#------------------------------------------------------------------------------ #$Date: 2021-10-11 01:56:38 +0300 (Mon, 11 Oct 2021) $ #$Revision: 269885 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/85/7708536.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_7708536 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 112.406(8) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 19.049(7) _cell_length_b 12.722(5) _cell_length_c 19.512(7) _cell_measurement_reflns_used 7630 _cell_measurement_temperature 104(2) _cell_measurement_theta_max 24.99 _cell_measurement_theta_min 2.48 _cell_volume 4372(3) _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 104(2) _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _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 0.0357 _diffrn_reflns_av_unetI/netI 0.0597 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 13517 _diffrn_reflns_point_group_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_theta_full 24.999 _diffrn_reflns_theta_max 24.999 _diffrn_reflns_theta_min 2.484 _exptl_absorpt_coefficient_mu 0.876 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS; Bruker, 2000' _exptl_crystal_colour black _exptl_crystal_density_diffrn 1.652 _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 0.110 _exptl_crystal_size_min 0.100 _exptl_transmission_factor_max 0.916 _exptl_transmission_factor_min 0.892 _refine_diff_density_max 1.360 _refine_diff_density_min -1.114 _refine_diff_density_rms 0.088 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 629 _refine_ls_number_reflns 7630 _refine_ls_number_restraints 13 _refine_ls_restrained_S_all 1.150 _refine_ls_R_factor_all 0.0739 _refine_ls_R_factor_gt 0.0545 _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^)+(0.0378P)^2^+12.5114P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1263 _refine_ls_wR_factor_ref 0.1367 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6021 _reflns_number_total 7630 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt02394b2.cif _cod_data_source_block 111 _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_absorpt_correction_type' value 'Multi-scan' was changed to 'multi-scan' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas ; _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 7708536 _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 0.895 _shelx_estimated_absorpt_t_max 0.917 _shelx_res_file ; 111.res created by SHELXL-2014/7 TITL 111 CELL 0.71073 19.0487 12.7223 19.5123 90.0000 112.4063 90.0000 ZERR 8.0 0.0072 0.0046 0.0070 0.0000 0.0077 0.0000 LATT 1 SYMM 0.50000-X, 0.50000+Y, 0.50000-Z SFAC C H N O F Cl Fe UNIT 160 176 32 48 16 8 8 omit 2 0 0 OMIT -2 50 L.S. 