#------------------------------------------------------------------------------ #$Date: 2024-06-29 01:08:40 +0300 (Sat, 29 Jun 2024) $ #$Revision: 292645 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/20/1572009.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_1572009 loop_ _publ_author_name 'Wang, Xia' 'Wang, Shao-Jie' 'Xin, Xiaolan' 'An, Hao' 'Tu, Zhifeng' 'Yang, Hui' 'Wong, Ming Wah' 'Lu, Shenci' _publ_section_title ; Enantioconvergent and Diastereoselective Synthesis of Atropisomeric Hydrazides Bearing a Cyclic Quaternary Stereocenter through Ternary Catalysis ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC03190C _journal_year 2024 _chemical_absolute_configuration rmad _chemical_formula_moiety 'C24 H33 N3 O7' _chemical_formula_sum 'C24 H33 N3 O7' _chemical_formula_weight 475.53 _space_group_crystal_system triclinic _space_group_IT_number 1 _space_group_name_Hall 'P 1' _space_group_name_H-M_alt 'P 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2023-04-06 _audit_creation_method ; Olex2 1.5-alpha (compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748) ; _audit_update_record ; 2023-04-06 deposited with the CCDC. 2024-06-27 downloaded from the CCDC. ; _cell_angle_alpha 97.915(6) _cell_angle_beta 92.615(6) _cell_angle_gamma 118.101(6) _cell_formula_units_Z 2 _cell_length_a 10.4813(16) _cell_length_b 10.5048(16) _cell_length_c 13.991(2) _cell_measurement_reflns_used 9807 _cell_measurement_temperature 298.0 _cell_measurement_theta_max 51.694 _cell_measurement_theta_min 2.80 _cell_volume 1335.1(4) _computing_cell_refinement 'SAINT V8.38A (Bruker, 2018)' _computing_data_reduction 'SAINT V8.38A (Bruker, 2018)' _computing_molecular_graphics 'Olex2 1.5-alpha (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5-alpha (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 298.0 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.972 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type GaK\a _diffrn_radiation_wavelength 1.34139 _diffrn_reflns_av_R_equivalents 0.0414 _diffrn_reflns_av_unetI/netI 0.0376 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.972 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 45082 _diffrn_reflns_point_group_measured_fraction_full 0.983 _diffrn_reflns_point_group_measured_fraction_max 0.927 _diffrn_reflns_theta_full 53.594 _diffrn_reflns_theta_max 65.108 _diffrn_reflns_theta_min 2.797 _diffrn_source_current 2.86 _diffrn_source_power 0.1997996 _diffrn_source_voltage 69.86 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.460 _exptl_absorpt_correction_T_max 0.7526 _exptl_absorpt_correction_T_min 0.6592 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1160 before and 0.0597 after correction. The Ratio of minimum to maximum transmission is 0.8759. The \l/2 correction factor is Not present. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.183 _exptl_crystal_description block _exptl_crystal_F_000 508 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _refine_diff_density_max 0.360 _refine_diff_density_min -0.144 _refine_diff_density_rms 0.034 _refine_ls_abs_structure_details ; Flack x determined using 3410 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.05(7) _refine_ls_extinction_coef 0.043(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 628 _refine_ls_number_reflns 12815 _refine_ls_number_restraints 3 _refine_ls_restrained_S_all 1.002 _refine_ls_R_factor_all 0.0777 _refine_ls_R_factor_gt 0.0527 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1066P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1450 _refine_ls_wR_factor_ref 0.1627 _reflns_Friedel_coverage 0.907 _reflns_Friedel_fraction_full 0.972 _reflns_Friedel_fraction_max 0.881 _reflns_number_gt 8482 _reflns_number_total 12815 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc03190c2.cif _cod_data_source_block 20220728bl_0m _cod_original_cell_volume 1335.2(4) _cod_database_code 1572009 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.991 _shelx_estimated_absorpt_t_min 0.947 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C36(H36), C12(H12) 2.b Secondary CH2 refined with riding coordinates: C16(H16A,H16B), C19(H19A,H19B), C40(H40A,H40B), C43(H43A,H43B) 2.c Aromatic/amide H refined with riding coordinates: N3(H3), N4(H4A), C6(H6), C2(H2), C3(H3A), C4(H4), C5(H5), C31(H31), C27(H27), C33(H33), C8(H8), C28(H28), C29(H29), C30(H30) 2.d Idealised Me refined as rotating group: C38(H38A,H38B,H38C), C14(H14A,H14B,H14C), C13(H13A,H13B,H13C), C37(H37A,H37B, H37C), C01H(H01A,H01B,H01C), C23(H23A,H23B,H23C), C01J(H01D,H01E,H01F), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C01N(H01G,H01H,H01I), C41(H41A,H41B, H41C), C17(H17A,H17B,H17C), C44(H44A,H44B,H44C), C20(H20A,H20B,H20C) ; _shelx_res_file ; TITL 20220728bl_0m_a.res in P1 20220728bl_0m.res created by SHELXL-2018/3 at 16:29:12 on 06-Apr-2023 REM Old TITL 20220728bl_0m_a.res in P1 REM SHELXT solution in P1: R1 0.180, Rweak 0.062, Alpha 0.000 REM 0.000 for 0 systematic absences, Orientation as input REM Flack x = 0.249 ( 0.046 ) from 3576 Parsons' quotients REM Formula found by SHELXT: C42 N7 O15 CELL 1.34139 10.4813 10.5048 13.9913 97.915 92.615 118.101 ZERR 2 0.0016 0.0016 0.0022 0.006 0.006 0.006 LATT -1 SFAC C H N O DISP C 0.0137 0.0067 57.1 DISP H 0 0 0.6 DISP N 0.0241 0.0134 109.9 DISP O 0.0389 0.0241 193.4 UNIT 48 66 6 14 L.S. 15 PLAN 50 SIZE 0.12 0.04 0.02 TEMP 24.85 CONF list 4 MORE -1 BOND $H fmap 2 acta REM REM REM WGHT 0.106600 EXTI 0.043436 FVAR 1.85720 O2 4 