11.00000 0.05 0.32 Q13 1 0.2344 0.2961 0.2806 11.00000 0.05 0.31 Q14 1 0.5814 0.5814 0.3071 11.00000 0.05 0.30 Q15 1 0.3633 0.4607 0.3373 11.00000 0.05 0.29 Q16 1 0.1406 0.1434 0.3420 11.00000 0.05 0.29 Q17 1 0.2759 0.8617 0.4620 11.00000 0.05 0.29 Q18 1 0.1031 0.7003 0.1837 11.00000 0.05 0.29 Q19 1 0.2540 0.4216 0.1151 11.00000 0.05 0.28 Q20 1 0.3364 0.9795 0.3817 11.00000 0.05 0.28 ; _shelx_res_checksum 31781 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 0.24967(4) 0.60581(3) 0.28259(2) 0.03086(10) Uani 1 1 d . . . . . P2 P 0.41212(4) 0.68317(3) 0.25215(3) 0.03595(11) Uani 1 1 d . . . . . F1 F -0.02854(8) 0.20140(7) 0.25331(5) 0.0329(2) Uani 1 1 d . . . . . F11 F 0.12383(8) 0.02336(7) 0.27736(5) 0.0325(2) Uani 1 1 d . . . . . F15 F 0.17178(9) 0.34483(7) 0.40769(5) 0.0352(2) Uani 1 1 d . . . . . F10 F 0.34944(9) 0.16758(9) 0.36267(5) 0.0382(2) Uani 1 1 d . . . . . F6 F 0.35166(9) 0.25889(8) 0.15778(5) 0.0373(2) Uani 1 1 d . . . . . F5 F 0.22235(9) 0.06010(8) 0.14039(5) 0.0384(2) Uani 1 1 d . . . . . F12 F 0.00976(10) -0.04505(8) 0.37470(6) 0.0409(2) Uani 1 1 d . . . . . F14 F 0.06077(10) 0.27442(8) 0.50350(5) 0.0423(3) Uani 1 1 d . . . . . F7 F 0.55803(10) 0.25001(9) 0.14141(6) 0.0446(3) Uani 1 1 d . . . . . F3 F -0.16356(10) -0.05336(8) 0.04613(6) 0.0482(3) Uani 1 1 d . . . . . F9 F 0.54904(9) 0.15188(9) 0.34232(6) 0.0459(3) Uani 1 1 d . . . . . F2 F -0.19994(9) 0.07995(9) 0.15382(6) 0.0451(3) Uani 1 1 d . . . . . F4 F 0.05072(11) -0.06119(8) 0.04429(6) 0.0466(3) Uani 1 1 d . . . . . F13 F -0.02509(11) 0.07877(9) 0.48899(6) 0.0468(3) Uani 1 1 d . . . . . F8 F 0.65761(9) 0.19100(9) 0.23084(7) 0.0471(3) Uani 1 1 d . . . . . N1 N 0.20534(11) 0.40683(9) 0.26593(6) 0.0236(3) Uani 1 1 d . . . . . N2 N 0.37488(11) 0.50086(10) 0.32423(7) 0.0250(3) Uani 1 1 d . . . . . N3 N 0.48514(13) 0.84714(11) 0.20638(7) 0.0322(3) Uani 1 1 d . . . . . N4 N 0.31425(12) 0.82418(11) 0.23841(7) 0.0306(3) Uani 1 1 d . . . . . C2 C 0.25122(13) 0.34278(11) 0.28108(8) 0.0245(3) Uani 1 1 d . . . . . C40 C 0.14972(13) 0.18765(12) 0.33431(8) 0.0264(3) Uani 1 1 d . . . . . C1 C 0.28203(13) 0.50291(11) 0.29127(8) 0.0252(3) Uani 1 1 d . . . . . C3 C 0.35699(13) 0.40517(11) 0.31737(8) 0.0258(3) Uani 1 1 d . . . . . H3 H 0.410976 0.385313 0.335452 0.031 Uiso 1 1 calc R U . . . C28 C 0.11102(14) 0.14685(12) 0.20014(8) 0.0279(3) Uani 1 1 d . . . . . C41 C 0.10702(14) 0.08915(12) 0.33165(8) 0.0280(3) Uani 1 1 d . . . . . C4 C 0.09328(13) 0.38298(11) 0.22855(8) 0.0265(3) Uani 1 1 d . . . . . C42 C 0.04961(14) 0.05109(13) 0.38199(9) 0.0317(3) Uani 1 1 d . . . . . C61 C 0.20745(14) 0.79050(13) 0.26857(9) 0.0301(3) Uani 1 1 d . . . . . C16 C 0.47142(13) 0.58322(11) 0.36965(8) 0.0276(3) Uani 1 1 d . . . . . C29 C -0.00187(14) 0.14250(12) 0.19965(8) 0.0298(3) Uani 1 1 d . . . . . C39 C 0.39346(14) 0.18564(12) 0.30473(8) 0.0296(3) Uani 1 1 d . . . . . C5 C 0.08109(14) 0.35213(12) 0.15626(8) 0.0291(3) Uani 1 1 d . . . . . C45 C 0.13250(14) 0.24689(12) 0.39504(8) 0.0286(3) Uani 1 1 d . . . . . C44 C 0.07536(15) 0.21207(13) 0.44683(9) 0.0322(3) Uani 1 1 d . . . . . C33 C 0.12196(15) 0.07392(12) 0.14581(9) 0.0317(3) Uani 1 1 d . . . . . C34 C 0.33501(14) 0.21022(11) 0.25957(8) 0.0269(3) Uani 1 1 d . . . . . C62 C 0.21161(15) 0.82906(13) 0.33965(9) 0.0324(3) Uani 1 1 d . . . . . C9 C 0.00327(14) 0.39444(12) 0.26654(9) 0.0302(3) Uani 1 1 d . . . . . C17 C 0.45148(16) 0.62279(13) 0.43689(9) 0.0340(4) Uani 1 1 d . . . . . C46 C 0.39728(14) 0.78666(13) 0.23348(8) 0.0300(3) Uani 1 1 d . . . . . C30 C -0.09377(15) 0.07812(13) 0.14938(9) 0.0354(4) Uani 1 1 d . . . . . C36 C 0.50362(15) 0.22684(13) 0.19496(9) 0.0342(4) Uani 1 1 d . . . . . C43 C 0.03269(15) 0.11376(14) 0.44010(9) 0.0339(4) Uani 1 1 d . . . . . C35 C 0.39705(15) 0.23183(12) 0.20503(9) 0.0308(3) Uani 1 1 d . . . . . C13 C 0.01380(14) 