#------------------------------------------------------------------------------ #$Date: 2021-07-29 04:49:56 +0300 (Thu, 29 Jul 2021) $ #$Revision: 267793 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/42/1564259.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_1564259 loop_ _publ_author_name 'Jia, Xiangqing' 'Nitsch, J\"orn' 'Wu, Zhu' 'Friedrich, Alexandra' 'Krebs, Johannes' 'Krummenacher, Ivo' 'Fantuzzi, Felipe' 'Braunschweig, Holger' 'Moos, Michael' 'Lambert, Christoph' 'Engels, Bernd' 'Marder, Todd B.' _publ_section_title ; One- and Two-Electron Reduction of Triarylborane-Based Helical Donor-Acceptor Compounds ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D1SC02409D _journal_year 2021 _chemical_formula_moiety 'C54 H48 B N, C12 H24 K O6' _chemical_formula_sum 'C66 H72 B K N O6' _chemical_formula_weight 1025.15 _chemical_name_systematic '13-(dimesitylboryl)-N,N-di-p-tolyldibenzo[c,g]phenanthren-8-amine (3-B(Mes)2-[5]helix-12-N(p-Tol)2) monoanion' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2020-11-13 deposited with the CCDC. 2021-07-27 downloaded from the CCDC. ; _cell_angle_alpha 73.438(9) _cell_angle_beta 86.260(12) _cell_angle_gamma 86.518(8) _cell_formula_units_Z 2 _cell_length_a 8.842(3) _cell_length_b 13.762(6) _cell_length_c 24.038(12) _cell_measurement_reflns_used 6206 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 20.95 _cell_measurement_theta_min 2.31 _cell_volume 2795(2) _computing_cell_refinement 'Saint+ ver. V8.37A (Bruker AXS)' _computing_data_collection 'APEX2 ver. 2014.9 (Bruker AXS)' _computing_data_reduction 'Saint+ ver. V8.37A (Bruker AXS)' _computing_molecular_graphics 'ShelXLe (Huebschle et all, 2011)' _computing_publication_material 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT (Sheldrick, 2014)' _diffrn_ambient_temperature 100(2) _diffrn_detector 'CCD area detector (APEX2 CCD)' _diffrn_detector_area_resol_mean 10.24 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker X8-APEX II' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator 'multi-layer mirror' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1598 _diffrn_reflns_av_unetI/netI 0.1156 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_number 99934 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 26.000 _diffrn_reflns_theta_max 26.403 _diffrn_reflns_theta_min 2.311 _diffrn_source 'rotating-anode (Nonius FR-591)' _exptl_absorpt_coefficient_mu 0.148 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.7003 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SadAbs 2016/2 (Bruker AXS)' _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.218 _exptl_crystal_description needle _exptl_crystal_F_000 1094 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Tetrahydrofuran' _exptl_crystal_size_max 0.216 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.059 _refine_diff_density_max 0.248 _refine_diff_density_min -0.254 _refine_diff_density_rms 0.057 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 684 _refine_ls_number_reflns 11400 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.996 _refine_ls_R_factor_all 0.1467 _refine_ls_R_factor_gt 0.0580 _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^)+(0.0422P)^2^+0.9681P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1019 _refine_ls_wR_factor_ref 0.1311 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5926 _reflns_number_total 11400 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1sc02409d2.cif _cod_data_source_block cmpd_2K1 _cod_database_code 1564259 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.969 _shelx_estimated_absorpt_t_max 0.991 _shelx_res_file ; JoKr014_XiJi_a.res created by SHELXL-2014/7 TITL JoKr014_XiJi_a.res in P-1 REM Old TITL JoKr014_XiJi in P-1 REM SHELXT solution in P-1 REM R1 0.209, Rweak 0.029, Alpha 0.084, Orientation as input REM Formula found by SHELXT: C67 N2 O5 K CELL 0.71073 8.8417 13.7617 24.0378 73.438 86.260 86.518 ZERR 2.000 0.0034 0.0064 0.0124 0.009 0.012 0.008 LATT 1 SFAC C H B N O K UNIT 132 144 2 2 12 2 TEMP -173.000 SIZE 0.059 0.09 0.216 L.S. 10 CONF OMIT 0 0 1 OMIT 0 1 0 OMIT 0 -1 1 OMIT 0 1 2 BOND $H LIST 4 ACTA 52 FMAP 2 PLAN 2 REM ##### WGHT 0.042200 0.968100 FVAR 0.38724 RESI 1 MAIN N1 4 0.391618 0.742910 0.458791 11.00000 0.04450 0.03160 = 0.02506 -0.01702 0.00505 -0.00663 B2 3 0.605545 0.503961 0.178231 11.00000 0.02171 0.01952 = 0.02320 -0.01015 -0.00580 -0.00239 C3 1 0.449660 0.797255 0.402827 11.00000 0.03394 0.03044 = 0.02533 -0.01448 0.00213 -0.00804 C4 1 0.555044 0.749065 0.371193 11.00000 0.03519 0.02074 = 0.02482 -0.00703 -0.00240 -0.00044 AFIX 43 H4 2 0.587624 0.680403 0.387857 11.00000 -1.20000 AFIX 0 C5 1 0.610531 0.800222 0.316897 11.00000 0.02628 0.01931 = 0.02757 -0.01195 -0.00170 -0.00085 AFIX 43 H5 2 0.678894 0.765353 0.296280 11.00000 -1.20000 AFIX 0 C6 1 0.569210 0.903838 0.290341 11.00000 0.02232 0.01853 = 0.02962 -0.01346 -0.00377 -0.00052 C7 1 0.477870 0.954194 0.325331 11.00000 0.02720 0.02336 = 0.03008 -0.01444 -0.00355 -0.00216 C8 1 0.415207 0.898928 0.379762 11.00000 0.03016 0.02902 = 0.03186 -0.01935 0.00217 0.00068 AFIX 43 H8 2 0.347366 0.932901 0.401050 11.00000 -1.20000 AFIX 0 C9 1 0.625251 0.961139 0.233220 11.00000 0.02132 0.02024 = 0.02680 -0.00926 -0.00302 -0.00348 C10 1 0.623507 1.068589 0.221697 11.00000 0.02350 0.01571 = 0.03290 -0.00885 -0.00782 -0.00280 C11 1 0.535609 1.116693 0.259283 11.00000 0.03149 0.01562 = 0.04116 -0.01305 -0.00418 -0.00029 AFIX 43 H11 2 0.531492 1.188617 0.250313 11.00000 -1.20000 AFIX 0 C12 1 0.458841 1.062610 0.306909 11.00000 0.03019 0.02435 = 0.03939 -0.01808 -0.00472 0.00695 AFIX 43 H01D 2 0.391571 1.096335 0.328515 11.00000 -1.20000 AFIX 0 C13 1 0.690811 0.917241 0.188134 11.00000 0.01685 0.01702 = 0.02499 -0.00562 -0.00371 0.00162 C14 1 0.791152 0.978365 0.144973 11.00000 0.02496 0.01708 = 0.02676 -0.00444 -0.00386 -0.00544 C15 1 0.796037 1.083141 0.138611 11.00000 0.02995 0.01933 = 0.03706 -0.00408 -0.00350 -0.00894 AFIX 43 H01E 2 0.863095 1.122955 0.109735 11.00000 -1.20000 AFIX 0 C16 1 0.706129 1.128347 0.173209 11.00000 0.03074 0.01194 = 0.04141 -0.00733 -0.00566 -0.00317 AFIX 43 H16 2 0.699207 1.200221 0.164601 11.00000 -1.20000 AFIX 0 C17 1 0.655529 0.820519 0.181802 11.00000 0.01928 0.01589 = 0.02199 -0.00521 -0.00363 -0.00044 C18 1 0.743919 0.777873 0.141953 11.00000 0.01551 0.01871 = 0.01970 -0.00420 -0.00354 -0.00032 C19 1 0.858199 0.837511 0.105111 11.00000 0.02268 0.02300 = 0.02510 -0.00683 0.00038 0.00031 AFIX 43 H19 2 0.921481 0.808815 0.079873 11.00000 -1.20000 AFIX 0 C20 1 0.877728 0.934021 0.105581 11.00000 0.02289 0.02238 = 0.02856 -0.00210 0.00040 -0.00385 AFIX 43 H20 2 0.950636 0.973051 0.079116 11.00000 -1.20000 AFIX 0 C21 1 0.528511 0.762735 0.210385 11.00000 0.01974 0.02357 = 0.02138 -0.01084 -0.00127 0.00027 AFIX 43 H21 2 0.456789 0.791508 0.233028 11.00000 -1.20000 AFIX 0 C22 1 0.507673 0.668077 0.206053 11.00000 0.01982 0.02125 = 0.02045 -0.00886 -0.00026 -0.00542 AFIX 43 H22 2 0.420932 0.633932 0.225733 11.00000 -1.20000 AFIX 0 C23 1 0.609644 0.616400 0.173296 11.00000 0.02006 0.01951 = 0.02281 -0.00917 0.00015 -0.00202 C24 1 0.719893 0.680995 0.138770 11.00000 0.02196 0.01723 = 0.02022 -0.00843 -0.00341 0.00395 AFIX 43 H24 2 0.781704 0.656178 0.111521 11.00000 -1.20000 AFIX 0 RESI 0 RESI 2 MES C1 1 0.489493 0.435186 0.225043 11.00000 0.02304 0.01481 = 0.02731 -0.00926 0.00261 0.00378 C2 1 0.384143 0.376156 0.208656 11.00000 0.02292 0.01272 = 0.02858 -0.00770 -0.00048 0.00274 C3 1 0.277937 0.321198 0.248971 11.00000 0.02518 0.01857 = 0.03976 -0.00837 0.00410 -0.00270 AFIX 43 H3 2 0.206376 0.284550 0.236150 11.00000 -1.20000 AFIX 0 C4 1 0.273385 0.318305 0.306947 11.00000 0.03174 0.01913 = 0.03571 -0.00381 0.00932 0.00007 C5 1 0.381412 0.370969 0.324383 11.00000 0.04066 0.02768 = 0.02335 -0.00718 0.00342 0.00147 AFIX 43 H5 2 0.384000 0.367367 0.364371 11.00000 -1.20000 AFIX 0 C6 1 0.486221 0.428992 0.284925 11.00000 0.02637 0.02096 = 0.02655 -0.00757 0.00045 0.00039 C7 1 