#------------------------------------------------------------------------------ #$Date: 2021-05-07 05:26:07 +0300 (Fri, 07 May 2021) $ #$Revision: 265025 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/73/7707356.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_7707356 loop_ _publ_author_name 'Wang, Kuiyuan' 'Prior, Timothy J.' 'Hughes, David L.' 'Arbaoui, Abdessamad' 'Redshaw, Carl' _publ_section_title ; Coordination chemistry of [2+2] Schiff-base macrocycles derived from the dianilines [(2-NH2C6H4)2X] (X = CH2CH2, O): Structural studies and ROP capability towards cyclic esters. ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D1DT00711D _journal_year 2021 _chemical_formula_moiety 'C52 H52 Br Fe N4 O2, Br, 5.5[CH3CN]' _chemical_formula_sum 'C52 H52 Br2 Fe N4 O2' _chemical_formula_weight 980.64 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _audit_creation_date 2021-04-28 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6257) ; _audit_update_record ; 2021-04-28 deposited with the CCDC. 2021-05-04 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 112.484(6) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.2077(6) _cell_length_b 27.6241(9) _cell_length_c 15.1579(8) _cell_measurement_reflns_used 16199 _cell_measurement_temperature 100.15 _cell_measurement_theta_max 2.148 _cell_measurement_theta_min 27.526 _cell_volume 5496.9(5) _computing_cell_refinement 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _diffrn_ambient_temperature 100.15 _diffrn_detector_area_resol_mean 28.5714 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measurement_device_type 'Rigaku HG Saturn724+ (2x2 bin mode)' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0562 _diffrn_reflns_av_unetI/netI 0.0498 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.989 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 47911 _diffrn_reflns_point_group_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.989 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.485 _diffrn_reflns_theta_min 3.097 _diffrn_source 'fine-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 1.766 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.55484 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour brown _exptl_crystal_density_diffrn 1.185 _exptl_crystal_description plate _exptl_crystal_F_000 2016 _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.045 _exptl_crystal_size_min 0.01 _refine_diff_density_max 0.901 _refine_diff_density_min -1.613 _refine_diff_density_rms 0.110 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 556 _refine_ls_number_reflns 12466 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.050 _refine_ls_R_factor_all 0.0880 _refine_ls_R_factor_gt 0.0668 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0724P)^2^+20.1735P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1681 _refine_ls_wR_factor_ref 0.1796 _reflns_Friedel_coverage 0.000 _reflns_number_gt 9446 _reflns_number_total 12466 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt00711d2.cif _cod_data_source_block ferop3 _cod_database_code 7707356 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.983 _shelx_estimated_absorpt_t_min 0.657 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Secondary CH2 refined with riding coordinates: C18(H18A,H18B), C19(H19A,H19B), C44(H44A,H44B), C45(H45A,H45B) 2.b Aromatic/amide H refined with riding coordinates: C3(H3), C5(H5), C11(H11), C13(H13), C14(H14), C15(H15), C16(H16), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26), C29(H29), C31(H31), C37(H37), C39(H39), C40(H40), C41(H41), C42(H42), C47(H47), C48(H48), C49(H49), C50(H50), C52(H52), N2(H2), N3(H3A) 2.c Idealised Me refined as rotating group: C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C) ; _smtbx_masks_special_details ; A solvent mask was calculated and 496 electrons were found in a volume of 1544\%A^3^ in 1 void per unit cell. This is consistent with the presence of 5.5[CH3CN] per Asymmetric Unit which account for 484 electrons per unit cell. ; _smtbx_masks_void_probe_radius 1.2 _smtbx_masks_void_truncation_radius 1.2 _shelx_res_file ; TITL shelxt_a.res in P2(1)/n ferop3.res created by SHELXL-2018/3 at 17:14:18 on 28-Apr-2021 CELL 0.71073 14.2077 27.6241 15.1579 90 112.484 90 ZERR 4 0.0006 0.0009 0.0008 0 0.006 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H Br Fe N O UNIT 208 208 8 4 16 8 L.S. 10 PLAN 24 SIZE 0.01 0.045 0.26 TEMP -173 CONF BOND $H LIST 6 MORE -1 ABIN fmap 2 acta MERG 2 SHEL 6.6 0.65 OMIT 0 5 2 REM REM REM WGHT 0.072400 20.173500 FVAR 2.20612 C1 1 0.159647 0.444374 0.511215 11.00000 0.01662 0.02787 = 0.01953 0.00119 0.00813 -0.00116 C2 1 0.077778 0.455093 0.423712 11.00000 0.02042 0.03001 = 0.03205 0.00309 0.01401 -0.00083 C3 1 0.036153 0.418759 0.354388 11.00000 0.02545 0.03277 = 0.03016 0.00348 0.00753 -0.00570 AFIX 43 H3 2 -0.019398 0.426832 0.297100 11.00000 -1.20000 AFIX 0 C4 1 0.072730 0.371981 0.366282 11.00000 0.02738 0.02933 = 0.02403 -0.00020 0.00868 -0.00436 C5 1 0.157572 0.363044 0.450101 11.00000 0.02499 0.01958 = 0.03847 0.00234 0.01021 -0.00224 AFIX 43 H5 2 0.186597 0.331548 0.459240 11.00000 -1.20000 AFIX 0 C6 1 0.202242 0.397591 0.521195 11.00000 0.02699 0.02596 = 0.02439 0.00411 0.00957 0.00111 C7 1 0.027024 0.331325 0.295178 11.00000 0.03028 0.03415 = 0.03231 -0.00335 0.00705 -0.00725 C8 1 -0.053762 0.350722 0.201932 11.00000 0.07162 0.03498 = 0.03877 -0.00007 -0.00718 -0.01686 AFIX 137 H8A 2 -0.111187 0.364015 0.214809 11.00000 -1.50000 H8B 2 -0.077837 0.324300 0.155531 11.00000 -1.50000 H8C 2 -0.023781 0.376222 0.175989 11.00000 -1.50000 AFIX 0 C9 1 -0.023435 0.293987 0.336988 11.00000 0.03933 0.02935 = 0.04243 -0.00443 0.01704 -0.00621 AFIX 137 H9A 2 0.028406 0.278612 0.392707 11.00000 -1.50000 H9B 2 -0.057131 0.269318 0.288754 11.00000 -1.50000 H9C 2 -0.073998 0.310042 0.356364 11.00000 -1.50000 AFIX 0 C10 1 0.110344 0.306143 0.270995 11.00000 0.05608 