#------------------------------------------------------------------------------ #$Date: 2021-07-31 04:51:44 +0300 (Sat, 31 Jul 2021) $ #$Revision: 267841 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/42/1564276.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_1564276 loop_ _publ_author_name 'Zhang, Mengru' 'Li, Hexin' 'Zhao, Jinbo' 'Li, Yan' 'Zhang, Qian' _publ_section_title ; Copper-catalyzed [3+1] cyclization of cyclopropenes/diazo compounds and bromodifluoroacetamides: facile synthesis of \a,\a-difluoro-\b-lactam derivatives ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D1SC02930D _journal_year 2021 _chemical_formula_moiety 'C18 H14 Cl F2 N O' _chemical_formula_sum 'C18 H14 Cl F2 N O' _chemical_formula_weight 333.75 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2019-05-24 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2020-08-09 deposited with the CCDC. 2021-07-29 downloaded from the CCDC. ; _cell_angle_alpha 70.47(3) _cell_angle_beta 79.17(4) _cell_angle_gamma 66.85(3) _cell_formula_units_Z 4 _cell_length_a 10.946(7) _cell_length_b 11.711(6) _cell_length_c 14.387(8) _cell_measurement_reflns_used 4067 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 63.16 _cell_measurement_theta_min 4.29 _cell_volume 1594.8(16) _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 292.73 _diffrn_measured_fraction_theta_full 0.955 _diffrn_measured_fraction_theta_max 0.921 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0931 _diffrn_reflns_av_unetI/netI 0.1071 _diffrn_reflns_Laue_measured_fraction_full 0.955 _diffrn_reflns_Laue_measured_fraction_max 0.921 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 14956 _diffrn_reflns_point_group_measured_fraction_full 0.955 _diffrn_reflns_point_group_measured_fraction_max 0.921 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 70.273 _diffrn_reflns_theta_min 3.266 _exptl_absorpt_coefficient_mu 2.343 _exptl_absorpt_correction_type none _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 1.390 _exptl_crystal_description plate _exptl_crystal_F_000 688 _refine_diff_density_max 0.277 _refine_diff_density_min -0.470 _refine_diff_density_rms 0.077 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 417 _refine_ls_number_reflns 5599 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.021 _refine_ls_R_factor_all 0.1495 _refine_ls_R_factor_gt 0.0826 _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^)+(0.0922P)^2^+1.2857P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1813 _refine_ls_wR_factor_ref 0.2199 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3203 _reflns_number_total 5599 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1sc02930d2.cif _cod_data_source_block ss _cod_original_cell_volume 1594.9(16) _cod_database_code 1564276 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C27(H27), C9(H9) 2.b Aromatic/amide H refined with riding coordinates: C36(H36), C3(H3), C23(H23), C14(H14), C28(H28), C10(H10), C2(H2), C1(H1), C5(H5), C21(H21), C24(H24), C32(H32), C33(H33), C34(H34), C6(H6), C19(H19), C18(H18), C20(H20), C16(H16), C17(H17) 2.c Idealised Me refined as rotating group: C12(H12A,H12B,H12C), C30(H30A,H30B,H30C) ; _shelx_res_file ; ss.res created by SHELXL-2014/7 TITL ss_a.res in P-1 REM Old TITL ss in P-1 #2 REM SHELXT solution in P-1 REM R1 0.238, Rweak 0.098, Alpha 0.071, Orientation as input REM Formula found by SHELXT: C36 N2 O3 F3 Cl2 CELL 1.54178 10.9464 11.7112 14.3873 70.47 79.175 66.847 ZERR 4 0.0066 0.006 0.0075 0.033 0.036 0.034 LATT 1 SFAC C H Cl F N O UNIT 72 56 4 8 4 4 L.S. 8 PLAN 5 TEMP 19.58 BOND $H list 4 fmap 2 53 acta OMIT 4 8 15 OMIT 2 -11 1 OMIT -2 -12 2 REM REM REM WGHT 0.092200 1.285700 FVAR 0.52310 CL2 3 1.272084 0.967976 0.433901 11.00000 0.07897 0.07954 = 0.05440 -0.01576 0.00163 -0.03036 CL1 3 0.114266 0.840133 1.004262 11.00000 0.07774 0.07717 = 0.08746 -0.04458 0.01106 0.00372 F2 4 0.615303 0.363660 0.864177 11.00000 0.06853 0.07474 = 0.05823 -0.01881 -0.01270 -0.00599 F1 4 0.757966 0.325713 0.742278 11.00000 0.04072 0.08138 = 0.08623 -0.03017 -0.00628 0.00462 F4 4 0.770460 0.586123 0.760301 11.00000 0.04507 0.11419 = 0.08094 -0.03363 -0.00863 -0.02594 F3 4 0.910511 0.626498 0.638469 11.00000 0.07942 0.11602 = 0.04683 -0.02456 -0.01146 -0.02775 N2 5 1.046579 0.501962 0.833510 11.00000 0.03744 0.04624 = 0.04967 -0.01702 -0.00859 -0.00553 N1 5 0.470667 0.432582 0.681221 11.00000 0.04228 0.04739 = 0.05975 -0.02246 -0.00351 -0.00637 O2 6 1.035269 0.338692 0.777432 11.00000 0.08526 0.07260 = 0.11461 -0.05240 -0.00637 -0.02254 O1 6 0.542612 0.206202 0.752150 11.00000 0.08589 0.04846 = 0.11045 -0.02005 -0.01653 -0.01619 C22 1 1.148956 0.453753 0.896374 11.00000 0.03524 0.05049 = 0.04530 -0.01535 0.00000 -0.01177 C27 1 0.947219 0.637081 0.798517 11.00000 0.03315 0.04895 = 0.04774 -0.01400 -0.00226 -0.00349 AFIX 13 H27 2 0.882283 0.663482 0.851369 11.00000 -1.20000 AFIX 0 C9 1 0.546053 0.504416 0.699035 11.00000 0.03933 0.04991 = 0.05027 -0.01786 -0.00086 -0.01080 AFIX 13 H9 2 0.599088 0.534632 0.639924 11.00000 -1.20000 AFIX 0 C36 1 1.108903 0.924268 0.596215 11.00000 0.05273 0.04644 = 0.04443 -0.01755 -0.01302 -0.00542 AFIX 43 H36 2 1.107411 0.858745 0.574130 11.00000 -1.20000 AFIX 0 C11 1 0.466170 0.729963 0.717391 11.00000 0.03619 0.04734 = 0.05087 -0.01335 -0.00982 -0.00955 C4 1 0.369944 0.474389 0.617402 11.00000 0.03812 0.05650 = 0.04960 -0.02670 0.00468 -0.01097 C3 1 0.330865 0.599824 0.553585 11.00000 0.05287 0.05368 = 0.05221 -0.02584 -0.00263 -0.01138 AFIX 43 H3 2 0.371094 0.656399 0.553876 11.00000 -1.20000 AFIX 0 C13 1 0.397091 0.816736 0.783270 11.00000 0.04612 0.03804 = 0.05345 -0.01124 -0.01386 -0.00832 C31 1 1.036996 0.943600 0.684811 11.00000 0.05013 0.04156 = 0.04597 -0.01577 -0.01269 0.00366 C23 1 1.160446 0.532681 0.946234 11.00000 0.04886 0.05731 = 0.04243 -0.01296 -0.00579 -0.01515 AFIX 43 H23 2 1.098067 0.615965 0.939502 11.00000 -1.20000 AFIX 0 C14 1 0.294904 0.797802 0.851265 11.00000 0.04644 0.03576 = 0.06413 -0.01674 -0.01342 -0.00346 AFIX 43 H14 2 0.262312 0.734714 0.853058 11.00000 -1.20000 AFIX 0 C29 1 0.965719 0.857257 0.746789 11.00000 0.04475 0.04833 = 0.03985 -0.01664 -0.00572 0.00379 C28 1 1.007933 0.734232 0.743242 11.00000 0.04002 0.05062 = 0.04746 -0.01850 0.00248 -0.00010 AFIX 43 H28 2 1.082923 0.708064 0.701727 11.00000 -1.20000 AFIX 0 C8 1 0.627295 0.371636 0.766774 11.00000 0.03909 0.05816 = 0.05486 -0.01964 -0.00624 0.00304 C25 1 1.002293 0.447098 0.782308 11.00000 0.04029 0.07282 = 0.06155 -0.03085 -0.00063 -0.01550 C10 1 0.470243 0.607234 0.748809 11.00000 0.03964 0.05789 = 0.04775 -0.02364 0.00456 -0.01508 AFIX 43 H10 2 0.421006 0.583999 0.807318 11.00000 -1.20000 AFIX 0 C35 1 1.180416 0.998870 0.542157 11.00000 0.05983 0.04657 = 0.04769 -0.01161 -0.01332 -0.01215 C26 1 0.897369 0.578785 0.738431 11.00000 0.03925 0.08137 = 0.05473 -0.02621 -0.00535 -0.01777 C7 1 0.545774 0.312009 0.737246 11.00000 0.04986 0.05667 = 0.06576 -0.02443 -0.00325 -0.00651 C2 1 0.232877 0.640190 0.490128 11.00000 0.05840 0.05467 = 0.05842 -0.02567 -0.00600 -0.00448 AFIX 43 H2 2 0.207664 0.724125 0.447587 11.00000 -1.20000 AFIX 0 C15 1 0.239604 0.871490 0.917326 11.00000 0.05947 0.04751 = 0.06544 -0.02232 -0.01053 0.00315 C1 1 0.172324 0.559879 0.488426 11.00000 0.04994 0.08587 = 0.06580 -0.03595 -0.00379 -0.01662 AFIX 43 H1 2 0.106586 0.588177 0.444787 11.00000 -1.20000 AFIX 0 C5 1 0.307947 0.392370 0.616056 11.00000 0.05567 0.05758 = 0.06562 -0.01688 -0.00153 -0.01848 AFIX 43 H5 2 0.332884 0.308206 0.658221 11.00000 -1.20000 AFIX 0 C21 1 1.240338 0.329476 0.907517 11.00000 0.05178 0.05716 = 0.06307 -0.02041 -0.00720 -0.00154 AFIX 43 H21 2 1.232134 0.276497 0.875032 11.00000 -1.20000 AFIX 0 C12 1 0.534781 0.785179 0.621103 11.00000 0.06594 0.05886 = 0.05769 -0.00814 -0.00449 -0.01767 AFIX 137 H12A 2 0.474267 0.867711 0.586260 11.00000 -1.50000 H12B 2 0.562090 0.726823 0.581275 11.00000 -1.50000 H12C 2 0.611480 0.796004 0.634736 11.00000 -1.50000 AFIX 0 C24 1 1.265301 0.485840 1.005595 11.00000 0.06704 0.09641 = 0.04727 -0.01012 -0.01171 -0.03698 AFIX 43 H24 2 1.274271 0.537856 1.038636 11.00000 -1.20000 AFIX 0 C32 1 1.037990 1.046166 0.713340 11.00000 0.08273 0.04577 = 0.05213 -0.01824 -0.00806 -0.00195 AFIX 43 H32 2 0.989130 1.063784 0.770434 11.00000 -1.20000 AFIX 0 C33 1 1.110405 1.120788 0.657781 11.00000 0.11405 0.04408 = 0.07930 -0.02190 -0.01064 -0.02130 AFIX 43 H33 2 1.110564 1.188082 0.678291 11.00000 -1.20000 AFIX 0 C34 1 1.183773 1.098616 0.571441 11.00000 0.09358 0.05737 = 0.06584 -0.01203 -0.00978 -0.02523 AFIX 43 H34 2 1.233525 1.149252 0.534551 11.00000 -1.20000 AFIX 0 C30 1 0.848585 0.911578 0.814123 11.00000 0.07282 0.06311 = 0.06220 -0.02773 0.00870 0.00665 AFIX 137 H30A 2 0.880530 0.913084 0.871288 11.00000 -1.50000 H30B 2 0.795286 0.857951 0.834421 11.00000 -1.50000 H30C 2 0.795651 0.998147 0.779364 11.00000 -1.50000 AFIX 0 C6 1 0.209316 0.435293 0.552304 11.00000 0.06211 0.08673 = 0.07990 -0.03940 -0.00002 -0.03262 AFIX 43 H6 2 0.167223 0.380130 0.552168 11.00000 -1.20000 AFIX 0 C19 1 1.357100 0.361241 1.015841 11.00000 0.04891 0.10947 = 0.06026 0.00019 -0.02018 -0.01740 AFIX 43 H19 2 1.427923 0.329212 1.055689 11.00000 -1.20000 AFIX 0 C18 1 0.439508 0.915332 0.780281 11.00000 0.07469 0.05991 = 0.07801 -0.01865 -0.01229 -0.02173 AFIX 43 H18 2 0.506022 0.932797 0.733577 11.00000 -1.20000 AFIX 0 C20 1 1.342658 0.285334 0.966633 11.00000 0.05604 0.07408 = 0.07766 -0.01599 -0.01621 0.00999 AFIX 43 H20 2 1.404376 0.201667 0.973912 11.00000 -1.20000 AFIX 0 C16 1 0.283582 0.966533 0.915807 11.00000 0.11211 0.05544 = 0.08347 -0.03402 -0.01628 -0.01628 AFIX 43 H16 2 0.246707 1.014933 0.960543 11.00000 -1.20000 AFIX 0 C17 1 0.382110 0.988844 0.847723 11.00000 0.11669 0.06219 = 0.10017 -0.03691 -0.00837 -0.03617 AFIX 43 H17 2 0.412158 1.053773 0.845625 11.00000 -1.20000 AFIX 0 HKLF 4 REM ss_a.res in P-1 REM R1 = 0.0826 for 3203 Fo > 4sig(Fo) and 0.1495 for all 5599 data REM 417 parameters refined using 0 restraints END WGHT 0.0922 1.2857 REM Highest difference peak 0.277, deepest hole -0.470, 1-sigma level 0.077 Q1 1 1.5288 0.0154 1.0134 11.00000 0.05 0.28 Q2 1 1.1836 0.9277 0.4575 11.00000 0.05 0.26 Q3 1 1.1365 1.0007 0.4410 11.00000 0.05 0.25 Q4 1 0.8624 0.5869 0.9022 11.00000 0.05 0.24 Q5 1 1.3784 0.9845 0.4200 11.00000 0.05 0.23 ; _shelx_res_checksum 78192 _shelx_hkl_file ; -1 0 0 154.63 16.43 -1 0 0 199.55 16.48 1 0 0 174.08 16.43 1 0 0 192.27 16.47 -2 0 0 0.72 1.12 -2 0 0 1.38 1.05 -2 0 0 0.68 0.89 2 0 0 0.78 0.65 2 0 0 0.02 1.14 -3 0 0 31.53 3.15 -3 0 0 33.39 3.73 -3 0 0 27.03 3.12 3 0 0 27.60 3.38 3 0 0 25.94 2.83 -4 0 0 177.93 16.48 -4 0 0 193.54 16.93 -4 0 0 161.09 17.43 4 0 0 186.83 16.11 4 0 0 150.08 16.80 4 0 0 181.22 16.72 -5 0 0 2.52 2.05 -5 0 0 0.09 3.87 -5 0 0 -0.63 2.06 5 0 0 -0.65 3.11 5 0 0 1.71 1.02 5 0 0 0.08 2.71 -6 0 0 85.37 7.94 -6 0 0 72.66 8.71 -6 0 0 75.26 9.76 6 0 0 87.96 7.62 6 0 0 69.97 11.42 6 0 0 77.23 9.11 -7 0 0 -2.30 4.39 -7 0 0 2.78 2.45 -7 0 0 6.49 3.70 7 0 0 7.80 8.07 7 0 0 1.55 1.89 7 0 0 2.12 3.98 -8 0 0 98.68 12.22 -8 0 0 81.17 12.04 8 0 0 102.68 11.28 -9 0 0 6.18 6.57 9 0 0 1.12 3.97 9 0 0 5.81 10.06 -10 0 0 44.85 8.92 10 0 0 44.11 7.85 -11 0 0 11.20 4.55 11 0 0 3.55 3.58 -12 0 0 11.81 6.03 12 0 0 3.71 3.23 11 -1 0 5.66 4.08 -11 1 0 2.89 4.71 10 -1 0 31.75 6.42 -10 1 0 20.75 5.46 9 -1 0 19.33 4.69 9 -1 0 8.83 12.90 -9 1 0 11.10 10.32 8 -1 0 -5.41 4.06 -8 1 0 -2.65 4.95 7 -1 0 329.07 38.19 7 -1 0 380.72 33.19 7 -1 0 391.17 34.06 -7 1 0 363.19 33.40 -7 1 0 388.51 34.31 -7 1 0 305.40 34.56 6 -1 0 48.92 4.32 6 -1 0 37.71 6.07 6 -1 0 43.10 8.10 -6 1 0 39.08 6.25 -6 1 0 32.63 6.40 -6 1 0 41.88 4.87 5 -1 0 168.34 15.59 5 -1 0 170.69 16.92 5 -1 0 170.76 16.37 -5 1 0 168.25 16.47 -5 1 0 169.77 16.66 4 -1 0 134.30 13.26 4 -1 0 149.50 12.46 4 -1 0 124.27 13.11 -4 1 0 121.26 13.35 -4 1 0 144.89 13.10 -4 1 0 133.21 12.81 3 -1 0 14.18 2.88 3 -1 0 18.41 1.88 -3 1 0 18.32 2.17 -3 1 0 18.11 2.55 2 -1 0 170.54 15.08 2 -1 0 152.88 15.33 -2 1 0 178.85 15.34 -2 1 0 157.93 15.13 1 -1 0 0.48 0.66 -1 1 0 0.07 0.65 0 -1 0 867.27 78.71 -1 -1 0 640.23 59.38 1 1 0 692.70 59.37 1 1 0 614.80 59.33 1 1 0 665.42 59.36 -2 -1 0 873.31 71.24 -2 -1 0 740.80 71.07 -2 -1 0 698.00 71.04 2 1 0 815.85 71.15 -3 -1 0 1.45 1.11 -3 -1 0 -0.12 0.86 -3 -1 0 2.13 1.57 3 1 0 -0.16 1.15 3 1 0 0.40 0.74 -4 -1 0 233.92 23.15 -4 -1 0 264.55 23.07 4 1 0 244.07 22.93 4 1 0 262.01 23.38 -5 -1 0 33.44 5.94 -5 -1 0 24.86 5.87 -5 -1 0 21.05 3.30 5 1 0 26.06 4.43 5 1 0 27.77 4.41 -6 -1 0 265.23 25.17 -6 -1 0 257.53 26.17 6 1 0 276.47 25.57 6 1 0 274.21 25.70 -7 -1 0 20.72 4.35 -7 -1 0 26.33 5.69 -7 -1 0 20.12 3.22 7 1 0 20.17 6.13 7 1 0 20.83 3.15 7 1 0 17.33 4.61 -8 -1 0 1.28 4.09 -8 -1 0 0.17 5.15 -8 -1 0 -0.15 3.24 8 1 0 1.43 4.13 8 1 0 7.62 5.56 -9 -1 0 1.15 6.34 9 1 0 -5.99 9.16 9 1 0 -0.01 5.03 -10 -1 0 1.10 6.06 10 1 0 6.20 4.13 10 1 0 11.86 14.28 -11 -1 0 20.69 6.66 11 1 0 13.53 4.56 -12 -1 0 -2.56 5.41 12 1 0 0.60 3.18 11 -2 0 2.77 3.82 -11 2 0 5.98 4.25 10 -2 0 8.56 3.31 -10 2 0 7.85 4.19 9 -2 0 15.15 17.28 9 -2 0 13.94 4.15 -9 2 0 18.91 4.65 8 -2 0 -0.35 5.30 -8 2 0 -5.46 8.19 7 -2 0 108.41 11.66 -7 2 0 105.20 11.95 6 -2 0 87.41 16.72 6 -2 0 117.00 11.35 6 -2 0 105.47 10.09 -6 2 0 107.33 10.49 -6 2 0 90.66 12.37 -6 2 0 119.89 11.47 5 -2 0 29.98 6.42 5 -2 0 36.97 3.50 -5 2 0 31.94 5.59 -5 2 0 27.00 5.33 -5 2 0 36.34 4.04 4 -2 0 228.01 21.83 4 -2 0 212.88 22.31 -4 2 0 235.61 21.92 -4 2 0 254.13 21.45 3 -2 0 63.51 7.82 3 -2 0 80.51 7.05 3 -2 0 65.60 7.60 -3 2 0 73.71 7.75 -3 2 0 84.73 7.10 -3 2 0 76.27 7.86 2 -2 0 1303.52 110.91 2 -2 0 1144.00 111.21 -2 2 0 1287.49 110.95 -2 2 0 1150.48 111.21 1 -2 0 10.49 1.15 -1 2 0 7.64 1.42 -1 2 0 11.02 1.66 0 -2 0 2227.84 202.15 -1 -2 0 2437.41 203.88 1 2 0 2055.86 203.82 -2 -2 0 74.45 7.66 -2 -2 0 89.21 7.91 2 2 0 82.59 7.69 -3 -2 0 24.64 2.90 -3 -2 0 29.27 3.65 -3 -2 0 27.12 2.87 3 2 0 23.41 2.72 3 