#------------------------------------------------------------------------------ #$Date: 2024-11-26 02:37:22 +0200 (Tue, 26 Nov 2024) $ #$Revision: 296105 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/96/7249639.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_7249639 loop_ _publ_author_name 'Huang, Mengjun' 'Wang, Guoqiang' 'Li, Heyin' 'Zou, Zhenlei' 'Jia, Xingye' 'Karotsis, Georgios' 'Pan, Yi' 'Zhang, Weigang' 'Ma, Jing' 'Wang, Yi' _publ_section_title ; EDA complex mediated [3+2] cyclization for the construction of CF3-oxadiazoles ; _journal_name_full 'Green Chemistry' _journal_paper_doi 10.1039/D4GC05267F _journal_year 2024 _chemical_formula_moiety '2(C10 H8 F3 N3 O)' _chemical_formula_sum 'C20 H16 F6 N6 O2' _chemical_formula_weight 486.39 _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 _atom_sites_solution_primary iterative _audit_block_doi 10.5517/ccdc.csd.cc2g0n27 _audit_creation_date 2023-05-23 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2023-05-23 deposited with the CCDC. 2024-11-25 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 95.113(19) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 5.900(3) _cell_length_b 12.748(6) _cell_length_c 28.745(15) _cell_measurement_reflns_used 4557 _cell_measurement_temperature 193.0 _cell_measurement_theta_max 48.09 _cell_measurement_theta_min 2.69 _cell_volume 2153.4(19) _computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)' _computing_data_reduction 'SAINT v8.37A (Bruker, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'olex2.solve (Bourhis et al., 2015)' _diffrn_ambient_temperature 193.0 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type GaK\a _diffrn_radiation_wavelength 1.34139 _diffrn_reflns_av_R_equivalents 0.0995 _diffrn_reflns_av_unetI/netI 0.0935 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_number 26562 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 53.594 _diffrn_reflns_theta_max 53.972 _diffrn_reflns_theta_min 2.685 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.766 _exptl_absorpt_correction_T_max 0.7506 _exptl_absorpt_correction_T_min 0.5961 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1383 before and 0.0899 after correction. The Ratio of minimum to maximum transmission is 0.7942. The \l/2 correction factor is Not present. ; _exptl_crystal_colour 'clear light colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.500 _exptl_crystal_description block _exptl_crystal_F_000 992 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.282 _refine_diff_density_min -0.288 _refine_diff_density_rms 0.074 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 307 _refine_ls_number_reflns 3932 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.024 _refine_ls_R_factor_all 0.1061 _refine_ls_R_factor_gt 0.0641 _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^)+(0.0901P)^2^+0.3134P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1601 _refine_ls_wR_factor_ref 0.1915 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2396 _reflns_number_total 3932 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4gc05267f2.cif _cod_data_source_block hmj_a _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 ; _cod_original_cell_volume 2153.3(19) _cod_database_code 7249639 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.927 _shelx_estimated_absorpt_t_min 0.927 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H) groups 2.a Secondary CH2 refined with riding coordinates: C17(H17A,H17B), C7(H7A,H7B) 2.b Aromatic/amide H refined with riding coordinates: N1(H1), N4(H4A), C6(H6), C12(H12), C2(H2), C3(H3), C16(H16), C5(H5), C4(H4), C13(H13), C14(H14), C15(H15) ; _shelx_res_file ; hmj_a.res created by SHELXL-2014/7 TITL HMJ_a.res in P2(1)/n REM Old TITL HMJ in P-1 REM SHELXT solution in P2(1)/n REM R1 0.206, Rweak 0.020, Alpha 0.034, Orientation as input REM Formula found by SHELXT: C21 F6 N5 O2 CELL 1.34139 5.8998 12.7477 28.7454 90 95.113 90 ZERR 4 0.0031 0.0062 0.0153 0 0.019 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H F N O DISP C 0.0148 0.007 57.7477 DISP F 0.0599 0.0411 317.6292 DISP N 0.0253 0.0136 110.5121 