0.383572 0.369065 0.147022 11.00000 0.02303 0.02090 = 0.03420 -0.01244 0.00022 -0.00391 AFIX 137 H00C 2 0.414717 0.433336 0.119911 11.00000 -1.50000 H00D 2 0.281167 0.355258 0.138815 11.00000 -1.50000 H00E 2 0.454462 0.314007 0.142409 11.00000 -1.50000 AFIX 0 C8 1 0.156086 0.258926 0.350345 11.00000 0.04707 0.03835 = 0.04676 -0.00605 0.01729 -0.00877 AFIX 137 H025 2 0.126073 0.201861 0.337360 11.00000 -1.50000 H026 2 0.066876 0.303475 0.353145 11.00000 -1.50000 H027 2 0.199632 0.233132 0.388527 11.00000 -1.50000 AFIX 0 C9 1 0.601808 0.479193 0.310865 11.00000 0.04107 0.03819 = 0.02686 -0.01277 -0.00269 -0.00534 AFIX 137 H01J 2 0.666514 0.520875 0.279554 11.00000 -1.50000 H01K 2 0.664611 0.426781 0.336937 11.00000 -1.50000 H01L 2 0.548589 0.522186 0.332776 11.00000 -1.50000 AFIX 0 RESI 0 RESI 3 MES C1 1 0.721889 0.453746 0.139666 11.00000 0.01997 0.01654 = 0.03213 -0.01317 0.00151 -0.00749 C2 1 0.727703 0.484119 0.078015 11.00000 0.02333 0.01717 = 0.02928 -0.01114 0.00417 -0.00658 C3 1 0.832523 0.437681 0.046638 11.00000 0.03213 0.02251 = 0.03249 -0.01144 0.00671 -0.00531 AFIX 43 H3 2 0.833052 0.459211 0.005401 11.00000 -1.20000 AFIX 0 C4 1 0.935287 0.361873 0.073030 11.00000 0.02619 0.01915 = 0.04180 -0.01445 0.01256 -0.00811 C5 1 0.932279 0.333184 0.132895 11.00000 0.02200 0.01399 = 0.04774 -0.00759 0.00089 -0.00246 AFIX 43 H5 2 1.003422 0.282094 0.152118 11.00000 -1.20000 AFIX 0 C6 1 0.828657 0.376345 0.166365 11.00000 0.02347 0.01342 = 0.03692 -0.01045 0.00063 -0.00573 C7 1 0.619435 0.564435 0.043782 11.00000 0.02776 0.02868 = 0.02703 -0.01009 0.00347 -0.00356 AFIX 137 H01A 2 0.627455 0.564373 0.002937 11.00000 -1.50000 H01B 2 0.644969 0.631069 0.046684 11.00000 -1.50000 H01C 2 0.515472 0.550094 0.059463 11.00000 -1.50000 AFIX 0 C8 1 1.044519 0.310100 0.037919 11.00000 0.04141 0.02533 = 0.05998 -0.01997 0.02044 -0.00482 AFIX 137 H01Q 2 1.010498 0.242101 0.041301 11.00000 -1.50000 H01R 2 1.146239 0.304639 0.052773 11.00000 -1.50000 H01S 2 1.047319 0.350146 -0.002979 11.00000 -1.50000 AFIX 0 C9 1 0.834276 0.338444 0.231636 11.00000 0.02798 0.02601 = 0.04140 -0.01124 -0.00475 -0.00118 AFIX 137 H01G 2 0.915536 0.285798 0.242003 11.00000 -1.50000 H01H 2 0.736931 0.310012 0.248252 11.00000 -1.50000 H01I 2 0.854013 0.394906 0.247046 11.00000 -1.50000 AFIX 0 RESI 0 RESI 4 TOL C1 1 0.334247 0.644652 0.470412 11.00000 0.03453 0.02893 = 0.02394 -0.00873 -0.00271 0.00049 C2 1 0.305663 0.588714 0.527720 11.00000 0.04784 0.03558 = 0.02134 -0.00832 -0.00497 -0.00233 AFIX 43 H01F 2 0.329647 0.615317 0.558299 11.00000 -1.20000 AFIX 0 C3 1 0.242958 0.495111 0.540811 11.00000 0.04755 0.03255 = 0.02469 -0.00114 -0.00163 0.00007 AFIX 43 H01T 2 0.223355 0.458984 0.580411 11.00000 -1.20000 AFIX 0 C4 1 0.207593 0.452029 0.497983 11.00000 0.03313 0.02654 = 0.03647 -0.00425 -0.00033 0.00046 C5 1 0.238415 0.507546 0.440861 11.00000 0.03931 0.02912 = 0.03092 -0.01385 -0.00349 -0.00057 AFIX 43 H5 2 0.216844 0.479826 0.410445 11.00000 -1.20000 AFIX 0 C6 1 0.299763 0.602279 0.426854 11.00000 0.03699 0.03244 = 0.02041 -0.00804 -0.00398 -0.00031 AFIX 43 H6 2 0.318463 0.638633 0.387234 11.00000 -1.20000 AFIX 0 C7 1 0.136998 0.350292 0.512676 11.00000 0.05039 0.03333 = 0.05279 -0.00871 -0.00188 -0.00286 AFIX 137 H029 2 0.133283 0.328777 0.477296 11.00000 -1.50000 H02A 2 0.033832 0.355664 0.529421 11.00000 -1.50000 H02B 2 0.197962 0.300262 0.540868 11.00000 -1.50000 AFIX 0 RESI 0 RESI 5 TOL C1 1 0.336786 0.803323 0.496310 11.00000 0.04502 0.03531 = 0.02386 -0.01403 0.00443 -0.00581 C2 1 0.439645 0.845959 0.522219 11.00000 0.04280 0.07360 = 0.04538 -0.04055 -0.00150 -0.00011 AFIX 43 H028 2 0.545319 0.832138 0.516849 11.00000 -1.20000 AFIX 0 C3 1 0.388644 0.909124 0.556172 11.00000 0.05274 0.09655 = 0.06270 -0.06170 -0.00319 -0.00583 AFIX 43 H02K 2 0.460528 0.938789 0.573333 11.00000 -1.20000 AFIX 0 C4 1 0.235280 0.929733 0.565516 11.00000 0.05678 0.06385 = 0.04602 -0.03762 0.00497 0.00050 C5 1 0.134370 0.885331 0.539716 11.00000 0.04265 0.05647 = 0.04524 -0.02349 0.01435 -0.00729 AFIX 43 H024 2 0.028581 0.897705 0.545835 11.00000 -1.20000 AFIX 0 C6 1 0.183333 0.823141 0.505102 11.00000 0.04081 0.04132 = 0.04150 -0.01983 0.00640 -0.01011 AFIX 43 H01Y 2 0.111509 0.794246 0.487485 11.00000 -1.20000 AFIX 0 C7 1 0.181043 0.997921 0.602982 11.00000 0.07936 0.10828 = 0.08366 -0.07370 0.00846 0.01225 AFIX 137 H02L 2 0.246012 1.056105 0.594564 11.00000 -1.50000 H02M 2 0.185874 0.959737 0.644072 11.00000 -1.50000 H02N 2 0.076136 1.022057 0.594560 11.00000 -1.50000 REM ##### REM ##### AFIX 0 RESI 0 RESI 6 KRON K1 6 1.183260 0.829724 0.165252 11.00000 0.03434 0.02345 = 0.02827 -0.00847 -0.00173 -0.00014 O2 5 1.144490 0.944121 0.242305 11.00000 0.03740 0.04346 = 0.03606 -0.02134 -0.00237 0.00778 C3 1 1.135416 1.051827 0.219636 11.00000 0.04046 0.03832 = 0.05565 -0.02860 -0.01489 0.01040 AFIX 23 H014 2 1.151253 1.083709 0.250760 11.00000 -1.20000 H015 2 1.033789 1.074445 0.204542 11.00000 -1.20000 AFIX 0 C4 1 1.253787 1.082725 0.172161 11.00000 0.03942 0.03372 = 0.06567 -0.02749 -0.00940 -0.00058 AFIX 23 H02C 2 1.256391 1.157663 0.158968 11.00000 -1.20000 H02D 2 1.354379 1.055309 0.186697 11.00000 -1.20000 AFIX 0 O5 5 1.222620 1.045749 0.124790 11.00000 0.02852 0.03018 = 0.04398 -0.01442 -0.00136 -0.00469 C6 1 1.337672 1.070179 0.079739 11.00000 0.02698 0.02909 = 0.06018 -0.00748 0.00524 -0.00407 AFIX 23 H01W 2 1.437196 1.041857 0.095023 11.00000 -1.20000 H01X 2 1.343416 1.144776 0.064508 11.00000 -1.20000 AFIX 0 C7 1 1.301492 1.026954 0.032580 11.00000 0.03430 0.03290 = 0.04209 -0.00136 0.00567 0.00016 AFIX 23 H01U 2 1.197758 1.049823 0.019883 11.00000 -1.20000 H01V 2 1.373893 1.049969 -0.001214 11.00000 -1.20000 AFIX 0 O8 5 1.311947 0.919064 0.054371 11.00000 0.03925 0.02752 = 0.03006 -0.00555 -0.00187 0.00319 C9 1 1.276902 0.869340 0.012993 11.00000 0.03631 0.04922 = 0.02934 -0.00990 0.00346 0.00135 AFIX 23 H01Z 2 1.339460 0.895207 -0.023368 11.00000 -1.20000 H010 2 1.168738 0.883111 0.003885 11.00000 -1.20000 AFIX 0 C10 1 1.307920 0.758032 0.037148 11.00000 0.03994 0.04376 = 0.03899 -0.01977 0.00516 0.00670 AFIX 23 H020 2 1.300808 0.723705 0.006449 11.00000 -1.20000 H021 2 1.411551 0.744733 0.051685 11.00000 -1.20000 AFIX 0 O11 5 1.199011 0.720046 0.083428 11.00000 0.03287 0.02740 = 0.03473 -0.01149 -0.00372 0.00673 C12 1 1.225150 0.613747 0.110644 11.00000 0.03755 0.03157 = 0.04523 -0.02219 -0.01322 0.00956 AFIX 23 H01O 2 1.327208 0.601449 0.126625 11.00000 -1.20000 H01P 2 1.221255 0.575723 0.081500 11.00000 -1.20000 AFIX 0 C13 1 1.108003 0.577344 0.158248 11.00000 0.03282 0.02666 = 0.05584 -0.01689 -0.01749 0.00028 AFIX 23 H01M 2 1.005574 0.591672 0.142650 11.00000 -1.20000 H01N 2 1.122333 0.503118 0.175344 11.00000 -1.20000 AFIX 0 O14 5 1.121478 0.627776 0.201549 11.00000 0.03239 0.02718 = 0.03930 -0.00807 -0.00053 -0.00706 C15 1 1.018727 0.593177 0.250444 11.00000 0.04026 0.03582 = 0.04270 0.00588 0.00008 -0.01142 AFIX 23 H022 2 1.029042 0.518383 0.265721 11.00000 -1.20000 H023 2 0.913018 0.612014 0.238984 11.00000 -1.20000 AFIX 0 C16 1 1.055041 0.641268 0.295721 11.00000 0.05061 0.04903 = 0.03688 0.00351 0.00449 -0.00966 AFIX 23 H02E 2 0.988350 0.615674 0.330985 11.00000 -1.20000 H02F 2 1.161549 0.623444 0.306369 11.00000 -1.20000 AFIX 0 O17 5 1.033837 0.747793 0.274507 11.00000 0.04789 0.04531 = 0.03077 -0.00771 0.00030 -0.00224 C18 1 1.068075 0.798693 0.315719 11.00000 0.07638 0.06553 = 0.02688 -0.01391 0.00208 -0.00166 AFIX 23 H02I 2 1.175432 0.783793 0.325823 11.00000 -1.20000 H02J 2 1.003259 0.774537 0.351659 11.00000 -1.20000 AFIX 0 C19 1 1.040828 0.909479 0.290561 11.00000 0.05685 0.06566 = 0.03665 -0.02936 0.00171 0.00744 AFIX 23 H02G 2 0.935420 0.924053 0.277957 11.00000 -1.20000 H02H 2 1.055030 0.945084 0.320163 11.00000 -1.20000 RESI 0 AFIX 0 HKLF 4 REM JoKr014_XiJi_a.res in P-1 REM R1 = 0.0580 for 5926 Fo > 4sig(Fo) and 0.1467 for all 11400 data REM 684 parameters refined using 0 restraints END WGHT 0.0422 0.9681 REM Highest difference peak 0.248, deepest