2 0 22.84 2.91 3 2 0 28.00 3.06 -4 -2 0 524.14 46.59 -4 -2 0 532.44 46.69 4 2 0 509.60 46.47 4 2 0 558.05 46.81 4 2 0 491.60 46.67 4 2 0 445.11 47.05 -5 -2 0 226.49 23.61 -5 -2 0 235.21 22.20 5 2 0 214.04 22.24 5 2 0 236.15 22.80 5 2 0 256.91 21.93 5 2 0 261.96 22.50 -6 -2 0 50.55 8.97 -6 -2 0 36.34 4.69 6 2 0 45.35 4.31 6 2 0 44.32 6.15 6 2 0 28.82 5.20 6 2 0 34.52 6.29 -7 -2 0 4.64 2.73 -7 -2 0 6.71 5.94 7 2 0 3.51 4.21 7 2 0 20.68 10.20 7 2 0 7.24 3.92 7 2 0 4.97 2.22 7 2 0 8.29 5.11 -8 -2 0 13.24 5.86 8 2 0 -3.77 9.26 8 2 0 21.09 5.09 8 2 0 6.08 5.52 -9 -2 0 92.82 14.16 9 2 0 113.03 12.68 -10 -2 0 1.58 6.25 10 2 0 1.34 10.80 10 2 0 -0.14 4.59 -11 -2 0 0.92 6.14 11 2 0 11.18 4.46 -12 -2 0 -3.27 5.88 12 2 0 5.36 3.21 10 -3 0 0.19 4.35 -10 3 0 10.01 4.92 -10 3 0 3.42 10.61 9 -3 0 0.69 3.47 -9 3 0 4.13 3.86 -8 3 0 7.57 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13 -8.54 7.19 -3 7 13 31.00 7.49 2 -7 -13 2.11 1.94 -2 7 13 -6.78 5.82 1 -7 -13 20.74 3.32 -1 7 13 29.70 6.72 0 -7 -13 0.08 2.22 0 7 13 10.33 5.86 1 7 13 4.84 5.91 2 7 13 23.70 6.62 2 7 13 27.92 5.38 3 7 13 109.85 14.43 3 7 13 153.23 18.15 3 7 13 109.83 13.08 4 7 13 5.05 8.46 4 7 13 14.66 7.34 4 7 13 5.45 6.59 5 7 13 4.60 6.70 5 7 13 -0.52 6.99 6 7 13 2.55 7.47 6 7 13 6.99 6.25 7 7 13 4.79 5.37 -8 -7 -13 8.53 3.90 8 7 13 11.88 4.34 9 7 13 6.65 5.96 10 7 13 7.19 4.42 -3 8 13 15.84 5.22 -2 8 13 4.04 6.15 1 -8 -13 25.23 3.37 -1 8 13 25.80 5.82 0 8 13 10.47 5.24 1 8 13 7.00 5.58 2 8 13 1.01 5.32 3 8 13 25.85 6.64 4 8 13 34.24 11.15 4 8 13 24.22 7.03 5 8 13 1.95 6.89 5 8 13 -3.70 8.76 6 8 13 18.97 8.12 6 8 13 23.88 8.00 7 8 13 21.61 7.21 7 8 13 20.31 8.04 8 8 13 3.03 4.73 9 8 13 8.76 5.86 10 8 13 1.31 4.14 -2 9 13 -0.22 4.10 -1 9 13 -0.74 4.26 0 -9 -13 8.40 4.63 0 9 13 18.42 5.65 -1 -9 -13 -2.02 4.69 1 9 13 5.28 4.82 2 9 13 3.04 5.17 3 9 13 3.05 5.74 4 9 13 1.86 5.64 5 9 13 4.70 10.75 5 9 13 12.68 6.82 6 9 13 -6.06 6.62 6 9 13 7.62 9.14 7 9 13 2.30 7.60 7 9 13 3.10 6.42 8 9 13 4.17 7.10 9 9 13 13.75 6.09 10 9 13 15.21 5.72 -1 10 13 10.40 4.67 0 10 13 1.42 3.88 1 10 13 8.96 5.25 2 10 13 -3.04 4.72 3 10 13 -8.64 4.91 4 10 13 -2.05 5.31 5 10 13 1.90 6.09 6 10 13 7.05 10.24 6 10 13 4.07 6.00 8 10 13 -5.51 6.74 9 10 13 -2.23 6.62 1 11 13 4.78 4.51 2 11 13 5.42 4.65 4 11 13 5.05 6.66 5 11 13 0.19 5.45 6 11 13 6.94 5.39 7 11 13 -18.32 16.81 7 11 13 5.86 5.12 8 11 13 4.49 8.74 3 12 13 5.28 3.85 4 12 13 6.45 4.36 5 12 13 -2.96 4.35 6 12 13 2.39 4.62 0 -3 14 -0.94 5.21 1 -3 14 4.33 5.88 2 2 -14 4.80 3.91 -2 -2 14 0.03 4.49 1 2 -14 1.02 3.63 -1 -2 14 5.68 3.95 0 2 -14 -7.51 3.22 0 -2 14 -5.83 6.60 -1 2 -14 -0.65 3.02 1 -2 14 2.18 4.20 -2 2 -14 3.37 2.85 2 -2 14 5.04 5.09 3 -2 14 12.62 4.88 4 -2 14 2.26 4.56 3 1 -14 -4.99 3.83 -3 -1 14 0.36 4.60 2 1 -14 11.95 3.90 -2 -1 14 3.03 4.75 1 1 -14 -1.00 3.47 -1 -1 14 6.77 5.61 0 1 -14 6.72 3.52 0 -1 14 16.67 6.21 -1 1 -14 61.49 7.30 -2 1 -14 8.43 3.08 2 -1 14 17.15 6.76 -3 1 -14 3.66 2.83 3 -1 14 -4.03 6.29 -4 1 -14 5.87 2.73 4 -1 14 0.08 6.48 5 -1 14 11.42 6.26 6 -1 14 13.35 6.40 4 0 -14 0.80 6.10 3 0 -14 4.89 3.47 -3 0 14 2.82 4.27 2 0 -14 6.76 3.50 -2 0 14 7.80 4.60 1 0 -14 4.71 3.39 -1 0 14 -2.02 4.57 0 0 -14 4.86 3.54 0 0 14 3.15 5.51 -1 0 -14 -2.07 3.25 1 0 14 1.99 5.89 -2 0 -14 8.52 3.33 2 0 14 11.15 6.18 -3 0 -14 0.44 2.80 3 0 14 1.25 2.44 3 0 14 -1.68 6.16 -4 0 -14 -4.62 2.46 4 0 14 0.50 2.98 -5 0 -14 -3.39 2.55 5 0 14 -11.76 11.05 5 0 14 2.15 2.72 6 0 14 -4.61 5.77 7 0 14 2.34 8.42 4 -1 -14 7.32 3.51 3 -1 -14 -6.98 2.94 -3 1 14 -7.40 4.18 2 -1 -14 2.05 3.12 -2 1 14 -1.53 4.19 1 -1 -14 6.72 3.26 -1 1 14 -0.07 4.24 0 -1 -14 5.93 6.41 0 1 14 26.51 5.87 -1 -1 -14 7.77 4.39 1 1 14 -4.03 3.59 2 1 14 17.46 6.62 2 1 14 24.95 5.04 -3 -1 -14 5.95 3.23 3 1 14 2.83 2.85 3 1 14 -6.65 6.08 -4 -1 -14 0.43 2.81 4 1 14 4.90 6.93 4 1 14 5.65 3.12 -5 -1 -14 5.68 2.61 5 1 14 -2.30 6.96 -6 -1 -14 -1.38 2.58 6 1 14 0.68 9.58 7 1 14 1.46 7.67 7 1 14 7.18 3.00 4 -2 -14 -2.99 3.31 3 -2 -14 2.35 2.95 2 -2 -14 17.45 3.52 1 -2 -14 3.97 4.82 -1 2 14 1.99 3.43 0 -2 -14 -1.63 3.84 0 2 14 -1.74 4.16 -1 -2 -14 -1.15 3.51 1 2 14 6.81 4.90 1 2 14 3.21 4.05 -2 -2 -14 3.00 4.15 2 2 14 5.45 3.76 2 2 14 5.25 5.23 3 2 14 65.82 9.85 3 2 14 42.63 6.97 -4 -2 -14 43.31 5.70 4 2 14 26.73 5.94 4 2 14 47.12 9.20 -5 -2 -14 0.25 2.85 5 2 14 4.94 7.73 5 2 14 1.71 3.19 -6 -2 -14 5.34 2.87 6 2 14 8.42 9.21 6 2 14 1.98 2.76 7 2 14 6.55 8.73 7 2 14 7.88 3.24 8 2 14 4.04 5.06 8 2 14 3.00 3.10 3 -3 -14 5.63 2.91 2 -3 -14 1.55 2.82 -2 3 14 0.85 3.28 1 -3 -14 6.51 4.08 -1 3 14 17.33 4.14 0 3 14 1.66 3.80 -1 -3 -14 27.45 5.44 1 3 14 17.48 5.64 1 3 14 22.23 4.97 2 3 14 2.98 4.70 2 3 14 