#------------------------------------------------------------------------------ #$Date: 2020-07-06 04:54:20 +0300 (Mon, 06 Jul 2020) $ #$Revision: 253801 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/65/7126510.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_7126510 loop_ _publ_author_name 'Stewart, Hannah L.' 'Hanby, Abigail R.' 'King, Thomas A.' 'Bond, Andrew D.' 'Moss, Thomas A.' 'Sore, Hannah F.' 'Spring, David R.' _publ_section_title ; An efficient, stereocontrolled and versatile synthetic route to bicyclic partially saturated privileged scaffolds. ; _journal_issue 50 _journal_name_full 'Chemical communications (Cambridge, England)' _journal_page_first 6818 _journal_page_last 6821 _journal_paper_doi 10.1039/d0cc02728f _journal_volume 56 _journal_year 2020 _chemical_absolute_configuration ad _chemical_formula_moiety 'C25 H22 F3 N4 +, Cl -' _chemical_formula_sum 'C25 H22 Cl F3 N4' _chemical_formula_weight 470.91 _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2018/1 _audit_update_record ; 2019-05-08 deposited with the CCDC. 2020-05-11 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 99.160(7) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 5.6933(4) _cell_length_b 12.7845(10) _cell_length_c 15.7666(13) _cell_measurement_reflns_used 3058 _cell_measurement_temperature 180(2) _cell_measurement_theta_max 65.15 _cell_measurement_theta_min 2.84 _cell_volume 1132.95(15) _computing_cell_refinement 'SAINT (Bruker, 2016)' _computing_data_collection 'APEX3 (Bruker, 2016)' _computing_data_reduction SAINT _computing_molecular_graphics 'Mercury (Macrae et al., 2008)' _computing_publication_material SHELXL _computing_structure_refinement 'SHELXL (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_temperature 180(2) _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measurement_device_type 'Bruker D8-QUEST PHOTON-100' _diffrn_measurement_method '\w and \f-scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.1006 _diffrn_reflns_av_unetI/netI 0.1281 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 10800 _diffrn_reflns_point_group_measured_fraction_full 0.971 _diffrn_reflns_point_group_measured_fraction_max 0.971 _diffrn_reflns_theta_full 66.770 _diffrn_reflns_theta_max 66.770 _diffrn_reflns_theta_min 2.839 _diffrn_source 'Incoatec I\mS Cu microsource' _exptl_absorpt_coefficient_mu 1.887 _exptl_absorpt_correction_T_max 0.7528 _exptl_absorpt_correction_T_min 0.4585 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Bruker, 2014)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.380 _exptl_crystal_description plate _exptl_crystal_F_000 488 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Methanol' _exptl_crystal_size_max 0.680 _exptl_crystal_size_mid 0.420 _exptl_crystal_size_min 0.005 _refine_diff_density_max 0.549 _refine_diff_density_min -0.477 _refine_diff_density_rms 0.069 _refine_ls_abs_structure_details ; Flack x determined using 654 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.01(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 335 _refine_ls_number_reflns 3903 _refine_ls_number_restraints 49 _refine_ls_restrained_S_all 1.036 _refine_ls_R_factor_all 0.1503 _refine_ls_R_factor_gt 0.0854 _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^)+(0.0522P)^2^+2.3325P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1705 _refine_ls_wR_factor_ref 0.2028 _reflns_Friedel_coverage 0.867 _reflns_Friedel_fraction_full 0.948 _reflns_Friedel_fraction_max 0.948 _reflns_number_gt 2319 _reflns_number_total 3903 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0cc02728f2.cif _cod_data_source_block DS_B1_0025 _cod_depositor_comments 'Adding full bibliography for 7126510.cif.' _cod_original_sg_symbol_H-M 'P 21' _cod_database_code 7126510 _cambridge_user_name 'Hanna Stewart' _cambridge_user_crsid hlo28 _cambridge_supervisor_name 'David Spring' _cambridge_supervisor_crsid drs36 _cambridge_crystallographer_name 'Andrew Bond' _cambridge_crystallographer_crsid adb29 _cambridge_sample_id HLS732 _cambridge_data_id DS_B1_0025 _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 0.360 _shelx_estimated_absorpt_t_max 0.991 _shelx_res_file ; TITL DS_B1_0025 in P2(1) DS_B1_0025.res created by SHELXL-2018/1 at 10:33:03 on 02-Aug-2018 CELL 1.54178 5.6933 12.7845 15.7666 90.000 99.160 90.000 ZERR 2.000 0.0004 0.0010 0.0013 0.000 0.007 0.000 LATT -1 SYMM -X, 1/2+Y, -Z SFAC C H N F CL UNIT 50 44 8 6 2 SIZE 0.68 0.42 0.005 TEMP -93 L.S. 30 ACTA EXYZ C19 C19A EXYZ C22 C22A EADP