0.05712 = 0.04787 -0.02476 0.03143 -0.01797 AFIX 137 H10A 2 0.148648 0.330390 0.251158 11.00000 -1.50000 H10B 2 0.078981 0.283017 0.218937 11.00000 -1.50000 H10C 2 0.156649 0.288928 0.327436 11.00000 -1.50000 AFIX 0 C11 1 0.295980 0.383614 0.598857 11.00000 0.02717 0.02725 = 0.02428 0.00570 0.01238 0.00417 AFIX 43 H11 2 0.318348 0.351270 0.598024 11.00000 -1.20000 AFIX 0 C12 1 0.443529 0.388081 0.733624 11.00000 0.02017 0.02478 = 0.02618 0.00019 0.00953 0.00236 C13 1 0.535631 0.401432 0.727482 11.00000 0.02247 0.03763 = 0.03466 0.00653 0.01152 0.00505 AFIX 43 H13 2 0.535932 0.424202 0.680622 11.00000 -1.20000 AFIX 0 C14 1 0.626763 0.381631 0.789448 11.00000 0.01888 0.04679 = 0.04038 0.01194 0.01247 0.00515 AFIX 43 H14 2 0.689268 0.391342 0.785693 11.00000 -1.20000 AFIX 0 C15 1 0.626639 0.347862 0.856477 11.00000 0.02224 0.03810 = 0.03393 0.00205 0.00775 0.00667 AFIX 43 H15 2 0.688640 0.334030 0.898930 11.00000 -1.20000 AFIX 0 C16 1 0.533790 0.334375 0.860819 11.00000 0.03122 0.02279 = 0.02994 0.00114 0.01501 0.00189 AFIX 43 H16 2 0.533492 0.310250 0.905376 11.00000 -1.20000 AFIX 0 C17 1 0.442601 0.354783 0.802835 11.00000 0.02360 0.02261 = 0.02511 -0.00196 0.01222 0.00018 C18 1 0.345598 0.341716 0.815935 11.00000 0.02080 0.02907 = 0.02903 0.00380 0.00717 -0.00388 AFIX 23 H18A 2 0.350001 0.307664 0.837515 11.00000 -1.20000 H18B 2 0.287691 0.344181 0.753580 11.00000 -1.20000 AFIX 0 C19 1 0.324461 0.374501 0.888943 11.00000 0.02012 0.03338 = 0.03839 0.00579 0.01493 0.00189 AFIX 23 H19A 2 0.325754 0.408787 0.870427 11.00000 -1.20000 H19B 2 0.255486 0.367442 0.887279 11.00000 -1.20000 AFIX 0 C20 1 0.401353 0.367264 0.989267 11.00000 0.03210 0.02277 = 0.03352 0.00274 0.01881 0.00430 C21 1 0.386272 0.329344 1.044169 11.00000 0.02994 0.03109 = 0.03470 0.00260 0.02011 0.00086 AFIX 43 H21 2 0.327275 0.309653 1.017595 11.00000 -1.20000 AFIX 0 C22 1 0.454905 0.319836 1.135896 11.00000 0.05328 0.02684 = 0.03370 0.00817 0.02827 0.00764 AFIX 43 H22 2 0.442958 0.293807 1.171245 11.00000 -1.20000 AFIX 0 C23 1 0.540401 0.348136 1.175746 11.00000 0.05227 0.02964 = 0.02473 0.00256 0.01803 0.00711 AFIX 43 H23 2 0.587100 0.341452 1.238787 11.00000 -1.20000 AFIX 0 C24 1 0.559693 0.386331 1.125447 11.00000 0.03830 0.02859 = 0.02337 0.00174 0.01272 0.00439 AFIX 43 H24 2 0.618584 0.405953 1.153474 11.00000 -1.20000 AFIX 0 C25 1 0.490452 0.395122 1.032832 11.00000 0.03159 0.02310 = 0.02364 0.00114 0.01317 0.00265 C26 1 0.594674 0.455647 0.995540 11.00000 0.02767 0.02698 = 0.02690 -0.00025 0.01205 0.00333 AFIX 43 H26 2 0.650549 0.447688 1.052660 11.00000 -1.20000 AFIX 0 C27 1 0.531536 0.503486 0.845641 11.00000 0.02018 0.02500 = 0.02689 -0.00179 0.01169 0.00210 C28 1 0.609993 0.491240 0.935429 11.00000 0.02051 0.02473 = 0.02733 -0.00241 0.01063 0.00254 C29 1 0.707024 0.512201 0.962890 11.00000 0.02458 0.02907 = 0.02979 0.00293 0.00933 0.00467 AFIX 43 H29 2 0.757861 0.503416 1.022745 11.00000 -1.20000 AFIX 0 C30 1 0.731776 0.545312 0.906031 11.00000 0.02301 0.03728 = 0.02147 -0.00074 0.01052 0.00136 C31 1 0.655904 0.555529 0.818238 11.00000 0.02623 0.02822 = 0.02947 -0.00047 0.01657 0.00192 AFIX 43 H31 2 0.670860 0.578118 0.778150 11.00000 -1.20000 AFIX 0 C32 1 0.558899 0.534874 0.784652 11.00000 0.02132 0.02799 = 0.02328 -0.00179 0.01007 0.00367 C33 1 0.838877 0.566767 0.935571 11.00000 0.02160 0.03779 = 0.03316 0.00011 0.00942 -0.00120 C34 1 0.907973 0.551418 1.036165 11.00000 0.02482 0.06028 = 0.04633 0.00728 -0.00056 -0.01205 AFIX 137 H34A 2 0.876111 0.560176 1.080991 11.00000 -1.50000 H34B 2 0.973794 0.567898 1.054431 11.00000 -1.50000 H34C 2 0.918436 0.516312 1.037744 11.00000 -1.50000 AFIX 0 C35 1 0.833841 0.622038 0.932485 11.00000 0.02842 0.04273 = 0.03880 -0.00231 0.01517 -0.00683 AFIX 137 H35A 2 0.813451 0.633862 0.983518 11.00000 -1.50000 H35B 2 0.783868 0.632539 0.870521 11.00000 -1.50000 H35C 2 0.900974 0.635151 0.941438 11.00000 -1.50000 AFIX 0 C36 1 0.885261 0.548827 0.864696 11.00000 0.02180 0.05426 = 0.05843 -0.01309 0.02086 -0.00439 AFIX 137 H36A 2 0.956786 0.558814 0.886930 11.00000 -1.50000 H36B 2 0.847490 0.562823 0.801565 11.00000 -1.50000 H36C 2 0.881001 0.513439 0.860528 11.00000 -1.50000 AFIX 0 C37 1 0.493711 0.543777 0.685845 11.00000 0.01923 0.02730 = 0.03116 0.00342 0.01453 0.00482 AFIX 43 H37 2 0.517711 0.566106 0.651553 11.00000 -1.20000 AFIX 0 C38 1 0.359937 0.532356 0.538636 11.00000 0.01833 0.03370 = 0.02290 0.00422 0.01108 0.00026 C39 1 0.357409 0.492967 0.480752 11.00000 0.02367 0.03134 = 0.03481 -0.00232 0.01509 0.00291 AFIX 43 H39 2 0.389623 0.463470 0.508418 11.00000 -1.20000 AFIX 0 C40 1 0.307552 0.496832 0.382114 11.00000 0.03183 0.04085 = 0.03013 -0.00772 0.01767 -0.00409 AFIX 43 H40 2 0.303321 0.469606 0.342483 11.00000 -1.20000 AFIX 0 C41 1 0.264365 0.540265 0.342152 11.00000 0.02432 0.04785 = 0.02027 0.00450 0.00882 -0.00133 AFIX 43 H41 2 0.232258 0.543382 0.274764 11.00000 -1.20000 AFIX 0 C42 1 0.267889 0.579081 0.400120 11.00000 0.02833 0.03540 = 0.02873 0.00961 0.01460 0.00025 AFIX 43 H42 2 0.238292 0.608888 0.371614 11.00000 -1.20000 AFIX 0 C43 1 0.313602 0.576122 0.499642 11.00000 0.01652 0.03163 = 0.02778 0.00322 0.01106 -0.00055 C44 1 0.305118 0.617326 0.560407 11.00000 0.02651 0.02288 = 0.03130 0.00025 0.01234 0.00085 AFIX 23 H44A 2 0.308932 0.648243 0.528908 11.00000 -1.20000 H44B 2 0.363490 0.616199 0.622632 11.00000 -1.20000 AFIX 0 C45 1 0.205337 0.616028 0.577834 11.00000 0.03022 0.02393 = 0.03116 0.00027 0.01754 0.00058 AFIX 23 H45A 2 0.198205 0.583857 0.603388 11.00000 -1.20000 H45B 2 0.208711 0.640580 0.626531 11.00000 -1.20000 AFIX 0 C46 1 0.112705 0.625719 0.488075 11.00000 0.02279 0.03059 = 0.04113 -0.00017 0.01964 0.00195 C47 1 0.089702 0.673784 0.458183 11.00000 0.02802 0.02428 = 0.04392 0.00161 0.01622 -0.00034 AFIX 43 H47 2 0.130354 0.699200 0.496058 11.00000 -1.20000 AFIX 0 C48 1 0.008288 0.684865 0.373934 11.00000 0.02725 0.03304 = 0.06794 0.01460 0.01930 0.00360 