#------------------------------------------------------------------------------ #$Date: 2021-09-16 01:09:07 +0300 (Thu, 16 Sep 2021) $ #$Revision: 269156 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/46/1564659.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_1564659 loop_ _publ_author_name 'Ramachandran, Kuppan' 'Anbarasan, Pazhamalai' _publ_section_title ; Cobalt-Catalyzed Multisubstituted Allylation of Chelation-Assisted C-H bond of (Hetero)arenes with Cyclopropenes ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D1SC03476F _journal_year 2021 _chemical_formula_moiety 'C23 H25 N2, F6 Sb' _chemical_formula_sum 'C23 H25 F6 N2 Sb' _chemical_formula_weight 565.20 _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 ; 2021-06-22 deposited with the CCDC. 2021-09-15 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 102.305(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.1550(5) _cell_length_b 15.9851(10) _cell_length_c 18.1298(11) _cell_measurement_reflns_used 9852 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 25.00 _cell_measurement_theta_min 3.02 _cell_volume 2309.1(2) _computing_cell_refinement 'APEX3/SAINT (Bruker, 2016)' _computing_data_collection 'APEX3 (Bruker, 2016)' _computing_data_reduction 'SAINT/XPREP (Bruker, 2016)' _computing_molecular_graphics 'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)' _computing_publication_material 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT-2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker axs kappa apex3 CMOS Diffractometer' _diffrn_measurement_method '\w and \f scan' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0918 _diffrn_reflns_av_unetI/netI 0.0470 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 43544 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 24.997 _diffrn_reflns_theta_max 24.997 _diffrn_reflns_theta_min 3.308 _exptl_absorpt_coefficient_mu 1.256 _exptl_absorpt_correction_T_max 0.7453 _exptl_absorpt_correction_T_min 0.5799 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Bruker, 2016)' _exptl_crystal_colour green _exptl_crystal_density_diffrn 1.626 _exptl_crystal_description BLOCK _exptl_crystal_F_000 1128 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: dichloromethane and hexane' _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _refine_diff_density_max 0.607 _refine_diff_density_min -0.480 _refine_diff_density_rms 0.111 _refine_ls_extinction_coef 0.0050(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.131 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 350 _refine_ls_number_reflns 4052 _refine_ls_number_restraints 66 _refine_ls_restrained_S_all 1.147 _refine_ls_R_factor_all 0.1044 _refine_ls_R_factor_gt 0.0724 _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^)+(0.0401P)^2^+11.4700P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1457 _refine_ls_wR_factor_ref 0.1587 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2976 _reflns_number_total 4052 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1sc03476f2.cif _cod_data_source_block shelx _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 1564659 _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 0.834 _shelx_estimated_absorpt_t_max 0.885 _shelx_res_file ; TITL shelxt_a.res in P2(1)/n shelx.res created by SHELXL-2018/3 at 15:46:18 on 28-Jul-2020 CELL 0.71073 8.1550 15.9851 18.1298 90.000 102.305 90.000 ZERR 4.00 0.0005 0.0010 0.0011 0.000 0.002 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N F SB UNIT 92 100 8 24 4 MERG 2 OMIT -3.00 50.00 OMIT -1 1 1 OMIT 1 0 1 OMIT 1 1 1 SADI 0.02 SB1 F1 SB1 F1' SADI 0.02 SB1 F2 SB1 F2' SADI 0.02 SB1 F3 SB1 F3' SADI 0.02 SB1 F4 SB1 F4' SADI 0.02 SB1 F5 SB1 F5' SADI 0.02 SB1 F6 SB1 F6' SIMU 0.02 0.04 F1 > F6' HTAB C5 F4' EQIV $1 -x+1, -y+1, -z+1 HTAB C7 F5_$1 EQIV $2 -x+1/2, y-1/2, -z+1/2 HTAB C14 F2_$2 EQIV $3 x+1/2, -y+3/2, z-1/2 HTAB C14 F1'_$3 HTAB C20 F4 HTAB C20 F4' EQIV $4 x-1/2, -y+3/2, z-1/2 HTAB C22 F1_$4 HTAB C22 F1'_$4 HTAB C23 F1_$4 FMAP 2 PLAN 20 SIZE 0.100 0.100 0.150 ACTA