#------------------------------------------------------------------------------ #$Date: 2021-10-11 01:56:38 +0300 (Mon, 11 Oct 2021) $ #$Revision: 269885 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/85/7708537.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_7708537 loop_ _publ_author_name 'Yu, Zong-Mei' 'Zhao, Sheng-Ze' 'Wang, Yu-Ting' 'Xu, Peng-Yu' 'Qin, Chun-Yan' 'Li, Yong-Hua' 'Zhou, Xin-Hui' 'Wang, Shi' _publ_section_title ; Anion-driven supramolecular modulation of spin-crossover properties in mononuclear iron(III) Schiff-base complexes. ; _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_paper_doi 10.1039/d1dt02394b _journal_year 2021 _chemical_formula_sum 'C20 H22 Cl F2 Fe N4 O6' _chemical_formula_weight 543.71 _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 mixed _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2021-07-19 deposited with the CCDC. 2021-10-08 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 112.019(13) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 19.281(10) _cell_length_b 13.028(6) _cell_length_c 19.511(10) _cell_measurement_reflns_used 10829 _cell_measurement_temperature 299(2) _cell_measurement_theta_max 27.87 _cell_measurement_theta_min 2.25 _cell_volume 4544(4) _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 299(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0435 _diffrn_reflns_av_unetI/netI 0.0452 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 37668 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.876 _diffrn_reflns_theta_min 2.252 _exptl_absorpt_coefficient_mu 0.843 _exptl_crystal_colour black _exptl_crystal_density_diffrn 1.590 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 2232 _exptl_crystal_preparation 'Magnetic properties' _exptl_crystal_size_max 0.130 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.100 _exptl_transmission_factor_max 0.919 _exptl_transmission_factor_min 0.896 _refine_diff_density_max 1.382 _refine_diff_density_min -0.808 _refine_diff_density_rms 0.082 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 629 _refine_ls_number_reflns 10829 _refine_ls_number_restraints 13 _refine_ls_restrained_S_all 1.049 _refine_ls_R_factor_all 0.0977 _refine_ls_R_factor_gt 0.0613 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0900P)^2^+6.3039P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1597 _refine_ls_wR_factor_ref 0.1841 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7293 _reflns_number_total 10829 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt02394b2.cif _cod_data_source_block 22222 _cod_original_cell_volume 4543(4) _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 7708537 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.898 _shelx_estimated_absorpt_t_max 0.920 _shelx_res_file ; 22222.res created by SHELXL-2014/7 TITL 22222 REM Yadorkari-X generated CELL 0.71073 19.2805 13.0275 19.5115 90.0000 112.0188 90.0000 ZERR 8.0 0.0097 0.0063 0.0099 0.0000 0.0127 0.0000 LATT 1 SYMM 0.50000-X, 0.50000+Y, 0.50000-Z REM SPGR P21/n monoclinic SFAC C H N O F Cl Fe UNIT 160 176 32 48 16 8 8 TEMP 25.6 L.S. 20 FMAP 2 PLAN -10 ACTA BOND$H size 0.10 0.12 0.13 DFIX 1.5 0.01 C28 C29 ISOR 0.005 C28 C29 WGHT 0.090000 6.303900 FVAR 0.10397 FE1 7 0.187569 0.179645 0.727982 11.00000 0.03045 0.03717 = 0.03317 0.00038 0.00896 -0.00070 O1 4 0.196773 0.139159 0.825211 11.00000 0.03851 0.06562 = 0.04424 0.01452 0.01816 0.00310 C1 1 0.257143 0.120856 0.884699 11.00000 0.04283 0.03669 = 0.03845 -0.00285 0.01578 -0.00033 C2 1 0.249408 0.068123 0.944838 11.00000 0.05691 0.05155 = 0.04541 0.00360 0.02015 -0.00739 AFIX 43 H1 2 0.201948 0.050745 0.942969 11.00000 -1.20000 AFIX 0 C3 1 0.312094 0.041871 1.006909 11.00000 0.08279 0.05722 = 0.03858 0.00335 0.01591 -0.01224 AFIX 43 H2 2 0.306689 0.006717 1.046095 11.00000 -1.20000 AFIX 0 C4 1 0.382283 0.068794 1.009377 11.00000 0.06527 0.05390 = 0.03930 0.00102 -0.00396 -0.01212 F1 5 0.443745 0.040715 1.070403 11.00000 0.08065 0.10046 = 0.05921 0.02225 -0.01936 -0.02059 C5 1 0.393046 0.124011 0.954622 11.00000 0.04617 0.04679 = 0.05085 -0.00320 0.00389 -0.00813 AFIX 43 H3 2 0.441009 