AFIX 43 H48 2 -0.004789 0.717643 0.354035 11.00000 -1.20000 AFIX 0 C49 1 -0.053297 0.649030 0.319285 11.00000 0.02252 0.03691 = 0.06623 0.01761 0.01107 0.00290 AFIX 43 H49 2 -0.109159 0.657049 0.262197 11.00000 -1.20000 AFIX 0 C50 1 -0.034072 0.601069 0.347320 11.00000 0.02064 0.03294 = 0.04600 0.00729 0.00839 -0.00233 AFIX 43 H50 2 -0.077134 0.576083 0.310354 11.00000 -1.20000 AFIX 0 C51 1 0.049286 0.589992 0.430470 11.00000 0.02051 0.02664 = 0.04007 0.00830 0.01810 0.00346 C52 1 0.041935 0.502802 0.399184 11.00000 0.01739 0.03337 = 0.03095 0.00315 0.00809 -0.00346 AFIX 43 H52 2 -0.009944 0.507974 0.337922 11.00000 -1.20000 AFIX 0 N1 5 0.352040 0.410441 0.668792 11.00000 0.02071 0.02833 = 0.03025 0.00236 0.01379 0.00159 N2 5 0.075162 0.540440 0.454935 11.00000 0.01876 0.02873 = 0.02766 0.00362 0.01070 -0.00096 AFIX 43 H2 2 0.117953 0.534618 0.513684 11.00000 -1.20000 AFIX 0 N3 5 0.508778 0.433012 0.977675 11.00000 0.02550 0.02442 = 0.02191 0.00274 0.01008 0.00162 AFIX 43 H3A 2 0.456830 0.442074 0.926289 11.00000 -1.20000 AFIX 0 N4 5 0.405443 0.524006 0.639885 11.00000 0.02210 0.02635 = 0.02438 -0.00142 0.01191 0.00000 O1 6 0.192962 0.477568 0.575931 11.00000 0.01836 0.02675 = 0.02901 0.00056 0.00704 0.00111 O2 6 0.441211 0.485794 0.823878 11.00000 0.01997 0.03439 = 0.02268 0.00315 0.00763 -0.00184 FE1 4 0.319455 0.482080 0.698159 11.00000 0.01860 0.02464 = 0.02453 0.00070 0.00833 -0.00047 BR1 3 0.208811 0.516913 0.778463 11.00000 0.02126 0.05460 = 0.02595 -0.00377 0.00937 0.00400 BR2 3 0.330231 0.748767 0.636521 11.00000 0.03929 0.02942 = 0.04610 -0.00136 0.01980 0.00320 HKLF 4 REM shelxt_a.res in P2(1)/n REM wR2 = 0.1796, GooF = S = 1.050, Restrained GooF = 1.050 for all data REM R1 = 0.0668 for 9446 Fo > 4sig(Fo) and 0.0880 for all 12466 data REM 556 parameters refined using 0 restraints END WGHT 0.0724 20.1551 REM Highest difference peak 0.901, deepest hole -1.613, 1-sigma level 0.110 Q1 1 0.3346 0.7157 0.6446 11.00000 0.05 0.90 Q2 1 0.1200 0.5199 0.7022 11.00000 0.05 0.87 Q3 1 0.3393 0.4497 0.7133 11.00000 0.05 0.86 Q4 1 0.3357 0.7827 0.6443 11.00000 0.05 0.85 Q5 1 0.1816 0.4854 0.7606 11.00000 0.05 0.80 Q6 1 0.2900 0.5098 0.8555 11.00000 0.05 0.78 Q7 1 0.2261 0.4845 0.7945 11.00000 0.05 0.76 Q8 1 0.2045 0.5276 0.7248 11.00000 0.05 0.75 Q9 1 0.2424 0.7515 0.5634 11.00000 0.05 0.72 Q10 1 0.2742 0.5196 0.7813 11.00000 0.05 0.69 Q11 1 0.4069 0.4825 0.7841 11.00000 0.05 0.69 Q12 1 0.2302 0.4793 0.6129 11.00000 0.05 0.65 Q13 1 0.3820 0.4840 0.7032 11.00000 0.05 0.65 Q14 1 0.1923 0.5519 0.7591 11.00000 0.05 0.64 Q15 1 0.3956 0.7494 0.6540 11.00000 0.05 0.60 Q16 1 0.1532 0.5182 0.7789 11.00000 0.05 0.60 Q17 1 0.2199 0.5449 0.8130 11.00000 0.05 0.56 Q18 1 0.3287 0.5158 0.7134 11.00000 0.05 0.49 Q19 1 -0.0765 0.4781 0.3622 11.00000 0.05 0.45 Q20 1 0.1848 0.5065 0.5781 11.00000 0.05 0.44 Q21 1 1.0189 0.5149 1.0195 11.00000 0.05 0.43 Q22 1 0.3039 0.7469 0.5229 11.00000 0.05 0.43 Q23 1 0.2054 0.4247 0.5317 11.00000 0.05 0.41 Q24 1 0.3068 0.6854 0.5936 11.00000 0.05 0.41 ; _shelx_res_checksum 97911 _shelx_fab_file ; -18 0 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-4.1027 0.3057 6 9 13 -1.9327 -0.0035 6 9 14 2.3310 -0.2013 6 10 6 -8.0153 0.2498 6 10 7 1.5287 0.0436 6 10 8 -1.7061 -0.2279 6 10 9 3.0524 0.1091 6 10 10 2.8824 0.1516 6 10 11 -3.7874 -0.0983 6 10 12 0.4792 0.1217 6 10 13 0.6703 -0.1954 6 11 6 -1.1098 -0.0879 6 11 7 0.6368 -0.0225 6 11 8 4.3940 0.0062 6 11 9 -1.9352 0.0320 6 11 10 10.0828 0.2083 6 11 11 0.2566 -0.0096 6 11 12 7.6335 0.0877 6 11 13 2.8690 0.2287 6 12 6 3.3733 -0.0555 6 12 7 -0.0194 0.1845 6 12 8 3.0566 0.0461 6 12 9 -2.2945 -0.2788 6 12 10 -3.3622 0.1047 6 12 11 0.2227 0.1098 6 12 12 1.7506 -0.3338 6 12 13 -4.7743 -0.2791 6 13 6 -4.4831 0.0512 6 13 7 -1.4837 -0.1862 6 13 8 -2.0337 -0.0597 6 13 9 4.5933 -0.1690 6 13 10 -5.7651 0.0649 6 13 11 1.1692 0.0755 6 13 12 -0.7013 -0.0388 6 13 13 -1.2872 -0.0753 6 14 6 -1.8364 -0.3088 6 14 7 -0.6083 -0.0445 6 14 8 -4.7522 0.3094 6 14 9 0.8435 0.2103 6 14 10 0.8908 -0.1548 6 14 11 2.5501 0.0338 6 14 12 -1.3440 0.0661 6 14 13 0.7666 0.4781 6 15 6 4.0314 0.0200 6 15 7 3.9833 0.0820 6 15 8 -1.1988 -0.0419 6 15 9 -2.7649 -0.0945 6 15 10 1.2645 -0.4073 6 15 11 0.0809 0.0479 6 15 12 -2.5530 0.0056 6 16 6 2.0151 0.0869 6 16 7 -0.0919 -0.1388 6 16 8 -0.3855 -0.1702 6 16 9 0.5129 0.1452 6 16 10 1.6704 0.0768 6 16 11 -2.1502 -0.0578 6 16 12 5.4908 0.2706 6 17 6 -2.0745 0.0706 6 17 7 -2.2180 0.0959 6 17 8 3.5690 -0.0031 6 17 9 0.6593 -0.0119 6 17 10 -0.9266 0.3004 6 17 11 0.1156 -0.1233 6 17 12 -0.5680 0.1140 6 18 6 -5.0851 0.0729 6 18 7 0.3831 0.0974 6 18 8 1.8557 -0.1133 6 18 9 -5.0583 -0.0936 6 18 10 0.5383 0.1509 6 18 11 1.5062 0.1221 6 18 12 -5.5103 -0.6844 6 19 6 2.3556 -0.0279 6 19 7 0.9844 -0.0777 6 19 8 -1.6429 0.1354 6 19 9 -1.0552 0.1760 6 19 10 1.8691 -0.2577 6 19 11 -1.9448 -0.0016 6 20 6 6.2806 0.0087 6 20 7 -2.7677 -0.0091 6 20 8 -0.5567 0.1236 6 20 9 0.8050 0.0140 6 20 10 -0.2016 -0.2914 6 20 11 -0.8271 -0.0265 6 21 6 1.1423 0.0540 6 21 7 -0.2718 0.2341 6 21 8 0.6297 -0.1849 6 21 9 1.3731 -0.1291 6 21 10 -2.0159 0.0203 6 21 11 -0.6932 0.1636 6 22 6 -2.5714 -0.0938 6 22 7 0.6588 -0.0468 6 22 8 0.9069 -0.0229 6 22 9 3.7301 -0.0386 6 22 10 0.5467 0.3310 6 23 6 -1.0007 0.0101 6 23 7 1.7512 -0.1508 6 23 8 0.2217 0.1507 6 23 9 -3.8402 0.0226 6 23 10 2.8362 0.2366 6 24 6 -1.2226 0.1192 6 24 7 -1.9662 -0.1224 6 24 8 1.3308 0.0696 6 24 9 -1.4539 0.1197 6 25 6 0.3308 0.0556 6 25 7 -4.7507 0.0554 6 25 8 0.9737 -0.0604 6 25 9 3.0345 0.0602 6 26 6 -0.9783 -0.0749 6 26 7 5.2755 0.0391 6 26 8 -1.2347 -0.2376 6 27 6 -1.6343 -0.1707 6 27 7 0.8147 -0.0641 6 28 6 1.6260 -0.1066 6 28 7 -3.3376 0.1614 6 29 6 -0.6086 0.1908 7 0 7 5.8960 -4.2043 7 0 9 4.3021 -0.0125 7 0 11 7.4111 -1.2400 7 0 13 1.3386 1.2084 7 1 7 8.1010 0.6159 7 1 8 -2.7162 -0.2259 7 1 9 22.3389 -0.0673 7 1 10 -0.9253 0.2844 7 1 11 9.9375 0.3814 7 1 12 -3.5023 -0.0314 7 1 13 -0.3951 