0.18 4.15 3 3 14 5.20 5.26 3 3 14 -0.74 3.71 -4 -3 -14 21.81 6.44 4 3 14 23.47 7.49 4 3 14 27.92 5.25 -5 -3 -14 2.08 3.68 5 3 14 2.38 3.21 5 3 14 8.76 7.28 -6 -3 -14 5.32 3.31 6 3 14 13.54 3.66 6 3 14 12.09 8.30 -7 -3 -14 -1.40 3.09 7 3 14 1.61 2.89 7 3 14 18.06 11.03 8 3 14 8.57 6.36 8 3 14 3.83 2.80 3 -4 -14 7.52 2.70 2 -4 -14 -2.08 2.64 1 -4 -14 4.72 3.22 -1 4 14 -1.43 3.09 0 4 14 -1.36 3.70 1 4 14 37.28 6.91 1 4 14 49.30 8.31 2 4 14 35.08 7.52 2 4 14 43.45 7.26 3 4 14 -1.49 4.55 3 4 14 9.02 4.98 4 4 14 73.83 10.77 4 4 14 66.09 9.34 5 4 14 14.72 4.16 -6 -4 -14 -1.28 3.75 6 4 14 4.98 3.37 6 4 14 8.42 8.26 -7 -4 -14 -3.20 3.41 7 4 14 4.46 10.70 7 4 14 -1.57 3.34 8 4 14 2.44 3.14 8 4 14 5.30 7.06 9 4 14 -1.41 3.12 2 -5 -14 0.30 2.47 1 -5 -14 2.72 2.90 -1 5 14 10.21 11.77 -1 5 14 -0.76 3.58 0 5 14 24.83 4.72 1 5 14 17.43 4.25 2 5 14 18.94 7.91 2 5 14 11.38 4.23 3 5 14 9.31 5.10 3 5 14 1.21 5.98 4 5 14 28.23 5.99 4 5 14 13.17 5.74 5 5 14 -0.44 4.09 5 5 14 10.29 6.45 6 5 14 73.16 9.54 6 5 14 80.23 12.09 -7 -5 -14 8.42 4.44 7 5 14 -4.93 9.96 7 5 14 7.02 3.49 8 5 14 3.76 3.58 9 5 14 7.57 3.61 -3 6 14 4.00 11.41 -2 6 14 5.06 9.67 -1 6 14 6.82 8.77 0 6 14 26.38 8.56 0 6 14 12.01 4.39 1 6 14 11.34 4.56 1 6 14 2.28 7.63 2 6 14 30.96 5.67 2 6 14 19.95 8.42 3 6 14 37.78 9.78 3 6 14 39.31 7.74 4 6 14 -5.82 5.18 4 6 14 6.98 6.72 5 6 14 -4.08 5.54 6 6 14 -1.80 8.09 6 6 14 8.86 4.71 7 6 14 14.26 4.90 8 6 14 18.91 8.12 9 6 14 2.55 3.41 -2 7 14 19.40 9.53 -1 7 14 8.20 9.60 0 7 14 11.90 7.98 1 7 14 35.60 8.65 2 7 14 -0.71 5.18 2 7 14 7.33 7.42 3 7 14 -1.50 5.47 3 7 14 10.63 7.88 4 7 14 62.13 11.06 4 7 14 13.89 9.40 5 7 14 -13.41 8.78 5 7 14 10.98 7.27 6 7 14 12.48 6.20 7 7 14 1.97 4.78 8 7 14 3.11 9.55 9 7 14 -4.48 3.79 -2 8 14 19.03 7.93 -1 8 14 26.64 7.58 0 8 14 8.06 9.66 1 8 14 16.69 7.86 2 8 14 15.20 7.80 3 8 14 13.11 8.13 4 8 14 26.99 8.57 5 8 14 -5.07 9.22 5 8 14 -4.95 8.64 6 8 14 16.28 8.30 6 8 14 15.69 15.22 7 8 14 15.30 6.94 8 8 14 12.49 5.88 9 8 14 -2.05 4.59 -1 9 14 17.00 6.29 0 9 14 -7.66 6.19 1 9 14 35.08 8.95 2 9 14 7.77 7.27 3 9 14 9.53 7.28 4 9 14 12.93 8.05 5 9 14 21.90 8.76 6 9 14 0.24 9.33 6 9 14 28.38 10.65 7 9 14 0.07 7.03 8 9 14 3.89 6.34 9 9 14 -3.24 6.37 0 10 14 20.90 6.89 1 10 14 -0.91 5.40 2 10 14 -3.76 6.08 3 10 14 -2.44 6.58 4 10 14 24.76 7.49 5 10 14 -2.68 7.11 6 10 14 16.43 7.64 7 10 14 -18.21 9.98 2 11 14 -2.83 4.86 3 11 14 11.95 6.15 5 11 14 20.75 6.37 6 11 14 10.02 6.51 -2 -1 15 9.77 5.16 -1 -1 15 0.37 3.71 0 -1 15 10.28 4.24 1 -1 15 -5.13 4.93 2 -1 15 -2.25 4.60 3 -1 15 10.84 5.65 4 -1 15 2.34 6.01 -2 0 15 7.19 4.44 1 0 -15 6.53 5.02 -1 0 15 7.66 6.02 0 0 -15 2.24 4.36 0 0 15 0.26 7.78 -1 0 -15 4.49 4.47 1 0 15 0.43 6.39 -2 0 -15 -4.93 4.32 2 0 15 -0.66 7.10 3 0 15 -1.32 6.71 4 0 15 7.26 5.62 5 0 15 18.31 6.63 -2 1 15 9.27 6.09 1 -1 -15 16.39 4.48 0 -1 -15 4.98 4.17 0 1 15 -2.66 5.37 -1 -1 -15 83.71 11.10 1 1 15 118.19 13.09 -2 -1 -15 4.29 4.55 2 1 15 15.19 6.30 -3 -1 -15 1.28 4.37 3 1 15 -3.21 6.11 3 1 15 -3.03 3.07 4 1 15 6.44 2.78 5 1 15 -2.05 2.32 5 1 15 -0.10 7.50 6 1 15 12.28 7.63 -2 2 15 -0.35 4.35 -1 2 15 34.17 6.03 0 -2 -15 3.66 4.34 0 2 15 12.28 4.85 -1 -2 -15 18.03 4.68 1 2 15 -4.01 4.82 -2 -2 -15 7.51 4.91 2 2 15 18.22 6.44 2 2 15 8.35 3.88 -3 -2 -15 6.28 5.06 3 2 15 -2.80 3.10 3 2 15 -1.49 6.90 -4 -2 -15 -2.56 5.78 4 2 15 -1.63 2.84 4 2 15 5.13 7.54 5 2 15 4.57 2.88 5 2 15 2.60 14.29 6 2 15 -2.75 7.99 6 2 15 9.19 3.35 7 2 15 8.67 6.94 7 2 15 4.37 2.64 1 -3 -15 5.00 4.63 -1 3 15 2.08 3.95 0 3 15 7.70 4.44 1 3 15 9.51 5.05 2 3 15 55.61 8.94 2 3 15 59.76 8.85 3 3 15 3.48 6.22 3 3 15 3.66 4.24 4 3 15 0.82 3.11 4 3 15 7.07 7.25 5 3 15 6.19 3.57 5 3 15 -0.83 8.64 6 3 15 13.17 5.51 6 3 15 0.56 8.49 7 3 15 7.55 2.98 7 3 15 -1.71 6.08 -1 4 15 0.97 3.47 0 4 15 15.97 4.64 1 4 15 4.39 3.97 2 4 15 9.43 6.34 2 4 15 19.49 5.38 3 4 15 3.27 4.97 3 4 15 16.41 6.03 4 4 15 -2.19 6.23 4 4 15 7.51 4.62 5 4 15 11.61 4.34 5 4 15 19.61 7.36 6 4 15 4.11 7.52 6 4 15 1.31 3.43 7 4 15 3.77 2.84 7 4 15 4.03 5.92 8 4 15 15.35 3.68 0 5 15 2.28 3.85 1 5 15 2.49 3.89 2 5 15 4.98 4.96 3 5 15 3.72 6.85 3 5 15 7.19 5.01 4 5 15 -5.76 5.89 4 5 15 1.03 5.38 5 5 15 0.19 4.40 5 5 15 -3.55 7.34 6 5 15 36.24 6.97 6 5 15 38.05 8.94 7 5 15 -7.51 7.45 7 5 15 6.66 3.76 8 5 15 -1.58 2.94 1 6 15 32.03 6.08 2 6 15 4.69 4.78 3 6 15 -2.79 5.23 4 6 15 10.94 7.99 4 6 15 -0.18 7.53 5 6 15 1.10 6.07 5 6 15 12.83 6.98 6 6 15 -7.53 5.95 7 6 15 3.26 3.74 8 6 15 0.87 3.35 -1 7 15 27.50 16.44 0 7 15 31.37 12.46 1 7 15 27.50 12.52 4 7 15 16.41 10.60 5 7 15 4.34 8.72 6 7 15 11.76 7.56 7 7 15 -7.14 4.56 8 7 15 7.01 4.98 0 8 15 26.82 10.47 1 8 15 -1.80 10.36 2 8 15 