0.142907 0.958894 11.00000 -1.20000 AFIX 0 C6 1 0.329985 0.152173 0.891071 11.00000 0.04449 0.03325 = 0.03798 -0.00302 0.01137 -0.00285 C7 1 0.343005 0.217741 0.836971 11.00000 0.03781 0.04226 = 0.04548 -0.01242 0.01446 -0.00957 AFIX 43 H4 2 0.391886 0.239124 0.847153 11.00000 -1.20000 AFIX 0 N1 3 0.292607 0.248671 0.776205 11.00000 0.03953 0.03910 = 0.03991 -0.00339 0.01764 -0.00725 C8 1 0.313557 0.319754 0.727486 11.00000 0.04921 0.05128 = 0.04906 0.00044 0.02060 -0.01488 AFIX 23 H5 2 0.366734 0.314646 0.737873 11.00000 -1.20000 H6 2 0.302360 0.389993 0.736260 11.00000 -1.20000 AFIX 0 C9 1 0.269190 0.290241 0.647839 11.00000 0.05373 0.05420 = 0.04929 0.00432 0.02843 -0.00257 AFIX 23 H7 2 0.273623 0.343614 0.615056 11.00000 -1.20000 H8 2 0.288821 0.226998 0.636007 11.00000 -1.20000 AFIX 0 N2 3 0.189646 0.276287 0.637245 11.00000 0.05067 0.04086 = 0.03583 0.00288 0.01879 0.00069 H9 2 0.168087 0.230270 0.593916 11.00000 0.07161 C10 1 0.145562 0.373216 0.629849 11.00000 0.05169 0.03873 = 0.05254 0.01151 0.01781 0.00495 AFIX 23 H10 2 0.098098 0.366921 0.588531 11.00000 -1.20000 H11 2 0.172781 0.430123 0.619782 11.00000 -1.20000 AFIX 0 C11 1 0.131405 0.395073 0.700375 11.00000 0.05786 0.03448 = 0.05526 -0.00503 0.01961 0.00409 AFIX 23 H12 2 0.176425 0.422493 0.737920 11.00000 -1.20000 H13 2 0.091996 0.445789 0.690408 11.00000 -1.20000 AFIX 0 N3 3 0.109399 0.299701 0.727262 11.00000 0.05244 0.04728 = 0.03477 0.00213 0.01946 0.00936 H14 2 0.116681 0.303135 0.767857 11.00000 0.04946 C12 1 0.031024 0.267321 0.683386 11.00000 0.04267 0.05436 = 0.06408 0.01387 0.02310 0.01298 AFIX 23 H15 2 0.018225 0.283850 0.631610 11.00000 -1.20000 H16 2 -0.003410 0.303179 0.700683 11.00000 -1.20000 AFIX 0 C13 1 0.025208 0.152582 0.692687 11.00000 0.03734 0.05704 = 0.05129 0.01119 0.02065 0.00511 AFIX 23 H17 2 0.030960 0.136440 0.743063 11.00000 -1.20000 H18 2 -0.023030 0.127354 0.659488 11.00000 -1.20000 AFIX 0 N4 3 0.085697 0.105836 0.674964 11.00000 0.03136 0.04358 = 0.04312 0.01044 0.01114 0.00250 C14 1 0.071889 0.032297 0.627109 11.00000 0.03370 0.04270 = 0.04531 0.01013 0.00761 -0.00450 AFIX 43 H19 2 0.023132 0.007549 0.607088 11.00000 -1.20000 AFIX 0 C15 1 0.126172 -0.014068 0.602531 11.00000 0.03926 0.03490 = 0.04012 0.00859 0.01066 -0.00141 C16 1 0.100576 -0.082093 0.541614 11.00000 0.05086 0.04102 = 0.04244 0.00523 0.00559 -0.00618 AFIX 43 H20 2 0.050099 -0.098905 0.520161 11.00000 -1.20000 AFIX 0 C17 1 0.150170 -0.122839 0.514534 11.00000 0.07244 0.03961 = 0.03782 0.00002 0.01272 -0.00192 F2 5 0.124620 -0.186734 0.454088 11.00000 0.09340 0.07007 = 0.05556 -0.01864 0.01755 -0.00592 C18 1 0.226404 -0.103093 0.546149 11.00000 0.06364 0.04931 = 0.04751 0.00287 0.02446 0.00797 AFIX 43 H21 2 0.259125 -0.133285 0.527175 11.00000 -1.20000 AFIX 0 C19 1 0.252720 -0.038284 0.605874 11.00000 0.04415 0.04732 = 0.04355 0.00297 0.01433 0.00275 AFIX 43 H22 2 0.303753 -0.024859 0.627225 11.00000 -1.20000 AFIX 0 C20 1 0.203999 0.008612 0.635742 11.00000 0.04022 0.03459 = 0.03853 0.00522 0.01092 0.00292 O2 4 0.232786 0.069246 0.694524 11.00000 0.03337 0.04556 = 0.04831 -0.00328 0.00861 0.00473 FE2 7 0.272439 0.142352 0.292748 11.00000 0.03346 0.04011 = 0.03827 0.00589 0.00745 0.00089 O3 4 0.173228 0.095745 0.275472 11.00000 0.04085 0.06783 = 0.04287 0.01297 0.00603 -0.01225 C21 1 0.108629 0.096091 0.217979 11.00000 0.03504 0.03650 = 0.04266 0.00311 0.01015 -0.00039 C22 1 0.044890 0.053632 0.226633 11.00000 0.04099 0.04740 = 0.05400 0.00916 0.01742 -0.00130 AFIX 43 H23 2 0.048176 0.031468 0.273059 11.00000 -1.20000 AFIX 0 C23 1 -0.022016 0.044628 0.167265 11.00000 0.03856 0.06008 = 0.08185 0.01568 0.01397 -0.00498 AFIX 43 H24 2 -0.063561 0.015839 0.173178 11.00000 -1.20000 AFIX 0 C24 1 -0.026342 0.079135 0.098724 11.00000 0.04574 0.07301 = 0.07001 0.02320 -0.01166 -0.01172 F3 5 -0.093385 0.069305 0.039989 11.00000 0.06343 0.15077 = 0.10058 0.05621 -0.03376 -0.04234 C25 1 0.032268 0.124726 0.088254 11.00000 0.05436 0.07881 = 0.05452 0.02631 -0.00200 -0.00660 AFIX 43 H25 2 0.027001 0.149005 0.041740 11.00000 -1.20000 AFIX 0 C26 1 0.100859 0.134990 0.148063 11.00000 0.03894 0.04601 = 0.05059 