0.4003 7 2 7 -1.9279 1.2868 7 2 8 -4.8923 -0.8250 7 2 9 -2.8423 -0.2893 7 2 10 0.1104 0.6925 7 2 11 -5.5171 0.6445 7 2 12 -4.9941 -0.9260 7 2 13 1.1529 -0.5386 7 3 7 -6.6170 -0.4043 7 3 8 2.0717 0.4046 7 3 9 -15.3976 0.3393 7 3 10 -0.6000 -0.2799 7 3 11 -2.6639 -0.0296 7 3 12 3.7503 0.0623 7 3 13 1.6147 0.1179 7 4 7 -0.1171 0.6897 7 4 8 6.9769 -0.0967 7 4 9 4.8032 0.1877 7 4 10 -3.6640 -0.6590 7 4 11 7.0004 0.0647 7 4 12 -1.1142 0.3912 7 4 13 0.5539 0.1533 7 5 7 2.1626 0.2761 7 5 8 0.7115 -0.1928 7 5 9 13.9994 0.4825 7 5 10 0.1263 0.4049 7 5 11 1.0184 0.2813 7 5 12 -1.0850 -0.1477 7 5 13 1.6658 -0.2200 7 6 7 -3.5996 0.2320 7 6 8 -2.9983 0.0137 7 6 9 -4.4533 0.0569 7 6 10 0.7457 -0.3148 7 6 11 -4.0767 -0.1936 7 6 12 3.8674 0.1951 7 6 13 -1.1136 -0.1326 7 7 7 -4.6836 -0.2247 7 7 8 0.6118 -0.2450 7 7 9 -11.4876 -0.2863 7 7 10 1.9257 -0.0560 7 7 11 3.4039 -0.0456 7 7 12 -0.8256 0.4465 7 7 13 -3.0142 -0.0338 7 8 7 3.6607 -0.0752 7 8 8 -0.7668 0.2625 7 8 9 2.4503 0.2366 7 8 10 0.5004 0.4209 7 8 11 -2.1887 -0.2248 7 8 12 -3.8702 -0.3278 7 8 13 -2.5356 0.2522 7 9 7 5.3327 -0.0789 7 9 8 -2.1688 -0.0880 7 9 9 1.1872 -0.2523 7 9 10 -2.6553 -0.0001 7 9 11 -8.1444 -0.0809 7 9 12 3.5242 -0.1959 7 9 13 1.0954 -0.2637 7 10 7 -1.5360 0.2488 7 10 8 2.9126 0.0399 7 10 9 -5.3044 -0.2249 7 10 10 1.3807 0.0854 7 10 11 -3.9765 0.1156 7 10 12 1.9734 -0.1139 7 10 13 -1.7577 -0.2734 7 11 7 -3.5260 -0.0731 7 11 8 1.5557 -0.0124 7 11 9 3.6479 0.0358 7 11 10 4.1825 -0.0247 7 11 11 10.0287 0.0767 7 11 12 1.5814 -0.1663 7 11 13 2.6719 0.7804 7 12 7 4.7906 -0.1420 7 12 8 1.1357 0.1073 7 12 9 3.0579 0.0169 7 12 10 -4.1827 -0.2451 7 12 11 7.4631 0.0705 7 12 12 -1.2597 -0.0407 7 13 7 3.8417 0.0872 7 13 8 -0.2363 -0.0667 7 13 9 -0.7781 -0.0126 7 13 10 -1.6263 -0.0373 7 13 11 -4.8112 0.1629 7 13 12 -6.2810 0.3211 7 14 7 -7.1003 -0.2209 7 14 8 -6.7216 -0.1060 7 14 9 -1.5519 0.2144 7 14 10 7.5029 0.1002 7 14 11 -4.1002 -0.0893 7 14 12 -0.1332 0.0596 7 15 7 -2.0423 0.1020 7 15 8 3.0503 0.0380 7 15 9 -0.3105 0.0696 7 15 10 1.5587 -0.0697 7 15 11 -2.1456 -0.1432 7 15 12 2.9429 -0.0879 7 16 7 2.6425 0.1369 7 16 8 6.1767 -0.1008 7 16 9 0.6683 -0.0951 7 16 10 -4.3522 0.2041 7 16 11 3.6985 -0.0441 7 17 7 1.6568 -0.0812 7 17 8 -3.2729 0.0795 7 17 9 -1.0979 -0.2241 7 17 10 0.7401 0.0106 7 17 11 0.3517 -0.1266 7 18 7 -2.1805 -0.0950 7 18 8 -5.1191 0.1750 7 18 9 -0.3098 -0.0922 7 18 10 1.2323 -0.1222 7 18 11 -3.3610 0.2386 7 19 7 -3.0804 -0.0067 7 19 8 4.2253 -0.0606 7 19 9 1.5186 0.1880 7 19 10 -2.8646 -0.0046 7 20 7 -0.0671 0.0448 7 20 8 2.7586 -0.0532 7 20 9 1.3091 0.1133 7 20 10 -1.5460 0.0693 7 21 7 2.5926 0.1125 7 21 8 -4.2828 0.1316 7 21 9 -1.3776 -0.1481 7 21 10 -1.7473 -0.0029 7 22 7 3.8729 -0.0429 7 22 8 -0.4491 0.0157 7 22 9 0.1497 -0.0402 7 23 7 1.6859 -0.1749 7 23 8 1.7647 -0.0293 7 23 9 0.4610 0.0337 7 24 7 -0.5848 -0.0336 7 24 8 0.5975 0.0197 7 25 7 -0.9567 0.1994 7 25 8 -5.4332 -0.0398 7 26 7 0.9588 0.3039 8 0 8 -4.3813 -3.2145 8 0 10 2.5212 0.2284 8 0 12 2.0473 -1.1336 8 1 8 17.1008 0.4167 8 1 9 0.6695 -0.2990 8 1 10 19.7896 -0.1726 8 1 11 0.9909 0.1049 8 1 12 2.3349 -0.0775 8 2 8 6.0691 0.9723 8 2 9 -4.4999 -0.6425 8 2 10 -4.2445 -0.3680 8 2 11 -3.2208 0.7254 8 2 12 -2.8866 0.5019 8 2 13 -5.2367 -0.4878 8 3 8 -13.2558 -0.2853 8 3 9 -1.1530 0.3151 8 3 10 -12.4784 0.1736 8 3 11 -0.1127 -0.1807 8 3 12 2.3229 -0.0101 8 3 13 -1.0997 -0.0335 8 4 8 -4.3947 0.4920 8 4 9 4.2689 -0.0135 8 4 10 5.0394 0.2471 8 4 11 -0.1820 -0.4076 8 4 12 4.5906 -0.1311 8 4 13 4.2180 0.1690 8 5 8 11.9843 0.0517 8 5 9 1.2755 -0.0781 8 5 10 8.0561 0.3761 8 5 11 -0.5663 0.3616 8 5 12 0.1331 0.2401 8 6 8 2.6262 0.1550 8 6 9 -4.2961 0.0519 8 6 10 -2.9556 0.0143 8 6 11 2.9489 -0.3800 8 6 12 -3.3223 0.0044 8 7 8 -10.5449 -0.0271 8 7 9 -0.3903 -0.3053 8 7 10 -1.8137 -0.1164 8 7 11 0.0464 -0.0461 8 7 12 -0.2220 0.1180 8 8 8 -3.4043 0.0304 8 8 9 1.8799 0.1324 8 8 10 3.2208 0.3021 8 8 11 -6.5239 0.2896 8 8 12 -1.4598 -0.2035 8 9 8 5.4000 0.0027 8 9 9 -5.4306 -0.0891 8 9 10 -1.8181 -0.2405 8 9 11 -1.1708 -0.0309 8 9 12 -1.5892 -0.3708 8 10 8 4.6769 0.1307 8 10 10 -5.4460 -0.3664 8 10 11 5.1096 0.0407 8 10 12 -0.1737 0.0781 8 11 8 -3.0637 -0.1051 8 11 9 5.6202 0.1474 8 11 10 1.8584 0.0791 8 11 11 4.6576 -0.1197 8 11 12 0.8807 0.4958 8 12 8 -7.7859 -0.1038 8 12 9 -2.0052 0.0132 8 12 10 4.7737 0.1369 8 12 11 -1.3245 -0.2635 8 13 8 3.8562 0.0535 8 13 9 2.1869 -0.2059 8 13 10 1.2206 0.0273 8 13 11 -8.8465 0.0851 8 14 8 4.9631 -0.1685 8 14 9 2.3816 -0.0483 8 14 10 -3.1096 0.1581 8 14 11 0.9230 0.1556 8 15 8 0.3001 0.1381 8 15 9 -1.8958 0.0642 8 15 10 -5.0743 -0.0554 8 15 11 5.9763 -0.0849 8 16 8 -0.9183 0.1927 8 16 9 0.2794 -0.0853 8 16 10 2.8488 0.0376 8 17 8 -3.3575 -0.0967 8 17 9 0.5822 -0.0476 8 17 10 3.0137 -0.0314 8 18 8 -0.7292 0.0101 8 18 9 -3.3338 0.1548 8 18 10 -1.8443 -0.1542 8 19 8 1.8361 -0.1546 8 19 9 -1.6644 0.0516 8 20 8 -1.1960 -0.1784 8 20 9 4.7246 -0.0166 8 21 8 -3.4161 0.3543 8 21 9 -0.6539 0.0148 8 22 8 2.3844 0.2117 8 23 8 1.3856 -0.3553 9 0 9 -2.8237 -2.3636 9 0 11 -1.3126 0.4953 9 1 9 4.7865 0.2372 9 1 10 1.1352 -0.2586 9 1 11 6.6190 0.0278 9 2 9 3.3525 0.7802 9 2 10 -1.8215 -0.5773 9 2 11 -0.6684 -0.3683 9 2 12 -0.9978 0.3612 9 3 9 0.8183 -0.0776 9 3 10 -0.9046 0.1416 9 3 11 -3.9763 -0.1889 9 3 12 -7.2200 -0.0998 9 4 9 -4.0944 0.2765 9 4 10 1.4275 0.0598 9 4 11 1.8461 0.0638 9 4 12 0.0058 -0.2564 9 5 9 -5.0970 -0.1278 9 5 10 1.6142 -0.0369 9 5 11 4.8211 0.4743 9 5 12 4.6640 0.5400 9 6 9 2.8240 0.2699 9 6 10 3.0524 0.0482 9 6 11 -1.1365 -0.0432 9 7 9 4.9993 -0.0122 9 7 10 -2.2003 -0.0571 9 7 11 -5.3138 -0.1731 9 8 9 0.7913 -0.1541 9 8 10 -4.1606 0.0963 9 8 11 -0.1254 0.1013 9 9 9 -5.1214 -0.0181 9 9 10 -1.2677 -0.1814 9 9 11 1.0790 -0.0305 9 10 9 -0.8905 0.1413 9 10 10 -0.1972 -0.1095 9 10 11 0.9670 0.0813 9 11 9 7.1475 -0.0100 9 11 10 3.1948 0.0995 9 11 11 1.5236 -0.0794 9 12 9 -2.1921 -0.0427 9 12 10 1.1203 0.3113 9 13 9 -3.4329 -0.0468 9 13 10 -4.3413 -0.1726 