#------------------------------------------------------------------------------ #$Date: 2020-08-22 05:19:28 +0300 (Sat, 22 Aug 2020) $ #$Revision: 255578 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/52/7705248.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_7705248 loop_ _publ_author_name 'Hill, Anthony' 'Frogley, Benjamin' _publ_section_title ; Carbyne decorated porphyrins ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D0DT02809F _journal_year 2020 _chemical_formula_moiety 'C23 H26 B N7 O2 W' _chemical_formula_sum 'C23 H26 B N7 O2 W' _chemical_formula_weight 627.17 _space_group_crystal_system orthorhombic _space_group_IT_number 33 _space_group_name_Hall 'P 2c -2n' _space_group_name_H-M_alt 'P n a 21' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2020-06-08 deposited with the CCDC. 2020-08-21 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 31.9296(6) _cell_length_b 8.15350(10) _cell_length_c 18.8459(3) _cell_measurement_reflns_used 11510 _cell_measurement_temperature 150.0(1) _cell_measurement_theta_max 70.5300 _cell_measurement_theta_min 5.4580 _cell_volume 4906.30(13) _computing_cell_refinement 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT-2018/3 (Sheldrick, 2018)' _diffrn_ambient_temperature 150.0(1) _diffrn_detector_area_resol_mean 8.1297 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, EosS2' _diffrn_measurement_method '\w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0381 _diffrn_reflns_av_unetI/netI 0.0445 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 27305 _diffrn_reflns_point_group_measured_fraction_full 0.957 _diffrn_reflns_point_group_measured_fraction_max 0.945 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 70.870 _diffrn_reflns_theta_min 3.628 _diffrn_source 'micro-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 9.008 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.89932 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear orange' _exptl_crystal_density_diffrn 1.698 _exptl_crystal_description plate _exptl_crystal_F_000 2464 _exptl_crystal_size_max 0.099 _exptl_crystal_size_mid 0.053 _exptl_crystal_size_min 0.044 _refine_diff_density_max 2.423 _refine_diff_density_min -1.612 _refine_diff_density_rms 0.131 _refine_ls_abs_structure_details ; Flack x determined using 3299 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.005(8) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 610 _refine_ls_number_reflns 8918 _refine_ls_number_restraints 12 _refine_ls_restrained_S_all 1.110 _refine_ls_R_factor_all 0.0565 _refine_ls_R_factor_gt 0.0515 _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^)+(0.0434P)^2^+28.1869P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1198 _refine_ls_wR_factor_ref 0.1226 _reflns_Friedel_coverage 0.842 _reflns_Friedel_fraction_full 0.911 _reflns_Friedel_fraction_max 0.893 _reflns_number_gt 8288 _reflns_number_total 8918 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02809f2.cif _cod_data_source_block Compound_9 _cod_database_code 7705248 _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_res_file ; TITL bf3pynmr2_b.res in Pna2(1) shelx.res created by SHELXL-2018/3 at 11:03:16 on 05-Jun-2020 CELL 1.54184 31.9296 8.1535 18.8459 90.000 90.000 90.000 ZERR 8.00 0.0006 0.0001 0.0003 0.000 0.000 0.000 LATT -1 SYMM - X, - Y, 1/2 + Z SYMM 1/2 + X, 1/2 - Y, Z SYMM 1/2 - X, 1/2 + Y, 1/2 + Z SFAC C H B N O W UNIT 184 208 8 56 16 8 MERG 2 OMIT 1 4 -18 OMIT 1 4 -20 OMIT 1 9 -7 OMIT 1 4 18 TWIN -1.00 0.00 0.00 0.00 1.00 0.00 0.00 0.00 -1.00 2 DFIX 1.84 W2 C101 W3 C109 EADP B3 B2 DFIX 1.47 C101 C104 C109 C110 DFIX 1.15 B1 H1 B2 H2 B3 H3 DFIX 1.5 C142 C140 C148 C146 DFIX 1.37 C144 C146 C142 C144 MORE -1 FMAP 2 PLAN 5 ACTA BOND $H CONF LIST 6 L.S. 8 WGHT 0.043400 28.186901 BASF 0.36466 FVAR 1.70062 0.56307 W1 6 0.046362 0.134627 0.083059 11.00000 0.03258 0.02310 = 0.02432 0.00031 -0.00046 0.00039 PART 1 W2 6 0.200556 0.526922 0.435750 21.00000 0.03957 0.04497 = 0.05089 -0.00050 -0.00855 0.00030 PART 2 W3 6 0.215869 0.585783 0.378364 -21.00000 0.05096 0.03652 = 0.06394 -0.00028 -0.01639 -0.00109 PART 0 N5 4 0.079994 0.009238 0.171269 11.00000 0.03919 0.03209 = 0.01459 0.00036 -0.00071 0.00551 N3 4 0.032454 0.308025 0.169421 11.00000 0.04955 0.01975 = 0.02246 -0.00766 0.00089 0.00716 N2 4 -0.013767 -0.012102 0.203327 11.00000 0.02941 0.03001 = 0.03815 0.00722 0.00509 0.00145 N4 4 0.020662 0.255832 0.235512 11.00000 0.03943 0.03462 = 0.01383 -0.00336 0.00351 0.00526 O2 5 -0.010773 0.297935 -0.032731 11.00000 0.06297 0.08163 = 0.03433 0.01930 -0.02245 0.01189 N1 4 -0.009376 -0.005986 0.131457 11.00000 0.02842 0.03403 = 0.02795 0.00109 0.00271 -0.00910 O1 5 0.062270 -0.140759 -0.031050 11.00000 0.09795 0.03098 = 0.03554 -0.02216 0.00356 0.00386 N6 4 0.062068 -0.004985 0.235932 11.00000 0.03894 0.02798 = 0.01729 0.00370 -0.00375 0.00114 PART 1 N17 4 0.192416 0.499498 0.266926 21.00000 0.02908 PART 0 C22 1 0.011586 0.384912 0.276750 11.00000 0.04234 0.02188 = 0.04326 -0.00422 -0.00125 0.00502 C2 1 0.056336 -0.045056 0.010194 11.00000 0.05005 0.02657 = 0.03868 0.01298 -0.00350 -0.00230 C17 1 0.087604 -0.097625 0.277890 11.00000 0.05315 0.02460 = 0.02760 0.00352 -0.00319 0.00233 PART 1 N11 4 0.228922 0.783058 0.300782 21.00000 0.03046 PART 0 C16 1 0.122358 -0.138415 0.239287 11.00000 0.03497 0.05274 = 0.04405 0.00766 -0.00871 0.00142 AFIX 43 H16 2 0.145212 -0.199574 0.254640 11.00000 -1.20000 AFIX 0 PART 1 N14 4 0.266162 0.506909 0.304103 21.00000 0.04998 PART 0 C3 1 0.009520 0.236502 0.012211 11.00000 0.04995 0.05002 = 0.04696 -0.01432 0.01686 -0.01685 C15 1 0.116534 -0.069316 0.171876 11.00000 0.03817 0.04730 = 0.03476 -0.00151 -0.00665 0.01146 B1 3 0.019024 0.070641 0.251374 11.00000 0.03591 0.03441 = 0.02295 -0.00274 0.00129 -0.00621 AFIX 14 H1 2 0.010458 0.050158 0.309584 11.00000 -1.20000 AFIX 0 C14 1 0.145545 -0.074557 0.110505 11.00000 0.05042 0.08188 = 0.05870 0.00700 0.01257 0.03185 AFIX 137 H14A 2 0.129993 -0.096919 0.067996 11.00000 -1.50000 H14B 2 0.165947 -0.159392 0.117781 11.00000 -1.50000 H14C 2 0.159483 0.029247 0.105995 11.00000 -1.50000 AFIX 0 C11 1 -0.066121 -0.151656 0.158255 11.00000 0.03447 0.05037 = 0.05895 0.00800 -0.00224 -0.00849 AFIX 43 H11 2 -0.090172 -0.215200 0.153892 11.00000 -1.20000 AFIX 0 C21 1 0.018365 0.523035 0.238123 11.00000 0.05600 0.02414 = 0.05741 -0.00784 0.01005 0.00874 AFIX 43 H21 2 0.014771 0.630122 0.253985 11.00000 -1.20000 AFIX 0 C20 1 0.031581 0.476716 0.170899 11.00000 0.05633 0.01424 = 0.04744 -0.00999 0.00020 