DISP O 0.0412 0.025 193.9543 UNIT 80 64 24 24 8 L.S. 10 PLAN 20 SIZE 0.1 0.1 0.1 TEMP -80.15 LIST 6 fmap 2 acta REM REM REM WGHT 0.090100 0.313400 FVAR 0.42093 O1 5 0.198363 0.837012 0.482773 11.00000 0.05080 0.06915 = 0.04980 0.00215 0.01163 0.00350 O2 5 0.598042 0.514973 0.605499 11.00000 0.05214 0.06892 = 0.05204 0.00050 0.00441 -0.00072 F6 3 0.270788 0.519303 0.519302 11.00000 0.11939 0.11636 = 0.06226 -0.00273 -0.00819 -0.00994 F1 3 -0.077450 0.801693 0.395247 11.00000 0.14075 0.12137 = 0.05298 0.00296 0.00741 -0.01772 F3 3 -0.008501 0.663901 0.435149 11.00000 0.12929 0.07935 = 0.09701 -0.02285 -0.01205 0.00846 F2 3 -0.332646 0.738872 0.434409 11.00000 0.07587 0.15251 = 0.09619 -0.02283 -0.00217 -0.02941 N1 4 0.420511 0.922519 0.540865 11.00000 0.04982 0.07490 = 0.05202 0.00753 0.01157 -0.00424 AFIX 43 H1 2 0.534871 0.917725 0.523307 11.00000 -1.20000 AFIX 0 N4 4 0.825400 0.439812 0.665847 11.00000 0.04904 0.07977 = 0.05243 0.00098 0.00667 0.00796 AFIX 43 H4A 2 0.939639 0.443885 0.648225 11.00000 -1.20000 AFIX 0 N3 4 -0.141034 0.857440 0.508007 11.00000 0.05137 0.06909 = 0.05842 0.00419 0.00881 -0.00366 N2 4 0.017306 0.907098 0.540564 11.00000 0.04717 0.06908 = 0.05524 0.00314 0.01255 0.00228 N5 4 0.423958 0.455264 0.666253 11.00000 0.04897 0.07414 = 0.06196 -0.00433 0.00610 -0.00308 N6 4 0.262841 0.499433 0.632794 11.00000 0.04937 0.08237 = 0.06808 -0.01030 0.00065 0.00235 F4 3 0.402943 0.662507 0.544137 11.00000 0.18934 0.09996 = 0.12588 0.04763 -0.06492 -0.04325 C8 1 0.214880 0.891799 0.523988 11.00000 0.05576 0.05444 = 0.04494 0.00668 0.01239 0.00150 C18 1 0.618717 0.467295 0.648422 11.00000 0.05353 0.05890 = 0.05052 -0.00394 0.00775 -0.00271 C11 1 0.864804 0.488795 0.749883 11.00000 0.05592 0.05553 = 0.05145 0.00391 0.00110 0.00571 C1 1 0.479154 0.878245 0.624748 11.00000 0.05423 0.05614 = 0.04787 -0.00093 0.00289 -0.00655 C6 1 0.670490 0.814955 0.630144 11.00000 0.05013 0.06780 = 0.06152 0.00044 0.00808 -0.00341 AFIX 43 H6 2 0.790091 0.825115 0.610557 11.00000 -1.20000 AFIX 0 C9 1 -0.029485 0.819276 0.475924 11.00000 0.05139 0.06328 = 0.05282 0.00945 0.00816 0.00149 C12 1 0.687316 0.498119 0.778088 11.00000 0.05723 0.06519 = 0.05683 0.00724 0.00542 0.00028 AFIX 43 H12 2 0.563405 0.450378 0.774296 11.00000 -1.20000 AFIX 0 C2 1 0.305420 0.860985 0.653405 11.00000 0.05306 0.06525 = 0.05584 -0.00344 0.00948 -0.00104 AFIX 43 H2 2 0.172199 0.903131 0.649878 11.00000 -1.20000 AFIX 0 F5 3 0.069167 0.614502 0.558088 11.00000 0.11472 0.24459 = 0.10676 0.01127 -0.01709 0.09583 C17 1 0.866413 0.402711 0.714080 11.00000 0.06493 0.06239 = 0.05597 0.00108 0.00332 0.00752 AFIX 23 H17A 2 1.015677 0.366771 0.717827 11.00000 -1.20000 H17B 2 0.748187 0.350549 0.720097 11.00000 -1.20000 AFIX 0 C19 1 0.369674 0.532476 0.599244 11.00000 0.05256 0.07122 = 0.06014 -0.00834 0.00193 0.00144 C7 1 0.459867 0.964164 0.588142 11.00000 0.06199 0.06371 = 0.05585 0.00512 0.00544 -0.00730 AFIX 23 H7A 2 0.332893 1.011506 0.594281 11.00000 -1.20000 H7B 2 0.601772 1.006023 0.590665 11.00000 -1.20000 AFIX 0 C3 1 0.324141 0.783324 0.686935 11.00000 0.06509 0.07387 = 0.05565 0.00320 0.01161 -0.01422 AFIX 43 H3 2 0.204406 0.772472 0.706423 11.00000 -1.20000 AFIX 0 C16 1 1.042258 0.560082 0.756159 11.00000 0.05810 0.07105 = 0.06211 0.00473 0.00305 -0.00511 AFIX 43 H16 2 1.165435 0.555363 0.737110 11.00000 -1.20000 AFIX 0 C5 1 0.689124 0.736987 0.663826 11.00000 0.06620 0.06314 = 0.06196 -0.00071 -0.00066 0.00430 AFIX 43 H5 2 0.821384 0.694202 0.667332 11.00000 -1.20000 AFIX 0 C4 1 0.516287 0.721429 0.692217 11.00000 0.08574 0.05747 = 0.05469 0.00420 -0.00600 -0.00980 AFIX 43 H4 2 0.529361 0.668147 0.715407 11.00000 -1.20000 AFIX 0 C13 1 0.687610 0.575277 0.811447 11.00000 0.07570 0.07548 = 0.05655 0.00454 0.01166 0.01282 AFIX 43 H13 2 0.564420 0.580369 0.830476 11.00000 -1.20000 AFIX 0 C14 1 0.865354 0.645203 0.817441 11.00000 0.09983 0.05736 = 0.05474 -0.00110 -0.00170 0.00659 AFIX 43 H14 2 0.865753 0.698326 0.840627 11.00000 -1.20000 AFIX 0 C10 1 -0.113334 0.755777 0.435217 11.00000 0.07623 0.07739 = 0.06084 0.00141 0.00261 -0.00241 C15 1 1.043155 0.637565 0.789494 11.00000 