#------------------------------------------------------------------------------ #$Date: 2020-10-23 01:32:18 +0300 (Fri, 23 Oct 2020) $ #$Revision: 258561 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/00/36/4003698.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_4003698 loop_ _publ_author_name 'Kumagai, Shohei' 'Ishii, Hiroyuki' 'Watanabe, Go' 'Annaka, Tatsuro' 'Fukuzaki, Eiji' 'Tani, Yukio' 'Sugiura, Hiroki' 'Watanabe, Tetsuya' 'Kurosawa, Tadanori' 'Takeya, Jun' 'Okamoto, Toshihiro' _publ_section_title ; Cooperative Aggregations of Nitrogen-Containing Perylene Diimides Driven by Rigid and Flexible Functional Groups ; _journal_name_full 'Chemistry of Materials' _journal_paper_doi 10.1021/acs.chemmater.0c01888 _journal_year 2020 _chemical_formula_moiety 'C36 H20 N4 O4' _chemical_formula_sum 'C36 H20 N4 O4' _chemical_formula_weight 572.56 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.0000 _cell_angle_beta 94.412(7) _cell_angle_gamma 90.0000 _cell_formula_units_Z 2 _cell_length_a 7.7598(4) _cell_length_b 4.7937(3) _cell_length_c 35.5839(19) _cell_measurement_reflns_used 8970 _cell_measurement_temperature 302 _cell_measurement_theta_max 68.22 _cell_measurement_theta_min 3.74 _cell_volume 1319.73(13) _computing_cell_refinement 'RAPID AUTO' _computing_data_collection 'RAPID AUTO (Rigaku, ????)' _computing_data_reduction 'RAPID AUTO' _computing_molecular_graphics 'CrystalStructure 4.2.2' _computing_publication_material 'CrystalStructure 4.2.2 (Rigaku, 2016)' _computing_structure_refinement 'SHELXL Version 2014/7 (Sheldrick, 2008)' _computing_structure_solution 'SHELXT Version 2014/4 (Sheldrick, 2014)' _diffrn_ambient_temperature 302 _diffrn_detector_area_resol_mean 10.000 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method \w _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54187 _diffrn_reflns_av_R_equivalents 0.1312 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_number 12888 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 67.687 _diffrn_reflns_theta_max 68.254 _diffrn_reflns_theta_min 4.986 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.782 _exptl_absorpt_correction_T_max 0.996 _exptl_absorpt_correction_T_min 0.974 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'ABSCOR (Rigaku, 1995)' _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.441 _exptl_crystal_density_method 'not measured' _exptl_crystal_description platelet _exptl_crystal_F_000 592.00 _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.028 _exptl_crystal_size_min 0.005 _refine_diff_density_max 0.24 _refine_diff_density_min -0.28 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_hydrogen_treatment refxyz _refine_ls_number_parameters 229 _refine_ls_number_reflns 2414 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1715 _refine_ls_R_factor_gt 0.0851 _refine_ls_shift/su_max 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.1150P)^2^+0.5583P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2029 _refine_ls_wR_factor_ref 0.2688 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1129 _reflns_number_total 2414 _reflns_threshold_expression F^2^>2.0\s(F^2^) _cod_data_source_file cm0c01888_si_002.cif _cod_data_source_block 180402_PhC1BQQDI _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 4003698 _shelx_res_file ; shelxl.res created by SHELXL-2014/7 TITL 180402_PhC1BQQDI CELL 1.54187 7.75980 4.79370 35.58390 90.00000 94.41230 90.00000 ZERR 2 0.00040 0.00030 0.00190 0.00000 