0.00386 C4 1 0.109815 0.307401 -0.028265 11.00000 0.03535 0.02043 = 0.03903 0.00467 0.00959 -0.00491 C9 1 -0.047609 -0.115088 0.024182 11.00000 0.05535 0.06959 = 0.04959 -0.00026 -0.02119 -0.02005 AFIX 137 H9A 2 -0.033030 -0.212069 0.009207 11.00000 -1.50000 H9B 2 -0.036674 -0.021702 -0.000701 11.00000 -1.50000 H9C 2 -0.076914 -0.126542 0.013928 11.00000 -1.50000 AFIX 0 PART 1 C141 1 0.139419 0.379359 0.314007 21.00000 0.04759 PART 2 C125 1 0.226444 0.965245 0.313732 -21.00000 0.03623 PART 0 C18 1 0.077176 -0.138374 0.352484 11.00000 0.06875 0.05388 = 0.03651 0.00902 -0.01131 0.00829 AFIX 137 H18A 2 0.075157 -0.039191 0.379720 11.00000 -1.50000 H18B 2 0.098730 -0.206911 0.372030 11.00000 -1.50000 H18C 2 0.050889 -0.195408 0.354009 11.00000 -1.50000 AFIX 0 C10 1 -0.041617 -0.091299 0.103407 11.00000 0.03684 0.04257 = 0.04191 0.00579 -0.00689 -0.00771 C1 1 0.085253 0.237148 0.029590 11.00000 0.05341 0.02804 = 0.02642 -0.00832 -0.01043 0.01390 N7 4 0.118192 0.520067 -0.115124 11.00000 0.05636 0.06174 = 0.06786 0.00148 0.02726 -0.00520 C12 1 -0.048097 -0.099726 0.219720 11.00000 0.03683 0.03923 = 0.05452 0.00962 -0.00079 -0.00812 C5 1 0.098650 0.452199 -0.060959 11.00000 0.03386 0.06256 = 0.05707 0.02834 0.01787 0.00307 AFIX 43 H5 2 0.075300 0.506741 -0.043259 11.00000 -1.20000 AFIX 0 C6 1 0.151533 0.442310 -0.139565 11.00000 0.06876 0.05465 = 0.04723 -0.00687 0.02694 -0.01832 AFIX 43 H6 2 0.165556 0.487048 -0.178244 11.00000 -1.20000 AFIX 0 PART 1 C133 1 0.322783 0.369245 0.337068 21.00000 0.04615 AFIX 43 H133 2 0.349127 0.320603 0.336527 21.00000 -1.20000 AFIX 0 PART 0 C23 1 -0.005017 0.365327 0.349949 11.00000 0.07152 0.05410 = 0.05006 -0.01433 0.01030 0.01265 AFIX 137 H23A 2 -0.034527 0.343261 0.347927 11.00000 -1.50000 H23B 2 -0.000264 0.464355 0.376300 11.00000 -1.50000 H23C 2 0.009015 0.275715 0.372894 11.00000 -1.50000 AFIX 0 PART 2 C136 1 0.317226 0.422116 0.240202 -21.00000 0.05048 B3 3 0.251351 0.611929 0.218760 -21.00000 0.01914 AFIX 14 H3 2 0.263944 0.618224 0.161932 -21.00000 -1.20000 AFIX 0 PART 0 C13 1 -0.061752 -0.126513 0.294572 11.00000 0.05803 0.06783 = 0.06263 0.02392 0.01753 -0.02053 AFIX 137 H13A 2 -0.068809 -0.023081 0.315771 11.00000 -1.50000 H13B 2 -0.039410 -0.176618 0.320881 11.00000 -1.50000 H13C 2 -0.085819 -0.197070 0.295209 11.00000 -1.50000 AFIX 0 PART 1 N16 4 0.171127 0.464689 0.333768 21.00000 0.03399 C131 1 0.294918 0.367311 0.392130 21.00000 0.04190 PART 0 C8 1 0.144889 0.232203 -0.055446 11.00000 0.07903 0.03867 = 0.08606 0.00685 0.04789 0.01193 AFIX 43 H8 2 0.154430 0.133996 -0.036246 11.00000 -1.20000 AFIX 0 PART 2 C124 1 0.205012 1.040529 0.376596 -21.00000 0.04940 AFIX 137 H12G 2 0.224450 1.048597 0.415302 -21.00000 -1.50000 H12H 2 0.181744 0.973155 0.390420 -21.00000 -1.50000 H12I 2 0.195122 1.148031 0.364312 -21.00000 -1.50000 AFIX 0 PART 1 B2 3 0.233386 0.606423 0.268141 21.00000 0.01914 AFIX 14 H2 2 0.243804 0.622707 0.210358 21.00000 -1.20000 AFIX 0 PART 2 C146 1 0.181834 0.463787 0.161407 -21.00000 0.08386 PART 0 C7 1 0.165983 0.304864 -0.112113 11.00000 0.10265 0.03926 = 0.11740 0.00182 0.07553 -0.00147 AFIX 43 H7 2 0.190074 0.256658 -0.130395 11.00000 -1.20000 AFIX 0 PART 2 C127 1 0.257970 0.930977 0.214449 -21.00000 0.04240 C117 1 0.214539 0.383203 0.438663 -21.00000 0.04840 PART 1 C145 1 0.168209 0.433048 0.215915 21.00000 0.04188 O102 5 0.254612 0.640134 0.563496 21.00000 0.08266 C106 1 0.096793 0.574276 0.695409 21.00000 0.06046 AFIX 43 H106 2 0.084059 0.581675 0.739675 21.00000 -1.20000 AFIX 0 C143 1 0.134227 0.358224 0.244454 21.00000 0.04953 AFIX 43 H143 2 0.112491 0.304899 0.221070 21.00000 -1.20000 AFIX 0 PART 2 N15 4 0.281898 0.507631 0.260741 -21.00000 0.04803 PART 1 C122 1 0.245647 0.986868 0.225202 21.00000 0.06199 AFIX 137 H12A 2 0.272985 1.031802 0.233669 21.00000 -1.50000 H12B 2 0.227603 1.070902 0.206807 21.00000 -1.50000 H12C 2 0.247678 0.899075 0.191433 21.00000 -1.50000 AFIX 0 C104 1 0.134161 0.563836 0.565251 21.00000 0.05096 PART 2 N18 4 0.208315 0.520470 0.214986 -21.00000 0.06023 PART 1 C105 1 0.151632 0.502026 0.623243 21.00000 0.04518 AFIX 43 H105 2 0.178198 0.456683 0.618306 21.00000 -1.20000 AFIX 0 PART 2 O101 5 0.261590 0.740780 0.509750 -21.00000 0.07517 PART 1 N12 4 0.207391 0.752812 0.378789 21.00000 0.04558 C116 1 0.237227 0.598707 0.516414 21.00000 0.05760 C101 1 0.158562 0.561848 0.500641 21.00000 0.06017 C102 1 0.197155 0.312893 0.490763 21.00000 0.04462 PART 0 C19 1 0.043110 0.580201 0.108660 11.00000 0.08440 0.02809 = 0.01763 0.01069 0.01118 0.00530 AFIX 137 H19A 2 0.023451 0.561938 0.070938 11.00000 -1.50000 H19B 2 0.070740 0.551556 0.092852 11.00000 -1.50000 H19C 2 0.042563 0.693738 0.122120 11.00000 -1.50000 AFIX 0 PART 2 C142 1 0.153475 0.407315 0.262599 -21.00000 0.05254 PART 1 N9 4 0.133927 0.498524 0.691075 21.00000 0.06526 C108 1 0.091812 0.632726 0.574770 21.00000 0.06654 AFIX 43 H108 2 0.076257 0.669550 0.536211 21.00000 -1.20000 AFIX 0 C107 1 0.076886 0.640221 0.639399 21.00000 0.07784 AFIX 43 H107 2 0.051486 0.693312 0.646860 21.00000 -1.20000 AFIX 0 O104 5 0.191249 0.195160 0.523307 21.00000 0.09982 N13 4 0.259357 0.450994 0.374653 21.00000 0.04339 C139 1 0.110122 0.319365 0.373518 21.00000 0.06335 AFIX 137 H13D 2 0.123924 0.235378 0.400493 21.00000 -1.50000 H13E 2 0.084944 0.275780 0.353033 21.00000 -1.50000 H13F 2 0.103236 0.409543 0.404122 21.00000 -1.50000 AFIX 0 PART 2 N10 4 0.246800 0.773166 0.241899 -21.00000 0.05000 C144 1 0.147887 0.390255 0.191757 -21.00000 0.07498 AFIX 43 H144 2 0.125659 0.339303 0.168713 -21.00000 -1.20000 AFIX 0 PART 1 C118 1 0.180224 0.950121 0.469703 21.00000 0.06829 AFIX 137 H11A 2 0.158546 0.870901 0.478141 21.00000 -1.50000 H11B 2 0.168239 1.058067 0.468507 21.00000 -1.50000 H11C 2 0.200599 0.944216 0.507076 21.00000 -1.50000 AFIX 0 C137 1 0.321095 0.500312 0.214979 21.00000 0.06601 AFIX 137 H13G 2 0.302839 0.460363 0.178382 21.00000 -1.50000 H13H 2 0.348374 0.452568 0.209307 21.00000 -1.50000 H13I 2 0.323187 0.617519 0.211671 21.00000 -1.50000 AFIX 0 PART 2 C113 1 0.109244 0.781177 0.590994 -21.00000 0.06704 AFIX 43 H113 2 0.108013 0.879374 0.616013 -21.00000 -1.20000 AFIX 0 C110 1 0.140995 0.641255 0.490563 -21.00000 0.05736 N8 4 0.089895 0.499547 0.560939 -21.00000 0.10532 C114 1 0.136110 0.770012 0.531567 -21.00000 0.07362 AFIX 43 H114 2 0.151805 0.862611 0.520472 -21.00000 -1.20000 AFIX 0 C111 1 0.118245 0.507364 0.504931 -21.00000 0.10281 AFIX 43 H111 2 0.121531 0.415503 0.476213 -21.00000 -1.20000 AFIX 0 C128 1 0.275282 0.934903 0.139182 -21.00000 0.09257 AFIX 137 H12J 2 0.298208 0.859242 0.135352 -21.00000 -1.50000 H12K 2 0.284905 1.043615 0.128369 -21.00000 -1.50000 H12L 2 0.253649 0.904327 0.106372 -21.00000 -1.50000 AFIX 0 C149 1 0.245967 0.679434 0.460901 -21.00000 0.04708 PART 1 C119 1 0.200164 0.915876 0.402760 21.00000 0.05148 PART 2 C134 1 0.335248 0.350350 0.297252 -21.00000 0.03857 AFIX 43 H134 2 0.360186 0.291486 0.298480 -21.00000 -1.20000 AFIX 0 C148 1 0.194770 0.490816 0.085735 -21.00000 0.08496 AFIX 137 H14G 2 0.218898 0.561000 0.084396 -21.00000 -1.50000 H14H 2 0.172197 0.541374 0.060167 -21.00000 -1.50000 H14I 2 0.201490 0.387360 0.064245 -21.00000 -1.50000 AFIX 0 C138 1 0.330989 0.419138 0.163639 -21.00000 0.06195 AFIX 137 H13J 2 0.314495 0.340619 0.137948 -21.00000 -1.50000 H13K 2 0.360012 0.388967 0.161082 -21.00000 -1.50000 H13L 2 0.327217 0.525931 0.143163 -21.00000 -1.50000 AFIX 0 O103 5 0.215768 0.288344 0.480117 -21.00000 0.12431 C140 1 0.126633 0.354616 0.322609 -21.00000 0.06218 AFIX 137 H14J 2 0.097752 0.359670 0.308618 -21.00000 -1.50000 H14K 2 0.131163 0.425930 0.362408 -21.00000 -1.50000 H14L 2 0.133603 0.244125 0.335656 -21.00000 -1.50000 AFIX 0 PART 1 C123 1 0.212473 1.008785 0.344108 21.00000 0.05598 AFIX 43 H123 2 0.209631 1.122217 0.342212 21.00000 -1.20000 AFIX 0 C121 1 0.228208 0.923454 0.292497 21.00000 0.04700 C147 1 0.182188 0.450155 0.140584 21.00000 0.06239 AFIX 33 H14D 2 0.162276 0.397778 0.109873 21.00000 -1.50000 H14E 2 0.184167 0.564336 0.128615 21.00000 -1.50000 H14F 2 0.209100 0.399338 0.134883 21.00000 -1.50000 AFIX 0 PART 2 C126 1 0.242734 1.041160 0.260834 -21.00000 0.05675 AFIX 43 H126 2 0.243826 1.154457 0.255442 -21.00000 -1.20000 AFIX 0 PART 1 C129 1 0.300123 0.282600 0.462053 21.00000 0.06927 AFIX 137 H12D 2 0.291067 0.354120 0.499496 21.00000 -1.50000 H12E 2 0.329072 0.255033 0.468906 21.00000 -1.50000 H12F 2 0.283568 0.184324 0.462595 21.00000 -1.50000 AFIX 0 C135 1 0.304638 0.456606 0.282474 21.00000 0.05403 PART 2 C132 1 0.306985 0.385331 0.356840 -21.00000 0.04054 C130 1 0.309730 0.331775 0.427844 -21.00000 0.05834 AFIX 137 H13M 2 0.306816 0.214653 0.429527 -21.00000 -1.50000 H13N 2 0.287812 0.381695 0.455219 -21.00000 -1.50000 H13O 2 0.336431 0.362521 0.447117 -21.00000 -1.50000 AFIX 0 C112 1 0.082914 0.641502 0.614855 -21.00000 0.11739 AFIX 43 H112 2 0.065559 0.639296 0.654474 -21.00000 -1.20000 AFIX 0 C109 1 0.172056 0.647104 0.433480 -21.00000 0.06338 N17A 4 0.185645 0.486490 0.286544 -21.00000 0.04421 N14A 4 0.272250 0.477551 0.331584 -21.00000 0.03650 N11A 4 0.220588 0.775912 0.320376 -21.00000 0.03608 HKLF 4 REM bf3pynmr2_b.res in Pna2(1) REM wR2 = 0.1226, GooF = S = 1.110, Restrained GooF = 1.110 for all data REM R1 = 0.0515 for 8288 Fo > 4sig(Fo) and 0.0565 for all 8918 data REM 610 parameters refined using 12 restraints END WGHT 0.0434 28.1980 REM Highest difference peak 2.423, deepest hole -1.612, 1-sigma level 0.131 Q1 1 0.1996 0.6456 0.4186 11.00000 0.05 2.42 Q2 1 0.3010 1.1292 0.2492 11.00000 0.05 1.76 Q3 1 0.0470 0.1438 0.1314 11.00000 0.05 1.33 Q4 1 0.0470 0.1388 0.0376 11.00000 0.05 1.31 Q5 1 0.0274 0.1482 0.0832 11.00000 0.05 1.21 ; _shelx_res_checksum 12119 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' 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 W1 W 0.04636(2) 0.13463(6) 0.08306(4) 0.02667(13) Uani 1 1 d . . . . . W2 W 0.20056(4) 0.52692(15) 0.43575(8) 0.0451(4) Uani 0.563(3) 1 d D . P A 1 W3 W 0.21587(5) 0.5858(2) 0.37836(11) 0.0505(6) Uani 0.437(3) 1 d D . P A 2 N5 N 0.0800(3) 0.0092(13) 0.1713(5) 0.029(2) Uani 1 1 d . . . . . N3 N 0.0325(4) 0.3080(13) 0.1694(6) 0.031(2) Uani 1 1 d . . . . . N2 N -0.0138(3) -0.0121(14) 0.2033(6) 0.033(2) Uani 1 1 d . . . . . N4 N 0.0207(3) 0.2558(13) 0.2355(5) 0.029(2) Uani 1 1 d . . . . . O2 O -0.0108(4) 0.2979(17) -0.0327(6) 0.060(3) Uani 1 1 d . . . . . N1 N -0.0094(3) -0.0060(14) 0.1315(6) 0.030(2) Uani 1 1 d . . . . . O1 O 0.0623(4) -0.1408(12) -0.0310(6) 0.055(3) Uani 1 1 d . . . . . N6 N 0.0621(3) -0.0050(12) 0.2359(5) 0.028(2) Uani 1 1 d . . . . . N17 N 0.1924(7) 0.499(3) 0.2669(14) 0.029(6) Uiso 0.563(3) 1 d . . P A 1 C22 C 0.0116(4) 0.3849(15) 0.2768(8) 0.036(3) Uani 1 1 d . . . . . C2 C 0.0563(5) -0.0451(16) 0.0102(8) 0.038(3) Uani 1 1 d . . . . . C17 C 0.0876(5) -0.0976(15) 0.2779(7) 0.035(3) Uani 1 1 d . . . . . N11 N 0.2289(7) 0.783(3) 0.3008(13) 0.030(5) Uiso 0.563(3) 1 d . . P A 1 C16 C 0.1224(4) -0.138(2) 0.2393(8) 0.044(3) Uani 1 1 d . . . . . H16 H 0.145212 -0.199574 0.254640 0.053 Uiso 1 1 calc R U . . . N14 N 0.2662(9) 0.507(3) 0.3041(17) 0.050(6) Uiso 0.563(3) 1 d . . P A 1 C3 C 0.0095(5) 0.237(2) 0.0122(9) 0.049(4) Uani 1 1 d . . . . . C15 C 0.1165(4) -0.0693(19) 0.1719(8) 0.040(3) Uani 1 1 d . . . . . B1 B 0.0190(5) 0.0706(19) 0.2514(8) 0.031(3) Uani 1 1 d D . . . . H1 H 0.0105(5) 0.0502(19) 0.3096(16) 0.037 Uiso 1 1 calc DR U . . . C14 C 0.1455(5) -0.075(3) 0.1105(10) 0.064(5) Uani 1 1 d . . . . . H14A H 0.129993 -0.096919 0.067996 0.096 Uiso 1 1 calc R U . . . H14B H 0.165947 -0.159392 0.117781 0.096 Uiso 1 1 calc R U . . . H14C H 0.159483 0.029247 0.105995 0.096 Uiso 1 1 calc R U . . . C11 C -0.0661(5) -0.152(2) 0.1583(10) 0.048(4) Uani 1 1 d . . . . . H11 H -0.090172 -0.215200 0.153892 0.058 Uiso 1 1 calc R U . . . C21 C 0.0184(5) 0.5230(17) 0.2381(9) 0.046(4) Uani 1 1 d . . . . . H21 H 0.014771 0.630122 0.253985 0.055 Uiso 1 1 calc R U . . . C20 C 0.0316(5) 0.4767(15) 0.1709(8) 0.039(3) Uani 1 1 d . . . . . C4 C 0.1098(4) 0.3074(15) -0.0283(7) 0.032(3) Uani 1 1 d . . . . . C9 C -0.0476(6) -0.115(2) 0.0242(11) 0.058(5) Uani 1 1 d . . . . . H9A H -0.033030 -0.212069 0.009207 0.087 Uiso 1 1 calc R U . . . H9B H -0.036674 -0.021702 -0.000701 0.087 Uiso 1 1 calc R U . . . H9C H -0.076914 -0.126542 0.013928 0.087 Uiso 1 1 calc R U . . . C141 C 0.1394(12) 0.379(4) 0.3140(19) 0.048(8) Uiso 0.563(3) 1 d . . P A 1 C125 C 0.2264(12) 0.965(5) 0.314(3) 0.036(9) Uiso 0.437(3) 1 d . . P A 2 C18 C 0.0772(6) -0.138(2) 0.3525(8) 0.053(4) Uani 1 1 d . . . . . H18A H 0.075157 -0.039191 0.379720 0.080 Uiso 1 1 calc R U . . . H18B H 0.098730 -0.206911 0.372030 0.080 Uiso 1 1 calc R U . . . H18C H 0.050889 -0.195408 0.354009 0.080 Uiso 1 1 calc R U . . . C10 C -0.0416(4) -0.0913(19) 0.1034(8) 0.040(4) Uani 1 1 d . . . . . C1 C 0.0853(4) 0.2371(16) 0.0296(7) 0.036(3) Uani 1 1 d . . . . . N7 N 0.1182(4) 0.5201(19) -0.1151(9) 0.062(4) Uani 1 1 d . . . . . C12 C -0.0481(4) -0.0997(18) 0.2197(9) 0.044(3) Uani 1 1 d . . . . . C5 C 0.0987(4) 0.452(2) -0.0610(10) 0.051(4) Uani 1 1 