hole -0.254, 1-sigma level 0.057 Q1 1 0.2237 0.1913 0.3794 11.00000 0.05 0.25 Q2 1 0.8117 0.8009 0.1366 11.00000 0.05 0.23 ; _shelx_res_checksum 86767 _shelx_hkl_file ; 1 0 0 559.74 30.70 1 0 0 542.75 30.60 1 0 0 549.05 30.40 1 0 0 541.15 30.70 1 0 0 577.04 30.40 1 0 0 553.34 30.60 1 0 0 574.94 30.10 -2 0 0 1636.34 87.49 -2 0 0 1684.73 87.69 -2 0 0 1565.54 86.79 -2 0 0 1559.34 87.49 -2 0 0 1646.74 87.29 -2 0 0 1670.23 88.39 -2 0 0 1617.44 87.99 2 0 0 1604.04 87.39 2 0 0 1643.84 87.39 2 0 0 1682.23 87.39 2 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2035.90 103.99 -2 -2 0 1919.91 99.49 -2 -2 0 1983.00 100.99 -2 -2 0 1878.11 102.49 -2 -2 0 1921.41 103.89 -2 -2 0 1944.91 104.09 -2 -2 0 1951.10 103.49 2 2 0 1993.60 104.29 2 2 0 2017.20 102.89 2 2 0 1916.91 104.39 2 2 0 1869.91 104.39 2 2 0 1913.71 100.69 2 2 0 1980.70 103.69 2 2 0 1943.21 103.69 2 2 0 1975.20 100.69 2 2 0 1931.71 102.89 2 2 0 1946.81 101.19 2 2 0 1948.61 103.29 2 2 0 1951.90 101.09 2 2 0 1998.00 103.79 -3 -2 0 24.70 10.60 -3 -2 0 7.00 9.40 -3 -2 0 11.50 8.70 -3 -2 0 -8.50 8.50 -3 -2 0 9.80 3.50 -3 -2 0 19.70 10.10 -3 -2 0 4.10 9.30 -3 -2 0 5.30 3.40 3 2 0 8.10 8.80 3 2 0 2.90 10.30 3 2 0 13.10 3.30 3 2 0 13.80 4.00 3 2 0 4.20 8.20 3 2 0 5.70 3.10 3 2 0 14.90 9.00 3 2 0 18.00 4.20 3 2 0 6.20 7.80 3 2 0 -0.80 7.90 3 2 0 23.30 8.20 3 2 0 24.50 9.40 3 2 0 16.70 10.50 -4 -2 0 283.47 25.40 -4 -2 0 311.67 29.10 -4 -2 0 279.57 28.20 -4 -2 0 328.77 28.70 -4 -2 0 237.78 27.10 -4 -2 0 313.77 27.90 -4 -2 0 304.57 26.20 4 2 0 310.07 28.10 4 2 0 357.26 27.30 4 2 0 287.27 16.90 4 2 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20.90 0 -4 24 17.00 21.60 0 -4 24 13.90 24.30 0 4 -24 4.80 18.20 0 4 -24 29.20 23.50 0 4 -24 24.90 32.60 -1 -4 24 16.80 22.40 -1 -4 24 65.59 26.00 -1 -4 24 36.50 22.30 1 4 -24 -21.70 34.50 1 4 -24 -19.30 20.70 1 4 -24 30.50 24.40 1 4 -24 22.90 23.20 -2 -4 24 8.20 21.80 -2 -4 24 -9.60 22.90 -2 -4 24 21.60 18.30 -2 -4 24 11.90 20.00 2 4 -24 -3.80 19.00 2 4 -24 -31.50 32.30 2 4 -24 -14.90 20.30 2 4 -24 4.60 23.80 -3 -4 24 10.50 17.60 -3 -4 24 30.70 21.00 -3 -4 24 21.00 21.80 3 4 -24 -3.70 21.00 3 4 -24 -21.50 31.40 3 4 -24 36.10 26.70 3 4 -24 -20.90 20.10 4 -3 25 -32.00 20.80 4 -3 25 -23.30 19.90 4 -3 25 0.70 20.60 4 -3 25 -15.00 22.00 -4 3 -25 -13.90 24.10 -4 3 -25 22.80 21.90 3 -3 25 19.80 23.40 3 -3 25 10.10 23.30 3 -3 25 -5.70 25.70 -3 3 -25 25.80 22.70 -3 3 -25 34.60 25.10 2 -3 25 5.00 20.20 2 -3 25 57.29 26.20 2 -3 25 89.99 29.50 -2 3 -25 17.00 20.30 -2 3 -25 14.90 23.60 1 -3 25 -2.90 20.80 1 -3 25 1.40 23.50 1 -3 25 8.80 21.30 -1 3 -25 41.90 29.30 -1 3 -25 -8.70 21.00 -1 3 -25 0.90 20.90 0 -3 25 18.20 21.90 0 -3 25 38.30 22.80 0 -3 25 19.20 23.10 0 3 -25 -13.40 19.00 0 3 -25 14.30 22.30 0 3 -25 -41.80 27.40 -1 -3 25 47.40 26.10 -1 -3 25 51.99 22.50 -1 -3 25 82.29 25.50 -1 -3 25 48.20 18.70 1 3 -25 39.70 25.10 1 3 -25 54.29 25.10 1 3 -25 18.00 22.30 1 3 -25 57.49 35.30 -2 -3 25 9.30 21.10 -2 -3 25 34.10 18.00 -2 -3 25 -34.40 17.10 -2 -3 25 -44.60 21.30 2 3 -25 -77.59 27.90 2 3 -25 28.80 23.50 2 3 -25 18.60 23.00 2 3 -25 17.20 22.20 -3 -3 25 -9.90 19.30 -3 -3 25 -5.70 19.60 -3 -3 25 18.50 17.80 3 3 -25 -21.30 20.80 3 3 -25 -1.60 24.70 3 3 -25 -36.60 33.10 3 3 -25 -5.40 21.50 4 -2 26 -1.10 23.10 4 -2 26 12.50 23.40 4 -2 26 22.20 26.10 4 -2 26 26.90 23.00 -4 2 -26 -3.60 23.80 3 -2 26 -10.20 22.40 3 -2 26 -12.80 19.20 3 -2 26 -2.50 23.20 -3 2 -26 -18.70 20.40 -3 2 -26 0.70 19.70 2 -2 26 -13.70 20.90 2 -2 26 29.50 25.20 2 -2 26 -14.00 23.90 -2 2 -26 -22.10 21.30 -2 2 -26 -38.20 18.30 1 -2 26 6.20 21.00 1 -2 26 -5.50 22.50 1 -2 26 -9.80 21.40 -1 2 -26 -2.10 26.60 -1 2 -26 9.30 21.30 -1 2 -26 -4.10 20.50 0 -2 26 20.10 19.90 0 -2 26 -7.20 24.50 0 -2 26 -26.50 15.30 0 -2 26 -34.10 19.40 0 2 -26 -3.30 19.10 0 2 -26 -28.50 29.70 0 2 -26 -22.00 20.30 -1 -2 26 139.29 30.30 -1 -2 26 78.79 20.90 -1 -2 26 119.29 32.10 -1 -2 26 68.49 22.80 1 2 -26 71.19 33.60 1 2 -26 80.99 27.00 1 2 -26 88.19 28.20 -2 -2 26 -32.20 22.80 -2 -2 26 -0.80 17.80 -2 -2 26 6.10 21.30 -2 -2 26 -0.60 18.60 2 2 -26 -12.10 21.30 2 2 -26 -0.20 18.40 2 2 -26 -33.10 32.00 -3 -2 26 -13.10 19.90 -3 -2 26 -0.90 17.50 -3 -2 26 2.80 19.50 3 2 -26 15.10 22.20 3 2 -26 7.10 23.30 3 2 -26 29.50 33.10 3 -1 27 28.30 24.60 3 -1 27 -2.80 24.30 3 -1 27 -0.90 23.30 -3 1 -27 -9.20 23.90 -3 1 -27 -6.00 19.60 2 -1 27 43.20 24.80 2 -1 27 18.30 22.60 2 -1 27 6.50 22.00 -2 1 -27 -6.30 24.60 -2 1 -27 3.20 20.90 1 -1 27 17.40 25.00 1 -1 27 47.50 23.80 1 -1 27 -24.00 20.20 -1 1 -27 -9.30 23.10 -1 1 -27 12.20 21.90 0 -1 27 -11.50 19.70 0 -1 27 -15.50 18.20 0 -1 27 7.70 23.50 0 1 -27 17.40 29.20 0 1 -27 16.80 21.20 0 1 -27 -5.80 21.90 -1 -1 27 1.80 24.70 -1 -1 27 -0.20 17.70 -1 -1 27 9.60 23.00 -1 -1 27 15.80 20.00 1 1 -27 14.80 20.30 1 1 -27 -36.80 30.00 1 1 -27 14.30 21.10 -2 -1 27 0.10 21.50 -2 -1 27 -20.50 21.90 -2 -1 27 3.80 19.20 -2 -1 27 8.50 18.00 2 1 -27 -9.10 21.00 2 1 -27 -9.90 20.10 2 1 -27 -53.09 29.40 3 0 28 -21.30 22.80 3 0 28 42.20 26.50 3 0 28 55.99 25.70 -3 0 -28 11.10 22.80 -3 0 -28 37.10 26.90 2 0 28 -29.50 20.30 2 0 28 7.70 25.10 2 0 28 41.20 22.60 -2 0 -28 -5.10 21.10 -2 0 -28 -5.70 23.90 1 0 28 2.50 17.20 1 0 28 0.20 23.30 1 0 28 -20.70 23.30 -1 0 -28 -16.20 23.50 -1 0 -28 -13.50 20.30 0 0 28 31.00 27.00 0 0 28 58.39 28.00 0 0 28 55.89 23.40 0 0 -28 15.90 23.40 0 0 -28 72.49 26.90 -1 0 28 27.20 26.90 -1 0 28 -7.30 18.50 -1 0 28 9.60 23.20 1 0 -28 -17.60 22.40 1 0 -28 -30.40 30.40 1 0 -28 15.00 21.20 -2 0 28 2.00 25.40 -2 0 28 -12.80 20.70 2 1 29 4.40 25.90 2 1 29 16.90 21.00 1 1 29 18.50 27.80 1 1 29 1.80 22.00 1 1 29 -6.30 19.70 -1 -1 -29 -15.90 20.70 -1 -1 -29 28.40 25.20 0 1 29 -45.20 17.10 0 1 29 56.19 25.50 0 1 29 -19.80 22.00 0 -1 -29 -4.30 20.90 0 -1 -29 18.10 25.70 0 -9 20 8.00 22.70 0 -9 20 19.80 23.80 0 -9 20 -28.20 20.20 0 9 -20 -35.80 25.20 0 9 -20 45.30 36.90 2 -8 21 -3.30 22.40 2 -8 21 11.80 23.40 2 -8 21 -5.80 25.40 -2 8 -21 50.69 36.20 -2 8 -21 23.20 25.60 1 -8 21 -20.90 23.20 1 -8 21 33.50 24.40 1 -8 21 9.40 20.40 -1 8 -21 -2.30 33.50 -1 8 -21 12.70 24.40 -1 8 -21 -17.70 20.40 0 -8 21 -55.99 19.00 0 -8 21 19.70 24.20 0 -8 21 -11.20 22.00 0 8 -21 -29.40 21.00 0 8 -21 -12.70 20.70 0 8 -21 10.40 36.20 -1 -8 21 2.80 20.30 -1 -8 21 -4.40 19.80 -1 -8 21 -1.60 22.10 1 8 -21 -0.70 20.00 1 8 -21 48.10 35.60 1 8 -21 2.40 21.60 2 -7 22 -2.40 22.00 2 -7 22 30.60 23.90 2 -7 22 30.40 24.60 -2 7 -22 76.79 31.70 -2 7 -22 9.70 24.70 -2 7 -22 -0.60 22.80 1 -7 22 -6.10 22.50 1 -7 22 26.60 24.60 1 -7 22 -2.60 22.10 -1 7 -22 -14.20 22.90 -1 7 -22 4.90 22.40 -1 7 -22 54.29 35.20 0 -7 22 -10.00 21.20 0 -7 22 15.50 22.20 0 -7 22 -27.30 21.80 0 7 -22 24.50 35.20 0 7 -22 10.60 19.90 0 7 -22 30.30 24.10 -1 -7 22 1.90 18.80 -1 -7 22 6.00 22.30 -1 -7 22 1.40 23.00 1 7 -22 -19.10 19.00 1 7 -22 -14.40 19.10 1 7 -22 12.20 35.20 -2 -7 22 -51.09 19.30 -2 -7 22 24.70 23.80 -2 -7 22 -15.80 19.50 2 7 -22 -2.30 21.10 2 7 -22 -10.30 38.20 2 7 -22 -17.10 22.00 2 7 -22 5.30 26.10 3 -6 23 0.70 22.70 3 -6 23 -9.30 21.30 3 -6 23 13.00 26.00 -3 6 -23 17.90 25.60 -3 6 -23 -20.90 31.00 2 -6 23 8.20 23.40 2 -6 23 13.80 25.90 2 -6 23 26.40 24.10 -2 6 -23 17.40 26.20 -2 6 -23 82.99 35.30 -2 6 -23 -10.90 21.20 1 -6 23 13.00 26.00 1 -6 23 19.60 24.70 1 -6 23 31.00 24.30 -1 6 -23 23.90 26.70 -1 6 -23 9.30 22.10 -1 6 -23 66.99 33.80 0 -6 23 30.90 23.50 0 -6 23 4.70 21.10 0 -6 23 52.29 24.40 0 6 -23 17.20 25.60 0 6 -23 55.39 33.60 0 6 -23 -1.10 22.00 -1 -6 23 0.70 24.60 -1 -6 23 6.40 23.50 -1 -6 23 39.00 22.90 1 6 -23 22.10 36.50 1 6 -23 -15.40 22.80 1 6 -23 -21.40 18.60 -2 -6 23 9.70 23.20 -2 -6 23 6.10 21.70 -2 -6 23 -38.50 22.30 2 6 -23 -45.70 34.20 2 6 -23 8.10 21.80 2 6 -23 -9.70 22.00 2 6 -23 -41.60 26.00 3 -5 24 -1.60 21.30 3 -5 24 -8.30 21.00 3 -5 24 -3.20 25.40 -3 5 -24 7.10 24.90 -3 5 -24 -29.40 20.40 2 -5 24 -44.50 22.10 2 -5 24 -7.90 19.50 2 -5 24 -7.60 21.50 -2 5 -24 35.10 23.00 -2 5 -24 27.50 31.60 -2 5 -24 0.00 25.40 1 -5 24 46.40 24.20 1 -5 24 23.30 25.10 1 -5 24 -25.40 19.70 -1 5 -24 -2.20 30.50 -1 5 -24 -8.80 