0.07871 0.06519 = 0.06675 0.00251 -0.00365 -0.01217 AFIX 43 H15 2 1.166143 0.685810 0.793278 11.00000 -1.20000 AFIX 0 C20 1 0.277129 0.582862 0.555160 11.00000 0.08151 0.08193 = 0.07490 0.00045 -0.01639 0.00516 HKLF 4 REM HMJ_a.res in P2(1)/n REM R1 = 0.0641 for 2396 Fo > 4sig(Fo) and 0.1061 for all 3932 data REM 307 parameters refined using 0 restraints END WGHT 0.0901 0.3134 REM Highest difference peak 0.282, deepest hole -0.288, 1-sigma level 0.074 Q1 1 0.2292 0.6823 0.5702 11.00000 0.05 0.28 Q2 1 0.1830 0.8683 0.4374 11.00000 0.05 0.26 Q3 1 0.7859 0.7578 0.5898 11.00000 0.05 0.23 Q4 1 0.8034 1.0345 0.5607 11.00000 0.05 0.21 Q5 1 0.5049 0.7723 0.5520 11.00000 0.05 0.21 Q6 1 0.6066 0.8572 0.5521 11.00000 0.05 0.20 Q7 1 0.0085 0.9975 0.5620 11.00000 0.05 0.19 Q8 1 0.1495 0.6204 0.6693 11.00000 0.05 0.19 Q9 1 0.5488 0.8560 0.5277 11.00000 0.05 0.19 Q10 1 1.0142 0.4997 0.6442 11.00000 0.05 0.18 Q11 1 0.6602 0.7863 0.5713 11.00000 0.05 0.18 Q12 1 0.8380 0.6412 0.6483 11.00000 0.05 0.18 Q13 1 1.1035 0.5718 0.6991 11.00000 0.05 0.18 Q14 1 -0.0150 0.8819 0.4327 11.00000 0.05 0.18 Q15 1 0.4584 0.6762 0.5378 11.00000 0.05 0.17 Q16 1 1.0093 0.2351 0.7048 11.00000 0.05 0.17 Q17 1 0.8316 1.0849 0.5910 11.00000 0.05 0.17 Q18 1 0.1770 0.5307 0.6752 11.00000 0.05 0.17 Q19 1 0.1650 1.0580 0.5618 11.00000 0.05 0.17 Q20 1 0.7805 0.6971 0.6169 11.00000 0.05 0.17 ; _shelx_res_checksum 48736 _shelx_hkl_file ; -1 0 0 1.10 2.10 -1 0 0 -0.10 0.90 -1 0 0 0.00 0.60 1 0 0 0.50 2.00 -2 0 0 11.30 2.50 -2 0 0 11.60 2.50 -2 0 0 4.90 3.70 2 0 0 12.40 2.30 -2 0 0 9.50 2.40 2 0 0 10.90 5.10 -3 0 0 0.90 1.20 -3 0 0 1.10 1.00 -3 0 0 -1.10 5.60 3 0 0 1.20 7.00 -3 0 0 -2.20 1.40 -3 0 0 -2.70 1.50 -4 0 0 10.20 3.10 -4 0 0 16.30 3.70 4 0 0 16.50 3.10 -4 0 0 16.00 3.20 -4 0 0 8.30 4.00 -4 0 0 9.80 3.40 -5 0 0 1.30 2.30 -5 0 0 2.70 4.20 -5 0 0 -1.20 3.60 -5 0 0 -0.70 2.10 5 0 0 -1.60 1.50 6 0 0 21.10 3.90 -6 0 0 12.10 4.20 -6 0 0 18.40 4.70 -6 0 0 2.20 7.00 -7 0 0 5.40 3.30 7 0 0 0.20 1.90 0 -1 0 0.20 0.20 0 -1 0 -0.40 0.70 0 -1 0 0.30 0.50 0 -1 0 0.20 0.20 0 1 0 0.00 0.20 0 1 0 0.20 0.50 1 -1 0 13.90 4.00 -1 -1 0 23.40 5.10 1 -1 0 16.50 3.20 -1 -1 0 13.50 3.00 -1 1 0 20.80 4.00 1 1 0 17.70 5.10 -1 1 0 14.30 3.10 -1 1 0 13.50 3.00 -2 -1 0 1.20 3.70 2 -1 0 3.60 1.30 2 -1 0 -3.60 3.40 -2 -1 0 5.60 1.60 -2 1 0 6.10 1.60 -2 1 0 3.40 1.30 -2 1 0 3.40 1.20 -2 1 0 4.10 3.70 2 1 0 4.00 1.20 2 1 0 -0.10 4.10 -2 1 0 4.50 1.30 -3 -1 0 232.28 44.50 -3 -1 0 188.48 46.50 3 -1 0 224.78 44.40 -3 -1 0 231.78 44.40 -3 -1 0 229.88 44.50 -3 -1 0 211.98 44.30 3 -1 0 252.37 46.60 -3 1 0 233.38 44.50 -3 1 0 240.58 44.50 3 1 0 220.68 44.40 3 1 0 248.48 47.10 -3 1 0 269.67 44.70 -3 1 0 233.58 44.40 -3 1 0 205.48 46.30 -3 1 0 241.58 44.40 -4 -1 0 95.19 20.20 -4 -1 0 89.39 19.90 -4 -1 0 123.09 19.80 -4 -1 0 93.69 19.60 4 1 0 111.99 19.60 -4 1 0 102.89 19.60 -4 1 0 101.69 19.80 -4 1 0 102.19 20.20 -4 1 0 90.99 19.90 -5 -1 0 1.00 2.00 -5 -1 0 0.50 4.00 5 -1 0 -1.70 1.50 -5 -1 0 0.80 4.20 -5 -1 0 3.00 2.50 5 1 0 -0.30 1.50 -5 1 0 3.20 2.60 -5 1 0 -1.20 2.00 -5 1 0 3.10 4.20 -6 -1 0 13.80 7.10 6 -1 0 9.60 2.70 -6 -1 0 9.10 3.90 -6 -1 0 9.50 3.20 -6 1 0 12.60 3.50 6 1 0 8.50 2.80 -6 1 0 13.10 3.90 -6 1 0 -7.10 6.20 7 -1 0 3.80 2.00 -7 1 0 -1.70 2.70 7 1 0 1.00 2.20 0 -2 0 878.51 172.78 0 -2 0 1036.30 172.58 0 -2 0 803.12 172.48 0 -2 0 834.62 172.48 0 2 0 956.90 172.58 -1 -2 0 38.70 8.00 -1 -2 0 48.60 9.60 1 -2 0 44.70 8.20 -1 -2 0 44.30 8.00 -1 2 0 35.80 8.10 -1 2 0 34.50 8.00 1 2 0 50.19 11.30 -1 2 0 47.30 8.80 2 -2 0 24.70 5.00 2 -2 0 26.80 6.70 2 -2 0 25.10 4.70 -2 -2 0 13.70 6.10 -2 -2 0 20.10 4.60 -2 -2 0 29.00 4.90 2 2 0 17.70 4.60 -2 2 0 22.30 4.60 -2 2 0 20.70 6.40 -2 2 0 27.00 4.90 2 2 0 21.20 6.70 -2 2 0 28.50 4.80 -2 2 0 24.30 4.90 -2 2 0 24.20 4.70 -3 -2 0 165.68 32.30 -3 -2 0 168.78 32.40 -3 -2 0 169.88 32.40 -3 -2 0 185.18 32.60 3 -2 0 163.68 32.40 3 -2 0 172.78 34.90 -3 -2 0 119.29 34.80 -3 2 0 155.08 32.50 -3 2 0 170.68 32.40 -3 2 0 193.68 32.70 -3 2 0 146.19 34.40 -3 2 0 160.38 32.40 3 2 0 154.68 36.00 -3 2 0 160.78 32.40 -3 2 0 193.28 32.40 -4 -2 0 0.70 2.40 -4 -2 0 1.30 2.10 4 -2 0 0.40 1.20 -4 -2 0 -5.30 