C19 C19A EADP C22 C22A ISOR 0.01 C20 C21 C23 C24 ISOR 0.01 C20A C21A C23A C24A BOND $H CONF LIST 4 FMAP 2 PLAN -10 WGHT 0.052200 2.332500 FVAR 0.97000 0.54531 CL1 5 0.235756 0.673127 0.490103 11.00000 0.01857 0.06311 = 0.07826 -0.01156 0.00737 -0.00348 F1 4 0.617879 0.433005 0.047143 11.00000 0.23097 0.08843 = 0.04760 -0.02070 0.02913 -0.05674 F2 4 0.928635 0.521872 0.065556 11.00000 0.11782 0.15268 = 0.07179 0.01859 0.04680 0.00461 F3 4 0.602666 0.597933 0.051612 11.00000 0.16562 0.10806 = 0.04068 0.00875 0.00914 0.05424 N1 3 0.523507 0.484309 0.692775 11.00000 0.05087 0.02981 = 0.03977 -0.00026 0.02056 -0.00120 N2 3 0.330744 0.370697 0.592963 11.00000 0.04776 0.03770 = 0.05981 0.00744 0.02489 -0.01017 N3 3 0.496396 0.428284 0.559257 11.00000 0.04395 0.02714 = 0.04641 -0.00430 0.01825 -0.00846 N4 3 0.747465 0.585187 0.501484 11.00000 0.02502 0.02042 = 0.05200 -0.00512 0.01454 -0.00558 AFIX 23 H4A 2 0.867060 0.625063 0.486725 11.00000 -1.20000 H4B 2 0.608320 0.620084 0.485121 11.00000 -1.20000 AFIX 0 C1 1 0.356031 0.404091 0.673497 11.00000 0.04479 0.04244 = 0.04601 0.00878 0.01870 0.00677 C2 1 0.598748 0.495673 0.618609 11.00000 0.04912 0.02152 = 0.03959 -0.00541 0.01276 0.00524 C3 1 0.786429 0.571324 0.596859 11.00000 0.03449 0.02646 = 0.03177 -0.00020 0.00991 -0.00403 AFIX 13 H3A 2 0.947440 0.540101 0.615446 11.00000 -1.20000 AFIX 0 C4 1 0.738623 0.482589 0.453752 11.00000 0.03052 0.02073 = 0.04347 -0.00867 0.01044 0.00491 AFIX 13 H4 2 0.880870 0.439838 0.477727 11.00000 -1.20000 AFIX 0 C5 1 0.514043 0.425214 0.469101 11.00000 0.05612 0.01790 = 0.04411 -0.00397 0.01454 -0.00977 AFIX 23 H5A 2 0.372390 0.458801 0.435446 11.00000 -1.20000 H5B 2 0.519948 0.351656 0.449930 11.00000 -1.20000 AFIX 0 C6 1 0.214568 0.366621 0.735444 11.00000 0.04651 0.03312 = 0.05543 0.01575 0.02321 0.01583 C7 1 0.014959 0.309128 0.708516 11.00000 0.03278 0.09825 = 0.07089 0.03035 0.00571 -0.00911 AFIX 43 H7A 2 -0.027253 0.292187 0.649385 11.00000 -1.20000 AFIX 0 C8 1 -0.128462 0.274830 0.767511 11.00000 0.03837 0.20888 = 0.07631 0.06820 0.00339 -0.04128 AFIX 43 H8A 2 -0.265506 0.233700 0.748170 11.00000 -1.20000 AFIX 0 C9 1 -0.072319 0.300297 0.853495 11.00000 0.04370 0.16417 = 0.08198 0.07091 0.01479 0.00457 AFIX 43 H9A 2 -0.173731 0.279813 0.892916 11.00000 -1.20000 AFIX 0 C10 1 0.132029 0.355602 0.881124 11.00000 0.09904 0.08289 = 0.06061 0.02286 0.04367 0.02373 AFIX 43 H10A 2 0.176343 0.371088 0.940446 11.00000 -1.20000 AFIX 0 C11 1 0.274963 0.389165 0.822270 11.00000 0.08296 0.04276 = 0.05337 0.00795 0.03961 -0.00633 AFIX 43 H11A 2 0.415436 0.427950 0.841908 11.00000 -1.20000 AFIX 0 C12 1 0.776607 0.679572 0.639838 11.00000 0.04103 0.02036 = 0.04769 0.00008 0.01037 -0.00461 AFIX 23 H12A 2 0.871862 0.729371 0.611270 11.00000 -1.20000 H12B 2 0.609772 0.704386 0.629527 11.00000 -1.20000 AFIX 0 C13 1 0.864199 0.682653 0.733945 11.00000 0.04310 0.02486 = 0.04135 0.00240 0.01216 -0.00750 C14 1 0.727058 0.724866 0.790327 11.00000 0.04778 0.08857 = 0.04960 -0.01768 0.02034 -0.00852 AFIX 43 H14A 2 0.572768 0.750480 0.768274 11.00000 -1.20000 AFIX 0 C15 1 0.806048 0.730993 0.876796 11.00000 0.06944 0.12580 = 0.04527 -0.02955 0.02458 -0.01622 AFIX 43 H15A 2 0.707763 0.760913 0.913740 11.00000 -1.20000 AFIX 0 C16 1 1.026637 0.693952 0.909803 11.00000 0.10552 0.07791 = 0.02808 -0.00049 0.01116 -0.03752 AFIX 43 H16A 2 1.082049 0.696977 0.969859 11.00000 -1.20000 AFIX 0 C17 1 1.166180 0.652694 0.855835 11.00000 0.08051 0.04581 = 0.05606 0.00831 -0.00155 0.00992 AFIX 43 H17A 2 1.319911 0.627187 0.878788 11.00000 -1.20000 AFIX 0 C18 1 1.089710 0.647123 0.768983 11.00000 0.06634 0.05299 = 0.04404 0.00506 0.01331 0.00868 AFIX 43 H18A 2 1.191388 0.618821 0.732520 11.00000 -1.20000 AFIX 0 PART 1 C19 1 0.735010 0.497150 0.359195 21.00000 0.02546 0.03419 = 0.04474 -0.00636 0.00564 0.00217 C20 1 0.695628 0.586974 0.320014 21.00000 0.04133 0.02995 = 0.04511 -0.00746 0.01049 0.00593 AFIX 43 H20A 2 0.674755 0.648076 0.352287 21.00000 -1.20000 AFIX 0 C21 1 0.684153 0.593755 0.232355 21.00000 0.03839 0.02307 = 0.05120 0.00021 0.00621 0.00321 AFIX 43 H21A 2 0.649429 0.659607 0.205337 21.00000 -1.20000 AFIX 0 C22 1 0.720689 0.509569 0.182508 21.00000 0.04851 0.03636 = 0.04214 -0.00615 0.00818 0.00111 C23 1 0.785078 0.413727 0.227605 21.00000 0.06512 0.03568 = 0.04383 -0.00955 0.00817 0.00859 AFIX 43 H23A 2 0.823264 0.353789 0.196889 21.00000 -1.20000 AFIX 0 C24 1 0.791914 0.408088 0.316439 21.00000 0.06055 0.03702 = 0.03781 -0.00949 0.00538 0.01088 