d . . . . . H5 H 0.075300 0.506741 -0.043259 0.061 Uiso 1 1 calc R U . . . C6 C 0.1515(6) 0.442(2) -0.1396(10) 0.057(5) Uani 1 1 d . . . . . H6 H 0.165556 0.487048 -0.178244 0.068 Uiso 1 1 calc R U . . . C133 C 0.3228(11) 0.369(4) 0.3371(19) 0.046(7) Uiso 0.563(3) 1 d . . P A 1 H133 H 0.349127 0.320603 0.336527 0.055 Uiso 0.563(3) 1 calc R U P A 1 C23 C -0.0050(6) 0.365(2) 0.3499(10) 0.059(4) Uani 1 1 d . . . . . H23A H -0.034527 0.343261 0.347927 0.088 Uiso 1 1 calc R U . . . H23B H -0.000264 0.464355 0.376300 0.088 Uiso 1 1 calc R U . . . H23C H 0.009015 0.275715 0.372894 0.088 Uiso 1 1 calc R U . . . C136 C 0.3172(12) 0.422(5) 0.240(2) 0.050(9) Uiso 0.437(3) 1 d . . P A 2 B3 B 0.2514(8) 0.612(3) 0.2188(15) 0.019(3) Uiso 0.437(3) 1 d D . P A 2 H3 H 0.2639(9) 0.618(3) 0.162(2) 0.023 Uiso 0.437(3) 1 calc DR U P A 2 C13 C -0.0618(6) -0.127(2) 0.2946(10) 0.063(5) Uani 1 1 d . . . . . H13A H -0.068809 -0.023081 0.315771 0.094 Uiso 1 1 calc R U . . . H13B H -0.039410 -0.176618 0.320881 0.094 Uiso 1 1 calc R U . . . H13C H -0.085819 -0.197070 0.295209 0.094 Uiso 1 1 calc R U . . . N16 N 0.1711(6) 0.465(2) 0.3338(12) 0.034(4) Uiso 0.563(3) 1 d . . P A 1 C131 C 0.2949(9) 0.367(3) 0.3921(17) 0.042(6) Uiso 0.563(3) 1 d . . P A 1 C8 C 0.1449(6) 0.232(2) -0.0554(12) 0.068(6) Uani 1 1 d . . . . . H8 H 0.154430 0.133996 -0.036246 0.082 Uiso 1 1 calc R U . . . C124 C 0.2050(12) 1.041(5) 0.377(2) 0.049(9) Uiso 0.437(3) 1 d . . P A 2 H12G H 0.224450 1.048597 0.415302 0.074 Uiso 0.437(3) 1 calc R U P A 2 H12H H 0.181744 0.973155 0.390420 0.074 Uiso 0.437(3) 1 calc R U P A 2 H12I H 0.195122 1.148031 0.364312 0.074 Uiso 0.437(3) 1 calc R U P A 2 B2 B 0.2334(6) 0.606(3) 0.2681(12) 0.019(3) Uiso 0.563(3) 1 d D . P A 1 H2 H 0.2438(7) 0.623(3) 0.2104(19) 0.023 Uiso 0.563(3) 1 calc DR U P A 1 C146 C 0.1818(19) 0.464(9) 0.161(3) 0.08(2) Uiso 0.437(3) 1 d D . P A 2 C7 C 0.1660(7) 0.305(2) -0.1121(14) 0.086(8) Uani 1 1 d . . . . . H7 H 0.190074 0.256658 -0.130395 0.104 Uiso 1 1 calc R U . . . C127 C 0.2580(12) 0.931(5) 0.214(2) 0.042(8) Uiso 0.437(3) 1 d . . P A 2 C117 C 0.2145(11) 0.383(5) 0.439(2) 0.048(8) Uiso 0.437(3) 1 d . . P A 2 C145 C 0.1682(8) 0.433(3) 0.2159(15) 0.042(6) Uiso 0.563(3) 1 d . . P A 1 O102 O 0.2546(8) 0.640(3) 0.5635(15) 0.083(8) Uiso 0.563(3) 1 d . . P A 1 C106 C 0.0968(10) 0.574(4) 0.695(2) 0.060(8) Uiso 0.563(3) 1 d . . P A 1 H106 H 0.084059 0.581675 0.739675 0.073 Uiso 0.563(3) 1 calc R U P A 1 C143 C 0.1342(10) 0.358(4) 0.2445(17) 0.050(7) Uiso 0.563(3) 1 d . . P A 1 H143 H 0.112491 0.304899 0.221070 0.059 Uiso 0.563(3) 1 calc R U P A 1 N15 N 0.2819(10) 0.508(4) 0.2607(18) 0.048(7) Uiso 0.437(3) 1 d . . P A 2 C122 C 0.2456(12) 0.987(5) 0.225(2) 0.062(9) Uiso 0.563(3) 1 d . . P A 1 H12A H 0.272985 1.031802 0.233669 0.093 Uiso 0.563(3) 1 calc R U P A 1 H12B H 0.227603 1.070902 0.206807 0.093 Uiso 0.563(3) 1 calc R U P A 1 H12C H 0.247678 0.899075 0.191433 0.093 Uiso 0.563(3) 1 calc R U P A 1 C104 C 0.1342(8) 0.564(4) 0.5653(13) 0.051(7) Uiso 0.563(3) 1 d D . P A 1 N18 N 0.2083(11) 0.520(4) 0.215(2) 0.060(9) Uiso 0.437(3) 1 d . . P A 2 C105 C 0.1516(9) 0.502(3) 0.6232(15) 0.045(6) Uiso 0.563(3) 1 d . . P A 1 H105 H 0.178198 0.456683 0.618306 0.054 Uiso 0.563(3) 1 calc R U P A 1 O101 O 0.2616(10) 0.741(4) 0.5097(19) 0.075(9) Uiso 0.437(3) 1 d . . P A 2 N12 N 0.2074(6) 0.753(3) 0.3788(13) 0.046(5) Uiso 0.563(3) 1 d . . P A 1 C116 C 0.2372(10) 0.599(4) 0.5164(19) 0.058(8) Uiso 0.563(3) 1 d . . P A 1 C101 C 0.1586(9) 0.562(4) 0.5006(15) 0.060(8) Uiso 0.563(3) 1 d D . P A 1 C102 C 0.1972(10) 0.313(4) 0.4908(16) 0.045(6) Uiso 0.563(3) 1 d . . P A 1 C19 C 0.0431(5) 0.5802(17) 0.1087(7) 0.043(4) Uani 1 1 d . . . . . H19A H 0.023451 0.561938 0.070938 0.065 Uiso 1 1 calc R U . . . H19B H 0.070740 0.551556 0.092852 0.065 Uiso 1 1 calc R U . . . H19C H 0.042563 0.693738 0.122120 0.065 Uiso 1 1 calc R U . . . C142 C 0.1535(13) 0.407(5) 0.2626(19) 0.053(9) Uiso 0.437(3) 1 d D . P A 2 N9 N 0.1339(9) 0.499(4) 0.6911(16) 0.065(7) Uiso 0.563(3) 1 d . . P A 1 C108 C 0.0918(11) 0.633(5) 0.575(3) 0.067(9) Uiso 0.563(3) 1 d . . P A 1 H108 H 0.076257 0.669550 0.536211 0.080 Uiso 0.563(3) 1 calc R U P A 1 C107 C 0.0769(18) 0.640(7) 0.639(3) 0.078(13) Uiso 0.563(3) 1 d . . P A 1 H107 H 0.051486 0.693312 0.646860 0.093 Uiso 0.563(3) 1 calc R U P A 1 O104 O 0.1912(10) 0.195(4) 0.5233(19) 0.100(9) Uiso 0.563(3) 1 d . . P A 1 N13 N 0.2594(7) 0.451(3) 0.3747(14) 0.043(5) Uiso 0.563(3) 1 d . . P A 1 C139 C 0.1101(10) 0.319(4) 0.374(2) 0.063(8) Uiso 0.563(3) 1 d . . P A 1 H13D H 0.123924 0.235378 0.400493 0.095 Uiso 0.563(3) 1 calc R U P A 1 H13E H 0.084944 0.275780 0.353033 0.095 Uiso 0.563(3) 1 calc R U P A 1 H13F H 0.103236 0.409543 0.404122 0.095 Uiso 0.563(3) 1 calc R U P A 1 N10 N 0.2468(9) 0.773(4) 0.2419(18) 0.050(7) Uiso 0.437(3) 1 d . . P A 2 C144 C 0.1479(15) 0.390(6) 0.192(2) 0.075(13) Uiso 0.437(3) 1 d D . P A 2 H144 H 0.125659 0.339303 0.168713 0.090 Uiso 0.437(3) 1 calc R U P A 2 C118 C 0.1802(12) 0.950(5) 0.470(2) 0.068(9) Uiso 0.563(3) 1 d . . P A 1 H11A H 0.158546 0.870901 0.478141 0.102 Uiso 0.563(3) 1 calc R U P A 1 H11B H 0.168239 1.058067 0.468507 0.102 Uiso 0.563(3) 1 calc R U P A 1 H11C H 0.200599 0.944216 0.507076 0.102 Uiso 0.563(3) 1 calc R U P A 1 C137 C 0.3211(11) 0.500(5) 0.215(2) 0.066(9) Uiso 0.563(3) 1 d . . P A 1 H13G H 0.302839 0.460363 0.178382 0.099 Uiso 0.563(3) 1 calc R U P A 1 H13H H 0.348374 0.452568 0.209307 0.099 Uiso 0.563(3) 1 calc R U P A 1 H13I H 0.323187 0.617519 0.211671 0.099 Uiso 0.563(3) 1 calc R U P A 1 C113 C 0.1092(12) 0.781(5) 0.591(3) 0.067(11) Uiso 0.437(3) 1 d . . P A 2 H113 H 0.108013 0.879374 0.616013 0.080 Uiso 0.437(3) 1 calc R U P A 2 C110 C 0.1410(12) 0.641(5) 0.491(2) 0.057(10) Uiso 0.437(3) 1 d D . P A 2 N8 N 0.0899(17) 0.500(7) 0.561(3) 0.105(16) Uiso 0.437(3) 1 d . . P A 2 C114 C 0.1361(15) 0.770(7) 0.532(3) 0.074(13) Uiso 0.437(3) 1 d . . P A 2 H114 H 0.151805 0.862611 0.520472 0.088 Uiso 0.437(3) 1 calc R U P A 2 C111 C 0.118(2) 0.507(9) 0.505(4) 0.10(2) Uiso 0.437(3) 1 d . . P A 2 H111 H 0.121531 0.415503 0.476213 0.123 Uiso 0.437(3) 1 calc R U P A 2 C128 C 0.2753(19) 0.935(8) 0.139(3) 0.093(17) Uiso 0.437(3) 1 d . . P A 2 H12J H 0.298208 0.859242 0.135352 0.139 Uiso 0.437(3) 1 calc R U P A 2 H12K H 0.284905 1.043615 0.128369 0.139 Uiso 0.437(3) 1 calc R U P A 2 H12L H 0.253649 0.904327 0.106372 0.139 Uiso 0.437(3) 1 calc R U P A 2 C149 C 0.2460(11) 0.679(5) 0.461(2) 0.047(8) Uiso 0.437(3) 1 d . . P A 2 C119 C 0.2002(10) 0.916(4) 0.4028(18) 