2.60 -4 -2 0 0.50 1.40 -4 2 0 -0.90 1.50 -4 2 0 3.40 2.10 4 2 0 0.50 1.30 -4 2 0 -0.60 3.10 -5 -2 0 10.90 3.70 5 -2 0 12.40 2.90 -5 -2 0 15.20 5.30 -5 -2 0 15.50 4.70 -5 -2 0 4.40 3.50 -5 -2 0 13.30 3.20 -5 2 0 9.50 3.50 -5 2 0 10.30 3.20 -5 2 0 9.50 4.90 5 2 0 10.50 2.80 -6 -2 0 10.40 6.40 6 -2 0 35.80 6.00 -6 -2 0 29.20 9.00 -6 -2 0 22.90 6.10 6 2 0 34.40 6.10 -6 2 0 36.10 6.60 -6 2 0 8.10 9.30 7 -2 0 0.40 2.00 -7 -2 0 -0.60 3.00 7 2 0 0.20 2.10 -7 2 0 1.90 2.90 0 -3 0 2.50 2.40 0 -3 0 2.20 0.80 0 -3 0 4.70 1.80 0 -3 0 2.90 1.00 0 3 0 1.00 1.80 0 3 0 3.60 1.40 1 -3 0 106.39 19.00 -1 -3 0 99.99 18.90 -1 -3 0 115.19 20.50 -1 -3 0 103.49 18.90 -1 3 0 101.89 19.40 -1 3 0 95.29 18.90 -1 3 0 80.99 18.80 -1 3 0 94.49 19.50 1 3 0 91.39 21.00 -2 -3 0 74.69 16.30 2 -3 0 83.69 16.50 -2 -3 0 84.19 18.30 -2 -3 0 69.79 16.30 2 -3 0 80.49 16.20 -2 -3 0 89.79 16.20 -2 3 0 93.69 16.20 -2 3 0 103.59 16.40 -2 3 0 81.19 16.30 -2 3 0 91.29 17.70 -2 3 0 80.19 16.30 -3 -3 0 19.70 4.90 -3 -3 0 2.60 12.60 3 -3 0 22.40 5.40 -3 -3 0 26.80 5.40 3 -3 0 32.20 9.40 -3 -3 0 19.90 4.90 3 -3 0 26.50 4.80 -3 -3 0 26.70 4.80 -3 3 0 26.00 5.10 -3 3 0 25.50 5.10 -3 3 0 3.00 8.50 3 3 0 25.40 4.80 -3 3 0 18.90 5.20 -3 3 0 25.50 4.80 3 3 0 11.40 11.20 -3 3 0 24.40 4.80 -4 -3 0 9.10 7.10 -4 -3 0 20.20 6.30 -4 -3 0 23.50 6.20 -4 -3 0 29.90 5.60 -4 -3 0 25.70 5.90 4 -3 0 33.00 5.70 4 3 0 31.10 5.70 -4 3 0 28.20 6.00 -4 3 0 33.10 5.70 -4 3 0 24.20 6.50 5 -3 0 3.50 1.90 -5 -3 0 -1.10 2.60 -5 -3 0 5.90 3.00 -5 -3 0 6.10 4.60 -5 -3 0 0.00 3.80 -5 3 0 4.00 2.70 5 3 0 6.20 1.80 -5 3 0 3.20 2.70 -5 3 0 -2.30 4.60 -6 -3 0 2.60 2.40 -6 -3 0 2.20 7.30 6 -3 0 3.50 2.10 -6 -3 0 -1.70 6.50 -6 3 0 -0.30 6.70 6 3 0 1.70 2.10 -6 3 0 3.10 2.90 0 -4 0 46.00 7.10 0 -4 0 30.90 6.60 0 -4 0 30.70 6.50 0 -4 0 31.50 7.70 0 4 0 41.40 8.10 0 4 0 33.20 6.90 -1 -4 0 125.09 23.70 1 -4 0 129.09 23.90 -1 -4 0 140.09 23.90 -1 -4 0 111.69 24.80 -1 -4 0 113.09 23.60 1 4 0 112.59 23.60 -1 4 0 124.99 24.50 -1 4 0 128.89 24.30 1 4 0 138.89 25.40 -1 4 0 124.59 23.60 -1 4 0 118.09 23.70 -2 -4 0 306.67 65.39 2 -4 0 380.46 65.49 -2 -4 0 340.67 65.39 -2 -4 0 377.56 65.19 2 -4 0 315.07 65.19 -2 4 0 345.27 65.29 -2 4 0 319.67 65.39 -2 4 0 338.77 65.19 -2 4 0 346.37 66.09 2 4 0 331.57 67.09 -2 4 0 392.26 65.39 2 4 0 324.47 65.19 -2 4 0 303.77 66.09 3 -4 0 215.88 43.20 3 -4 0 245.78 43.60 -3 -4 0 180.28 43.20 -3 -4 0 236.78 43.40 -3 -4 0 189.98 46.40 -3 -4 0 252.97 43.20 -3 -4 0 254.77 43.40 3 4 0 202.28 43.20 -3 4 0 223.38 43.40 3 4 0 209.98 43.20 -3 4 0 233.18 45.10 -3 4 0 234.78 43.20 -3 4 0 208.08 43.10 -3 4 0 250.17 43.30 3 4 0 310.37 50.39 -3 4 0 216.98 43.40 -4 -4 0 73.49 12.40 -4 -4 0 64.09 13.00 -4 -4 0 60.19 12.60 4 -4 0 54.09 12.30 -4 -4 0 54.99 12.90 -4 4 0 61.39 12.70 -4 4 0 79.99 13.30 4 4 0 62.79 12.30 -4 4 0 61.39 12.50 -5 -4 0 18.60 6.70 -5 -4 0 25.60 5.30 -5 -4 0 31.70 6.60 -5 4 0 25.70 5.60 -5 4 0 25.70 7.00 5 4 0 19.00 5.00 6 -4 0 5.20 2.30 -6 -4 0 3.00 7.20 -6 -4 0 -2.30 2.20 -6 -4 0 2.30 7.60 -6 4 0 -2.40 7.00 -6 4 0 6.60 3.10 6 4 0 2.50 1.90 0 -5 0 1.30 0.80 0 -5 0 1.60 0.90 0 -5 0 -1.10 2.00 0 -5 0 1.80 1.00 0 -5 0 0.30 3.40 0 5 0 5.00 3.80 0 5 0 1.20 1.00 -1 -5 0 717.63 140.09 -1 -5 0 816.42 141.19 -1 -5 0 736.13 140.19 1 -5 0 803.72 140.39 -1 -5 0 715.63 140.29 1 5 0 662.13 140.09 -1 5 0 704.23 140.09 1 5 0 672.13 140.09 -1 5 0 765.72 140.69 -1 5 0 729.13 140.09 -1 5 0 768.02 140.09 -1 5 0 670.73 140.19 1 5 0 799.32 141.49 -2 -5 0 196.08 40.00 2 -5 0 190.88 40.00 -2 -5 0 155.38 41.90 -2 -5 0 189.68 40.30 -2 -5 0 224.68 40.20 2 -5 0 247.98 40.50 -2 5 0 181.48 41.10 -2 5 0 178.68 40.90 -2 5 0 201.58 40.30 2 5 0 215.28 40.10 -2 5 0 220.58 40.10 2 5 0 210.88 43.20 -2 5 0 198.58 40.10 2 5 0 247.08 40.10 -2 5 0 238.68 40.20 3 -5 0 2.50 3.20 -3 -5 0 1.70 2.50 -3 -5 0 -10.30 12.80 -3 -5 0 -1.30 1.30 -3 -5 0 0.80 2.30 3 -5 0 -0.90 1.20 3 5 0 0.70 1.30 -3 5 0 1.80 1.80 -3 5 0 2.80 2.20 -3 5 0 -1.60 6.70 -3 5 0 4.40 3.20 3 5 0 -14.60 13.80 -3 5 0 0.60 1.20 3 5 0 -1.80 1.90 4 -5 0 5.50 1.70 -4 -5 0 -2.70 2.80 -4 -5 0 6.00 1.90 -4 -5 0 5.10 3.50 -4 -5 0 -1.40 4.50 -4 5 0 -0.60 3.30 -4 5 0 4.30 2.70 -4 5 0 3.40 1.90 4 5 0 