0.605869 0.190201 0.225567 11.00000 0.09376 0.06171 = 0.08552 0.02166 0.02662 0.04572 O3 4 0.510868 0.209734 0.364429 11.00000 0.10879 0.08539 = 0.09366 0.04303 0.04082 0.06795 O13 4 0.582817 0.378177 0.885810 11.00000 0.10628 0.09145 = 0.07450 0.01727 -0.00731 0.01785 O1 4 0.387355 0.563515 0.197459 11.00000 0.08612 0.11023 = 0.13837 0.05624 0.01370 0.06729 O14 4 0.868335 0.429513 0.798054 11.00000 0.08684 0.09033 = 0.11669 0.01098 -0.01577 0.05633 O5 4 0.288458 0.229745 0.148889 11.00000 0.09366 0.10496 = 0.07044 0.01805 0.00184 0.02362 O11 4 0.474896 0.623567 0.821474 11.00000 0.06191 0.08579 = 0.10160 -0.01079 0.00849 0.03409 N3 3 0.304046 0.290328 0.402660 11.00000 0.06886 0.07593 = 0.07129 0.01855 0.00983 0.04232 AFIX 43 H3 2 0.363508 0.276218 0.438411 11.00000 -1.20000 AFIX 0 N1 3 0.581841 0.389206 0.272855 11.00000 0.06301 0.05529 = 0.07506 0.02002 0.00708 0.03490 O10 4 0.401883 0.459814 0.680883 11.00000 0.07027 0.10963 = 0.11631 -0.03163 -0.02564 0.05237 O4 4 0.148338 0.099323 0.254843 11.00000 0.08252 0.07795 = 0.08966 0.01426 0.00183 0.00990 O8 4 0.322262 0.025397 0.538798 11.00000 0.08188 0.09276 = 0.11983 -0.03608 -0.02659 0.04472 O7 4 0.159308 0.214819 0.512618 11.00000 0.08264 0.11371 = 0.09234 0.03134 0.02954 0.05727 O6 4 0.105522 0.327465 0.403887 11.00000 0.09211 0.14103 = 0.13128 0.05156 0.02824 0.08058 N6 3 0.638993 0.580234 0.748074 11.00000 0.05703 0.07089 = 0.06827 0.00983 -0.00108 0.03473 N2 3 0.333452 0.323619 0.309915 11.00000 0.06287 0.06937 = 0.06999 0.01626 0.00700 0.03059 N4 3 0.459419 0.230683 0.638910 11.00000 0.07294 0.07415 = 0.07460 -0.00818 -0.01528 0.03746 AFIX 43 H4A 2 0.413240 0.265180 0.608181 11.00000 -1.20000 AFIX 0 C1 1 0.786562 0.456077 0.168960 11.00000 0.05307 0.05919 = 0.07449 0.01803 0.00068 0.02527 C21 1 0.561876 0.255840 0.293838 11.00000 0.06915 0.05871 = 0.07671 0.02331 0.01477 0.03922 N5 3 0.557217 0.315489 0.721523 11.00000 0.06793 0.06706 = 0.06968 0.00715 -0.00679 0.02504 C00L 1 0.495668 0.548113 0.744869 11.00000 0.06028 0.08001 = 0.08205 0.00318 0.00051 0.03938 O9 4 0.509617 0.040752 0.633858 11.00000 0.12418 0.09062 = 0.19259 -0.01750 -0.05559 0.06337 O12 4 0.388120 0.171537 0.806196 11.00000 0.10837 0.08804 = 0.10427 0.02141 0.00548 -0.00453 C10 1 0.467600 0.512321 0.209205 11.00000 0.06467 0.07443 = 0.10116 0.03148 0.00091 0.03839 C6 1 0.822177 0.466562 0.075010 11.00000 0.06561 0.07654 = 0.06956 0.01797 -0.00123 0.03266 AFIX 43 H6 2 0.755851 0.462683 0.026686 11.00000 -1.20000 AFIX 0 C2 1 0.887496 0.460879 0.240178 11.00000 0.06851 0.08029 = 0.07592 0.01955 0.00059 0.03881 AFIX 43 H2 2 0.865433 0.453717 0.303507 11.00000 -1.20000 AFIX 0 C26 1 0.770467 0.840035 0.839604 11.00000 0.06866 0.06957 = 0.07527 0.01774 0.00910 0.03359 C34 1 0.808817 0.504345 0.791579 11.00000 0.06416 0.07324 = 0.08120 0.01718 -0.00685 0.03603 C36 1 0.720785 0.465772 0.613158 11.00000 0.07840 0.10440 = 0.07231 0.01004 0.00967 0.04971 AFIX 13 H36 2 0.634034 0.438360 0.567954 11.00000 -1.20000 AFIX 0 C3 1 1.019084 0.476150 0.216743 11.00000 0.06779 0.10408 = 0.09357 0.01776 -0.01040 0.04704 AFIX 43 H3A 2 1.085330 0.477852 0.264122 11.00000 -1.20000 AFIX 0 C18 1 0.257812 0.216328 0.229504 11.00000 0.07114 0.07235 = 0.07911 0.01274 -0.00024 0.02480 C7 1 0.648911 0.450634 0.193231 11.00000 0.05632 0.06035 = 0.06967 0.01746 0.00116 0.02609 C42 1 0.511860 0.293569 0.812073 11.00000 0.08357 0.07238 = 0.07926 0.01381 -0.00804 0.01785 C32 1 0.754069 0.691653 0.814626 11.00000 0.06165 0.06740 = 0.06545 0.01480 0.00311 0.02979 C39 1 0.437120 0.092233 0.606843 11.00000 0.08329 0.08163 = 0.10914 -0.01527 -0.01756 0.04497 C12 1 0.539135 0.561424 0.392183 11.00000 0.07933 0.05956 = 0.10000 0.00708 -0.00021 0.03989 AFIX 13 H12 2 0.549102 0.513943 0.445491 11.00000 -1.20000 AFIX 0 C38 1 0.835913 0.621141 0.603937 11.00000 0.11049 0.13215 = 0.09503 0.03384 0.03639 0.04077 AFIX 137 H38A 2 0.802934 0.689554 0.627175 11.00000 -1.50000 H38B 2 0.850908 0.624486 0.536953 11.00000 -1.50000 H38C 2 0.925942 0.646609 0.641914 11.00000 -1.50000 AFIX 0 C11 1 0.474388 0.442398 0.299139 11.00000 0.06267 0.05950 = 0.07913 0.01833 0.00562 0.03700 C4 1 1.053736 0.488990 0.123387 11.00000 0.06560 0.11000 = 0.09673 0.01927 0.01222 0.04363 AFIX 43 H4 2 1.144071 0.501933 0.108234 11.00000 -1.20000 AFIX 0 C5 1 0.954326 0.482584 0.052938 11.00000 0.07219 0.09698 = 0.08407 0.01966 0.01293 0.03920 AFIX 43 H5 2 0.976890 0.489179 -0.010331 11.00000 -1.20000 AFIX 0 C31 1 0.713553 0.896281 0.776750 11.00000 0.08267 0.07867 = 0.09680 0.02181 0.00720 0.03891 AFIX 43 H31 2 0.658133 0.837287 0.718468 11.00000 -1.20000 AFIX 0 C35 1 0.675865 0.459495 0.715711 11.00000 0.06216 0.07078 = 0.06482 0.00859 0.00073 0.03612 C15 1 0.180689 0.280670 0.435247 11.00000 0.06549 0.08272 = 0.08847 0.01771 0.01268 0.03913 C14 1 0.692284 0.683783 0.383455 11.00000 0.08907 0.06609 = 0.13165 0.00012 -0.00724 0.03039 AFIX 137 H14A 2 0.754955 0.641946 0.369761 11.00000 -1.50000 H14B 2 0.730937 0.753016 0.443483 11.00000 -1.50000 H14C 2 0.686641 0.732833 0.331668 11.00000 -1.50000 AFIX 0 C27 1 0.851610 0.930361 0.926009 11.00000 0.10633 0.07489 = 0.08174 0.00839 -0.00035 0.04155 AFIX 43 H27 2 0.889060 0.894047 0.970153 11.00000 -1.20000 AFIX 0 C13 1 0.441549 0.628787 0.421183 11.00000 0.11540 0.07629 = 0.13127 0.00596 0.01138 0.06426 AFIX 137 H13A 2 0.430958 0.678125 0.370984 11.00000 -1.50000 H13B 2 0.485188 0.697848 0.481020 11.00000 -1.50000 H13C 2 0.347418 0.552553 0.429699 11.00000 -1.50000 AFIX 0 C33 1 0.852891 0.650136 