#------------------------------------------------------------------------------ #$Date: 2017-07-16 00:29:33 +0300 (Sun, 16 Jul 2017) $ #$Revision: 198746 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/41/4514164.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_4514164 loop_ _publ_author_name 'He, Congfa' 'Hou, Mengqing' 'Zhu, Zixi' 'Gu, Zhenhua' _publ_section_title ; Enantioselective Synthesis of Indole-Based Biaryl Atropisomers via Palladium-Catalyzed Dynamic Kinetic Intramolecular C--H Cyclization ; _journal_name_full 'ACS Catalysis' _journal_page_first 5316 _journal_paper_doi 10.1021/acscatal.7b01855 _journal_year 2017 _chemical_absolute_configuration ad _chemical_formula_sum 'C55 H44 Cl2 N2 O4' _chemical_formula_weight 867.82 _chemical_name_systematic ; ? ; _space_group_crystal_system monoclinic _space_group_IT_number 5 _space_group_name_Hall 'C 2y' _space_group_name_H-M_alt 'C 1 2 1' _symmetry_space_group_name_Hall 'C 2y' _symmetry_space_group_name_H-M 'C 1 2 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2013 _cell_angle_alpha 90 _cell_angle_beta 127.077(4) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 22.1203(5) _cell_length_b 7.61230(10) _cell_length_c 16.3803(4) _cell_measurement_reflns_used 7752 _cell_measurement_temperature 290(2) _cell_measurement_theta_max 71.2550 _cell_measurement_theta_min 4.9950 _cell_volume 2200.58(14) _computing_cell_refinement 'CrysAlisPro (Agilent Technologies)' _computing_data_collection 'CrysAlisPro (Agilent Technologies)' _computing_data_reduction 'CrysAlisPro (Agilent Technologies)' _computing_molecular_graphics 'Ortep-3 (L. J. Farrugia, 2001)' _computing_publication_material SHELXL-2013 _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _diffrn_ambient_temperature 290(2) _diffrn_detector_area_resol_mean 15.9149 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.983 _diffrn_measurement_device_type 'Gemini S Ultra, Agilent Technologies' _diffrn_measurement_method '\w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0159 _diffrn_reflns_av_unetI/netI 0.0124 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.983 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 9442 _diffrn_reflns_point_group_measured_fraction_full 0.925 _diffrn_reflns_point_group_measured_fraction_max 0.903 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 71.286 _diffrn_reflns_theta_min 4.013 _diffrn_source 'Enhance Ultra (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 1.728 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.33485 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.310 _exptl_crystal_description block _exptl_crystal_F_000 908 _exptl_crystal_size_max 0.320 _exptl_crystal_size_mid 0.240 _exptl_crystal_size_min 0.220 _refine_diff_density_max 0.238 _refine_diff_density_min -0.382 _refine_diff_density_rms 0.035 _refine_ls_abs_structure_details ; Flack x determined using 1545 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack 0.058(9) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 286 _refine_ls_number_reflns 3869 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.056 _refine_ls_R_factor_all 0.0371 _refine_ls_R_factor_gt 0.0365 _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^)+(0.0610P)^2^+0.6499P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1008 _refine_ls_wR_factor_ref 0.1017 _reflns_Friedel_coverage 0.702 _reflns_Friedel_fraction_full 0.841 _reflns_Friedel_fraction_max 0.810 _reflns_number_gt 3794 _reflns_number_total 3869 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file cs7b01855_si_002.cif _cod_data_source_block shelxl _cod_original_cell_volume 2200.58(12) _cod_database_code 4514164 _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 0.608 _shelx_estimated_absorpt_t_max 0.702 _shelxl_version_number 2013-4 _shelx_res_file ; TITL hcf-asy84_a.res in C2 CELL 1.54184 22.1203 7.6123 16.3803 90.000 127.077 90.000 ZERR 2.00 0.0005 0.0001 0.0004 0.000 0.004 0.000 LATT -7 SYMM - X, Y, - Z SFAC C H N O CL UNIT 110 88 4 8 4 MERG 2 MORE -1 FMAP 2 PLAN 20 BOND $H CONF LIST 6 L.S. 10 acta size 0.32 0.24 0.22 WGHT 0.061000 0.649900 FVAR 0.36931 CL1 5 0.496583 0.763379 0.585258 11.00000 0.26620 0.12538 = 0.12628 -0.03251 0.13849 -0.07499 O1 4 0.422350 0.667701 0.746406 11.00000 0.03613 0.04004 = 0.06603 -0.00490 0.02756 0.00175 N1 3 0.303562 0.212329 0.604294 11.00000 0.02816 0.04087 = 0.04977 -0.00329 0.01893 -0.00582 O2 4 0.446587 0.901367 0.854984 11.00000 0.05898 0.06408 = 0.08200 -0.02326 0.03919 -0.00333 C17 1 0.561336 0.349064 0.785181 11.00000 0.03053 0.04358 = 0.03209 0.00257 0.01979 -0.00147 C25 1 0.491634 0.597485 0.781718 11.00000 0.03170 0.04011 = 0.03922 -0.00045 0.02045 -0.00101 C7 1 0.418357 0.336685 0.677487 11.00000 0.02753 0.03859 = 0.03551 -0.00170 0.01695 -0.00071 C8 1 0.365788 0.289086 0.691803 11.00000 0.02890 0.03714 = 0.04122 -0.00120 0.01867 -0.00106 C16 1 0.490863 0.429506 0.749865 11.00000 0.02870 0.04103 = 0.03139 0.00136 0.01790 -0.00302 C22 1 0.630247 0.445727 0.850300 11.00000 0.03142 0.04857 = 0.03450 0.00518 0.01938 -0.00269 C6 1 0.386042 0.287289 0.573649 11.00000 0.03285 0.03907 = 0.03693 -0.00367 0.01712 0.00078 C1 1 0.314354 0.209719 0.530617 11.00000 0.03474 0.03684 = 0.04183 -0.00167 0.01608 -0.00024 C24 1 0.559961 0.692695 0.847168 11.00000 0.03994 0.04114 = 0.04573 -0.00599 0.02364 -0.00831 AFIX 43 H24 2 0.559253 0.805338 0.868560 11.00000 -1.20000 AFIX 0 C23 1 0.626991 0.617539 0.878638 11.00000 0.03327 0.05142 = 0.04020 -0.00427 0.01836 -0.01168 AFIX 43 H23 2 0.671557 0.681863 0.919860 11.00000 -1.20000 AFIX 0 C18 1 0.565736 0.174763 0.759517 11.00000 0.03564 0.04765 = 0.04365 -0.00042 0.02421 -0.00208 AFIX 43 H18 2 0.521474 0.109777 0.717375 11.00000 -1.20000 AFIX 0 C9 1 0.351008 0.293036 0.767057 11.00000 0.03940 0.03582 = 0.05643 0.00482 0.03355 0.00361 C15 1 0.395018 0.349536 0.867941 11.00000 0.05608 0.04977 = 0.06074 -0.00404 0.04342 -0.00448 AFIX 43 H15 2 0.443216 0.395278 0.898524 11.00000 -1.20000 AFIX 0 C10 1 0.278097 0.223370 0.720789 11.00000 0.04166 0.03968 = 0.07519 0.00605 0.03977 0.00281 C19 1 0.634134 0.099260 0.795586 11.00000 0.04612 0.05010 = 0.05107 0.00733 0.03043 0.01106 AFIX 43 H19 2 0.635730 -0.016269 0.778500 11.00000 -1.20000 AFIX 0 C11 1 0.242785 0.169710 0.612211 11.00000 0.03275 0.04706 = 0.07415 0.00307 0.02960 -0.00568 AFIX 23 H11A 2 0.230837 0.045344 0.601663 11.00000 -1.20000 H11B 2 0.197268 0.236809 0.563775 11.00000 -1.20000 AFIX 0 C2 1 0.267972 0.148509 0.429425 11.00000 0.04268 0.04693 = 0.04698 -0.00887 0.01256 -0.00373 AFIX 43 H2 2 0.221455 0.095850 0.402177 11.00000 -1.20000 AFIX 0 C21 1 0.699682 0.363586 0.884906 11.00000 0.03014 0.06467 = 0.04045 0.00712 0.01756 -0.00012 AFIX 43 H21 2 0.744772 0.425841 0.926758 11.00000 -1.20000 AFIX 0 C20 1 0.701419 0.195490 0.857937 11.00000 0.03546 0.06905 = 0.04925 0.01230 0.02494 0.01222 AFIX 43 H20 2 0.747396 0.144454 0.880974 11.00000 -1.20000 AFIX 0 C5 1 0.410553 0.306733 0.512809 11.00000 0.04510 0.05387 = 0.04374 -0.00416 0.02622 0.00150 AFIX 43 H5 2 0.457237 0.357605 0.539209 11.00000 -1.20000 AFIX 0 C26 1 0.417369 0.851145 0.757033 11.00000 0.05176 0.03946 = 0.07288 0.00096 0.03381 0.00452 AFIX 23 H26A 2 0.444262 0.912838 0.735971 11.00000 -1.20000 H26B 2 0.364592 0.886271 0.711426 11.00000 -1.20000 AFIX 0 C12 1 0.249977 0.212772 0.776451 11.00000 0.05982 0.05301 = 0.10754 0.00512 0.06429 -0.00179 AFIX 43 H12 2 0.201752 0.167895 0.746621 11.00000 -1.20000 AFIX 0 C3 1 0.294008 0.169444 0.372069 11.00000 0.06221 0.06102 = 0.03956 -0.01343 0.01734 0.00139 AFIX 43 H3 2 0.264420 0.129931 0.304735 11.00000 -1.20000 AFIX 0 C4 1 0.363725 0.248510 