#------------------------------------------------------------------------------ #$Date: 2024-05-26 01:16:18 +0300 (Sun, 26 May 2024) $ #$Revision: 292040 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/17/1571718.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_1571718 loop_ _publ_author_name 'Chen, Yi-Kuan' 'Lei, Jian' 'Wu, Tien-Lin' _publ_section_title ; Elevating upconversion performance of a multiple resonance thermally activated delayed fluorescence emitter via an embedded azepine approach ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC02351J _journal_year 2024 _chemical_formula_moiety '2(C48 H42 B N3)' _chemical_formula_sum 'C96 H84 B2 N6' _chemical_formula_weight 1343.31 _chemical_name_systematic TTABN _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2023-03-10 _audit_creation_method ; Olex2 1.5 (compiled 2023.02.24 svn.rf166f9f3 for OlexSys, GUI svn.r6725) ; _audit_update_record ; 2024-04-09 deposited with the CCDC. 2024-05-23 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 94.7230(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.7232(2) _cell_length_b 9.88890(10) _cell_length_c 51.6585(6) _cell_measurement_reflns_used 25541 _cell_measurement_temperature 99.98(12) _cell_measurement_theta_max 73.0580 _cell_measurement_theta_min 2.9930 _cell_volume 7495.74(15) _computing_cell_refinement 'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)' _computing_data_collection 'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)' _computing_data_reduction 'CrysAlisPro 1.171.42.58a (Rigaku OD, 2022)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 99.98(12) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type 'HyPix-Arc 150' _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w 24.00 64.00 0.50 3.08 -- 61.89 -95.00 30.00 80 2 \w 24.00 70.00 0.50 3.08 -- 61.89 -95.00 0.00 92 3 \w 24.00 64.00 0.50 3.08 -- 61.89 -95.00-150.00 80 4 \w 24.00 67.00 0.50 3.08 -- 61.89 -95.00 -60.00 86 5 \w 57.00 99.00 0.50 3.08 -- 61.89 0.00 -30.00 84 6 \w 44.00 69.00 0.50 3.08 -- 61.89 -95.00 90.00 50 7 \w 27.00 64.00 0.50 3.08 -- 61.89 -95.00-120.00 74 8 \w 24.00 64.00 0.50 3.08 -- 61.89 -95.00 120.00 80 9 \w 32.00 58.00 0.50 3.08 -- 61.89 -95.00-180.00 52 10 \w -95.00 -36.00 0.50 3.08 -- -64.95 0.00 -90.00 118 11 \w -70.00 -45.00 0.50 3.08 -- -64.95 -15.00 30.00 50 12 \w -105.00 -74.00 0.50 3.08 -- -64.95 -15.00 30.00 62 13 \w 52.00 82.00 0.50 3.08 -- 73.73 -95.00-150.00 60 14 \w 37.00 77.00 0.50 3.08 -- 74.76-125.00 150.00 80 15 \w 57.00 82.00 0.50 3.08 -- 74.76 -95.00 120.00 50 16 \w 37.00 77.00 0.50 3.08 -- 74.76 -95.00-120.00 80 17 \w 36.00 98.00 0.50 3.08 -- 74.76-125.00 30.00 124 18 \w 38.00 64.00 0.50 3.08 -- 74.76 -95.00 -90.00 52 19 \w 56.00 81.00 0.50 3.08 -- 74.76 -95.00-180.00 50 20 \w 39.00 64.00 0.50 3.08 -- 74.76-125.00 -60.00 50 21 \w -120.00 -78.00 0.50 3.08 -- -77.70-125.00 -60.00 84 22 \w -117.00 -75.00 0.50 3.08 -- -77.70-125.00-120.00 84 23 \w -118.00 -92.00 0.50 3.08 -- -77.70-125.00 150.00 52 24 \w -102.00 -75.00 0.50 3.08 -- -77.70-125.00 -30.00 54 25 \w -115.00 -79.00 0.50 3.08 -- -77.70 0.00 90.00 72 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy R, DW system, HyPix-Arc 150' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0518159000 _diffrn_orient_matrix_UB_12 0.1353940000 _diffrn_orient_matrix_UB_13 -0.0020107000 _diffrn_orient_matrix_UB_21 0.0451659000 _diffrn_orient_matrix_UB_22 0.0420794000 _diffrn_orient_matrix_UB_23 0.0267596000 _diffrn_orient_matrix_UB_31 0.0793429000 _diffrn_orient_matrix_UB_32 0.0645390000 _diffrn_orient_matrix_UB_33 -0.0132564000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0282 _diffrn_reflns_av_unetI/netI 0.0264 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 61 _diffrn_reflns_limit_l_min -61 _diffrn_reflns_number 54420 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 67.075 _diffrn_reflns_theta_max 67.075 _diffrn_reflns_theta_min 3.012 _diffrn_source 'Rotating-anode X-ray tube' _diffrn_source_type 'Rigaku (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 0.523 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.87563 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.42.58a (Rigaku Oxford Diffraction, 2022) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.190 _exptl_crystal_description plate _exptl_crystal_F_000 2848 _exptl_crystal_preparation Luminescent _exptl_crystal_recrystallization_method Sublimation _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _refine_diff_density_max 0.360 _refine_diff_density_min -0.276 _refine_diff_density_rms 0.058 _refine_ls_extinction_coef 0.00057(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.118 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 950 _refine_ls_number_reflns 13332 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.118 _refine_ls_R_factor_all 0.0629 _refine_ls_R_factor_gt 0.0539 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0506P)^2^+6.8119P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1342 _refine_ls_wR_factor_ref 0.1385 _reflns_Friedel_coverage 0.000 _reflns_number_gt 11515 _reflns_number_total 13332 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc02351j2.cif _cod_data_source_block 230312lt_auto _cod_original_cell_volume 7495.75(15) _cod_database_code 1571718 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.984 _shelx_estimated_absorpt_t_min 0.959 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Aromatic/amide H refined with riding coordinates: C2(H2), C4(H4), C9(H9), C11(H11), C12(H12), C17(H17), C18(H18), C20(H20), C21(H21), C23(H23), C24(H24), C26(H26), C27(H27), C31(H31), C32(H32), C34(H34), C35(H35), C39(H39), C40(H40), C42(H42), C45(H45), C46(H46), C48(H48), C49(H49), C54(H54), C56(H56), C61(H61), C63(H63), C64(H64), C69(H69), C70(H70), C72(H72), C73(H73), C75(H75), C76(H76), C78(H78), C79(H79), C83(H83), C84(H84), C86(H86), C87(H87), C91(H91), C93(H93), C94(H94), C97(H97), C98(H98), C100(H100), C101(H101) 2.b Idealised Me refined as rotating group: C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C36(H36A,H36B,H36C), C50(H50A,H50B, H50C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C80(H80A,H80B,H80C), C81(H81A, H81B,H81C), C88(H88A,H88B,H88C), C102(H10A,H10B,H10C), C103(H10D,H10E,H10F), C104(H10G,H10H,H10I) ; _shelx_res_file ; TITL 230312lt_auto_a.res in P2(1)/c 230312lt_auto.res created by SHELXL-2018/3 at 15:24:31 on 10-Mar-2023 REM Old TITL 230312LT_auto in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.133, Rweak 0.017, Alpha 0.035 REM 2.567 for 870 systematic absences, Orientation as input REM Formula found by SHELXT: C98 N67 CELL 1.54184 14.7232 9.8889 51.6585 90 94.723 90 ZERR 4 0.0002 0.0001 0.0006 0 0.001 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H B N UNIT 384 336 8 24 L.S. 4 PLAN 7 SIZE 0.08 0.06 0.03 TEMP -173.17(12) CONF fmap 2 MORE -1 BOND $H ACTA SHEL 99 0.837 OMIT 0 0 2 OMIT 7 2 2 OMIT 6 0 2 OMIT 2 2 1 REM REM REM WGHT 0.050600 6.811900 EXTI 0.000568 FVAR 1.31075 B7 3 0.484133 0.717899 0.380187 11.00000 0.02061 0.01622 = 0.02366 -0.00191 0.00297 -0.00015 C1 1 0.618012 0.798469 0.356106 11.00000 0.01749 0.01805 = 0.01911 -0.00171 -0.00093 0.00134 C2 1 0.657812 0.831740 0.333389 11.00000 0.01462 0.02342 = 0.02058 -0.00010 -0.00025 -0.00105 AFIX 43 H2 2 0.721545 0.847648 0.333791 11.00000 -1.20000 AFIX 0 C3 1 0.603478 0.841490 0.310100 11.00000 0.02062 0.01992 = 0.01932 0.00098 0.00110 -0.00030 C4 1 0.509726 0.819159 0.309265 11.00000 0.01862 0.02249 = 0.01990 0.00074 -0.00382 -0.00050 AFIX 43 H4 2 0.472736 0.828506 0.293410 11.00000 -1.20000 AFIX 0 C5 1 0.471030 0.782914 0.332029 11.00000 0.01690 0.01609 = 0.02388 -0.00052 -0.00004 -0.00035 C6 1 0.524056 0.767416 0.356056 11.00000 0.01696 0.01680 = 0.02190 -0.00150 0.00021 0.00041 C8 1 0.553024 0.695003 0.404025 11.00000 0.01982 0.02075 = 0.02149 -0.00017 0.00323 0.00023 C9 1 0.534996 0.630150 0.427356 11.00000 0.02125 0.03017 = 0.02648 0.00382 0.00420 -0.00084 AFIX 43 H9 2 0.477028 0.588904 0.428174 11.00000 -1.20000 AFIX 0 C10 1 0.596031 0.622541 0.449134 11.00000 0.02767 0.03469 = 0.02235 0.00627 0.00392 0.00310 