0.42877(13) 0.34509(9) 0.0322(3) Uani 1 1 d . . . . . H13 H 0.095450 0.444657 0.363499 0.039 Uiso 1 1 calc R U . . . C21 C 0.57985(14) 0.61412(12) 0.34547(9) 0.0308(3) Uani 1 1 d . . . . . C38 C 0.49992(15) 0.17803(13) 0.29605(9) 0.0335(4) Uani 1 1 d . . . . . C10 C 0.18193(15) 0.35064(13) 0.11551(9) 0.0325(3) Uani 1 1 d . . . . . H10 H 0.246731 0.356492 0.147754 0.039 Uiso 1 1 calc R U . . . C31 C -0.07591(16) 0.01044(13) 0.09552(9) 0.0377(4) Uani 1 1 d . . . . . C32 C 0.03234(17) 0.00747(13) 0.09456(9) 0.0363(4) Uani 1 1 d . . . . . C66 C 0.10629(15) 0.72301(13) 0.22487(9) 0.0349(4) Uani 1 1 d . . . . . C47 C 0.45610(17) 0.91999(14) 0.19524(9) 0.0368(4) Uani 1 1 d . . . . . H47 H 0.502447 0.970763 0.176989 0.044 Uiso 1 1 calc R U . . . C63 C 0.10851(16) 0.79488(14) 0.36816(10) 0.0373(4) Uani 1 1 d . . . . . H63 H 0.108006 0.817730 0.416650 0.045 Uiso 1 1 calc R U . . . C37 C 0.55499(15) 0.19812(13) 0.24060(10) 0.0355(4) Uani 1 1 d . . . . . C54 C 0.68916(16) 0.90355(14) 0.24974(11) 0.0392(4) Uani 1 1 d . . . . . C6 C -0.02799(15) 0.32652(14) 0.12154(9) 0.0367(4) Uani 1 1 d . . . . . H6 H -0.040002 0.302885 0.072479 0.044 Uiso 1 1 calc R U . . . C48 C 0.34977(17) 0.90578(14) 0.21503(9) 0.0369(4) Uani 1 1 d . . . . . H48 H 0.307097 0.944604 0.213257 0.044 Uiso 1 1 calc R U . . . C49 C 0.59828(16) 0.84308(14) 0.19710(10) 0.0361(4) Uani 1 1 d . . . . . C25 C 0.60156(15) 0.56272(13) 0.27514(10) 0.0344(4) Uani 1 1 d . . . . . H25 H 0.524652 0.522820 0.245928 0.041 Uiso 1 1 calc R U . . . C19 C 0.65159(17) 0.73767(14) 0.45720(11) 0.0434(4) Uani 1 1 d . . . . . H19 H 0.713505 0.792884 0.486978 0.052 Uiso 1 1 calc R U . . . C64 C 0.00677(16) 0.72793(14) 0.32656(11) 0.0413(4) Uani 1 1 d . . . . . H64 H -0.063002 0.705762 0.346842 0.050 Uiso 1 1 calc R U . . . C8 C -0.10285(15) 0.36997(15) 0.22852(10) 0.0378(4) Uani 1 1 d . . . . . H8 H -0.165326 0.377661 0.252308 0.045 Uiso 1 1 calc R U . . . C18 C 0.54459(18) 0.70302(14) 0.47973(10) 0.0416(4) Uani 1 1 d . . . . . H18 H 0.533761 0.734041 0.525063 0.050 Uiso 1 1 calc R U . . . C20 C 0.67061(15) 0.69353(14) 0.39194(11) 0.0404(4) Uani 1 1 d . . . . . H20 H 0.746214 0.717171 0.378194 0.048 Uiso 1 1 calc R U . . . C58 C 0.67363(16) 0.96790(15) 0.31725(11) 0.0414(4) Uani 1 1 d . . . . . H58 H 0.593220 0.966111 0.312686 0.050 Uiso 1 1 calc R U . . . C15 C -0.06843(16) 0.34904(15) 0.37414(10) 0.0399(4) Uani 1 1 d . . . . . H15A H -0.149310 0.335714 0.359556 0.060 Uiso 1 1 calc R U . . . H15B H -0.053761 0.371635 0.424731 0.060 Uiso 1 1 calc R U . . . H15C H -0.054695 0.288915 0.356658 0.060 Uiso 1 1 calc R U . . . C65 C 0.00500(16) 0.69295(14) 0.25629(11) 0.0417(4) Uani 1 1 d . . . . . H65 H -0.066183 0.647659 0.228688 0.050 Uiso 1 1 calc R U . . . C50 C 0.61039(18) 0.78156(15) 0.13538(11) 0.0419(4) Uani 1 1 d . . . . . C12 C 0.15034(18) 0.25593(14) 0.05629(9) 0.0387(4) Uani 1 1 d . . . . . H12A H 0.113241 0.199486 0.073661 0.058 Uiso 1 1 calc R U . . . H12B H 0.221078 0.253448 0.037018 0.058 Uiso 1 1 calc R U . . . H12C H 0.096434 0.254060 0.020190 0.058 Uiso 1 1 calc R U . . . C7 C -0.11926(16) 0.33499(16) 0.15743(10) 0.0418(4) Uani 1 1 d . . . . . H7 H -0.193204 0.316619 0.132940 0.050 Uiso 1 1 calc R U . . . C67 C 0.32170(16) 0.90676(15) 0.38539(10) 0.0397(4) Uani 1 1 d . . . . . H67 H 0.382373 0.928420 0.354740 0.048 Uiso 1 1 calc R U . . . C14 C -0.01038(17) 0.52181(15) 0.37149(11) 0.0430(4) Uani 1 1 d . . . . . H14A H 0.042774 0.573426 0.353845 0.064 Uiso 1 1 calc R U . . . H14B H 0.001585 0.543976 0.422135 0.064 Uiso 1 1 calc R U . . . H14C H -0.090944 0.507413 0.355338 0.064 Uiso 1 1 calc R U . . . C22 C 0.33829(18) 0.57858(15) 0.46555(10) 0.0421(4) Uani 1 1 d . . . . . H22 H 0.284657 0.521092 0.427497 0.051 Uiso 1 1 calc R U . . . C60 C 0.75961(17) 1.07484(15) 0.33294(12) 0.0459(5) Uani 1 1 d . . . . . H60A