BOND $H CONF L.S. 10 TEMP 23.00 WGHT 0.040100 11.469999 EXTI 0.005021 FVAR 0.35494 0.49749 SB1 5 0.138338 0.807552 0.551196 11.00000 0.07391 0.06801 = 0.05725 -0.01153 0.01288 -0.01218 PART 1 F1 4 0.116558 0.890003 0.616923 21.00000 0.07322 0.19684 = 0.16144 -0.10090 -0.02451 0.04198 F2 4 0.110530 0.896864 0.486202 21.00000 0.19396 0.14346 = 0.13600 0.05040 0.08048 0.00749 F3 4 0.362927 0.829989 0.574829 21.00000 0.07759 0.19291 = 0.26660 -0.03544 0.06770 -0.00709 F4 4 0.164110 0.720152 0.493152 21.00000 0.28981 0.13330 = 0.17708 -0.12092 0.05643 0.00759 F5 4 0.148302 0.734761 0.626732 21.00000 0.20146 0.16273 = 0.13923 0.05281 0.04300 0.04998 F6 4 -0.094540 0.802549 0.534600 21.00000 0.09177 0.15229 = 0.17654 -0.02561 -0.00931 -0.03866 PART 2 F1' 4 0.064239 0.866043 0.621876 -21.00000 0.11023 0.26792 = 0.11311 -0.00528 0.04774 0.07833 F2' 4 0.222667 0.897991 0.513294 -21.00000 0.19303 0.16809 = 0.25748 0.03281 0.03854 -0.07116 F3' 4 0.340132 0.790264 0.620604 -21.00000 0.08108 0.15891 = 0.16992 -0.06330 -0.04266 0.04237 F4' 4 0.223335 0.760784 0.477323 -21.00000 0.32383 0.16364 = 0.14080 -0.01970 0.07031 0.07025 F5' 4 0.091658 0.706675 0.586981 -21.00000 0.20478 0.10934 = 0.18193 0.02161 -0.03360 -0.05018 F6' 4 -0.045285 0.808415 0.477908 -21.00000 0.13528 0.20600 = 0.12675 -0.00879 -0.07732 0.00969 PART 0 C1 1 0.615000 0.494910 0.404944 11.00000 0.05339 0.07803 = 0.05385 0.01647 0.00712 -0.01261 C2 1 0.762851 0.508323 0.459599 11.00000 0.06968 0.12438 = 0.05987 0.01761 0.00251 -0.02949 AFIX 43 H2 2 0.850462 0.469984 0.465506 11.00000 -1.20000 AFIX 0 C3 1 0.776685 0.576324 0.502898 11.00000 0.07663 0.14150 = 0.06347 -0.00334 0.00093 -0.04792 AFIX 43 H3 2 0.874629 0.584470 0.539249 11.00000 -1.20000 AFIX 0 C4 1 0.652113 0.634248 0.495648 11.00000 0.12763 0.09630 = 0.04810 -0.02201 0.02587 -0.06649 AFIX 43 H4 2 0.666804 0.680779 0.527165 11.00000 -1.20000 AFIX 0 C5 1 0.500670 0.625228 0.441187 11.00000 0.08682 0.06941 = 0.06628 -0.01977 0.01457 -0.02820 AFIX 43 H5 2 0.416717 0.665627 0.434267 11.00000 -1.20000 AFIX 0 C6 1 0.485212 0.552044 0.398589 11.00000 0.06217 0.06157 = 0.04214 -0.00159 0.00699 -0.02343 C7 1 0.567424 0.432381 0.349628 11.00000 0.05239 0.06832 = 0.06885 0.00438 0.01086 0.00001 AFIX 43 H7 2 0.633219 0.387105 0.341738 11.00000 -1.20000 AFIX 0 C8 1 0.412281 0.448712 0.310310 11.00000 0.04815 0.04971 = 0.05502 -0.00231 0.01368 -0.00595 C9 1 0.296911 0.405703 0.246313 11.00000 0.05300 0.04325 = 0.04616 -0.00822 0.01115 0.00566 C10 1 0.172559 0.342928 0.272620 11.00000 0.06196 0.04519 = 0.05838 0.00517 0.01845 0.00410 AFIX 13 H10 2 0.131134 0.368302 0.314365 11.00000 -1.20000 AFIX 0 C11 1 0.029911 0.340932 0.202912 11.00000 0.06527 0.03480 = 0.06275 -0.01058 0.02047 -0.00528 C12 1 0.036419 0.407173 0.158879 11.00000 0.05613 0.04994 = 0.05021 -0.01425 0.00744 -0.00552 C13 1 0.174488 0.466337 0.196317 11.00000 0.04535 0.04146 = 0.04359 -0.00308 0.01103 -0.00348 C14 1 0.247847 0.525496 0.145752 11.00000 0.08614 0.05649 = 0.05264 0.00327 0.02709 -0.00926 AFIX 137 H14A 2 0.283137 0.493939 0.106837 11.00000 -1.50000 H14B 2 0.342506 0.554401 0.175411 11.00000 -1.50000 H14C 2 0.164070 0.565385 0.123182 11.00000 -1.50000 AFIX 0 C15 1 0.406610 0.361131 0.198356 11.00000 0.07162 0.07159 = 0.06596 -0.01653 0.02300 0.00758 AFIX 137 H15A 2 0.473241 0.401787 0.179026 11.00000 -1.50000 H15B 2 0.335602 0.332415 0.157068 11.00000 -1.50000 H15C 2 0.479029 0.321544 0.229229 11.00000 -1.50000 AFIX 0 C16 1 0.248125 0.258844 0.297788 11.00000 0.11570 0.04134 = 0.08368 0.00348 0.02591 0.01004 AFIX 137 H16A 2 0.175896 0.229449 0.324397 11.00000 -1.50000 H16B 2 0.356175 0.266648 0.330543 11.00000 -1.50000 H16C 2 0.260404 0.226915 0.254443 11.00000 -1.50000 AFIX 0 C17 1 -0.097107 0.273473 0.191920 11.00000 0.09157 0.06302 = 0.09417 -0.01529 0.03118 -0.03858 AFIX 137 H17A 2 -0.158259 0.275652 0.231641 11.00000 -1.50000 H17B 2 -0.042206 0.220236 0.192883 11.00000 -1.50000 H17C 2 -0.173300 0.280743 0.144100 11.00000 -1.50000 AFIX 0 C18 1 -0.070877 0.424596 0.081445 