C11 1 0.680586 0.686267 0.447907 11.00000 0.02482 0.03813 = 0.01915 0.00240 -0.00181 0.00506 AFIX 43 H11 2 0.722282 0.688744 0.462946 11.00000 -1.20000 AFIX 0 C12 1 0.704258 0.745274 0.425316 11.00000 0.01853 0.03192 = 0.02032 -0.00057 0.00060 0.00055 AFIX 43 H12 2 0.762485 0.786133 0.424818 11.00000 -1.20000 AFIX 0 C13 1 0.642889 0.745645 0.402904 11.00000 0.02047 0.02242 = 0.01775 0.00045 0.00235 0.00227 C16 1 0.606120 0.829786 0.262265 11.00000 0.01867 0.02764 = 0.01741 0.00010 0.00026 -0.00155 C17 1 0.578438 0.697010 0.257902 11.00000 0.03124 0.02461 = 0.02191 0.00413 0.00205 0.00014 AFIX 43 H17 2 0.581313 0.634458 0.271903 11.00000 -1.20000 AFIX 0 C18 1 0.546596 0.655338 0.233176 11.00000 0.03366 0.02281 = 0.02535 -0.00044 0.00218 -0.00267 AFIX 43 H18 2 0.527407 0.564288 0.230558 11.00000 -1.20000 AFIX 0 C19 1 0.542001 0.743475 0.212069 11.00000 0.02097 0.02860 = 0.02126 -0.00142 0.00108 -0.00102 C20 1 0.569370 0.876295 0.216782 11.00000 0.02952 0.02935 = 0.01945 0.00526 -0.00174 -0.00443 AFIX 43 H20 2 0.566622 0.938824 0.202778 11.00000 -1.20000 AFIX 0 C21 1 0.600657 0.919789 0.241490 11.00000 0.02723 0.02530 = 0.02268 0.00204 -0.00169 -0.00696 AFIX 43 H21 2 0.618401 1.011386 0.244217 11.00000 -1.20000 AFIX 0 C22 1 0.732692 0.934381 0.288488 11.00000 0.02102 0.02520 = 0.01742 0.00397 -0.00074 -0.00316 C23 1 0.753064 1.049612 0.303393 11.00000 0.02644 0.02731 = 0.01975 -0.00006 0.00342 -0.00082 AFIX 43 H23 2 0.706750 1.092293 0.312225 11.00000 -1.20000 AFIX 0 C24 1 0.840649 1.102151 0.305377 11.00000 0.03200 0.02738 = 0.02079 -0.00102 0.00085 -0.00729 AFIX 43 H24 2 0.853821 1.179237 0.316003 11.00000 -1.20000 AFIX 0 C25 1 0.909548 1.044883 0.292218 11.00000 0.02380 0.03039 = 0.02490 0.00256 -0.00133 -0.00594 C26 1 0.887607 0.932198 0.276871 11.00000 0.02219 0.03269 = 0.03067 -0.00077 0.00426 -0.00002 AFIX 43 H26 2 0.933260 0.892262 0.267379 11.00000 -1.20000 AFIX 0 C27 1 0.800953 0.876563 0.275048 11.00000 0.02640 0.02469 = 0.02528 -0.00195 0.00087 -0.00271 AFIX 43 H27 2 0.788139 0.798752 0.264594 11.00000 -1.20000 AFIX 0 C28 1 1.004744 1.103726 0.294497 11.00000 0.02742 0.05010 = 0.03767 -0.00394 -0.00079 -0.01239 AFIX 137 H28A 2 1.049475 1.030325 0.294532 11.00000 -1.50000 H28B 2 1.014328 1.155155 0.310708 11.00000 -1.50000 H28C 2 1.012082 1.163808 0.279727 11.00000 -1.50000 AFIX 0 C29 1 0.509362 0.697031 0.185131 11.00000 0.03856 0.03191 = 0.02301 -0.00359 -0.00259 -0.00381 AFIX 137 H29A 2 0.452297 0.743333 0.179479 11.00000 -1.50000 H29B 2 0.499005 0.599148 0.185251 11.00000 -1.50000 H29C 2 0.555545 0.718393 0.173135 11.00000 -1.50000 AFIX 0 C30 1 0.765859 0.837596 0.378725 11.00000 0.01675 0.02475 = 0.01463 -0.00070 -0.00177 -0.00123 C31 1 0.787425 0.973762 0.377719 11.00000 0.01887 0.02202 = 0.02199 -0.00368 -0.00127 0.00242 AFIX 43 H31 2 0.741752 1.040411 0.379313 11.00000 -1.20000 AFIX 0 C32 1 0.876548 1.011883 0.374353 11.00000 0.02250 0.02128 = 0.02863 -0.00180 -0.00054 -0.00165 AFIX 43 H32 2 0.891330 1.105249 0.373640 11.00000 -1.20000 AFIX 0 C33 1 0.944493 0.916081 0.372011 11.00000 0.01997 0.02611 = 0.02986 -0.00296 0.00060 -0.00285 C34 1 0.921001 0.779721 0.373423 11.00000 0.01886 0.02382 = 0.03213 -0.00228 0.00131 0.00295 AFIX 43 H34 2 0.966714 0.712830 0.372123 11.00000 -1.20000 AFIX 0 C35 1 0.832434 0.739739 0.376681 11.00000 0.01923 0.02097 = 0.02198 0.00070 0.00028 -0.00045 AFIX 43 H35 2 0.817491 0.646467 0.377504 11.00000 -1.20000 AFIX 0 C36 1 1.040560 0.959072 0.368125 11.00000 0.02050 0.03179 = 0.06971 -0.00228 0.00721 -0.00473 AFIX 137 H36A 2 1.040130 1.051451 0.361249 11.00000 -1.50000 H36B 2 1.066584 0.897678 0.355808 11.00000 -1.50000 H36C 2 1.077475 0.956060 0.384791 11.00000 -1.50000 AFIX 0 C38 1 0.331273 0.722410 0.352962 11.00000 0.01943 0.01591 = 0.02764 -0.00295 0.00298 0.00046 C39 1 0.236321 0.703340 0.349679 11.00000 0.01833 0.02213 = 0.03090 -0.00481 -0.00131 0.00174 AFIX 43 H39 2 0.204775 0.715352 0.333045 11.00000 -1.20000 AFIX 0 C40 1 0.188966 0.667238 0.370571 11.00000 0.01712 0.02425 = 0.03751 -0.00638 0.00426 -0.00082 AFIX 43 H40 2 0.125259 0.651286 0.367884 11.00000 -1.20000 AFIX 0 C41 1 0.231788 0.653479 0.395488 11.00000 0.02262 0.02084 = 0.03214 -0.00667 0.00739 -0.00075 C42 1 0.325202 0.671051 0.398314 11.00000 0.02176 0.02138 = 0.02483 -0.00432 0.00401 -0.00051 AFIX 43 H42 2 0.355181 0.661755 0.415220 11.00000 -1.20000 AFIX 0 C43 1 0.378980 0.701955 0.377671 11.00000 0.01860 0.01556 = 0.02453 -0.00326 0.00260 -0.00022 C44 1 0.323162 0.801564 0.307846 11.00000 0.01465 0.02621 = 0.02269 0.00104 -0.00140 0.00022 C45 1 0.294507 0.934160 0.304580 11.00000 0.02196 0.02521 = 0.02816 -0.00351 -0.00283 -0.00021 AFIX 43 H45 2 0.307592 0.998298 0.318064 11.00000 -1.20000 AFIX 0 C46 1 0.246362 0.973277 0.281427 11.00000 0.02553 0.02495 = 0.03234 0.00386 -0.00304 0.00347 AFIX 43 H46 2 0.226372 1.064229 0.279279 11.00000 -1.20000 AFIX 0 C47 1 0.227184 0.880644 0.261394 11.00000 0.01829 0.03518 = 0.02514 0.00290 -0.00114 -0.00017 C48 1 0.256736 0.748097 0.265007 11.00000 0.02108 0.03291 = 0.02404 -0.00457 -0.00067 -0.00063 AFIX 43 H48 2 0.244376 0.683855 0.251502 11.00000 -1.20000 AFIX 0 C49 1 0.304326 0.708067 0.288206 11.00000 0.01982 0.02364 = 0.02658 -0.00191 0.00051 0.00135 AFIX 43 H49 2 0.323739 0.616933 0.290515 11.00000 -1.20000 AFIX 0 C50 1 0.173955 0.922810 0.236508 11.00000 0.03991 0.04497 = 0.02984 0.00631 -0.00797 0.00434 AFIX 137 H50A 2 0.192335 0.867085 0.222146 11.00000 -1.50000 H50B 2 0.186271 1.018149 0.232980 11.00000 -1.50000 H50C 2 0.108672 0.910593 0.238227 11.00000 -1.50000 AFIX 0 C51 1 0.179249 0.615990 0.418375 11.00000 0.02601 0.03973 = 0.03946 -0.00937 0.01234 -0.00521 AFIX 137 H51A 2 0.114719 0.604212 0.412519 11.00000 -1.50000 H51B 2 0.185568 0.688103 0.431411 11.00000 -1.50000 H51C 2 0.203394 0.531345 0.426034 11.00000 -1.50000 AFIX 0 C52 1 0.571329 0.551531 0.473458 11.00000 0.03608 0.05349 = 0.02712 0.01406 0.00364 -0.00109 AFIX 137 H52A 2 0.508672 0.574760 0.476822 11.00000 -1.50000 H52B 2 0.613049 0.580228 0.488195 11.00000 -1.50000 H52C 2 0.576234 0.453515 0.471145 11.00000 -1.50000 AFIX 0 N14 4 0.672161 0.796700 0.379668 11.00000 0.01501 0.02295 = 0.01741 0.00130 0.00070 -0.00100 N15 4 0.643499 0.875651 0.287135 11.00000 0.02115 0.03124 = 0.01642 0.00117 -0.00060 -0.00543 N37 4 0.376482 0.762726 0.331396 11.00000 0.01500 0.02400 = 0.02145 0.00019 -0.00211 0.00063 B59 3 -0.025259 0.376668 0.363442 11.00000 0.02142 0.01599 = 0.02057 -0.00185 -0.00032 0.00051 C53 1 0.115911 0.281865 0.388907 11.00000 0.01972 0.01750 = 0.02123 -0.00083 0.00117 -0.00072 C54 1 0.161600 0.236627 0.412018 11.00000 0.01883 0.02592 = 0.02230 0.00030 -0.00023 0.00226 AFIX 43 H54 2 0.225395 0.220510 0.412950 11.00000 -1.20000 AFIX 0 C55 1 0.113342 0.215227 0.433687 11.00000 0.02308 0.02628 = 0.01999 0.00037 -0.00206 0.00310 C56 1 0.019570 0.240571 0.432802 11.00000 0.02191 0.02811 = 0.01999 0.00204 0.00161 0.00326 AFIX 43 H56 2 -0.013454 0.221685 0.447426 11.00000 -1.20000 AFIX 0 C57 1 -0.024675 0.293880 0.410178 11.00000 0.01858 0.01930 = 0.02175 -0.00113 0.00101 0.00112 C58 1 0.022045 0.316724 0.387587 11.00000 0.01863 0.01792 = 0.01962 -0.00101 0.00017 0.00025 C60 1 0.037333 0.410799 0.341786 11.00000 0.01906 0.01914 = 0.01891 -0.00193 -0.00091 -0.00172 C61 1 0.013977 0.495817 0.320338 11.00000 0.01956 0.02419 = 0.02250 0.00009 -0.00079 0.00043 AFIX 43 H61 2 -0.043605 0.539683 0.319403 11.00000 -1.20000 AFIX 0 C62 1 0.069996 0.519018 0.300600 11.00000 0.02458 0.02541 = 0.02080 0.00228 -0.00010 -0.00234 C63 1 0.152149 0.446360 0.301481 11.00000 0.02395 0.02846 = 0.02025 -0.00016 0.00447 -0.00352 AFIX 43 H63 2 0.188633 0.451301 0.287175 11.00000 -1.20000 AFIX 0 C64 1 0.181002 0.368022 0.322655 11.00000 0.01891 0.02528 = 0.02346 -0.00161 0.00268 -0.00020 AFIX 43 H64 2 0.237687 0.321880 0.323021 11.00000 -1.20000 AFIX 0 C65 1 0.126722 0.356195 0.343737 11.00000 0.02139 0.01928 = 0.01829 -0.00097 -0.00123 -0.00133 C68 1 0.250726 0.118029 0.457126 11.00000 0.02226 0.03345 = 0.01778 0.00342 -0.00017 0.00615 C69 1 0.318469 0.177001 0.473626 11.00000 0.03129 0.04423 = 0.02693 -0.01007 -0.00246 0.00976 AFIX 43 H69 2 0.303381 0.247594 0.484986 11.00000 -1.20000 AFIX 0 C70 1 0.407800 0.133919 0.473684 11.00000 0.02693 0.05474 = 0.03092 -0.01130 -0.00677 0.00315 AFIX 43 H70 2 0.453090 0.174726 0.485315 11.00000 -1.20000 AFIX 0 C71 1 0.432863 0.032290 0.457118 11.00000 0.02548 0.04133 = 0.02571 0.00262 -0.00021 0.00762 C72 1 0.364183 -0.027711 0.441029 11.00000 0.03121 0.02800 = 0.02248 0.00221 0.00295 0.00627 AFIX 43 H72 2 0.379262 -0.098558 0.429724 11.00000 -1.20000 AFIX 0 C73 1 0.274072 0.013233 0.441050 11.00000 0.02533 0.02656 = 0.02300 0.00220 -0.00272 0.00231 AFIX 43 H73 2 0.228235 -0.030505 0.430046 11.00000 -1.20000 AFIX 0 C74 1 0.121763 0.180643 0.481244 11.00000 0.02189 0.04382 = 0.01970 0.00055 -0.00198 0.01027 C75 1 0.122291 0.071299 0.497864 11.00000 0.03922 0.05494 = 0.03065 0.01215 0.00778 0.01861 AFIX 43 H75 2 0.146177 -0.012963 0.492769 11.00000 -1.20000 AFIX 0 C76 1 0.088092 0.083966 0.521967 11.00000 0.04369 0.09294 = 0.03268 0.02194 0.01225 0.02153 AFIX 43 H76 2 0.090892 0.008601 0.533409 11.00000 -1.20000 AFIX 0 C77 1 0.050353 0.202481 0.529697 11.00000 0.03284 0.11934 = 0.02464 -0.00342 0.00103 0.02806 C78 1 0.049735 0.311686 0.512913 11.00000 0.04065 0.08593 = 0.03309 -0.02301 -0.00853 0.02953 AFIX 43 H78 2 0.023874 0.394834 0.517864 11.00000 -1.20000 AFIX 0 C79 1 0.086089 0.302433 0.488985 11.00000 0.04144 0.04721 = 0.02833 -0.00800 -0.00691 0.01445 AFIX 43 H79 2 0.086484 0.379332 0.477972 11.00000 -1.20000 AFIX 0 C80 1 0.010522 0.210658 0.555781 11.00000 0.05274 0.22187 = 0.03516 -0.00622 0.01365 0.05082 AFIX 137 H80A 2 0.000537 0.305620 0.560171 11.00000 -1.50000 H80B 2 0.052934 0.169571 0.569141 11.00000 -1.50000 H80C 2 -0.047663 0.162071 0.554899 11.00000 -1.50000 AFIX 0 C81 1 0.531028 -0.009270 0.456546 11.00000 0.02762 0.06660 = 0.04087 -0.00195 -0.00097 0.01292 AFIX 137 H81A 2 0.534226 -0.097174 0.447909 11.00000 -1.50000 H81B 2 0.559196 -0.016160 0.474357 11.00000 -1.50000 H81C 2 0.563575 0.058464 0.446999 11.00000 -1.50000 AFIX 0 C82 1 0.256778 0.248940 0.368915 11.00000 0.01765 0.02318 = 0.01858 -0.00037 0.00156 0.00141 C83 1 0.279010 0.112975 0.368291 11.00000 0.02070 0.02161 = 0.02242 -0.00201 0.00275 -0.00258 AFIX 43 H83 2 0.232847 0.047266 0.364372 11.00000 -1.20000 AFIX 0 C84 1 0.369096 0.073230 0.373422 11.00000 0.02469 0.02061 = 0.02305 0.00066 0.00321 0.00296 AFIX 43 H84 2 0.383912 -0.020194 0.372966 11.00000 -1.20000 AFIX 0 C85 1 0.438324 0.167201 0.379227 11.00000 0.01970 0.02631 = 0.01993 0.00086 0.00051 0.00131 C86 1 0.414622 0.303662 0.379212 11.00000 0.01962 0.02360 = 0.02851 -0.00205 0.00156 -0.00331 AFIX 43 H86 2 0.460775 0.369775 0.382778 11.00000 -1.20000 AFIX 0 C87 1 0.324766 0.344684 0.374079 11.00000 0.02058 0.01974 = 0.02853 -0.00180 0.00194 0.00133 AFIX 43 H87 2 0.309848 0.438146 0.374101 11.00000 -1.20000 AFIX 0 C88 1 0.535895 0.122175 0.384875 11.00000 0.02302 0.03282 = 0.03351 0.00315 -0.00055 0.00283 AFIX 137 H88A 2 0.566958 0.124229 0.368815 11.00000 -1.50000 H88B 2 0.537076 0.029894 0.391811 11.00000 -1.50000 H88C 2 0.567003 0.183166 0.397668 11.00000 -1.50000 AFIX 0 C90 1 -0.129610 0.393437 0.363601 11.00000 0.01965 0.01645 = 0.02109 -0.00155 0.00114 0.00010 C91 1 -0.189031 0.429115 0.341864 11.00000 0.02088 0.01936 = 0.02058 -0.00101 0.00111 -0.00080 AFIX 43 H91 2 -0.163596 0.440913 0.325701 11.00000 -1.20000 AFIX 0 C92 1 -0.281961 0.448078 0.342523 11.00000 0.02041 0.01798 = 0.02546 -0.00052 -0.00218 0.00008 C93 1 -0.317582 0.432341 0.366610 11.00000 0.01628 0.02450 = 0.03008 0.00134 0.00063 -0.00027 AFIX 43 H93 2 -0.380583 0.448866 0.367952 11.00000 -1.20000 AFIX 0 C94 1 -0.264012 0.393627 0.388409 11.00000 0.01909 0.02458 = 0.02695 0.00168 0.00487 0.00027 AFIX 43 H94 2 -0.290542 0.382480 0.404425 11.00000 -1.20000 AFIX 0 C95 1 -0.170012 0.370354 0.387167 11.00000 0.01968 0.01652 = 0.02225 -0.00044 0.00055 0.00057 C96 1 -0.162482 0.305938 0.433098 11.00000 0.01927 0.03239 = 0.02003 0.00328 0.00179 0.00417 C97 1 -0.162014 0.408226 0.451177 11.00000 0.03361 0.03052 = 0.02796 0.00124 0.00557 0.00498 AFIX 43 H97 2 -0.134252 0.492541 0.447893 11.00000 -1.20000 AFIX 0 C98 1 -0.202393 0.387631 0.474299 11.00000 0.04820 0.04637 = 0.02597 -0.00059 0.00921 0.01507 AFIX 43 H98 2 -0.201159 0.458058 0.486831 11.00000 -1.20000 AFIX 0 C99 1 -0.244454 0.265789 0.479346 11.00000 0.03344 0.05217 = 0.02861 0.01355 0.01025 0.01366 C100 1 -0.244912 0.164323 0.460758 11.00000 0.02793 0.04645 = 0.03150 0.01298 0.00491 0.00063 AFIX 43 H100 2 -0.273682 0.080479 0.463799 11.00000 -1.20000 AFIX 0 C101 1 -0.203764 0.183793 0.437715 11.00000 0.02565 0.03679 = 0.02578 0.00429 0.00119 -0.00207 AFIX 43 H101 2 -0.204080 0.113314 0.425211 11.00000 -1.20000 AFIX 0 C102 1 -0.288106 0.243807 0.504550 11.00000 0.06315 0.07645 = 0.03948 0.02041 0.02600 0.02338 AFIX 137 H10A 2 -0.345963 0.293131 0.504007 11.00000 -1.50000 H10B 2 -0.247187 0.276994 0.519092 11.00000 -1.50000 H10C 2 -0.299415 0.147070 0.506863 11.00000 -1.50000 AFIX 0 C103 1 -0.341371 0.486253 0.318445 11.00000 0.02270 0.03022 = 0.02736 0.00146 -0.00340 0.00197 AFIX 137 H10D 2 -0.310443 0.555163 0.308745 11.00000 -1.50000 H10E 2 -0.399421 0.522328 0.323433 11.00000 -1.50000 H10F 2 -0.352845 0.406068 0.307515 11.00000 -1.50000 AFIX 0 C104 1 0.045566 0.622384 0.279664 11.00000 0.02903 0.03798 = 0.02681 0.00967 0.00330 0.00265 AFIX 137 H10G 2 -0.020531 0.636601 0.278079 11.00000 -1.50000 H10H 2 0.064977 0.589684 0.263081 11.00000 -1.50000 H10I 2 0.076397 0.707954 0.284244 11.00000 -1.50000 AFIX 0 N66 4 0.162542 0.291069 0.366520 11.00000 0.01592 0.02239 = 0.02039 0.00062 -0.00040 0.00167 N67 4 0.158931 0.165817 0.456741 11.00000 0.02258 0.04122 = 0.01833 0.00378 0.00046 0.01162 N89 4 -0.117363 0.325431 0.409523 11.00000 0.01806 0.02554 = 0.01894 0.00230 0.00224 0.00236 HKLF 4 REM 230312lt_auto_a.res in P2(1)/c REM wR2 = 0.1385, GooF = S = 1.118, Restrained GooF = 1.118 for all data REM R1 = 0.0539 for 11515 Fo > 4sig(Fo) and 0.0629 for all 13332 data REM 950 parameters refined using 0 restraints END WGHT 0.0506 6.8103 REM Highest difference peak 0.360, deepest hole -0.276, 1-sigma level 0.058 Q1 1 0.5003 0.7155 0.3651 11.00000 0.05 0.36 Q2 1 0.5243 0.6957 0.3906 11.00000 0.05 0.34 Q3 1 0.5064 0.7726 0.3693 11.00000 0.05 0.31 Q4 1 0.0292 0.2057 0.3744 11.00000 0.05 0.31 Q5 1 -0.0821 0.5320 0.3709 11.00000 0.05 0.31 Q6 1 0.5154 0.4882 0.4695 11.00000 0.05 0.30 Q7 1 1.0417 1.0865 0.2770 11.00000 0.05 0.29 ; _shelx_res_checksum 59120 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.248 _oxdiff_exptl_absorpt_empirical_full_min 0.863 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group B7 B 0.48413(15) 0.7179(2) 0.38019(4) 0.0201(5) Uani 1 1 d . . . . . C1 C 0.61801(13) 0.7985(2) 0.35611(4) 0.0183(4) Uani 1 1 d . . . . . C2 C 0.65781(13) 0.8317(2) 0.33339(4) 0.0196(4) Uani 1 1 d . . . . . H2 H 0.721545 0.847648 0.333791 0.024 Uiso 1 1 calc R U . . . C3 C 0.60348(13) 0.8415(2) 0.31010(4) 0.0200(4) Uani 1 1 d . . . . . C4 C 0.50973(13) 0.8192(2) 0.30927(4) 0.0206(4) Uani 1 1 d . . . . . H4 H 0.472736 0.828506 0.293410 0.025 Uiso 1 1 calc R U . . . C5 C 0.47103(13) 0.7829(2) 0.33203(4) 0.0191(4) Uani 1 1 d . . . . . C6 C 0.52406(13) 0.7674(2) 0.35606(4) 0.0186(4) Uani 1 1 d . . . . . C8 C 0.55302(13) 0.6950(2) 0.40402(4) 0.0206(4) Uani 1 1 d . . . . . C9 C 0.53500(14) 0.6302(2) 0.42736(4) 0.0258(5) Uani 1 1 d . . . . . H9 H 0.477028 0.588904 0.428174 0.031 Uiso 1 1 calc R U . . . C10 C 0.59603(15) 0.6225(2) 0.44913(4) 0.0281(5) Uani 1 1 d . . . . . C11 C 0.68059(14) 0.6863(2) 0.44791(4) 0.0276(5) Uani 1 1 d . . . . . H11 H 0.722282 0.688744 0.462946 0.033 Uiso 1 1 calc R U . . . C12 C 0.70426(14) 0.7453(2) 0.42532(4) 0.0236(4) Uani 1 1 d . . . . . H12 H 0.762485 0.786133 0.424818 0.028 Uiso 1 1 calc R U . . . C13 C 0.64289(13) 0.7456(2) 0.40290(4) 0.0202(4) Uani 1 1 d . . . . . C16 C 0.60612(13) 0.8298(2) 0.26226(4) 0.0213(4) Uani 1 1 d . . . . . C17 C 0.57844(14) 0.6970(2) 0.25790(4) 0.0259(5) Uani 1 1 d . . . . . H17 H 0.581313 0.634458 0.271903 0.031 Uiso 1 1 calc R U . . . C18 C 0.54660(15) 0.6553(2) 0.23318(4) 0.0273(5) Uani 