0.840463 11.00000 0.05991 0.07120 = 0.08205 0.01248 -0.01227 0.02817 AFIX 43 H33 2 0.937422 0.708134 0.883826 11.00000 -1.20000 AFIX 0 C22 1 0.598659 0.048257 0.232500 11.00000 0.10606 0.06433 = 0.11297 0.01608 0.02643 0.05441 C8 1 0.582791 0.518072 0.155293 11.00000 0.06433 0.08438 = 0.09640 0.04306 0.00774 0.03665 AFIX 43 H8 2 0.608269 0.562752 0.101102 11.00000 -1.20000 AFIX 0 C28 1 0.877762 1.072969 0.947652 11.00000 0.13253 0.07697 = 0.10260 -0.00706 0.01065 0.04511 AFIX 43 H28 2 0.934468 1.133203 1.005265 11.00000 -1.20000 AFIX 0 C37 1 0.778227 0.358413 0.581040 11.00000 0.10567 0.14449 = 0.11083 -0.00484 0.01731 0.08283 AFIX 137 H37A 2 0.784143 0.350559 0.512392 11.00000 -1.50000 H37B 2 0.713100 0.263691 0.595154 11.00000 -1.50000 H37C 2 0.873326 0.393914 0.615509 11.00000 -1.50000 AFIX 0 C29 1 0.819821 1.125858 0.883872 11.00000 0.13056 0.07850 = 0.12219 0.01630 0.02711 0.05557 AFIX 43 H29 2 0.836679 1.222004 0.898535 11.00000 -1.20000 AFIX 0 C01H 1 0.364135 0.714768 0.930666 11.00000 0.11846 0.13376 = 0.16420 -0.02793 0.03956 0.06327 AFIX 137 H01A 2 0.426329 0.813084 0.921064 11.00000 -1.50000 H01B 2 0.413208 0.690586 0.978819 11.00000 -1.50000 H01C 2 0.275776 0.707658 0.952308 11.00000 -1.50000 AFIX 0 C23 1 0.443093 -0.067815 0.218056 11.00000 0.12349 0.06523 = 0.16691 0.01567 0.02324 0.03683 AFIX 137 H23A 2 0.395847 -0.051516 0.271954 11.00000 -1.50000 H23B 2 0.437748 -0.162220 0.213950 11.00000 -1.50000 H23C 2 0.395346 -0.064573 0.158947 11.00000 -1.50000 AFIX 0 C01J 1 0.228281 0.455435 0.848080 11.00000 0.08088 0.11600 = 0.20277 0.01137 0.05126 0.03666 AFIX 137 H01D 2 0.136500 0.447326 0.862909 11.00000 -1.50000 H01E 2 0.271234 0.432587 0.900656 11.00000 -1.50000 H01F 2 0.213024 0.388069 0.789411 11.00000 -1.50000 AFIX 0 C24 1 0.672560 0.029686 0.143131 11.00000 0.16177 0.11014 = 0.13568 -0.00008 0.04095 0.08917 AFIX 137 H24A 2 0.633202 0.051903 0.088424 11.00000 -1.50000 H24B 2 0.654985 -0.069661 0.128507 11.00000 -1.50000 H24C 2 0.775624 0.095225 0.156676 11.00000 -1.50000 AFIX 0 C25 1 0.685421 0.060122 0.324835 11.00000 0.14934 0.11108 = 0.12931 0.03111 0.01413 0.09806 AFIX 137 H25A 2 0.780203 0.144718 0.331893 11.00000 -1.50000 H25B 2 0.695554 -0.026414 0.322427 11.00000 -1.50000 H25C 2 0.635996 0.069649 0.379237 11.00000 -1.50000 AFIX 0 C30 1 0.737357 1.037867 0.798799 11.00000 0.11603 0.09514 = 0.12193 0.03918 0.01980 0.06329 AFIX 43 H30 2 0.697460 1.073792 0.755945 11.00000 -1.20000 AFIX 0 C01N 1 0.274209 0.652571 0.751955 11.00000 0.10656 0.14319 = 0.18016 -0.00401 -0.00210 0.08661 AFIX 137 H01G 2 0.344776 0.750385 0.746200 11.00000 -1.50000 H01H 2 0.183448 0.649896 0.763444 11.00000 -1.50000 H01I 2 0.259943 0.586389 0.692870 11.00000 -1.50000 AFIX 0 C01O 1 0.327553 0.607745 0.834546 11.00000 0.06938 0.10382 = 0.14772 -0.01032 0.01783 0.04897 C16 1 0.037166 0.201323 0.561685 11.00000 0.09891 0.15592 = 0.11349 0.02686 0.04589 0.06541 AFIX 23 H16A 2 -0.047748 0.170628 0.515028 11.00000 -1.20000 H16B 2 0.059717 0.294241 0.601593 11.00000 -1.20000 AFIX 0 C19 1 0.055352 -0.014806 0.174513 11.00000 0.12617 0.09371 = 0.12059 0.00217 -0.01780 -0.00055 AFIX 23 H19A 2 0.002170 0.020334 0.137134 11.00000 -1.20000 H19B 2 0.114955 -0.038240 0.132136 11.00000 -1.20000 AFIX 0 C40 1 0.284133 -0.120902 0.491555 11.00000 0.12931 0.09339 = 0.17695 -0.05112 -0.03593 0.05473 AFIX 23 H40A 2 0.359416 -0.116868 0.452277 11.00000 -1.20000 H40B 2 0.278977 -0.179738 0.540433 11.00000 -1.20000 AFIX 0 C43 1 0.335970 0.141058 0.903475 11.00000 0.16598 0.12231 = 0.14283 0.05469 0.03410 0.01172 AFIX 23 H43A 2 0.407764 0.134185 0.945576 11.00000 -1.20000 H43B 2 0.318308 0.218391 0.935179 11.00000 -1.20000 AFIX 0 C41 1 0.153198 -0.185605 0.433773 11.00000 0.12925 0.16469 = 0.19587 -0.07820 -0.01355 0.02172 AFIX 137 H41A 2 0.161755 -0.134687 0.380448 11.00000 -1.50000 H41B 2 0.080329 -0.181390 0.471207 11.00000 -1.50000 H41C 2 0.125535 -0.286188 0.409074 11.00000 -1.50000 AFIX 0 C17 1 0.010076 0.089120 0.622821 11.00000 0.20095 0.23916 = 0.25510 0.12948 0.15577 0.11134 AFIX 137 H17A 2 -0.031095 -0.005870 0.582123 11.00000 -1.50000 H17B 2 -0.056638 0.089754 0.667430 11.00000 -1.50000 H17C 2 0.100371 0.110623 0.658606 11.00000 -1.50000 AFIX 0 C44 1 0.208980 0.009771 0.883439 11.00000 0.19714 0.19180 = 0.25258 0.06842 0.11194 0.03717 AFIX 137 H44A 2 0.211736 -0.048135 0.824976 11.00000 -1.50000 H44B 2 0.127755 0.027614 0.874835 11.00000 -1.50000 H44C 2 0.198594 -0.042028 0.936487 11.00000 -1.50000 AFIX 0 C20 1 -0.040619 -0.137703 0.205463 11.00000 0.15543 0.09193 = 0.21452 0.02948 -0.01294 0.00271 AFIX 137 H20A 2 -0.078926 -0.219464 0.152447 11.00000 -1.50000 H20B 2 -0.119012 -0.124317 0.228738 11.00000 -1.50000 H20C 2 0.008095 -0.156390 0.257129 11.00000 -1.50000 AFIX 0 HKLF 4 REM 20220728bl_0m_a.res in P1 REM wR2 = 0.1627, GooF = S = 1.002, Restrained GooF = 1.002 for all data REM R1 = 0.0527 for 8482 Fo > 4sig(Fo) and 0.0777 for all 12815 data REM 628 parameters refined using 3 restraints END WGHT 0.1067 0.0000 REM Highest difference peak 0.360, deepest hole -0.144, 1-sigma level 0.034 Q1 1 -0.0865 0.0688 0.5326 11.00000 0.05 0.36 Q2 1 0.0641 -0.1267 0.1597 11.00000 0.05 0.33 Q3 1 0.3670 0.0596 0.9437 11.00000 0.05 0.33 Q4 1 0.1882 -0.2160 0.5188 11.00000 0.05 0.26 Q5 1 0.3223 0.2169 0.4130 11.00000 0.05 0.17 Q6 1 0.3791 0.2435 0.6423 11.00000 0.05 0.12 Q7 1 0.3936 0.2118 0.4029 11.00000 0.05 0.12 Q8 1 0.1866 0.0379 0.2803 11.00000 0.05 0.12 Q9 1 0.7829 1.0377 0.7697 11.00000 0.05 0.11 Q10 1 0.2528 