9 14 9 0.3269 -0.0326 9 14 10 0.6859 -0.2839 9 15 9 -1.3944 0.0706 9 15 10 4.2615 0.0306 9 16 9 2.3098 0.1076 9 17 9 1.2358 0.1742 9 18 9 -0.0446 0.0558 10 0 10 -1.0823 -1.7518 10 1 10 4.1800 -0.1156 10 2 10 0.1709 0.5122 10 2 11 -0.8925 -0.3171 10 3 10 1.3983 0.1008 10 3 11 -5.5069 0.0948 10 4 10 3.2073 0.3285 10 4 11 -0.0547 -0.1864 10 5 10 -3.6733 -0.1999 10 6 10 -4.3221 0.0486 10 7 10 -0.9471 0.0075 10 8 10 3.1443 -0.0350 10 9 10 1.2513 0.2047 10 10 10 -3.6024 0.0271 10 11 10 3.3192 -0.4351 0 0 0 0.0 0.0 ; _shelx_fab_checksum 12188 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -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 C1 C 0.1596(3) 0.44437(15) 0.5112(3) 0.0210(8) Uani 1 1 d . . . . . C2 C 0.0778(3) 0.45509(16) 0.4237(3) 0.0263(9) Uani 1 1 d . . . . . C3 C 0.0362(3) 0.41876(17) 0.3544(3) 0.0304(10) Uani 1 1 d . . . . . H3 H -0.019398 0.426832 0.297100 0.036 Uiso 1 1 calc R U . . . C4 C 0.0727(3) 0.37198(16) 0.3663(3) 0.0273(9) Uani 1 1 d . . . . . C5 C 0.1576(3) 0.36304(15) 0.4501(3) 0.0283(10) Uani 1 1 d . . . . . H5 H 0.186597 0.331548 0.459240 0.034 Uiso 1 1 calc R U . . . C6 C 0.2022(3) 0.39759(15) 0.5212(3) 0.0259(9) Uani 1 1 d . . . . . C7 C 0.0270(4) 0.33132(17) 0.2952(4) 0.0337(10) Uani 1 1 d . . . . . C8 C -0.0538(5) 0.3507(2) 0.2019(4) 0.0569(17) Uani 1 1 d . . . . . H8A H -0.111187 0.364015 0.214809 0.085 Uiso 1 1 calc R U . . . H8B H -0.077837 0.324300 0.155531 0.085 Uiso 1 1 calc R U . . . H8C H -0.023781 0.376222 0.175989 0.085 Uiso 1 1 calc R U . . . C9 C -0.0234(4) 0.29399(17) 0.3370(4) 0.0366(11) Uani 1 1 d . . . . . H9A H 0.028406 0.278612 0.392707 0.055 Uiso 1 1 calc R U . . . H9B H -0.057131 0.269318 0.288754 0.055 Uiso 1 1 calc R U . . . H9C H -0.073998 0.310042 0.356364 0.055 Uiso 1 1 calc R U . . . C10 C 0.1103(5) 0.3061(2) 0.2710(4) 0.0502(15) Uani 1 1 d . . . . . H10A H 0.148648 0.330390 0.251158 0.075 Uiso 1 1 calc R U . . . H10B H 0.078981 0.283017 0.218937 0.075 Uiso 1 1 calc R U . . . H10C H 0.156649 0.288928 0.327436 0.075 Uiso 1 1 calc R U . . . C11 C 0.2960(3) 0.38361(16) 0.5989(3) 0.0255(9) Uani 1 1 d . . . . . H11 H 0.318348 0.351270 0.598024 0.031 Uiso 1 1 calc R U . . . C12 C 0.4435(3) 0.38808(15) 0.7336(3) 0.0235(9) Uani 1 1 d . . . . . C13 C 0.5356(3) 0.40143(17) 0.7275(4) 0.0314(10) Uani 1 1 d . . . . . H13 H 0.535932 0.424202 0.680622 0.038 Uiso 1 1 calc R U . . . C14 C 0.6268(3) 0.38163(18) 0.7894(4) 0.0350(11) Uani 1 1 d . . . . . H14 H 0.689268 0.391342 0.785693 0.042 Uiso 1 1 calc R U . . . C15 C 0.6266(3) 0.34786(18) 0.8565(4) 0.0323(10) Uani 1 1 d . . . . . H15 H 0.688640 0.334030 0.898930 0.039 Uiso 1 1 calc R U . . . C16 C 0.5338(3) 0.33437(15) 0.8608(3) 0.0270(9) Uani 1 1 d . . . . . H16 H 0.533492 0.310250 0.905376 0.032 Uiso 1 1 calc R U . . . C17 C 0.4426(3) 0.35478(15) 0.8028(3) 0.0229(8) Uani 1 1 d . . . . . C18 C 0.3456(3) 0.34172(16) 0.8159(3) 0.0270(9) Uani 1 1 d . . . . . H18A H 0.350001 0.307664 0.837515 0.032 Uiso 1 1 calc R U . . . H18B H 0.287691 0.344181 0.753580 0.032 Uiso 1 1 calc R U . . . C19 C 0.3245(3) 0.37450(17) 0.8889(3) 0.0295(10) Uani 1 1 d . . . . . H19A H 0.325754 0.408787 0.870427 0.035 Uiso 1 1 calc R U . . . H19B H 0.255486 0.367442 0.887279 0.035 Uiso 1 1 calc R U . . . C20 C 0.4014(3) 0.36726(15) 0.9893(3) 0.0276(9) Uani 1 1 d . . . . . C21 C 0.3863(3) 0.32934(16) 1.0442(3) 0.0296(10) Uani 1 1 d . . . . . H21 H 0.327275 0.309653 1.017595 0.036 Uiso 1 1 calc R U . . . C22 C 0.4549(4) 0.31984(17) 1.1359(4) 0.0345(11) Uani 1 1 d . . . . . H22 H 0.442958 0.293807 1.171245 0.041 Uiso 1 1 calc R U . . . C23 C 0.5404(4) 0.34814(17) 1.1757(3) 0.0346(11) Uani 1 1 d . . . . . H23 H 0.587100 0.341452 1.238787 0.041 Uiso 1 1 calc R U . . . C24 C 0.5597(4) 0.38633(16) 1.1254(3) 0.0298(10) Uani 1 1 d . . . . . H24 H 0.618584 0.405953 1.153474 0.036 Uiso 1 1 calc R U . . . C25 C 0.4905(3) 0.39512(15) 1.0328(3) 0.0253(9) Uani 1 1 d . . . . . C26 C 0.5947(3) 0.45565(16) 0.9955(3) 0.0267(9) Uani 1 1 d . . . . . H26 H 0.650549 0.447688 1.052660 0.032 Uiso 1 1 calc R U . . . C27 C 0.5315(3) 0.50349(15) 0.8456(3) 0.0232(9) Uani 1 1 d . . . . . C28 C 0.6100(3) 0.49124(15) 0.9354(3) 0.0237(9) Uani 1 1 d . . . . . C29 C 0.7070(3) 0.51220(16) 0.9629(3) 0.0281(9) Uani 1 1 d . . . . . H29 H 0.757861 0.503416 1.022745 0.034 Uiso 1 1 calc R U . . . C30 C 0.7318(3) 0.54531(17) 0.9060(3) 0.0267(9) Uani 1 1 d . . . . . C31 C 0.6559(3) 0.55553(16) 0.8182(3) 0.0262(9) Uani 1 1 d . . . . . H31 H 0.670860 0.578118 0.778150 0.031 Uiso 1 1 calc R U . . . C32 C 0.5589(3) 0.53487(15) 0.7847(3) 0.0237(9) Uani 1 1 d . . . . . C33 C 0.8389(3) 0.56677(17) 0.9356(4) 0.0312(10) Uani 1 1 d . . . . . C34 C 0.9080(4) 0.5514(2) 1.0362(4) 0.0480(14) Uani 1 1 d . . . . . H34A H 0.876111 0.560176 1.080991 0.072 Uiso 1 1 calc R U . . . H34B H 0.973794 0.567898 1.054431 0.072 Uiso 1 1 calc R U . . . H34C H 0.918436 0.516312 1.037744 0.072 Uiso 1 1 calc R U . . . C35 C 0.8338(4) 0.62204(18) 0.9325(4) 0.0360(11) Uani 1 1 d . . . . . H35A H 0.813451 0.633862 0.983518 0.054 Uiso 1 1 calc R U . . . H35B H 0.783868 0.632539 0.870521 0.054 Uiso 1 1 calc R U . . . H35C H 0.900974 0.635151 0.941438 0.054 Uiso 1 1 calc R U . . . C36 C 0.8853(4) 0.5488(2) 0.8647(4) 0.0432(13) Uani 1 1 d . . . . . H36A H 0.956786 0.558814 0.886930 0.065 Uiso 1 1 calc R U . . . H36B H 0.847490 0.562823 0.801565 0.065 Uiso 1 1 calc R U . . . H36C H 0.881001 0.513439 0.860528 0.065 Uiso 1 1 calc R U . . . C37 C 0.4937(3) 0.54378(15) 0.6858(3) 0.0244(9) Uani 1 1 d . . . . . H37 H 0.517711 0.566106 0.651553 0.029 Uiso 1 1 calc R U . . . C38 C 0.3599(3) 0.53236(16) 0.5386(3) 0.0240(9) Uani 1 1 d . . . . . C39 C 0.3574(3) 0.49297(17) 0.4808(3) 0.0288(10) Uani 1 1 d . . . . . H39 H 0.389623 0.463470 0.508418 0.035 Uiso 1 1 calc R U . . . C40 C 0.3076(4) 0.49683(18) 0.3821(3) 0.0325(10) Uani 1 1 d . . . . . H40 H 0.303321 0.469606 0.342483 0.039 Uiso 1 1 calc R U . . . C41 C 0.2644(3) 