1 1 d . . . . . H18 H 0.527407 0.564288 0.230558 0.033 Uiso 1 1 calc R U . . . C19 C 0.54200(14) 0.7435(2) 0.21207(4) 0.0236(4) Uani 1 1 d . . . . . C20 C 0.56937(14) 0.8763(2) 0.21678(4) 0.0263(5) Uani 1 1 d . . . . . H20 H 0.566622 0.938824 0.202778 0.032 Uiso 1 1 calc R U . . . C21 C 0.60066(14) 0.9198(2) 0.24149(4) 0.0253(5) Uani 1 1 d . . . . . H21 H 0.618401 1.011386 0.244217 0.030 Uiso 1 1 calc R U . . . C22 C 0.73269(13) 0.9344(2) 0.28849(4) 0.0213(4) Uani 1 1 d . . . . . C23 C 0.75306(14) 1.0496(2) 0.30339(4) 0.0244(4) Uani 1 1 d . . . . . H23 H 0.706750 1.092293 0.312225 0.029 Uiso 1 1 calc R U . . . C24 C 0.84065(15) 1.1022(2) 0.30538(4) 0.0268(5) Uani 1 1 d . . . . . H24 H 0.853821 1.179237 0.316003 0.032 Uiso 1 1 calc R U . . . C25 C 0.90955(14) 1.0449(2) 0.29222(4) 0.0265(5) Uani 1 1 d . . . . . C26 C 0.88761(14) 0.9322(2) 0.27687(4) 0.0284(5) Uani 1 1 d . . . . . H26 H 0.933260 0.892262 0.267379 0.034 Uiso 1 1 calc R U . . . C27 C 0.80095(14) 0.8766(2) 0.27505(4) 0.0255(5) Uani 1 1 d . . . . . H27 H 0.788139 0.798752 0.264594 0.031 Uiso 1 1 calc R U . . . C28 C 1.00474(16) 1.1037(3) 0.29450(5) 0.0386(6) Uani 1 1 d . . . . . H28A H 1.049475 1.030325 0.294532 0.058 Uiso 1 1 calc R U . . . H28B H 1.014328 1.155155 0.310708 0.058 Uiso 1 1 calc R U . . . H28C H 1.012082 1.163808 0.279727 0.058 Uiso 1 1 calc R U . . . C29 C 0.50936(16) 0.6970(2) 0.18513(4) 0.0314(5) Uani 1 1 d . . . . . H29A H 0.452297 0.743333 0.179479 0.047 Uiso 1 1 calc R U . . . H29B H 0.499005 0.599148 0.185251 0.047 Uiso 1 1 calc R U . . . H29C H 0.555545 0.718393 0.173135 0.047 Uiso 1 1 calc R U . . . C30 C 0.76586(13) 0.8376(2) 0.37872(4) 0.0189(4) Uani 1 1 d . . . . . C31 C 0.78743(13) 0.9738(2) 0.37772(4) 0.0211(4) Uani 1 1 d . . . . . H31 H 0.741752 1.040411 0.379313 0.025 Uiso 1 1 calc R U . . . C32 C 0.87655(14) 1.0119(2) 0.37435(4) 0.0243(4) Uani 1 1 d . . . . . H32 H 0.891330 1.105249 0.373640 0.029 Uiso 1 1 calc R U . . . C33 C 0.94449(14) 0.9161(2) 0.37201(4) 0.0254(5) Uani 1 1 d . . . . . C34 C 0.92100(14) 0.7797(2) 0.37342(4) 0.0250(5) Uani 1 1 d . . . . . H34 H 0.966714 0.712830 0.372123 0.030 Uiso 1 1 calc R U . . . C35 C 0.83243(13) 0.7397(2) 0.37668(4) 0.0208(4) Uani 1 1 d . . . . . H35 H 0.817491 0.646467 0.377504 0.025 Uiso 1 1 calc R U . . . C36 C 1.04056(15) 0.9591(3) 0.36813(6) 0.0405(6) Uani 1 1 d . . . . . H36A H 1.040130 1.051451 0.361249 0.061 Uiso 1 1 calc R U . . . H36B H 1.066584 0.897678 0.355808 0.061 Uiso 1 1 calc R U . . . H36C H 1.077475 0.956060 0.384791 0.061 Uiso 1 1 calc R U . . . C38 C 0.33127(13) 0.7224(2) 0.35296(4) 0.0209(4) Uani 1 1 d . . . . . C39 C 0.23632(13) 0.7033(2) 0.34968(4) 0.0240(4) Uani 1 1 d . . . . . H39 H 0.204775 0.715352 0.333045 0.029 Uiso 1 1 calc R U . . . C40 C 0.18897(14) 0.6672(2) 0.37057(4) 0.0262(5) Uani 1 1 d . . . . . H40 H 0.125259 0.651286 0.367884 0.031 Uiso 1 1 calc R U . . . C41 C 0.23179(14) 0.6535(2) 0.39549(4) 0.0249(5) Uani 1 1 d . . . . . C42 C 0.32520(14) 0.6711(2) 0.39831(4) 0.0225(4) Uani 1 1 d . . . . . H42 H 0.355181 0.661755 0.415220 0.027 Uiso 1 1 calc R U . . . C43 C 0.37898(13) 0.7020(2) 0.37767(4) 0.0195(4) Uani 1 1 d . . . . . C44 C 0.32316(13) 0.8016(2) 0.30785(4) 0.0213(4) Uani 1 1 d . . . . . C45 C 0.29451(14) 0.9342(2) 0.30458(4) 0.0254(5) Uani 1 1 d . . . . . H45 H 0.307592 0.998298 0.318064 0.030 Uiso 1 1 calc R U . . . C46 C 0.24636(14) 0.9733(2) 0.28143(4) 0.0279(5) Uani 1 1 d . . . . . H46 H 0.226372 1.064229 0.279279 0.033 Uiso 1 1 calc R U . . . C47 C 0.22718(14) 0.8806(2) 0.26139(4) 0.0264(5) Uani 1 1 d . . . . . C48 C 0.25674(14) 0.7481(2) 0.26501(4) 0.0262(5) Uani 1 1 d . . . . . H48 H 0.244376 0.683855 0.251502 0.031 Uiso 1 1 calc R U . . . C49 C 0.30433(13) 0.7081(2) 0.28821(4) 0.0234(4) Uani 1 1 d . . . . . H49 H 0.323739 0.616933 0.290515 0.028 Uiso 1 1 calc R U . . . C50 C 0.17395(17) 0.9228(3) 0.23651(4) 0.0388(6) Uani 1 1 d . . . . . H50A H 0.192335 0.867085 0.222146 0.058 Uiso 1 1 calc R U . . . H50B H 0.186271 1.018149 0.232980 0.058 Uiso 1 1 calc R U . . . H50C H 0.108672 0.910593 0.238227 0.058 Uiso 1 1 calc R U . . . C51 C 0.17925(15) 0.6160(3) 0.41837(5) 0.0345(5) Uani 1 1 d . . . . . H51A H 0.114719 0.604212 0.412519 0.052 Uiso 1 1 calc R U . . . H51B H 0.185568 0.688103 0.431411 0.052 Uiso 1 1 calc R U . . . H51C H 0.203394 0.531345 0.426034 0.052 Uiso 1 1 calc R U . . . C52 C 0.57133(17) 0.5515(3) 0.47346(4) 0.0388(6) Uani 1 1 d . . . . . H52A H 0.508672 0.574760 0.476822 0.058 Uiso 1 1 calc R U . . . H52B H 0.613049 0.580228 0.488195 0.058 Uiso 1 1 calc R U . . . H52C H 0.576234 0.453515 0.471145 0.058 Uiso 1 1 calc R U . . . N14 N 0.67216(10) 0.79670(17) 0.37967(3) 0.0185(3) Uani 1 1 d . . . . . N15 N 0.64350(11) 0.87565(19) 0.28713(3) 0.0231(4) Uani 1 1 d . . . . . N37 N 0.37648(11) 0.76273(17) 0.33140(3) 0.0203(4) Uani 1 1 d . . . . . B59 B -0.02526(15) 0.3767(2) 0.36344(4) 0.0194(5) Uani 1 1 d . . . . . C53 C 0.11591(13) 0.2819(2) 0.38891(4) 0.0195(4) Uani 1 1 d . . . . . C54 C 0.16160(14) 0.2366(2) 0.41202(4) 0.0225(4) Uani 1 1 d . . . . . H54 H 0.225395 0.220510 0.412950 0.027 Uiso 1 1 calc R U . . . C55 C 0.11334(14) 0.2152(2) 0.43369(4) 0.0233(4) Uani 1 1 d . . . . . C56 C 0.01957(14) 0.2406(2) 0.43280(4) 0.0233(4) Uani 1 1 d . . . . . H56 H -0.013454 0.221685 0.447426 0.028 Uiso 1 1 calc R U . . . C57 C -0.02468(13) 0.2939(2) 0.41018(4) 0.0199(4) Uani 1 1 d . . . . . C58 C 0.02204(13) 0.3167(2) 0.38759(4) 0.0188(4) Uani 1 1 d . . . . . C60 C 0.03733(13) 0.4108(2) 0.34179(4) 0.0192(4) Uani 1 1 d . . . . . C61 C 0.01398(13) 0.4958(2) 0.32034(4) 0.0222(4) Uani 1 1 d . . . . . H61 H -0.043605 0.539683 0.319403 0.027 Uiso 1 1 calc R U . . . C62 C 0.07000(14) 0.5190(2) 0.30060(4) 0.0237(4) Uani 1 1 d . . . . . C63 C 0.15215(14) 0.4464(2) 0.30148(4) 0.0241(4) Uani 1 1 d . . . . . H63 H 0.188633 0.451301 0.287175 0.029 Uiso 1 1 calc R U . . . C64 C 0.18100(13) 0.3680(2) 0.32266(4) 0.0225(4) Uani 1 1 d . . . . . H64 H 0.237687 0.321880 0.323021 0.027 Uiso 1 1 calc R U . . . C65 C 0.12672(13) 0.3562(2) 0.34374(4) 0.0198(4) Uani 1 1 d . . . . . C68 C 0.25073(14) 0.1180(2) 0.45713(4) 0.0246(5) Uani 1 1 d . . . . . C69 C 0.31847(16) 0.1770(3) 0.47363(4) 0.0344(5) Uani 1 1 d . . . . . H69 H 0.303381 0.247594 0.484986 0.041 Uiso 1 1 calc R U . . . C70 C 0.40780(16) 0.1339(3) 0.47368(5) 0.0380(6) Uani 1 1 d . . . . . H70 H 0.453090 0.174726 0.485315 0.046 Uiso 1 1 calc R U . . . C71 C 0.43286(15) 0.0323(3) 0.45712(4) 0.0310(5) Uani 1 1 d . . . . . C72 C 0.36418(15) -0.0277(2) 0.44103(4) 0.0272(5) Uani 1 1 d . . . . . H72 H 0.379262 -0.098558 0.429724 0.033 Uiso 1 1 calc R U . . . C73 C 0.27407(14) 0.0132(2) 0.44105(4) 0.0252(5) Uani 1 1 d . . . . . H73 H 0.228235 -0.030505 0.430046 0.030 Uiso 1 1 calc R U . . . C74 C 0.12176(14) 0.1806(3) 0.48124(4) 0.0287(5) Uani 1 1 d . . . . . C75 C 0.12229(17) 0.0713(3) 0.49786(5) 0.0413(6) Uani 1 1 d . . . . . H75 H 0.146177 -0.012963 0.492769 0.050 Uiso 1 1 calc R U . . . C76 C 0.08809(19) 0.0840(4) 0.52197(5) 0.0559(9) Uani 1 1 d . . . . . H76 H 0.090892 0.008601 0.533409 0.067 Uiso 1 1 calc R U . . . C77 C 0.05035(18) 0.2025(4) 0.52970(5) 0.0590(10) Uani 1 1 d . . . . . C78 C 0.04973(18) 0.3117(4) 0.51291(5) 0.0539(8) Uani 1 1 d . . . . . H78 H 0.023874 0.394834 0.517864 0.065 Uiso 1 1 calc R U . . . C79 C 0.08609(17) 0.3024(3) 0.48898(5) 0.0395(6) Uani 1 1 d . . . . . H79 H 0.086484 0.379332 0.477972 0.047 Uiso 1 1 calc R U . . . C80 C 0.0105(2) 0.2107(6) 0.55578(6) 0.1027(18) Uani 1 1 d . . . . . H80A H 0.000537 0.305620 0.560171 0.154 Uiso 1 1 calc R U . . . H80B H 0.052934 0.169571 0.569141 0.154 Uiso 1 1 calc R U . . . H80C H -0.047663 0.162071 0.554899 0.154 Uiso 1 1 calc R U . . . C81 C 0.53103(16) -0.0093(3) 0.45655(5) 0.0452(7) Uani 1 1 d . . . . . H81A H 0.534226 -0.097174 0.447909 0.068 Uiso 1 1 calc R U . . . H81B H 0.559196 -0.016160 0.474357 0.068 Uiso 1 1 calc R U . . . H81C H 0.563575 0.058464 0.446999 0.068 Uiso 1 1 calc R U . . . C82 C 0.25678(13) 0.2489(2) 0.36892(4) 0.0198(4) Uani 1 1 d . . . . . C83 C 0.27901(14) 0.1130(2) 0.36829(4) 0.0215(4) Uani 1 1 d . . . . . H83 H 