0.30 1.60 -5 -5 0 14.60 5.90 5 -5 0 11.60 2.70 -5 -5 0 5.10 4.90 -5 -5 0 9.80 3.10 -5 5 0 3.30 3.20 5 5 0 10.10 3.00 -5 5 0 15.90 5.90 -6 -5 0 -14.50 7.70 6 -5 0 3.40 2.20 -6 -5 0 1.60 2.20 -6 5 0 2.70 2.40 6 5 0 -0.80 2.20 0 -6 0 371.36 76.09 0 -6 0 407.76 75.89 0 -6 0 412.36 76.99 0 -6 0 386.56 75.79 0 6 0 395.06 76.99 0 6 0 404.16 75.89 1 -6 0 89.89 16.60 -1 -6 0 103.49 16.50 1 -6 0 74.49 16.00 -1 -6 0 92.19 16.00 -1 -6 0 91.99 16.10 -1 6 0 81.29 17.50 1 6 0 55.69 17.80 -1 6 0 78.69 16.40 -1 6 0 84.69 16.00 1 6 0 83.59 16.00 -1 6 0 73.29 16.00 1 6 0 79.99 16.00 -1 6 0 81.49 16.00 2 -6 0 13.70 5.20 -2 -6 0 23.80 9.80 -2 -6 0 17.50 4.00 -2 -6 0 24.70 4.50 -2 -6 0 18.30 4.80 2 -6 0 17.30 4.10 -2 6 0 12.70 6.40 2 6 0 4.70 11.40 -2 6 0 21.30 4.30 2 6 0 21.40 4.30 2 6 0 25.70 4.20 -2 6 0 24.70 4.20 -2 6 0 17.70 4.40 -3 -6 0 23.30 6.40 -3 -6 0 33.00 6.00 -3 -6 0 16.80 15.70 3 -6 0 25.40 7.30 -3 -6 0 27.70 6.90 -3 -6 0 27.40 6.50 3 -6 0 33.20 6.00 3 6 0 24.20 5.90 -3 6 0 32.40 6.00 -3 6 0 34.80 6.30 3 6 0 39.20 6.20 3 6 0 28.00 19.40 -3 6 0 29.90 6.60 -3 6 0 2.80 9.90 -4 -6 0 3.00 3.50 -4 -6 0 1.80 2.00 -4 -6 0 -0.30 3.70 4 -6 0 0.10 1.60 -4 6 0 3.60 1.80 -4 6 0 4.20 2.50 4 6 0 3.50 1.90 -4 6 0 4.20 3.50 -5 -6 0 1.90 4.90 -5 -6 0 0.60 2.40 -5 -6 0 4.50 5.70 5 -6 0 1.40 1.70 5 6 0 0.60 2.00 -5 6 0 3.70 5.10 -5 6 0 7.70 3.30 -6 -6 0 -0.50 2.20 6 -6 0 0.50 2.20 -6 6 0 0.80 2.30 6 6 0 0.30 2.30 0 -7 0 1.30 2.70 0 -7 0 1.30 1.40 0 -7 0 -7.40 5.90 0 -7 0 -0.20 1.10 0 7 0 2.50 5.90 0 7 0 0.30 1.10 -1 -7 0 21.20 4.80 1 -7 0 20.30 5.60 -1 -7 0 21.80 4.50 -1 -7 0 35.50 5.90 1 -7 0 20.40 4.50 -1 -7 0 5.20 7.80 1 7 0 24.30 4.60 -1 7 0 27.90 4.60 1 7 0 20.40 4.60 -1 7 0 18.70 4.60 -1 7 0 28.20 8.00 1 7 0 21.40 10.70 2 -7 0 28.70 7.60 2 -7 0 25.30 6.10 -2 -7 0 26.90 6.90 -2 -7 0 24.80 6.40 -2 -7 0 2.80 11.90 -2 -7 0 36.90 6.20 -2 7 0 19.50 8.80 -2 7 0 31.30 6.30 2 7 0 37.20 6.20 -2 7 0 29.40 6.10 -2 7 0 30.60 6.30 2 7 0 25.60 14.00 2 7 0 41.20 6.30 3 -7 0 73.29 12.60 -3 -7 0 66.69 13.30 -3 -7 0 46.30 12.90 -3 -7 0 43.70 13.30 -3 -7 0 74.19 12.60 3 -7 0 46.10 13.80 3 7 0 74.29 12.70 -3 7 0 49.60 12.80 -3 7 0 74.69 12.60 -3 7 0 77.49 12.80 -4 -7 0 1.70 4.40 -4 -7 0 1.80 1.90 -4 -7 0 1.10 3.70 4 -7 0 0.00 1.70 -4 7 0 2.50 2.40 -4 7 0 6.10 4.10 4 7 0 0.50 1.90 -4 7 0 1.10 1.80 -5 -7 0 2.40 2.50 -5 -7 0 10.30 7.30 -5 -7 0 2.40 5.50 5 -7 0 4.00 2.00 5 7 0 3.40 2.30 -5 7 0 -0.60 2.80 -5 7 0 3.70 6.60 6 -7 0 3.50 2.50 -6 -7 0 -2.40 1.90 6 7 0 0.80 2.10 -6 7 0 1.20 2.10 0 -8 0 29.80 6.00 0 -8 0 28.10 11.10 0 -8 0 19.50 6.90 0 -8 0 30.00 6.10 0 8 0 37.80 6.10 0 8 0 26.30 12.50 1 -8 0 72.59 13.50 -1 -8 0 67.99 13.50 1 -8 0 60.39 14.30 -1 -8 0 39.70 18.10 -1 -8 0 83.59 13.80 -1 -8 0 77.69 14.70 -1 8 0 35.70 16.40 1 8 0 45.50 19.20 1 8 0 72.39 13.50 1 8 0 73.49 13.60 -1 8 0 75.49 13.50 -1 8 0 60.49 13.60 -2 -8 0 46.60 9.60 -2 -8 0 49.20 10.40 -2 -8 0 50.09 9.20 2 -8 0 45.20 9.20 2 -8 0 62.19 11.10 -2 -8 0 32.30 9.30 2 8 0 59.09 9.40 -2 8 0 37.10 9.20 -2 8 0 47.00 9.40 2 8 0 52.59 9.30 -2 8 0 30.60 14.20 -2 8 0 54.99 9.30 3 -8 0 3.10 7.60 -3 -8 0 3.60 3.30 -3 -8 0 -1.10 3.60 3 -8 0 -2.10 1.70 -3 -8 0 -0.30 1.60 -3 -8 0 -7.60 6.70 -3 8 0 -2.80 2.10 -3 8 0 1.10 1.60 -3 8 0 -2.70 3.20 3 8 0 0.70 1.90 4 -8 0 2.00 1.90 -4 -8 0 -4.20 4.50 -4 -8 0 1.00 2.10 -4 -8 0 -7.10 5.70 -4 8 0 2.10 1.90 -4 8 0 -0.70 2.30 4 8 0 1.50 2.10 -4 8 0 -1.30 5.20 5 -8 0 0.20 1.90 -5 -8 0 0.00 5.30 -5 -8 0 0.80 2.40 -5 8 0 4.40 3.00 5 8 0 1.30 2.20 6 -8 0 -2.60 2.70 -6 -8 0 -0.30 2.00 6 8 0 -3.00 2.30 -6 8 0 -1.70 2.50 0 -9 0 -2.70 4.30 0 -9 0 1.30 2.30 0 -9 0 2.20 1.30 0 9 0 1.70 1.50 -1 -9 0 3.70 5.30 1 -9 0 14.10 2.80 1 -9 0 8.20 5.30 -1 -9 0 11.80 2.70 -1 -9 0 6.50 3.30 1 9 0 18.30 2.90 1 9 0 11.70 3.10 -1 9 0 9.10 3.00 -1 9 0 7.30 2.70 2 -9 0 9.50 2.90 2 -9 0 4.20 7.00 -2 -9 0 14.30 2.90 -2 -9 0 9.60 6.80 -2 -9 0 6.00 3.90 -2 9 0 15.40 3.10 -2 9 0 8.30 3.20 2 9 0 18.30 3.40 2 9 0 11.40 3.00 3 -9 0 5.30 2.00 -3 -9 0 3.80 4.10 -3 -9 0 0.00 1.90 -3 9 0 -2.00 2.20 -3 9 0 1.80 1.90 3 9 0 2.40 2.60 -4 -9 0 5.40 2.60 -4 -9 0 9.00 5.70 4 -9 0 9.00 2.60 -4 9 0 8.90 2.70 -4 9 0 5.70 2.90 4 9 0 4.20 3.00 5 -9 0 6.00 