14 ACTA BOND $H FMAP 2 PLAN -10 size 0.10 0.11 0.13 DFIX 1.50 0.01 C28 C29 ISOR 0.005 C28 C29 TEMP -169.3 WGHT 0.037800 12.511400 FVAR 0.06512 FE1 7 0.817400 0.308821 0.774894 11.00000 0.01683 0.01992 = 0.01899 -0.00139 0.00556 -0.00018 O1 4 0.812998 0.362831 0.684073 11.00000 0.01980 0.02853 = 0.02780 0.00436 0.00925 0.00030 C1 1 0.751121 0.377714 0.623251 11.00000 0.02785 0.01539 = 0.02642 -0.00380 0.01294 0.00286 C2 1 0.759091 0.431647 0.563488 11.00000 0.02978 0.02636 = 0.02965 -0.00038 0.01296 -0.00368 AFIX 43 H1 2 0.808193 0.452587 0.566923 11.00000 -1.20000 AFIX 0 C3 1 0.696921 0.454467 0.500251 11.00000 0.04547 0.02616 = 0.02346 -0.00186 0.01454 -0.00890 AFIX 43 H2 2 0.703033 0.490883 0.460380 11.00000 -1.20000 AFIX 0 C4 1 0.625474 0.423872 0.495318 11.00000 0.03638 0.02518 = 0.02067 -0.00481 -0.00329 -0.00602 C5 1 0.614213 0.367083 0.550023 11.00000 0.02630 0.02214 = 0.02699 -0.00611 0.00456 -0.00599 AFIX 43 H3 2 0.564666 0.345066 0.544419 11.00000 -1.20000 AFIX 0 F1 5 0.563779 0.448920 0.432886 11.00000 0.04515 0.05299 = 0.03046 0.00771 -0.00681 -0.01772 C6 1 0.677587 0.341928 0.614826 11.00000 0.02605 0.01580 = 0.02161 -0.00368 0.01038 0.00033 C7 1 0.664415 0.274244 0.667945 11.00000 0.01778 0.01673 = 0.02971 -0.00688 0.00870 -0.00370 AFIX 43 H4 2 0.614005 0.250361 0.656802 11.00000 -1.20000 AFIX 0 N1 3 0.715927 0.243941 0.729220 11.00000 0.02036 0.01714 = 0.02709 0.00091 0.01118 -0.00146 C8 1 0.693508 0.173331 0.777792 11.00000 0.02673 0.02527 = 0.02857 0.00269 0.01393 -0.00276 AFIX 23 H5 2 0.704815 0.099243 0.770313 11.00000 -1.20000 H6 2 0.638508 0.179902 0.766904 11.00000 -1.20000 AFIX 0 C9 1 0.739464 0.207741 0.856132 11.00000 0.03010 0.02407 = 0.03134 0.00357 0.01776 -0.00059 AFIX 23 H7 2 0.718985 0.274454 0.866966 11.00000 -1.20000 H8 2 0.736664 0.153785 0.891562 11.00000 -1.20000 AFIX 0 N2 3 0.820131 0.222656 0.864143 11.00000 0.02579 0.01656 = 0.02130 0.00017 0.00850 -0.00070 H9 2 0.842860 0.260448 0.905174 11.00000 0.02196 C10 1 0.862867 0.121752 0.871605 11.00000 0.03144 0.01974 = 0.02839 0.00557 0.01117 0.00292 AFIX 23 H10 2 0.836942 0.065130 0.887722 11.00000 -1.20000 H11 2 0.914770 0.129661 0.909715 11.00000 -1.20000 AFIX 0 C11 1 0.867262 0.092590 0.798411 11.00000 0.03247 0.01660 = 0.03083 0.00047 0.00968 0.00334 AFIX 23 H12 2 0.907416 0.039282 0.806087 11.00000 -1.20000 H13 2 0.818246 0.062703 0.764760 11.00000 -1.20000 AFIX 0 N3 3 0.884813 0.188590 0.765783 11.00000 0.03042 0.02517 = 0.02001 -0.00076 0.01212 0.00460 H14 2 0.874661 0.176928 0.723143 11.00000 0.02338 C12 1 0.966401 0.218047 0.801191 11.00000 0.02761 0.02945 = 0.03954 0.00349 0.01740 0.00874 AFIX 23 H15 2 0.995613 0.183627 0.774974 11.00000 -1.20000 H16 2 0.987339 0.194633 0.853525 11.00000 -1.20000 AFIX 0 C13 1 0.972864 0.337037 0.797309 11.00000 0.02081 0.03622 = 0.02323 0.00641 0.01096 0.00556 AFIX 23 H17 2 1.024187 0.360942 0.830036 11.00000 -1.20000 H18 2 0.963142 0.359669 0.745947 11.00000 -1.20000 AFIX 0 N4 3 0.914925 0.380303 0.822312 11.00000 0.01997 0.02248 = 0.02074 0.00639 0.00474 0.00341 C14 1 0.930428 0.457520 0.867958 11.00000 0.02252 0.02128 = 0.01994 0.00653 0.00506 -0.00213 AFIX 43 H19 2 0.980354 0.485739 0.885324 11.00000 -1.20000 AFIX 0 C15 1 0.876114 0.504215 0.894575 11.00000 0.02472 0.01821 = 0.02200 0.00631 0.00739 0.00234 C16 1 0.903401 0.573059 0.955593 11.00000 0.02794 0.01949 = 0.02566 0.00234 0.00417 -0.00165 AFIX 43 H20 2 0.955759 0.590784 0.977033 11.00000 -1.20000 AFIX 0 C17 1 0.853479 0.614010 0.983525 11.00000 0.04041 0.01742 = 0.02317 0.00273 0.01034 0.00199 F2 5 0.880472 0.676829 1.045095 11.00000 0.05548 0.03221 = 0.02832 -0.00996 0.01329 0.00010 C18 1 0.775930 0.595052 0.952341 11.00000 0.03841 0.02470 = 0.02811 0.00554 0.01768 0.00735 AFIX 43 H21 2 0.742594 0.627067 0.972021 11.00000 -1.20000 AFIX 0 C19 1 0.748197 0.528064 0.891591 11.00000 0.02440 0.02547 = 0.02423 0.00497 0.00880 0.00468 AFIX 43 H22 2 0.695292 0.513792 0.869923 11.00000 -1.20000 AFIX 0 C20 1 0.797159 0.480843 0.861488 11.00000 0.02810 0.01583 = 0.01904 0.00716 0.00818 0.00428 O2 4 0.766303 0.418516 0.802861 11.00000 0.02035 0.02521 = 0.02275 -0.00315 0.00742 0.00517 O3 4 0.326695 0.104024 0.718503 11.00000 0.02924 0.04143 = 0.02543 -0.00738 -0.00052 0.01383 C21 1 0.390734 0.103221 0.776610 11.00000 0.02400 0.02082 = 0.02408 0.00123 0.00376 -0.00118 C22 1 0.456233 0.059976 0.769839 11.00000 0.03182 0.02221 = 0.03044 -0.00364 0.01475 -0.00058 AFIX 43 H23 2 0.453868 0.037610 0.722556 11.00000 -1.20000 AFIX 0 C23 1 0.523442 0.049648 0.830519 11.00000 0.02248 0.02837 = 0.04805 -0.00834 0.01041 -0.00001 AFIX 43 H24 2 0.567125 0.020236 0.825599 11.00000 -1.20000 AFIX 0 FE2 7 0.225517 0.148234 0.701050 11.00000 0.02220 0.02067 = 0.02520 -0.00264 0.00002 0.00070 C24 1 0.525588 0.083106 0.898485 11.00000 0.02756 0.03505 = 0.04507 -0.01255 -0.00469 0.00533 C25 1 0.465775 0.129739 0.907817 11.00000 0.03558 0.03661 = 0.02912 -0.01489 0.00234 0.00421 AFIX 43 H25 2 0.470153 0.153468 0.955440 11.00000 -1.20000 AFIX 0 C26 1 0.397352 0.142567 0.846379 11.00000 0.02272 0.02355 = 0.03121 -0.00659 0.00604 -0.00116 C27 1 0.337430 0.202189 0.856035 11.00000 0.03117 0.05210 = 0.03971 -0.02994 0.00820 -0.00192 AFIX 43 H26 2 0.346973 0.229537 0.904064 11.00000 -1.20000 AFIX 0 F3 5 0.592112 0.069771 0.958917 11.00000 0.03930 0.08106 = 0.05506 -0.03338 -0.02298 0.02744 N5 3 0.272742 0.221263 