#------------------------------------------------------------------------------ #$Date: 2024-12-06 18:41:39 +0200 (Fri, 06 Dec 2024) $ #$Revision: 296393 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/27/1572743.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_1572743 loop_ _publ_author_name 'Valdés, Hugo' 'Alpuente, Nora' 'Salvador, Pedro' 'Hashmi, A Stephen K' 'Ribas, Xavi' _publ_section_title ; CCC-NHC Au(iii) pincer complexes as a reliable platform for isolating elusive species. ; _journal_issue 42 _journal_name_full 'Chemical science' _journal_page_first 17618 _journal_page_last 17628 _journal_paper_doi 10.1039/d4sc02999b _journal_volume 15 _journal_year 2024 _chemical_formula_moiety '2(C30 H35 N6), 6(B F4), C2 H3 N' _chemical_formula_sum 'C62 H73 B6 F24 N13' _chemical_formula_weight 1521.19 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _audit_update_record ; 2024-02-20 deposited with the CCDC. 2024-10-02 downloaded from the CCDC. ; _cell_angle_alpha 95.25(4) _cell_angle_beta 99.16(4) _cell_angle_gamma 108.37(3) _cell_formula_units_Z 2 _cell_length_a 14.84(2) _cell_length_b 15.50(2) _cell_length_c 16.50(3) _cell_measurement_reflns_used 8974 _cell_measurement_temperature 100.(2) _cell_measurement_theta_max 26.1310 _cell_measurement_theta_min 2.8878 _cell_volume 3515(9) _computing_cell_refinement 'SAINT V8.38A (Bruker AXS Inc., 2017)' _computing_data_collection 'Bruker Instrument Service vV6.2.9' _computing_data_reduction 'SAINT V8.38A (Bruker AXS Inc., 2017)' _computing_molecular_graphics 'shelXle (C.B. Huebschle, rev 882)' _computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 100.(2) _diffrn_detector_area_resol_mean 7.3910 _diffrn_measured_fraction_theta_full 0.966 _diffrn_measured_fraction_theta_max 0.966 _diffrn_measurement_device_type 'D8 QUEST ECO' _diffrn_measurement_method 'omega scans' _diffrn_radiation_monochromator 'doubly curved silicon crystal Bruker Triumph' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71076 _diffrn_reflns_av_R_equivalents 0.0603 _diffrn_reflns_av_unetI/netI 0.1016 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 33289 _diffrn_reflns_theta_full 26.20 _diffrn_reflns_theta_max 26.20 _diffrn_reflns_theta_min 2.69 _diffrn_source_type 'Ceramic x-ray tube' _exptl_absorpt_coefficient_mu 0.130 _exptl_absorpt_correction_T_max 0.75 _exptl_absorpt_correction_T_min 0.61 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.438 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 1564 _exptl_crystal_size_max 0.220 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.080 _refine_diff_density_max 0.724 _refine_diff_density_min -0.400 _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 959 _refine_ls_number_reflns 13648 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.019 _refine_ls_R_factor_all 0.1383 _refine_ls_R_factor_gt 0.0668 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0563P)^2^+3.2360P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1409 _refine_ls_wR_factor_ref 0.1654 _reflns_number_gt 7491 _reflns_number_total 13648 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc02999b3.cif _cod_data_source_block HV164 _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was changed to 'multi-scan' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas Adding full bibliography for 1572736--1572746.cif. ; _cod_original_cell_volume 3515.(9) _cod_database_code 1572743 _shelx_res_file ; TITL HV164_0m_a.res in P-1 HV164_0m_a.res created by SHELXL-2017/1 at 13:05:33 on 24-Nov-2021 REM Old TITL Integration of HV164 REM SHELXT solution in P-1 REM R1 0.213, Rweak 0.040, Alpha 0.084, Orientation as input REM Formula found by SHELXT: C64 B6 F24 N11 CELL 0.71076 14.8371 15.5015 16.4971 95.251 99.159 108.369 ZERR 2.000 0.0223 0.0222 0.0261 0.044 0.040 0.034 LATT 1 SFAC C H B F N UNIT 124 146 12 48 26 TEMP -173.190 SIZE 0.080 0.120 0.220 L.S. 10 BOND $H conf acta LIST 6 FMAP 2 PLAN 20 dfix 1.54 0.001 c21' c22' EADP c21' c21 eadp c22' c22 OMIT 1 1 1 OMIT 8 10 6 OMIT 11 5 9 OMIT -17 1 6 OMIT -16 0 8 OMIT 8 9 7 OMIT -16 -1 9 OMIT 8 8 10 OMIT -17 1 7 OMIT 8 9 8 OMIT 8 8 9 OMIT -16 0 7 OMIT -16 0 9 OMIT -15 -2 8 OMIT 15 -3 4 OMIT 1 -2 1 OMIT -1 1 2 WGHT 0.056300 3.236000 FVAR 0.37248 0.88296 N7 5 0.167519 0.111656 0.581184 11.00000 0.01200 0.01571 = 0.02052 0.00357 0.00865 0.00472 N8 5 0.137011 0.130090 0.523575 11.00000 0.01708 0.02467 = 0.02284 0.00826 0.00588 0.00888 N10 5 0.000952 0.057243 0.761609 11.00000 0.01031 0.02626 = 0.01805 0.00312 0.00499 0.00494 N12 5 -0.062126 0.035587 0.871476 11.00000 0.01739 0.02443 = 0.01916 0.00358 0.00636 0.00598 N24 5 0.455915 0.119368 0.615428 11.00000 0.01068 0.01421 = 0.02030 0.00673 0.00744 0.00502 N26 5 0.607283 0.137045 0.615181 11.00000 0.00968 0.01466 = 0.01792 0.00366 0.00403 0.00230 C1 1 0.208810 0.089484 0.656687 11.00000 0.01412 0.01515 = 0.01485 0.00226 0.00031 0.00578 C2 1 0.147939 0.057761 0.711129 11.00000 0.01714 0.02086 = 0.01729 -0.00002 0.00441 0.00748 C3 1 0.192045 0.042377 0.785558 11.00000 0.01873 0.03174 = 0.01942 0.00737 0.00986 0.00855 AFIX 43 H3 2 0.154193 0.020381 0.825438 11.00000 -1.20000 AFIX 0 C4 1 0.290523 0.058429 0.803175 11.00000 0.02158 0.03018 = 0.01513 0.00699 0.00246 0.01113 AFIX 43 H4 2 0.319295 0.047618 0.855230 11.00000 -1.20000 AFIX 0 C5 1 0.348254 0.089889 0.746775 11.00000 0.01512 0.01880 = 0.02324 0.00000 0.00152 0.00745 AFIX 43 H5 2 0.415886 0.100382 0.760376 11.00000 -1.20000 AFIX 0 C6 1 0.308264 0.106037 0.671182 11.00000 0.01361 0.01197 = 0.01699 0.00121 0.00242 0.00509 C9 1 0.039188 0.037339 0.688692 11.00000 0.01522 0.04008 = 0.01600 0.00472 0.00918 0.01006 AFIX 23 H9A 2 0.024851 0.075064 0.646390 11.00000 -1.20000 H9AB 2 0.006941 -0.028224 0.664433 11.00000 -1.20000 AFIX 0 C11 1 -0.044188 -0.005399 0.804803 11.00000 0.01415 0.02837 = 0.02349 0.00430 0.00373 0.00979 AFIX 43 H11 2 -0.061084 -0.069994 0.790048 11.00000 -1.20000 AFIX 0 C13 1 -0.026891 0.129969 0.871912 11.00000 0.01024 0.02744 = 0.02221 0.00126 0.00076 0.00566 C14 1 -0.024525 0.203466 0.928021 11.00000 0.02421 0.03541 = 0.02672 -0.00327 0.00410 0.01111 AFIX 43 H14 2 -0.050077 0.194592 0.977067 11.00000 -1.20000 AFIX 0 C15 1 0.016593 0.289354 0.908855 11.00000 0.02783 0.02860 = 0.05031 -0.00507 0.00413 0.01110 AFIX 43 H15 2 0.019905 0.341453 0.945859 11.00000 -1.20000 AFIX 0 C16 1 0.053770 0.302923 0.836849 11.00000 0.02100 0.02577 = 0.05355 0.01064 0.00405 0.00489 AFIX 43 H16 2 0.080430 0.363869 0.825682 11.00000 -1.20000 AFIX 0 C17 1 0.052994 0.230405 0.781276 11.00000 0.01934 0.03187 = 0.03259 0.00938 0.00354 0.00727 AFIX 43 H17 2 0.078533 0.239375 0.732232 11.00000 -1.20000 AFIX 0 C18 1 0.012716 0.144025 0.801568 11.00000 0.01061 0.02490 = 0.01943 0.00050 -0.00020 0.00532 C19 1 -0.117463 -0.013144 0.930124 11.00000 0.02590 0.03137 = 0.02706 0.00967 0.01387 0.00940 AFIX 23 H19A 2 -0.097752 0.026746 0.984750 11.00000 -1.20000 H19B 2 -0.100959 -0.069384 0.937646 11.00000 -1.20000 AFIX 0 C20 1 -0.224474 -0.039381 0.901842 11.00000 0.03208 0.06153 = 0.04080 0.02988 0.01798 0.01549 AFIX 23 part 1 21 H20A 2 -0.256923 -0.072346 0.943513 21.00000 -1.20000 H20B 2 -0.244557 -0.082419 0.848971 21.00000 -1.20000 AFIX 23 part 2 -21 H20C 2 -0.251210 -0.107205 0.887635 -21.00000 -1.20000 H20D 2 -0.236261 -0.013944 0.849825 -21.00000 -1.20000 AFIX 0 part 1 21 C21 1 -0.258376 0.040663 0.889127 21.00000 0.03006 0.04886 = 0.05959 0.03294 0.01574 0.01499 AFIX 23 H21A 2 -0.227347 0.072199 0.846114 21.00000 -1.20000 H21B 2 -0.235739 0.084728 0.941468 21.00000 -1.20000 AFIX 0 C22 1 -0.365857 0.017069 0.863623 21.00000 0.03930 0.04759 = 0.13286 0.04706 0.02733 0.01952 AFIX 137 H22A 2 -0.380884 0.072709 0.853049 21.00000 -1.50000 H22B 2 -0.397215 -0.008585 0.908169 21.00000 -1.50000 H22C 2 -0.389778 -0.028350 0.812967 21.00000 -1.50000 AFIX 0 part 2 -21 C21' 1 -0.287853 -0.007758 0.965332 -21.00000 0.03006 0.04886 = 0.05959 0.03294 0.01574 0.01499 AFIX 23 H21C 2 -0.302104 -0.058366 0.998949 -21.00000 -1.20000 H21D 2 -0.238551 0.045047 1.003283 -21.00000 -1.20000 AFIX 0 C22' 1 -0.379653 0.019651 0.957618 -21.00000 0.03930 0.04759 = 0.13286 0.04706 0.02733 0.01952 AFIX 137 H22D 2 -0.364794 0.082221 0.944027 -21.00000 -1.50000 H22E 2 -0.402051 0.017306 1.010404 -21.00000 -1.50000 H22F 2 -0.430535 -0.023130 0.913513 -21.00000 -1.50000 AFIX 0 part 0 C23 1 0.366681 0.141760 0.607193 11.00000 0.01174 0.02214 = 0.02343 0.00424 0.00337 0.01032 AFIX 23 H23A 2 0.326840 0.115092 0.551038 11.00000 -1.20000 H23B 2 0.383135 0.209365 0.612899 11.00000 -1.20000 AFIX 0 C25 1 0.543677 0.179457 0.618890 11.00000 0.01516 0.01694 = 0.01819 0.00476 0.00602 0.00711 AFIX 43 H25 2 0.558396 0.244167 0.623423 11.00000 -1.20000 AFIX 0 C27 1 0.559323 0.042935 0.608621 11.00000 0.01516 0.02055 = 0.01138 0.00607 0.00340 0.00565 C28 1 0.592348 -0.031005 0.601166 11.00000 0.01184 0.02018 = 0.02158 0.00696 0.00461 0.00840 AFIX 43 H28 2 0.658526 -0.022805 0.601004 11.00000 -1.20000 AFIX 0 C29 1 0.524383 -0.117003 0.594001 11.00000 0.02015 0.01970 = 0.02314 0.00539 0.00635 0.01041 AFIX 43 H29 2 0.543925 -0.169697 0.589095 11.00000 -1.20000 AFIX 0 C30 1 0.427414 -0.128158 0.593816 11.00000 0.01747 0.01344 = 0.02532 0.00596 0.00460 0.00233 AFIX 43 H30 2 0.382835 -0.188684 0.588978 11.00000 -1.20000 AFIX 0 C31 1 0.393369 -0.055400 0.600329 11.00000 0.01258 0.02050 = 0.02062 0.00331 0.00264 0.00320 AFIX 43 H31 2 0.326975 -0.063726 0.599495 11.00000 -1.20000 AFIX 0 C32 1 0.462623 0.030890 0.608190 11.00000 0.01524 0.01593 = 0.01446 0.00326 0.00356 0.00734 C33 1 0.710633 0.180212 0.614056 11.00000 0.01035 0.01846 = 0.02540 0.00285 0.00458 0.00280 AFIX 23 H33A 2 0.722828 0.244854 0.605090 11.00000 -1.20000 H33B 2 0.726805 0.147762 0.566883 11.00000 -1.20000 AFIX 0 C34 1 0.776109 0.178289 0.693667 11.00000 0.01679 0.01763 = 0.02926 0.00566 0.00313 0.00574 AFIX 23 H34A 2 0.844298 0.203542 0.687251 11.00000 -1.20000 H34B 2 0.763428 0.113513 0.702360 11.00000 -1.20000 AFIX 0 C35 1 0.763690 0.232032 0.770432 11.00000 0.03289 0.02852 = 0.02352 0.00778 0.00338 0.01155 AFIX 23 H35A 2 0.695689 0.206413 0.777251 11.00000 -1.20000 H35B 2 0.805625 0.223261 0.819755 11.00000 -1.20000 AFIX 0 C36 1 0.788044 0.333916 0.767731 11.00000 0.05558 0.02511 = 0.03304 0.00114 0.00523 0.01505 AFIX 137 H36A 2 0.854659 0.359707 0.759353 11.00000 -1.50000 H36B 2 0.781940 0.364461 0.820266 11.00000 -1.50000 H36C 2 0.743319 0.343629 0.721826 11.00000 -1.50000 AFIX 0 N7A 5 0.328384 0.384907 0.406705 11.00000 0.01433 0.02082 = 0.01872 0.00385 0.00762 0.00792 N8A 5 0.360980 0.363721 0.461874 11.00000 0.01630 0.03118 = 0.02479 0.00956 0.00484 0.00925 N10A 5 0.501472 0.467424 0.234255 11.00000 0.01624 0.02575 = 0.01789 0.00423 0.00556 0.00584 N12A 5 0.595884 0.514014 0.147540 11.00000 0.01861 0.02855 = 0.02077 0.01061 0.00693 0.01137 N24A 5 0.040148 0.376220 0.376166 11.00000 0.01234 0.01742 = 0.02167 0.00586 0.00683 0.00796 N26A 5 -0.110649 0.362520 0.374380 11.00000 0.01062 0.01276 = 0.02294 0.00396 0.00604 0.00205 C1A 1 0.286010 0.409082 0.333268 11.00000 0.01614 0.01758 = 0.01492 0.00206 0.00164 0.00825 C2A 1 0.347242 0.446531 0.280311 11.00000 0.01461 0.02308 = 0.01874 0.00098 0.00603 0.00751 C3A 1 0.302398 0.462749 0.206529 11.00000 0.02018 0.02725 = 0.01642 0.00336 0.01037 0.00580 AFIX 43 H3A 2 0.340411 0.488986 0.168075 11.00000 -1.20000 AFIX 0 C4A 1 0.203502 0.441659 0.187434 11.00000 0.02157 0.02504 = 0.01784 0.00282 -0.00015 0.01084 AFIX 43 H4A 2 0.174238 0.451403 0.135103 11.00000 -1.20000 AFIX 0 C5A 1 0.145760 0.406539 0.242880 11.00000 0.01878 0.02065 = 0.02335 0.00155 0.00512 0.01041 AFIX 43 H5A 2 0.077821 0.394235 0.228854 11.00000 -1.20000 AFIX 0 C6A 1 0.185707 0.389310 0.317959 11.00000 0.01335 0.01414 = 0.02155 0.00245 0.00627 0.00561 C9A 1 0.455794 0.471138 0.305550 11.00000 0.01273 0.04292 = 0.01865 0.00384 0.00515 0.00648 AFIX 23 H9AA 2 0.483485 0.533912 0.337612 11.00000 -1.20000 H9AC 2 0.470287 0.428032 0.342136 11.00000 -1.20000 AFIX 0 C11A 1 0.558881 0.539135 0.208915 11.00000 0.01585 0.02960 = 0.02361 0.00924 0.00769 0.01138 AFIX 43 H11A 2 0.571803 0.601196 0.232202 11.00000 -1.20000 AFIX 0 C13A 1 0.560514 0.419021 0.130357 11.00000 0.01629 0.03628 = 0.01782 0.00375 0.00255 0.01269 C14A 1 0.574697 0.358706 0.070502 11.00000 0.02515 0.03746 = 0.02908 0.00273 0.00472 0.01643 AFIX 43 H14A 2 0.615065 0.379356 0.031985 11.00000 -1.20000 AFIX 0 C15A 1 0.527560 0.268759 0.070350 11.00000 0.02440 0.04497 = 0.04336 -0.00210 0.00402 0.01682 AFIX 43 H15A 2 0.534648 0.225086 0.029740 11.00000 -1.20000 AFIX 0 C16A 1 0.469385 0.236937 0.126414 11.00000 0.03049 0.02285 = 0.06073 0.00222 -0.00482 0.00420 AFIX 43 H16A 2 0.439412 0.172512 0.123650 11.00000 -1.20000 AFIX 0 C17A 1 0.453149 0.296745 0.187326 11.00000 0.01897 0.03294 = 0.04724 0.01065 -0.00022 0.00552 AFIX 43 H17A 2 0.413047 0.275647 0.225923 11.00000 -1.20000 AFIX 0 C18A 1 0.500345 0.388559 0.186282 11.00000 0.01444 0.02168 = 0.02784 0.00034 -0.00187 0.00567 C19A 1 0.672554 0.578054 0.112914 11.00000 0.01759 0.03708 = 0.02967 0.01058 0.01008 0.01067 AFIX 23 H19C 2 0.726196 0.553139 0.111783 11.00000 -1.20000 H19D 2 0.698755 0.638002 0.149908 11.00000 -1.20000 AFIX 0 C20A 1 0.636505 0.592833 0.027212 11.00000 0.02452 0.02854 = 0.03446 0.00862 0.00862 0.01137 AFIX 23 H20E 2 0.581017 0.615268 0.027481 11.00000 -1.20000 H20F 2 0.613509 0.533634 -0.010744 11.00000 -1.20000 AFIX 0 C21A 1 0.715428 0.661843 -0.004089 11.00000 0.02738 0.03101 = 0.03035 0.01198 0.00901 0.01038 AFIX 23 H21E 2 0.772705 0.641473 0.001160 11.00000 -1.20000 H21F 2 0.692503 0.661351 -0.063919 11.00000 -1.20000 AFIX 0 C22A 1 0.746852 0.759239 0.039715 11.00000 0.03422 0.02771 = 0.04393 0.01208 -0.00230 0.00698 AFIX 137 H22G 2 0.796743 0.798928 0.014342 11.00000 -1.50000 H22H 2 0.773264 0.761513 0.098535 11.00000 -1.50000 H22I 2 0.690998 0.780651 0.034769 11.00000 -1.50000 AFIX 0 C23A 1 0.127244 0.350886 0.380891 11.00000 0.01540 0.01987 = 0.02492 0.00718 0.00556 0.00991 AFIX 23 H23C 2 0.108517 0.283020 0.371734 11.00000 -1.20000 H23D 2 0.167818 0.373797 0.437269 11.00000 -1.20000 AFIX 0 C25A 1 -0.048880 0.318286 0.367173 11.00000 0.01400 0.01627 = 0.01691 0.00539 0.00587 0.00505 AFIX 43 H25A 2 -0.066247 0.253255 0.356861 11.00000 -1.20000 AFIX 0 C27A 1 -0.058734 0.456119 0.388651 11.00000 0.01215 0.01933 = 0.01780 0.00589 0.00566 0.00473 C28A 1 -0.088645 0.531732 0.402126 11.00000 0.01609 0.02141 = 0.02140 0.00599 0.00528 0.00815 AFIX 43 H28A 2 -0.154634 0.525189 0.401397 11.00000 -1.20000 AFIX 0 C29A 1 -0.017537 0.616276 0.416527 11.00000 0.02235 0.01699 = 0.02233 0.00598 0.00670 0.00939 AFIX 43 H29A 2 -0.034795 0.670001 0.424789 11.00000 -1.20000 AFIX 0 C30A 1 0.079733 0.625405 0.419357 11.00000 0.02115 0.01931 = 0.02279 0.00404 0.00442 0.00410 AFIX 43 H30A 2 0.126848 0.685264 0.430519 11.00000 -1.20000 AFIX 0 C31A 1 0.109527 0.550583 0.406513 11.00000 0.01653 0.02375 = 0.02196 0.00784 0.00800 0.00767 AFIX 43 H31A 2 0.175709 0.557108 0.408408 11.00000 -1.20000 AFIX 0 C32A 1 0.037584 0.465336 0.390687 11.00000 0.01556 0.01507 = 0.01690 0.00496 0.00583 0.00530 C33A 1 -0.215502 0.321490 0.368039 11.00000 0.01144 0.01905 = 0.03134 0.00325 0.00776 0.00228 AFIX 23 H33C 2 -0.234964 0.352020 0.414305 11.00000 -1.20000 H33D 2 -0.231500 0.255598 0.373705 11.00000 -1.20000 AFIX 0 C34A 1 -0.272383 0.330225 0.286590 11.00000 0.01575 0.02403 = 0.03309 0.00633 -0.00297 0.00367 AFIX 23 H34C 2 -0.255797 0.396191 0.281063 11.00000 -1.20000 H34D 2 -0.342366 0.305997 0.287562 11.00000 -1.20000 AFIX 0 C35A 1 -0.253812 0.279940 0.211475 11.00000 0.03024 0.04307 = 0.02721 0.00423 -0.00313 0.00897 AFIX 23 H35C 2 -0.286158 0.296046 0.160701 11.00000 -1.20000 H35D 2 -0.183301 0.301455 0.212392 11.00000 -1.20000 AFIX 0 C36A 1 -0.289174 0.176469 0.206797 11.00000 0.05595 0.04668 = 0.04291 -0.00941 -0.00038 0.01909 AFIX 137 H36D 2 -0.358385 0.154696 0.208323 11.00000 -1.50000 H36E 2 -0.253034 0.159421 0.254109 11.00000 -1.50000 H36F 2 -0.279013 0.148251 0.154927 11.00000 -1.50000 AFIX 0 F2U 4 0.045555 0.185711 0.132935 11.00000 0.08998 0.07966 = 0.06665 0.03921 0.04668 0.06441 F3U 4 -0.115675 0.114024 0.102441 11.00000 0.11962 0.03768 = 0.02613 -0.00298 0.01181 -0.01020 F4U 4 -0.041520 0.175710 0.233904 11.00000 0.05096 0.07775 = 0.02352 -0.00366 0.00281 0.03739 F5U 4 -0.054685 0.267225 0.136632 11.00000 0.04092 0.03301 = 0.08131 0.00862 -0.00496 0.01824 B1U 3 -0.041286 0.186332 0.151843 11.00000 0.04812 0.03150 = 0.02542 0.00125 0.00660 0.01894 F2T 4 0.551987 0.716223 0.144417 11.00000 0.03845 0.03924 = 0.05776 0.00841 0.01626 0.01906 F3T 4 0.393485 0.629448 0.112953 11.00000 0.05951 0.03415 = 0.02666 0.00266 0.00243 -0.00716 F4T 4 0.464277 0.694890 0.244469 11.00000 0.05027 0.07189 = 0.02641 -0.00621 0.00333 0.03297 F5T 4 0.438020 0.783120 0.147136 11.00000 0.03138 0.03656 = 0.09622 0.01354 -0.00045 0.01739 B1T 3 0.461647 0.706060 0.162374 11.00000 0.02889 0.02751 = 0.03536 0.00170 -0.00076 0.01190 F2S 4 0.273017 0.429686 0.679315 11.00000 0.03131 0.02227 = 0.03887 -0.00540 -0.00574 0.01568 F3S 4 0.355058 0.342309 0.630587 11.00000 0.02775 0.04693 = 0.03431 -0.00283 0.00308 0.02123 F4S 4 0.206344 0.328140 0.559572 11.00000 0.02922 0.03069 = 0.02576 0.00245 -0.00094 0.01361 F5S 4 0.223709 0.277202 0.682952 11.00000 0.06544 0.02967 = 0.03245 0.01253 0.02212 0.01172 B1S 3 0.263661 0.344821 0.637819 11.00000 0.02142 0.02036 = 0.02595 0.00719 0.00703 0.01013 F2R 4 0.694152 0.471603 0.489131 11.00000 0.03370 0.02071 = 0.03992 0.00976 0.00719 0.00625 F3R 4 0.560838 0.353718 0.418847 11.00000 0.05701 0.03373 = 0.03583 -0.00264 -0.00477 0.00360 F4R 4 0.560013 0.427671 0.539464 11.00000 0.02902 0.09123 = 0.09876 -0.06012 0.03321 -0.00976 F5R 4 0.650094 0.334913 0.532490 11.00000 0.03819 0.04562 = 0.10330 0.04948 -0.01996 -0.00423 B1R 3 0.615292 0.396411 0.495225 11.00000 0.01459 0.02659 = 