0.54027(18) 0.3422(3) 0.0307(10) Uani 1 1 d . . . . . H41 H 0.232258 0.543382 0.274764 0.037 Uiso 1 1 calc R U . . . C42 C 0.2679(3) 0.57908(17) 0.4001(3) 0.0297(10) Uani 1 1 d . . . . . H42 H 0.238292 0.608888 0.371614 0.036 Uiso 1 1 calc R U . . . C43 C 0.3136(3) 0.57612(16) 0.4996(3) 0.0245(9) Uani 1 1 d . . . . . C44 C 0.3051(3) 0.61733(15) 0.5604(3) 0.0265(9) Uani 1 1 d . . . . . H44A H 0.308932 0.648243 0.528908 0.032 Uiso 1 1 calc R U . . . H44B H 0.363490 0.616199 0.622632 0.032 Uiso 1 1 calc R U . . . C45 C 0.2053(3) 0.61603(16) 0.5778(3) 0.0267(9) Uani 1 1 d . . . . . H45A H 0.198205 0.583857 0.603388 0.032 Uiso 1 1 calc R U . . . H45B H 0.208711 0.640580 0.626531 0.032 Uiso 1 1 calc R U . . . C46 C 0.1127(3) 0.62572(16) 0.4881(4) 0.0293(10) Uani 1 1 d . . . . . C47 C 0.0897(3) 0.67378(16) 0.4582(4) 0.0313(10) Uani 1 1 d . . . . . H47 H 0.130354 0.699200 0.496058 0.038 Uiso 1 1 calc R U . . . C48 C 0.0083(4) 0.68487(19) 0.3739(4) 0.0424(13) Uani 1 1 d . . . . . H48 H -0.004789 0.717643 0.354035 0.051 Uiso 1 1 calc R U . . . C49 C -0.0533(4) 0.64903(19) 0.3193(5) 0.0437(13) Uani 1 1 d . . . . . H49 H -0.109159 0.657049 0.262197 0.052 Uiso 1 1 calc R U . . . C50 C -0.0341(3) 0.60107(18) 0.3473(4) 0.0345(11) Uani 1 1 d . . . . . H50 H -0.077134 0.576083 0.310354 0.041 Uiso 1 1 calc R U . . . C51 C 0.0493(3) 0.58999(16) 0.4305(3) 0.0271(9) Uani 1 1 d . . . . . C52 C 0.0419(3) 0.50280(16) 0.3992(3) 0.0276(9) Uani 1 1 d . . . . . H52 H -0.009944 0.507974 0.337922 0.033 Uiso 1 1 calc R U . . . N1 N 0.3520(3) 0.41044(13) 0.6688(3) 0.0252(8) Uani 1 1 d . . . . . N2 N 0.0752(3) 0.54044(13) 0.4549(3) 0.0245(8) Uani 1 1 d . . . . . H2 H 0.117953 0.534618 0.513684 0.029 Uiso 1 1 calc R U . . . N3 N 0.5088(3) 0.43301(12) 0.9777(3) 0.0236(7) Uani 1 1 d . . . . . H3A H 0.456830 0.442074 0.926289 0.028 Uiso 1 1 calc R U . . . N4 N 0.4054(3) 0.52401(13) 0.6399(3) 0.0234(7) Uani 1 1 d . . . . . O1 O 0.1930(2) 0.47757(10) 0.5759(2) 0.0253(6) Uani 1 1 d . . . . . O2 O 0.4412(2) 0.48579(11) 0.8239(2) 0.0258(6) Uani 1 1 d . . . . . Fe1 Fe 0.31946(4) 0.48208(2) 0.69816(4) 0.02257(14) Uani 1 1 d . . . . . Br1 Br 0.20881(3) 0.51691(2) 0.77846(3) 0.03384(13) Uani 1 1 d . . . . . Br2 Br 0.33023(4) 0.74877(2) 0.63652(4) 0.03723(14) Uani 1 1 d . . . . . 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 C1 0.0166(18) 0.028(2) 0.020(2) 0.0012(17) 0.0081(16) -0.0012(16) C2 0.020(2) 0.030(2) 0.032(2) 0.0031(19) 0.0140(19) -0.0008(17) C3 0.025(2) 0.033(2) 0.030(3) 0.0035(19) 0.008(2) -0.0057(18) C4 0.027(2) 0.029(2) 0.024(2) -0.0002(18) 0.0087(19) -0.0044(18) C5 0.025(2) 0.020(2) 0.038(3) 0.0023(18) 0.010(2) -0.0022(16) C6 0.027(2) 0.026(2) 0.024(2) 0.0041(18) 0.0096(19) 0.0011(17) C7 0.030(2) 0.034(2) 0.032(3) -0.003(2) 0.007(2) -0.007(2) C8 0.072(4) 0.035(3) 0.039(3) 0.000(2) -0.007(3) -0.017(3) C9 0.039(3) 0.029(2) 0.042(3) -0.004(2) 0.017(2) -0.006(2) C10 0.056(3) 0.057(4) 0.048(3) -0.025(3) 0.031(3) -0.018(3) C11 0.027(2) 0.027(2) 0.024(2) 0.0057(18) 0.0124(19) 0.0042(17) C12 0.020(2) 0.025(2) 0.026(2) 0.0002(17) 0.0095(18) 0.0024(16) C13 0.022(2) 0.038(3) 0.035(3) 0.007(2) 0.012(2) 0.0050(19) C14 0.019(2) 0.047(3) 0.040(3) 0.012(2) 0.012(2) 0.0052(19) C15 0.022(2) 0.038(3) 0.034(3) 0.002(2) 0.008(2) 0.0067(19) C16 0.031(2) 0.023(2) 0.030(2) 0.0011(18) 0.015(2) 0.0019(17) C17 0.024(2) 0.023(2) 0.025(2) -0.0020(17) 0.0122(18) 0.0002(16) C18 0.021(2) 0.029(2) 0.029(2) 0.0038(18) 0.0072(18) -0.0039(17) C19 0.020(2) 0.033(2) 0.038(3) 0.006(2) 0.015(2) 0.0019(17) C20 0.032(2) 0.023(2) 0.034(3) 0.0027(18) 0.019(2) 0.0043(17) C21 0.030(2) 0.031(2) 0.035(3) 0.003(2) 0.020(2) 0.0009(18) C22 0.053(3) 0.027(2) 0.034(3) 0.008(2) 0.028(2) 0.008(2) C23 0.052(3) 0.030(2) 0.025(2) 0.0026(19) 0.018(2) 0.007(2) C24 0.038(3) 0.029(2) 0.023(2) 0.0017(18) 0.013(2) 0.0044(19) C25 0.032(2) 0.023(2) 0.024(2) 0.0011(17) 0.0132(19) 0.0027(17) C26 0.028(2) 0.027(2) 0.027(2) -0.0002(18) 0.0120(19) 0.0033(17) C27 0.020(2) 0.025(2) 0.027(2) -0.0018(17) 0.0117(18) 0.0021(16) C28 0.021(2) 0.025(2) 0.027(2) -0.0024(17) 0.0106(18) 0.0025(16) C29 0.025(2) 0.029(2) 0.030(2) 0.0029(19) 0.0093(19) 0.0047(17) C30 0.023(2) 0.037(2) 0.021(2) -0.0007(18) 0.0105(18) 0.0014(18) C31 0.026(2) 0.028(2) 0.029(2) -0.0005(18) 0.017(2) 0.0019(17) C32 0.021(2) 0.028(2) 0.023(2) -0.0018(17) 0.0101(18) 0.0037(16) C33 0.022(2) 0.038(3) 0.033(3) 0.000(2) 0.009(2) -0.0012(18) C34 0.025(2) 0.060(4) 0.046(3) 0.007(3) -0.001(2) -0.012(2) C35 0.028(2) 0.043(3) 0.039(3) -0.002(2) 0.015(2) -0.007(2) C36 0.022(2) 0.054(3) 0.058(4) -0.013(3) 0.021(2) -0.004(2) C37 0.0192(19) 0.027(2) 0.031(2) 0.0034(18) 0.0145(18) 0.0048(16) C38 0.0183(19) 0.034(2) 0.023(2) 0.0042(18) 0.0111(17) 0.0003(17) C39 0.024(2) 0.031(2) 0.035(3) -0.0023(19) 0.015(2) 0.0029(17) C40 0.032(2) 0.041(3) 0.030(3) -0.008(2) 0.018(2) -0.004(2) C41 0.024(2) 0.048(3) 0.020(2) 0.004(2) 0.0088(19) -0.001(2) C42 0.028(2) 0.035(2) 0.029(2) 0.010(2) 0.015(2) 0.0002(19) C43 0.0165(19) 0.032(2) 0.028(2) 0.0032(18) 0.0111(18) -0.0006(16) C44 0.027(2) 0.023(2) 0.031(2) 0.0003(18) 0.0123(19) 0.0009(17) C45 0.030(2) 0.024(2) 0.031(2) 0.0003(18) 0.018(2) 0.0006(17) C46 0.023(2) 0.031(2) 0.041(3) 0.000(2) 0.020(2) 0.0019(18) C47 0.028(2) 0.024(2) 0.044(3) 0.002(2) 0.016(2) -0.0003(18) C48 0.027(2) 0.033(3) 0.068(4) 0.015(3) 0.019(3) 0.004(2) C49 0.023(2) 0.037(3) 0.066(4) 0.018(3) 0.011(2) 0.003(2) C50 0.021(2) 0.033(2) 0.046(3) 0.007(2) 0.008(2) -0.0023(18) C51 0.021(2) 0.027(2) 0.040(3) 0.0083(19) 0.018(2) 0.0035(16) C52 0.0174(19) 0.033(2) 0.031(3) 0.0032(19) 0.0081(18) -0.0035(17) N1 0.0207(17) 0.0283(19) 0.030(2) 0.0024(16) 0.0138(16) 0.0016(14) N2 0.0188(17) 0.0287(19) 0.028(2) 0.0036(15) 0.0107(15) -0.0010(14) N3 0.0255(18) 0.0244(18) 0.0219(19) 0.0027(14) 0.0101(15) 0.0016(14) N4 0.0221(17) 0.0263(18) 0.0244(19) -0.0014(15) 0.0119(15) 0.0000(14) O1 0.0184(14) 0.0268(15) 0.0290(17) 0.0006(13) 0.0070(13) 0.0011(12) O2 0.0200(14) 