0.01406 0.00742 -0.00070 C27 1 0.159796 0.190971 0.135613 11.00000 0.05039 0.08017 = 0.05587 0.03454 0.01101 -0.00180 AFIX 43 H26 2 0.150136 0.215771 0.088224 11.00000 -1.20000 AFIX 0 N5 3 0.224485 0.208810 0.185387 11.00000 0.04037 0.08406 = 0.06306 0.03947 0.00739 -0.01007 C28 1 0.278039 0.266054 0.161959 11.00000 0.08163 0.12253 = 0.09672 0.04666 0.02409 -0.03060 AFIX 23 H27 2 0.301967 0.219519 0.138799 11.00000 -1.20000 H28 2 0.251693 0.318104 0.126099 11.00000 -1.20000 AFIX 0 C29 1 0.332189 0.312432 0.223588 11.00000 0.13565 0.14321 = 0.09899 0.00161 0.05639 -0.07485 AFIX 23 H29 2 0.315178 0.381608 0.227052 11.00000 -1.20000 H30 2 0.377495 0.318656 0.213325 11.00000 -1.20000 AFIX 0 N6 3 0.352858 0.265392 0.296468 11.00000 0.04165 0.07507 = 0.06719 -0.00844 0.02558 -0.01351 H31 2 0.394504 0.228138 0.313857 11.00000 0.08109 C30 1 0.359182 0.345235 0.353127 11.00000 0.06064 0.04727 = 0.07336 -0.00442 0.02615 -0.00940 AFIX 23 H32 2 0.370530 0.411129 0.336649 11.00000 -1.20000 H33 2 0.399540 0.327756 0.399198 11.00000 -1.20000 AFIX 0 C31 1 0.286380 0.352090 0.365290 11.00000 0.06125 0.04910 = 0.07274 -0.00219 0.02351 0.01296 AFIX 23 H34 2 0.292941 0.395164 0.407824 11.00000 -1.20000 H35 2 0.248219 0.382874 0.322396 11.00000 -1.20000 AFIX 0 N7 3 0.262493 0.248348 0.377714 11.00000 0.03409 0.05475 = 0.05582 -0.00118 0.01894 0.00445 H36 2 0.217602 0.249230 0.366056 11.00000 0.05243 C32 1 0.304221 0.209025 0.453534 11.00000 0.04864 0.07693 = 0.04456 -0.00290 0.02057 0.00961 AFIX 23 H37 2 0.282292 0.235663 0.487263 11.00000 -1.20000 H38 2 0.355953 0.231289 0.470548 11.00000 -1.20000 AFIX 0 C33 1 0.300460 0.093809 0.451963 11.00000 0.04965 0.06974 = 0.05195 0.01592 0.02814 0.00792 AFIX 23 H39 2 0.332645 0.065667 0.499229 11.00000 -1.20000 H40 2 0.249641 0.070862 0.441472 11.00000 -1.20000 AFIX 0 N8 3 0.325920 0.060431 0.392864 11.00000 0.03626 0.04497 = 0.04193 0.00684 0.01443 -0.00187 C34 1 0.381244 -0.001680 0.408141 11.00000 0.04227 0.04717 = 0.04024 0.01035 0.01187 0.00242 AFIX 43 H41 2 0.402300 -0.026002 0.456390 11.00000 -1.20000 AFIX 0 C35 1 0.413506 -0.036926 0.356436 11.00000 0.04214 0.03947 = 0.04351 0.00135 0.01176 -0.00071 C36 1 0.478295 -0.098984 0.383993 11.00000 0.04816 0.06453 = 0.05473 0.00654 0.01350 0.01087 AFIX 43 H42 2 0.498107 -0.117749 0.433588 11.00000 -1.20000 AFIX 0 C37 1 0.511521 -0.131125 0.336861 11.00000 0.05145 0.06425 = 0.07701 -0.00916 0.02007 0.01255 F4 5 0.575852 -0.188642 0.364302 11.00000 0.07066 0.11654 = 0.10024 0.00101 0.03027 0.04278 C38 1 0.482585 -0.109124 0.262769 11.00000 0.06969 0.08162 = 0.06820 -0.01843 0.03140 0.01182 AFIX 43 H43 2 0.505537 -0.133926 0.231831 11.00000 -1.20000 AFIX 0 C39 1 0.418855 -0.049592 0.234738 11.00000 0.08458 0.07618 = 0.04573 -0.01112 0.01955 0.01300 AFIX 43 H44 2 0.399335 -0.033836 0.184595 11.00000 -1.20000 AFIX 0 C40 1 0.382659 -0.012094 0.280700 11.00000 0.05451 0.04304 = 0.03976 -0.00684 0.00803 0.00274 O4 4 0.321538 0.045830 0.251473 11.00000 0.07576 0.06125 = 0.03720 -0.00157 0.00849 0.02257 CL1 6 0.556491 0.202790 0.410896 11.00000 0.04649 0.06648 = 0.04399 0.00498 0.01836 0.00141 O5 4 0.583408 0.118124 0.387181 11.00000 0.16384 0.15052 = 0.47583 -0.09181 0.20828 -0.01696 O6 4 0.500709 0.177813 0.439779 11.00000 0.07487 0.09773 = 0.08687 0.01642 0.04874 -0.00097 O7 4 0.613831 0.249106 0.458543 11.00000 0.18200 0.51905 = 0.17623 -0.21081 0.12070 -0.20704 CL2 6 0.082715 0.210035 0.432981 11.00000 0.04064 0.07527 = 0.05153 0.00618 0.01907 -0.00032 O8 4 0.112930 0.111743 0.428940 11.00000 0.19952 0.13944 = 0.23398 0.03980 0.12559 0.07132 O9 4 0.061409 0.209959 0.495513 11.00000 0.09515 0.16936 = 0.07307 -0.03547 0.04350 -0.04748 O10 4 0.134305 0.283171 0.434603 11.00000 0.13287 0.14237 = 0.26294 -0.03577 0.13830 -0.05245 O11 4 0.018468 0.208161 0.369696 11.00000 0.07793 0.29045 = 0.08902 0.02134 0.01724 -0.01151 O12 4 0.523825 0.246207 0.346493 11.00000 0.12184 0.53745 = 0.20835 0.23736 0.10600 0.09694 HKLF 4 REM 22222 REM R1 = 0.0613 for 7293 Fo > 4sig(Fo) and 0.0977 for all 10829 data REM 629 parameters refined using 13 restraints END WGHT 0.0900 6.3038 REM Highest difference