0.01992 0.00390 0.00394 0.00845 F2Q 4 0.294698 0.219227 0.307180 11.00000 0.06652 0.02918 = 0.03221 0.01172 0.01860 0.00256 F3Q 4 0.227023 0.065989 0.303208 11.00000 0.02612 0.02461 = 0.03259 -0.00116 -0.00018 0.01452 F4Q 4 0.147113 0.160621 0.338613 11.00000 0.03394 0.04567 = 0.04026 -0.00708 -0.00353 0.02966 F5Q 4 0.281106 0.161932 0.426696 11.00000 0.02492 0.02790 = 0.02276 0.00588 0.00385 0.01181 B1Q 3 0.237893 0.151697 0.344451 11.00000 0.02275 0.01879 = 0.02466 0.00581 0.00237 0.01070 F2P 4 0.941135 0.072193 0.456982 11.00000 0.02197 0.04341 = 0.06148 -0.02146 0.01846 0.00145 F3P 4 0.807462 0.036584 0.512128 11.00000 0.02561 0.01692 = 0.03410 0.00630 0.01098 0.00638 F4P 4 0.850226 0.165926 0.454578 11.00000 0.02777 0.04170 = 0.06090 0.03440 -0.00090 0.00473 F5P 4 0.941569 0.157652 0.574083 11.00000 0.04433 0.02530 = 0.02821 -0.00397 0.00017 0.00478 B1P 3 0.884957 0.108617 0.499328 11.00000 0.01630 0.02163 = 0.02173 0.00621 0.00546 0.00635 N1M 5 0.159858 0.522814 -0.030893 11.00000 0.07095 0.04757 = 0.14138 -0.00433 0.02333 0.01132 C2M 1 0.182403 0.597577 -0.015162 11.00000 0.04357 0.04697 = 0.06083 -0.00494 0.01279 0.01686 C3M 1 0.214837 0.697331 0.005467 11.00000 0.05052 0.04917 = 0.03558 0.00708 0.00926 0.02707 AFIX 137 H3MA 2 0.200909 0.724032 -0.044673 11.00000 -1.50000 H3MB 2 0.284747 0.720658 0.027878 11.00000 -1.50000 H3MC 2 0.180679 0.714426 0.047078 11.00000 -1.50000 REM ##### AFIX 0 HKLF 4 REM HV164_0m_a.res in P-1 REM R1 = 0.0668 for 7491 Fo > 4sig(Fo) and 0.1383 for all 13648 data REM 959 parameters refined using 1 restraints END WGHT 0.0563 3.2360 REM Highest difference peak 0.724, deepest hole -0.400, 1-sigma level 0.064 Q1 1 0.0672 0.5249 0.8216 11.00000 0.05 0.72 Q2 1 0.5548 0.3701 0.5692 11.00000 0.05 0.57 Q3 1 -0.3029 0.0457 0.9360 11.00000 0.05 0.55 Q4 1 0.6380 0.5196 0.0689 11.00000 0.05 0.43 Q5 1 -0.2904 -0.0182 0.8465 11.00000 0.05 0.41 Q6 1 0.6743 0.6350 0.0863 11.00000 0.05 0.40 Q7 1 0.4457 0.2066 0.1758 11.00000 0.05 0.35 Q8 1 0.9434 0.1200 0.4278 11.00000 0.05 0.33 Q9 1 -0.2158 0.0313 0.9017 11.00000 0.05 0.30 Q10 1 0.0755 0.5486 -0.1069 11.00000 0.05 0.29 Q11 1 0.5022 0.3231 0.4274 11.00000 0.05 0.29 Q12 1 0.5442 0.4298 0.5150 11.00000 0.05 0.29 Q13 1 0.4390 0.7888 0.2041 11.00000 0.05 0.28 Q14 1 0.1824 0.5449 -0.0105 11.00000 0.05 0.27 Q15 1 0.6545 0.4733 0.5312 11.00000 0.05 0.26 Q16 1 0.5407 -0.0878 0.5532 11.00000 0.05 0.26 Q17 1 0.6460 0.3797 0.5735 11.00000 0.05 0.25 Q18 1 0.4548 0.2896 0.2425 11.00000 0.05 0.25 Q19 1 0.5143 0.2215 0.1108 11.00000 0.05 0.25 Q20 1 0.3636 0.1934 0.4498 11.00000 0.05 0.25 ; _shelx_res_checksum 60378 _shelx_hkl_file ; -2 0 0 183.57 7.16 -3 0 0 59.95 5.88 3 0 0 46.55 3.85 3 0 0 58.22 5.58 -4 0 0 1431.34 39.00 4 0 0 1367.65 37.73 4 0 0 1430.67 39.09 -5 0 0 152.10 9.08 5 0 0 144.03 6.68 5 0 0 155.42 9.11 -6 0 0 187.69 10.64 6 0 0 171.82 8.07 6 0 0 190.56 10.21 6 0 0 172.67 7.97 -7 0 0 22.97 6.22 7 0 0 31.32 5.96 7 0 0 34.15 4.19 7 0 0 25.89 6.15 -8 0 0 709.64 23.82 8 0 0 650.28 20.53 8 0 0 723.06 20.77 8 0 0 729.58 24.01 -9 0 0 7.02 6.75 9 0 0 5.63 6.23 9 0 0 5.64 3.90 9 0 0 0.95 4.29 -10 0 0 558.75 21.63 10 0 0 577.69 21.95 -11 0 0 -0.67 7.46 11 0 0 9.95 7.44 12 0 0 742.69 27.80 13 0 0 8.11 8.59 14 0 0 36.19 9.97 15 0 0 5.27 9.62 16 0 0 2.42 10.06 17 0 0 0.02 10.86 17 -1 0 95.54 13.94 16 -1 0 0.36 9.54 15 -1 0 69.31 11.35 14 -1 0 12.35 8.84 13 -1 0 61.51 10.19 12 -1 0 8.12 7.44 12 -1 0 1.63 5.56 11 -1 0 27.71 5.97 11 -1 0 23.96 7.63 -11 1 0 26.13 8.03 10 -1 0 37.38 7.55 10 -1 0 38.57 6.24 10 -1 0 49.36 9.02 -10 1 0 33.62 7.88 9 -1 0 6.50 6.19 9 -1 0 14.30 5.52 9 -1 0 11.11 5.60 -9 1 0 8.38 6.62 8 -1 0 39.21 5.77 8 -1 0 30.70 6.50 8 -1 0 35.85 5.99 -8 1 0 38.53 6.82 7 -1 0 153.93 10.32 7 -1 0 150.03 9.46 -7 1 0 159.20 10.45 6 -1 0 92.71 7.34 6 -1 0 93.16 8.63 -6 1 0 81.16 8.43 -6 1 0 96.05 6.71 5 -1 0 89.26 7.42 5 -1 0 73.40 6.46 -5 1 0 77.54 6.34 -5 1 0 88.76 7.53 4 -1 0 605.99 18.10 4 -1 0 612.42 18.36 -4 1 0 601.66 18.31 -4 1 0 602.25 17.98 3 -1 0 1796.95 47.40 3 -1 0 1758.84 47.11 -3 1 0 1716.16 47.22 -3 1 0 1769.85 47.12 -2 1 0 0.32 1.67 -2 -1 0 42.57 4.77 2 1 0 37.88 4.53 -3 -1 0 1159.55 32.15 3 1 0 1135.78 32.04 -4 -1 0 12.74 4.53 4 1 0 27.30 4.76 -5 -1 0 1768.20 49.13 5 1 0 1760.78 49.07 -6 -1 0 -3.09 5.41 6 1 0 -2.97 5.32 -7 -1 0 31.47 6.59 7 1 0 34.93 6.54 -8 -1 0 43.67 7.37 8 1 0 33.67 7.19 -9 -1 0 165.31 12.36 9 1 0 155.88 12.50 -10 -1 0 3.92 7.13 10 1 0 10.30 7.33 11 1 0 119.73 12.94 12 1 0 55.08 10.03 13 1 0 86.41 11.46 14 1 0 8.80 9.50 15 1 0 4.55 9.71 16 1 0 18.99 11.42 17 -2 0 13.37 10.03 16 -2 0 -3.36 8.82 15 -2 0 0.17 8.72 14 -2 0 9.36 7.38 14 -2 0 23.34 8.98 13 -2 0 0.72 6.93 13 -2 0 27.39 9.14 13 -2 0 1.60 7.70 12 -2 0 21.14 8.25 12 -2 0 9.12 7.38 12 -2 0 9.13 6.88 11 -2 0 0.81 6.37 11 -2 0 10.18 7.05 11 -2 0 -1.46 6.35 10 -2 0 264.18 14.25 10 -2 0 252.77 13.75 10 -2 0 253.70 13.93 -10 2 0 251.00 14.19 9 -2 0 43.71 7.13 9 -2 0 51.43 7.49 -9 2 0 45.90 7.27 8 -2 0 224.31 11.88 8 -2 0 204.26 12.38 -8 2 0 207.74 10.82 -8 2 0 216.73 12.04 7 -2 0 35.17 6.12 7 -2 0 36.37 5.97 -7 2 0 30.45 5.94 -7 2 0 39.36 5.75 6 -2 0 86.07 8.07 6 -2 0 84.54 7.62 -6 2 0 80.99 7.67 5 -2 0 3.36 4.24 5 -2 0 -6.43 3.64 -5 2 0 -2.12 4.01 4 -2 0 6537.49 171.84 4 -2 0 6507.54 170.93 4 -2 0 6553.03 170.67 -4 2 0 6511.30 171.81 3 -2 0 28.12 3.73 3 -2 0 25.78 4.65 -3 2 0 28.75 4.47 -3 2 0 28.29 3.74 -2 2 0 24.32 2.34 -2 2 0 32.28 4.34 -1 2 0 -0.77 1.11 0 2 0 -0.06 1.46 -1 -2 0 3.07 2.48 -1 -2 0 -2.92 2.64 1 2 0 -0.76 2.59 1 2 0 -0.12 2.53 -2 -2 0 2.54 3.62 -2 -2 0 4.93 2.44 2 2 0 3.86 2.39 2 2 0 5.94 3.73 -3 -2 0 16.46 4.36 3 2 0 18.29 4.46 -4 -2 0 5.60 4.63 4 2 0 3.15 4.51 -5 -2 0 -1.59 5.07 5 2 0 1.14 5.01 -6 -2 0 661.61 22.40 6 2 0 660.67 22.26 -7 -2 0 18.30 6.63 7 2 0 17.63 6.46 -8 -2 0 49.58 7.87 8 2 0 47.07 7.65 -9 -2 0 7.85 6.97 9 2 0 1.28 6.64 -10 -2 0 254.98 15.92 10 2 0 268.29 16.06 11 2 0 -0.62 7.94 12 2 0 135.42 15.45 13 2 0 29.02 9.99 14 2 0 45.09 11.34 15 2 0 7.67 10.67 16 2 0 31.01 12.40 17 -3 0 10.50 9.56 15 -3 0 365.95 18.74 15 -3 0 381.04 20.11 14 -3 0 3.61 7.86 14 -3 0 -0.39 8.14 13 -3 0 102.94 13.25 13 -3 0 116.08 13.10 12 -3 0 31.82 9.22 12 -3 0 12.54 7.14 12 -3 0 20.13 8.04 12 -3 0 8.94 5.89 11 -3 0 169.35 13.41 11 -3 0 169.73 14.12 11 -3 0 149.63 10.84 11 -3 0 162.52 12.21 10 -3 0 18.54 6.49 10 -3 0 18.33 7.73 10 -3 0 7.88 5.11 9 -3 0 1430.44 40.95 9 -3 0 1429.14 41.90 9 -3 0 1433.57 42.75 -9 3 0 1431.32 42.01 8 -3 0 -2.31 4.91 8 -3 0 -0.81 6.22 8 -3 0 0.62 4.15 -8 3 0 -4.91 5.27 7 -3 0 104.78 9.55 7 -3 0 94.02 7.33 7 -3 0 101.73 8.48 -7 3 0 97.42 8.78 6 -3 0 95.62 8.95 6 -3 0 97.43 7.55 6 -3 0 102.68 6.50 -6 3 0 101.31 8.71 5 -3 0 416.12 15.55 5 -3 0 414.15 13.14 5 -3 0 423.52 13.75 -5 3 0 409.81 15.18 4 -3 0 30.47 4.26 4 -3 0 37.79 5.79 -4 3 0 40.20 5.86 -4 3 0 32.38 4.57 3 -3 0 1886.32 52.69 3 -3 0 1945.88 50.59 -3 3 0 1879.01 52.60 -3 3 0 1901.12 50.54 2 -3 0 457.36 15.72 2 -3 0 463.42 13.55 -2 3 0 470.43 15.66 -2 3 0 467.04 13.48 1 -3 0 644.33 19.98 1 -3 0 674.85 18.41 -1 3 0 645.47 18.30 -1 3 0 652.04 19.96 0 -3 0 286.01 10.84 0 -3 0 304.62 9.98 0 3 0 300.33 11.08 0 3 0 302.77 10.06 -1 -3 0 2319.35 63.54 -1 -3 0 2396.55 63.51 1 3 0 2353.78 63.48 1 3 0 2428.73 63.63 -2 -3 0 11.46 4.08 -2 -3 0 9.46 3.37 2 3 0 10.89 3.36 2 3 0 10.97 4.27 -3 -3 0 637.54 18.88 -3 -3 0 685.37 20.84 3 3 0 682.34 20.92 -4 -3 0 11.97 5.12 4 3 0 13.04 5.29 -5 -3 0 1088.66 32.70 5 3 0 1083.55 32.74 -6 -3 0 51.54 7.15 6 3 0 54.97 7.39 -7 -3 0 1752.88 50.72 7 3 0 1734.39 50.72 -8 -3 0 23.93 7.29 8 3 0 18.78 7.24 -9 -3 0 4.66 7.10 9 3 0 -0.53 7.09 10 3 0 10.51 8.04 11 3 0 23.12 9.03 12 3 0 -3.58 8.72 13 3 0 72.45 11.68 14 3 0 17.86 10.67 15 3 0 17.98 11.74 17 -4 0 -8.81 10.24 17 -4 0 -0.28 8.86 15 -4 0 9.89 8.17 14 -4 0 4.72 9.03 14 -4 0 11.19 7.49 13 -4 0 -5.57 7.17 13 -4 0 3.12 8.58 13 -4 0 40.53 11.29 13 -4 0 13.21 7.34 12 -4 0 16.25 9.72 12 -4 0 18.96 6.93 12 -4 0 5.45 5.74 12 -4 0 2.36 8.44 11 -4 0 12.87 8.80 11 -4 0 -4.05 4.98 11 -4 0 2.21 5.97 10 -4 0 230.30 12.92 10 -4 0 239.77 16.14 10 -4 0 232.28 11.41 -10 4 0 244.49 13.44 9 -4 0 0.17 4.39 9 -4 0 -7.65 6.53 9 -4 0 -2.64 5.02 -9 4 0 0.70 5.65 8 -4 0 324.82 12.19 8 -4 0 311.62 13.11 8 -4 0 300.28 15.54 -8 4 0 300.34 14.48 7 -4 0 2.01 4.45 7 -4 0 -1.15 3.70 7 -4 0 4.04 5.99 -7 4 0 -1.84 5.16 6 -4 0 218.45 11.93 6 -4 0 222.80 8.78 -6 4 0 208.54 12.20 5 -4 0 -0.81 2.95 5 -4 0 -1.29 5.20 -5 4 0 0.04 3.09 -5 4 0 -0.43 5.04 4 -4 0 497.39 18.29 4 -4 0 518.99 15.22 -4 4 0 496.65 15.13 -4 4 0 522.20 18.33 3 -4 0 27.81 3.65 3 -4 0 26.71 5.99 -3 4 0 28.82 3.43 -3 4 0 36.96 6.21 2 -4 0 608.17 20.41 2 -4 0 635.12 17.86 -2 4 0 600.78 20.26 -2 4 0 616.95 17.88 1 -4 0 26.61 5.59 1 -4 0 31.54 3.87 -1 4 0 22.64 5.24 0 -4 0 1629.27 45.59 0 -4 0 1651.40 44.51 0 4 0 1625.90 45.51 0 4 0 1631.22 44.41 -1 -4 0 1.07 3.89 -1 -4 0 -2.62 4.05 1 4 0 0.02 4.05 1 4 0 -0.52 3.92 -2 -4 0 -1.33 3.88 -2 -4 0 -1.40 4.22 2 4 0 -0.22 4.57 