H 0.839194 1.078999 0.339457 0.069 Uiso 1 1 calc R U . . . H60B H 0.743398 1.114625 0.375157 0.069 Uiso 1 1 calc R U . . . H60C H 0.751285 1.099372 0.294265 0.069 Uiso 1 1 calc R U . . . C51 C 0.7230(2) 0.78378(17) 0.12788(12) 0.0500(5) Uani 1 1 d . . . . . H51 H 0.736261 0.744151 0.086551 0.060 Uiso 1 1 calc R U . . . C26 C 0.67714(17) 0.63463(16) 0.23857(12) 0.0450(5) Uani 1 1 d . . . . . H26A H 0.641587 0.680251 0.235616 0.067 Uiso 1 1 calc R U . . . H26B H 0.683426 0.598261 0.191907 0.067 Uiso 1 1 calc R U . . . H26C H 0.754878 0.671503 0.264743 0.067 Uiso 1 1 calc R U . . . C27 C 0.65838(17) 0.49261(15) 0.28160(12) 0.0434(4) Uani 1 1 d . . . . . H27A H 0.733995 0.530214 0.310159 0.065 Uiso 1 1 calc R U . . . H27B H 0.669440 0.458095 0.235543 0.065 Uiso 1 1 calc R U . . . H27C H 0.607946 0.444803 0.303220 0.065 Uiso 1 1 calc R U . . . C70 C 0.10566(19) 0.68449(17) 0.14748(10) 0.0461(5) Uani 1 1 d . . . . . H70 H 0.186736 0.691970 0.138693 0.055 Uiso 1 1 calc R U . . . B1 B 0.20875(15) 0.22242(13) 0.26764(9) 0.0257(3) Uani 1 1 d . . . . . C52 C 0.81410(19) 0.84220(17) 0.17920(14) 0.0519(5) Uani 1 1 d . . . . . H52 H 0.889058 0.841794 0.173039 0.062 Uiso 1 1 calc R U . . . C55 C 0.5097(2) 0.71893(16) 0.07953(11) 0.0491(5) Uani 1 1 d . . . . . H55 H 0.436237 0.709622 0.101250 0.059 Uiso 1 1 calc R U . . . C11 C 0.2261(2) 0.43875(15) 0.08680(12) 0.0491(5) Uani 1 1 d . . . . . H11A H 0.164042 0.434152 0.054643 0.074 Uiso 1 1 calc R U . . . H11B H 0.293427 0.438680 0.062456 0.074 Uiso 1 1 calc R U . . . H11C H 0.248857 0.499651 0.124995 0.074 Uiso 1 1 calc R U . . . C53 C 0.79832(17) 0.90111(16) 0.23923(13) 0.0479(5) Uani 1 1 d . . . . . H53 H 0.862439 0.940779 0.274123 0.058 Uiso 1 1 calc R U . . . C69 C 0.3000(2) 0.99568(15) 0.42608(13) 0.0500(5) Uani 1 1 d . . . . . H69A H 0.265414 1.018417 0.394359 0.075 Uiso 1 1 calc R U . . . H69B H 0.373897 1.048242 0.450211 0.075 Uiso 1 1 calc R U . . . H69C H 0.246667 0.977740 0.459902 0.075 Uiso 1 1 calc R U . . . C59 C 0.6840(3) 0.92683(19) 0.37654(13) 0.0614(6) Uani 1 1 d . . . . . H59A H 0.628125 0.858469 0.365304 0.092 Uiso 1 1 calc R U . . . H59B H 0.667565 0.965764 0.419066 0.092 Uiso 1 1 calc R U . . . H59C H 0.763128 0.929945 0.383221 0.092 Uiso 1 1 calc R U . . . C24 C 0.3570(2) 0.5400(2) 0.52438(13) 0.0638(7) Uani 1 1 d . . . . . H24A H 0.392996 0.492889 0.508239 0.096 Uiso 1 1 calc R U . . . H24B H 0.281887 0.507423 0.539613 0.096 Uiso 1 1 calc R U . . . H24C H 0.408137 0.594734 0.563091 0.096 Uiso 1 1 calc R U . . . C23 C 0.2780(2) 0.6502(2) 0.48793(14) 0.0611(6) Uani 1 1 d . . . . . H23A H 0.328867 0.708096 0.524841 0.092 Uiso 1 1 calc R U . . . H23B H 0.204637 0.617769 0.504892 0.092 Uiso 1 1 calc R U . . . H23C H 0.262223 0.670226 0.448337 0.092 Uiso 1 1 calc R U . . . C68 C 0.3689(2) 0.86686(18) 0.43458(15) 0.0683(8) Uani 1 1 d . . . . . H68A H 0.311175 0.845919 0.465624 0.102 Uiso 1 1 calc R U . . . H68B H 0.440978 0.918305 0.461869 0.102 Uiso 1 1 calc R U . . . H68C H 0.384729 0.810740 0.407835 0.102 Uiso 1 1 calc R U . . . C71 C 0.0263(2) 0.57578(19) 0.11845(14) 0.0651(7) Uani 1 1 d . . . . . H71A H 0.045799 0.538708 0.145347 0.098 Uiso 1 1 calc R U . . . H71B H 0.037185 0.551621 0.070047 0.098 Uiso 1 1 calc R U . . . H71C H -0.054991 0.567300 0.121353 0.098 Uiso 1 1 calc R U . . . C57 C 0.5090(3) 0.61699(18) 0.04452(16) 0.0681(7) Uani 1 1 d . . . . . H57A H 0.576931 0.623862 0.019394 0.102 Uiso 1 1 calc R U . . . H57B H 0.437761 0.577092 0.012096 0.102 Uiso 1 1 calc R U . . . H57C H 0.511722 0.584983 0.079735 0.102 Uiso 1 1 calc R U . . . C72 C 0.0713(3) 0.7451(2) 0.11010(13) 0.0785(9) Uani 1 1 d . . . . . H72A H -0.009503 0.736314 0.115828 0.118 Uiso 1 1 calc R U . . . H72B H 0.078604 0.723323 0.060809 0.118 Uiso 1 1 calc R U . . . H72C H 0.122565 0.814547 0.129651 0.118 Uiso 1 1 calc