11.00000 0.08122 0.09521 = 0.05310 -0.00516 -0.01341 -0.01319 AFIX 137 H18A 2 -0.180628 0.401202 0.078133 11.00000 -1.50000 H18B 2 -0.019951 0.399711 0.043647 11.00000 -1.50000 H18C 2 -0.080113 0.483928 0.073435 11.00000 -1.50000 AFIX 0 C19 1 0.193237 0.549853 0.319218 11.00000 0.06711 0.02496 = 0.04251 -0.00001 0.01426 -0.00086 C20 1 0.118417 0.600505 0.364567 11.00000 0.07630 0.05154 = 0.04925 -0.00102 0.01964 0.01228 AFIX 43 H20 2 0.180227 0.618005 0.411179 11.00000 -1.20000 AFIX 0 C21 1 -0.042806 0.624788 0.342055 11.00000 0.10000 0.06540 = 0.05575 0.00747 0.03455 0.02772 AFIX 43 H21 2 -0.091742 0.658688 0.373077 11.00000 -1.20000 AFIX 0 C22 1 -0.134654 0.599332 0.273167 11.00000 0.06891 0.08453 = 0.07838 0.01366 0.01706 0.04386 AFIX 43 H22 2 -0.245392 0.616412 0.256543 11.00000 -1.20000 AFIX 0 C23 1 -0.059433 0.548219 0.229515 11.00000 0.06994 0.06577 = 0.05675 0.00426 0.00838 0.01837 AFIX 43 H23 2 -0.121745 0.529952 0.183267 11.00000 -1.20000 AFIX 0 N1 3 0.356218 0.523545 0.338423 11.00000 0.04980 0.04331 = 0.04637 -0.00680 0.00964 -0.00125 N2 3 0.102750 0.523294 0.251351 11.00000 0.04855 0.04004 = 0.04260 -0.00065 0.00921 0.00332 HKLF 4 REM shelxt_a.res in P2(1)/n REM wR2 = 0.1587, GooF = S = 1.131, Restrained GooF = 1.147 for all data REM R1 = 0.0724 for 2976 Fo > 4sig(Fo) and 0.1044 for all 4052 data REM 350 parameters refined using 66 restraints END WGHT 0.0401 11.4687 REM Highest difference peak 0.607, deepest hole -0.480, 1-sigma level 0.111 Q1 1 -0.0215 0.7844 0.5929 11.00000 0.05 0.61 Q2 1 0.2951 0.8169 0.5105 11.00000 0.05 0.53 Q3 1 0.1180 0.3739 0.3302 11.00000 0.05 0.49 Q4 1 0.1586 0.8845 0.5645 11.00000 0.05 0.48 Q5 1 0.0889 0.8039 0.6170 11.00000 0.05 0.47 Q6 1 0.0351 0.8228 0.5323 11.00000 0.05 0.46 Q7 1 0.1733 0.8018 0.5151 11.00000 0.05 0.43 Q8 1 0.8184 0.4637 0.4206 11.00000 0.05 0.43 Q9 1 0.1876 0.8144 0.4885 11.00000 0.05 0.42 Q10 1 -0.1057 0.4805 -0.0235 11.00000 0.05 0.40 Q11 1 -0.0319 0.4638 -0.0008 11.00000 0.05 0.40 Q12 1 0.0575 0.4593 0.0423 11.00000 0.05 0.40 Q13 1 0.1634 0.4977 0.0769 11.00000 0.05 0.37 Q14 1 0.6539 0.3267 0.2664 11.00000 0.05 0.37 Q15 1 0.1830 0.5752 0.0707 11.00000 0.05 0.36 Q16 1 0.8827 0.5926 0.4721 11.00000 0.05 0.36 Q17 1 0.7951 0.5364 0.4051 11.00000 0.05 0.35 Q18 1 0.2630 0.8101 0.4443 11.00000 0.05 0.34 Q19 1 0.8812 0.3995 0.4877 11.00000 0.05 0.34 Q20 1 0.1525 0.6565 0.5284 11.00000 0.05 0.34 ; _shelx_res_checksum 16218 _shelx_hkl_file ; -2 0 0 34.30 4.70 -2 0 0 44.00 5.20 -2 0 0 39.20 5.30 2 0 0 33.30 7.50 -2 0 0 37.00 4.70 -3 0 0 8.30 5.10 3 0 0 5.20 5.00 -3 0 0 9.50 7.50 -4 0 0 2713.93 163.88 -4 0 0 2626.54 159.98 -4 0 0 2688.43 160.48 -4 0 0 2827.92 162.98 4 0 0 2803.62 163.58 -5 0 0 1.30 4.80 -5 0 0 -8.20 7.00 -5 0 0 9.30 3.80 -5 0 0 -1.60 6.00 5 0 0 -3.80 11.10 -5 0 0 3.10 4.30 -6 0 0 33.10 9.80 -6 0 0 47.30 10.50 -6 0 0 33.70 6.50 -6 0 0 45.50 7.50 6 0 0 35.60 10.00 -6 0 0 39.50 10.50 7 0 0 11.50 10.80 -7 0 0 0.50 8.80 -7 0 0 2.80 10.30 -7 0 0 6.40 6.80 -7 0 0 -1.60 7.40 -7 0 0 -9.90 7.60 -8 0 0 20.30 12.00 -8 0 0 75.29 15.10 8 0 0 45.50 13.70 -8 0 0 36.00 9.70 -9 0 0 3.10 15.80 -9 0 0 -2.70 19.50 -9 0 0 8.80 12.30 2 -1 0 4541.75 249.28 -2 -1 0 4251.27 248.48 -2 -1 0 4017.90 246.38 -2 -1 0 4130.29 246.48 2 -1 0 4483.65 248.08 2 -1 0 4099.89 246.58 2 -1 0 4150.38 246.58 -2 1 0 4040.10 246.88 -2 1 0 4319.27 248.98 2 1 0 4440.06 248.68 -2 1 0 4161.88 246.88 -3 -1 0 30.50 5.80 -3 -1 0 23.70 4.60 3 -1 0 20.50 6.10 3 -1 0 31.80 8.10 -3 -1 0 28.90 5.80 3 -1 0 26.90 4.10 -3 1 0 23.20 5.00 3 1 0 24.60 6.70 -3 1 0 22.20 3.90 -3 1 0 40.00 6.70 4 -1 0 159.78 16.40 -4 -1 0 180.78 13.00 -4 -1 0 150.78 13.10 -4 -1 0 152.98 11.10 -4 -1 0 149.29 13.40 4 1 0 170.98 17.20 -4 1 0 161.08 13.70 -4 1 0 161.98 11.10 -4 1 0 182.98 12.90 -4 1 0 159.68 13.70 -5 -1 0 87.19 9.30 -5 -1 0 70.69 10.70 -5 -1 0 70.89 10.50 5 -1 0 80.99 13.80 -5 -1 0 86.39 7.00 -5 1 0 80.19 11.50 -5 1 0 97.19 7.40 -5 1 0 63.09 12.80 -5 1 0 84.39 9.30 -5 1 0 99.89 11.80 5 1 0 94.49 14.90 -6 -1 0 370.66 27.50 -6 -1 0 371.86 26.20 -6 -1 0 354.46 