AFIX 43 H24A 2 0.834406 0.344934 0.346787 21.00000 -1.20000 AFIX 0 PART 2 C19A 1 0.735010 0.497150 0.359195 -21.00000 0.02546 0.03419 = 0.04474 -0.00636 0.00564 0.00217 C20A 1 0.550290 0.562374 0.303120 -21.00000 0.03317 0.03911 = 0.03470 -0.00269 0.01017 0.01467 AFIX 43 H20B 2 0.438224 0.600967 0.329162 -21.00000 -1.20000 AFIX 0 C21A 1 0.540085 0.567344 0.216024 -21.00000 0.03278 0.04290 = 0.04261 -0.00172 0.00733 0.01411 AFIX 43 H21B 2 0.421536 0.606376 0.180179 -21.00000 -1.20000 AFIX 0 C22A 1 0.720689 0.509569 0.182508 -21.00000 0.04851 0.03636 = 0.04214 -0.00615 0.00818 0.00111 C23A 1 0.883374 0.453230 0.226687 -21.00000 0.03065 0.04078 = 0.04086 -0.00376 0.00784 0.00211 AFIX 43 H23B 2 0.995493 0.417023 0.198912 -21.00000 -1.20000 AFIX 0 C24A 1 0.894386 0.445601 0.314439 -21.00000 0.02575 0.03653 = 0.04219 -0.00359 0.00883 0.00485 AFIX 43 H24B 2 1.015478 0.403503 0.345931 -21.00000 -1.20000 AFIX 0 PART 0 C25 1 0.719126 0.515132 0.089219 11.00000 0.08260 0.04199 = 0.05467 -0.00403 0.01669 0.00343 HKLF 4 REM DS_B1_0025 in P2(1) REM R1 = 0.0854 for 2319 Fo > 4sig(Fo) and 0.1503 for all 3903 data REM 335 parameters refined using 49 restraints END WGHT 0.0522 2.3324 REM Highest difference peak 0.549, deepest hole -0.477, 1-sigma level 0.069 Q1 1 0.2434 0.6776 0.5628 11.00000 0.05 0.55 Q2 1 0.2214 0.6721 0.4182 11.00000 0.05 0.40 Q3 1 0.3039 0.6708 0.6536 11.00000 0.05 0.36 Q4 1 0.4143 0.6529 0.5309 11.00000 0.05 0.35 Q5 1 0.0433 0.6646 0.4396 11.00000 0.05 0.34 Q6 1 0.4300 0.7145 0.5514 11.00000 0.05 0.31 Q7 1 0.0459 0.7015 0.5315 11.00000 0.05 0.27 Q8 1 0.4237 0.7112 0.4587 11.00000 0.05 0.27 Q9 1 0.7417 0.4784 0.5221 11.00000 0.05 0.26 Q10 1 0.8809 0.5769 0.6968 11.00000 0.05 0.26 ; _shelx_res_checksum 67923 _shelx_hkl_file ; 1 0 0 -4.10 5.40 -1 0 0 3.60 7.70 -1 0 0 2.90 6.00 1 0 0 -6.40 8.80 1 0 0 0.60 5.00 2 0 0 2912.11 164.18 2 0 0 3003.50 167.38 2 0 0 2768.62 163.98 -2 0 0 2797.62 165.78 -2 0 0 2859.41 164.88 -2 0 0 3071.49 164.58 3 0 0 149.39 38.00 -3 0 0 200.08 35.30 -3 0 0 222.78 34.70 -3 0 0 156.18 29.80 4 0 0 817.22 55.19 -4 0 0 739.53 55.19 5 0 0 45.20 20.70 -5 0 0 4.10 27.10 -6 0 0 143.49 25.40 0 -1 0 -1.10 1.90 0 1 0 0.00 2.10 1 -1 0 4741.63 286.77 -1 -1 0 5909.81 287.47 -1 -1 0 4757.52 286.37 1 -1 0 5409.86 287.27 1 -1 0 4786.42 286.77 -1 1 0 5029.00 287.87 -1 1 0 4911.51 288.17 -1 1 0 5482.55 288.67 2 -1 0 865.71 58.79 2 -1 0 1113.89 61.09 -2 -1 0 941.41 59.49 2 -1 0 943.31 59.29 -2 1 0 925.71 59.49 -2 1 0 942.11 58.19 -2 1 0 989.10 61.09 3 -1 0 79.29 24.40 3 -1 0 33.50 36.00 -3 -1 0 83.59 27.40 3 -1 0 8.30 21.00 -3 1 0 46.80 16.40 -3 1 0 32.60 21.10 -3 1 0 37.80 25.00 4 -1 0 10.00 16.90 4 -1 0 11.50 15.20 -4 1 0 28.00 18.20 -5 -1 0 230.98 38.70 5 -1 0 204.88 37.70 -5 1 0 165.98 33.60 5 1 0 227.58 35.60 6 -1 0 257.37 32.30 0 -2 0 2698.53 152.58 0 -2 0 2726.53 152.58 0 2 0 2424.56 136.49 0 2 0 2422.76 136.39 1 -2 0 6080.79 327.07 1 -2 0 5587.04 326.27 1 -2 0 5773.62 326.37 -1 2 0 5530.25 314.47 -1 2 0 5680.23 314.97 2 -2 0 1130.39 68.29 -2 -2 0 1155.18 67.69 -2 -2 0 1020.50 65.49 2 -2 0 1066.19 68.19 -2 2 0 1114.09 72.89 -2 2 0 1390.36 76.89 -2 2 0 1117.99 75.29 3 -2 0 49.60 38.50 -3 -2 0 43.10 27.20 3 -2 0 66.69 29.50 3 -2 0 41.70 16.30 -3 2 0 26.10 13.90 3 2 0 33.60 19.60 -3 2 0 47.40 31.10 -3 2 0 39.90 22.80 4 -2 0 177.88 33.30 4 2 0 105.79 21.00 -4 2 0 122.69 19.60 5 -2 0 178.68 34.40 5 -2 0 103.79 17.70 5 2 0 241.48 36.30 -6 -2 0 193.98 54.89 6 -2 0 329.77 32.90 -6 2 0 191.28 28.50 0 -3 0 -7.30 8.20 0 -3 0 -11.70 8.00 0 3 0 0.40 8.00 0 3 0 -9.40 6.80 -1 -3 0 7788.02 404.46 1 -3 0 7213.18 404.66 1 -3 0 6811.32 403.36 1 -3 0 6933.51 403.56 -1 3 0 6670.93 374.46 -1 3 0 6668.03 375.06 2 -3 0 161.18 32.20 -2 -3 0 218.58 28.70 2 -3 0 232.78 34.70 -2 -3 0 217.78 35.50 2 -3 0 199.48 31.40 -2 3 0 183.68 27.50 -2 3 0 267.97 35.10 -2 3 0 195.58 21.10 3 -3 0 327.57 62.29 -3 -3 0 172.38 35.00 3 -3 0 253.97 31.60 3 -3 0 242.58 50.69 -3 3 0 294.17 29.10 -3 3 0 322.57 47.40 -3 3 0 268.67 45.80 3 3 0 218.98 36.90 4 -3 0 42.10 15.50 4 3 0 44.30 17.70 -4 3 0 31.90 17.50 5 -3 0 238.38 28.20 5 -3 0 292.57 39.40 -5 3 0 241.38 29.90 5 3 0 346.47 37.60 6 -3 0 23.00 17.80 0 -4 0 3218.68 179.58 0 -4 0 3106.79 179.58 0 4 0 3123.49 177.38 0 4 0 3141.99 178.08 -1 -4 0 211.28 28.20 1 -4 0 214.48 26.90 1 -4 0 245.08 27.10 1 -4 0 209.88 26.30 -1 4 0 218.28 22.70 2 -4 0 521.55 50.09 2 -4 0 540.65 51.39 2 -4 0 500.35 40.80 2 -4 0 549.35 54.69 -2 -4 0 522.35 47.80 -2 4 0 532.45 51.59 -2 4 0 464.55 34.00 -2 4 0 482.05 