2 4 0 1.11 3.72 -3 -4 0 104.27 6.94 -3 -4 0 104.91 8.54 3 4 0 104.82 8.74 -4 -4 0 1798.38 50.55 -4 -4 0 1865.01 52.86 -4 -4 0 1944.29 50.72 4 4 0 1931.50 53.19 -5 -4 0 58.58 7.14 5 4 0 55.60 7.31 -6 -4 0 136.65 11.53 6 4 0 133.40 11.37 -7 -4 0 112.60 11.45 7 4 0 123.50 11.74 -8 -4 0 156.66 12.77 8 4 0 172.57 13.12 9 4 0 2.75 7.64 10 4 0 114.05 14.43 11 4 0 21.69 9.70 12 4 0 2.07 9.15 13 4 0 30.26 10.80 14 4 0 182.84 18.57 15 4 0 -14.02 10.77 18 -5 0 8.26 8.98 17 -5 0 214.36 19.98 17 -5 0 264.92 17.68 15 -5 0 17.33 7.85 14 -5 0 37.28 12.54 14 -5 0 6.17 7.53 14 -5 0 4.60 9.76 13 -5 0 76.95 11.42 13 -5 0 56.49 11.38 13 -5 0 57.95 7.83 12 -5 0 -3.30 5.21 12 -5 0 -2.46 8.63 12 -5 0 2.11 6.33 12 -5 0 6.99 10.40 11 -5 0 56.03 7.55 11 -5 0 86.67 15.08 11 -5 0 56.23 6.87 10 -5 0 70.43 7.96 10 -5 0 75.69 13.13 10 -5 0 65.16 9.12 -10 5 0 67.12 10.15 9 -5 0 560.27 23.10 9 -5 0 567.37 18.53 9 -5 0 564.92 19.50 -9 5 0 561.89 21.28 8 -5 0 12.57 4.13 8 -5 0 12.24 6.81 8 -5 0 16.51 5.18 -8 5 0 16.58 6.83 7 -5 0 47.87 8.21 7 -5 0 45.95 6.00 -7 5 0 56.15 8.20 6 -5 0 -1.83 6.39 6 -5 0 -3.61 3.55 -6 5 0 -5.59 3.54 -6 5 0 2.94 6.28 5 -5 0 366.61 12.32 5 -5 0 376.59 16.27 -5 5 0 380.55 16.02 -5 5 0 364.64 12.23 4 -5 0 253.52 13.19 4 -5 0 251.27 9.34 -4 5 0 246.34 12.92 -4 5 0 252.51 9.24 3 -5 0 760.98 21.53 3 -5 0 752.27 24.41 -3 5 0 730.14 21.39 -3 5 0 736.90 24.60 2 -5 0 83.29 6.10 2 -5 0 88.72 9.26 -2 5 0 74.59 8.86 -2 5 0 88.61 6.33 1 -5 0 776.67 22.56 1 -5 0 771.06 25.05 -1 5 0 771.93 22.46 -1 5 0 766.94 24.65 0 -5 0 8.61 5.39 0 -5 0 8.49 4.00 0 5 0 9.06 4.86 0 5 0 12.24 4.32 -1 -5 0 179.98 9.46 -1 -5 0 186.04 9.86 1 5 0 176.70 9.54 1 5 0 186.14 9.68 -2 -5 0 70.23 7.99 -2 -5 0 62.35 7.78 2 5 0 66.07 7.23 2 5 0 78.49 8.78 -3 -5 0 199.94 11.42 -3 -5 0 193.88 10.60 3 5 0 202.79 11.79 -4 -5 0 -0.58 4.53 -4 -5 0 -6.22 4.33 -4 -5 0 -1.41 5.33 4 5 0 6.65 5.88 -5 -5 0 108.31 10.44 -5 -5 0 119.19 7.17 5 5 0 124.18 11.02 -6 -5 0 -3.90 6.13 6 5 0 1.49 6.49 -7 -5 0 133.40 12.06 7 5 0 159.04 12.75 -8 -5 0 -5.73 10.47 8 5 0 -0.08 7.45 9 5 0 41.96 9.42 10 5 0 47.46 10.33 11 5 0 7.17 9.50 12 5 0 5.95 9.94 13 5 0 37.37 11.61 14 5 0 7.42 12.02 18 -6 0 29.94 9.22 18 -6 0 5.10 12.30 16 -6 0 237.82 20.27 16 -6 0 244.01 16.04 15 -6 0 11.31 7.48 15 -6 0 6.70 10.33 14 -6 0 41.95 8.38 14 -6 0 34.40 11.19 13 -6 0 4.75 11.80 13 -6 0 -3.33 6.39 13 -6 0 9.41 9.99 13 -6 0 -0.17 5.23 12 -6 0 463.54 19.17 12 -6 0 545.62 25.56 12 -6 0 471.03 18.06 11 -6 0 2.30 5.50 11 -6 0 3.97 9.09 11 -6 0 2.25 4.57 -11 6 0 4.61 6.80 10 -6 0 -8.57 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18.07 -4 0 19 3.54 7.99 3 0 -19 36.64 18.74 -3 0 19 9.71 8.11 2 0 -19 68.04 19.58 -2 0 19 33.06 8.64 1 0 -19 36.67 18.26 -1 0 19 14.72 8.00 0 0 -19 72.99 19.41 -1 0 -19 45.32 19.75 -2 0 -19 94.59 20.99 2 0 19 57.36 8.96 9 -1 -19 33.42 14.16 9 -1 -19 55.91 19.35 8 -1 -19 46.14 19.11 7 -1 -19 31.47 18.70 -7 1 19 15.57 9.17 6 -1 -19 20.90 17.81 -6 1 19 6.13 8.57 5 -1 -19 13.54 17.42 -5 1 19 -5.05 7.95 4 -1 -19 28.72 17.83 -4 1 19 12.65 8.38 3 -1 -19 21.71 17.43 -3 1 19 -0.68 7.98 2 -1 -19 62.72 19.07 1 -1 -19 37.35 18.79 -1 1 19 10.51 7.94 0 -1 -19 42.92 18.41 0 1 19 -0.76 7.73 -1 -1 -19 63.96 19.66 -2 -1 -19 57.61 20.70 9 -2 -19 46.44 19.65 8 -2 -19 31.13 19.01 -8 2 19 8.96 9.06 7 -2 -19 39.59 19.01 -7 2 19 17.68 9.45 6 -2 -19 37.19 19.25 -6 2 19 4.71 8.56 5 -2 -19 56.00 19.82 -5 2 19 20.69 9.10 4 -2 -19 32.88 18.82 -4 2 19 4.47 8.48 3 -2 -19 27.16 18.62 -3 2 19 0.38 8.27 2 -2 -19 30.14 18.07 -2 2 19 25.97 9.05 1 -2 -19 40.12 18.77 -1 2 19 17.14 8.76 0 -2 -19 50.87 19.11 0 2 19 4.00 7.93 -1 -2 -19 54.86 19.19 1 2 19 4.30 8.20 9 -3 -19 29.51 19.34 -9 3 19 11.76 9.71 8 -3 -19 56.12 19.35 -8 3 19 4.70 9.50 7 -3 -19 58.42 19.98 -7 3 19 6.18 9.12 6 -3 -19 38.70 19.19 5 -3 -19 55.12 18.93 -5 3 19 38.35 9.67 4 -3 -19 23.95 18.50 -4 3 19 -1.77 8.41 3 -3 -19 21.67 18.76 -3 3 19 9.50 8.63 2 -3 -19 26.84 18.33 -2 3 19 15.02 8.77 1 -3 -19 55.44 20.18 0 -3 -19 61.38 19.46 0 3 19 24.64 9.01 8 -4 -19 86.04 22.28 -8 4 19 39.74 10.52 7 -4 -19 75.83 21.46 -7 4 19 51.85 11.02 6 -4 -19 25.07 18.86 -6 4 19 3.58 8.52 5 -4 -19 48.27 19.66 -5 4 19 -0.22 8.74 4 -4 -19 9.75 17.76 -4 4 19 -8.53 8.27 3 -4 -19 30.44 19.39 -3 4 19 5.36 8.71 2 -4 -19 34.48 19.16 -2 4 19 17.20 8.90 1 -4 -19 37.52 19.54 -1 4 19 -1.41 8.23 7 -5 -19 14.73 20.89 -7 5 19 10.63 9.21 6 -5 -19 26.10 20.68 -6 5 19 3.14 8.92 5 -5 -19 96.39 21.63 -5 5 19 61.83 10.88 4 -5 -19 51.64 19.94 3 -5 -19 31.17 18.98 -3 5 19 8.39 8.75 4 5 -20 38.59 19.18 3 5 -20 8.35 9.70 3 5 -20 45.03 19.40 2 5 -20 55.73 19.20 2 5 -20 21.18 9.71 1 5 -20 -9.02 8.94 1 5 -20 35.72 18.78 0 5 -20 69.23 10.19 5 4 -20 -9.83 10.52 5 4 -20 56.44 19.44 4 4 -20 32.78 17.91 4 4 -20 -8.74 9.96 3 4 -20 17.55 10.44 3 4 -20 36.89 18.84 2 4 -20 61.78 19.59 2 4 -20 13.00 10.28 1 4 -20 30.61 18.74 1 4 -20 1.37 9.43 0 4 -20 126.16 15.75 0 4 -20 147.12 14.33 5 3 -20 58.14 19.09 4 3 -20 55.56 18.57 4 3 -20 -1.21 10.57 3 3 -20 -1.89 10.24 3 3 -20 26.05 17.77 2 3 -20 33.53 18.03 1 3 -20 44.04 18.54 0 3 -20 63.24 19.57 -1 3 -20 59.58 19.68 6 2 -20 353.20 33.44 5 2 -20 -7.00 10.99 5 2 -20 43.08 18.71 4 2 -20 33.25 18.13 3 2 -20 50.49 18.88 2 2 -20 66.83 19.18 1 2 -20 43.48 18.15 -1 -2 20 7.49 7.44 0 2 -20 257.84 28.97 0 -2 20 201.73 13.77 6 1 -20 62.63 18.59 6 1 -20 6.68 11.72 5 1 -20 41.95 17.75 4 1 -20 31.74 18.21 3 1 -20 47.31 18.48 -3 -1 20 5.22 7.98 2 1 -20 53.53 19.47 1 1 -20 79.93 19.78 -1 -1 20 34.60 8.81 0 1 -20 137.28 26.49 6 0 -20 69.67 20.14 5 0 -20 61.29 19.10 -5 0 20 4.09 8.34 4 0 -20 39.48 18.11 -4 0 20 1.67 8.40 3 0 -20 42.38 17.65 -3 0 20 -0.07 8.01 2 0 -20 65.67 18.47 1 0 -20 144.96 26.88 6 -1 -20 55.50 18.67 -6 1 20 12.94 9.25 5 -1 -20 73.95 19.57 -5 1 20 15.72 9.03 4 -1 -20 28.30 17.95 -4 1 20 -5.33 8.22 3 -1 -20 52.35 18.92 -3 1 20 -1.95 8.15 2 -1 -20 45.96 18.29 -2 1 20 -4.51 8.01 5 -2 -20 65.45 19.70 -5 2 20 36.33 9.98 4 -2 -20 40.81 18.45 -4 2 20 3.48 8.45 3 -2 -20 46.92 18.62 -3 2 20 5.55 8.49 0 0 0 0.00 0.00 _exptl_absorpt_process_details ) SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ) _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.7453 _exptl_absorpt_correction_T_min 0.6097 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 0.71152 14.914 15.583 16.601 95.218 99.249 108.417 ) _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 12790 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_flags_posn _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group N N7 0.16752(19) 0.11166(18) 0.58118(18) 0.0154(6) Uani d . . . 1.0 . . N N8 0.1370(2) 0.13009(19) 0.52357(19) 0.0205(7) Uani d . . . 1.0 . . N N10 0.00095(19) 0.05724(19) 0.76161(17) 0.0183(6) Uani d . . . 1.0 . . N N12 -0.0621(2) 0.03559(19) 0.87148(17) 0.0202(7) Uani d . . . 1.0 . . N N24 0.45591(19) 0.11937(17) 0.61543(17) 0.0141(6) Uani d . . . 1.0 . . N N26 0.60728(18) 0.13705(17) 0.61518(16) 0.0143(6) Uani d . . . 1.0 . . C C1 0.2088(2) 0.0895(2) 0.6567(2) 0.0148(7) Uani d . . . 1.0 . . C C2 0.1479(2) 0.0578(2) 0.7111(2) 0.0182(8) Uani d . . . 1.0 . . C C3 0.1920(2) 0.0424(2) 0.7856(2) 0.0223(8) Uani d . . . 1.0 . . H H3 0.154193 0.020381 0.825438 0.027 Uiso calc U . R 1.0 . . C C4 0.2905(3) 0.0584(2) 0.8032(2) 0.0216(8) Uani d . . . 1.0 . . H H4 0.319295 0.047618 0.85523 0.026 Uiso calc U . R 1.0 . . C C5 0.3483(2) 0.0899(2) 0.7468(2) 0.0191(8) Uani d . . . 1.0 . . H H5 0.415886 0.100382 0.760376 0.023 Uiso calc U . R 1.0 . . C C6 0.3083(2) 0.1060(2) 0.6712(2) 0.0141(7) Uani d . . . 1.0 . . C C9 0.0392(2) 0.0373(3) 0.6887(2) 0.0228(8) Uani d . . . 1.0 . . H H9A 0.024851 0.075064 0.64639 0.027 Uiso calc U . R 1.0 . . H H9AB 0.006941 -0.028224 0.664433 0.027 Uiso calc U . R 1.0 . . C C11 -0.0442(2) -0.0054(2) 0.8048(2) 0.0213(8) Uani d . . . 1.0 . . H H11 -0.061084 -0.069994 0.790048 0.026 Uiso calc U . R 1.0 . . C C13 -0.0269(2) 0.1300(2) 0.8719(2) 0.0206(8) Uani d . . . 1.0 . . C C14 -0.0245(3) 0.2035(3) 0.9280(2) 0.0292(9) Uani d . . . 1.0 . . H H14 -0.050077 0.194592 0.977067 0.035 Uiso calc U . R 1.0 . . C C15 0.0166(3) 0.2894(3) 0.9089(3) 0.0363(10) Uani d . . . 1.0 . . H H15 0.019905 0.341453 0.945859 0.044 Uiso calc U . R 1.0 . . C C16 0.0538(3) 0.3029(3) 0.8368(3) 0.0342(10) Uani d . . . 1.0 . . H H16 0.08043 0.363869 0.825682 0.041 Uiso calc U . R 1.0 . . C C17 0.0530(3) 0.2304(3) 0.7813(2) 0.0281(9) Uani d . . . 1.0 . . H H17 0.078533 0.239375 0.732232 0.034 Uiso calc U . R 1.0 . . C C18 0.0127(2) 0.1440(2) 0.8016(2) 0.0190(8) Uani d . . . 1.0 . . C C19 -0.1175(3) -0.0131(3) 0.9301(2) 0.0268(9) Uani d . . . 1.0 . . H H19A -0.097752 0.026746 0.98475 0.032 Uiso calc U . R 1.0 . . H H19B -0.100959 -0.069384 0.937646 0.032 Uiso calc U . R 1.0 . . C C20 -0.2245(3) -0.0394(3) 0.9018(3) 0.0421(11) Uani d . . . 