23.80 -6 -1 0 400.96 28.40 -6 -1 0 346.17 25.90 6 -1 0 404.66 31.20 -6 1 0 362.46 26.70 -6 1 0 388.36 28.80 -6 1 0 348.87 27.20 6 1 0 419.16 31.90 -6 1 0 361.76 24.10 -6 1 0 416.26 27.40 -7 -1 0 51.39 11.30 7 -1 0 23.90 11.00 -7 -1 0 52.79 12.70 -7 -1 0 40.90 8.90 -7 -1 0 42.50 11.50 -7 -1 0 43.40 8.40 7 1 0 30.00 12.20 -7 1 0 49.30 12.20 -7 1 0 36.40 9.10 -7 1 0 43.10 9.50 -8 -1 0 9.20 11.70 -8 -1 0 10.10 12.30 8 -1 0 7.60 12.50 -8 -1 0 -4.00 8.00 -8 -1 0 17.00 8.70 -8 -1 0 5.50 10.40 -8 1 0 18.20 13.40 -8 1 0 6.40 9.00 -8 1 0 16.30 10.20 8 1 0 -2.20 14.30 -8 1 0 9.70 10.30 -8 1 0 11.70 12.80 -9 -1 0 -18.80 12.40 9 -1 0 -5.60 22.40 -9 -1 0 -11.10 15.10 -9 -1 0 18.30 9.40 -9 -1 0 11.80 11.80 -9 1 0 13.40 13.40 -9 1 0 5.70 17.30 -9 1 0 -2.10 16.50 -1 -2 0 3681.63 237.98 -1 -2 0 4153.88 237.88 -1 2 0 4409.56 238.68 -1 2 0 4031.60 238.48 -1 2 0 4499.45 239.08 -1 2 0 3782.32 238.48 -2 -2 0 22.50 4.60 -2 -2 0 19.50 4.40 2 -2 0 24.70 6.00 2 -2 0 26.80 6.70 2 -2 0 30.80 5.50 2 -2 0 32.60 6.10 -2 -2 0 17.20 4.50 -2 -2 0 22.30 4.30 -2 2 0 24.20 4.50 -2 2 0 35.70 5.90 -2 2 0 19.70 5.90 2 2 0 30.40 6.50 -2 2 0 32.30 5.00 -3 -2 0 399.76 25.70 -3 -2 0 375.76 23.90 3 -2 0 391.66 24.00 3 -2 0 409.46 29.10 -3 -2 0 331.67 23.90 3 -2 0 402.26 26.50 -3 -2 0 360.86 23.90 -3 2 0 406.76 26.20 -3 2 0 411.96 25.10 -3 2 0 396.16 24.10 3 2 0 363.26 27.70 -3 2 0 364.16 24.80 -3 2 0 358.26 25.70 -4 -2 0 575.74 36.00 4 -2 0 568.84 36.80 -4 -2 0 511.65 33.00 4 -2 0 555.24 42.80 4 -2 0 529.55 32.90 -4 -2 0 522.25 33.80 4 -2 0 539.05 33.00 -4 2 0 471.65 36.00 -4 2 0 532.85 34.80 -4 2 0 553.94 36.70 4 2 0 591.44 38.70 -4 2 0 579.74 33.70 -5 -2 0 223.38 18.50 -5 -2 0 197.08 17.40 5 -2 0 227.68 21.00 -5 -2 0 208.78 17.10 -5 -2 0 230.88 14.90 -5 2 0 255.27 20.40 -5 2 0 224.18 15.40 -5 2 0 252.77 17.30 5 2 0 260.27 23.00 -5 2 0 215.48 20.00 -5 2 0 225.88 18.70 -6 -2 0 73.99 10.40 6 -2 0 97.39 15.80 -6 -2 0 95.09 12.30 -6 -2 0 108.39 8.30 -6 -2 0 85.49 11.50 -6 -2 0 81.89 8.50 -6 2 0 86.89 11.10 -6 2 0 123.49 14.70 -6 2 0 76.09 9.40 -6 2 0 103.49 13.10 6 2 0 108.39 19.30 -7 -2 0 5.90 6.50 7 -2 0 18.60 10.30 -7 -2 0 3.00 6.40 -7 -2 0 9.30 8.00 -7 -2 0 4.90 5.40 -7 -2 0 5.10 9.00 -7 -2 0 18.30 9.30 -7 2 0 12.10 6.90 -7 2 0 -0.40 9.00 7 2 0 0.60 11.10 -7 2 0 7.50 11.40 -7 2 0 5.80 8.50 -7 2 0 4.30 11.00 -8 -2 0 31.50 11.80 8 -2 0 9.50 12.70 -8 -2 0 23.50 8.80 -8 -2 0 26.40 7.70 -8 -2 0 26.90 11.60 -8 -2 0 21.40 7.10 -8 -2 0 26.40 15.70 8 2 0 -1.60 15.50 -8 2 0 21.80 13.80 -8 2 0 15.30 12.90 -8 2 0 18.90 11.40 -8 2 0 16.20 9.30 9 -2 0 19.50 18.80 -9 -2 0 28.90 11.80 -9 -2 0 4.90 8.50 -9 -2 0 1.20 13.70 -9 -2 0 20.20 15.00 -9 2 0 24.10 14.10 -9 2 0 -6.10 16.30 -9 2 0 12.00 17.70 0 -3 0 -0.60 2.60 0 -3 0 -1.70 4.50 0 -3 0 0.10 3.60 0 -3 0 1.90 4.80 0 3 0 1.80 2.80 0 3 0 0.50 4.20 0 3 0 1.40 3.80 1 -3 0 1020.10 58.59 1 -3 0 1030.70 58.99 1 -3 0 1023.40 59.99 -1 -3 0 1029.80 58.19 1 -3 0 954.80 58.59 1 -3 0 954.70 58.59 -1 -3 0 950.60 57.59 -1 -3 0 910.41 57.79 -1 3 0 1007.70 59.19 1 3 0 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21 17.30 21.50 -4 2 21 18.00 22.90 4 2 -21 2.40 27.50 4 2 -21 4.70 19.40 4 2 -21 -29.60 23.00 3 -2 -21 -24.60 18.00 3 -2 -21 -11.40 19.50 3 -2 -21 -7.40 22.20 -3 -2 21 23.00 20.20 -3 -2 21 6.30 16.20 -3 2 21 11.20 20.70 3 2 -21 -27.10 19.40 3 2 -21 6.00 19.10 3 2 -21 10.50 23.90 -2 -2 21 4.60 19.50 2 -2 -21 13.80 22.40 2 -2 -21 -6.90 20.10 2 2 -21 34.90 23.60 2 2 -21 24.90 19.20 -2 2 21 5.20 31.50 2 2 -21 13.30 17.40 -2 2 21 31.00 21.00 -1 -2 21 37.30 31.90 1 -2 -21 30.50 28.90 1 -2 -21 -2.80 16.10 -1 -2 21 70.59 17.40 1 -2 -21 28.10 19.40 1 2 -21 86.49 22.30 1 2 -21 35.20 20.30 0 -2 -21 12.20 22.80 0 -2 -21 -0.30 20.60 0 -2 21 29.50 19.20 0 2 -21 -1.20 19.10 0 2 -21 12.60 21.90 -4 -3 21 28.60 22.00 4 -3 -21 35.50 24.40 4 -3 -21 -15.30 19.90 4 3 -21 -18.50 23.40 -4 3 21 40.20 23.40 4 3 -21 37.20 25.80 4 3 -21 23.40 19.20 3 -3 -21 -20.30 19.80 3 -3 -21 -12.40 20.00 3 -3 -21 11.90 23.00 -3 -3 21 8.50 19.80 -3 3 21 23.70 22.80 3 3 -21 -0.70 18.60 3 3 -21 -7.20 24.50 