0.805524 11.00000 0.02624 0.06414 = 0.05849 -0.04538 -0.00389 0.01000 C28 1 0.221155 0.287212 0.825156 11.00000 0.06825 0.11120 = 0.09972 -0.06286 0.01727 0.02808 AFIX 23 H27 2 0.207585 0.250841 0.863256 11.00000 -1.20000 H28 2 0.247441 0.353387 0.847176 11.00000 -1.20000 AFIX 0 C29 1 0.156062 0.310879 0.765945 11.00000 0.11596 0.13903 = 0.07208 0.01571 0.05207 0.08149 AFIX 23 H29 2 0.154163 0.388384 0.761048 11.00000 -1.20000 H30 2 0.113095 0.290279 0.779790 11.00000 -1.20000 AFIX 0 N6 3 0.140605 0.269468 0.694233 11.00000 0.03207 0.05242 = 0.04730 0.02222 0.02479 0.01539 H31 2 0.095218 0.236314 0.679235 11.00000 0.07074 C30 1 0.133856 0.350899 0.638552 11.00000 0.02773 0.02080 = 0.03218 0.00198 0.00875 0.00423 AFIX 23 H32 2 0.120797 0.419046 0.655165 11.00000 -1.20000 H33 2 0.092709 0.331997 0.590941 11.00000 -1.20000 AFIX 0 C31 1 0.208575 0.360971 0.627631 11.00000 0.02838 0.02536 = 0.03010 0.00243 0.00762 -0.00399 AFIX 23 H34 2 0.201565 0.405926 0.584095 11.00000 -1.20000 H35 2 0.247384 0.393927 0.671833 11.00000 -1.20000 AFIX 0 N7 3 0.233816 0.255080 0.616055 11.00000 0.01392 0.03306 = 0.03268 -0.00139 0.00855 -0.00242 H36 2 0.280362 0.253433 0.623383 11.00000 0.01519 C32 1 0.192720 0.212133 0.540540 11.00000 0.03222 0.04276 = 0.02553 -0.00405 0.01592 -0.00745 AFIX 23 H37 2 0.216206 0.238290 0.506453 11.00000 -1.20000 H38 2 0.139068 0.235322 0.521526 11.00000 -1.20000 AFIX 0 C33 1 0.196682 0.092762 0.544261 11.00000 0.02731 0.04103 = 0.03632 -0.01133 0.01746 -0.00171 AFIX 23 H39 2 0.163287 0.061857 0.496340 11.00000 -1.20000 H40 2 0.249326 0.068538 0.555645 11.00000 -1.20000 AFIX 0 N8 3 0.171349 0.061591 0.603143 11.00000 0.02202 0.02270 = 0.02793 -0.00558 0.00634 0.00322 C34 1 0.115306 -0.002489 0.589308 11.00000 0.02540 0.02296 = 0.02644 -0.00734 0.00324 0.00185 AFIX 43 H41 2 0.093004 -0.029439 0.540308 11.00000 -1.20000 AFIX 0 C35 1 0.083487 -0.036865 0.641649 11.00000 0.02946 0.01753 = 0.02398 0.00109 0.00470 0.00154 C36 1 0.016813 -0.098187 0.615993 11.00000 0.03287 0.03195 = 0.02877 0.00004 0.00743 -0.00023 AFIX 43 H42 2 -0.005869 -0.116815 0.565081 11.00000 -1.20000 AFIX 0 C37 1 -0.015003 -0.130622 0.663704 11.00000 0.03087 0.03255 = 0.04004 0.00292 0.01373 -0.00015 F4 5 -0.080928 -0.188511 0.637657 11.00000 0.03981 0.06028 = 0.05373 0.00515 0.01882 -0.01294 C38 1 0.016771 -0.107626 0.738675 11.00000 0.05547 0.03719 = 0.04123 0.00694 0.02237 0.00270 AFIX 43 H43 2 -0.005720 -0.132834 0.771394 11.00000 -1.20000 AFIX 0 C39 1 0.082413 -0.046736 0.765032 11.00000 0.06162 0.02953 = 0.02835 0.00723 0.00905 0.00365 AFIX 43 H44 2 0.104411 -0.029684 0.816260 11.00000 -1.20000 AFIX 0 C40 1 0.116794 -0.009992 0.717460 11.00000 0.04541 