42.80 3 -4 0 305.97 49.10 -3 -4 0 385.06 57.89 -3 -4 0 255.57 55.19 -3 4 0 342.47 27.90 -3 4 0 390.26 58.59 3 4 0 321.97 40.40 3 4 0 299.47 35.50 3 4 0 250.87 53.79 -3 4 0 240.68 60.69 4 -4 0 53.09 17.60 4 -4 0 57.99 23.50 4 4 0 80.69 25.00 -4 4 0 114.19 19.70 4 4 0 135.99 30.00 4 4 0 67.99 47.20 5 -4 0 33.30 23.50 5 -4 0 39.10 15.80 -5 4 0 33.50 17.10 5 4 0 58.89 19.00 0 -5 0 -11.20 14.20 0 -5 0 1.30 17.10 0 -5 0 -12.00 13.40 0 5 0 -4.00 14.10 0 5 0 -12.90 10.80 1 -5 0 448.36 46.40 -1 -5 0 572.64 36.60 -1 -5 0 534.05 35.10 1 -5 0 490.45 45.30 -1 -5 0 575.64 49.30 1 -5 0 451.85 52.79 1 -5 0 391.36 45.20 1 -5 0 458.45 45.90 -1 5 0 399.06 36.00 -1 5 0 376.56 42.80 -2 -5 0 19.80 25.60 2 -5 0 22.70 20.60 2 -5 0 80.59 31.90 2 -5 0 0.40 33.40 -2 -5 0 17.10 34.40 2 -5 0 8.30 28.40 2 -5 0 38.00 42.40 -2 5 0 63.49 22.80 -2 5 0 81.09 34.20 3 -5 0 137.39 71.49 3 -5 0 178.48 21.10 3 5 0 183.08 24.70 3 5 0 212.08 28.00 3 5 0 208.88 35.10 -3 5 0 188.28 23.00 4 -5 0 31.30 27.70 4 -5 0 49.90 17.30 4 5 0 65.59 21.20 4 5 0 108.99 21.10 4 5 0 29.30 36.00 -4 5 0 95.39 18.60 5 -5 0 153.98 24.60 5 -5 0 142.19 32.30 -5 5 0 141.59 27.00 0 -6 0 251.87 33.90 0 -6 0 267.67 38.90 0 -6 0 221.88 47.10 0 -6 0 243.18 38.40 0 6 0 268.77 40.60 0 6 0 241.08 30.40 1 -6 0 964.10 76.39 1 -6 0 811.22 78.49 1 -6 0 934.11 71.99 -1 -6 0 975.10 61.09 1 -6 0 828.32 84.39 -1 -6 0 986.50 63.39 -1 -6 0 1108.99 76.79 -1 6 0 815.92 72.69 -1 6 0 871.71 62.29 2 -6 0 805.22 81.29 -2 -6 0 920.51 81.79 2 -6 0 767.72 61.09 2 -6 0 732.83 63.89 -2 -6 0 885.01 88.49 2 -6 0 741.63 68.99 2 6 0 934.21 63.39 2 6 0 813.92 56.69 -2 6 0 771.52 71.59 -2 6 0 880.01 54.39 -2 6 0 822.62 64.89 3 -6 0 90.29 112.19 -3 6 0 -2.40 14.90 3 6 0 19.60 25.90 3 6 0 17.40 17.40 -3 6 0 59.39 34.80 3 6 0 12.40 20.00 4 -6 0 50.49 19.10 -4 6 0 113.69 20.60 4 6 0 71.39 36.80 4 6 0 66.69 20.30 5 6 0 97.89 22.80 -5 6 0 54.89 19.90 -6 6 0 80.89 25.70 6 6 0 104.89 20.30 0 -7 0 9.50 29.90 0 -7 0 6.90 30.10 0 -7 0 19.50 27.40 0 -7 0 21.80 31.80 0 7 0 2.20 21.40 0 7 0 14.50 22.20 -1 -7 0 1773.82 114.69 -1 -7 0 2097.79 128.49 1 -7 0 1720.93 125.99 -1 -7 0 1750.12 111.19 -1 -7 0 2084.39 129.59 1 -7 0 1541.75 130.69 1 -7 0 1831.42 124.39 1 7 0 1906.61 125.49 -1 7 0 2162.18 123.09 -1 7 0 1790.62 120.39 1 7 0 2245.18 118.09 2 -7 0 337.67 67.89 2 -7 0 253.47 42.10 2 -7 0 289.27 53.89 2 -7 0 344.37 49.00 -2 -7 0 295.67 63.09 -2 7 0 295.27 41.50 2 7 0 352.46 42.00 -2 7 0 285.57 37.00 -2 7 0 408.96 79.29 2 7 0 336.67 30.50 3 -7 0 144.59 23.70 -3 7 0 161.58 27.80 3 7 0 105.19 19.70 3 7 0 205.98 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-2 -16 32.40 12.30 3 2 -16 29.40 11.20 -3 2 16 26.30 29.30 -2 -2 16 181.58 76.09 2 2 -16 44.90 14.00 -2 2 16 29.00 21.20 1 -2 -16 1.80 18.70 -1 -2 16 20.10 21.00 1 2 -16 29.20 14.90 -1 2 16 20.60 16.90 0 -2 -16 42.80 71.49 0 -2 16 21.50 17.40 0 -2 -16 36.60 27.90 0 -2 16 16.60 20.30 0 2 16 20.90 14.80 0 2 -16 30.30 18.20 -1 -2 -16 30.10 50.59 1 -2 16 19.90 13.20 1 2 16 14.40 12.30 1 2 16 35.50 16.00 -1 2 -16 54.19 25.40 2 -2 16 9.60 10.40 2 -2 16 15.60 13.10 -2 -2 -16 49.00 44.60 2 2 16 13.10 11.60 2 2 16 23.50 10.70 4 -3 -16 3.60 7.80 4 -3 -16 8.20 16.40 -4 -3 16 50.69 25.00 4 3 -16 2.50 12.60 -3 -3 16 0.20 30.60 3 -3 -16 -12.20 10.30 -3 3 16 -1.20 24.70 3 3 -16 6.50 9.70 -2 -3 16 35.40 40.20 2 -3 -16 16.10 15.00 -2 3 16 -9.20 19.10 2 3 -16 11.80 12.10 1 -3 -16 13.40 21.50 -1 -3 16 37.30 26.30 -1 3 16 16.50 14.40 1 3 -16 46.70 15.90 0 -3 -16 78.19 61.59 0 3 -16 35.00 17.80 0 3 16 18.20 12.90 -1 -3 -16 97.89 44.50 1 3 16 -0.40 10.90 1 3 16 -22.30 15.30 2 -3 16 1.80 9.90 -2 -3 -16 -12.10 40.20 2 -3 16 6.70 11.90 2 3 16 14.30 11.80 3 -4 -16 3.80 12.40 -3 -4 16 27.70 31.40 -3 4 16 16.00 21.00 3 4 -16 19.40 10.50 -2 -4 16 68.49 39.00 2 4 -16 7.40 12.30 -2 4 16 30.60 15.70 -1 -4 16 19.70 29.60 1 -4 -16 19.90 24.30 -1 4 16 11.80 14.30 1 4 -16 24.30 13.00 0 -4 -16 136.19 57.39 0 4 16 22.80 14.10 0 4 -16 4.90 14.90 -1 -4 -16 119.09 47.30 1 4 16 20.70 16.00 -1 4 -16 24.10 17.90 1 4 16 1.50 12.00 2 -4 16 16.90 10.40 2 -4 16 17.10 12.00 -2 -4 -16 44.20 37.20 2 4 16 6.40 11.90 -3 -5 16 -6.40 24.80 3 -5 -16 20.30 11.40 3 5 -16 18.50 17.00 -3 5 16 -1.30 18.40 3 5 -16 8.80 9.50 2 -5 -16 13.70 17.20 -2 -5 16 31.60 46.70 -2 5 16 4.60 14.70 2 5 -16 11.50 10.80 1 -5 -16 49.99 27.70 -1 5 16 2.70 14.10 1 5 -16 29.60 11.70 0 -5 -16 140.39 84.09 0 5 16 -13.40 11.90 0 5 -16 29.50 12.20 -1 -5 -16 14.40 38.90 1 -5 16 3.60 13.30 -1 5 -16 11.00 14.20 1 5 16 18.30 11.40 -3 -6 16 9.20 26.70 3 -6 -16 4.60 10.90 3 6 -16 34.70 17.60 2 -6 -16 22.60 18.40 -2 -6 16 -14.80 36.90 2 6 -16 10.80 10.30 -2 6 16 1.70 12.80 1 6 -16 27.80 10.90 -1 6 16 15.10 13.10 0 -6 -16 -60.39 55.29 0 -6 16 -18.40 23.40 0 6 16 1.40 11.60 0 6 -16 19.30 11.20 -1 -6 -16 69.99 38.50 -1 6 -16 15.50 13.60 -2 -7 16 -49.30 53.79 2 7 -16 16.50 9.30 -2 7 16 -11.50 12.90 -1 7 16 -4.30 11.80 1 7 -16 1.80 9.10 0 -7 16 5.30 31.40 0 -7 -16 146.89 65.59 0 7 -16 9.30 9.90 0 7 16 7.20 10.90 3 0 -17 0.40 9.50 2 0 -17 2.70 13.00 -2 0 17 31.40 24.30 -1 0 17 17.60 17.50 1 0 -17 27.90 15.80 0 0 -17 12.00 22.00 0 0 17 6.20 13.70 1 0 17 7.10 12.10 1 0 17 17.00 19.20 3 -1 -17 4.80 9.30 3 1 -17 17.20 10.00 2 -1 -17 31.70 12.40 -2 -1 17 42.50 29.50 2 1 -17 20.00 12.90 -2 1 17 -13.00 18.70 1 -1 -17 16.80 17.80 -1 -1 17 39.30 18.70 1 1 -17 38.20 16.60 -1 1 17 41.00 17.20 0 -1 -17 -21.30 25.80 0 -1 17 18.90 13.50 0 1 17 16.80 12.80 0 1 -17 1.60 19.10 1 -1 17 5.50 15.90 1 -1 17 20.20 12.00 1 1 17 39.60 20.10 3 -2 -17 12.90 9.50 -3 2 17 30.10 27.20 3 2 -17 9.30 8.80 2 -2 -17 9.70 13.20 -2 2 17 19.80 17.60 2 2 -17 24.50 10.90 1 -2 -17 -2.00 18.20 -1 -2 17 -0.60 20.20 -1 2 17 17.30 14.40 1 2 -17 11.00 13.70 0 -2 17 19.70 16.10 0 2 -17 32.00 18.00 0 2 17 16.70 12.20 1 -2 17 5.80 11.20 1 -2 17 45.80 16.30 1 2 17 7.10 10.00 -1 2 -17 -43.10 27.20 3 -3 -17 17.40 10.50 -3 3 17 55.79 25.40 2 -3 -17 1.60 12.60 2 3 -17 13.30 11.50 -2 3 17 26.30 15.20 1 -3 -17 44.40 22.00 -1 -3 17 -16.50 24.30 1 3 -17 14.30 12.60 -1 3 17 1.10 13.20 0 -3 17 10.20 14.70 0 3 17 13.40 12.80 0 3 -17 19.60 15.40 -1 -3 -17 174.08 91.19 1 -3 17 -7.90 23.90 1 3 17 -0.50 10.80 -1 3 -17 -18.40 23.60 3 -4 -17 140.69 30.00 3 4 -17 18.50 8.80 3 4 -17 34.50 15.70 -3 4 17 20.60 21.80 2 -4 -17 14.70 14.80 2 4 -17 0.10 9.50 -2 4 17 8.30 14.60 1 -4 -17 36.70 24.40 -1 -4 17 14.80 28.10 -1 4 17 47.30 14.10 1 4 -17 56.89 13.50 0 -4 17 14.50 17.40 0 4 -17 17.80 13.90 0 4 17 12.50 11.50 1 -4 17 51.19 14.80 -1 -4 -17 181.18 110.39 1 -4 17 25.30 11.60 1 4 17 47.30 11.10 -1 4 -17 81.29 19.60 2 -5 -17 23.00 18.20 -2 5 17 3.60 13.80 2 5 -17 9.00 8.80 -1 5 17 12.60 12.00 1 5 -17 25.80 10.70 0 -5 17 11.60 21.70 0 5 17 8.30 10.40 0 5 -17 14.30 12.70 2 -6 -17 2.10 20.90 2 6 -17 8.90 8.30 -2 6 17 7.50 12.00 2 6 -17 47.20 17.00 1 6 -17 9.30 8.90 -1 6 17 7.40 9.80 0 -6 17 -37.20 24.30 0 6 17 12.60 9.80 0 6 -17 18.90 10.40 -2 0 18 26.50 31.20 2 0 -18 7.30 11.20 -1 0 18 21.20 16.60 1 0 -18 48.20 16.60 0 0 -18 -2.90 25.20 0 0 18 17.60 12.00 2 -1 -18 8.30 11.90 -2 -1 18 25.20 27.90 2 1 -18 4.10 11.40 -2 1 18 23.00 22.70 1 -1 -18 15.80 17.10 -1 -1 18 7.10 15.90 1 1 -18 18.80 13.10 -1 1 18 17.20 15.60 0 -1 18 9.50 12.30 0 -1 -18 31.00 27.00 0 1 -18 -8.80 22.70 0 1 18 -3.90 11.20 2 -2 -18 12.40 11.20 -2 2 18 30.50 16.10 2 2 -18 4.20 10.20 -1 -2 18 -4.20 19.80 1 -2 -18 23.10 18.80 1 2 -18 6.30 13.30 -1 2 18 2.50 13.00 0 -2 18 14.00 12.60 0 2 18 11.80 10.60 0 2 -18 -0.60 17.80 2 -3 -18 5.50 14.10 -2 3 18 15.20 14.90 2 3 -18 15.90 8.90 1 -3 -18 36.00 22.40 -1 -3 18 13.40 24.50 1 3 -18 22.80 12.30 -1 3 18 14.00 12.30 0 -3 18 25.30 14.60 0 3 18 9.30 10.30 0 3 -18 19.60 19.50 -1 -4 18 35.10 28.60 -1 4 18 18.80 10.60 1 4 -18 22.70 11.40 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 95167 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -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 Cl1 Cl 0.2358(4) 0.6731(3) 0.4901(2) 0.0534(8) Uani 1 1 d . . . . . F1 F 0.618(2) 0.4330(8) 0.0471(5) 0.122(4) Uani 1 1 d . . . . . F2 F 0.929(2) 0.5219(10) 0.0656(6) 0.111(4) Uani 1 1 d . . . . . F3 F 0.6027(19) 0.5979(8) 0.0516(5) 0.106(4) Uani 1 1 d . . . . . N1 N 0.5235(16) 0.4843(7) 0.6928(6) 0.039(2) Uani 1 1 d . . . . . N2 N 0.3307(16) 0.3707(8) 0.5930(6) 0.047(2) Uani 1 1 d . . . . . N3 N 0.4964(16) 0.4283(6) 0.5593(6) 0.038(2) Uani 1 1 d . . . . . N4 N 0.7475(14) 0.5852(5) 0.5015(5) 0.032(2) Uani 1 1 d . . . . . H4A H 0.867060 0.625063 0.486725 0.038 Uiso 1 1 calc R U . . . H4B H 0.608320 0.620084 0.485121 0.038 Uiso 1 1 calc R U . . . C1 C 0.356(2) 0.4041(9) 0.6735(7) 0.043(3) Uani 1 1 d . . . . . C2 C 0.5987(19) 0.4957(8) 0.6186(7) 0.036(2) Uani 1 1 d . . . . . C3 C 0.7864(18) 0.5713(7) 0.5969(6) 0.030(2) Uani 1 1 d . . . . . H3A H 0.947440 0.540101 0.615446 0.036 Uiso 1 1 calc R U . . . C4 C 0.7386(18) 0.4826(7) 0.4538(7) 0.031(2) Uani 1 1 d . . . . . H4 H 0.880870 0.439838 0.477727 0.037 Uiso 1 1 calc R U . A 1 C5 C 0.514(2) 0.4252(8) 0.4691(7) 0.039(3) Uani 1 1 d . . . . . H5A H 0.372390 0.458801 0.435446 0.046 Uiso 1 1 