#------------------------------------------------------------------------------ #$Date: 2020-02-04 22:18:14 +0200 (Tue, 04 Feb 2020) $ #$Revision: 247648 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/64/1556414.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_1556414 loop_ _publ_author_name 'Wilson, Daniel W. N.' 'Franco, Mauricio P.' 'Myers, William K.' 'McGrady, John E.' 'Goicoechea, Jose M.' _publ_section_title ; Base induced isomerisation of a phosphaethynolato-borane: mechanistic insights into boryl migration and decarbonylation to afford a triplet phosphinidene ; _journal_issue 3 _journal_name_full 'Chemical Science' _journal_page_first 862 _journal_paper_doi 10.1039/C9SC05969E _journal_volume 11 _journal_year 2020 _chemical_formula_moiety 'C65 H92 B2 N6 O2 P2, 1.5(C6 H14)' _chemical_formula_sum 'C74 H113 B2 N6 O2 P2' _chemical_formula_weight 1202.26 _chemical_name_systematic ; cyclo-[(Me2IPr)C(O)CPB[{N(2,6-iPr-C6H3)}2(CH)2]PoB[{N(2,6-iPr-C6H3)}2(CH)2]*1.5hex ; _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-2018/1 _audit_update_record ; 2019-11-01 deposited with the CCDC. 2019-12-02 downloaded from the CCDC. ; _cell_angle_alpha 73.781(2) _cell_angle_beta 76.257(2) _cell_angle_gamma 67.558(2) _cell_formula_units_Z 2 _cell_length_a 14.0563(4) _cell_length_b 14.7947(4) _cell_length_c 20.1864(5) _cell_measurement_reflns_used 24760 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 76.4960 _cell_measurement_theta_min 3.3020 _cell_volume 3684.82(18) _computing_cell_refinement 'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)' _computing_structure_refinement 'SHELXL-2018/1 (Sheldrick, 2018)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 150(2) _diffrn_detector_area_resol_mean 10.4102 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.990 _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator mirror _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0366 _diffrn_reflns_av_unetI/netI 0.0291 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.990 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 59780 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.990 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 76.678 _diffrn_reflns_theta_min 2.305 _exptl_absorpt_coefficient_mu 0.880 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.70810 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.084 _exptl_crystal_description block _exptl_crystal_F_000 1310 _exptl_crystal_size_max 0.340 _exptl_crystal_size_mid 0.220 _exptl_crystal_size_min 0.140 _refine_diff_density_max 1.053 _refine_diff_density_min -0.718 _refine_diff_density_rms 0.048 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 797 _refine_ls_number_reflns 15378 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.043 _refine_ls_R_factor_all 0.0640 _refine_ls_R_factor_gt 0.0523 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0756P)^2^+1.7565P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1399 _refine_ls_wR_factor_ref 0.1508 _reflns_Friedel_coverage 0.000 _reflns_number_gt 12676 _reflns_number_total 15378 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9sc05969e2.cif _cod_data_source_block DW372C _cod_depositor_comments 'Adding full bibliography for 1556409--1556415.cif.' _cod_database_code 1556414 _shelx_shelxl_version_number 2018/1 _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 0.754 _shelx_estimated_absorpt_t_max 0.887 _shelx_res_file ; TITL p-1 in P-1 shelx.res created by SHELXL-2018/1 at 09:01:58 on 23-Feb-2019 CELL 1.54184 14.0563 14.7947 20.1864 73.781 76.257 67.558 ZERR 2.00 0.0004 0.0004 0.0005 0.002 0.002 0.002 LATT 1 SFAC C H B N O P UNIT 148 226 4 12 4 4 MERG 2 FMAP 2 PLAN 20 SIZE 0.140 0.220 0.340 ACTA BOND $H L.S. 24 TEMP -123.00 WGHT 0.075600 1.756500 FVAR 0.12387 P1 6 0.827248 0.129823 0.225589 11.00000 0.03376 0.02526 = 0.02369 -0.00123 -0.00775 -0.01114 P2 6 0.687422 0.173618 0.173756 11.00000 0.02524 0.02490 = 0.02418 -0.00328 -0.00076 -0.01155 O2 5 0.661361 0.066712 0.190601 11.00000 0.02913 0.02854 = 0.02791 -0.00681 0.00342 -0.01552 B1 3 0.812235 0.237053 0.267093 11.00000 0.02379 0.03115 = 0.02225 -0.00249 -0.00108 -0.01299 N1 4 0.784098 0.343872 0.246411 11.00000 0.02709 0.02921 = 0.02510 -0.00496 0.00080 -0.01264 N2 4 0.827173 0.215339 0.338764 11.00000 0.03333 0.03299 = 0.02223 -0.00423 -0.00040 -0.01572 B2 3 0.584327 0.042841 0.240264 11.00000 0.02771 0.02666 = 0.02268 -0.00489 -0.00064 -0.01180 N3 4 0.483524 0.104042 0.268339 11.00000 0.02661 0.02443 = 0.02624 -0.00209 0.00290 -0.01013 N4 4 0.593311 -0.058318 0.275085 11.00000 0.03044 0.02449 = 0.03204 -0.00559 0.00490 -0.01033 N5 4 0.797874 0.233483 -0.025256 11.00000 0.03624 0.03640 = 0.02170 -0.00195 -0.00407 -0.01218 N6 4 0.803460 0.079082 0.006534 11.00000 0.03090 0.03748 = 0.02732 -0.00781 -0.00355 -0.01323 C1 1 0.875018 0.160913 0.129216 11.00000 0.02547 0.03115 = 0.02692 -0.00827 -0.00045 -0.01007 O1 5 0.957831 0.174848 0.099975 11.00000 0.03026 0.06399 = 0.04042 -0.02035 0.00524 -0.02415 C2 1 0.791819 0.159589 0.102560 11.00000 0.02607 0.02762 = 0.02097 -0.00182 -0.00139 -0.01222 C3 1 0.781532 0.380729 0.303960 11.00000 0.04559 0.03423 = 0.03200 -0.01220 0.00441 -0.01787 AFIX 43 H3 2 0.764199 0.449296 0.304260 11.00000 -1.20000 AFIX 0 C4 1 0.807224 0.304602 0.358442 11.00000 0.04974 0.04267 = 0.02710 -0.01249 0.00271 -0.02191 AFIX 43 H4 2 0.811189 0.310572 0.403279 11.00000 -1.20000 AFIX 0 C5 1 0.778627 0.411483 0.179138 11.00000 0.02853 0.02450 = 0.02829 -0.00424 0.00096 -0.01231 C6 1 0.870790 0.426833 0.140689 11.00000 0.02836 0.02891 = 0.03567 -0.00362 0.00057 -0.01269 C7 1 0.862699 0.502825 0.081028 11.00000 0.03467 0.03626 = 0.03601 -0.00165 0.00503 -0.01810 AFIX 43 H7 2 0.923777 0.515283 0.054727 11.00000 -1.20000 AFIX 0 C8 1 0.767542 0.560381 0.059411 11.00000 0.04347 0.03413 = 0.03235 0.00242 -0.00263 -0.01750 AFIX 43 H8 2 0.763086 0.613589 0.019592 11.00000 -1.20000 AFIX 0 C9 1 0.678845 0.540424 0.095809 11.00000 0.03456 0.03289 = 0.03745 -0.00079 -0.00827 -0.01251 AFIX 43 H9 2 0.614032 0.578531 0.079525 11.00000 -1.20000 AFIX 0 C10 1 0.682591 0.465336 0.156068 11.00000 0.02896 0.02773 = 0.03380 -0.00503 -0.00113 -0.01339 C11 1 0.976021 0.364986 0.163531 11.00000 0.02539 0.03624 = 0.05337 0.00669 0.00056 -0.01227 AFIX 13 H11 2 0.970222 0.300953 0.194584 11.00000 -1.20000 AFIX 0 C12 1 1.061734 0.338378 0.102206 