1.0 . . H H20A -0.256923 -0.072346 0.943513 0.051 Uiso calc U P R 0.883(5) A 1 H H20B -0.244557 -0.082419 0.848971 0.051 Uiso calc U P R 0.883(5) A 1 H H20C -0.25121 -0.107205 0.887635 0.051 Uiso calc U P R 0.117(5) A 2 H H20D -0.236261 -0.013944 0.849825 0.051 Uiso calc U P R 0.117(5) A 2 C C21 -0.2584(3) 0.0407(3) 0.8891(3) 0.0433(14) Uani d . P . 0.883(5) A 1 H H21A -0.227347 0.072199 0.846114 0.052 Uiso calc U P R 0.883(5) A 1 H H21B -0.235739 0.084728 0.941468 0.052 Uiso calc U P R 0.883(5) A 1 C C22 -0.3659(4) 0.0171(4) 0.8636(5) 0.069(2) Uani d . P . 0.883(5) A 1 H H22A -0.380884 0.072709 0.853049 0.103 Uiso calc U P R 0.883(5) A 1 H H22B -0.397215 -0.008585 0.908169 0.103 Uiso calc U P R 0.883(5) A 1 H H22C -0.389778 -0.02835 0.812967 0.103 Uiso calc U P R 0.883(5) A 1 C C21' -0.2879(16) -0.008(2) 0.965(2) 0.0433(14) Uani d . P D 0.117(5) A 2 H H21C -0.302104 -0.058366 0.998949 0.052 Uiso calc U P R 0.117(5) A 2 H H21D -0.238551 0.045047 1.003283 0.052 Uiso calc U P R 0.117(5) A 2 C C22' -0.3797(17) 0.020(2) 0.958(3) 0.069(2) Uani d . P D 0.117(5) A 2 H H22D -0.364794 0.082221 0.944027 0.103 Uiso calc U P R 0.117(5) A 2 H H22E -0.402051 0.017306 1.010404 0.103 Uiso calc U P R 0.117(5) A 2 H H22F -0.430535 -0.02313 0.913513 0.103 Uiso calc U P R 0.117(5) A 2 C C23 0.3667(2) 0.1418(2) 0.6072(2) 0.0179(8) Uani d . . . 1.0 . . H H23A 0.32684 0.115092 0.551038 0.022 Uiso calc U . R 1.0 . . H H23B 0.383135 0.209365 0.612899 0.022 Uiso calc U . R 1.0 . . C C25 0.5437(2) 0.1795(2) 0.6189(2) 0.0159(7) Uani d . . . 1.0 . . H H25 0.558396 0.244167 0.623423 0.019 Uiso calc U . R 1.0 . . C C27 0.5593(2) 0.0429(2) 0.6086(2) 0.0154(7) Uani d . . . 1.0 . . C C28 0.5923(2) -0.0310(2) 0.6012(2) 0.0167(7) Uani d . . . 1.0 . . H H28 0.658526 -0.022805 0.601004 0.02 Uiso calc U . R 1.0 . . C C29 0.5244(2) -0.1170(2) 0.5940(2) 0.0197(8) Uani d . . . 1.0 . . H H29 0.543925 -0.169697 0.589095 0.024 Uiso calc U . R 1.0 . . C C30 0.4274(2) -0.1282(2) 0.5938(2) 0.0192(8) Uani d . . . 1.0 . . H H30 0.382835 -0.188684 0.588978 0.023 Uiso calc U . R 1.0 . . C C31 0.3934(2) -0.0554(2) 0.6003(2) 0.0185(8) Uani d . . . 1.0 . . H H31 0.326975 -0.063726 0.599495 0.022 Uiso calc U . R 1.0 . . C C32 0.4626(2) 0.0309(2) 0.6082(2) 0.0146(7) Uani d . . . 1.0 . . C C33 0.7106(2) 0.1802(2) 0.6141(2) 0.0185(8) Uani d . . . 1.0 . . H H33A 0.722828 0.244854 0.60509 0.022 Uiso calc U . R 1.0 . . H H33B 0.726805 0.147762 0.566883 0.022 Uiso calc U . R 1.0 . . C C34 0.7761(2) 0.1783(2) 0.6937(2) 0.0213(8) Uani d . . . 1.0 . . H H34A 0.844298 0.203542 0.687251 0.026 Uiso calc U . R 1.0 . . H H34B 0.763428 0.113513 0.70236 0.026 Uiso calc U . R 1.0 . . C C35 0.7637(3) 0.2320(2) 0.7704(2) 0.0280(9) Uani d . . . 1.0 . . H H35A 0.695689 0.206413 0.777251 0.034 Uiso calc U . R 1.0 . . H H35B 0.805625 0.223261 0.819755 0.034 Uiso calc U . R 1.0 . . C C36 0.7880(3) 0.3339(2) 0.7677(3) 0.0382(10) Uani d . . . 1.0 . . H H36A 0.854659 0.359707 0.759353 0.057 Uiso calc U . R 1.0 . . H H36B 0.78194 0.364461 0.820266 0.057 Uiso calc U . R 1.0 . . H H36C 0.743319 0.343629 0.721826 0.057 Uiso calc U . R 1.0 . . N N7A 0.3284(2) 0.38491(18) 0.40670(18) 0.0169(6) Uani d . . . 1.0 . . N N8A 0.3610(2) 0.3637(2) 0.4619(2) 0.0233(7) Uani d . . . 1.0 . . N N10A 0.5015(2) 0.46742(19) 0.23425(17) 0.0199(7) Uani d . . . 1.0 . . N N12A 0.5959(2) 0.51401(19) 0.14754(17) 0.0210(7) Uani d . . . 1.0 . . N N24A 0.04015(19) 0.37622(18) 0.37617(17) 0.0158(6) Uani d . . . 1.0 . . N N26A -0.11065(19) 0.36252(17) 0.37438(17) 0.0155(6) Uani d . . . 1.0 . . C C1A 0.2860(2) 0.4091(2) 0.3333(2) 0.0158(7) Uani d . . . 1.0 . . C C2A 0.3472(2) 0.4465(2) 0.2803(2) 0.0184(8) Uani d . . . 1.0 . . C C3A 0.3024(2) 0.4627(2) 0.2065(2) 0.0210(8) Uani d . . . 1.0 . . H H3A 0.340411 0.488986 0.168075 0.025 Uiso calc U . R 1.0 . . C C4A 0.2035(2) 0.4417(2) 0.1874(2) 0.0213(8) Uani d . . . 1.0 . . H H4A 0.174238 0.451403 0.135103 0.026 Uiso calc U . R 1.0 . . C C5A 0.1458(3) 0.4065(2) 0.2429(2) 0.0200(8) Uani d . . . 1.0 . . H H5A 0.077821 0.394235 0.228854 0.024 Uiso calc U . R 1.0 . . C C6A 0.1857(2) 0.3893(2) 0.3180(2) 0.0158(7) Uani d . . . 1.0 . . C C9A 0.4558(2) 0.4711(3) 0.3055(2) 0.0253(9) Uani d . . . 1.0 . . H H9AA 0.483485 0.533912 0.337612 0.03 Uiso calc U . R 1.0 . . H H9AC 0.470287 0.428032 0.342136 0.03 Uiso calc U . R 1.0 . . C C11A 0.5589(2) 0.5391(2) 0.2089(2) 0.0213(8) Uani d . . . 1.0 . . H H11A 0.571803 0.601196 0.232202 0.026 Uiso calc U . R 1.0 . . C C13A 0.5605(2) 0.4190(3) 0.1304(2) 0.0226(8) Uani d . . . 1.0 . . C C14A 0.5747(3) 0.3587(3) 0.0705(2) 0.0294(9) Uani d . . . 1.0 . . H H14A 0.615065 0.379356 0.031985 0.035 Uiso calc U . R 1.0 . . C C15A 0.5276(3) 0.2688(3) 0.0703(3) 0.0372(10) Uani d . . . 1.0 . . H H15A 0.534648 0.225086 0.02974 0.045 Uiso calc U . R 1.0 . . C C16A 0.4694(3) 0.2369(3) 0.1264(3) 0.0411(11) Uani d . . . 1.0 . . H H16A 0.439412 0.172512 0.12365 0.049 Uiso calc U . R 1.0 . . C C17A 0.4531(3) 0.2967(3) 0.1873(3) 0.0343(10) Uani d . . . 1.0 . . H H17A 0.413047 0.275647 0.225923 0.041 Uiso calc U . R 1.0 . . C C18A 0.5003(2) 0.3886(2) 0.1863(2) 0.0223(8) Uani d . . . 1.0 . . C C19A 0.6726(3) 0.5781(3) 0.1129(2) 0.0268(9) Uani d . . . 1.0 . . H H19C 0.726196 0.553139 0.111783 0.032 Uiso calc U . R 1.0 . . H H19D 0.698755 0.638002 0.149908 0.032 Uiso calc U . R 1.0 . . C C20A 0.6365(3) 0.5928(2) 0.0272(2) 0.0280(9) Uani d . . . 1.0 . . H H20E 0.581017 0.615268 0.027481 0.034 Uiso calc U . R 1.0 . . H H20F 0.613509 0.533634 -0.010744 0.034 Uiso calc U . R 1.0 . . C C21A 0.7154(3) 0.6618(2) -0.0041(2) 0.0286(9) Uani d . . . 1.0 . . H H21E 0.772705 0.641473 0.00116 0.034 Uiso calc U . R 1.0 . . H H21F 0.692503 0.661351 -0.063919 0.034 Uiso calc U . R 1.0 . . C C22A 0.7469(3) 0.7592(2) 0.0397(3) 0.0368(10) Uani d . . . 1.0 . . H H22G 0.796743 0.798928 0.014342 0.055 Uiso calc U . R 1.0 . . H H22H 0.773264 0.761513 0.098535 0.055 Uiso calc U . R 1.0 . . H H22I 0.690998 0.780651 0.034769 0.055 Uiso calc U . R 1.0 . . C C23A 0.1272(2) 0.3509(2) 0.3809(2) 0.0187(8) Uani d . . . 1.0 . . H H23C 0.108517 0.28302 0.371734 0.022 Uiso calc U . R 1.0 . . H H23D 0.167818 0.373797 0.437269 0.022 Uiso calc U . R 1.0 . . C C25A -0.0489(2) 0.3183(2) 0.3672(2) 0.0152(7) Uani d . . . 1.0 . . H H25A -0.066247 0.253255 0.356861 0.018 Uiso calc U . R 1.0 . . C C27A -0.0587(2) 0.4561(2) 0.3887(2) 0.0160(7) Uani d . . . 1.0 . . C C28A -0.0886(2) 0.5317(2) 0.4021(2) 0.0188(8) Uani d . . . 1.0 . . H H28A -0.154634 0.525189 0.401397 0.023 Uiso calc U . R 1.0 . . C C29A -0.0175(2) 0.6163(2) 0.4165(2) 0.0194(8) Uani d . . . 1.0 . . H H29A -0.034795 0.670001 0.424789 0.023 Uiso calc U . R 1.0 . . C C30A 0.0797(3) 0.6254(2) 0.4194(2) 0.0217(8) Uani d . . . 1.0 . . H H30A 0.126848 0.685264 0.430519 0.026 Uiso calc U . R 1.0 . . C C31A 0.1095(2) 0.5506(2) 0.4065(2) 0.0197(8) Uani d . . . 1.0 . . H H31A 0.175709 0.557108 0.408408 0.024 Uiso calc U . R 1.0 . . C C32A 0.0376(2) 0.4653(2) 0.3907(2) 0.0153(7) Uani d . . . 1.0 . . C C33A -0.2155(2) 0.3215(2) 0.3680(2) 0.0209(8) Uani d . . . 1.0 . . H H33C -0.234964 0.35202 0.414305 0.025 Uiso calc U . R 1.0 . . H H33D -0.2315 0.255598 0.373705 0.025 Uiso calc U . R 1.0 . . C C34A -0.2724(3) 0.3302(2) 0.2866(2) 0.0258(9) Uani d . . . 1.0 . . H H34C -0.255797 0.396191 0.281063 0.031 Uiso calc U . R 1.0 . . H H34D -0.342366 0.305997 0.287562 0.031 Uiso calc U . R 1.0 . . C C35A -0.2538(3) 0.2799(3) 0.2115(2) 0.0354(10) Uani d . . . 1.0 . . H H35C -0.286158 0.296046 0.160701 0.042 Uiso calc U . R 1.0 . . H H35D -0.183301 0.301455 0.212392 0.042 Uiso calc U . R 1.0 . . C C36A -0.2892(3) 0.1765(3) 0.2068(3) 0.0503(12) Uani d . . . 1.0 . . H H36D -0.358385 0.154696 0.208323 0.075 Uiso calc U . R 1.0 . . H H36E -0.253034 0.159421 0.254109 0.075 Uiso calc U . R 1.0 . . H H36F -0.279013 0.148251 0.154927 0.075 Uiso calc U . R 1.0 . . F F2U 0.0456(2) 0.18571(19) 0.13293(17) 0.0646(8) Uani d . . . 1.0 . . F F3U -0.1157(2) 0.11402(17) 0.10244(15) 0.0708(9) Uani d . . . 1.0 . . F F4U -0.04152(17) 0.17571(18) 0.23390(13) 0.0482(7) Uani d . . . 1.0 . . F F5U -0.05469(17) 0.26722(15) 0.13663(17) 0.0523(7) Uani d . . . 1.0 . . B B1U -0.0413(4) 0.1863(3) 0.1518(3) 0.0340(11) Uani d . . . 1.0 . . F F2T 0.55199(16) 0.71622(15) 0.14442(15) 0.0428(6) Uani d . . . 1.0 . . F F3T 0.39348(18) 0.62945(15) 0.11295(13) 0.0465(7) Uani d . . . 1.0 . . F F4T 0.46428(17) 0.69489(18) 0.24447(14) 0.0479(7) Uani d . . . 1.0 . . F F5T 0.43802(16) 0.78312(15) 0.14714(18) 0.0546(7) Uani d . . . 1.0 . . B B1T 0.4616(3) 0.7061(3) 0.1624(3) 0.0310(11) Uani d . . . 1.0 . . F F2S 0.27302(15) 0.42969(13) 0.67931(13) 0.0314(5) Uani d . . . 1.0 . . F F3S 0.35506(15) 0.34231(15) 0.63059(13) 0.0352(6) Uani d . . . 1.0 . . F F4S 0.20634(14) 0.32814(13) 0.55957(12) 0.0286(5) Uani d . . . 1.0 . . F F5S 0.22371(18) 0.27720(14) 0.68295(13) 0.0416(6) Uani d . . . 1.0 . . B B1S 0.2637(3) 0.3448(3) 0.6378(3) 0.0213(9) Uani d . . . 1.0 . . F F2R 0.69415(15) 0.47160(13) 0.48913(13) 0.0318(5) Uani d . . . 1.0 . . F F3R 0.56084(18) 0.35372(15) 0.41885(14) 0.0471(7) Uani d . . . 