2.40 -5 -9 0 3.00 8.20 -5 -9 0 8.00 2.90 -5 9 0 4.00 2.60 5 9 0 5.90 3.10 0 -10 0 1.10 6.70 0 -10 0 5.80 2.30 0 -10 0 8.50 3.70 0 10 0 13.90 2.50 -1 -10 0 3.20 3.40 1 -10 0 5.40 2.10 -1 -10 0 6.20 2.00 -1 10 0 5.20 2.10 1 10 0 9.50 2.30 -2 -10 0 6.60 4.20 2 -10 0 8.00 2.50 -2 -10 0 8.00 2.50 2 10 0 8.20 2.70 -2 10 0 6.50 2.70 2 10 0 9.70 3.40 -2 10 0 10.30 3.10 -3 -10 0 1.60 2.10 -3 -10 0 -10.00 4.60 3 -10 0 0.70 2.00 -3 10 0 1.50 2.40 3 10 0 0.70 2.90 -3 10 0 0.30 1.90 -4 -10 0 8.10 2.80 -4 -10 0 4.20 5.60 4 -10 0 10.30 2.80 -4 10 0 5.70 2.60 -4 10 0 2.40 2.70 4 10 0 9.40 3.60 -5 -10 0 2.50 2.70 5 -10 0 -1.40 2.30 5 10 0 4.50 3.30 -5 10 0 0.60 2.60 0 -11 0 -0.60 1.80 0 11 0 -1.20 1.80 -1 -11 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0.00 0.90 -2 0 -1 -1.50 2.90 -2 0 -1 -0.30 1.20 -3 0 -1 57.99 11.20 3 0 1 54.59 11.00 -3 0 -1 50.59 11.10 -3 0 -1 60.19 11.10 -3 0 -1 87.39 15.00 -3 0 -1 52.89 11.50 3 0 1 52.39 13.80 -4 0 -1 2.10 1.50 -4 0 -1 3.00 2.50 4 0 1 0.50 1.20 -4 0 -1 -4.80 2.90 -4 0 -1 -4.30 1.70 -5 0 -1 54.69 9.40 -5 0 -1 30.20 9.30 -5 0 -1 53.99 10.60 -5 0 -1 36.40 9.80 5 0 1 55.49 9.20 -6 0 -1 -0.20 2.80 -6 0 -1 -1.30 2.40 -6 0 -1 -1.10 6.70 6 0 1 -2.10 1.70 7 0 1 2.60 2.10 -7 0 -1 2.50 3.30 7 -1 -1 0.30 1.90 -7 1 1 -2.00 2.70 7 1 -1 1.70 2.00 -6 -1 1 0.80 2.90 6 -1 -1 -1.30 1.80 -6 -1 1 -0.50 2.30 -6 -1 1 -9.20 6.60 -6 1 1 -1.40 6.30 -6 1 1 2.10 2.60 -6 1 1 3.20 3.00 6 1 -1 0.10 1.70 -5 -1 1 65.79 14.60 5 -1 -1 73.69 14.30 -5 -1 1 76.19 15.10 -5 -1 1 77.29 14.40 -5 -1 1 76.49 15.40 -5 1 1 65.49 15.30 -5 1 1 62.09 14.50 5 1 -1 80.09 14.30 -5 1 1 71.69 14.40 -4 -1 1 0.00 2.70 -4 -1 1 1.50 1.40 -4 -1 1 2.60 2.10 -4 -1 1 -1.70 1.20 -4 -1 1 -2.40 1.80 -4 -1 1 0.40 2.10 4 1 -1 1.50 1.40 -4 1 1 -1.60 2.70 -4 1 1 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4.00 2.20 -1 -1 -32 0.40 2.00 1 1 32 -3.60 2.00 -1 1 -32 1.40 1.90 2 -1 32 12.70 2.80 -2 -1 -32 -0.40 1.90 2 1 32 1.40 2.20 -2 1 -32 1.70 2.00 -3 -2 32 1.50 1.80 3 -2 -32 0.90 2.60 -3 2 32 0.70 1.60 3 2 -32 5.30 2.40 2 -2 -32 5.50 3.50 -2 -2 32 7.30 2.10 -2 2 32 3.30 1.90 2 2 -32 3.10 2.70 2 2 -32 1.10 2.60 -1 -2 32 0.40 1.70 1 2 -32 3.40 2.90 -1 2 32 1.20 2.00 1 2 -32 0.70 2.00 0 -2 32 2.50 1.80 0 -2 -32 -3.70 2.50 0 2 32 -0.10 1.90 0 2 -32 2.10 1.80 1 -2 32 2.00 2.20 -1 -2 -32 -1.40 2.10 -1 2 -32 2.00 1.90 1 2 32 1.50 2.00 -2 -3 32 2.50 1.80 2 3 -32 -2.30 2.20 -2 3 32 3.20 2.00 2 3 -32 2.40 2.30 -1 -3 32 1.10 1.70 -1 3 32 1.60 1.80 1 3 -32 -4.30 2.60 1 3 -32 -0.20 1.80 0 -3 32 0.40 1.80 0 3 -32 0.80 1.60 0 3 32 2.20 2.00 -1 -3 -32 1.90 2.50 -1 3 -32 0.90 1.80 1 3 32 -0.30 2.00 -2 -4 32 -1.20 1.80 -2 4 32 3.30 1.80 2 4 -32 1.40 2.20 -1 -4 32 2.00 1.80 1 4 -32 -0.20 1.80 1 4 -32 0.20 2.50 -1 4 32 2.60 1.80 0 -4 32 -1.20 2.10 0 4 -32 0.10 3.00 0 4 -32 0.60 1.60 0 4 32 -1.20 1.90 -1 4 -32 -0.60 1.50 1 4 32 1.10 1.90 -1 -5 32 -1.50 1.90 1 5 -32 1.10 2.20 1 5 -32 -2.70 1.70 -1 5 32 -0.90 1.80 0 5 -32 0.90 1.80 0 5 32 7.70 2.10 0 5 -32 0.80 2.90 -2 0 33 -0.10 1.60 2 0 -33 -1.80 3.00 -1 0 33 12.60 3.20 0 0 -33 0.20 2.00 0 0 33 0.60 2.00 1 0 33 1.60 2.10 -1 0 -33 -0.90 1.70 -2 -1 33 -1.20 1.60 2 -1 -33 -1.00 3.30 2 1 -33 0.00 2.80 -2 1 33 1.30 1.80 -1 -1 33 0.70 1.80 -1 1 33 7.00 2.10 1 1 -33 5.90 6.20 1 1 -33 -0.40 2.40 0 -1 33 7.20 2.20 0 -1 -33 -1.20 2.50 0 1 33 7.50 2.30 0 1 -33 5.20 2.30 -1 -1 -33 0.50 1.90 1 -1 33 -0.50 2.20 -1 1 -33 1.10 1.90 1 1 33 -4.30 2.00 -2 -2 33 3.70 1.80 -2 2 33 1.20 1.80 2 2 -33 2.90 2.60 -1 -2 33 1.00 1.70 1 2 -33 1.70 2.10 1 2 -33 2.50 3.10 -1 2 33 1.60 1.80 0 -2 33 8.30 2.40 0 2 -33 3.00 2.40 0 2 33 10.80 2.60 1 -2 33 -2.00 2.20 -1 -2 -33 3.10 2.30 -1 2 -33 -0.80 1.80 1 2 33 -1.30 2.00 -2 -3 33 0.40 1.60 2 3 -33 0.40 2.50 -2 3 33 0.80 1.80 -1 -3 33 1.90 1.70 -1 3 33 -2.40 2.00 1 3 -33 2.40 2.80 1 3 -33 1.10 1.90 0 -3 33 3.90 2.10 0 3 -33 2.50 2.20 0 3 33 5.50 2.20 1 3 33 0.90 2.00 -1 -4 33 4.10 2.10 1 4 -33 3.50 2.70 -1 4 33 9.70 2.40 1 4 -33 3.00 2.10 0 -4 33 1.60 2.30 0 4 -33 2.80 2.00 0 4 33 3.60 2.00 -1 0 34 1.10 1.70 0 0 -34 21.10 4.90 -1 -1 34 4.00 1.90 1 1 -34 1.90 2.70 -1 1 34 1.80 1.80 0 -1 34 1.30 1.80 0 -1 -34 2.10 4.20 0 1 -34 1.60 2.10 