#------------------------------------------------------------------------------ #$Date: 2021-07-05 20:43:40 +0300 (Mon, 05 Jul 2021) $ #$Revision: 267192 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/73/7707354.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_7707354 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_issue 23 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 8057 _journal_page_last 8069 _journal_paper_doi 10.1039/d1dt00711d _journal_volume 50 _journal_year 2021 _chemical_formula_moiety '2(C46 H40 Br Fe N4 O2), 2(C2 H3 N), Br6 Fe2 O' _chemical_formula_sum 'C96 H86 Br8 Fe4 N10 O5' _chemical_formula_weight 2322.42 _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 _atom_sites_solution_primary dual _audit_creation_date 2021-04-29 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272) ; _audit_update_record ; 2021-04-29 deposited with the CCDC. 2021-05-04 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 99.896(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 15.6606(4) _cell_length_b 16.0326(4) _cell_length_c 37.4062(11) _cell_measurement_reflns_used 8333 _cell_measurement_temperature 100.15 _cell_measurement_theta_max 67.1860 _cell_measurement_theta_min 2.8890 _cell_volume 9252.2(4) _computing_cell_refinement 'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)' _computing_data_collection 'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)' _computing_data_reduction 'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)' _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)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.00(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 28.14 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -12.00 23.00 0.50 10.00 -- 5.00 8.00 -14.00 70 2 \w -28.00 89.00 0.50 10.00 -- 0.00 57.00 90.00 234 3 \w -87.00 -38.00 0.50 10.00 -- 0.00 57.00 90.00 98 4 \w -162.00 -4.00 0.50 40.00 -- -90.00 8.00 -14.00 316 5 \w -172.00-146.00 0.50 40.00 -- -90.00 43.00 -30.00 52 6 \w -137.00-110.00 0.50 40.00 -- -90.00 43.00 -30.00 54 7 \w -141.00 -82.00 0.50 40.00 -- -90.00 57.00 -30.00 118 8 \w -38.00 -12.00 0.50 40.00 -- -90.00 57.00 -30.00 52 9 \w -179.00 -83.00 0.50 40.00 -- -90.00 57.00-180.00 192 10 \w -50.00 -12.00 0.50 40.00 -- -90.00 57.00-180.00 76 11 \w -178.00-145.00 0.50 40.00 -- -90.00 57.00 -30.00 66 12 \w -179.00 -86.00 0.50 40.00 -- -90.00 57.00-150.00 186 13 \w -141.00 -1.00 0.50 40.00 -- -90.00 60.00 60.00 280 14 \w -133.00 -83.00 0.50 40.00 -- -90.00 60.00 150.00 100 15 \w -65.00 -39.00 0.50 40.00 -- -90.00 60.00 -60.00 52 16 \w -179.00-145.00 0.50 40.00 -- -90.00 60.00 150.00 68 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB AFC11 (RCD3): quarter-chi single' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0642516000 _diffrn_orient_matrix_UB_12 0.0032284000 _diffrn_orient_matrix_UB_13 0.0361068000 _diffrn_orient_matrix_UB_21 0.0752689000 _diffrn_orient_matrix_UB_22 0.0139140000 _diffrn_orient_matrix_UB_23 -0.0209892000 _diffrn_orient_matrix_UB_31 -0.0130809000 _diffrn_orient_matrix_UB_32 0.0950512000 _diffrn_orient_matrix_UB_33 0.0018606000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.1067 _diffrn_reflns_av_unetI/netI 0.1062 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_number 68070 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 68.248 _diffrn_reflns_theta_min 2.909 _diffrn_source 'Rotating-anode X-ray tube' _diffrn_source_type 'Rigaku (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 9.439 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.75491 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour orange _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.667 _exptl_crystal_description plate _exptl_crystal_F_000 4624 _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _refine_diff_density_max 1.424 _refine_diff_density_min -0.864 _refine_diff_density_rms 0.139 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1127 _refine_ls_number_reflns 16805 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.013 _refine_ls_R_factor_all 0.1292 _refine_ls_R_factor_gt 0.0698 _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^)+(0.0877P)^2^+1.8599P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1523 _refine_ls_wR_factor_ref 0.1778 _reflns_Friedel_coverage 0.000 _reflns_number_gt 9942 _reflns_number_total 16805 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt00711d2.cif _cod_data_source_block FeROP1 _cod_depositor_comments 'Adding full bibliography for 7707347--7707359.cif.' _cod_database_code 7707354 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'C96 H86 Br8 Fe4 N10 O5' _chemical_oxdiff_usercomment FeMeEhtyl _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 0.834 _shelx_estimated_absorpt_t_min 0.519 _reflns_odcompleteness_completeness 99.30 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 68.13 _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. Restrained distances Fe3-Br4 \\sim Fe3-Br5 \\sim Fe3-Br3 \\sim Fe3-Br3A \\sim Fe3-Br4A \\sim Fe3-Br5A with sigma of 0.02 Br3-Br4 \\sim Br4-Br5 \\sim Br5-Br3 with sigma of 0.02 3. Others Sof(Br5A)=Sof(Fe3A)=Sof(Br4A)=Sof(Br3A)=1-FVAR(1) Sof(Br3)=Sof(Br4)=Sof(Br5)=Sof(Fe3)=FVAR(1) Fixed Uiso: Br5A(0.065) Fe3A(0.028) Br4A(0.065) Br3A(0.065) 4.a Secondary CH2 refined with riding coordinates: C15(H15A,H15B), C16(H16A,H16B), C38(H38A,H38B), C39(H39A,H39B), C65(H65A, H65B), C66(H66A,H66B), C88(H88A,H88B), C89(H89A,H89B) 4.b Aromatic/amide H refined with riding coordinates: N2(H2), N4(H4), C3(H3), C5(H5), C8(H8), C10(H10), C11(H11), C12(H12), C13(H13), C18(H18), C19(H19), C20(H20), C21(H21), C23(H23), C26(H26), C28(H28), C31(H31), C33(H33), C34(H34), C35(H35), C36(H36), C41(H41), C42(H42), C43(H43), C44(H44), C46(H46), N6(H6), N8(H8A), C53(H53), C55(H55), C58(H58), C60(H60), C61(H61), C62(H62), C63(H63), C68(H68), C69(H69), C70(H70), C71(H71), C73(H73), C76(H76), C78(H78), C81(H81), C83(H83), C84(H84), C85(H85), C86(H86), C91(H91), C92(H92), C93(H93), C94(H94), C96(H96) 4.c Idealised Me refined as rotating group: C7(H7A,H7B,H7C), C30(H30A,H30B,H30C), C57(H57A,H57B,H57C), C80(H80A,H80B, H80C), C102(H10A,H10B,H10C), C104(H10D,H10E,H10F) ; _shelx_res_file ; TITL shelxt_a.res in P2(1)/n 2018ncs0262.res created by SHELXL-2018/3 at 11:52:30 on 29-Apr-2021 CELL 1.54184 15.6606 16.0326 37.4062 90 99.896 90 ZERR 4 0.0004 0.0004 0.0011 0 0.003 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H Br Fe N O UNIT 384 344 32 16 40 20 SADI Fe3 Br4 Fe3 Br5 Fe3 Br3 Fe3 Br3A Fe3 Br4A Fe3 Br5A SADI Br3 Br4 Br4 Br5 Br5 Br3 L.S. 8 PLAN 15 SIZE 0.02 0.05 0.08 TEMP -173.15(10) CONF BOND $H LIST 6 MORE -1 fmap 2 acta MERG 2 OMIT 0 4 8 OMIT -1 16 13 REM REM REM WGHT 0.087700 1.859900 FVAR 0.10144 0.93367 FE1 4 0.633017 0.552944 0.407442 11.00000 0.01823 0.02179 = 0.01620 -0.00046 0.00423 -0.00057 BR1 3 0.701748 0.430508 0.443004 11.00000 0.02875 0.03323 = 0.02350 0.00872 0.00673 0.00387 O1 6 0.542723 0.564781 0.439076 11.00000 0.01715 0.03179 = 0.02037 -0.00561 0.00138 -0.00032 O2 6 0.727885 0.545581 0.377262 11.00000 0.02203 0.02402 = 0.01850 0.00190 0.00494 0.00001 N1 5 0.527145 0.534666 0.363951 11.00000 0.02642 0.02142 = 0.01780 -0.00108 0.00954 -0.00239 N2 5 0.763403 0.428737 0.334706 11.00000 0.02033 0.02010 = 0.01826 0.00278 0.00545 0.00274 AFIX 43 H2 2 0.743071 0.442592 0.354406 11.00000 -1.20000 AFIX 0 N3 5 0.655971 0.684517 0.406983 11.00000 0.01963 0.02836 = 0.01775 -0.00499 0.00058 0.00795 N4 5 0.538392 0.616370 0.503901 11.00000 0.02182 0.01851 = 0.01826 -0.00302 0.00625 -0.00586 AFIX 43 H4 2 0.567281 0.602240 0.486620 11.00000 -1.20000 AFIX 0 C1 1 0.457169 0.561203 0.433220 11.00000 0.02152 0.01737 = 0.01893 0.00246 0.00344 -0.00309 C2 1 0.411284 0.579995 0.461929 11.00000 0.02063 0.01579 = 0.02364 0.00440 0.00132 0.00069 C3 1 0.320121 0.571264 0.456299 11.00000 0.02154 0.01922 = 0.02881 -0.00071 0.00780 -0.00323 AFIX 43 H3 2 0.290479 0.584367 0.475707 11.00000 -1.20000 AFIX 0 C4 1 0.272297 0.544558 0.423866 11.00000 0.02334 0.01621 = 0.02350 0.00218 0.00308 -0.00388 C5 1 0.318020 0.529620 0.395477 11.00000 0.01825 0.01949 = 0.01711 -0.00102 0.00123 -0.00339 AFIX 43 H5 2 0.286345 0.512467 0.372697 11.00000 -1.20000 AFIX 0 C6 1 0.408300 0.538660 0.398898 11.00000 0.02123 0.02229 = 0.01164 0.00212 -0.00083 0.00133 C7 1 0.176902 0.531510 0.419136 11.00000 0.01707 0.03259 = 0.02200 0.00167 -0.00192 -0.00886 AFIX 137 H7A 2 0.164321 0.471596 0.418131 11.00000 -1.50000 H7B 2 0.148872 0.557934 0.396517 11.00000 -1.50000 H7C 2 0.154714 0.556411 0.439647 11.00000 -1.50000 AFIX 0 C8 1 0.446211 0.527851 0.366603 11.00000 0.03120 0.01994 = 0.01727 0.00153 0.00056 -0.00058 AFIX 43 H8 2 0.407437 0.514257 0.344963 11.00000 -1.20000 AFIX 0 C9 1 0.550160 0.529842 