peak 1.382, deepest hole -0.808, 1-sigma level 0.082 Q1 1 0.5586 0.3149 0.4107 11.00000 0.05 1.38 Q2 1 0.2700 0.3188 0.1873 11.00000 0.05 1.20 Q3 1 0.3579 0.2600 0.2292 11.00000 0.05 0.98 Q4 1 0.6190 0.1528 0.4557 11.00000 0.05 0.95 Q5 1 0.1572 0.1735 0.4896 11.00000 0.05 0.81 Q6 1 0.5369 0.1766 0.3436 11.00000 0.05 0.76 Q7 1 0.0372 0.3094 0.4035 11.00000 0.05 0.71 Q8 1 0.0532 0.1294 0.3936 11.00000 0.05 0.52 Q9 1 0.4176 0.0905 1.0810 11.00000 0.05 0.34 Q10 1 0.0501 0.2720 0.4594 11.00000 0.05 0.34 ; _shelx_res_checksum 66338 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 0.18757(3) 0.17964(4) 0.72798(3) 0.03446(14) Uani 1 1 d . . . . . O1 O 0.19677(14) 0.1392(2) 0.82521(15) 0.0487(7) Uani 1 1 d . . . . . C1 C 0.2571(2) 0.1209(3) 0.8847(2) 0.0392(8) Uani 1 1 d . . . . . C2 C 0.2494(3) 0.0681(3) 0.9448(2) 0.0510(10) Uani 1 1 d . . . . . H1 H 0.2019 0.0507 0.9430 0.061 Uiso 1 1 calc R U . . . C3 C 0.3121(3) 0.0419(4) 1.0069(2) 0.0615(12) Uani 1 1 d . . . . . H2 H 0.3067 0.0067 1.0461 0.074 Uiso 1 1 calc R U . . . C4 C 0.3823(3) 0.0688(4) 1.0094(2) 0.0597(12) Uani 1 1 d . . . . . F1 F 0.44374(18) 0.0407(3) 1.07040(16) 0.0934(11) Uani 1 1 d . . . . . C5 C 0.3930(2) 0.1240(3) 0.9546(2) 0.0521(10) Uani 1 1 d . . . . . H3 H 0.4410 0.1429 0.9589 0.063 Uiso 1 1 calc R U . . . C6 C 0.3300(2) 0.1522(3) 0.8911(2) 0.0398(8) Uani 1 1 d . . . . . C7 C 0.3430(2) 0.2177(3) 0.8370(2) 0.0422(9) Uani 1 1 d . . . . . H4 H 0.3919 0.2391 0.8472 0.051 Uiso 1 1 calc R U . . . N1 N 0.29261(17) 0.2487(2) 0.77620(17) 0.0387(7) Uani 1 1 d . . . . . C8 C 0.3136(2) 0.3198(3) 0.7275(2) 0.0492(10) Uani 1 1 d . . . . . H5 H 0.3667 0.3146 0.7379 0.059 Uiso 1 1 calc R U . . . H6 H 0.3024 0.3900 0.7363 0.059 Uiso 1 1 calc R U . . . C9 C 0.2692(2) 0.2902(4) 0.6478(2) 0.0498(10) Uani 1 1 d . . . . . H7 H 0.2736 0.3436 0.6151 0.060 Uiso 1 1 calc R U . . . H8 H 0.2888 0.2270 0.6360 0.060 Uiso 1 1 calc R U . . . N2 N 0.18965(19) 0.2763(3) 0.63724(18) 0.0417(7) Uani 1 1 d . . . . . H9 H 0.168(3) 0.230(4) 0.594(3) 0.072(15) Uiso 1 1 d . . . . . C10 C 0.1456(2) 0.3732(3) 0.6298(2) 0.0482(9) Uani 1 1 d . . . . . H10 H 0.0981 0.3669 0.5885 0.058 Uiso 1 1 calc R U . . . H11 H 0.1728 0.4301 0.6198 0.058 Uiso 1 1 calc R U . . . C11 C 0.1314(2) 0.3951(3) 0.7004(2) 0.0497(10) Uani 1 1 d . . . . . H12 H 0.1764 0.4225 0.7379 0.060 Uiso 1 1 calc R U . . . H13 H 0.0920 0.4458 0.6904 0.060 Uiso 1 1 calc R U . . . N3 N 0.1094(2) 0.2997(3) 0.7273(2) 0.0439(8) Uani 1 1 d . . . . . H14 H 0.117(3) 0.303(4) 0.768(3) 0.049(14) Uiso 1 1 d . . . . . C12 C 0.0310(2) 0.2673(3) 0.6834(3) 0.0528(10) Uani 1 1 d . . . . . H15 H 0.0182 0.2839 0.6316 0.063 Uiso 1 1 calc R U . . . H16 H -0.0034 0.3032 0.7007 0.063 Uiso 1 1 calc R U . . . C13 C 0.0252(2) 0.1526(3) 0.6927(2) 0.0474(9) Uani 1 1 d . . . . . H17 H 0.0310 0.1364 0.7431 0.057 Uiso 1 1 calc R U . . . H18 H -0.0230 0.1274 0.6595 0.057 Uiso 1 1 calc R U . . . N4 N 0.08570(16) 0.1058(3) 0.67496(17) 0.0402(7) Uani 1 1 d . . . . . C14 C 0.0719(2) 0.0323(3) 0.6271(2) 0.0427(9) Uani 1 1 d . . . . . H19 H 0.0231 0.0075 0.6071 0.051 Uiso 1 1 calc R U . . . C15 C 0.1262(2) -0.0141(3) 0.6025(2) 0.0393(8) Uani 1 1 d . . . . . C16 C 0.1006(2) -0.0821(3) 0.5416(2) 0.0482(10) Uani 1 1 d . . . . . H20 H 0.0501 -0.0989 0.5202 0.058 Uiso 1 1 calc R U . . . C17 C 0.1502(3) -0.1228(3) 0.5145(2) 0.0523(10) Uani 1 1 d . . . . . F2 F 0.12462(19) -0.1867(2) 0.45409(16) 0.0760(8) Uani 1 1 d . . . . . C18 C 0.2264(3) -0.1031(3) 0.5461(2) 0.0524(10) Uani 1 1 d . . . . . H21 H 0.2591 -0.1333 0.5272 0.063 Uiso 1 1 calc R U . . . C19 C 0.2527(2) -0.0383(3) 0.6059(2) 0.0456(9) Uani 1 1 d . . . . . H22 H 0.3038 -0.0249 0.6272 0.055 Uiso 1 1 calc R U . . . C20 C 0.2040(2) 0.0086(3) 0.6357(2) 0.0389(8) Uani 1 1 d . . . . . O2 O 0.23279(13) 0.0692(2) 0.69452(15) 0.0444(6) Uani 1 1 d . . . . . Fe2 Fe 0.27244(3) 0.14235(4) 0.29275(3) 0.03902(15) Uani 1 1 d . . . . . O3 O 0.17323(15) 0.0957(2) 0.27547(15) 0.0533(7) Uani 1 1 d . . . . . C21 C 0.10863(19) 0.0961(3) 0.2180(2) 0.0393(8) Uani 1 1 d . . . . . C22 C 0.0449(2) 0.0536(3) 0.2266(2) 0.0476(9) Uani 1 1 d . . . . . H23 H 0.0482 0.0315 