#------------------------------------------------------------------------------ #$Date: 2022-02-04 21:30:26 +0200 (Fri, 04 Feb 2022) $ #$Revision: 272646 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/88/7708874.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_7708874 loop_ _publ_author_name 'Nakamura, Masashi' 'Gon, Masayuki' 'Natsuda, Shin-Ichiro' 'Tamai, Yasunari' 'Ohkita, Hideo' 'Tanaka, Kazuo' 'Chujo, Yoshiki' _publ_section_title ; Development of NIR emissive fully-fused bisboron complexes with \p-conjugated systems including multiple azo groups. ; _journal_issue 1 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 74 _journal_page_last 84 _journal_paper_doi 10.1039/d1dt03652a _journal_volume 51 _journal_year 2021 _chemical_formula_moiety 'C44 H50 B2 F2 N4 O4' _chemical_formula_sum 'C44 H50 B2 F2 N4 O4' _chemical_formula_weight 758.50 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2021-11-14 deposited with the CCDC. 2021-11-17 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 96.077(11) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 7.656(6) _cell_length_b 21.051(15) _cell_length_c 12.118(9) _cell_measurement_reflns_used 3173 _cell_measurement_temperature 143(2) _cell_measurement_theta_max 27.5 _cell_measurement_theta_min 3.0 _cell_volume 1942(3) _computing_cell_refinement 'CrystalClear-SM Expert 2.1 b46 (Rigaku, 2016)' _computing_data_collection 'CrystalClear-SM Expert 2.1 b46 (Rigaku, 2016)' _computing_data_reduction 'CrystalClear-SM Expert 2.1 b46 (Rigaku, 2016)' _computing_molecular_graphics 'Yadokari-XG (Wakita, 2000)' _computing_publication_material 'Yadokari-XG (Wakita, 2000)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT-2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 143(2) _diffrn_detector_area_resol_mean 28.5714 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measurement_device_type 'Rigaku Saturn724+ (4x4 bin mode)' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71075 _diffrn_reflns_av_R_equivalents 0.1255 _diffrn_reflns_av_unetI/netI 0.1864 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.989 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 15609 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.989 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.498 _diffrn_reflns_theta_min 3.162 _exptl_absorpt_coefficient_mu 0.089 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.864 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(REQAB; Rigaku, 1998)' _exptl_crystal_colour Blue _exptl_crystal_density_diffrn 1.297 _exptl_crystal_description Plate _exptl_crystal_F_000 804 _exptl_crystal_preparation Luminescent _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.110 _exptl_crystal_size_min 0.040 _refine_diff_density_max 0.188 _refine_diff_density_min -0.205 _refine_diff_density_rms 0.045 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.905 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 362 _refine_ls_number_reflns 4407 _refine_ls_number_restraints 232 _refine_ls_restrained_S_all 0.892 _refine_ls_R_factor_all 0.1594 _refine_ls_R_factor_gt 0.0608 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0181P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0809 _refine_ls_wR_factor_ref 0.0981 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2145 _reflns_number_total 4407 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt03652a2.cif _cod_data_source_block anti-B2b _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 7556 2019-12-06 15:28:31Z antanas Adding full bibliography for 7708873--7708874.cif. ; _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 7708874 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.982 _shelx_estimated_absorpt_t_max 0.996 _shelx_res_file ; TITL anti-B2b anti-B2b.res created by SHELXL-2018/3 at 01:08:56 on 12-Nov-2021 REM Yadorkari-X generated CELL 0.71075 7.6560 21.0510 12.1180 90.0000 96.0770 90.0000 ZERR 2.0 0.0060 0.0150 0.0090 0.0000 0.0110 0.0000 LATT 1 SYMM 1/2-X, 1/2+Y, 1/2-Z REM SPGR P21/n monoclinic SFAC C H N O B F UNIT 88 100 8 8 4 4 SIZE 0.11 0.20 0.04 TEMP -130.0 L.S. 50 FMAP 2 PLAN -40 ACTA CONF LIST 4 BOND $H MERG 2 OMIT -10.000000 55.000000 SADI 0.02 C4A C5A C4B C5B SADI 0.02 C4A C13A C4B C13B SADI 0.02 C4A N2A C4B N2B SADI 0.02 C5A C6A C5B C6B SADI 0.02 C5A O2A C5B O2B SADI 0.02 C6A C7A C6B C7B SADI 0.02 C7A C8A C7B C8B SADI 0.02 C8A C9A C8B C9B SADI 0.02 C8A C13A C8B C13B SADI 0.02 C9A C10A C9B C10B SADI 0.02 C12A C13A C12B C13B SADI 0.02 O2A B1 O2B B1 SADI 0.04 C4A C6A C4B C6B SADI 0.04 C4A C8A C4B C8B SADI 0.04 C4A C12A C4B C12B SADI 0.04 C4A N1 C4B N1 SADI 0.04 C4A O2A C4B O2B SADI 0.04 C5A C7A C5B C7B SADI 0.04 C5A C13A C5B C13B SADI 0.04 C5A N2A C5B N2B SADI 0.04 C5A B1 C5B B1 SADI 0.04 C6A C8A C6B C8B SADI 0.04 