18.30 10.53 3 8 15 30.16 10.73 4 8 15 82.45 15.92 5 8 15 -1.47 10.57 6 8 15 7.39 8.25 7 8 15 9.53 6.93 8 8 15 -2.73 5.17 1 9 15 -4.65 9.53 2 9 15 0.27 9.18 3 9 15 28.77 10.37 4 9 15 29.15 10.31 5 9 15 0.73 10.81 7 9 15 -0.25 10.11 3 10 15 -11.40 8.84 4 10 15 18.57 9.46 5 10 15 -13.03 12.69 0 0 16 7.97 4.20 1 0 16 -3.15 5.33 2 0 16 7.23 5.20 3 0 16 17.00 6.46 -1 1 16 3.11 4.74 0 1 16 2.33 5.61 1 1 16 -2.45 5.22 2 1 16 -2.22 6.81 3 1 16 0.41 6.37 4 1 16 23.44 7.93 -1 2 16 6.00 5.37 0 2 16 3.93 4.97 1 2 16 2.76 6.36 2 2 16 10.19 6.36 3 2 16 -8.34 6.75 5 2 16 -0.57 2.35 5 2 16 2.47 7.73 -1 3 16 14.95 5.16 0 3 16 5.01 5.02 1 3 16 9.04 6.95 2 3 16 10.81 6.62 3 3 16 -3.78 7.17 4 3 16 19.17 7.76 5 3 16 1.07 3.48 5 3 16 -0.59 7.50 6 3 16 6.69 3.28 0 4 16 8.13 4.67 1 4 16 5.21 5.08 2 4 16 52.78 9.99 3 4 16 3.29 5.55 3 4 16 0.55 6.32 4 4 16 -4.47 4.66 4 4 16 6.28 6.97 5 4 16 9.98 4.23 5 4 16 -9.65 7.67 6 4 16 -0.54 3.60 1 5 16 -4.85 4.43 2 5 16 3.21 4.63 3 5 16 23.00 6.20 4 5 16 3.36 6.62 4 5 16 22.08 6.81 5 5 16 0.41 4.78 5 5 16 -1.29 5.41 6 5 16 -1.01 4.37 7 5 16 -2.64 3.61 2 6 16 16.14 5.73 3 6 16 3.55 6.22 4 6 16 -4.64 6.26 4 6 16 -13.16 9.78 5 6 16 5.31 6.41 6 6 16 4.96 5.53 7 6 16 -6.93 4.91 5 7 16 -20.57 12.12 6 7 16 4.06 7.64 1 3 17 10.12 6.02 2 3 17 -2.88 6.68 3 3 17 2.84 5.99 1 4 17 20.64 9.17 2 4 17 3.60 7.01 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 65993 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 Cl2 Cl 1.27208(13) 0.96798(13) 0.43390(9) 0.0721(4) Uani 1 1 d . . . . . Cl1 Cl 0.11427(14) 0.84013(14) 1.00426(11) 0.0877(5) Uani 1 1 d . . . . . F2 F 0.6153(3) 0.3637(3) 0.8642(2) 0.0724(8) Uani 1 1 d . . . . . F1 F 0.7580(2) 0.3257(3) 0.7423(2) 0.0761(9) Uani 1 1 d . . . . . F4 F 0.7705(3) 0.5861(3) 0.7603(2) 0.0787(9) Uani 1 1 d . . . . . F3 F 0.9105(3) 0.6265(3) 0.6385(2) 0.0817(9) Uani 1 1 d . . . . . N2 N 1.0466(3) 0.5020(3) 0.8335(3) 0.0458(9) Uani 1 1 d . . . . . N1 N 0.4707(3) 0.4326(3) 0.6812(3) 0.0510(10) Uani 1 1 d . . . . . O2 O 1.0353(4) 0.3387(4) 0.7774(3) 0.0858(12) Uani 1 1 d . . . . . O1 O 0.5426(4) 0.2062(4) 0.7521(3) 0.0834(12) Uani 1 1 d . . . . . C22 C 1.1490(4) 0.4538(4) 0.8964(3) 0.0448(11) Uani 1 1 d . . . . . C27 C 0.9472(4) 0.6371(4) 0.7985(3) 0.0469(11) Uani 1 1 d . . . . . H27 H 0.8823 0.6635 0.8514 0.056 Uiso 1 1 calc R . . . . C9 C 0.5461(4) 0.5044(4) 0.6990(3) 0.0475(11) Uani 1 1 d . . . . . H9 H 0.5991 0.5346 0.6399 0.057 Uiso 1 1 calc R . . . . C36 C 1.1089(4) 0.9243(4) 0.5962(3) 0.0492(12) Uani 1 1 d . . . . . H36 H 1.1074 0.8587 0.5741 0.059 Uiso 1 1 calc R . . . . C11 C 0.4662(4) 0.7300(4) 0.7174(3) 0.0457(11) Uani 1 1 d . . . . . C4 C 0.3699(4) 0.4744(4) 0.6174(3) 0.0480(11) Uani 1 1 d . . . . . C3 C 0.3309(4) 0.5998(5) 0.5536(3) 0.0527(12) Uani 1 1 d . . . . . H3 H 0.3711 0.6564 0.5539 0.063 Uiso 1 1 calc R . . . . C13 C 0.3971(4) 0.8167(4) 0.7833(3) 0.0470(11) Uani 1 1 d . . . . . C31 C 1.0370(4) 0.9436(4) 0.6848(3) 0.0502(12) Uani 1 1 d . . . . . C23 C 1.1604(4) 0.5327(5) 0.9462(3) 0.0507(11) Uani 1 1 d . . . . . H23 H 1.0981 0.6160 0.9395 0.061 Uiso 1 1 calc R . . . . C14 C 0.2949(4) 0.7978(4) 0.8513(3) 0.0504(12) Uani 1 1 d . . . . . H14 H 0.2623 0.7347 0.8531 0.060 Uiso 1 1 calc R . . . . C29 C 0.9657(4) 0.8573(4) 0.7468(3) 0.0494(12) Uani 1 1 d . . . . . C28 C 1.0079(4) 0.7342(4) 0.7432(3) 0.0508(12) Uani 1 1 d . . . . . H28 H 1.0829 0.7081 0.7017 0.061 Uiso 1 1 calc R . . . . C8 C 0.6273(4) 0.3716(5) 0.7668(3) 0.0560(13) Uani 1 1 d . . . . . C25 C 1.0023(4) 0.4471(5) 0.7823(4) 0.0570(13) Uani 1 1 d . . . . . C10 C 0.4702(4) 0.6072(4) 0.7488(3) 0.0480(11) Uani 1 1 d . . . . . H10 H 0.4210 0.5840 0.8073 0.058 Uiso 1 1 calc R . . . . C35 C 1.1804(5) 0.9989(4) 0.5422(3) 0.0527(12) Uani 1 1 d . . . . . C26 C 0.8974(4) 0.5788(5) 0.7384(4) 0.0576(13) Uani 1 1 d . . . . . C7 C 0.5458(5) 0.3120(5) 0.7372(4) 0.0597(13) Uani 1 1 d . . . . . C2 C 0.2329(5) 0.6402(5) 0.4901(4) 0.0594(13) Uani 1 1 d . . . . . H2 H 0.2077 0.7241 0.4476 0.071 Uiso 1 1 calc R . . . . C15 C 0.2396(5) 0.8715(5) 0.9173(4) 0.0621(14) Uani 1 1 d . . . . . C1 C 0.1723(5) 0.5599(6) 0.4884(4) 0.0659(14) Uani 1 1 d . . . . . H1 H 0.1066 0.5882 0.4448 0.079 Uiso 1 1 calc R . . . . C5 C 0.3079(5) 0.3924(5) 0.6161(4) 0.0608(13) Uani 1 1 d . . . . . H5 H 0.3329 0.3082 0.6582 0.073 Uiso 1 1 calc R . . . . C21 C 1.2403(4) 0.3295(5) 0.9075(4) 0.0618(13) Uani 1 1 d . . . . . H21 H 1.2321 0.2765 0.8750 0.074 Uiso 1 1 calc R . . . . C12 C 0.5348(5) 0.7852(5) 0.6211(3) 0.0646(14) Uani 1 1 d . . . . . H12A H 0.4743 0.8677 0.5863 0.097 Uiso 1 1 calc GR . . . . H12B H 0.5621 0.7268 0.5813 0.097 Uiso 1 1 calc GR . . . . H12C H 