0.232847 0.047266 0.364372 0.026 Uiso 1 1 calc R U . . . C84 C 0.36910(14) 0.0732(2) 0.37342(4) 0.0227(4) Uani 1 1 d . . . . . H84 H 0.383912 -0.020194 0.372966 0.027 Uiso 1 1 calc R U . . . C85 C 0.43832(13) 0.1672(2) 0.37923(4) 0.0220(4) Uani 1 1 d . . . . . C86 C 0.41462(14) 0.3037(2) 0.37921(4) 0.0239(4) Uani 1 1 d . . . . . H86 H 0.460775 0.369775 0.382778 0.029 Uiso 1 1 calc R U . . . C87 C 0.32477(13) 0.3447(2) 0.37408(4) 0.0230(4) Uani 1 1 d . . . . . H87 H 0.309848 0.438146 0.374101 0.028 Uiso 1 1 calc R U . . . C88 C 0.53589(14) 0.1222(2) 0.38488(4) 0.0299(5) Uani 1 1 d . . . . . H88A H 0.566958 0.124229 0.368815 0.045 Uiso 1 1 calc R U . . . H88B H 0.537076 0.029894 0.391811 0.045 Uiso 1 1 calc R U . . . H88C H 0.567003 0.183166 0.397668 0.045 Uiso 1 1 calc R U . . . C90 C -0.12961(13) 0.3934(2) 0.36360(4) 0.0191(4) Uani 1 1 d . . . . . C91 C -0.18903(13) 0.4291(2) 0.34186(4) 0.0203(4) Uani 1 1 d . . . . . H91 H -0.163596 0.440913 0.325701 0.024 Uiso 1 1 calc R U . . . C92 C -0.28196(13) 0.4481(2) 0.34252(4) 0.0215(4) Uani 1 1 d . . . . . C93 C -0.31758(13) 0.4323(2) 0.36661(4) 0.0237(4) Uani 1 1 d . . . . . H93 H -0.380583 0.448866 0.367952 0.028 Uiso 1 1 calc R U . . . C94 C -0.26401(13) 0.3936(2) 0.38841(4) 0.0234(4) Uani 1 1 d . . . . . H94 H -0.290542 0.382480 0.404425 0.028 Uiso 1 1 calc R U . . . C95 C -0.17001(13) 0.3704(2) 0.38717(4) 0.0196(4) Uani 1 1 d . . . . . C96 C -0.16248(13) 0.3059(2) 0.43310(4) 0.0239(4) Uani 1 1 d . . . . . C97 C -0.16201(15) 0.4082(2) 0.45118(4) 0.0305(5) Uani 1 1 d . . . . . H97 H -0.134252 0.492541 0.447893 0.037 Uiso 1 1 calc R U . . . C98 C -0.20239(18) 0.3876(3) 0.47430(5) 0.0398(6) Uani 1 1 d . . . . . H98 H -0.201159 0.458058 0.486831 0.048 Uiso 1 1 calc R U . . . C99 C -0.24445(16) 0.2658(3) 0.47935(5) 0.0377(6) Uani 1 1 d . . . . . C100 C -0.24491(15) 0.1643(3) 0.46076(4) 0.0352(6) Uani 1 1 d . . . . . H100 H -0.273682 0.080479 0.463799 0.042 Uiso 1 1 calc R U . . . C101 C -0.20376(14) 0.1838(2) 0.43771(4) 0.0295(5) Uani 1 1 d . . . . . H101 H -0.204080 0.113314 0.425211 0.035 Uiso 1 1 calc R U . . . C102 C -0.2881(2) 0.2438(4) 0.50455(5) 0.0585(9) Uani 1 1 d . . . . . H10A H -0.345963 0.293131 0.504007 0.088 Uiso 1 1 calc R U . . . H10B H -0.247187 0.276994 0.519092 0.088 Uiso 1 1 calc R U . . . H10C H -0.299415 0.147070 0.506863 0.088 Uiso 1 1 calc R U . . . C103 C -0.34137(14) 0.4863(2) 0.31844(4) 0.0271(5) Uani 1 1 d . . . . . H10D H -0.310443 0.555163 0.308745 0.041 Uiso 1 1 calc R U . . . H10E H -0.399421 0.522328 0.323433 0.041 Uiso 1 1 calc R U . . . H10F H -0.352845 0.406068 0.307515 0.041 Uiso 1 1 calc R U . . . C104 C 0.04557(15) 0.6224(2) 0.27966(4) 0.0312(5) Uani 1 1 d . . . . . H10G H -0.020531 0.636601 0.278079 0.047 Uiso 1 1 calc R U . . . H10H H 0.064977 0.589684 0.263081 0.047 Uiso 1 1 calc R U . . . H10I H 0.076397 0.707954 0.284244 0.047 Uiso 1 1 calc R U . . . N66 N 0.16254(11) 0.29107(17) 0.36652(3) 0.0197(4) Uani 1 1 d . . . . . N67 N 0.15893(12) 0.1658(2) 0.45674(3) 0.0274(4) Uani 1 1 d . . . . . N89 N -0.11736(11) 0.32543(18) 0.40952(3) 0.0208(4) 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 B7 0.0206(11) 0.0162(11) 0.0237(11) -0.0019(9) 0.0030(9) -0.0002(9) C1 0.0175(9) 0.0180(10) 0.0191(9) -0.0017(8) -0.0009(7) 0.0013(8) C2 0.0146(9) 0.0234(10) 0.0206(10) -0.0001(8) -0.0003(7) -0.0011(8) C3 0.0206(10) 0.0199(10) 0.0193(10) 0.0010(8) 0.0011(8) -0.0003(8) C4 0.0186(10) 0.0225(10) 0.0199(10) 0.0007(8) -0.0038(8) -0.0005(8) C5 0.0169(9) 0.0161(9) 0.0239(10) -0.0005(8) 0.0000(8) -0.0003(8) C6 0.0170(9) 0.0168(10) 0.0219(10) -0.0015(8) 0.0002(8) 0.0004(8) C8 0.0198(10) 0.0207(10) 0.0215(10) -0.0002(8) 0.0032(8) 0.0002(8) C9 0.0212(10) 0.0302(12) 0.0265(11) 0.0038(9) 0.0042(8) -0.0008(9) C10 0.0277(11) 0.0347(12) 0.0224(10) 0.0063(9) 0.0039(8) 0.0031(10) C11 0.0248(11) 0.0381(13) 0.0192(10) 0.0024(9) -0.0018(8) 0.0051(10) C12 0.0185(10) 0.0319(12) 0.0203(10) -0.0006(9) 0.0006(8) 0.0006(9) C13 0.0205(10) 0.0224(10) 0.0178(9) 0.0004(8) 0.0023(8) 0.0023(8) C16 0.0187(10) 0.0276(11) 0.0174(10) 0.0001(8) 0.0003(7) -0.0016(8) C17 0.0312(11) 0.0246(11) 0.0219(10) 0.0041(9) 0.0021(9) 0.0001(9) C18 0.0337(12) 0.0228(11) 0.0253(11) -0.0004(9) 0.0022(9) -0.0027(9) C19 0.0210(10) 0.0286(11) 0.0213(10) -0.0014(9) 0.0011(8) -0.0010(9) C20 0.0295(11) 0.0293(12) 0.0195(10) 0.0053(9) -0.0017(8) -0.0044(9) C21 0.0272(11) 0.0253(11) 0.0227(10) 0.0020(9) -0.0017(8) -0.0070(9) C22 0.0210(10) 0.0252(11) 0.0174(9) 0.0040(8) -0.0007(8) -0.0032(8) C23 0.0264(11) 0.0273(11) 0.0198(10) -0.0001(9) 0.0034(8) -0.0008(9) C24 0.0320(12) 0.0274(11) 0.0208(10) -0.0010(9) 0.0008(8) -0.0073(9) C25 0.0238(11) 0.0304(12) 0.0249(10) 0.0026(9) -0.0013(8) -0.0059(9) C26 0.0222(11) 0.0327(12) 0.0307(11) -0.0008(10) 0.0043(9) 0.0000(9) C27 0.0264(11) 0.0247(11) 0.0253(10) -0.0020(9) 0.0009(8) -0.0027(9) C28 0.0274(12) 0.0501(16) 0.0377(13) -0.0039(12) -0.0008(10) -0.0124(11) C29 0.0386(13) 0.0319(12) 0.0230(11) -0.0036(9) -0.0026(9) -0.0038(10) C30 0.0168(9) 0.0247(10) 0.0146(9) -0.0007(8) -0.0018(7) -0.0012(8) C31 0.0189(10) 0.0220(10) 0.0220(10) -0.0037(8) -0.0013(8) 0.0024(8) C32 0.0225(10) 0.0213(11) 0.0286(11) -0.0018(9) -0.0005(8) -0.0017(9) C33 0.0200(10) 0.0261(11) 0.0299(11) -0.0030(9) 0.0006(8) -0.0029(9) C34 0.0189(10) 0.0238(11) 0.0321(11) -0.0023(9) 0.0013(8) 0.0029(8) C35 0.0192(10) 0.0210(10) 0.0220(10) 0.0007(8) 0.0003(8) -0.0005(8) C36 0.0205(11) 0.0318(13) 0.0697(18) -0.0023(12) 0.0072(11) -0.0047(10) C38 0.0194(10) 0.0159(10) 0.0276(11) -0.0030(8) 0.0030(8) 0.0005(8) C39 0.0183(10) 0.0221(11) 0.0309(11) -0.0048(9) -0.0013(8) 0.0017(8) C40 0.0171(10) 0.0243(11) 0.0375(12) -0.0064(9) 0.0043(9) -0.0008(8) C41 0.0226(10) 0.0208(11) 0.0321(11) -0.0067(9) 0.0074(9) -0.0007(8) C42 0.0218(10) 0.0214(10) 0.0248(10) -0.0043(8) 0.0040(8) -0.0005(8) C43 0.0186(10) 0.0156(10) 0.0245(10) -0.0033(8) 0.0026(8) -0.0002(8) C44 0.0146(9) 0.0262(11) 0.0227(10) 0.0010(9) -0.0014(8) 0.0002(8) C45 0.0220(10) 0.0252(11) 0.0282(11) -0.0035(9) -0.0028(8) -0.0002(9) C46 0.0255(11) 0.0249(11) 0.0323(12) 0.0039(9) -0.0030(9) 0.0035(9) C47 0.0183(10) 0.0352(12) 0.0251(11) 0.0029(9) -0.0011(8) -0.0002(9) C48 0.0211(10) 0.0329(12) 0.0240(11) -0.0046(9) -0.0007(8) -0.0006(9) C49 0.0198(10) 0.0236(11) 0.0266(11) -0.0019(9) 0.0005(8) 0.0014(8) C50 0.0399(14) 0.0450(15) 0.0298(12) 0.0063(11) -0.0080(10) 0.0043(12) C51 0.0260(11) 0.0397(14) 0.0395(13) -0.0094(11) 0.0123(10) -0.0052(10) C52 0.0361(13) 0.0535(16) 0.0271(12) 0.0141(11) 0.0036(10) -0.0011(12) N14 0.0150(8) 0.0229(9) 0.0174(8) 0.0013(7) 0.0007(6) -0.0010(7) N15 0.0212(9) 0.0312(10) 0.0164(8) 0.0012(7) -0.0006(6) -0.0054(7) N37 0.0150(8) 0.0240(9) 0.0214(8) 0.0002(7) -0.0021(6) 0.0006(7) B59 0.0214(11) 0.0160(11) 0.0206(11) -0.0018(9) -0.0003(9) 0.0005(9) C53 0.0197(10) 0.0175(10) 0.0212(10) -0.0008(8) 0.0012(8) -0.0007(8) C54 0.0188(10) 0.0259(11) 0.0223(10) 0.0003(8) -0.0002(8) 0.0023(8) C55 0.0231(10) 0.0263(11) 0.0200(10) 0.0004(8) -0.0021(8) 0.0031(9) C56 0.0219(10) 0.0281(11) 0.0200(10) 0.0020(9) 0.0016(8) 0.0033(9) C57 0.0186(10) 0.0193(10) 0.0218(10) -0.0011(8) 0.0010(8) 0.0011(8) C58 0.0186(10) 0.0179(10) 0.0196(10) -0.0010(8) 0.0002(8) 0.0003(8) C60 0.0191(10) 0.0191(10) 0.0189(9) -0.0019(8) -0.0009(7) -0.0017(8) C61 0.0196(10) 0.0242(11) 0.0225(10) 0.0001(8) -0.0008(8) 0.0004(8) C62 0.0246(10) 0.0254(11) 0.0208(10) 0.0023(9) -0.0001(8) -0.0023(9) C63 0.0240(10) 0.0285(11) 0.0203(10) -0.0002(9) 0.0045(8) -0.0035(9) C64 0.0189(10) 0.0253(11) 0.0235(10) -0.0016(9) 0.0027(8) -0.0002(8) C65 0.0214(10) 0.0193(10) 0.0183(9) -0.0010(8) -0.0012(8) -0.0013(8) C68 0.0223(10) 0.0335(12) 0.0178(10) 0.0034(9) -0.0002(8) 0.0062(9) C69 0.0313(12) 0.0442(14) 0.0269(11) -0.0101(10) -0.0025(9) 0.0098(11) C70 0.0269(12) 0.0547(16) 0.0309(12) -0.0113(12) -0.0068(9) 0.0031(11) C71 0.0255(11) 0.0413(14) 0.0257(11) 0.0026(10) -0.0002(9) 0.0076(10) C72 0.0312(12) 0.0280(12) 0.0225(10) 0.0022(9) 0.0029(9) 0.0063(9) C73 0.0253(11) 0.0266(11) 0.0230(10) 0.0022(9) -0.0027(8) 0.0023(9) C74 0.0219(10) 0.0438(14) 0.0197(10) 0.0005(10) -0.0020(8) 0.0103(10) C75 0.0392(14) 