1.0 . . F F4R 0.56001(18) 0.4277(2) 0.5395(2) 0.0828(11) Uani d . . . 1.0 . . F F5R 0.65009(18) 0.33491(17) 0.53249(19) 0.0682(9) Uani d . . . 1.0 . . B B1R 0.6153(3) 0.3964(3) 0.4952(3) 0.0199(9) Uani d . . . 1.0 . . F F2Q 0.29470(18) 0.21923(14) 0.30718(14) 0.0444(6) Uani d . . . 1.0 . . F F3Q 0.22702(14) 0.06599(13) 0.30321(12) 0.0274(5) Uani d . . . 1.0 . . F F4Q 0.14711(15) 0.16062(15) 0.33861(14) 0.0382(6) Uani d . . . 1.0 . . F F5Q 0.28111(14) 0.16193(13) 0.42670(12) 0.0244(5) Uani d . . . 1.0 . . B B1Q 0.2379(3) 0.1517(3) 0.3445(3) 0.0213(9) Uani d . . . 1.0 . . F F2P 0.94113(15) 0.07219(15) 0.45698(15) 0.0453(7) Uani d . . . 1.0 . . F F3P 0.80746(14) 0.03658(12) 0.51213(12) 0.0250(5) Uani d . . . 1.0 . . F F4P 0.85023(15) 0.16593(15) 0.45458(15) 0.0445(6) Uani d . . . 1.0 . . F F5P 0.94157(16) 0.15765(14) 0.57408(13) 0.0356(6) Uani d . . . 1.0 . . B B1P 0.8850(3) 0.1086(3) 0.4993(3) 0.0195(9) Uani d . . . 1.0 . . N N1M 0.1599(4) 0.5228(3) -0.0309(4) 0.0897(17) Uani d . . . 1.0 . . C C2M 0.1824(3) 0.5976(4) -0.0152(3) 0.0506(13) Uani d . . . 1.0 . . C C3M 0.2148(3) 0.6973(3) 0.0055(3) 0.0425(11) Uani d . . . 1.0 . . H H3MA 0.200909 0.724032 -0.044673 0.064 Uiso calc U . R 1.0 . . H H3MB 0.284747 0.720658 0.027878 0.064 Uiso calc U . R 1.0 . . H H3MC 0.180679 0.714426 0.047078 0.064 Uiso calc U . R 1.0 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 N7 0.0120(15) 0.0157(15) 0.0205(17) 0.0047(13) 0.0087(13) 0.0036(13) N8 0.0171(16) 0.0247(17) 0.0228(17) 0.0089(14) 0.0059(13) 0.0083(14) N10 0.0103(15) 0.0263(16) 0.0180(15) 0.0049(13) 0.0050(12) 0.0031(13) N12 0.0174(16) 0.0244(16) 0.0192(16) 0.0060(14) 0.0064(13) 0.0036(13) N24 0.0107(15) 0.0142(14) 0.0203(15) 0.0050(12) 0.0074(12) 0.0067(12) N26 0.0097(15) 0.0147(14) 0.0179(15) 0.0023(12) 0.0040(12) 0.0037(12) C1 0.0141(18) 0.0151(17) 0.0148(18) 0.0058(15) 0.0003(14) 0.0023(14) C2 0.0171(19) 0.0209(18) 0.0173(18) 0.0075(16) 0.0044(15) 0.0000(15) C3 0.019(2) 0.032(2) 0.0194(19) 0.0085(17) 0.0099(16) 0.0074(17) C4 0.022(2) 0.030(2) 0.0151(18) 0.0111(17) 0.0025(16) 0.0070(16) C5 0.0151(19) 0.0188(18) 0.023(2) 0.0074(16) 0.0015(16) 0.0000(15) C6 0.0136(18) 0.0120(16) 0.0170(18) 0.0051(14) 0.0024(14) 0.0012(14) C9 0.0152(19) 0.040(2) 0.0160(18) 0.0101(17) 0.0092(15) 0.0047(17) C11 0.0142(19) 0.028(2) 0.023(2) 0.0098(16) 0.0037(16) 0.0043(17) C13 0.0102(18) 0.027(2) 0.022(2) 0.0057(16) 0.0008(15) 0.0013(16) C14 0.024(2) 0.035(2) 0.027(2) 0.0111(19) 0.0041(17) -0.0033(18) C15 0.028(2) 0.029(2) 0.050(3) 0.0111(19) 0.004(2) -0.005(2) C16 0.021(2) 0.026(2) 0.054(3) 0.0049(18) 0.004(2) 0.011(2) C17 0.019(2) 0.032(2) 0.033(2) 0.0073(18) 0.0035(17) 0.0094(18) C18 0.0106(18) 0.025(2) 0.0194(19) 0.0053(16) -0.0002(15) 0.0005(16) C19 0.026(2) 0.031(2) 0.027(2) 0.0094(18) 0.0139(17) 0.0097(17) C20 0.032(2) 0.062(3) 0.041(3) 0.015(2) 0.018(2) 0.030(2) C21 0.030(3) 0.049(3) 0.060(3) 0.015(2) 0.016(2) 0.033(3) C22 0.039(3) 0.048(3) 0.133(6) 0.020(3) 0.027(4) 0.047(4) C21' 0.030(3) 0.049(3) 0.060(3) 0.015(2) 0.016(2) 0.033(3) C22' 0.039(3) 0.048(3) 0.133(6) 0.020(3) 0.027(4) 0.047(4) C23 0.0117(18) 0.0221(18) 0.0234(19) 0.0103(15) 0.0034(15) 0.0042(16) C25 0.0152(19) 0.0169(17) 0.0182(18) 0.0071(16) 0.0060(15) 0.0048(15) C27 0.0152(18) 0.0205(18) 0.0114(17) 0.0057(15) 0.0034(14) 0.0061(14) C28 0.0118(18) 0.0202(18) 0.0216(19) 0.0084(15) 0.0046(15) 0.0070(15) C29 0.020(2) 0.0197(19) 0.023(2) 0.0104(16) 0.0063(16) 0.0054(15) C30 0.0175(19) 0.0134(17) 0.025(2) 0.0023(15) 0.0046(16) 0.0060(15) C31 0.0126(18) 0.0205(19) 0.0206(19) 0.0032(15) 0.0026(15) 0.0033(15) C32 0.0152(18) 0.0159(17) 0.0145(17) 0.0073(15) 0.0036(14) 0.0033(14) C33 0.0103(18) 0.0185(18) 0.025(2) 0.0028(15) 0.0046(15) 0.0028(15) C34 0.0168(19) 0.0176(18) 0.029(2) 0.0057(16) 0.0031(16) 0.0057(16) C35 0.033(2) 0.029(2) 0.024(2) 0.0116(18) 0.0034(18) 0.0078(17) C36 0.056(3) 0.025(2) 0.033(2) 0.015(2) 0.005(2) 0.0011(18) N7A 0.0143(16) 0.0208(16) 0.0187(16) 0.0079(13) 0.0076(13) 0.0039(13) N8A 0.0163(17) 0.0312(18) 0.0248(18) 0.0093(15) 0.0048(14) 0.0096(15) N10A 0.0162(16) 0.0258(16) 0.0179(16) 0.0058(14) 0.0056(13) 0.0042(13) N12A 0.0186(16) 0.0285(17) 0.0208(16) 0.0114(14) 0.0069(13) 0.0106(14) N24A 0.0123(15) 0.0174(15) 0.0217(16) 0.0080(13) 0.0068(12) 0.0059(12) N26A 0.0106(15) 0.0128(14) 0.0229(16) 0.0021(12) 0.0060(12) 0.0040(12) C1A 0.0161(19) 0.0176(17) 0.0149(18) 0.0083(15) 0.0016(15) 0.0021(15) C2A 0.0146(19) 0.0231(19) 0.0187(19) 0.0075(16) 0.0060(15) 0.0010(15) C3A 0.020(2) 0.027(2) 0.0164(19) 0.0058(17) 0.0104(16) 0.0034(16) C4A 0.022(2) 0.0250(19) 0.0178(19) 0.0108(17) -0.0002(16) 0.0028(16) C5A 0.0188(19) 0.0206(19) 0.023(2) 0.0104(16) 0.0051(16) 0.0015(16) C6A 0.0133(18) 0.0141(17) 0.0215(19) 0.0056(15) 0.0063(15) 0.0024(15) C9A 0.0127(19) 0.043(2) 0.0186(19) 0.0065(17) 0.0052(15) 0.0038(17) C11A 0.0158(19) 0.030(2) 0.024(2) 0.0114(17) 0.0077(16) 0.0092(17) C13A 0.0163(19) 0.036(2) 0.0178(19) 0.0127(18) 0.0026(15) 0.0038(17) C14A 0.025(2) 0.037(2) 0.029(2) 0.0164(19) 0.0047(18) 0.0027(19) C15A 0.024(2) 0.045(3) 0.043(3) 0.017(2) 0.004(2) -0.002(2) C16A 0.030(2) 0.023(2) 0.061(3) 0.0042(19) -0.005(2) 0.002(2) C17A 0.019(2) 0.033(2) 0.047(3) 0.0055(19) -0.0002(19) 0.011(2) C18A 0.0144(19) 0.0217(19) 0.028(2) 0.0057(16) -0.0019(16) 0.0003(16) C19A 0.018(2) 0.037(2) 0.030(2) 0.0107(18) 0.0101(17) 0.0106(18) C20A 0.025(2) 0.029(2) 0.034(2) 0.0114(18) 0.0086(18) 0.0086(18) C21A 0.027(2) 0.031(2) 0.030(2) 0.0104(18) 0.0090(18) 0.0120(18) C22A 0.034(2) 0.028(2) 0.044(3) 0.0070(19) -0.002(2) 0.0121(19) C23A 0.0154(19) 0.0199(18) 0.025(2) 0.0099(16) 0.0056(15) 0.0072(16) C25A 0.0140(19) 0.0163(17) 0.0169(18) 0.0051(15) 0.0059(14) 0.0054(14) C27A 0.0121(18) 0.0193(18) 0.0178(18) 0.0047(15) 0.0057(14) 0.0059(15) C28A 0.0161(19) 0.0214(19) 0.0214(19) 0.0081(16) 0.0053(15) 0.0060(16) C29A 0.022(2) 0.0170(18) 0.0223(19) 0.0094(16) 0.0067(16) 0.0060(15) C30A 0.021(2) 0.0193(19) 0.023(2) 0.0041(16) 0.0044(16) 0.0040(16) C31A 0.0165(19) 0.0237(19) 0.0220(19) 0.0077(16) 0.0080(15) 0.0078(16) C32A 0.0156(19) 0.0151(17) 0.0169(18) 0.0053(15) 0.0058(15) 0.0050(14) C33A 0.0114(18) 0.0191(18) 0.031(2) 0.0023(15) 0.0078(16) 0.0033(16) C34A 0.016(2) 0.024(2) 0.033(2) 0.0037(17) -0.0030(17) 0.0063(17) C35A 0.030(2) 0.043(3) 0.027(2) 0.009(2) -0.0031(18) 0.0042(19) C36A 0.056(3) 0.047(3) 0.043(3) 0.019(2) 0.000(2) -0.009(2) F2U 0.090(2) 0.080(2) 0.0666(19) 0.0644(18) 0.0467(17) 0.0392(16) F3U 0.120(3) 0.0377(15) 0.0261(14) -0.0102(16) 0.0118(16) -0.0030(12) F4U 0.0510(16) 0.0777(18) 0.0235(13) 0.0374(15) 0.0028(11) -0.0037(12) F5U 0.0409(15) 0.0330(13) 0.081(2) 0.0182(12) -0.0050(14) 0.0086(13) B1U 0.048(3) 0.031(3) 0.025(3) 0.019(2) 0.007(2) 0.001(2) F2T 0.0384(15) 0.0392(14) 0.0578(16) 0.0191(12) 0.0163(12) 0.0084(12) F3T 0.0595(17) 0.0342(13) 0.0267(13) -0.0072(12) 0.0024(12) 0.0027(11) F4T 0.0503(16) 0.0719(18) 0.0264(13) 0.0330(14) 0.0033(11) -0.0062(12) F5T 0.0314(14) 0.0366(14) 0.096(2) 0.0174(12) -0.0005(14) 0.0135(14) B1T 0.029(3) 0.028(2) 0.035(3) 0.012(2) -0.001(2) 0.002(2) F2S 0.0313(13) 0.0223(11) 0.0389(13) 0.0157(10) -0.0057(10) -0.0054(10) F3S 0.0278(13) 0.0469(14) 0.0343(13) 0.0212(11) 0.0031(10) -0.0028(11) F4S 0.0292(12) 0.0307(12) 0.0258(12) 0.0136(10) -0.0009(10) 0.0025(10) F5S 0.0654(17) 0.0297(12) 0.0325(13) 0.0117(12) 0.0221(12) 0.0125(11) B1S 0.021(2) 0.020(2) 0.026(2) 0.0101(19) 0.0070(19) 0.0072(18) F2R 0.0337(13) 0.0207(11) 0.0399(13) 0.0063(10) 0.0072(11) 0.0098(10) F3R 0.0570(17) 0.0337(13) 0.0358(14) 0.0036(12) -0.0048(12) -0.0026(11) F4R 0.0290(16) 0.091(2) 0.099(2) -0.0098(15) 0.0332(15) -0.0601(19) F5R 0.0382(16) 0.0456(16) 0.103(2) -0.0042(13) -0.0200(15) 0.0495(16) B1R 0.015(2) 0.027(2) 0.020(2) 0.0085(19) 0.0039(18) 0.0039(19) F2Q 0.0665(17) 0.0292(13) 0.0322(13) 0.0026(12) 0.0186(13) 0.0117(11) F3Q 0.0261(12) 0.0246(11) 0.0326(12) 0.0145(10) -0.0002(10) -0.0012(9) F4Q 0.0339(13) 0.0457(14) 0.0403(14) 0.0297(12) -0.0035(11) -0.0071(11) F5Q 0.0249(11) 0.0279(11) 0.0228(11) 0.0118(9) 0.0039(9) 0.0059(9) B1Q 0.023(2) 0.019(2) 0.025(2) 0.0107(19) 0.0024(19) 0.0058(18) F2P 0.0220(13) 0.0434(14) 0.0615(17) 0.0015(11) 0.0185(12) -0.0215(12) F3P 0.0256(12) 0.0169(10) 0.0341(12) 0.0064(9) 0.0110(10) 0.0063(9) F4P 0.0278(13) 0.0417(14) 0.0609(16) 0.0047(11) -0.0009(12) 0.0344(13) F5P 0.0443(14) 0.0253(12) 0.0282(12) 0.0048(11) 0.0002(11) -0.0040(10) B1P 0.016(2) 0.022(2) 0.022(2) 0.0064(19) 0.0055(18) 0.0062(19) N1M 0.071(4) 0.048(3) 0.141(5) 0.011(3) 0.023(3) -0.004(3) C2M 0.044(3) 0.047(3) 0.061(3) 0.017(3) 0.013(2) -0.005(3) C3M 0.051(3) 0.049(3) 0.036(3) 0.027(2) 0.009(2) 0.007(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N8 N7 C1 . . 178.8(3) ? C11 N10 C18 . . 108.8(3) ? C11 N10 C9 . . 124.9(3) ? C18 N10 C9 . . 126.1(3) ? C11 N12 C13 . . 108.3(3) ? C11 N12 C19 . . 124.5(3) ? C13 N12 C19 . . 127.0(3) ? C25 N24 C32 . . 108.1(3) ? C25 N24 C23 . . 124.9(3) ? C32 N24 C23 . . 