11.00000 0.03070 0.05197 = 0.07649 -0.01400 0.00889 -0.01378 AFIX 137 H12A 2 1.040576 0.306326 0.074518 11.00000 -1.50000 H12B 2 1.126226 0.292336 0.119937 11.00000 -1.50000 H12C 2 1.073305 0.399426 0.072879 11.00000 -1.50000 AFIX 0 C13 1 1.006470 0.417825 0.205828 11.00000 0.03255 0.08097 = 0.05255 -0.00423 -0.01185 -0.01671 AFIX 137 H13A 2 1.012375 0.481235 0.176735 11.00000 -1.50000 H13B 2 1.073486 0.375198 0.221409 11.00000 -1.50000 H13C 2 0.953117 0.431000 0.246524 11.00000 -1.50000 AFIX 0 C14 1 0.583412 0.445719 0.194886 11.00000 0.02555 0.03153 = 0.05226 -0.00060 -0.00059 -0.01194 AFIX 13 H14 2 0.603400 0.379918 0.228509 11.00000 -1.20000 AFIX 0 C15 1 0.521649 0.438746 0.144480 11.00000 0.04486 0.05832 = 0.08492 0.02071 -0.03041 -0.03098 AFIX 137 H15A 2 0.496346 0.504110 0.113366 11.00000 -1.50000 H15B 2 0.462328 0.418572 0.171075 11.00000 -1.50000 H15C 2 0.566759 0.389095 0.116751 11.00000 -1.50000 AFIX 0 C16 1 0.517219 0.525610 0.236337 11.00000 0.05543 0.05665 = 0.10213 -0.02806 0.03861 -0.02556 AFIX 137 H16A 2 0.554268 0.521937 0.272984 11.00000 -1.50000 H16B 2 0.451100 0.514709 0.257625 11.00000 -1.50000 H16C 2 0.503569 0.591745 0.205154 11.00000 -1.50000 AFIX 0 C17 1 0.875268 0.118765 0.380481 11.00000 0.03362 0.03776 = 0.02113 -0.00520 -0.00495 -0.01328 C18 1 0.983718 0.074521 0.367100 11.00000 0.03438 0.06105 = 0.02209 -0.00765 -0.00616 -0.01288 C19 1 1.028954 -0.021237 0.405180 11.00000 0.03693 0.06120 = 0.03572 -0.01375 -0.01193 0.00038 AFIX 43 H19 2 1.102175 -0.053230 0.396596 11.00000 -1.20000 AFIX 0 C20 1 0.969490 -0.070478 0.455092 11.00000 0.05656 0.03982 = 0.04582 -0.00497 -0.02454 -0.00450 AFIX 43 H20 2 1.001825 -0.135795 0.480536 11.00000 -1.20000 AFIX 0 C21 1 0.863007 -0.025005 0.468158 11.00000 0.05052 0.04057 = 0.03772 0.00396 -0.01511 -0.01858 AFIX 43 H21 2 0.822723 -0.059467 0.502788 11.00000 -1.20000 AFIX 0 C22 1 0.813587 0.070614 0.431407 11.00000 0.03749 0.03732 = 0.02661 -0.00138 -0.00705 -0.01459 C23 1 1.051803 0.127959 0.313192 11.00000 0.03046 0.09933 = 0.02788 0.00456 -0.00333 -0.01799 AFIX 13 H23 2 1.003220 0.193839 0.291771 11.00000 -1.20000 AFIX 0 C24 1 1.108992 0.075924 0.255196 11.00000 0.08728 0.18869 = 0.06463 -0.06738 0.03554 -0.07654 AFIX 137 H24A 2 1.158385 0.010684 0.273425 11.00000 -1.50000 H24B 2 1.146904 0.116309 0.220690 11.00000 -1.50000 H24C 2 1.059530 0.066346 0.233095 11.00000 -1.50000 AFIX 0 C25 1 1.123204 0.151577 0.345468 11.00000 0.07960 0.07577 = 0.05477 -0.00746 0.00527 -0.04541 AFIX 137 H25A 2 1.173638 0.089147 0.366534 11.00000 -1.50000 H25B 2 1.082291 0.189693 0.381495 11.00000 -1.50000 H25C 2 1.160234 0.191290 0.309416 11.00000 -1.50000 AFIX 0 C26 1 0.697133 0.120512 0.448583 11.00000 0.03645 0.04525 = 0.03536 0.01017 -0.00247 -0.01602 AFIX 13 H26 2 0.674843 0.180734 0.410570 11.00000 -1.20000 AFIX 0 C27 1 0.635711 0.053393 0.452238 11.00000 0.04586 0.06931 = 0.07840 0.01459 -0.01902 -0.03052 AFIX 137 H27A 2 0.647248 0.036796 0.406597 11.00000 -1.50000 H27B 2 0.561411 0.088428 0.465187 11.00000 -1.50000 H27C 2 0.658957 -0.008226 0.487280 11.00000 -1.50000 AFIX 0 C28 1 0.672323 0.156659 0.516913 11.00000 0.05250 0.07334 = 0.04816 -0.01094 0.01280 -0.01403 AFIX 137 H28A 2 0.691119 0.098857 0.555474 11.00000 -1.50000 H28B 2 0.597767 0.194194 0.525677 11.00000 -1.50000 H28C 2 0.712226 0.200029 0.513257 11.00000 -1.50000 AFIX 0 C29 1 0.438685 0.039189 0.320135 11.00000 0.03276 0.03202 = 0.03219 -0.00287 0.00901 -0.01510 AFIX 43 H29 2 0.372842 0.059742 0.348216 11.00000 -1.20000 AFIX 0 C30 1 0.502577 -0.055020 0.323661 11.00000 0.03924 0.02869 = 0.03628 -0.00243 0.00945 -0.01571 AFIX 43 H30 2 0.488840 -0.111688 0.354489 11.00000 -1.20000 AFIX 0 C31 1 0.418514 0.205012 0.245305 11.00000 0.02299 0.02664 = 0.02987 -0.00241 0.00065 -0.00978 C32 1 0.391533 0.236021 0.177555 11.00000 0.02389 0.03395 = 0.03228 -0.00307 -0.00179 -0.01398 C33 1 0.318347 0.330824 0.160048 11.00000 0.02939 0.03693 = 0.03991 0.00149 -0.01022 -0.01388 AFIX 43 H33 2 0.299073 0.353179 0.114660 11.00000 -1.20000 AFIX 0 C34 1 0.273188 0.393029 0.207142 11.00000 0.02697 0.02979 = 0.05330 -0.00078 -0.00917 -0.00799 AFIX 43 H34 2 0.221995 0.456509 0.194476 11.00000 -1.20000 AFIX 0 C35 1 0.302485 0.362883 0.272426 11.00000 0.03018 0.02892 = 0.04431 -0.00818 0.00110 -0.00798 AFIX 43 H35 2 0.272385 0.406745 0.304099 11.00000 -1.20000 AFIX 0 C36 1 0.375629 0.269017 0.292912 11.00000 0.02880 0.02933 = 0.03207 -0.00427 0.00193 -0.01004 C37 1 0.437109 0.170868 0.123386 11.00000 0.03071 0.04284 = 0.03255 -0.00781 -0.00661 -0.01194 AFIX 13 H37 2 0.490916 0.108340 0.143906 11.00000 -1.20000 AFIX 0 C38 1 0.491675 0.221975 0.056959 11.00000 0.05551 0.06971 = 0.03340 -0.00844 -0.00073 -0.02463 AFIX 137 H38A 2 0.440187 0.281649 0.034038 11.00000 -1.50000 H38B 2 0.526142 0.175545 0.025252 11.00000 -1.50000 H38C 2 0.543612 0.241430 0.069083 11.00000 -1.50000 AFIX 0 C39 1 0.355260 0.140084 0.105966 11.00000 0.04286 0.07018 = 0.07203 -0.03594 -0.00658 -0.02141 AFIX 137 H39A 2 0.323982 0.104138 0.148622 11.00000 -1.50000 H39B 2 0.388244 0.096461 0.072293 11.00000 -1.50000 H39C 2 0.301080 0.199916 0.085814 11.00000 -1.50000 AFIX 0 C40 1 0.407200 0.240488 0.364796 11.00000 0.04445 0.03207 = 0.03028 -0.00694 -0.00119 -0.00834 AFIX 13 H40 2 0.458896 0.171068 0.370430 11.00000 -1.20000 AFIX 0 C41 1 0.459976 0.309642 0.372218 11.00000 0.05732 0.04719 = 0.04464 -0.00918 -0.01255 -0.01732 AFIX 137 H41A 2 0.521567 0.306058 0.336570 11.00000 -1.50000 H41B 2 0.480970 0.288658 0.418637 11.00000 -1.50000 H41C 2 0.411222 0.378537 0.366205 11.00000 -1.50000 AFIX 0 C42 1 0.314629 0.240095 0.422842 11.00000 0.06282 0.05956 = 0.03563 -0.01007 0.00919 -0.02297 AFIX 137 H42A 2 0.265688 0.308551 0.421256 11.00000 -1.50000 H42B 2 0.339433 0.213424 0.468200 11.00000 -1.50000 H42C 2 0.279508 0.198060 0.416229 11.00000 -1.50000 AFIX 0 C43 1 0.659815 -0.148651 0.251944 11.00000 0.03630 0.02408 = 0.03414 -0.00497 0.00331 -0.01119 C44 1 0.617822 -0.192531 0.217639 11.00000 0.04258 0.03227 = 0.04848 -0.01093 0.00017 -0.01522 C45 1 0.682016 -0.281954 0.197720 11.00000 0.05821 0.03726 = 0.06287 -0.02125 -0.00460 -0.01570 AFIX 43 H45 2 0.654769 -0.314407 0.176177 11.00000 -1.20000 AFIX 0 C46 1 0.784165 -0.324049 0.208714 11.00000 0.05903 0.03346 = 0.06330 -0.02187 -0.00064 -0.00607 AFIX 43 H46 2 0.826792 -0.384902 0.194509 11.00000 -1.20000 AFIX 0 C47 1 0.825181 -0.278360 