R U . . . C56 C 0.5107(3) 0.7714(2) 0.02582(15) 0.0831(10) Uani 1 1 d . . . . . H56A H 0.515988 0.837779 0.048970 0.125 Uiso 1 1 calc R U . . . H56B H 0.438955 0.734951 -0.006477 0.125 Uiso 1 1 calc R U . . . H56C H 0.577942 0.775349 0.000396 0.125 Uiso 1 1 calc R U . . . O100 O 0.5155(3) 1.0268(3) 0.07893(18) 0.0567(8) Uani 0.5 1 d D U P A -1 C101 C 0.4071(9) 0.9978(15) 0.0352(7) 0.069(3) Uani 0.5 1 d D U P A -1 H10A H 0.385217 1.054453 0.041565 0.083 Uiso 0.5 1 calc R U P A -1 H10B H 0.343478 0.945091 0.047572 0.083 Uiso 0.5 1 calc R U P A -1 C102 C 0.4267(9) 0.9619(12) -0.0383(7) 0.065(3) Uani 0.5 1 d D U P A -1 H10C H 0.397681 0.991980 -0.067705 0.078 Uiso 0.5 1 calc R U P A -1 H10D H 0.385549 0.889735 -0.056327 0.078 Uiso 0.5 1 calc R U P A -1 C103 C 0.5594(8) 0.9925(12) -0.0381(6) 0.054(2) Uani 0.5 1 d D U P A -1 H10E H 0.580455 0.935025 -0.048035 0.065 Uiso 0.5 1 calc R U P A -1 H10F H 0.589633 1.028967 -0.071915 0.065 Uiso 0.5 1 calc R U P A -1 C104 C 0.6032(9) 1.0577(12) 0.0353(6) 0.057(2) Uani 0.5 1 d D U P A -1 H10G H 0.675322 1.053383 0.051252 0.068 Uiso 0.5 1 calc R U P A -1 H10H H 0.621254 1.126724 0.037509 0.068 Uiso 0.5 1 calc R U P A -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 0.0253(2) 0.0289(2) 0.0395(2) 0.01010(17) 0.00751(16) 0.01191(16) P2 0.0314(2) 0.0376(2) 0.0507(3) 0.0217(2) 0.01634(19) 0.02022(19) F1 0.0252(4) 0.0354(5) 0.0337(5) 0.0059(4) 0.0056(4) 0.0105(4) F11 0.0354(5) 0.0307(5) 0.0320(5) 0.0065(4) 0.0077(4) 0.0158(4) F15 0.0442(6) 0.0304(5) 0.0293(5) 0.0063(4) 0.0129(4) 0.0147(4) F10 0.0292(5) 0.0591(7) 0.0294(5) 0.0166(5) 0.0055(4) 0.0185(5) F6 0.0397(5) 0.0492(6) 0.0336(5) 0.0181(5) 0.0143(4) 0.0249(5) F5 0.0394(5) 0.0377(5) 0.0336(5) -0.0009(4) 0.0054(4) 0.0186(4) F12 0.0457(6) 0.0364(5) 0.0511(6) 0.0222(5) 0.0166(5) 0.0211(5) F14 0.0576(7) 0.0493(6) 0.0312(5) 0.0142(5) 0.0219(5) 0.0316(5) F7 0.0416(6) 0.0561(7) 0.0459(6) 0.0209(5) 0.0252(5) 0.0257(5) F3 0.0449(6) 0.0399(6) 0.0369(6) 0.0030(5) -0.0118(5) -0.0016(5) F9 0.0332(5) 0.0637(7) 0.0500(7) 0.0221(6) 0.0038(5) 0.0253(5) F2 0.0258(5) 0.0494(6) 0.0493(6) 0.0104(5) -0.0034(4) 0.0067(5) F4 0.0598(7) 0.0347(6) 0.0308(5) -0.0044(4) 0.0019(5) 0.0131(5) F13 0.0603(7) 0.0551(7) 0.0484(6) 0.0329(6) 0.0326(6) 0.0353(6) F8 0.0299(5) 0.0575(7) 0.0628(7) 0.0196(6) 0.0169(5) 0.0257(5) N1 0.0193(6) 0.0266(6) 0.0226(6) 0.0041(5) 0.0040(5) 0.0087(5) N2 0.0207(6) 0.0269(6) 0.0240(6) 0.0038(5) 0.0020(5) 0.0082(5) N3 0.0336(7) 0.0351(7) 0.0325(7) 0.0121(6) 0.0107(6) 0.0170(6) N4 0.0299(7) 0.0370(7) 0.0295(7) 0.0093(6) 0.0054(5) 0.0187(6) C2 0.0228(7) 0.0292(7) 0.0201(7) 0.0049(6) 0.0061(5) 0.0107(6) C40 0.0218(7) 0.0312(8) 0.0262(7) 0.0076(6) 0.0038(6) 0.0112(6) C1 0.0209(7) 0.0284(7) 0.0247(7) 0.0049(6) 0.0051(5) 0.0101(6) C3 0.0234(7) 0.0294(8) 0.0240(7) 0.0059(6) 0.0036(6) 0.0113(6) C28 0.0287(8) 0.0271(7) 0.0248(7) 0.0070(6) 0.0035(6) 0.0081(6) C41 0.0246(7) 0.0339(8) 0.0276(8) 0.0077(6) 0.0054(6) 0.0148(6) C4 0.0198(7) 0.0279(7) 0.0289(8) 0.0062(6) 0.0015(6) 0.0081(6) C42 0.0291(8) 0.0342(8) 0.0393(9) 0.0170(7) 0.0076(7) 0.0163(7) C61 0.0260(8) 0.0352(8) 0.0343(8) 0.0088(7) 0.0054(6) 0.0188(7) C16 0.0236(7) 0.0262(7) 0.0289(8) 0.0056(6) -0.0026(6) 0.0076(6) C29 0.0295(8) 0.0288(8) 0.0265(8) 0.0062(6) 0.0032(6) 0.0081(6) C39 0.0260(8) 0.0321(8) 0.0274(8) 0.0053(6) 0.0053(6) 0.0104(6) C5 0.0251(7) 0.0291(8) 0.0290(8) 0.0050(6) 0.0018(6) 0.0090(6) C45 0.0283(8) 0.0319(8) 0.0273(8) 0.0090(6) 0.0065(6) 0.0136(6) C44 0.0347(8) 0.0421(9) 0.0268(8) 0.0107(7) 0.0106(7) 0.0225(7) C33 0.0338(8) 0.0313(8) 0.0264(8) 0.0061(6) 0.0037(6) 0.0109(7) C34 0.0256(7) 0.0254(7) 0.0258(7) 0.0023(6) 0.0046(6) 0.0098(6) C62 0.0300(8) 0.0349(8) 0.0352(9) 0.0074(7) 0.0058(7) 0.0182(7) C9 0.0234(7) 0.0328(8) 0.0338(8) 0.0092(7) 0.0060(6) 0.0111(6) C17 0.0366(9) 0.0320(8) 0.0293(8) 