0.01799 = 0.02795 0.00361 0.00557 0.00335 O4 4 0.179530 0.048340 0.745573 11.00000 0.06160 0.02701 = 0.02116 0.00326 -0.00166 -0.01408 CL1 6 0.919252 0.288786 0.070016 11.00000 0.02046 0.03959 = 0.03066 0.00480 0.00945 0.00069 CL2 6 0.935632 0.206327 0.583310 11.00000 0.02844 0.03183 = 0.02429 -0.00401 0.01234 -0.00340 O5 4 0.962005 0.296376 0.627306 11.00000 0.10071 0.10109 = 0.15342 -0.08983 0.09945 -0.05816 O6 4 0.867359 0.229030 0.523690 11.00000 0.03970 0.17236 = 0.05296 0.04252 0.01874 0.02093 O7 4 0.919712 0.125673 0.626499 11.00000 0.06617 0.07211 = 0.08697 0.03351 0.05004 0.01544 O8 4 0.992763 0.172997 0.555957 11.00000 0.03860 0.04022 = 0.04576 -0.01158 0.02429 -0.00132 O9 4 0.866767 0.208989 0.068393 11.00000 0.06557 0.06266 = 0.13800 -0.02179 0.06990 -0.02961 O10 4 0.939127 0.283397 0.006221 11.00000 0.04040 0.07456 = 0.03329 -0.01759 0.01607 -0.01646 O11 4 0.986194 0.282982 0.134870 11.00000 0.04052 0.12974 = 0.04486 0.02298 0.01543 0.00775 O12 4 0.886621 0.390420 0.071652 11.00000 0.09076 0.05332 = 0.09562 0.01772 0.05320 0.03075 HKLF 4 REM 111 REM R1 = 0.0545 for 6021 Fo > 4sig(Fo) and 0.0739 for all 7630 data REM 629 parameters refined using 13 restraints END WGHT 0.0417 14.7927 REM Highest difference peak 1.360, deepest hole -1.114, 1-sigma level 0.088 Q1 1 0.1831 0.3483 0.7757 11.00000 0.05 1.36 Q2 1 0.2175 0.3216 0.7989 11.00000 0.05 1.28 Q3 1 0.1418 0.2633 0.7630 11.00000 0.05 1.16 Q4 1 0.9765 0.2042 0.6608 11.00000 0.05 0.88 Q5 1 0.2041 0.2481 0.8321 11.00000 0.05 0.84 Q6 1 0.9122 0.3096 0.5616 11.00000 0.05 0.69 Q7 1 0.2203 0.3995 0.7761 11.00000 0.05 0.62 Q8 1 0.7777 0.3334 0.7271 11.00000 0.05 0.59 Q9 1 0.8834 0.1280 0.5592 11.00000 0.05 0.59 Q10 1 0.9757 0.2068 0.1045 11.00000 0.05 0.56 ; _shelx_res_checksum 22762 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 0.81740(3) 0.30882(5) 0.77489(3) 0.01896(15) Uani 1 1 d . . . . . O1 O 0.81300(15) 0.3628(2) 0.68407(16) 0.0253(7) Uani 1 1 d . . . . . C1 C 0.7511(2) 0.3777(3) 0.6233(2) 0.0224(9) Uani 1 1 d . . . . . C2 C 0.7591(3) 0.4316(3) 0.5635(2) 0.0281(10) Uani 1 1 d . . . . . H1 H 0.8082 0.4526 0.5669 0.034 Uiso 1 1 calc R U . . . C3 C 0.6969(3) 0.4545(4) 0.5003(2) 0.0313(11) Uani 1 1 d . . . . . H2 H 0.7030 0.4909 0.4604 0.038 Uiso 1 1 calc R U . . . C4 C 0.6255(3) 0.4239(4) 0.4953(2) 0.0316(11) Uani 1 1 d . . . . . C5 C 0.6142(2) 0.3671(3) 0.5500(2) 0.0268(10) Uani 1 1 d . . . . . H3 H 0.5647 0.3451 0.5444 0.032 Uiso 1 1 calc R U . . . F1 F 0.56378(17) 0.4489(2) 0.43289(15) 0.0492(8) Uani 1 1 d . . . . . C6 C 0.6776(2) 0.3419(3) 0.6148(2) 0.0208(9) Uani 1 1 d . . . . . C7 C 0.6644(2) 0.2742(3) 0.6679(2) 0.0215(9) Uani 1 1 d . . . . . H4 H 0.6140 