0.00660 0.00000 LATT 1 SYMM -X, .50+Y, .50-Z SFAC C H N O UNIT 72 40 8 8 L.S. 64 FMAP 2 PLAN 21 WPDB -2 HTAB BOND $H CONF LIST 4 TEMP 29.0 ACTA SIZE 0.400 0.028 0.005 WGHT 0.115000 0.558300 FVAR 0.65305 O1 4 0.702209 0.421891 0.586050 11.00000 0.05858 0.09296 = 0.07749 -0.01124 -0.01205 0.00572 O2 4 0.362618 1.072934 0.637218 11.00000 0.07980 0.10614 = 0.08522 -0.03727 -0.01846 0.01132 N3 3 0.312197 0.212501 0.502726 11.00000 0.05720 0.06525 = 0.06088 -0.00584 -0.00769 0.00271 N4 3 0.534376 0.748800 0.611588 11.00000 0.05973 0.07586 = 0.05505 -0.00834 -0.01032 -0.00129 C5 1 0.131665 0.561447 0.528518 11.00000 0.05053 0.06957 = 0.04709 0.00201 -0.00196 -0.00160 C6 1 0.162828 0.353162 0.501867 11.00000 0.05479 0.06639 = 0.05042 0.00411 -0.00071 -0.00211 C7 1 0.261970 0.624474 0.557091 11.00000 0.05211 0.06606 = 0.05035 0.00165 -0.00195 -0.00379 C8 1 -0.028972 0.713578 0.527711 11.00000 0.05595 0.06723 = 0.04750 0.00268 -0.00217 -0.00015 C9 1 0.237759 0.830232 0.584298 11.00000 0.05869 0.06592 = 0.05327 -0.00198 -0.00313 -0.00670 C10 1 0.562293 0.541720 0.585470 11.00000 0.05525 0.07996 = 0.05868 0.00566 -0.00533 -0.00422 C11 1 0.419824 0.476675 0.557203 11.00000 0.05501 0.06867 = 0.05800 0.00473 -0.00397 -0.00293 C12 1 0.082492 0.973431 0.582905 11.00000 0.06552 0.07187 = 0.05581 -0.01144 -0.00063 0.00284 C13 1 -0.048289 0.915167 0.554936 11.00000 0.05360 0.07303 = 0.05865 -0.00212 -0.00068 0.00079 C14 1 0.435324 0.276239 0.529929 11.00000 0.05372 0.07159 = 0.06260 -0.00207 -0.00718 0.00606 C15 1 0.377846 0.897297 0.613520 11.00000 0.06603 0.08021 = 0.05827 -0.01110 -0.00652 -0.00305 C16 1 0.682194 0.822615 0.638756 11.00000 0.06809 0.07755 = 0.06297 -0.00909 -0.00819 -0.00860 C17 1 0.721771 0.608175 0.668695 11.00000 0.09084 0.07227 = 0.06728 -0.01116 -0.03058 0.00033 C18 1 0.599710 0.530804 0.692302 11.00000 0.16086 0.08474 = 0.07003 0.00730 -0.00213 -0.00171 C19 1 0.887910 0.493301 0.673093 11.00000 0.10229 0.09633 = 0.13245 -0.01329 -0.06488 0.00338 C20 1 0.924282 0.301647 0.702028 11.00000 0.22923 0.10221 = 0.18067 -0.01371 -0.15696 0.03025 C21 1 0.805539 0.219689 0.724877 11.00000 0.36482 0.08989 = 0.11306 0.00848 -0.10363 0.00633 C22 1 0.642784 0.339625 0.720488 11.00000 0.27979 0.09777 = 0.08938 0.01423 0.00432 0.00256 H12 2 0.067785 1.113739 0.603002 11.00000 10.07836 H13 2 -0.164351 0.999876 0.554242 11.00000 10.07481 H14 2 0.542811 0.181504 0.529518 11.00000 10.07639 H16A 2 0.649946 0.987938 0.650219 11.00000 10.08505 H16B 2 0.780626 0.866643 0.622180 11.00000 10.08505 H18 2 0.472655 0.600583 0.687343 11.00000 10.12822 H19 2 0.970372 0.567833 0.654515 11.00000 10.13876 H20 2 1.025072 0.227823 0.705065 11.00000 10.21250 H21 2 0.817117 0.097451 0.745011 11.00000 10.23083 H22 2 0.548847 0.286851 0.734784 11.00000 10.18771 HKLF 4 REM 180402_PhC1BQQDI REM R1 = 0.0851 for 1129 Fo > 4sig(Fo) and 0.1715 for all 2405 data REM 229 parameters refined using 0 restraints END WGHT 0.1163 0.4140 REM Instructions for potential hydrogen bonds EQIV $1 -x+1, -y, -z+1 HTAB C14 N3_$1 HTAB C16 O2 REM Highest difference peak 0.245, deepest hole -0.283, 1-sigma level 0.065 Q1 1 0.8699 0.7921 0.5917 11.00000 0.05 0.24 Q2 1 0.2998 0.3092 0.4775 11.00000 0.05 0.21 Q3 1 0.3584 0.9854 0.6691 11.00000 0.05 0.20 Q4 1 0.7046 0.5089 0.5574 11.00000 0.05 0.20 Q5 1 -0.0353 0.5730 0.5826 11.00000 0.05 0.19 Q6 1 1.0328 0.8329 0.6298 11.00000 0.05 0.19 Q7 1 0.0153 0.8828 0.6097 11.00000 0.05 0.18 Q8 1 0.1979 1.1011 0.6660 11.00000 0.05 0.18 