0.0047(7) -0.0003(7) 0.0123(7) C46 0.0280(8) 0.0353(8) 0.0286(8) 0.0088(7) 0.0061(6) 0.0152(7) C30 0.0275(8) 0.0355(9) 0.0364(9) 0.0112(7) -0.0005(7) 0.0052(7) C36 0.0322(8) 0.0352(9) 0.0358(9) 0.0089(7) 0.0141(7) 0.0151(7) C43 0.0339(8) 0.0468(10) 0.0344(9) 0.0224(8) 0.0149(7) 0.0231(8) C35 0.0316(8) 0.0318(8) 0.0300(8) 0.0074(6) 0.0081(6) 0.0149(7) C13 0.0262(8) 0.0371(9) 0.0334(8) 0.0075(7) 0.0098(6) 0.0145(7) C21 0.0241(7) 0.0305(8) 0.0396(9) 0.0117(7) 0.0003(6) 0.0119(6) C38 0.0281(8) 0.0356(9) 0.0366(9) 0.0080(7) 0.0016(7) 0.0145(7) C10 0.0289(8) 0.0392(9) 0.0253(8) 0.0024(7) 0.0024(6) 0.0140(7) C31 0.0377(9) 0.0318(8) 0.0291(8) 0.0056(7) -0.0056(7) 0.0007(7) C32 0.0454(10) 0.0284(8) 0.0261(8) 0.0031(7) 0.0023(7) 0.0087(7) C66 0.0324(8) 0.0370(9) 0.0377(9) 0.0032(7) -0.0014(7) 0.0218(7) C47 0.0446(10) 0.0369(9) 0.0338(9) 0.0129(7) 0.0109(7) 0.0198(8) C63 0.0357(9) 0.0404(9) 0.0397(10) 0.0084(8) 0.0119(7) 0.0216(8) C37 0.0249(8) 0.0347(9) 0.0457(10) 0.0062(7) 0.0099(7) 0.0145(7) C54 0.0309(9) 0.0382(9) 0.0539(11) 0.0232(8) 0.0143(8) 0.0129(7) C6 0.0298(8) 0.0438(10) 0.0312(9) 0.0081(7) -0.0022(7) 0.0112(7) C48 0.0437(10) 0.0410(9) 0.0335(9) 0.0110(7) 0.0073(7) 0.0247(8) C49 0.0359(9) 0.0391(9) 0.0434(10) 0.0206(8) 0.0194(8) 0.0197(8) C25 0.0241(8) 0.0394(9) 0.0433(10) 0.0147(8) 0.0081(7) 0.0146(7) C19 0.0368(10) 0.0342(9) 0.0481(11) 0.0025(8) -0.0132(8) 0.0092(8) C64 0.0287(8) 0.0414(10) 0.0571(12) 0.0127(9) 0.0129(8) 0.0186(8) C8 0.0233(8) 0.0476(10) 0.0447(10) 0.0152(8) 0.0077(7) 0.0153(7) C18 0.0460(10) 0.0359(9) 0.0334(9) 0.0008(7) -0.0064(8) 0.0128(8) C20 0.0231(8) 0.0360(9) 0.0585(12) 0.0133(8) -0.0031(8) 0.0086(7) C58 0.0309(9) 0.0430(10) 0.0482(11) 0.0162(9) 0.0061(8) 0.0107(8) C15 0.0347(9) 0.0467(10) 0.0356(9) 0.0108(8) 0.0152(7) 0.0142(8) C65 0.0264(8) 0.0384(9) 0.0576(12) 0.0048(8) -0.0020(8) 0.0165(7) C50 0.0477(11) 0.0424(10) 0.0454(11) 0.0216(8) 0.0242(9) 0.0224(9) C12 0.0513(11) 0.0376(9) 0.0259(8) 0.0057(7) 0.0063(7) 0.0190(8) C7 0.0244(8) 0.0547(11) 0.0440(10) 0.0148(9) -0.0013(7) 0.0134(8) C67 0.0341(9) 0.0462(10) 0.0327(9) 0.0026(8) 0.0040(7) 0.0157(8) C14 0.0380(10) 0.0452(10) 0.0484(11) 0.0082(9) 0.0141(8) 0.0233(8) C22 0.0453(10) 0.0431(10) 0.0286(9) 0.0036(8) 0.0084(8) 0.0125(8) C60 0.0322(9) 0.0419(10) 0.0628(13) 0.0178(9) 0.0013(9) 0.0125(8) C51 0.0590(13) 0.0518(12) 0.0599(13) 0.0302(10) 0.0390(11) 0.0342(11) C26 0.0345(9) 0.0543(12) 0.0582(12) 0.0267(10) 0.0191(9) 0.0235(9) C27 0.0365(10) 0.0427(10) 0.0578(12) 0.0160(9) 0.0126(9) 0.0221(8) C70 0.0445(11) 0.0575(12) 0.0366(10) -0.0004(9) -0.0059(8) 0.0308(10) B1 0.0242(8) 0.0278(8) 0.0233(8) 0.0051(7) 0.0051(6) 0.0101(7) C52 0.0376(10) 0.0548(12) 0.0788(16) 0.0364(12) 0.0296(11) 0.0231(10) C55 0.0627(13) 0.0507(12) 0.0405(11) 0.0144(9) 0.0233(10) 0.0287(10) C11 0.0509(12) 0.0393(10) 0.0477(11) 0.0064(9) 0.0241(9) 0.0122(9) C53 0.0317(9) 0.0480(11) 0.0702(14) 0.0281(10) 0.0163(9) 0.0149(8) C69 0.0500(12) 0.0330(10) 0.0616(13) 0.0065(9) -0.0058(10) 0.0161(9) C59 0.0738(16) 0.0547(13) 0.0556(14) 0.0245(11) 0.0096(12) 0.0197(12) C24 0.0676(16) 0.0727(16) 0.0428(12) 0.0248(12) 0.0084(11) 0.0140(13) C23 0.0560(14) 0.0648(15) 0.0570(14) 0.0059(11) 0.0217(11) 0.0265(12) C68 0.0721(16) 0.0456(12) 0.0767(17) -0.0108(12) -0.0335(14) 0.0329(12) C71 0.0632(15) 0.0622(15) 0.0546(14) -0.0139(11) -0.0114(11) 0.0306(12) C57 0.0759(17) 0.0459(13) 0.0781(18) 0.0113(12) 0.0291(14) 0.0243(12) C72 0.120(3) 0.086(2) 0.0416(13) 0.0068(13) -0.0138(14) 0.062(2) C56 0.127(3) 0.0630(17) 0.0532(15) 0.0204(13) -0.0041(16) 0.0291(18) O100 0.067(2) 0.063(2) 0.0474(18) 0.0236(15) 0.0122(18) 0.0286(17) C101 0.067(5) 0.073(6) 0.065(5) 0.021(4) 0.005(4) 0.026(5) C102 0.070(5) 0.076(7) 0.056(4) 0.017(4) 0.019(4) 0.038(5) C103 0.067(5) 0.057(4) 0.039(3) 0.017(3) -0.003(3) 0.024(5) C104 0.057(4) 0.078(6) 0.048(3) 