#------------------------------------------------------------------------------ #$Date: 2019-12-21 03:44:49 +0200 (Sat, 21 Dec 2019) $ #$Revision: 245463 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/56/7125674.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_7125674 loop_ _publ_author_name 'Livshits-Kritsman, Yulia' 'Tumanskii, Boris L.' 'Menard, Gabriel' 'Dobrovetsky, Roman' _publ_section_title ; Isolable Cyclic (Alkyl)(amino)carbene−Phosphonyl Radical Adducts ; _journal_name_full 'Chemical Communications' _journal_paper_doi 10.1039/C9CC09244G _journal_year 2020 _chemical_formula_moiety 'C24 B F20, C32 H41 N O P ' _chemical_formula_sum 'C56 H41 B F20 N O P' _chemical_formula_weight 1165.68 _space_group_crystal_system orthorhombic _space_group_IT_number 32 _space_group_name_Hall 'P 2 -2ab' _space_group_name_H-M_alt 'P b a 2' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2018/1 _audit_update_record ; 2019-11-21 deposited with the CCDC. 2019-12-20 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 35.439(4) _cell_length_b 35.468(4) _cell_length_c 7.9392(8) _cell_measurement_reflns_used 43433 _cell_measurement_temperature 110(2) _cell_measurement_theta_max 25.213 _cell_measurement_theta_min 1.816 _cell_volume 9979.2(19) _computing_cell_refinement 'Saint, Bruker-AXS' _computing_data_collection 'Apex2, Bruker-AXS' _computing_data_reduction 'Saint, Bruker-AXS' _computing_structure_refinement 'SHELXL-2018/1 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' _diffrn_ambient_temperature 110(2) _diffrn_detector_area_resol_mean 1.75 _diffrn_measured_fraction_theta_full 0.986 _diffrn_measured_fraction_theta_max 0.986 _diffrn_measurement_device_type 'ApexDuo, Bruker-AXS' _diffrn_measurement_method '1 deg. \f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0775 _diffrn_reflns_av_unetI/netI 0.0736 _diffrn_reflns_Laue_measured_fraction_full 0.986 _diffrn_reflns_Laue_measured_fraction_max 0.986 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -3 _diffrn_reflns_number 43433 _diffrn_reflns_point_group_measured_fraction_full 0.706 _diffrn_reflns_point_group_measured_fraction_max 0.706 _diffrn_reflns_theta_full 25.213 _diffrn_reflns_theta_max 25.213 _diffrn_reflns_theta_min 1.816 _diffrn_source 'ImuS micro-focus' _exptl_absorpt_coefficient_mu 0.174 _exptl_absorpt_correction_T_max 0.977 _exptl_absorpt_correction_T_min 0.960 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Sadabs, Bruker-AXS' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.552 _exptl_crystal_description prism _exptl_crystal_F_000 4736 _exptl_crystal_size_max 0.437 _exptl_crystal_size_mid 0.196 _exptl_crystal_size_min 0.134 _refine_diff_density_max 0.260 _refine_diff_density_min -0.357 _refine_diff_density_rms 0.054 _refine_ls_abs_structure_details ; Flack x determined using 2149 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.03(11) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1458 _refine_ls_number_reflns 12732 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.019 _refine_ls_R_factor_all 0.0649 _refine_ls_R_factor_gt 0.0466 _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^)+(0.0387P)^2^+0.2452P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0911 _refine_ls_wR_factor_ref 0.0982 _reflns_Friedel_coverage 0.328 _reflns_Friedel_fraction_full 0.379 _reflns_Friedel_fraction_max 0.379 _reflns_number_gt 10231 _reflns_number_total 12732 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9cc09244g2.cif _cod_data_source_block rom49 _cod_database_code 7125674 _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 0.928 _shelx_estimated_absorpt_t_max 0.977 _shelx_res_file ; TITL mo_rom49a_0ma_a.res in Pba2 rom49.res created by SHELXL-2018/1 at 11:58:46 on 18-Feb-2019 REM Old TITL mo_rom49a_0ma in Pba2 REM SHELXT solution in Pba2 REM R1 0.107, Rweak 0.029, Alpha 0.002, Orientation as input REM Flack x = -0.026 ( 0.105 ) from Parsons' quotients REM Formula found by SHELXT: C112 B2 N2 O F41 P2 CELL 0.71073 35.4388 35.4681 7.9392 90.000 90.000 90.000 ZERR 8.000 0.0041 0.0041 0.0008 0.000 0.000 0.000 LATT -1 SYMM -X, -Y, Z SYMM 1/2+X, 1/2-Y, Z SYMM 1/2-X, 1/2+Y, Z SFAC C H B N O F P UNIT 448 328 8 8 8 160 8 TEMP -163.000 SIZE 0.134 0.196 0.437 ACTA L.S. 10 OMIT 2 1 0 BOND $H LIST 6 FMAP 2 PLAN 20 WGHT 0.038700 0.245200 FVAR 0.18096 P1 7 0.210051 0.510563 0.766004 11.00000 0.02242 0.02454 = 0.02024 0.00045 0.00111 0.00070 C2 1 0.239571 0.505793 0.570200 11.00000 0.01796 0.01383 = 0.02219 -0.00147 0.00029 -0.00054 C3 1 0.227470 0.513625 0.389334 11.00000 0.01959 0.02911 = 0.01489 0.00019 -0.00214 -0.00123 C4 1 0.188494 0.498827 0.332635 11.00000 0.02750 0.04588 = 0.02291 0.00165 -0.00791 -0.00089 AFIX 137 H4A 2 0.188502 0.471203 0.335227 11.00000 -1.50000 H4B 2 0.183274 0.507498 0.217771 11.00000 -1.50000 H4C 2 0.168978 0.508393 0.408934 11.00000 -1.50000 AFIX 0 C5 1 0.227150 0.557117 0.363223 11.00000 0.03004 0.02688 = 0.03129 0.00870 -0.00276 0.00606 AFIX 137 H5A 2 0.225255 0.562770 0.242693 11.00000 -1.50000 H5B 2 0.250520 0.567933 0.408166 11.00000 -1.50000 H5C 2 0.205475 0.568030 0.422370 11.00000 -1.50000 AFIX 0 C6 1 0.259001 0.494475 0.287640 11.00000 0.02629 0.03651 = 0.02279 0.00475 -0.00051 0.00278 AFIX 23 H6A 2 0.251097 0.468880 0.252576 11.00000 -1.20000 H6AB 2 0.264867 0.509369 0.185481 11.00000 -1.20000 AFIX 0 C7 1 0.293393 0.492276 0.401792 11.00000 0.02231 0.02819 = 0.01237 0.00009 -0.00070 0.00141 C8 1 0.322623 0.523586 0.376895 11.00000 0.02444 0.02681 = 0.02513 -0.00099 0.00462 -0.00239 AFIX 137 H8A 2 0.333703 0.521470 0.264195 11.00000 -1.50000 H8B 2 0.342527 0.521122 0.461877 11.00000 -1.50000 H8C 2 0.310343 0.548201 0.388682 11.00000 -1.50000 AFIX 0 C9 1 0.312079 0.454026 0.385521 11.00000 0.03283 0.03341 = 0.02378 -0.00155 -0.00105 0.00968 AFIX 137 H9A 2 0.322633 0.451305 0.272076 11.00000 -1.50000 H9B 2 0.293339 0.434183 0.405051 11.00000 -1.50000 H9C 2 0.332351 0.451849 0.468911 11.00000 -1.50000 AFIX 0 N10 4 0.274866 0.496404 0.578153 11.00000 0.02482 0.01573 = 0.01293 0.00090 -0.00060 -0.00088 C11 1 0.299375 0.491452 0.728683 11.00000 0.01792 0.02357 = 0.00555 -0.00092 -0.00011 -0.00165 C12 1 0.305120 0.454597 0.787643 11.00000 0.01908 0.02858 = 0.01704 -0.00071 -0.00002 0.00401 C13 1 0.333636 0.449384 0.907260 11.00000 0.02559 0.02652 = 0.01745 0.00245 0.00089 0.00387 AFIX 43 H13 2 0.338325 0.424729 0.949067 11.00000 -1.20000 AFIX 0 C14 1 0.355361 0.479279 0.966886 11.00000 0.02010 0.02914 = 0.02045 0.00089 -0.00278 0.00087 AFIX 43 H14 2 0.375255 0.475083 1.044868 11.00000 -1.20000 AFIX 0 C15 1 0.347262 0.515178 0.909820 11.00000 0.02037 0.02558 = 0.01831 -0.00341 0.00127 -0.00080 AFIX 43 H15 2 0.361536 0.535725 0.952631 11.00000 -1.20000 AFIX 0 C16 1 0.319130 0.522487 0.792497 11.00000 0.01543 0.02630 = 0.02272 0.00047 0.00271 0.00426 C17 1 0.281510 0.420238 0.744856 11.00000 0.02973 0.01695 = 0.02727 0.00167 -0.00493 -0.00015 AFIX 13 H17 2 0.264322 0.427051 0.649710 11.00000 -1.20000 AFIX 0 C18 1 0.305008 0.386148 0.690878 11.00000 0.04895 0.01913 = 0.04150 -0.00478 -0.00476 -0.00156 AFIX 137 H18A 2 0.321912 0.393437 0.598775 11.00000 -1.50000 H18B 2 0.288187 0.365958 0.652620 11.00000 -1.50000 H18C 2 0.319982 0.377204 0.786653 11.00000 -1.50000 AFIX 0 C19 1 0.256884 0.409366 0.898168 11.00000 0.03221 0.03219 = 0.03224 0.00809 -0.00081 -0.00361 AFIX 137 H19A 2 0.239204 0.389409 0.865617 11.00000 -1.50000 H19B 2 0.242734 0.431501 0.936487 11.00000 -1.50000 H19C 2 0.273110 0.400299 0.989547 11.00000 -1.50000 AFIX 0 C20 1 0.310875 0.564349 0.755677 11.00000 0.01862 0.02343 = 0.02745 0.00184 -0.00271 -0.00017 AFIX 13 H20 2 0.290541 0.565875 0.668612 11.00000 -1.20000 AFIX 0 C21 1 0.296726 0.583263 0.917614 11.00000 0.02629 0.02644 = 0.03134 -0.00946 0.00366 -0.00075 AFIX 137 H21A 2 0.287778 0.608756 0.891715 11.00000 -1.50000 H21B 2 0.317393 0.584685 0.999383 11.00000 -1.50000 H21C 2 0.275972 0.568428 0.965171 11.00000 -1.50000 AFIX 0 C22 1 0.345236 0.586695 0.693135 11.00000 0.03354 0.02476 = 0.03634 0.00211 0.00122 -0.01079 AFIX 137 H22A 2 0.338050 0.613079 0.675380 11.00000 -1.50000 H22B 2 0.354177 0.575894 0.586760 11.00000 -1.50000 H22C 2 0.365411 0.585375 0.777347 11.00000 -1.50000 AFIX 0 O23 5 0.233820 0.513373 0.917119 11.00000 0.03208 0.03715 = 0.02812 0.00099 -0.00366 0.00062 C24 1 0.182940 0.552653 0.729466 11.00000 0.01675 0.02647 = 0.02086 0.00036 0.00069 -0.00076 C25 1 0.147170 0.552610 0.656559 11.00000 0.01922 0.02744 = 0.02934 0.00063 0.00388 0.00148 AFIX 43 H25 2 0.134991 0.529407 0.631701 11.00000 -1.20000 AFIX 0 C26 1 0.129365 0.586485 0.620320 11.00000 0.02427 0.03116 = 0.03643 -0.00070 -0.00311 0.00402 AFIX 43 H26 2 0.105249 0.586484 0.568075 11.00000 -1.20000 AFIX 0 C27 1 0.146700 0.620254 0.660198 11.00000 0.02600 0.03070 = 0.03381 0.00098 0.00130 0.01306 AFIX 43 H27 2 0.134702 0.643387 0.632456 11.00000 -1.20000 AFIX 0 C28 1 0.181288 0.620609 0.739969 11.00000 0.03371 0.01675 = 0.03774 -0.00468 -0.00287 0.00304 AFIX 43 H28 2 0.192727 0.643905 0.769633 11.00000 -1.20000 AFIX 0 C29 1 0.199325 0.586904 0.776770 11.00000 0.02141 0.02624 = 0.03643 -0.00289 -0.00937 0.00074 AFIX 43 H29 2 0.222842 0.587092 0.834193 11.00000 -1.20000 AFIX 0 C30 1 0.179563 0.470287 0.761472 11.00000 0.01383 0.02709 = 0.02451 0.00468 0.00025 0.00256 C31 1 0.152175 0.468283 0.888108 11.00000 0.03085 0.03380 = 0.02895 0.00246 0.00149 0.00470 AFIX 43 H31 2 0.148447 0.489275 0.960541 11.00000 -1.20000 AFIX 0 C32 1 0.130545 0.436409 0.909499 11.00000 0.02571 0.03360 = 0.03385 0.00838 0.00568 0.00037 AFIX 43 H32 2 0.112283 0.435309 0.996956 11.00000 -1.20000 AFIX 0 C33 1 0.135640 0.405592 0.801427 11.00000 0.03040 0.02582 = 0.04715 0.01297 -0.00250 -0.00499 AFIX 43 H33 2 0.120467 0.383728 0.815238 11.00000 -1.20000 AFIX 0 C34 1 0.162317 0.406564 0.675567 11.00000 0.02489 0.02469 = 0.04460 -0.00158 -0.00012 -0.00158 AFIX 43 H34 2 0.165845 0.385465 0.603558 11.00000 -1.20000 AFIX 0 C35 1 0.184404 0.439454 0.655053 11.00000 0.02487 0.03074 = 0.02720 -0.00537 -0.00396 0.00139 AFIX 43 H35 2 0.202722 0.440524 0.567822 11.00000 -1.20000 AFIX 0 P36 7 0.459830 0.288717 0.084634 11.00000 0.02050 0.01927 = 0.01671 -0.00037 -0.00005 0.00204 C37 1 0.463320 0.259275 0.281540 11.00000 0.00480 0.01851 = 0.02267 0.00181 -0.00079 -0.00049 C38 1 0.461764 0.273201 0.462504 11.00000 0.01831 0.02628 = 0.01476 -0.00042 0.00304 0.00077 C39 1 0.420099 0.282830 0.506904 11.00000 0.02645 0.03134 = 0.02682 -0.00236 0.00849 0.00439 AFIX 137 H39A 2 0.413358 0.307191 0.457033 11.00000 -1.50000 H39B 2 0.417256 0.284177 0.629541 11.00000 -1.50000 H39C 2 0.403442 0.263186 0.462102 11.00000 -1.50000 AFIX 0 C40 1 0.486009 0.308087 0.506578 11.00000 0.03775 0.02169 = 0.02766 -0.00636 -0.00647 -0.00455 AFIX 137 H40A 2 0.512752 0.302079 0.490237 11.00000 -1.50000 H40B 2 0.481678 0.315150 0.624339 11.00000 -1.50000 H40C 2 0.478962 0.329141 0.433085 11.00000 -1.50000 AFIX 0 C41 1 0.476596 0.238857 0.557779 11.00000 0.02346 0.02870 = 0.01677 -0.00139 -0.00014 0.00344 AFIX 23 H41A 2 0.504179 0.241011 0.575037 11.00000 -1.20000 H41B 2 0.464248 0.236895 0.669289 11.00000 -1.20000 AFIX 0 C42 1 0.467594 0.204487 0.451826 11.00000 0.02013 0.02245 = 0.01201 0.00039 -0.00064 0.00075 C43 1 0.499045 0.175102 0.458515 11.00000 0.02226 0.02705 = 0.01669 0.00182 -0.00129 0.00123 AFIX 137 H43A 2 0.493560 0.154833 0.378277 11.00000 -1.50000 H43B 2 0.500644 0.164617 0.572498 11.00000 -1.50000 H43C 2 0.523118 0.186995 0.429064 11.00000 -1.50000 AFIX 0 C44 1 0.430139 0.185260 0.493963 11.00000 0.01979 0.03189 = 0.01846 0.00550 0.00249 0.00083 AFIX 137 H44A 2 0.409357 0.203028 0.475792 11.00000 -1.50000 H44B 2 0.430326 0.177207 0.612039 11.00000 -1.50000 H44C 2 0.426733 0.163225 0.421061 11.00000 -1.50000 AFIX 0 N45 4 0.464945 0.222770 0.274621 11.00000 0.01018 0.02509 = 0.01558 -0.00225 -0.00146 0.00008 C46 1 0.463099 0.197110 0.126158 11.00000 0.02411 0.01499 = 0.01314 -0.00016 0.00070 0.00200 C47 1 0.497348 0.184349 0.057262 11.00000 0.02245 0.01543 = 0.01432 0.00154 -0.00133 -0.00135 C48 1 0.495477 0.155978 -0.063074 11.00000 0.02002 0.01913 = 0.01899 0.00217 0.00111 0.00848 AFIX 43 H48 2 0.518112 0.147141 -0.113580 11.00000 -1.20000 AFIX 0 C49 1 0.461268 0.140258 -0.111145 11.00000 0.03024 0.01612 = 0.01198 -0.00003 -0.00378 0.00123 AFIX 43 H49 2 0.460719 0.119948 -0.189115 11.00000 -1.20000 AFIX 0 C50 1 0.427991 0.154258 -0.045166 11.00000 0.02080 0.01762 = 0.01707 -0.00163 -0.00524 -0.00180 AFIX 43 H50 2 0.404717 0.143747 -0.081509 11.00000 -1.20000 AFIX 0 C51 1 0.427530 0.183487 0.073711 11.00000 0.01934 0.01641 = 0.01455 0.00856 -0.00032 -0.00159 C52 1 0.536080 0.201183 0.093033 11.00000 0.01963 0.02330 = 0.02092 -0.00399 0.00297 0.00282 AFIX 13 H52 2 0.533681 0.218884 0.190486 11.00000 -1.20000 AFIX 0 C53 1 0.565746 0.171266 0.137651 11.00000 0.01727 0.03600 = 0.02688 -0.00471 0.00706 0.00251 AFIX 137 H53A 2 0.570392 0.155199 0.039395 11.00000 -1.50000 H53B 2 0.556503 0.155780 0.231180 11.00000 -1.50000 H53C 2 0.589282 0.183723 0.170860 11.00000 -1.50000 AFIX 0 C54 1 0.549843 0.223768 -0.060686 11.00000 0.02511 0.03830 = 0.02253 0.00374 0.00604 -0.00456 AFIX 137 H54A 2 0.553659 0.206634 -0.156016 11.00000 -1.50000 H54B 2 0.573718 0.236288 -0.033276 11.00000 -1.50000 H54C 2 0.530915 0.242764 -0.090643 11.00000 -1.50000 AFIX 0 C55 1 0.388919 0.199081 0.119433 11.00000 0.01303 0.01792 = 0.02920 -0.00857 0.00109 0.00064 AFIX 13 H55 2 0.392134 0.219563 0.204794 11.00000 -1.20000 AFIX 0 C56 1 0.370625 0.215798 -0.039301 11.00000 0.02018 0.02955 = 0.03989 -0.00834 -0.01071 0.00243 AFIX 137 H56A 2 0.388136 0.233597 -0.092257 11.00000 -1.50000 H56B 2 0.347345 0.228992 -0.008266 11.00000 -1.50000 H56C 2 0.364725 0.195468 -0.118640 11.00000 -1.50000 AFIX 0 C57 1 0.362082 0.169019 0.191039 11.00000 0.02151 0.03734 = 0.03129 -0.00381 0.00487 -0.00581 AFIX 137 H57A 2 0.356167 0.150526 0.103210 11.00000 -1.50000 H57B 2 0.338746 0.181109 0.229369 11.00000 -1.50000 H57C 2 0.374228 0.156264 0.286172 11.00000 -1.50000 AFIX 0 O58 5 0.451141 0.264773 -0.061764 11.00000 0.02592 0.02114 = 0.01753 -0.00486 0.00166 0.00153 C59 1 0.422861 0.322035 0.128949 11.00000 0.02059 0.01526 = 0.01750 -0.00227 0.00288 0.00234 C60 1 0.386199 0.310577 0.093634 11.00000 0.02702 0.01818 = 0.04140 -0.00274 -0.00546 0.00156 AFIX 43 H60 2 0.381912 0.286777 0.042181 11.00000 -1.20000 AFIX 0 C61 1 0.355892 0.333564 0.132833 11.00000 0.01981 0.02902 = 0.05314 -0.00537 0.00075 0.00615 AFIX 43 H61 2 0.330926 0.325706 0.107030 11.00000 -1.20000 AFIX 0 C62 1 0.362044 0.367919 0.209482 11.00000 0.02314 0.03130 = 0.04308 -0.00790 0.00482 0.01013 AFIX 43 H62 2 0.341198 0.383259 0.240519 11.00000 -1.20000 AFIX 0 C63 1 0.398356 0.380132 0.241338 11.00000 0.03644 0.01781 = 0.03353 -0.00396 0.00341 0.00400 AFIX 43 H63 2 0.402503 0.404307 0.289413 11.00000 -1.20000 AFIX 0 C64 1 0.428636 0.357137 0.203183 11.00000 0.02148 0.02130 = 0.02450 -0.00024 -0.00137 -0.00040 AFIX 43 H64 2 0.453560 0.365324 0.227746 11.00000 -1.20000 AFIX 0 C65 1 0.503946 0.313321 0.076712 11.00000 0.02816 0.01749 = 0.02077 -0.00412 0.00468 0.00088 C66 1 0.536270 0.302379 0.163704 11.00000 0.02255 0.02284 = 0.04397 -0.00249 -0.00379 0.00126 AFIX 43 H66 2 0.535178 0.282138 0.241923 11.00000 -1.20000 AFIX 0 C67 1 0.569932 0.321036 0.135959 11.00000 0.01974 0.03461 = 0.05891 -0.00900 -0.00399 -0.00208 AFIX 43 H67 2 0.591924 0.313735 0.196109 11.00000 -1.20000 AFIX 0 C68 1 0.571751 0.350098 0.021789 11.00000 0.02797 0.03221 = 0.05930 -0.01312 0.01961 -0.01155 AFIX 43 H68 2 0.595129 0.362497 0.002813 11.00000 -1.20000 AFIX 0 C69 1 0.540410 0.361423 -0.064872 11.00000 0.04042 0.02507 = 0.04665 -0.00201 0.01396 -0.00945 AFIX 43 H69 2 0.541913 0.381800 -0.142239 11.00000 -1.20000 AFIX 0 C70 1 0.506610 0.343073 -0.039235 11.00000 0.03837 0.01910 = 0.03100 -0.00725 0.01000 0.00271 AFIX 43 H70 2 0.484891 0.350642 -0.100684 11.00000 -1.20000 AFIX 0 B71 3 0.211871 0.252102 0.923158 11.00000 0.01616 0.01726 = 0.02666 -0.00154 0.00168 0.00121 C72 1 0.247948 0.250357 0.789479 11.00000 0.01189 0.02374 = 0.02129 -0.00054 0.00003 0.00194 C73 1 0.276646 0.276487 0.768425 11.00000 0.02085 0.01653 = 0.02382 -0.00127 0.00242 0.00217 C74 1 0.306016 0.272921 0.654690 11.00000 0.01610 0.02764 = 0.03496 0.00550 0.00347 -0.00219 C75 1 0.307610 0.241882 0.555014 11.00000 0.01363 0.03538 = 0.02633 -0.00078 0.00654 0.00229 C76 1 0.280092 0.215163 0.564592 11.00000 0.02033 0.02799 = 0.01961 -0.00784 -0.00164 0.00260 C77 1 0.250894 0.219910 0.680373 11.00000 0.01601 0.02341 = 0.02387 0.00094 -0.00117 -0.00331 C78 1 0.211332 0.215609 1.049972 11.00000 0.01037 0.02214 = 0.02348 -0.00485 -0.00047 -0.00266 C79 1 0.239178 0.188363 1.071283 11.00000 0.02281 0.02117 = 0.02145 -0.00519 0.00742 -0.00680 C80 1 0.237359 0.158531 1.182588 11.00000 0.02004 0.02130 = 0.03273 0.00116 -0.00159 -0.00267 C81 1 0.206877 0.155430 1.288960 11.00000 0.03017 0.02181 = 0.02401 