0.3270 0.8430 11.00000 0.05 0.11 Q11 1 0.3048 0.1790 0.1523 11.00000 0.05 0.11 Q12 1 0.4412 0.4593 0.2586 11.00000 0.05 0.11 Q13 1 1.0155 0.7187 0.9453 11.00000 0.05 0.11 Q14 1 0.7513 1.1054 0.7397 11.00000 0.05 0.11 Q15 1 0.7344 0.4614 0.1787 11.00000 0.05 0.10 Q16 1 0.8722 0.2621 0.2920 11.00000 0.05 0.10 Q17 1 0.1211 0.4623 0.6984 11.00000 0.05 0.10 Q18 1 0.6246 -0.0823 0.3338 11.00000 0.05 0.10 Q19 1 0.6128 0.1625 0.6436 11.00000 0.05 0.10 Q20 1 -0.0204 -0.0218 0.2093 11.00000 0.05 0.10 Q21 1 0.0840 0.1549 0.4734 11.00000 0.05 0.10 Q22 1 0.9166 1.0848 1.0712 11.00000 0.05 0.10 Q23 1 0.3337 0.4659 0.1720 11.00000 0.05 0.10 Q24 1 0.2433 0.1744 0.8075 11.00000 0.05 0.10 Q25 1 0.8426 0.4948 0.2132 11.00000 0.05 0.10 Q26 1 0.1781 0.0505 1.0127 11.00000 0.05 0.10 Q27 1 0.6353 0.6401 0.7040 11.00000 0.05 0.09 Q28 1 0.9583 0.5189 0.7340 11.00000 0.05 0.09 Q29 1 0.2029 0.1921 0.2484 11.00000 0.05 0.09 Q30 1 0.4318 0.0281 0.6633 11.00000 0.05 0.09 Q31 1 0.6234 -0.1022 0.1698 11.00000 0.05 0.09 Q32 1 0.6698 0.2572 0.2699 11.00000 0.05 0.09 Q33 1 0.2835 -0.0657 0.5712 11.00000 0.05 0.09 Q34 1 0.0963 -0.3412 0.4532 11.00000 0.05 0.09 Q35 1 0.2580 0.5413 0.5710 11.00000 0.05 0.09 Q36 1 0.5996 0.3995 0.9869 11.00000 0.05 0.09 Q37 1 0.6760 0.2463 0.3681 11.00000 0.05 0.09 Q38 1 0.5005 0.0324 0.5851 11.00000 0.05 0.09 Q39 1 0.2551 -0.1084 0.3043 11.00000 0.05 0.09 Q40 1 0.6882 0.2745 0.5053 11.00000 0.05 0.09 Q41 1 0.6057 0.0304 0.4346 11.00000 0.05 0.09 Q42 1 0.3459 -0.1406 0.4928 11.00000 0.05 0.09 Q43 1 0.9254 0.5967 0.5308 11.00000 0.05 0.09 Q44 1 0.5260 0.3783 0.6835 11.00000 0.05 0.09 Q45 1 1.0216 0.7382 0.8816 11.00000 0.05 0.09 Q46 1 0.4292 0.5750 0.4936 11.00000 0.05 0.09 Q47 1 1.1135 0.3649 -0.0057 11.00000 0.05 0.09 Q48 1 0.5994 -0.1101 0.3883 11.00000 0.05 0.09 Q49 1 0.3042 0.5665 0.2309 11.00000 0.05 0.09 Q50 1 0.3382 0.4672 0.2206 11.00000 0.05 0.09 ; _shelx_res_checksum 74527 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O2 O 0.6059(3) 0.1902(2) 0.22557(17) 0.0755(6) Uani 1 1 d . . . . . O3 O 0.5109(3) 0.2097(3) 0.36443(19) 0.0833(7) Uani 1 1 d . . . . . O13 O 0.5828(3) 0.3782(3) 0.8858(2) 0.1035(9) Uani 1 1 d . . . . . O1 O 0.3874(3) 0.5635(3) 0.1975(2) 0.0997(8) Uani 1 1 d . . . . . O14 O 0.8683(3) 0.4295(3) 0.7981(2) 0.0942(8) Uani 1 1 d . . . . . O5 O 0.2885(3) 0.2297(3) 0.1489(2) 0.0998(8) Uani 1 1 d . . . . . O11 O 0.4749(2) 0.6236(3) 0.8215(2) 0.0868(7) Uani 1 1 d . . . . . N3 N 0.3040(3) 0.2903(3) 0.40266(19) 0.0684(6) Uani 1 1 d . . . . . H3 H 0.363508 0.276218 0.438411 0.082 Uiso 1 1 calc R U . . . N1 N 0.5818(2) 0.3892(2) 0.27286(18) 0.0610(5) Uani 1 1 d . . . . . O10 O 0.4019(3) 0.4598(3) 0.6809(2) 0.1019(9) Uani 1 1 d . . . . . O4 O 0.1483(3) 0.0993(3) 0.2548(2) 0.0957(8) Uani 1 1 d . . . . . O8 O 0.3223(3) 0.0254(3) 0.5388(2) 0.1044(9) Uani 1 1 d . . . . . O7 O 0.1593(3) 0.2148(3) 0.5126(2) 0.0901(7) Uani 1 1 d . . . . . O6 O 0.1055(3) 0.3275(4) 0.4039(3) 0.1080(10) Uani 1 1 d . . . . . N6 N 0.6390(3) 0.5802(3) 0.74807(18) 0.0644(6) Uani 1 1 d . . . . . N2 N 0.3335(3) 0.3236(3) 0.30992(19) 0.0676(6) Uani 1 1 d . . . . . N4 N 0.4594(3) 0.2307(3) 0.6389(2) 0.0763(7) Uani 1 1 d . . . . . H4A H 0.413240 0.265180 0.608181 0.092 Uiso 1 1 calc R U . . . C1 C 0.7866(3) 0.4561(3) 0.1690(2) 0.0626(6) Uani 1 1 d . . . . . C21 C 0.5619(3) 0.2558(3) 0.2938(2) 0.0633(7) Uani 1 1 d . . . . . N5 N 0.5572(3) 0.3155(3) 0.72152(19) 0.0724(7) Uani 1 1 d . . . . . C00L C 0.4957(3) 0.5481(4) 0.7449(3) 0.0734(8) Uani 1 1 d . . . . . O9 O 0.5096(4) 0.0408(4) 0.6339(4) 0.1383(16) Uani 1 1 d . . . . . O12 O 0.3881(4) 0.1715(3) 0.8062(2) 0.1215(12) Uani 1 1 d . . . . . C10 C 0.4676(4) 0.5123(4) 0.2092(3) 0.0767(8) Uani 1 1 d . . . . . C6 C 0.8222(3) 0.4666(4) 0.0750(2) 0.0711(7) Uani 1 1 d . . . . . H6 H 0.755851 0.462683 0.026686 0.085 Uiso 1 1 calc R U . . . C2 C 0.8875(4) 0.4609(4) 0.2402(2) 0.0734(8) Uani 1 1 d . . . . . H2 H 0.865433 0.453717 0.303507 0.088 Uiso 1 1 calc R U . . . C26 C 0.7705(3) 0.8400(3) 0.8396(2) 0.0706(7) Uani 1 1 d . . . . . C34 C 0.8088(3) 0.5043(4) 0.7916(3) 0.0719(7) Uani 1 1 d . . . . . C36 C 0.7208(4) 0.4658(5) 0.6132(3) 0.0833(9) Uani 1 1 d . . . . . H36 H 0.634034 0.438360 0.567954 0.100 Uiso 1 1 calc R U . . . C3 C 1.0191(4) 0.4761(5) 0.2167(3) 0.0869(10) Uani 1 1 d . . . . . H3A H 1.085330 0.477852 0.264122 0.104 Uiso 1 1 calc R U . . . C18 C 0.2578(4) 0.2163(4) 0.2295(3) 0.0787(9) Uani 1 1 d . . . . . C7 C 0.6489(3) 0.4506(3) 0.1932(2) 0.0626(6) Uani 1 1 d . . . . . C42 C 0.5119(4) 0.2936(4) 0.8121(3) 0.0872(10) Uani 1 1 d . . . . . C32 C 0.7541(3) 0.6917(3) 0.8146(2) 0.0653(7) Uani 1 1 d . . . . . C39 C 0.4371(5) 0.0922(5) 0.6068(3) 0.0938(11) Uani 1 1 d . . . . . C12 C 0.5391(4) 0.5614(3) 0.3922(3) 0.0782(9) Uani 1 1 d . . . . . H12 H 0.549102 0.513943 0.445491 0.094 Uiso 1 1 calc R U . . . C38 C 0.8359(6) 0.6211(6) 0.6039(4) 0.1176(16) Uani 1 1 d . . . . . H38A H 0.802934 0.689554 0.627175 0.176 Uiso 1 1 calc R U . . . H38B H 0.850908 0.624486 0.536953 0.176 Uiso 1 1 calc R U . . . H38C H 0.925942 0.646609 0.641914 0.176 Uiso 1 1 calc R U . . . C11 C 0.4744(3) 0.4424(3) 0.2991(2) 0.0635(6) Uani 1 1 d . . . . . C4 C 1.0537(4) 0.4890(5) 0.1234(3) 0.0901(10) Uani 1 1 d . . . . . H4 H 1.144071 0.501933 0.108234 0.108 Uiso 1 1 calc R U . . . C5 C 0.9543(4) 0.4826(5) 0.0529(3) 0.0846(9) Uani 1 1 d . . . . . H5 H 0.976890 0.489179 -0.010331 0.102 Uiso 1 1 calc R U . . . C31 C 0.7136(4) 0.8963(4) 0.7768(3) 0.0856(9) Uani 1 1 d . . . . . H31 H 0.658133 