0.0549(17) 0.0307(12) 0.0121(12) 0.0078(10) 0.0186(12) C76 0.0437(15) 0.093(2) 0.0327(14) 0.0219(15) 0.0123(12) 0.0215(16) C77 0.0328(14) 0.119(3) 0.0246(13) -0.0034(16) 0.0010(10) 0.0281(17) C78 0.0406(15) 0.086(2) 0.0331(14) -0.0230(15) -0.0085(11) 0.0295(15) C79 0.0414(14) 0.0472(15) 0.0283(12) -0.0080(11) -0.0069(10) 0.0145(12) C80 0.053(2) 0.222(6) 0.0352(17) -0.006(2) 0.0136(14) 0.051(3) C81 0.0276(13) 0.0666(19) 0.0409(14) -0.0019(13) -0.0010(10) 0.0129(13) C82 0.0177(10) 0.0232(10) 0.0186(9) -0.0004(8) 0.0016(7) 0.0014(8) C83 0.0207(10) 0.0216(10) 0.0224(10) -0.0020(8) 0.0028(8) -0.0026(8) C84 0.0247(10) 0.0206(10) 0.0230(10) 0.0007(8) 0.0032(8) 0.0030(8) C85 0.0197(10) 0.0263(11) 0.0199(10) 0.0009(8) 0.0005(8) 0.0013(8) C86 0.0196(10) 0.0236(11) 0.0285(11) -0.0021(9) 0.0016(8) -0.0033(8) C87 0.0206(10) 0.0197(10) 0.0285(11) -0.0018(9) 0.0019(8) 0.0013(8) C88 0.0230(11) 0.0328(12) 0.0335(12) 0.0032(10) -0.0006(9) 0.0028(9) C90 0.0196(10) 0.0165(9) 0.0211(10) -0.0015(8) 0.0011(8) 0.0001(8) C91 0.0209(10) 0.0194(10) 0.0206(10) -0.0010(8) 0.0011(8) -0.0008(8) C92 0.0204(10) 0.0180(10) 0.0255(10) -0.0005(8) -0.0022(8) 0.0001(8) C93 0.0163(10) 0.0245(11) 0.0301(11) 0.0013(9) 0.0006(8) -0.0003(8) C94 0.0191(10) 0.0246(11) 0.0270(10) 0.0017(9) 0.0049(8) 0.0003(8) C95 0.0197(10) 0.0165(10) 0.0222(10) -0.0004(8) 0.0006(8) 0.0006(8) C96 0.0193(10) 0.0324(12) 0.0200(10) 0.0033(9) 0.0018(8) 0.0042(9) C97 0.0336(12) 0.0305(12) 0.0280(11) 0.0012(10) 0.0056(9) 0.0050(10) C98 0.0482(15) 0.0464(15) 0.0260(12) -0.0006(11) 0.0092(10) 0.0151(12) C99 0.0334(13) 0.0522(16) 0.0286(12) 0.0135(11) 0.0102(10) 0.0137(12) C100 0.0279(12) 0.0464(15) 0.0315(12) 0.0130(11) 0.0049(9) 0.0006(11) C101 0.0256(11) 0.0368(13) 0.0258(11) 0.0043(10) 0.0012(9) -0.0021(10) C102 0.0632(19) 0.076(2) 0.0395(15) 0.0204(15) 0.0260(14) 0.0234(17) C103 0.0227(10) 0.0302(12) 0.0274(11) 0.0015(9) -0.0034(8) 0.0020(9) C104 0.0290(12) 0.0380(13) 0.0268(11) 0.0097(10) 0.0033(9) 0.0027(10) N66 0.0159(8) 0.0224(9) 0.0204(8) 0.0006(7) -0.0004(6) 0.0017(7) N67 0.0226(9) 0.0412(11) 0.0183(8) 0.0038(8) 0.0005(7) 0.0116(8) N89 0.0181(8) 0.0255(9) 0.0189(8) 0.0023(7) 0.0022(6) 0.0024(7) 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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 B7 C8 115.62(18) . . ? C6 B7 C43 114.80(18) . . ? C8 B7 C43 129.54(18) . . ? C2 C1 C6 121.86(17) . . ? C2 C1 N14 119.11(17) . . ? N14 C1 C6 119.02(17) . . ? C1 C2 H2 120.2 . . ? C3 C2 C1 119.51(18) . . ? C3 C2 H2 120.2 . . ? C2 C3 C4 120.83(18) . . ? C2 C3 N15 119.60(17) . . ? C4 C3 N15 119.56(17) . . ? C3 C4 H4 120.5 . . ? C5 C4 C3 119.10(17) . . ? C5 C4 H4 120.5 . . ? C4 C5 C6 122.11(17) . . ? C4 C5 N37 119.33(17) . . ? N37 C5 C6 118.56(17) . . ? C1 C6 B7 121.16(18) . . ? C1 C6 C5 116.42(17) . . ? C5 C6 B7 122.41(18) . . ? C9 C8 B7 126.17(18) . . ? C9 C8 C13 115.90(18) . . ? C13 C8 B7 117.91(17) . . ? C8 C9 H9 117.8 . . ? C10 C9 C8 124.4(2) . . ? C10 C9 H9 117.8 . . ? C9 C10 C11 117.32(19) . . ? C9 C10 C52 121.2(2) . . ? C11 C10 C52 121.50(19) . . ? C10 C11 H11 119.4 . . ? C12 C11 C10 121.16(19) . . ? C12 C11 H11 119.4 . . ? C11 C12 H12 119.7 . . ? C11 C12 C13 120.55(19) . . ? C13 C12 H12 119.7 . . ? C12 C13 C8 120.14(18) . . ? N14 C13 C8 120.98(17) . . ? N14 C13 C12 118.87(17) . . ? C17 C16 C21 118.84(18) . . ? C17 C16 N15 122.17(18) . . ? C21 C16 N15 118.94(19) . . ? C16 C17 H17 119.9 . . ? C18 C17 C16 120.22(19) . . ? C18 C17 H17 119.9 . . ? C17 C18 H18 119.1 . . ? C17 C18 C19 121.7(2) . . ? C19 C18 H18 119.1 . . ? C18 C19 C29 121.6(2) . . ? C20 C19 C18 117.36(19) . . ? C20 C19 C29 121.07(19) . . ? C19 C20 H20 119.2 . . ? C21 C20 C19 121.5(2) . . ? C21 C20 H20 119.2 . . ? C16 C21 H21 119.9 . . ? C20 C21 C16 120.3(2) . . ? C20 C21 H21 119.9 . . ? C23 C22 N15 120.87(18) . . ? C27 C22 C23 118.71(19) . . ? C27 C22 N15 120.42(19) . . ? C22 C23 H23 119.9 . . ? C24 C23 C22 120.2(2) . . ? C24 C23 H23 119.9 . . ? C23 C24 H24 119.2 . . ? C23 C24 C25 121.6(2) . . ? C25 C24 H24 119.2 . . ? C24 C25 C26 117.49(19) . . ? C24 C25 C28 121.0(2) . . ? C26 C25 C28 121.5(2) . . ? C25 C26 H26 119.1 . . ? C27 C26 C25 121.8(2) . . ? C27 C26 H26 119.1 . . ? C22 C27 H27 119.9 . . ? C26 C27 C22 120.1(2) . . ? C26 C27 H27 119.9 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C19 C29 H29A 109.5 . . ? C19 C29 H29B 109.5 . . ? C19 C29 H29C 109.5 . . ? H29A C29 H29B 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31 C30 C35 120.63(18) . . ? C31 C30 N14 119.78(18) . . ? C35 C30 N14 119.38(18) . . ? C30 C31 H31 120.3 . . ? C30 C31 C32 119.34(19) . . ? C32 C31 H31 120.3 . . ? C31 C32 H32 119.3 . . ? C31 C32 C33 121.3(2) . . ? C33 C32 H32 119.3 . . ? C32 C33 C34 118.08(19) . . ? C32 C33 C36 120.6(2) . . ? C34 C33 C36 121.3(2) . . ? C33 C34 H34 119.3 . . ? C35 C34 C33 121.44(19) . . ? C35 C34 H34 119.3 . . ? C30 C35 H35 120.4 . . ? C34 C35 C30 119.20(19) . . ? C34 C35 H35 120.4 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36B 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C39 C38 C43 120.15(18) . . ? N37 C38 C39 118.32(18) . . ? N37 C38 C43 121.52(17) . . ? C38 C39 H39 119.9 . . ? C40 C39 C38 120.11(19) . . ? C40 C39 H39 119.9 . . ? C39 C40 H40 119.0 . . ? C39 C40 C41 121.94(19) . . ? C41 C40 H40 119.0 . . ? C40 C41 C51 121.68(19) . . ? C42 C41 C40 117.14(19) . . ? C42 C41 C51 121.1(2) . . ? C41 C42 H42 117.9 . . ? C41 C42 C43 124.20(19) . . ? C43 C42 H42 117.9 . . ? C38 C43 B7 118.51(17) . . ? C42 C43 B7 125.19(18) . . ? C42 C43 C38 116.28(18) . . ? C45 C44 N37 119.59(18) . . ? C49 C44 C45 120.21(19) . . ? C49 C44 N37 120.14(18) . . ? C44 C45 H45 120.1 . . ? C44 C45 C46 119.7(2) . . ? C46 C45 H45 120.1 . . ? C45 C46 H46 119.6 . . ? C47 C46 C45 120.8(2) . . ? C47 C46 H46 119.6 . . ? C46 C47 C50 120.7(2) . . ? C48 C47 C46 118.59(19) . . ? C48 C47 C50 120.7(2) . . ? C47 C48 H48 119.6 . . ? C47 C48 C49 120.9(2) . . ? C49 C48 H48 119.6 . . ? C44 C49 C48 119.8(2) . . ? C44 C49 H49 120.1 . . ? C48 C49 H49 120.1 . . ? C47 C50 H50A 109.5 . . ? C47 C50 H50B 109.5 . . ? C47 C50 H50C 109.5 . . ? H50A C50 H50B 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C41 C51 H51A 109.5 . . ? C41 C51 H51B 109.5 . . ? C41 C51 H51C 109.5 . . ? H51A C51 H51B 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C10 C52 H52A 109.5 . . ? C10 C52 H52B 109.5 . . ? C10 C52 H52C 109.5 . . ? H52A C52 H52B 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C1 N14 C13 123.77(16) . . ? C1 N14 C30 116.44(15) . . ? C13 N14 C30 119.48(15) . . ? C3 N15 C16 121.61(16) . . ? C3 N15 C22 120.11(16) . . ? C16 N15 C22 117.14(16) . . ? C5 N37 C44 116.80(16) . . ? C38 N37 C5 123.82(16) . . ? C38 N37 C44 118.96(16) . . ? C58 B59 C60 115.15(18) . . ? C58 B59 C90 115.57(18) . . ? C60 B59 C90 129.27(18) . . ? C54 C53 C58 121.17(18) . . ? C54 C53 N66 119.65(17) . . ? N66 C53 C58 119.17(17) . . ? C53 C54 H54 120.2 . . ? C55 C54 C53 119.70(18) . . ? C55 C54 H54 120.2 . . ? C54 C55 C56 120.95(18) . . ? C54 C55 N67 119.66(18) . . ? C56 C55 N67 119.38(18) . . ? C55 C56 H56 120.4 . . ? C57 C56 C55 119.12(18) . . ? C57 C56 H56 120.4 . . ? C56 C57 C58 121.63(18) . . ? C56 C57 N89 119.52(17) . . ? N89 C57 C58 118.85(17) . . ? C53 C58 B59 121.28(18) . . ? C57 C58 B59 121.53(18) . . ? C57 C58 C53 117.19(17) . . ? C61 C60 B59 125.30(18) . . ? C61 C60 C65 116.58(17) . . ? C65 C60 B59 118.09(17) . . ? C60 C61 H61 118.1 . . ? C62 C61 C60 123.82(19) . . ? C62 C61 H61 118.1 . . ? C61 C62 C63 117.11(19) . . ? C61 C62 C104 121.28(19) . . ? C63 C62 C104 121.55(18) . . ? C62 C63 H63 119.3 . . ? C64 C63 C62 121.43(18) . . ? C64 C63 H63 119.3 . . ? C63 C64 H64 119.9 . . ? C63 C64 C65 120.20(19) . . ? C65 C64 H64 119.9 . . ? C64 C65 C60 119.73(18) . . ? N66 C65 C60 121.05(17) . . ? N66 C65 C64 119.21(17) . . ? C69 C68 C73 118.73(19) . . ? C69 C68 N67 120.1(2) . . ? C73 C68 N67 121.22(19) . . ? C68 C69 H69 119.7 . . ? C70 C69 C68 120.5(2) . . ? C70 C69 H69 119.7 . . ? C69 C70 H70 119.2 . . ? C69 C70 C71 121.5(2) . . ? C71 C70 H70 119.2 . . ? C70 C71 C81 120.9(2) . . ? C72 C71 C70 117.4(2) . . ? C72 C71 C81 121.7(2) . . ? C71 C72 H72 119.2 . . ? C73 C72 C71 121.6(2) . . ? C73 