0.051(7) Uiso 0.563(3) 1 d . . P A 1 C134 C 0.3352(10) 0.350(4) 0.2973(19) 0.039(7) Uiso 0.437(3) 1 d . . P A 2 H134 H 0.360186 0.291486 0.298480 0.046 Uiso 0.437(3) 1 calc R U P A 2 C148 C 0.1948(15) 0.491(6) 0.086(3) 0.085(13) Uiso 0.437(3) 1 d D . P A 2 H14G H 0.218898 0.561000 0.084396 0.127 Uiso 0.437(3) 1 calc R U P A 2 H14H H 0.172197 0.541374 0.060167 0.127 Uiso 0.437(3) 1 calc R U P A 2 H14I H 0.201490 0.387360 0.064245 0.127 Uiso 0.437(3) 1 calc R U P A 2 C138 C 0.3310(14) 0.419(6) 0.164(2) 0.062(11) Uiso 0.437(3) 1 d . . P A 2 H13J H 0.314495 0.340619 0.137948 0.093 Uiso 0.437(3) 1 calc R U P A 2 H13K H 0.360012 0.388967 0.161082 0.093 Uiso 0.437(3) 1 calc R U P A 2 H13L H 0.327217 0.525931 0.143163 0.093 Uiso 0.437(3) 1 calc R U P A 2 O103 O 0.2158(17) 0.288(7) 0.480(3) 0.124(18) Uiso 0.437(3) 1 d . . P A 2 C140 C 0.1266(16) 0.355(6) 0.323(2) 0.062(14) Uiso 0.437(3) 1 d D . P A 2 H14J H 0.097752 0.359670 0.308618 0.093 Uiso 0.437(3) 1 calc R U P A 2 H14K H 0.131163 0.425930 0.362408 0.093 Uiso 0.437(3) 1 calc R U P A 2 H14L H 0.133603 0.244125 0.335656 0.093 Uiso 0.437(3) 1 calc R U P A 2 C123 C 0.2125(11) 1.009(5) 0.344(2) 0.056(8) Uiso 0.563(3) 1 d . . P A 1 H123 H 0.209631 1.122217 0.342212 0.067 Uiso 0.563(3) 1 calc R U P A 1 C121 C 0.2282(10) 0.923(5) 0.292(2) 0.047(9) Uiso 0.563(3) 1 d . . P A 1 C147 C 0.1822(13) 0.450(6) 0.141(3) 0.062(12) Uiso 0.563(3) 1 d . . P A 1 H14D H 0.162276 0.397778 0.109873 0.094 Uiso 0.563(3) 1 calc R U P A 1 H14E H 0.184167 0.564336 0.128615 0.094 Uiso 0.563(3) 1 calc R U P A 1 H14F H 0.209100 0.399338 0.134883 0.094 Uiso 0.563(3) 1 calc R U P A 1 C126 C 0.2427(13) 1.041(6) 0.261(3) 0.057(10) Uiso 0.437(3) 1 d . . P A 2 H126 H 0.243826 1.154457 0.255442 0.068 Uiso 0.437(3) 1 calc R U P A 2 C129 C 0.3001(12) 0.283(5) 0.462(2) 0.069(9) Uiso 0.563(3) 1 d . . P A 1 H12D H 0.291067 0.354120 0.499496 0.104 Uiso 0.563(3) 1 calc R U P A 1 H12E H 0.329072 0.255033 0.468906 0.104 Uiso 0.563(3) 1 calc R U P A 1 H12F H 0.283568 0.184324 0.462595 0.104 Uiso 0.563(3) 1 calc R U P A 1 C135 C 0.3046(10) 0.457(4) 0.2825(19) 0.054(8) Uiso 0.563(3) 1 d . . P A 1 C132 C 0.3070(14) 0.385(4) 0.357(2) 0.041(8) Uiso 0.437(3) 1 d . . P A 2 C130 C 0.3097(13) 0.332(5) 0.428(3) 0.058(10) Uiso 0.437(3) 1 d . . P A 2 H13M H 0.306816 0.214653 0.429527 0.088 Uiso 0.437(3) 1 calc R U P A 2 H13N H 0.287812 0.381695 0.455219 0.088 Uiso 0.437(3) 1 calc R U P A 2 H13O H 0.336431 0.362521 0.447117 0.088 Uiso 0.437(3) 1 calc R U P A 2 C112 C 0.083(3) 0.642(14) 0.615(6) 0.12(3) Uiso 0.437(3) 1 d . . P A 2 H112 H 0.065559 0.639296 0.654474 0.141 Uiso 0.437(3) 1 calc R U P A 2 C109 C 0.1721(11) 0.647(5) 0.433(2) 0.063(10) Uiso 0.437(3) 1 d D . P A 2 N17A N 0.1856(11) 0.486(5) 0.287(2) 0.044(10) Uiso 0.437(3) 1 d . . P A 2 N14A N 0.2723(9) 0.478(4) 0.332(2) 0.036(7) Uiso 0.437(3) 1 d . . P A 2 N11A N 0.2206(10) 0.776(4) 0.3204(19) 0.036(8) Uiso 0.437(3) 1 d . . P A 2 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 W1 0.0326(2) 0.0231(2) 0.0243(2) 0.0003(3) -0.0005(3) 0.0004(2) W2 0.0396(6) 0.0450(7) 0.0509(8) -0.0005(6) -0.0085(6) 0.0003(5) W3 0.0510(10) 0.0365(9) 0.0639(13) -0.0003(8) -0.0164(8) -0.0011(7) N5 0.039(6) 0.032(6) 0.015(5) 0.000(4) -0.001(4) 0.006(4) N3 0.050(6) 0.020(5) 0.022(5) -0.008(4) 0.001(4) 0.007(4) N2 0.029(5) 0.030(5) 0.038(6) 0.007(5) 0.005(4) 0.001(4) N4 0.039(5) 0.035(6) 0.014(5) -0.003(4) 0.004(4) 0.005(4) O2 0.063(7) 0.082(9) 0.034(6) 0.019(6) -0.022(5) 0.012(6) N1 0.028(5) 0.034(5) 0.028(6) 0.001(4) 0.003(4) -0.009(4) O1 0.098(9) 0.031(5) 0.036(6) -0.022(5) 0.004(5) 0.004(6) N6 0.039(5) 0.028(5) 0.017(5) 0.004(4) -0.004(4) 0.001(4) C22 0.042(7) 0.022(6) 0.043(8) -0.004(6) -0.001(6) 0.005(5) C2 0.050(8) 0.027(7) 0.039(8) 0.013(6) -0.003(6) -0.002(6) C17 0.053(8) 0.025(6) 0.028(7) 0.004(5) -0.003(5) 0.002(6) C16 0.035(7) 0.053(9) 0.044(8) 0.008(7) -0.009(6) 0.001(7) C3 0.050(9) 0.050(9) 0.047(9) -0.014(7) 0.017(7) -0.017(7) C15 0.038(7) 0.047(8) 0.035(7) -0.002(6) -0.007(6) 0.011(6) B1 0.036(7) 0.034(8) 0.023(7) -0.003(6) 0.001(5) -0.006(6) C14 0.050(9) 0.082(13) 0.059(10) 0.007(9) 0.013(8) 0.032(9) C11 0.034(8) 0.050(9) 0.059(10) 0.008(8) -0.002(7) -0.008(7) C21 0.056(9) 0.024(7) 0.057(10) -0.008(6) 0.010(7) 0.009(6) C20 0.056(8) 0.014(6) 0.047(9) -0.010(5) 0.000(7) 0.004(5) C4 0.035(6) 0.020(6) 0.039(7) 0.005(5) 0.010(5) -0.005(5) C9 0.055(11) 0.070(12) 0.050(12) 0.000(9) -0.021(8) -0.020(9) C18 0.069(10) 0.054(9) 0.037(8) 0.009(7) -0.011(7) 0.008(8) C10 0.037(7) 0.043(7) 0.042(11) 0.006(6) -0.007(5) -0.008(6) C1 0.053(8) 0.028(6) 0.026(6) -0.008(5) -0.010(6) 0.014(6) N7 0.056(8) 0.062(9) 0.068(10) 0.001(8) 0.027(8) -0.005(7) C12 0.037(7) 0.039(8) 0.055(9) 0.010(7) -0.001(6) -0.008(6) C5 0.034(7) 0.063(10) 0.057(10) 0.028(9) 0.018(7) 0.003(7) C6 0.069(11) 0.055(11) 0.047(10) -0.007(8) 0.027(8) -0.018(9) C23 0.072(11) 0.054(10) 0.050(10) -0.014(8) 0.010(8) 0.013(9) C13 0.058(10) 0.068(11) 0.063(12) 0.024(10) 0.018(9) -0.021(9) C8 0.079(12) 0.039(9) 0.086(14) 0.007(9) 0.048(11) 0.012(8) C7 0.103(16) 0.039(9) 0.12(2) 0.002(11) 0.076(15) -0.001(10) C19 0.084(11) 0.028(6) 0.018(5) 0.011(5) 0.011(6) 0.005(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -5.4734 5.5774 '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 C1 W1 C3 80.6(6) . . ? C1 W1 C2 81.3(6) . . ? C3 W1 C2 86.5(6) . . ? C1 W1 N3 104.7(5) . . ? C3 W1 N3 96.3(5) . . ? C2 W1 N3 173.7(5) . . ? C1 W1 N5 107.3(5) . . ? C3 W1 N5 172.0(5) . . ? C2 W1 N5 95.6(5) . . ? N3 W1 N5 80.8(4) . . ? C1 W1 N1 169.3(5) . . ? C3 W1 N1 91.0(5) . . ? C2 W1 N1 91.7(5) . . ? N3 W1 N1 82.6(4) . . ? N5 W1 N1 81.3(4) . . ? C101 W2 C116 82.9(15) . . ? C101 W2 C102 75.8(14) . . ? C116 W2 C102 84.0(13) . . ? C101 W2 N12 105.9(13) . . ? C116 W2 N12 94.0(12) . . ? C102 W2 N12 177.2(10) . . ? C101 W2 N16 107.8(12) . . ? C116 W2 N16 168.3(11) . . ? C102 W2 N16 103.0(10) . . ? N12 W2 N16 78.7(8) . . ? C101 W2 N13 167.4(13) . . ? C116 W2 N13 88.9(11) . . ? C102 W2 N13 93.9(11) . . ? N12 W2 N13 84.1(8) . . ? N16 W2 N13 81.3(8) . . ? C109 W3 N11A 99.5(17) . . ? C109 W3 C149 79.5(18) . . ? N11A W3 C149 95.7(15) . . ? C109 W3 C117 83.5(17) . . ? N11A W3 C117 176.6(14) . . ? C149 W3 C117 83.3(16) . . ? C109 W3 N17A 102.7(18) . . ? N11A W3 N17A 83.1(14) . . ? C149 W3 N17A 177.6(16) . . ? C117 W3 N17A 97.9(15) . . ? C109 W3 N14A 167.5(17) . . ? N11A W3 N14A 91.8(14) . . ? C149 W3 N14A 94.2(14) . . ? C117 W3 N14A 85.0(14) . . ? N17A W3 N14A 83.8(13) . . ? C15 N5 N6 108.8(10) . . ? C15 N5 W1 130.5(9) . . ? N6 