0.240301 11.00000 0.04142 0.03465 = 0.05384 -0.01162 -0.00128 -0.00274 AFIX 43 H47 2 0.896326 -0.307487 0.246576 11.00000 -1.20000 AFIX 0 C48 1 0.763652 -0.189856 0.263216 11.00000 0.03612 0.02797 = 0.03555 -0.00556 0.00218 -0.00930 C49 1 0.506667 -0.145310 0.200913 11.00000 0.04556 0.04222 = 0.06251 -0.01659 -0.00567 -0.01846 AFIX 13 H49 2 0.480496 -0.074148 0.205916 11.00000 -1.20000 AFIX 0 C50 1 0.501303 -0.144891 0.125890 11.00000 0.05707 0.07792 = 0.07729 -0.02866 -0.01748 -0.02438 AFIX 137 H50A 2 0.546386 -0.110071 0.093384 11.00000 -1.50000 H50B 2 0.429430 -0.110422 0.116488 11.00000 -1.50000 H50C 2 0.524660 -0.213912 0.119817 11.00000 -1.50000 AFIX 0 C51 1 0.433195 -0.197175 0.251665 11.00000 0.05426 0.05691 = 0.09740 -0.02320 0.00279 -0.02872 AFIX 137 H51A 2 0.362309 -0.162704 0.240331 11.00000 -1.50000 H51B 2 0.434037 -0.194820 0.299553 11.00000 -1.50000 H51C 2 0.456450 -0.267031 0.247431 11.00000 -1.50000 AFIX 0 C52 1 0.807204 -0.144247 0.302829 11.00000 0.03724 0.03241 = 0.04330 -0.00651 -0.00393 -0.00989 AFIX 13 H52 2 0.766700 -0.070993 0.295541 11.00000 -1.20000 AFIX 0 C53 1 0.921694 -0.155734 0.278185 11.00000 0.03933 0.05121 = 0.07798 -0.01438 -0.00680 -0.01267 AFIX 137 H53A 2 0.964479 -0.226288 0.290635 11.00000 -1.50000 H53B 2 0.941227 -0.115877 0.300633 11.00000 -1.50000 H53C 2 0.932972 -0.132419 0.227447 11.00000 -1.50000 AFIX 0 C54 1 0.788811 -0.188379 0.380770 11.00000 0.09378 0.07195 = 0.04439 -0.00862 -0.00943 -0.04323 AFIX 137 H54A 2 0.714079 -0.174807 0.396441 11.00000 -1.50000 H54B 2 0.815198 -0.157853 0.406455 11.00000 -1.50000 H54C 2 0.825349 -0.260807 0.389452 11.00000 -1.50000 AFIX 0 C55 1 0.795425 0.158775 0.030395 11.00000 0.02549 0.03384 = 0.02336 -0.00219 -0.00330 -0.01235 C56 1 0.808064 0.200407 -0.085856 11.00000 0.04166 0.04909 = 0.02204 -0.00597 -0.00525 -0.01013 C57 1 0.812173 0.104158 -0.065942 11.00000 0.03584 0.05085 = 0.02801 -0.01244 -0.00672 -0.01109 C58 1 0.813325 0.262641 -0.158287 11.00000 0.08110 0.06779 = 0.02388 -0.00211 -0.00940 -0.01649 AFIX 137 H58A 2 0.818177 0.223342 -0.191574 11.00000 -1.50000 H58B 2 0.874748 0.283239 -0.168997 11.00000 -1.50000 H58C 2 0.750497 0.322097 -0.161722 11.00000 -1.50000 AFIX 0 C59 1 0.827129 0.033568 -0.111053 11.00000 0.06070 0.06163 = 0.04015 -0.02485 -0.01198 -0.01196 AFIX 137 H59A 2 0.842621 0.064864 -0.160096 11.00000 -1.50000 H59B 2 0.763441 0.017581 -0.104088 11.00000 -1.50000 H59C 2 0.885123 -0.027995 -0.098533 11.00000 -1.50000 AFIX 0 C60 1 0.787680 0.334171 -0.018286 11.00000 0.04613 0.03119 = 0.02755 0.00116 -0.00406 -0.01343 AFIX 13 H60 2 0.781515 0.330861 0.032652 11.00000 -1.20000 AFIX 0 C61 1 0.687786 0.411884 -0.041994 11.00000 0.05251 0.04043 = 0.04391 0.00187 -0.00973 -0.00771 AFIX 137 H61A 2 0.692834 0.421801 -0.092613 11.00000 -1.50000 H61B 2 0.676944 0.475239 -0.030011 11.00000 -1.50000 H61C 2 0.629057 0.388808 -0.018673 11.00000 -1.50000 AFIX 0 C62 1 0.885028 0.360263 -0.053439 11.00000 0.05370 0.04848 = 0.04343 -0.00415 0.00101 -0.02453 AFIX 137 H62A 2 0.946048 0.307236 -0.035287 11.00000 -1.50000 H62B 2 0.878902 0.423742 -0.043757 11.00000 -1.50000 H62C 2 0.892851 0.366622 -0.103918 11.00000 -1.50000 AFIX 0 C63 1 0.811511 -0.019707 0.054721 11.00000 0.03630 0.03375 = 0.03457 -0.00877 0.00019 -0.01583 AFIX 13 H63 2 0.787704 -0.006485 0.102958 11.00000 -1.20000 AFIX 0 C64 1 0.739526 -0.066154 0.043020 11.00000 0.08749 0.06339 = 0.09501 -0.00184 -0.03392 -0.04833 AFIX 137 H64A 2 0.670061 -0.015805 0.039771 11.00000 -1.50000 H64B 2 0.735223 -0.121991 0.082124 11.00000 -1.50000 H64C 2 0.766646 -0.090766 -0.000420 11.00000 -1.50000 AFIX 0 C65 1 0.923568 -0.088164 0.052683 11.00000 0.04601 0.04973 = 0.04265 0.00113 0.00343 -0.00559 AFIX 137 H65A 2 0.950874 -0.102314 0.005886 11.00000 -1.50000 H65B 2 0.927573 -0.150909 0.086790 11.00000 -1.50000 H65C 2 0.964936 -0.055669 0.064053 11.00000 -1.50000 AFIX 0 C1S 1 0.754852 0.324922 0.643055 11.00000 0.17110 0.21735 = 0.11763 -0.02360 0.02505 -0.11404 AFIX 33 H1S1 2 0.783434 0.305594 0.686735 11.00000 -1.50000 H1S2 2 0.687728 0.379122 0.646500 11.00000 -1.50000 H1S3 2 0.745053 0.267204 0.634559 11.00000 -1.50000 AFIX 0 C2S 1 0.818139 0.354830 0.592483 11.00000 0.26252 0.42878 = 0.12127 0.03125 0.00494 -0.22722 AFIX 23 H2S1 2 0.825167 0.404291 0.613741 11.00000 -1.20000 H2S2 2 0.880859 0.295559 0.602140 11.00000 -1.20000 AFIX 0 C3S 1 0.853224 0.388287 0.530257 11.00000 0.20647 0.20807 = 0.10833 -0.06272 0.02327 -0.13065 AFIX 23 H3S1 2 0.792006 0.449304 0.520874 11.00000 -1.20000 H3S2 2 0.843885 0.340767 0.508302 11.00000 -1.20000 AFIX 0 C4S 1 0.922267 0.417692 0.478381 11.00000 0.17152 0.27824 = 0.10403 -0.01471 -0.01601 -0.13703 AFIX 23 H4S1 2 0.937354 0.460347 0.501692 11.00000 -1.20000 H4S2 2 0.982061 0.354487 0.484190 11.00000 -1.20000 AFIX 0 C5S 1 0.952399 0.454938 0.415995 11.00000 0.27294 0.36902 = 0.10853 -0.06612 0.03842 -0.24217 AFIX 23 H5S1 2 0.891216 0.516535 0.408332 11.00000 -1.20000 H5S2 2 0.942677 0.409686 0.392136 11.00000 -1.20000 AFIX 0 C6S 1 1.024989 0.485665 0.366879 11.00000 0.12171 0.22923 = 0.10647 -0.04461 -0.00658 -0.07101 AFIX 33 H6S1 2 0.999836 0.511324 0.321638 11.00000 -1.50000 H6S2 2 1.037297 0.538718 0.380126 11.00000 -1.50000 H6S3 2 1.090101 0.429078 0.363507 11.00000 -1.50000 AFIX 0 C1T 1 0.370701 0.359188 0.589160 11.00000 0.08204 0.06546 = 0.10304 0.00857 0.01524 -0.02897 AFIX 33 H1T1 2 0.337897 0.348178 0.637929 11.00000 -1.50000 H1T2 2 0.317540 0.383649 0.558506 11.00000 -1.50000 H1T3 2 0.422582 0.296095 0.579081 11.00000 -1.50000 AFIX 0 C2T 1 0.421499 0.433171 0.577185 11.00000 0.10948 0.07864 = 0.06601 -0.01761 0.01610 -0.04803 AFIX 23 H2T1 2 0.472586 0.407928 0.610105 11.00000 -1.20000 H2T2 2 0.368027 0.495080 0.589625 11.00000 -1.20000 AFIX 0 C3T 1 0.476104 0.460718 0.506297 11.00000 0.07969 0.06047 = 0.05942 -0.01093 0.00116 -0.03360 AFIX 23 H3T1 2 0.425885 0.483154 0.473068 11.00000 -1.20000 H3T2 2 0.531746 0.399384 0.494672 11.00000 -1.20000 AFIX 0 HKLF 4 REM p-1 in P-1 REM R1 = 0.0523 for 12676 Fo > 4sig(Fo) and 0.0640 for all 15378 data REM 797 parameters refined using 0 restraints END WGHT 0.0739 1.7838 REM Highest difference peak 1.053, deepest hole -0.718, 1-sigma level 0.048 Q1 1 0.8419 0.3244 0.5911 11.00000 0.05 0.38 Q2 1 0.9231 0.4757 0.4164 11.00000 0.05 0.37 Q3 1 1.0754 0.1739 0.3260 11.00000 0.05 0.36 Q4 1 0.7453 0.1576 0.1297 11.00000 