0.328419 11.00000 0.01662 0.03413 = 0.01699 -0.00030 -0.00377 0.00722 C10 1 0.571142 0.604303 0.312791 11.00000 0.02517 0.03756 = 0.01926 0.01633 0.00409 0.01098 AFIX 43 H10 2 0.566203 0.655462 0.325086 11.00000 -1.20000 AFIX 0 C11 1 0.598736 0.604935 0.280033 11.00000 0.03326 0.07224 = 0.02209 0.01712 0.00190 0.01647 AFIX 43 H11 2 0.612430 0.656080 0.269505 11.00000 -1.20000 AFIX 0 C12 1 0.606493 0.529724 0.262326 11.00000 0.02275 0.09179 = 0.02458 0.00213 -0.00113 0.01726 AFIX 43 H12 2 0.627615 0.529291 0.239990 11.00000 -1.20000 AFIX 0 C13 1 0.583677 0.455725 0.277025 11.00000 0.02084 0.07191 = 0.01894 -0.01205 -0.00911 0.01388 AFIX 43 H13 2 0.587423 0.405139 0.264159 11.00000 -1.20000 AFIX 0 C14 1 0.555083 0.453611 0.310542 11.00000 0.02460 0.04884 = 0.01685 -0.00773 -0.00362 0.00711 C15 1 0.534974 0.371956 0.326410 11.00000 0.02823 0.03810 = 0.03627 -0.01426 -0.00498 -0.00630 AFIX 23 H15A 2 0.512372 0.332990 0.306490 11.00000 -1.20000 H15B 2 0.488985 0.380336 0.341206 11.00000 -1.20000 AFIX 0 C16 1 0.615985 0.331883 0.350668 11.00000 0.04350 0.02094 = 0.03534 -0.00683 0.01545 -0.01489 AFIX 23 H16A 2 0.643399 0.374394 0.368153 11.00000 -1.20000 H16B 2 0.595986 0.285871 0.364834 11.00000 -1.20000 AFIX 0 C17 1 0.683190 0.298413 0.330568 11.00000 0.03382 0.01973 = 0.02622 -0.00085 0.00251 0.00412 C18 1 0.674175 0.216320 0.317926 11.00000 0.04857 0.02152 = 0.03300 0.00238 -0.00206 0.00159 AFIX 43 H18 2 0.625471 0.184460 0.321840 11.00000 -1.20000 AFIX 0 C19 1 0.734639 0.180819 0.299899 11.00000 0.06478 0.01559 = 0.04110 -0.00490 -0.00003 0.00577 AFIX 43 H19 2 0.727648 0.124894 0.291515 11.00000 -1.20000 AFIX 0 C20 1 0.805870 0.227068 0.294022 11.00000 0.05018 0.03247 = 0.01968 -0.00085 0.01166 0.01370 AFIX 43 H20 2 0.848443 0.201908 0.282239 11.00000 -1.20000 AFIX 0 C21 1 0.815423 0.307608 0.304878 11.00000 0.04263 0.02262 = 0.01791 0.00406 0.00547 0.00742 AFIX 43 H21 2 0.863591 0.339357 0.300271 11.00000 -1.20000 AFIX 0 C22 1 0.753329 0.343466 0.322989 11.00000 0.03320 0.02043 = 0.01312 0.00081 -0.00193 0.00554 C23 1 0.800052 0.487032 0.318606 11.00000 0.01754 0.03070 = 0.02473 0.00244 0.00187 0.00674 AFIX 43 H23 2 0.827924 0.471323 0.298990 11.00000 -1.20000 AFIX 0 C24 1 0.760457 0.600440 0.357469 11.00000 0.01792 0.02238 = 0.02085 0.00319 -0.00068 -0.00076 C25 1 0.801319 0.572655 0.328316 11.00000 0.02118 0.01933 = 0.02644 0.00224 0.00261 -0.00056 C26 1 0.837064 0.629620 0.306589 11.00000 0.01681 0.02741 = 0.02146 0.00960 0.00164 0.00153 AFIX 43 H26 2 0.865214 0.609244 0.287783 11.00000 -1.20000 AFIX 0 C27 1 0.832352 0.714978 0.311868 11.00000 0.01716 0.03676 = 0.02803 0.01523 0.00297 -0.00515 C28 1 0.790471 0.741445 0.339447 11.00000 0.02761 0.01836 = 0.03420 0.00556 0.00226 -0.00538 AFIX 43 H28 2 0.786850 0.799774 0.343401 11.00000 -1.20000 AFIX 0 C29 1 0.752697 0.687474 0.362141 11.00000 0.02614 0.01849 = 0.01492 0.00186 0.00182 -0.00388 C30 1 0.871297 0.775834 0.288567 11.00000 0.02932 0.03761 = 0.03318 0.01011 0.00956 -0.00511 AFIX 137 H30A 2 0.826220 0.795786 0.268964 11.00000 -1.50000 H30B 2 0.917127 0.748110 0.278157 11.00000 -1.50000 H30C 2 0.895895 0.823223 0.303410 11.00000 -1.50000 AFIX 0 C31 1 0.704565 0.725121 0.387752 11.00000 0.01946 0.02496 = 0.02432 0.00185 -0.00081 0.00302 AFIX 43 H31 2 0.708634 0.783893 0.390809 11.00000 -1.20000 AFIX 0 C32 1 0.609536 0.737623 0.428412 11.00000 0.03102 0.01903 = 0.01955 0.00072 0.00837 -0.00247 C33 1 0.528269 0.765232 0.412879 11.00000 0.03048 0.03622 = 0.02939 -0.00948 0.00874 0.00619 AFIX 43 H33 2 0.505012 0.749819 0.388637 11.00000 -1.20000 AFIX 0 C34 1 0.480553 0.814668 0.431971 11.00000 0.03181 0.04492 = 0.04402 -0.00501 0.00345 0.01202 AFIX 43 H34 2 0.424547 0.833322 0.421048 11.00000 -1.20000 AFIX 0 C35 1 0.514529 0.837187 0.467244 11.00000 0.05263 0.02589 = 0.04018 -0.00541 0.02086 0.00189 AFIX 43 H35 2 0.482295 0.872068 0.480569 11.00000 -1.20000 AFIX 0 C36 1 0.595387 0.808790 0.482982 11.00000 0.03591 0.02922 = 0.02195 -0.00152 0.00668 0.00075 AFIX 43 H36 2 0.618199 0.824343 0.507252 11.00000 -1.20000 AFIX 0 C37 1 0.644429 0.757810 0.464122 11.00000 0.02982 0.02666 = 0.02141 -0.00157 0.00834 -0.00192 C38 1 0.730485 0.724470 0.483201 11.00000 0.02377 0.03014 = 0.02417 -0.00398 0.00113 -0.00936 AFIX 23 H38A 2 0.759428 0.767896 0.499827 11.00000 -1.20000 H38B 2 0.767748 0.713033 0.464900 11.00000 -1.20000 AFIX 0 C39 1 0.722555 0.643299 0.505343 11.00000 0.02586 0.02983 = 0.02016 -0.00782 -0.00380 -0.00234 AFIX 23 H39A 2 0.690172 0.600993 0.489110 11.00000 -1.20000 H39B 2 0.781318 0.620932 0.514172 11.00000 -1.20000 AFIX 0 C40 1 0.677793 0.656860 0.536941 11.00000 0.03521 0.01747 = 0.01949 0.00417 -0.00220 -0.00176 C41 1 0.728426 0.684093 0.569325 11.00000 0.03837 0.03598 = 0.01893 -0.00124 -0.00052 -0.00462 AFIX 43 H41 2 0.789211 0.690436 0.570680 11.00000 -1.20000 AFIX 0 C42 1 0.690710 0.702133 0.599775 11.00000 0.05296 0.04131 = 0.03041 0.00035 -0.00535 -0.02573 AFIX 43 H42 2 0.725759 0.722381 0.621290 11.00000 -1.20000 AFIX 0 C43 1 0.603275 0.690737 0.598747 11.00000 0.06906 0.03495 = 0.01487 -0.00786 0.00823 -0.00767 AFIX 43 H43 2 0.578188 0.703012 0.619531 11.00000 -1.20000 AFIX 0 C44 1 0.551110 0.661021 0.567056 11.00000 0.03288 0.02407 = 0.02745 0.00195 0.00687 -0.00924 AFIX 43 H44 2 0.490907 0.651874 0.566346 11.00000 -1.20000 AFIX 0 C45 1 0.588914 0.645082 0.536583 11.00000 0.03012 0.02046 = 0.01728 -0.00036 -0.00025 -0.00012 C46 1 0.454266 0.608176 0.496130 11.00000 0.03301 0.01683 = 0.02005 0.00145 0.00863 0.00152 AFIX 43 H46 2 0.420631 0.621692 0.514179 11.00000 -1.20000 AFIX 0 FE2 4 0.364631 0.448203 0.089507 11.00000 0.01754 0.01878 = 0.01506 -0.00110 0.00167 -0.00048 BR2 3 0.286685 0.568249 0.055195 11.00000 0.02815 0.03192 = 0.02275 0.00755 0.00575 0.00513 N5 5 0.351302 0.314703 0.087019 11.00000 0.01865 0.02685 = 0.01457 -0.00176 0.00701 0.00158 N6 5 0.473418 0.388746 -0.005006 11.00000 0.02072 0.01548 = 0.01725 -0.00003 -0.00110 0.00024 AFIX 43 H6 2 0.440458 0.403683 0.010724 11.00000 -1.20000 AFIX 0 N7 5 0.466187 0.466648 0.134674 11.00000 0.02487 0.01587 = 0.01379 0.00115 0.00286 -0.00032 N8 5 0.221430 0.549563 0.164184 11.00000 0.01751 0.01577 = 0.01799 -0.00773 0.00221 0.00093 AFIX 43 H8A 2 0.239759 0.542459 0.143434 11.00000 -1.20000 AFIX 0 O3 6 0.266390 0.443659 0.118504 11.00000 0.02630 0.02132 = 0.01935 0.00061 0.00687 0.00168 O4 6 0.459389 0.446505 0.058968 11.00000 0.02086 0.02643 = 0.01753 -0.00181 0.00139 -0.00052 C51 1 0.238175 0.383004 0.136828 11.00000 0.01693 0.02375 = 0.02000 0.00435 0.00068 0.00066 C52 1 0.194861 0.402456 0.166330 11.00000 0.01651 0.03004 = 0.01987 0.00080 0.00695 0.00423 C53 1 0.165367 0.337752 0.186636 11.00000 0.01186 0.03137 = 0.03142 0.00192 0.00572 -0.00188 AFIX 43 H53 2 0.136775 0.352221 0.206200 11.00000 -1.20000 AFIX 0 C54 1 0.175940 0.255635 0.179521 11.00000 0.02168 0.02321 = 0.02909 0.00605 0.00829 -0.00245 C55 1 0.219556 0.236838 0.150933 11.00000 0.02213 0.01780 = 0.03808 -0.00614 0.00408 -0.00418 AFIX 43 H55 2 0.228080 0.179777 0.145672 11.00000 -1.20000 AFIX 0 C56 1 0.251677 0.297650 0.129423 11.00000 0.02256 0.01613 = 0.01771 -0.00187 -0.00098 0.00242 C57 1 0.148118 0.187092 0.202044 11.00000 0.03897 0.02773 = 0.04547 0.00392 0.01442 0.00069 AFIX 137 H57A 2 0.194686 0.145783 0.207399 11.00000 -1.50000 H57B 2 0.095984 0.160288 0.188698 11.00000 -1.50000 H57C 2 0.135440 0.210258 0.224806 11.00000 -1.50000 AFIX 0 C58 1 0.303690 0.269483 0.103737 11.00000 0.02458 0.02314 = 0.02139 -0.00424 0.00112 0.00337 AFIX 43 H58 2 0.302616 0.211400 0.098653 11.00000 -1.20000 AFIX 0 C59 1 0.403793 0.267780 0.065872 11.00000 0.02842 0.02126 = 0.02514 -0.00057 0.00990 0.00566 C60 1 0.485956 0.245966 0.082186 11.00000 0.03954 0.02940 = 0.02044 0.00136 0.00952 0.01243 AFIX 43 H60 2 0.506999 0.263684 0.106327 11.00000 -1.20000 AFIX 0 C61 1 0.538479 0.198717 0.064085 11.00000 0.03612 0.05661 = 0.02743 -0.00421 0.00776 0.01633 AFIX 43 H61 2 0.595477 0.184183 0.075506 11.00000 -1.20000 AFIX 0 C62 1 0.506523 0.172487 0.028615 11.00000 0.04066 0.04299 = 0.03851 -0.00028 0.01775 0.01027 AFIX 43 H62 2 0.541713 0.139601 0.015796 11.00000 -1.20000 AFIX 0 C63 1 0.424280 0.194386 0.012417 11.00000 0.04864 0.02813 = 0.02896 -0.00432 0.01560 -0.00453 AFIX 43 H63 2 0.402728 0.175102 -0.011443 11.00000 -1.20000 AFIX 0 C64 1 0.371570 0.244106 0.030006 11.00000 0.03119 0.01523 = 0.02711 -0.00537 0.00713 0.00134 C65 1 0.284118 0.272639 0.010372 11.00000 0.03265 0.03210 = 0.01847 -0.00954 0.00452 -0.01262 AFIX 23 H65A 2 0.245544 0.282532 0.028318 11.00000 -1.20000 H65B 2 0.258023 0.227823 -0.006191 11.00000 -1.20000 AFIX 0 C66 1 0.289807 0.354165 -0.012019 11.00000 0.03085 0.03146 = 0.01940 -0.00206 -0.00003 -0.00429 AFIX 23 H66A 2 0.230539 0.372753 -0.022566 