N5 W1 120.5(8) . . ? N4 N3 C20 106.7(10) . . ? N4 N3 W1 121.9(8) . . ? C20 N3 W1 131.4(10) . . ? C12 N2 N1 109.4(12) . . ? C12 N2 B1 130.7(13) . . ? N1 N2 B1 119.9(10) . . ? C22 N4 N3 110.1(10) . . ? C22 N4 B1 130.5(11) . . ? N3 N4 B1 119.4(10) . . ? C10 N1 N2 107.0(11) . . ? C10 N1 W1 133.6(9) . . ? N2 N1 W1 119.4(8) . . ? N5 N6 C17 108.5(10) . . ? N5 N6 B1 121.1(10) . . ? C17 N6 B1 130.4(11) . . ? C145 N17 N16 106(2) . . ? C145 N17 B2 135(2) . . ? N16 N17 B2 118.9(19) . . ? N4 C22 C21 107.8(13) . . ? N4 C22 C23 122.1(13) . . ? C21 C22 C23 130.0(14) . . ? O1 C2 W1 178.1(13) . . ? N6 C17 C16 108.1(12) . . ? N6 C17 C18 122.7(13) . . ? C16 C17 C18 129.2(13) . . ? C121 N11 B2 149(3) . . ? C121 N11 N12 105(3) . . ? B2 N11 N12 104.5(18) . . ? C17 C16 C15 106.1(12) . . ? C17 C16 H16 127.0 . . ? C15 C16 H16 127.0 . . ? C135 N14 N13 109(3) . . ? C135 N14 B2 132(3) . . ? N13 N14 B2 120(2) . . ? O2 C3 W1 176.4(13) . . ? N5 C15 C16 108.5(13) . . ? N5 C15 C14 123.7(13) . . ? C16 C15 C14 127.8(13) . . ? N6 B1 N2 108.8(10) . . ? N6 B1 N4 109.1(10) . . ? N2 B1 N4 109.8(11) . . ? N6 B1 H1 109.7 . . ? N2 B1 H1 109.7 . . ? N4 B1 H1 109.7 . . ? C15 C14 H14A 109.5 . . ? C15 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C15 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C11 C10 106.6(13) . . ? C12 C11 H11 126.7 . . ? C10 C11 H11 126.7 . . ? C22 C21 C20 108.2(12) . . ? C22 C21 H21 125.9 . . ? C20 C21 H21 125.9 . . ? N3 C20 C21 107.3(13) . . ? N3 C20 C19 123.0(13) . . ? C21 C20 C19 129.7(12) . . ? C8 C4 C5 115.2(13) . . ? C8 C4 C1 122.7(13) . . ? C5 C4 C1 122.1(12) . . ? C10 C9 H9A 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C10 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N16 C141 C143 117(3) . . ? N16 C141 C139 116(3) . . ? C143 C141 C139 127(3) . . ? C126 C125 C124 127(4) . . ? C126 C125 N11A 126(5) . . ? C124 C125 N11A 107(3) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N1 C10 C11 108.7(13) . . ? N1 C10 C9 123.2(14) . . ? C11 C10 C9 128.1(14) . . ? C4 C1 W1 165.5(11) . . ? C5 N7 C6 116.7(16) . . ? N2 C12 C11 108.3(14) . . ? N2 C12 C13 122.2(15) . . ? C11 C12 C13 129.4(15) . . ? N7 C5 C4 125.7(15) . . ? N7 C5 H5 117.2 . . ? C4 C5 H5 117.2 . . ? C7 C6 N7 123.6(16) . . ? C7 C6 H6 118.2 . . ? N7 C6 H6 118.2 . . ? C131 C133 C135 107(3) . . ? C131 C133 H133 126.3 . . ? C135 C133 H133 126.3 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C134 C136 N15 110(4) . . ? C134 C136 C138 129(4) . . ? N15 C136 C138 121(4) . . ? N10 B3 N15 116(3) . . ? N10 B3 N18 112(3) . . ? N15 B3 N18 109(2) . . ? N10 B3 H3 106.7 . . ? N15 B3 H3 106.7 . . ? N18 B3 H3 106.7 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C141 N16 N17 103(2) . . ? C141 N16 W2 136(2) . . ? N17 N16 W2 120.7(14) . . ? N13 C131 C133 111(3) . . ? N13 C131 C129 122(3) . . ? C133 C131 C129 127(3) . . ? C4 C8 C7 119.3(17) . . ? C4 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? C125 C124 H12G 109.5 . . ? C125 C124 H12H 109.5 . . ? H12G C124 H12H 109.5 . . ? C125 C124 H12I 109.5 . . ? H12G C124 H12I 109.5 . . ? H12H C124 H12I 109.5 . . ? N14 B2 N17 106.8(19) . . ? N14 B2 N11 112.6(19) . . ? N17 B2 N11 116.0(18) . . ? N14 B2 H2 107.0 . . ? N17 B2 H2 107.0 . . ? N11 B2 H2 107.0 . . ? C144 C146 N18 109(5) . . ? C144 C146 C148 133(6) . . ? N18 C146 C148 118(4) . . ? C6 C7 C8 119.5(17) . . ? C6 C7 H7 120.2 . . ? C8 C7 H7 120.2 . . ? C126 C127 N10 106(3) . . ? C126 C127 C128 136(4) . . ? N10 C127 C128 116(4) . . ? O103 C117 W3 169(5) . . ? N17 C145 C143 111(3) . . ? N17 C145 C147 118(3) . . ? C143 C145 C147 131(3) . . ? N9 C106 C107 124(4) . . ? N9 C106 H106 118.1 . . ? C107 C106 H106 118.1 . . ? C141 C143 C145 103(3) . . ? C141 C143 H143 128.3 . . ? C145 C143 H143 128.3 . . ? C136 N15 N14A 111(3) . . ? C136 N15 B3 131(3) . . ? N14A N15 B3 117(3) . . ? C121 C122 H12A 109.5 . . ? C121 C122 H12B 109.5 . . ? H12A C122 H12B 109.5 . . ? C121 C122 H12C 109.5 . . ? H12A C122 H12C 109.5 . . ? H12B C122 H12C 109.5 . . ? C105 C104 C101 118(3) . . ? C105 C104 C108 115(3) . . ? C101 C104 C108 127(3) . . ? C146 N18 N17A 107(3) . . ? C146 N18 B3 136(4) . . ? N17A N18 B3 117(3) . . ? C104 C105 N9 126(3) . . ? C104 C105 H105 116.9 . . ? N9 C105 H105 116.9 . . ? C119 N12 N11 102(2) . . ? C119 N12 W2 129(2) . . ? N11 N12 W2 128.3(15) . . ? O102 C116 W2 175(3) . . ? C104 C101 W2 163(3) . . ? O104 C102 W2 173(3) . . ? C20 C19 H19A 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C20 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N17A C142 C144 120(4) . . ? N17A C142 C140 110(4) . . ? C144 C142 C140 130(4) . . ? C106 N9 C105 114(3) . . ? C107 C108 C104 118(4) . . ? C107 C108 H108 121.2 . . ? C104 C108 H108 121.2 . . ? C108 C107 C106 123(5) . . ? C108 C107 H107 118.7 . . ? C106 C107 H107 118.7 . . ? C131 N13 N14 105(2) . . ? C131 N13 W2 134(2) . . ? N14 N13 W2 120.6(17) . . ? C141 C139 H13D 109.5 . . ? C141 C139 H13E 109.5 . . ? H13D C139 H13E 109.5 . . ? C141 C139 H13F 109.5 . . ? H13D C139 H13F 109.5 . . ? H13E C139 H13F 109.5 . . ? B3 N10 C127 135(3) . . ? B3 N10 N11A 110(3) . . ? C127 N10 N11A 115(3) . . ? C142 C144 C146 105(4) . . ? C142 C144 H144 127.4 . . ? C146 C144 H144 127.4 . . ? C119 C118 H11A 109.5 . . ? C119 C118 H11B 109.5 . . ? H11A C118 H11B 109.5 . . ? C119 C118 H11C 109.5 . . ? H11A C118 H11C 109.5 . . ? H11B C118 H11C 109.5 . . ? C135 C137 H13G 109.5 . . ? C135 C137 H13H 109.5 . . ? H13G C137 H13H 109.5 . . ? C135 C137 H13I 109.5 . . ? H13G C137 H13I 109.5 . . ? H13H C137 H13I 109.5 . . ? C114 C113 C112 122(6) . . ? C114 C113 H113 118.9 . . ? C112 C113 H113 118.9 . . ? C114 C110 C111 118(5) . . ? C114 C110 C109 119(4) . . ? C111 C110 C109 123(5) . . ? C111 N8 C112 124(7) . . ? C110 C114 C113 126(5) . . ? C110 C114 H114 116.9 . . ? C113 C114 H114 116.9 . . ? C110 C111 N8 123(6) . . ? C110 C111 H111 118.5 . . ? N8 C111 H111 118.5 . . ? C127 C128 H12J 109.5 . . ? C127 C128 H12K 109.5 . . ? H12J C128 H12K 109.5 . . ? C127 C128 H12L 109.5 . . ? H12J C128 H12L 109.5 . . ? H12K C128 H12L 109.5 . . ? O101 C149 W3 176(3) . . ? C123 C119 N12 102(3) . . ? C123 C119 C118 135(4) . . ? N12 C119 C118 122(3) . . ? C136 C134 C132 105(3) . . ? C136 C134 H134 127.4 . . ? C132 C134 H134 127.4 . . ? C146 C148 H14G 109.5 . . ? C146 C148 H14H 109.5 . . ? H14G C148 H14H 109.5 . . ? C146 C148 H14I 109.5 . . ? H14G C148 H14I 109.5 . . ? H14H C148 H14I 109.5 . . ? C136 C138 H13J 109.5 . . ? C136 C138 H13K 109.5 . . ? H13J C138 H13K 109.5 . . ? C136 C138 H13L 109.5 . . ? H13J C138 H13L 109.5 . . ? H13K C138 H13L 109.5 . . ? C142 