0.00304 -0.00029 -0.00724 C82 1 0.179087 0.182403 1.280386 11.00000 0.02378 0.02981 = 0.02165 -0.00280 0.00385 -0.00795 C83 1 0.181883 0.211191 1.166593 11.00000 0.01960 0.01761 = 0.02736 -0.00066 0.00355 0.00266 C84 1 0.174747 0.253154 0.793683 11.00000 0.01340 0.02205 = 0.02457 -0.00080 0.00518 0.00334 C85 1 0.147008 0.225716 0.773019 11.00000 0.02309 0.02999 = 0.01691 0.00442 0.00332 0.00248 C86 1 0.117562 0.228061 0.659333 11.00000 0.01807 0.03870 = 0.03014 -0.00718 -0.00017 -0.00460 C87 1 0.114198 0.259397 0.559771 11.00000 0.01680 0.04218 = 0.02754 0.00305 -0.00014 0.00725 C88 1 0.140994 0.287190 0.570200 11.00000 0.02723 0.03026 = 0.02184 0.00347 0.00245 0.00719 C89 1 0.169920 0.283259 0.684596 11.00000 0.01972 0.01999 = 0.03023 -0.00377 0.00064 0.00330 C90 1 0.213641 0.288920 1.050302 11.00000 0.01741 0.02089 = 0.02147 0.00227 0.00998 -0.00150 C91 1 0.186726 0.317198 1.072806 11.00000 0.01938 0.02360 = 0.03205 -0.00218 0.00237 0.00095 C92 1 0.190828 0.346673 1.183719 11.00000 0.03368 0.02186 = 0.02767 -0.00079 0.00779 0.00718 C93 1 0.221974 0.349397 1.285326 11.00000 0.03834 0.02774 = 0.02245 -0.00514 0.00527 -0.00698 C94 1 0.249252 0.321533 1.271671 11.00000 0.02437 0.03082 = 0.02615 -0.00392 -0.00295 -0.00300 C95 1 0.244141 0.292629 1.160695 11.00000 0.01814 0.01954 = 0.02725 -0.00007 0.00455 0.00431 F96 6 0.277107 0.309032 0.859875 11.00000 0.02648 0.01851 = 0.03912 -0.00546 0.01029 -0.00332 F97 6 0.333528 0.299325 0.647040 11.00000 0.02326 0.03265 = 0.05873 -0.00579 0.01640 -0.01084 F98 6 0.336521 0.237533 0.442709 11.00000 0.02735 0.04953 = 0.04848 -0.01174 0.01600 -0.00408 F99 6 0.281907 0.183739 0.468141 11.00000 0.02924 0.03721 = 0.03763 -0.01547 0.00222 0.00038 F100 6 0.225114 0.191559 0.686423 11.00000 0.02301 0.03016 = 0.03637 -0.00882 0.00277 -0.00724 F101 6 0.271368 0.189200 0.977856 11.00000 0.02045 0.02674 = 0.03248 0.00256 0.00368 0.00455 F102 6 0.265552 0.133234 1.191239 11.00000 0.03168 0.02196 = 0.04445 0.00384 -0.00113 0.00962 F103 6 0.204718 0.126984 1.401240 11.00000 0.03960 0.02873 = 0.04307 0.01471 0.00755 0.00102 F104 6 0.148834 0.179903 1.384847 11.00000 0.03172 0.04046 = 0.03068 0.00651 0.01268 -0.00470 F105 6 0.152677 0.236339 1.162363 11.00000 0.01886 0.03247 = 0.03355 0.00207 0.00806 0.00556 F106 6 0.148438 0.192813 0.862363 11.00000 0.02985 0.02782 = 0.02985 0.00438 -0.00479 -0.01006 F107 6 0.091749 0.200126 0.648452 11.00000 0.02768 0.04695 = 0.04214 -0.00360 -0.00622 -0.01428 F108 6 0.085243 0.262065 0.448089 11.00000 0.03119 0.05436 = 0.04179 0.00417 -0.01402 0.00085 F109 6 0.138093 0.318049 0.471687 11.00000 0.04153 0.03983 = 0.04155 0.01460 -0.00893 0.00628 F110 6 0.195535 0.312118 0.688208 11.00000 0.02617 0.02469 = 0.03658 0.00780 -0.00373 -0.00393 F111 6 0.153900 0.316604 0.986529 11.00000 0.02237 0.03626 = 0.03782 -0.00237 0.00049 0.00885 F112 6 0.163170 0.373047 1.198819 11.00000 0.04282 0.03498 = 0.04807 -0.00872 0.00798 0.01634 F113 6 0.226938 0.378501 1.391462 11.00000 0.05482 0.03504 = 0.04443 -0.02046 0.00309 -0.00045 F114 6 0.280669 0.323638 1.368791 11.00000 0.03216 0.04176 = 0.03680 -0.00981 -0.00974 -0.00311 F115 6 0.272664 0.266911 1.153344 11.00000 0.02357 0.02459 = 0.03433 -0.00437 -0.00700 0.00410 B116 3 0.500000 0.500000 0.068964 10.50000 0.02229 0.02027 = 0.01598 0.00000 0.00000 -0.00220 C117 1 0.483231 0.532966 0.193899 11.00000 0.02611 0.01508 = 0.02143 0.00167 0.00387 -0.00413 C118 1 0.506983 0.551168 0.307392 11.00000 0.02338 0.02558 = 0.02800 0.00072 -0.00374 -0.00164 C119 1 0.496321 0.579819 0.413549 11.00000 0.04084 0.02042 = 0.02208 0.00293 -0.00947 -0.00995 C120 1 0.459262 0.591501 0.415927 11.00000 0.03676 0.01998 = 0.02511 -0.00089 0.00445 0.00349 C121 1 0.434152 0.574363 0.312372 11.00000 0.02234 0.02506 = 0.02448 0.00239 0.00484 0.00185 C122 1 0.446123 0.545343 0.207049 11.00000 0.02375 0.01832 = 0.02740 -0.00036 -0.00468 -0.00438 C123 1 0.467879 0.483179 -0.065923 11.00000 0.02037 0.02612 = 0.02232 -0.00056 0.00548 -0.00140 C124 1 0.451592 0.507112 -0.184669 11.00000 0.01969 0.02694 = 0.03026 -0.00999 0.00396 -0.00363 C125 1 0.427481 0.495625 -0.308664 11.00000 0.02351 0.03365 = 0.02222 0.00344 0.00208 0.00133 C126 1 0.417985 0.458343 -0.321978 11.00000 0.01776 0.04112 = 0.02235 -0.01413 0.00032 -0.00537 C127 1 0.433049 0.433147 -0.210652 11.00000 0.02294 0.02727 = 0.03648 -0.00652 0.00763 -0.00580 C128 1 0.457476 0.445951 -0.088406 11.00000 0.02335 0.02189 = 0.02501 -0.00196 0.00328 0.00446 F129 6 0.544451 0.541574 0.307728 11.00000 0.02068 0.02897 = 0.03672 -0.00197 -0.00948 -0.00083 F130 6 0.522029 0.596814 0.515260 11.00000 0.04393 0.02590 = 0.03675 -0.00441 -0.01794 -0.00447 F131 6 0.448431 0.619439 0.519823 11.00000 0.05063 0.03129 = 0.03869 -0.01128 0.00142 0.00453 F132 6 0.397296 0.584384 0.312984 11.00000 0.02810 0.03546 = 0.04378 -0.00585 0.00889 0.00588 F133 6 0.418239 0.529087 0.115688 11.00000 0.02180 0.03774 = 0.03828 -0.00905 -0.00232 -0.00279 F134 6 0.459039 0.544775 -0.177891 11.00000 0.03062 0.01982 = 0.03847 0.00235 -0.00588 -0.00282 F135 6 0.412183 0.520837 -0.417830 11.00000 0.03227 0.04483 = 0.02985 0.00489 -0.00505 0.00182 F136 6 0.394288 0.446600 -0.444528 11.00000 0.03165 0.05858 = 0.03187 -0.01736 -0.00557 -0.00988 F137 6 0.424152 0.396173 -0.221499 11.00000 0.04077 0.03022 = 0.04715 -0.01517 0.00261 -0.01327 F138 6 0.472114 0.418390 0.010015 11.00000 0.03985 0.01935 = 0.03928 -0.00116 -0.00226 -0.00443 B139 3 0.500000 0.000000 0.792861 10.50000 0.01657 0.02012 = 0.02086 0.00000 0.00000 0.00050 C140 1 0.530700 0.020495 0.665438 11.00000 0.01217 0.02297 = 0.01724 0.00181 -0.00182 -0.00104 C141 1 0.537564 0.058705 0.646969 11.00000 0.01331 0.02457 = 0.02543 -0.00142 -0.00292 0.00128 C142 1 0.563462 0.073984 0.538187 11.00000 0.02201 0.01930 = 0.03140 0.00343 -0.00283 -0.00239 C143 1 0.584118 0.050799 0.434772 11.00000 0.01729 0.03374 = 0.02290 0.00058 0.00290 -0.00598 C144 1 0.577639 0.012397 0.442914 11.00000 0.01117 0.03773 = 0.01782 -0.00396 -0.00019 0.00743 C145 1 0.551438 -0.001319 0.554105 11.00000 0.02108 0.02246 = 0.02789 -0.00167 -0.00579 0.00119 C146 1 0.479875 0.030002 0.926928 11.00000 0.01863 0.01206 = 0.02510 0.00239 0.00041 0.00467 C147 1 0.441491 0.035452 0.951910 11.00000 0.01786 0.01804 = 0.02548 0.00512 -0.00226 -0.00515 C148 1 0.426295 0.058913 1.072358 11.00000 0.02016 0.02651 = 0.02666 0.00602 0.00479 0.00780 C149 1 0.449535 0.077506 1.182729 11.00000 0.03277 0.02016 = 0.02331 0.00438 0.00838 0.00632 C150 1 0.488133 0.072689 1.166598 11.00000 0.02918 0.01520 = 0.01908 0.00145 -0.00481 0.00214 C151 1 0.501844 0.049670 1.041045 11.00000 0.01398 0.01957 = 0.02968 0.00275 -0.00134 0.00419 F152 6 0.518235 0.084722 0.738031 11.00000 0.02813 0.01747 = 0.03717 0.00057 0.00890 0.00670 F153 6 0.568556 0.111729 0.528736 11.00000 0.03301 0.02204 = 0.04017 0.00703 0.00251 -0.00392 F154 6 0.609486 0.064713 0.324281 11.00000 0.02820 0.04661 = 0.02867 0.00226 0.00748 -0.00687 F155 6 0.597531 -0.011186 0.342099 11.00000 0.02615 0.04123 = 0.02857 -0.01303 0.00674 0.00371 F156 6 0.547267 -0.039548 0.558097 11.00000 0.02336 0.02053 = 0.03741 -0.00475 -0.00032 0.00132 F157 6 0.540236 0.046724 1.032454 11.00000 0.01787 0.02862 = 0.03455 -0.00492 -0.00337 0.00403 F158 6 0.511793 0.091495 1.269378 11.00000 0.03713 0.02880 = 0.02813 -0.00623 -0.00670 0.00517 F159 6 0.435839 0.100375 1.302534 11.00000 0.04255 0.02921 = 0.02687 -0.00120 0.01154 0.01195 F160 6 0.388419 0.063160 1.087167 11.00000 0.02164 0.03552 = 0.04357 0.00186 0.01213 0.00986 F161 6 0.415478 0.016915 0.856634 11.00000 0.01711 0.03148 = 0.03645 0.00057 0.00025 0.00283 HKLF 4 REM mo_rom49a_0ma_a.res in Pba2 REM R1 = 0.0466 for 10231 Fo > 4sig(Fo) and 0.0649 for all 12732 data REM 1458 parameters refined using 1 restraints END WGHT 0.0386 0.2803 REM Highest difference peak 0.260, deepest hole -0.357, 1-sigma level 0.054 Q1 1 0.4631 0.2863 -0.0579 11.00000 0.05 0.26 Q2 1 0.5393 0.0369 0.6917 11.00000 0.05 0.26 Q3 1 0.3502 0.4047 0.2735 11.00000 0.05 0.26 Q4 1 0.1565 0.4493 0.7542 11.00000 0.05 0.25 Q5 1 0.2361 0.1606 1.0308 11.00000 0.05 0.24 Q6 1 0.2171 0.3562 1.2094 11.00000 0.05 0.23 Q7 1 0.4918 0.5144 0.1630 11.00000 0.05 0.22 Q8 1 0.1365 0.1903 1.0776 11.00000 0.05 0.22 Q9 1 0.2362 0.3009 1.2811 11.00000 0.05 0.22 Q10 1 0.5002 0.3406 0.0900 11.00000 0.05 0.21 Q11 1 0.4320 0.5000 -0.2171 11.00000 0.05 0.21 Q12 1 0.2035 0.5116 0.9312 11.00000 0.05 0.21 Q13 1 0.4630 0.2840 0.2140 11.00000 0.05 0.21 