Q9 1 0.8472 1.0244 0.6073 11.00000 0.05 0.18 Q10 1 -0.1864 0.7334 0.5659 11.00000 0.05 0.18 Q11 1 0.5745 0.2204 0.5063 11.00000 0.05 0.18 Q12 1 -0.0043 0.5875 0.5493 11.00000 0.05 0.18 Q13 1 0.3268 0.5242 0.4906 11.00000 0.05 0.18 Q14 1 0.5605 0.1971 0.4917 11.00000 0.05 0.18 Q15 1 0.7124 0.3030 0.5273 11.00000 0.05 0.18 Q16 1 0.1586 0.6537 0.5015 11.00000 0.05 0.18 Q17 1 0.2611 0.5346 0.5799 11.00000 0.05 0.18 Q18 1 0.3267 0.1179 0.4639 11.00000 0.05 0.17 Q19 1 0.3426 0.1427 0.6990 11.00000 0.05 0.17 Q20 1 -0.1588 1.1386 0.5231 11.00000 0.05 0.17 Q21 1 0.0212 1.0309 0.6513 11.00000 0.05 0.16 ; _shelx_res_checksum 15296 _shelx_hkl_file ; 0 0 -3 -1.61 1.07 0 0 -3 -1.29 1.93 0 0 -3 -0.78 0.86 0 0 -3 3.98 1.89 0 0 3 -1.68 2.04 0 0 3 -1.88 1.29 0 0 3 -1.03 0.89 0 0 3 3.90 1.49 0 0 -3 2.96 0.88 0 0 4 50.07 2.79 0 0 4 55.57 1.37 0 0 -4 54.09 2.77 0 0 4 62.57 1.85 0 0 4 55.92 2.92 0 0 -4 66.90 2.74 0 0 -4 57.62 1.27 0 0 -4 57.44 1.57 0 0 4 69.38 2.77 0 0 4 55.85 1.12 -1 0 0 755.08 8.61 -1 0 0 889.60 4.96 -1 0 0 931.70 3.28 -1 0 0 861.76 4.06 1 0 0 836.27 3.05 1 0 0 933.17 3.80 1 0 0 921.99 12.52 1 0 0 1253.89 6.04 1 0 0 1051.96 3.83 1 0 -1 11.17 2.56 1 0 -1 26.80 8.85 1 0 -1 3.15 1.36 1 0 -1 5.09 3.00 -1 0 1 -2.74 7.69 -1 0 1 10.92 3.06 -1 0 1 3.75 2.16 1 0 -1 14.28 4.25 -1 0 1 6.10 2.67 1 0 -1 5.46 2.11 1 0 1 9.52 2.98 -1 0 -1 20.35 11.95 1 0 1 3.87 0.80 1 0 1 2.16 2.86 -1 0 -1 2.16 3.54 1 0 1 9.68 12.06 -1 0 -1 6.43 2.71 -1 0 -1 2.59 1.00 -1 0 -1 12.34 3.32 1 0 1 8.19 3.37 1 0 -2 136.31 8.61 1 0 -2 125.71 2.08 1 0 -2 74.90 2.15 -1 0 2 153.21 2.64 -1 0 2 129.93 1.65 -1 0 2 160.44 6.58 1 0 -2 133.56 2.22 1 0 -2 139.85 3.38 0 0 -5 1.89 1.58 0 0 -5 5.62 2.01 0 0 5 1.36 1.38 0 0 -5 2.99 3.43 0 0 5 3.60 4.54 0 0 5 2.67 1.99 0 0 5 7.46 3.44 0 0 5 2.81 1.73 0 0 5 8.73 3.63 -1 0 -2 451.07 7.59 1 0 2 509.27 3.44 -1 0 -2 416.20 3.13 -1 0 -2 429.00 12.05 1 0 2 481.33 1.13 1 0 2 460.26 9.72 -1 0 -2 492.75 2.62 -1 0 -2 476.62 1.95 1 0 -3 3.06 1.86 1 0 -3 -8.53 3.96 -1 0 3 -0.66 5.42 1 0 -3 0.88 2.47 -1 0 3 2.35 2.11 -1 0 3 3.03 2.15 -1 0 3 -3.92 3.22 1 0 -3 5.86 7.22 1 0 -3 -3.49 2.09 -1 0 3 1.17 2.09 -1 0 -3 2.69 3.90 -1 0 -3 2.78 3.08 -1 0 -3 -2.51 0.99 -1 0 -3 15.62 11.21 -1 0 -3 5.37 4.91 -1 0 -3 -1.21 3.48 1 0 3 7.01 7.50 1 0 3 0.83 1.21 1 0 3 2.50 3.65 1 0 3 3.59 3.51 1 0 -4 9999.00 29.50 1 0 -4 8518.36 34.35 0 0 6 45.85 2.40 0 0 6 52.19 2.73 0 0 -6 -2.05 3.89 0 0 -6 52.85 2.27 0 0 -6 45.27 4.14 0 0 6 46.87 4.30 0 0 6 47.11 2.03 0 0 -6 52.19 3.77 0 0 6 59.90 4.13 0 0 6 46.75 1.56 -1 0 -4 455.07 2.79 -1 0 -4 459.71 11.04 1 0 4 446.08 1.65 1 0 4 447.50 3.22 -1 0 -4 478.88 4.43 -1 0 -4 538.90 1.50 -1 0 -4 431.39 3.92 1 0 4 506.57 4.70 1 0 4 420.84 6.24 1 0 -5 2.93 2.52 -1 0 5 -1.07 2.74 -1 0 5 -6.93 5.23 1 0 -5 -0.11 2.45 -1 0 5 4.96 3.42 1 0 -5 5.46 4.04 -1 0 5 2.09 2.26 -1 0 5 -2.52 3.60 1 0 -5 4.67 6.92 1 0 -5 -2.18 2.53 0 0 7 1.12 2.69 0 0 -7 -6.67 9.62 0 0 -7 1.78 2.23 0 0 7 -3.44 3.10 0 0 7 -5.27 4.70 0 0 7 7.01 4.22 0 0 7 1.85 2.18 0 0 7 -0.87 4.55 0 0 -7 6.71 4.29 -1 0 -5 1.19 4.09 1 0 5 -2.61 2.60 1 0 5 -2.02 4.22 1 0 5 5.90 5.35 1 0 5 4.69 3.25 -1 0 -5 1.97 3.89 -1 0 -5 10.33 9.36 1 0 5 0.51 3.29 -1 0 -5 3.32 3.20 1 0 -6 53.00 2.21 -1 0 6 66.55 5.73 1 0 -6 40.15 2.23 1 0 -6 60.07 4.36 -1 0 6 58.20 4.72 1 0 -6 35.93 6.63 -1 0 6 52.34 3.88 1 0 -6 62.34 2.73 -1 0 6 62.63 3.75 -1 0 6 67.37 2.90 0 -1 0 -7.60 3.66 0 -1 0 0.30 1.15 0 1 0 1.86 3.61 0 1 0 -10.03 10.44 0 1 0 -5.87 3.87 0 1 0 0.52 0.98 0 1 0 6.80 7.09 0 -1 0 