C6A O2A C6B O2B SADI 0.04 C7A C9A C7B C9B SADI 0.04 C7A C13A C7B C13B SADI 0.04 C8A C10A C8B C10B SADI 0.04 C8A C12A C8B C12B SADI 0.04 C9A C11A C9B C11B SADI 0.04 C9A C13A C9B C13B SADI 0.04 C10A C12A C10B C12B SADI 0.04 C11A C13A C11B C13B SADI 0.04 C13A N2A C13B N2B RIGU 0.004 0.004 N2A C4A > C13A O2A RIGU 0.004 0.004 N2B C4B > C13B O2B SADI 0.02 N1 N2A N1 N2B ISOR 0.005 N2A N2B SADI 0.01 N1 N2A N1 N2B WGHT 0.018100 FVAR 4.00733 0.56065 C1 1 0.589574 0.485706 0.410564 11.00000 0.02053 0.02434 = 0.01341 -0.00204 0.00445 -0.00261 C2 1 0.606034 0.443912 0.501271 11.00000 0.02201 0.01706 = 0.01687 -0.00040 0.00259 -0.00339 C3 1 0.485929 0.540244 0.410160 11.00000 0.02228 0.02675 = 0.01884 0.00458 0.00017 -0.00152 AFIX 43 H13 2 0.478188 0.567360 0.347165 11.00000 -1.20000 PART 1 AFIX 0 C4A 1 0.719681 0.494505 0.139134 21.00000 0.01394 0.03290 = 0.01704 -0.00620 0.00766 0.00461 C5A 1 0.801738 0.436040 0.129965 21.00000 0.01799 0.02854 = 0.02520 -0.00564 0.00638 0.00150 C6A 1 0.852783 0.416944 0.023983 21.00000 0.04002 0.02972 = 0.03898 -0.01954 0.01482 -0.00774 AFIX 43 H1 2 0.905782 0.376658 0.015713 21.00000 -1.20000 AFIX 0 C7A 1 0.824487 0.457227 -0.064982 21.00000 0.02856 0.05358 = 0.01883 -0.01747 0.00947 -0.01530 AFIX 43 H2 2 0.857359 0.443476 -0.134539 21.00000 -1.20000 AFIX 0 C8A 1 0.748964 0.518119 -0.058482 21.00000 0.02270 0.05138 = 0.02071 -0.00921 -0.00272 -0.01196 C9A 1 0.729192 0.559143 -0.151184 21.00000 0.03232 0.07859 = 0.01389 0.00262 0.00534 -0.00959 AFIX 43 H3 2 0.765934 0.546297 -0.220246 21.00000 -1.20000 AFIX 0 C10A 1 0.656437 0.617466 -0.139627 21.00000 0.03736 0.07131 = 0.01987 0.01273 -0.00025 -0.01144 AFIX 43 H4 2 0.642258 0.645238 -0.201724 21.00000 -1.20000 AFIX 0 C11A 1 0.601925 0.637586 -0.038478 21.00000 0.04089 0.05871 = 0.02227 0.01317 -0.00069 -0.01241 AFIX 43 H5 2 0.553518 0.678868 -0.032873 21.00000 -1.20000 AFIX 0 C12A 1 0.617557 0.598453 0.052511 21.00000 0.02593 0.04552 = 0.02572 0.00690 0.00298 0.00112 AFIX 43 H6 2 0.574922 0.611612 0.119702 21.00000 -1.20000 PART 2 AFIX 0 C4B 1 0.749582 0.478574 0.140461 -21.00000 0.00760 0.03048 = 0.01152 -0.00627 0.00257 0.00505 C6B 1 0.878061 0.393486 0.039372 -21.00000 0.02092 0.02924 = 0.02888 -0.01281 0.00984 -0.00585 AFIX 43 H7 2 0.925484 0.351887 0.036520 -21.00000 -1.20000 AFIX 0 C7B 1 0.854059 0.430171 -0.053040 -21.00000 0.02072 0.03993 = 0.02634 -0.01256 0.01092 -0.00369 AFIX 43 H8 2 0.890368 0.413641 -0.119901 -21.00000 -1.20000 AFIX 0 C12B 1 0.647252 0.577665 0.039488 -21.00000 0.02084 0.03740 = 0.01359 -0.00050 0.00392 -0.00029 AFIX 43 H9 2 0.612262 0.595337 0.105851 -21.00000 -1.20000 PART 1 AFIX 0 C13A 1 0.697592 0.538470 0.045282 21.00000 0.02431 0.03149 = 0.01431 -0.00673 0.00688 -0.01226 PART 2 O2B 4 0.859186 0.383948 0.229993 -21.00000 0.01260 0.03366 = 0.02821 -0.00693 -0.00064 0.00970 C5B 1 0.830466 0.418905 0.140287 -21.00000 0.00638 0.02638 = 0.02511 -0.01285 0.00384 0.00022 C8B 1 0.777982 0.491773 -0.055982 -21.00000 0.01843 0.03140 = 0.01731 -0.00699 0.00652 -0.00831 C9B 1 0.763184 0.528316 -0.152790 -21.00000 0.02393 0.05671 = 0.01803 0.00177 -0.00496 -0.01175 AFIX 43 H10 2 0.802662 0.511573 -0.218595 -21.00000 -1.20000 AFIX 0 C10B 1 0.692507 0.587851 -0.153611 -21.00000 0.02362 0.05522 = 0.02063 0.00661 -0.00450 -0.00630 AFIX 43 H11 2 0.685867 0.612465 -0.219631 -21.00000 -1.20000 AFIX 0 C11B 1 0.629707 0.613149 -0.058642 -21.00000 0.03603 0.04675 = 0.02282 0.00577 -0.00189 -0.00244 AFIX 43 H12 2 0.575896 0.653857 -0.060761 -21.00000 -1.20000 AFIX 0 C13B 1 0.716331 0.516156 0.039861 -21.00000 0.01883 0.02465 = 0.01967 -0.00859 -0.00086 -0.00646 PART 0 C14 1 0.712638 0.382342 0.505135 11.00000 0.02611 0.01974 = 0.02967 0.00124 0.00248 -0.00131 C15 1 0.864287 0.388389 0.598175 11.00000 0.02568 0.02754 = 0.03363 0.00081 -0.00042 0.00128 AFIX 23 H14 2 0.939018 0.424626 0.580645 11.00000 -1.20000 H15 2 0.814259 0.398670 0.668092 11.00000 -1.20000 AFIX 0 C16 1 0.980388 0.329900 0.617794 11.00000 0.03026 0.02999 = 0.03934 0.00415 0.00530 0.00657 AFIX 23 H16 2 0.906954 0.293314 0.635391 11.00000 -1.20000 H17 2 1.033340 0.319744 0.548835 11.00000 -1.20000 AFIX 0 C17 1 1.125282 0.339196 0.711361 11.00000 0.03854 0.04220 = 0.05278 0.01164 -0.00274 0.01029 AFIX 23 H18 2 1.073484 0.356445 0.776581 11.00000 -1.20000 H19 2 1.209141 0.371114 0.688257 11.00000 -1.20000 AFIX 0 C18 1 1.225469 0.278719 0.745651 11.00000 0.04579 0.06667 = 0.04736 0.01584 0.00781 0.02732 AFIX 33 H20 2 1.316825 0.288213 0.806297 11.00000 -1.50000 H21 2 1.144150 0.247149 0.770587 11.00000 -1.50000 H22 2 1.279970 0.261835 0.682158 11.00000 -1.50000 AFIX 0 C19 1 0.593170 0.325676 0.523717 11.00000 0.03023 0.02221 = 0.04208 0.00033 0.00470 -0.00163 AFIX 23 H23 2 0.662360 0.286042 0.521668 11.00000 -1.20000 H24 2 