0.05 0.35 Q5 1 0.3266 0.5191 0.5001 11.00000 0.05 0.34 Q6 1 1.0675 0.0718 0.3095 11.00000 0.05 0.34 Q7 1 0.8930 0.1144 0.1903 11.00000 0.05 0.29 Q8 1 0.5618 0.4969 0.2730 11.00000 0.05 0.27 Q9 1 0.8351 0.4096 0.5205 11.00000 0.05 0.27 Q10 1 0.8242 0.1723 0.1092 11.00000 0.05 0.26 Q11 1 0.6671 0.1178 0.1876 11.00000 0.05 0.25 Q12 1 0.5335 0.0850 0.2576 11.00000 0.05 0.24 Q13 1 0.7193 0.4310 0.5485 11.00000 0.05 0.23 Q14 1 0.9879 0.0286 0.3714 11.00000 0.05 0.23 Q15 1 0.4580 0.1470 0.2606 11.00000 0.05 0.23 Q16 1 0.7595 0.0935 0.4325 11.00000 0.05 0.23 Q17 1 0.9179 0.3987 0.1552 11.00000 0.05 0.23 Q18 1 0.3398 0.2707 0.1758 11.00000 0.05 0.23 Q19 1 0.6044 -0.0120 0.2620 11.00000 0.05 0.22 Q20 1 0.8359 0.4004 0.1502 11.00000 0.05 0.22 ; _shelx_res_checksum 34665 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 P1 P 0.82725(3) 0.12982(3) 0.22559(2) 0.02742(10) Uani 1 1 d . . P2 P 0.68742(3) 0.17362(3) 0.17376(2) 0.02476(10) Uani 1 1 d . . O2 O 0.66136(9) 0.06671(9) 0.19060(6) 0.0280(2) Uani 1 1 d . . B1 B 0.81223(14) 0.23705(14) 0.26709(9) 0.0257(4) Uani 1 1 d . . N1 N 0.78410(11) 0.34387(10) 0.24641(7) 0.0272(3) Uani 1 1 d . . N2 N 0.82717(12) 0.21534(11) 0.33876(7) 0.0291(3) Uani 1 1 d . . B2 B 0.58433(15) 0.04284(14) 0.24026(9) 0.0255(4) Uani 1 1 d . . N3 N 0.48352(11) 0.10404(10) 0.26834(7) 0.0272(3) Uani 1 1 d . . N4 N 0.59331(12) -0.05832(10) 0.27508(8) 0.0305(3) Uani 1 1 d . . N5 N 0.79787(12) 0.23348(12) -0.02526(7) 0.0324(3) Uani 1 1 d . . N6 N 0.80346(12) 0.07908(11) 0.00653(7) 0.0313(3) Uani 1 1 d . . C1 C 0.87502(13) 0.16091(13) 0.12922(9) 0.0278(3) Uani 1 1 d . . O1 O 0.95783(10) 0.17485(12) 0.09997(7) 0.0422(3) Uani 1 1 d . . C2 C 0.79182(13) 0.15959(12) 0.10256(8) 0.0250(3) Uani 1 1 d . . C3 C 0.78153(16) 0.38073(14) 0.30396(10) 0.0366(4) Uani 1 1 d . . H3 H 0.764199 0.449296 0.304260 0.044 Uiso 1 1 calc R U C4 C 0.80722(16) 0.30460(15) 0.35844(10) 0.0383(4) Uani 1 1 d . . H4 H 0.811189 0.310572 0.403279 0.046 Uiso 1 1 calc R U C5 C 0.77863(13) 0.41148(12) 0.17914(9) 0.0273(3) Uani 1 1 d . . C6 C 0.87079(14) 0.42683(13) 0.14069(9) 0.0317(4) Uani 1 1 d . . C7 C 0.86270(15) 0.50283(14) 0.08103(10) 0.0369(4) Uani 1 1 d . . H7 H 0.923777 0.515283 0.054727 0.044 Uiso 1 1 calc R U C8 C 0.76754(16) 0.56038(14) 0.05941(10) 0.0379(4) Uani 1 1 d . . H8 H 0.763086 0.613589 0.019592 0.045 Uiso 1 1 calc R U C9 C 0.67885(15) 0.54042(14) 0.09581(10) 0.0355(4) Uani 1 1 d . . H9 H 0.614032 0.578531 0.079525 0.043 Uiso 1 1 calc R U C10 C 0.68259(14) 0.46534(13) 0.15607(9) 0.0299(4) Uani 1 1 d . . C11 C 0.97602(14) 0.36499(15) 0.16353(11) 0.0424(5) Uani 1 1 d . . H11 H 0.970222 0.300953 0.194584 0.051 Uiso 1 1 calc R U C12 C 1.06173(17) 0.33838(18) 0.10221(14) 0.0561(6) Uani 1 1 d . . H12A H 1.040576 0.306326 0.074518 0.084 Uiso 1 1 calc R U H12B H 1.126226 0.292336 0.119937 0.084 Uiso 1 1 calc R U H12C H 1.073305 0.399426 0.072879 0.084 Uiso 1 1 calc R U C13 C 1.00647(17) 0.4178(2) 0.20583(13) 0.0572(6) Uani 1 1 d . . H13A H 1.012375 0.481235 0.176735 0.086 Uiso 1 1 calc R U H13B H 1.073486 0.375198 0.221409 0.086 Uiso 1 1 calc R U H13C H 0.953117 0.431000 0.246524 0.086 Uiso 1 1 calc R U C14 C 0.58341(14) 0.44572(14) 0.19489(11) 0.0385(4) Uani 1 1 d . . H14 H 0.603400 0.379918 0.228509 0.046 Uiso 1 1 calc R U C15 C 0.52165(19) 0.4387(2) 0.14448(15) 0.0625(7) Uani 1 1 d . . H15A H 0.496346 0.504110 0.113366 0.094 Uiso 1 1 calc R U H15B H 0.462328 0.418572 0.171075 0.094 Uiso 1 1 calc R U H15C H 0.566759 0.389095 0.116751 0.094 Uiso 1 1 calc R U C16 C 0.5172(2) 0.5256(2) 0.23634(18) 0.0761(9) Uani 1 1 d . . H16A H 0.554268 0.521937 0.272984 0.114 Uiso 1 1 calc R U H16B H 0.451100 0.514709 0.257625 0.114 Uiso 1 1 calc R U H16C H 0.503569 0.591745 0.205154 0.114 Uiso 1 1 calc R U C17 C 0.87527(14) 0.11877(14) 0.38048(8) 0.0305(4) Uani 1 1 d . . C18 C 0.98372(15) 0.07452(17) 0.36710(9) 0.0400(4) Uani 1 1 d . . C19 C 1.02895(17) -0.02124(18) 0.40518(11) 0.0479(5) Uani 1 1 d . . H19 H 1.102175 -0.053230 0.396596 0.057 Uiso 1 1 calc R U C20 C 0.96949(19) -0.07048(16) 0.45509(12) 0.0488(5) Uani 1 1 d . . H20 H 1.001825 -0.135795 0.480536 0.059 Uiso 1 1 calc R U C21 C 0.86301(17) -0.02500(15) 0.46816(11) 0.0430(5) Uani 1 1 d . . H21 H 0.822723 -0.059467 0.502788 0.052 Uiso 1 1 calc R U C22 C 0.81359(15) 0.07061(14) 0.43141(9) 0.0339(4) Uani 1 1 d . . C23 C 1.05180(17) 0.1280(2) 0.31319(11) 0.0578(7) Uani 1 1 d . . H23 H 1.003220 0.193839 0.291771 0.069 Uiso 1 1 calc R U C24 C 1.1090(3) 0.0759(4) 0.25520(17) 0.1040(14) Uani 1 1 d . . H24A H 1.158385 0.010684 0.273425 0.156 Uiso 1 1 calc R U H24B H 1.146904 0.116309 0.220690 0.156 Uiso 1 1 calc R U H24C H 1.059530 0.066346 0.233095 0.156 Uiso 1 1 calc R U C25 C 1.1232(2) 0.1516(2) 0.34547(14) 0.0683(7) Uani 1 1 d . . H25A H 1.173638 0.089147 0.366534 0.102 Uiso 1 1 calc R U H25B H 1.082291 0.189693 0.381495 0.102 Uiso 1 1 calc R U H25C H 1.160234 0.191290 0.309416 0.102 Uiso 1 1 calc R U C26 C 0.69713(16) 0.12051(16) 0.44858(10) 0.0429(5) Uani 1 1 d . . H26 H 0.674843 0.180734 0.410570 0.051 Uiso 1 1 calc R U C27 C 0.6357(2) 0.0534(2) 0.45224(16) 0.0659(8) Uani 1 1 d . . H27A H 0.647248 0.036796 0.406597 0.099 Uiso 1 1 calc R U H27B H 0.561411 0.088428 0.465187 0.099 Uiso 1 1 calc R U H27C H 0.658957 -0.008226 0.487280 0.099 Uiso 1 1 calc R U C28 C 0.6723(2) 0.1567(2) 0.51691(13) 0.0643(7) Uani 1 1 d . . H28A H 0.691119 0.098857 0.555474 0.096 Uiso 1 1 calc R U H28B H 0.597767 0.194194 0.525677 0.096 Uiso 1 1 calc R U H28C H 0.712226 0.200029 0.513257 0.096 Uiso 1 1 calc R U C29 C 0.43869(15) 0.03919(13) 0.32014(9) 0.0344(4) Uani 1 1 d . . H29 H 0.372842 0.059742 0.348216 0.041 Uiso 1 1 calc R U C30 C 0.50258(15) -0.05502(14) 0.32366(10) 0.0371(4) Uani 1 1 d . . H30 H 0.488840 -0.111688 0.354489 0.045 Uiso 1 1 calc R U C31 C 0.41851(13) 0.20501(12) 0.24530(9) 0.0277(3) Uani 1 1 d . . C32 C 0.39153(13) 0.23602(13) 0.17756(9) 0.0300(4) Uani 1 1 d . . C33 C 0.31835(14) 0.33082(14) 0.16005(10) 0.0357(4) Uani 1 1 d . . H33 H 0.299073 0.353179 0.114660 0.043 Uiso 1 1 calc R U C34 C 0.27319(14) 0.39303(14) 0.20714(11) 0.0383(4) Uani 1 1 d . . H34 H 0.221995 0.456509 0.194476 0.046 Uiso 1 1 calc R U C35 C 0.30248(14) 0.36288(14) 0.27243(10) 0.0362(4) Uani 1 1 d . . H35 H 0.272385 0.406745 0.304099 0.043 Uiso 1 1 calc R U C36 C 0.37563(14) 0.26902(13) 0.29291(9) 0.0316(4) Uani 1 1 d . . C37 C 0.43711(15) 0.17087(15) 