126.3(3) ? C25 N26 C27 . . 108.3(3) ? C25 N26 C33 . . 126.4(3) ? C27 N26 C33 . . 125.2(3) ? C2 C1 C6 . . 125.8(3) ? C2 C1 N7 . . 117.5(3) ? C6 C1 N7 . . 116.7(3) ? C3 C2 C1 . . 115.5(3) ? C3 C2 C9 . . 122.1(3) ? C1 C2 C9 . . 122.4(3) ? C2 C3 C4 . . 120.9(3) ? C2 C3 H3 . . 119.5 ? C4 C3 H3 . . 119.5 ? C3 C4 C5 . . 121.5(3) ? C3 C4 H4 . . 119.3 ? C5 C4 H4 . . 119.3 ? C6 C5 C4 . . 120.3(3) ? C6 C5 H5 . . 119.9 ? C4 C5 H5 . . 119.9 ? C5 C6 C1 . . 116.0(3) ? C5 C6 C23 . . 123.3(3) ? C1 C6 C23 . . 120.6(3) ? N10 C9 C2 . . 111.0(3) ? N10 C9 H9A . . 109.4 ? C2 C9 H9A . . 109.4 ? N10 C9 H9AB . . 109.4 ? C2 C9 H9AB . . 109.4 ? H9A C9 H9AB . . 108.0 ? N12 C11 N10 . . 110.0(3) ? N12 C11 H11 . . 125.0 ? N10 C11 H11 . . 125.0 ? C18 C13 C14 . . 121.2(3) ? C18 C13 N12 . . 107.0(3) ? C14 C13 N12 . . 131.8(3) ? C15 C14 C13 . . 116.4(4) ? C15 C14 H14 . . 121.8 ? C13 C14 H14 . . 121.8 ? C14 C15 C16 . . 122.2(4) ? C14 C15 H15 . . 118.9 ? C16 C15 H15 . . 118.9 ? C17 C16 C15 . . 121.9(4) ? C17 C16 H16 . . 119.0 ? C15 C16 H16 . . 119.0 ? C16 C17 C18 . . 115.6(4) ? C16 C17 H17 . . 122.2 ? C18 C17 H17 . . 122.2 ? C17 C18 C13 . . 122.7(3) ? C17 C18 N10 . . 131.3(3) ? C13 C18 N10 . . 106.0(3) ? N12 C19 C20 . . 113.1(3) ? N12 C19 H19A . . 109.0 ? C20 C19 H19A . . 109.0 ? N12 C19 H19B . . 109.0 ? C20 C19 H19B . . 109.0 ? H19A C19 H19B . . 107.8 ? C19 C20 C21 . . 113.8(4) ? C19 C20 C21' . . 118.7(11) ? C19 C20 H20A . . 108.8 ? C21 C20 H20A . . 108.8 ? C19 C20 H20B . . 108.8 ? C21 C20 H20B . . 108.8 ? H20A C20 H20B . . 107.7 ? C19 C20 H20C . . 107.6 ? C21' C20 H20C . . 107.6 ? C19 C20 H20D . . 107.6 ? C21' C20 H20D . . 107.6 ? H20C C20 H20D . . 107.1 ? C20 C21 C22 . . 115.2(4) ? C20 C21 H21A . . 108.5 ? C22 C21 H21A . . 108.5 ? C20 C21 H21B . . 108.5 ? C22 C21 H21B . . 108.5 ? H21A C21 H21B . . 107.5 ? C21 C22 H22A . . 109.5 ? C21 C22 H22B . . 109.5 ? H22A C22 H22B . . 109.5 ? C21 C22 H22C . . 109.5 ? H22A C22 H22C . . 109.5 ? H22B C22 H22C . . 109.5 ? C22' C21' C20 . . 137.(3) ? C22' C21' H21C . . 102.9 ? C20 C21' H21C . . 102.9 ? C22' C21' H21D . . 102.9 ? C20 C21' H21D . . 102.8 ? H21C C21' H21D . . 105.0 ? C21' C22' H22D . . 109.5 ? C21' C22' H22E . . 109.5 ? H22D C22' H22E . . 109.5 ? C21' C22' H22F . . 109.5 ? H22D C22' H22F . . 109.5 ? H22E C22' H22F . . 109.5 ? N24 C23 C6 . . 112.4(3) ? N24 C23 H23A . . 109.1 ? C6 C23 H23A . . 109.1 ? N24 C23 H23B . . 109.1 ? C6 C23 H23B . . 109.1 ? H23A C23 H23B . . 107.9 ? N26 C25 N24 . . 110.7(3) ? N26 C25 H25 . . 124.6 ? N24 C25 H25 . . 124.6 ? C28 C27 C32 . . 121.7(3) ? C28 C27 N26 . . 131.3(3) ? C32 C27 N26 . . 107.0(3) ? C29 C28 C27 . . 116.6(3) ? C29 C28 H28 . . 121.7 ? C27 C28 H28 . . 121.7 ? C28 C29 C30 . . 121.2(3) ? C28 C29 H29 . . 119.4 ? C30 C29 H29 . . 119.4 ? C31 C30 C29 . . 122.9(3) ? C31 C30 H30 . . 118.5 ? C29 C30 H30 . . 118.5 ? C30 C31 C32 . . 115.4(3) ? C30 C31 H31 . . 122.3 ? C32 C31 H31 . . 122.3 ? C27 C32 C31 . . 122.3(3) ? C27 C32 N24 . . 105.8(3) ? C31 C32 N24 . . 131.9(3) ? N26 C33 C34 . . 112.6(3) ? N26 C33 H33A . . 109.1 ? C34 C33 H33A . . 109.1 ? N26 C33 H33B . . 109.1 ? C34 C33 H33B . . 109.1 ? H33A C33 H33B . . 107.8 ? C33 C34 C35 . . 114.4(3) ? C33 C34 H34A . . 108.7 ? C35 C34 H34A . . 108.7 ? C33 C34 H34B . . 108.7 ? C35 C34 H34B . . 108.7 ? H34A C34 H34B . . 107.6 ? C36 C35 C34 . . 114.0(3) ? C36 C35 H35A . . 108.7 ? C34 C35 H35A . . 108.7 ? C36 C35 H35B . . 108.7 ? C34 C35 H35B . . 108.7 ? H35A C35 H35B . . 107.6 ? C35 C36 H36A . . 109.5 ? C35 C36 H36B . . 109.5 ? H36A C36 H36B . . 109.5 ? C35 C36 H36C . . 109.5 ? H36A C36 H36C . . 109.5 ? H36B C36 H36C . . 109.5 ? N8A N7A C1A . . 177.7(3) ? C11A N10A C18A . . 108.1(3) ? C11A N10A C9A . . 125.2(3) ? C18A N10A C9A . . 126.4(3) ? C11A N12A C13A . . 107.9(3) ? C11A N12A C19A . . 124.0(3) ? C13A N12A C19A . . 127.6(3) ? C25A N24A C32A . . 108.2(3) ? C25A N24A C23A . . 125.5(3) ? C32A N24A C23A . . 125.9(3) ? C25A N26A C27A . . 107.8(3) ? C25A N26A C33A . . 126.8(3) ? C27A N26A C33A . . 125.5(3) ? C2A C1A C6A . . 125.6(3) ? C2A C1A N7A . . 117.1(3) ? C6A C1A N7A . . 117.3(3) ? C3A C2A C1A . . 115.5(3) ? C3A C2A C9A . . 123.3(3) ? C1A C2A C9A . . 121.2(3) ? C4A C3A C2A . . 121.2(3) ? C4A C3A H3A . . 119.4 ? C2A C3A H3A . . 119.4 ? C3A C4A C5A . . 121.3(3) ? C3A C4A H4A . . 119.3 ? C5A C4A H4A . . 119.3 ? C6A C5A C4A . . 120.6(3) ? C6A C5A H5A . . 119.7 ? C4A C5A H5A . . 119.7 ? C5A C6A C1A . . 115.8(3) ? C5A C6A C23A . . 123.4(3) ? C1A C6A C23A . . 120.8(3) ? N10A C9A C2A . . 112.1(3) ? N10A C9A H9AA . . 109.2 ? C2A C9A H9AA . . 109.2 ? N10A C9A H9AC . . 109.2 ? C2A C9A H9AC . . 109.2 ? H9AA C9A H9AC . . 107.9 ? N12A C11A N10A . . 111.5(3) ? N12A C11A H11A . . 124.3 ? N10A C11A H11A . . 124.3 ? C14A C13A N12A . . 131.1(3) ? C14A C13A C18A . . 122.0(4) ? N12A C13A C18A . . 106.8(3) ? C15A C14A C13A . . 115.7(4) ? C15A C14A H14A . . 122.1 ? C13A C14A H14A . . 122.1 ? C14A C15A C16A . . 123.2(4) ? C14A C15A H15A . . 118.4 ? C16A C15A H15A . . 118.4 ? C15A C16A C17A . . 122.2(4) ? C15A C16A H16A . . 118.9 ? C17A C16A H16A . . 118.9 ? C18A C17A C16A . . 114.3(4) ? C18A C17A H17A . . 122.9 ? C16A C17A H17A . . 122.9 ? C17A C18A N10A . . 131.7(4) ? C17A C18A C13A . . 122.6(4) ? N10A C18A C13A . . 105.7(3) ? N12A C19A C20A . . 112.8(3) ? N12A C19A H19C . . 109.0 ? C20A C19A H19C . . 109.0 ? N12A C19A H19D . . 109.0 ? C20A C19A H19D . . 109.0 ? H19C C19A H19D . . 107.8 ? C19A C20A C21A . . 111.1(3) ? C19A C20A H20E . . 109.4 ? C21A C20A H20E . . 109.4 ? C19A C20A H20F . . 109.4 ? C21A C20A H20F . . 109.4 ? H20E C20A H20F . . 108.0 ? C22A C21A C20A . . 115.4(3) ? C22A C21A H21E . . 108.4 ? C20A C21A H21E . . 108.4 ? C22A C21A H21F . . 108.4 ? C20A C21A H21F . . 108.4 ? H21E C21A H21F . . 107.5 ? C21A C22A H22G . . 109.5 ? C21A C22A H22H . . 109.5 ? H22G C22A H22H . . 109.5 ? C21A C22A H22I . . 109.5 ? H22G C22A H22I . . 109.5 ? H22H C22A H22I . . 109.5 ? N24A C23A C6A . . 112.3(3) ? N24A C23A H23C . . 109.1 ? C6A C23A H23C . . 109.1 ? N24A C23A H23D . . 109.1 ? C6A C23A H23D . . 109.1 ? H23C C23A H23D . . 107.9 ? N24A C25A N26A . . 111.1(3) ? N24A C25A H25A . . 124.5 ? N26A C25A H25A . . 124.5 ? C32A C27A N26A . . 107.0(3) ? C32A C27A C28A . . 122.1(3) ? N26A C27A C28A . . 130.9(3) ? C29A C28A C27A . . 116.2(3) ? C29A C28A H28A . . 121.9 ? C27A C28A H28A . . 121.9 ? C28A C29A C30A . . 121.6(3) ? C28A C29A H29A . . 119.2 ? C30A C29A H29A . . 119.2 ? C31A C30A C29A . . 122.2(3) ? C31A C30A H30A . . 118.9 ? C29A C30A H30A . . 118.9 ? C30A C31A C32A . . 116.2(3) ? C30A C31A H31A . . 121.9 ? C32A C31A H31A . . 121.9 ? C31A C32A C27A . . 121.7(3) ? C31A C32A N24A . . 132.3(3) ? C27A C32A N24A . . 106.0(3) ? N26A C33A C34A . . 112.3(3) ? N26A C33A H33C . . 109.1 ? C34A C33A H33C . . 109.1 ? N26A C33A H33D . . 109.1 ? C34A C33A H33D . . 109.1 ? H33C C33A H33D . . 107.9 ? C33A C34A C35A . . 113.8(3) ? C33A C34A H34C . . 108.8 ? C35A C34A H34C . . 108.8 ? C33A C34A H34D . . 108.8 ? C35A C34A H34D . . 108.8 ? H34C C34A H34D . . 107.7 ? C36A C35A C34A . . 113.8(4) ? C36A C35A H35C . . 108.8 ? C34A C35A H35C . . 108.8 ? C36A C35A H35D . . 108.8 ? C34A C35A H35D . . 108.8 ? H35C C35A H35D . . 107.7 ? C35A C36A H36D . . 109.5 ? C35A C36A H36E . . 109.5 ? H36D C36A H36E . . 109.5 ? C35A C36A H36F . . 109.5 ? H36D C36A H36F . . 109.5 ? H36E C36A H36F . . 109.5 ? F5U B1U F2U . . 109.3(4) ? F5U B1U F4U . . 110.8(4) ? F2U B1U F4U . . 109.7(4) ? F5U B1U F3U . . 109.1(4) ? F2U B1U F3U . . 109.2(4) ? F4U B1U F3U . . 108.7(4) ? F4T B1T F5T . . 110.6(4) ? F4T B1T F3T . . 109.1(4) ? F5T B1T F3T . . 109.5(3) ? F4T B1T F2T . . 108.9(3) ? F5T B1T F2T . . 109.0(4) ? F3T B1T F2T . . 109.7(4) ? F5S B1S F2S . . 109.5(3) ? F5S B1S F4S . . 109.7(3) ? F2S B1S F4S . . 111.0(3) ? F5S B1S F3S . . 108.0(3) ? F2S B1S F3S . . 109.2(3) ? F4S B1S F3S . . 109.3(3) ? F4R B1R F3R . . 108.9(3) ? F4R B1R F5R . . 112.5(4) ? F3R B1R F5R . . 108.3(3) ? F4R B1R F2R . . 107.6(3) ? F3R B1R F2R . . 111.6(3) ? F5R B1R F2R . . 108.0(3) ? F5Q B1Q F2Q . . 109.1(3) ? F5Q B1Q F3Q . . 110.9(3) ? F2Q B1Q F3Q . . 109.4(3) ? F5Q B1Q F4Q . . 109.8(3) ? F2Q B1Q F4Q . . 109.1(3) ? F3Q B1Q F4Q . . 108.5(3) ? F4P B1P F5P . . 109.4(3) ? F4P B1P F2P . . 111.0(3) ? F5P B1P F2P . . 108.3(3) ? F4P B1P F3P . . 109.2(3) ? F5P B1P F3P . . 110.6(3) ? F2P B1P F3P . . 108.3(3) ? N1M C2M C3M . . 178.6(6) ? C2M C3M H3MA . . 109.5 ? C2M C3M H3MB . . 109.5 ? H3MA C3M H3MB . . 109.5 ? C2M C3M H3MC . . 109.5 ? H3MA C3M H3MC . . 109.5 ? H3MB C3M H3MC . . 109.5 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag N7 N8 . 1.088(4) ? N7 C1 . 1.419(5) ? N10 C11 . 1.330(5) ? N10 C18 . 1.388(5) ? N10 C9 . 1.457(4) ? N12 C11 . 1.325(4) ? N12 C13 . 1.389(5) ? N12 C19 . 1.475(5) ? N24 C25 . 1.330(4) ? N24 C32 . 1.402(4) ? N24 C23 . 1.460(4) ? N26 C25 . 1.315(4) ? N26 C27 . 1.392(4) ? N26 C33 . 1.471(4) ? C1 C2 . 1.387(5) ? C1 C6 . 1.392(5) ? C2 C3 . 1.374(5) ? C2 C9 . 1.519(5) ? C3 C4 . 1.380(5) ? C3 H3 . 0.95 ? C4 C5 . 