0.553292 0.329199 0.598569 11.00000 -1.20000 AFIX 0 C20 1 0.432383 0.320912 0.438126 11.00000 0.03310 0.03200 = 0.04598 -0.00693 0.00402 -0.00695 AFIX 23 H25 2 0.343851 0.352404 0.456454 11.00000 -1.20000 H26 2 0.467235 0.331772 0.364044 11.00000 -1.20000 AFIX 0 C21 1 0.349418 0.255101 0.433145 11.00000 0.04953 0.04028 = 0.05111 -0.01588 0.02356 -0.01915 AFIX 23 H27 2 0.438858 0.223550 0.416478 11.00000 -1.20000 H28 2 0.312571 0.244654 0.506899 11.00000 -1.20000 AFIX 0 C22 1 0.191755 0.249469 0.346743 11.00000 0.04804 0.07807 = 0.07536 -0.03884 0.01180 -0.03350 AFIX 33 H29 2 0.144462 0.206232 0.347590 11.00000 -1.50000 H30 2 0.101266 0.279828 0.363647 11.00000 -1.50000 H31 2 0.227651 0.258707 0.273157 11.00000 -1.50000 AFIX 0 N1 3 0.685200 0.471421 0.319109 11.00000 0.02660 0.02902 = 0.01872 -0.00309 0.00429 -0.00645 PART 2 N2B 3 0.662460 0.501111 0.224683 -21.00000 0.01842 0.02437 = 0.02021 -0.01020 0.00374 -0.00197 PART 1 N2A 3 0.645947 0.510533 0.235516 21.00000 0.02333 0.04004 = 0.00867 -0.00647 0.00935 -0.00787 PART 0 O1 4 0.780399 0.369331 0.402038 11.00000 0.03147 0.02550 = 0.03433 -0.00689 0.01200 -0.00127 PART 1 O2A 4 0.823084 0.395680 0.214062 21.00000 0.01895 0.02991 = 0.02921 -0.00633 0.00439 0.00776 PART 0 B1 5 0.830983 0.417653 0.332112 11.00000 0.02472 0.03019 = 0.03456 -0.00999 0.01188 -0.00513 F1 6 0.987640 0.448729 0.365831 11.00000 0.02344 0.03841 = 0.04432 -0.00747 0.00616 -0.00523 HKLF 4 REM anti-B2b REM wR2 = 0.0981, GooF = S = 0.905, Restrained GooF = 0.892 for all data REM R1 = 0.0608 for 2145 Fo > 4sig(Fo) and 0.1594 for all 4407 data REM 362 parameters refined using 232 restraints END WGHT 0.0181 0.0000 REM Highest difference peak 0.188, deepest hole -0.205, 1-sigma level 0.045 Q1 1 0.6814 0.4187 0.5067 11.00000 0.05 0.19 Q2 1 0.6561 0.4783 0.2751 11.00000 0.05 0.18 Q3 1 0.4989 0.4962 0.4021 11.00000 0.05 0.17 Q4 1 1.1582 0.4002 0.7450 11.00000 0.05 0.17 Q5 1 0.9109 0.5519 -0.2169 11.00000 0.05 0.17 Q6 1 0.4920 0.6489 0.1712 11.00000 0.05 0.16 Q7 1 0.6064 0.4632 0.4634 11.00000 0.05 0.16 Q8 1 1.0541 0.3759 0.0619 11.00000 0.05 0.16 Q9 1 0.2667 0.2458 0.3923 11.00000 0.05 0.16 Q10 1 0.7873 0.3937 0.3627 11.00000 0.05 0.16 Q11 1 1.0797 0.2293 0.7247 11.00000 0.05 0.16 Q12 1 0.5652 0.5003 -0.0208 11.00000 0.05 0.15 Q13 1 0.6885 0.5366 0.4794 11.00000 0.05 0.15 Q14 1 0.8829 0.5555 0.0220 11.00000 0.05 0.15 Q15 1 0.6984 0.5071 0.0838 11.00000 0.05 0.15 Q16 1 0.5077 0.4791 0.1710 11.00000 0.05 0.15 Q17 1 0.3881 0.2947 0.4259 11.00000 0.05 0.15 Q18 1 0.8517 0.4906 -0.0568 11.00000 0.05 0.15 Q19 1 0.3307 0.3654 0.3979 11.00000 0.05 0.15 Q20 1 0.5169 0.3320 0.4886 11.00000 0.05 0.15 Q21 1 1.2634 0.2669 0.8195 11.00000 0.05 0.15 Q22 1 0.5851 0.5018 0.2286 11.00000 0.05 0.14 Q23 1 0.9954 0.5011 0.3592 11.00000 0.05 0.14 Q24 1 0.9461 0.5199 0.1745 11.00000 0.05 0.13 Q25 1 0.8798 0.5111 0.2379 11.00000 0.05 0.13 Q26 1 0.4898 0.5558 0.3653 11.00000 0.05 0.13 Q27 1 0.7996 0.2917 0.6467 11.00000 0.05 0.13 Q28 1 0.6342 0.4865 0.3810 11.00000 0.05 0.13 Q29 1 0.3677 0.4783 0.4307 11.00000 0.05 0.13 Q30 1 0.5663 0.4361 0.3809 11.00000 0.05 0.13 Q31 1 0.8463 0.5014 0.5020 11.00000 0.05 0.13 Q32 1 0.4598 0.6141 0.0654 11.00000 0.05 0.13 Q33 1 0.8986 0.3477 0.2287 11.00000 0.05 0.13 Q34 1 0.6203 0.4794 0.4923 11.00000 0.05 0.13 Q35 1 0.5648 0.5775 0.2017 11.00000 0.05 0.13 Q36 1 0.8063 0.3597 0.6614 11.00000 0.05 0.13 Q37 1 0.6293 0.3629 0.5230 11.00000 0.05 0.13 Q38 1 0.9015 0.3995 0.6183 11.00000 0.05 0.13 Q39 1 0.6107 0.3480 0.3024 11.00000 0.05 0.13 Q40 1 0.6283 0.2735 0.4452 11.00000 0.05 0.13 ; _shelx_res_checksum 79310 _shelx_hkl_file ; 0 0 2100751.9 2975.94 0 0 -297190.67 2824.01 0 0 2103997.6 2926.21 0 0 -297927.08 2755.58 0 0 3 -645.05 699.52 0 0 -3 -542.65 362.45 0 0 -3 -73.30 38.21 0 0 -3 10.18 26.21 0 0 420159.72 1421.29 0 0 -416718.35 735.62 0 0 -418355.30 525.87 0 0 -418720.81 545.12 0 0 5 385.14 532.30 0 0 -5 296.77 199.83 0 0 -5 -17.94 36.08 0 0 -5 -58.88 63.95 0 0 6 3197.16 1336.84 0 0 -6 2638.73 917.73 0 0 -6 2519.23 764.38 0 0 -6 2732.13 834.52 0 0 -7 -807.18 1121.24 0 0 -7 10.61 32.01 0 0 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602.41 1697.20 0 11 4 1282.48 178.90 0 11 -4 1435.23 484.91 0 11 -5 124.01 1609.98 0 11 5 498.32 100.48 0 11 -6 -44.67 1985.94 0 11 6 261.90 116.00 0 11 -6 -0.98 77.61 0 -11 -7 99.04 83.85 0 -11 -7 422.20 206.68 0 11 -7-2791.46 2164.57 0 11 7 122.37 62.22 0 11 -7 229.21 104.09 0 -11 -8 1383.31 586.26 0 -11 -8 1219.67 614.70 0 11 -8 4237.22 2028.79 0 11 8 387.37 152.99 0 11 -8 184.24 101.68 0 -11 -9 1226.29 834.02 0 11 -9 7112.15 3088.73 0 11 9 2549.94 1075.30 0 11 -9 2997.09 1235.59 0 11 10 132.63 108.58 0 11 -10 -68.79 78.28 0 11 -11 110.50 2181.63 0 11 11 -102.20 86.31 0 11 -11 85.25 77.14 0 11 -12 5059.96 4214.54 