C72 H72 119.2 . . ? C68 C73 H73 119.9 . . ? C72 C73 C68 120.1(2) . . ? C72 C73 H73 119.9 . . ? C75 C74 C79 119.0(2) . . ? C75 C74 N67 119.2(2) . . ? C79 C74 N67 121.8(2) . . ? C74 C75 H75 119.9 . . ? C74 C75 C76 120.3(3) . . ? C76 C75 H75 119.9 . . ? C75 C76 H76 119.2 . . ? C77 C76 C75 121.7(3) . . ? C77 C76 H76 119.2 . . ? C76 C77 C78 117.8(2) . . ? C76 C77 C80 120.0(3) . . ? C78 C77 C80 122.2(3) . . ? C77 C78 H78 119.3 . . ? C77 C78 C79 121.5(3) . . ? C79 C78 H78 119.3 . . ? C74 C79 C78 119.8(3) . . ? C74 C79 H79 120.1 . . ? C78 C79 H79 120.1 . . ? C77 C80 H80A 109.5 . . ? C77 C80 H80B 109.5 . . ? C77 C80 H80C 109.5 . . ? H80A C80 H80B 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C71 C81 H81A 109.5 . . ? C71 C81 H81B 109.5 . . ? C71 C81 H81C 109.5 . . ? H81A C81 H81B 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C83 C82 C87 119.92(18) . . ? C83 C82 N66 120.35(18) . . ? C87 C82 N66 119.50(18) . . ? C82 C83 H83 120.2 . . ? C82 C83 C84 119.64(19) . . ? C84 C83 H83 120.2 . . ? C83 C84 H84 119.2 . . ? C83 C84 C85 121.5(2) . . ? C85 C84 H84 119.2 . . ? C84 C85 C86 117.83(18) . . ? C84 C85 C88 120.83(19) . . ? C86 C85 C88 121.33(19) . . ? C85 C86 H86 119.4 . . ? C87 C86 C85 121.17(19) . . ? C87 C86 H86 119.4 . . ? C82 C87 C86 119.89(19) . . ? C82 C87 H87 120.1 . . ? C86 C87 H87 120.1 . . ? C85 C88 H88A 109.5 . . ? C85 C88 H88B 109.5 . . ? C85 C88 H88C 109.5 . . ? H88A C88 H88B 109.5 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? C91 C90 B59 125.04(17) . . ? C91 C90 C95 116.59(17) . . ? C95 C90 B59 118.36(17) . . ? C90 C91 H91 117.8 . . ? C92 C91 C90 124.33(18) . . ? C92 C91 H91 117.8 . . ? C91 C92 C93 116.79(18) . . ? C91 C92 C103 121.39(18) . . ? C93 C92 C103 121.81(18) . . ? C92 C93 H93 119.1 . . ? C94 C93 C92 121.87(19) . . ? C94 C93 H93 119.1 . . ? C93 C94 H94 119.8 . . ? C93 C94 C95 120.49(19) . . ? C95 C94 H94 119.8 . . ? C94 C95 C90 119.74(18) . . ? N89 C95 C90 120.90(17) . . ? N89 C95 C94 119.36(17) . . ? C97 C96 C101 120.2(2) . . ? C97 C96 N89 119.7(2) . . ? C101 C96 N89 120.04(19) . . ? C96 C97 H97 120.1 . . ? C96 C97 C98 119.7(2) . . ? C98 C97 H97 120.1 . . ? C97 C98 H98 119.5 . . ? C99 C98 C97 121.1(2) . . ? C99 C98 H98 119.5 . . ? C98 C99 C102 120.9(3) . . ? C100 C99 C98 118.3(2) . . ? C100 C99 C102 120.8(3) . . ? C99 C100 H100 119.6 . . ? C99 C100 C101 120.9(2) . . ? C101 C100 H100 119.6 . . ? C96 C101 C100 119.8(2) . . ? C96 C101 H101 120.1 . . ? C100 C101 H101 120.1 . . ? C99 C102 H10A 109.5 . . ? C99 C102 H10B 109.5 . . ? C99 C102 H10C 109.5 . . ? H10A C102 H10B 109.5 . . ? H10A C102 H10C 109.5 . . ? H10B C102 H10C 109.5 . . ? C92 C103 H10D 109.5 . . ? C92 C103 H10E 109.5 . . ? C92 C103 H10F 109.5 . . ? H10D C103 H10E 109.5 . . ? H10D C103 H10F 109.5 . . ? H10E C103 H10F 109.5 . . ? C62 C104 H10G 109.5 . . ? C62 C104 H10H 109.5 . . ? C62 C104 H10I 109.5 . . ? H10G C104 H10H 109.5 . . ? H10G C104 H10I 109.5 . . ? H10H C104 H10I 109.5 . . ? C53 N66 C65 123.19(16) . . ? C53 N66 C82 116.42(15) . . ? C65 N66 C82 119.70(16) . . ? C55 N67 C68 120.75(16) . . ? C55 N67 C74 121.63(17) . . ? C74 N67 C68 116.90(16) . . ? C57 N89 C95 124.09(16) . . ? C57 N89 C96 117.70(16) . . ? C95 N89 C96 118.17(16) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B7 C6 1.503(3) . ? B7 C8 1.546(3) . ? B7 C43 1.551(3) . ? C1 C2 1.394(3) . ? C1 C6 1.417(3) . ? C1 N14 1.399(2) . ? C2 H2 0.9500 . ? C2 C3 1.392(3) . ? C3 C4 1.395(3) . ? C3 N15 1.409(2) . ? C4 H4 0.9500 . ? C4 C5 1.395(3) . ? C5 C6 1.419(3) . ? C5 N37 1.404(2) . ? C8 C9 1.410(3) . ? C8 C13 1.420(3) . ? C9 H9 0.9500 . ? C9 C10 1.383(3) . ? C10 C11 1.401(3) . ? C10 C52 1.510(3) . ? C11 H11 0.9500 . ? C11 C12 1.375(3) . ? C12 H12 0.9500 . ? C12 C13 1.409(3) . ? C13 N14 1.402(2) . ? C16 C17 1.388(3) . ? C16 C21 1.391(3) . ? C16 N15 1.429(2) . ? C17 H17 0.9500 . ? C17 C18 1.387(3) . ? C18 H18 0.9500 . ? C18 C19 1.393(3) . ? C19 C20 1.389(3) . ? C19 C29 1.506(3) . ? C20 H20 0.9500 . ? C20 C21 1.389(3) . ? C21 H21 0.9500 . ? C22 C23 1.394(3) . ? C22 C27 1.391(3) . ? C22 N15 1.432(3) . ? C23 H23 0.9500 . ? C23 C24 1.386(3) . ? C24 H24 0.9500 . ? C24 C25 1.388(3) . ? C25 C26 1.390(3) . ? C25 C28 1.513(3) . ? C26 H26 0.9500 . ? C26 C27 1.385(3) . ? C27 H27 0.9500 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.385(3) . ? C30 C35 1.388(3) . ? C30 N14 1.442(2) . ? C31 H31 0.9500 . ? C31 C32 1.390(3) . ? C32 H32 0.9500 . ? C32 C33 1.390(3) . ? C33 C34 1.395(3) . ? C33 C36 1.506(3) . ? C34 H34 0.9500 . ? C34 C35 1.386(3) . ? C35 H35 0.9500 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C38 C39 1.407(3) . ? C38 C43 1.420(3) . ? C38 N37 1.402(3) . ? C39 H39 0.9500 . ? C39 C40 1.379(3) . ? C40 H40 0.9500 . ? C40 C41 1.393(3) . ? C41 C42 1.382(3) . ? C41 C51 1.511(3) . ? C42 H42 0.9500 . ? C42 C43 1.413(3) . ? C44 C45 1.383(3) . ? C44 C49 1.384(3) . ? C44 N37 1.444(2) . ? C45 H45 0.9500 . ? C45 C46 1.394(3) . ? C46 H46 0.9500 . ? C46 C47 1.393(3) . ? C47 C48 1.389(3) . ? C47 C50 1.508(3) . ? C48 H48 0.9500 . ? C48 C49 1.395(3) . ? C49 H49 0.9500 . ? 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 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? B59 C58 1.500(3) . ? B59 C60 1.544(3) . ? B59 C90 1.546(3) . ? C53 C54 1.395(3) . ? C53 C58 1.421(3) . ? C53 N66 1.396(2) . ? C54 H54 0.9500 . ? C54 C55 1.391(3) . ? C55 C56 1.400(3) . ? C55 N67 1.406(3) . ? C56 H56 0.9500 . ? C56 C57 1.394(3) . ? C57 C58 1.421(3) . ? C57 N89 1.398(2) . ? C60 C61 1.411(3) . ? C60 C65 1.418(3) . ? C61 H61 0.9500 . ? C61 C62 1.382(3) . ? C62 C63 1.404(3) . ? C62 C104 1.510(3) . ? C63 H63 0.9500 . ? C63 C64 1.379(3) . ? C64 H64 0.9500 . ? C64 C65 1.408(3) . ? C65 N66 1.406(2) . ? C68 C69 1.386(3) . ? C68 C73 1.389(3) . ? C68 N67 1.430(3) . ? C69 H69 0.9500 . ? C69 C70 1.382(3) . ? C70 H70 0.9500 . ? C70 C71 1.389(3) . ? C71 C72 1.388(3) . ? C71 C81 1.505(3) . ? C72 H72 0.9500 . ? C72 C73 1.387(3) . ? C73 H73 0.9500 . ? C74 C75 1.380(3) . ? C74 C79 1.386(3) . ? C74 N67 1.427(3) . ? C75 H75 0.9500 . ? C75 C76 1.387(3) . ? C76 H76 0.9500 . ? C76 C77 1.371(5) . ? C77 C78 1.384(5) . ? C77 C80 1.515(4) . ? C78 H78 0.9500 . ? C78 C79 1.390(4) . ? C79 H79 0.9500 . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? C82 C83 1.385(3) . ? C82 C87 1.388(3) . ? C82 N66 1.444(2) . ? C83 H83 0.9500 . ? C83 C84 1.388(3) . ? C84 H84 0.9500 . ? C84 C85 1.394(3) . ? C85 C86 1.394(3) . ? C85 C88 1.509(3) . ? C86 H86 0.9500 . ? C86 C87 1.388(3) . ? C87 H87 0.9500 . ? C88 H88A 0.9800 . ? C88 H88B 0.9800 . ? C88 H88C 0.9800 . ? C90 C91 1.410(3) . ? C90 C95 1.417(3) . ? C91 H91 0.9500 . ? C91 C92 1.384(3) . ? C92 C93 1.398(3) . ? C92 C103 1.509(3) . ? C93 H93 0.9500 . ? C93 C94 1.375(3) . ? C94 H94 0.9500 . ? C94 C95 1.410(3) . ? C95 N89 1.409(2) . ? C96 C97 1.376(3) . ? C96 C101 1.382(3) . ? C96 N89 1.447(2) . ? C97 H97 0.9500 . ? C97 C98 1.392(3) . ? C98 H98 0.9500 . ? C98 C99 1.389(4) . ? C99 C100 1.388(4) . ? C99 C102 1.514(3) . ? C100 H100 0.9500 . ? C100 C101 1.393(3) . ? C101 H101 0.9500 . ? C102 H10A 0.9800 . ? C102 H10B 0.9800 . ? C102 H10C 0.9800 . ? C103 H10D 0.9800 . ? C103 H10E 0.9800 . ? C103 H10F 0.9800 . ? C104 H10G 0.9800 . ? C104 H10H 0.9800 . ? C104 H10I 0.9800 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag B7 C8 C9 C10 -173.8(2) . . . . ? B7 C8 C13 C12 170.70(19) . . . . ? B7 C8 C13 N14 -9.3(3) . . . . ? C1 C2 C3 C4 0.4(3) . . . . ? C1 C2 C3 N15 179.74(18) . . . . ? C2 C1 C6 B7 173.63(19) . . . . ? C2 C1 C6 C5 -5.1(3) . . . . ? C2 C1 N14 C13 -170.13(19) . . . . ? C2 C1 N14 C30 3.4(3) . . . . ? C2 C3 C4 C5 -1.8(3) . . . . ? C2 C3 N15 C16 150.94(19) . . . . ? C2 C3 N15 C22 -16.5(3) . . . . ? C3 C4 C5 C6 -0.3(3) . . . . ? C3 C4 C5 N37 178.85(18) . . . . ? C4 C3 N15 C16 -29.7(3) . . . . ? C4 C3 N15 C22 162.86(19) . . . . ? C4 C5 C6 B7 -175.10(19) . . . . ? C4 C5 C6 C1 3.6(3) . . . . ? C4 C5 N37 C38 178.08(18) . . . . ? C4 C5 N37 C44 -9.4(3) . . . . ? C6 B7 C8 C9 -169.6(2) . . . . ? C6 B7 C8 C13 11.7(3) . . . . ? C6 B7 C43 C38 5.6(3) . . . . ? C6 B7 C43 C42 -172.92(19) . . . . ? C6 C1 C2 C3 3.2(3) . . . . ? C6 C1 N14 C13 10.4(3) . . . . ? C6 C1 N14 C30 -176.14(17) . . . . ? C6 