1.43 2.88 0 -1 0 5.14 10.83 0 -1 0 -6.96 2.69 0 -1 -1 839.02 6.63 0 1 -1 810.12 1.94 0 -1 1 701.57 3.83 0 -1 1 770.82 4.38 0 -1 1 778.16 3.33 0 -1 1 683.15 9.02 0 -1 1 842.50 2.05 0 -1 -1 854.91 2.02 0 -1 -1 703.06 3.69 0 1 -1 730.62 6.67 0 1 1 775.92 2.25 0 1 1 965.22 19.01 0 -1 -1 726.88 3.95 0 1 1 740.96 4.27 0 1 -1 774.29 4.28 0 1 -1 660.02 3.74 0 1 1 724.66 3.47 0 1 -1 791.68 12.41 0 1 1 771.72 4.28 0 -1 -2 1015.60 4.36 0 1 2 1230.86 9.23 0 1 2 1059.86 4.21 0 -1 -2 1121.19 6.53 0 1 -2 1148.02 3.74 0 -1 2 1084.09 4.67 0 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-4.38 3.88 1 5 -19 -3.04 4.35 -1 -5 19 2.88 3.10 -9 0 10 7.79 7.37 0 -2 -39 23.28 11.02 0 -2 39 -0.35 3.54 -2 0 -40 -20.03 13.30 -2 0 -40 -2.70 4.88 3 -4 25 9.52 3.80 -3 4 -25 2.50 4.12 -3 -4 -25 0.61 6.05 3 4 25 4.73 4.99 9 0 4 -0.74 4.54 -9 0 -4 -2.18 4.49 -4 5 -5 -5.64 3.40 8 0 -23 -7.85 4.81 8 -1 16 3.81 4.62 -8 -1 -16 3.82 3.88 -8 1 -16 -7.77 4.70 8 1 16 2.23 4.33 8 -1 16 4.88 5.18 4 -5 -8 5.71 4.77 4 5 -8 -6.89 4.09 4 0 -39 13.16 19.76 4 0 -39 -0.35 4.73 6 4 -13 9.99 8.63 6 -4 -13 -3.61 5.64 -6 -4 13 -0.32 3.73 -8 -2 -11 -4.23 3.36 -8 2 -11 -1.03 4.67 8 2 11 0.38 4.75 8 -2 11 -2.50 4.55 8 -2 11 -5.25 5.38 -9 -1 3 13.42 9.20 -9 1 3 1.16 3.91 -7 2 -20 -3.39 4.63 7 -2 20 0.08 5.31 7 -2 20 3.44 4.39 7 2 20 2.43 4.72 -9 1 4 0.88 3.71 -9 -1 4 6.97 9.34 6 -2 -30 -0.07 4.43 6 2 -30 13.28 19.13 -6 2 30 -7.98 4.49 -9 1 2 -3.39 3.98 -9 -1 2 -0.40 3.78 5 -1 -36 8.46 9.61 5 1 -36 -6.44 23.46 5 -1 -36 8.78 20.77 5 1 -36 -6.26 5.09 -5 1 36 -4.12 4.41 -5 -1 36 1.39 3.87 4 2 -36 0.69 4.84 4 2 -36 20.82 20.97 -4 -2 36 25.24 3.76 -4 2 36 29.63 8.82 -5 -2 -30 -5.48 6.48 -5 2 -30 -1.61 4.55 5 2 30 -1.41 4.92 7 -2 -25 2.03 4.48 -5 4 -17 -3.80 4.38 5 4 17 -0.88 5.13 -9 1 5 2.48 3.98 -3 5 15 -5.69 3.56 3 -5 -15 14.62 5.29 2 5 -18 -3.00 3.64 2 -5 -18 16.66 7.55 -2 5 18 3.47 3.19 -4 -3 -29 4.20 6.66 -4 3 -29 -4.96 3.97 4 3 29 4.16 5.03 -4 3 -29 -5.85 3.76 6 4 9 2.65 5.29 -6 4 -9 -5.42 3.81 6 -4 9 11.38 6.82 -2 3 35 33.50 4.82 -2 3 35 15.01 4.16 -2 -3 35 1.05 3.25 9 -1 -1 9.26 4.07 -9 -1 1 1.39 3.91 -9 1 1 2.27 4.00 9 0 -11 8.62 4.62 -9 0 11 19.44 5.08 -3 5 -13 -3.92 2.81 -3 5 -13 3.21 3.99 1 0 -42 53.81 16.14 -1 0 42 13.96 7.18 1 0 -42 15.41 10.46 -9 -1 6 -11.58 5.34 -9 1 6 29.55 4.74 -7 3 -13 -6.88 8.82 7 -3 13 -0.37 4.62 7 -3 13 0.66 3.55 7 3 13 9.41 5.18 5 3 -29 14.55 17.90 -5 3 29 12.28 4.55 -8 -2 17 5.65 3.85 8 2 -17 20.87 11.91 8 -2 -17 1.38 5.41 -9 1 0 -4.01 3.99 9 -1 0 1.55 3.94 -9 -1 0 -1.92 3.81 7 3 -18 8.66 12.59 -7 -3 18 -0.33 6.73 7 -3 -18 4.38 4.07 -4 5 -6 5.63 3.39 1 -4 29 6.99 4.19 -1 4 -29 -0.23 3.56 1 4 29 7.25 4.89 -4 -4 -22 21.73 5.49 -4 4 -22 4.92 4.13 4 4 22 -2.86 4.68 -3 1 40 -0.47 3.97 3 1 -40 -2.68 9.77 -3 -1 40 5.27 3.80 3 -1 -40 -6.81 4.31 3 -1 -40 12.34 15.85 -9 0 -5 1.19 4.57 9 0 5 4.47 4.36 8 1 -22 7.23 4.19 8 -1 -22 5.52 4.92 8 1 -22 -13.05 15.07 -2 -4 29 -2.00 3.44 -2 4 29 -2.33 4.10 2 4 -29 0.93 3.34 6 1 -33 4.73 4.15 6 -1 -33 -2.53 4.60 -6 1 33 1.79 4.00 6 1 -33 -5.72 21.83 4 -5 -9 -2.04 4.89 -4 5 9 7.64 3.76 4 5 -9 -8.17 4.14 -2 -1 41 8.32 3.71 2 -1 -41 -13.73 14.59 2 1 -41 -0.23 5.06 -2 1 41 15.44 7.43 2 -1 -41 1.63 4.43 -6 2 -26 3.42 3.80 -6 2 -26 2.43 3.75 6 2 26 17.36 10.93 -6 -2 -26 14.82 11.31 -9 -1 7 -1.38 5.20 -4 3 32 -4.30 4.54 -4 -3 32 -3.32 3.30 -1 -3 -35 15.70 8.20 1 3 35 7.34 4.55 1 -3 35 13.69 3.16 0 0 -42 -4.48 5.55 0 0 -42 25.64 13.68 5 0 -37 0.96 5.37 -5 0 37 -0.82 3.93 5 0 -37 -12.40 22.78 1 -5 19 -1.68 