0.2731 0.057 Uiso 1 1 calc R U . . . C23 C -0.0220(2) 0.0446(4) 0.1673(3) 0.0627(13) Uani 1 1 d . . . . . H24 H -0.0636 0.0158 0.1732 0.075 Uiso 1 1 calc R U . . . C24 C -0.0263(3) 0.0791(4) 0.0987(3) 0.0726(16) Uani 1 1 d . . . . . F3 F -0.09338(18) 0.0693(4) 0.0400(2) 0.1237(17) Uani 1 1 d . . . . . C25 C 0.0323(3) 0.1247(4) 0.0883(3) 0.0691(14) Uani 1 1 d . . . . . H25 H 0.0270 0.1490 0.0417 0.083 Uiso 1 1 calc R U . . . C26 C 0.1009(2) 0.1350(3) 0.1481(2) 0.0479(10) Uani 1 1 d . . . . . C27 C 0.1598(3) 0.1910(4) 0.1356(3) 0.0647(14) Uani 1 1 d . . . . . H26 H 0.1501 0.2158 0.0882 0.078 Uiso 1 1 calc R U . . . N5 N 0.2245(2) 0.2088(3) 0.1854(2) 0.0660(12) Uani 1 1 d . . . . . C28 C 0.2780(4) 0.2661(6) 0.1620(4) 0.103(2) Uani 1 1 d D U . . . H27 H 0.3020 0.2195 0.1388 0.124 Uiso 1 1 calc R U . . . H28 H 0.2517 0.3181 0.1261 0.124 Uiso 1 1 calc R U . . . C29 C 0.3322(5) 0.3124(7) 0.2236(4) 0.122(3) Uani 1 1 d D U . . . H29 H 0.3152 0.3816 0.2271 0.147 Uiso 1 1 calc R U . . . H30 H 0.3775 0.3187 0.2133 0.147 Uiso 1 1 calc R U . . . N6 N 0.3529(2) 0.2654(4) 0.2965(2) 0.0598(10) Uani 1 1 d . . . . . H31 H 0.395(3) 0.228(5) 0.314(3) 0.081(18) Uiso 1 1 d . . . . . C30 C 0.3592(3) 0.3452(4) 0.3531(3) 0.0601(12) Uani 1 1 d . . . . . H32 H 0.3705 0.4111 0.3366 0.072 Uiso 1 1 calc R U . . . H33 H 0.3995 0.3278 0.3992 0.072 Uiso 1 1 calc R U . . . C31 C 0.2864(3) 0.3521(4) 0.3653(3) 0.0615(12) Uani 1 1 d . . . . . H34 H 0.2929 0.3952 0.4078 0.074 Uiso 1 1 calc R U . . . H35 H 0.2482 0.3829 0.3224 0.074 Uiso 1 1 calc R U . . . N7 N 0.26249(19) 0.2483(3) 0.3777(2) 0.0476(8) Uani 1 1 d . . . . . H36 H 0.218(3) 0.249(4) 0.366(2) 0.052(13) Uiso 1 1 d . . . . . C32 C 0.3042(2) 0.2090(4) 0.4535(2) 0.0558(11) Uani 1 1 d . . . . . H37 H 0.2823 0.2357 0.4873 0.067 Uiso 1 1 calc R U . . . H38 H 0.3560 0.2313 0.4705 0.067 Uiso 1 1 calc R U . . . C33 C 0.3005(2) 0.0938(4) 0.4520(2) 0.0545(11) Uani 1 1 d . . . . . H39 H 0.3326 0.0657 0.4992 0.065 Uiso 1 1 calc R U . . . H40 H 0.2496 0.0709 0.4415 0.065 Uiso 1 1 calc R U . . . N8 N 0.32592(17) 0.0604(2) 0.39286(17) 0.0411(7) Uani 1 1 d . . . . . C34 C 0.3812(2) -0.0017(3) 0.4081(2) 0.0443(9) Uani 1 1 d . . . . . H41 H 0.4023 -0.0260 0.4564 0.053 Uiso 1 1 calc R U . . . C35 C 0.4135(2) -0.0369(3) 0.3564(2) 0.0430(8) Uani 1 1 d . . . . . C36 C 0.4783(2) -0.0990(4) 0.3840(3) 0.0575(11) Uani 1 1 d . . . . . H42 H 0.4981 -0.1177 0.4336 0.069 Uiso 1 1 calc R U . . . C37 C 0.5115(3) -0.1311(4) 0.3369(3) 0.0654(13) Uani 1 1 d . . . . . F4 F 0.57585(18) -0.1886(3) 0.3643(2) 0.0963(11) Uani 1 1 d . . . . . C38 C 0.4826(3) -0.1091(5) 0.2628(3) 0.0716(14) Uani 1 1 d . . . . . H43 H 0.5055 -0.1339 0.2318 0.086 Uiso 1 1 calc R U . . . C39 C 0.4189(3) -0.0496(4) 0.2347(3) 0.0703(14) Uani 1 1 d . . . . . H44 H 0.3993 -0.0338 0.1846 0.084 Uiso 1 1 calc R U . . . C40 C 0.3827(2) -0.0121(3) 0.2807(2) 0.0486(10) Uani 1 1 d . . . . . O4 O 0.32154(19) 0.0458(3) 0.25147(15) 0.0618(9) Uani 1 1 d . . . . . Cl1 Cl 0.55649(6) 0.20279(9) 0.41090(6) 0.0519(3) Uani 1 1 d . . . . . O5 O 0.5834(5) 0.1181(6) 0.3872(7) 0.238(5) Uani 1 1 d . . . . . O6 O 0.5007(2) 0.1778(3) 0.4398(2) 0.0811(11) Uani 1 1 d . . . . . O7 O 0.6138(5) 0.2491(11) 0.4585(5) 0.277(7) Uani 1 1 d . . . . . Cl2 Cl 0.08271(6) 0.21003(10) 0.43298(6) 0.0553(3) Uani 1 1 d . . . . . O8 O 0.1129(4) 0.1117(6) 0.4289(5) 0.178(3) Uani 1 1 d . . . . . O9 O 0.0614(3) 0.2100(5) 0.4955(2) 0.1090(17) Uani 1 1 d . . . . . O10 O 0.1343(3) 0.2832(5) 0.4346(5) 0.161(3) Uani 1 1 d . . . . . O11 O 0.0185(3) 0.2082(7) 0.3697(3) 0.157(3) Uani 1 1 d . . . . . O12 O 0.5238(4) 0.2462(11) 0.3465(5) 0.276(7) 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 Fe1 0.0304(2) 0.0372(3) 0.0332(3) 0.0004(2) 0.0090(2) -0.0007(2) O1 0.0385(13) 0.0656(19) 0.0442(15) 0.0145(13) 0.0182(12) 0.0031(13) C1 0.0428(19) 0.0367(19) 0.0385(19) -0.0028(15) 0.0158(16) -0.0003(15) C2 0.057(2) 0.052(2) 0.045(2) 0.0036(19) 0.0202(19) -0.007(2) C3 0.083(3) 0.057(3) 0.039(2) 0.003(2) 0.016(2) -0.012(2) C4 0.065(3) 0.054(3) 0.039(2) 0.0010(19) -0.004(2) -0.012(2) F1 0.081(2) 0.100(2) 0.0592(17) 0.0222(17) -0.0194(15) -0.0206(18) C5 0.046(2) 