C140 H14J 109.5 . . ? C142 C140 H14K 109.5 . . ? H14J C140 H14K 109.5 . . ? C142 C140 H14L 109.5 . . ? H14J C140 H14L 109.5 . . ? H14K C140 H14L 109.5 . . ? C121 C123 C119 114(3) . . ? C121 C123 H123 122.8 . . ? C119 C123 H123 122.8 . . ? N11 C121 C123 116(3) . . ? N11 C121 C122 117(4) . . ? C123 C121 C122 127(4) . . ? C145 C147 H14D 109.5 . . ? C145 C147 H14E 109.5 . . ? H14D C147 H14E 109.5 . . ? C145 C147 H14F 109.5 . . ? H14D C147 H14F 109.5 . . ? H14E C147 H14F 109.5 . . ? C125 C126 C127 109(4) . . ? C125 C126 H126 125.4 . . ? C127 C126 H126 125.4 . . ? C131 C129 H12D 109.5 . . ? C131 C129 H12E 109.5 . . ? H12D C129 H12E 109.5 . . ? C131 C129 H12F 109.5 . . ? H12D C129 H12F 109.5 . . ? H12E C129 H12F 109.5 . . ? N14 C135 C133 108(3) . . ? N14 C135 C137 122(3) . . ? C133 C135 C137 130(3) . . ? C130 C132 N14A 122(4) . . ? C130 C132 C134 129(4) . . ? N14A C132 C134 109(3) . . ? C132 C130 H13M 109.5 . . ? C132 C130 H13N 109.5 . . ? H13M C130 H13N 109.5 . . ? C132 C130 H13O 109.5 . . ? H13M C130 H13O 109.5 . . ? H13N C130 H13O 109.5 . . ? C113 C112 N8 107(7) . . ? C113 C112 H112 126.5 . . ? N8 C112 H112 126.5 . . ? C110 C109 W3 159(4) . . ? C142 N17A N18 99(3) . . ? C142 N17A W3 146(3) . . ? N18 N17A W3 115(2) . . ? N15 N14A C132 104(3) . . ? N15 N14A W3 120(3) . . ? C132 N14A W3 136(3) . . ? C125 N11A N10 83(3) . . ? C125 N11A W3 150(3) . . ? N10 N11A W3 122(2) . . ? 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 W1 C1 1.804(15) . ? W1 C3 1.964(19) . ? W1 C2 2.033(15) . ? W1 N3 2.201(10) . ? W1 N5 2.228(10) . ? W1 N1 2.305(10) . ? W2 C101 1.84(2) . ? W2 C116 2.01(3) . ? W2 C102 2.03(3) . ? W2 N12 2.14(2) . ? W2 N16 2.20(2) . ? W2 N13 2.29(2) . ? W3 C109 1.81(2) . ? W3 N11A 1.90(3) . ? W3 C149 1.98(4) . ? W3 C117 2.01(4) . ? W3 N17A 2.14(4) . ? W3 N14A 2.19(3) . ? N5 C15 1.331(17) . ? N5 N6 1.351(14) . ? N3 N4 1.369(15) . ? N3 C20 1.376(16) . ? N2 C12 1.344(17) . ? N2 N1 1.363(16) . ? N2 B1 1.540(18) . ? N4 C22 1.340(17) . ? N4 B1 1.540(18) . ? O2 C3 1.18(2) . ? N1 C10 1.350(17) . ? O1 C2 1.118(18) . ? N6 C17 1.364(16) . ? N6 B1 1.534(18) . ? N17 C145 1.35(4) . ? N17 N16 1.46(3) . ? N17 B2 1.57(3) . ? C22 C21 1.36(2) . ? C22 C23 1.49(2) . ? C17 C16 1.37(2) . ? C17 C18 1.48(2) . ? N11 C121 1.16(4) . ? N11 B2 1.57(3) . ? N11 N12 1.64(3) . ? C16 C15 1.40(2) . ? C16 H16 0.9300 . ? N14 C135 1.36(4) . ? N14 N13 1.42(4) . ? N14 B2 1.49(4) . ? C15 C14 1.48(2) . ? B1 H1 1.14(3) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C11 C12 1.36(2) . ? C11 C10 1.39(2) . ? C11 H11 0.9300 . ? C21 C20 1.39(2) . ? C21 H21 0.9300 . ? C20 C19 1.49(2) . ? C4 C8 1.38(2) . ? C4 C5 1.38(2) . ? C4 C1 1.460(19) . ? C9 C10 1.52(3) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C141 N16 1.28(4) . ? C141 C143 1.33(5) . ? C141 C139 1.54(5) . ? C125 C126 1.28(6) . ? C125 C124 1.50(6) . ? C125 N11A 1.56(5) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? N7 C5 1.32(2) . ? N7 C6 1.32(2) . ? C12 C13 1.49(2) . ? C5 H5 0.9300 . ? C6 C7 1.32(3) . ? C6 H6 0.9300 . ? C133 C131 1.37(4) . ? C133 C135 1.38(5) . ? C133 H133 0.9300 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C136 C134 1.35(6) . ? C136 N15 1.38(5) . ? C136 C138 1.51(6) . ? B3 N10 1.39(4) . ? B3 N15 1.52(4) . ? B3 N18 1.57(4) . ? B3 H3 1.15(3) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C131 N13 1.37(4) . ? C131 C129 1.50(5) . ? C8 C7 1.39(3) . ? C8 H8 0.9300 . ? C124 H12G 0.9600 . ? C124 H12H 0.9600 . ? C124 H12I 0.9600 . ? B2 H2 1.15(3) . ? C146 C144 1.36(3) . ? C146 N18 1.40(8) . ? C146 C148 1.50(3) . ? C7 H7 0.9300 . ? C127 C126 1.34(6) . ? C127 N10 1.43(5) . ? C127 C128 1.52(7) . ? C117 O103 1.10(6) . ? C145 C143 1.36(4) . ? C145 C147 1.49(5) . ? O102 C116 1.10(4) . ? C106 N9 1.34(4) . ? C106 C107 1.34(7) . ? C106 H106 0.9300 . ? C143 H143 0.9300 . ? N15 N14A 1.39(5) . ? C122 C121 1.48(5) . ? C122 H12A 0.9600 . ? C122 H12B 0.9600 . ? C122 H12C 0.9600 . ? C104 C105 1.33(4) . ? C104 C101 1.45(2) . ? C104 C108 1.48(5) . ? N18 N17A 1.56(5) . ? C105 N9 1.40(4) . ? C105 H105 0.9300 . ? O101 C149 1.16(5) . ? N12 C119 1.42(4) . ? C102 O104 1.15(4) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C142 N17A 1.29(5) . ? C142 C144 1.35(3) . ? C142 C140 1.48(3) . ? C108 C107 1.31(8) . ? C108 H108 0.9300 . ? C107 H107 0.9300 . ? C139 H13D 0.9600 . ? C139 H13E 0.9600 . ? C139 H13F 0.9600 . ? N10 N11A 1.70(5) . ? C144 H144 0.9300 . ? C118 C119 1.44(5) . ? C118 H11A 0.9600 . ? C118 H11B 0.9600 . ? C118 H11C 0.9600 . ? C137 C135 1.42(5) . ? C137 H13G 0.9600 . ? C137 H13H 0.9600 . ? C137 H13I 0.9600 . ? C113 C114 1.41(7) . ? C113 C112 1.49(11) . ? C113 H113 0.9300 . ? C110 C114 1.31(6) . ? C110 C111 1.34(8) . ? C110 C109 1.46(3) . ? N8 C111 1.39(8) . ? N8 C112 1.56(12) . ? C114 H114 0.9300 . ? C111 H111 0.9300 . ? C128 H12J 0.9600 . ? C128 H12K 0.9600 . ? C128 H12L 0.9600 . ? C119 C123 1.40(5) . ? C134 C132 1.47(5) . ? C134 H134 0.9300 . ? C148 H14G 0.9600 . ? C148 H14H 0.9600 . ? C148 H14I 0.9600 . ? C138 H13J 0.9600 . ? C138 H13K 0.9600 . ? C138 H13L 0.9600 . ? C140 H14J 0.9600 . ? C140 H14K 0.9600 . ? C140 H14L 0.9600 . ? C123 C121 1.30(5) . ? C123 H123 0.9300 . ? C147 H14D 0.9600 . ? C147 H14E 0.9600 . ? C147 H14F 0.9600 . ? C126 H126 0.9300 . ? C129 H12D 0.9600 . ? C129 H12E 0.9600 . ? C129 H12F 0.9600 . ? C132 C130 1.41(6) . ? C132 N14A 1.42(5) . ? C130 H13M 0.9600 . ? C130 H13N 0.9600 . ? C130 H13O 0.9600 . ? C112 H112 0.9300 . ? 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 C20 N3 N4 C22 1.6(15) . . . . ? W1 N3 N4 C22 -176.2(9) . . . . ? C20 N3 N4 B1 -179.3(11) . . . . ? W1 N3 N4 B1 3.0(15) . . . . ? C12 N2 N1 C10 0.0(15) . . . . ? B1 N2 N1 C10 178.4(12) . . . . ? C12 N2 N1 W1 -180.0(9) . . . . ? B1 N2 N1 W1 -1.6(15) . . . . ? C15 N5 N6 C17 -1.2(15) . . . . ? W1 N5 N6 C17 175.1(8) . . . . ? C15 N5 N6 B1 -178.9(12) . . . . ? W1 N5 N6 B1 -2.6(15) . . . . ? N3 N4 C22 C21 -1.4(15) . . . . ? B1 N4 C22 C21 179.6(13) . . . . ? N3 N4 C22 C23 175.7(14) . . . . ? B1 N4 C22 C23 -3(2) . . . . ? N5 N6 C17 C16 1.4(15) . . . . ? B1 N6 C17 C16 178.8(13) . . . . ? N5 N6 C17 C18 -179.6(13) . . . . ? B1 N6 C17 C18 -2(2) . . . . ? N6 C17 C16 C15 -1.0(17) . . . . ? C18 C17 C16 C15 -180.0(15) . . . . ? N6 N5 C15 C16 0.6(17) . . . . ? W1 N5 C15 C16 -175.2(10) . . . . ? N6 N5 C15 C14 -177.8(16) . . . . ? W1 N5 C15 C14 6(2) . . . . ? C17 C16 C15 N5 0.3(18) . . . . ? C17 C16 C15 C14 178.6(17) . . . . ? N5 N6 B1 N2 62.8(15) . . . . ? C17 N6 B1 N2 -114.3(14) . . . . ? N5 N6 B1 N4 -56.9(14) . . . . ? C17 N6 B1 N4 126.0(13) . . . . ? C12 N2 B1 