Q14 1 0.5532 0.2604 0.0297 11.00000 0.05 0.21 Q15 1 0.1694 0.2638 1.2317 11.00000 0.05 0.21 Q16 1 0.2842 0.2800 0.6674 11.00000 0.05 0.21 Q17 1 0.4224 0.1656 0.1035 11.00000 0.05 0.20 Q18 1 0.4272 0.0596 1.2356 11.00000 0.05 0.20 Q19 1 0.5071 0.1193 0.0388 11.00000 0.05 0.20 Q20 1 0.4140 0.5227 -0.5435 11.00000 0.05 0.19 ; _shelx_res_checksum 56035 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, 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 P1 P 0.21005(4) 0.51056(4) 0.76600(19) 0.0224(3) Uani 1 1 d . . . C2 C 0.23957(13) 0.50579(12) 0.5702(7) 0.0180(11) Uani 1 1 d . . . C3 C 0.22747(14) 0.51362(13) 0.3893(7) 0.0212(12) Uani 1 1 d . . . C4 C 0.18849(14) 0.49883(15) 0.3326(7) 0.0321(14) Uani 1 1 d . . . H4A H 0.188502 0.471203 0.335227 0.048 Uiso 1 1 calc R U . H4B H 0.183274 0.507498 0.217771 0.048 Uiso 1 1 calc R U . H4C H 0.168978 0.508393 0.408934 0.048 Uiso 1 1 calc R U . C5 C 0.22715(15) 0.55712(13) 0.3632(8) 0.0294(14) Uani 1 1 d . . . H5A H 0.225255 0.562770 0.242693 0.044 Uiso 1 1 calc R U . H5B H 0.250520 0.567933 0.408166 0.044 Uiso 1 1 calc R U . H5C H 0.205475 0.568030 0.422370 0.044 Uiso 1 1 calc R U . C6 C 0.25900(13) 0.49448(15) 0.2876(8) 0.0285(13) Uani 1 1 d . . . H6A H 0.251097 0.468880 0.252576 0.034 Uiso 1 1 calc R U . H6AB H 0.264867 0.509369 0.185481 0.034 Uiso 1 1 calc R U . C7 C 0.29339(14) 0.49228(13) 0.4018(7) 0.0210(12) Uani 1 1 d . . . C8 C 0.32262(14) 0.52359(13) 0.3769(7) 0.0255(13) Uani 1 1 d . . . H8A H 0.333703 0.521470 0.264195 0.038 Uiso 1 1 calc R U . H8B H 0.342527 0.521122 0.461877 0.038 Uiso 1 1 calc R U . H8C H 0.310343 0.548201 0.388682 0.038 Uiso 1 1 calc R U . C9 C 0.31208(15) 0.45403(13) 0.3855(7) 0.0300(14) Uani 1 1 d . . . H9A H 0.322633 0.451305 0.272076 0.045 Uiso 1 1 calc R U . H9B H 0.293339 0.434183 0.405051 0.045 Uiso 1 1 calc R U . H9C H 0.332351 0.451849 0.468911 0.045 Uiso 1 1 calc R U . N10 N 0.27487(11) 0.49640(10) 0.5782(5) 0.0178(9) Uani 1 1 d . . . C11 C 0.29937(13) 0.49145(13) 0.7287(6) 0.0157(11) Uani 1 1 d . . . C12 C 0.30512(13) 0.45460(14) 0.7876(7) 0.0216(12) Uani 1 1 d . . . C13 C 0.33364(14) 0.44938(14) 0.9073(7) 0.0232(12) Uani 1 1 d . . . H13 H 0.338325 0.424729 0.949067 0.028 Uiso 1 1 calc R U . C14 C 0.35536(14) 0.47928(13) 0.9669(7) 0.0232(12) Uani 1 1 d . . . H14 H 0.375255 0.475083 1.044868 0.028 Uiso 1 1 calc R U . C15 C 0.34726(13) 0.51518(13) 0.9098(7) 0.0214(12) Uani 1 1 d . . . H15 H 0.361536 0.535725 0.952631 0.026 Uiso 1 1 calc R U . C16 C 0.31913(13) 0.52249(13) 0.7925(7) 0.0215(12) Uani 1 1 d . . . C17 C 0.28151(14) 0.42024(13) 0.7449(7) 0.0247(13) Uani 1 1 d . . . H17 H 0.264322 0.427051 0.649710 0.030 Uiso 1 1 calc R U . C18 C 0.30501(16) 0.38615(13) 0.6909(8) 0.0365(15) Uani 1 1 d . . . H18A H 0.321912 0.393437 0.598775 0.055 Uiso 1 1 calc R U . H18B H 0.288187 0.365958 0.652620 0.055 Uiso 1 1 calc R U . H18C H 0.319982 0.377204 0.786653 0.055 Uiso 1 1 calc R U . C19 C 0.25688(15) 0.40937(14) 0.8982(7) 0.0322(14) Uani 1 1 d . . . H19A H 0.239204 0.389409 0.865617 0.048 Uiso 1 1 calc R U . H19B H 0.242734 0.431501 0.936487 0.048 Uiso 1 1 calc R U . H19C H 0.273110 0.400299 0.989547 0.048 Uiso 1 1 calc R U . C20 C 0.31087(13) 0.56435(13) 0.7557(7) 0.0232(12) Uani 1 1 d . . . H20 H 0.290541 0.565875 0.668612 0.028 Uiso 1 1 calc R U . C21 C 0.29673(14) 0.58326(13) 0.9176(7) 0.0280(13) Uani 1 1 d . . . H21A H 0.287778 0.608756 0.891715 0.042 Uiso 1 1 calc R U . H21B H 0.317393 0.584685 0.999383 0.042 Uiso 1 1 calc R U . H21C H 0.275972 0.568428 0.965171 0.042 Uiso 1 1 calc R U . C22 C 0.34524(14) 0.58669(14) 0.6931(8) 0.0315(14) Uani 1 1 d . . . H22A H 0.338050 0.613079 0.675380 0.047 Uiso 1 1 calc R U . H22B H 0.354177 0.575894 0.586760 0.047 Uiso 1 1 calc R U . H22C H 0.365411 0.585375 0.777347 0.047 Uiso 1 1 calc R U . O23 O 0.23382(10) 0.51337(9) 0.9171(5) 0.0325(10) Uani 1 1 d . . . C24 C 0.18294(13) 0.55265(13) 0.7295(7) 0.0214(12) Uani 1 1 d . . . C25 C 0.14717(13) 0.55261(14) 0.6566(7) 0.0253(13) Uani 1 1 d . . . H25 H 0.134991 0.529407 0.631701 0.030 Uiso 1 1 calc R U . C26 C 0.12937(15) 0.58649(14) 0.6203(8) 0.0306(14) Uani 1 1 d . . . H26 H 0.105249 0.586484 0.568075 0.037 Uiso 1 1 calc R U . C27 C 0.14670(14) 0.62025(14) 0.6602(7) 0.0302(14) Uani 1 1 d . . . H27 H 0.134702 0.643387 0.632456 0.036 Uiso 1 1 calc R U . C28 C 0.18129(15) 0.62061(13) 0.7400(8) 0.0294(14) Uani 1 1 d . . . H28 H 0.192727 0.643905 0.769633 0.035 Uiso 1 1 calc R U . C29 C 0.19932(14) 0.58690(13) 0.7768(8) 0.0280(13) Uani 1 1 d . . . H29 H 0.222842 0.587092 0.834193 0.034 Uiso 1 1 calc R U . C30 C 0.17956(13) 0.47029(13) 0.7615(7) 0.0218(12) Uani 1 1 d . . . C31 C 0.15218(14) 0.46828(15) 0.8881(8) 0.0312(14) Uani 1 1 d . . . H31 H 0.148447 0.489275 0.960541 0.037 Uiso 1 1 calc R U . C32 C 0.13055(15) 0.43641(14) 0.9095(8) 0.0311(14) Uani 1 1 d . . . H32 H 0.112283 0.435309 0.996956 0.037 Uiso 1 1 calc R U . C33 C 0.13564(15) 0.40559(14) 0.8014(8) 0.0345(15) Uani 1 1 d . . . H33 H 0.120467 0.383728 0.815238 0.041 Uiso 1 1 calc R U . C34 C 0.16232(14) 0.40656(14) 0.6756(8) 0.0314(14) Uani 1 1 d . . . H34 H 0.165845 0.385465 0.603558 0.038 Uiso 1 1 calc R U . C35 C 0.18440(14) 0.43945(13) 0.6551(7) 0.0276(13) Uani 1 1 d . . . H35 H 0.202722 0.440524 0.567822 0.033 Uiso 1 1 calc R U . P36 P 0.45983(4) 0.28872(3) 0.08463(18) 0.0188(3) Uani 1 1 d . . . C37 C 0.46332(12) 0.25927(13) 0.2815(7) 0.0153(11) Uani 1 1 d . . . C38 C 0.46176(13) 0.27320(13) 0.4625(7) 0.0198(12) Uani 1 1 d . . . C39 C 0.42010(13) 0.28283(14) 0.5069(7) 0.0282(14) Uani 1 1 d . . . H39A H 0.413358 0.307191 0.457033 0.042 Uiso 1 1 calc R U . H39B H 0.417256 0.284177 0.629541 0.042 Uiso 1 1 calc R U . H39C H 0.403442 0.263186 0.462102 0.042 Uiso 1 1 calc R U . C40 C 0.48601(15) 0.30809(13) 0.5066(7) 0.0290(14) Uani 1 1 d . . . H40A H 0.512752 0.302079 0.490237 0.044 Uiso 1 1 calc R U . H40B H 0.481678 0.315150 0.624339 0.044 Uiso 1 1 calc R U . H40C H 0.478962 0.329141 0.433085 0.044 Uiso 1 1 calc R U . C41 C 0.47660(14) 0.23886(13) 0.5578(7) 0.0230(12) Uani 1 1 d . . . H41A H 0.504179 0.241011 0.575037 0.028 Uiso 1 1 calc R U . H41B H 0.464248 0.236895 0.669289 0.028 Uiso 1 1 calc R U . C42 C 0.46759(13) 0.20449(13) 0.4518(7) 0.0182(11) Uani 1 1 d . . . C43 C 0.49905(13) 0.17510(13) 0.4585(7) 0.0220(12) Uani 1 1 d . . . H43A H 0.493560 0.154833 0.378277 0.033 Uiso 1 1 calc R U . H43B H 0.500644 0.164617 0.572498 0.033 Uiso 1 1 calc R U . H43C H 0.523118 0.186995 0.429064 0.033 Uiso 1 1 calc R U . C44 C 0.43014(13) 0.18526(14) 0.4940(7) 0.0234(12) Uani 1 1 d . . . H44A H 0.409357 0.203028 0.475792 0.035 Uiso 1 1 calc R U . H44B H 0.430326 0.177207 0.612039 0.035 Uiso 1 1 calc R U . H44C H 0.426733 0.163225 0.421061 0.035 Uiso 1 1 calc R U . N45 N 0.46494(10) 0.22277(11) 0.2746(6) 0.0169(9) Uani 1 1 d . . . C46 C 0.46310(13) 0.19711(12) 0.1262(6) 0.0174(12) Uani 1 1 d . . . C47 C 0.49735(13) 0.18435(12) 0.0573(7) 0.0174(11) Uani 1 1 d . . . C48 C 0.49548(13) 0.15598(12) -0.0631(7) 0.0194(12) Uani 1 1 d . . . H48 H 0.518112 0.147141 -0.113580 0.023 Uiso 1 1 calc R U . C49 C 0.46127(13) 0.14026(13) -0.1111(7) 0.0194(12) Uani 1 1 d . . . H49 H 0.460719 0.119948 -0.189115 0.023 Uiso 1 1 calc R U . C50 C 0.42799(13) 0.15426(12) -0.0452(7) 0.0185(11) Uani 1 1 d . . . H50 H 0.404717 0.143747 -0.081509 0.022 Uiso 1 1 calc R U . C51 C 0.42753(13) 0.18349(12) 0.0737(7) 0.0168(11) Uani 1 1 d . . . C52 C 0.53608(13) 0.20118(13) 0.0930(7) 0.0213(12) Uani 1 1 d . . . H52 H 0.533681 0.218884 0.190486 0.026 Uiso 1 1 calc R U . C53 C 0.56575(13) 0.17127(14) 0.1377(7) 0.0267(13) Uani 1 1 d . . . H53A H 0.570392 0.155199 0.039395 0.040 Uiso 1 1 calc R U . H53B H 0.556503 0.155780 0.231180 0.040 Uiso 1 1 calc R U . H53C H 0.589282 0.183723 0.170860 0.040 Uiso 1 1 calc R U . C54 C 0.54984(14) 0.22377(14) -0.0607(7) 0.0286(13) Uani 1 1 d . . . H54A H 0.553659 0.206634 -0.156016 0.043 Uiso 1 1 calc R U . H54B H 0.573718 0.236288 -0.033276 0.043 Uiso 1 1 calc R U . H54C H 0.530915 0.242764 -0.090643 0.043 Uiso 1 1 calc R U . C55 C 0.38892(12) 0.19908(13) 0.1194(7) 0.0201(12) Uani 1 1 d . . . H55 H 0.392134 0.219563 0.204794 0.024 Uiso 1 1 calc R U . C56 C 0.37063(14) 0.21580(14) -0.0393(8) 0.0299(14) Uani 1 1 d . . . H56A H 0.388136 0.233597 -0.092257 0.045 Uiso 1 1 calc R U . H56B H 0.347345 0.228992 -0.008266 0.045 Uiso 1 1 calc R U . H56C H 0.364725 0.195468 -0.118640 0.045 Uiso 1 1 calc R U . C57 C 0.36208(14) 0.16902(14) 0.1910(8) 