0.412393 11.00000 0.06737 0.06591 = 0.04618 -0.00536 0.03404 0.00643 AFIX 43 H4 2 0.379081 0.262416 0.370970 11.00000 -1.20000 AFIX 0 C14 1 0.365618 0.336331 0.922062 11.00000 0.08504 0.06154 = 0.07787 -0.00345 0.06535 -0.00108 AFIX 43 H14 2 0.394453 0.373071 0.989886 11.00000 -1.20000 AFIX 0 C13 1 0.294041 0.269292 0.876499 11.00000 0.09079 0.06303 = 0.10227 0.00012 0.08244 -0.00088 AFIX 43 H13 2 0.275166 0.262109 0.914036 11.00000 -1.20000 AFIX 0 C27 1 0.401348 0.852101 0.886590 11.00000 0.08610 0.08194 = 0.09037 -0.00439 0.05763 0.01163 AFIX 137 H27A 2 0.349968 0.888875 0.835909 11.00000 -1.50000 H27B 2 0.420741 0.907438 0.950720 11.00000 -1.50000 H27C 2 0.402890 0.726835 0.894411 11.00000 -1.50000 AFIX 0 C28 1 0.500000 0.883395 0.500000 10.50000 0.21427 0.07875 = 0.13386 0.00000 0.12746 0.00000 AFIX 23 H28A 2 0.544280 0.958763 0.538046 10.50000 -1.20000 H28B 2 0.455720 0.958761 0.461954 10.50000 -1.20000 AFIX 0 HKLF 4 REM hcf-asy84_a.res in C2 REM R1 = 0.0365 for 3794 Fo > 4sig(Fo) and 0.0371 for all 3869 data REM 286 parameters refined using 1 restraints END WGHT 0.0594 0.6750 REM Highest difference peak 0.238, deepest hole -0.382, 1-sigma level 0.035 Q1 1 0.4624 0.7452 0.5208 11.00000 0.05 0.24 Q2 1 0.5449 0.6773 0.5920 11.00000 0.05 0.17 Q3 1 0.5667 0.8028 0.6013 11.00000 0.05 0.11 Q4 1 0.5782 0.6051 0.5893 11.00000 0.05 0.11 Q5 1 0.1686 0.1467 0.6704 11.00000 0.05 0.10 Q6 1 0.4271 0.7487 0.4382 11.00000 0.05 0.10 Q7 1 0.5311 1.0937 0.4681 11.00000 0.05 0.10 Q8 1 0.1183 0.2182 0.4298 11.00000 0.05 0.10 Q9 1 0.2857 0.2359 0.4804 11.00000 0.05 0.10 Q10 1 0.5007 0.4807 0.8791 11.00000 0.05 0.10 Q11 1 0.5287 0.6705 0.7889 11.00000 0.05 0.10 Q12 1 0.1874 0.2688 0.5064 11.00000 0.05 0.10 Q13 1 0.5353 0.6537 0.7324 11.00000 0.05 0.09 Q14 1 0.6723 0.1249 0.8567 11.00000 0.05 0.09 Q15 1 0.5965 0.4116 0.7982 11.00000 0.05 0.09 Q16 1 0.4603 0.7541 1.0430 11.00000 0.05 0.09 Q17 1 0.3600 0.3333 0.7286 11.00000 0.05 0.09 Q18 1 0.4054 0.3352 0.6201 11.00000 0.05 0.09 Q19 1 0.7857 0.5277 0.9339 11.00000 0.05 0.09 Q20 1 0.3173 0.2420 0.7484 11.00000 0.05 0.09 ; _shelx_res_checksum 19302 _shelx_hkl_file ; 0 0 -2 1790.88 3.40 0 0 -2 1806.42 4.23 0 0 -3 3290.90 6.99 0 0 -3 3308.60 5.80 0 0 -4 552.58 2.71 0 0 -4 549.29 3.31 0 0 -4 555.36 2.69 0 0 -5 73.02 1.11 0 0 -5 72.15 1.12 0 0 -5 69.13 1.33 0 0 -6 1275.96 5.12 0 0 -6 1287.06 5.25 0 0 -7 329.79 2.93 0 0 -7 309.01 3.38 0 0 -8 464.24 3.78 0 0 -9 44.95 1.14 0 0 -9 48.10 1.20 0 0 -9 46.32 1.14 0 0 -9 46.19 1.15 0 0 -10 0.21 0.12 0 0 -10 0.05 0.12 0 0 -10 0.03 0.12 0 0 -11 326.40 3.44 0 0 -11 317.11 3.31 0 0 -11 319.82 3.02 0 0 -12 0.74 0.22 0 0 -13 10.47 0.62 0 0 -14 1.40 0.22 0 0 -14 1.42 0.22 0 0 -15 0.64 0.14 0 0 -15 0.64 0.14 0 -2 0 9999.00 10.38 0 2 1 1828.00 3.32 0 2 -1 1842.31 3.70 0 -2 -2 93.82 1.30 0 -2 2 99.41 1.12 0 -2 3 134.21 1.29 0 2 -3 134.87 1.51 0 -2 -3 132.49 1.66 0 2 -4 128.90 2.04 0 -2 -4 123.90 1.74 0 2 -4 129.83 1.69 0 2 -5 686.09 4.42 0 -2 -5 728.87 4.45 0 2 -5 663.34 5.17 0 -2 -5 717.66 4.69 0 -2 -6 484.43 3.95 0 2 -6 491.40 4.85 0 -2 -6 488.77 4.08 0 2 -7 97.97 1.97 0 -2 -7 101.38 1.92 0 -2 -7 104.40 2.04 0 -2 -8 12.46 0.76 0 2 -8 14.02 0.69 0 -2 -8 13.33 0.65 0 -2 -8 13.90 0.78 0 -2 -8 12.06 0.72 0 2 -8 14.99 1.00 0 -2 -8 12.89 0.60 0 -2 -9 29.35 0.96 0 2 -9 27.26 1.02 0 -2 -9 28.43 1.17 0 -2 -9 28.88 1.06 0 -2 -9 29.09 0.98 0 2 -9 28.04 1.00 0 -2 -9 29.56 1.22 0 2 -9 29.65 1.50 0 -2 -9 30.80 0.99 0 -2 -10 22.21 0.87 0 2 -10 24.03 1.42 0 2 -10 22.11 0.92 0 -2 -10 21.92 1.07 0 2 -10 23.05 0.98 0 -2 -10 22.55 0.88 0 -2 -10 22.33 0.91 0 -2 -11 65.85 1.52 0 -2 -11 65.60 1.47 0 -2 -11 63.99 1.52 0 -2 -11 67.18 1.37 0 2 -11 71.11 1.74 0 2 -11 69.27 1.64 0 -2 -11 64.74 1.50 0 -2 -11 67.44 1.46 0 2 -12 16.83 0.86 0 -2 -12 14.40 0.67 0 -2 -12 15.26 0.62 0 -2 -12 14.09 0.69 0 -2 -12 14.53 