2 -3 -21 -21.30 17.80 2 -3 -21 -8.20 19.20 2 -3 -21 11.90 22.50 -2 -3 21 4.20 19.20 -2 3 21 -1.10 22.60 2 3 -21 -9.70 22.90 -2 3 21 33.10 30.60 2 3 -21 10.30 19.60 1 -3 -21 45.70 22.60 1 -3 -21 -2.70 21.40 -1 -3 21 43.40 37.80 -1 -3 21 -6.60 25.40 1 3 -21 9.30 23.20 1 3 -21 5.10 18.80 0 -3 21 54.09 19.80 0 -3 -21 57.59 22.50 0 -3 -21 10.70 20.60 0 3 -21 5.50 22.00 0 3 -21 7.70 20.90 4 -4 -21 27.60 24.20 -4 -4 21 -2.00 23.90 -4 4 21 23.70 26.20 4 4 -21 11.10 20.30 4 4 -21 11.70 26.90 3 -4 -21 -10.70 18.50 -3 -4 21 -3.40 21.30 3 -4 -21 24.60 24.00 3 -4 -21 -27.20 19.00 3 4 -21 8.00 20.60 3 4 -21 18.40 53.09 3 4 -21 8.50 25.50 -3 4 21 -8.40 22.00 2 -4 -21 17.70 19.80 2 -4 -21 54.69 18.30 -2 -4 21 66.69 19.50 2 -4 -21 72.39 23.30 2 4 -21 106.19 24.10 -2 4 21 84.69 34.10 -2 4 21 72.99 23.20 2 4 -21 62.89 20.30 1 -4 -21 16.30 23.00 -1 -4 21 -4.30 35.00 1 -4 -21 -7.50 20.80 -1 -4 21 13.50 21.10 1 4 -21 3.70 19.50 -1 4 21 6.10 16.20 1 4 -21 24.60 23.60 0 -4 -21 50.79 23.20 0 -4 21 52.49 18.90 0 -4 -21 8.50 22.70 0 4 -21 5.60 20.80 0 4 -21 39.20 25.00 3 -5 -21 5.70 23.90 -3 -5 21 12.70 22.10 3 -5 -21 -37.10 21.00 3 5 -21 -21.00 25.60 -3 5 21 0.90 22.00 3 5 -21 -1.10 21.10 2 -5 -21 21.50 23.90 -2 -5 21 8.30 20.90 2 -5 -21 -10.20 21.00 2 -5 -21 -6.70 18.30 -2 -5 21 16.00 17.30 2 5 -21 20.10 24.50 -2 5 21 10.70 25.50 2 5 -21 8.50 20.00 1 -5 -21 11.30 23.30 -1 -5 21 8.80 18.60 1 -5 -21 -2.90 21.50 1 5 -21 5.00 21.30 -1 5 21 -1.20 20.90 1 5 -21 9.60 25.20 2 -6 -21 -28.00 21.80 2 -6 -21 15.10 17.90 -2 -6 21 2.50 21.60 2 -6 -21 25.40 24.00 2 6 -21 16.00 25.70 -2 6 21 -7.80 23.50 2 6 -21 11.30 21.40 3 0 -22 28.30 26.90 3 0 -22 -3.30 22.30 -3 0 22 -13.00 23.10 2 0 -22 9.10 26.60 2 0 -22 10.70 23.30 -2 0 22 1.40 21.10 1 0 -22 4.80 21.20 3 -1 -22 -17.50 21.60 3 1 -22 -0.30 21.80 2 -1 -22 5.50 22.60 2 -1 -22 20.00 27.20 -2 -1 22 37.10 21.70 2 1 -22 12.00 20.90 -2 1 22 15.30 20.90 2 1 -22 15.80 26.40 2 -2 -22 3.10 22.50 2 -2 -22 27.60 25.90 2 2 -22 6.80 22.80 2 2 -22 17.00 26.20 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 55962 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 Sb1 Sb 0.13834(8) 0.80755(4) 0.55120(3) 0.0666(3) Uani 1 1 d D . . . . F1 F 0.117(4) 0.890(2) 0.617(2) 0.151(13) Uani 0.497(19) 1 d D U P A 1 F2 F 0.111(4) 0.8969(12) 0.4862(12) 0.151(8) Uani 0.497(19) 1 d D U P A 1 F3 F 0.3629(19) 0.8300(18) 0.5748(19) 0.174(9) Uani 0.497(19) 1 d D U P A 1 F4 F 0.164(5) 0.7202(17) 0.4932(19) 0.199(12) Uani 0.497(19) 1 d D U P A 1 F5 F 0.148(4) 0.7348(16) 0.6267(13) 0.167(8) Uani 0.497(19) 1 d D U P A 1 F6 F -0.0945(15) 0.8025(12) 0.5346(15) 0.146(8) Uani 0.497(19) 1 d D U P A 1 F1' F 0.064(4) 0.866(2) 0.6219(18) 0.160(12) Uani 0.503(19) 1 d D U P A 2 F2' F 0.223(4) 0.8980(16) 0.5133(19) 0.208(11) Uani 0.503(19) 1 d D U P A 2 F3' F 0.340(2) 0.7903(15) 0.6206(13) 0.147(8) Uani 0.503(19) 1 d D U P A 2 F4' F 0.223(5) 0.7608(19) 0.4773(16) 0.206(13) Uani 0.503(19) 1 d D U P A 2 F5' F 0.092(4) 0.7067(12) 0.5870(15) 0.176(9) Uani 0.503(19) 1 d D U P A 2 F6' F -0.045(3) 0.8084(15) 0.4779(13) 0.172(9) Uani 0.503(19) 1 d D U P A 2 C1 C 0.6150(10) 0.4949(6) 0.4049(4) 0.062(2) Uani 1 1 d . . . . . C2 C 0.7629(12) 0.5083(8) 0.4596(5) 0.086(3) Uani 1 1 d . . . . . H2 H 0.850462 0.469984 0.465506 0.104 Uiso 1 1 calc R U . . . C3 C 0.7767(14) 0.5763(9) 0.5029(6) 0.096(4) Uani 1 1 d . . . . . H3 H 0.874629 0.584470 0.539249 0.115 Uiso 1 1 calc R U . . . C4 C 0.6521(16) 0.6342(7) 0.4956(5) 0.090(4) Uani 1 1 d . . . . . H4 H 0.666804 0.680779 0.527165 0.108 Uiso 1 1 calc R U . . . C5 C 0.5007(12) 0.6252(6) 0.4412(5) 0.074(3) Uani 1 1 d . . . . . H5 H 0.416717 0.665627 0.434267 0.089 Uiso 1 1 calc R U . . . C6 C 0.4852(10) 0.5520(5) 0.3986(4) 0.056(2) Uani 1 1 d . . . . . C7 C 0.5674(10) 0.4324(6) 0.3496(5) 0.063(2) Uani 1 1 d . . . . . H7 H 0.633219 0.387105 0.341738 0.076 Uiso 1 1 calc R U . . . C8 C 0.4123(9) 0.4487(5) 0.3103(4) 0.0506(18) Uani 1 1 d . . . . . C9 C 0.2969(9) 0.4057(4) 0.2463(4) 0.0474(17) Uani 1 1 d . . . . . C10 C 0.1726(9) 0.3429(5) 0.2726(4) 0.0543(19) Uani 