0.025(3) 0.016(3) 0.035(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 '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 C1 P1 P2 96.79(5) C46 P2 P1 105.15(6) C1 N1 C2 111.48(12) C1 N1 C4 119.66(13) C2 N1 C4 128.86(13) C1 N2 C3 109.35(13) C1 N2 C16 127.60(13) C3 N2 C16 122.37(13) C46 N3 C47 110.37(14) C46 N3 C49 125.85(14) C47 N3 C49 123.48(15) C46 N4 C48 110.49(14) C46 N4 C61 126.18(14) C48 N4 C61 123.16(14) C3 C2 N1 103.08(13) C3 C2 B1 119.35(14) N1 C2 B1 137.55(13) C45 C40 C41 112.88(14) C45 C40 B1 127.04(14) C41 C40 B1 120.04(14) N2 C1 N1 105.43(13) N2 C1 P1 131.28(12) N1 C1 P1 123.19(11) C2 C3 N2 110.63(14) C29 C28 C33 112.54(15) C29 C28 B1 119.17(14) C33 C28 B1 127.59(15) F11 C41 C42 115.42(15) F11 C41 C40 119.57(14) C42 C41 C40 124.99(15) C5 C4 C9 122.96(14) C5 C4 N1 118.29(13) C9 C4 N1 118.73(14) F12 C42 C43 119.93(15) F12 C42 C41 121.02(16) C43 C42 C41 119.04(16) C62 C61 C66 124.06(16) C62 C61 N4 117.56(15) C66 C61 N4 118.37(15) C21 C16 C17 123.97(15) C21 C16 N2 118.48(14) C17 C16 N2 117.42(14) F1 C29 C30 115.48(15) F1 C29 C28 119.17(14) C30 C29 C28 125.27(16) F10 C39 C34 121.05(14) F10 C39 C38 114.38(15) C34 C39 C38 124.57(15) C6 C5 C4 117.33(15) C6 C5 C10 119.83(15) C4 C5 C10 122.77(14) F15 C45 C44 114.68(14) F15 C45 C40 121.18(14) C44 C45 C40 124.14(16) F14 C44 C43 119.76(15) F14 C44 C45 120.26(16) C43 C44 C45 119.97(16) F5 C33 C32 114.00(15) F5 C33 C28 121.82(15) C32 C33 C28 124.14(17) C39 C34 C35 112.77(14) C39 C34 B1 126.93(14) C35 C34 B1 120.17(14) C63 C62 C61 116.94(16) C63 C62 C67 120.16(16) C61 C62 C67 122.88(16) C8 C9 C4 116.70(16) C8 C9 C13 118.88(15) C4 C9 C13 124.40(14) C18 C17 C16 116.83(17) C18 C17 C22 119.85(16) C16 C17 C22 123.19(15) N4 C46 N3 104.63(14) N4 C46 P2 135.78(13) N3 C46 P2 119.59(12) F2 C30 C31 120.26(16) F2 C30 C29 120.55(16) C31 C30 C29 119.17(17) F7 C36 C37 119.71(15) F7 C36 C35 120.74(16) C37 C36 C35 119.54(16) F13 C43 C44 120.64(16) F13 C43 C42 120.43(16) C44 C43 C42 118.93(15) F6 C35 C36 116.09(15) F6 C35 C34 119.28(14) C36 C35 C34 124.62(16) C9 C13 C14 111.67(15) C9 C13 C15 112.04(15) C14 C13 C15 109.01(14) C16 C21 C20 116.06(16) C16 C21 C25 122.68(15) C20 C21 C25 121.18(16) F9 C38 C37 120.16(15) F9 C38 C39 120.16(16) C37 C38 C39 119.68(16) C5 C10 C12 112.72(15) C5 C10 C11 110.25(15) C12 C10 C11 109.48(15) F3 C31 C32 120.78(17) F3 C31 C30 120.56(18) C32 C31 C30 118.63(16) F4 C32 C31 119.88(16) F4 C32 C33 120.01(17) C31 C32 C33 120.11(16) C65 C66 C61 116.35(17) C65 C66 C70 121.52(17) C61 C66 C70 122.14(17) C48 C47 N3 107.24(16) C64 C63 C62 120.59(18) F8 C37 C38 120.90(17) F8 C37 C36 120.35(16) C38 C37 C36 118.74(15) C49 C54 C53 116.96(19) C49 C54 C58 123.23(16) C53 C54 C58 119.78(19) C7 C6 C5 121.09(17) C47 C48 N4 107.27(15) C54 C49 C50 124.00(17) C54 C49 N3 117.56(16) C50 C49 N3 118.40(18) C21 C25 C26 112.48(16) C21 C25 C27 110.30(15) C26 C25 C27 109.76(15) C18 C19 C20 121.02(17) C65 C64 C63 121.03(17) C7 C8 C9 121.69(16) C19 C18 C17 120.87(18) C19 C20 C21 121.06(17) C54 C58 C59 110.21(18) C54 C58 C60 112.00(16) C59 C58 C60 111.06(18) C64 C65 C66 121.00(17) C49 C50 C51 116.0(2) C49 C50 C55 121.90(18) C51 C50 C55 122.08(19) C8 C7 C6 120.10(16) C69 C67 C62 110.69(16) C69 C67 C68 110.04(18) C62 C67 C68 112.03(18) C17 C22 C24 111.07(18) C17 C22 C23 112.55(18) C24 C22 C23 111.21(19) C52 C51 C50 121.2(2) C66 C70 C72 110.60(17) C66 C70 C71 112.2(2) C72 C70 C71 110.6(2) C28 B1 C40 103.89(12) C28 B1 C34 110.95(12) C40 B1 C34 110.82(13) C28 B1 C2 118.07(13) C40 B1 C2 112.03(12) C34 B1 C2 101.22(12) C53 C52 C51 120.92(19) C50 C55 C56 110.0(2) C50 C55 C57 112.9(2) C56 C55 C57 110.1(2) C52 C53 C54 120.9(2) C104 O100 C101 103.2(9) O100 C101 C102 107.7(10) C101 C102 C103 106.4(8) C104 C103 C102 101.1(7) O100 C104 C103 109.2(9) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance P1 C1 1.8342(16) P1 P2 