22.50 -1 5 -24 28.40 24.20 0 -5 24 4.20 22.50 0 -5 24 14.50 24.10 0 -5 24 39.60 25.40 0 5 -24 0.30 19.50 0 5 -24 2.10 33.50 0 5 -24 42.40 23.60 -1 -5 24 14.30 20.30 -1 -5 24 17.90 25.20 -1 -5 24 10.60 23.30 1 5 -24 14.50 21.50 1 5 -24 -3.50 19.80 1 5 -24 -21.00 32.30 -2 -5 24 22.70 21.10 -2 -5 24 16.00 24.30 -2 -5 24 -15.00 21.40 2 5 -24 -24.80 35.10 2 5 -24 21.90 28.20 2 5 -24 -5.60 20.60 2 5 -24 30.30 23.40 3 -4 25 9.90 21.20 3 -4 25 -2.50 22.20 3 -4 25 24.60 25.90 -3 4 -25 28.80 26.70 -3 4 -25 -3.60 21.00 2 -4 25 24.70 22.30 2 -4 25 9.40 24.10 2 -4 25 -11.40 21.20 -2 4 -25 -46.80 21.80 -2 4 -25 15.70 22.20 -2 4 -25 72.59 40.20 1 -4 25 28.50 25.70 1 -4 25 49.30 24.60 1 -4 25 16.80 23.80 -1 4 -25 2.80 23.90 -1 4 -25 22.00 30.00 -1 4 -25 4.90 22.00 0 -4 25 27.80 21.80 0 -4 25 12.00 23.90 0 -4 25 4.90 21.90 0 4 -25 -1.70 18.50 0 4 -25 24.20 24.50 0 4 -25 -60.79 30.30 -1 -4 25 27.40 24.60 -1 -4 25 30.60 19.90 -1 -4 25 6.50 23.20 1 4 -25 -16.90 35.00 1 4 -25 7.30 24.20 1 4 -25 4.60 21.90 -2 -4 25 28.30 23.80 -2 -4 25 -8.30 21.40 -2 -4 25 25.20 21.30 2 4 -25 14.30 22.40 2 4 -25 10.30 26.20 2 4 -25 2.40 36.80 2 4 -25 33.00 25.10 3 -3 26 12.80 21.80 3 -3 26 -8.30 25.50 3 -3 26 -1.10 20.90 -3 3 -26 -7.50 26.20 2 -3 26 11.20 22.10 2 -3 26 -37.20 19.30 2 -3 26 -16.60 24.50 -2 3 -26 -63.89 19.10 -2 3 -26 -0.80 21.20 1 -3 26 63.79 27.80 1 -3 26 66.09 25.90 1 -3 26 78.89 29.20 -1 3 -26 14.10 24.00 -1 3 -26 85.79 31.60 -1 3 -26 27.00 23.10 0 -3 26 27.80 25.30 0 -3 26 -36.50 19.80 0 -3 26 -11.90 18.80 0 3 -26 -47.90 18.60 0 3 -26 -28.30 28.50 0 3 -26 -14.10 20.50 -1 -3 26 -16.30 18.50 -1 -3 26 27.80 24.60 -1 -3 26 -23.10 21.40 1 3 -26 -52.09 28.30 1 3 -26 35.90 22.80 1 3 -26 -10.60 20.20 -2 -3 26 -7.10 24.90 -2 -3 26 1.40 19.20 -2 -3 26 -13.40 20.60 -2 -3 26 11.60 20.00 2 3 -26 0.50 25.00 2 3 -26 -34.80 35.80 2 3 -26 -15.00 21.80 2 3 -26 -4.80 22.20 2 -2 27 30.00 25.50 2 -2 27 -11.80 24.40 2 -2 27 51.19 20.90 -2 2 -27 26.70 28.10 -2 2 -27 -31.20 18.30 1 -2 27 24.80 23.10 1 -2 27 51.99 28.50 1 -2 27 44.30 22.50 -1 2 -27 24.80 26.50 -1 2 -27 19.20 22.30 0 -2 27 -1.00 22.20 0 -2 27 -0.80 23.60 0 -2 27 32.70 22.60 0 2 -27 14.30 24.50 0 2 -27 -12.20 22.70 0 2 -27 -29.70 31.80 -1 -2 27 60.99 23.70 -1 -2 27 3.50 22.20 -1 -2 27 38.00 18.70 -1 -2 27 32.30 28.00 1 2 -27 5.60 35.60 1 2 -27 -15.50 20.90 1 2 -27 40.30 25.50 2 -1 28 -13.60 23.50 1 -1 28 76.09 25.70 1 -1 28 93.39 29.90 1 -1 28 75.99 28.60 -1 1 -28 89.49 29.50 -1 1 -28 44.20 25.10 0 -1 28 7.10 21.60 0 -1 28 -38.70 19.30 0 -1 28 -27.20 24.80 0 1 -28 24.80 24.10 0 1 -28 -8.20 20.50 0 -6 24 35.00 28.30 0 6 -24 -10.10 34.60 1 -5 25 21.90 28.10 1 -5 25 -4.10 20.60 -1 5 -25 39.10 33.80 0 -5 25 21.40 27.70 0 -5 25 -8.00 23.10 0 -5 25 11.30 19.70 0 5 -25 51.39 26.80 0 5 -25 -0.40 32.00 0 -4 26 23.30 26.70 0 4 -26 58.99 34.90 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 75915 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group N1_1 N 0.3916(3) 0.74291(19) 0.45879(10) 0.0319(6) Uani 1 1 d . . . . . B2_1 B 0.6055(3) 0.5040(2) 0.17823(14) 0.0203(7) Uani 1 1 d . . . . . C3_1 C 0.4497(3) 0.7973(2) 0.40283(13) 0.0284(7) Uani 1 1 d . . . . . C4_1 C 0.5550(3) 0.7491(2) 0.37119(12) 0.0268(7) Uani 1 1 d . . . . . H4_1 H 0.5876 0.6804 0.3879 0.032 Uiso 1 1 calc R U . . . C5_1 C 0.6105(3) 0.8002(2) 0.31690(12) 0.0233(7) Uani 1 1 d . . . . . H5_1 H 0.6789 0.7654 0.2963 0.028 Uiso 1 1 calc R U . . . C6_1 C 0.5692(3) 0.9038(2) 0.29034(12) 0.0220(7) Uani 1 1 d . . . . . C7_1 C 0.4779(3) 0.9542(2) 0.32533(13) 0.0253(7) Uani 1 1 d . . . . . C8_1 C 0.4152(3) 0.8989(2) 0.37976(13) 0.0284(7) Uani 1 1 d . . . . . H8_1 H 0.3474 0.9329 0.4010 0.034 Uiso 1 1 calc R U . . . C9_1 C 0.6253(3) 0.9611(2) 0.23322(12) 0.0221(7) Uani 1 1 d . . . . . C10_1 C 0.6235(3) 1.0686(2) 0.22170(13) 0.0232(7) Uani 1 1 d . . . . . C11_1 C 0.5356(3) 1.1167(2) 0.25928(13) 0.0283(7) Uani 1 1 d . . . . . H11_1 H 0.5315 1.1886 0.2503 0.034 Uiso 1 1 calc R U . . . C12_1 C 0.4588(3) 1.0626(2) 0.30691(14) 0.0296(7) Uani 1 1 d . . . . . H01D_1 H 0.3916 1.0963 0.3285 0.036 Uiso 1 1 calc R U . . . C13_1 C 0.6908(3) 0.9172(2) 0.18813(12) 0.0197(6) Uani 1 1 d . . . . . C14_1 C 0.7912(3) 0.9784(2) 0.14497(12) 0.0230(7) Uani 1 1 d . . . . . C15_1 C 0.7960(3) 1.0831(2) 0.13861(13) 0.0292(7) Uani 1 1 d . . . . . H01E_1 H 0.8631 1.1230 0.1097 0.035 Uiso 1 1 calc R U . . . C16_1 C 0.7061(3) 1.1283(2) 0.17321(13) 0.0278(7) Uani 1 1 d . . . . . H16_1 H 0.6992 1.2002 0.1646 0.033 Uiso 1 1 calc R U . . . C17_1 C 0.6555(3) 0.8205(2) 0.18180(12) 0.0190(6) Uani 1 1 d . . . . . C18_1 C 0.7439(3) 0.7779(2) 0.14195(11) 0.0181(6) Uani 1 1 d . . . . . C19_1 C 0.8582(3) 0.8375(2) 0.10511(12) 0.0237(7) Uani 1 1 d . . . . . H19_1 H 0.9215 0.8088 0.0799 0.028 Uiso 1 1 calc R U . . . C20_1 C 0.8777(3) 0.9340(2) 0.10558(12) 0.0256(7) Uani 1 1 d . . . . . H20_1 H 0.9506 0.9731 0.0791 0.031 Uiso 1 1 calc R U . . . C21_1 C 0.5285(3) 0.7627(2) 0.21039(12) 0.0207(6) Uani 1 1 d . . . . . H21_1 H 0.4568 0.7915 0.2330 0.025 Uiso 1 1 calc R U . . . C22_1 C 0.5077(3) 0.6681(2) 0.20605(11) 0.0197(6) Uani 1 1 d . . . . . H22_1 H 0.4209 0.6339 0.2257 0.024 Uiso 1 1 calc R U . . . C23_1 C 0.6096(3) 0.6164(2) 0.17330(12) 0.0201(6) Uani 1 1 d . . . . . C24_1 C 0.7199(3) 0.68099(19) 0.13877(12) 0.0192(6) Uani 1 1 d . . . . . H24_1 H 0.7817 0.6562 0.1115 0.023 Uiso 1 1 calc R U . . . C1_2 C 0.4895(3) 0.4352(2) 0.22504(12) 0.0214(7) Uani 1 1 d . . . . . C2_2 C 0.3841(3) 0.37616(19) 0.20866(12) 0.0212(6) Uani 1 1 d . . . . . C3_2 C 0.2779(3) 0.3212(2) 0.24897(13) 0.0280(7) Uani 1 1 d . . . . . H3_2 H 0.2064 0.2846 0.2361 0.034 Uiso 1 1 calc R U . . . C4_2 C 0.2734(3) 0.3183(2) 0.30695(14) 0.0302(7) Uani 1 1 d . . . . . C5_2 C 0.3814(3) 0.3710(2) 0.32438(13) 0.0309(7) Uani 1 1 d . . . . . H5_2 H 0.3840 0.3674 0.3644 0.037 Uiso 1 1 calc R U . . . C6_2 C 0.4862(3) 0.4290(2) 0.28492(13) 0.0246(7) Uani 1 1 d . . . . . C7_2 C 0.3836(3) 0.3691(2) 0.14702(12) 0.0250(7) Uani 1 1 d . . . . . H00C_2 H 0.4147 0.4333 0.1199 0.038 Uiso 1 1 calc R U . . . H00D_2 H 0.2812 0.3553 0.1388 0.038 Uiso 1 1 calc R U . . . H00E_2 H 0.4545 0.3140 0.1424 0.038 Uiso 1 1 calc R U . . . C8_2 C 0.1561(4) 0.2589(2) 0.35034(15) 0.0459(9) Uani 1 1 d . . . . . H025_2 H 0.1261 0.2019 0.3374 0.069 Uiso 1 1 calc R U . . . H026_2 H 0.0669 0.3035 0.3531 0.069 Uiso 1 1 calc R U . . . H027_2 H 0.1996 0.2331 0.3885 0.069 Uiso 1 1 calc R U . . . C9_2 C 0.6018(3) 0.4792(2) 0.31087(13) 0.0344(8) Uani 1 1 d . . . . . H01J_2 H 0.6665 0.5209 0.2796 0.052 Uiso 1 1 calc R U . . . H01K_2 H 0.6646 0.4268 0.3369 0.052 Uiso 1 1 calc R U . . . H01L_2 H 0.5486 0.5222 0.3328 0.052 Uiso 1 1 calc R U . . . C1_3 C 0.7219(3) 0.4537(2) 0.13967(12) 0.0214(7) Uani 1 1 d . . . . . C2_3 C 0.7277(3) 0.4841(2) 0.07801(13) 0.0223(7) Uani 1 1 d . . . . . C3_3 C 0.8325(3) 0.4377(2) 0.04664(13) 0.0285(7) Uani 1 1 d . . . . . H3_3 H 0.8331 0.4592 0.0054 0.034 Uiso 1 1 calc R U . . . C4_3 C 0.9353(3) 0.3619(2) 0.07303(14) 0.0282(7) Uani 1 1 d . . . . . C5_3 C 0.9323(3) 0.3332(2) 0.13289(14) 0.0282(7) Uani 1 1 d . . . . . H5_3 H 1.0034 0.2821 0.1521 0.034 Uiso 1 1 calc R U . . . C6_3 C 0.8287(3) 0.3763(2) 0.16636(13) 0.0238(7) Uani 1 1 d . . . . . C7_3 C 0.6194(3) 0.5644(2) 0.04378(12) 0.0275(7) Uani 1 1 d . . . . . H01A_3 H 0.6275 0.5644 0.0029 0.041 Uiso 1 1 calc R U . . . H01B_3 H 0.6450 0.6311 0.0467 0.041 Uiso 1 1 calc R U . . . H01C_3 H 0.5155 0.5501 0.0595 0.041 Uiso 1 1 calc R U . . . C8_3 C 1.0445(3) 0.3101(2) 0.03792(15) 0.0415(9) Uani 1 1 d . . . . . H01Q_3 H 1.0105 0.2421 0.0413 0.062 Uiso 1 1 calc R U . . . H01R_3 H 1.1462 0.3046 0.0528 0.062 Uiso 1 1 calc R U . . . H01S_3 H 1.0473 0.3501 -0.0030 0.062 Uiso 1 1 calc R U . . . C9_3 C 0.8343(3) 0.3384(2) 0.23164(13) 0.0313(8) Uani 1 1 d . . . . . H01G_3 H 0.9155 0.2858 0.2420 0.047 Uiso 1 1 calc R U . . . H01H_3 H 0.7369 0.3100 0.2483 0.047 Uiso 1 1 calc R U . . . H01I_3 H 0.8540 0.3949 0.2470 0.047 Uiso 1 1 calc R U . . . C1_4 C 0.3342(3) 0.6447(2) 0.47041(13) 0.0289(7) Uani 1 1 d . . . . . C2_4 