11.00000 -1.20000 H66B 2 0.317265 0.398679 0.004386 11.00000 -1.20000 AFIX 0 C67 1 0.340807 0.341521 -0.041769 11.00000 0.03256 0.02089 = 0.02885 -0.00075 0.00157 -0.00753 C68 1 0.299723 0.307696 -0.074749 11.00000 0.03085 0.03744 = 0.02262 -0.00754 -0.00631 -0.01189 AFIX 43 H68 2 0.239143 0.297359 -0.078054 11.00000 -1.20000 AFIX 0 C69 1 0.343448 0.288845 -0.102528 11.00000 0.06076 0.04070 = 0.01687 -0.01534 -0.00280 -0.02064 AFIX 43 H69 2 0.313064 0.266294 -0.124578 11.00000 -1.20000 AFIX 0 C70 1 0.432356 0.302800 -0.098362 11.00000 0.05950 0.03176 = 0.01783 -0.00096 0.01360 -0.00865 AFIX 43 H70 2 0.463144 0.288928 -0.117322 11.00000 -1.20000 AFIX 0 C71 1 0.475669 0.337264 -0.066156 11.00000 0.03252 0.02375 = 0.02234 -0.00225 0.00378 -0.00951 AFIX 43 H71 2 0.536187 0.347818 -0.063051 11.00000 -1.20000 AFIX 0 C72 1 0.429573 0.356147 -0.038525 11.00000 0.03401 0.01751 = 0.01298 -0.00687 0.00334 -0.00492 C73 1 0.556245 0.399131 0.005190 11.00000 0.02471 0.02092 = 0.02021 -0.00463 0.00603 0.00103 AFIX 43 H73 2 0.593249 0.386551 -0.011718 11.00000 -1.20000 AFIX 0 C74 1 0.544222 0.448469 0.067212 11.00000 0.01992 0.01644 = 0.01844 0.00754 -0.00301 -0.00349 C75 1 0.594628 0.428026 0.039931 11.00000 0.01868 0.01248 = 0.02154 0.00432 0.00319 -0.00078 C76 1 0.685388 0.436045 0.047546 11.00000 0.02424 0.01911 = 0.01978 0.00210 0.00610 0.00184 AFIX 43 H76 2 0.717654 0.425319 0.028731 11.00000 -1.20000 AFIX 0 C77 1 0.729779 0.459130 0.081649 11.00000 0.01858 0.02561 = 0.02146 0.00418 -0.00129 -0.00531 C78 1 0.681117 0.473514 0.108624 11.00000 0.02131 0.02559 = 0.01734 0.00365 -0.00205 -0.00216 AFIX 43 H78 2 0.710151 0.489058 0.132096 11.00000 -1.20000 AFIX 0 C79 1 0.589370 0.465896 0.102516 11.00000 0.01279 0.02531 = 0.02038 -0.00025 0.00039 -0.00436 C80 1 0.826309 0.470605 0.088471 11.00000 0.02401 0.04489 = 0.02836 -0.00173 0.00508 -0.00463 AFIX 137 H80A 2 0.839991 0.530104 0.087411 11.00000 -1.50000 H80B 2 0.851351 0.440536 0.069935 11.00000 -1.50000 H80C 2 0.850628 0.448667 0.112523 11.00000 -1.50000 AFIX 0 C81 1 0.549337 0.474202 0.134475 11.00000 0.02473 0.02221 = 0.02134 -0.00292 0.00451 -0.00188 AFIX 43 H81 2 0.586016 0.485965 0.156881 11.00000 -1.20000 AFIX 0 C82 1 0.441883 0.464644 0.170315 11.00000 0.01481 0.03574 = 0.01224 -0.00261 0.00415 -0.00219 C83 1 0.423117 0.386174 0.182878 11.00000 0.01937 0.03410 = 0.02591 0.00224 0.00090 -0.00364 AFIX 43 H83 2 0.429012 0.337943 0.168750 11.00000 -1.20000 AFIX 0 C84 1 0.395595 0.378569 0.216315 11.00000 0.02310 0.04686 = 0.02293 0.02063 0.00198 0.00380 AFIX 43 H84 2 0.385038 0.325007 0.225506 11.00000 -1.20000 AFIX 0 C85 1 0.383806 0.449362 0.235952 11.00000 0.01961 0.05535 = 0.02008 0.00519 0.00426 0.00409 AFIX 43 H85 2 0.363246 0.444847 0.258334 11.00000 -1.20000 AFIX 0 C86 1 0.401979 0.526392 0.222940 11.00000 0.02025 0.04296 = 0.01944 -0.00375 -0.00102 0.00690 AFIX 43 H86 2 0.394234 0.574619 0.236788 11.00000 -1.20000 AFIX 0 C87 1 0.431288 0.535882 0.190202 11.00000 0.02124 0.03429 = 0.01887 -0.00786 0.00089 0.00182 C88 1 0.447205 0.623047 0.176928 11.00000 0.02457 0.02781 = 0.02366 -0.00741 -0.00186 -0.00349 AFIX 23 H88A 2 0.493451 0.620553 0.161938 11.00000 -1.20000 H88B 2 0.467994 0.659096 0.198127 11.00000 -1.20000 AFIX 0 C89 1 0.365061 0.662886 0.154242 11.00000 0.04398 0.02318 = 0.01501 -0.00353 0.00431 -0.00494 AFIX 23 H89A 2 0.382158 0.714675 0.142902 11.00000 -1.20000 H89B 2 0.341286 0.624019 0.134454 11.00000 -1.20000 AFIX 0 C90 1 0.294624 0.683544 0.175622 11.00000 0.03927 0.02075 = 0.01315 0.00212 -0.00713 0.00665 C91 1 0.297395 0.761236 0.194254 11.00000 0.04076 0.01713 = 0.03101 0.00082 -0.00929 -0.00130 AFIX 43 H91 2 0.344804 0.797959 0.193801 11.00000 -1.20000 AFIX 0 C92 1 0.232363 0.784088 0.212960 11.00000 0.05383 0.02840 = 0.03744 -0.01732 -0.00006 0.01049 AFIX 43 H92 2 0.234396 0.837074 0.224443 11.00000 -1.20000 AFIX 0 C93 1 0.164850 0.730881 0.215090 11.00000 0.03872 0.04195 = 0.04130 -0.01735 -0.00112 0.00348 AFIX 43 H93 2 0.120914 0.746708 0.228380 11.00000 -1.20000 AFIX 0 C94 1 0.160676 0.655068 0.198112 11.00000 0.02784 0.01639 = 0.03684 -0.00818 -0.00279 0.01102 AFIX 43 H94 2 0.113122 0.618846 0.199086 11.00000 -1.20000 AFIX 0 C95 1 0.225919 0.631158 0.179485 11.00000 0.02525 0.03158 = 0.01948 -0.00081 -0.00238 -0.00138 C96 1 0.191981 0.485482 0.179059 11.00000 0.01593 0.02645 = 0.03116 -0.00451 0.00812 -0.00123 AFIX 43 H96 2 0.166571 0.494629 0.200030 11.00000 -1.20000 AFIX 0 N9 5 0.432971 0.839118 0.553633 11.00000 0.03875 0.12213 = 0.12400 -0.03022 -0.00663 0.02878 C101 1 0.488173 0.878569 0.568527 11.00000 0.03746 0.09260 = 0.05882 -0.00532 -0.00671 0.03171 C102 1 0.559913 0.929542 0.585053 11.00000 0.03615 0.10552 = 0.06906 -0.02504 0.01599 -0.00281 AFIX 137 H10A 2 0.585362 0.957517 0.566089 11.00000 -1.50000 H10B 2 0.603815 0.894344 0.599655 11.00000 -1.50000 H10C 2 0.539385 0.971456 0.600663 11.00000 -1.50000 AFIX 0 N10 5 0.555332 0.134247 -0.052649 11.00000 0.03639 0.11145 = 0.05889 -0.03018 0.00774 0.01613 C103 1 0.498693 0.092500 -0.065530 11.00000 0.03325 0.09521 = 0.02889 -0.00705 0.00579 0.02706 C104 1 0.427366 0.039529 -0.081757 11.00000 0.04365 0.08855 = 0.07025 -0.00726 0.01372 -0.00118 AFIX 137 H10D 2 0.450326 -0.011870 -0.090659 11.00000 -1.50000 H10E 2 0.392051 0.068986 -0.102042 11.00000 -1.50000 H10F 2 0.391533 0.025684 -0.063532 11.00000 -1.50000 AFIX 0 PART 1 BR3 3 0.724288 0.946792 0.285074 21.00000 0.03022 0.04099 = 0.03785 0.00355 0.00584 0.00422 BR4 3 0.526375 1.008708 0.326076 21.00000 0.03512 0.07160 = 0.03488 -0.00910 0.00474 0.00712 BR5 3 0.520854 0.813190 0.263570 21.00000 0.05053 0.03515 = 0.07235 -0.00673 0.03233 -0.00778 FE3 4 0.571791 0.949989 0.275057 21.00000 0.02431 0.02727 = 0.02474 0.00178 0.00462 0.00122 PART 0 O5 6 0.532841 1.010137 0.235931 11.00000 0.03952 0.04323 = 0.04558 0.01171 -0.00353 -0.01199 FE4 4 0.444002 1.016045 0.199493 11.00000 0.02717 0.03664 = 0.03079 0.00531 -0.00085 -0.00264 BR6 3 0.310401 0.999415 0.219497 11.00000 0.04892 0.04627 = 0.05258 -0.00381 0.02353 -0.00747 BR7 3 0.463489 0.909329 0.157785 11.00000 0.05238 0.05544 = 0.03815 0.00321 0.01447 0.01025 BR8 3 0.437462 1.147012 0.170773 11.00000 0.04219 0.04355 = 0.05073 0.01362 -0.00563 -0.00546 PART 2 BR5A 3 0.557649 0.842119 0.326325 -21.00000 10.06500 FE3A 4 0.554588 0.972422 0.298122 -21.00000 10.02800 BR4A 3 0.539509 1.081956 0.340319 -21.00000 10.06500 BR3A 3 0.686289 0.990520 0.281147 -21.00000 10.06500 HKLF 4 REM shelxt_a.res in P2(1)/n REM wR2 = 0.1778, GooF = S = 1.012, Restrained GooF = 1.013 for all data REM R1 = 0.0698 for 9942 Fo > 4sig(Fo) and 0.1292 for all 16805 data REM 1127 parameters refined using 6 restraints END WGHT 0.0877 1.9280 REM Highest difference peak 1.424, deepest hole -0.864, 1-sigma level 0.139 Q1 1 0.4710 0.9849 0.1721 11.00000 0.05 1.42 Q2 1 0.4251 1.0410 0.2222 11.00000 0.05 1.37 Q3 1 0.5190 1.0649 0.2708 11.00000 0.05 1.36 Q4 1 0.5555 0.8175 0.2903 11.00000 0.05 1.14 Q5 1 0.2728 1.0616 0.2167 11.00000 0.05 1.13 Q6 1 0.2566 1.0480 0.2126 11.00000 0.05 1.12 Q7 1 1.0192 0.6837 0.2646 11.00000 0.05 1.08 Q8 1 0.4891 0.9079 0.1883 11.00000 0.05 1.08 Q9 1 0.6398 0.5719 0.4071 11.00000 0.05 0.99 Q10 1 0.2954 0.5950 0.0549 11.00000 0.05 0.99 Q11 1 0.3783 0.4366 0.0984 11.00000 0.05 0.95 Q12 1 0.7168 0.4460 0.4496 11.00000 0.05 0.93 Q13 1 0.4446 0.9184 0.4868 11.00000 0.05 0.89 Q14 1 0.4473 1.1759 0.2049 11.00000 0.05 0.61 Q15 1 0.4569 0.9628 0.2275 11.00000 0.05 0.58 ; _shelx_res_checksum 93894 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.350 _oxdiff_exptl_absorpt_empirical_full_min 0.759 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 Fe1 Fe 0.63302(7) 0.55294(7) 0.40744(3) 0.0186(3) Uani 1 1 d . . . . . Br1 Br 0.70175(5) 0.43051(5) 0.44300(2) 0.0282(2) Uani 1 1 d . . . . . O1 O 0.5427(3) 0.5648(3) 0.43908(13) 0.0233(12) Uani 1 1 d . . . . . O2 O 0.7279(3) 0.5456(3) 0.37726(13) 0.0213(11) Uani 1 1 d . . . . . N1 N 0.5271(4) 0.5347(4) 0.36395(17) 0.0212(14) Uani 1 1 d . . . . . N2 N 0.7634(4) 0.4287(4) 0.33471(16) 0.0193(14) Uani 1 1 d . . . . . H2 H 0.743071 0.442592 0.354406 0.023 Uiso 1 1 calc R U . . . N3 N 0.6560(4) 0.6845(4) 0.40698(17) 0.0222(14) Uani 1 1 d . . . . . N4 N 0.5384(4) 0.6164(4) 0.50390(16) 0.0192(14) Uani 1 1 d . . . . . H4 H 0.567281 0.602240 0.486620 0.023 Uiso 1 1 calc R U . . . C1 C 0.4572(5) 0.5612(4) 0.4332(2) 0.0193(16) Uani 1 1 d . . . . . C2 C 0.4113(5) 0.5800(4) 0.4619(2) 0.0203(16) Uani 1 1 d . . . . . C3 C 0.3201(5) 0.5713(4) 0.4563(2) 0.0228(17) Uani 1 1 d . . . . . H3 H 0.290479 0.584367 0.475707 0.027 Uiso 1 1 calc R U . . . C4 C 0.2723(5) 0.5446(5) 0.4239(2) 0.0211(17) Uani 1 1 d . . . . . C5 C 0.3180(5) 0.5296(4) 0.3955(2) 0.0185(16) Uani 1 1 d . . . . . H5 H 0.286345 0.512467 