calc R U . . . H5B H 0.519948 0.351656 0.449930 0.046 Uiso 1 1 calc R U . . . C6 C 0.215(2) 0.3666(9) 0.7354(8) 0.043(3) Uani 1 1 d . . . . . C7 C 0.015(2) 0.3091(12) 0.7085(10) 0.068(4) Uani 1 1 d . . . . . H7A H -0.027253 0.292187 0.649385 0.081 Uiso 1 1 calc R U . . . C8 C -0.128(2) 0.2748(18) 0.7675(11) 0.108(8) Uani 1 1 d . . . . . H8A H -0.265506 0.233700 0.748170 0.130 Uiso 1 1 calc R U . . . C9 C -0.072(3) 0.3003(16) 0.8535(11) 0.096(7) Uani 1 1 d . . . . . H9A H -0.173731 0.279813 0.892916 0.115 Uiso 1 1 calc R U . . . C10 C 0.132(3) 0.3556(13) 0.8811(9) 0.077(5) Uani 1 1 d . . . . . H10A H 0.176343 0.371088 0.940446 0.093 Uiso 1 1 calc R U . . . C11 C 0.275(3) 0.3892(10) 0.8223(8) 0.057(4) Uani 1 1 d . . . . . H11A H 0.415436 0.427950 0.841908 0.068 Uiso 1 1 calc R U . . . C12 C 0.7766(16) 0.6796(8) 0.6398(6) 0.036(2) Uani 1 1 d . . . . . H12A H 0.871862 0.729371 0.611270 0.043 Uiso 1 1 calc R U . . . H12B H 0.609772 0.704386 0.629527 0.043 Uiso 1 1 calc R U . . . C13 C 0.8642(17) 0.6827(9) 0.7339(7) 0.036(2) Uani 1 1 d . . . . . C14 C 0.727(2) 0.7249(11) 0.7903(8) 0.061(4) Uani 1 1 d . . . . . H14A H 0.572768 0.750480 0.768274 0.073 Uiso 1 1 calc R U . . . C15 C 0.806(3) 0.7310(13) 0.8768(9) 0.078(5) Uani 1 1 d . . . . . H15A H 0.707763 0.760913 0.913740 0.094 Uiso 1 1 calc R U . . . C16 C 1.027(3) 0.6940(12) 0.9098(8) 0.070(4) Uani 1 1 d . . . . . H16A H 1.082049 0.696977 0.969859 0.085 Uiso 1 1 calc R U . . . C17 C 1.166(3) 0.6527(10) 0.8558(8) 0.062(4) Uani 1 1 d . . . . . H17A H 1.319911 0.627187 0.878788 0.075 Uiso 1 1 calc R U . . . C18 C 1.090(2) 0.6471(9) 0.7690(8) 0.054(3) Uani 1 1 d . . . . . H18A H 1.191388 0.618821 0.732520 0.065 Uiso 1 1 calc R U . . . C19 C 0.7350(17) 0.4972(8) 0.3592(7) 0.035(2) Uani 0.55(3) 1 d . . P B 1 C20 C 0.696(5) 0.5870(17) 0.3200(14) 0.038(6) Uani 0.55(3) 1 d . U P B 1 H20A H 0.674755 0.648076 0.352287 0.046 Uiso 0.55(3) 1 calc R U P B 1 C21 C 0.684(4) 0.5938(16) 0.2324(14) 0.038(6) Uani 0.55(3) 1 d . U P B 1 H21A H 0.649429 0.659607 0.205337 0.045 Uiso 0.55(3) 1 calc R U P B 1 C22 C 0.721(2) 0.5096(9) 0.1825(7) 0.042(3) Uani 0.55(3) 1 d . . P B 1 C23 C 0.785(5) 0.414(2) 0.2276(16) 0.048(7) Uani 0.55(3) 1 d . U P B 1 H23A H 0.823264 0.353789 0.196889 0.058 Uiso 0.55(3) 1 calc R U P B 1 C24 C 0.792(5) 0.408(2) 0.3164(15) 0.045(7) Uani 0.55(3) 1 d . U P B 1 H24A H 0.834406 0.344934 0.346787 0.054 Uiso 0.55(3) 1 calc R U P B 1 C19A C 0.7350(17) 0.4972(8) 0.3592(7) 0.035(2) Uani 0.45(3) 1 d . . P B 2 C20A C 0.550(5) 0.562(2) 0.3031(16) 0.035(7) Uani 0.45(3) 1 d . U P B 2 H20B H 0.438224 0.600967 0.329162 0.042 Uiso 0.45(3) 1 calc R U P B 2 C21A C 0.540(5) 0.567(2) 0.2160(16) 0.039(7) Uani 0.45(3) 1 d . U P B 2 H21B H 0.421536 0.606376 0.180179 0.047 Uiso 0.45(3) 1 calc R U P B 2 C22A C 0.721(2) 0.5096(9) 0.1825(7) 0.042(3) Uani 0.45(3) 1 d . . P B 2 C23A C 0.883(5) 0.453(2) 0.2267(18) 0.037(7) Uani 0.45(3) 1 d . U P B 2 H23B H 0.995493 0.417023 0.198912 0.045 Uiso 0.45(3) 1 calc R U P B 2 C24A C 0.894(5) 0.446(2) 0.3144(18) 0.034(7) Uani 0.45(3) 1 d . U P B 2 H24B H 1.015478 0.403503 0.345931 0.041 Uiso 0.45(3) 1 calc R U P B 2 C25 C 0.719(3) 0.5151(10) 0.0892(9) 0.059(4) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cl1 0.0186(12) 0.0631(18) 0.078(2) -0.0116(19) 0.0074(11) -0.0035(15) F1 0.231(13) 0.088(7) 0.048(5) -0.021(5) 0.029(6) -0.057(8) F2 0.118(8) 0.153(10) 0.072(6) 0.019(7) 0.047(6) 0.005(7) F3 0.166(10) 0.108(7) 0.041(5) 0.009(5) 0.009(5) 0.054(7) N1 0.051(6) 0.030(5) 0.040(5) 0.000(4) 0.021(4) -0.001(4) N2 0.048(6) 0.038(5) 0.060(7) 0.007(5) 0.025(5) -0.010(5) N3 0.044(6) 0.027(5) 0.046(6) -0.004(5) 0.018(5) -0.008(4) N4 0.025(4) 0.020(4) 0.052(6) -0.005(4) 0.015(4) -0.006(4) C1 0.045(7) 0.042(7) 0.046(7) 0.009(6) 0.019(6) 0.007(5) C2 0.049(7) 0.022(5) 0.040(6) -0.005(5) 0.013(5) 0.005(5) C3 0.034(6) 0.026(5) 0.032(6) 0.000(5) 0.010(5) -0.004(4) C4 0.031(5) 0.021(5) 0.043(6) -0.009(5) 0.010(5) 0.005(4) C5 0.056(7) 0.018(5) 0.044(7) -0.004(5) 0.015(6) -0.010(5) C6 0.047(7) 0.033(6) 0.055(8) 0.016(6) 0.023(6) 0.016(6) C7 0.033(7) 0.098(11) 0.071(10) 0.030(9) 0.006(6) -0.009(7) C8 0.038(8) 0.21(2) 0.076(12) 0.068(13) 0.003(8) -0.041(11) C9 0.044(9) 0.164(19) 0.082(13) 0.071(13) 0.015(8) 0.005(10) C10 0.099(12) 0.083(12) 0.061(10) 0.023(9) 0.044(9) 0.024(10) C11 0.083(9) 0.043(7) 0.053(8) 0.008(7) 0.040(7) -0.006(7) C12 0.041(5) 0.020(5) 0.048(6) 0.000(5) 0.010(5) -0.005(5) C13 0.043(6) 0.025(5) 0.041(6) 0.002(5) 0.012(5) -0.008(6) C14 0.048(8) 