C 0.3057(3) 0.5887(2) 0.52772(13) 0.0347(8) Uani 1 1 d . . . . . H01F_4 H 0.3296 0.6153 0.5583 0.042 Uiso 1 1 calc R U . . . C3_4 C 0.2430(3) 0.4951(2) 0.54081(14) 0.0365(8) Uani 1 1 d . . . . . H01T_4 H 0.2234 0.4590 0.5804 0.044 Uiso 1 1 calc R U . . . C4_4 C 0.2076(3) 0.4520(2) 0.49798(14) 0.0331(8) Uani 1 1 d . . . . . C5_4 C 0.2384(3) 0.5075(2) 0.44086(14) 0.0320(8) Uani 1 1 d . . . . . H5_4 H 0.2168 0.4798 0.4104 0.038 Uiso 1 1 calc R U . . . C6_4 C 0.2998(3) 0.6023(2) 0.42685(13) 0.0298(7) Uani 1 1 d . . . . . H6_4 H 0.3185 0.6386 0.3872 0.036 Uiso 1 1 calc R U . . . C7_4 C 0.1370(4) 0.3503(2) 0.51268(15) 0.0462(9) Uani 1 1 d . . . . . H029_4 H 0.1333 0.3288 0.4773 0.069 Uiso 1 1 calc R U . . . H02A_4 H 0.0338 0.3557 0.5294 0.069 Uiso 1 1 calc R U . . . H02B_4 H 0.1980 0.3003 0.5409 0.069 Uiso 1 1 calc R U . . . C1_5 C 0.3368(4) 0.8033(2) 0.49631(13) 0.0337(8) Uani 1 1 d . . . . . C2_5 C 0.4396(4) 0.8460(3) 0.52222(15) 0.0491(10) Uani 1 1 d . . . . . H028_5 H 0.5453 0.8321 0.5168 0.059 Uiso 1 1 calc R U . . . C3_5 C 0.3886(4) 0.9091(3) 0.55617(16) 0.0624(12) Uani 1 1 d . . . . . H02K_5 H 0.4605 0.9388 0.5733 0.075 Uiso 1 1 calc R U . . . C4_5 C 0.2353(4) 0.9297(3) 0.56552(16) 0.0514(10) Uani 1 1 d . . . . . C5_5 C 0.1344(4) 0.8853(3) 0.53972(15) 0.0468(9) Uani 1 1 d . . . . . H024_5 H 0.0286 0.8977 0.5458 0.056 Uiso 1 1 calc R U . . . C6_5 C 0.1833(4) 0.8231(2) 0.50510(14) 0.0396(8) Uani 1 1 d . . . . . H01Y_5 H 0.1115 0.7942 0.4875 0.047 Uiso 1 1 calc R U . . . C7_5 C 0.1810(5) 0.9979(3) 0.60298(19) 0.0820(15) Uani 1 1 d . . . . . H02L_5 H 0.2460 1.0561 0.5946 0.123 Uiso 1 1 calc R U . . . H02M_5 H 0.1859 0.9597 0.6441 0.123 Uiso 1 1 calc R U . . . H02N_5 H 0.0761 1.0221 0.5946 0.123 Uiso 1 1 calc R U . . . K1_6 K 1.18326(7) 0.82972(5) 0.16525(3) 0.02849(17) Uani 1 1 d . . . . . O2_6 O 1.1445(2) 0.94412(16) 0.24231(9) 0.0373(5) Uani 1 1 d . . . . . C3_6 C 1.1354(4) 1.0518(2) 0.21964(15) 0.0416(9) Uani 1 1 d . . . . . H014_6 H 1.1513 1.0837 0.2508 0.050 Uiso 1 1 calc R U . . . H015_6 H 1.0338 1.0744 0.2045 0.050 Uiso 1 1 calc R U . . . C4_6 C 1.2538(4) 1.0827(2) 0.17216(15) 0.0432(9) Uani 1 1 d . . . . . H02C_6 H 1.2564 1.1577 0.1590 0.052 Uiso 1 1 calc R U . . . H02D_6 H 1.3544 1.0553 0.1867 0.052 Uiso 1 1 calc R U . . . O5_6 O 1.2226(2) 1.04575(15) 0.12479(9) 0.0333(5) Uani 1 1 d . . . . . C6_6 C 1.3377(3) 1.0702(2) 0.07974(15) 0.0400(9) Uani 1 1 d . . . . . H01W_6 H 1.4372 1.0419 0.0950 0.048 Uiso 1 1 calc R U . . . H01X_6 H 1.3434 1.1448 0.0645 0.048 Uiso 1 1 calc R U . . . C7_6 C 1.3015(4) 1.0270(2) 0.03258(14) 0.0388(8) Uani 1 1 d . . . . . H01U_6 H 1.1978 1.0498 0.0199 0.047 Uiso 1 1 calc R U . . . H01V_6 H 1.3739 1.0500 -0.0012 0.047 Uiso 1 1 calc R U . . . O8_6 O 1.3119(2) 0.91906(15) 0.05437(9) 0.0330(5) Uani 1 1 d . . . . . C9_6 C 1.2769(4) 0.8693(2) 0.01299(14) 0.0389(8) Uani 1 1 d . . . . . H01Z_6 H 1.3395 0.8952 -0.0234 0.047 Uiso 1 1 calc R U . . . H010_6 H 1.1687 0.8831 0.0039 0.047 Uiso 1 1 calc R U . . . C10_6 C 1.3079(4) 0.7580(2) 0.03715(14) 0.0399(8) Uani 1 1 d . . . . . H020_6 H 1.3008 0.7237 0.0064 0.048 Uiso 1 1 calc R U . . . H021_6 H 1.4116 0.7447 0.0517 0.048 Uiso 1 1 calc R U . . . O11_6 O 1.1990(2) 0.72005(15) 0.08343(9) 0.0314(5) Uani 1 1 d . . . . . C12_6 C 1.2251(3) 0.6137(2) 0.11064(14) 0.0357(8) Uani 1 1 d . . . . . H01O_6 H 1.3272 0.6014 0.1266 0.043 Uiso 1 1 calc R U . . . H01P_6 H 1.2213 0.5757 0.0815 0.043 Uiso 1 1 calc R U . . . C13_6 C 1.1080(3) 0.5773(2) 0.15825(14) 0.0367(8) Uani 1 1 d . . . . . H01M_6 H 1.0056 0.5917 0.1427 0.044 Uiso 1 1 calc R U . . . H01N_6 H 1.1223 0.5031 0.1753 0.044 Uiso 1 1 calc R U . . . O14_6 O 1.1215(2) 0.62778(15) 0.20155(9) 0.0330(5) Uani 1 1 d . . . . . C15_6 C 1.0187(4) 0.5932(3) 0.25044(14) 0.0428(9) Uani 1 1 d . . . . . H022_6 H 1.0290 0.5184 0.2657 0.051 Uiso 1 1 calc R U . . . H023_6 H 0.9130 0.6120 0.2390 0.051 Uiso 1 1 calc R U . . . C16_6 C 1.0550(4) 0.6413(3) 0.29572(15) 0.0487(10) Uani 1 1 d . . . . . H02E_6 H 0.9884 0.6157 0.3310 0.058 Uiso 1 1 calc R U . . . H02F_6 H 1.1615 0.6234 0.3064 0.058 Uiso 1 1 calc R U . . . O17_6 O 1.0338(2) 0.74779(17) 0.27451(9) 0.0420(6) Uani 1 1 d . . . . . C18_6 C 1.0681(4) 0.7987(3) 0.31572(15) 0.0564(11) Uani 1 1 d . . . . . H02I_6 H 1.1754 0.7838 0.3258 0.068 Uiso 1 1 calc R U . . . H02J_6 H 1.0033 0.7745 0.3517 0.068 Uiso 1 1 calc R U . . . C19_6 C 1.0408(4) 0.9095(3) 0.29056(15) 0.0506(10) Uani 1 1 d . . . . . H02G_6 H 0.9354 0.9241 0.2780 0.061 Uiso 1 1 calc R U . . . H02H_6 H 1.0550 0.9451 0.3202 0.061 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 N1_1 0.0445(16) 0.0316(16) 0.0251(15) -0.0170(13) 0.0051(12) -0.0066(12) B2_1 0.0217(17) 0.0195(18) 0.0232(19) -0.0102(15) -0.0058(14) -0.0024(14) C3_1 0.0339(18) 0.0304(19) 0.0253(18) -0.0145(15) 0.0021(14) -0.0080(14) C4_1 0.0352(18) 0.0207(16) 0.0248(18) -0.0070(14) -0.0024(14) -0.0004(13) C5_1 0.0263(16) 0.0193(16) 0.0276(18) -0.0120(14) -0.0017(13) -0.0008(12) C6_1 0.0223(15) 0.0185(16) 0.0296(18) -0.0135(14) -0.0038(13) -0.0005(12) C7_1 0.0272(16) 0.0234(17) 0.0301(19) -0.0144(15) -0.0036(14) -0.0022(13) C8_1 0.0302(17) 0.0290(18) 0.0319(19) -0.0193(16) 0.0022(14) 0.0007(14) C9_1 0.0213(15) 0.0202(16) 0.0268(18) -0.0093(14) -0.0030(13) -0.0035(12) C10_1 0.0235(16) 0.0157(16) 0.0329(19) -0.0089(14) -0.0078(13) -0.0028(12) C11_1 0.0315(17) 0.0156(16) 0.041(2) -0.0130(15) -0.0042(15) -0.0003(13) C12_1 0.0302(17) 0.0244(17) 0.039(2) -0.0181(16) -0.0047(15) 0.0070(13) C13_1 0.0169(14) 0.0170(15) 0.0250(17) -0.0056(13) -0.0037(12) 0.0016(12) C14_1 0.0250(16) 0.0171(16) 0.0268(18) -0.0044(13) -0.0039(13) -0.0054(12) C15_1 0.0299(17) 0.0193(17) 0.037(2) -0.0041(15) -0.0035(14) -0.0089(13) C16_1 0.0307(17) 0.0119(15) 0.041(2) -0.0073(15) -0.0057(15) -0.0032(13) C17_1 0.0193(15) 0.0159(15) 0.0220(16) -0.0052(13) -0.0036(12) -0.0004(12) C18_1 0.0155(14) 0.0187(15) 0.0197(16) -0.0042(13) -0.0035(12) -0.0003(11) C19_1 0.0227(16) 0.0230(17) 0.0251(17) -0.0068(14) 0.0004(13) 0.0003(12) C20_1 0.0229(16) 0.0224(17) 0.0286(18) -0.0021(14) 0.0004(13) -0.0038(13) C21_1 0.0197(15) 0.0236(16) 0.0214(16) -0.0108(13) -0.0013(12) 0.0003(12) C22_1 0.0198(15) 0.0212(16) 0.0205(16) -0.0089(13) -0.0003(12) -0.0054(12) C23_1 0.0201(15) 0.0195(16) 0.0228(17) -0.0092(13) 0.0002(12) -0.0020(12) C24_1 0.0220(15) 0.0172(15) 0.0202(16) -0.0084(13) -0.0034(12) 0.0039(12) C1_2 0.0230(15) 0.0148(15) 0.0273(18) -0.0093(13) 0.0026(13) 0.0038(12) C2_2 0.0229(15) 0.0127(15) 0.0286(18) -0.0077(13) -0.0005(13) 0.0027(12) C3_2 0.0252(16) 0.0186(16) 0.040(2) -0.0084(15) 0.0041(14) -0.0027(13) C4_2 0.0317(18) 0.0191(17) 0.036(2) -0.0038(15) 0.0093(15) 0.0001(13) C5_2 0.0407(19) 0.0277(18) 0.0233(18) -0.0072(15) 0.0034(15) 0.0015(15) C6_2 0.0264(16) 0.0210(16) 0.0265(18) -0.0076(14) 0.0005(13) 0.0004(13) C7_2 0.0230(16) 0.0209(16) 0.0342(19) -0.0124(14) 0.0002(13) -0.0039(12) C8_2 0.047(2) 0.038(2) 0.047(2) -0.0060(18) 0.0173(17) -0.0088(17) C9_2 0.0411(19) 0.038(2) 0.0269(19) -0.0128(16) -0.0027(15) -0.0053(15) C1_3 0.0200(15) 0.0165(15) 0.0321(18) -0.0132(14) 0.0015(13) -0.0075(12) C2_3 0.0233(16) 0.0172(16) 0.0293(18) -0.0111(14) 0.0042(13) -0.0066(12) C3_3 0.0321(17) 0.0225(17) 0.0325(19) -0.0114(15) 0.0067(14) -0.0053(14) C4_3 0.0262(17) 0.0192(17) 0.042(2) -0.0145(15) 0.0126(15) -0.0081(13) C5_3 0.0220(16) 0.0140(16) 0.048(2) -0.0076(15) 0.0009(14) -0.0025(12) C6_3 0.0235(16) 0.0134(15) 0.0369(19) -0.0105(14) 0.0006(14) -0.0057(12) C7_3 0.0278(16) 0.0287(18) 0.0270(18) -0.0101(15) 0.0035(13) -0.0036(13) C8_3 0.041(2) 0.0253(19) 0.060(2) -0.0200(18) 0.0204(17) -0.0048(15) C9_3 0.0280(17) 0.0260(18) 0.041(2) -0.0112(16) -0.0048(14) -0.0012(13) C1_4 0.0345(18) 0.0289(18) 0.0239(18) -0.0087(15) -0.0027(14) 0.0005(14) C2_4 0.048(2) 0.036(2) 0.0213(19) -0.0083(16) -0.0050(15) -0.0023(16) C3_4 0.048(2) 0.033(2) 0.0247(19) -0.0011(16) -0.0016(15) 0.0001(16) C4_4 0.0331(18) 0.0265(18) 0.036(2) -0.0043(16) -0.0003(15) 0.0005(14) C5_4 0.0393(19) 0.0291(19) 0.031(2) -0.0139(16) -0.0035(15) -0.0006(15) C6_4 