0.047(2) 0.051(2) -0.0032(19) 0.0039(18) -0.0081(18) C6 0.0445(19) 0.0333(18) 0.0380(19) -0.0030(15) 0.0114(16) -0.0029(15) C7 0.0378(18) 0.042(2) 0.045(2) -0.0124(17) 0.0145(16) -0.0096(16) N1 0.0395(15) 0.0391(16) 0.0399(16) -0.0034(13) 0.0176(14) -0.0073(13) C8 0.049(2) 0.051(2) 0.049(2) 0.0004(19) 0.0206(19) -0.0149(19) C9 0.054(2) 0.054(2) 0.049(2) 0.0043(19) 0.028(2) -0.0026(19) N2 0.0507(18) 0.0409(17) 0.0358(16) 0.0029(14) 0.0188(14) 0.0007(15) C10 0.052(2) 0.039(2) 0.053(2) 0.0115(18) 0.0178(19) 0.0050(17) C11 0.058(2) 0.0345(19) 0.055(2) -0.0050(18) 0.020(2) 0.0041(18) N3 0.0524(19) 0.047(2) 0.0348(18) 0.0021(15) 0.0195(16) 0.0094(15) C12 0.043(2) 0.054(3) 0.064(3) 0.014(2) 0.023(2) 0.0130(19) C13 0.0373(19) 0.057(2) 0.051(2) 0.0112(19) 0.0206(17) 0.0051(17) N4 0.0314(14) 0.0436(17) 0.0431(17) 0.0104(15) 0.0111(13) 0.0025(13) C14 0.0337(17) 0.043(2) 0.045(2) 0.0101(17) 0.0076(16) -0.0045(16) C15 0.0393(18) 0.0349(19) 0.0401(19) 0.0086(15) 0.0107(15) -0.0014(15) C16 0.051(2) 0.041(2) 0.042(2) 0.0052(17) 0.0056(18) -0.0062(18) C17 0.072(3) 0.040(2) 0.038(2) 0.0000(17) 0.013(2) -0.002(2) F2 0.093(2) 0.0701(19) 0.0556(16) -0.0186(14) 0.0176(15) -0.0059(16) C18 0.064(3) 0.049(2) 0.048(2) 0.0029(19) 0.024(2) 0.008(2) C19 0.044(2) 0.047(2) 0.044(2) 0.0030(18) 0.0143(17) 0.0027(17) C20 0.0402(18) 0.0346(18) 0.0385(19) 0.0052(15) 0.0109(15) 0.0029(15) O2 0.0334(12) 0.0456(15) 0.0483(15) -0.0033(12) 0.0086(11) 0.0047(11) Fe2 0.0335(3) 0.0401(3) 0.0383(3) 0.0059(2) 0.0075(2) 0.0009(2) O3 0.0409(14) 0.0678(19) 0.0429(15) 0.0130(14) 0.0060(12) -0.0123(14) C21 0.0350(17) 0.0365(19) 0.043(2) 0.0031(16) 0.0101(15) -0.0004(15) C22 0.041(2) 0.047(2) 0.054(2) 0.0092(19) 0.0174(18) -0.0013(17) C23 0.039(2) 0.060(3) 0.082(3) 0.016(3) 0.014(2) -0.005(2) C24 0.046(2) 0.073(3) 0.070(3) 0.023(3) -0.012(2) -0.012(2) F3 0.0634(19) 0.151(4) 0.101(3) 0.056(3) -0.0338(18) -0.042(2) C25 0.054(3) 0.079(3) 0.055(3) 0.026(3) -0.002(2) -0.007(2) C26 0.0389(19) 0.046(2) 0.051(2) 0.0141(18) 0.0074(17) -0.0007(17) C27 0.050(2) 0.080(3) 0.056(3) 0.035(2) 0.011(2) -0.002(2) N5 0.0404(18) 0.084(3) 0.063(2) 0.039(2) 0.0074(17) -0.0101(18) C28 0.082(3) 0.123(4) 0.097(4) 0.047(3) 0.024(3) -0.031(3) C29 0.136(4) 0.143(5) 0.099(4) 0.002(3) 0.056(3) -0.075(4) N6 0.0416(19) 0.075(3) 0.067(3) -0.008(2) 0.0256(19) -0.0135(19) C30 0.061(3) 0.047(2) 0.073(3) -0.004(2) 0.026(2) -0.009(2) C31 0.061(3) 0.049(2) 0.073(3) -0.002(2) 0.024(2) 0.013(2) N7 0.0341(17) 0.055(2) 0.056(2) -0.0012(17) 0.0189(16) 0.0044(15) C32 0.049(2) 0.077(3) 0.045(2) -0.003(2) 0.0206(19) 0.010(2) C33 0.050(2) 0.070(3) 0.052(2) 0.016(2) 0.028(2) 0.008(2) N8 0.0363(15) 0.0450(18) 0.0419(17) 0.0068(14) 0.0144(13) -0.0019(14) C34 0.0423(19) 0.047(2) 0.040(2) 0.0103(17) 0.0119(16) 0.0024(17) C35 0.0421(19) 0.039(2) 0.044(2) 0.0014(16) 0.0118(17) -0.0007(16) C36 0.048(2) 0.065(3) 0.055(3) 0.007(2) 0.013(2) 0.011(2) C37 0.051(2) 0.064(3) 0.077(3) -0.009(3) 0.020(2) 0.013(2) F4 0.071(2) 0.117(3) 0.100(3) 0.001(2) 0.0303(18) 0.0428(19) C38 0.070(3) 0.082(4) 0.068(3) -0.018(3) 0.031(3) 0.012(3) C39 0.085(3) 0.076(3) 0.046(3) -0.011(2) 0.020(2) 0.013(3) C40 0.055(2) 0.043(2) 0.040(2) -0.0068(17) 0.0080(18) 0.0027(18) O4 0.076(2) 0.0613(19) 0.0372(15) -0.0016(14) 0.0085(14) 0.0226(17) Cl1 0.0465(5) 0.0665(7) 0.0440(5) 0.0050(5) 0.0184(4) 0.0014(5) O5 0.164(6) 0.151(6) 0.476(16) -0.092(8) 0.208(9) -0.017(5) O6 0.075(2) 0.098(3) 0.087(3) 0.016(2) 0.049(2) -0.001(2) O7 0.182(7) 0.519(18) 0.176(7) -0.211(10) 0.121(6) -0.207(10) Cl2 0.0406(5) 0.0753(7) 0.0515(6) 0.0062(5) 0.0191(4) -0.0003(5) O8 0.200(7) 0.139(6) 0.234(8) 0.040(6) 0.126(7) 0.071(5) O9 0.095(3) 0.169(5) 0.073(3) -0.035(3) 0.043(2) -0.047(3) O10 0.133(5) 0.142(5) 0.263(9) -0.036(5) 0.138(6) -0.052(4) O11 0.078(3) 0.290(9) 0.089(4) 0.021(5) 0.017(3) -0.012(4) O12 0.122(5) 0.537(19) 0.208(8) 0.237(11) 0.106(6) 0.097(8) 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' 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' 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 O2 104.23(13) . . ? O1 Fe1 N4 94.87(12) . . ? O2 Fe1 N4 87.08(12) . . ? O1 Fe1 N1 