2.1239(6) P2 C46 1.8135(17) F1 C29 1.3479(19) F11 C41 1.3573(18) F15 C45 1.3475(19) F10 C39 1.3525(19) F6 C35 1.345(2) F5 C33 1.354(2) F12 C42 1.338(2) F14 C44 1.3459(19) F7 C36 1.343(2) F3 C31 1.343(2) F9 C38 1.346(2) F2 C30 1.344(2) F4 C32 1.347(2) F13 C43 1.3414(19) F8 C37 1.3424(19) N1 C1 1.371(2) N1 C2 1.414(2) N1 C4 1.4565(19) N2 C1 1.353(2) N2 C3 1.374(2) N2 C16 1.4503(19) N3 C46 1.374(2) N3 C47 1.378(2) N3 C49 1.453(2) N4 C46 1.363(2) N4 C48 1.383(2) N4 C61 1.444(2) C2 C3 1.362(2) C2 B1 1.668(2) C40 C45 1.392(2) C40 C41 1.392(2) C40 B1 1.663(2) C28 C29 1.390(2) C28 C33 1.393(2) C28 B1 1.659(2) C41 C42 1.384(2) C4 C5 1.399(2) C4 C9 1.408(2) C42 C43 1.380(3) C61 C62 1.393(2) C61 C66 1.398(2) C16 C21 1.398(2) C16 C17 1.399(2) C29 C30 1.383(2) C39 C34 1.383(2) C39 C38 1.391(2) C5 C6 1.394(2) C5 C10 1.517(2) C45 C44 1.388(2) C44 C43 1.370(3) C33 C32 1.385(2) C34 C35 1.397(2) C34 B1 1.666(2) C62 C63 1.391(2) C62 C67 1.522(3) C9 C8 1.396(2) C9 C13 1.522(2) C17 C18 1.396(3) C17 C22 1.517(3) C30 C31 1.375(3) C36 C37 1.379(3) C36 C35 1.379(2) C13 C14 1.535(2) C13 C15 1.536(2) C21 C20 1.406(2) C21 C25 1.512(3) C38 C37 1.368(3) C10 C12 1.527(2) C10 C11 1.536(3) C31 C32 1.374(3) C66 C65 1.397(3) C66 C70 1.517(3) C47 C48 1.347(3) C63 C64 1.383(3) C54 C49 1.392(3) C54 C53 1.398(3) C54 C58 1.518(3) C6 C7 1.387(3) C49 C50 1.398(3) C25 C26 1.528(3) C25 C27 1.536(2) C19 C18 1.373(3) C19 C20 1.380(3) C64 C65 1.375(3) C8 C7 1.377(3) C58 C59 1.530(3) C58 C60 1.530(3) C50 C51 1.408(3) C50 C55 1.504(3) C67 C69 1.519(3) C67 C68 1.526(3) C22 C24 1.525(3) C22 C23 1.537(3) C51 C52 1.374(4) C70 C72 1.525(3) C70 C71 1.528(3) C52 C53 1.372(3) C55 C56 1.522(3) C55 C57 1.537(3) O100 C104 1.435(10) O100 C101 1.461(11) C101 C102 1.497(11) C102 C103 1.545(12) C103 C104 1.510(10) 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 C1 N1 C2 C3 1.04(16) C4 N1 C2 C3 -179.29(14) C1 N1 C2 B1 179.45(16) C4 N1 C2 B1 -0.9(3) C3 N2 C1 N1 1.83(16) C16 N2 C1 N1 -168.73(14) C3 N2 C1 P1 178.34(12) C16 N2 C1 P1 7.8(2) C2 N1 C1 N2 -1.80(16) C4 N1 C1 N2 178.50(13) C2 N1 C1 P1 -178.67(10) C4 N1 C1 P1 1.64(19) P2 P1 C1 N2 48.93(15) P2 P1 C1 N1 -135.09(12) N1 C2 C3 N2 0.13(16) B1 C2 C3 N2 -178.64(12) C1 N2 C3 C2 -1.26(18) C16 N2 C3 C2 169.89(14) C45 C40 C41 F11 -176.03(13) B1 C40 C41 F11 6.3(2) C45 C40 C41 C42 2.1(2) B1 C40 C41 C42 -175.63(15) C1 N1 C4 C5 98.88(17) C2 N1 C4 C5 -80.8(2) C1 N1 C4 C9 -79.45(19) C2 N1 C4 C9 100.91(18) F11 C41 C42 F12 -2.9(2) C40 C41 C42 F12 178.95(15) F11 C41 C42 C43 177.73(14) C40 C41 C42 C43 -0.4(3) C46 N4 C61 C62 86.0(2) C48 N4 C61 C62 -88.8(2) C46 N4 C61 C66 -95.2(2) C48 N4 C61 C66 90.0(2) C1 N2 C16 C21 -107.63(18) C3 N2 C16 C21 82.93(19) C1 N2 C16 C17 76.4(2) C3 N2 C16 C17 -93.04(18) C33 C28 C29 F1 172.68(14) B1 C28 C29 F1 1.5(2) C33 C28 C29 C30 -3.9(2) B1 C28 C29 C30 -175.07(16) C9 C4 C5 C6 -3.8(2) N1 C4 C5 C6 177.90(15) C9 C4 C5 C10 173.04(16) N1 C4 C5 C10 -5.2(2) C41 C40 C45 F15 177.71(14) B1 C40 C45 F15 -4.8(2) C41 C40 C45 C44 -2.1(2) B1 C40 C45 C44 175.38(15) F15 C45 C44 F14 1.3(2) C40 C45 C44 F14 -178.87(15) F15 C45 C44 C43 -179.27(15) C40 C45 C44 C43 0.6(3) C29 C28 C33 F5 -174.21(15) B1 C28 C33 F5 -3.9(3) C29 C28 C33 C32 3.3(2) B1 C28 C33 C32 173.62(16) F10 C39 C34 C35 176.41(14) C38 C39 C34 C35 -3.0(2) F10 C39 C34 B1 0.5(3) C38 C39 C34 B1 -178.87(16) C66 C61 C62 C63 2.2(3) N4 C61 C62 C63 -179.06(15) C66 C61 C62 C67 -176.49(17) N4 C61 C62 C67 2.3(2) C5 C4 C9 C8 2.2(3) N1 C4 C9 C8 -179.53(15) C5 C4 C9 C13 -179.37(16) N1 C4 C9 C13 -1.1(2) C21 C16 C17 C18 5.3(3) N2 C16 C17 C18 -179.01(15) C21 C16 C17 C22 -170.50(17) N2 C16 C17 C22 5.2(2) C48 N4 C46 N3 -0.04(19) C61 N4 C46 N3 -175.37(15) C48 N4 C46 P2 -178.90(15) C61 N4 C46 P2 5.8(3) C47 N3 C46 N4 0.12(19) C49 N3 C46 N4 174.02(16) C47 N3 C46 P2 179.21(12) C49 N3 C46 P2 -6.9(2) P1 P2 C46 N4 4.36(19) P1 P2 C46 