3.34 -1 5 -19 -4.83 3.92 1 5 19 29.36 4.81 -9 -1 -1 6.56 3.83 9 -1 1 4.45 4.03 -9 1 -1 -2.43 4.04 -3 -3 34 7.24 6.80 -3 3 34 0.06 4.24 2 -5 17 3.74 2.70 -2 5 -17 -2.97 4.24 -4 4 25 3.49 3.86 4 4 -25 0.27 4.22 4 -4 -25 8.16 13.17 -3 1 -38 8.96 4.78 -3 -1 -38 12.28 7.54 5 -4 -21 8.89 5.41 5 4 -21 0.44 4.33 -5 4 21 7.11 7.69 -6 0 34 11.94 7.58 6 0 -34 4.95 4.66 6 0 -34 37.80 19.59 -6 -3 25 1.97 3.20 6 3 -25 15.13 16.04 -6 3 25 2.77 3.58 -2 -2 39 2.38 3.78 -2 2 39 -3.78 4.28 2 2 -39 3.08 4.40 2 -2 -39 -5.88 13.71 0 5 20 -0.16 3.64 0 -5 20 8.72 3.20 0 5 -20 -0.78 8.18 -6 -4 14 0.16 3.58 -6 4 14 -1.40 7.14 6 -4 -14 6.17 5.32 6 4 -14 16.44 8.08 9 0 -12 8.11 4.67 -9 -1 8 2.66 5.17 8 0 18 -3.00 4.84 8 0 18 4.03 4.63 -8 0 -18 4.89 8.00 3 -2 -38 8.80 14.91 -3 -2 38 -1.99 3.78 -3 2 38 7.17 8.30 3 2 -38 6.31 4.11 3 3 32 -1.17 5.37 -3 3 -32 34.44 5.31 -3 -3 -32 3.97 13.85 9 -1 2 2.11 3.96 -9 1 -2 -1.14 4.19 -9 -1 -2 3.94 3.78 6 1 29 4.25 4.99 -6 1 -29 4.71 4.40 6 -1 29 4.01 4.17 6 4 10 8.84 5.11 -6 4 -10 5.24 3.73 1 4 -30 1.78 3.88 -1 4 30 -1.46 4.24 -1 -4 30 -6.53 3.66 1 5 -20 -4.28 4.31 -1 5 20 0.80 3.85 -1 -5 20 -0.47 4.02 0 4 30 2.30 4.19 0 4 -30 0.81 4.08 0 -4 30 4.72 7.97 -8 2 -12 14.26 4.73 8 -2 12 -0.86 5.29 8 -2 12 4.74 4.54 9 0 6 -2.86 4.45 -9 0 -6 -0.34 4.70 -4 5 10 -1.30 3.68 4 5 -10 10.93 4.13 4 -5 -10 -9.42 4.85 7 0 25 7.13 4.62 -7 0 -25 27.34 9.04 -7 1 -24 30.98 5.20 -7 1 -24 7.69 3.64 7 1 24 -5.22 4.57 7 -1 24 6.64 4.47 6 3 21 -1.82 5.28 -6 3 -21 -1.82 4.15 6 3 21 2.79 4.50 -6 3 -21 3.15 3.46 -3 -2 -36 4.66 7.20 -3 2 -36 -4.26 4.55 3 2 36 -2.05 4.80 3 5 -16 -10.68 7.99 -3 5 16 -1.61 3.51 3 -5 -16 1.69 5.24 -5 -2 34 -2.62 7.13 -5 2 34 9.02 4.53 2 3 34 1.85 5.10 -2 -3 -34 7.34 7.01 -9 -1 9 6.22 8.72 7 0 -30 0.27 4.84 7 1 -29 1.41 4.18 7 1 -29 -22.15 18.45 7 -1 -29 -10.65 4.84 -3 0 41 5.27 4.00 3 0 -41 5.67 4.69 3 0 -41 10.97 20.05 6 0 30 14.40 4.43 2 -4 28 24.56 4.03 -2 4 -28 12.37 4.24 2 4 28 14.86 4.81 -2 -4 -28 55.51 8.32 -3 5 -14 -6.26 3.97 3 -5 14 -1.46 2.62 -1 3 36 9.89 3.91 -1 -3 36 7.66 3.28 8 -1 17 8.73 4.65 -8 1 -17 9.29 4.52 8 1 17 0.73 4.28 -1 1 -41 -4.48 5.06 -1 -1 -41 -6.98 11.06 -5 1 -33 -5.11 8.63 5 1 33 2.44 4.67 -9 1 -3 -8.39 4.12 9 -1 3 -3.13 4.92 -9 -1 -3 8.15 3.75 9 -1 3 8.41 4.00 8 0 -24 7.43 4.68 5 3 26 -0.81 4.77 -5 -3 -26 -5.23 5.81 -5 3 -26 12.13 3.88 -5 3 -26 -3.54 4.07 8 -2 -18 4.80 5.35 8 2 -18 4.46 11.72 -8 -2 18 0.00 3.92 2 -5 -19 -14.65 7.32 2 5 -19 -4.55 3.68 -2 5 19 -3.08 3.25 7 -3 14 9.06 4.79 7 3 14 -2.98 5.09 7 -3 14 -5.24 4.12 -7 3 -14 0.77 4.11 -1 2 -39 -1.48 4.67 -1 -2 -39 -6.88 8.42 -4 1 -36 11.09 4.37 4 1 36 -0.48 8.95 2 0 -42 0.69 4.94 -2 0 42 2.12 3.78 0 -3 36 -2.75 3.08 0 -3 -36 3.53 10.57 0 3 36 7.40 3.87 5 4 18 0.86 5.12 -5 4 -18 4.48 4.06 3 -4 -28 -0.52 7.59 -3 4 28 -1.24 3.41 3 4 -28 -5.37 4.12 -3 -4 28 1.36 2.96 -7 -3 19 7.59 3.19 7 3 -19 5.46 12.39 7 -3 -19 13.25 4.77 -4 5 -8 -1.17 2.76 -3 0 -39 -0.33 4.32 -7 -2 -21 16.13 5.23 7 2 21 3.15 4.67 7 -2 21 5.52 5.07 -7 2 -21 -10.78 4.43 7 -2 21 12.08 4.16 9 -1 -10 4.89 5.13 -9 -1 10 -1.82 8.30 6 4 -15 17.83 7.88 -6 -4 15 -5.64 3.59 -2 1 -40 5.68 9.81 -2 -1 -40 5.80 10.68 4 5 -11 4.80 8.24 -4 5 11 -8.90 3.69 4 -5 -11 1.50 4.91 3 4 26 5.82 8.51 -3 4 -26 -7.59 4.14 -3 -4 -26 11.29 6.02 9 0 7 58.14 6.09 -9 0 -7 -1.65 4.50 7 -2 -26 8.99 4.67 7 2 -26 2.30 16.57 -9 1 -4 4.01 4.09 9 -1 4 -4.50 5.01 -9 -1 -4 -6.96 3.75 9 -1 4 -3.90 3.99 8 -1 -23 -3.49 4.86 8 1 -23 135.81 20.11 -2 -2 -38 3.50 8.46 -2 2 -38 10.44 4.35 2 2 38 -1.61 4.77 6 4 11 -1.35 5.13 -6 4 -11 2.12 3.73 -5 0 -34 57.91 5.72 4 1 -39 1.97 4.55 4 -1 -39 -4.74 5.11 4 1 -39 -22.13 23.17 4 -1 -39 -0.66 18.29 -4 1 39 0.83 4.33 -4 -1 39 2.33 3.91 2 -5 18 0.42 2.62 -2 5 -18 7.98 7.91 -1 5 -20 6.22 3.73 1 -5 20 6.51 3.25 -6 2 31 2.62 4.33 6 2 -31 -6.49 18.48 -4 -4 -23 3.03 5.41 4 4 23 -5.81 4.62 -4 4 -23 1.10 4.05 8 -2 13 1.87 4.40 8 -2 13 7.45 5.09 -8 2 -13 12.60 9.11 -4 -2 -34 17.10 7.03 -4 2 -34 1.80 4.28 4 2 34 6.68 4.74 -5 4 22 3.20 7.43 9 -1 -11 6.14 5.08 -9 -1 11 9.41 8.46 -4 0 -37 7.99 4.28 -1 -1 42 72.09 7.23 1 1 -42 47.30 17.81 1 -1 -42 -1.97 14.69 1 1 -42 32.67 5.81 0 -5 21 6.10 3.15 0 5 -21 -2.38 4.22 0 5 21 0.94 3.85 9 0 -14 -11.37 9.91 3 -5 -17 -10.15 5.18 -3 5 17 5.73 3.42 1 2 -40 -0.28 5.02 1 -2 -40 -10.53 13.89 -1 -2 40 4.28 3.55 -4 5 -9 6.92 2.72 -5 3 30 3.87 4.38 5 3 -30 4.09 32.77 8 0 19 -4.50 4.62 4 3 30 6.46 4.80 -4 -3 -30 -4.21 6.44 -1 0 -42 -6.92 5.42 -1 0 -42 140.60 16.84 9 -1 5 25.28 8.16 9 -1 5 7.13 4.89 -9 1 -5 16.98 4.14 -9 -1 -5 10.61 3.67 -5 -2 -31 -3.61 5.97 5 2 31 4.28 4.83 -5 2 -31 1.39 4.22 -3 5 -15 -4.45 4.02 3 -5 15 2.18 2.57 -4 4 26 18.49 3.75 4 -4 -26 24.13 5.36 6 3 -26 -0.28 15.70 -6 3 26 4.77 3.58 -4 5 12 -1.09 3.62 4 -5 -12 -6.11 4.88 1 5 -21 5.08 4.29 -1 -5 21 2.12 4.09 -9 0 -8 -3.95 4.43 -2 -4 30 1.81 3.50 1 -4 30 -1.23 7.50 1 4 30 5.47 4.56 8 2 -19 -20.29 11.91 8 -2 -19 2.61 5.30 0 -1 -42 9.04 14.28 0 1 -42 19.25 5.51 -5 1 37 -2.58 4.07 5 1 -37 0.82 4.95 5 -1 -37 -2.52 4.41 -5 -1 37 -0.95 3.72 0 -2 -40 14.41 10.66 0 -2 40 37.30 4.72 0 2 -40 5.61 5.25 -6 2 -27 4.43 8.10 -6 -2 -27 7.29 6.05 6 2 27 6.37 4.71 -4 2 37 10.95 4.44 -4 -2 37 0.52 3.66 4 2 -37 -16.50 19.94 -6 -4 16 0.25 3.44 6 -4 -16 -1.05 5.20 6 4 -16 8.73 7.98 -2 -3 36 4.43 3.28 -7 3 -15 11.68 4.11 7 3 15 5.39 5.22 7 -3 15 40.84 6.43 7 -3 15 23.19 4.02 -2 0 -41 5.52 4.70 -4 0 40 5.71 3.92 4 0 -40 -10.59 19.29 -6 1 34 3.29 8.30 6 1 -34 -0.63 4.04 6 1 -34 -15.15 21.03 6 -1 -34 1.79 4.37 7 3 -20 -12.99 12.06 8 -1 18 10.21 4.87 -8 1 -18 5.77 4.38 -6 -3 -22 -2.21 5.57 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 39046 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 +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 _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.7022(4) 0.4219(7) 0.58605(9) 0.0772(11) Uani 1 1 d . . . . . O2 O 0.3626(4) 1.0729(9) 0.63722(10) 0.0917(13) Uani 1 1 d . . . . . N3 N 0.3122(5) 0.2125(8) 0.50273(10) 0.0617(11) Uani 1 1 d . . . . . N4 N 0.5344(5) 0.7488(8) 0.61159(10) 0.0643(11) Uani 1 1 d . . . . . C5 C 0.1317(5) 0.5614(10) 0.52852(12) 0.0560(12) Uani 1 1 d . . . . . C6 C 0.1628(5) 0.3532(10) 0.50187(12) 0.0574(12) Uani 1 1 d . . . . . C7 C 0.2620(5) 0.6245(10) 0.55709(11) 0.0565(12) Uani 1 1 d . . . . . C8 C -0.0290(5) 0.7136(10) 0.52771(11) 0.0572(12) Uani 1 1 d . . . . . C9 C 0.2378(6) 0.8302(10) 0.58430(12) 0.0597(12) Uani 1 1 d . . . . . C10 C 0.5623(6) 0.5417(11) 0.58547(13) 0.0651(13) Uani 1 1 d . . . . . C11 C 0.4198(6) 0.4767(10) 0.55720(12) 0.0610(13) Uani 1 1 d . . . . . C12 C 0.0825(6) 0.9734(11) 0.58290(13) 0.0647(13) Uani 1 1 d . . . . . C13 C -0.0483(6) 0.9152(11) 0.55494(13) 0.0620(13) Uani 1 1 d . . . . . C14 C 0.4353(6) 0.2762(11) 0.52993(13) 0.0632(13) Uani 1 1 d . . . . . C15 C 0.3778(6) 0.8973(12) 0.61352(14) 0.0688(14) Uani 1 1 d . . . . . C16 C 0.6822(7) 0.8226(12) 0.63876(14) 0.0702(15) Uani 1 1 d . . . . . C17 C 0.7218(8) 0.6082(12) 0.66870(16) 0.0787(16) Uani 1 1 d . . . . . C18 C 0.5997(12) 0.5308(14) 