1.382(5) ? C4 H4 . 0.95 ? C5 C6 . 1.373(5) ? C5 H5 . 0.95 ? C6 C23 . 1.506(5) ? C9 H9A . 0.99 ? C9 H9AB . 0.99 ? C11 H11 . 0.95 ? C13 C18 . 1.386(5) ? C13 C14 . 1.388(5) ? C14 C15 . 1.368(6) ? C14 H14 . 0.95 ? C15 C16 . 1.393(6) ? C15 H15 . 0.95 ? C16 C17 . 1.380(5) ? C16 H16 . 0.95 ? C17 C18 . 1.380(5) ? C17 H17 . 0.95 ? C19 C20 . 1.492(6) ? C19 H19A . 0.99 ? C19 H19B . 0.99 ? C20 C21 . 1.498(6) ? C20 C21' . 1.65(3) ? C20 H20A . 0.99 ? C20 H20B . 0.99 ? C20 H20C . 0.99 ? C20 H20D . 0.99 ? C21 C22 . 1.498(7) ? C21 H21A . 0.99 ? C21 H21B . 0.99 ? C22 H22A . 0.98 ? C22 H22B . 0.98 ? C22 H22C . 0.98 ? C21' C22' . 1.540(2) ? C21' H21C . 0.99 ? C21' H21D . 0.99 ? C22' H22D . 0.98 ? C22' H22E . 0.98 ? C22' H22F . 0.98 ? C23 H23A . 0.99 ? C23 H23B . 0.99 ? C25 H25 . 0.95 ? C27 C28 . 1.384(5) ? C27 C32 . 1.386(5) ? C28 C29 . 1.376(5) ? C28 H28 . 0.95 ? C29 C30 . 1.393(5) ? C29 H29 . 0.95 ? C30 C31 . 1.376(5) ? C30 H30 . 0.95 ? C31 C32 . 1.386(5) ? C31 H31 . 0.95 ? C33 C34 . 1.513(5) ? C33 H33A . 0.99 ? C33 H33B . 0.99 ? C34 C35 . 1.520(5) ? C34 H34A . 0.99 ? C34 H34B . 0.99 ? C35 C36 . 1.512(5) ? C35 H35A . 0.99 ? C35 H35B . 0.99 ? C36 H36A . 0.98 ? C36 H36B . 0.98 ? C36 H36C . 0.98 ? N7A N8A . 1.088(4) ? N7A C1A . 1.412(5) ? N10A C11A . 1.318(4) ? N10A C18A . 1.388(5) ? N10A C9A . 1.453(5) ? N12A C11A . 1.311(4) ? N12A C13A . 1.383(5) ? N12A C19A . 1.485(5) ? N24A C25A . 1.319(4) ? N24A C32A . 1.394(4) ? N24A C23A . 1.457(4) ? N26A C25A . 1.319(4) ? N26A C27A . 1.389(4) ? N26A C33A . 1.466(5) ? C1A C2A . 1.392(5) ? C1A C6A . 1.397(5) ? C2A C3A . 1.375(5) ? C2A C9A . 1.511(5) ? C3A C4A . 1.375(5) ? C3A H3A . 0.95 ? C4A C5A . 1.383(5) ? C4A H4A . 0.95 ? C5A C6A . 1.372(5) ? C5A H5A . 0.95 ? C6A C23A . 1.503(5) ? C9A H9AA . 0.99 ? C9A H9AC . 0.99 ? C11A H11A . 0.95 ? C13A C14A . 1.384(5) ? C13A C18A . 1.395(5) ? C14A C15A . 1.348(6) ? C14A H14A . 0.95 ? C15A C16A . 1.383(6) ? C15A H15A . 0.95 ? C16A C17A . 1.405(6) ? C16A H16A . 0.95 ? C17A C18A . 1.377(5) ? C17A H17A . 0.95 ? C19A C20A . 1.494(5) ? C19A H19C . 0.99 ? C19A H19D . 0.99 ? C20A C21A . 1.512(5) ? C20A H20E . 0.99 ? C20A H20F . 0.99 ? C21A C22A . 1.506(5) ? C21A H21E . 0.99 ? C21A H21F . 0.99 ? C22A H22G . 0.98 ? C22A H22H . 0.98 ? C22A H22I . 0.98 ? C23A H23C . 0.99 ? C23A H23D . 0.99 ? C25A H25A . 0.95 ? C27A C32A . 1.385(5) ? C27A C28A . 1.390(5) ? C28A C29A . 1.371(5) ? C28A H28A . 0.95 ? C29A C30A . 1.398(5) ? C29A H29A . 0.95 ? C30A C31A . 1.376(5) ? C30A H30A . 0.95 ? C31A C32A . 1.383(5) ? C31A H31A . 0.95 ? C33A C34A . 1.510(5) ? C33A H33C . 0.99 ? C33A H33D . 0.99 ? C34A C35A . 1.512(6) ? C34A H34C . 0.99 ? C34A H34D . 0.99 ? C35A C36A . 1.513(6) ? C35A H35C . 0.99 ? C35A H35D . 0.99 ? C36A H36D . 0.98 ? C36A H36E . 0.98 ? C36A H36F . 0.98 ? F2U B1U . 1.376(6) ? F3U B1U . 1.380(6) ? F4U B1U . 1.379(5) ? F5U B1U . 1.369(5) ? F2T B1T . 1.382(5) ? F3T B1T . 1.379(5) ? F4T B1T . 1.377(6) ? F5T B1T . 1.380(5) ? F2S B1S . 1.381(5) ? F3S B1S . 1.392(5) ? F4S B1S . 1.381(5) ? F5S B1S . 1.377(5) ? F2R B1R . 1.392(5) ? F3R B1R . 1.366(5) ? F4R B1R . 1.348(5) ? F5R B1R . 1.367(5) ? F2Q B1Q . 1.382(5) ? F3Q B1Q . 1.385(5) ? F4Q B1Q . 1.386(5) ? F5Q B1Q . 1.377(5) ? F2P B1P . 1.383(5) ? F3P B1P . 1.387(5) ? F4P B1P . 1.374(5) ? F5P B1P . 1.379(5) ? N1M C2M . 1.093(6) ? C2M C3M . 1.456(7) ? C3M H3MA . 0.98 ? C3M H3MB . 0.98 ? C3M H3MC . 0.98 ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C6 C1 C2 C3 . . . . 0.3(5) ? N7 C1 C2 C3 . . . . -176.3(3) ? C6 C1 C2 C9 . . . . -177.1(3) ? N7 C1 C2 C9 . . . . 6.3(5) ? C1 C2 C3 C4 . . . . 0.2(5) ? C9 C2 C3 C4 . . . . 177.7(3) ? C2 C3 C4 C5 . . . . -0.4(5) ? C3 C4 C5 C6 . . . . 0.0(5) ? C4 C5 C6 C1 . . . . 0.5(5) ? C4 C5 C6 C23 . . . . 179.0(3) ? C2 C1 C6 C5 . . . . -0.6(5) ? N7 C1 C6 C5 . . . . 175.9(3) ? C2 C1 C6 C23 . . . . -179.2(3) ? N7 C1 C6 C23 . . . . -2.6(4) ? C11 N10 C9 C2 . . . . -100.5(4) ? C18 N10 C9 C2 . . . . 73.5(4) ? C3 C2 C9 N10 . . . . 35.8(5) ? C1 C2 C9 N10 . . . . -147.0(3) ? C13 N12 C11 N10 . . . . 0.0(4) ? C19 N12 C11 N10 . . . . 175.4(3) ? C18 N10 C11 N12 . . . . -0.5(4) ? C9 N10 C11 N12 . . . . 174.4(3) ? C11 N12 C13 C18 . . . . 0.5(4) ? C19 N12 C13 C18 . . . . -174.8(3) ? C11 N12 C13 C14 . . . . -178.0(4) ? C19 N12 C13 C14 . . . . 6.7(6) ? C18 C13 C14 C15 . . . . 1.5(5) ? N12 C13 C14 C15 . . . . 179.8(4) ? C13 C14 C15 C16 . . . . 0.3(6) ? C14 C15 C16 C17 . . . . -1.3(6) ? C15 C16 C17 C18 . . . . 0.3(5) ? C16 C17 C18 C13 . . . . 1.6(5) ? C16 C17 C18 N10 . . . . -179.1(3) ? C14 C13 C18 C17 . . . . -2.6(5) ? N12 C13 C18 C17 . . . . 178.7(3) ? C14 C13 C18 N10 . . . . 178.0(3) ? N12 C13 C18 N10 . . . . -0.7(4) ? C11 N10 C18 C17 . . . . -178.6(4) ? C9 N10 C18 C17 . . . . 6.6(6) ? C11 N10 C18 C13 . . . . 0.7(4) ? C9 N10 C18 C13 . . . . -174.0(3) ? C11 N12 C19 C20 . . . . -83.2(4) ? C13 N12 C19 C20 . . . . 91.4(4) ? N12 C19 C20 C21 . . . . -59.3(5) ? N12 C19 C20 C21' . . . . -126.5(12) ? C19 C20 C21 C22 . . . . -177.9(5) ? C19 C20 C21' C22' . . . . 148.(3) ? C25 N24 C23 C6 . . . . -129.4(3) ? C32 N24 C23 C6 . . . . 61.1(4) ? C5 C6 C23 N24 . . . . 25.5(4) ? C1 C6 C23 N24 . . . . -156.1(3) ? C27 N26 C25 N24 . . . . 0.2(4) ? C33 N26 C25 N24 . . . . 177.5(3) ? C32 N24 C25 N26 . . . . -0.5(4) ? C23 N24 C25 N26 . . . . -171.6(3) ? C25 N26 C27 C28 . . . . 178.5(3) ? C33 N26 C27 C28 . . . . 1.1(6) ? C25 N26 C27 C32 . . . . 0.3(4) ? C33 N26 C27 C32 . . . . -177.1(3) ? C32 C27 C28 C29 . . . . -0.5(5) ? N26 C27 C28 C29 . . . . -178.5(3) ? C27 C28 C29 C30 . . . . 0.4(5) ? C28 C29 C30 C31 . . . . 0.3(5) ? C29 C30 C31 C32 . . . . -0.7(5) ? C28 C27 C32 C31 . . . . 0.0(5) ? N26 C27 C32 C31 . . . . 178.4(3) ? C28 C27 C32 N24 . . . . -179.0(3) ? N26 C27 C32 N24 . . . . -0.6(4) ? C30 C31 C32 C27 . . . . 0.6(5) ? C30 C31 C32 N24 . . . . 179.4(3) ? C25 N24 C32 C27 . . . . 0.7(4) ? C23 N24 C32 C27 . . . . 171.6(3) ? C25 N24 C32 C31 . . . . -178.2(3) ? C23 N24 C32 C31 . . . . -7.3(6) ? C25 N26 C33 C34 . . . . 109.9(4) ? C27 N26 C33 C34 . . . . -73.2(4) ? N26 C33 C34 C35 . . . . -63.0(4) ? C33 C34 C35 C36 . . . . -62.5(4) ? C6A C1A C2A C3A . . . . -1.4(5) ? N7A C1A C2A C3A . . . . 175.3(3) ? C6A C1A C2A C9A . . . . 175.9(3) ? N7A C1A C2A C9A . . . . -7.5(5) ? C1A C2A C3A C4A . . . . -0.8(5) ? C9A C2A C3A C4A . . . . -178.0(3) ? C2A C3A C4A C5A . . . . 2.4(5) ? C3A C4A C5A C6A . . . . -1.9(5) ? C4A C5A C6A C1A . . . . -0.2(5) ? C4A C5A C6A C23A . . . . -179.8(3) ? C2A C1A C6A C5A . . . . 1.9(5) ? N7A C1A C6A C5A . . . . -174.7(3) ? C2A C1A C6A C23A . . . . -178.5(3) ? N7A C1A C6A C23A . . . . 4.8(4) ? C11A N10A C9A C2A . . . . 111.2(4) ? C18A N10A C9A C2A . . . . -75.5(4) ? C3A C2A C9A N10A . . . . -29.9(5) ? C1A C2A C9A N10A . . . . 153.1(3) ? C13A N12A C11A N10A . . . . 0.3(4) ? C19A N12A C11A N10A . . . . -172.0(3) ? C18A N10A C11A N12A . . . . 0.2(4) ? C9A N10A C11A N12A . . . . 174.5(3) ? C11A N12A C13A C14A . . . . 178.0(4) ? C19A N12A C13A C14A . . . . -10.1(6) ? C11A N12A C13A C18A . . . . -0.6(4) ? C19A N12A C13A C18A . . . . 171.3(3) ? N12A C13A C14A C15A . . . . -179.2(4) ? C18A C13A C14A C15A . . . . -0.7(5) ? C13A C14A C15A C16A . . . . -0.8(6) ? C14A C15A C16A C17A . . . . 1.4(6) ? C15A C16A C17A C18A . . . . -0.4(6) ? C16A C17A C18A N10A . . . . 178.7(3) ? C16A C17A C18A C13A . . . . -1.2(5) ? C11A N10A C18A C17A . . . . 179.6(4) ? C9A N10A C18A C17A . . . . 5.4(6) ? C11A N10A C18A C13A . . . . -0.5(4) ? C9A N10A C18A C13A . . . . -174.8(3) ? C14A C13A C18A C17A . . . . 1.8(5) ? N12A C13A C18A C17A . . . . -179.4(3) ? C14A C13A C18A N10A . . . . -178.1(3) ? N12A C13A C18A N10A . . . . 0.7(4) ? C11A N12A C19A C20A . . . . -110.6(4) ? C13A N12A C19A C20A . . . . 78.7(4) ? N12A C19A C20A C21A . . . . 177.3(3) ? C19A C20A C21A C22A . . . . -68.2(4) ? C25A N24A C23A C6A . . . . 125.7(3) ? C32A N24A C23A C6A . . . . -62.9(4) ? C5A C6A C23A N24A . . . . -28.9(4) ? C1A C6A C23A N24A . . . . 151.6(3) ? C32A N24A C25A N26A . . . . 0.2(4) ? C23A N24A C25A N26A . . . . 172.9(3) ? C27A N26A C25A N24A . . . . 0.4(4) ? C33A N26A C25A N24A . . . . 179.9(3) ? C25A N26A C27A C32A . . . . -0.8(4) ? C33A N26A C27A C32A . . . . 179.6(3) ? C25A N26A C27A C28A . . . . -178.6(4) ? C33A N26A C27A C28A . . . . 1.8(6) ? C32A C27A C28A C29A . . . . 0.8(5) ? N26A C27A C28A C29A . . . . 178.4(3) ? C27A C28A C29A C30A . . . . -1.4(5) ? C28A C29A C30A C31A . . . . 1.1(6) ? C29A C30A C31A C32A . . . . -0.1(5) ? C30A C31A C32A C27A . . . . -0.5(5) ? C30A C31A C32A N24A . . . . -179.0(3) ? N26A C27A C32A C31A . . . . -177.9(3) ? C28A C27A C32A C31A . . . . 0.2(5) ? N26A C27A C32A N24A . . . . 0.9(4) ? C28A C27A C32A N24A . . . . 179.0(3) ? C25A N24A C32A C31A . . . . 177.9(4) ? C23A N24A C32A C31A . . . . 5.2(6) ? C25A N24A C32A C27A . . . . -0.7(4) ? C23A N24A C32A C27A . . . . -173.4(3) ? C25A N26A C33A C34A . . . . -104.8(4) ? C27A N26A C33A C34A . . . . 74.7(4) ? N26A C33A C34A C35A . . . . 63.0(4) ? C33A C34A C35A C36A . . . . 66.4(4) ?