87.60(12) . . ? O2 Fe1 N1 89.34(12) . . ? N4 Fe1 N1 176.06(13) . . ? O1 Fe1 N3 90.64(13) . . ? O2 Fe1 N3 160.36(13) . . ? N4 Fe1 N3 78.80(14) . . ? N1 Fe1 N3 104.27(14) . . ? O1 Fe1 N2 160.01(14) . . ? O2 Fe1 N2 90.43(13) . . ? N4 Fe1 N2 99.44(13) . . ? N1 Fe1 N2 78.92(13) . . ? N3 Fe1 N2 78.64(13) . . ? C1 O1 Fe1 130.2(2) . . ? O1 C1 C2 119.0(3) . . ? O1 C1 C6 122.7(3) . . ? C2 C1 C6 118.3(4) . . ? C3 C2 C1 120.8(4) . . ? C3 C2 H1 119.6 . . ? C1 C2 H1 119.6 . . ? C4 C3 C2 119.1(4) . . ? C4 C3 H2 120.4 . . ? C2 C3 H2 120.4 . . ? C5 C4 F1 118.8(4) . . ? C5 C4 C3 122.7(4) . . ? F1 C4 C3 118.5(4) . . ? C4 C5 C6 119.1(4) . . ? C4 C5 H3 120.4 . . ? C6 C5 H3 120.4 . . ? C5 C6 C1 119.7(4) . . ? C5 C6 C7 117.5(4) . . ? C1 C6 C7 122.7(3) . . ? N1 C7 C6 125.4(3) . . ? N1 C7 H4 117.3 . . ? C6 C7 H4 117.3 . . ? C7 N1 C8 119.5(3) . . ? C7 N1 Fe1 123.4(3) . . ? C8 N1 Fe1 115.5(2) . . ? N1 C8 C9 108.3(3) . . ? N1 C8 H5 110.0 . . ? C9 C8 H5 110.0 . . ? N1 C8 H6 110.0 . . ? C9 C8 H6 110.0 . . ? H5 C8 H6 108.4 . . ? N2 C9 C8 109.3(3) . . ? N2 C9 H7 109.8 . . ? C8 C9 H7 109.8 . . ? N2 C9 H8 109.8 . . ? C8 C9 H8 109.8 . . ? H7 C9 H8 108.3 . . ? C9 N2 C10 115.5(3) . . ? C9 N2 Fe1 106.9(2) . . ? C10 N2 Fe1 112.4(2) . . ? C9 N2 H9 106(3) . . ? C10 N2 H9 113(3) . . ? Fe1 N2 H9 102(3) . . ? N2 C10 C11 110.9(3) . . ? N2 C10 H10 109.5 . . ? C11 C10 H10 109.5 . . ? N2 C10 H11 109.5 . . ? C11 C10 H11 109.5 . . ? H10 C10 H11 108.0 . . ? N3 C11 C10 109.7(3) . . ? N3 C11 H12 109.7 . . ? C10 C11 H12 109.7 . . ? N3 C11 H13 109.7 . . ? C10 C11 H13 109.7 . . ? H12 C11 H13 108.2 . . ? C11 N3 C12 113.6(3) . . ? C11 N3 Fe1 108.6(3) . . ? C12 N3 Fe1 110.6(3) . . ? C11 N3 H14 111(4) . . ? C12 N3 H14 112(4) . . ? Fe1 N3 H14 100(4) . . ? N3 C12 C13 108.4(3) . . ? N3 C12 H15 110.0 . . ? C13 C12 H15 110.0 . . ? N3 C12 H16 110.0 . . ? C13 C12 H16 110.0 . . ? H15 C12 H16 108.4 . . ? N4 C13 C12 106.3(3) . . ? N4 C13 H17 110.5 . . ? C12 C13 H17 110.5 . . ? N4 C13 H18 110.5 . . ? C12 C13 H18 110.5 . . ? H17 C13 H18 108.7 . . ? C14 N4 C13 120.7(3) . . ? C14 N4 Fe1 127.0(3) . . ? C13 N4 Fe1 112.1(3) . . ? N4 C14 C15 125.0(3) . . ? N4 C14 H19 117.5 . . ? C15 C14 H19 117.5 . . ? C16 C15 C20 119.2(4) . . ? C16 C15 C14 118.4(3) . . ? C20 C15 C14 122.4(3) . . ? C17 C16 C15 119.7(4) . . ? C17 C16 H20 120.1 . . ? C15 C16 H20 120.1 . . ? C16 C17 F2 119.4(4) . . ? C16 C17 C18 122.4(4) . . ? F2 C17 C18 118.2(4) . . ? C19 C18 C17 118.9(4) . . ? C19 C18 H21 120.5 . . ? C17 C18 H21 120.5 . . ? C18 C19 C20 121.6(4) . . ? C18 C19 H22 119.2 . . ? C20 C19 H22 119.2 . . ? O2 C20 C19 119.0(3) . . ? O2 C20 C15 122.9(3) . . ? C19 C20 C15 118.1(3) . . ? C20 O2 Fe1 130.0(2) . . ? O3 Fe2 O4 109.60(15) . . ? O3 Fe2 N8 96.39(12) . . ? O4 Fe2 N8 84.90(13) . . ? O3 Fe2 N5 85.36(13) . . ? O4 Fe2 N5 87.38(16) . . ? N8 Fe2 N5 172.23(17) . . ? O3 Fe2 N6 151.42(16) . . ? O4 Fe2 N6 92.21(16) . . ? N8 Fe2 N6 103.97(15) . . ? N5 Fe2 N6 77.19(16) . . ? O3 Fe2 N7 88.19(14) . . ? O4 Fe2 N7 155.96(13) . . ? N8 Fe2 N7 76.92(14) . . ? N5 Fe2 N7 110.75(17) . . ? N6 Fe2 N7 77.32(15) . . ? C21 O3 Fe2 135.0(2) . . ? O3 C21 C26 123.0(3) . . ? O3 C21 C22 118.7(3) . . ? C26 C21 C22 118.3(3) . . ? C23 C22 C21 121.0(4) . . ? C23 C22 H23 119.5 . . ? C21 C22 H23 119.5 . . ? C22 C23 C24 118.9(4) . . ? C22 C23 H24 120.6 . . ? C24 C23 H24 120.6 . . ? C25 C24 F3 119.4(5) . . ? C25 C24 C23 122.4(4) . . ? F3 C24 C23 118.2(4) . . ? C24 C25 C26 119.6(4) . . ? C24 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? C25 C26 C21 119.7(4) . . ? C25 C26 C27 117.6(4) . . ? C21 C26 C27 122.6(4) . . ? N5 C27 C26 124.5(4) . . ? N5 C27 H26 117.7 . . ? C26 C27 H26 117.7 . . ? C27 N5 C28 116.8(4) . . ? C27 N5 Fe2 127.7(3) . . ? C28 N5 Fe2 114.4(3) . . ? C29 C28 N5 109.5(5) . . ? C29 C28 H27 109.8 . . ? N5 C28 H27 109.8 . . ? C29 C28 H28 109.8 . . ? N5 C28 H28 109.8 . . ? H27 C28 H28 108.2 . . ? C28 C29 N6 119.9(5) . . ? C28 C29 H29 107.3 . . ? N6 C29 H29 107.3 . . ? C28 C29 H30 107.3 . . ? N6 C29 H30 107.3 . . ? H29 C29 H30 106.9 . . ? C29 N6 C30 110.3(5) . . ? C29 N6 Fe2 109.9(3) . . ? C30 N6 Fe2 113.1(3) . . ? C29 N6 H31 119(4) . . ? C30 N6 H31 107(4) . . ? Fe2 N6 H31 