0.0300(14) Uani 1 1 d . . . H57A H 0.356167 0.150526 0.103210 0.045 Uiso 1 1 calc R U . H57B H 0.338746 0.181109 0.229369 0.045 Uiso 1 1 calc R U . H57C H 0.374228 0.156264 0.286172 0.045 Uiso 1 1 calc R U . O58 O 0.45114(9) 0.26477(8) -0.0618(5) 0.0215(8) Uani 1 1 d . . . C59 C 0.42286(13) 0.32204(12) 0.1289(6) 0.0178(12) Uani 1 1 d . . . C60 C 0.38620(14) 0.31058(13) 0.0936(8) 0.0289(13) Uani 1 1 d . . . H60 H 0.381912 0.286777 0.042181 0.035 Uiso 1 1 calc R U . C61 C 0.35589(14) 0.33356(14) 0.1328(8) 0.0340(15) Uani 1 1 d . . . H61 H 0.330926 0.325706 0.107030 0.041 Uiso 1 1 calc R U . C62 C 0.36204(15) 0.36792(14) 0.2095(8) 0.0325(15) Uani 1 1 d . . . H62 H 0.341198 0.383259 0.240519 0.039 Uiso 1 1 calc R U . C63 C 0.39836(15) 0.38013(14) 0.2413(7) 0.0293(14) Uani 1 1 d . . . H63 H 0.402503 0.404307 0.289413 0.035 Uiso 1 1 calc R U . C64 C 0.42864(14) 0.35714(13) 0.2032(7) 0.0224(12) Uani 1 1 d . . . H64 H 0.453560 0.365324 0.227746 0.027 Uiso 1 1 calc R U . C65 C 0.50395(14) 0.31332(12) 0.0767(7) 0.0221(12) Uani 1 1 d . . . C66 C 0.53627(14) 0.30238(14) 0.1637(8) 0.0298(14) Uani 1 1 d . . . H66 H 0.535178 0.282138 0.241923 0.036 Uiso 1 1 calc R U . C67 C 0.56993(15) 0.32104(15) 0.1360(9) 0.0378(16) Uani 1 1 d . . . H67 H 0.591924 0.313735 0.196109 0.045 Uiso 1 1 calc R U . C68 C 0.57175(16) 0.35010(15) 0.0218(9) 0.0398(17) Uani 1 1 d . . . H68 H 0.595129 0.362497 0.002813 0.048 Uiso 1 1 calc R U . C69 C 0.54041(16) 0.36142(15) -0.0649(8) 0.0374(16) Uani 1 1 d . . . H69 H 0.541913 0.381800 -0.142239 0.045 Uiso 1 1 calc R U . C70 C 0.50661(15) 0.34307(13) -0.0392(8) 0.0295(14) Uani 1 1 d . . . H70 H 0.484891 0.350642 -0.100684 0.035 Uiso 1 1 calc R U . B71 B 0.21187(15) 0.25210(15) 0.9232(9) 0.0200(13) Uani 1 1 d . . . C72 C 0.24795(12) 0.25036(12) 0.7895(7) 0.0190(12) Uani 1 1 d . . . C73 C 0.27665(13) 0.27649(13) 0.7684(7) 0.0204(12) Uani 1 1 d . . . C74 C 0.30602(14) 0.27292(14) 0.6547(8) 0.0262(13) Uani 1 1 d . . . C75 C 0.30761(13) 0.24188(14) 0.5550(7) 0.0251(13) Uani 1 1 d . . . C76 C 0.28009(13) 0.21516(13) 0.5646(7) 0.0226(12) Uani 1 1 d . . . C77 C 0.25089(13) 0.21991(13) 0.6804(7) 0.0211(12) Uani 1 1 d . . . C78 C 0.21133(12) 0.21561(13) 1.0500(7) 0.0187(12) Uani 1 1 d . . . C79 C 0.23918(13) 0.18836(13) 1.0713(7) 0.0218(12) Uani 1 1 d . . . C80 C 0.23736(14) 0.15853(13) 1.1826(7) 0.0247(13) Uani 1 1 d . . . C81 C 0.20688(14) 0.15543(13) 1.2890(7) 0.0253(13) Uani 1 1 d . . . C82 C 0.17909(14) 0.18240(14) 1.2804(7) 0.0251(12) Uani 1 1 d . . . C83 C 0.18188(13) 0.21119(13) 1.1666(7) 0.0215(12) Uani 1 1 d . . . C84 C 0.17475(13) 0.25315(12) 0.7937(7) 0.0200(12) Uani 1 1 d . . . C85 C 0.14701(14) 0.22572(14) 0.7730(7) 0.0233(12) Uani 1 1 d . . . C86 C 0.11756(14) 0.22806(15) 0.6593(8) 0.0290(14) Uani 1 1 d . . . C87 C 0.11420(14) 0.25940(15) 0.5598(8) 0.0288(13) Uani 1 1 d . . . C88 C 0.14099(14) 0.28719(14) 0.5702(7) 0.0264(13) Uani 1 1 d . . . C89 C 0.16992(14) 0.28326(13) 0.6846(7) 0.0233(13) Uani 1 1 d . . . C90 C 0.21364(13) 0.28892(13) 1.0503(7) 0.0199(12) Uani 1 1 d . . . C91 C 0.18673(14) 0.31720(13) 1.0728(8) 0.0250(13) Uani 1 1 d . . . C92 C 0.19083(15) 0.34667(13) 1.1837(7) 0.0277(13) Uani 1 1 d . . . C93 C 0.22197(15) 0.34940(14) 1.2853(8) 0.0295(13) Uani 1 1 d . . . C94 C 0.24925(14) 0.32153(14) 1.2717(8) 0.0271(13) Uani 1 1 d . . . C95 C 0.24414(13) 0.29263(13) 1.1607(7) 0.0216(12) Uani 1 1 d . . . F96 F 0.27711(8) 0.30903(7) 0.8599(4) 0.0280(7) Uani 1 1 d . . . F97 F 0.33353(8) 0.29932(8) 0.6470(5) 0.0382(9) Uani 1 1 d . . . F98 F 0.33652(8) 0.23753(8) 0.4427(5) 0.0418(9) Uani 1 1 d . . . F99 F 0.28191(8) 0.18374(8) 0.4681(4) 0.0347(8) Uani 1 1 d . . . F100 F 0.22511(7) 0.19156(7) 0.6864(4) 0.0298(8) Uani 1 1 d . . . F101 F 0.27137(7) 0.18920(7) 0.9779(4) 0.0266(7) Uani 1 1 d . . . F102 F 0.26555(8) 0.13323(7) 1.1912(4) 0.0327(8) Uani 1 1 d . . . F103 F 0.20472(8) 0.12698(8) 1.4012(4) 0.0371(8) Uani 1 1 d . . . F104 F 0.14883(8) 0.17990(8) 1.3848(4) 0.0343(8) Uani 1 1 d . . . F105 F 0.15268(7) 0.23634(7) 1.1624(4) 0.0283(7) Uani 1 1 d . . . F106 F 0.14844(8) 0.19281(7) 0.8624(4) 0.0292(8) Uani 1 1 d . . . F107 F 0.09175(8) 0.20013(8) 0.6485(4) 0.0389(9) Uani 1 1 d . . . F108 F 0.08524(8) 0.26206(9) 0.4481(5) 0.0424(9) Uani 1 1 d . . . F109 F 0.13809(9) 0.31805(8) 0.4717(4) 0.0410(9) Uani 1 1 d . . . F110 F 0.19554(8) 0.31212(7) 0.6882(4) 0.0291(7) Uani 1 1 d . . . F111 F 0.15390(8) 0.31660(8) 0.9865(4) 0.0322(8) Uani 1 1 d . . . F112 F 0.16317(9) 0.37305(8) 1.1988(4) 0.0420(9) Uani 1 1 d . . . F113 F 0.22694(9) 0.37850(8) 1.3915(4) 0.0448(9) Uani 1 1 d . . . F114 F 0.28067(8) 0.32364(8) 1.3688(4) 0.0369(8) Uani 1 1 d . . . F115 F 0.27266(7) 0.26691(7) 1.1533(4) 0.0275(7) Uani 1 1 d . . . B116 B 0.500000 0.500000 0.0690(11) 0.0195(19) Uani 1 2 d S T P C117 C 0.48323(14) 0.53297(12) 0.1939(7) 0.0209(12) Uani 1 1 d . . . C118 C 0.50698(14) 0.55117(14) 0.3074(7) 0.0257(13) Uani 1 1 d . . . C119 C 0.49632(15) 0.57982(13) 0.4135(7) 0.0278(14) Uani 1 1 d . . . C120 C 0.45926(15) 0.59150(14) 0.4159(7) 0.0273(13) Uani 1 1 d . . . C121 C 0.43415(14) 0.57436(14) 0.3124(7) 0.0240(13) Uani 1 1 d . . . C122 C 0.44612(14) 0.54534(13) 0.2070(7) 0.0232(13) Uani 1 1 d . . . C123 C 0.46788(13) 0.48318(13) -0.0659(7) 0.0229(12) Uani 1 1 d . . . C124 C 0.45159(14) 0.50711(14) -0.1847(7) 0.0256(13) Uani 1 1 d . . . C125 C 0.42748(14) 0.49563(14) -0.3087(7) 0.0265(13) Uani 1 1 d . . . C126 C 0.41798(14) 0.45834(15) -0.3220(7) 0.0271(13) Uani 1 1 d . . . C127 C 0.43305(14) 0.43315(14) -0.2107(8) 0.0289(14) Uani 1 1 d . . . C128 C 0.45748(14) 0.44595(13) -0.0884(7) 0.0234(13) Uani 1 1 d . . . F129 F 0.54445(7) 0.54157(7) 0.3077(4) 0.0288(8) Uani 1 1 d . . . F130 F 0.52203(9) 0.59681(8) 0.5153(4) 0.0355(8) Uani 1 1 d . . . F131 F 0.44843(9) 0.61944(8) 0.5198(4) 0.0402(9) Uani 1 1 d . . . F132 F 0.39730(8) 0.58438(8) 0.3130(4) 0.0358(8) Uani 1 1 d . . . F133 F 0.41824(7) 0.52909(8) 0.1157(4) 0.0326(8) Uani 1 1 d . . . F134 F 0.45904(8) 0.54478(7) -0.1779(4) 0.0296(8) Uani 1 1 d . . . F135 F 0.41218(8) 0.52084(8) -0.4178(4) 0.0357(8) Uani 1 1 d . . . F136 F 0.39429(8) 0.44660(9) -0.4445(4) 0.0407(9) Uani 1 1 d . . . F137 F 0.42415(8) 0.39617(8) -0.2215(5) 0.0394(8) Uani 1 1 d . . . F138 F 0.47211(8) 0.41839(7) 0.0100(4) 0.0328(8) Uani 1 1 d . . . B139 B 0.500000 0.000000 0.7929(11) 0.0192(19) Uani 1 2 d S T P C140 C 0.53070(12) 0.02049(13) 0.6654(7) 0.0175(11) Uani 1 1 d . . . C141 C 0.53756(13) 0.05870(13) 0.6470(7) 0.0211(12) Uani 1 1 d . . . C142 C 0.56346(14) 0.07398(13) 0.5382(7) 0.0242(13) Uani 1 1 d . . . C143 C 0.58412(14) 0.05080(14) 0.4348(7) 0.0246(13) Uani 1 1 d . . . C144 C 0.57764(13) 0.01240(14) 0.4429(7) 0.0222(12) Uani 1 1 d . . . C145 C 0.55144(14) -0.00132(13) 0.5541(7) 0.0238(12) Uani 1 1 d . . . C146 C 0.47987(13) 0.03000(12) 0.9269(7) 0.0186(12) Uani 1 1 d . . . C147 C 0.44149(13) 0.03545(13) 0.9519(7) 0.0205(12) Uani 1 1 d . . . C148 C 0.42629(14) 0.05891(14) 1.0724(8) 0.0244(12) Uani 1 1 d . . . C149 C 0.44954(15) 0.07751(13) 1.1827(7) 0.0254(13) Uani 1 1 d . . . C150 C 0.48813(14) 0.07269(13) 1.1666(7) 0.0212(12) Uani 1 1 d . . . C151 C 0.50184(13) 0.04967(13) 1.0410(7) 0.0211(12) Uani 1 1 d . . . F152 F 0.51824(8) 0.08472(7) 0.7380(4) 0.0276(7) Uani 1 1 d . . . F153 F 0.56856(8) 0.11173(7) 0.5287(4) 0.0317(8) Uani 1 1 d . . . F154 F 0.60949(8) 0.06471(8) 0.3243(4) 0.0345(8) Uani 1 1 d . . . F155 F 0.59753(8) -0.01119(8) 0.3421(4) 0.0320(8) Uani 1 1 d . . . F156 F 0.54727(7) -0.03955(7) 0.5581(4) 0.0271(7) Uani 1 1 d . . . F157 F 0.54024(7) 0.04672(7) 1.0325(4) 0.0270(7) Uani 1 1 d . . . F158 F 0.51179(8) 0.09149(8) 1.2694(4) 0.0314(7) Uani 1 1 d . . . F159 F 0.43584(8) 0.10037(7) 1.3025(4) 0.0329(8) Uani 1 1 d . . . F160 F 0.38842(7) 0.06316(7) 1.0872(4) 0.0336(8) Uani 1 1 d . . . F161 F 0.41548(7) 0.01691(8) 0.8566(4) 0.0283(8) Uani 1 1 d . . . 