0.0370(18) 0.0324(19) 0.0204(17) -0.0080(15) -0.0040(14) -0.0003(14) C7_4 0.050(2) 0.033(2) 0.053(2) -0.0087(18) -0.0019(18) -0.0029(17) C1_5 0.045(2) 0.035(2) 0.0239(18) -0.0140(16) 0.0044(15) -0.0058(15) C2_5 0.043(2) 0.074(3) 0.045(2) -0.041(2) -0.0015(17) -0.0001(19) C3_5 0.053(2) 0.097(3) 0.063(3) -0.062(3) -0.003(2) -0.006(2) C4_5 0.057(2) 0.064(3) 0.046(2) -0.038(2) 0.0050(19) 0.001(2) C5_5 0.043(2) 0.056(2) 0.045(2) -0.023(2) 0.0144(18) -0.0073(18) C6_5 0.041(2) 0.041(2) 0.042(2) -0.0198(18) 0.0064(16) -0.0101(16) C7_5 0.079(3) 0.108(4) 0.084(3) -0.074(3) 0.008(3) 0.012(3) K1_6 0.0343(4) 0.0235(4) 0.0283(4) -0.0085(3) -0.0017(3) -0.0001(3) O2_6 0.0374(13) 0.0435(15) 0.0361(14) -0.0213(12) -0.0024(10) 0.0078(10) C3_6 0.040(2) 0.038(2) 0.056(2) -0.0286(19) -0.0149(18) 0.0104(16) C4_6 0.039(2) 0.034(2) 0.066(3) -0.0275(19) -0.0094(18) -0.0006(16) O5_6 0.0285(12) 0.0302(13) 0.0440(14) -0.0144(11) -0.0014(10) -0.0047(9) C6_6 0.0270(18) 0.0291(19) 0.060(3) -0.0075(18) 0.0052(17) -0.0041(14) C7_6 0.0343(19) 0.033(2) 0.042(2) -0.0014(17) 0.0057(16) 0.0002(15) O8_6 0.0392(12) 0.0275(12) 0.0301(13) -0.0056(10) -0.0019(10) 0.0032(10) C9_6 0.0363(19) 0.049(2) 0.029(2) -0.0099(17) 0.0035(15) 0.0014(16) C10_6 0.040(2) 0.044(2) 0.039(2) -0.0198(18) 0.0052(16) 0.0067(16) O11_6 0.0329(12) 0.0274(12) 0.0347(13) -0.0115(10) -0.0037(10) 0.0067(9) C12_6 0.0375(19) 0.032(2) 0.045(2) -0.0222(17) -0.0132(16) 0.0096(15) C13_6 0.0328(18) 0.0267(18) 0.056(2) -0.0169(17) -0.0175(17) 0.0003(14) O14_6 0.0324(12) 0.0272(12) 0.0393(14) -0.0081(11) -0.0005(10) -0.0071(9) C15_6 0.040(2) 0.036(2) 0.043(2) 0.0059(17) 0.0001(17) -0.0114(16) C16_6 0.051(2) 0.049(2) 0.037(2) 0.0035(19) 0.0045(17) -0.0097(18) O17_6 0.0479(14) 0.0453(15) 0.0308(14) -0.0077(12) 0.0003(11) -0.0022(11) C18_6 0.076(3) 0.066(3) 0.027(2) -0.014(2) 0.0021(19) -0.002(2) C19_6 0.057(2) 0.066(3) 0.037(2) -0.029(2) 0.0017(18) 0.007(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -1.00 1.00 1.00 0.0530 1.00 -1.00 -1.00 0.0880 0.00 1.00 1.00 0.0350 0.00 -1.00 -1.00 0.0350 0.00 0.00 1.00 0.0270 0.00 0.00 -1.00 0.0290 1.00 1.00 1.00 0.0900 -1.00 -1.00 -1.00 0.0640 0.00 -1.00 -2.00 0.0270 0.00 1.00 2.00 0.0250 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 C1_4 N1_1 C3_1 122.4(2) . . ? C1_4 N1_1 C1_5 117.2(2) . . ? C3_1 N1_1 C1_5 115.9(2) . . ? C23_1 B2_1 C1_3 120.2(2) . . ? C23_1 B2_1 C1_2 119.3(2) . . ? C1_3 B2_1 C1_2 120.4(2) . . ? C8_1 C3_1 C4_1 118.1(3) . . ? C8_1 C3_1 N1_1 121.5(3) . . ? C4_1 C3_1 N1_1 120.2(3) . . ? C5_1 C4_1 C3_1 120.8(3) . . ? C5_1 C4_1 H4_1 119.6 . . ? C3_1 C4_1 H4_1 119.6 . . ? C4_1 C5_1 C6_1 122.2(3) . . ? C4_1 C5_1 H5_1 118.9 . . ? C6_1 C5_1 H5_1 118.9 . . ? C7_1 C6_1 C5_1 116.2(3) . . ? C7_1 C6_1 C9_1 119.4(3) . . ? C5_1 C6_1 C9_1 124.2(2) . . ? C8_1 C7_1 C6_1 120.4(3) . . ? C8_1 C7_1 C12_1 120.0(3) . . ? C6_1 C7_1 C12_1 119.5(3) . . ? C3_1 C8_1 C7_1 121.7(3) . . ? C3_1 C8_1 H8_1 119.1 . . ? C7_1 C8_1 H8_1 119.1 . . ? C10_1 C9_1 C6_1 116.9(2) . . ? C10_1 C9_1 C13_1 117.8(3) . . ? C6_1 C9_1 C13_1 125.2(2) . . ? C16_1 C10_1 C9_1 120.7(3) . . ? C16_1 C10_1 C11_1 119.5(3) . . ? C9_1 C10_1 C11_1 119.8(3) . . ? C12_1 C11_1 C10_1 121.5(3) . . ? C12_1 C11_1 H11_1 119.2 . . ? C10_1 C11_1 H11_1 119.2 . . ? C11_1 C12_1 C7_1 120.3(3) . . ? C11_1 C12_1 H01D_1 119.9 . . ? C7_1 C12_1 H01D_1 119.9 . . ? C14_1 C13_1 C17_1 117.8(2) . . ? C14_1 C13_1 C9_1 117.0(2) . . ? C17_1 C13_1 C9_1 125.2(2) . . ? C15_1 C14_1 C20_1 120.2(3) . . ? C15_1 C14_1 C13_1 120.3(3) . . ? C20_1 C14_1 C13_1 119.4(3) . . ? C16_1 C15_1 C14_1 121.1(3) . . ? C16_1 C15_1 H01E_1 119.4 . . ? C14_1 C15_1 H01E_1 119.4 . . ? C15_1 C16_1 C10_1 120.1(3) . . ? C15_1 C16_1 H16_1 120.0 . . ? C10_1 C16_1 H16_1 120.0 . . ? C18_1 C17_1 C21_1 114.8(2) . . ? C18_1 C17_1 C13_1 120.2(2) . . ? C21_1 C17_1 C13_1 124.9(2) . . ? C24_1 C18_1 C17_1 121.0(2) . . ? C24_1 C18_1 C19_1 120.5(2) . . ? C17_1 C18_1 C19_1 118.5(2) . . ? C20_1 C19_1 C18_1 121.2(3) . . ? C20_1 C19_1 K1_6 74.78(16) . . ? C18_1 C19_1 K1_6 114.75(17) . . ? C20_1 C19_1 H19_1 119.4 . . ? C18_1 C19_1 H19_1 119.4 . . ? K1_6 C19_1 H19_1 80.9 . . ? C19_1 C20_1 C14_1 121.4(3) . . ? C19_1 C20_1 K1_6 81.19(16) . . ? C14_1 C20_1 K1_6 108.65(18) . . ? C19_1 C20_1 H20_1 119.3 . . ? C14_1 C20_1 H20_1 119.3 . . ? K1_6 C20_1 H20_1 80.2 . . ? C22_1 C21_1 C17_1 122.1(2) . . ? C22_1 C21_1 K1_6 88.53(16) . 1_455 ? C17_1 C21_1 K1_6 120.52(17) . 1_455 ? C22_1 C21_1 H21_1 119.0 . . ? C17_1 C21_1 H21_1 119.0 . . ? K1_6 C21_1 H21_1 60.2 1_455 . ? C21_1 C22_1 C23_1 123.9(2) . . ? C21_1 C22_1 K1_6 68.83(15) . 1_455 ? C23_1 C22_1 K1_6 131.17(18) . 1_455 ? C21_1 C22_1 H22_1 118.1 . . ? C23_1 C22_1 H22_1 118.1 . . ? K1_6 C22_1 H22_1 71.6 1_455 . ? C24_1 C23_1 C22_1 112.3(2) . . ? C24_1 C23_1 B2_1 123.8(2) . . ? C22_1 C23_1 B2_1 123.8(2) . . ? C18_1 C24_1 C23_1 124.6(2) . . ? C18_1 C24_1 H24_1 117.7 . . ? C23_1 C24_1 H24_1 117.7 . . ? C2_2 C1_2 C6_2 115.9(2) . . ? C2_2 C1_2 B2_1 121.6(3) . . ? C6_2 C1_2 B2_1 122.6(2) . . ? C3_2 C2_2 C1_2 121.2(3) . . ? C3_2 C2_2 C7_2 117.3(2) . . ? C1_2 C2_2 C7_2 121.5(2) . . ? C4_2 C3_2 C2_2 122.1(3) . . ? C4_2 C3_2 H3_2 118.9 . . ? C2_2 C3_2 H3_2 118.9 . . ? C3_2 C4_2 C5_2 117.4(3) . . ? C3_2 C4_2 C8_2 121.6(3) . . ? C5_2 C4_2 C8_2 121.0(3) . . ? C4_2 C5_2 C6_2 121.9(3) . . ? C4_2 C5_2 H5_2 119.1 . . ? C6_2 C5_2 H5_2 119.1 . . ? C5_2 C6_2 C1_2 121.4(3) . . ? C5_2 C6_2 C9_2 115.8(3) . . ? C1_2 C6_2 C9_2 122.7(2) . . ? C2_2 C7_2 H00C_2 109.5 . . ? C2_2 C7_2 H00D_2 109.5 . . ? H00C_2 C7_2 H00D_2 109.5 . . ? C2_2 C7_2 H00E_2 109.5 . . ? H00C_2 C7_2 H00E_2 109.5 . . ? H00D_2 C7_2 H00E_2 109.5 . . ? C4_2 C8_2 H025_2 109.5 . . ? C4_2 C8_2 H026_2 109.5 . . ? H025_2 C8_2 H026_2 109.5 . . ? C4_2 C8_2 H027_2 109.5 . . ? H025_2 C8_2 H027_2 109.5 . . ? H026_2 C8_2 H027_2 109.5 . . ? C6_2 C9_2 H01J_2 109.5 . . ? C6_2 C9_2 H01K_2 109.5 . . ? H01J_2 C9_2 H01K_2 109.5 . . ? C6_2 C9_2 H01L_2 109.5 . . ? H01J_2 C9_2 H01L_2 109.5 . . ? H01K_2 C9_2 H01L_2 109.5 . . ? C6_3 C1_3 C2_3 116.3(2) . . ? C6_3 C1_3 B2_1 120.5(3) . . ? C2_3 C1_3 B2_1 123.2(2) . . ? C3_3 C2_3 C1_3 120.6(3) . . ? C3_3 C2_3 C7_3 117.3(3) . . ? C1_3 C2_3 C7_3 122.1(2) . . ? C4_3 C3_3 C2_3 122.7(3) . . ? C4_3 C3_3 H3_3 118.7 . . ? C2_3 C3_3 H3_3 118.7 . . ? C3_3 C4_3 C5_3 117.1(3) . . ? C3_3 C4_3 C8_3 121.6(3) . . ? C5_3 C4_3 C8_3 121.3(3) . . ? C4_3 C5_3 C6_3 122.5(3) . . ? C4_3 C5_3 H5_3 118.7 . . ? C6_3 C5_3 H5_3 118.7 . . ? C5_3 C6_3 C1_3 120.8(3) . . ? C5_3 C6_3 C9_3 118.1(3) . . ? C1_3 C6_3 C9_3 121.1(2) . . ? C2_3 C7_3 H01A_3 109.5 . . ? C2_3 C7_3 H01B_3 109.5 . . ? H01A_3 C7_3 H01B_3 109.5 . . ? C2_3 C7_3 H01C_3 109.5 . . ? H01A_3 C7_3 H01C_3 109.5 . . ? H01B_3 C7_3 H01C_3 109.5 . . ? C4_3 C8_3 H01Q_3 109.5 . . ? C4_3 C8_3 H01R_3 109.5 . . ? H01Q_3 C8_3 H01R_3 109.5 . . ? C4_3 C8_3 H01S_3 109.5 . . ? H01Q_3 C8_3 H01S_3 109.5 . . ? H01R_3 C8_3 H01S_3 109.5 . . ? C6_3 C9_3 H01G_3 109.5 . . ? C6_3 C9_3 H01H_3 109.5 . . ? H01G_3 C9_3 H01H_3 109.5 . . ? C6_3 C9_3 H01I_3 109.5 . . ? H01G_3 C9_3 H01I_3 109.5 . . ? H01H_3 C9_3 H01I_3 109.5 . . ? C2_4 C1_4 C6_4 117.8(3) . . ? C2_4 C1_4 N1_1 119.0(3) . . ? C6_4 C1_4 N1_1 123.1(3) . . ? C3_4 C2_4 C1_4 120.8(3) . . ? C3_4 C2_4 H01F_4 119.6 . . ? C1_4 C2_4 H01F_4 119.6 . . ? C2_4 C3_4 C4_4 122.0(3) . . ? C2_4 C3_4 H01T_4 119.0 . . ? C4_4 C3_4 H01T_4 119.0 . . ? C3_4 C4_4 C5_4 116.9(3) . . ? C3_4 C4_4 C7_4 121.7(3) . . ? C5_4 C4_4 C7_4 121.4(3) . . ? C6_4 C5_4 C4_4 121.9(3) . . ? C6_4 C5_4 H5_4 119.1 . . ? C4_4 C5_4 H5_4 119.1 . . ? C5_4 C6_4 C1_4 120.5(3) . . ? C5_4 C6_4 H6_4 119.7 . . ? C1_4 C6_4 H6_4 119.7 . . ? C4_4 C7_4 H029_4 109.5 . . ? C4_4 C7_4 H02A_4 109.5 . . ? H029_4 C7_4 H02A_4 109.5 . . ? C4_4 C7_4 H02B_4 109.5 . . ? H029_4 C7_4 H02B_4 109.5 . . ? H02A_4 C7_4 H02B_4 109.5 . . ? C2_5 C1_5 C6_5 119.3(3) . . ? C2_5 C1_5 N1_1 119.3(3) . . ? C6_5 C1_5 N1_1 121.3(3) . . ? C1_5 C2_5 C3_5 120.0(3) . . ? C1_5 C2_5 H028_5 120.0 . . ? C3_5 C2_5 H028_5 120.0 . . ? C4_5 C3_5 C2_5 121.4(3) . . ? C4_5 C3_5 H02K_5 119.3 . . ? C2_5 C3_5 