0.12339(10) 0.0352(4) Uani 1 1 d . . H37 H 0.490916 0.108340 0.143906 0.042 Uiso 1 1 calc R U C38 C 0.4917(2) 0.2220(2) 0.05696(11) 0.0534(6) Uani 1 1 d . . H38A H 0.440187 0.281649 0.034038 0.080 Uiso 1 1 calc R U H38B H 0.526142 0.175545 0.025252 0.080 Uiso 1 1 calc R U H38C H 0.543612 0.241430 0.069083 0.080 Uiso 1 1 calc R U C39 C 0.35526(19) 0.1401(2) 0.10597(15) 0.0568(6) Uani 1 1 d . . H39A H 0.323982 0.104138 0.148622 0.085 Uiso 1 1 calc R U H39B H 0.388244 0.096461 0.072293 0.085 Uiso 1 1 calc R U H39C H 0.301080 0.199916 0.085814 0.085 Uiso 1 1 calc R U C40 C 0.40720(16) 0.24049(14) 0.36480(10) 0.0377(4) Uani 1 1 d . . H40 H 0.458896 0.171068 0.370430 0.045 Uiso 1 1 calc R U C41 C 0.45998(19) 0.30964(17) 0.37222(12) 0.0490(5) Uani 1 1 d . . H41A H 0.521567 0.306058 0.336570 0.074 Uiso 1 1 calc R U H41B H 0.480970 0.288658 0.418637 0.074 Uiso 1 1 calc R U H41C H 0.411222 0.378537 0.366205 0.074 Uiso 1 1 calc R U C42 C 0.3146(2) 0.24010(19) 0.42284(11) 0.0550(6) Uani 1 1 d . . H42A H 0.265688 0.308551 0.421256 0.082 Uiso 1 1 calc R U H42B H 0.339433 0.213424 0.468200 0.082 Uiso 1 1 calc R U H42C H 0.279508 0.198060 0.416229 0.082 Uiso 1 1 calc R U C43 C 0.65981(15) -0.14865(13) 0.25194(9) 0.0330(4) Uani 1 1 d . . C44 C 0.61782(16) -0.19253(15) 0.21764(11) 0.0410(4) Uani 1 1 d . . C45 C 0.68202(19) -0.28195(16) 0.19772(13) 0.0514(5) Uani 1 1 d . . H45 H 0.654769 -0.314407 0.176177 0.062 Uiso 1 1 calc R U C46 C 0.7842(2) -0.32405(16) 0.20871(13) 0.0539(6) Uani 1 1 d . . H46 H 0.826792 -0.384902 0.194509 0.065 Uiso 1 1 calc R U C47 C 0.82518(18) -0.27836(15) 0.24030(12) 0.0470(5) Uani 1 1 d . . H47 H 0.896326 -0.307487 0.246576 0.056 Uiso 1 1 calc R U C48 C 0.76365(15) -0.18986(13) 0.26322(10) 0.0353(4) Uani 1 1 d . . C49 C 0.50667(18) -0.14531(17) 0.20091(13) 0.0482(5) Uani 1 1 d . . H49 H 0.480496 -0.074148 0.205916 0.058 Uiso 1 1 calc R U C50 C 0.5013(2) -0.1449(2) 0.12589(16) 0.0662(7) Uani 1 1 d . . H50A H 0.546386 -0.110071 0.093384 0.099 Uiso 1 1 calc R U H50B H 0.429430 -0.110422 0.116488 0.099 Uiso 1 1 calc R U H50C H 0.524660 -0.213912 0.119817 0.099 Uiso 1 1 calc R U C51 C 0.4332(2) -0.1972(2) 0.25167(17) 0.0675(7) Uani 1 1 d . . H51A H 0.362309 -0.162704 0.240331 0.101 Uiso 1 1 calc R U H51B H 0.434037 -0.194820 0.299553 0.101 Uiso 1 1 calc R U H51C H 0.456450 -0.267031 0.247431 0.101 Uiso 1 1 calc R U C52 C 0.80720(16) -0.14425(15) 0.30283(11) 0.0389(4) Uani 1 1 d . . H52 H 0.766700 -0.070993 0.295541 0.047 Uiso 1 1 calc R U C53 C 0.92169(18) -0.15573(19) 0.27819(15) 0.0571(6) Uani 1 1 d . . H53A H 0.964479 -0.226288 0.290635 0.086 Uiso 1 1 calc R U H53B H 0.941227 -0.115877 0.300633 0.086 Uiso 1 1 calc R U H53C H 0.932972 -0.132419 0.227447 0.086 Uiso 1 1 calc R U C54 C 0.7888(3) -0.1884(2) 0.38077(13) 0.0663(7) Uani 1 1 d . . H54A H 0.714079 -0.174807 0.396441 0.099 Uiso 1 1 calc R U H54B H 0.815198 -0.157853 0.406455 0.099 Uiso 1 1 calc R U H54C H 0.825349 -0.260807 0.389452 0.099 Uiso 1 1 calc R U C55 C 0.79542(13) 0.15877(13) 0.03039(8) 0.0277(3) Uani 1 1 d . . C56 C 0.80806(16) 0.20041(16) -0.08586(9) 0.0394(4) Uani 1 1 d . . C57 C 0.81217(15) 0.10416(16) -0.06594(10) 0.0381(4) Uani 1 1 d . . C58 C 0.8133(2) 0.2626(2) -0.15829(11) 0.0616(7) Uani 1 1 d . . H58A H 0.818177 0.223342 -0.191574 0.092 Uiso 1 1 calc R U H58B H 0.874748 0.283239 -0.168997 0.092 Uiso 1 1 calc R U H58C H 0.750497 0.322097 -0.161722 0.092 Uiso 1 1 calc R U C59 C 0.8271(2) 0.03357(19) -0.11105(12) 0.0529(6) Uani 1 1 d . . H59A H 0.842621 0.064864 -0.160096 0.079 Uiso 1 1 calc R U H59B H 0.763441 0.017581 -0.104088 0.079 Uiso 1 1 calc R U H59C H 0.885123 -0.027995 -0.098533 0.079 Uiso 1 1 calc R U C60 C 0.78768(16) 0.33417(14) -0.01829(9) 0.0367(4) Uani 1 1 d . . H60 H 0.781515 0.330861 0.032652 0.044 Uiso 1 1 calc R U C61 C 0.68779(18) 0.41188(16) -0.04199(12) 0.0499(5) Uani 1 1 d . . H61A H 0.692834 0.421801 -0.092613 0.075 Uiso 1 1 calc R U H61B H 0.676944 0.475239 -0.030011 0.075 Uiso 1 1 calc R U H61C H 0.629057 0.388808 -0.018673 0.075 Uiso 1 1 calc R U C62 C 0.88503(18) 0.36026(17) -0.05344(12) 0.0490(5) Uani 1 1 d . . H62A H 0.946048 0.307236 -0.035287 0.073 Uiso 1 1 calc R U H62B H 0.878902 0.423742 -0.043757 0.073 Uiso 1 1 calc R U H62C H 0.892851 0.366622 -0.103918 0.073 Uiso 1 1 calc R U C63 C 0.81151(15) -0.01971(14) 0.05472(10) 0.0343(4) Uani 1 1 d . . H63 H 0.787704 -0.006485 0.102958 0.041 Uiso 1 1 calc R U C64 C 0.7395(3) -0.0662(2) 0.04302(18) 0.0744(9) Uani 1 1 d . . H64A H 0.670061 -0.015805 0.039771 0.112 Uiso 1 1 calc R U H64B H 0.735223 -0.121991 0.082124 0.112 Uiso 1 1 calc R U H64C H 0.766646 -0.090766 -0.000420 0.112 Uiso 1 1 calc R U C65 C 0.92357(18) -0.08816(18) 0.05268(12) 0.0536(6) Uani 1 1 d . . H65A H 0.950874 -0.102314 0.005886 0.080 Uiso 1 1 calc R U H65B H 0.927573 -0.150909 0.086790 0.080 Uiso 1 1 calc R U H65C H 0.964936 -0.055669 0.064053 0.080 Uiso 1 1 calc R U C1S C 0.7549(5) 0.3249(5) 0.6431(3) 0.165(2) Uani 1 1 d . . H1S1 H 0.783434 0.305594 0.686735 0.247 Uiso 1 1 calc R U H1S2 H 0.687728 0.379122 0.646500 0.247 Uiso 1 1 calc R U H1S3 H 0.745053 0.267204 0.634559 0.247 Uiso 1 1 calc R U C2S C 0.8181(7) 0.3548(8) 0.5925(4) 0.262(6) Uani 1 1 d . . H2S1 H 0.825167 0.404291 0.613741 0.315 Uiso 1 1 calc R U H2S2 H 0.880859 0.295559 0.602140 0.315 Uiso 1 1 calc R U C3S C 0.8532(5) 0.3883(5) 0.5303(3) 0.158(2) Uani 1 1 d . . H3S1 H 0.792006 0.449304 0.520874 0.189 Uiso 1 1 calc R U H3S2 H 0.843885 0.340767 0.508302 0.189 Uiso 1 1 calc R U C4S C 0.9223(5) 0.4177(6) 0.4784(3) 0.172(3) Uani 1 1 d . . H4S1 H 0.937354 0.460347 0.501692 0.207 Uiso 1 1 calc R U H4S2 H 0.982061 0.354487 0.484190 0.207 Uiso 1 1 calc R U C5S C 0.9524(7) 0.4549(7) 0.4160(3) 0.218(4) Uani 1 1 d . . H5S1 H 0.891216 0.516535 0.408332 0.261 Uiso 1 1 calc R U H5S2 H 0.942677 0.409686 0.392136 0.261 Uiso 1 1 calc R U C6S C 1.0250(4) 0.4857(5) 0.3669(3) 0.149(2) Uani 1 1 d . . H6S1 H 0.999836 0.511324 0.321638 0.223 Uiso 1 1 calc R U H6S2 H 1.037297 0.538718 0.380126 0.223 Uiso 1 1 calc R U H6S3 H 1.090101 0.429078 0.363507 0.223 Uiso 1 1 calc R U C1T C 0.3707(3) 0.3592(2) 0.5892(2) 0.0932(12) Uani 1 1 d . . H1T1 H 0.337897 0.348178 0.637929 0.140 Uiso 1 1 calc R U H1T2 H 0.317540 0.383649 0.558506 0.140 Uiso 1 1 calc R U H1T3 H 0.422582 0.296095 0.579081 0.140 Uiso 1 1 calc R U C2T C 0.4215(3) 0.4332(3) 0.57719(17) 0.0845(10) Uani 1 1 d . . H2T1 H 0.472586 0.407928 0.610105 0.101 Uiso 1 1 calc R U H2T2 H 0.368027 0.495080 0.589625 0.101 Uiso 1 1 calc R U C3T C 0.4761(2) 0.4607(2) 0.50630(15) 0.0659(7) Uani 1 1 d . . H3T1 H 0.425885 0.483154 0.473068 0.079 Uiso 1 1 calc R U H3T2 H 0.531746 0.399384 0.494672 0.079 Uiso 1 1 calc R U loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0338(2) 0.0253(2) 0.0237(2) -0.00123(15) -0.00775(16) -0.01114(17) P2 0.0252(2) 0.0249(2) 0.02418(19) -0.00328(15) -0.00076(15) -0.01155(16) O2 0.0291(6) 0.0285(6) 0.0279(6) -0.0068(5) 0.0034(5) -0.0155(5) B1 0.0238(9) 0.0312(9) 0.0223(8) -0.0025(7) -0.0011(7) -0.0130(7) N1 0.0271(7) 0.0292(7) 0.0251(7) -0.0050(5) 0.0008(5) -0.0126(6) N2 0.0333(8) 0.0330(7) 0.0222(6) -0.0042(6) -0.0004(6) -0.0157(6) B2 0.0277(9) 0.0267(9) 0.0227(8) -0.0049(7) -0.0006(7) -0.0118(7) N3 0.0266(7) 0.0244(7) 0.0262(7) -0.0021(5) 0.0029(5) -0.0101(6) N4 0.0304(7) 0.0245(7) 0.0320(7) -0.0056(6) 0.0049(6) -0.0103(6) N5 0.0362(8) 0.0364(8) 0.0217(7) -0.0020(6) -0.0041(6) -0.0122(7) N6 0.0309(8) 0.0375(8) 0.0273(7) -0.0078(6) -0.0035(6) -0.0132(6) C1 0.0255(8) 0.0311(8) 0.0269(8) -0.0083(6) -0.0004(6) -0.0101(7) O1 0.0303(7) 0.0640(9) 0.0404(7) -0.0203(7) 0.0052(6) -0.0241(7) C2 0.0261(8) 0.0276(8) 0.0210(7) -0.0018(6) -0.0014(6) -0.0122(6) C3 0.0456(11) 0.0342(9) 0.0320(9) -0.0122(7) 0.0044(8) -0.0179(8) C4 0.0497(11) 0.0427(10) 0.0271(8) -0.0125(8) 0.0027(8) -0.0219(9) C5 0.0285(8) 0.0245(8) 0.0283(8) -0.0042(6) 0.0010(6) -0.0123(7) C6 0.0284(9) 0.0289(8) 0.0357(9) -0.0036(7) 0.0006(7) -0.0127(7) C7 0.0347(10) 0.0363(9) 0.0360(9) -0.0017(8) 0.0050(7) -0.0181(8) C8 0.0435(11) 0.0341(9) 0.0324(9) 0.0024(7) -0.0026(8) -0.0175(8) C9 0.0346(10) 0.0329(9) 0.0374(9) -0.0008(7) -0.0083(8) -0.0125(8) C10 0.0290(9) 0.0277(8) 0.0338(9) -0.0050(7) -0.0011(7) -0.0134(7) C11 0.0254(9) 0.0362(10) 0.0534(12) 0.0067(9) 0.0006(8) -0.0123(8) C12 0.0307(11) 0.0520(13) 0.0765(17) -0.0140(12) 0.0089(10) -0.0138(10) C13 0.0326(11) 0.0810(17) 0.0525(13) -0.0042(12) -0.0118(10) -0.0167(11) C14 0.0256(9) 0.0315(9) 0.0523(11) -0.0006(8) -0.0006(8) -0.0119(7) C15 0.0449(13) 0.0583(14) 0.0849(18) 0.0207(13) -0.0304(13) -0.0310(11) C16 0.0554(15) 0.0567(15) 0.102(2) -0.0281(15) 0.0386(15) -0.0256(13) C17 0.0336(9) 0.0378(9) 0.0211(7) -0.0052(7) -0.0049(7) -0.0133(8) C18 0.0344(10) 0.0610(13) 0.0221(8) -0.0076(8) -0.0062(7) -0.0129(9) C19 0.0369(11) 0.0612(13) 0.0357(10) -0.0137(9) -0.0119(8) 0.0004(10) C20 0.0566(13) 0.0398(11) 0.0458(11) -0.0050(9) -0.0245(10) -0.0045(10) C21 0.0505(12) 0.0406(11) 0.0377(10) 0.0040(8) -0.0151(9) -0.0186(9) C22 0.0375(10) 0.0373(9) 0.0266(8) -0.0014(7) -0.0071(7) -0.0146(8) C23 0.0305(10) 0.099(2) 0.0279(9) 0.0046(11) -0.0033(8) -0.0180(12) C24 0.087(2) 0.189(4) 0.0646(19) -0.067(2) 0.0355(17) -0.077(3) C25 0.0796(19) 0.0758(18) 0.0548(15) -0.0075(13) 0.0053(13) -0.0454(16) C26 0.0364(10) 0.0453(11) 0.0354(10) 0.0102(8) -0.0025(8) -0.0160(9) C27 0.0459(13) 0.0693(16) 0.0784(18) 0.0146(14) -0.0190(13) -0.0305(13) C28 0.0525(14) 0.0733(17) 0.0482(13) -0.0109(12) 0.0128(11) -0.0140(13) C29 0.0328(9) 0.0320(9) 0.0322(9) -0.0029(7) 0.0090(7) -0.0151(8) C30 0.0392(10) 0.0287(9) 0.0363(9) -0.0024(7) 0.0095(8) -0.0157(8) C31 0.0230(8) 0.0266(8) 0.0299(8) -0.0024(6) 0.0006(6) -0.0098(6) C32 0.0239(8) 0.0339(9) 0.0323(8) -0.0031(7) -0.0018(7) -0.0140(7) C33 0.0294(9) 0.0369(10) 0.0399(10) 0.0015(8) -0.0102(8) -0.0139(8) C34 0.0270(9) 0.0298(9) 0.0533(11) -0.0008(8) -0.0092(8) -0.0080(7) C35 0.0302(9) 0.0289(9) 0.0443(10) -0.0082(8) 0.0011(8) -0.0080(7) C36 0.0288(9) 0.0293(8) 0.0321(9) -0.0043(7) 0.0019(7) -0.0100(7) C37 0.0307(9) 0.0428(10) 0.0326(9) -0.0078(8) -0.0066(7) -0.0119(8) C38 0.0555(14) 0.0697(15) 0.0334(10) -0.0084(10) -0.0007(9) -0.0246(12) C39 0.0429(12) 0.0702(16) 0.0720(16) -0.0359(13) -0.0066(11) -0.0214(11) C40 0.0445(11) 0.0321(9) 0.0303(9) -0.0069(7) -0.0012(8) -0.0083(8) C41 0.0573(14) 0.0472(12) 0.0446(11) -0.0092(9) -0.0126(10) -0.0173(10) C42 0.0628(15) 0.0596(14) 0.0356(11) -0.0101(10) 0.0092(10) -0.0230(12) C43 0.0363(9) 0.0241(8) 0.0341(9) -0.0050(7) 0.0033(7) -0.0112(7) C44 0.0426(11) 0.0323(9) 0.0485(11) -0.0109(8) 0.0002(9) -0.0152(8) C45 0.0582(14) 0.0373(11) 0.0629(14) -0.0213(10) -0.0046(11) -0.0157(10) C46 0.0590(14) 0.0335(10) 0.0633(14) -0.0219(10) -0.0006(11) -0.0061(10) C47 0.0414(11) 0.0347(10) 0.0538(12) -0.0116(9) -0.0013(9) -0.0027(9) C48 0.0361(10) 0.0280(9) 0.0355(9) -0.0056(7) 0.0022(7) -0.0093(7) C49 0.0456(12) 0.0422(11) 0.0625(14) -0.0166(10) -0.0057(10) -0.0185(10) C50 0.0571(15) 0.0779(18) 0.0773(18) -0.0287(15) -0.0175(13) -0.0244(14) C51 0.0543(15) 0.0569(15) 0.097(2) -0.0232(15) 0.0028(14) -0.0287(12) C52 0.0372(10) 0.0324(9) 0.0433(10) -0.0065(8) -0.0039(8) -0.0099(8) C53 0.0393(12) 0.0512(13) 0.0780(17) -0.0144(12) -0.0068(11) -0.0127(10) C54 0.094(2) 0.0719(17) 0.0444(13) -0.0086(12) -0.0094(13) -0.0432(16) C55 0.0255(8) 0.0338(9) 0.0234(8) -0.0022(6) -0.0033(6) -0.0124(7) C56 0.0417(11) 0.0491(11) 0.0220(8) -0.0060(8) -0.0052(7) -0.0101(9) C57 0.0358(10) 0.0509(11) 0.0280(9) -0.0124(8) -0.0067(7) -0.0111(9) C58 0.0811(18) 0.0678(16) 0.0239(10) -0.0021(10) -0.0094(10) -0.0165(14) C59 0.0607(14) 0.0616(14) 0.0402(11) -0.0249(10) -0.0120(10) -0.0120(12) C60 0.0461(11) 0.0312(9) 0.0275(8) 0.0012(7) -0.0041(8) -0.0134(8) C61 0.0525(13) 0.0404(11) 0.0439(11) 0.0019(9) -0.0097(10) -0.0077(10) C62 0.0537(13) 0.0485(12) 0.0434(11) -0.0041(9) 0.0010(10) -0.0245(11) C63 0.0363(10) 0.0337(9) 0.0346(9) -0.0088(7) 0.0002(7) -0.0158(8) C64 0.087(2) 0.0634(17) 0.095(2) -0.0018(15) -0.0339(18) -0.0483(16) C65 0.0460(12) 0.0497(12) 0.0426(11) 0.0011(10) 0.0034(10) -0.0056(10) C1S 0.171(6) 0.217(7) 0.118(4) -0.024(4) 0.025(4) -0.114(5) C2S 0.263(10) 0.429(16) 0.121(5) 0.031(7) 0.005(6) -0.227(11) C3S 0.206(6) 0.208(6) 0.108(4) -0.063(4) 0.023(4) -0.131(6) C4S 0.172(6) 0.278(9) 0.104(4) -0.015(5) -0.016(4) -0.137(6) C5S 0.273(9) 0.369(12) 0.109(4) -0.066(6) 0.038(5) -0.242(9) C6S 0.122(4) 0.229(7) 0.106(4) -0.045(4) -0.007(3) -0.071(4) C1T 0.082(2) 0.0655(19) 0.103(3) 0.0086(18) 0.0152(19) -0.0290(17) C2T 0.109(3) 0.079(2) 0.0660(18) -0.0176(16) 0.0161(18) -0.048(2) C3T 0.0797(19) 0.0605(15) 0.0594(15) -0.0109(12) 0.0012(14) -0.0336(14) 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' 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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 