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 0.0224(7) 0.0245(7) 0.0202(8) 0.0005(6) 0.0011(7) 0.0007(6) C2 0.018(3) 0.014(2) 0.022(3) -0.001(2) 0.000(2) -0.001(2) C3 0.020(3) 0.029(3) 0.015(3) 0.000(2) -0.002(2) -0.001(2) C4 0.027(3) 0.046(3) 0.023(4) 0.002(3) -0.008(3) -0.001(3) C5 0.030(3) 0.027(3) 0.031(4) 0.009(3) -0.003(3) 0.006(2) C6 0.026(3) 0.037(3) 0.023(4) 0.005(3) -0.001(3) 0.003(2) C7 0.022(3) 0.028(3) 0.012(3) 0.000(2) -0.001(2) 0.001(2) C8 0.024(3) 0.027(3) 0.025(4) -0.001(2) 0.005(3) -0.002(2) C9 0.033(3) 0.033(3) 0.024(4) -0.002(3) -0.001(3) 0.010(3) N10 0.025(2) 0.016(2) 0.013(3) 0.0009(19) -0.001(2) -0.0009(17) C11 0.018(3) 0.024(3) 0.006(3) -0.001(2) 0.000(2) -0.002(2) C12 0.019(3) 0.029(3) 0.017(3) -0.001(2) 0.000(2) 0.004(2) C13 0.026(3) 0.027(3) 0.017(3) 0.002(2) 0.001(2) 0.004(2) C14 0.020(3) 0.029(3) 0.020(3) 0.001(2) -0.003(2) 0.001(2) C15 0.020(3) 0.026(3) 0.018(3) -0.003(2) 0.001(2) -0.001(2) C16 0.015(3) 0.026(3) 0.023(3) 0.000(2) 0.003(2) 0.004(2) C17 0.030(3) 0.017(3) 0.027(4) 0.002(2) -0.005(3) 0.000(2) C18 0.049(4) 0.019(3) 0.041(4) -0.005(3) -0.005(3) -0.002(3) C19 0.032(3) 0.032(3) 0.032(4) 0.008(3) -0.001(3) -0.004(3) C20 0.019(3) 0.023(3) 0.027(4) 0.002(2) -0.003(3) 0.000(2) C21 0.026(3) 0.026(3) 0.031(4) -0.009(3) 0.004(3) -0.001(2) C22 0.034(3) 0.025(3) 0.036(4) 0.002(3) 0.001(3) -0.011(2) O23 0.032(2) 0.037(2) 0.028(3) 0.0010(18) -0.0037(19) 0.0006(17) C24 0.017(3) 0.026(3) 0.021(3) 0.000(2) 0.001(2) -0.001(2) C25 0.019(3) 0.027(3) 0.029(4) 0.001(3) 0.004(3) 0.001(2) C26 0.024(3) 0.031(3) 0.036(4) -0.001(3) -0.003(3) 0.004(2) C27 0.026(3) 0.031(3) 0.034(4) 0.001(3) 0.001(3) 0.013(2) C28 0.034(3) 0.017(3) 0.038(4) -0.005(2) -0.003(3) 0.003(2) C29 0.021(3) 0.026(3) 0.036(4) -0.003(3) -0.009(3) 0.001(2) C30 0.014(3) 0.027(3) 0.025(3) 0.005(2) 0.000(2) 0.003(2) C31 0.031(3) 0.034(3) 0.029(4) 0.002(3) 0.001(3) 0.005(3) C32 0.026(3) 0.034(3) 0.034(4) 0.008(3) 0.006(3) 0.000(3) C33 0.030(3) 0.026(3) 0.047(5) 0.013(3) -0.003(3) -0.005(2) C34 0.025(3) 0.025(3) 0.045(4) -0.002(3) 0.000(3) -0.002(2) C35 0.025(3) 0.031(3) 0.027(4) -0.005(3) -0.004(3) 0.001(2) P36 0.0205(7) 0.0193(7) 0.0167(8) -0.0004(6) -0.0001(6) 0.0020(5) C37 0.005(2) 0.019(3) 0.023(3) 0.002(2) -0.001(2) -0.0005(19) C38 0.018(3) 0.026(3) 0.015(3) 0.000(2) 0.003(2) 0.001(2) C39 0.026(3) 0.031(3) 0.027(4) -0.002(3) 0.008(3) 0.004(2) C40 0.038(3) 0.022(3) 0.028(4) -0.006(2) -0.006(3) -0.005(2) C41 0.023(3) 0.029(3) 0.017(3) -0.001(2) 0.000(2) 0.003(2) C42 0.020(3) 0.022(3) 0.012(3) 0.000(2) -0.001(2) 0.001(2) C43 0.022(3) 0.027(3) 0.017(3) 0.002(2) -0.001(2) 0.001(2) C44 0.020(3) 0.032(3) 0.018(3) 0.005(2) 0.002(2) 0.001(2) N45 0.010(2) 0.025(2) 0.016(3) -0.0023(19) -0.0015(19) 0.0001(17) C46 0.024(3) 0.015(2) 0.013(3) 0.000(2) 0.001(2) 0.002(2) C47 0.022(3) 0.015(2) 0.014(3) 0.002(2) -0.001(2) -0.001(2) C48 0.020(3) 0.019(3) 0.019(3) 0.002(2) 0.001(2) 0.008(2) C49 0.030(3) 0.016(3) 0.012(3) 0.000(2) -0.004(2) 0.001(2) C50 0.021(3) 0.018(3) 0.017(3) -0.002(2) -0.005(2) -0.002(2) C51 0.019(3) 0.016(2) 0.015(3) 0.009(2) 0.000(2) -0.002(2) C52 0.020(3) 0.023(3) 0.021(3) -0.004(2) 0.003(2) 0.003(2) C53 0.017(3) 0.036(3) 0.027(4) -0.005(3) 0.007(2) 0.003(2) C54 0.025(3) 0.038(3) 0.023(4) 0.004(3) 0.006(3) -0.005(2) C55 0.013(3) 0.018(3) 0.029(4) -0.009(2) 0.001(2) 0.001(2) C56 0.020(3) 0.030(3) 0.040(4) -0.008(3) -0.011(3) 0.002(2) C57 0.022(3) 0.037(3) 0.031(4) -0.004(3) 0.005(3) -0.006(2) O58 0.026(2) 0.0211(18) 0.018(2) -0.0049(16) 0.0017(17) 0.0015(15) C59 0.021(3) 0.015(2) 0.018(3) -0.002(2) 0.003(2) 0.002(2) C60 0.027(3) 0.018(3) 0.041(4) -0.003(3) -0.005(3) 0.002(2) C61 0.020(3) 0.029(3) 0.053(5) -0.005(3) 0.001(3) 0.006(2) C62 0.023(3) 0.031(3) 0.043(4) -0.008(3) 0.005(3) 0.010(2) C63 0.036(3) 0.018(3) 0.034(4) -0.004(2) 0.003(3) 0.004(2) C64 0.021(3) 0.021(3) 0.025(3) 0.000(2) -0.001(2) 0.000(2) C65 0.028(3) 0.017(3) 0.021(3) -0.004(2) 0.005(3) 0.001(2) C66 0.023(3) 0.023(3) 0.044(4) -0.002(3) -0.004(3) 0.001(2) C67 0.020(3) 0.035(3) 0.059(5) -0.009(3) -0.004(3) -0.002(3) C68 0.028(3) 0.032(3) 0.059(5) -0.013(3) 0.020(3) -0.012(3) C69 0.040(4) 0.025(3) 0.047(4) -0.002(3) 0.014(3) -0.009(3) C70 0.038(3) 0.019(3) 0.031(4) -0.007(3) 0.010(3) 0.003(2) B71 0.016(3) 0.017(3) 0.027(4) -0.002(3) 0.002(3) 0.001(2) C72 0.012(2) 0.024(3) 0.021(3) -0.001(2) 0.000(2) 0.002(2) C73 0.021(3) 0.017(3) 0.024(3) -0.001(2) 0.002(3) 0.002(2) C74 0.016(3) 0.028(3) 0.035(4) 0.006(3) 0.003(3) -0.002(2) C75 0.014(3) 0.035(3) 0.026(4) -0.001(3) 0.007(2) 0.002(2) C76 0.020(3) 0.028(3) 0.020(3) -0.008(3) -0.002(2) 0.003(2) C77 0.016(3) 0.023(3) 0.024(3) 0.001(2) -0.001(2) -0.003(2) C78 0.010(2) 0.022(3) 0.023(3) -0.005(2) 0.000(2) -0.003(2) C79 0.023(3) 0.021(3) 0.021(3) -0.005(2) 0.007(3) -0.007(2) C80 0.020(3) 0.021(3) 0.033(4) 0.001(3) -0.002(3) -0.003(2) C81 0.030(3) 0.022(3) 0.024(3) 0.003(2) 0.000(3) -0.007(2) C82 0.024(3) 0.030(3) 0.022(3) -0.003(3) 0.004(3) -0.008(2) C83 0.020(3) 0.018(3) 0.027(3) -0.001(2) 0.004(2) 0.003(2) C84 0.013(3) 0.022(3) 0.025(3) -0.001(2) 0.005(2) 0.003(2) C85 0.023(3) 0.030(3) 0.017(3) 0.004(2) 0.003(3) 0.002(2) C86 0.018(3) 0.039(3) 0.030(4) -0.007(3) 0.000(3) -0.005(2) C87 0.017(3) 0.042(3) 0.028(4) 0.003(3) 0.000(3) 0.007(2) C88 0.027(3) 0.030(3) 0.022(3) 0.003(3) 0.002(3) 0.007(2) C89 0.020(3) 0.020(3) 0.030(4) -0.004(2) 0.001(3) 0.003(2) C90 0.017(3) 0.021(3) 0.021(3) 0.002(2) 0.010(2) -0.001(2) C91 0.019(3) 0.024(3) 0.032(4) -0.002(3) 0.002(3) 0.001(2) C92 0.034(3) 0.022(3) 0.028(4) -0.001(2) 0.008(3) 0.007(2) C93 0.038(3) 0.028(3) 0.022(4) -0.005(3) 0.005(3) -0.007(3) C94 0.024(3) 0.031(3) 0.026(4) -0.004(3) -0.003(3) -0.003(2) C95 0.018(3) 0.020(3) 0.027(3) 0.000(2) 0.005(2) 0.004(2) F96 0.0265(17) 0.0185(15) 0.039(2) -0.0055(14) 0.0103(15) -0.0033(13) F97 0.0233(17) 0.0327(17) 0.059(3) -0.0058(17) 0.0164(17) -0.0108(14) F98 0.0274(18) 0.050(2) 0.048(2) -0.0117(18) 0.0160(18) -0.0041(15) F99 0.0292(18) 0.0372(18) 0.038(2) -0.0155(16) 0.0022(16) 0.0004(14) F100 0.0230(16) 0.0302(17) 0.036(2) -0.0088(15) 0.0028(15) -0.0072(13) F101 0.0205(16) 0.0267(15) 0.032(2) 0.0026(14) 0.0037(14) 0.0045(12) F102 0.0317(17) 0.0220(15) 0.044(2) 0.0038(15) -0.0011(16) 0.0096(13) F103 0.0396(19) 0.0287(17) 0.043(2) 0.0147(16) 0.0076(17) 0.0010(14) F104 0.0317(18) 0.0405(18) 0.031(2) 0.0065(15) 0.0127(16) -0.0047(14) F105 0.0189(16) 0.0325(16) 0.034(2) 0.0021(15) 0.0081(14) 0.0056(13) F106 0.0299(17) 0.0278(16) 0.030(2) 0.0044(14) -0.0048(15) -0.0101(13) F107 0.0277(17) 0.0469(19) 0.042(2) -0.0036(17) -0.0062(16) -0.0143(15) F108 0.0312(18) 0.054(2) 0.042(2) 0.0042(18) -0.0140(17) 0.0008(16) F109 0.042(2) 0.0398(19) 0.042(2) 0.0146(17) -0.0089(17) 0.0063(15) F110 0.0262(17) 0.0247(16) 0.037(2) 0.0078(14) -0.0037(15) -0.0039(13) F111 0.0224(17) 0.0363(17) 0.038(2) -0.0024(15) 0.0005(15) 0.0088(13) F112 0.043(2) 0.0350(18) 0.048(2) -0.0087(16) 0.0080(18) 0.0163(15) F113 0.055(2) 0.0350(18) 0.044(3) -0.0205(17) 0.0031(19) -0.0005(16) F114 0.0322(19) 0.0418(18) 0.037(2) -0.0098(16) -0.0097(16) -0.0031(15) F115 0.0236(16) 0.0246(15) 0.034(2) -0.0044(14) -0.0070(14) 0.0041(13) B116 0.022(5) 0.020(4) 0.016(5) 0.000 0.000 -0.002(3) C117 0.026(3) 0.015(3) 0.021(3) 0.002(2) 0.004(2) -0.004(2) C118 0.023(3) 0.026(3) 0.028(4) 0.001(3) -0.004(3) -0.002(2) C119 0.041(4) 0.020(3) 0.022(4) 0.003(2) -0.009(3) -0.010(2) C120 0.037(3) 0.020(3) 0.025(4) -0.001(2) 0.004(3) 0.003(2) C121 0.022(3) 0.025(3) 0.024(4) 0.002(2) 0.005(2) 0.002(2) C122 0.024(3) 0.018(3) 0.027(4) 0.000(2) -0.005(3) -0.004(2) C123 0.020(3) 0.026(3) 0.022(3) -0.001(2) 0.005(2) -0.001(2) C124 0.020(3) 0.027(3) 0.030(4) -0.010(3) 0.004(3) -0.004(2) C125 0.024(3) 0.034(3) 0.022(4) 0.003(3) 0.002(3) 0.001(2) C126 0.018(3) 0.041(3) 0.022(4) -0.014(3) 0.000(3) -0.005(2) C127 0.023(3) 0.027(3) 0.036(4) -0.007(3) 0.008(3) -0.006(2) C128 0.023(3) 0.022(3) 0.025(4) -0.002(2) 0.003(3) 0.004(2) F129 0.0207(16) 0.0290(16) 0.037(2) -0.0020(14) -0.0095(15) -0.0008(13) F130 0.0439(19) 0.0259(16) 0.037(2) -0.0044(14) -0.0179(17) -0.0045(14) F131 0.051(2) 0.0313(17) 0.039(2) -0.0113(16) 0.0014(17) 0.0045(15) F132 0.0281(18) 0.0355(18) 0.044(2) -0.0059(16) 0.0089(16) 0.0059(14) F133 0.0218(16) 0.0377(17) 0.038(2) -0.0090(16) -0.0023(15) -0.0028(13) F134 0.0306(17) 0.0198(15) 0.038(2) 0.0023(14) -0.0059(15) -0.0028(13) F135 0.0323(18) 0.0448(19) 0.030(2) 0.0049(16) -0.0051(16) 0.0018(14) F136 0.0316(18) 0.059(2) 0.032(2) -0.0174(17) -0.0056(16) -0.0099(15) F137 0.0408(19) 0.0302(17) 0.047(2) -0.0152(16) 0.0026(18) -0.0133(14) F138 0.0399(19) 0.0193(15) 0.039(2) -0.0012(14) -0.0023(16) -0.0044(13) B139 0.017(4) 0.020(4) 0.021(5) 0.000 0.000 0.001(3) C140 0.012(3) 0.023(3) 0.017(3) 0.002(2) -0.002(2) -0.001(2) C141 0.013(3) 0.025(3) 0.025(3) -0.001(2) -0.003(2) 0.001(2) C142 0.022(3) 0.019(3) 0.031(4) 0.003(2) -0.003(3) -0.002(2) C143 0.017(3) 0.034(3) 0.023(4) 0.001(3) 0.003(2) -0.006(2) C144 0.011(3) 0.038(3) 0.018(3) -0.004(3) 0.000(2) 0.007(2) C145 0.021(3) 0.022(3) 0.028(4) -0.002(2) -0.006(3) 0.001(2) C146 