0 11 12 1935.51 1328.11 0 11 -12 2433.65 1360.97 0 11 -13 6318.98 4806.28 0 11 13 847.67 380.17 0 11 -14 1102.71 1751.28 0 12 0 701.79 317.49 0 12 0 -446.60 862.89 0 12 0 940.83 123.06 0 12 -1 2299.44 819.65 0 12 1 3147.08 1187.32 0 12 1 2581.69 1354.33 0 12 -1 2026.03 1115.82 0 12 1 2471.67 801.96 0 12 -1 3127.46 1008.10 0 12 2 1127.24 337.23 0 12 2 606.37 404.60 0 12 -2 648.35 1142.09 0 12 2 708.97 105.35 0 12 -2 731.75 114.23 0 12 3 9388.23 1038.09 0 12 310677.41 830.75 0 12 -311526.46 2195.01 0 12 310320.02 604.71 0 12 -310434.94 604.14 0 12 4 263.25 82.21 0 12 -4 4355.67 1644.19 0 12 4 734.23 135.59 0 12 -4 838.62 154.74 0 12 -5 269.89 1671.51 0 12 5 1102.00 488.23 0 12 -6-3168.40 2033.75 0 12 6 833.55 315.50 0 12 -6 903.17 361.56 0 12 -7 5202.32 2970.44 0 12 7 1861.19 802.22 0 12 -7 2396.96 1033.85 0 12 8 1134.84 382.04 0 12 -8 1456.85 484.73 0 12 -9 746.87 2194.45 0 12 9 903.66 513.90 0 12 -9 707.09 408.91 0 12 -10 -203.63 2058.98 0 12 10 3153.33 328.38 0 12 -10 3203.80 398.90 0 12 -11 7326.79 3440.90 0 12 11 1592.67 992.03 0 12 -11 1516.28 900.00 0 12 -12 2267.36 2932.26 0 12 12 1599.26 873.70 0 12 -12 2135.65 1431.62 0 12 -13-3879.69 2228.72 0 12 -14 1798.06 2068.44 0 12 14 107.96 90.65 0 13 0 404.82 179.36 0 13 0 157.65 82.00 0 13 114699.97 1353.84 0 13 112203.11 1171.15 0 13 -111680.25 1766.04 0 13 114455.61 824.32 0 13 -115840.51 892.57 0 13 2 1828.97 637.49 0 13 2 1596.65 711.67 0 13 -2 4803.94 1880.76 0 13 2 2355.29 753.44 0 13 -2 2304.20 741.83 0 13 3 212.31 155.73 0 13 3 406.47 167.91 0 13 -3 2251.36 1672.15 0 13 3 740.11 118.93 0 13 -3 460.83 81.71 0 13 4 279.40 124.59 0 13 -4 1128.87 1594.03 0 13 4 201.33 95.34 0 13 -4 377.72 150.47 0 13 -5-1303.23 1769.23 0 13 5 1093.10 486.41 0 13 -6 9287.50 2191.95 0 13 6 4222.37 421.55 0 13 -6 4248.25 358.88 0 13 -712636.77 3195.52 0 13 7 4105.57 469.70 0 13 -7 4656.60 656.52 0 13 -8 -746.36 1867.44 0 13 8 392.17 216.15 0 13 -8 149.86 108.10 0 13 -9 1718.58 2350.20 0 13 9 1256.34 694.20 0 13 -9 854.75 538.00 0 13 -10 3613.17 2444.43 0 13 10 3865.32 1286.18 0 13 -10 3561.75 1213.38 0 13 -11 -207.63 2368.75 0 13 11 470.93 128.45 0 13 -11 523.49 182.87 0 13 -12 5078.55 3509.39 0 13 12 370.67 190.30 0 13 -12 264.76 87.12 0 13 -13 5536.41 4273.28 0 13 13 260.55 163.81 0 14 016545.78 1844.63 0 14 027912.91 2580.84 0 14 022099.43 1359.01 0 14 1 1953.20 771.59 0 14 1 1358.60 1030.87 0 14 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1520.65 0 22 0 28.79 78.25 0 22 1 943.43 729.35 0 22 -1 2213.34 1000.43 0 22 1 328.58 242.52 0 22 -1 13.22 103.95 0 22 -2 2068.88 1708.59 0 22 2 149.31 67.51 0 22 -2 341.17 54.76 0 22 -3 852.30 1640.07 0 22 3 1546.70 921.16 0 22 -3 1358.77 835.07 0 22 -4 3150.14 2479.80 0 22 4 486.26 152.02 0 22 -5 4341.65 3404.50 0 22 5 -1.50 116.57 0 22 -5 434.20 118.17 0 22 -6 6092.92 4743.96 0 22 6 534.45 132.72 0 22 -6 510.90 119.48 0 22 -7 -639.27 2026.27 0 22 7 -0.44 99.84 0 22 -7 546.57 212.69 0 22 -8 1898.84 2475.31 0 22 8 169.42 107.73 0 22 -8 102.69 89.00 0 22 -9 4171.13 3500.54 0 22 9 137.82 114.14 0 22 -9 120.23 86.31 0 23 0 1728.89 1291.20 0 23 0 164.46 133.35 0 23 -1 3287.13 2279.46 0 23 1 1405.49 837.21 0 23 -1 1313.43 758.95 0 23 -2 5415.88 3410.10 0 23 2 977.54 550.88 0 23 -2 723.11 240.16 0 23 -3 985.23 1588.24 0 23 3 289.29 227.78 0 23 -3 123.89 132.48 0 23 -4-1838.99 1780.93 0 23 4 787.96 224.80 0 23 -4 884.81 477.08 0 23 -5 6111.45 4020.89 0 23 5 230.56 173.20 0 23 -5 1062.53 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312.96 389.83 9 -6 -4 598.59 434.86 9 6 -4 699.46 441.34 9 -6 -3 1004.73 462.73 9 6 -3 1018.36 708.86 -9 6 3 472.23 186.01 9 -6 -2 -60.53 268.49 9 6 -2 417.23 613.76 -9 6 2 -7.46 92.30 -9 -6 2 278.06 155.34 9 -6 -1 197.81 279.26 9 6 -1 716.87 562.48 -9 6 1 392.12 212.60 -9 -6 1 120.77 87.66 9 -6 0 -539.76 502.88 9 6 0 -455.58 611.36 -9 6 0 197.67 97.43 -9 -6 0 145.93 112.44 9 -6 1 -699.58 475.56 9 6 1 339.86 485.95 -9 6 -1 64.47 94.53 -9 -6 -1 160.42 84.77 9 -6 2 2895.07 2159.99 9 6 2 976.75 489.15 -9 6 -2 546.11 363.15 -9 -6 -2 792.56 379.74 9 -6 3 -870.44 623.30 9 6 3 400.69 351.40 -9 6 -3 551.87 302.86 -9 -6 -3 -172.56 145.84 9 -6 4 0.25 357.12 9 6 4 1022.14 621.21 -9 6 -4 59.65 95.62 -9 -6 -4 207.34 194.32 9 -7 -6 199.92 270.70 9 7 -6 1075.15 842.08 9 -7 -5 524.56 260.96 9 7 -5 1379.37 993.80 9 -7 -4 -57.29 347.71 9 7 -4 631.35 496.38 9 -7 -3 387.06 520.53 9 7 -3 1393.42 979.87 9 -7 -2 1790.21 1127.23 9 7 -2 646.97 707.36 -9 7 2 759.14 354.36 -9 -7 2 914.70 415.61 9 -7 -1 535.52 291.95 9 7 -1 227.53 451.91 -9 7 1 649.97 297.71 -9 -7 1 287.84 176.35 9 -7 0 2071.53 1392.57 9 7 0 1365.73 902.94 -9 7 0 1110.54 653.01 -9 -7 0 1016.27 447.58 9 -7 1 1724.57 1189.28 9 7 1 -258.29 503.21 -9 7 -1 710.85 401.02 -9 -7 -1 872.87 415.67 9 -7 2 2407.06 1760.89 9 7 2 451.88 