H02K_5 119.3 . . ? C5_5 C4_5 C3_5 117.5(3) . . ? C5_5 C4_5 C7_5 121.5(3) . . ? C3_5 C4_5 C7_5 121.0(3) . . ? C4_5 C5_5 C6_5 121.8(3) . . ? C4_5 C5_5 H024_5 119.1 . . ? C6_5 C5_5 H024_5 119.1 . . ? C1_5 C6_5 C5_5 119.9(3) . . ? C1_5 C6_5 H01Y_5 120.1 . . ? C5_5 C6_5 H01Y_5 120.1 . . ? C4_5 C7_5 H02L_5 109.5 . . ? C4_5 C7_5 H02M_5 109.5 . . ? H02L_5 C7_5 H02M_5 109.5 . . ? C4_5 C7_5 H02N_5 109.5 . . ? H02L_5 C7_5 H02N_5 109.5 . . ? H02M_5 C7_5 H02N_5 109.5 . . ? O14_6 K1_6 O2_6 119.66(7) . . ? O14_6 K1_6 O11_6 61.20(7) . . ? O2_6 K1_6 O11_6 175.20(6) . . ? O14_6 K1_6 O8_6 121.61(7) . . ? O2_6 K1_6 O8_6 118.45(7) . . ? O11_6 K1_6 O8_6 61.39(7) . . ? O14_6 K1_6 O17_6 59.92(7) . . ? O2_6 K1_6 O17_6 60.58(7) . . ? O11_6 K1_6 O17_6 119.19(7) . . ? O8_6 K1_6 O17_6 175.85(6) . . ? O14_6 K1_6 O5_6 175.32(6) . . ? O2_6 K1_6 O5_6 60.31(7) . . ? O11_6 K1_6 O5_6 118.39(7) . . ? O8_6 K1_6 O5_6 59.13(6) . . ? O17_6 K1_6 O5_6 118.99(7) . . ? O14_6 K1_6 C20_1 102.92(7) . . ? O2_6 K1_6 C20_1 89.61(7) . . ? O11_6 K1_6 C20_1 85.62(7) . . ? O8_6 K1_6 C20_1 82.42(7) . . ? O17_6 K1_6 C20_1 93.49(7) . . ? O5_6 K1_6 C20_1 72.46(7) . . ? O14_6 K1_6 C19_1 80.07(7) . . ? O2_6 K1_6 C19_1 107.48(7) . . ? O11_6 K1_6 C19_1 67.80(7) . . ? O8_6 K1_6 C19_1 88.05(7) . . ? O17_6 K1_6 C19_1 88.48(7) . . ? O5_6 K1_6 C19_1 95.43(6) . . ? C20_1 K1_6 C19_1 24.03(7) . . ? O14_6 K1_6 C21_1 87.45(7) . 1_655 ? O2_6 K1_6 C21_1 88.94(7) . 1_655 ? O11_6 K1_6 C21_1 95.84(6) . 1_655 ? O8_6 K1_6 C21_1 88.49(7) . 1_655 ? O17_6 K1_6 C21_1 95.48(7) . 1_655 ? O5_6 K1_6 C21_1 97.22(6) . 1_655 ? C20_1 K1_6 C21_1 168.77(7) . 1_655 ? C19_1 K1_6 C21_1 162.81(7) . 1_655 ? O14_6 K1_6 C22_1 66.54(6) . 1_655 ? O2_6 K1_6 C22_1 106.51(7) . 1_655 ? O11_6 K1_6 C22_1 78.23(6) . 1_655 ? O8_6 K1_6 C22_1 92.42(6) . 1_655 ? O17_6 K1_6 C22_1 91.71(7) . 1_655 ? O5_6 K1_6 C22_1 118.12(6) . 1_655 ? C20_1 K1_6 C22_1 163.55(7) . 1_655 ? C19_1 K1_6 C22_1 140.89(7) . 1_655 ? C21_1 K1_6 C22_1 22.64(6) 1_655 1_655 ? C19_6 O2_6 C3_6 111.9(2) . . ? C19_6 O2_6 K1_6 116.97(19) . . ? C3_6 O2_6 K1_6 118.27(18) . . ? O2_6 C3_6 C4_6 108.8(3) . . ? O2_6 C3_6 H014_6 109.9 . . ? C4_6 C3_6 H014_6 109.9 . . ? O2_6 C3_6 H015_6 109.9 . . ? C4_6 C3_6 H015_6 109.9 . . ? H014_6 C3_6 H015_6 108.3 . . ? O5_6 C4_6 C3_6 110.1(2) . . ? O5_6 C4_6 H02C_6 109.6 . . ? C3_6 C4_6 H02C_6 109.6 . . ? O5_6 C4_6 H02D_6 109.6 . . ? C3_6 C4_6 H02D_6 109.6 . . ? H02C_6 C4_6 H02D_6 108.1 . . ? C6_6 O5_6 C4_6 111.4(2) . . ? C6_6 O5_6 K1_6 111.45(16) . . ? C4_6 O5_6 K1_6 109.86(18) . . ? O5_6 C6_6 C7_6 108.9(2) . . ? O5_6 C6_6 H01W_6 109.9 . . ? C7_6 C6_6 H01W_6 109.9 . . ? O5_6 C6_6 H01X_6 109.9 . . ? C7_6 C6_6 H01X_6 109.9 . . ? H01W_6 C6_6 H01X_6 108.3 . . ? O8_6 C7_6 C6_6 108.2(3) . . ? O8_6 C7_6 H01U_6 110.1 . . ? C6_6 C7_6 H01U_6 110.1 . . ? O8_6 C7_6 H01V_6 110.1 . . ? C6_6 C7_6 H01V_6 110.1 . . ? H01U_6 C7_6 H01V_6 108.4 . . ? C9_6 O8_6 C7_6 113.1(2) . . ? C9_6 O8_6 K1_6 112.85(17) . . ? C7_6 O8_6 K1_6 118.10(17) . . ? O8_6 C9_6 C10_6 109.2(3) . . ? O8_6 C9_6 H01Z_6 109.8 . . ? C10_6 C9_6 H01Z_6 109.8 . . ? O8_6 C9_6 H010_6 109.8 . . ? C10_6 C9_6 H010_6 109.8 . . ? H01Z_6 C9_6 H010_6 108.3 . . ? O11_6 C10_6 C9_6 108.5(2) . . ? O11_6 C10_6 H020_6 110.0 . . ? C9_6 C10_6 H020_6 110.0 . . ? O11_6 C10_6 H021_6 110.0 . . ? C9_6 C10_6 H021_6 110.0 . . ? H020_6 C10_6 H021_6 108.4 . . ? C10_6 O11_6 C12_6 111.9(2) . . ? C10_6 O11_6 K1_6 112.18(17) . . ? C12_6 O11_6 K1_6 111.01(17) . . ? O11_6 C12_6 C13_6 110.0(2) . . ? O11_6 C12_6 H01O_6 109.7 . . ? C13_6 C12_6 H01O_6 109.7 . . ? O11_6 C12_6 H01P_6 109.7 . . ? C13_6 C12_6 H01P_6 109.7 . . ? H01O_6 C12_6 H01P_6 108.2 . . ? O14_6 C13_6 C12_6 109.0(2) . . ? O14_6 C13_6 H01M_6 109.9 . . ? C12_6 C13_6 H01M_6 109.9 . . ? O14_6 C13_6 H01N_6 109.9 . . ? C12_6 C13_6 H01N_6 109.9 . . ? H01M_6 C13_6 H01N_6 108.3 . . ? C13_6 O14_6 C15_6 112.7(2) . . ? C13_6 O14_6 K1_6 117.70(17) . . ? C15_6 O14_6 K1_6 118.62(18) . . ? O14_6 C15_6 C16_6 108.2(3) . . ? O14_6 C15_6 H022_6 110.1 . . ? C16_6 C15_6 H022_6 110.1 . . ? O14_6 C15_6 H023_6 110.1 . . ? C16_6 C15_6 H023_6 110.1 . . ? H022_6 C15_6 H023_6 108.4 . . ? O17_6 C16_6 C15_6 109.8(3) . . ? O17_6 C16_6 H02E_6 109.7 . . ? C15_6 C16_6 H02E_6 109.7 . . ? O17_6 C16_6 H02F_6 109.7 . . ? C15_6 C16_6 H02F_6 109.7 . . ? H02E_6 C16_6 H02F_6 108.2 . . ? C16_6 O17_6 C18_6 112.6(3) . . ? C16_6 O17_6 K1_6 113.29(18) . . ? C18_6 O17_6 K1_6 112.07(19) . . ? O17_6 C18_6 C19_6 109.3(3) . . ? O17_6 C18_6 H02I_6 109.8 . . ? C19_6 C18_6 H02I_6 109.8 . . ? O17_6 C18_6 H02J_6 109.8 . . ? C19_6 C18_6 H02J_6 109.8 . . ? H02I_6 C18_6 H02J_6 108.3 . . ? O2_6 C19_6 C18_6 108.9(3) . . ? O2_6 C19_6 H02G_6 109.9 . . ? C18_6 C19_6 H02G_6 109.9 . . ? O2_6 C19_6 H02H_6 109.9 . . ? C18_6 C19_6 H02H_6 109.9 . . ? H02G_6 C19_6 H02H_6 108.3 . . ? 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 N1_1 C1_4 1.419(4) . ? N1_1 C3_1 1.420(4) . ? N1_1 C1_5 1.436(4) . ? B2_1 C23_1 1.520(4) . ? B2_1 C1_3 1.597(4) . ? B2_1 C1_2 1.605(4) . ? C3_1 C8_1 1.373(4) . ? C3_1 C4_1 1.416(4) . ? C4_1 C5_1 1.369(4) . ? C4_1 H4_1 0.9500 . ? C5_1 C6_1 1.422(4) . ? C5_1 H5_1 0.9500 . ? C6_1 C7_1 1.420(4) . ? C6_1 C9_1 1.447(4) . ? C7_1 C8_1 1.409(4) . ? C7_1 C12_1 1.433(4) . ? C8_1 H8_1 0.9500 . ? C9_1 C10_1 1.424(4) . ? C9_1 C13_1 1.457(4) . ? C10_1 C16_1 1.409(4) . ? C10_1 C11_1 1.430(4) . ? C11_1 C12_1 1.341(4) . ? C11_1 H11_1 0.9500 . ? C12_1 H01D_1 0.9500 . ? C13_1 C14_1 1.430(4) . ? C13_1 C17_1 1.437(4) . ? C14_1 C15_1 1.409(4) . ? C14_1 C20_1 1.426(4) . ? C15_1 C16_1 1.364(4) . ? C15_1 H01E_1 0.9500 . ? C16_1 H16_1 0.9500 . ? C17_1 C18_1 1.428(4) . ? C17_1 C21_1 1.436(3) . ? C18_1 C24_1 1.387(3) . ? C18_1 C19_1 1.431(4) . ? C19_1 C20_1 1.353(4) . ? C19_1 K1_6 3.283(3) . ? C19_1 H19_1 0.9500 . ? C20_1 K1_6 3.206(3) . ? C20_1 H20_1 0.9500 . ? C21_1 C22_1 1.360(3) . ? C21_1 K1_6 3.296(3) 1_455 ? C21_1 H21_1 0.9500 . ? C22_1 C23_1 1.445(4) . ? C22_1 K1_6 3.534(3) 1_455 ? C22_1 H22_1 0.9500 . ? C23_1 C24_1 1.417(4) . ? C24_1 H24_1 0.9500 . ? C1_2 C2_2 1.416(4) . ? C1_2 C6_2 1.416(4) . ? C2_2 C3_2 1.394(4) . ? C2_2 C7_2 1.513(4) . ? C3_2 C4_2 1.381(4) . ? C3_2 H3_2 0.9500 . ? C4_2 C5_2 1.387(4) . ? C4_2 C8_2 1.519(4) . ? C5_2 C6_2 1.393(4) . ? C5_2 H5_2 0.9500 . ? C6_2 C9_2 1.525(4) . ? C7_2 H00C_2 0.9800 . ? C7_2 H00D_2 0.9800 . ? C7_2 H00E_2 0.9800 . ? C8_2 H025_2 0.9800 . ? C8_2 H026_2 0.9800 . ? C8_2 H027_2 0.9800 . ? C9_2 H01J_2 0.9800 . ? C9_2 H01K_2 0.9800 . ? C9_2 H01L_2 0.9800 . ? C1_3 C6_3 1.416(4) . ? C1_3 C2_3 1.419(4) . ? C2_3 C3_3 1.396(4) . ? C2_3 C7_3 1.507(4) . ? C3_3 C4_3 1.378(4) . ? C3_3 H3_3 0.9500 . ? C4_3 C5_3 1.378(4) . ? C4_3 C8_3 1.518(4) . ? C5_3 C6_3 1.396(4) . ? C5_3 H5_3 0.9500 . ? C6_3 C9_3 1.509(4) . ? C7_3 H01A_3 0.9800 . ? C7_3 H01B_3 0.9800 . ? C7_3 H01C_3 0.9800 . ? C8_3 H01Q_3 0.9800 . ? C8_3 H01R_3 0.9800 . ? C8_3 H01S_3 0.9800 . ? C9_3 H01G_3 0.9800 . ? C9_3 H01H_3 0.9800 . ? C9_3 H01I_3 0.9800 . ? C1_4 C2_4 1.388(4) . ? C1_4 C6_4 1.393(4) . ? C2_4 C3_4 1.378(4) . ? C2_4 H01F_4 0.9500 . ? C3_4 C4_4 1.386(4) . ? C3_4 H01T_4 0.9500 . ? C4_4 C5_4 1.386(4) . ? C4_4 C7_4 1.507(4) . ? C5_4 C6_4 1.385(4) . ? C5_4 H5_4 0.9500 . ? C6_4 H6_4 0.9500 . ? C7_4 H029_4 0.9800 . ? C7_4 H02A_4 0.9800 . ? C7_4 H02B_4 0.9800 . ? C1_5 C2_5 1.381(4) . ? C1_5 C6_5 1.382(4) . ? C2_5 C3_5 1.391(4) . ? C2_5 H028_5 0.9500 . ? C3_5 C4_5 1.385(5) . ? C3_5 H02K_5 0.9500 . ? C4_5 C5_5 1.381(5) . ? C4_5 C7_5 1.514(5) . ? C5_5 C6_5 1.388(4) . ? C5_5 H024_5 0.9500 . ? C6_5 H01Y_5 0.9500 . ? C7_5 H02L_5 0.9800 . ? C7_5 H02M_5 0.9800 . ? C7_5 H02N_5 0.9800 . ? K1_6 O14_6 2.743(2) . ? K1_6 O2_6 2.746(2) . ? K1_6 O11_6 2.792(2) . ? K1_6 O8_6 2.796(2) . ? K1_6 O17_6 2.820(2) . ? K1_6 O5_6 2.888(2) . ? K1_6 C21_1 3.296(3) 1_655 ? K1_6 C22_1 3.534(3) 1_655 ? O2_6 C19_6 1.418(4) . ? O2_6 C3_6 1.425(4) . ? C3_6 C4_6 1.483(4) . ? C3_6 H014_6 0.9900 . ? C3_6 H015_6 0.9900 . ? C4_6 O5_6 1.421(4) . ? C4_6 H02C_6 0.9900 . ? C4_6 H02D_6 0.9900 . ? O5_6 C6_6 1.418(3) . ? C6_6 C7_6 1.482(4) . ? C6_6 H01W_6 0.9900 . ? C6_6 H01X_6 0.9900 . ? C7_6 O8_6 1.426(3) . ? C7_6 H01U_6 0.9900 . ? C7_6 H01V_6 0.9900 . ? O8_6 C9_6 1.417(4) . ? C9_6 C10_6 1.490(4) . ? C9_6 H01Z_6 0.9900 . ? C9_6 H010_6 0.9900 . ? C10_6 O11_6 1.424(3) . ? C10_6 H020_6 0.9900 . ? C10_6 H021_6 0.9900 . ? O11_6 C12_6 1.433(3) . ? C12_6 C13_6 1.488(4) . ? C12_6 H01O_6 0.9900 . ? C12_6 H01P_6 0.9900 . ? C13_6 O14_6 1.420(3) . ? C13_6 H01M_6 0.9900 . ? C13_6 H01N_6 0.9900 . ? O14_6 C15_6 1.424(3) . ? C15_6 C16_6 1.486(5) . ? C15_6 H022_6 0.9900 . ? C15_6 H023_6 0.9900 . ? C16_6 O17_6 1.413(4) . ? C16_6 H02E_6 0.9900 . ? C16_6 H02F_6 0.9900 . ? O17_6 C18_6 1.423(4) . ? C18_6 C19_6 1.482(5) . ? C18_6 H02I_6 0.9900 . ? C18_6 H02J_6 0.9900 . ? C19_6 H02G_6 0.9900 . ? C19_6 H02H_6 0.9900 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1_4 N1_1 C3_1 C8_1 137.0(3) . . . . ? C1_5 N1_1 C3_1 C8_1 -18.7(4) . . . . ? C1_4 N1_1 C3_1 C4_1 -48.0(4) . . . . ? C1_5 N1_1 C3_1 C4_1 156.3(3) . . . . ? C8_1 C3_1 C4_1 C5_1 -5.7(4) . . . . ? N1_1 C3_1 C4_1 C5_1 179.2(2) . . . . ? C3_1 C4_1 C5_1 C6_1 1.7(4) . . . . ? C4_1 C5_1 C6_1 C7_1 5.5(4) . . . . ? C4_1 C5_1 C6_1 C9_1 179.8(3) . . . . ? C5_1 C6_1 C7_1 C8_1 -9.0(4) . . . . ? C9_1 C6_1 C7_1 C8_1 176.5(2) . . . . ? C5_1 C6_1 C7_1 C12_1 166.5(2) . . . . ? C9_1 C6_1 C7_1 C12_1 -8.0(4) . . . . ? C4_1 C3_1 C8_1 C7_1 2.1(4) . . . . ? N1_1 C3_1 C8_1 C7_1 177.2(3) . . . . ? C6_1 C7_1 C8_1 C3_1 5.4(4) . . . . ? C12_1 C7_1 C8_1 C3_1 -170.0(3) . . . . ? C7_1 C6_1 C9_1 C10_1 17.8(4) . . . . ? C5_1 C6_1 C9_1 C10_1 -156.2(3) . . . . ? C7_1 C6_1 C9_1 C13_1 -165.9(2) . . . . ? C5_1 C6_1 C9_1 C13_1 20.1(4) . . . . ? C6_1 C9_1 C10_1 C16_1 165.4(2) . . . . ? C13_1 C9_1 C10_1 C16_1 -11.2(4) . . . . ? C6_1 C9_1 C10_1 C11_1 -15.3(4) . . . . ? C13_1 C9_1 C10_1 C11_1 168.1(2) . . . . ? C16_1 C10_1 C11_1 C12_1 -178.0(3) . . . . ? C9_1 C10_1 C11_1 C12_1 2.8(4) . . . . ? C10_1 C11_1 C12_1 C7_1 7.7(4) . . . . ? C8_1 C7_1 C12_1 C11_1 170.5(3) . . . . ? C6_1 C7_1 C12_1 C11_1 -5.0(4) . . . . ? C10_1 C9_1 C13_1 C14_1 20.1(4) . . . . ? C6_1 C9_1 C13_1 C14_1 -156.2(3) . . . . ? C10_1 C9_1 C13_1 C17_1 -156.0(3) . . . . ? C6_1 C9_1 C13_1 C17_1 27.7(4) . . . . ? C17_1 C13_1 C14_1 C15_1 161.5(2) . . . . ? C9_1 C13_1 C14_1 C15_1 -14.9(4) . . . . ? C17_1 C13_1 C14_1 C20_1 -13.8(4) . . . . ? C9_1 C13_1 C14_1 C20_1 169.8(2) . . . . ? C20_1 C14_1 C15_1 C16_1 175.3(3) . . . . ? C13_1 C14_1 C15_1 C16_1 0.1(4) . . . . ? C14_1 C15_1 C16_1 C10_1 9.6(4) . . . . ? C9_1 C10_1 C16_1 C15_1 -3.9(4) . . . . ? C11_1 C10_1 C16_1 C15_1 176.9(3) . . . . ? C14_1 C13_1 C17_1 C18_1 14.0(4) . . . . ? C9_1 C13_1 C17_1 C18_1 -169.9(2) . . . . ? C14_1 C13_1 C17_1 C21_1 -161.8(3) . . . . ? C9_1 C13_1 C17_1 C21_1 14.2(4) . . . . ? C21_1 C17_1 C18_1 C24_1 -9.3(4) . . . . ? C13_1 C17_1 C18_1 C24_1 174.5(2) . . . . ? C21_1 C17_1 C18_1 C19_1 170.6(2) . . . . ? C13_1 C17_1 C18_1 C19_1 -5.6(4) . . . . ? C24_1 C18_1 C19_1 C20_1 176.6(3) . . . . ? C17_1 C18_1 C19_1 C20_1 -3.3(4) . . . . ? C24_1 C18_1 C19_1 K1_6 -96.8(3) . . . . ? C17_1 C18_1 C19_1 K1_6 83.3(3) . . . . ? C18_1 C19_1 C20_1 C14_1 3.5(4) . . . . ? K1_6 C19_1 C20_1 C14_1 -106.5(3) . . . . ? C18_1 C19_1 C20_1 K1_6 110.0(2) . . . . ? C15_1 C14_1 C20_1 C19_1 -170.0(3) . . . . ? C13_1 C14_1 C20_1 C19_1 5.3(4) . . . . ? C15_1 C14_1 C20_1 K1_6 99.1(3) . . . . ? C13_1 C14_1 C20_1 K1_6 -85.6(3) . . . . ? C18_1 C17_1 C21_1 C22_1 9.1(4) . . . . ? C13_1 C17_1 C21_1 C22_1 -174.9(3) . . . . ? C18_1 C17_1 C21_1 K1_6 -100.5(2) . . . 1_455 ? C13_1 C17_1 C21_1 K1_6 75.6(3) . . . 1_455 ? C17_1 C21_1 C22_1 C23_1 0.5(4) . . . . ? K1_6 C21_1 C22_1 C23_1 126.2(2) 1_455 . . . ? C17_1 C21_1 C22_1 K1_6 -125.7(3) . . . 1_455 ? C21_1 C22_1 C23_1 C24_1 -9.5(4) . . . . ? K1_6 C22_1 C23_1 C24_1 81.1(3) 1_455 . . . ? C21_1 C22_1 C23_1 B2_1 166.9(3) . . . . ? K1_6 C22_1 C23_1 B2_1 -102.6(3) 1_455 . . . ? C1_3 B2_1 C23_1 C24_1 -4.8(4) . . . . ? C1_2 B2_1 C23_1 C24_1 171.9(2) . . . . ? C1_3 B2_1 C23_1 C22_1 179.3(2) . . . . ? C1_2 B2_1 C23_1 C22_1 -4.0(4) . . . . ? C17_1 C18_1 C24_1 C23_1 0.0(4) . . . . ? C19_1 C18_1 C24_1 C23_1 -179.9(3) . . . . ? C22_1 C23_1 C24_1 C18_1 9.2(4) . . . . ? B2_1 C23_1 C24_1 C18_1 -167.1(3) . . . . ? C23_1 B2_1 C1_2 C2_2 125.2(3) . . . . ? C1_3 B2_1 C1_2 C2_2 -58.2(4) . . . . ? C23_1 B2_1 C1_2 C6_2 -55.2(4) . . . . ? C1_3 B2_1 C1_2 C6_2 121.4(3) . . . . ? C6_2 C1_2 C2_2 C3_2 4.1(4) . . . . ? B2_1 C1_2 C2_2 C3_2 -176.3(2) . . . . ? C6_2 C1_2 C2_2 C7_2 -175.1(2) . . . . ? B2_1 C1_2 C2_2 C7_2 4.5(4) . . . . ? C1_2 C2_2 C3_2 C4_2 -2.4(4) . . . . ? C7_2 C2_2 C3_2 C4_2 176.8(3) . . . . ? C2_2 C3_2 C4_2 C5_2 -1.3(4) . . . . ? C2_2 C3_2 C4_2 C8_2 179.4(3) . . . . ? C3_2 C4_2 C5_2 C6_2 3.2(4) . . . . ? C8_2 C4_2 C5_2 C6_2 -177.5(3) . . . . ? C4_2 C5_2 C6_2 C1_2 -1.4(4) . . . . ? C4_2 C5_2 C6_2 C9_2 -177.7(3) . . . . ? C2_2 C1_2 C6_2 C5_2 -2.2(4) . . . . ? B2_1 C1_2 C6_2 C5_2 178.1(3) . . . . ? C2_2 C1_2 C6_2 C9_2 173.8(2) . . . . ? B2_1 C1_2 C6_2 C9_2 -5.8(4) . . . . ? C23_1 B2_1 C1_3 C6_3 117.5(3) . . . . ? C1_2 B2_1 C1_3 C6_3 -59.1(3) . . . . ? C23_1 B2_1 C1_3 C2_3 -61.1(4) . . . . ? C1_2 B2_1 C1_3 C2_3 122.3(3) . . . . ? C6_3 C1_3 C2_3 C3_3 1.0(4) . . . . ? B2_1 C1_3 C2_3 C3_3 179.7(2) . . . . ? C6_3 C1_3 C2_3 C7_3 179.0(2) . . . . ? B2_1 C1_3 C2_3 C7_3 -2.3(4) . . . . ? C1_3 C2_3 C3_3 C4_3 -0.6(4) . . . . ? C7_3 C2_3 C3_3 C4_3 -178.7(2) . . . . ? C2_3 C3_3 C4_3 C5_3 -0.6(4) . . . . ? C2_3 C3_3 C4_3 C8_3 177.9(3) . . . . ? C3_3 C4_3 C5_3 C6_3 1.3(4) . . . . ? C8_3 C4_3 C5_3 C6_3 -177.1(3) . . . . ? C4_3 C5_3 C6_3 C1_3 -0.9(4) . . . . ? C4_3 C5_3 C6_3 C9_3 179.3(2) . . . . ? C2_3 C1_3 C6_3 C5_3 -0.3(4) . . . . ? B2_1 C1_3 C6_3 C5_3 -179.0(2) . . . . ? C2_3 C1_3 C6_3 C9_3 179.5(2) . . . . ? B2_1 C1_3 C6_3 C9_3 0.7(4) . . . . ? C3_1 N1_1 C1_4 C2_4 168.2(3) . . . . ? C1_5 N1_1 C1_4 C2_4 -36.4(4) . . . . ? C3_1 N1_1 C1_4 C6_4 -14.1(4) . . . . ? C1_5 N1_1 C1_4 C6_4 141.3(3) . . . . ? C6_4 C1_4 C2_4 C3_4 -1.0(4) . . . . ? N1_1 C1_4 C2_4 C3_4 176.8(3) . . . . ? C1_4 C2_4 C3_4 C4_4 0.9(5) . . . . ? C2_4 C3_4 C4_4 C5_4 0.1(5) . . . . ? C2_4 C3_4 C4_4 C7_4 -179.1(3) . . . . ? C3_4 C4_4 C5_4 C6_4 -0.8(4) . . . . ? C7_4 C4_4 C5_4 C6_4 178.3(3) . . . . ? C4_4 C5_4 C6_4 C1_4 0.7(4) . . . . ? C2_4 C1_4 C6_4 C5_4 0.3(4) . . . . ? N1_1 C1_4 C6_4 C5_4 -177.4(3) . . . . ? C1_4 N1_1 C1_5 C2_5 127.9(3) . . . . ? C3_1 N1_1 C1_5 C2_5 -75.1(4) . . . . ? C1_4 N1_1 C1_5 C6_5 -54.9(4) . . . . ? C3_1 N1_1 C1_5 C6_5 102.2(3) . . . . ? C6_5 C1_5 C2_5 C3_5 -0.8(5) . . . . ? N1_1 C1_5 C2_5 C3_5 176.5(3) . . . . ? C1_5 C2_5 C3_5 C4_5 0.9(6) . . . . ? C2_5 C3_5 C4_5 C5_5 -0.1(6) . . . . ? C2_5 C3_5 C4_5 C7_5 179.5(4) . . . . ? C3_5 C4_5 C5_5 C6_5 -0.7(6) . . . . ? C7_5 C4_5 C5_5 C6_5 179.7(4) . . . . ? C2_5 C1_5 C6_5 C5_5 0.0(5) . . . . ? N1_1 C1_5 C6_5 C5_5 -177.3(3) . . . . ? C4_5 C5_5 C6_5 C1_5 0.8(5) . . . . ? C19_6 O2_6 C3_6 C4_6 176.1(3) . . . . ? K1_6 O2_6 C3_6 C4_6 -43.4(3) . . . . ? O2_6 C3_6 C4_6 O5_6 65.6(3) . . . . ? C3_6 C4_6 O5_6 C6_6 -177.3(3) . . . . ? C3_6 C4_6 O5_6 K1_6 -53.3(3) . . . . ? C4_6 O5_6 C6_6 C7_6 178.2(3) . . . . ? K1_6 O5_6 C6_6 C7_6 55.1(3) . . . . ? O5_6 C6_6 C7_6 O8_6 -66.3(3) . . . . ? C6_6 C7_6 O8_6 C9_6 179.0(2) . . . . ? C6_6 C7_6 O8_6 K1_6 44.1(3) . . . . ? C7_6 O8_6 C9_6 C10_6 173.6(2) . . . . ? K1_6 O8_6 C9_6 C10_6 -49.1(3) . . . . ? O8_6 C9_6 C10_6 O11_6 69.2(3) . . . . ? C9_6 C10_6 O11_6 C12_6 -177.6(2) . . . . ? C9_6 C10_6 O11_6 K1_6 -52.0(3) . . . . ? C10_6 O11_6 C12_6 C13_6 -179.5(2) . . . . ? K1_6 O11_6 C12_6 C13_6 54.3(3) . . . . ? O11_6 C12_6 C13_6 O14_6 -63.1(3) . . . . ? C12_6 C13_6 O14_6 C15_6 -176.7(2) . . . . ? C12_6 C13_6 O14_6 K1_6 39.5(3) . . . . ? C13_6 O14_6 C15_6 C16_6 173.2(3) . . . . ? K1_6 O14_6 C15_6 C16_6 -43.4(3) . . . . ? O14_6 C15_6 C16_6 O17_6 62.2(3) . . . . ? C15_6 C16_6 O17_6 C18_6 -179.5(3) . . . . ? C15_6 C16_6 O17_6 K1_6 -51.0(3) . . . . ? C16_6 O17_6 C18_6 C19_6 -179.2(3) . . . . ? K1_6 O17_6 C18_6 C19_6 51.7(3) . . . . ? C3_6 O2_6 C19_6 C18_6 -173.9(3) . . . . ? K1_6 O2_6 C19_6 C18_6 45.1(3) . . . . ? O17_6 C18_6 C19_6 O2_6 -64.8(4) . . . . ?