0.67 0 -2 -12 15.14 0.74 0 2 -12 16.98 0.79 0 2 -13 1.33 0.23 0 -2 -13 0.83 0.18 0 2 -13 1.37 0.26 0 -2 -13 0.81 0.16 0 -2 -13 0.96 0.17 0 2 -14 0.60 0.15 0 -2 -14 0.31 0.11 0 -2 -14 0.48 0.13 0 2 -14 0.40 0.15 0 2 -15 -0.01 0.10 0 2 -15 0.06 0.07 0 -4 0 274.43 2.67 0 -4 0 269.45 2.88 0 4 -1 387.34 4.21 0 -4 -1 424.03 3.77 0 -4 -1 405.94 3.58 0 -4 1 434.78 3.78 0 -4 1 411.36 2.86 0 -4 2 231.13 2.60 0 -4 -2 237.66 2.93 0 -4 -2 239.08 2.92 0 4 -2 228.96 3.41 0 -4 3 103.70 1.64 0 -4 -3 106.13 2.01 0 4 -3 103.74 2.36 0 -4 -3 101.05 2.04 0 -4 -4 14.99 0.83 0 -4 -4 14.98 0.79 0 -4 4 15.44 0.63 0 -4 -5 102.21 2.18 0 -4 -5 102.52 2.24 0 4 -6 8.62 0.54 0 4 -6 8.30 0.80 0 -4 -6 12.12 0.82 0 4 6 9.18 0.56 0 4 -6 8.12 0.55 0 -4 -6 11.47 0.77 0 4 -7 80.47 1.83 0 -4 -7 90.84 1.60 0 4 -7 79.37 2.64 0 -4 -7 77.75 2.20 0 -4 -7 89.77 2.35 0 -4 -7 90.28 2.25 0 4 7 82.13 1.71 0 4 -7 76.68 1.67 0 -4 -8 153.05 2.14 0 4 8 151.21 2.36 0 -4 -8 153.38 2.70 0 -4 -8 146.96 2.38 0 4 -8 145.95 2.57 0 -4 -8 150.13 3.12 0 4 -8 144.32 3.74 0 -4 -8 151.41 3.03 0 4 -8 144.24 2.38 0 4 -9 183.43 2.72 0 4 9 188.37 2.62 0 4 -9 179.50 2.95 0 -4 -9 190.03 2.66 0 -4 -9 187.40 2.44 0 4 -10 92.81 1.90 0 -4 -10 87.94 1.76 0 -4 -10 87.12 1.79 0 4 -10 90.06 2.09 0 -4 -10 86.20 1.92 0 4 10 95.16 1.81 0 4 -11 14.48 0.72 0 -4 -11 12.36 0.67 0 -4 -11 12.71 0.67 0 -4 -11 11.20 0.61 0 4 -11 13.18 0.79 0 -4 -12 18.49 0.73 0 4 -12 17.34 0.71 0 -4 -12 17.93 0.68 0 -4 -12 17.17 0.73 0 4 -12 17.49 0.84 0 -4 -12 16.41 0.70 0 4 -13 15.50 0.71 0 -4 -13 13.83 0.56 0 -4 -13 13.69 0.59 0 -4 -13 13.57 0.49 0 -4 -14 3.13 0.24 0 -4 -14 2.89 0.22 0 4 -14 3.49 0.29 0 6 0 31.31 1.00 0 6 0 29.41 0.94 0 -6 0 28.47 1.30 0 6 -1 6.88 0.44 0 6 1 7.84 0.52 0 6 -1 8.24 0.52 0 6 1 7.73 0.51 0 -6 -1 6.50 0.61 0 -6 1 7.75 0.65 0 -6 -2 6.22 0.61 0 6 -2 5.68 0.43 0 6 2 5.31 0.44 0 6 2 6.10 0.46 0 6 -3 5.17 0.68 0 6 -3 5.61 0.43 0 6 3 5.85 0.45 0 -6 -3 6.17 0.63 0 6 3 5.02 0.44 0 6 4 4.94 0.46 0 -6 -4 5.51 0.62 0 -6 -4 6.36 0.65 0 6 4 5.44 0.43 0 6 5 15.23 0.80 0 6 6 1.90 0.31 0 -6 -7 10.17 0.61 0 6 7 9.50 0.64 0 -6 -8 26.76 0.90 0 6 8 27.38 1.02 0 -6 -8 26.29 0.89 0 -6 -9 8.09 0.62 0 -6 -9 8.35 0.49 0 -6 -9 8.72 0.48 0 6 9 8.37 0.53 0 6 10 5.59 0.39 0 -6 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5.27 0.41 1 -1 -9 5.48 0.43 1 -1 -8 37.37 1.13 1 -1 -8 38.36 1.16 1 -1 -7 76.88 1.49 1 1 -7 77.60 1.41 1 -1 -7 78.30 1.55 1 1 -6 7.48 0.40 1 1 -6 6.93 0.45 1 -1 -5 37.11 0.89 1 -1 -5 37.12 0.87 1 -1 -4 377.45 2.58 1 1 -4 379.77 2.26 1 -1 -4 378.37 2.50 1 1 -4 381.00 2.60 1 -1 -3 211.96 1.67 1 -1 -3 212.47 1.73 1 1 -3 214.52 1.66 -1 -1 2 912.78 2.05 1 1 -2 929.44 2.73 1 -1 -1 107.73 0.94 1 -1 -1 106.13 0.89 1 -1 -1 105.98 0.87 -1 1 0 420.86 1.70 -1 1 0 421.17 1.94 -1 -1 -1 519.13 1.84 1 -1 1 515.77 2.05 -1 -1 -2 43.46 0.75 1 -1 2 42.89 0.66 -1 1 -2 42.58 0.76 -1 1 -2 41.90 0.46 -1 -1 -2 44.54 0.73 -1 -1 -3 60.83 1.02 -1 1 -3 60.60 1.05 -1 -1 -3 61.39 0.97 -1 1 -3 61.34 0.71 -1 -1 -4 18.85 0.60 -1 1 -4 23.38 0.74 -1 1 -4 23.32 0.53 -1 -1 -4 18.51 0.64 -1 -1 -5 250.95 2.65 -1 -1 -5 262.96 2.44 -1 1 -5 285.59 2.11 -1 1 -5 285.94 2.89 -1 -1 -5 261.53 2.56 -1 -1 -6 162.50 2.18 -1 -1 -6 166.35 2.09 -1 -1 -6 162.00 2.35 -1 1 -6 161.78 1.78 -1 -1 -7 166.26 2.38 -1 -1 -7 166.15 2.27 -1 1 -7 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23 -1 -4 5.29 0.36 -23 1 4 4.93 0.30 23 -1 -3 1.73 0.19 23 1 -3 1.71 0.18 23 -1 -3 1.82 0.20 -23 1 3 1.62 0.16 23 3 -17 0.32 0.09 23 -3 -16 5.75 0.33 23 3 -16 5.96 0.34 23 -3 -15 5.30 0.35 23 3 -15 5.75 0.35 -23 3 15 5.25 0.31 23 -3 -14 3.35 0.30 23 3 -14 3.03 0.28 -23 3 14 2.99 0.27 23 -3 -13 17.52 0.68 23 3 -13 17.72 0.65 -23 3 13 16.84 0.64 23 -3 -12 21.91 0.79 23 -3 -12 21.55 0.71 23 3 -12 22.21 0.73 -23 3 12 21.13 0.76 23 -3 -11 9.43 0.53 23 -3 -11 8.87 0.48 23 3 -11 9.19 0.46 -23 3 