0.089(11) 0.050(8) -0.018(7) 0.020(6) -0.009(7) C15 0.069(10) 0.126(15) 0.045(9) -0.030(9) 0.025(7) -0.016(9) C16 0.106(12) 0.078(11) 0.028(7) 0.000(7) 0.011(7) -0.038(10) C17 0.081(9) 0.046(8) 0.056(9) 0.008(7) -0.002(7) 0.010(7) C18 0.066(8) 0.053(8) 0.044(7) 0.005(6) 0.013(6) 0.009(6) C19 0.025(5) 0.034(6) 0.045(6) -0.006(6) 0.006(5) 0.002(5) C20 0.041(11) 0.030(9) 0.045(10) -0.007(8) 0.010(9) 0.006(8) C21 0.038(11) 0.023(9) 0.051(11) 0.000(8) 0.006(9) 0.003(8) C22 0.049(7) 0.036(6) 0.042(6) -0.006(6) 0.008(5) 0.001(5) C23 0.065(13) 0.036(11) 0.044(11) -0.010(9) 0.008(10) 0.009(10) C24 0.061(12) 0.037(11) 0.038(10) -0.009(9) 0.005(9) 0.011(10) C19A 0.025(5) 0.034(6) 0.045(6) -0.006(6) 0.006(5) 0.002(5) C20A 0.033(12) 0.039(11) 0.035(11) -0.003(9) 0.010(9) 0.015(9) C21A 0.033(12) 0.043(12) 0.043(12) -0.002(9) 0.007(9) 0.014(10) C22A 0.049(7) 0.036(6) 0.042(6) -0.006(6) 0.008(5) 0.001(5) C23A 0.031(11) 0.041(12) 0.041(12) -0.004(10) 0.008(9) 0.002(10) C24A 0.026(11) 0.037(12) 0.042(12) -0.004(10) 0.009(9) 0.005(9) C25 0.083(10) 0.042(8) 0.055(8) -0.004(7) 0.017(8) 0.003(7) 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' N N 0.0311 0.0180 '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' Cl Cl 0.3639 0.7018 '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 C2 N1 C1 101.2(9) . . ? C1 N2 N3 102.8(9) . . ? C2 N3 N2 109.0(9) . . ? C2 N3 C5 128.1(8) . . ? N2 N3 C5 121.9(8) . . ? C3 N4 C4 112.7(7) . . ? C3 N4 H4A 109.0 . . ? C4 N4 H4A 109.0 . . ? C3 N4 H4B 109.0 . . ? C4 N4 H4B 109.0 . . ? H4A N4 H4B 107.8 . . ? N2 C1 N1 114.2(9) . . ? N2 C1 C6 123.7(11) . . ? N1 C1 C6 122.0(10) . . ? N1 C2 N3 112.6(10) . . ? N1 C2 C3 127.6(9) . . ? N3 C2 C3 119.8(9) . . ? N4 C3 C2 107.8(8) . . ? N4 C3 C12 109.0(8) . . ? C2 C3 C12 113.3(8) . . ? N4 C3 H3A 108.9 . . ? C2 C3 H3A 108.9 . . ? C12 C3 H3A 108.9 . . ? C19A C4 N4 112.5(8) . . ? C19 C4 N4 112.5(8) . . ? C19A C4 C5 109.8(8) . . ? C19 C4 C5 109.8(8) . . ? N4 C4 C5 107.5(7) . . ? C19 C4 H4 109.0 . . ? N4 C4 H4 109.0 . . ? C5 C4 H4 109.0 . . ? N3 C5 C4 109.6(8) . . ? N3 C5 H5A 109.8 . . ? C4 C5 H5A 109.8 . . ? N3 C5 H5B 109.8 . . ? C4 C5 H5B 109.8 . . ? H5A C5 H5B 108.2 . . ? C7 C6 C11 118.9(11) . . ? C7 C6 C1 119.7(12) . . ? C11 C6 C1 121.4(11) . . ? C6 C7 C8 120.4(15) . . ? C6 C7 H7A 119.8 . . ? C8 C7 H7A 119.8 . . ? C9 C8 C7 120.6(15) . . ? C9 C8 H8A 119.7 . . ? C7 C8 H8A 119.7 . . ? C10 C9 C8 119.0(14) . . ? C10 C9 H9A 120.5 . . ? C8 C9 H9A 120.5 . . ? C9 C10 C11 120.1(15) . . ? C9 C10 H10A 119.9 . . ? C11 C10 H10A 119.9 . . ? C6 C11 C10 120.9(14) . . ? C6 C11 H11A 119.6 . . ? C10 C11 H11A 119.6 . . ? C13 C12 C3 115.5(9) . . ? C13 C12 H12A 108.4 . . ? C3 C12 H12A 108.4 . . ? C13 C12 H12B 108.4 . . ? C3 C12 H12B 108.4 . . ? H12A C12 H12B 107.5 . . ? C14 C13 C18 116.9(11) . . ? C14 C13 C12 121.1(10) . . ? C18 C13 C12 121.9(10) . . ? C15 C14 C13 122.2(13) . . ? C15 C14 H14A 118.9 . . ? C13 C14 H14A 118.9 . . ? C16 C15 C14 119.8(14) . . ? C16 C15 H15A 120.1 . . ? C14 C15 H15A 120.1 . . ? C17 C16 C15 119.3(13) . . ? C17 C16 H16A 120.3 . . ? C15 C16 H16A 120.3 . . ? C16 C17 C18 121.4(13) . . ? C16 C17 H17A 119.3 . . ? C18 C17 H17A 119.3 . . ? C17 C18 C13 120.4(12) . . ? C17 C18 H18A 119.8 . . ? C13 C18 H18A 119.8 . . ? C20 C19 C24 121.8(17) . . ? C20 C19 C4 123.6(12) . . ? C24 C19 C4 114.4(14) . . ? C19 C20 C21 120.5(18) . . ? C19 C20 H20A 119.8 . . ? C21 C20 H20A 119.8 . . ? C22 C21 C20 122.7(19) . . ? C22 C21 H21A 118.6 . . ? C20 C21 H21A 118.6 . . ? C21 C22 C23 115.9(15) . . ? C21 C22 C25 124.0(14) . . ? C23 C22 C25 119.8(14) . . ? C24 C23 C22 120.3(19) . . ? C24 C23 H23A 119.8 . . ? C22 C23 H23A 119.8 . . ? C19 C24 C23 118(2) . . ? C19 C24 H24A 120.9 . . ? C23 C24 H24A 120.9 . . ? C24A C19A C4 122.4(14) . . ? C24A C19A C20A 114.3(16) . . ? C4 C19A C20A 123.2(12) . . ? C21A C20A C19A 121.8(19) . . ? C21A C20A H20B 119.1 . . ? C19A C20A H20B 119.1 . . ? C20A C21A C22A 115(2) . . ? C20A C21A H21B 122.3 . . ? C22A C21A H21B 122.3 . . ? C23A C22A C21A 125.8(19) . . ? C23A C22A C25 117.2(16) . . ? C21A C22A C25 116.9(15) . . ? C22A C23A C24A 120(2) . . ? C22A C23A H23B 120.1 . . ? C24A C23A H23B 120.1 . . ? C23A C24A C19A 123(2) . . ? C23A C24A H24B 118.6 . . ? C19A C24A H24B 118.6 . . ? F2 C25 F1 104.7(12) . . ? F2 C25 F3 103.4(12) . . ? F1 C25 F3 105.1(12) . . ? F2 C25 C22A 115.3(12) . . ? F1 C25 C22A 113.3(11) . . ? F3 C25 C22A 113.9(11) . . ? F2 C25 C22 115.3(12) . . ? F1 C25 C22 113.3(11) . . ? F3 C25 C22 113.9(11) . . ? 