C5 N37 C38 -2.8(3) . . . . ? C6 C5 N37 C44 169.75(18) . . . . ? C8 B7 C6 C1 -3.8(3) . . . . ? C8 B7 C6 C5 174.84(18) . . . . ? C8 B7 C43 C38 -176.6(2) . . . . ? C8 B7 C43 C42 4.8(3) . . . . ? C8 C9 C10 C11 1.4(3) . . . . ? C8 C9 C10 C52 179.8(2) . . . . ? C8 C13 N14 C1 -1.9(3) . . . . ? C8 C13 N14 C30 -175.23(18) . . . . ? C9 C8 C13 C12 -8.1(3) . . . . ? C9 C8 C13 N14 171.91(19) . . . . ? C9 C10 C11 C12 -4.7(3) . . . . ? C10 C11 C12 C13 1.4(3) . . . . ? C11 C12 C13 C8 5.3(3) . . . . ? C11 C12 C13 N14 -174.8(2) . . . . ? C12 C13 N14 C1 178.10(18) . . . . ? C12 C13 N14 C30 4.8(3) . . . . ? C13 C8 C9 C10 4.9(3) . . . . ? C16 C17 C18 C19 0.6(3) . . . . ? C17 C16 C21 C20 -1.0(3) . . . . ? C17 C16 N15 C3 -45.3(3) . . . . ? C17 C16 N15 C22 122.5(2) . . . . ? C17 C18 C19 C20 -1.0(3) . . . . ? C17 C18 C19 C29 178.6(2) . . . . ? C18 C19 C20 C21 0.4(3) . . . . ? C19 C20 C21 C16 0.6(3) . . . . ? C21 C16 C17 C18 0.5(3) . . . . ? C21 C16 N15 C3 137.3(2) . . . . ? C21 C16 N15 C22 -54.9(3) . . . . ? C22 C23 C24 C25 1.8(3) . . . . ? C23 C22 C27 C26 0.9(3) . . . . ? C23 C22 N15 C3 -53.6(3) . . . . ? C23 C22 N15 C16 138.4(2) . . . . ? C23 C24 C25 C26 0.0(3) . . . . ? C23 C24 C25 C28 179.8(2) . . . . ? C24 C25 C26 C27 -1.3(3) . . . . ? C25 C26 C27 C22 0.9(3) . . . . ? C27 C22 C23 C24 -2.2(3) . . . . ? C27 C22 N15 C3 125.9(2) . . . . ? C27 C22 N15 C16 -42.1(3) . . . . ? C28 C25 C26 C27 178.9(2) . . . . ? C29 C19 C20 C21 -179.2(2) . . . . ? C30 C31 C32 C33 -0.1(3) . . . . ? C31 C30 C35 C34 -0.5(3) . . . . ? C31 C30 N14 C1 78.9(2) . . . . ? C31 C30 N14 C13 -107.3(2) . . . . ? C31 C32 C33 C34 -0.7(3) . . . . ? C31 C32 C33 C36 179.4(2) . . . . ? C32 C33 C34 C35 0.9(3) . . . . ? C33 C34 C35 C30 -0.4(3) . . . . ? C35 C30 C31 C32 0.7(3) . . . . ? C35 C30 N14 C1 -95.9(2) . . . . ? C35 C30 N14 C13 77.9(2) . . . . ? C36 C33 C34 C35 -179.2(2) . . . . ? C38 C39 C40 C41 2.5(3) . . . . ? C39 C38 C43 B7 177.35(18) . . . . ? C39 C38 C43 C42 -4.0(3) . . . . ? C39 C38 N37 C5 -178.90(18) . . . . ? C39 C38 N37 C44 8.7(3) . . . . ? C39 C40 C41 C42 -3.1(3) . . . . ? C39 C40 C41 C51 179.0(2) . . . . ? C40 C41 C42 C43 0.1(3) . . . . ? C41 C42 C43 B7 -178.1(2) . . . . ? C41 C42 C43 C38 3.4(3) . . . . ? C43 B7 C6 C1 174.25(18) . . . . ? C43 B7 C6 C5 -7.1(3) . . . . ? C43 B7 C8 C9 12.7(4) . . . . ? C43 B7 C8 C13 -166.0(2) . . . . ? C43 C38 C39 C40 1.3(3) . . . . ? C43 C38 N37 C5 1.6(3) . . . . ? C43 C38 N37 C44 -170.77(18) . . . . ? C44 C45 C46 C47 -0.5(3) . . . . ? C45 C44 C49 C48 0.4(3) . . . . ? C45 C44 N37 C5 -85.4(2) . . . . ? C45 C44 N37 C38 87.5(2) . . . . ? C45 C46 C47 C48 0.3(3) . . . . ? C45 C46 C47 C50 179.2(2) . . . . ? C46 C47 C48 C49 0.2(3) . . . . ? C47 C48 C49 C44 -0.6(3) . . . . ? C49 C44 C45 C46 0.1(3) . . . . ? C49 C44 N37 C5 91.8(2) . . . . ? C49 C44 N37 C38 -95.3(2) . . . . ? C50 C47 C48 C49 -178.6(2) . . . . ? C51 C41 C42 C43 178.0(2) . . . . ? C52 C10 C11 C12 176.9(2) . . . . ? N14 C1 C2 C3 -176.26(18) . . . . ? N14 C1 C6 B7 -6.9(3) . . . . ? N14 C1 C6 C5 174.40(17) . . . . ? N14 C30 C31 C32 -173.99(17) . . . . ? N14 C30 C35 C34 174.23(17) . . . . ? N15 C3 C4 C5 178.82(18) . . . . ? N15 C16 C17 C18 -176.91(19) . . . . ? N15 C16 C21 C20 176.43(19) . . . . ? N15 C22 C23 C24 177.36(18) . . . . ? N15 C22 C27 C26 -178.64(19) . . . . ? N37 C5 C6 B7 5.8(3) . . . . ? N37 C5 C6 C1 -175.52(17) . . . . ? N37 C38 C39 C40 -178.25(19) . . . . ? N37 C38 C43 B7 -3.2(3) . . . . ? N37 C38 C43 C42 175.54(18) . . . . ? N37 C44 C45 C46 177.29(18) . . . . ? N37 C44 C49 C48 -176.78(18) . . . . ? B59 C60 C61 C62 -176.7(2) . . . . ? B59 C60 C65 C64 170.60(18) . . . . ? B59 C60 C65 N66 -9.9(3) . . . . ? B59 C90 C91 C92 -177.77(19) . . . . ? B59 C90 C95 C94 175.73(18) . . . . ? B59 C90 C95 N89 -3.7(3) . . . . ? C53 C54 C55 C56 -1.1(3) . . . . ? C53 C54 C55 N67 178.1(2) . . . . ? C54 C53 C58 B59 174.64(19) . . . . ? C54 C53 C58 C57 -4.6(3) . . . . ? C54 C53 N66 C65 -169.04(19) . . . . ? C54 C53 N66 C82 1.4(3) . . . . ? C54 C55 C56 C57 -3.0(3) . . . . ? C54 C55 N67 C68 -9.5(3) . . . . ? C54 C55 N67 C74 160.5(2) . . . . ? C55 C56 C57 C58 3.2(3) . . . . ? C55 C56 C57 N89 -177.02(19) . . . . ? C56 C55 N67 C68 169.7(2) . . . . ? C56 C55 N67 C74 -20.3(3) . . . . ? C56 C57 C58 B59 -178.76(19) . . . . ? C56 C57 C58 C53 0.5(3) . . . . ? C56 C57 N89 C95 -175.20(19) . . . . ? C56 C57 N89 C96 2.5(3) . . . . ? C58 B59 C60 C61 -163.88(19) . . . . ? C58 B59 C60 C65 14.2(3) . . . . ? C58 B59 C90 C91 -170.50(19) . . . . ? C58 B59 C90 C95 8.9(3) . . . . ? C58 C53 C54 C55 5.0(3) . . . . ? C58 C53 N66 C65 12.0(3) . . . . ? C58 C53 N66 C82 -177.55(18) . . . . ? C58 C57 N89 C95 4.6(3) . . . . ? C58 C57 N89 C96 -177.73(18) . . . . ? C60 B59 C58 C53 -6.2(3) . . . . ? C60 B59 C58 C57 173.02(18) . . . . ? C60 B59 C90 C91 8.5(3) . . . . ? C60 B59 C90 C95 -172.2(2) . . . . ? C60 C61 C62 C63 4.1(3) . . . . ? C60 C61 C62 C104 -173.4(2) . . . . ? C60 C65 N66 C53 -3.5(3) . . . . ? C60 C65 N66 C82 -173.64(18) . . . . ? C61 C60 C65 C64 -11.2(3) . . . . ? C61 C60 C65 N66 168.32(18) . . . . ? C61 C62 C63 C64 -7.7(3) . . . . ? C62 C63 C64 C65 1.8(3) . . . . ? C63 C64 C65 C60 8.0(3) . . . . ? C63 C64 C65 N66 -171.54(19) . . . . ? C64 C65 N66 C53 175.99(18) . . . . ? C64 C65 N66 C82 5.9(3) . . . . ? C65 C60 C61 C62 5.2(3) . . . . ? C68 C69 C70 C71 0.9(4) . . . . ? C69 C68 C73 C72 -2.2(3) . . . . ? C69 C68 N67 C55 121.4(2) . . . . ? C69 C68 N67 C74 -49.0(3) . . . . ? C69 C70 C71 C72 -2.0(4) . . . . ? C69 C70 C71 C81 177.2(2) . . . . ? C70 C71 C72 C73 1.1(3) . . . . ? C71 C72 C73 C68 1.0(3) . . . . ? C73 C68 C69 C70 1.2(4) . . . . ? C73 C68 N67 C55 -58.1(3) . . . . ? C73 C68 N67 C74 131.4(2) . . . . ? C74 C75 C76 C77 2.2(4) . . . . ? C75 C74 C79 C78 -1.5(4) . . . . ? C75 C74 N67 C55 134.5(2) . . . . ? C75 C74 N67 C68 -55.1(3) . . . . ? C75 C76 C77 C78 -1.9(5) . . . . ? C75 C76 C77 C80 177.7(3) . . . . ? C76 C77 C78 C79 -0.1(4) . . . . ? C77 C78 C79 C74 1.7(4) . . . . ? C79 C74 C75 C76 -0.4(4) . . . . ? C79 C74 N67 C55 -46.3(3) . . . . ? C79 C74 N67 C68 124.1(2) . . . . ? C80 C77 C78 C79 -179.6(3) . . . . ? C81 C71 C72 C73 -178.2(2) . . . . ? C82 C83 C84 C85 0.0(3) . . . . ? C83 C82 C87 C86 -1.5(3) . . . . ? C83 C82 N66 C53 79.9(2) . . . . ? C83 C82 N66 C65 -109.3(2) . . . . ? C83 C84 C85 C86 -1.3(3) . . . . ? C83 C84 C85 C88 179.73(19) . . . . ? C84 C85 C86 C87 1.2(3) . . . . ? C85 C86 C87 C82 0.2(3) . . . . ? C87 C82 C83 C84 1.4(3) . . . . ? C87 C82 N66 C53 -94.6(2) . . . . ? C87 C82 N66 C65 76.2(2) . . . . ? C88 C85 C86 C87 -179.82(19) . . . . ? C90 B59 C58 C53 172.88(18) . . . . ? C90 B59 C58 C57 -7.9(3) . . . . ? C90 B59 C60 C61 17.2(3) . . . . ? C90 B59 C60 C65 -164.8(2) . . . . ? C90 C91 C92 C93 1.0(3) . . . . ? C90 C91 C92 C103 180.00(19) . . . . ? C90 C95 N89 C57 -3.3(3) . . . . ? C90 C95 N89 C96 178.98(18) . . . . ? C91 C90 C95 C94 -4.8(3) . . . . ? C91 C90 C95 N89 175.70(18) . . . . ? C91 C92 C93 C94 -3.0(3) . . . . ? C92 C93 C94 C95 1.0(3) . . . . ? C93 C94 C95 C90 3.1(3) . . . . ? C93 C94 C95 N89 -177.42(19) . . . . ? C94 C95 N89 C57 177.21(19) . . . . ? C94 C95 N89 C96 -0.5(3) . . . . ? C95 C90 C91 C92 2.9(3) . . . . ? C96 C97 C98 C99 -0.9(4) . . . . ? C97 C96 C101 C100 -0.1(3) . . . . ? C97 C96 N89 C57 87.5(2) . . . . ? C97 C96 N89 C95 -94.6(2) . . . . ? C97 C98 C99 C100 0.3(4) . . . . ? C97 C98 C99 C102 179.9(2) . . . . ? C98 C99 C100 C101 0.4(4) . . . . ? C99 C100 C101 C96 -0.5(3) . . . . ? C101 C96 C97 C98 0.8(3) . . . . ? C101 C96 N89 C57 -90.8(2) . . . . ? C101 C96 N89 C95 87.0(2) . . . . ? C102 C99 C100 C101 -179.2(2) . . . . ? C103 C92 C93 C94 178.0(2) . . . . ? C104 C62 C63 C64 169.8(2) . . . . ? N66 C53 C54 C55 -173.95(19) . . . . ? N66 C53 C58 B59 -6.4(3) . . . . ? N66 C53 C58 C57 174.28(17) . . . . ? N66 C82 C83 C84 -173.03(17) . . . . ? N66 C82 C87 C86 173.00(18) . . . . ? N67 C55 C56 C57 177.84(19) . . . . ? N67 C68 C69 C70 -178.4(2) . . . . ? N67 C68 C73 C72 177.41(19) . . . . ? N67 C74 C75 C76 178.8(2) . . . . ? N67 C74 C79 C78 179.3(2) . . . . ? N89 C57 C58 B59 1.5(3) . . . . ? N89 C57 C58 C53 -179.25(18) . . . . ? N89 C96 C97 C98 -177.5(2) . . . . ? N89 C96 C101 C100 178.24(19) . . . . ?