11 8.98 0.50 23 -3 -11 9.10 0.56 23 -3 -10 4.98 0.40 23 -3 -10 4.69 0.36 -23 3 10 4.54 0.37 23 -3 -10 4.76 0.42 23 -3 -9 9.97 0.56 23 -3 -9 9.35 0.51 23 -3 -9 9.39 0.43 -23 3 9 9.10 0.50 23 -3 -9 9.59 0.56 23 -3 -8 7.31 0.47 23 -3 -8 7.59 0.46 23 -3 -8 6.71 0.38 -23 3 8 7.41 0.43 23 -3 -8 7.60 0.48 23 -3 -7 20.08 0.74 23 -3 -7 19.44 0.71 -23 3 7 18.45 0.62 23 -3 -7 19.68 0.71 23 -3 -6 6.83 0.42 23 -3 -6 7.29 0.43 -23 3 6 6.71 0.35 23 -3 -5 26.17 0.74 23 -3 -5 26.12 0.77 -23 3 5 25.39 0.64 23 -3 -4 1.09 0.16 24 0 -18 0.43 0.10 24 0 -17 0.12 0.08 24 0 -17 0.12 0.09 24 0 -16 6.68 0.39 -24 0 16 6.34 0.34 24 0 -15 0.36 0.13 -24 0 15 0.44 0.13 24 0 -14 0.12 0.10 24 0 -13 3.53 0.31 24 0 -12 0.81 0.17 24 0 -12 0.90 0.20 24 0 -11 0.81 0.17 24 0 -11 0.96 0.21 24 0 -11 0.88 0.18 24 0 -10 2.42 0.26 24 0 -10 2.53 0.30 24 0 -10 2.15 0.26 24 0 -9 7.24 0.47 24 0 -9 6.86 0.44 24 0 -8 0.34 0.14 24 0 -8 0.34 0.13 24 0 -7 1.54 0.22 24 0 -7 1.42 0.21 -24 0 7 1.39 0.18 24 0 -6 1.77 0.22 24 0 -6 2.03 0.24 24 0 -5 4.57 0.31 24 0 -5 4.58 0.32 24 0 -4 0.39 0.11 24 -2 -17 4.86 0.29 24 2 -17 5.30 0.30 24 -2 -16 9.38 0.44 24 2 -16 9.27 0.43 -24 2 16 8.42 0.35 24 -2 -15 15.68 0.60 24 2 -15 15.02 0.58 24 -2 -14 23.57 0.77 24 2 -14 22.87 0.74 -24 2 14 21.00 0.68 24 -2 -13 27.04 0.85 24 -2 -13 25.47 0.79 -24 2 13 25.03 0.78 24 -2 -12 38.10 1.00 -24 2 12 37.74 0.99 24 -2 -11 8.23 0.49 24 -2 -11 8.02 0.48 -24 2 11 8.02 0.47 24 -2 -10 7.83 0.47 24 -2 -10 7.76 0.47 24 -2 -10 7.11 0.39 -24 2 10 7.63 0.45 24 -2 -9 2.51 0.28 24 -2 -9 2.63 0.29 24 2 -9 2.80 0.29 24 -2 -9 2.74 0.26 -24 2 9 2.63 0.27 24 -2 -8 9.63 0.50 24 -2 -8 9.19 0.51 24 2 -8 9.85 0.50 24 -2 -8 8.66 0.44 -24 2 8 8.88 0.44 24 -2 -7 2.99 0.27 24 -2 -7 3.05 0.29 24 2 -7 3.07 0.28 24 -2 -7 2.97 0.27 -24 2 7 2.80 0.23 24 -2 -6 3.57 0.27 24 -2 -6 3.84 0.31 24 2 -6 3.71 0.28 24 -2 -6 3.44 0.28 24 -2 -5 12.87 0.51 24 -2 -5 11.70 0.46 24 -4 -13 0.75 0.13 -24 4 13 0.79 0.12 24 -4 -12 0.47 0.12 -24 4 12 0.40 0.10 24 -4 -11 3.70 0.27 -24 4 11 3.90 0.27 24 -4 -10 1.87 0.20 -24 4 10 2.19 0.20 24 -4 -9 3.19 0.25 -24 4 9 3.07 0.22 24 -4 -9 3.39 0.27 24 -4 -8 4.99 0.30 25 -1 -17 2.07 0.19 25 1 -17 1.87 0.18 25 -1 -16 3.52 0.26 25 1 -16 3.26 0.26 -25 1 16 2.94 0.21 -25 -1 16 3.15 0.22 25 -1 -15 9.65 0.45 -25 1 15 8.37 0.39 25 -1 -14 10.26 0.48 -25 1 14 9.34 0.44 25 -1 -13 0.67 0.16 25 -1 -13 0.61 0.15 -25 1 13 0.56 0.13 25 -1 -12 1.52 0.20 25 -1 -12 1.64 0.23 25 -1 -12 1.48 0.17 -25 1 12 1.61 0.21 25 -1 -11 5.49 0.36 25 -1 -11 5.39 0.39 25 -1 -11 5.16 0.33 -25 1 11 5.37 0.37 25 -1 -10 0.82 0.16 25 1 -10 0.92 0.17 25 -1 -10 0.91 0.18 25 1 -10 0.68 0.15 25 -1 -10 0.79 0.14 -25 1 10 0.72 0.15 25 -1 -9 1.18 0.17 25 1 -9 1.41 0.20 25 -1 -9 1.23 0.20 25 -1 -9 1.27 0.18 25 1 -9 1.24 0.19 -25 1 9 1.22 0.17 25 1 -8 7.79 0.40 25 -1 -8 8.11 0.44 25 1 -8 8.20 0.44 25 -1 -8 7.68 0.41 -25 1 8 7.11 0.35 25 -1 -7 6.68 0.38 25 1 -7 6.71 0.38 25 -1 -7 6.15 0.35 25 -1 -6 7.70 0.38 25 1 -6 7.56 0.36 25 -1 -6 6.91 0.35 25 -3 -14 26.75 0.67 -25 3 14 25.71 0.62 25 -3 -13 18.52 0.59 -25 3 13 16.67 0.54 25 -3 -12 5.74 0.34 25 -3 -12 5.36 0.30 -25 3 12 5.82 0.33 25 -3 -11 14.99 0.54 25 -3 -11 13.94 0.49 -25 3 11 14.56 0.52 25 -3 -10 7.57 0.39 25 -3 -10 7.55 0.37 -25 3 10 7.48 0.36 25 -3 -9 0.59 0.13 25 -3 -9 0.47 0.11 25 -3 -8 2.29 0.20 26 0 -16 1.69 0.17 -26 0 15 1.40 0.16 -26 0 14 13.17 0.49 -26 0 13 1.89 0.20 -26 0 12 3.68 0.28 26 0 -11 0.45 0.13 26 0 -11 0.36 0.11 -26 0 11 0.49 0.12 26 0 -10 0.64 0.14 26 0 -10 0.62 0.13 -26 0 10 0.54 0.11 26 0 -9 0.94 0.15 26 0 -9 0.83 0.14 -26 0 9 0.80 0.12 26 0 -8 7.24 0.35 26 0 -8 6.89 0.35 26 0 -7 1.95 0.18 26 -2 -14 8.40 0.37 -26 2 14 7.90 0.35 26 -2 -13 0.36 0.11 -26 2 13 0.37 0.10 26 -2 -12 0.84 0.14 26 -2 -12 0.79 0.13 -26 2 12 0.71 0.12 26 -2 -11 0.86 0.14 26 -2 -11 0.87 0.14 -26 2 11 0.90 0.13 26 -2 -10 3.10 0.24 -26 2 10 3.16 0.22 26 -2 -9 7.12 0.35 0 0 0 0.00 0.00 TITL hcf-asy84 in C2/m REM C2/m (#12 in standard setting) CELL 1.54184 22.120331 7.612273 16.380344 90.0000 127.0775 90.0000 ZERR 5.00 0.000511 0.000118 0.000393 0.0000 0.0036 0.0000 LATT 7 SYMM -x, y,-z SFAC C H N O UNIT 100.00 100.00 5.00 10.