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 F1 C25 1.324(15) . ? F2 C25 1.308(16) . ? F3 C25 1.337(15) . ? N1 C2 1.316(13) . ? N1 C1 1.400(14) . ? N2 C1 1.326(14) . ? N2 N3 1.369(11) . ? N3 C2 1.336(13) . ? N3 C5 1.441(12) . ? N4 C3 1.495(12) . ? N4 C4 1.509(11) . ? N4 H4A 0.9100 . ? N4 H4B 0.9100 . ? C1 C6 1.443(14) . ? C2 C3 1.520(13) . ? C3 C12 1.546(13) . ? C3 H3A 1.0000 . ? C4 C19A 1.499(14) . ? C4 C19 1.499(14) . ? C4 C5 1.526(14) . ? C4 H4 1.0000 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.363(17) . ? C6 C11 1.388(16) . ? C7 C8 1.402(17) . ? C7 H7A 0.9500 . ? C8 C9 1.38(2) . ? C8 H8A 0.9500 . ? C9 C10 1.37(2) . ? C9 H9A 0.9500 . ? C10 C11 1.396(16) . ? C10 H10A 0.9500 . ? C11 H11A 0.9500 . ? C12 C13 1.489(13) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.383(14) . ? C13 C18 1.391(15) . ? C14 C15 1.368(18) . ? C14 H14A 0.9500 . ? C15 C16 1.37(2) . ? C15 H15A 0.9500 . ? C16 C17 1.360(18) . ? C16 H16A 0.9500 . ? C17 C18 1.371(16) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C19 C20 1.31(2) . ? C19 C24 1.39(2) . ? C20 C21 1.38(3) . ? C20 H20A 0.9500 . ? C21 C22 1.37(2) . ? C21 H21A 0.9500 . ? C22 C23 1.43(3) . ? C22 C25 1.471(17) . ? C23 C24 1.40(3) . ? C23 H23A 0.9500 . ? C24 H24A 0.9500 . ? C19A C24A 1.40(3) . ? C19A C20A 1.51(3) . ? C20A C21A 1.37(3) . ? C20A H20B 0.9500 . ? C21A C22A 1.43(3) . ? C21A H21B 0.9500 . ? C22A C23A 1.29(3) . ? C22A C25 1.471(17) . ? C23A C24A 1.38(4) . ? C23A H23B 0.9500 . ? C24A H24B 0.9500 . ? 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 C1 N2 N3 C2 -3.6(12) . . . . ? C1 N2 N3 C5 -173.3(9) . . . . ? N3 N2 C1 N1 2.7(12) . . . . ? N3 N2 C1 C6 179.1(10) . . . . ? C2 N1 C1 N2 -0.8(12) . . . . ? C2 N1 C1 C6 -177.2(10) . . . . ? C1 N1 C2 N3 -1.7(12) . . . . ? C1 N1 C2 C3 -179.5(10) . . . . ? N2 N3 C2 N1 3.5(13) . . . . ? C5 N3 C2 N1 172.4(10) . . . . ? N2 N3 C2 C3 -178.5(9) . . . . ? C5 N3 C2 C3 -9.7(16) . . . . ? C4 N4 C3 C2 -53.1(10) . . . . ? C4 N4 C3 C12 -176.4(7) . . . . ? N1 C2 C3 N4 -158.8(10) . . . . ? N3 C2 C3 N4 23.5(13) . . . . ? N1 C2 C3 C12 -38.2(15) . . . . ? N3 C2 C3 C12 144.1(9) . . . . ? C3 N4 C4 C19A -171.7(8) . . . . ? C3 N4 C4 C19 -171.7(8) . . . . ? C3 N4 C4 C5 67.3(10) . . . . ? C2 N3 C5 C4 21.7(14) . . . . ? N2 N3 C5 C4 -170.7(9) . . . . ? C19A C4 C5 N3 -169.5(8) . . . . ? C19 C4 C5 N3 -169.5(8) . . . . ? N4 C4 C5 N3 -46.9(11) . . . . ? N2 C1 C6 C7 -12.9(17) . . . . ? N1 C1 C6 C7 163.1(11) . . . . ? N2 C1 C6 C11 168.1(12) . . . . ? N1 C1 C6 C11 -15.8(17) . . . . ? C11 C6 C7 C8 1(2) . . . . ? C1 C6 C7 C8 -178.0(14) . . . . ? C6 C7 C8 C9 1(3) . . . . ? C7 C8 C9 C10 -3(3) . . . . ? C8 C9 C10 C11 3(3) . . . . ? C7 C6 C11 C10 -1.3(19) . . . . ? C1 C6 C11 C10 177.7(12) . . . . ? C9 C10 C11 C6 -1(2) . . . . ? N4 C3 C12 C13 -167.1(8) . . . . ? C2 C3 C12 C13 73.0(11) . . . . ? C3 C12 C13 C14 -127.7(11) . . . . ? C3 C12 C13 C18 54.8(13) . . . . ? C18 C13 C14 C15 -0.6(19) . . . . ? C12 C13 C14 C15 -178.3(12) . . . . ? C13 C14 C15 C16 0(2) . . . . ? C14 C15 C16 C17 1(2) . . . . ? C15 C16 C17 C18 0(2) . . . . ? C16 C17 C18 C13 -1(2) . . . . ? C14 C13 C18 C17 1.3(18) . . . . ? C12 C13 C18 C17 178.9(11) . . . . ? N4 C4 C19 C20 -12.9(19) . . . . ? C5 C4 C19 C20 106.7(17) . . . . ? N4 C4 C19 C24 163.2(16) . . . . ? C5 C4 C19 C24 -77.1(17) . . . . ? C24 C19 C20 C21 7(3) . . . . ? C4 C19 C20 C21 -177.0(16) . . . . ? C19 C20 C21 C22 -2(3) . . . . ? C20 C21 C22 C23 -3(3) . . . . ? C20 C21 C22 C25 -177.4(18) . . . . ? C21 C22 C23 C24 4(3) . . . . ? C25 C22 C23 C24 179(2) . . . . ? C20 C19 C24 C23 -6(3) . . . . ? C4 C19 C24 C23 178(2) . . . . ? C22 C23 C24 C19 0(4) . . . . ? N4 C4 C19A C24A 128.2(18) . . . . ? C5 C4 C19A C24A -112.1(18) . . . . ? N4 C4 C19A C20A -56.0(18) . . . . ? C5 C4 C19A C20A 63.6(18) . . . . ? C24A C19A C20A C21A 1(3) . . . . ? C4 C19A C20A C21A -175(2) . . . . ? C19A C20A C21A C22A -2(4) . . . . ? C20A C21A C22A C23A 2(4) . . . . ? C20A C21A C22A C25 -179(2) . . . . ? C21A C22A C23A C24A -1(4) . . . . ? C25 C22A C23A C24A 180(2) . . . . ? C22A C23A C24A C19A 0(4) . . . . ? C4 C19A C24A C23A 176(2) . . . . ? C20A C19A C24A C23A 0(3) . . . . ? C23A C22A C25 F2 -40(2) . . . . ? C21A C22A C25 F2 140.0(18) . . . . ? C23A C22A C25 F1 80(2) . . . . ? C21A C22A C25 F1 -99(2) . . . . ? C23A C22A C25 F3 -159(2) . . . . ? C21A C22A C25 F3 21(2) . . . . ? C21 C22 C25 F2 97.8(19) . . . . ? C23 C22 C25 F2 -76(2) . . . . ? C21 C22 C25 F1 -141.6(18) . . . . ? C23 C22 C25 F1 44(2) . . . . ? C21 C22 C25 F3 -22(2) . . . . ? C23 C22 C25 F3 164.5(19) . . . . ?