347.22 -9 7 -2 65.91 130.48 -9 -7 -2 674.49 417.24 9 -7 3 2006.04 1559.77 9 7 3 1205.09 862.65 -9 7 -3 438.91 218.54 -9 -7 -3 105.60 147.10 9 -8 -6 617.62 428.68 9 8 -6 -934.22 706.08 9 -8 -5 344.07 311.34 9 8 -5 1643.65 966.44 9 -8 -4 808.99 583.75 9 8 -4 690.78 383.40 9 -8 -3 450.19 342.57 9 8 -3 54.81 498.54 -9 8 3 491.96 199.47 9 -8 -2 146.89 435.24 9 8 -2 -98.93 632.53 -9 8 2 54.12 94.77 -9 -8 2 199.36 152.60 9 -8 -1 912.76 670.99 -9 8 1 -36.94 117.41 -9 -8 1 179.54 131.48 9 -8 0 938.33 673.22 9 8 0 481.51 492.15 -9 8 0 174.53 148.10 -9 -8 0 46.01 84.17 9 -8 1 -15.28 502.54 9 8 1 -51.63 498.00 -9 8 -1 -46.11 132.07 -9 -8 -1 129.29 89.41 9 -8 2 1575.33 1177.61 9 8 2 1274.79 800.29 -9 8 -2 780.24 330.56 -9 -8 -2 461.11 217.02 9 -8 3 2470.25 1712.36 9 8 3 1625.68 1127.31 -9 8 -3 1123.24 652.77 -9 -8 -3 859.11 368.67 9 -9 -5 1068.58 577.82 9 9 -5 969.98 621.03 9 -9 -4 480.53 344.14 9 9 -4-1769.21 681.57 9 9 -3 -480.08 602.72 -9 9 3 101.26 72.34 9 -9 -2 266.13 327.20 9 9 -2 298.88 608.90 -9 9 2 780.28 354.77 9 -9 -1 963.60 719.30 9 9 -1 1761.50 1390.21 -9 9 1 1449.25 915.07 -9 -9 1 1171.36 551.71 9 -9 0 622.02 314.03 9 9 0 86.39 507.90 -9 9 0 751.63 375.88 -9 -9 0 152.63 145.00 9 -9 1 1375.22 916.42 9 9 1 996.01 468.22 -9 9 -1 197.73 130.76 -9 -9 -1 215.31 168.44 9 -9 2 3630.56 2644.19 9 9 2 875.49 688.64 -9 9 -2 1344.81 753.13 -9 -9 -2 1352.19 824.82 9 -10 -4 727.70 408.28 9 10 -4 1353.07 1112.40 9 -10 -3 1127.93 728.91 9 10 -3 176.32 372.54 -9 10 3 105.09 92.07 9 -10 -2 965.14 497.78 9 10 -2 1240.77 779.65 -9 10 2 -64.43 91.89 9 -10 -1 320.21 560.14 9 10 -1 1139.59 745.11 -9 10 1 -62.02 105.14 -9 -10 1 -52.90 61.97 9 -10 0 252.54 430.36 9 10 0 -972.22 543.92 -9 10 0 410.66 201.56 -9 -10 0 300.40 232.39 9 -10 1 1692.80 1093.68 9 10 1 35.10 507.30 -9 10 -1 271.32 196.58 -9 -10 -1 850.36 349.20 9 -11 -3 664.02 548.09 9 11 -3 809.95 642.35 -9 11 3 116.88 106.64 9 -11 -2 479.93 309.73 9 11 -2 894.66 513.99 -9 11 2 -62.53 85.92 9 -11 -1 -318.51 578.71 9 11 -1 1614.15 954.91 -9 11 1 183.82 121.47 -9 -11 1 59.99 58.31 9 11 0 894.09 625.92 -9 11 0 523.36 262.94 -9 -11 0 121.39 84.32 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 16967 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -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 C1 C 0.5896(2) 0.48571(10) 0.41056(17) 0.0192(5) Uani 1 1 d . . . . . C2 C 0.6060(2) 0.44391(10) 0.50127(18) 0.0186(5) Uani 1 1 d . . . . . C3 C 0.4859(2) 0.54024(10) 0.41016(18) 0.0228(5) Uani 1 1 d . . . . . H13 H 0.478188 0.567360 0.347165 0.027 Uiso 1 1 calc R U . . . C4A C 0.720(2) 0.4945(6) 0.1391(8) 0.0209(19) Uani 0.56(2) 1 d D . P A 1 C5A C 0.8017(18) 0.4360(6) 0.1300(7) 0.0236(19) Uani 0.56(2) 1 d D . P A 1 C6A C 0.8528(15) 0.4169(5) 0.0240(8) 0.035(2) Uani 0.56(2) 1 d D . P A 1 H1 H 0.905782 0.376658 0.015713 0.043 Uiso 0.56(2) 1 calc R U P A 1 C7A C 0.8245(13) 0.4572(6) -0.0650(7) 0.033(2) Uani 0.56(2) 1 d D . P A 1 H2 H 0.857359 0.443476 -0.134539 0.040 Uiso 0.56(2) 1 calc R U P A 1 C8A C 0.7490(14) 0.5181(7) -0.0585(6) 0.032(2) Uani 0.56(2) 1 d D . P A 1 C9A C 0.7292(13) 0.5591(8) -0.1512(7) 0.041(3) Uani 0.56(2) 1 d D . P A 1 H3 H 0.765934 0.546297 -0.220246 0.050 Uiso 0.56(2) 1 calc R U P A 1 C10A C 0.6564(14) 0.6175(7) -0.1396(7) 0.043(2) Uani 0.56(2) 1 d D . P A 1 H4 H 0.642258 0.645238 -0.201724 0.052 Uiso 0.56(2) 1 calc R U P A 1 C11A C 0.6019(16) 0.6376(6) -0.0385(9) 0.041(2) Uani 0.56(2) 1 d D . P A 1 H5 H 0.553518 0.678868 -0.032873 0.049 Uiso 0.56(2) 1 calc R U P A 1 C12A C 0.6176(18) 0.5985(6) 0.0525(9) 0.032(2) Uani 0.56(2) 1 d D . P A 1 H6 H 0.574922 0.611612 0.119702 0.039 Uiso 0.56(2) 1 calc R U P A 1 C4B C 0.750(2) 0.4786(7) 0.1405(9) 0.016(2) Uani 0.44(2) 1 d D . P A 2 C6B C 0.8781(16) 0.3935(7) 0.0394(9) 0.026(2) Uani 0.44(2) 1 d D . P A 2 H7 H 0.925484 0.351887 0.036520 0.031 Uiso 0.44(2) 1 calc R U P A 2 C7B C 0.8541(17) 0.4302(7) -0.0530(10) 0.028(2) Uani 0.44(2) 1 d D . P A 2 H8 H 0.890368 0.413641 -0.119901 0.034 Uiso 0.44(2) 1 calc R U P A 2 C12B C 0.647(2) 0.5777(7) 0.0395(10) 0.024(2) Uani 0.44(2) 1 d D . P A 2 H9 H 0.612262 0.595337 0.105851 0.029 Uiso 0.44(2) 1 calc R U P A 2 C13A C 0.6976(15) 0.5385(6) 0.0453(6) 0.0230(19) Uani 0.56(2) 1 d D . P A 1 O2B O 0.8592(17) 0.3839(6) 0.2300(8) 0.0250(19) Uani 0.44(2) 1 d D . P A 2 C5B C 0.830(2) 0.4189(7) 0.1403(9) 0.019(2) Uani 0.44(2) 1 d D . P A 2 C8B C 0.7780(15) 0.4918(6) -0.0560(7) 0.022(2) Uani 0.44(2) 1 d D . P A 2 C9B C 0.7632(17) 0.5283(8) -0.1528(8) 0.033(2) Uani 0.44(2) 1 d D . P A 2 H10 H 0.802662 0.511573 -0.218595 0.040 Uiso 0.44(2) 1 calc R U P A 2 C10B C 0.6925(17) 0.5879(8) -0.1536(10) 0.034(3) Uani 0.44(2) 1 d D . P A 2 H11 H 0.685867 0.612465 -0.219631 0.040 Uiso 0.44(2) 1 calc R U P A 2 C11B C 0.6297(19) 0.6131(7) -0.0586(11) 