0 1 34 0.40 1.90 -1 -2 34 0.60 1.70 1 2 -34 1.30 2.30 -1 2 34 2.10 1.90 0 -2 34 0.10 1.70 0 2 -34 0.00 1.90 0 2 34 -1.40 1.90 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 20156 _olex2_submission_special_instructions 'No special instructions were received' 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 O1 O 0.1984(3) 0.83701(16) 0.48277(6) 0.0562(5) Uani 1 1 d . . . . . O2 O 0.5980(3) 0.51497(16) 0.60550(7) 0.0577(5) Uani 1 1 d . . . . . F6 F 0.2708(4) 0.5193(2) 0.51930(7) 0.1003(8) Uani 1 1 d . . . . . F1 F -0.0775(4) 0.8017(2) 0.39525(7) 0.1051(8) Uani 1 1 d . . . . . F3 F -0.0085(4) 0.66390(18) 0.43515(8) 0.1032(8) Uani 1 1 d . . . . . F2 F -0.3326(4) 0.7389(2) 0.43441(8) 0.1088(8) Uani 1 1 d . . . . . N1 N 0.4205(4) 0.9225(2) 0.54087(8) 0.0585(7) Uani 1 1 d . . . . . H1 H 0.5349 0.9177 0.5233 0.070 Uiso 1 1 calc R . . . . N4 N 0.8254(4) 0.4398(2) 0.66585(8) 0.0603(7) Uani 1 1 d . . . . . H4A H 0.9396 0.4439 0.6482 0.072 Uiso 1 1 calc R . . . . N3 N -0.1410(4) 0.8574(2) 0.50801(9) 0.0594(7) Uani 1 1 d . . . . . N2 N 0.0173(4) 0.9071(2) 0.54056(8) 0.0567(6) Uani 1 1 d . . . . . N5 N 0.4240(4) 0.4553(2) 0.66625(9) 0.0616(7) Uani 1 1 d . . . . . N6 N 0.2628(4) 0.4994(2) 0.63279(10) 0.0669(7) Uani 1 1 d . . . . . F4 F 0.4029(6) 0.6625(2) 0.54414(10) 0.1431(12) Uani 1 1 d . . . . . C8 C 0.2149(5) 0.8918(2) 0.52399(9) 0.0512(7) Uani 1 1 d . . . . . C18 C 0.6187(5) 0.4673(2) 0.64842(10) 0.0541(7) Uani 1 1 d . . . . . C11 C 0.8648(5) 0.4888(2) 0.74988(10) 0.0545(7) Uani 1 1 d . . . . . C1 C 0.4792(5) 0.8782(2) 0.62475(10) 0.0528(7) Uani 1 1 d . . . . . C6 C 0.6705(5) 0.8150(3) 0.63014(11) 0.0596(8) Uani 1 1 d . . . . . H6 H 0.7901 0.8251 0.6106 0.072 Uiso 1 1 calc R . . . . C9 C -0.0295(5) 0.8193(2) 0.47592(10) 0.0556(7) Uani 1 1 d . . . . . C12 C 0.6873(5) 0.4981(2) 0.77809(11) 0.0597(8) Uani 1 1 d . . . . . H12 H 0.5634 0.4504 0.7743 0.072 Uiso 1 1 calc R . . . . C2 C 0.3054(5) 0.8610(2) 0.65341(10) 0.0578(8) Uani 1 1 d . . . . . H2 H 0.1722 0.9031 0.6499 0.069 Uiso 1 1 calc R . . . . F5 F 0.0692(5) 0.6145(3) 0.55809(9) 0.1570(14) Uani 1 1 d . . . . . C17 C 0.8664(5) 0.4027(3) 0.71408(10) 0.0612(8) Uani 1 1 d . . . . . H17A H 1.0157 0.3668 0.7178 0.073 Uiso 1 1 calc R . . . . H17B H 0.7482 0.3505 0.7201 0.073 Uiso 1 1 calc R . . . . C19 C 0.3697(5) 0.5325(3) 0.59924(11) 0.0615(8) Uani 1 1 d . . . . . C7 C 0.4599(5) 0.9642(2) 0.58814(10) 0.0605(8) Uani 1 1 d . . . . . H7A H 0.3329 1.0115 0.5943 0.073 Uiso 1 1 calc R . . . . H7B H 0.6018 1.0060 0.5907 0.073 Uiso 1 1 calc R . . . . C3 C 0.3241(5) 0.7833(3) 0.68694(11) 0.0645(8) Uani 1 1 d . . . . . H3 H 0.2044 0.7725 0.7064 0.077 Uiso 1 1 calc R . . . . C16 C 1.0423(5) 0.5601(3) 0.75616(11) 0.0639(8) Uani 1 1 d . . . . . H16 H 1.1654 0.5554 0.7371 0.077 Uiso 1 1 calc R . . . . C5 C 0.6891(5) 0.7370(3) 0.66383(11) 0.0641(8) Uani 1 1 d . . . . . H5 H 0.8214 0.6942 0.6673 0.077 Uiso 1 1 calc R . . . . C4 C 0.5163(6) 0.7214(3) 0.69222(11) 0.0667(9) Uani 1 1 d . . . . . H4 H 0.5294 0.6681 0.7154 0.080 Uiso 1 1 calc R . . . . C13 C 0.6876(6) 0.5753(3) 0.81145(11) 0.0689(9) Uani 1 1 d . . . . . H13 H 0.5644 0.5804 0.8305 0.083 Uiso 1 1 calc R . . . . C14 C 0.8654(6) 0.6452(3) 0.81744(11) 0.0712(9) Uani 1 1 d . . . . . H14 H 0.8658 0.6983 0.8406 0.085 Uiso 1 1 calc R . . . . C10 C -0.1133(6) 0.7558(3) 0.43522(12) 0.0717(9) Uani 1 1 d . . . . . C15 C 1.0432(6) 0.6376(3) 0.78949(12) 0.0708(9) Uani 1 1 d . . . . . H15 H 1.1661 0.6858 0.7933 0.085 Uiso 1 1 calc R . . . . C20 C 0.2771(7) 0.5829(3) 0.55516(13) 0.0808(10) 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 O1 0.0508(12) 0.0692(13) 0.0498(11) 0.0021(10) 0.0116(8) 0.0035(9) O2 0.0521(12) 0.0689(13) 0.0520(12) 0.0005(10) 0.0044(9) -0.0007(9) F6 0.1194(19) 0.1164(18) 0.0623(13) -0.0027(12) -0.0082(12) -0.0099(14) F1 0.141(2) 0.1214(19) 0.0530(12) 0.0030(12) 0.0074(12) -0.0177(15) F3 0.1293(19) 0.0794(15) 0.0970(17) -0.0228(12) -0.0120(14) 0.0085(13) F2 0.0759(15) 0.153(2) 0.0962(16) -0.0228(15) -0.0022(12) -0.0294(14) N1 0.0498(14) 0.0749(17) 0.0520(14) 0.0075(13) 0.0116(11) -0.0042(12) N4 0.0490(14) 0.0798(18) 0.0524(14) 0.0010(12) 0.0067(11) 