0.837287 0.718468 0.103 Uiso 1 1 calc R U . . . C35 C 0.6759(3) 0.4595(3) 0.7157(2) 0.0649(7) Uani 1 1 d . . . . . C15 C 0.1807(4) 0.2807(4) 0.4352(3) 0.0771(8) Uani 1 1 d . . . . . C14 C 0.6923(5) 0.6838(4) 0.3835(4) 0.1012(12) Uani 1 1 d . . . . . H14A H 0.754955 0.641946 0.369761 0.152 Uiso 1 1 calc R U . . . H14B H 0.730937 0.753016 0.443483 0.152 Uiso 1 1 calc R U . . . H14C H 0.686641 0.732833 0.331668 0.152 Uiso 1 1 calc R U . . . C27 C 0.8516(5) 0.9304(4) 0.9260(3) 0.0896(10) Uani 1 1 d . . . . . H27 H 0.889060 0.894047 0.970153 0.108 Uiso 1 1 calc R U . . . C13 C 0.4415(6) 0.6288(5) 0.4212(4) 0.1017(12) Uani 1 1 d . . . . . H13A H 0.430958 0.678125 0.370984 0.153 Uiso 1 1 calc R U . . . H13B H 0.485188 0.697848 0.481020 0.153 Uiso 1 1 calc R U . . . H13C H 0.347418 0.552553 0.429699 0.153 Uiso 1 1 calc R U . . . C33 C 0.8529(3) 0.6501(3) 0.8405(2) 0.0734(8) Uani 1 1 d . . . . . H33 H 0.937422 0.708134 0.883826 0.088 Uiso 1 1 calc R U . . . C22 C 0.5987(5) 0.0483(4) 0.2325(3) 0.0885(10) Uani 1 1 d . . . . . C8 C 0.5828(3) 0.5181(4) 0.1553(3) 0.0786(9) Uani 1 1 d . . . . . H8 H 0.608269 0.562752 0.101102 0.094 Uiso 1 1 calc R U . . . C28 C 0.8778(6) 1.0730(5) 0.9477(4) 0.1089(14) Uani 1 1 d . . . . . H28 H 0.934468 1.133203 1.005265 0.131 Uiso 1 1 calc R U . . . C37 C 0.7782(6) 0.3584(7) 0.5810(4) 0.1139(15) Uani 1 1 d . . . . . H37A H 0.784143 0.350559 0.512392 0.171 Uiso 1 1 calc R U . . . H37B H 0.713100 0.263691 0.595154 0.171 Uiso 1 1 calc R U . . . H37C H 0.873326 0.393914 0.615509 0.171 Uiso 1 1 calc R U . . . C29 C 0.8198(6) 1.1259(5) 0.8839(4) 0.1081(14) Uani 1 1 d . . . . . H29 H 0.836679 1.222004 0.898535 0.130 Uiso 1 1 calc R U . . . C01H C 0.3641(7) 0.7148(7) 0.9307(5) 0.143(2) Uani 1 1 d . . . . . H01A H 0.426329 0.813084 0.921064 0.214 Uiso 1 1 calc R U . . . H01B H 0.413208 0.690586 0.978819 0.214 Uiso 1 1 calc R U . . . H01C H 0.275776 0.707658 0.952308 0.214 Uiso 1 1 calc R U . . . C23 C 0.4431(6) -0.0678(5) 0.2181(5) 0.1225(17) Uani 1 1 d . . . . . H23A H 0.395847 -0.051516 0.271954 0.184 Uiso 1 1 calc R U . . . H23B H 0.437748 -0.162220 0.213950 0.184 Uiso 1 1 calc R U . . . H23C H 0.395346 -0.064573 0.158947 0.184 Uiso 1 1 calc R U . . . C01J C 0.2283(6) 0.4554(7) 0.8481(6) 0.138(2) Uani 1 1 d . . . . . H01D H 0.136500 0.447326 0.862909 0.208 Uiso 1 1 calc R U . . . H01E H 0.271234 0.432587 0.900656 0.208 Uiso 1 1 calc R U . . . H01F H 0.213024 0.388069 0.789411 0.208 Uiso 1 1 calc R U . . . C24 C 0.6726(8) 0.0297(7) 0.1431(5) 0.1277(18) Uani 1 1 d . . . . . H24A H 0.633202 0.051903 0.088424 0.192 Uiso 1 1 calc R U . . . H24B H 0.654985 -0.069661 0.128507 0.192 Uiso 1 1 calc R U . . . H24C H 0.775624 0.095225 0.156676 0.192 Uiso 1 1 calc R U . . . C25 C 0.6854(7) 0.0601(6) 0.3248(4) 0.1144(15) Uani 1 1 d . . . . . H25A H 0.780203 0.144718 0.331893 0.172 Uiso 1 1 calc R U . . . H25B H 0.695554 -0.026414 0.322427 0.172 Uiso 1 1 calc R U . . . H25C H 0.635996 0.069649 0.379237 0.172 Uiso 1 1 calc R U . . . C30 C 0.7374(6) 1.0379(5) 0.7988(4) 0.1036(12) Uani 1 1 d . . . . . H30 H 0.697460 1.073792 0.755945 0.124 Uiso 1 1 calc R U . . . C01N C 0.2742(7) 0.6526(8) 0.7520(6) 0.137(2) Uani 1 1 d . . . . . H01G H 0.344776 0.750385 0.746200 0.205 Uiso 1 1 calc R U . . . H01H H 0.183448 0.649896 0.763444 0.205 Uiso 1 1 calc R U . . . H01I H 0.259943 0.586389 0.692870 0.205 Uiso 1 1 calc R U . . . C01O C 0.3276(4) 0.6077(5) 0.8345(4) 0.1074(15) Uani 1 1 d . . . . . C16 C 0.0372(6) 0.2013(7) 0.5617(4) 0.1197(17) Uani 1 1 d . . . . . H16A H -0.047748 0.170628 0.515028 0.144 Uiso 1 1 calc R U . . . H16B H 0.059717 0.294241 0.601593 0.144 Uiso 1 1 calc R U . . . C19 C 0.0554(7) -0.0148(6) 0.1745(5) 0.139(2) Uani 1 1 d . . . . . H19A H 0.002170 0.020334 0.137134 0.166 Uiso 1 1 calc R U . . . H19B H 0.114955 -0.038240 0.132136 0.166 Uiso 1 1 calc R U . . . C40 C 0.2841(7) -0.1209(6) 0.4916(6) 0.143(2) Uani 1 1 d . . . . . H40A H 0.359416 -0.116868 0.452277 0.171 Uiso 1 1 calc R U . . . H40B H 0.278977 -0.179738 0.540433 0.171 Uiso 1 1 calc R U . . . C43 C 0.3360(9) 0.1411(8) 0.9035(6) 0.164(3) Uani 1 1 d . . . . . H43A H 0.407764 0.134185 0.945576 0.197 Uiso 1 1 calc R U . . . H43B H 0.318308 0.218391 0.935179 0.197 Uiso 1 1 calc R U . . . C41 C 0.1532(9) -0.1856(11) 0.4338(8) 0.197(4) Uani 1 1 d . . . . . H41A H 0.161755 -0.134687 0.380448 0.295 Uiso 1 1 calc R U . . . H41B H 0.080329 -0.181390 0.471207 0.295 Uiso 1 1 calc R U . . . H41C H 0.125535 -0.286188 0.409074 0.295 Uiso 1 1 calc R U . . . C17 C 0.0101(12) 0.0891(14) 0.6228(9) 0.216(5) Uani 1 1 d . . . . . H17A H -0.031095 -0.005870 0.582123 0.324 Uiso 1 1 calc R U . . . H17B H -0.056638 0.089754 0.667430 0.324 Uiso 1 1 calc R U . . . H17C H 0.100371 0.110623 0.658606 0.324 Uiso 1 1 calc R U . . . C44 C 0.2090(14) 0.0098(13) 0.8834(11) 0.231(6) Uani 1 1 d . . . . . H44A H 0.211736 -0.048135 0.824976 0.347 Uiso 1 1 calc R U . . . H44B H 0.127755 0.027614 0.874835 0.347 Uiso 1 1 calc R U . . . H44C H 0.198594 -0.042028 0.936487 0.347 Uiso 1 1 calc R U . . . C20 C -0.0406(10) -0.1377(7) 0.2055(8) 0.179(3) Uani 1 1 d . . . . . H20A H -0.078926 -0.219464 0.152447 0.268 Uiso 1 1 calc R U . . . H20B H -0.119012 -0.124317 0.228738 0.268 Uiso 1 1 calc R U . . . H20C H 0.008095 -0.156390 0.257129 0.268 Uiso 1 1 calc R 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 O2 0.0938(15) 0.0617(11) 0.0855(13) 0.0217(10) 0.0266(12) 0.0457(11) O3 0.1088(17) 0.0854(14) 0.0937(16) 0.0430(13) 0.0408(14) 0.0680(14) O13 0.1063(19) 0.0915(17) 