0.036(3) Uani 0.44(2) 1 d D . P A 2 H12 H 0.575896 0.653857 -0.060761 0.043 Uiso 0.44(2) 1 calc R U P A 2 C13B C 0.716(2) 0.5162(6) 0.0399(8) 0.021(2) Uani 0.44(2) 1 d D . P A 2 C14 C 0.7126(3) 0.38234(10) 0.5051(2) 0.0252(6) Uani 1 1 d . . . . . C15 C 0.8643(3) 0.38839(10) 0.59817(19) 0.0292(6) Uani 1 1 d . . . . . H14 H 0.939018 0.424626 0.580645 0.035 Uiso 1 1 calc R U . . . H15 H 0.814259 0.398670 0.668092 0.035 Uiso 1 1 calc R U . . . C16 C 0.9804(3) 0.32990(11) 0.6178(2) 0.0331(6) Uani 1 1 d . . . . . H16 H 0.906954 0.293314 0.635391 0.040 Uiso 1 1 calc R U . . . H17 H 1.033340 0.319744 0.548835 0.040 Uiso 1 1 calc R U . . . C17 C 1.1253(3) 0.33920(12) 0.7114(2) 0.0450(7) Uani 1 1 d . . . . . H18 H 1.073484 0.356445 0.776581 0.054 Uiso 1 1 calc R U . . . H19 H 1.209141 0.371114 0.688257 0.054 Uiso 1 1 calc R U . . . C18 C 1.2255(3) 0.27872(12) 0.7457(2) 0.0531(9) Uani 1 1 d . . . . . H20 H 1.316825 0.288213 0.806297 0.080 Uiso 1 1 calc R U . . . H21 H 1.144150 0.247149 0.770587 0.080 Uiso 1 1 calc R U . . . H22 H 1.279970 0.261835 0.682158 0.080 Uiso 1 1 calc R U . . . C19 C 0.5932(3) 0.32568(10) 0.5237(2) 0.0314(6) Uani 1 1 d . . . . . H23 H 0.662360 0.286042 0.521668 0.038 Uiso 1 1 calc R U . . . H24 H 0.553292 0.329199 0.598569 0.038 Uiso 1 1 calc R U . . . C20 C 0.4324(3) 0.32091(11) 0.4381(2) 0.0370(7) Uani 1 1 d . . . . . H25 H 0.343851 0.352404 0.456454 0.044 Uiso 1 1 calc R U . . . H26 H 0.467235 0.331772 0.364044 0.044 Uiso 1 1 calc R U . . . C21 C 0.3494(3) 0.25510(12) 0.4331(2) 0.0457(7) Uani 1 1 d . . . . . H27 H 0.438858 0.223550 0.416478 0.055 Uiso 1 1 calc R U . . . H28 H 0.312571 0.244654 0.506899 0.055 Uiso 1 1 calc R U . . . C22 C 0.1918(3) 0.24947(15) 0.3467(2) 0.0668(10) Uani 1 1 d . . . . . H29 H 0.144462 0.206232 0.347590 0.100 Uiso 1 1 calc R U . . . H30 H 0.101266 0.279828 0.363647 0.100 Uiso 1 1 calc R U . . . H31 H 0.227651 0.258707 0.273157 0.100 Uiso 1 1 calc R U . . . N1 N 0.6852(2) 0.47142(9) 0.31911(15) 0.0246(5) Uani 1 1 d D . . . . N2B N 0.662(2) 0.5011(7) 0.2247(8) 0.021(2) Uani 0.44(2) 1 d D U P A 2 N2A N 0.6459(19) 0.5105(5) 0.2355(6) 0.023(2) Uani 0.56(2) 1 d D U P A 1 O1 O 0.78040(18) 0.36933(7) 0.40204(13) 0.0298(4) Uani 1 1 d . . . . . O2A O 0.8231(15) 0.3957(5) 0.2141(7) 0.0259(15) Uani 0.56(2) 1 d D . P A 1 B1 B 0.8310(3) 0.41765(13) 0.3321(3) 0.0292(7) Uani 1 1 d D . . . . F1 F 0.98764(14) 0.44873(6) 0.36583(11) 0.0352(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 C1 0.0205(10) 0.0243(12) 0.0134(12) -0.0020(10) 0.0045(10) -0.0026(9) C2 0.0220(10) 0.0171(12) 0.0169(13) -0.0004(10) 0.0026(10) -0.0034(9) C3 0.0223(10) 0.0268(13) 0.0188(13) 0.0046(11) 0.0002(10) -0.0015(9) C4A 0.014(5) 0.033(5) 0.017(3) -0.006(3) 0.008(3) 0.005(3) C5A 0.018(5) 0.029(5) 0.025(3) -0.006(3) 0.006(3) 0.002(3) C6A 0.040(4) 0.030(5) 0.039(4) -0.020(4) 0.015(4) -0.008(4) C7A 0.029(5) 0.054(7) 0.019(3) -0.017(4) 0.009(3) -0.015(5) C8A 0.023(3) 0.051(6) 0.021(3) -0.009(3) -0.003(2) -0.012(4) C9A 0.032(7) 0.079(10) 0.014(3) 0.003(5) 0.005(3) -0.010(7) C10A 0.037(4) 0.071(7) 0.020(4) 0.013(4) 0.000(3) -0.011(4) C11A 0.041(4) 0.059(6) 0.022(4) 0.013(4) -0.001(3) -0.012(4) C12A 0.026(4) 0.046(6) 0.026(4) 0.007(4) 0.003(3) 0.001(4) C4B 0.008(5) 0.030(6) 0.012(4) -0.006(3) 0.003(3) 0.005(4) C6B 0.021(4) 0.029(5) 0.029(4) -0.013(3) 0.010(3) -0.006(4) C7B 0.021(4) 0.040(6) 0.026(4) -0.013(4) 0.011(4) -0.004(4) C12B 0.021(6) 0.037(7) 0.014(4) -0.001(4) 0.004(3) 0.000(5) C13A 0.024(4) 0.031(6) 0.014(3) -0.007(3) 0.007(2) -0.012(4) O2B 0.013(4) 0.034(5) 0.028(3) -0.007(3) -0.001(3) 0.010(2) C5B 0.006(4) 0.026(6) 0.025(4) -0.013(3) 0.004(4) 0.000(4) C8B 0.018(5) 0.031(6) 0.017(4) -0.007(4) 0.007(3) -0.008(5) C9B 0.024(4) 0.057(7) 0.018(4) 0.002(4) -0.005(3) -0.012(4) C10B 0.024(7) 0.055(9) 0.021(4) 0.007(6) -0.005(4) -0.006(6) C11B 0.036(5) 0.047(7) 0.023(5) 0.006(4) -0.002(4) -0.002(4) C13B 0.019(4) 0.025(6) 0.020(4) -0.009(3) -0.001(3) -0.006(4) C14 0.0261(11) 0.0197(13) 0.0297(15) 0.0012(11) 0.0025(11) -0.0013(9) C15 0.0257(11) 0.0275(14) 0.0336(16) 0.0008(12) -0.0004(11) 0.0013(10) C16 0.0303(12) 0.0300(15) 0.0393(17) 0.0042(12) 0.0053(12) 0.0066(10) C17 0.0385(14) 0.0422(18) 0.0528(19) 0.0116(15) -0.0027(14) 0.0103(12) C18 0.0458(16) 0.067(2) 0.047(2) 0.0158(16) 0.0078(15) 0.0273(15) C19 0.0302(12) 0.0222(14) 0.0421(17) 0.0003(12) 0.0047(12) -0.0016(10) C20 0.0331(13) 0.0320(15) 0.0460(18) -0.0069(13) 0.0040(13) -0.0069(11) C21 0.0495(15) 0.0403(17) 0.051(2) -0.0159(15) 0.0236(14) -0.0191(13) C22 0.0480(17) 0.078(2) 0.075(3) -0.0388(19) 0.0118(17) -0.0335(16) N1 0.0266(10) 0.0290(12) 0.0187(12) -0.0031(9) 0.0043(9) -0.0064(8) N2B 0.018(4) 0.024(4) 0.020(4) -0.010(3) 0.004(3) -0.002(3) N2A 0.023(3) 0.040(4) 0.009(3) -0.006(3) 0.009(2) -0.008(3) O1 0.0315(8) 