0.0344(16) 0.0227(16) 0.0032(13) 0.0076(12) -0.0018(12) Fe1 0.0186(3) 0.0246(3) 0.0245(3) 0.0007(2) 0.0083(2) -0.0005(2) Br1 0.0213(2) 0.0546(3) 0.0260(2) -0.0038(2) 0.00937(18) 0.0040(2) Br2 0.0393(3) 0.0294(2) 0.0461(3) -0.0014(2) 0.0198(2) 0.00320(19) 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 C2 117.1(4) . . ? O1 C1 C2 119.5(4) . . ? O1 C1 C6 123.4(4) . . ? C3 C2 C1 120.5(4) . . ? C3 C2 C52 117.6(4) . . ? C52 C2 C1 121.7(4) . . ? C2 C3 H3 118.6 . . ? C4 C3 C2 122.7(4) . . ? C4 C3 H3 118.6 . . ? C3 C4 C5 115.8(4) . . ? C3 C4 C7 124.2(4) . . ? C5 C4 C7 120.0(4) . . ? C4 C5 H5 118.0 . . ? C6 C5 C4 124.0(4) . . ? C6 C5 H5 118.0 . . ? C1 C6 C11 123.6(4) . . ? C5 C6 C1 119.6(4) . . ? C5 C6 C11 116.7(4) . . ? C4 C7 C8 111.2(4) . . ? C4 C7 C9 110.3(4) . . ? C4 C7 C10 110.2(4) . . ? C9 C7 C8 108.3(4) . . ? C9 C7 C10 108.7(4) . . ? C10 C7 C8 108.2(5) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C6 C11 H11 116.6 . . ? N1 C11 C6 126.9(4) . . ? N1 C11 H11 116.6 . . ? C13 C12 C17 120.1(4) . . ? C13 C12 N1 117.8(4) . . ? C17 C12 N1 122.0(4) . . ? C12 C13 H13 119.8 . . ? C14 C13 C12 120.4(4) . . ? C14 C13 H13 119.8 . . ? C13 C14 H14 120.0 . . ? C15 C14 C13 120.1(4) . . ? C15 C14 H14 120.0 . . ? C14 C15 H15 120.6 . . ? C14 C15 C16 118.8(4) . . ? C16 C15 H15 120.6 . . ? C15 C16 H16 118.8 . . ? C17 C16 C15 122.4(4) . . ? C17 C16 H16 118.8 . . ? C12 C17 C18 121.8(4) . . ? C16 C17 C12 118.1(4) . . ? C16 C17 C18 120.1(4) . . ? C17 C18 H18A 109.0 . . ? C17 C18 H18B 109.0 . . ? C17 C18 C19 113.0(4) . . ? H18A C18 H18B 107.8 . . ? C19 C18 H18A 109.0 . . ? C19 C18 H18B 109.0 . . ? C18 C19 H19A 109.1 . . ? C18 C19 H19B 109.1 . . ? H19A C19 H19B 107.9 . . ? C20 C19 C18 112.3(4) . . ? C20 C19 H19A 109.1 . . ? C20 C19 H19B 109.1 . . ? C21 C20 C19 118.7(4) . . ? C21 C20 C25 116.3(4) . . ? C25 C20 C19 125.0(4) . . ? C20 C21 H21 119.1 . . ? C22 C21 C20 121.9(4) . . ? C22 C21 H21 119.1 . . ? C21 C22 H22 120.1 . . ? C23 C22 C21 119.9(4) . . ? C23 C22 H22 120.1 . . ? C22 C23 H23 119.4 . . ? C22 C23 C24 121.2(5) . . ? C24 C23 H23 119.4 . . ? C23 C24 H24 120.9 . . ? C23 C24 C25 118.3(5) . . ? C25 C24 H24 120.9 . . ? C20 C25 N3 117.3(4) . . ? C24 C25 C20 122.5(4) . . ? C24 C25 N3 120.2(4) . . ? C28 C26 H26 117.9 . . ? N3 C26 H26 117.9 . . ? N3 C26 C28 124.2(4) . . ? C32 C27 C28 117.0(4) . . ? O2 C27 C28 119.3(4) . . ? O2 C27 C32 123.7(4) . . ? C26 C28 C27 121.4(4) . . ? C29 C28 C26 118.2(4) . . ? C29 C28 C27 120.3(4) . . ? C28 C29 H29 118.7 . . ? C30 C29 C28 122.7(4) . . ? C30 C29 H29 118.7 . . ? C29 C30 C33 122.1(4) . . ? C31 C30 C29 116.2(4) . . ? C31 C30 C33 121.6(4) . . ? C30 C31 H31 117.8 . . ? C30 C31 C32 124.4(4) . . ? C32 C31 H31 117.8 . . ? C27 C32 C37 123.3(4) . . ? C31 C32 C27 119.2(4) . . ? C31 C32 C37 117.3(4) . . ? C30 C33 C36 108.3(4) . . ? C34 C33 C30 111.9(4) . . ? C34 C33 C35 108.3(4) . . ? C34 C33 C36 108.9(4) . . ? C35 C33 C30 110.4(4) . . ? C35 C33 C36 109.1(4) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34B 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35B 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36B 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C32 C37 H37 117.0 . . ? N4 C37 C32 126.0(4) . . ? N4 C37 H37 117.0 . . ? C39 C38 C43 121.1(4) . . ? C39 C38 N4 116.2(4) . . ? C43 C38 N4 122.5(4) . . ? C38 C39 H39 120.1 . . ? C38 C39 C40 119.8(4) . . ? C40 C39 H39 120.1 . . ? C39 C40 H40 120.1 . . ? C41 C40 C39 119.8(4) . . ? C41 C40 H40 120.1 . . ? C40 C41 H41 120.1 . . ? C42 C41 C40 119.8(4) . . ? C42 C41 H41 120.1 . . ? C41 C42 H42 118.9 . . ? C41 C42 C43 122.2(4) . . ? C43 C42 H42 118.9 . . ? C38 C43 C42 117.2(4) . . ? C38 C43 C44 122.3(4) . . ? C42 C43 C44 120.4(4) . . ? C43 C44 H44A 109.1 . . ? C43 C44 H44B 109.1 . . ? C43 C44 C45 112.6(4) . . ? H44A C44 H44B 107.8 . . ? C45 C44 H44A 109.1 . . ? C45 C44 H44B 109.1 . . ? C44 C45 H45A 109.1 . . ? C44 C45 H45B 109.1 . . ? H45A C45 H45B 107.8 . . ? C46 C45 C44 112.6(4) . . ? C46 C45 H45A 109.1 . . ? C46 C45 H45B 109.1 . . ? C47 C46 C45 118.3(4) . . ? C51 C46 C45 124.7(4) . . ? C51 C46 C47 116.9(4) . . ? C46 C47 H47 119.5 . . ? C48 C47 C46 121.0(5) . . ? C48 C47 H47 119.5 . . ? C47 C48 H48 119.6 . . ? C49 C48 C47 120.7(5) . . ? C49 C48 H48 119.6 . . ? C48 C49 H49 120.0 . . ? C48 C49 C50 120.0(5) . . ? C50 C49 H49 120.0 . . ? C49 C50 H50 120.4 . . ? C49 C50 C51 119.1(5) . . ? C51 C50 H50 120.4 . . ? C46 C51 N2 118.3(4) . . ? C50 C51 C46 122.2(4) . . ? C50 C51 N2 119.4(4) . . ? C2 C52 H52 117.7 . . ? N2 C52 C2 124.6(4) . . ? N2 C52 H52 117.7 . . ? C11 N1 C12 115.4(4) . . ? C11 N1 Fe1 126.4(3) . . ? C12 N1 Fe1 118.1(3) . . ? C51 N2 H2 116.6 . . ? C52 N2 C51 126.9(4) . . ? C52 N2 H2 116.6 . . ? C25 N3 H3A 116.7 . . ? C26 N3 C25 126.7(4) . . ? C26 N3 H3A 116.7 . . ? C37 N4 C38 116.9(4) . . ? C37 N4 Fe1 127.0(3) . . ? C38 N4 Fe1 116.1(3) . . ? C1 O1 Fe1 132.4(3) . . ? C27 O2 Fe1 131.7(3) . . ? N1 Fe1 Br1 133.28(10) . . ? N4 Fe1 N1 102.54(13) . . ? N4 Fe1 Br1 124.18(10) . . ? O1 Fe1 N1 86.52(13) . . ? O1 Fe1 N4 95.96(13) . . ? O1 Fe1 Br1 88.07(9) . . ? O2 Fe1 N1 93.92(13) . . ? O2 Fe1 N4 86.74(13) . . ? O2 Fe1 O1 177.11(12) . . ? O2 Fe1 Br1 89.56(9) . . ? 