0.69230(18) 0.106(2) Uani 1 1 d . . . . . C19 C 0.8879(8) 0.4933(15) 0.6731(2) 0.114(3) Uani 1 1 d . . . . . C20 C 0.9243(19) 0.302(2) 0.7020(4) 0.180(6) Uani 1 1 d . . . . . C21 C 0.806(3) 0.220(3) 0.7249(3) 0.196(9) Uani 1 1 d . . . . . C22 C 0.643(2) 0.340(2) 0.7205(2) 0.156(4) Uani 1 1 d . . . . . H12 H 0.068(6) 1.114(10) 0.6030(13) 0.078 Uiso 1 1 d . U . . . H13 H -0.164(6) 1.000(9) 0.5542(12) 0.075 Uiso 1 1 d . U . . . H14 H 0.543(6) 0.182(10) 0.5295(12) 0.076 Uiso 1 1 d . U . . . H16A H 0.650(6) 0.988(11) 0.6502(14) 0.085 Uiso 1 1 d . U . . . H16B H 0.781(6) 0.867(10) 0.6222(14) 0.085 Uiso 1 1 d . U . . . H18 H 0.473(8) 0.601(14) 0.6873(18) 0.128 Uiso 1 1 d . U . . . H19 H 0.970(8) 0.568(16) 0.6545(19) 0.139 Uiso 1 1 d . U . . . H20 H 1.025(12) 0.23(2) 0.705(3) 0.212 Uiso 1 1 d . U . . . H21 H 0.817(13) 0.10(2) 0.745(3) 0.231 Uiso 1 1 d . U . . . H22 H 0.549(12) 0.29(2) 0.735(2) 0.188 Uiso 1 1 d . U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.059(2) 0.093(3) 0.077(2) -0.0112(19) -0.0120(17) 0.0057(19) O2 0.080(2) 0.106(3) 0.085(3) -0.037(2) -0.0185(19) 0.011(2) N3 0.057(2) 0.065(3) 0.061(2) -0.0058(19) -0.0077(18) 0.003(2) N4 0.060(2) 0.076(3) 0.055(2) -0.008(2) -0.0103(18) -0.001(2) C5 0.051(3) 0.070(3) 0.047(2) 0.002(2) -0.002(2) -0.002(2) C6 0.055(3) 0.066(3) 0.050(3) 0.004(2) -0.001(2) -0.002(2) C7 0.052(3) 0.066(3) 0.050(3) 0.002(2) -0.002(2) -0.004(2) C8 0.056(3) 0.067(3) 0.047(3) 0.003(2) -0.002(2) 0.000(2) C9 0.059(3) 0.066(3) 0.053(3) -0.002(2) -0.003(2) -0.007(2) C10 0.055(3) 0.080(4) 0.059(3) 0.006(3) -0.005(2) -0.004(3) C11 0.055(3) 0.069(3) 0.058(3) 0.005(2) -0.004(2) -0.003(2) C12 0.066(3) 0.072(3) 0.056(3) -0.011(2) -0.001(2) 0.003(3) C13 0.054(3) 0.073(3) 0.059(3) -0.002(2) -0.001(2) 0.001(2) C14 0.054(3) 0.072(3) 0.063(3) -0.002(3) -0.007(2) 0.006(2) C15 0.066(3) 0.080(4) 0.058(3) -0.011(3) -0.007(2) -0.003(3) C16 0.068(3) 0.078(4) 0.063(3) -0.009(3) -0.008(3) -0.009(3) C17 0.091(4) 0.072(4) 0.067(3) -0.011(3) -0.031(3) 0.000(3) C18 0.161(7) 0.085(5) 0.070(4) 0.007(4) -0.002(4) -0.002(5) C19 0.102(5) 0.096(5) 0.132(6) -0.013(5) -0.065(4) 0.003(4) C20 0.229(13) 0.102(7) 0.181(11) -0.014(7) -0.157(10) 0.030(8) C21 0.36(2) 0.090(8) 0.113(9) 0.008(6) -0.104(12) 0.006(10) C22 0.280(15) 0.098(7) 0.089(6) 0.014(5) 0.004(7) 0.003(8) 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 for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (Vol. C, Table 6.1.1.4) ; N N 0.0311 0.0180 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.0492 0.0322 ; International Tables for Crystallography (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 C6 N3 C14 118.0(4) . . ? C10 N4 C15 124.8(4) . . ? C10 N4 C16 117.0(4) . . ? C15 N4 C16 118.1(4) . . ? C7 C5 C6 119.1(4) . . ? C7 C5 C8 118.5(4) . . ? C6 C5 C8 122.5(4) . . ? N3 C6 C5 122.3(4) . . ? N3 C6 C8 118.3(4) . 3_566 ? C5 C6 C8 119.5(4) . 3_566 ? C9 C7 C5 121.4(4) . . ? C9 C7 C11 120.8(4) . . ? C5 C7 C11 117.9(4) . . ? C13 C8 C5 118.6(4) . . ? C13 C8 C6 123.3(4) . 3_566 ? C5 C8 C6 118.1(4) . 