0.0080(12) N3 0.0514(14) 0.0691(17) 0.0584(15) 0.0042(13) 0.0088(12) -0.0037(12) N2 0.0472(13) 0.0691(16) 0.0552(14) 0.0031(12) 0.0125(11) 0.0023(12) N5 0.0490(14) 0.0741(18) 0.0620(15) -0.0043(13) 0.0061(12) -0.0031(12) N6 0.0494(15) 0.0824(19) 0.0681(17) -0.0103(15) 0.0006(13) 0.0024(13) F4 0.189(3) 0.1000(19) 0.126(2) 0.0476(17) -0.065(2) -0.0432(19) C8 0.0558(17) 0.0544(17) 0.0449(15) 0.0067(13) 0.0124(12) 0.0015(14) C18 0.0535(18) 0.0589(18) 0.0505(17) -0.0039(14) 0.0077(13) -0.0027(14) C11 0.0559(18) 0.0555(18) 0.0515(17) 0.0039(13) 0.0011(13) 0.0057(14) C1 0.0542(17) 0.0561(17) 0.0479(16) -0.0009(13) 0.0029(13) -0.0066(14) C6 0.0501(17) 0.068(2) 0.0615(18) 0.0004(16) 0.0081(13) -0.0034(15) C9 0.0514(17) 0.0633(19) 0.0528(17) 0.0094(14) 0.0082(13) 0.0015(14) C12 0.0572(18) 0.065(2) 0.0568(18) 0.0072(15) 0.0054(14) 0.0003(14) C2 0.0531(17) 0.0653(19) 0.0558(18) -0.0034(15) 0.0095(13) -0.0010(14) F5 0.115(2) 0.245(4) 0.107(2) 0.011(2) -0.0171(16) 0.096(2) C17 0.0649(19) 0.0624(19) 0.0560(18) 0.0011(15) 0.0033(14) 0.0075(15) C19 0.0526(18) 0.071(2) 0.0601(19) -0.0083(16) 0.0019(15) 0.0014(15) C7 0.0620(19) 0.0637(19) 0.0558(18) 0.0051(15) 0.0054(14) -0.0073(15) C3 0.065(2) 0.074(2) 0.0557(18) 0.0032(16) 0.0116(15) -0.0142(17) C16 0.0581(19) 0.071(2) 0.0621(19) 0.0047(17) 0.0030(14) -0.0051(16) C5 0.066(2) 0.063(2) 0.0620(19) -0.0007(16) -0.0007(16) 0.0043(16) C4 0.086(2) 0.0575(19) 0.0547(18) 0.0042(15) -0.0060(16) -0.0098(18) C13 0.076(2) 0.075(2) 0.0565(19) 0.0045(17) 0.0117(16) 0.0128(19) C14 0.100(3) 0.057(2) 0.0547(19) -0.0011(15) -0.0017(18) 0.0066(19) C10 0.076(2) 0.077(2) 0.061(2) 0.0014(18) 0.0026(17) -0.0024(19) C15 0.079(2) 0.065(2) 0.067(2) 0.0025(17) -0.0037(18) -0.0122(17) C20 0.082(3) 0.082(3) 0.075(3) 0.000(2) -0.0164(19) 0.005(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0148 0.0070 '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' F F 0.0599 0.0411 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0253 0.0136 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0412 0.0250 '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 C9 O1 C8 101.7(2) . . ? C19 O2 C18 101.5(2) . . ? C8 N1 C7 120.9(2) . . ? C18 N4 C17 120.8(2) . . ? C9 N3 N2 107.3(2) . . ? C8 N2 N3 104.4(2) . . ? C18 N5 N6 104.4(3) . . ? C19 N6 N5 107.5(3) . . ? N1 C8 O1 117.3(2) . . ? N2 C8 O1 113.1(2) . . ? N2 C8 N1 129.6(3) . . ? N4 C18 O2 117.6(3) . . ? N5 C18 O2 113.2(3) . . ? N5 C18 N4 129.2(3) . . ? C12 C11 C17 120.9(3) . . ? C12 C11 C16 118.0(3) . . ? C16 C11 C17 121.1(3) . . ? C6 C1 C2 118.6(3) . . ? C6 C1 C7 120.6(3) . . ? C2 C1 C7 120.8(3) . . ? C1 C6 C5 120.6(3) . . ? O1 C9 C10 117.7(3) . . ? N3 C9 O1 113.5(3) . . ? N3 C9 C10 128.7(3) . . ? C13 C12 C11 121.1(3) . . ? C3 C2 C1 120.7(3) . . ? N4 C17 C11 113.7(3) . . ? O2 C19 C20 118.0(3) . . ? N6 C19 O2 113.4(3) . . ? N6 C19 C20 128.6(3) . . ? N1 C7 C1 112.3(2) . . ? C4 C3 C2 120.1(3) . . ? C15 C16 C11 121.2(3) . . ? C4 C5 C6 120.1(3) . . ? C5 C4 C3 119.9(3) . . ? C12 C13 C14 120.3(3) . . ? C13 C14 C15 119.5(3) . . ? F1 C10 F3 106.2(3) . . ? F1 C10 C9 112.2(3) . . ? F3 C10 C9 111.3(3) . . ? F2 C10 F1 107.0(3) . . ? F2 C10 F3 108.4(3) . . ? F2 C10 C9 111.5(3) . . ? C16 C15 C14 120.0(3) . . ? F6 C20 F4 105.4(4) . . ? F6 C20 C19 112.8(3) . . ? F4 C20 C19 111.6(3) . . ? F5 C20 F6 106.4(3) . . ? F5 C20 F4 109.4(4) . . ? F5 C20 C19 110.9(3) . . ? 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 O1 C8 1.371(3) . ? O1 C9 1.360(3) . ? O2 C18 1.371(3) . ? O2 C19 1.362(4) . ? F6 C20 1.309(4) . ? F1 C10 1.323(4) . ? F3 C10 1.325(4) . ? F2 C10 1.310(4) . ? N1 C8 1.325(4) . ? N1 C7 1.458(4) . ? N4 C18 1.324(4) . ? N4 C17 1.465(4) . ? N3 N2 1.412(3) . ? N3 C9 1.276(4) . ? N2 C8 1.313(4) . ? N5 N6 1.408(4) . ? N5 C18 1.308(4) . ? N6 C19 1.270(4) . ? F4 C20 1.313(5) . ? C11 C12 1.385(4) . ? C11 C17 1.505(4) . ? C11 C16 1.386(4) . ? C1 C6 1.385(4) . ? C1 C2 1.389(4) . ? C1 C7 1.516(4) . ? C6 C5 1.385(4) . ? C9 C10 1.472(5) . ? C12 C13 1.374(4) . ? C2 C3 1.379(4) . ? F5 C20 1.301(5) . ? C19 C20 1.481(5) . ? C3 C4 1.378(5) . ? C16 C15 1.376(5) . ? C5 C4 1.376(4) . ? C13 C14 1.375(5) . ? C14 C15 1.380(5) . ?