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 C1 C2 1.421(6) . ? C1 C6 1.410(6) . ? C1 O1 1.293(5) . ? C2 C3 1.409(6) . ? C2 C52 1.411(6) . ? C3 H3 0.9500 . ? C3 C4 1.379(6) . ? C4 C5 1.399(6) . ? C4 C7 1.520(6) . ? C5 H5 0.9500 . ? C5 C6 1.397(6) . ? C6 C11 1.452(6) . ? C7 C8 1.537(7) . ? C7 C9 1.525(7) . ? C7 C10 1.533(7) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11 0.9500 . ? C11 N1 1.289(6) . ? C12 C13 1.396(6) . ? C12 C17 1.399(6) . ? C12 N1 1.435(5) . ? C13 H13 0.9500 . ? C13 C14 1.388(6) . ? C14 H14 0.9500 . ? C14 C15 1.380(7) . ? C15 H15 0.9500 . ? C15 C16 1.396(6) . ? C16 H16 0.9500 . ? C16 C17 1.378(6) . ? C17 C18 1.509(6) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C18 C19 1.546(6) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C19 C20 1.508(7) . ? C20 C21 1.404(6) . ? C20 C25 1.411(6) . ? C21 H21 0.9500 . ? C21 C22 1.384(7) . ? C22 H22 0.9500 . ? C22 C23 1.375(7) . ? C23 H23 0.9500 . ? C23 C24 1.389(6) . ? C24 H24 0.9500 . ? C24 C25 1.393(6) . ? C25 N3 1.424(5) . ? C26 H26 0.9500 . ? C26 C28 1.413(6) . ? C26 N3 1.304(6) . ? C27 C28 1.431(6) . ? C27 C32 1.426(6) . ? C27 O2 1.293(5) . ? C28 C29 1.404(6) . ? C29 H29 0.9500 . ? C29 C30 1.391(6) . ? C30 C31 1.384(6) . ? C30 C33 1.532(6) . ? C31 H31 0.9500 . ? C31 C32 1.396(6) . ? C32 C37 1.449(6) . ? C33 C34 1.524(7) . ? C33 C35 1.528(7) . ? C33 C36 1.541(7) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37 0.9500 . ? C37 N4 1.299(5) . ? C38 C39 1.390(6) . ? C38 C43 1.395(6) . ? C38 N4 1.438(6) . ? C39 H39 0.9500 . ? C39 C40 1.392(7) . ? C40 H40 0.9500 . ? C40 C41 1.378(7) . ? C41 H41 0.9500 . ? C41 C42 1.375(7) . ? C42 H42 0.9500 . ? C42 C43 1.398(6) . ? C43 C44 1.498(6) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C44 C45 1.539(6) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C45 C46 1.512(7) . ? C46 C47 1.401(6) . ? C46 C51 1.395(7) . ? C47 H47 0.9500 . ? C47 C48 1.390(7) . ? C48 H48 0.9500 . ? C48 C49 1.370(8) . ? C49 H49 0.9500 . ? C49 C50 1.386(7) . ? C50 H50 0.9500 . ? C50 C51 1.394(7) . ? C51 N2 1.429(5) . ? C52 H52 0.9500 . ? C52 N2 1.309(6) . ? N1 Fe1 2.118(4) . ? N2 H2 0.8800 . ? N3 H3A 0.8800 . ? N4 Fe1 2.107(3) . ? O1 Fe1 2.033(3) . ? O2 Fe1 2.028(3) . ? Fe1 Br1 2.5184(7) . ? 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 C2 C3 C4 -1.2(7) . . . . ? C1 C2 C52 N2 -4.1(7) . . . . ? C1 C6 C11 N1 1.0(7) . . . . ? C2 C1 C6 C5 -5.6(6) . . . . ? C2 C1 C6 C11 169.6(4) . . . . ? C2 C1 O1 Fe1 -168.1(3) . . . . ? C2 C3 C4 C5 -2.9(6) . . . . ? C2 C3 C4 C7 177.2(4) . . . . ? C2 C52 N2 C51 173.2(4) . . . . ? C3 C2 C52 N2 -178.1(4) . . . . ? C3 C4 C5 C6 2.7(7) . . . . ? C3 C4 C7 C8 8.9(7) . . . . ? C3 C4 C7 C9 -111.1(5) . . . . ? C3 C4 C7 C10 128.8(5) . . . . ? C4 C5 C6 C1 1.6(7) . . . . ? C4 C5 C6 C11 -173.9(4) . . . . ? C5 C4 C7 C8 -170.9(5) . . . . ? C5 C4 C7 C9 69.0(5) . . . . ? C5 C4 C7 C10 -51.0(6) . . . . ? C5 C6 C11 N1 176.3(4) . . . . ? C6 C1 C2 C3 5.5(6) . . . . ? C6 C1 C2 C52 -168.4(4) . . . . ? C6 C1 O1 Fe1 10.0(6) . . . . ? C6 C11 N1 C12 -177.2(4) . . . . ? C6 C11 N1 Fe1 4.8(6) . . . . ? C7 C4 C5 C6 -177.4(4) . . . . ? C12 C13 C14 C15 1.2(8) . . . . ? C12 C17 C18 C19 -90.4(5) . . . . ? C13 C12 C17 C16 -2.8(6) . . . . ? C13 C12 C17 C18 176.1(4) . . . . ? C13 C12 N1 C11 104.3(5) . . . . ? C13 C12 N1 Fe1 -77.6(4) . . . . ? C13 C14 C15 C16 -0.3(8) . . . . ? C14 C15 C16 C17 -2.3(7) . . . . ? C15 C16 C17 C12 3.8(7) . . . . ? C15 C16 C17 C18 -175.1(4) . . . . ? C16 C17 C18 C19 88.5(5) . . . . ? C17 C12 C13 C14 0.4(7) . . . . ? C17 C12 N1 C11 -77.3(5) . . . . ? C17 C12 N1 Fe1 100.9(4) . . . . ? C17 C18 C19 C20 -67.2(5) . . . . ? C18 C19 C20 C21 -84.3(5) . . . . ? C18 C19 C20 C25 93.9(5) . . . . ? C19 C20 C21 C22 178.4(4) . . . . ? C19 C20 C25 C24 -179.0(4) . . . . ? C19 C20 C25 N3 0.1(6) . . . . ? C20 C21 C22 C23 0.4(7) . . . . ? C20 C25 N3 C26 -164.1(4) . . . . ? C21 C20 C25 C24 -0.7(6) . . . . ? C21 C20 C25 N3 178.4(4) . . . . ? C21 C22 C23 C24 -0.1(7) . . . . ? C22 C23 C24 C25 -0.5(7) . . . . ? C23 C24 C25 C20 1.0(7) . . . . ? C23 C24 C25 N3 -178.2(4) . . . . ? C24 C25 N3 C26 15.1(6) . . . . ? C25 C20 C21 C22 0.0(6) . . . . ? C26 C28 C29 C30 175.9(4) . . . . ? C27 C28 C29 C30 0.2(6) . . . . ? C27 C32 C37 N4 -2.0(7) . . . . ? C28 C26 N3 C25 176.4(4) . . . . ? C28 C27 C32 C31 -6.1(6) . . . . ? C28 C27 C32 C37 168.9(4) . . . . ? C28 C27 O2 Fe1 -165.5(3) . . . . ? C28 C29 C30 C31 -2.1(6) . . . . ? C28 C29 C30 C33 -178.2(4) . . . . ? C29 C30 C31 C32 -0.2(6) . . . . ? C29 C30 C33 C34 -5.8(6) . . . . ? C29 C30 C33 C35 -126.4(5) . . . . ? C29 C30 C33 C36 114.3(5) . . . . ? C30 C31 C32 C27 4.4(6) . . . . ? C30 C31 C32 C37 -170.9(4) . . . . ? C31 C30 C33 C34 178.4(5) . . . . ? C31 C30 C33 C35 57.8(6) . . . . ? C31 C30 C33 C36 -61.5(6) . . . . ? C31 C32 C37 N4 173.1(4) . . . . ? C32 C27 C28 C26 -171.7(4) . . . . ? C32 C27 C28 C29 4.0(6) . . . . ? C32 C27 O2 Fe1 14.2(6) . . . . ? C32 C37 N4 C38 -171.1(4) . . . . ? C32 C37 N4 Fe1 10.4(6) . . . . ? C33 C30 C31 C32 175.9(4) . . . . ? C38 C39 C40 C41 2.5(6) . . . . ? C38 C43 C44 C45 -91.4(5) . . . . ? C39 C38 C43 C42 -2.2(6) . . . . ? C39 C38 C43 C44 173.1(4) . . . . ? C39 C38 N4 C37 108.6(4) . . . . ? C39 C38 N4 Fe1 -72.8(4) . . . . ? C39 C40 C41 C42 -2.1(7) . . . . ? C40 C41 C42 C43 -0.5(7) . . . . ? C41 C42 C43 C38 2.6(6) . . . . ? C41 C42 C43 C44 -172.8(4) . . . . ? C42 C43 C44 C45 83.8(5) . . . . ? C43 C38 C39 C40 -0.3(6) . . . . ? C43 C38 N4 C37 -76.3(5) . . . . ? C43 C38 N4 Fe1 102.4(4) . . . . ? C43 C44 C45 C46 -68.0(5) . . . . ? C44 C45 C46 C47 -79.9(5) . . . . ? C44 C45 C46 C51 98.1(5) . . . . ? C45 C46 C47 C48 177.0(4) . . . . ? C45 C46 C51 C50 -178.7(4) . . . . ? C45 C46 C51 N2 -2.8(6) . . . . ? C46 C47 C48 C49 1.8(8) . . . . ? C46 C51 N2 C52 -161.7(4) . . . . ? C47 C46 C51 C50 -0.7(6) . . . . ? C47 C46 C51 N2 175.3(4) . . . . ? C47 C48 C49 C50 -0.7(8) . . . . ? C48 C49 C50 C51 -1.1(8) . . . . ? C49 C50 C51 C46 1.8(7) . . . . ? C49 C50 C51 N2 -174.1(4) . . . . ? C50 C51 N2 C52 14.4(6) . . . . ? C51 C46 C47 C48 -1.1(7) . . . . ? C52 C2 C3 C4 172.9(4) . . . . ? N1 C12 C13 C14 178.9(4) . . . . ? N1 C12 C17 C16 178.7(4) . . . . ? N1 C12 C17 C18 -2.3(6) . . . . ? N3 C26 C28 C27 -3.4(7) . . . . ? N3 C26 C28 C29 -179.1(4) . . . . ? N4 C38 C39 C40 174.9(4) . . . . ? N4 C38 C43 C42 -177.1(4) . . . . ? N4 C38 C43 C44 -1.8(6) . . . . ? O1 C1 C2 C3 -176.2(4) . . . . ? O1 C1 C2 C52 9.9(6) . . . . ? O1 C1 C6 C5 176.2(4) . . . . ? O1 C1 C6 C11 -8.6(6) . . . . ? O2 C27 C28 C26 8.1(6) . . . . ? O2 C27 C28 C29 -176.3(4) . . . . ? O2 C27 C32 C31 174.2(4) . . . . ? O2 C27 C32 C37 -10.8(6) . . . . ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 0.304 0.250 0.386 772.1 248.4 '11 CH3CN' 2 -0.663 0.750 -0.744 772.1 238.5 '11 CH3CN'