C1 P1 B1 109.32(8) . . C1 P1 P2 75.04(5) . . B1 P1 P2 108.05(6) . . O2 P2 C2 103.38(7) . . O2 P2 P1 103.69(5) . . C2 P2 P1 77.15(5) . . B2 O2 P2 125.73(11) . . N1 B1 N2 104.00(15) . . N1 B1 P1 136.72(13) . . N2 B1 P1 119.23(13) . . C3 N1 B1 108.25(14) . . C3 N1 C5 118.02(14) . . B1 N1 C5 132.51(14) . . C4 N2 C17 122.93(15) . . C4 N2 B1 109.02(15) . . C17 N2 B1 126.89(15) . . O2 B2 N4 122.55(16) . . O2 B2 N3 131.70(15) . . N4 B2 N3 105.75(14) . . C29 N3 C31 118.43(14) . . C29 N3 B2 106.95(14) . . C31 N3 B2 133.17(14) . . C30 N4 B2 107.37(14) . . C30 N4 C43 121.67(14) . . B2 N4 C43 127.87(14) . . C55 N5 C56 109.29(16) . . C55 N5 C60 122.07(15) . . C56 N5 C60 128.62(15) . . C55 N6 C57 109.26(15) . . C55 N6 C63 121.16(14) . . C57 N6 C63 129.32(16) . . O1 C1 C2 131.76(16) . . O1 C1 P1 128.70(13) . . C2 C1 P1 99.50(11) . . C1 C2 C55 123.93(15) . . C1 C2 P2 103.95(11) . . C55 C2 P2 131.74(12) . . C4 C3 N1 109.70(16) . . C4 C3 H3 125.1 . . N1 C3 H3 125.1 . . C3 C4 N2 109.02(16) . . C3 C4 H4 125.5 . . N2 C4 H4 125.5 . . C10 C5 C6 121.53(15) . . C10 C5 N1 120.00(14) . . C6 C5 N1 118.30(15) . . C7 C6 C5 117.97(16) . . C7 C6 C11 120.21(16) . . C5 C6 C11 121.80(15) . . C8 C7 C6 121.19(17) . . C8 C7 H7 119.4 . . C6 C7 H7 119.4 . . C7 C8 C9 119.82(17) . . C7 C8 H8 120.1 . . C9 C8 H8 120.1 . . C8 C9 C10 121.25(17) . . C8 C9 H9 119.4 . . C10 C9 H9 119.4 . . C5 C10 C9 118.05(16) . . C5 C10 C14 122.15(15) . . C9 C10 C14 119.80(16) . . C6 C11 C13 111.14(18) . . C6 C11 C12 112.62(19) . . C13 C11 C12 110.04(18) . . C6 C11 H11 107.6 . . C13 C11 H11 107.6 . . C12 C11 H11 107.6 . . C11 C12 H12A 109.5 . . C11 C12 H12B 109.5 . . H12A C12 H12B 109.5 . . C11 C12 H12C 109.5 . . H12A C12 H12C 109.5 . . H12B C12 H12C 109.5 . . C11 C13 H13A 109.5 . . C11 C13 H13B 109.5 . . H13A C13 H13B 109.5 . . C11 C13 H13C 109.5 . . H13A C13 H13C 109.5 . . H13B C13 H13C 109.5 . . C10 C14 C16 110.95(17) . . C10 C14 C15 110.89(18) . . C16 C14 C15 110.9(2) . . C10 C14 H14 108.0 . . C16 C14 H14 108.0 . . C15 C14 H14 108.0 . . C14 C15 H15A 109.5 . . C14 C15 H15B 109.5 . . H15A C15 H15B 109.5 . . C14 C15 H15C 109.5 . . H15A C15 H15C 109.5 . . H15B C15 H15C 109.5 . . C14 C16 H16A 109.5 . . C14 C16 H16B 109.5 . . H16A C16 H16B 109.5 . . C14 C16 H16C 109.5 . . H16A C16 H16C 109.5 . . H16B C16 H16C 109.5 . . C22 C17 C18 121.94(17) . . C22 C17 N2 119.83(16) . . C18 C17 N2 118.21(16) . . C19 C18 C17 117.77(19) . . C19 C18 C23 120.03(19) . . C17 C18 C23 122.20(19) . . C20 C19 C18 121.2(2) . . C20 C19 H19 119.4 . . C18 C19 H19 119.4 . . C19 C20 C21 120.1(2) . . C19 C20 H20 120.0 . . C21 C20 H20 120.0 . . C20 C21 C22 121.1(2) . . C20 C21 H21 119.4 . . C22 C21 H21 119.4 . . C21 C22 C17 117.85(18) . . C21 C22 C26 120.12(17) . . C17 C22 C26 121.99(16) . . C24 C23 C25 111.7(2) . . C24 C23 C18 113.4(3) . . C25 C23 C18 112.69(18) . . C24 C23 H23 106.1 . . C25 C23 H23 106.1 . . C18 C23 H23 106.1 . . C23 C24 H24A 109.5 . . C23 C24 H24B 109.5 . . H24A C24 H24B 109.5 . . C23 C24 H24C 109.5 . . H24A C24 H24C 109.5 . . H24B C24 H24C 109.5 . . C23 C25 H25A 109.5 . . C23 C25 H25B 109.5 . . H25A C25 H25B 109.5 . . C23 C25 H25C 109.5 . . H25A C25 H25C 109.5 . . H25B C25 H25C 109.5 . . C22 C26 C27 113.0(2) . . C22 C26 C28 109.68(18) . . C27 C26 C28 110.9(2) . . C22 C26 H26 107.7 . . C27 C26 H26 107.7 . . C28 C26 H26 107.7 . . C26 C27 H27A 109.5 . . C26 C27 H27B 109.5 . . H27A C27 H27B 109.5 . . C26 C27 H27C 109.5 . . H27A C27 H27C 109.5 . . H27B C27 H27C 109.5 . . C26 C28 H28A 109.5 . . C26 C28 H28B 109.5 . . H28A C28 H28B 109.5 . . C26 C28 H28C 109.5 . . H28A C28 H28C 109.5 . . H28B C28 H28C 109.5 . . C30 C29 N3 109.82(15) . . C30 C29 H29 125.1 . . N3 C29 H29 125.1 . . C29 C30 N4 110.04(15) . . C29 C30 H30 125.0 . . N4 C30 H30 125.0 . . C36 C31 C32 121.04(16) . . C36 C31 N3 119.08(15) . . C32 C31 N3 119.66(15) . . C33 C32 C31 117.86(17) . . C33 C32 C37 118.79(16) . . C31 C32 C37 123.35(16) . . C34 C33 C32 121.58(18) . . C34 C33 H33 119.2 . . C32 C33 H33 119.2 . . C35 C34 C33 119.91(17) . . C35 C34 H34 120.0 . . C33 C34 H34 120.0 . . C34 C35 C36 121.16(18) . . C34 C35 H35 119.4 . . C36 C35 H35 119.4 . . C35 C36 C31 118.39(17) . . C35 C36 C40 119.05(17) . . C31 C36 C40 122.55(16) . . C32 C37 C39 112.15(16) . . C32 C37 C38 111.59(17) . . C39 C37 C38 110.55(18) . . C32 C37 H37 107.4 . . C39 C37 H37 107.4 . . C38 C37 H37 107.4 . . C37 C38 H38A 109.5 . . C37 C38 H38B 109.5 . . H38A C38 H38B 109.5 . . C37 C38 H38C 109.5 . . H38A C38 H38C 109.5 . . H38B C38 H38C 109.5 . . C37 C39 H39A 109.5 . . C37 C39 H39B 109.5 . . H39A C39 H39B 109.5 . . C37 C39 H39C 109.5 . . H39A C39 H39C 109.5 . . H39B C39 H39C 109.5 . . C36 C40 C41 111.16(16) . . C36 C40 C42 111.96(18) . . C41 C40 C42 110.27(18) . . C36 C40 H40 107.8 . . C41 C40 H40 107.8 . . C42 C40 H40 107.8 . . C40 C41 H41A 109.5 . . C40 C41 H41B 109.5 . . H41A C41 H41B 109.5 . . C40 C41 H41C 109.5 . . H41A C41 H41C 109.5 . . H41B C41 H41C 109.5 . . C40 C42 H42A 109.5 . . C40 C42 H42B 109.5 . . H42A C42 H42B 109.5 . . C40 C42 H42C 109.5 . . H42A C42 H42C 109.5 . . H42B C42 H42C 109.5 . . C48 C43 C44 121.95(17) . . C48 C43 N4 119.64(17) . . C44 C43 N4 118.40(17) . . C45 C44 C43 117.8(2) . . C45 C44 C49 119.5(2) . . C43 C44 C49 122.72(18) . . C46 C45 C44 121.1(2) . . C46 C45 H45 119.5 . . C44 C45 H45 119.5 . . C45 C46 C47 120.4(2) . . C45 C46 H46 119.8 . . C47 C46 H46 119.8 . . C46 C47 C48 121.1(2) . . C46 C47 H47 119.4 . . C48 C47 H47 119.4 . . C43 C48 C47 117.58(19) . . C43 C48 C52 121.57(16) . . C47 C48 C52 120.74(18) . . C44 C49 C50 112.2(2) . . C44 C49 C51 112.2(2) . . C50 C49 C51 109.3(2) . . C44 C49 H49 107.6 . . C50 C49 H49 107.6 . . C51 C49 H49 107.6 . . C49 C50 H50A 109.5 . . C49 C50 H50B 109.5 . . H50A C50 H50B 109.5 . . C49 C50 H50C 109.5 . . H50A C50 H50C 109.5 . . H50B C50 H50C 109.5 . . C49 C51 H51A 109.5 . . C49 C51 H51B 109.5 . . H51A C51 H51B 109.5 . . C49 C51 H51C 109.5 . . H51A C51 H51C 109.5 . . H51B C51 H51C 109.5 . . C48 C52 C53 114.13(18) . . C48 C52 C54 109.36(17) . . C53 C52 C54 110.7(2) . . C48 C52 H52 107.4 . . C53 C52 H52 107.4 . . C54 C52 H52 107.4 . . C52 C53 H53A 109.5 . . C52 C53 H53B 109.5 . . H53A C53 H53B 109.5 . . C52 C53 H53C 109.5 . . H53A C53 H53C 109.5 . . H53B C53 H53C 109.5 . . C52 C54 H54A 109.5 . . C52 C54 H54B 109.5 . . H54A C54 H54B 109.5 . . C52 C54 H54C 109.5 . . H54A C54 H54C 109.5 . . H54B C54 H54C 109.5 . . N5 C55 N6 