0.372697 0.022 Uiso 1 1 calc R U . . . C6 C 0.4083(5) 0.5387(5) 0.39890(19) 0.0188(16) Uani 1 1 d . . . . . C7 C 0.1769(5) 0.5315(5) 0.4191(2) 0.0245(18) Uani 1 1 d . . . . . H7A H 0.164321 0.471596 0.418131 0.037 Uiso 1 1 calc R U . . . H7B H 0.148872 0.557934 0.396517 0.037 Uiso 1 1 calc R U . . . H7C H 0.154714 0.556411 0.439647 0.037 Uiso 1 1 calc R U . . . C8 C 0.4462(5) 0.5279(5) 0.3666(2) 0.0232(17) Uani 1 1 d . . . . . H8 H 0.407437 0.514257 0.344963 0.028 Uiso 1 1 calc R U . . . C9 C 0.5502(5) 0.5298(5) 0.3284(2) 0.0234(18) Uani 1 1 d . . . . . C10 C 0.5711(5) 0.6043(5) 0.3128(2) 0.0273(19) Uani 1 1 d . . . . . H10 H 0.566203 0.655462 0.325086 0.033 Uiso 1 1 calc R U . . . C11 C 0.5987(6) 0.6049(7) 0.2800(2) 0.043(3) Uani 1 1 d . . . . . H11 H 0.612430 0.656080 0.269505 0.051 Uiso 1 1 calc R U . . . C12 C 0.6065(6) 0.5297(7) 0.2623(3) 0.047(3) Uani 1 1 d . . . . . H12 H 0.627615 0.529291 0.239990 0.056 Uiso 1 1 calc R U . . . C13 C 0.5837(5) 0.4557(7) 0.2770(2) 0.039(2) Uani 1 1 d . . . . . H13 H 0.587423 0.405139 0.264159 0.046 Uiso 1 1 calc R U . . . C14 C 0.5551(5) 0.4536(6) 0.3105(2) 0.031(2) Uani 1 1 d . . . . . C15 C 0.5350(6) 0.3720(5) 0.3264(2) 0.035(2) Uani 1 1 d . . . . . H15A H 0.512372 0.332990 0.306490 0.043 Uiso 1 1 calc R U . . . H15B H 0.488985 0.380336 0.341206 0.043 Uiso 1 1 calc R U . . . C16 C 0.6160(6) 0.3319(5) 0.3507(2) 0.032(2) Uani 1 1 d . . . . . H16A H 0.643399 0.374394 0.368153 0.039 Uiso 1 1 calc R U . . . H16B H 0.595986 0.285871 0.364834 0.039 Uiso 1 1 calc R U . . . C17 C 0.6832(5) 0.2984(5) 0.3306(2) 0.0269(18) Uani 1 1 d . . . . . C18 C 0.6742(6) 0.2163(5) 0.3179(2) 0.035(2) Uani 1 1 d . . . . . H18 H 0.625471 0.184460 0.321840 0.043 Uiso 1 1 calc R U . . . C19 C 0.7346(7) 0.1808(5) 0.2999(3) 0.042(2) Uani 1 1 d . . . . . H19 H 0.727648 0.124894 0.291515 0.050 Uiso 1 1 calc R U . . . C20 C 0.8059(6) 0.2271(5) 0.2940(2) 0.033(2) Uani 1 1 d . . . . . H20 H 0.848443 0.201908 0.282239 0.040 Uiso 1 1 calc R U . . . C21 C 0.8154(6) 0.3076(5) 0.3049(2) 0.0277(19) Uani 1 1 d . . . . . H21 H 0.863591 0.339357 0.300271 0.033 Uiso 1 1 calc R U . . . C22 C 0.7533(5) 0.3435(5) 0.3230(2) 0.0229(17) Uani 1 1 d . . . . . C23 C 0.8001(5) 0.4870(5) 0.3186(2) 0.0245(18) Uani 1 1 d . . . . . H23 H 0.827924 0.471323 0.298990 0.029 Uiso 1 1 calc R U . . . C24 C 0.7605(5) 0.6004(5) 0.3575(2) 0.0209(17) Uani 1 1 d . . . . . C25 C 0.8013(5) 0.5727(5) 0.3283(2) 0.0225(17) Uani 1 1 d . . . . . C26 C 0.8371(5) 0.6296(5) 0.3066(2) 0.0221(17) Uani 1 1 d . . . . . H26 H 0.865214 0.609244 0.287783 0.027 Uiso 1 1 calc R U . . . C27 C 0.8324(5) 0.7150(5) 0.3119(2) 0.0274(19) Uani 1 1 d . . . . . C28 C 0.7905(5) 0.7414(5) 0.3394(2) 0.0271(19) Uani 1 1 d . . . . . H28 H 0.786850 0.799774 0.343401 0.033 Uiso 1 1 calc R U . . . C29 C 0.7527(5) 0.6875(5) 0.3621(2) 0.0201(16) Uani 1 1 d . . . . . C30 C 0.8713(6) 0.7758(5) 0.2886(2) 0.033(2) Uani 1 1 d . . . . . H30A H 0.826220 0.795786 0.268964 0.049 Uiso 1 1 calc R U . . . H30B H 0.917127 0.748110 0.278157 0.049 Uiso 1 1 calc R U . . . H30C H 0.895895 0.823223 0.303410 0.049 Uiso 1 1 calc R U . . . C31 C 0.7046(5) 0.7251(5) 0.3878(2) 0.0235(17) Uani 1 1 d . . . . . H31 H 0.708634 0.783893 0.390809 0.028 Uiso 1 1 calc R U . . . C32 C 0.6095(5) 0.7376(5) 0.4284(2) 0.0227(17) Uani 1 1 d . . . . . C33 C 0.5283(5) 0.7652(5) 0.4129(2) 0.032(2) Uani 1 1 d . . . . . H33 H 0.505012 0.749819 0.388637 0.038 Uiso 1 1 calc R U . . . C34 C 0.4806(6) 0.8147(6) 0.4320(3) 0.041(2) Uani 1 1 d . . . . . H34 H 0.424547 0.833322 0.421048 0.049 Uiso 1 1 calc R U . . . C35 C 0.5145(6) 0.8372(5) 0.4672(3) 0.038(2) Uani 1 1 d . . . . . H35 H 0.482295 0.872068 0.480569 0.046 Uiso 1 1 calc R U . . . C36 C 0.5954(6) 0.8088(5) 0.4830(2) 0.0288(19) Uani 1 1 d . . . . . H36 H 0.618199 0.824343 0.507252 0.035 Uiso 1 1 calc R U . . . C37 C 0.6444(5) 0.7578(5) 0.4641(2) 0.0255(18) Uani 1 1 d . . . . . C38 C 0.7305(5) 0.7245(5) 0.4832(2) 0.0264(18) Uani 1 1 d . . . . . H38A H 0.759428 0.767896 0.499827 0.032 Uiso 1 1 calc R U . . . H38B H 0.767748 0.713033 0.464900 0.032 Uiso 1 1 calc R U . . . C39 C 0.7226(5) 0.6433(5) 0.5053(2) 0.0262(18) Uani 1 1 d . . . . . H39A H 0.690172 0.600993 0.489110 0.031 Uiso 1 1 calc R U . . . H39B H 0.781318 0.620932 0.514172 0.031 Uiso 1 1 calc R U . . . C40 C 0.6778(5) 0.6569(5) 0.5369(2) 0.0249(18) Uani 1 1 d . . . . . C41 C 0.7284(6) 0.6841(5) 0.5693(2) 0.032(2) Uani 1 1 d . . . . . H41 H 0.789211 0.690436 0.570680 0.038 Uiso 1 1 calc R U . . . C42 C 0.6907(7) 0.7021(6) 0.5998(3) 0.043(2) Uani 1 1 d . . . . . H42 H 0.725759 0.722381 0.621290 0.052 Uiso 1 1 calc R U . . . C43 C 0.6033(7) 0.6907(5) 0.5987(2) 0.040(2) Uani 1 1 d . . . . . H43 H 0.578188 0.703012 0.619531 0.047 Uiso 1 1 calc R U . . . C44 C 0.5511(6) 0.6610(5) 0.5671(2) 0.0279(19) Uani 1 1 d . . . . . H44 H 0.490907 0.651874 0.566346 0.034 Uiso 1 1 calc R U . . . C45 C 0.5889(5) 0.6451(5) 0.5366(2) 0.0231(17) Uani 1 1 d . . . . . C46 C 0.4543(5) 0.6082(4) 0.4961(2) 0.0228(17) Uani 1 1 d . . . . . H46 H 0.420631 0.621692 0.514179 0.027 Uiso 1 1 calc R U . . . Fe2 Fe 0.36463(7) 0.44820(7) 0.08951(3) 0.0173(3) Uani 1 1 d . . . . . Br2 Br 0.28668(5) 0.56825(5) 0.05520(2) 0.0274(2) Uani 1 1 d . . . . . N5 N 0.3513(4) 0.3147(4) 0.08702(16) 0.0195(14) Uani 1 1 d . . . . . N6 N 0.4734(4) 0.3887(4) -0.00501(16) 0.0183(14) Uani 1 1 d . . . . . H6 H 0.440458 0.403683 0.010724 0.022 Uiso 1 1 calc R U . . . N7 N 0.4662(4) 0.4666(4) 0.13467(16) 0.0182(13) Uani 1 1 d . . . . . N8 N 0.2214(4) 0.5496(4) 0.16418(16) 0.0172(13) Uani 1 1 d . . . . . H8A H 0.239759 0.542459 0.143434 0.021 Uiso 1 1 calc R U . . . O3 O 0.2664(3) 0.4437(3) 0.11850(13) 0.0220(11) Uani 1 1 d . . . . . O4 O 0.4594(3) 0.4465(3) 0.05897(13) 0.0218(11) Uani 1 1 d . . . . . C51 C 0.2382(5) 0.3830(5) 0.1368(2) 0.0205(17) Uani 1 1 d . . . . . C52 C 0.1949(5) 0.4025(5) 0.1663(2) 0.0217(17) Uani 1 1 d . . . . . C53 C 0.1654(5) 0.3378(5) 0.1866(2) 0.0246(18) Uani 1 1 d . . . . . H53 H 0.136775 0.352221 0.206200 0.030 Uiso 1 1 calc R U . . . C54 C 0.1759(5) 0.2556(5) 0.1795(2) 0.0242(18) Uani 1 1 d . . . . . C55 C 0.2196(5) 0.2368(5) 0.1509(2) 0.0261(18) Uani 1 1 d . . . . . H55 H 0.228080 0.179777 0.145672 0.031 Uiso 1 1 calc R U . . . C56 C 0.2517(5) 0.2977(4) 0.1294(2) 0.0193(16) Uani 1 1 d . . . . . C57 C 0.1481(6) 0.1871(5) 0.2020(3) 0.037(2) Uani 1 1 d . . . . . H57A H 0.194686 0.145783 0.207399 0.055 Uiso 1 1 calc R U . . . H57B H 0.095984 0.160288 0.188698 0.055 Uiso 1 1 calc R U . . . H57C H 0.135440 0.210258 0.224806 0.055 Uiso 1 1 calc R U . . . C58 C 0.3037(5) 0.2695(5) 0.1037(2) 0.0234(17) Uani 1 1 d . . . . . H58 H 0.302616 0.211400 0.098653 0.028 Uiso 1 1 calc R U . . . C59 C 0.4038(5) 0.2678(5) 0.0659(2) 0.0243(18) Uani 1 1 d . . . . . C60 C 0.4860(6) 0.2460(5) 0.0822(2) 0.029(2) Uani 1 1 d . . . . . H60 H 0.506999 0.263684 0.106327 0.035 Uiso 1 1 calc R U . . . C61 C 0.5385(6) 0.1987(6) 0.0641(2) 0.040(2) Uani 1 1 d . . . . . H61 H 0.595477 0.184183 0.075506 0.048 Uiso 1 1 calc R U . . . C62 C 0.5065(6) 0.1725(6) 0.0286(3) 0.039(2) Uani 1 1 d . . . . . H62 H 0.541713 0.139601 0.015796 0.047 Uiso 1 1 calc R U . . . C63 C 0.4243(6) 0.1944(5) 0.0124(2) 0.034(2) Uani 1 1 d . . . . . H63 H 0.402728 0.175102 -0.011443 0.041 Uiso 1 1 calc R U . . . C64 C 0.3716(5) 0.2441(5) 0.0300(2) 0.0243(18) Uani 1 1 d . . . . . C65 C 0.2841(5) 0.2726(5) 0.0104(2) 0.0277(19) Uani 1 1 d . . . . . H65A H 0.245544 0.282532 0.028318 0.033 Uiso 1 1 calc R U . . . H65B H 0.258023 0.227823 -0.006191 0.033 Uiso 1 1 calc R U . . . C66 C 0.2898(5) 0.3542(5) -0.0120(2) 0.0277(19) Uani 1 1 d . . . . . H66A H 0.230539 0.372753 -0.022566 0.033 Uiso 1 1 calc R U . . . H66B H 0.317265 0.398679 0.004386 0.033 Uiso 1 1 calc R U . . . C67 C 0.3408(5) 0.3415(5) -0.0418(2) 0.0279(19) Uani 1 1 d . . . . . C68 C 0.2997(6) 0.3077(5) -0.0747(2) 0.032(2) Uani 1 1 d . . . . . H68 H 0.239143 0.297359 -0.078054 0.038 Uiso 1 1 calc R U . . . C69 C 0.3434(7) 0.2888(6) -0.1025(2) 0.041(2) Uani 1 1 d . . . . . H69 H 0.313064 0.266294 -0.124578 0.049 Uiso 1 1 calc R U . . . C70 C 0.4324(6) 0.3028(5) -0.0984(2) 0.036(2) Uani 1 1 d . . . . . H70 H 0.463144 0.288928 -0.117322 0.043 Uiso 1 1 calc R U . . . C71 C 0.4757(6) 0.3373(5) -0.0662(2) 0.0263(18) Uani 1 1 d . . . . . H71 H 0.536187 0.347818 -0.063051 0.032 Uiso 1 1 calc R U . . . C72 C 0.4296(5) 0.3561(5) -0.0385(2) 0.0216(17) Uani 1 1 d . . . . . C73 C 0.5562(5) 0.3991(5) 0.0052(2) 0.0217(17) Uani 1 1 d . . . . . H73 H 0.593249 0.386551 -0.011718 0.026 Uiso 1 1 calc R U . . . C74 C 0.5442(5) 0.4485(4) 0.0672(2) 0.0190(16) Uani 1 1 d . . . . . C75 C 0.5946(5) 0.4280(4) 0.0399(2) 0.0176(16) Uani 1 1 d . . . . . C76 C 0.6854(5) 0.4360(4) 0.0475(2) 0.0208(16) Uani 1 1 d . . . . . H76 H 0.717654 0.425319 0.028731 0.025 Uiso 1 1 calc R U . . . C77 C 0.7298(5) 0.4591(5) 0.0816(2) 0.0224(17) Uani 1 1 d . . . . . C78 C 0.6811(5) 0.4735(5) 0.1086(2) 0.0221(17) Uani 1 1 d . . . . . H78 H 0.710151 0.489058 0.132096 0.026 Uiso 1 1 calc R U . . . C79 C 0.5894(5) 0.4659(5) 0.1025(2) 0.0198(17) Uani 1 1 d . . . . . C80 C 0.8263(5) 0.4706(6) 0.0885(2) 0.032(2) Uani 1 1 d . . . . . H80A H 0.839991 0.530104 0.087411 0.049 Uiso 1 1 calc R U . . . H80B H 0.851351 0.440536 0.069935 0.049 Uiso 1 1 calc R U . . . H80C H 0.850628 0.448667 0.112523 0.049 Uiso 1 1 calc R U . . . C81 C 0.5493(5) 0.4742(5) 0.1345(2) 0.0227(17) Uani 1 1 d . . . . . H81 H 0.586016 0.485965 0.156881 0.027 Uiso 1 1 calc R U . . . C82 C 0.4419(5) 0.4646(5) 0.1703(2) 0.0207(17) Uani 1 1 d . . . . . C83 C 0.4231(5) 0.3862(5) 0.1829(2) 0.0268(19) Uani 1 1 d . . . . . H83 H 0.429012 0.337943 0.168750 0.032 Uiso 1 1 calc R U . . . C84 C 0.3956(5) 0.3786(6) 0.2163(2) 0.031(2) Uani 1 1 d . . . . . H84 H 0.385038 0.325007 0.225506 0.037 Uiso 1 1 calc R U . . . C85 C 0.3838(5) 0.4494(6) 0.2360(2) 0.032(2) Uani 1 1 d . . . . . H85 H 0.363246 0.444847 0.258334 0.038 Uiso 1 1 calc R U . . . C86 C 0.4020(5) 0.5264(6) 0.2229(2) 0.0281(19) Uani 1 1 d . . . . . H86 H 0.394234 0.574619 0.236788 0.034 Uiso 1 1 calc R U . . . C87 C 0.4313(5) 0.5359(5) 0.1902(2) 0.0251(18) Uani 1 1 d . . . . . C88 C 0.4472(5) 0.6230(5) 0.1769(2) 0.0261(18) Uani 1 1 d . . . . . H88A H 0.493451 0.620553 0.161938 0.031 Uiso 1 1 calc R U . . . H88B H 0.467994 0.659096 0.198127 0.031 Uiso 1 1 calc R U . . . C89 C 0.3651(6) 0.6629(5) 0.1542(2) 0.0275(19) Uani 1 1 d . . . . . H89A H 0.382158 0.714675 0.142902 0.033 Uiso 1 1 calc R U . . . H89B H 0.341286 0.624019 0.134454 0.033 Uiso 1 1 calc R U . . . C90 C 0.2946(5) 0.6835(5) 0.1756(2) 0.0258(18) Uani 1 1 d . . . . . C91 C 0.2974(6) 0.7612(5) 0.1943(2) 0.031(2) Uani 1 1 d . . . . . H91 H 0.344804 0.797959 0.193801 0.038 Uiso 1 1 calc R U . . . C92 C 0.2324(7) 0.7841(6) 0.2130(3) 0.041(2) Uani 1 1 d . . . . . H92 H 0.234396 0.837074 0.224443 0.049 Uiso 1 1 calc R U . . . C93 C 0.1648(6) 0.7309(6) 0.2151(3) 0.042(2) Uani 1 1 d . . . . . H93 H 0.120914 0.746708 0.228380 0.050 Uiso 1 1 calc R U . . . C94 C 0.1607(5) 0.6551(5) 0.1981(2) 0.0280(19) Uani 1 1 d . . . . . H94 H 0.113122 0.618846 0.199086 0.034 Uiso 1 1 calc R U . . . C95 C 0.2259(5) 0.6312(5) 0.1795(2) 0.0262(18) Uani 1 1 d . . . . . C96 C 0.1920(5) 0.4855(5) 0.1791(2) 0.0240(18) Uani 1 1 d . . . . . H96 H 0.166571 0.494629 0.200030 0.029 Uiso 1 1 calc R U . . . N9 N 0.4330(7) 0.8391(8) 0.5536(4) 0.097(4) Uani 1 1 d . . . . . C101 C 0.4882(8) 0.8786(9) 0.5685(3) 0.065(4) Uani 1 1 d . . . . . C102 C 0.5599(7) 0.9295(8) 0.5851(3) 0.069(4) Uani 1 1 d . . . . . H10A H 0.585362 0.957517 0.566089 0.104 Uiso 1 1 calc R U . . . H10B H 0.603815 0.894344 0.599655 0.104 Uiso 1 1 calc R U . . . H10C H 0.539385 0.971456 0.600663 0.104 Uiso 1 1 calc R U . . . N10 N 0.5553(6) 0.1342(7) -0.0526(3) 0.069(3) Uani 1 1 d . . . . . C103 C 0.4987(7) 0.0925(8) -0.0655(3) 0.052(3) Uani 1 1 d . . . . . C104 C 0.4274(7) 0.0395(8) -0.0818(3) 0.067(3) Uani 1 1 d . . . . . H10D H 0.450326 -0.011870 -0.090659 0.101 Uiso 1 1 calc R U . . . H10E H 0.392051 0.068986 -0.102042 0.101 Uiso 1 1 calc R U . . . H10F H 0.391533 0.025684 -0.063532 0.101 Uiso 1 1 calc R U . . . Br3 Br 0.72429(7) 0.94679(7) 0.28507(3) 0.0364(3) Uani 0.9337(14) 1 d D . P A 1 Br4 Br 0.52637(7) 1.00871(8) 0.32608(3) 0.0474(3) Uani 0.9337(14) 1 d D . P A 1 Br5 Br 0.52085(8) 0.81319(7) 0.26357(4) 0.0501(3) Uani 0.9337(14) 1 d D . P A 1 Fe3 Fe 0.57179(9) 0.94999(8) 0.27506(4) 0.0254(3) Uani 0.9337(14) 1 d D . P A 1 O5 O 0.5328(4) 1.0101(4) 0.23593(17) 0.0441(17) Uani 1 1 d . . . . . Fe4 Fe 0.44400(9) 1.01605(9) 0.19949(4) 0.0322(3) Uani 1 1 d . . . . . Br6 Br 0.31040(7) 0.99942(6) 0.21950(3) 0.0475(3) Uani 1 1 d . . . . . Br7 Br 0.46349(7) 0.90933(7) 0.15779(3) 0.0479(3) Uani 1 1 d . . . . . Br8 Br 0.43746(7) 1.14701(6) 0.17077(3) 0.0471(3) Uani 1 1 d . . . . . Br5A Br 0.5576(13) 0.8421(12) 0.3263(5) 0.065 Uiso 0.0663(14) 1 d . U P A 2 Fe3A Fe 0.5546(13) 0.9724(12) 0.2981(6) 0.028 Uiso 0.0663(14) 1 d . U P A 2 Br4A Br 0.5395(13) 1.0820(12) 0.3403(6) 0.065 Uiso 0.0663(14) 1 d . U P A 2 Br3A Br 0.6863(15) 0.9905(14) 0.2811(6) 0.065 Uiso 0.0663(14) 1 d . U 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 Fe1 0.0182(6) 0.0218(6) 0.0162(6) -0.0005(5) 0.0042(5) -0.0006(5) Br1 0.0287(5) 0.0332(5) 0.0235(4) 0.0087(4) 0.0067(3) 0.0039(4) O1 0.017(3) 0.032(3) 0.020(3) -0.006(2) 0.001(2) 0.000(2) O2 0.022(3) 0.024(3) 0.019(3) 0.002(2) 0.005(2) 0.000(2) N1 0.026(4) 0.021(3) 0.018(3) -0.001(3) 0.010(3) -0.002(3) N2 0.020(3) 0.020(3) 0.018(3) 0.003(3) 0.005(3) 0.003(3) N3 0.020(3) 0.028(4) 0.018(3) -0.005(3) 0.001(3) 0.008(3) N4 0.022(4) 0.019(3) 0.018(3) -0.003(3) 0.006(3) -0.006(3) C1 0.022(4) 0.017(4) 0.019(4) 0.002(3) 0.003(3) -0.003(3) C2 0.021(4) 0.016(4) 0.024(4) 0.004(3) 0.001(3) 0.001(3) C3 0.022(4) 0.019(4) 0.029(5) -0.001(3) 0.008(3) -0.003(3) C4 0.023(4) 0.016(4) 0.023(4) 0.002(3) 0.003(3) -0.004(3) C5 0.018(4) 0.019(4) 0.017(4) -0.001(3) 0.001(3) -0.003(3) C6 0.021(4) 0.022(4) 0.012(4) 0.002(3) -0.001(3) 0.001(3) C7 0.017(4) 0.033(5) 0.022(4) 0.002(3) -0.002(3) -0.009(3) C8 0.031(5) 0.020(4) 0.017(4) 0.002(3) 0.001(3) -0.001(3) C9 0.017(4) 0.034(5) 0.017(4) 0.000(3) -0.004(3) 0.007(3) C10 0.025(4) 0.038(5) 0.019(4) 0.016(4) 0.004(3) 0.011(4) C11 0.033(5) 0.072(7) 0.022(5) 0.017(5) 0.002(4) 0.016(5) C12 0.023(5) 0.092(9) 0.025(5) 0.002(5) -0.001(4) 0.017(5) C13 0.021(5) 0.072(7) 0.019(5) -0.012(5) -0.009(4) 0.014(5) C14 0.025(4) 0.049(6) 0.017(4) -0.008(4) -0.004(3) 0.007(4) C15 0.028(5) 0.038(5) 0.036(5) -0.014(4) -0.005(4) -0.006(4) C16 0.043(5) 0.021(4) 0.035(5) -0.007(4) 0.015(4) -0.015(4) C17 0.034(5) 0.020(4) 0.026(5) -0.001(3) 0.003(4) 0.004(4) C18 0.049(6) 0.022(5) 0.033(5) 0.002(4) -0.002(4) 0.002(4) C19 0.065(7) 0.016(5) 0.041(6) -0.005(4) 0.000(5) 0.006(4) C20 0.050(6) 0.032(5) 0.020(5) -0.001(4) 0.012(4) 0.014(4) C21 0.043(5) 0.023(5) 0.018(4) 0.004(3) 0.005(4) 0.007(4) C22 0.033(5) 0.020(4) 0.013(4) 0.001(3) -0.002(3) 0.006(3) C23 0.018(4) 0.031(5) 0.025(4) 0.002(4) 0.002(3) 0.007(3) C24 0.018(4) 0.022(4) 0.021(4) 0.003(3) -0.001(3) -0.001(3) C25 0.021(4) 0.019(4) 0.026(4) 0.002(3) 0.003(3) -0.001(3) C26 0.017(4) 0.027(5) 0.021(4) 0.010(3) 0.002(3) 0.002(3) C27 0.017(4) 0.037(5) 0.028(5) 0.015(4) 0.003(3) -0.005(4) C28 0.028(5) 0.018(4) 0.034(5) 0.006(4) 0.002(4) -0.005(3) C29 0.026(4) 0.018(4) 0.015(4) 0.002(3) 0.002(3) -0.004(3) C30 0.029(5) 0.038(5) 0.033(5) 0.010(4) 0.010(4) -0.005(4) C31 0.019(4) 0.025(4) 0.024(4) 0.002(3) -0.001(3) 0.003(3) C32 0.031(5) 0.019(4) 0.020(4) 0.001(3) 0.008(3) -0.002(3) C33 0.030(5) 0.036(5) 0.029(5) -0.009(4) 0.009(4) 0.006(4) C34 0.032(5) 0.045(6) 0.044(6) -0.005(5) 0.003(4) 0.012(4) C35 0.053(6) 0.026(5) 0.040(6) -0.005(4) 0.021(5) 0.002(4) C36 0.036(5) 0.029(5) 0.022(5) -0.002(4) 0.007(4) 0.001(4) C37 0.030(5) 0.027(5) 0.021(4) -0.002(3) 0.008(4) -0.002(4) C38 0.024(4) 0.030(5) 0.024(5) -0.004(3) 0.001(3) -0.009(4) C39 0.026(4) 0.030(5) 0.020(4) -0.008(3) -0.004(3) -0.002(4) C40 0.035(5) 0.017(4) 0.019(4) 0.004(3) -0.002(3) -0.002(4) C41 0.038(5) 0.036(5) 0.019(4) -0.001(4) -0.001(4) -0.005(4) C42 0.053(6) 0.041(6) 0.030(5) 0.000(4) -0.005(5) -0.026(5) C43 0.069(7) 0.035(5) 0.015(4) -0.008(4) 0.008(4) -0.008(5) C44 0.033(5) 0.024(4) 0.027(5) 0.002(3) 0.007(4) -0.009(4) C45 0.030(5) 0.020(4) 0.017(4) 0.000(3) 0.000(3) 0.000(3) C46 0.033(5) 0.017(4) 0.020(4) 0.001(3) 0.009(3) 0.002(3) Fe2 0.0175(6) 0.0188(6) 0.0151(6) -0.0011(5) 0.0017(5) -0.0005(5) Br2 0.0282(5) 0.0319(5) 0.0227(4) 0.0075(4) 0.0057(3) 0.0051(4) N5 0.019(3) 0.027(4) 0.015(3) -0.002(3) 0.007(3) 0.002(3) N6 0.021(3) 0.015(3) 0.017(3) 0.000(3) -0.001(3) 0.000(3) N7 0.025(4) 0.016(3) 0.014(3) 0.001(2) 0.003(3) 0.000(3) N8 0.018(3) 0.016(3) 0.018(3) -0.008(3) 0.002(2) 0.001(3) O3 0.026(3) 0.021(3) 0.019(3) 0.001(2) 0.007(2) 0.002(2) O4 0.021(3) 0.026(3) 0.018(3) -0.002(2) 0.001(2) -0.001(2) C51 0.017(4) 0.024(4) 0.020(4) 0.004(3) 0.001(3) 0.001(3) C52 0.017(4) 0.030(5) 0.020(4) 0.001(3) 0.007(3) 0.004(3) C53 0.012(4) 0.031(5) 0.031(5) 0.002(4) 0.006(3) -0.002(3) C54 0.022(4) 0.023(4) 0.029(5) 0.006(3) 0.008(3) -0.002(3) C55 0.022(4) 0.018(4) 0.038(5) -0.006(4) 0.004(4) -0.004(3) C56 0.023(4) 0.016(4) 0.018(4) -0.002(3) -0.001(3) 0.002(3) C57 0.039(5) 0.028(5) 0.045(6) 0.004(4) 0.014(4) 0.001(4) C58 0.025(4) 0.023(4) 0.021(4) -0.004(3) 0.001(3) 0.003(3) C59 0.028(5) 0.021(4) 0.025(4) -0.001(3) 0.010(4) 0.006(3) C60 0.040(5) 0.029(5) 0.020(4) 0.001(3) 0.010(4) 0.012(4) C61 0.036(5) 0.057(6) 0.027(5) -0.004(4) 0.008(4) 0.016(5) C62 0.041(6) 0.043(6) 