1 1 d . . . . . H10 H 0.131134 0.368302 0.314365 0.065 Uiso 1 1 calc R U . . . C11 C 0.0299(10) 0.3409(4) 0.2029(4) 0.0533(19) Uani 1 1 d . . . . . C12 C 0.0364(9) 0.4072(5) 0.1589(4) 0.0527(19) Uani 1 1 d . . . . . C13 C 0.1745(8) 0.4663(4) 0.1963(4) 0.0432(16) Uani 1 1 d . . . . . C14 C 0.2478(11) 0.5255(5) 0.1458(4) 0.063(2) Uani 1 1 d . . . . . H14A H 0.283137 0.493939 0.106837 0.095 Uiso 1 1 calc R U . . . H14B H 0.342506 0.554401 0.175411 0.095 Uiso 1 1 calc R U . . . H14C H 0.164070 0.565385 0.123182 0.095 Uiso 1 1 calc R U . . . C15 C 0.4066(11) 0.3611(5) 0.1984(5) 0.068(2) Uani 1 1 d . . . . . H15A H 0.473241 0.401787 0.179026 0.103 Uiso 1 1 calc R U . . . H15B H 0.335602 0.332415 0.157068 0.103 Uiso 1 1 calc R U . . . H15C H 0.479029 0.321544 0.229229 0.103 Uiso 1 1 calc R U . . . C16 C 0.2481(13) 0.2588(5) 0.2978(5) 0.080(3) Uani 1 1 d . . . . . H16A H 0.175896 0.229449 0.324397 0.119 Uiso 1 1 calc R U . . . H16B H 0.356175 0.266648 0.330543 0.119 Uiso 1 1 calc R U . . . H16C H 0.260404 0.226915 0.254443 0.119 Uiso 1 1 calc R U . . . C17 C -0.0971(12) 0.2735(6) 0.1919(6) 0.081(3) Uani 1 1 d . . . . . H17A H -0.158259 0.275652 0.231641 0.122 Uiso 1 1 calc R U . . . H17B H -0.042206 0.220236 0.192883 0.122 Uiso 1 1 calc R U . . . H17C H -0.173300 0.280743 0.144100 0.122 Uiso 1 1 calc R U . . . C18 C -0.0709(11) 0.4246(6) 0.0814(4) 0.081(3) Uani 1 1 d . . . . . H18A H -0.180628 0.401202 0.078133 0.121 Uiso 1 1 calc R U . . . H18B H -0.019951 0.399711 0.043647 0.121 Uiso 1 1 calc R U . . . H18C H -0.080113 0.483928 0.073435 0.121 Uiso 1 1 calc R U . . . C19 C 0.1932(9) 0.5499(4) 0.3192(4) 0.0445(17) Uani 1 1 d . . . . . C20 C 0.1184(10) 0.6005(5) 0.3646(4) 0.058(2) Uani 1 1 d . . . . . H20 H 0.180227 0.618005 0.411179 0.070 Uiso 1 1 calc R U . . . C21 C -0.0428(12) 0.6248(5) 0.3421(5) 0.071(2) Uani 1 1 d . . . . . H21 H -0.091742 0.658688 0.373077 0.085 Uiso 1 1 calc R U . . . C22 C -0.1347(11) 0.5993(6) 0.2732(5) 0.077(3) Uani 1 1 d . . . . . H22 H -0.245392 0.616412 0.256543 0.092 Uiso 1 1 calc R U . . . C23 C -0.0594(11) 0.5482(5) 0.2295(5) 0.065(2) Uani 1 1 d . . . . . H23 H -0.121745 0.529952 0.183267 0.078 Uiso 1 1 calc R U . . . N1 N 0.3562(7) 0.5235(4) 0.3384(3) 0.0466(14) Uani 1 1 d . . . . . N2 N 0.1028(7) 0.5233(3) 0.2514(3) 0.0438(14) 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 Sb1 0.0739(4) 0.0680(4) 0.0572(4) -0.0115(3) 0.0129(3) -0.0122(3) F1 0.073(15) 0.20(2) 0.16(2) -0.101(18) -0.025(12) 0.042(14) F2 0.19(2) 0.143(13) 0.136(14) 0.050(11) 0.080(14) 0.007(14) F3 0.078(10) 0.19(2) 0.27(2) -0.035(17) 0.068(13) -0.007(11) F4 0.29(2) 0.133(18) 0.177(19) -0.121(17) 0.056(15) 0.008(17) F5 0.20(2) 0.163(17) 0.139(15) 0.053(14) 0.043(15) 0.050(15) F6 0.092(10) 0.152(13) 0.177(19) -0.026(15) -0.009(11) -0.039(9) F1' 0.11(2) 0.27(3) 0.113(14) -0.005(15) 0.048(15) 0.078(19) F2' 0.19(2) 0.168(16) 0.26(2) 0.033(16) 0.039(19) -0.071(17) F3' 0.081(10) 0.159(17) 0.170(16) -0.063(13) -0.043(10) 0.042(10) F4' 0.32(3) 0.16(2) 0.141(15) -0.020(17) 0.070(17) 0.07(2) F5' 0.205(18) 0.109(12) 0.182(19) 0.022(13) -0.034(16) -0.050(12) F6' 0.135(14) 0.206(16) 0.127(14) -0.009(14) -0.077(11) 0.010(13) C1 0.053(5) 0.078(6) 0.054(5) 0.016(4) 0.007(4) -0.013(5) C2 0.070(6) 0.124(9) 0.060(6) 0.018(6) 0.003(5) -0.029(6) C3 0.077(7) 0.141(11) 0.063(6) -0.003(7) 0.001(5) -0.048(8) C4 0.128(9) 0.096(8) 0.048(5) -0.022(5) 0.026(6) -0.066(8) C5 0.087(6) 0.069(6) 0.066(5) -0.020(5) 0.015(5) -0.028(5) C6 0.062(5) 0.062(5) 0.042(4) -0.002(4) 0.007(4) -0.023(4) C7 0.052(5) 0.068(5) 0.069(5) 0.004(5) 0.011(4) 0.000(4) C8 0.048(4) 0.050(4) 0.055(4) -0.002(4) 0.014(4) -0.006(3) C9 0.053(4) 0.043(4) 0.046(4) -0.008(3) 0.011(3) 0.006(3) C10 0.062(5) 0.045(4) 0.058(5) 0.005(4) 0.018(4) 0.004(4) C11 0.065(5) 0.035(4) 0.063(5) -0.011(4) 0.020(4) -0.005(4) C12 0.056(5) 0.050(5) 0.050(4) -0.014(4) 0.007(3) -0.006(4) C13 0.045(4) 0.041(4) 0.044(4) -0.003(3) 0.011(3) -0.003(3) C14 0.086(6) 0.056(5) 0.053(5) 0.003(4) 0.027(4) -0.009(4) C15 0.072(6) 0.072(6) 0.066(5) -0.017(5) 