0.019(3) 0.012(2) 0.025(3) 0.002(2) 0.000(2) 0.005(2) C147 0.018(3) 0.018(3) 0.025(3) 0.005(2) -0.002(2) -0.005(2) C148 0.020(3) 0.027(3) 0.027(3) 0.006(3) 0.005(3) 0.008(2) C149 0.033(3) 0.020(3) 0.023(4) 0.004(2) 0.008(3) 0.006(2) C150 0.029(3) 0.015(3) 0.019(3) 0.001(2) -0.005(3) 0.002(2) C151 0.014(3) 0.020(3) 0.030(4) 0.003(2) -0.001(2) 0.004(2) F152 0.0281(16) 0.0175(15) 0.037(2) 0.0006(14) 0.0089(15) 0.0067(13) F153 0.0330(18) 0.0220(16) 0.040(2) 0.0070(14) 0.0025(15) -0.0039(13) F154 0.0282(18) 0.0466(19) 0.029(2) 0.0023(16) 0.0075(15) -0.0069(15) F155 0.0261(17) 0.0412(18) 0.029(2) -0.0130(15) 0.0067(14) 0.0037(14) F156 0.0234(16) 0.0205(15) 0.037(2) -0.0048(14) -0.0003(15) 0.0013(12) F157 0.0179(16) 0.0286(16) 0.035(2) -0.0049(14) -0.0034(14) 0.0040(12) F158 0.0371(18) 0.0288(16) 0.028(2) -0.0062(14) -0.0067(17) 0.0052(14) F159 0.0426(19) 0.0292(17) 0.027(2) -0.0012(14) 0.0115(16) 0.0119(14) F160 0.0216(16) 0.0355(17) 0.044(2) 0.0019(16) 0.0121(16) 0.0099(13) F161 0.0171(15) 0.0315(17) 0.036(2) 0.0006(15) 0.0003(14) 0.0028(13) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 O23 P1 C30 114.6(2) . . O23 P1 C24 112.4(2) . . C30 P1 C24 109.7(2) . . O23 P1 C2 111.2(2) . . C30 P1 C2 104.3(2) . . C24 P1 C2 103.8(2) . . N10 C2 C3 111.4(4) . . N10 C2 P1 121.3(4) . . C3 C2 P1 127.3(3) . . C2 C3 C6 102.1(4) . . C2 C3 C4 117.7(4) . . C6 C3 C4 110.3(4) . . C2 C3 C5 107.9(4) . . C6 C3 C5 111.9(4) . . C4 C3 C5 106.9(4) . . C3 C4 H4A 109.5 . . C3 C4 H4B 109.5 . . H4A C4 H4B 109.5 . . C3 C4 H4C 109.5 . . H4A C4 H4C 109.5 . . H4B C4 H4C 109.5 . . C3 C5 H5A 109.5 . . C3 C5 H5B 109.5 . . H5A C5 H5B 109.5 . . C3 C5 H5C 109.5 . . H5A C5 H5C 109.5 . . H5B C5 H5C 109.5 . . C7 C6 C3 107.0(5) . . C7 C6 H6A 110.3 . . C3 C6 H6A 110.3 . . C7 C6 H6AB 110.3 . . C3 C6 H6AB 110.3 . . H6A C6 H6AB 108.6 . . C9 C7 C6 110.2(4) . . C9 C7 C8 110.0(4) . . C6 C7 C8 115.3(4) . . C9 C7 N10 110.2(4) . . C6 C7 N10 101.2(4) . . C8 C7 N10 109.5(4) . . C7 C8 H8A 109.5 . . C7 C8 H8B 109.5 . . H8A C8 H8B 109.5 . . C7 C8 H8C 109.5 . . H8A C8 H8C 109.5 . . H8B C8 H8C 109.5 . . C7 C9 H9A 109.5 . . C7 C9 H9B 109.5 . . H9A C9 H9B 109.5 . . C7 C9 H9C 109.5 . . H9A C9 H9C 109.5 . . H9B C9 H9C 109.5 . . C2 N10 C11 129.3(4) . . C2 N10 C7 112.8(4) . . C11 N10 C7 117.8(3) . . C16 C11 C12 122.6(5) . . C16 C11 N10 119.3(4) . . C12 C11 N10 117.6(4) . . C13 C12 C11 117.0(5) . . C13 C12 C17 116.4(4) . . C11 C12 C17 126.4(4) . . C14 C13 C12 122.0(5) . . C14 C13 H13 119.0 . . C12 C13 H13 119.0 . . C15 C14 C13 118.4(5) . . C15 C14 H14 120.8 . . C13 C14 H14 120.8 . . C14 C15 C16 122.8(5) . . C14 C15 H15 118.6 . . C16 C15 H15 118.6 . . C15 C16 C11 117.1(4) . . C15 C16 C20 116.3(4) . . C11 C16 C20 126.4(4) . . C12 C17 C18 113.4(4) . . C12 C17 C19 109.6(4) . . C18 C17 C19 109.3(4) . . C12 C17 H17 108.1 . . C18 C17 H17 108.1 . . C19 C17 H17 108.1 . . C17 C18 H18A 109.5 . . C17 C18 H18B 109.5 . . H18A C18 H18B 109.5 . . C17 C18 H18C 109.5 . . H18A C18 H18C 109.5 . . H18B C18 H18C 109.5 . . C17 C19 H19A 109.5 . . C17 C19 H19B 109.5 . . H19A C19 H19B 109.5 . . C17 C19 H19C 109.5 . . H19A C19 H19C 109.5 . . H19B C19 H19C 109.5 . . C21 C20 C22 107.7(4) . . C21 C20 C16 108.9(4) . . C22 C20 C16 114.1(4) . . C21 C20 H20 108.7 . . C22 C20 H20 108.7 . . C16 C20 H20 108.7 . . C20 C21 H21A 109.5 . . C20 C21 H21B 109.5 . . H21A C21 H21B 109.5 . . C20 C21 H21C 109.5 . . H21A C21 H21C 109.5 . . H21B C21 H21C 109.5 . . C20 C22 H22A 109.5 . . C20 C22 H22B 109.5 . . H22A C22 H22B 109.5 . . C20 C22 H22C 109.5 . . H22A C22 H22C 109.5 . . H22B C22 H22C 109.5 . . C25 C24 C29 119.4(4) . . C25 C24 P1 123.5(4) . . C29 C24 P1 117.1(4) . . C26 C25 C24 119.9(5) . . C26 C25 H25 120.0 . . C24 C25 H25 120.0 . . C27 C26 C25 120.0(5) . . C27 C26 H26 120.0 . . C25 C26 H26 120.0 . . C28 C27 C26 120.5(5) . . C28 C27 H27 119.7 . . C26 C27 H27 119.7 . . C27 C28 C29 119.9(5) . . C27 C28 H28 120.1 . . C29 C28 H28 120.1 . . C28 C29 C24 120.1(5) . . C28 C29 H29 120.0 . . C24 C29 H29 120.0 . . C35 C30 C31 118.8(5) . . C35 C30 P1 124.3(4) . . C31 C30 P1 116.4(4) . . C32 C31 C30 121.1(5) . . C32 C31 H31 119.4 . . C30 C31 H31 119.4 . . C31 C32 C33 119.6(5) . . C31 C32 H32 120.2 . . C33 C32 H32 120.2 . . C34 C33 C32 120.9(5) . . C34 C33 H33 119.5 . . C32 C33 H33 119.5 . . C33 C34 C35 119.0(5) . . C33 C34 H34 120.5 . . C35 C34 H34 120.5 . . C30 C35 C34 120.6(5) . . C30 C35 H35 119.7 . . C34 C35 H35 119.7 . . O58 P36 C65 115.8(2) . . O58 P36 C59 112.4(2) . . C65 P36 C59 108.8(2) . . O58 P36 C37 110.4(2) . . C65 P36 C37 104.0(2) . . C59 P36 C37 104.5(2) . . N45 C37 C38 111.5(4) . . N45 C37 P36 121.4(4) . . C38 C37 P36 127.0(3) . . C37 C38 C41 101.3(4) . . C37 C38 C40 117.0(4) . . C41 C38 C40 109.6(4) . . C37 C38 C39 108.7(4) . . C41 C38 C39 112.9(4) . . C40 C38 C39 107.5(4) . . C38 C39 H39A 109.5 . . C38 C39 H39B 109.5 . . H39A C39 H39B 109.5 . . C38 C39 H39C 109.5 . . H39A C39 H39C 109.5 . . H39B C39 H39C 109.5 . . C38 C40 H40A 109.5 . . C38 C40 H40B 109.5 . . H40A C40 H40B 109.5 . . C38 C40 H40C 109.5 . . H40A C40 H40C 109.5 . . H40B C40 H40C 109.5 . . C42 C41 C38 107.1(4) . . C42 C41 H41A 110.3 . . C38 C41 H41A 110.3 . . C42 C41 H41B 110.3 . . C38 C41 H41B 110.3 . . H41A C41 H41B 108.5 . . C41 C42 C43 112.1(4) . . C41 C42 C44 114.8(4) . . C43 C42 C44 108.8(4) . . C41 C42 N45 100.4(4) . . C43 C42 N45 111.2(4) . . C44 C42 N45 109.4(4) . . C42 C43 H43A 109.5 . . C42 C43 H43B 109.5 . . H43A C43 H43B 109.5 . . C42 C43 H43C 109.5 . . H43A C43 H43C 109.5 . . H43B C43 H43C 109.5 . . C42 C44 H44A 109.5 . . C42 C44 H44B 109.5 . . H44A C44 H44B 109.5 . . C42 C44 H44C 109.5 . . H44A C44 H44C 109.5 . . H44B C44 H44C 109.5 . . C37 N45 C46 129.9(4) . . C37 N45 C42 112.4(4) . . C46 N45 C42 117.7(3) . . C47 C46 C51 123.1(4) . . C47 C46 N45 117.8(4) . . C51 C46 N45 118.8(4) . . C48 C47 C46 117.4(4) . . C48 C47 C52 117.1(4) . . C46 C47 C52 125.4(4) . . C49 C48 C47 121.5(4) . . C49 C48 H48 119.3 . . C47 C48 H48 119.3 . . C50 C49 C48 119.8(5) . . C50 C49 H49 120.1 . . C48 C49 H49 120.1 . . C49 C50 C51 122.0(4) . . C49 C50 H50 119.0 . . C51 C50 H50 119.0 . . C50 C51 C46 116.2(4) . . C50 C51 C55 116.1(4) . . C46 C51 C55 127.5(4) . . C47 C52 C53 112.9(4) . . C47 C52 C54 110.0(4) . . C53 C52 C54 109.0(4) . . C47 C52 H52 108.3 . . C53 C52 H52 108.3 . . C54 C52 H52 108.3 . . 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 . . C51 C55 C56 108.9(4) . . C51 C55 C57 113.1(4) . . C56 C55 C57 108.1(4) . . C51 C55 H55 108.9 . . C56 C55 H55 108.9 . . C57 C55 H55 108.9 . . C55 C56 H56A 109.5 . . C55 C56 H56B 109.5 . . H56A C56 H56B 109.5 . . C55 C56 H56C 109.5 . . H56A C56 H56C 109.5 . . H56B C56 H56C 109.5 . . C55 C57 H57A 109.5 . . C55 C57 H57B 109.5 . . H57A C57 H57B 109.5 . . C55 C57 H57C 109.5 . . H57A C57 H57C 109.5 . . H57B C57 H57C 109.5 . . C60 C59 C64 119.0(4) . . C60 C59 P36 116.7(3) . . C64 C59 P36 124.3(4) . . C61 C60 C59 120.5(5) . . C61 C60 H60 119.7 . . C59 C60 H60 119.7 . . C62 C61 C60 119.8(5) . . C62 C61 H61 120.1 . . C60 C61 H61 120.1 . . C61 C62 C63 120.3(5) . . C61 C62 H62 119.8 . . C63 C62 H62 119.8 . . C62 C63 C64 119.9(5) . . C62 C63 H63 120.1 . . C64 C63 H63 120.1 . . C63 C64 C59 120.4(5) . . C63 C64 H64 119.8 . . C59 C64 H64 119.8 . . C66 C65 C70 118.6(5) . . C66 C65 P36 124.4(4) . . C70 C65 P36 116.6(4) . . C67 C66 C65 119.8(5) . . C67 C66 H66 120.1 . . C65 C66 H66 120.1 . . C68 C67 C66 120.3(6) . . C68 C67 H67 119.8 . . C66 C67 H67 119.8 . . C69 C68 C67 121.0(5) . . C69 C68 H68 119.5 . . C67 C68 H68 119.5 . . C68 C69 C70 119.5(6) . . C68 C69 H69 120.2 . . C70 C69 H69 120.2 . . C69 C70 C65 120.7(5) . . C69 C70 H70 119.7 . . C65 C70 H70 119.7 . . C78 B71 C90 104.4(5) . . C78 B71 C72 111.8(4) . . C90 B71 C72 113.0(4) . . C78 B71 C84 112.7(4) . . C90 B71 C84 112.9(4) . . C72 B71 C84 102.3(4) . . C73 C72 C77 112.9(4) . . C73 C72 B71 128.0(4) . . C77 C72 B71 119.0(4) . . F96 C73 C74 114.6(4) . . F96 C73 C72 120.7(4) . . C74 C73 C72 124.7(5) . . F97 C74 C75 120.3(5) . . F97 C74 C73 120.5(5) . . C75 C74 C73 119.1(4) . . C74 C75 C76 120.1(5) . . C74 C75 F98 120.2(4) . . C76 C75 F98 119.6(5) . . F99 C76 C75 120.5(5) . . F99 C76 C77 120.5(4) . . C75 C76 C77 119.0(5) . . F100 C77 C72 120.2(4) . . F100 C77 C76 115.6(4) . . C72 C77 C76 124.1(4) . . C79 C78 C83 111.7(5) . . C79 C78 B71 127.9(4) . . C83 C78 B71 120.1(4) . . F101 C79 C80 113.9(4) . . F101 C79 C78 120.9(4) . . C80 C79 C78 125.3(5) . . F102 C80 C81 119.9(5) . . F102 C80 C79 120.6(5) . . C81 C80 C79 119.4(5) . . F103 C81 C82 120.8(5) . . F103 C81 C80 120.7(4) . . C82 C81 C80 118.5(5) . . F104 C82 C83 120.6(4) . . F104 C82 C81 119.3(5) . . C83 C82 C81 120.0(5) . . F105 C83 C82 116.7(4) . . F105 C83 C78 118.3(4) . . C82 C83 C78 125.0(4) . . C89 C84 C85 112.2(5) . . C89 C84 B71 120.0(4) . . C85 C84 B71 127.8(4) . . F106 C85 C86 114.7(4) . . F106 C85 C84 120.6(4) . . C86 C85 C84 124.6(5) . . F107 C86 C87 120.0(5) . . F107 C86 C85 120.6(5) . . C87 C86 C85 119.4(5) . . F108 C87 C86 119.9(5) . . F108 C87 C88 120.8(5) . . C86 C87 C88 119.2(5) . . F109 C88 C87 119.7(5) . . F109 C88 C89 121.4(5) . . C87 C88 C89 118.9(5) . . F110 C89 C88 115.6(4) . . F110 C89 C84 118.8(4) . . C88 C89 C84 125.6(5) . . C91 C90 C95 112.4(5) . . C91 C90 B71 128.4(5) . . C95 C90 B71 119.1(4) . . F111 C91 C92 115.3(4) . . F111 C91 C90 120.8(5) . . C92 C91 C90 123.8(5) . . F112 C92 C93 118.7(5) . . F112 C92 C91 120.2(5) . . C93 C92 C91 121.1(5) . . F113 C93 C92 121.9(5) . . F113 C93 C94 120.3(5) . . C92 C93 C94 117.7(5) . . F114 C94 C95 121.2(5) . . F114 C94 C93 119.2(5) . . C95 C94 C93 119.6(5) . . F115 C95 C94 115.6(4) . . F115 C95 C90 118.9(4) . . C94 C95 C90 125.3(4) . . C117 B116 C117 105.8(6) . 