0.2504 0.6568 0.026 Uiso 1 1 calc R U . . . N1 N 0.71593(18) 0.2439(3) 0.72922(19) 0.0209(7) Uani 1 1 d . . . . . C8 C 0.6935(2) 0.1733(3) 0.7778(2) 0.0258(10) Uani 1 1 d . . . . . H5 H 0.7048 0.0992 0.7703 0.031 Uiso 1 1 calc R U . . . H6 H 0.6385 0.1799 0.7669 0.031 Uiso 1 1 calc R U . . . C9 C 0.7395(2) 0.2077(3) 0.8561(2) 0.0267(10) Uani 1 1 d . . . . . H7 H 0.7190 0.2745 0.8670 0.032 Uiso 1 1 calc R U . . . H8 H 0.7367 0.1538 0.8916 0.032 Uiso 1 1 calc R U . . . N2 N 0.8201(2) 0.2227(3) 0.8641(2) 0.0214(8) Uani 1 1 d . . . . . H9 H 0.843(2) 0.260(4) 0.905(2) 0.022(12) Uiso 1 1 d . . . . . C10 C 0.8629(3) 0.1218(3) 0.8716(2) 0.0266(10) Uani 1 1 d . . . . . H10 H 0.8369 0.0651 0.8877 0.032 Uiso 1 1 calc R U . . . H11 H 0.9148 0.1297 0.9097 0.032 Uiso 1 1 calc R U . . . C11 C 0.8673(3) 0.0926(3) 0.7984(2) 0.0273(10) Uani 1 1 d . . . . . H12 H 0.9074 0.0393 0.8061 0.033 Uiso 1 1 calc R U . . . H13 H 0.8182 0.0627 0.7648 0.033 Uiso 1 1 calc R U . . . N3 N 0.8848(2) 0.1886(3) 0.7658(2) 0.0245(8) Uani 1 1 d . . . . . H14 H 0.875(3) 0.177(4) 0.723(3) 0.023(13) Uiso 1 1 d . . . . . C12 C 0.9664(2) 0.2180(4) 0.8012(3) 0.0308(10) Uani 1 1 d . . . . . H15 H 0.9956 0.1836 0.7750 0.037 Uiso 1 1 calc R U . . . H16 H 0.9873 0.1946 0.8535 0.037 Uiso 1 1 calc R U . . . C13 C 0.9729(2) 0.3370(4) 0.7973(2) 0.0260(10) Uani 1 1 d . . . . . H17 H 1.0242 0.3609 0.8300 0.031 Uiso 1 1 calc R U . . . H18 H 0.9631 0.3597 0.7459 0.031 Uiso 1 1 calc R U . . . N4 N 0.91493(18) 0.3803(3) 0.82231(18) 0.0220(8) Uani 1 1 d . . . . . C14 C 0.9304(2) 0.4575(3) 0.8680(2) 0.0222(9) Uani 1 1 d . . . . . H19 H 0.9804 0.4857 0.8853 0.027 Uiso 1 1 calc R U . . . C15 C 0.8761(2) 0.5042(3) 0.8946(2) 0.0221(9) Uani 1 1 d . . . . . C16 C 0.9034(2) 0.5731(3) 0.9556(2) 0.0262(10) Uani 1 1 d . . . . . H20 H 0.9558 0.5908 0.9770 0.031 Uiso 1 1 calc R U . . . C17 C 0.8535(3) 0.6140(3) 0.9835(2) 0.0275(10) Uani 1 1 d . . . . . F2 F 0.88047(17) 0.6768(2) 1.04510(14) 0.0395(7) Uani 1 1 d . . . . . C18 C 0.7759(3) 0.5951(3) 0.9523(2) 0.0289(10) Uani 1 1 d . . . . . H21 H 0.7426 0.6271 0.9720 0.035 Uiso 1 1 calc R U . . . C19 C 0.7482(2) 0.5281(3) 0.8916(2) 0.0248(9) Uani 1 1 d . . . . . H22 H 0.6953 0.5138 0.8699 0.030 Uiso 1 1 calc R U . . . C20 C 0.7972(2) 0.4808(3) 0.8615(2) 0.0212(9) Uani 1 1 d . . . . . O2 O 0.76630(15) 0.4185(2) 0.80286(15) 0.0230(6) Uani 1 1 d . . . . . O3 O 0.32669(17) 0.1040(3) 0.71850(17) 0.0353(8) Uani 1 1 d . . . . . C21 C 0.3907(2) 0.1032(3) 0.7766(2) 0.0246(9) Uani 1 1 d . . . . . C22 C 0.4562(2) 0.0600(3) 0.7698(2) 0.0273(10) Uani 1 1 d . . . . . H23 H 0.4539 0.0376 0.7226 0.033 Uiso 1 1 calc R U . . . C23 C 0.5234(2) 0.0496(4) 0.8305(3) 0.0339(11) Uani 1 