0.0255(10) 0.0343(11) -0.0069(8) 0.0120(8) -0.0013(7) O2A 0.019(4) 0.030(4) 0.029(3) -0.006(2) 0.004(3) 0.008(2) B1 0.0247(13) 0.0302(17) 0.0346(19) -0.0100(14) 0.0119(13) -0.0051(12) F1 0.0234(6) 0.0384(9) 0.0443(9) -0.0075(7) 0.0062(6) -0.0052(6) 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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 C3 C1 C2 121.5(2) . . ? C3 C1 N1 120.7(2) . . ? C2 C1 N1 117.8(2) . . ? C3 C2 C1 116.4(2) 3_666 . ? C3 C2 C14 119.6(2) 3_666 . ? C1 C2 C14 124.0(2) . . ? C2 C3 C1 122.1(2) 3_666 . ? C2 C3 H13 119.0 3_666 . ? C1 C3 H13 119.0 . . ? N2A C4A C5A 120.5(7) . . ? N2A C4A C13A 118.4(6) . . ? C5A C4A C13A 120.9(6) . . ? O2A C5A C4A 121.8(7) . . ? O2A C5A C6A 119.0(7) . . ? C4A C5A C6A 119.1(6) . . ? C7A C6A C5A 119.6(6) . . ? C7A C6A H1 120.2 . . ? C5A C6A H1 120.2 . . ? C6A C7A C8A 123.3(6) . . ? C6A C7A H2 118.3 . . ? C8A C7A H2 118.3 . . ? C7A C8A C9A 121.4(7) . . ? C7A C8A C13A 118.4(6) . . ? C9A C8A C13A 120.2(6) . . ? C10A C9A C8A 118.7(8) . . ? C10A C9A H3 120.7 . . ? C8A C9A H3 120.7 . . ? C9A C10A C11A 121.7(8) . . ? C9A C10A H4 119.2 . . ? C11A C10A H4 119.2 . . ? C12A C11A C10A 120.9(7) . . ? C12A C11A H5 119.6 . . ? C10A C11A H5 119.6 . . ? C11A C12A C13A 119.3(8) . . ? C11A C12A H6 120.3 . . ? C13A C12A H6 120.3 . . ? N2B C4B C5B 124.4(8) . . ? N2B C4B C13B 112.5(7) . . ? C5B C4B C13B 121.7(8) . . ? C7B C6B C5B 118.2(7) . . ? C7B C6B H7 120.9 . . ? C5B C6B H7 120.9 . . ? C6B C7B C8B 124.0(8) . . ? C6B C7B H8 118.0 . . ? C8B C7B H8 118.0 . . ? C13B C12B C11B 120.0(8) . . ? C13B C12B H9 120.0 . . ? C11B C12B H9 120.0 . . ? C12A C13A C8A 119.2(6) . . ? C12A C13A C4A 122.3(6) . . ? C8A C13A C4A 118.5(6) . . ? C5B O2B B1 113.7(9) . . ? O2B C5B C4B 122.5(8) . . ? O2B C5B C6B 117.9(8) . . ? C4B C5B C6B 119.6(8) . . ? C13B C8B C9B 119.4(8) . . ? C13B C8B C7B 119.2(7) . . ? C9B C8B C7B 121.3(8) . . ? C10B C9B C8B 120.6(10) . . ? C10B C9B H10 119.7 . . ? C8B C9B H10 119.7 . . ? C9B C10B C11B 120.9(11) . . ? C9B C10B H11 119.5 . . ? C11B C10B H11 119.5 . . ? C12B C11B C10B 119.1(8) . . ? C12B C11B H12 120.5 . . ? C10B C11B H12 120.5 . . ? C8B C13B C12B 119.9(8) . . ? C8B C13B C4B 116.9(7) . . ? C12B C13B C4B 122.6(8) . . ? O1 C14 C2 112.18(18) . . ? O1 C14 C19 104.86(18) . . ? C2 C14 C19 109.81(18) . . ? O1 C14 C15 109.97(18) . . ? C2 C14 C15 108.16(18) . . ? C19 C14 C15 111.89(19) . . ? C16 C15 C14 115.54(19) . . ? C16 C15 H14 108.4 . . ? C14 C15 H14 108.4 . . ? C16 C15 H15 108.4 . . ? C14 C15 H15 108.4 . . ? H14 C15 H15 107.5 . . ? C17 C16 C15 112.5(2) . . ? C17 C16 H16 109.1 . . ? C15 C16 H16 109.1 . . ? C17 C16 H17 109.1 . . ? C15 C16 H17 109.1 . . ? H16 C16 H17 107.8 . . ? C16 C17 C18 113.9(2) . . ? C16 C17 H18 108.8 . . ? C18 C17 H18 108.8 . . ? C16 C17 H19 108.8 . . ? C18 C17 H19 108.8 . . ? H18 C17 H19 107.7 . . ? C17 C18 H20 109.5 . . ? C17 C18 H21 109.5 . . ? H20 C18 H21 109.5 . . ? C17 C18 H22 109.5 . . ? H20 C18 H22 109.5 . . ? H21 C18 H22 109.5 . . ? C20 C19 C14 113.68(19) . . ? C20 C19 H23 108.8 . . ? C14 C19 H23 108.8 . . ? C20 C19 H24 108.8 . . ? C14 C19 H24 108.8 . . ? H23 C19 H24 107.7 . . ? C21 C20 C19 112.9(2) . . ? C21 C20 H25 109.0 . . ? C19 C20 H25 109.0 . . ? C21 C20 H26 109.0 . . ? C19 C20 H26 109.0 . . ? H25 C20 H26 107.8 . . ? C22 C21 C20 113.4(2) . . ? C22 C21 H27 108.9 . . ? C20 C21 H27 108.9 . . ? C22 C21 H28 108.9 . . ? C20 C21 H28 108.9 . . ? H27 C21 H28 107.7 . . ? C21 C22 H29 109.5 . . ? C21 C22 H30 109.5 . . ? H29 C22 H30 109.5 . . ? C21 C22 H31 109.5 . . ? H29 C22 H31 109.5 . . ? H30 C22 H31 109.5 . . ? N2B N1 C1 123.5(6) . . ? N2A N1 C1 111.9(5) . . ? N2B N1 B1 117.3(6) . . ? N2A N1 B1 128.6(5) . . ? C1 N1 B1 119.21(19) . . ? N1 N2B C4B 117.5(9) . . ? N1 N2A C4A 114.5(7) . . ? B1 O1 C14 122.51(19) . . ? C5A O2A B1 121.7(8) . . ? F1 B1 O1 116.6(2) . . ? F1 B1 O2B 106.1(6) . . ? O1 B1 O2B 103.5(6) . . ? F1 B1 O2A 111.9(5) . . ? O1 B1 O2A 111.5(5) . . ? F1 B1 N1 105.7(2) . . ? O1 B1 N1 109.9(2) . . ? O2B B1 N1 115.3(5) . . ? O2A B1 N1 99.7(4) . . ? 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 C1 C3 1.395(3) . ? C1 C2 1.403(3) . ? C1 N1 1.424(3) . ? C2 C3 1.385(3) 3_666 ? C2 C14 1.530(3) . ? C3 H13 0.9500 . ? C4A N2A 1.391(8) . ? C4A C5A 1.392(7) . ? C4A C13A 1.462(8) . ? C5A O2A 1.324(7) . ? C5A C6A 1.439(8) . ? C6A C7A 1.371(7) . ? C6A H1 0.9500 . ? C7A C8A 1.412(7) . ? C7A H2 0.9500 . ? C8A C9A 1.412(9) . ? C8A C13A 1.423(7) . ? C9A C10A 1.362(8) . ? C9A H3 0.9500 . ? C10A C11A 1.402(10) . ? C10A H4 0.9500 . ? C11A C12A 1.371(12) . ? C11A H5 0.9500 . ? C12A C13A 1.410(7) . ? C12A H6 0.9500 . ? C4B N2B 1.362(10) . ? C4B C5B 1.401(8) . ? C4B C13B 1.453(9) . ? C6B C7B 1.357(9) . ? C6B C5B 1.417(9) . ? C6B H7 0.9500 . ? C7B C8B 1.420(8) . ? C7B H8 0.9500 . ? C12B C13B 1.399(8) . ? C12B C11B 