0.039(6) 0.000(4) 0.018(5) 0.010(4) C63 0.049(6) 0.028(5) 0.029(5) -0.004(4) 0.016(4) -0.005(4) C64 0.031(5) 0.015(4) 0.027(5) -0.005(3) 0.007(4) 0.001(3) C65 0.033(5) 0.032(5) 0.018(4) -0.010(3) 0.005(4) -0.013(4) C66 0.031(5) 0.031(5) 0.019(4) -0.002(3) 0.000(3) -0.004(4) C67 0.033(5) 0.021(4) 0.029(5) -0.001(3) 0.002(4) -0.008(4) C68 0.031(5) 0.037(5) 0.023(5) -0.008(4) -0.006(4) -0.012(4) C69 0.061(7) 0.041(6) 0.017(5) -0.015(4) -0.003(4) -0.021(5) C70 0.059(6) 0.032(5) 0.018(4) -0.001(4) 0.014(4) -0.009(4) C71 0.033(5) 0.024(4) 0.022(4) -0.002(3) 0.004(4) -0.010(4) C72 0.034(5) 0.018(4) 0.013(4) -0.007(3) 0.003(3) -0.005(3) C73 0.025(4) 0.021(4) 0.020(4) -0.005(3) 0.006(3) 0.001(3) C74 0.020(4) 0.016(4) 0.018(4) 0.008(3) -0.003(3) -0.003(3) C75 0.019(4) 0.012(4) 0.022(4) 0.004(3) 0.003(3) -0.001(3) C76 0.024(4) 0.019(4) 0.020(4) 0.002(3) 0.006(3) 0.002(3) C77 0.019(4) 0.026(4) 0.021(4) 0.004(3) -0.001(3) -0.005(3) C78 0.021(4) 0.026(4) 0.017(4) 0.004(3) -0.002(3) -0.002(3) C79 0.013(4) 0.025(4) 0.020(4) 0.000(3) 0.000(3) -0.004(3) C80 0.024(5) 0.045(5) 0.028(5) -0.002(4) 0.005(4) -0.005(4) C81 0.025(4) 0.022(4) 0.021(4) -0.003(3) 0.005(3) -0.002(3) C82 0.015(4) 0.036(5) 0.012(4) -0.003(3) 0.004(3) -0.002(3) C83 0.019(4) 0.034(5) 0.026(5) 0.002(4) 0.001(3) -0.004(4) C84 0.023(4) 0.047(6) 0.023(5) 0.021(4) 0.002(4) 0.004(4) C85 0.020(4) 0.055(6) 0.020(4) 0.005(4) 0.004(3) 0.004(4) C86 0.020(4) 0.043(5) 0.019(4) -0.004(4) -0.001(3) 0.007(4) C87 0.021(4) 0.034(5) 0.019(4) -0.008(3) 0.001(3) 0.002(3) C88 0.025(4) 0.028(5) 0.024(4) -0.007(3) -0.002(3) -0.003(3) C89 0.044(5) 0.023(4) 0.015(4) -0.004(3) 0.004(4) -0.005(4) C90 0.039(5) 0.021(4) 0.013(4) 0.002(3) -0.007(3) 0.007(4) C91 0.041(5) 0.017(4) 0.031(5) 0.001(4) -0.009(4) -0.001(4) C92 0.054(6) 0.028(5) 0.037(6) -0.017(4) 0.000(5) 0.010(5) C93 0.039(6) 0.042(6) 0.041(6) -0.017(5) -0.001(4) 0.003(5) C94 0.028(5) 0.016(4) 0.037(5) -0.008(4) -0.003(4) 0.011(3) C95 0.025(4) 0.032(5) 0.019(4) -0.001(3) -0.002(3) -0.001(4) C96 0.016(4) 0.026(5) 0.031(5) -0.005(4) 0.008(3) -0.001(3) N9 0.039(6) 0.122(11) 0.124(11) -0.030(8) -0.007(7) 0.029(7) C101 0.037(7) 0.093(10) 0.059(8) -0.005(7) -0.007(6) 0.032(7) C102 0.036(6) 0.106(10) 0.069(9) -0.025(7) 0.016(6) -0.003(6) N10 0.036(6) 0.111(9) 0.059(7) -0.030(6) 0.008(5) 0.016(6) C103 0.033(6) 0.095(9) 0.029(6) -0.007(6) 0.006(5) 0.027(6) C104 0.044(7) 0.089(9) 0.070(9) -0.007(7) 0.014(6) -0.001(6) Br3 0.0302(5) 0.0410(6) 0.0378(6) 0.0035(5) 0.0058(4) 0.0042(5) Br4 0.0351(6) 0.0716(8) 0.0349(6) -0.0091(6) 0.0047(5) 0.0071(5) Br5 0.0505(7) 0.0351(6) 0.0724(9) -0.0067(6) 0.0323(6) -0.0078(5) Fe3 0.0243(7) 0.0273(8) 0.0247(8) 0.0018(6) 0.0046(6) 0.0012(6) O5 0.040(4) 0.043(4) 0.046(4) 0.012(3) -0.004(3) -0.012(3) Fe4 0.0272(8) 0.0366(8) 0.0308(8) 0.0053(6) -0.0009(6) -0.0026(6) Br6 0.0489(6) 0.0463(6) 0.0526(7) -0.0038(5) 0.0235(5) -0.0075(5) Br7 0.0524(7) 0.0554(7) 0.0381(6) 0.0032(5) 0.0145(5) 0.0102(5) Br8 0.0422(6) 0.0435(6) 0.0507(7) 0.0136(5) -0.0056(5) -0.0055(5) 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' Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 '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' 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 O1 Fe1 Br1 92.47(15) . . ? O1 Fe1 O2 176.9(2) . . ? O1 Fe1 N1 85.9(2) . . ? O1 Fe1 N3 92.7(2) . . ? O2 Fe1 Br1 87.75(15) . . ? O2 Fe1 N1 96.6(2) . . ? O2 Fe1 N3 85.0(2) . . ? N1 Fe1 Br1 120.22(17) . . ? N1 Fe1 N3 103.8(2) . . ? N3 Fe1 Br1 135.91(17) . . ? C1 O1 Fe1 134.2(5) . . ? C24 O2 Fe1 132.3(5) . . ? C8 N1 Fe1 126.6(5) . . ? C8 N1 C9 118.1(7) . . ? C9 N1 Fe1 115.3(5) . . ? C22 N2 H2 117.3 . . ? C23 N2 H2 117.3 . . ? C23 N2 C22 125.3(7) . . ? C31 N3 Fe1 127.6(5) . . ? C31 N3 C32 114.0(6) . . ? C32 N3 Fe1 118.3(5) . . ? C45 N4 H4 115.9 . . ? C46 N4 H4 115.9 . . ? C46 N4 C45 128.2(7) . . ? O1 C1 C2 119.7(7) . . ? O1 C1 C6 122.2(7) . . ? C2 C1 C6 118.1(7) . . ? C3 C2 C1 119.6(7) . . ? C46 C2 C1 121.8(7) . . ? C46 C2 C3 118.6(7) . . ? C2 C3 H3 118.5 . . ? C4 C3 C2 122.9(7) . . ? C4 C3 H3 118.5 . . ? C3 C4 C5 116.7(7) . . ? C3 C4 C7 122.0(7) . . ? C5 C4 C7 121.3(7) . . ? C4 C5 H5 118.3 . . ? C4 C5 C6 123.5(7) . . ? C6 C5 H5 118.3 . . ? C1 C6 C8 123.4(7) . . ? C5 C6 C1 119.0(7) . . ? C5 C6 C8 117.6(7) . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 C6 127.1(7) . . ? N1 C8 H8 116.5 . . ? C6 C8 H8 116.5 . . ? C10 C9 N1 117.2(7) . . ? C10 C9 C14 120.7(8) . . ? C14 C9 N1 122.1(7) . . ? C9 C10 H10 119.5 . . ? C11 C10 C9 121.1(9) . . ? C11 C10 H10 119.5 . . ? C10 C11 H11 120.4 . . ? C10 C11 C12 119.1(10) . . ? C12 C11 H11 120.4 . . ? C11 C12 H12 119.8 . . ? C13 C12 C11 120.4(9) . . ? C13 C12 H12 119.8 . . ? C12 C13 H13 119.3 . . ? C12 C13 C14 121.4(9) . . ? C14 C13 H13 119.3 . . ? C9 C14 C13 117.2(9) . . ? C9 C14 C15 122.8(8) . . ? C13 C14 C15 119.9(8) . . ? C14 C15 H15A 109.1 . . ? C14 C15 H15B 109.1 . . ? C14 C15 C16 112.6(7) . . ? H15A C15 H15B 107.8 . . ? C16 C15 H15A 109.1 . . ? C16 C15 H15B 109.1 . . ? C15 C16 H16A 108.5 . . ? C15 C16 H16B 108.5 . . ? H16A C16 H16B 107.5 . . ? C17 C16 C15 115.2(7) . . ? C17 C16 H16A 108.5 . . ? C17 C16 H16B 108.5 . . ? C18 C17 C16 118.0(8) . . ? C22 C17 C16 124.6(7) . . ? C22 C17 C18 117.4(8) . . ? C17 C18 H18 119.4 . . ? C19 C18 C17 121.1(9) . . ? C19 C18 H18 119.4 . . ? C18 C19 H19 120.1 . . ? C18 C19 C20 119.7(8) . . ? C20 C19 H19 120.1 . . ? C19 C20 H20 119.6 . . ? C21 C20 C19 120.8(8) . . ? C21 C20 H20 119.6 . . ? C20 C21 H21 120.4 . . ? C20 C21 C22 119.1(8) . . ? C22 C21 H21 120.4 . . ? C17 C22 N2 118.9(7) . . ? C17 C22 C21 121.8(7) . . ? C21 C22 N2 119.3(7) . . ? N2 C23 H23 117.8 . . ? N2 C23 C25 124.4(7) . . ? C25 C23 H23 117.8 . . ? O2 C24 C25 119.5(7) . . ? O2 C24 C29 122.9(7) . . ? C29 C24 C25 117.5(7) . . ? C23 C25 C24 120.6(7) . . ? C26 C25 C23 118.1(7) . . ? C26 C25 C24 121.1(7) . . ? C25 C26 H26 119.2 . . ? C27 C26 C25 121.6(7) . . ? C27 C26 H26 119.2 . . ? C26 C27 C30 121.4(7) . . ? C28 C27 C26 117.0(7) . . ? C28 C27 C30 121.7(8) . . ? C27 C28 H28 117.9 . . ? C27 C28 C29 124.3(7) . . ? C29 C28 H28 117.9 . . ? C24 C29 C31 123.9(7) . . ? C28 C29 C24 118.5(7) . . ? C28 C29 C31 117.5(7) . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30B 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N3 C31 C29 125.1(7) . . ? N3 C31 H31 117.5 . . ? C29 C31 H31 117.5 . . ? C33 C32 N3 118.1(7) . . ? C33 C32 C37 120.8(7) . . ? C37 C32 N3 121.1(7) . . ? C32 C33 H33 119.6 . . ? C34 C33 C32 120.8(8) . . ? C34 C33 H33 119.6 . . ? C33 C34 H34 120.2 . . ? C33 C34 C35 119.5(9) . . ? C35 C34 H34 120.2 . . ? C34 C35 H35 120.1 . . ? C36 C35 C34 119.7(8) . . ? C36 C35 H35 120.1 . . ? C35 C36 H36 119.2 . . ? C35 C36 C37 121.5(8) . . ? C37 C36 H36 119.2 . . ? C32 C37 C36 117.6(8) . . ? C32 C37 C38 122.9(7) . . ? C36 C37 C38 119.5(7) . . ? C37 C38 H38A 108.8 . . ? C37 C38 H38B 108.8 . . ? C37 C38 C39 113.6(6) . . ? H38A C38 H38B 107.7 . . ? C39 C38 H38A 108.8 . . ? C39 C38 H38B 108.8 . . ? C38 C39 H39A 109.0 . . ? C38 C39 H39B 109.0 . . ? H39A C39 H39B 107.8 . . ? C40 C39 C38 113.0(7) . . ? C40 C39 H39A 109.0 . . ? C40 C39 H39B 109.0 . . ? C41 C40 C39 117.3(7) . . ? C41 C40 C45 117.7(8) . . ? C45 C40 C39 125.0(7) . . ? C40 C41 H41 119.6 . . ? C40 C41 C42 120.9(9) . . ? C42 C41 H41 119.6 . . ? C41 C42 H42 119.8 . . ? C43 C42 C41 120.5(8) . . ? C43 C42 H42 119.8 . . ? C42 C43 H43 120.0 . . ? C42 C43 C44 120.1(9) . . ? C44 C43 H43 120.0 . . ? C43 C44 H44 120.5 . . ? C45 C44 C43 119.0(8) . . ? C45 C44 H44 120.5 . . ? C40 C45 N4 117.3(7) . . ? C44 C45 N4 120.9(7) . . ? C44 C45 C40 121.8(7) . . ? N4 C46 C2 122.6(7) . . ? N4 C46 H46 118.7 . . ? C2 C46 H46 118.7 . . ? N5 Fe2 Br2 134.88(17) . . ? N7 Fe2 Br2 121.98(16) . . ? N7 Fe2 N5 103.1(2) . . ? O3 Fe2 Br2 87.37(15) . . ? O3 Fe2 N5 84.9(2) . . ? O3 Fe2 N7 96.4(2) . . ? O4 Fe2 Br2 93.50(15) . . ? O4 Fe2 N5 92.1(2) . . ? O4 Fe2 N7 86.0(2) . . ? O4 Fe2 O3 176.5(2) . . ? C58 N5 Fe2 127.1(5) . . ? C58 N5 C59 114.0(6) . . ? C59 N5 Fe2 118.8(5) . . ? C72 N6 H6 116.1 . . ? C73 N6 H6 116.1 . . ? C73 N6 C72 127.8(7) . . ? C81 N7 Fe2 128.0(5) . . ? C81 N7 C82 115.2(6) . . ? C82 N7 Fe2 116.6(5) . . ? C95 N8 H8A 118.2 . . ? C96 N8 H8A 118.2 . . ? C96 N8 C95 123.7(7) . . ? C51 O3 Fe2 131.4(5) . . ? C74 O4 Fe2 132.7(5) . . ? O3 C51 C52 119.4(7) . . ? O3 C51 C56 122.6(7) . . ? C56 C51 C52 117.9(7) . . ? C53 C52 C51 120.0(7) . . ? C53 C52 C96 118.6(7) . . ? C96 C52 C51 120.8(7) . . ? C52 C53 H53 118.5 . . ? C54 C53 C52 123.0(7) . . ? C54 C53 H53 118.5 . . ? C53 C54 C55 116.8(7) . . ? C53 C54 C57 123.0(7) . . ? C55 C54 C57 120.1(7) . . ? C54 C55 H55 118.1 . . ? C54 C55 C56 123.8(7) . . ? C56 C55 H55 118.1 . . ? C51 C56 C58 123.7(7) . . ? C55 C56 C51 118.4(7) . . ? C55 C56 C58 117.6(7) . . ? C54 C57 H57A 109.5 . . ? C54 C57 H57B 