3_566 ? C12 C9 C7 119.1(4) . . ? C12 C9 C15 120.5(4) . . ? C7 C9 C15 120.4(4) . . ? O1 C10 N4 120.5(4) . . ? O1 C10 C11 122.0(5) . . ? N4 C10 C11 117.5(4) . . ? C14 C11 C7 118.0(4) . . ? C14 C11 C10 121.9(5) . . ? C7 C11 C10 120.1(5) . . ? C9 C12 C13 120.7(5) . . ? C9 C12 H12 117(3) . . ? C13 C12 H12 122(3) . . ? C8 C13 C12 121.8(5) . . ? C8 C13 H13 115(3) . . ? C12 C13 H13 123(3) . . ? N3 C14 C11 124.8(5) . . ? N3 C14 H14 117(3) . . ? C11 C14 H14 118(3) . . ? O2 C15 N4 121.1(4) . . ? O2 C15 C9 122.5(5) . . ? N4 C15 C9 116.3(4) . . ? N4 C16 C17 114.0(4) . . ? N4 C16 H16A 105(3) . . ? C17 C16 H16A 109(3) . . ? N4 C16 H16B 104(3) . . ? C17 C16 H16B 116(3) . . ? H16A C16 H16B 108(4) . . ? C18 C17 C19 120.1(6) . . ? C18 C17 C16 120.7(5) . . ? C19 C17 C16 119.2(6) . . ? C17 C18 C22 119.1(9) . . ? C17 C18 H18 120(4) . . ? C22 C18 H18 121(4) . . ? C20 C19 C17 118.3(10) . . ? C20 C19 H19 128(4) . . ? C17 C19 H19 114(4) . . ? C21 C20 C19 122.3(13) . . ? C21 C20 H20 118(8) . . ? C19 C20 H20 120(8) . . ? C20 C21 C22 118.4(12) . . ? C20 C21 H21 129(7) . . ? C22 C21 H21 113(7) . . ? C18 C22 C21 121.7(12) . . ? C18 C22 H22 114(7) . . ? C21 C22 H22 124(6) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C10 1.227(5) . ? O2 C15 1.204(5) . ? N3 C6 1.339(5) . ? N3 C14 1.342(5) . ? N4 C10 1.388(6) . ? N4 C15 1.414(6) . ? N4 C16 1.485(6) . ? C5 C7 1.410(6) . ? C5 C6 1.411(6) . ? C5 C8 1.443(6) . ? C6 C8 1.456(6) 3_566 ? C7 C9 1.405(6) . ? C7 C11 1.415(6) . ? C8 C13 1.385(6) . ? C8 C6 1.456(6) 3_566 ? C9 C12 1.384(6) . ? C9 C15 1.481(6) . ? C10 C11 1.470(6) . ? C11 C14 1.378(6) . ? C12 C13 1.394(6) . ? C12 H12 0.99(5) . ? C13 H13 0.99(4) . ? C14 H14 0.95(5) . ? C16 C17 1.495(8) . ? C16 H16A 0.93(5) . ? C16 H16B 1.02(5) . ? C17 C18 1.365(8) . ? C17 C19 1.400(8) . ? C18 C22 1.381(12) . ? C18 H18 1.04(6) . ? C19 C20 1.393(14) . ? C19 H19 1.02(6) . ? C20 C21 1.33(2) . ? C20 H20 0.86(10) . ? C21 C22 1.386(18) . ? C21 H21 0.92(12) . ? C22 H22 0.95(8) . ? 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 C14 N3 C6 C5 -0.5(7) . . . . ? C14 N3 C6 C8 179.6(4) . . . 3_566 ? C7 C5 C6 N3 0.0(6) . . . . ? C8 C5 C6 N3 180.0(4) . . . . ? C7 C5 C6 C8 179.9(4) . . . 3_566 ? C8 C5 C6 C8 -0.1(7) . . . 3_566 ? C6 C5 C7 C9 179.9(4) . . . . ? C8 C5 C7 C9 -0.1(6) . . . . ? C6 C5 C7 C11 0.9(6) . . . . ? C8 C5 C7 C11 -179.1(4) . . . . ? C7 C5 C8 C13 0.1(6) . . . . ? C6 C5 C8 C13 -179.8(4) . . . . ? C7 C5 C8 C6 -179.9(4) . . . 3_566 ? C6 C5 C8 C6 0.1(7) . . . 3_566 ? C5 C7 C9 C12 0.0(7) . . . . ? C11 C7 C9 C12 179.0(4) . . . . ? C5 C7 C9 C15 -178.6(4) . . . . ? C11 C7 C9 C15 0.4(7) . . . . ? C15 N4 C10 O1 -179.4(5) . . . . ? C16 N4 C10 O1 2.1(7) . . . . ? C15 N4 C10 C11 1.5(7) . . . . ? C16 N4 C10 C11 -177.0(4) . . . . ? C9 C7 C11 C14 179.6(4) . . . . ? C5 C7 C11 C14 -1.4(6) . . . . ? C9 C7 C11 C10 -1.4(7) . . . . ? C5 C7 C11 C10 177.7(4) . . . . ? O1 C10 C11 C14 0.4(8) . . . . ? N4 C10 C11 C14 179.5(4) . . . . ? O1 C10 C11 C7 -178.6(4) . . . . ? N4 C10 C11 C7 0.5(7) . . . . ? C7 C9 C12 C13 -0.1(7) . . . . ? C15 C9 C12 C13 178.6(4) . . . . ? C5 C8 C13 C12 -0.2(7) . . . . ? C6 C8 C13 C12 179.9(4) 3_566 . . . ? C9 C12 C13 C8 0.1(8) . . . . ? C6 N3 C14 C11 0.0(7) . . . . ? C7 C11 C14 N3 1.0(7) . . . . ? C10 C11 C14 N3 -178.0(5) . . . . ? C10 N4 C15 O2 179.3(5) . . . . ? C16 N4 C15 O2 -2.2(7) . . . . ? C10 N4 C15 C9 -2.4(7) . . . . ? C16 N4 C15 C9 176.0(4) . . . . ? C12 C9 C15 O2 1.0(8) . . . . ? C7 C9 C15 O2 179.7(5) . . . . ? C12 C9 C15 N4 -177.2(4) . . . . ? C7 C9 C15 N4 1.4(7) . . . . ? C10 N4 C16 C17 -73.4(6) . . . . ? C15 N4 C16 C17 108.1(6) . . . . ? N4 C16 C17 C18 -58.6(7) . . . . ? N4 C16 C17 C19 123.5(6) . . . . ? C19 C17 C18 C22 0.3(10) . . . . ? C16 C17 C18 C22 -177.7(6) . . . . ? C18 C17 C19 C20 -0.3(10) . . . . ? C16 C17 C19 C20 177.6(6) . . . . ? C17 C19 C20 C21 1.7(15) . . . . ? C19 C20 C21 C22 -3(2) . . . . ? C17 C18 C22 C21 -1.5(13) . . . . ? C20 C21 C22 C18 2.7(18) . . . . ?