0.0745(14) 0.0173(13) -0.0073(13) 0.0179(15) O1 0.0861(16) 0.1102(19) 0.138(2) 0.0562(17) 0.0137(15) 0.0673(15) O14 0.0868(16) 0.0903(16) 0.117(2) 0.0110(14) -0.0158(14) 0.0563(14) O5 0.0937(17) 0.1050(19) 0.0704(15) 0.0181(13) 0.0018(13) 0.0236(15) O11 0.0619(12) 0.0858(14) 0.1016(17) -0.0108(12) 0.0085(11) 0.0341(11) N3 0.0689(13) 0.0759(14) 0.0713(14) 0.0186(12) 0.0098(11) 0.0423(12) N1 0.0630(12) 0.0553(11) 0.0751(14) 0.0200(10) 0.0071(10) 0.0349(10) O10 0.0703(13) 0.1096(19) 0.116(2) -0.0316(16) -0.0256(13) 0.0524(14) O4 0.0825(15) 0.0780(14) 0.0897(16) 0.0143(12) 0.0018(12) 0.0099(12) O8 0.0819(15) 0.0928(17) 0.120(2) -0.0361(15) -0.0266(14) 0.0447(14) O7 0.0826(15) 0.1137(19) 0.0923(16) 0.0313(14) 0.0295(13) 0.0573(14) O6 0.0921(17) 0.141(3) 0.131(2) 0.052(2) 0.0282(17) 0.0806(19) N6 0.0570(12) 0.0709(13) 0.0683(13) 0.0098(11) -0.0011(10) 0.0347(11) N2 0.0629(13) 0.0694(14) 0.0700(14) 0.0163(11) 0.0070(11) 0.0306(11) N4 0.0729(15) 0.0742(15) 0.0746(15) -0.0082(12) -0.0153(12) 0.0375(13) C1 0.0531(13) 0.0592(14) 0.0745(17) 0.0180(12) 0.0007(12) 0.0253(11) C21 0.0691(16) 0.0587(14) 0.0767(17) 0.0233(13) 0.0148(14) 0.0392(13) N5 0.0679(14) 0.0671(14) 0.0697(15) 0.0072(11) -0.0068(11) 0.0250(11) C00L 0.0603(16) 0.0800(19) 0.0820(19) 0.0032(16) 0.0005(14) 0.0394(15) O9 0.124(3) 0.0906(19) 0.193(4) -0.017(2) -0.056(3) 0.063(2) O12 0.108(2) 0.0880(18) 0.104(2) 0.0214(15) 0.0055(17) -0.0045(16) C10 0.0647(16) 0.0744(17) 0.101(2) 0.0315(16) 0.0009(15) 0.0384(14) C6 0.0656(16) 0.0765(18) 0.0696(17) 0.0180(14) -0.0012(13) 0.0327(14) C2 0.0685(17) 0.0803(19) 0.0759(18) 0.0196(15) 0.0006(14) 0.0388(15) C26 0.0687(17) 0.0696(16) 0.0753(18) 0.0177(14) 0.0091(14) 0.0336(14) C34 0.0642(15) 0.0732(17) 0.0812(18) 0.0172(15) -0.0068(14) 0.0360(14) C36 0.078(2) 0.104(2) 0.0723(19) 0.0100(17) 0.0097(16) 0.0497(19) C3 0.0678(18) 0.104(2) 0.094(2) 0.0178(19) -0.0104(16) 0.0470(18) C18 0.0711(18) 0.0723(18) 0.079(2) 0.0127(15) -0.0002(16) 0.0248(15) C7 0.0563(13) 0.0603(14) 0.0697(16) 0.0175(12) 0.0012(12) 0.0261(11) C42 0.084(2) 0.0724(19) 0.079(2) 0.0138(16) -0.0080(17) 0.0178(16) C32 0.0617(15) 0.0674(16) 0.0655(16) 0.0148(13) 0.0031(12) 0.0298(13) C39 0.083(2) 0.082(2) 0.109(3) -0.015(2) -0.018(2) 0.0450(19) C12 0.0793(19) 0.0596(16) 0.100(2) 0.0071(15) -0.0002(17) 0.0399(15) C38 0.110(3) 0.132(4) 0.095(3) 0.034(3) 0.036(3) 0.041(3) C11 0.0627(14) 0.0595(14) 0.0791(18) 0.0183(13) 0.0056(13) 0.0370(12) C4 0.0656(18) 0.110(3) 0.097(3) 0.019(2) 0.0122(17) 0.0436(19) C5 0.0722(19) 0.097(2) 0.084(2) 0.0197(18) 0.0129(16) 0.0392(17) C31 0.083(2) 0.079(2) 0.097(2) 0.0218(18) 0.0072(18) 0.0389(17) C35 0.0622(15) 0.0708(16) 0.0648(16) 0.0086(13) 0.0007(12) 0.0361(13) C15 0.0655(17) 0.083(2) 0.088(2) 0.0177(16) 0.0127(15) 0.0391(15) C14 0.089(2) 0.0661(19) 0.132(3) 0.000(2) -0.007(2) 0.0304(18) C27 0.106(3) 0.0749(19) 0.082(2) 0.0084(16) -0.0003(19) 0.0416(19) C13 0.115(3) 0.076(2) 0.131(3) 0.006(2) 0.011(3) 0.064(2) C33 0.0599(15) 0.0712(17) 0.0821(19) 0.0125(14) -0.0123(14) 0.0282(13) C22 0.106(3) 0.0643(17) 0.113(3) 0.0161(17) 0.026(2) 0.0544(18) C8 0.0643(16) 0.084(2) 0.096(2) 0.0431(18) 0.0077(16) 0.0367(15) C28 0.133(4) 0.077(2) 0.103(3) -0.007(2) 0.011(3) 0.045(2) C37 0.106(3) 0.144(4) 0.111(3) -0.005(3) 0.017(2) 0.083(3) C29 0.131(4) 0.079(2) 0.122(4) 0.016(2) 0.027(3) 0.056(3) C01H 0.118(4) 0.134(4) 0.164(5) -0.028(4) 0.040(4) 0.063(3) C23 0.123(4) 0.065(2) 0.167(5) 0.016(3) 0.023(3) 0.037(2) C01J 0.081(3) 0.116(4) 0.203(6) 0.011(4) 0.051(3) 0.037(3) C24 0.162(5) 0.110(3) 0.136(4) 0.000(3) 0.041(4) 0.089(4) C25 0.149(4) 0.111(3) 0.129(4) 0.031(3) 0.014(3) 0.098(3) C30 0.116(3) 0.095(3) 0.122(3) 0.039(3) 0.020(3) 0.063(2) C01N 0.107(3) 0.143(4) 0.180(5) -0.004(4) -0.002(4) 0.087(4) C01O 0.069(2) 0.104(3) 0.148(4) -0.010(3) 0.018(2) 0.049(2) C16 0.099(3) 0.156(5) 0.113(3) 0.027(3) 0.046(3) 0.065(3) C19 0.126(4) 0.094(3) 0.121(4) 0.002(3) -0.018(3) -0.001(3) C40 0.129(4) 0.093(3) 0.177(5) -0.051(3) -0.036(4) 0.055(3) C43 0.166(6) 0.122(5) 0.143(5) 0.055(4) 0.034(4) 0.012(4) C41 0.129(5) 0.165(7) 0.196(8) -0.078(6) -0.014(5) 0.022(5) C17 0.201(9) 0.239(10) 0.255(11) 0.129(9) 0.156(9) 0.111(8) C44 0.197(9) 0.192(9) 0.253(12) 0.068(9) 0.112(9) 0.037(8) C20 0.155(6) 0.092(4) 0.215(8) 0.029(4) -0.013(5) 0.003(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0137 0.0067 '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 0.0241 0.0134 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0389 0.0241 '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 C21 O2 C22 121.0(3) . . ? C00L O11 C01O 121.5(3) . . ? N2 N3 H3 120.5 . . ? C15 N3 H3 120.5 . . ? C15 N3 N2 119.1(3) . . ? C21 N1 C7 124.5(2) . . ? C21 N1 C11 120.2(2) . . ? C7 N1 C11 109.1(2) . . ? C18 O4 C19 114.8(4) . . ? C39 O8 C40 116.9(4) . . ? C15 O7 C16 116.4(3) . . ? C00L N6 C32 125.4(3) . . ? C00L N6 C35 119.7(2) . . ? C32 N6 C35 109.0(2) . . ? N3 N2 C11 119.0(2) . . ? C18 N2 N3 119.1(2) . . ? C18 N2 C11 117.4(3) . . ? N5 N4 H4A 120.2 . . ? C39 N4 H4A 120.2 . . ? C39 N4 N5 119.5(3) . . ? C6 C1 C2 118.7(3) . . ? C6 C1 C7 119.7(2) . . ? C2 C1 C7 121.4(3) . . ? O2 C21 N1 110.8(2) . . ? O3 C21 O2 126.3(2) . . ? O3 C21 N1 123.0(3) . . ? N4 N5 C35 119.2(3) . . ? C42 N5 N4 118.9(3) . . ? C42 N5 C35 116.9(3) . . ? O11 C00L N6 111.3(3) . . ? O10 C00L O11 125.5(3) . . ? O10 C00L N6 123.1(3) . . ? C42 O12 C43 113.7(4) . . ? O1 C10 C11 123.2(3) . . ? O1 C10 C8 129.5(3) . . ? C8 C10 C11 106.8(2) . . ? C1 C6 H6 119.8 . . ? C5 C6 C1 120.5(3) . . ? C5 C6 