N3 -174.37(12) F1 C29 C30 F2 3.3(2) C28 C29 C30 F2 179.97(16) F1 C29 C30 C31 -175.16(15) C28 C29 C30 C31 1.5(3) F14 C44 C43 F13 1.0(3) C45 C44 C43 F13 -178.44(15) F14 C44 C43 C42 -179.30(15) C45 C44 C43 C42 1.3(3) F12 C42 C43 F13 -1.0(3) C41 C42 C43 F13 178.38(15) F12 C42 C43 C44 179.28(15) C41 C42 C43 C44 -1.3(3) F7 C36 C35 F6 1.3(2) C37 C36 C35 F6 -178.98(15) F7 C36 C35 C34 -179.24(16) C37 C36 C35 C34 0.5(3) C39 C34 C35 F6 -178.69(14) B1 C34 C35 F6 -2.5(2) C39 C34 C35 C36 1.9(2) B1 C34 C35 C36 178.04(16) C8 C9 C13 C14 -59.9(2) C4 C9 C13 C14 121.71(18) C8 C9 C13 C15 62.7(2) C4 C9 C13 C15 -115.68(18) C17 C16 C21 C20 -3.6(2) N2 C16 C21 C20 -179.30(15) C17 C16 C21 C25 173.20(16) N2 C16 C21 C25 -2.5(2) F10 C39 C38 F9 1.7(2) C34 C39 C38 F9 -178.81(16) F10 C39 C38 C37 -177.66(16) C34 C39 C38 C37 1.8(3) C6 C5 C10 C12 -48.4(2) C4 C5 C10 C12 134.74(17) C6 C5 C10 C11 74.2(2) C4 C5 C10 C11 -102.58(19) F2 C30 C31 F3 1.2(3) C29 C30 C31 F3 179.66(16) F2 C30 C31 C32 -176.74(16) C29 C30 C31 C32 1.7(3) F3 C31 C32 F4 -1.2(3) C30 C31 C32 F4 176.76(16) F3 C31 C32 C33 179.87(16) C30 C31 C32 C33 -2.2(3) F5 C33 C32 F4 -1.7(2) C28 C33 C32 F4 -179.44(16) F5 C33 C32 C31 177.22(16) C28 C33 C32 C31 -0.5(3) C62 C61 C66 C65 -0.9(3) N4 C61 C66 C65 -179.66(15) C62 C61 C66 C70 178.83(17) N4 C61 C66 C70 0.1(2) C46 N3 C47 C48 -0.2(2) C49 N3 C47 C48 -174.23(17) C61 C62 C63 C64 -1.9(3) C67 C62 C63 C64 176.78(17) F9 C38 C37 F8 0.8(3) C39 C38 C37 F8 -179.75(16) F9 C38 C37 C36 -178.57(16) C39 C38 C37 C36 0.8(3) F7 C36 C37 F8 -1.6(3) C35 C36 C37 F8 178.69(16) F7 C36 C37 C38 177.84(16) C35 C36 C37 C38 -1.9(3) C4 C5 C6 C7 2.4(3) C10 C5 C6 C7 -174.60(18) N3 C47 C48 N4 0.1(2) C46 N4 C48 C47 -0.1(2) C61 N4 C48 C47 175.44(16) C53 C54 C49 C50 -0.3(3) C58 C54 C49 C50 -178.33(17) C53 C54 C49 N3 -178.11(16) C58 C54 C49 N3 3.8(3) C46 N3 C49 C54 -93.7(2) C47 N3 C49 C54 79.4(2) C46 N3 C49 C50 88.3(2) C47 N3 C49 C50 -98.5(2) C16 C21 C25 C26 138.50(17) C20 C21 C25 C26 -44.8(2) C16 C21 C25 C27 -98.60(19) C20 C21 C25 C27 78.1(2) C62 C63 C64 C65 0.5(3) C4 C9 C8 C7 0.9(3) C13 C9 C8 C7 -177.56(18) C20 C19 C18 C17 -0.8(3) C16 C17 C18 C19 -2.9(3) C22 C17 C18 C19 172.99(19) C18 C19 C20 C21 2.5(3) C16 C21 C20 C19 -0.4(3) C25 C21 C20 C19 -177.26(17) C49 C54 C58 C59 108.6(2) C53 C54 C58 C59 -69.4(2) C49 C54 C58 C60 -127.22(19) C53 C54 C58 C60 54.8(2) C63 C64 C65 C66 0.8(3) C61 C66 C65 C64 -0.6(3) C70 C66 C65 C64 179.61(18) C54 C49 C50 C51 -0.6(3) N3 C49 C50 C51 177.27(16) C54 C49 C50 C55 -178.88(18) N3 C49 C50 C55 -1.1(3) C9 C8 C7 C6 -2.3(3) C5 C6 C7 C8 0.6(3) C63 C62 C67 C69 -53.9(2) C61 C62 C67 C69 124.75(19) C63 C62 C67 C68 69.3(2) C61 C62 C67 C68 -112.0(2) C18 C17 C22 C24 -61.1(2) C16 C17 C22 C24 114.6(2) C18 C17 C22 C23 64.4(2) C16 C17 C22 C23 -120.0(2) C49 C50 C51 C52 1.0(3) C55 C50 C51 C52 179.35(19) C65 C66 C70 C72 85.4(3) C61 C66 C70 C72 -94.3(2) C65 C66 C70 C71 -38.6(3) C61 C66 C70 C71 141.65(19) C29 C28 B1 C40 57.11(18) C33 C28 B1 C40 -112.60(17) C29 C28 B1 C34 176.24(14) C33 C28 B1 C34 6.5(2) C29 C28 B1 C2 -67.63(19) C33 C28 B1 C2 122.66(17) C45 C40 B1 C28 -127.21(16) C41 C40 B1 C28 50.14(18) C45 C40 B1 C34 113.57(17) C41 C40 B1 C34 -69.07(18) C45 C40 B1 C2 1.3(2) C41 C40 B1 C2 178.68(13) C39 C34 B1 C28 -121.78(17) C35 C34 B1 C28 62.63(19) C39 C34 B1 C40 -6.9(2) C35 C34 B1 C40 177.50(14) C39 C34 B1 C2 112.08(17) C35 C34 B1 C2 -63.51(17) C3 C2 B1 C28 -155.69(14) N1 C2 B1 C28 26.1(2) C3 C2 B1 C40 83.68(17) N1 C2 B1 C40 -94.5(2) C3 C2 B1 C34 -34.43(17) N1 C2 B1 C34 147.36(17) C50 C51 C52 C53 -0.7(3) C49 C50 C55 C56 95.5(2) C51 C50 C55 C56 -82.7(3) C49 C50 C55 C57 -141.1(2) C51 C50 C55 C57 40.7(3) C51 C52 C53 C54 -0.2(3) C49 C54 C53 C52 0.7(3) C58 C54 C53 C52 178.79(19) C104 O100 C101 C102 29.7(14) O100 C101 C102 C103 -13(2) C101 C102 C103 C104 -9(2) C101 O100 C104 C103 -36.7(12) C102 C103 C104 O100 28(2)