98(4) . . ? N6 C30 C31 109.6(4) . . ? N6 C30 H32 109.8 . . ? C31 C30 H32 109.8 . . ? N6 C30 H33 109.8 . . ? C31 C30 H33 109.8 . . ? H32 C30 H33 108.2 . . ? N7 C31 C30 109.7(4) . . ? N7 C31 H34 109.7 . . ? C30 C31 H34 109.7 . . ? N7 C31 H35 109.7 . . ? C30 C31 H35 109.7 . . ? H34 C31 H35 108.2 . . ? C31 N7 C32 113.2(4) . . ? C31 N7 Fe2 109.1(3) . . ? C32 N7 Fe2 111.3(3) . . ? C31 N7 H36 108(3) . . ? C32 N7 H36 114(3) . . ? Fe2 N7 H36 100(3) . . ? N7 C32 C33 108.7(4) . . ? N7 C32 H37 110.0 . . ? C33 C32 H37 110.0 . . ? N7 C32 H38 110.0 . . ? C33 C32 H38 110.0 . . ? H37 C32 H38 108.3 . . ? N8 C33 C32 106.4(3) . . ? N8 C33 H39 110.5 . . ? C32 C33 H39 110.4 . . ? N8 C33 H40 110.5 . . ? C32 C33 H40 110.5 . . ? H39 C33 H40 108.6 . . ? C34 N8 C33 119.7(3) . . ? C34 N8 Fe2 127.3(3) . . ? C33 N8 Fe2 112.4(2) . . ? N8 C34 C35 125.2(4) . . ? N8 C34 H41 117.4 . . ? C35 C34 H41 117.4 . . ? C40 C35 C36 119.7(4) . . ? C40 C35 C34 122.5(4) . . ? C36 C35 C34 117.8(4) . . ? C37 C36 C35 119.3(4) . . ? C37 C36 H42 120.4 . . ? C35 C36 H42 120.4 . . ? C36 C37 C38 122.5(4) . . ? C36 C37 F4 119.1(5) . . ? C38 C37 F4 118.4(5) . . ? C37 C38 C39 119.0(5) . . ? C37 C38 H43 120.5 . . ? C39 C38 H43 120.5 . . ? C38 C39 C40 121.4(5) . . ? C38 C39 H44 119.3 . . ? C40 C39 H44 119.3 . . ? O4 C40 C35 122.4(4) . . ? O4 C40 C39 119.4(4) . . ? C35 C40 C39 118.1(4) . . ? C40 O4 Fe2 133.3(3) . . ? O7 Cl1 O12 117.6(8) . . ? O7 Cl1 O5 106.7(7) . . ? O12 Cl1 O5 97.5(8) . . ? O7 Cl1 O6 112.9(4) . . ? O12 Cl1 O6 108.4(3) . . ? O5 Cl1 O6 112.7(4) . . ? O10 Cl2 O11 115.6(5) . . ? O10 Cl2 O8 108.6(5) . . ? O11 Cl2 O8 100.6(5) . . ? O10 Cl2 O9 114.9(4) . . ? O11 Cl2 O9 108.4(3) . . ? O8 Cl2 O9 107.6(4) . . ? 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 O1 1.912(3) . ? Fe1 O2 1.919(3) . ? Fe1 N4 2.081(3) . ? Fe1 N1 2.090(3) . ? Fe1 N3 2.168(3) . ? Fe1 N2 2.185(3) . ? O1 C1 1.321(4) . ? C1 C2 1.415(6) . ? C1 C6 1.422(5) . ? C2 C3 1.395(6) . ? C2 H1 0.9300 . ? C3 C4 1.381(7) . ? C3 H2 0.9300 . ? C4 C5 1.367(7) . ? C4 F1 1.378(5) . ? C5 C6 1.421(5) . ? C5 H3 0.9300 . ? C6 C7 1.451(6) . ? C7 N1 1.284(5) . ? C7 H4 0.9300 . ? N1 C8 1.487(5) . ? C8 C9 1.516(6) . ? C8 H5 0.9700 . ? C8 H6 0.9700 . ? C9 N2 1.480(5) . ? C9 H7 0.9700 . ? C9 H8 0.9700 . ? N2 C10 1.499(5) . ? N2 H9 0.99(5) . ? C10 C11 1.527(6) . ? C10 H10 0.9700 . ? C10 H11 0.9700 . ? C11 N3 1.472(5) . ? C11 H12 0.9700 . ? C11 H13 0.9700 . ? N3 C12 1.491(6) . ? N3 H14 0.75(5) . ? C12 C13 1.515(6) . ? C12 H15 0.9700 . ? C12 H16 0.9700 . ? C13 N4 1.467(5) . ? C13 H17 0.9700 . ? C13 H18 0.9700 . ? N4 C14 1.294(5) . ? C14 C15 1.438(6) . ? C14 H19 0.9300 . ? C15 C16 1.415(6) . ? C15 C20 1.425(5) . ? C16 C17 1.362(6) . ? C16 H20 0.9300 . ? C17 F2 1.375(5) . ? C17 C18 1.388(6) . ? C18 C19 1.373(6) . ? C18 H21 0.9300 . ? C19 C20 1.416(6) . ? C19 H22 0.9300 . ? C20 O2 1.330(5) . ? Fe2 O3 1.913(3) . ? Fe2 O4 1.923(3) . ? Fe2 N8 2.123(3) . ? Fe2 N5 2.131(4) . ? Fe2 N6 2.212(4) . ? Fe2 N7 2.220(4) . ? O3 C21 1.327(4) . ? C21 C26 1.410(6) . ? C21 C22 1.414(5) . ? C22 C23 1.378(6) . ? C22 H23 0.9300 . ? C23 C24 1.383(7) . ? C23 H24 0.9300 . ? C24 C25 1.358(7) . ? C24 F3 1.375(5) . ? C25 C26 1.404(6) . ? C25 H25 0.9300 . ? C26 C27 1.445(6) . ? C27 N5 1.282(6) . ? C27 H26 0.9300 . ? N5 C28 1.478(6) . ? C28 C29 1.400(7) . ? C28 H27 0.9700 . ? C28 H28 0.9700 . ? C29 N6 1.460(8) . ? C29 H29 0.9700 . ? C29 H30 0.9700 . ? N6 C30 1.489(6) . ? N6 H31 0.89(6) . ? C30 C31 1.511(7) . ? C30 H32 0.9700 . ? C30 H33 0.9700 . ? C31 N7 1.477(6) . ? C31 H34 0.9700 . ? C31 H35 0.9700 . ? N7 C32 1.485(6) . ? N7 H36 0.81(5) . ? C32 C33 1.502(7) . ? C32 H37 0.9700 . ? C32 H38 0.9700 . ? C33 N8 1.478(5) . ? C33 H39 0.9700 . ? C33 H40 0.9700 . ? N8 C34 1.282(5) . ? C34 C35 1.444(6) . ? C34 H41 0.9300 . ? C35 C40 1.408(6) . ? C35 C36 1.414(6) . ? C36 C37 1.369(7) . ? C36 H42 0.9300 . ? C37 C38 1.371(7) . ? C37 F4 1.374(5) . ? C38 C39 1.381(7) . ? C38 H43 0.9300 . ? C39 C40 1.414(7) . ? C39 H44 0.9300 . ? C40 O4 1.334(5) . ? Cl1 O7 1.296(6) . ? Cl1 O12 1.305(7) . ? Cl1 O5 1.371(7) . ? Cl1 O6 1.426(4) . ? Cl2 O10 1.369(5) . ? Cl2 O11 1.383(5) . ? Cl2 O8 1.421(7) . ? Cl2 O9 1.426(4) . ?