0.6115 0.7960 0.6347 0.097 Uiso 1 1 calc GR . . . . C24 C 1.2653(5) 0.4858(6) 1.0056(3) 0.0694(15) Uani 1 1 d . . . . . H24 H 1.2743 0.5379 1.0386 0.083 Uiso 1 1 calc R . . . . C32 C 1.0380(5) 1.0462(5) 0.7133(4) 0.0654(15) Uani 1 1 d . . . . . H32 H 0.9891 1.0638 0.7704 0.078 Uiso 1 1 calc R . . . . C33 C 1.1104(6) 1.1208(5) 0.6578(4) 0.0796(17) Uani 1 1 d . . . . . H33 H 1.1106 1.1881 0.6783 0.096 Uiso 1 1 calc R . . . . C34 C 1.1838(6) 1.0986(5) 0.5714(4) 0.0737(15) Uani 1 1 d . . . . . H34 H 1.2335 1.1493 0.5346 0.088 Uiso 1 1 calc R . . . . C30 C 0.8486(5) 0.9116(5) 0.8141(4) 0.0754(16) Uani 1 1 d . . . . . H30A H 0.8805 0.9131 0.8713 0.113 Uiso 1 1 calc GR . . . . H30B H 0.7953 0.8580 0.8344 0.113 Uiso 1 1 calc GR . . . . H30C H 0.7957 0.9981 0.7794 0.113 Uiso 1 1 calc GR . . . . C6 C 0.2093(5) 0.4353(6) 0.5523(4) 0.0708(15) Uani 1 1 d . . . . . H6 H 0.1672 0.3801 0.5522 0.085 Uiso 1 1 calc R . . . . C19 C 1.3571(5) 0.3612(7) 1.0158(4) 0.0806(18) Uani 1 1 d . . . . . H19 H 1.4279 0.3292 1.0557 0.097 Uiso 1 1 calc R . . . . C18 C 0.4395(5) 0.9153(5) 0.7803(4) 0.0709(15) Uani 1 1 d . . . . . H18 H 0.5060 0.9328 0.7336 0.085 Uiso 1 1 calc R . . . . C20 C 1.3427(5) 0.2853(6) 0.9666(4) 0.0799(17) Uani 1 1 d . . . . . H20 H 1.4044 0.2017 0.9739 0.096 Uiso 1 1 calc R . . . . C16 C 0.2836(7) 0.9665(5) 0.9158(5) 0.0829(18) Uani 1 1 d . . . . . H16 H 0.2467 1.0149 0.9605 0.099 Uiso 1 1 calc R . . . . C17 C 0.3821(7) 0.9888(6) 0.8477(5) 0.0878(19) Uani 1 1 d . . . . . H17 H 0.4122 1.0538 0.8456 0.105 Uiso 1 1 calc R . . . . 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 Cl2 0.0790(9) 0.0795(9) 0.0544(8) -0.0158(7) 0.0016(6) -0.0304(7) Cl1 0.0777(9) 0.0772(10) 0.0875(10) -0.0446(8) 0.0111(8) 0.0037(7) F2 0.0685(18) 0.0747(19) 0.0582(18) -0.0188(14) -0.0127(14) -0.0060(15) F1 0.0407(15) 0.081(2) 0.086(2) -0.0302(16) -0.0063(14) 0.0046(14) F4 0.0451(17) 0.114(2) 0.081(2) -0.0336(18) -0.0086(14) -0.0259(16) F3 0.079(2) 0.116(3) 0.0468(17) -0.0246(16) -0.0115(14) -0.0278(18) N2 0.0374(19) 0.046(2) 0.050(2) -0.0170(17) -0.0086(16) -0.0055(16) N1 0.042(2) 0.047(2) 0.060(2) -0.0225(19) -0.0035(18) -0.0064(18) O2 0.085(3) 0.073(3) 0.115(3) -0.052(2) -0.006(2) -0.023(2) O1 0.086(3) 0.048(2) 0.110(3) -0.020(2) -0.017(2) -0.016(2) C22 0.035(2) 0.050(3) 0.045(3) -0.015(2) 0.0000(19) -0.012(2) C27 0.033(2) 0.049(3) 0.048(3) -0.014(2) -0.0023(19) -0.003(2) C9 0.039(2) 0.050(3) 0.050(3) -0.018(2) -0.001(2) -0.011(2) C36 0.053(3) 0.046(3) 0.044(3) -0.018(2) -0.013(2) -0.005(2) C11 0.036(2) 0.047(3) 0.051(3) -0.013(2) -0.010(2) -0.010(2) C4 0.038(2) 0.056(3) 0.050(3) -0.027(2) 0.005(2) -0.011(2) C3 0.053(3) 0.054(3) 0.052(3) -0.026(2) -0.003(2) -0.011(2) C13 0.046(3) 0.038(3) 0.053(3) -0.011(2) -0.014(2) -0.008(2) C31 0.050(3) 0.042(3) 0.046(3) -0.016(2) -0.013(2) 0.004(2) C23 0.049(3) 0.057(3) 0.042(3) -0.013(2) -0.006(2) -0.015(2) C14 0.046(3) 0.036(2) 0.064(3) -0.017(2) -0.013(2) -0.003(2) C29 0.045(3) 0.048(3) 0.040(2) -0.017(2) -0.006(2) 0.004(2) C28 0.040(2) 0.051(3) 0.047(3) -0.019(2) 0.002(2) 0.000(2) C8 0.039(3) 0.058(3) 0.055(3) -0.020(2) -0.006(2) 0.003(2) C25 0.040(3) 0.073(4) 0.062(3) -0.031(3) -0.001(2) -0.016(2) C10 0.040(2) 0.058(3) 0.048(3) -0.024(2) 0.0046(19) -0.015(2) C35 0.060(3) 0.047(3) 0.048(3) -0.012(2) -0.013(2) -0.012(2) C26 0.039(3) 0.081(4) 0.055(3) -0.026(3) -0.005(2) -0.018(2) C7 0.050(3) 0.057(3) 0.066(3) -0.024(3) -0.003(2) -0.007(3) C2 0.058(3) 0.055(3) 0.058(3) -0.026(2) -0.006(2) -0.004(2) C15 0.059(3) 0.048(3) 0.065(3) -0.022(2) -0.011(2) 0.003(2) C1 0.050(3) 0.086(4) 0.066(3) -0.036(3) -0.004(2) -0.017(3) C5 0.056(3) 0.058(3) 0.066(3) -0.017(3) -0.002(3) -0.018(3) C21 0.052(3) 0.057(3) 0.063(3) -0.020(2) -0.007(2) -0.002(2) C12 0.066(3) 0.059(3) 0.058(3) -0.008(3) -0.004(3) -0.018(3) C24 0.067(3) 0.096(4) 0.047(3) -0.010(3) -0.012(3) -0.037(3) C32 0.083(4) 0.046(3) 0.052(3) -0.018(3) -0.008(3) -0.002(3) C33 0.114(5) 0.044(3) 0.079(4) -0.022(3) -0.011(4) -0.021(3) C34 0.094(4) 0.057(3) 0.066(4) -0.012(3) -0.010(3) -0.025(3) C30 0.073(4) 0.063(3) 0.062(3) -0.028(3) 0.009(3) 0.007(3) C6 0.062(3) 0.087(4) 0.080(4) -0.039(3) 0.000(3) -0.033(3) C19 0.049(3) 0.109(5) 0.060(3) 0.000(3) -0.020(3) -0.017(3) C18 0.075(4) 0.060(3) 0.078(4) -0.019(3) -0.012(3) -0.022(3) C20 0.056(3) 0.074(4) 0.078(4) -0.016(3) -0.016(3) 0.010(3) C16 0.112(5) 0.055(4) 0.083(4) -0.034(3) -0.016(4) -0.016(3) C17 0.117(5) 0.062(4) 0.100(5) -0.037(4) -0.008(4) -0.036(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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 C22 N2 C27 130.1(3) . . ? C25 N2 C22 133.5(4) . . ? C25 N2 C27 96.4(3) . . ? C4 