N6 119.2(15) . . . . ? N1 N2 B1 N6 -58.7(15) . . . . ? C12 N2 B1 N4 -121.5(15) . . . . ? N1 N2 B1 N4 60.6(15) . . . . ? C22 N4 B1 N6 -124.5(14) . . . . ? N3 N4 B1 N6 56.5(14) . . . . ? C22 N4 B1 N2 116.4(14) . . . . ? N3 N4 B1 N2 -62.6(14) . . . . ? N4 C22 C21 C20 0.6(17) . . . . ? C23 C22 C21 C20 -176.1(16) . . . . ? N4 N3 C20 C21 -1.1(16) . . . . ? W1 N3 C20 C21 176.4(10) . . . . ? N4 N3 C20 C19 179.1(14) . . . . ? W1 N3 C20 C19 -3(2) . . . . ? C22 C21 C20 N3 0.3(18) . . . . ? C22 C21 C20 C19 -180.0(16) . . . . ? N2 N1 C10 C11 -0.3(16) . . . . ? W1 N1 C10 C11 179.7(10) . . . . ? N2 N1 C10 C9 -179.2(15) . . . . ? W1 N1 C10 C9 1(2) . . . . ? C12 C11 C10 N1 0.5(18) . . . . ? C12 C11 C10 C9 179.3(17) . . . . ? C8 C4 C1 W1 -101(4) . . . . ? C5 C4 C1 W1 78(4) . . . . ? C3 W1 C1 C4 -38(4) . . . . ? C2 W1 C1 C4 50(4) . . . . ? N3 W1 C1 C4 -132(4) . . . . ? N5 W1 C1 C4 143(4) . . . . ? N1 W1 C1 C4 0(6) . . . . ? N1 N2 C12 C11 0.2(17) . . . . ? B1 N2 C12 C11 -177.9(13) . . . . ? N1 N2 C12 C13 -179.1(14) . . . . ? B1 N2 C12 C13 3(2) . . . . ? C10 C11 C12 N2 -0.4(18) . . . . ? C10 C11 C12 C13 178.8(17) . . . . ? C6 N7 C5 C4 -1(3) . . . . ? C8 C4 C5 N7 1(3) . . . . ? C1 C4 C5 N7 -177.2(17) . . . . ? C5 N7 C6 C7 -1(3) . . . . ? C143 C141 N16 N17 -4(4) . . . . ? C139 C141 N16 N17 179(3) . . . . ? C143 C141 N16 W2 -173(2) . . . . ? C139 C141 N16 W2 10(5) . . . . ? C145 N17 N16 C141 3(3) . . . . ? B2 N17 N16 C141 179(2) . . . . ? C145 N17 N16 W2 174.3(17) . . . . ? B2 N17 N16 W2 -9(3) . . . . ? C135 C133 C131 N13 0(3) . . . . ? C135 C133 C131 C129 178(3) . . . . ? C5 C4 C8 C7 0(3) . . . . ? C1 C4 C8 C7 178.2(19) . . . . ? C135 N14 B2 N17 123(3) . . . . ? N13 N14 B2 N17 -59(3) . . . . ? C135 N14 B2 N11 -109(3) . . . . ? N13 N14 B2 N11 70(3) . . . . ? C145 N17 B2 N14 -117(3) . . . . ? N16 N17 B2 N14 68(3) . . . . ? C145 N17 B2 N11 117(3) . . . . ? N16 N17 B2 N11 -58(3) . . . . ? C121 N11 B2 N14 127(5) . . . . ? N12 N11 B2 N14 -71(2) . . . . ? C121 N11 B2 N17 -110(5) . . . . ? N12 N11 B2 N17 53(2) . . . . ? N7 C6 C7 C8 2(4) . . . . ? C4 C8 C7 C6 -1(4) . . . . ? N16 N17 C145 C143 -1(3) . . . . ? B2 N17 C145 C143 -176(3) . . . . ? N16 N17 C145 C147 180(3) . . . . ? B2 N17 C145 C147 4(5) . . . . ? N16 C141 C143 C145 3(4) . . . . ? C139 C141 C143 C145 -180(3) . . . . ? N17 C145 C143 C141 -1(3) . . . . ? C147 C145 C143 C141 178(4) . . . . ? C134 C136 N15 N14A -8(5) . . . . ? C138 C136 N15 N14A 173(4) . . . . ? C134 C136 N15 B3 178(3) . . . . ? C138 C136 N15 B3 -1(6) . . . . ? N10 B3 N15 C136 -122(4) . . . . ? N18 B3 N15 C136 111(4) . . . . ? N10 B3 N15 N14A 64(4) . . . . ? N18 B3 N15 N14A -63(4) . . . . ? C144 C146 N18 N17A -4(7) . . . . ? C148 C146 N18 N17A 176(5) . . . . ? C144 C146 N18 B3 179(4) . . . . ? C148 C146 N18 B3 0(10) . . . . ? N10 B3 N18 C146 109(6) . . . . ? N15 B3 N18 C146 -122(6) . . . . ? N10 B3 N18 N17A -67(4) . . . . ? N15 B3 N18 N17A 62(4) . . . . ? C101 C104 C105 N9 177(3) . . . . ? C108 C104 C105 N9 -1(5) . . . . ? C121 N11 N12 C119 -4(3) . . . . ? B2 N11 N12 C119 -174(2) . . . . ? C121 N11 N12 W2 -176(2) . . . . ? B2 N11 N12 W2 14(2) . . . . ? C105 C104 C101 W2 4(11) . . . . ? C108 C104 C101 W2 -178(8) . . . . ? C116 W2 C101 C104 -44(9) . . . . ? C102 W2 C101 C104 41(9) . . . . ? N12 W2 C101 C104 -136(9) . . . . ? N16 W2 C101 C104 141(9) . . . . ? N13 W2 C101 C104 6(14) . . . . ? C107 C106 N9 C105 4(6) . . . . ? C104 C105 N9 C106 -4(5) . . . . ? C105 C104 C108 C107 6(5) . . . . ? C101 C104 C108 C107 -172(4) . . . . ? C104 C108 C107 C106 -6(7) . . . . ? N9 C106 C107 C108 2(7) . . . . ? C133 C131 N13 N14 0(3) . . . . ? C129 C131 N13 N14 -178(3) . . . . ? C133 C131 N13 W2 -174(2) . . . . ? C129 C131 N13 W2 8(4) . . . . ? C135 N14 N13 C131 0(3) . . . . ? B2 N14 N13 C131 -179(2) . . . . ? C135 N14 N13 W2 175(2) . . . . ? B2 N14 N13 W2 -4(3) . . . . ? N15 B3 N10 C127 111(4) . . . . ? N18 B3 N10 C127 -124(4) . . . . ? N15 B3 N10 N11A -71(3) . . . . ? N18 B3 N10 N11A 54(3) . . . . ? C126 C127 N10 B3 177(4) . . . . ? C128 C127 N10 B3 7(6) . . . . ? C126 C127 N10 N11A -1(4) . . . . ? C128 C127 N10 N11A -171(3) . . . . ? N17A C142 C144 C146 2(7) . . . . ? C140 C142 C144 C146 179(5) . . . . ? N18 C146 C144 C142 2(7) . . . . ? C148 C146 C144 C142 -179(7) . . . . ? C111 C110 C114 C113 1(8) . . . . ? C109 C110 C114 C113 -176(5) . . . . ? C112 C113 C114 C110 1(9) . . . . ? C114 C110 C111 N8 0(9) . . . . ? C109 C110 C111 N8 177(5) . . . . ? C112 N8 C111 C110 -3(11) . . . . ? N11 N12 C119 C123 4(3) . . . . ? W2 N12 C119 C123 176(2) . . . . ? N11 N12 C119 C118 178(3) . . . . ? W2 N12 C119 C118 -10(4) . . . . ? N15 C136 C134 C132 4(4) . . . . ? C138 C136 C134 C132 -176(4) . . . . ? N12 C119 C123 C121 -4(4) . . . . ? C118 C119 C123 C121 -177(4) . . . . ? B2 N11 C121 C123 163(4) . . . . ? N12 N11 C121 C123 1(4) . . . . ? B2 N11 C121 C122 -17(7) . . . . ? N12 N11 C121 C122 -180(3) . . . . ? C119 C123 C121 N11 2(5) . . . . ? C119 C123 C121 C122 -177(3) . . . . ? C124 C125 C126 C127 -178(4) . . . . ? N11A C125 C126 C127 -6(6) . . . . ? N10 C127 C126 C125 4(5) . . . . ? C128 C127 C126 C125 170(5) . . . . ? N13 N14 C135 C133 0(4) . . . . ? B2 N14 C135 C133 179(3) . . . . ? N13 N14 C135 C137 -177(3) . . . . ? B2 N14 C135 C137 1(6) . . . . ? C131 C133 C135 N14 0(4) . . . . ? C131 C133 C135 C137 177(4) . . . . ? C136 C134 C132 C130 176(4) . . . . ? C136 C134 C132 N14A 1(4) . . . . ? C114 C113 C112 N8 -3(10) . . . . ? C111 N8 C112 C113 4(11) . . . . ? C114 C110 C109 W3 129(9) . . . . ? C111 C110 C109 W3 -48(13) . . . . ? N11A W3 C109 C110 -173(10) . . . . ? C149 W3 C109 C110 -79(10) . . . . ? C117 W3 C109 C110 5(10) . . . . ? N17A W3 C109 C110 102(10) . . . . ? N14A W3 C109 C110 -19(16) . . . . ? C144 C142 N17A N18 -5(5) . . . . ? C140 C142 N17A N18 178(3) . . . . ? C144 C142 N17A W3 173(4) . . . . ? C140 C142 N17A W3 -4(7) . . . . ? C146 N18 N17A C142 5(5) . . . . ? B3 N18 N17A C142 -178(3) . . . . ? C146 N18 N17A W3 -173(4) . . . . ? B3 N18 N17A W3 4(4) . . . . ? C136 N15 N14A C132 8(4) . . . . ? B3 N15 N14A C132 -177(3) . . . . ? C136 N15 N14A W3 -177(2) . . . . ? B3 N15 N14A W3 -2(4) . . . . ? C130 C132 N14A N15 179(4) . . . . ? C134 C132 N14A N15 -5(4) . . . . ? C130 C132 N14A W3 5(6) . . . . ? C134 C132 N14A W3 -179(2) . . . . ? C126 C125 N11A N10 4(4) . . . . ? C124 C125 N11A N10 178(3) . . . . ? C126 C125 N11A W3 153(5) . . . . ? C124 C125 N11A W3 -34(6) . . . . ? B3 N10 N11A C125 -180(3) . . . . ? C127 N10 N11A C125 -1(3) . . . . ? B3 N10 N11A W3 18(3) . . . . ? C127 N10 N11A W3 -163(2) . . . . ?