0.023(4) 0.008(5) C16 0.116(8) 0.041(5) 0.084(6) 0.003(5) 0.026(6) 0.010(5) C17 0.092(7) 0.063(6) 0.094(7) -0.015(5) 0.031(6) -0.039(5) C18 0.081(6) 0.095(7) 0.053(5) -0.005(5) -0.013(4) -0.013(5) C19 0.067(5) 0.025(3) 0.043(4) 0.000(3) 0.014(3) -0.001(3) C20 0.076(6) 0.052(5) 0.049(4) -0.001(4) 0.020(4) 0.012(4) C21 0.100(7) 0.065(6) 0.056(5) 0.007(4) 0.035(5) 0.028(5) C22 0.069(6) 0.085(7) 0.078(6) 0.014(5) 0.017(5) 0.044(5) C23 0.070(5) 0.066(5) 0.057(5) 0.004(4) 0.008(4) 0.018(4) N1 0.050(4) 0.043(3) 0.046(3) -0.007(3) 0.010(3) -0.001(3) N2 0.049(3) 0.040(3) 0.043(3) -0.001(3) 0.009(3) 0.003(3) 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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 F5 Sb1 F4 87.2(14) . . ? F6' Sb1 F1' 99.9(15) . . ? F6' Sb1 F4' 81.0(16) . . ? F1' Sb1 F4' 173.0(17) . . ? F6' Sb1 F2' 92.2(12) . . ? F1' Sb1 F2' 93.9(18) . . ? F4' Sb1 F2' 79.1(17) . . ? F6' Sb1 F5' 93.8(11) . . ? F1' Sb1 F5' 94.6(17) . . ? F4' Sb1 F5' 92.3(14) . . ? F2' Sb1 F5' 168.6(16) . . ? F5 Sb1 F1 88.0(18) . . ? F4 Sb1 F1 175(2) . . ? F5 Sb1 F3 93.9(13) . . ? F4 Sb1 F3 93.1(14) . . ? F1 Sb1 F3 86.4(12) . . ? F5 Sb1 F2 168.3(11) . . ? F4 Sb1 F2 104.1(15) . . ? F1 Sb1 F2 80.8(17) . . ? F3 Sb1 F2 88.8(11) . . ? F5 Sb1 F6 88.5(11) . . ? F4 Sb1 F6 96.6(13) . . ? F1 Sb1 F6 84.1(11) . . ? F3 Sb1 F6 170.1(11) . . ? F2 Sb1 F6 87.0(10) . . ? F6' Sb1 F3' 170.4(10) . . ? F1' Sb1 F3' 88.8(14) . . ? F4' Sb1 F3' 90.9(15) . . ? F2' Sb1 F3' 91.3(11) . . ? F5' Sb1 F3' 81.3(10) . . ? C6 C1 C2 119.0(9) . . ? C6 C1 C7 108.6(7) . . ? C2 C1 C7 132.4(10) . . ? C3 C2 C1 119.5(11) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C2 C3 C4 122.1(10) . . ? C2 C3 H3 119.0 . . ? C4 C3 H3 119.0 . . ? C3 C4 C5 121.4(10) . . ? C3 C4 H4 119.3 . . ? C5 C4 H4 119.3 . . ? C6 C5 C4 115.8(10) . . ? C6 C5 H5 122.1 . . ? C4 C5 H5 122.1 . . ? C1 C6 C5 122.1(8) . . ? C1 C6 N1 106.3(7) . . ? C5 C6 N1 131.3(8) . . ? C8 C7 C1 109.0(8) . . ? C8 C7 H7 125.5 . . ? C1 C7 H7 125.5 . . ? C7 C8 N1 108.3(7) . . ? C7 C8 C9 133.6(7) . . ? N1 C8 C9 118.0(6) . . ? C8 C9 C13 112.9(6) . . ? C8 C9 C15 107.7(6) . . ? C13 C9 C15 109.8(6) . . ? C8 C9 C10 113.4(6) . . ? C13 C9 C10 101.6(5) . . ? C15 C9 C10 111.4(6) . . ? C16 C10 C11 115.0(7) . . ? C16 C10 C9 114.4(7) . . ? C11 C10 C9 100.9(6) . . ? C16 C10 H10 108.7 . . ? C11 C10 H10 108.7 . . ? C9 C10 H10 108.7 . . ? C12 C11 C17 127.9(8) . . ? C12 C11 C10 111.0(6) . . ? C17 C11 C10 121.0(7) . . ? C11 C12 C18 127.8(7) . . ? C11 C12 C13 110.4(6) . . ? C18 C12 C13 121.9(7) . . ? C12 C13 C14 117.8(6) . . ? C12 C13 C9 101.4(6) . . ? C14 C13 C9 117.1(6) . . ? C12 C13 N2 107.9(5) . . ? C14 C13 N2 105.8(5) . . ? C9 C13 N2 106.0(5) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C9 C15 H15A 109.5 . . ? C9 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C9 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C10 C16 H16A 109.5 . . ? C10 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C10 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C11 C17 H17A 109.5 . . ? C11 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C11 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C12 C18 H18A 109.5 . . ? C12 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C12 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N2 C19 N1 116.4(6) . . ? N2 C19 C20 119.8(7) . . ? N1 C19 C20 123.8(7) . . ? C21 C20 C19 120.9(8) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C20 C21 C22 119.8(8) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C23 C22 C21 118.5(8) . . ? C23 C22 H22 120.7 . . ? C21 C22 H22 120.7 . . ? N2 C23 C22 122.3(8) . . ? N2 C23 H23 118.8 . . ? C22 C23 H23 118.8 . . ? C19 N1 C8 122.7(6) . . ? C19 N1 C6 128.2(6) . . ? C8 N1 C6 107.8(6) . . ? C23 N2 C19 118.6(6) . . ? C23 N2 C13 117.5(6) . . ? C19 N2 C13 123.9(5) . . ? 