H6 119.8 . . ? C1 C2 H2 120.0 . . ? C3 C2 C1 120.1(3) . . ? C3 C2 H2 120.0 . . ? C31 C26 C32 122.0(3) . . ? C31 C26 C27 118.0(3) . . ? C27 C26 C32 119.9(3) . . ? O14 C34 C35 123.6(3) . . ? O14 C34 C33 129.0(3) . . ? C33 C34 C35 107.1(2) . . ? C38 C36 H36 107.7 . . ? C38 C36 C37 109.0(4) . . ? C35 C36 H36 107.7 . . ? C35 C36 C38 111.7(3) . . ? C35 C36 C37 112.9(4) . . ? C37 C36 H36 107.7 . . ? C2 C3 H3A 119.8 . . ? C2 C3 C4 120.4(3) . . ? C4 C3 H3A 119.8 . . ? O5 C18 O4 126.2(3) . . ? O5 C18 N2 123.2(3) . . ? O4 C18 N2 110.6(3) . . ? N1 C7 C1 121.7(2) . . ? C8 C7 N1 110.9(3) . . ? C8 C7 C1 126.7(3) . . ? O13 C42 N5 121.9(3) . . ? O13 C42 O12 126.3(4) . . ? O12 C42 N5 111.7(3) . . ? N6 C32 C26 122.0(3) . . ? C33 C32 N6 111.2(3) . . ? C33 C32 C26 126.2(3) . . ? O8 C39 N4 108.0(3) . . ? O9 C39 O8 125.9(4) . . ? O9 C39 N4 126.1(3) . . ? C11 C12 H12 107.2 . . ? C14 C12 H12 107.2 . . ? C14 C12 C11 111.7(3) . . ? C13 C12 H12 107.2 . . ? C13 C12 C11 113.5(3) . . ? C13 C12 C14 109.7(3) . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38B 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N1 C11 C10 100.6(2) . . ? N1 C11 C12 109.7(2) . . ? N2 C11 N1 112.3(2) . . ? N2 C11 C10 112.1(2) . . ? N2 C11 C12 111.4(3) . . ? C12 C11 C10 110.2(2) . . ? C3 C4 H4 120.1 . . ? C5 C4 C3 119.7(3) . . ? C5 C4 H4 120.1 . . ? C6 C5 C4 120.6(4) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C26 C31 H31 119.4 . . ? C30 C31 C26 121.1(4) . . ? C30 C31 H31 119.4 . . ? N6 C35 C34 100.6(2) . . ? N6 C35 C36 110.4(3) . . ? N5 C35 N6 112.1(2) . . ? N5 C35 C34 111.3(2) . . ? N5 C35 C36 111.4(3) . . ? C36 C35 C34 110.5(3) . . ? O7 C15 N3 107.7(3) . . ? O6 C15 N3 127.2(3) . . ? O6 C15 O7 125.1(3) . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C26 C27 H27 119.5 . . ? C28 C27 C26 121.1(4) . . ? C28 C27 H27 119.5 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C34 C33 H33 124.9 . . ? C32 C33 C34 110.3(3) . . ? C32 C33 H33 124.9 . . ? O2 C22 C23 109.0(3) . . ? O2 C22 C24 99.8(3) . . ? O2 C22 C25 110.6(3) . . ? C23 C22 C24 109.9(5) . . ? C23 C22 C25 115.2(4) . . ? C25 C22 C24 111.2(4) . . ? C10 C8 H8 124.4 . . ? C7 C8 C10 111.1(3) . . ? C7 C8 H8 124.4 . . ? C27 C28 H28 120.2 . . ? C29 C28 C27 119.7(4) . . ? C29 C28 H28 120.2 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37B 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C28 C29 H29 119.9 . . ? C30 C29 C28 120.3(4) . . ? C30 C29 H29 119.9 . . ? H01A C01H H01B 109.5 . . ? H01A C01H H01C 109.5 . . ? H01B C01H H01C 109.5 . . ? C01O C01H H01A 109.5 . . ? C01O C01H H01B 109.5 . . ? C01O C01H H01C 109.5 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? H01D C01J H01E 109.5 . . ? H01D C01J H01F 109.5 . . ? H01E C01J H01F 109.5 . . ? C01O C01J H01D 109.5 . . ? C01O C01J H01E 109.5 . . ? C01O C01J H01F 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C31 C30 H30 120.1 . . ? C29 C30 C31 119.9(4) . . ? C29 C30 H30 120.1 . . ? H01G C01N H01H 109.5 . . ? H01G C01N H01I 109.5 . . ? H01H C01N H01I 109.5 . . ? C01O C01N H01G 109.5 . . ? C01O C01N H01H 109.5 . . ? C01O C01N H01I 109.5 . . ? O11 C01O C01H 100.3(4) . . ? C01J C01O O11 109.1(4) . . ? C01J C01O C01H 109.9(6) . . ? C01N C01O O11 109.9(4) . . ? C01N C01O C01H 112.8(5) . . ? C01N C01O C01J 114.0(5) . . ? O7 C16 H16A 110.6 . . ? O7 C16 H16B 110.6 . . ? O7 C16 C17 105.7(5) . . ? H16A C16 H16B 108.7 . . ? C17 C16 H16A 110.6 . . ? C17 C16 H16B 110.6 . . ? O4 C19 H19A 109.3 . . ? O4 C19 H19B 109.3 . . ? H19A C19 H19B 108.0 . . ? C20 C19 O4 111.6(6) . . ? C20 C19 H19A 109.3 . . ? C20 C19 H19B 109.3 . . ? O8 C40 H40A 109.4 . . ? O8 C40 H40B 109.4 . . ? H40A C40 H40B 108.0 . . ? C41 C40 O8 111.4(6) . . ? C41 C40 H40A 109.4 . . ? C41 C40 H40B 109.4 . . ? O12 C43 H43A 110.6 . . ? O12 C43 H43B 110.6 . . ? H43A C43 H43B 108.8 . . ? C44 C43 O12 105.5(7) . . ? C44 C43 H43A 110.6 . . ? C44 C43 H43B 110.6 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41B 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44B 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O2 C21 1.326(4) . ? O2 C22 1.474(4) . ? O3 C21 1.197(4) . ? O13 C42 1.209(5) . ? O1 C10 1.209(4) . ? O14 C34 1.221(4) . ? O5 C18 1.196(4) . ? O11 C00L 1.332(4) . ? O11 C01O 1.496(4) . ? N3 H3 0.8600 . ? N3 N2 1.400(4) . ? N3 C15 1.354(4) . ? N1 C21 1.391(3) . ? N1 C7 1.412(4) . ? N1 C11 1.513(4) . ? O10 C00L 1.208(4) . ? O4 C18 1.335(4) . ? O4 C19 1.442(6) . ? O8 C39 1.328(5) . ? O8 C40 1.441(6) . ? O7 C15 1.335(5) . ? O7 C16 1.437(5) . ? O6 C15 1.203(4) . ? N6 C00L 1.373(4) . ? N6 C32 1.400(4) . ? N6 C35 1.511(4) . ? N2 C18 1.376(4) . ? N2 C11 1.448(4) . ? N4 H4A 0.8600 . ? N4 N5 1.389(4) . ? N4 C39 1.364(5) . ? C1 C6 1.388(5) . ? C1 C2 1.398(4) . ? C1 C7 1.474(4) . ? N5 C42 1.384(5) . ? N5 C35 1.453(4) . ? O9 C39 1.196(5) . ? O12 C42 1.314(5) . ? O12 C43 1.509(8) . ? C10 C11 1.557(5) . ? C10 C8 1.434(5) . ? C6 H6 0.9300 . ? C6 C5 1.370(5) . ? C2 H2 0.9300 . ? C2 C3 1.372(5) . ? C26 C32 1.474(5) . ? C26 C31 1.380(5) . ? C26 C27 1.384(5) . ? C34 C35 1.549(4) . ? C34 C33 1.429(5) . ? C36 H36 0.9800 . ? C36 C38 1.534(7) . ? C36 C35 1.531(5) . ? C36 C37 1.537(6) . ? C3 H3A 0.9300 . ? C3 C4 1.379(6) . ? C7 C8 1.340(4) . ? C32 C33 1.352(4) . ? C12 H12 0.9800 . ? C12 C11 1.546(5) . ? C12 C14 1.537(6) . ? C12 C13 1.534(5) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C4 H4 0.9300 . ? C4 C5 1.372(6) . ? C5 H5 0.9300 . ? C31 H31 0.9300 . ? C31 C30 1.374(6) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C27 H27 0.9300 . ? C27 C28 1.375(6) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C33 H33 0.9300 . ? C22 C23 1.488(7) . ? C22 C24 1.538(7) . ? C22 C25 1.501(7) . ? C8 H8 0.9300 . ? C28 H28 0.9300 . ? C28 C29 1.371(8) . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C29 H29 0.9300 . ? C29 C30 1.367(8) . ? C01H H01A 0.9600 . ? C01H H01B 0.9600 . ? C01H H01C 0.9600 . ? C01H C01O 1.533(8) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C01J H01D 0.9600 . ? C01J H01E 0.9600 . ? C01J H01F 0.9600 . ? C01J C01O 1.487(8) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C30 H30 0.9300 . ? C01N H01G 0.9600 . ? C01N H01H 0.9600 . ? C01N H01I 0.9600 . ? C01N C01O 1.486(9) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 C17 1.479(12) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 C20 1.355(10) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C40 C41 1.367(10) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C43 C44 1.372(13) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? 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 O1 C10 C11 N1 176.4(3) . . . . ? O1 C10 C11 N2 56.8(4) . . . . ? O1 C10 C11 C12 -67.9(4) . . . . ? O1 C10 C8 C7 178.3(4) . . . . ? O14 C34 C35 N6 173.9(3) . . . . ? O14 C34 C35 N5 54.9(4) . . . . ? O14 C34 C35 C36 -69.5(4) . . . . ? O14 C34 C33 C32 -178.4(4) . . . . ? N3 N2 C18 O5 -170.4(3) . . . . ? N3 N2 C18 O4 9.8(4) . . . . ? N3 N2 C11 N1 94.1(3) . . . . ? N3 N2 C11 C10 -153.5(3) . . . . ? N3 N2 C11 C12 -29.4(3) . . . . ? N1 C7 C8 C10 2.2(4) . . . . ? N6 C32 C33 C34 -0.1(4) . . . . ? N2 N3 C15 O7 165.4(3) . . . . ? N2 N3 C15 O6 -17.4(6) . . . . ? N4 N5 C42 O13 -168.1(4) . . . . ? N4 N5 C42 O12 13.3(5) . . . . ? N4 N5 C35 N6 95.5(3) . . . . ? N4 N5 C35 C34 -152.6(3) . . . . ? N4 N5 C35 C36 -28.7(4) . . . . ? C1 C6 C5 C4 -0.2(6) . . . . ? C1 C2 C3 C4 0.9(6) . . . . ? C1 C7 C8 C10 -168.5(3) . . . . ? C21 O2 C22 C23 69.5(5) . . . . ? C21 O2 C22 C24 -175.4(4) . . . . ? C21 O2 C22 C25 -58.2(5) . . . . ? C21 N1 C7 C1 -46.1(4) . . . . ? C21 N1 C7 C8 142.6(3) . . . . ? C21 N1 C11 N2 -22.2(4) . . . . ? C21 N1 C11 C10 -141.6(3) . . . . ? C21 N1 C11 C12 102.2(3) . . . . ? N5 N4 C39 O8 169.1(3) . . . . ? N5 N4 C39 O9 -12.1(8) . . . . ? C00L O11 C01O C01H 179.9(5) . . . . ? C00L O11 C01O C01J 64.6(6) . . . . ? C00L O11 C01O C01N -61.1(5) . . . . ? C00L N6 C32 C26 -44.3(4) . . . . ? C00L N6 C32 C33 143.8(3) . . . . ? C00L N6 C35 N5 -23.2(4) . . . . ? C00L N6 C35 C34 -141.6(3) . . . . ? C00L N6 C35 C36 101.6(3) . . . . ? C6 C1 C2 C3 0.2(5) . . . . ? C6 C1 C7 N1 157.0(3) . . . . ? C6 C1 C7 C8 -33.2(5) . . . . ? C2 C1 C6 C5 -0.6(5) . . . . ? C2 C1 C7 N1 -27.4(4) . . . . ? C2 C1 C7 C8 142.4(4) . . . . ? C2 C3 C4 C5 -1.7(6) . . . . ? C26 C32 C33 C34 -171.6(3) . . . . ? C26 C31 C30 C29 0.6(7) . . . . ? C26 C27 C28 C29 1.6(8) . . . . ? C3 C4 C5 C6 1.3(6) . . . . ? C18 O4 C19 C20 171.6(7) . . . . ? C18 N2 C11 N1 -61.9(3) . . . . ? C18 N2 C11 C10 50.5(4) . . . . ? C18 N2 C11 C12 174.5(3) . . . . ? C7 N1 C21 O2 -4.0(4) . . . . ? C7 N1 C21 O3 176.4(3) . . . . ? C7 N1 C11 N2 131.3(3) . . . . ? C7 N1 C11 C10 12.0(3) . . . . ? C7 N1 C11 C12 -104.2(3) . . . . ? C7 C1 C6 C5 175.2(3) . . . . ? C7 C1 C2 C3 -175.5(3) . . . . ? C42 N5 C35 N6 -59.1(4) . . . . ? C42 N5 C35 C34 52.8(4) . . . . ? C42 N5 C35 C36 176.7(3) . . . . ? C42 O12 C43 C44 -178.8(9) . . . . ? C32 N6 C00L O11 -8.3(5) . . . . ? C32 N6 C00L O10 173.1(3) . . . . ? C32 N6 C35 N5 131.1(2) . . . . ? C32 N6 C35 C34 12.7(3) . . . . ? C32 N6 C35 C36 -104.1(3) . . . . ? C32 C26 C31 C30 -176.1(4) . . . . ? C32 C26 C27 C28 175.0(4) . . . . ? C39 O8 C40 C41 171.2(7) . . . . ? C39 N4 N5 C42 -81.2(5) . . . . ? C39 N4 N5 C35 124.7(4) . . . . ? C38 C36 C35 N6 49.4(4) . . . . ? C38 C36 C35 N5 174.6(4) . . . . ? C38 C36 C35 C34 -61.0(4) . . . . ? C11 N1 C21 O2 145.3(3) . . . . ? C11 N1 C21 O3 -34.3(4) . . . . ? C11 N1 C7 C1 161.7(2) . . . . ? C11 N1 C7 C8 -9.6(4) . . . . ? C11 N2 C18 O5 -14.4(5) . . . . ? C11 N2 C18 O4 165.8(3) . . . . ? C11 C10 C8 C7 5.8(4) . . . . ? C31 C26 C32 N6 -25.3(5) . . . . ? C31 C26 C32 C33 145.4(4) . . . . ? C31 C26 C27 C28 -1.5(6) . . . . ? C35 N6 C00L O11 141.4(3) . . . . ? C35 N6 C00L O10 -37.1(5) . . . . ? C35 N6 C32 C26 163.2(3) . . . . ? C35 N6 C32 C33 -8.7(3) . . . . ? C35 N5 C42 O13 -13.4(6) . . . . ? C35 N5 C42 O12 168.0(4) . . . . ? C35 C34 C33 C32 8.5(4) . . . . ? C15 N3 N2 C18 -75.9(4) . . . . ? C15 N3 N2 C11 128.5(3) . . . . ? C15 O7 C16 C17 163.3(7) . . . . ? C14 C12 C11 N1 51.9(3) . . . . ? C14 C12 C11 N2 176.9(3) . . . . ? C14 C12 C11 C10 -58.0(4) . . . . ? C27 C26 C32 N6 158.3(3) . . . . ? C27 C26 C32 C33 -31.1(5) . . . . ? C27 C26 C31 C30 0.4(6) . . . . ? C27 C28 C29 C30 -0.5(8) . . . . ? C13 C12 C11 N1 176.5(3) . . . . ? C13 C12 C11 N2 -58.4(4) . . . . ? C13 C12 C11 C10 66.7(4) . . . . ? C33 C34 C35 N6 -12.5(3) . . . . ? C33 C34 C35 N5 -131.5(3) . . . . ? C33 C34 C35 C36 104.2(3) . . . . ? C22 O2 C21 O3 -1.6(5) . . . . ? C22 O2 C21 N1 178.7(3) . . . . ? C8 C10 C11 N1 -10.5(3) . . . . ? C8 C10 C11 N2 -130.0(3) . . . . ? C8 C10 C11 C12 105.3(3) . . . . ? C28 C29 C30 C31 -0.6(8) . . . . ? C37 C36 C35 N6 172.7(3) . . . . ? C37 C36 C35 N5 -62.1(4) . . . . ? C37 C36 C35 C34 62.3(4) . . . . ? C01O O11 C00L O10 -1.6(6) . . . . ? C01O O11 C00L N6 179.9(4) . . . . ? C16 O7 C15 N3 176.6(4) . . . . ? C16 O7 C15 O6 -0.7(6) . . . . ? C19 O4 C18 O5 -4.4(7) . . . . ? C19 O4 C18 N2 175.3(5) . . . . ? C40 O8 C39 N4 177.0(5) . . . . ? C40 O8 C39 O9 -1.8(9) . . . . ? C43 O12 C42 O13 0.1(8) . . . . ? C43 O12 C42 N5 178.6(5) . . . . ?