1.399(15) . ? C12B H9 0.9500 . ? O2B C5B 1.312(9) . ? O2B B1 1.462(10) . ? C8B C13B 1.397(9) . ? C8B C9B 1.397(9) . ? C9B C10B 1.365(9) . ? C9B H10 0.9500 . ? C10B C11B 1.399(14) . ? C10B H11 0.9500 . ? C11B H12 0.9500 . ? C14 O1 1.429(3) . ? C14 C19 1.534(3) . ? C14 C15 1.536(3) . ? C15 C16 1.522(3) . ? C15 H14 0.9900 . ? C15 H15 0.9900 . ? C16 C17 1.513(3) . ? C16 H16 0.9900 . ? C16 H17 0.9900 . ? C17 C18 1.521(3) . ? C17 H18 0.9900 . ? C17 H19 0.9900 . ? C18 H20 0.9800 . ? C18 H21 0.9800 . ? C18 H22 0.9800 . ? C19 C20 1.527(3) . ? C19 H23 0.9900 . ? C19 H24 0.9900 . ? C20 C21 1.523(3) . ? C20 H25 0.9900 . ? C20 H26 0.9900 . ? C21 C22 1.516(3) . ? C21 H27 0.9900 . ? C21 H28 0.9900 . ? C22 H29 0.9800 . ? C22 H30 0.9800 . ? C22 H31 0.9800 . ? N1 N2B 1.299(6) . ? N1 N2A 1.315(5) . ? N1 B1 1.586(3) . ? O1 B1 1.404(3) . ? O2A B1 1.499(8) . ? B1 F1 1.389(3) . ? 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 C3 C1 C2 C3 0.0(3) . . . 3_666 ? N1 C1 C2 C3 178.79(16) . . . 3_666 ? C3 C1 C2 C14 177.92(18) . . . . ? N1 C1 C2 C14 -3.3(3) . . . . ? C2 C1 C3 C2 0.0(3) . . . 3_666 ? N1 C1 C3 C2 -178.76(17) . . . 3_666 ? N2A C4A C5A O2A -5(2) . . . . ? C13A C4A C5A O2A 179.9(14) . . . . ? N2A C4A C5A C6A 170.6(15) . . . . ? C13A C4A C5A C6A -4.9(19) . . . . ? O2A C5A C6A C7A 177.2(11) . . . . ? C4A C5A C6A C7A 1.9(17) . . . . ? C5A C6A C7A C8A 1.0(15) . . . . ? C6A C7A C8A C9A 177.2(9) . . . . ? C6A C7A C8A C13A -0.8(15) . . . . ? C7A C8A C9A C10A -179.6(9) . . . . ? C13A C8A C9A C10A -1.6(16) . . . . ? C8A C9A C10A C11A 0.3(17) . . . . ? C9A C10A C11A C12A -1.1(18) . . . . ? C10A C11A C12A C13A 3.2(19) . . . . ? C5B C6B C7B C8B -2(2) . . . . ? C11A C12A C13A C8A -4.4(17) . . . . ? C11A C12A C13A C4A 179.6(14) . . . . ? C7A C8A C13A C12A -178.3(10) . . . . ? C9A C8A C13A C12A 3.7(15) . . . . ? C7A C8A C13A C4A -2.2(16) . . . . ? C9A C8A C13A C4A 179.8(12) . . . . ? N2A C4A C13A C12A 5(2) . . . . ? C5A C4A C13A C12A -179.0(12) . . . . ? N2A C4A C13A C8A -170.6(13) . . . . ? C5A C4A C13A C8A 5.0(19) . . . . ? B1 O2B C5B C4B -11(2) . . . . ? B1 O2B C5B C6B 171.2(13) . . . . ? N2B C4B C5B O2B -14(3) . . . . ? C13B C4B C5B O2B -179.0(17) . . . . ? N2B C4B C5B C6B 164.1(19) . . . . ? C13B C4B C5B C6B -1(2) . . . . ? C7B C6B C5B O2B -177.9(13) . . . . ? C7B C6B C5B C4B 4(2) . . . . ? C6B C7B C8B C13B -3(2) . . . . ? C6B C7B C8B C9B 177.4(12) . . . . ? C13B C8B C9B C10B 1.3(19) . . . . ? C7B C8B C9B C10B -178.9(12) . . . . ? C8B C9B C10B C11B -1(2) . . . . ? C13B C12B C11B C10B -4(2) . . . . ? C9B C10B C11B C12B 3(2) . . . . ? C9B C8B C13B C12B -2.6(19) . . . . ? C7B C8B C13B C12B 177.6(12) . . . . ? C9B C8B C13B C4B -174.6(14) . . . . ? C7B C8B C13B C4B 6(2) . . . . ? C11B C12B C13B C8B 4(2) . . . . ? C11B C12B C13B C4B 175.5(16) . . . . ? N2B C4B C13B C8B -170.7(15) . . . . ? C5B C4B C13B C8B -4(2) . . . . ? N2B C4B C13B C12B 18(2) . . . . ? C5B C4B C13B C12B -175.3(14) . . . . ? C3 C2 C14 O1 172.52(16) 3_666 . . . ? C1 C2 C14 O1 -5.3(3) . . . . ? C3 C2 C14 C19 56.3(3) 3_666 . . . ? C1 C2 C14 C19 -121.5(2) . . . . ? C3 C2 C14 C15 -66.0(2) 3_666 . . . ? C1 C2 C14 C15 116.1(2) . . . . ? O1 C14 C15 C16 -59.9(2) . . . . ? C2 C14 C15 C16 177.32(19) . . . . ? C19 C14 C15 C16 56.2(3) . . . . ? C14 C15 C16 C17 -179.4(2) . . . . ? C15 C16 C17 C18 170.7(2) . . . . ? O1 C14 C19 C20 -65.4(2) . . . . ? C2 C14 C19 C20 55.3(3) . . . . ? C15 C14 C19 C20 175.42(19) . . . . ? C14 C19 C20 C21 161.1(2) . . . . ? C19 C20 C21 C22 -178.8(2) . . . . ? C3 C1 N1 N2B -11.1(11) . . . . ? C2 C1 N1 N2B 170.1(11) . . . . ? C3 C1 N1 N2A -7.3(8) . . . . ? C2 C1 N1 N2A 173.9(8) . . . . ? C3 C1 N1 B1 167.44(18) . . . . ? C2 C1 N1 B1 -11.3(3) . . . . ? C1 N1 N2B C4B -173.5(12) . . . . ? B1 N1 N2B C4B 8(2) . . . . ? C5B C4B N2B N1 14(3) . . . . ? C13B C4B N2B N1 -179.0(15) . . . . ? C1 N1 N2A C4A -172.9(11) . . . . ? B1 N1 N2A C4A 13.0(17) . . . . ? C5A C4A N2A N1 10(2) . . . . ? C13A C4A N2A N1 -174.1(12) . . . . ? C2 C14 O1 B1 33.0(3) . . . . ? C19 C14 O1 B1 152.15(19) . . . . ? C15 C14 O1 B1 -87.4(2) . . . . ? C4A C5A O2A B1 -25.4(17) . . . . ? C6A C5A O2A B1 159.3(10) . . . . ? C14 O1 B1 F1 74.1(3) . . . . ? C14 O1 B1 O2B -169.8(5) . . . . ? C14 O1 B1 O2A -155.7(5) . . . . ? C14 O1 B1 N1 -46.1(3) . . . . ? C5B O2B B1 F1 -85.6(11) . . . . ? C5B O2B B1 O1 151.1(11) . . . . ? C5B O2B B1 N1 31.0(13) . . . . ? C5A O2A B1 F1 -72.3(10) . . . . ? C5A O2A B1 O1 155.0(9) . . . . ? C5A O2A B1 N1 39.0(10) . . . . ? N2B N1 B1 F1 86.0(10) . . . . ? N2A N1 B1 F1 81.1(9) . . . . ? C1 N1 B1 F1 -92.7(2) . . . . ? N2B N1 B1 O1 -147.4(10) . . . . ? N2A N1 B1 O1 -152.3(9) . . . . ? C1 N1 B1 O1 34.0(3) . . . . ? N2B N1 B1 O2B -30.8(12) . . . . ? C1 N1 B1 O2B 150.5(7) . . . . ? N2A N1 B1 O2A -35.1(10) . . . . ? C1 N1 B1 O2A 151.2(5) . . . . ?