N1 C9 130.4(4) . . ? C7 N1 C9 96.1(4) . . ? C7 N1 C4 133.0(4) . . ? N2 C22 C23 119.7(4) . . ? C21 C22 N2 119.9(4) . . ? C21 C22 C23 120.3(4) . . ? N2 C27 H27 112.6 . . ? N2 C27 C26 84.7(3) . . ? C28 C27 N2 113.8(3) . . ? C28 C27 H27 112.6 . . ? C28 C27 C26 117.6(4) . . ? C26 C27 H27 112.6 . . ? N1 C9 H9 112.2 . . ? N1 C9 C8 85.0(3) . . ? C8 C9 H9 112.2 . . ? C10 C9 N1 116.9(3) . . ? C10 C9 H9 112.2 . . ? C10 C9 C8 115.7(4) . . ? C31 C36 H36 119.2 . . ? C35 C36 H36 119.2 . . ? C35 C36 C31 121.5(4) . . ? C13 C11 C12 117.4(4) . . ? C10 C11 C13 119.0(4) . . ? C10 C11 C12 123.5(4) . . ? C3 C4 N1 120.2(4) . . ? C5 C4 N1 120.9(4) . . ? C5 C4 C3 118.9(4) . . ? C4 C3 H3 120.0 . . ? C2 C3 C4 120.1(5) . . ? C2 C3 H3 120.0 . . ? C14 C13 C11 121.7(4) . . ? C14 C13 C18 117.7(4) . . ? C18 C13 C11 120.5(4) . . ? C36 C31 C29 121.5(4) . . ? C32 C31 C36 117.3(5) . . ? C32 C31 C29 121.2(4) . . ? C22 C23 H23 120.3 . . ? C24 C23 C22 119.4(5) . . ? C24 C23 H23 120.3 . . ? C13 C14 H14 119.5 . . ? C13 C14 C15 121.1(5) . . ? C15 C14 H14 119.5 . . ? C31 C29 C30 117.7(4) . . ? C28 C29 C31 119.6(4) . . ? C28 C29 C30 122.6(5) . . ? C27 C28 H28 116.8 . . ? C29 C28 C27 126.4(4) . . ? C29 C28 H28 116.8 . . ? F2 C8 C9 115.2(3) . . ? F2 C8 C7 115.4(4) . . ? F1 C8 F2 106.4(4) . . ? F1 C8 C9 116.2(4) . . ? F1 C8 C7 114.8(4) . . ? C7 C8 C9 88.5(4) . . ? N2 C25 C26 90.0(4) . . ? O2 C25 N2 133.2(5) . . ? O2 C25 C26 136.8(5) . . ? C9 C10 H10 116.9 . . ? C11 C10 C9 126.3(4) . . ? C11 C10 H10 116.9 . . ? C36 C35 Cl2 119.8(4) . . ? C36 C35 C34 121.2(5) . . ? C34 C35 Cl2 119.1(4) . . ? F4 C26 F3 106.0(4) . . ? F4 C26 C27 115.2(4) . . ? F4 C26 C25 115.8(4) . . ? F3 C26 C27 115.9(4) . . ? F3 C26 C25 114.9(4) . . ? C25 C26 C27 88.9(3) . . ? N1 C7 C8 90.2(4) . . ? O1 C7 N1 132.1(5) . . ? O1 C7 C8 137.7(5) . . ? C3 C2 H2 119.4 . . ? C1 C2 C3 121.2(5) . . ? C1 C2 H2 119.4 . . ? C14 C15 Cl1 119.2(4) . . ? C16 C15 Cl1 119.7(4) . . ? C16 C15 C14 121.1(5) . . ? C2 C1 H1 120.3 . . ? C2 C1 C6 119.3(5) . . ? C6 C1 H1 120.3 . . ? C4 C5 H5 120.0 . . ? C6 C5 C4 120.0(5) . . ? C6 C5 H5 120.0 . . ? C22 C21 H21 120.4 . . ? C20 C21 C22 119.2(5) . . ? C20 C21 H21 120.4 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C23 C24 H24 120.1 . . ? C23 C24 C19 119.9(5) . . ? C19 C24 H24 120.1 . . ? C31 C32 H32 119.8 . . ? C33 C32 C31 120.4(5) . . ? C33 C32 H32 119.8 . . ? C32 C33 H33 119.2 . . ? C32 C33 C34 121.7(5) . . ? C34 C33 H33 119.2 . . ? C35 C34 C33 117.9(5) . . ? C35 C34 H34 121.1 . . ? C33 C34 H34 121.1 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30B 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C1 C6 H6 119.7 . . ? C5 C6 C1 120.5(5) . . ? C5 C6 H6 119.7 . . ? C24 C19 H19 120.3 . . ? C20 C19 C24 119.5(5) . . ? C20 C19 H19 120.3 . . ? C13 C18 H18 119.9 . . ? C13 C18 C17 120.2(6) . . ? C17 C18 H18 119.9 . . ? C21 C20 C19 121.7(5) . . ? C21 C20 H20 119.1 . . ? C19 C20 H20 119.1 . . ? C15 C16 H16 120.6 . . ? C17 C16 C15 118.7(5) . . ? C17 C16 H16 120.6 . . ? C18 C17 H17 119.4 . . ? C16 C17 C18 121.1(6) . . ? C16 C17 H17 119.4 . . ? 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 Cl2 C35 1.752(5) . ? Cl1 C15 1.740(6) . ? F2 C8 1.358(5) . ? F1 C8 1.339(5) . ? F4 C26 1.340(5) . ? F3 C26 1.360(5) . ? N2 C22 1.391(5) . ? N2 C27 1.503(5) . ? N2 C25 1.373(6) . ? N1 C9 1.491(6) . ? N1 C4 1.398(5) . ? N1 C7 1.376(6) . ? O2 C25 1.199(6) . ? O1 C7 1.198(6) . ? C22 C23 1.398(6) . ? C22 C21 1.380(6) . ? C27 H27 0.9800 . ? C27 C28 1.470(6) . ? C27 C26 1.541(6) . ? C9 H9 0.9800 . ? C9 C8 1.544(6) . ? C9 C10 1.490(6) . ? C36 H36 0.9300 . ? C36 C31 1.404(6) . ? C36 C35 1.355(6) . ? C11 C13 1.508(6) . ? C11 C10 1.340(6) . ? C11 C12 1.514(6) . ? C4 C3 1.391(6) . ? C4 C5 1.383(7) . ? C3 H3 0.9300 . ? C3 C2 1.374(6) . ? C13 C14 1.377(6) . ? C13 C18 1.390(7) . ? C31 C29 1.477(7) . ? C31 C32 1.398(7) . ? C23 H23 0.9300 . ? C23 C24 1.381(6) . ? C14 H14 0.9300 . ? C14 C15 1.391(6) . ? C29 C28 1.345(6) . ? C29 C30 1.514(6) . ? C28 H28 0.9300 . ? C8 C7 1.515(7) . ? C25 C26 1.525(7) . ? C10 H10 0.9300 . ? C35 C34 1.383(7) . ? C2 H2 0.9300 . ? C2 C1 1.355(7) . ? C15 C16 1.368(8) . ? C1 H1 0.9300 . ? C1 C6 1.384(8) . ? C5 H5 0.9300 . ? C5 C6 1.377(7) . ? C21 H21 0.9300 . ? C21 C20 1.361(7) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C24 H24 0.9300 . ? C24 C19 1.385(8) . ? C32 H32 0.9300 . ? C32 C33 1.368(8) . ? C33 H33 0.9300 . ? C33 C34 1.390(7) . ? C34 H34 0.9300 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C6 H6 0.9300 . ? C19 H19 0.9300 . ? C19 C20 1.375(8) . ? C18 H18 0.9300 . ? C18 C17 1.408(8) . ? C20 H20 0.9300 . ? C16 H16 0.9300 . ? C16 C17 1.358(8) . ? C17 H17 0.9300 . ?