107.29(15) . . N5 C55 C2 127.16(16) . . N6 C55 C2 125.44(15) . . C57 C56 N5 107.05(16) . . C57 C56 C58 128.0(2) . . N5 C56 C58 125.0(2) . . C56 C57 N6 107.10(17) . . C56 C57 C59 128.21(19) . . N6 C57 C59 124.66(19) . . C56 C58 H58A 109.5 . . C56 C58 H58B 109.5 . . H58A C58 H58B 109.5 . . C56 C58 H58C 109.5 . . H58A C58 H58C 109.5 . . H58B C58 H58C 109.5 . . C57 C59 H59A 109.5 . . C57 C59 H59B 109.5 . . H59A C59 H59B 109.5 . . C57 C59 H59C 109.5 . . H59A C59 H59C 109.5 . . H59B C59 H59C 109.5 . . N5 C60 C61 110.82(17) . . N5 C60 C62 111.46(17) . . C61 C60 C62 114.11(17) . . N5 C60 H60 106.7 . . C61 C60 H60 106.7 . . C62 C60 H60 106.7 . . C60 C61 H61A 109.5 . . C60 C61 H61B 109.5 . . H61A C61 H61B 109.5 . . C60 C61 H61C 109.5 . . H61A C61 H61C 109.5 . . H61B C61 H61C 109.5 . . C60 C62 H62A 109.5 . . C60 C62 H62B 109.5 . . H62A C62 H62B 109.5 . . C60 C62 H62C 109.5 . . H62A C62 H62C 109.5 . . H62B C62 H62C 109.5 . . N6 C63 C65 110.79(15) . . N6 C63 C64 112.52(18) . . C65 C63 C64 113.6(2) . . N6 C63 H63 106.5 . . C65 C63 H63 106.5 . . C64 C63 H63 106.5 . . C63 C64 H64A 109.5 . . C63 C64 H64B 109.5 . . H64A C64 H64B 109.5 . . C63 C64 H64C 109.5 . . H64A C64 H64C 109.5 . . H64B C64 H64C 109.5 . . C63 C65 H65A 109.5 . . C63 C65 H65B 109.5 . . H65A C65 H65B 109.5 . . C63 C65 H65C 109.5 . . H65A C65 H65C 109.5 . . H65B C65 H65C 109.5 . . C2S C1S H1S1 109.5 . . C2S C1S H1S2 109.5 . . H1S1 C1S H1S2 109.5 . . C2S C1S H1S3 109.5 . . H1S1 C1S H1S3 109.5 . . H1S2 C1S H1S3 109.5 . . C3S C2S C1S 158.0(9) . . C3S C2S H2S1 96.8 . . C1S C2S H2S1 96.8 . . C3S C2S H2S2 96.8 . . C1S C2S H2S2 96.8 . . H2S1 C2S H2S2 103.5 . . C2S C3S C4S 156.3(8) . . C2S C3S H3S1 97.3 . . C4S C3S H3S1 97.3 . . C2S C3S H3S2 97.3 . . C4S C3S H3S2 97.3 . . H3S1 C3S H3S2 103.6 . . C5S C4S C3S 154.0(7) . . C5S C4S H4S1 98.0 . . C3S C4S H4S1 98.0 . . C5S C4S H4S2 98.0 . . C3S C4S H4S2 98.0 . . H4S1 C4S H4S2 103.7 . . C4S C5S C6S 150.5(8) . . C4S C5S H5S1 99.0 . . C6S C5S H5S1 99.0 . . C4S C5S H5S2 99.0 . . C6S C5S H5S2 99.0 . . H5S1 C5S H5S2 103.9 . . C5S C6S H6S1 109.5 . . C5S C6S H6S2 109.5 . . H6S1 C6S H6S2 109.5 . . C5S C6S H6S3 109.5 . . H6S1 C6S H6S3 109.5 . . H6S2 C6S H6S3 109.5 . . C2T C1T H1T1 109.5 . . C2T C1T H1T2 109.5 . . H1T1 C1T H1T2 109.5 . . C2T C1T H1T3 109.5 . . H1T1 C1T H1T3 109.5 . . H1T2 C1T H1T3 109.5 . . C1T C2T C3T 118.1(3) . . C1T C2T H2T1 107.8 . . C3T C2T H2T1 107.8 . . C1T C2T H2T2 107.8 . . C3T C2T H2T2 107.8 . . H2T1 C2T H2T2 107.1 . . C2T C3T C3T 117.8(3) . 2_666 C2T C3T H3T1 107.8 . . C3T C3T H3T1 107.8 2_666 . C2T C3T H3T2 107.8 . . C3T C3T H3T2 107.8 2_666 . H3T1 C3T H3T2 107.2 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 P1 C1 1.8874(17) . P1 B1 1.915(2) . P1 P2 2.2369(6) . P2 O2 1.6835(12) . P2 C2 1.7872(16) . O2 B2 1.371(2) . B1 N1 1.436(2) . B1 N2 1.440(2) . N1 C3 1.403(2) . N1 C5 1.443(2) . N2 C4 1.392(2) . N2 C17 1.438(2) . B2 N4 1.435(2) . B2 N3 1.440(2) . N3 C29 1.414(2) . N3 C31 1.433(2) . N4 C30 1.406(2) . N4 C43 1.437(2) . N5 C55 1.342(2) . N5 C56 1.398(2) . N5 C60 1.485(2) . N6 C55 1.351(2) . N6 C57 1.393(2) . N6 C63 1.492(2) . C1 O1 1.239(2) . C1 C2 1.407(2) . C2 C55 1.449(2) . C3 C4 1.340(3) . C3 H3 0.9500 . C4 H4 0.9500 . C5 C10 1.394(2) . C5 C6 1.407(2) . C6 C7 1.392(2) . C6 C11 1.514(3) . C7 C8 1.380(3) . C7 H7 0.9500 . C8 C9 1.381(3) . C8 H8 0.9500 . C9 C10 1.396(2) . C9 H9 0.9500 . C10 C14 1.518(2) . C11 C13 1.525(3) . C11 C12 1.530(3) . C11 H11 1.0000 . C12 H12A 0.9800 . C12 H12B 0.9800 . C12 H12C 0.9800 . C13 H13A 0.9800 . C13 H13B 0.9800 . C13 H13C 0.9800 . C14 C16 1.518(3) . C14 C15 1.532(3) . C14 H14 1.0000 . C15 H15A 0.9800 . C15 H15B 0.9800 . C15 H15C 0.9800 . C16 H16A 0.9800 . C16 H16B 0.9800 . C16 H16C 0.9800 . C17 C22 1.398(2) . C17 C18 1.402(3) . C18 C19 1.392(3) . C18 C23 1.526(3) . C19 C20 1.378(3) . C19 H19 0.9500 . C20 C21 1.380(3) . C20 H20 0.9500 . C21 C22 1.394(3) . C21 H21 0.9500 . C22 C26 1.515(3) . C23 C24 1.481(4) . C23 C25 1.503(4) . C23 H23 1.0000 . C24 H24A 0.9800 . C24 H24B 0.9800 . C24 H24C 0.9800 . C25 H25A 0.9800 . C25 H25B 0.9800 . C25 H25C 0.9800 . C26 C27 1.523(3) . C26 C28 1.533(3) . C26 H26 1.0000 . C27 H27A 0.9800 . C27 H27B 0.9800 . C27 H27C 0.9800 . C28 H28A 0.9800 . C28 H28B 0.9800 . C28 H28C 0.9800 . C29 C30 1.332(3) . C29 H29 0.9500 . C30 H30 0.9500 . C31 C36 1.407(2) . C31 C32 1.410(2) . C32 C33 1.394(3) . C32 C37 1.523(3) . C33 C34 1.382(3) . C33 H33 0.9500 . C34 C35 1.376(3) . C34 H34 0.9500 . C35 C36 1.396(2) . C35 H35 0.9500 . C36 C40 1.517(3) . C37 C39 1.529(3) . C37 C38 1.532(3) . C37 H37 1.0000 . C38 H38A 0.9800 . C38 H38B 0.9800 . C38 H38C 0.9800 . C39 H39A 0.9800 . C39 H39B 0.9800 . C39 H39C 0.9800 . C40 C41 1.529(3) . C40 C42 1.531(3) . C40 H40 1.0000 . C41 H41A 0.9800 . C41 H41B 0.9800 . C41 H41C 0.9800 . C42 H42A 0.9800 . C42 H42B 0.9800 . C42 H42C 0.9800 . C43 C48 1.398(3) . C43 C44 1.410(3) . C44 C45 1.393(3) . C44 C49 1.526(3) . C45 C46 1.375(4) . C45 H45 0.9500 . C46 C47 1.382(3) . C46 H46 0.9500 . C47 C48 1.400(3) . C47 H47 0.9500 . C48 C52 1.523(3) . C49 C50 1.532(4) . C49 C51 1.539(3) . C49 H49 1.0000 . C50 H50A 0.9800 . C50 H50B 0.9800 . C50 H50C 0.9800 . C51 H51A 0.9800 . C51 H51B 0.9800 . C51 H51C 0.9800 . C52 C53 1.525(3) . C52 C54 1.527(3) . C52 H52 1.0000 . C53 H53A 0.9800 . C53 H53B 0.9800 . C53 H53C 0.9800 . C54 H54A 0.9800 . C54 H54B 0.9800 . C54 H54C 0.9800 . C56 C57 1.349(3) . C56 C58 1.497(3) . C57 C59 1.496(3) . C58 H58A 0.9800 . C58 H58B 0.9800 . C58 H58C 0.9800 . C59 H59A 0.9800 . C59 H59B 0.9800 . C59 H59C 0.9800 . C60 C61 1.517(3) . C60 C62 1.521(3) . C60 H60 1.0000 . C61 H61A 0.9800 . C61 H61B 0.9800 . C61 H61C 0.9800 . C62 H62A 0.9800 . C62 H62B 0.9800 . C62 H62C 0.9800 . C63 C65 1.511(3) . C63 C64 1.512(3) . C63 H63 1.0000 . C64 H64A 0.9800 . C64 H64B 0.9800 . C64 H64C 0.9800 . C65 H65A 0.9800 . C65 H65B 0.9800 . C65 H65C 0.9800 . C1S C2S 1.283(7) . C1S H1S1 0.9800 . C1S H1S2 0.9800 . C1S H1S3 0.9800 . C2S C3S 1.269(7) . C2S H2S1 0.9900 . C2S H2S2 0.9900 . C3S C4S 1.346(7) . C3S H3S1 0.9900 . C3S H3S2 0.9900 . C4S C5S 1.267(7) . C4S H4S1 0.9900 . C4S H4S2 0.9900 . C5S C6S 1.361(7) . C5S H5S1 0.9900 . C5S H5S2 0.9900 . C6S H6S1 0.9800 . C6S H6S2 0.9800 . C6S H6S3 0.9800 . C1T C2T 1.461(5) . C1T H1T1 0.9800 . C1T H1T2 0.9800 . C1T H1T3 0.9800 . C2T C3T 1.481(4) . C2T H2T1 0.9900 . C2T H2T2 0.9900 . C3T C3T 1.489(5) 2_666 C3T H3T1 0.9900 . C3T H3T2 0.9900 .