2_665 C117 B116 C123 113.2(2) . . C117 B116 C123 112.2(2) 2_665 . C117 B116 C123 112.2(2) . 2_665 C117 B116 C123 113.2(2) 2_665 2_665 C123 B116 C123 100.4(6) . 2_665 C122 C117 C118 112.1(4) . . C122 C117 B116 127.7(4) . . C118 C117 B116 120.1(4) . . F129 C118 C119 116.7(5) . . F129 C118 C117 118.2(5) . . C119 C118 C117 125.0(5) . . F130 C119 C118 120.6(5) . . F130 C119 C120 119.9(5) . . C118 C119 C120 119.6(5) . . F131 C120 C121 121.0(5) . . F131 C120 C119 120.1(5) . . C121 C120 C119 118.9(5) . . F132 C121 C120 120.9(5) . . F132 C121 C122 119.4(5) . . C120 C121 C122 119.7(5) . . F133 C122 C117 121.0(4) . . F133 C122 C121 114.5(4) . . C117 C122 C121 124.5(5) . . C128 C123 C124 112.6(5) . . C128 C123 B116 127.2(4) . . C124 C123 B116 119.8(4) . . F134 C124 C125 116.2(5) . . F134 C124 C123 119.3(5) . . C125 C124 C123 124.4(5) . . F135 C125 C124 120.9(5) . . F135 C125 C126 119.3(5) . . C124 C125 C126 119.9(5) . . F136 C126 C127 120.5(5) . . F136 C126 C125 120.4(5) . . C127 C126 C125 119.1(5) . . F137 C127 C126 120.2(5) . . F137 C127 C128 120.8(5) . . C126 C127 C128 119.1(5) . . F138 C128 C127 114.1(4) . . F138 C128 C123 120.8(5) . . C127 C128 C123 125.0(5) . . C140 B139 C140 104.6(6) 2_655 . C140 B139 C146 113.1(2) 2_655 2_655 C140 B139 C146 113.0(2) . 2_655 C140 B139 C146 113.0(2) 2_655 . C140 B139 C146 113.1(2) . . C146 B139 C146 100.6(6) 2_655 . C141 C140 C145 112.7(5) . . C141 C140 B139 127.6(4) . . C145 C140 B139 119.6(4) . . F152 C141 C142 113.8(4) . . F152 C141 C140 121.3(4) . . C142 C141 C140 124.8(5) . . F153 C142 C141 121.0(5) . . F153 C142 C143 119.2(5) . . C141 C142 C143 119.8(4) . . F154 C143 C142 121.6(4) . . F154 C143 C144 120.1(5) . . C142 C143 C144 118.3(5) . . F155 C144 C145 120.9(4) . . F155 C144 C143 119.6(5) . . C145 C144 C143 119.5(5) . . F156 C145 C144 116.2(5) . . F156 C145 C140 118.9(5) . . C144 C145 C140 124.9(5) . . C151 C146 C147 112.8(5) . . C151 C146 B139 120.0(4) . . C147 C146 B139 126.9(4) . . F161 C147 C148 114.4(4) . . F161 C147 C146 121.1(5) . . C148 C147 C146 124.5(5) . . F160 C148 C149 119.1(5) . . F160 C148 C147 121.0(5) . . C149 C148 C147 120.0(5) . . F159 C149 C148 121.8(5) . . F159 C149 C150 119.9(5) . . C148 C149 C150 118.4(5) . . F158 C150 C151 120.8(4) . . F158 C150 C149 119.9(4) . . C151 C150 C149 119.3(5) . . F157 C151 C150 115.6(4) . . F157 C151 C146 119.3(4) . . C150 C151 C146 125.1(5) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 P1 O23 1.469(4) . P1 C30 1.791(5) . P1 C24 1.799(5) . P1 C2 1.881(5) . C2 N10 1.296(6) . C2 C3 1.524(7) . C3 C6 1.537(7) . C3 C4 1.545(7) . C3 C5 1.556(6) . C4 H4A 0.9800 . C4 H4B 0.9800 . C4 H4C 0.9800 . C5 H5A 0.9800 . C5 H5B 0.9800 . C5 H5C 0.9800 . C6 C7 1.521(7) . C6 H6A 0.9900 . C6 H6AB 0.9900 . C7 C9 1.515(6) . C7 C8 1.531(6) . C7 N10 1.553(7) . C8 H8A 0.9800 . C8 H8B 0.9800 . C8 H8C 0.9800 . C9 H9A 0.9800 . C9 H9B 0.9800 . C9 H9C 0.9800 . N10 C11 1.488(6) . C11 C16 1.399(6) . C11 C12 1.403(6) . C12 C13 1.399(7) . C12 C17 1.517(7) . C13 C14 1.393(7) . C13 H13 0.9500 . C14 C15 1.382(6) . C14 H14 0.9500 . C15 C16 1.389(7) . C15 H15 0.9500 . C16 C20 1.541(6) . C17 C18 1.529(7) . C17 C19 1.547(7) . C17 H17 1.0000 . C18 H18A 0.9800 . C18 H18B 0.9800 . C18 H18C 0.9800 . C19 H19A 0.9800 . C19 H19B 0.9800 . C19 H19C 0.9800 . C20 C21 1.534(7) . C20 C22 1.535(7) . C20 H20 1.0000 . C21 H21A 0.9800 . C21 H21B 0.9800 . C21 H21C 0.9800 . C22 H22A 0.9800 . C22 H22B 0.9800 . C22 H22C 0.9800 . C24 C25 1.394(7) . C24 C29 1.398(7) . C25 C26 1.387(7) . C25 H25 0.9500 . C26 C27 1.383(7) . C26 H26 0.9500 . C27 C28 1.380(7) . C27 H27 0.9500 . C28 C29 1.387(7) . C28 H28 0.9500 . C29 H29 0.9500 . C30 C35 1.393(7) . C30 C31 1.399(7) . C31 C32 1.376(7) . C31 H31 0.9500 . C32 C33 1.401(8) . C32 H32 0.9500 . C33 C34 1.376(8) . C33 H33 0.9500 . C34 C35 1.414(7) . C34 H34 0.9500 . C35 H35 0.9500 . P36 O58 1.472(4) . P36 C65 1.792(5) . P36 C59 1.799(5) . P36 C37 1.884(5) . C37 N45 1.297(6) . C37 C38 1.520(7) . C38 C41 1.527(7) . C38 C40 1.547(6) . C38 C39 1.556(6) . C39 H39A 0.9800 . C39 H39B 0.9800 . C39 H39C 0.9800 . C40 H40A 0.9800 . C40 H40B 0.9800 . C40 H40C 0.9800 . C41 C42 1.515(7) . C41 H41A 0.9900 . C41 H41B 0.9900 . C42 C43 1.527(6) . C42 C44 1.529(6) . C42 N45 1.552(7) . C43 H43A 0.9800 . C43 H43B 0.9800 . C43 H43C 0.9800 . C44 H44A 0.9800 . C44 H44B 0.9800 . C44 H44C 0.9800 . N45 C46 1.491(6) . C46 C47 1.406(6) . C46 C51 1.413(6) . C47 C48 1.389(7) . C47 C52 1.524(6) . C48 C49 1.388(6) . C48 H48 0.9500 . C49 C50 1.383(6) . C49 H49 0.9500 . C50 C51 1.402(6) . C50 H50 0.9500 . C51 C55 1.520(6) . C52 C53 1.535(6) . C52 C54 1.539(7) . 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 . C55 C56 1.536(7) . C55 C57 1.538(7) . C55 H55 1.0000 . C56 H56A 0.9800 . C56 H56B 0.9800 . C56 H56C 0.9800 . C57 H57A 0.9800 . C57 H57B 0.9800 . C57 H57C 0.9800 . C59 C60 1.390(6) . C59 C64 1.393(6) . C60 C61 1.384(7) . C60 H60 0.9500 . C61 C62 1.379(7) . C61 H61 0.9500 . C62 C63 1.381(7) . C62 H62 0.9500 . C63 C64 1.381(7) . C63 H63 0.9500 . C64 H64 0.9500 . C65 C66 1.393(7) . C65 C70 1.403(7) . C66 C67 1.382(7) . C66 H66 0.9500 . C67 C68 1.374(8) . C67 H67 0.9500 . C68 C69 1.367(8) . C68 H68 0.9500 . C69 C70 1.378(7) . C69 H69 0.9500 . C70 H70 0.9500 . B71 C78 1.640(8) . B71 C90 1.652(8) . B71 C72 1.663(7) . B71 C84 1.670(8) . C72 C73 1.386(6) . C72 C77 1.388(7) . C73 F96 1.364(5) . C73 C74 1.384(7) . C74 F97 1.353(5) . C74 C75 1.357(7) . C75 C76 1.362(6) . C75 F98 1.367(6) . C76 F99 1.354(5) . C76 C77 1.394(7) . C77 F100 1.359(5) . C78 C79 1.392(6) . C78 C83 1.404(7) . C79 F101 1.361(5) . C79 C80 1.380(7) . C80 F102 1.345(5) . C80 C81 1.376(7) . C81 F103 1.349(6) . C81 C82 1.375(7) . C82 F104 1.358(6) . C82 C83 1.367(7) . C83 F105 1.367(5) . C84 C89 1.385(7) . C84 C85 1.393(6) . C85 F106 1.367(5) . C85 C86 1.382(7) . C86 F107 1.351(5) . C86 C87 1.369(7) . C87 F108 1.359(6) . C87 C88 1.371(7) . C88 F109 1.349(6) . C88 C89 1.377(7) . C89 F110 1.368(5) . C90 C91 1.396(6) . C90 C95 1.398(7) . C91 F111 1.350(6) . C91 C92 1.375(7) . C92 F112 1.360(5) . C92 C93 1.371(8) . C93 F113 1.344(6) . C93 C94 1.387(7) . C94 F114 1.356(6) . C94 C95 1.364(7) . C95 F115 1.363(5) . B116 C117 1.644(7) . B116 C117 1.644(7) 2_665 B116 C123 1.673(8) . B116 C123 1.673(8) 2_665 C117 C122 1.390(7) . C117 C118 1.392(7) . C118 F129 1.371(5) . C118 C119 1.373(7) . C119 F130 1.358(6) . C119 C120 1.377(7) . C120 F131 1.345(6) . C120 C121 1.355(7) . C121 F132 1.354(5) . C121 C122 1.392(7) . C122 F133 1.355(5) . C123 C128 1.382(6) . C123 C124 1.394(7) . C124 F134 1.363(5) . C124 C125 1.366(7) . C125 F135 1.358(6) . C125 C126 1.369(7) . C126 F136 1.351(6) . C126 C127 1.366(8) . C127 F137 1.351(5) . C127 C128 1.378(7) . C128 F138 1.355(6) . B139 C140 1.654(7) 2_655 B139 C140 1.654(7) . B139 C146 1.665(7) 2_655 B139 C146 1.666(7) . C140 C141 1.385(6) . C140 C145 1.386(7) . C141 F152 1.358(5) . C141 C142 1.372(7) . C142 F153 1.353(5) . C142 C143 1.373(7) . C143 F154 1.350(6) . C143 C144 1.383(6) . C144 F155 1.355(5) . C144 C145 1.370(7) . C145 F156 1.364(5) . C146 C151 1.383(7) . C146 C147 1.388(6) . C147 F161 1.362(5) . C147 C148 1.377(7) . C148 F160 1.356(5) . C148 C149 1.372(7) . C149 F159 1.341(6) . C149 C150 1.384(7) . C150 F158 1.347(6) . C150 C151 1.377(7) . C151 F157 1.366(5) .