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 34353 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, 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 Cl1 Cl 0.49658(13) 0.7634(3) 0.58526(12) 0.1599(8) Uani 1 1 d . . . O1 O 0.42235(9) 0.6677(2) 0.74641(14) 0.0494(4) Uani 1 1 d . . . N1 N 0.30356(10) 0.2123(3) 0.60429(15) 0.0425(4) Uani 1 1 d . . . O2 O 0.44659(11) 0.9014(3) 0.85498(17) 0.0704(6) Uani 1 1 d . . . C17 C 0.56134(11) 0.3491(3) 0.78518(15) 0.0348(5) Uani 1 1 d . . . C25 C 0.49163(11) 0.5975(3) 0.78172(16) 0.0376(5) Uani 1 1 d . . . C7 C 0.41836(11) 0.3367(3) 0.67749(15) 0.0352(4) Uani 1 1 d . . . C8 C 0.36579(11) 0.2891(3) 0.69180(16) 0.0373(5) Uani 1 1 d . . . C16 C 0.49086(11) 0.4295(3) 0.74987(15) 0.0338(4) Uani 1 1 d . . . C22 C 0.63025(11) 0.4457(3) 0.85030(16) 0.0385(5) Uani 1 1 d . . . C6 C 0.38604(11) 0.2873(3) 0.57365(16) 0.0388(5) Uani 1 1 d . . . C1 C 0.31435(12) 0.2097(3) 0.53062(17) 0.0422(5) Uani 1 1 d . . . C24 C 0.55996(12) 0.6927(3) 0.84717(17) 0.0436(5) Uani 1 1 d . . . H24 H 0.5593 0.8053 0.8686 0.052 Uiso 1 1 calc R U . C23 C 0.62699(12) 0.6175(4) 0.87864(17) 0.0440(6) Uani 1 1 d . . . H23 H 0.6716 0.6819 0.9199 0.053 Uiso 1 1 calc R U . C18 C 0.56574(12) 0.1748(3) 0.75952(17) 0.0421(5) Uani 1 1 d . . . H18 H 0.5215 0.1098 0.7174 0.051 Uiso 1 1 calc R U . C9 C 0.35101(12) 0.2930(3) 0.76706(18) 0.0409(5) Uani 1 1 d . . . C15 C 0.39502(15) 0.3495(4) 0.8679(2) 0.0503(6) Uani 1 1 d . . . H15 H 0.4432 0.3953 0.8985 0.060 Uiso 1 1 calc R U . C10 C 0.27810(13) 0.2234(4) 0.7208(2) 0.0493(6) Uani 1 1 d . . . C19 C 0.63413(14) 0.0993(4) 0.79559(19) 0.0484(6) Uani 1 1 d . . . H19 H 0.6357 -0.0163 0.7785 0.058 Uiso 1 1 calc R U . C11 C 0.24278(13) 0.1697(4) 0.6122(2) 0.0530(6) Uani 1 1 d . . . H11A H 0.2308 0.0453 0.6017 0.064 Uiso 1 1 calc R U . H11B H 0.1973 0.2368 0.5638 0.064 Uiso 1 1 calc R U . C2 C 0.26797(14) 0.1485(4) 0.42943(19) 0.0547(7) Uani 1 1 d . . . H2 H 0.2215 0.0959 0.4022 0.066 Uiso 1 1 calc R U . C21 C 0.69968(12) 0.3636(4) 0.88491(17) 0.0474(6) Uani 1 1 d . . . H21 H 0.7448 0.4258 0.9268 0.057 Uiso 1 1 calc R U . C20 C 0.70142(13) 0.1955(4) 0.85794(19) 0.0516(7) Uani 1 1 d . . . H20 H 0.7474 0.1445 0.8810 0.062 Uiso 1 1 calc R U . C5 C 0.41055(14) 0.3067(4) 0.51281(18) 0.0479(6) Uani 1 1 d . . . H5 H 0.4572 0.3576 0.5392 0.058 Uiso 1 1 calc R U . C26 C 0.41737(15) 0.8511(4) 0.7570(2) 0.0571(6) Uani 1 1 d . . . H26A H 0.4443 0.9128 0.7360 0.068 Uiso 1 1 calc R U . H26B H 0.3646 0.8863 0.7114 0.068 Uiso 1 1 calc R U . C12 C 0.24998(17) 0.2128(4) 0.7765(3) 0.0647(8) Uani 1 1 d . . . H12 H 0.2018 0.1679 0.7466 0.078 Uiso 1 1 calc R U . C3 C 0.29401(17) 0.1694(4) 0.3721(2) 0.0627(8) Uani 1 1 d . . . H3 H 0.2644 0.1299 0.3047 0.075 Uiso 1 1 calc R U . C4 C 0.36372(17) 0.2485(5) 0.4124(2) 0.0599(7) Uani 1 1 d . . . H4 H 0.3791 0.2624 0.3710 0.072 Uiso 1 1 calc R U . C14 C 0.3656(2) 0.3363(4) 0.9221(3) 0.0646(8) Uani 1 1 d . . . H14 H 0.3945 0.3731 0.9899 0.077 Uiso 1 1 calc R U . C13 C 0.2940(2) 0.2693(5) 0.8765(3) 0.0701(9) Uani 1 1 d . . . H13 H 0.2752 0.2621 0.9140 0.084 Uiso 1 1 calc R U . C27 C 0.4013(2) 0.8521(6) 0.8866(3) 0.0833(10) Uani 1 1 d . . . H27A H 0.3500 0.8889 0.8359 0.125 Uiso 1 1 calc R U . H27B H 0.4207 0.9074 0.9507 0.125 Uiso 1 1 calc R U . H27C H 0.4029 0.7268 0.8944 0.125 Uiso 1 1 calc R U . C28 C 0.5000 0.8834(11) 0.5000 0.128(3) Uani 1 2 d S T P H28A H 0.5443 0.9588 0.5380 0.154 Uiso 0.5 1 calc R U P H28B H 0.4557 0.9588 0.4620 0.154 Uiso 0.5 1 calc R U P 