109.5 . . ? C54 C57 H57C 109.5 . . ? H57A C57 H57B 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? N5 C58 C56 126.5(7) . . ? N5 C58 H58 116.7 . . ? C56 C58 H58 116.7 . . ? C60 C59 N5 117.9(7) . . ? C60 C59 C64 120.8(7) . . ? C64 C59 N5 121.3(7) . . ? C59 C60 H60 119.5 . . ? C59 C60 C61 121.0(8) . . ? C61 C60 H60 119.5 . . ? C60 C61 H61 120.5 . . ? C60 C61 C62 119.0(9) . . ? C62 C61 H61 120.5 . . ? C61 C62 H62 120.1 . . ? C63 C62 C61 119.8(8) . . ? C63 C62 H62 120.1 . . ? C62 C63 H63 119.1 . . ? C62 C63 C64 121.7(8) . . ? C64 C63 H63 119.1 . . ? C59 C64 C65 122.1(7) . . ? C63 C64 C59 117.5(8) . . ? C63 C64 C65 120.4(7) . . ? C64 C65 H65A 109.1 . . ? C64 C65 H65B 109.1 . . ? C64 C65 C66 112.6(6) . . ? H65A C65 H65B 107.8 . . ? C66 C65 H65A 109.1 . . ? C66 C65 H65B 109.1 . . ? C65 C66 H66A 109.2 . . ? C65 C66 H66B 109.2 . . ? H66A C66 H66B 107.9 . . ? C67 C66 C65 111.9(7) . . ? C67 C66 H66A 109.2 . . ? C67 C66 H66B 109.2 . . ? C68 C67 C66 119.1(8) . . ? C72 C67 C66 124.5(7) . . ? C72 C67 C68 116.3(8) . . ? C67 C68 H68 118.7 . . ? C69 C68 C67 122.6(8) . . ? C69 C68 H68 118.7 . . ? C68 C69 H69 120.0 . . ? C68 C69 C70 119.9(8) . . ? C70 C69 H69 120.0 . . ? C69 C70 H70 120.3 . . ? C71 C70 C69 119.3(8) . . ? C71 C70 H70 120.3 . . ? C70 C71 H71 120.3 . . ? C70 C71 C72 119.4(8) . . ? C72 C71 H71 120.3 . . ? C67 C72 N6 117.5(7) . . ? C71 C72 N6 120.1(7) . . ? C71 C72 C67 122.4(7) . . ? N6 C73 H73 118.0 . . ? N6 C73 C75 123.9(7) . . ? C75 C73 H73 118.0 . . ? O4 C74 C75 119.2(6) . . ? O4 C74 C79 123.2(7) . . ? C79 C74 C75 117.5(7) . . ? C73 C75 C74 122.1(7) . . ? C76 C75 C73 118.1(7) . . ? C76 C75 C74 119.8(7) . . ? C75 C76 H76 118.8 . . ? C77 C76 C75 122.5(7) . . ? C77 C76 H76 118.8 . . ? C76 C77 C80 121.2(7) . . ? C78 C77 C76 117.4(7) . . ? C78 C77 C80 121.4(7) . . ? C77 C78 H78 118.8 . . ? C77 C78 C79 122.5(7) . . ? C79 C78 H78 118.8 . . ? C74 C79 C78 119.8(7) . . ? C74 C79 C81 124.8(7) . . ? C78 C79 C81 115.4(7) . . ? C77 C80 H80A 109.5 . . ? C77 C80 H80B 109.5 . . ? C77 C80 H80C 109.5 . . ? H80A C80 H80B 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? N7 C81 C79 124.6(7) . . ? N7 C81 H81 117.7 . . ? C79 C81 H81 117.7 . . ? C83 C82 N7 115.8(7) . . ? C87 C82 N7 123.3(7) . . ? C87 C82 C83 120.7(7) . . ? C82 C83 H83 120.1 . . ? C82 C83 C84 119.8(8) . . ? C84 C83 H83 120.1 . . ? C83 C84 H84 120.2 . . ? C85 C84 C83 119.6(8) . . ? C85 C84 H84 120.2 . . ? C84 C85 H85 120.2 . . ? C86 C85 C84 119.7(8) . . ? C86 C85 H85 120.2 . . ? C85 C86 H86 119.0 . . ? C85 C86 C87 122.1(8) . . ? C87 C86 H86 119.0 . . ? C82 C87 C88 122.7(7) . . ? C86 C87 C82 118.1(8) . . ? C86 C87 C88 119.2(7) . . ? C87 C88 H88A 109.0 . . ? C87 C88 H88B 109.0 . . ? C87 C88 C89 113.0(6) . . ? H88A C88 H88B 107.8 . . ? C89 C88 H88A 109.0 . . ? C89 C88 H88B 109.0 . . ? C88 C89 H89A 108.6 . . ? C88 C89 H89B 108.6 . . ? H89A C89 H89B 107.6 . . ? C90 C89 C88 114.5(6) . . ? C90 C89 H89A 108.6 . . ? C90 C89 H89B 108.6 . . ? C91 C90 C89 119.2(8) . . ? C95 C90 C89 124.9(7) . . ? C95 C90 C91 115.8(8) . . ? C90 C91 H91 119.4 . . ? C92 C91 C90 121.1(8) . . ? C92 C91 H91 119.4 . . ? C91 C92 H92 119.7 . . ? C93 C92 C91 120.5(8) . . ? C93 C92 H92 119.7 . . ? C92 C93 H93 119.9 . . ? C94 C93 C92 120.1(9) . . ? C94 C93 H93 119.9 . . ? C93 C94 H94 120.0 . . ? C93 C94 C95 119.9(8) . . ? C95 C94 H94 120.0 . . ? C90 C95 N8 119.9(7) . . ? C94 C95 N8 117.8(7) . . ? C94 C95 C90 122.3(8) . . ? N8 C96 C52 124.6(7) . . ? N8 C96 H96 117.7 . . ? C52 C96 H96 117.7 . . ? N9 C101 C102 176.1(15) . . ? C101 C102 H10A 109.5 . . ? C101 C102 H10B 109.5 . . ? C101 C102 H10C 109.5 . . ? H10A C102 H10B 109.5 . . ? H10A C102 H10C 109.5 . . ? H10B C102 H10C 109.5 . . ? N10 C103 C104 179.8(16) . . ? C103 C104 H10D 109.5 . . ? C103 C104 H10E 109.5 . . ? C103 C104 H10F 109.5 . . ? H10D C104 H10E 109.5 . . ? H10D C104 H10F 109.5 . . ? H10E C104 H10F 109.5 . . ? Br4 Fe3 Br3 108.69(7) . . ? Br4 Fe3 Br5 112.51(7) . . ? Br5 Fe3 Br3 108.20(7) . . ? O5 Fe3 Br3 109.8(2) . . ? O5 Fe3 Br4 110.1(2) . . ? O5 Fe3 Br5 107.4(2) . . ? Fe3 O5 Fe4 141.0(4) . . ? Fe4 O5 Fe3A 136.8(6) . . ? O5 Fe4 Br6 111.8(2) . . ? O5 Fe4 Br7 107.1(2) . . ? O5 Fe4 Br8 111.4(2) . . ? Br6 Fe4 Br7 110.45(7) . . ? Br8 Fe4 Br6 105.95(7) . . ? Br8 Fe4 Br7 110.13(7) . . ? O5 Fe3A Br4A 116.4(10) . . ? Br5A Fe3A O5 131.2(11) . . ? Br5A Fe3A Br4A 110.7(11) . . ? Br3A Fe3A O5 71.2(8) . . ? Br3A Fe3A Br5A 106.9(11) . . ? Br3A Fe3A Br4A 106.6(11) . . ? 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 Fe1 Br1 2.5078(14) . ? Fe1 O1 2.003(5) . ? Fe1 O2 2.018(5) . ? Fe1 N1 2.134(7) . ? Fe1 N3 2.140(7) . ? O1 C1 1.321(9) . ? O2 C24 1.308(9) . ? N1 C8 1.293(10) . ? N1 C9 1.438(9) . ? N2 H2 0.8800 . ? N2 C22 1.436(9) . ? N2 C23 1.298(10) . ? N3 C31 1.307(10) . ? N3 C32 1.448(9) . ? N4 H4 0.8800 . ? N4 C45 1.414(9) . ? N4 C46 1.306(9) . ? C1 C2 1.423(10) . ? C1 C6 1.424(10) . ? C2 C3 1.414(10) . ? C2 C46 1.413(10) . ? C3 H3 0.9500 . ? C3 C4 1.380(10) . ? C4 C5 1.400(10) . ? C4 C7 1.489(10) . ? C5 H5 0.9500 . ? C5 C6 1.405(10) . ? C6 C8 1.445(10) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8 0.9500 . ? C9 C10 1.393(11) . ? C9 C14 1.402(11) . ? C10 H10 0.9500 . ? C10 C11 1.368(11) . ? C11 H11 0.9500 . ? C11 C12 1.391(14) . ? C12 H12 0.9500 . ? C12 C13 1.380(14) . ? C13 H13 0.9500 . ? C13 C14 1.402(12) . ? C14 C15 1.493(13) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C15 C16 1.565(12) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C16 C17 1.494(11) . ? C17 C18 1.397(11) . ? C17 C22 1.384(11) . ? C18 H18 0.9500 . ? C18 C19 1.376(13) . ? C19 H19 0.9500 . ? C19 C20 1.388(13) . ? C20 H20 0.9500 . ? C20 C21 1.354(11) . ? C21 H21 0.9500 . ? C21 C22 1.401(11) . ? C23 H23 0.9500 . ? C23 C25 1.419(11) . ? C24 C25 1.427(10) . ? C24 C29 1.414(10) . ? C25 C26 1.402(10) . ? C26 H26 0.9500 . ? C26 C27 1.386(11) . ? C27 C28 1.381(11) . ? C27 C30 1.505(10) . ? C28 H28 0.9500 . ? C28 C29 1.411(10) . ? C29 C31 1.449(10) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31 0.9500 . ? C32 C33 1.378(11) . ? C32 C37 1.392(11) . ? C33 H33 0.9500 . ? C33 C34 1.371(11) . ? C34 H34 0.9500 . ? C34 C35 1.383(13) . ? C35 H35 0.9500 . ? C35 C36 1.379(12) . ? C36 H36 0.9500 . ? C36 C37 1.394(11) . ? C37 C38 1.510(11) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C38 C39 1.559(11) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C39 C40 1.490(11) . ? C40 C41 1.399(11) . ? C40 C45 1.402(11) . ? C41 H41 0.9500 . ? C41 C42 1.400(13) . ? C42 H42 0.9500 . ? C42 C43 1.375(14) . ? C43 H43 0.9500 . ? C43 C44 1.402(11) . ? C44 H44 0.9500 . ? C44 C45 1.395(11) . ? C46 H46 0.9500 . ? Fe2 Br2 2.5106(14) . ? Fe2 N5 2.151(6) . ? Fe2 N7 2.133(6) . ? Fe2 O3 2.030(5) . ? Fe2 O4 2.023(5) . ? N5 C58 1.278(10) . ? N5 C59 1.446(9) . ? N6 H6 0.8800 . ? N6 C72 1.422(9) . ? N6 C73 1.298(9) . ? N7 C81 1.309(9) . ? N7 C82 1.448(9) . ? N8 H8A 0.8800 . ? N8 C95 1.425(10) . ? N8 C96 1.291(9) . ? O3 C51 1.310(9) . ? O4 C74 1.312(8) . ? C51 C52 1.426(10) . ? C51 C56 1.419(10) . ? C52 C53 1.410(11) . ? C52 C96 1.417(11) . ? C53 H53 0.9500 . ? C53 C54 1.359(11) . ? C54 C55 1.397(11) . ? C54 C57 1.494(11) . ? C55 H55 0.9500 . ? C55 C56 1.411(11) . ? C56 C58 1.435(10) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58 0.9500 . ? C59 C60 1.371(11) . ? C59 C64 1.402(11) . ? C60 H60 0.9500 . ? C60 C61 1.378(11) . ? C61 H61 0.9500 . ? C61 C62 1.400(12) . ? C62 H62 0.9500 . ? C62 C63 1.372(12) . ? C63 H63 0.9500 . ? C63 C64 1.392(11) . ? C64 C65 1.510(11) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C65 C66 1.563(11) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C66 C67 1.491(11) . ? C67 C68 1.399(11) . ? C67 C72 1.394(11) . ? C68 H68 0.9500 . ? C68 C69 1.373(12) . ? C69 H69 0.9500 . ? C69 C70 1.392(13) . ? C70 H70 0.9500 . ? C70 C71 1.391(11) . ? C71 H71 0.9500 . ? C71 C72 1.392(11) . ? C73 H73 0.9500 . ? C73 C75 1.413(10) . ? C74 C75 1.431(10) . ? C74 C79 1.415(10) . ? C75 C76 1.407(10) . ? C76 H76 0.9500 . ? C76 C77 1.394(10) . ? C77 C78 1.384(11) . ? C77 C80 1.501(11) . ? C78 H78 0.9500 . ? C78 C79 1.421(10) . ? C79 C81 1.448(10) . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C81 H81 0.9500 . ? C82 C83 1.392(11) . ? C82 C87 1.388(11) . ? C83 H83 0.9500 . ? C83 C84 1.397(11) . ? C84 H84 0.9500 . ? C84 C85 1.381(12) . ? C85 H85 0.9500 . ? C85 C86 1.375(12) . ? C86 H86 0.9500 . ? C86 C87 1.388(11) . ? C87 C88 1.518(11) . ? C88 H88A 0.9900 . ? C88 H88B 0.9900 . ? C88 C89 1.552(11) . ? C89 H89A 0.9900 . ? C89 H89B 0.9900 . ? C89 C90 1.506(11) . ? C90 C91 1.424(11) . ? C90 C95 1.392(11) . ? C91 H91 0.9500 . ? C91 C92 1.381(13) . ? C92 H92 0.9500 . ? C92 C93 1.371(13) . ? C93 H93 0.9500 . ? C93 C94 1.368(11) . ? C94 H94 0.9500 . ? C94 C95 1.386(11) . ? C96 H96 0.9500 . ? N9 C101 1.137(15) . ? C101 C102 1.440(17) . ? C102 H10A 0.9800 . ? C102 H10B 0.9800 . ? C102 H10C 0.9800 . ? N10 C103 1.149(14) . ? C103 C104 1.451(17) . ? C104 H10D 0.9800 . ? C104 H10E 0.9800 . ? C104 H10F 0.9800 . ? Br3 Fe3 2.3535(17) . ? Br4 Fe3 2.3454(18) . ? Br5 Fe3 2.3481(17) . ? Fe3 O5 1.771(6) . ? O5 Fe4 1.775(6) . ? O5 Fe3A 2.37(2) . ? Fe4 Br6 2.3552(17) . ? Fe4 Br7 2.3702(18) . ? Fe4 Br8 2.3528(17) . ? Br5A Fe3A 2.34(3) . ? Fe3A Br4A 2.40(3) . ? Fe3A Br3A 2.28(3) . ? 