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 Sb1 F6' 1.778(11) . ? Sb1 F5 1.786(14) . ? Sb1 F4 1.788(12) . ? Sb1 F1' 1.792(14) . ? Sb1 F4' 1.797(16) . ? Sb1 F2' 1.799(16) . ? Sb1 F5' 1.809(14) . ? Sb1 F1 1.811(13) . ? Sb1 F3 1.825(14) . ? Sb1 F2 1.834(13) . ? Sb1 F6 1.860(12) . ? Sb1 F3' 1.867(11) . ? C1 C6 1.384(11) . ? C1 C2 1.404(12) . ? C1 C7 1.410(11) . ? C2 C3 1.331(15) . ? C2 H2 0.9300 . ? C3 C4 1.360(15) . ? C3 H3 0.9300 . ? C4 C5 1.415(14) . ? C4 H4 0.9300 . ? C5 C6 1.393(11) . ? C5 H5 0.9300 . ? C6 N1 1.419(9) . ? C7 C8 1.339(10) . ? C7 H7 0.9300 . ? C8 N1 1.414(9) . ? C8 C9 1.496(10) . ? C9 C13 1.540(9) . ? C9 C15 1.548(10) . ? C9 C10 1.571(10) . ? C10 C16 1.508(10) . ? C10 C11 1.525(11) . ? C10 H10 0.9800 . ? C11 C12 1.334(10) . ? C11 C17 1.479(10) . ? C12 C18 1.513(10) . ? C12 C13 1.516(9) . ? C13 C14 1.525(9) . ? C13 N2 1.554(8) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 N2 1.361(8) . ? C19 N1 1.367(9) . ? C19 C20 1.385(10) . ? C20 C21 1.348(11) . ? C20 H20 0.9300 . ? C21 C22 1.374(12) . ? C21 H21 0.9300 . ? C22 C23 1.370(11) . ? C22 H22 0.9300 . ? C23 N2 1.357(9) . ? C23 H23 0.9300 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag C5 H5 F4'^b 0.93 2.44 3.30(3) 154.0 . yes C7 H7 F5^a 0.93 2.62 3.50(2) 158.9 3_666 yes C14 H14A F2^a 0.96 2.57 3.530(16) 173.6 2_545 yes C14 H14B F1'^b 0.96 2.56 3.21(3) 125.1 4_675 yes C20 H20 F4^a 0.93 2.23 2.977(18) 136.7 . yes C20 H20 F4'^b 0.93 2.57 3.28(3) 133.3 . yes C22 H22 F1^a 0.93 2.54 3.12(3) 120.3 4_575 yes C22 H22 F1'^b 0.93 2.61 3.31(4) 132.6 4_575 yes C23 H23 F1^a 0.93 2.56 3.13(3) 120.5 4_575 yes 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 C6 C1 C2 C3 -1.5(13) . . . . ? C7 C1 C2 C3 176.6(9) . . . . ? C1 C2 C3 C4 -0.6(15) . . . . ? C2 C3 C4 C5 -0.2(16) . . . . ? C3 C4 C5 C6 2.9(13) . . . . ? C2 C1 C6 C5 4.4(12) . . . . ? C7 C1 C6 C5 -174.1(7) . . . . ? C2 C1 C6 N1 178.6(7) . . . . ? C7 C1 C6 N1 0.2(9) . . . . ? C4 C5 C6 C1 -4.9(12) . . . . ? C4 C5 C6 N1 -177.6(8) . . . . ? C6 C1 C7 C8 -0.8(9) . . . . ? C2 C1 C7 C8 -179.0(9) . . . . ? C1 C7 C8 N1 1.1(9) . . . . ? C1 C7 C8 C9 -179.6(8) . . . . ? C7 C8 C9 C13 -151.9(8) . . . . ? N1 C8 C9 C13 27.4(9) . . . . ? C7 C8 C9 C15 -30.5(12) . . . . ? N1 C8 C9 C15 148.8(6) . . . . ? C7 C8 C9 C10 93.2(10) . . . . ? N1 C8 C9 C10 -87.5(8) . . . . ? C8 C9 C10 C16 -80.5(8) . . . . ? C13 C9 C10 C16 158.1(7) . . . . ? C15 C9 C10 C16 41.2(9) . . . . ? C8 C9 C10 C11 155.5(6) . . . . ? C13 C9 C10 C11 34.0(6) . . . . ? C15 C9 C10 C11 -82.8(7) . . . . ? C16 C10 C11 C12 -142.5(7) . . . . ? C9 C10 C11 C12 -18.9(8) . . . . ? C16 C10 C11 C17 39.7(11) . . . . ? C9 C10 C11 C17 163.3(7) . . . . ? C17 C11 C12 C18 -8.7(14) . . . . ? C10 C11 C12 C18 173.7(8) . . . . ? C17 C11 C12 C13 172.6(7) . . . . ? C10 C11 C12 C13 -5.0(9) . . . . ? C11 C12 C13 C14 156.5(7) . . . . ? C18 C12 C13 C14 -22.3(10) . . . . ? C11 C12 C13 C9 27.3(8) . . . . ? C18 C12 C13 C9 -151.5(7) . . . . ? C11 C12 C13 N2 -83.9(7) . . . . ? C18 C12 C13 N2 97.3(8) . . . . ? C8 C9 C13 C12 -158.7(6) . . . . ? C15 C9 C13 C12 81.1(7) . . . . ? C10 C9 C13 C12 -36.9(6) . . . . ? C8 C9 C13 C14 71.6(8) . . . . ? C15 C9 C13 C14 -48.5(8) . . . . ? C10 C9 C13 C14 -166.5(6) . . . . ? C8 C9 C13 N2 -46.1(7) . . . . ? C15 C9 C13 N2 -166.3(6) . . . . ? C10 C9 C13 N2 75.7(6) . . . . ? N2 C19 C20 C21 -0.8(11) . . . . ? N1 C19 C20 C21 179.5(7) . . . . ? C19 C20 C21 C22 -0.2(13) . . . . ? C20 C21 C22 C23 1.1(14) . . . . ? C21 C22 C23 N2 -1.2(14) . . . . ? N2 C19 N1 C8 -26.3(9) . . . . ? C20 C19 N1 C8 153.4(7) . . . . ? N2 C19 N1 C6 168.7(6) . . . . ? C20 C19 N1 C6 -11.6(11) . . . . ? C7 C8 N1 C19 -168.6(7) . . . . ? C9 C8 N1 C19 11.9(10) . . . . ? C7 C8 N1 C6 -1.0(8) . . . . ? C9 C8 N1 C6 179.6(6) . . . . ? C1 C6 N1 C19 167.3(7) . . . . ? C5 C6 N1 C19 -19.2(13) . . . . ? C1 C6 N1 C8 0.5(8) . . . . ? C5 C6 N1 C8 174.0(8) . . . . ? C22 C23 N2 C19 0.3(12) . . . . ? C22 C23 N2 C13 -179.1(7) . . . . ? N1 C19 N2 C23 -179.6(6) . . . . ? C20 C19 N2 C23 0.7(10) . . . . ? N1 C19 N2 C13 -0.2(9) . . . . ? C20 C19 N2 C13 -179.9(6) . . . . ? C12 C13 N2 C23 -37.0(8) . . . . ? C14 C13 N2 C23 90.0(7) . . . . ? C9 C13 N2 C23 -145.0(6) . . . . ? C12 C13 N2 C19 143.6(6) . . . . ? C14 C13 N2 C19 -89.4(7) . . . . ? C9 C13 N2 C19 35.6(8) . . . . ?