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 0.266(2) 0.1254(12) 0.1263(10) -0.0325(9) 0.1385(13) -0.0750(14) O1 0.0361(8) 0.0400(10) 0.0660(10) -0.0049(8) 0.0276(8) 0.0018(7) N1 0.0282(8) 0.0409(11) 0.0498(10) -0.0033(8) 0.0189(7) -0.0058(7) O2 0.0590(11) 0.0641(15) 0.0820(14) -0.0233(11) 0.0392(11) -0.0033(10) C17 0.0305(9) 0.0436(13) 0.0321(9) 0.0026(8) 0.0198(8) -0.0015(8) C25 0.0317(10) 0.0401(13) 0.0392(10) -0.0005(9) 0.0205(8) -0.0010(9) C7 0.0275(9) 0.0386(13) 0.0355(9) -0.0017(8) 0.0170(8) -0.0007(8) C8 0.0289(9) 0.0371(12) 0.0412(10) -0.0012(9) 0.0187(8) -0.0011(8) C16 0.0287(9) 0.0410(12) 0.0314(9) 0.0014(8) 0.0179(8) -0.0030(8) C22 0.0314(10) 0.0486(14) 0.0345(10) 0.0052(9) 0.0194(8) -0.0027(9) C6 0.0329(9) 0.0391(12) 0.0369(10) -0.0037(9) 0.0171(8) 0.0008(9) C1 0.0347(10) 0.0368(13) 0.0418(11) -0.0017(9) 0.0161(9) -0.0002(9) C24 0.0399(11) 0.0411(14) 0.0457(11) -0.0060(10) 0.0236(9) -0.0083(10) C23 0.0333(10) 0.0514(15) 0.0402(10) -0.0043(10) 0.0184(9) -0.0117(9) C18 0.0356(10) 0.0477(15) 0.0436(11) -0.0004(10) 0.0242(9) -0.0021(9) C9 0.0394(10) 0.0358(12) 0.0564(12) 0.0048(10) 0.0336(10) 0.0036(9) C15 0.0561(13) 0.0498(16) 0.0607(14) -0.0040(12) 0.0434(12) -0.0045(12) C10 0.0417(11) 0.0397(14) 0.0752(16) 0.0061(12) 0.0398(12) 0.0028(10) C19 0.0461(12) 0.0501(16) 0.0511(12) 0.0073(11) 0.0304(10) 0.0111(11) C11 0.0327(10) 0.0471(16) 0.0741(16) 0.0031(12) 0.0296(11) -0.0057(10) C2 0.0427(12) 0.0469(16) 0.0470(13) -0.0089(11) 0.0126(10) -0.0037(11) C21 0.0301(10) 0.0647(18) 0.0404(11) 0.0071(11) 0.0176(9) -0.0001(10) C20 0.0355(11) 0.069(2) 0.0493(12) 0.0123(12) 0.0249(10) 0.0122(11) C5 0.0451(11) 0.0539(16) 0.0437(11) -0.0042(10) 0.0262(10) 0.0015(11) C26 0.0518(14) 0.0395(15) 0.0729(17) 0.0010(12) 0.0338(13) 0.0045(11) C12 0.0598(15) 0.0530(18) 0.108(2) 0.0051(16) 0.0643(17) -0.0018(13) C3 0.0622(16) 0.061(2) 0.0396(12) -0.0134(12) 0.0173(12) 0.0014(13) C4 0.0674(16) 0.066(2) 0.0462(13) -0.0054(13) 0.0340(12) 0.0064(14) C14 0.0850(19) 0.062(2) 0.0779(18) -0.0035(16) 0.0654(17) -0.0011(16) C13 0.091(2) 0.063(2) 0.102(2) 0.0001(18) 0.082(2) -0.0009(17) C27 0.086(2) 0.082(3) 0.090(2) -0.004(2) 0.058(2) 0.012(2) C28 0.214(9) 0.079(5) 0.134(6) 0.000 0.127(6) 0.000 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' O O 0.0492 0.0322 '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 C25 O1 C26 118.61(19) . . C1 N1 C8 109.12(17) . . C1 N1 C11 137.4(2) . . C8 N1 C11 113.3(2) . . C26 O2 C27 114.3(3) . . C18 C17 C22 118.15(19) . . C18 C17 C16 122.32(19) . . C22 C17 C16 119.5(2) . . C16 C25 O1 116.38(18) . . C16 C25 C24 121.7(2) . . O1 C25 C24 121.9(2) . . C8 C7 C6 105.38(18) . . C8 C7 C16 127.83(18) . . C6 C7 C16 126.68(18) . . C7 C8 N1 110.64(18) . . C7 C8 C9 142.2(2) . . N1 C8 C9 107.19(18) . . C25 C16 C17 118.81(18) . . C25 C16 C7 120.49(18) . . C17 C16 C7 120.7(2) . . C23 C22 C21 122.4(2) . . C23 C22 C17 118.82(19) . . C21 C22 C17 118.7(2) . . C5 C6 C1 119.1(2) . . C5 C6 C7 133.1(2) . . C1 C6 C7 107.78(19) . . N1 C1 C2 131.1(2) . . N1 C1 C6 107.08(19) . . C2 C1 C6 121.9(2) . . C23 C24 C25 119.4(2) . . C23 C24 H24 120.3 . . C25 C24 H24 120.3 . . C24 C23 C22 121.7(2) . . C24 C23 H23 119.2 . . C22 C23 H23 119.2 . . C19 C18 C17 121.3(2) . . C19 C18 H18 119.3 . . C17 C18 H18 119.3 . . C15 C9 C10 120.8(2) . . C15 C9 C8 131.4(2) . . C10 C9 C8 107.8(2) . . C14 C15 C9 118.5(3) . . C14 C15 H15 120.7 . . C9 C15 H15 120.7 . . C12 C10 C9 119.5(3) . . C12 C10 C11 130.1(2) . . C9 C10 C11 110.4(2) . . C18 C19 C20 120.3(3) . . C18 C19 H19 119.8 . . C20 C19 H19 119.8 . . N1 C11 C10 101.22(19) . . N1 C11 H11A 111.5 . . C10 C11 H11A 111.5 . . N1 C11 H11B 111.5 . . C10 C11 H11B 111.5 . . H11A C11 H11B 109.3 . . C3 C2 C1 117.4(2) . . C3 C2 H2 121.3 . . C1 C2 H2 121.3 . . C20 C21 C22 121.3(2) . . C20 C21 H21 119.4 . . C22 C21 H21 119.4 . . C21 C20 