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 Fe1 O1 C1 C2 -174.5(5) . . . . ? Fe1 O1 C1 C6 5.8(11) . . . . ? Fe1 O2 C24 C25 -155.2(5) . . . . ? Fe1 O2 C24 C29 20.9(11) . . . . ? Fe1 N1 C8 C6 6.2(11) . . . . ? Fe1 N1 C9 C10 -75.5(7) . . . . ? Fe1 N1 C9 C14 101.9(7) . . . . ? Fe1 N3 C31 C29 0.6(11) . . . . ? Fe1 N3 C32 C33 -86.5(8) . . . . ? Fe1 N3 C32 C37 91.2(8) . . . . ? O1 C1 C2 C3 -176.2(6) . . . . ? O1 C1 C2 C46 4.5(11) . . . . ? O1 C1 C6 C5 174.9(7) . . . . ? O1 C1 C6 C8 -7.8(11) . . . . ? O2 C24 C25 C23 5.7(11) . . . . ? O2 C24 C25 C26 -179.9(7) . . . . ? O2 C24 C29 C28 179.8(7) . . . . ? O2 C24 C29 C31 -3.3(12) . . . . ? N1 C9 C10 C11 176.1(7) . . . . ? N1 C9 C14 C13 -175.9(7) . . . . ? N1 C9 C14 C15 1.5(12) . . . . ? N2 C23 C25 C24 -0.2(12) . . . . ? N2 C23 C25 C26 -174.8(7) . . . . ? N3 C32 C33 C34 179.0(8) . . . . ? N3 C32 C37 C36 -179.6(7) . . . . ? N3 C32 C37 C38 -1.8(11) . . . . ? C1 C2 C3 C4 0.3(11) . . . . ? C1 C2 C46 N4 -2.1(11) . . . . ? C1 C6 C8 N1 1.7(12) . . . . ? C2 C1 C6 C5 -4.8(10) . . . . ? C2 C1 C6 C8 172.4(7) . . . . ? C2 C3 C4 C5 -2.9(11) . . . . ? C2 C3 C4 C7 176.7(7) . . . . ? C3 C2 C46 N4 178.6(7) . . . . ? C3 C4 C5 C6 1.5(11) . . . . ? C4 C5 C6 C1 2.4(11) . . . . ? C4 C5 C6 C8 -175.0(7) . . . . ? C5 C6 C8 N1 179.0(7) . . . . ? C6 C1 C2 C3 3.6(10) . . . . ? C6 C1 C2 C46 -175.8(7) . . . . ? C7 C4 C5 C6 -178.1(7) . . . . ? C8 N1 C9 C10 104.4(8) . . . . ? C8 N1 C9 C14 -78.2(9) . . . . ? C9 N1 C8 C6 -173.7(7) . . . . ? C9 C10 C11 C12 -0.5(13) . . . . ? C9 C14 C15 C16 -88.4(10) . . . . ? C10 C9 C14 C13 1.4(11) . . . . ? C10 C9 C14 C15 178.8(7) . . . . ? C10 C11 C12 C13 2.3(13) . . . . ? C11 C12 C13 C14 -2.2(13) . . . . ? C12 C13 C14 C9 0.3(12) . . . . ? C12 C13 C14 C15 -177.1(8) . . . . ? C13 C14 C15 C16 88.9(9) . . . . ? C14 C9 C10 C11 -1.4(12) . . . . ? C14 C15 C16 C17 -71.5(9) . . . . ? C15 C16 C17 C18 -87.5(9) . . . . ? C15 C16 C17 C22 91.3(10) . . . . ? C16 C17 C18 C19 -178.6(8) . . . . ? C16 C17 C22 N2 -0.5(12) . . . . ? C16 C17 C22 C21 178.2(8) . . . . ? C17 C18 C19 C20 -0.1(14) . . . . ? C18 C17 C22 N2 178.3(7) . . . . ? C18 C17 C22 C21 -2.9(12) . . . . ? C18 C19 C20 C21 -1.9(14) . . . . ? C19 C20 C21 C22 1.5(13) . . . . ? C20 C21 C22 N2 179.7(7) . . . . ? C20 C21 C22 C17 1.0(12) . . . . ? C22 N2 C23 C25 173.0(7) . . . . ? C22 C17 C18 C19 2.5(13) . . . . ? C23 N2 C22 C17 -150.4(8) . . . . ? C23 N2 C22 C21 30.8(11) . . . . ? C23 C25 C26 C27 172.9(7) . . . . ? C24 C25 C26 C27 -1.7(11) . . . . ? C24 C29 C31 N3 -6.9(12) . . . . ? C25 C24 C29 C28 -4.1(11) . . . . ? C25 C24 C29 C31 172.8(7) . . . . ? C25 C26 C27 C28 -0.3(11) . . . . ? C25 C26 C27 C30 179.7(7) . . . . ? C26 C27 C28 C29 -0.1(12) . . . . ? C27 C28 C29 C24 2.4(12) . . . . ? C27 C28 C29 C31 -174.7(8) . . . . ? C28 C29 C31 N3 170.0(7) . . . . ? C29 C24 C25 C23 -170.6(7) . . . . ? C29 C24 C25 C26 3.8(11) . . . . ? C30 C27 C28 C29 180.0(8) . . . . ? C31 N3 C32 C33 89.9(9) . . . . ? C31 N3 C32 C37 -92.4(9) . . . . ? C32 N3 C31 C29 -175.4(7) . . . . ? C32 C33 C34 C35 0.1(14) . . . . ? C32 C37 C38 C39 -93.3(9) . . . . ? C33 C32 C37 C36 -1.9(12) . . . . ? C33 C32 C37 C38 175.8(7) . . . . ? C33 C34 C35 C36 -0.9(14) . . . . ? C34 C35 C36 C37 0.2(13) . . . . ? C35 C36 C37 C32 1.2(12) . . . . ? C35 C36 C37 C38 -176.7(8) . . . . ? C36 C37 C38 C39 84.4(9) . . . . ? C37 C32 C33 C34 1.4(13) . . . . ? C37 C38 C39 C40 -66.5(9) . . . . ? C38 C39 C40 C41 -85.5(9) . . . . ? C38 C39 C40 C45 94.0(9) . . . . ? C39 C40 C41 C42 176.9(8) . . . . ? C39 C40 C45 N4 1.5(11) . . . . ? C39 C40 C45 C44 -178.4(7) . . . . ? C40 C41 C42 C43 2.1(14) . . . . ? C41 C40 C45 N4 -179.1(7) . . . . ? C41 C40 C45 C44 1.0(11) . . . . ? C41 C42 C43 C44 -0.1(14) . . . . ? C42 C43 C44 C45 -1.4(13) . . . . ? C43 C44 C45 N4 -179.0(7) . . . . ? C43 C44 C45 C40 0.9(12) . . . . ? C45 N4 C46 C2 178.8(7) . . . . ? C45 C40 C41 C42 -2.6(12) . . . . ? C46 N4 C45 C40 -173.2(7) . . . . ? C46 N4 C45 C44 6.6(12) . . . . ? C46 C2 C3 C4 179.7(7) . . . . ? Fe2 N5 C58 C56 -3.4(11) . . . . ? Fe2 N5 C59 C60 85.0(8) . . . . ? Fe2 N5 C59 C64 -95.9(8) . . . . ? Fe2 N7 C81 C79 -4.2(11) . . . . ? Fe2 N7 C82 C83 73.8(7) . . . . ? Fe2 N7 C82 C87 -101.7(7) . . . . ? Fe2 O3 C51 C52 153.7(5) . . . . ? Fe2 O3 C51 C56 -23.9(11) . . . . ? Fe2 O4 C74 C75 166.3(5) . . . . ? Fe2 O4 C74 C79 -10.4(11) . . . . ? N5 C59 C60 C61 177.7(8) . . . . ? N5 C59 C64 C63 -175.9(7) . . . . ? N5 C59 C64 C65 5.7(11) . . . . ? N6 C73 C75 C74 0.1(11) . . . . ? N6 C73 C75 C76 179.6(7) . . . . ? N7 C82 C83 C84 -177.3(7) . . . . ? N7 C82 C87 C86 175.6(7) . . . . ? N7 C82 C87 C88 -2.1(12) . . . . ? O3 C51 C52 C53 -179.0(7) . . . . ? O3 C51 C52 C96 -8.3(11) . . . . ? O3 C51 C56 C55 179.3(7) . . . . ? O3 C51 C56 C58 5.9(12) . . . . ? O4 C74 C75 C73 -5.3(10) . . . . ? O4 C74 C75 C76 175.1(6) . . . . ? O4 C74 C79 C78 -174.9(7) . . . . ? O4 C74 C79 C81 7.4(12) . . . . ? C51 C52 C53 C54 -0.1(12) . . . . ? C51 C52 C96 N8 5.1(12) . . . . ? C51 C56 C58 N5 7.6(12) . . . . ? C52 C51 C56 C55 1.7(11) . . . . ? C52 C51 C56 C58 -171.8(7) . . . . ? C52 C53 C54 C55 1.0(12) . . . . ? C52 C53 C54 C57 177.3(8) . . . . ? C53 C52 C96 N8 175.9(7) . . . . ? C53 C54 C55 C56 -0.6(12) . . . . ? C54 C55 C56 C51 -0.8(12) . . . . ? C54 C55 C56 C58 173.0(7) . . . . ? C55 C56 C58 N5 -165.9(8) . . . . ? C56 C51 C52 C53 -1.3(11) . . . . ? C56 C51 C52 C96 169.4(7) . . . . ? C57 C54 C55 C56 -176.9(8) . . . . ? C58 N5 C59 C60 -92.1(9) . . . . ? C58 N5 C59 C64 87.0(9) . . . . ? C59 N5 C58 C56 173.4(7) . . . . ? C59 C60 C61 C62 -0.4(13) . . . . ? C59 C64 C65 C66 92.8(9) . . . . ? C60 C59 C64 C63 3.2(12) . . . . ? C60 C59 C64 C65 -175.3(7) . . . . ? C60 C61 C62 C63 0.4(14) . . . . ? C61 C62 C63 C64 1.5(14) . . . . ? C62 C63 C64 C59 -3.3(12) . . . . ? C62 C63 C64 C65 175.2(8) . . . . ? C63 C64 C65 C66 -85.6(9) . . . . ? C64 C59 C60 C61 -1.4(13) . . . . ? C64 C65 C66 C67 63.8(9) . . . . ? C65 C66 C67 C68 83.4(9) . . . . ? C65 C66 C67 C72 -92.3(9) . . . . ? C66 C67 C68 C69 -175.4(8) . . . . ? C66 C67 C72 N6 -2.8(12) . . . . ? C66 C67 C72 C71 174.9(8) . . . . ? C67 C68 C69 C70 0.4(14) . . . . ? C68 C67 C72 N6 -178.6(7) . . . . ? C68 C67 C72 C71 -0.9(12) . . . . ? C68 C69 C70 C71 -1.2(13) . . . . ? C69 C70 C71 C72 0.8(12) . . . . ? C70 C71 C72 N6 177.9(7) . . . . ? C70 C71 C72 C67 0.2(12) . . . . ? C72 N6 C73 C75 -176.5(7) . . . . ? C72 C67 C68 C69 0.6(13) . . . . ? C73 N6 C72 C67 172.5(7) . . . . ? C73 N6 C72 C71 -5.2(11) . . . . ? C73 C75 C76 C77 -176.0(7) . . . . ? C74 C75 C76 C77 3.6(11) . . . . ? C74 C79 C81 N7 0.0(12) . . . . ? C75 C74 C79 C78 8.3(10) . . . . ? C75 C74 C79 C81 -169.4(7) . . . . ? C75 C76 C77 C78 0.7(11) . . . . ? C75 C76 C77 C80 -177.4(7) . . . . ? C76 C77 C78 C79 -0.3(11) . . . . ? C77 C78 C79 C74 -4.3(11) . . . . ? C77 C78 C79 C81 173.6(7) . . . . ? C78 C79 C81 N7 -177.8(7) . . . . ? C79 C74 C75 C73 171.6(7) . . . . ? C79 C74 C75 C76 -8.0(10) . . . . ? C80 C77 C78 C79 177.8(7) . . . . ? C81 N7 C82 C83 -101.9(8) . . . . ? C81 N7 C82 C87 82.6(9) . . . . ? C82 N7 C81 C79 170.9(7) . . . . ? C82 C83 C84 C85 2.7(12) . . . . ? C82 C87 C88 C89 89.9(9) . . . . ? C83 C82 C87 C86 0.3(11) . . . . ? C83 C82 C87 C88 -177.3(7) . . . . ? C83 C84 C85 C86 -2.1(12) . . . . ? C84 C85 C86 C87 0.7(12) . . . . ? C85 C86 C87 C82 0.2(12) . . . . ? C85 C86 C87 C88 178.0(7) . . . . ? C86 C87 C88 C89 -87.8(9) . . . . ? C87 C82 C83 C84 -1.8(12) . . . . ? C87 C88 C89 C90 68.3(9) . . . . ? C88 C89 C90 C91 85.5(9) . . . . ? C88 C89 C90 C95 -93.1(9) . . . . ? C89 C90 C91 C92 177.4(8) . . . . ? C89 C90 C95 N8 3.5(12) . . . . ? C89 C90 C95 C94 -176.9(7) . . . . ? C90 C91 C92 C93 2.3(14) . . . . ? C91 C90 C95 N8 -175.2(7) . . . . ? C91 C90 C95 C94 4.4(11) . . . . ? C91 C92 C93 C94 -1.1(15) . . . . ? C92 C93 C94 C95 1.6(14) . . . . ? C93 C94 C95 N8 176.2(8) . . . . ? C93 C94 C95 C90 -3.4(13) . . . . ? C95 N8 C96 C52 -173.3(7) . . . . ? C95 C90 C91 C92 -3.9(12) . . . . ? C96 N8 C95 C90 144.7(8) . . . . ? C96 N8 C95 C94 -34.9(11) . . . . ? C96 C52 C53 C54 -171.0(7) . . . . ? Br3 Fe3 O5 Fe4 147.5(6) . . . . ? Br4 Fe3 O5 Fe4 -92.8(6) . . . . ? Br5 Fe3 O5 Fe4 30.1(7) . . . . ? Fe3 O5 Fe4 Br6 44.9(7) . . . . ? Fe3 O5 Fe4 Br7 -76.3(7) . . . . ? Fe3 O5 Fe4 Br8 163.2(6) . . . . ? Fe3A O5 Fe4 Br6 10.2(9) . . . . ? Fe3A O5 Fe4 Br7 -111.0(8) . . . . ? Fe3A O5 Fe4 Br8 128.5(8) . . . . ?