C19 120.2(2) . . C21 C20 H20 119.9 . . C19 C20 H20 119.9 . . C4 C5 C6 118.5(2) . . C4 C5 H5 120.7 . . C6 C5 H5 120.7 . . O2 C26 O1 113.6(3) . . O2 C26 H26A 108.8 . . O1 C26 H26A 108.8 . . O2 C26 H26B 108.8 . . O1 C26 H26B 108.8 . . H26A C26 H26B 107.7 . . C13 C12 C10 119.3(3) . . C13 C12 H12 120.3 . . C10 C12 H12 120.3 . . C2 C3 C4 121.7(2) . . C2 C3 H3 119.2 . . C4 C3 H3 119.2 . . C5 C4 C3 121.4(3) . . C5 C4 H4 119.3 . . C3 C4 H4 119.3 . . C13 C14 C15 120.7(3) . . C13 C14 H14 119.7 . . C15 C14 H14 119.7 . . C12 C13 C14 121.2(2) . . C12 C13 H13 119.4 . . C14 C13 H13 119.4 . . O2 C27 H27A 109.5 . . O2 C27 H27B 109.5 . . H27A C27 H27B 109.5 . . O2 C27 H27C 109.5 . . H27A C27 H27C 109.5 . . H27B C27 H27C 109.5 . . Cl1 C28 Cl1 115.3(5) . 2_656 Cl1 C28 H28A 108.4 . . Cl1 C28 H28A 108.4 2_656 . Cl1 C28 H28B 108.4 . . Cl1 C28 H28B 108.4 2_656 . H28A C28 H28B 107.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Cl1 C28 1.708(5) . O1 C25 1.378(3) . O1 C26 1.420(3) . N1 C1 1.364(3) . N1 C8 1.383(3) . N1 C11 1.463(3) . O2 C26 1.374(4) . O2 C27 1.426(5) . C17 C18 1.413(4) . C17 C22 1.429(3) . C17 C16 1.433(3) . C25 C16 1.377(3) . C25 C24 1.416(3) . C7 C8 1.366(3) . C7 C6 1.442(3) . C7 C16 1.478(3) . C8 C9 1.454(3) . C22 C23 1.404(4) . C22 C21 1.422(3) . C6 C5 1.400(3) . C6 C1 1.419(3) . C1 C2 1.402(3) . C24 C23 1.367(3) . C24 H24 0.9300 . C23 H23 0.9300 . C18 C19 1.375(3) . C18 H18 0.9300 . C9 C15 1.387(4) . C9 C10 1.408(3) . C15 C14 1.384(4) . C15 H15 0.9300 . C10 C12 1.382(4) . C10 C11 1.505(4) . C19 C20 1.401(4) . C19 H19 0.9300 . C11 H11A 0.9700 . C11 H11B 0.9700 . C2 C3 1.376(4) . C2 H2 0.9300 . C21 C20 1.362(4) . C21 H21 0.9300 . C20 H20 0.9300 . C5 C4 1.386(4) . C5 H5 0.9300 . C26 H26A 0.9700 . C26 H26B 0.9700 . C12 C13 1.377(5) . C12 H12 0.9300 . C3 C4 1.396(4) . C3 H3 0.9300 . C4 H4 0.9300 . C14 C13 1.378(5) . C14 H14 0.9300 . C13 H13 0.9300 . C27 H27A 0.9600 . C27 H27B 0.9600 . C27 H27C 0.9600 . C28 Cl1 1.708(5) 2_656 C28 H28A 0.9700 . C28 H28B 0.9700 . 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 C26 O1 C25 C16 -165.9(2) C26 O1 C25 C24 14.1(3) C6 C7 C8 N1 0.5(3) C16 C7 C8 N1 176.9(2) C6 C7 C8 C9 -178.0(3) C16 C7 C8 C9 -1.6(5) C1 N1 C8 C7 -0.4(3) C11 N1 C8 C7 -175.9(2) C1 N1 C8 C9 178.6(2) C11 N1 C8 C9 3.2(3) O1 C25 C16 C17 -179.25(19) C24 C25 C16 C17 0.8(3) O1 C25 C16 C7 3.0(3) C24 C25 C16 C7 -177.0(2) C18 C17 C16 C25 177.33(19) C22 C17 C16 C25 -1.5(3) C18 C17 C16 C7 -4.9(3) C22 C17 C16 C7 176.27(17) C8 C7 C16 C25 -62.7(3) C6 C7 C16 C25 113.0(3) C8 C7 C16 C17 119.6(2) C6 C7 C16 C17 -64.7(3) C18 C17 C22 C23 -178.4(2) C16 C17 C22 C23 0.5(3) C18 C17 C22 C21 0.9(3) C16 C17 C22 C21 179.78(19) C8 C7 C6 C5 177.3(3) C16 C7 C6 C5 0.9(4) C8 C7 C6 C1 -0.4(3) C16 C7 C6 C1 -176.9(2) C8 N1 C1 C2 -179.1(3) C11 N1 C1 C2 -5.3(5) C8 N1 C1 C6 0.1(3) C11 N1 C1 C6 174.0(3) C5 C6 C1 N1 -178.0(2) C7 C6 C1 N1 0.2(3) C5 C6 C1 C2 1.4(4) C7 C6 C1 C2 179.5(2) C16 C25 C24 C23 1.0(3) O1 C25 C24 C23 -179.0(2) C25 C24 C23 C22 -2.0(3) C21 C22 C23 C24 -178.0(2) C17 C22 C23 C24 1.3(3) C22 C17 C18 C19 -0.2(3) C16 C17 C18 C19 -179.0(2) C7 C8 C9 C15 -4.0(5) N1 C8 C9 C15 177.4(3) C7 C8 C9 C10 176.4(3) N1 C8 C9 C10 -2.1(3) C10 C9 C15 C14 -0.2(4) C8 C9 C15 C14 -179.7(3) C15 C9 C10 C12 0.6(4) C8 C9 C10 C12 -179.8(3) C15 C9 C10 C11 -179.2(2) C8 C9 C10 C11 0.4(3) C17 C18 C19 C20 -0.9(4) C1 N1 C11 C10 -176.4(3) C8 N1 C11 C10 -2.8(3) C12 C10 C11 N1 -178.4(3) C9 C10 C11 N1 1.3(3) N1 C1 C2 C3 177.9(3) C6 C1 C2 C3 -1.2(4) C23 C22 C21 C20 178.7(2) C17 C22 C21 C20 -0.6(3) C22 C21 C20 C19 -0.5(4) C18 C19 C20 C21 1.3(4) C1 C6 C5 C4 -0.3(4) C7 C6 C5 C4 -177.8(3) C27 O2 C26 O1 -72.2(3) C25 O1 C26 O2 -76.0(3) C9 C10 C12 C13 -0.5(5) C11 C10 C12 C13 179.2(3) C1 C2 C3 C4 -0.1(4) C6 C5 C4 C3 -1.0(5) C2 C3 C4 C5 1.2(5) C9 C15 C14 C13 -0.3(5) C10 C12 C13 C14 0.1(5) C15 C14 C13 C12 0.4(5)