1 d . . . . . H24 H 0.5671 0.0202 0.8256 0.041 Uiso 1 1 calc R U . . . Fe2 Fe 0.22552(3) 0.14823(5) 0.70105(3) 0.02537(17) Uani 1 1 d . . . . . C24 C 0.5256(3) 0.0831(4) 0.8985(3) 0.0414(13) Uani 1 1 d . . . . . C25 C 0.4658(3) 0.1297(4) 0.9078(3) 0.0367(12) Uani 1 1 d . . . . . H25 H 0.4702 0.1535 0.9554 0.044 Uiso 1 1 calc R U . . . C26 C 0.3974(2) 0.1426(3) 0.8464(2) 0.0271(10) Uani 1 1 d . . . . . C27 C 0.3374(3) 0.2022(4) 0.8560(3) 0.0426(13) Uani 1 1 d . . . . . H26 H 0.3470 0.2295 0.9041 0.051 Uiso 1 1 calc R U . . . F3 F 0.59211(17) 0.0698(3) 0.95892(18) 0.0707(12) Uani 1 1 d . . . . . N5 N 0.2727(2) 0.2213(4) 0.8055(3) 0.0556(14) Uani 1 1 d . . . . . C28 C 0.2212(4) 0.2872(7) 0.8252(4) 0.097(3) Uani 1 1 d D U . . . H27 H 0.2076 0.2508 0.8633 0.117 Uiso 1 1 calc R U . . . H28 H 0.2474 0.3534 0.8472 0.117 Uiso 1 1 calc R U . . . C29 C 0.1561(5) 0.3109(8) 0.7659(4) 0.104(3) Uani 1 1 d D U . . . H29 H 0.1542 0.3884 0.7610 0.125 Uiso 1 1 calc R U . . . H30 H 0.1131 0.2903 0.7798 0.125 Uiso 1 1 calc R U . . . N6 N 0.1406(2) 0.2695(4) 0.6942(3) 0.0411(11) Uani 1 1 d . . . . . H31 H 0.095(4) 0.236(5) 0.679(3) 0.07(2) Uiso 1 1 d . . . . . C30 C 0.1339(2) 0.3509(3) 0.6386(3) 0.0277(10) Uani 1 1 d . . . . . H32 H 0.1208 0.4190 0.6552 0.033 Uiso 1 1 calc R U . . . H33 H 0.0927 0.3320 0.5909 0.033 Uiso 1 1 calc R U . . . C31 C 0.2086(2) 0.3610(3) 0.6276(3) 0.0290(10) Uani 1 1 d . . . . . H34 H 0.2016 0.4059 0.5841 0.035 Uiso 1 1 calc R U . . . H35 H 0.2474 0.3939 0.6718 0.035 Uiso 1 1 calc R U . . . N7 N 0.2338(2) 0.2551(3) 0.6161(2) 0.0267(8) Uani 1 1 d . . . . . H36 H 0.280(2) 0.253(3) 0.623(2) 0.015(10) Uiso 1 1 d . . . . . C32 C 0.1927(3) 0.2121(4) 0.5405(2) 0.0320(11) Uani 1 1 d . . . . . H37 H 0.2162 0.2383 0.5065 0.038 Uiso 1 1 calc R U . . . H38 H 0.1391 0.2353 0.5215 0.038 Uiso 1 1 calc R U . . . C33 C 0.1967(3) 0.0928(4) 0.5443(3) 0.0333(11) Uani 1 1 d . . . . . H39 H 0.1633 0.0619 0.4963 0.040 Uiso 1 1 calc R U . . . H40 H 0.2493 0.0685 0.5556 0.040 Uiso 1 1 calc R U . . . N8 N 0.17135(19) 0.0616(3) 0.6031(2) 0.0252(8) Uani 1 1 d . . . . . C34 C 0.1153(2) -0.0025(3) 0.5893(2) 0.0269(10) Uani 1 1 d . . . . . H41 H 0.0930 -0.0294 0.5403 0.032 Uiso 1 1 calc R U . . . C35 C 0.0835(2) -0.0369(3) 0.6416(2) 0.0253(9) Uani 1 1 d . . . . . C36 C 0.0168(3) -0.0982(4) 0.6160(3) 0.0325(11) Uani 1 1 d . . . . . H42 H -0.0059 -0.1168 0.5651 0.039 Uiso 1 1 calc R U . . . C37 C -0.0150(3) -0.1306(4) 0.6637(3) 0.0344(11) Uani 1 1 d . . . . . F4 F -0.08093(16) -0.1885(3) 0.63766(17) 0.0510(8) Uani 1 1 d . . . . . C38 C 0.0168(3) -0.1076(4) 0.7387(3) 0.0435(13) Uani 1 1 d . . . . . H43 H -0.0057 -0.1328 0.7714 0.052 Uiso 1 1 calc R U . . . C39 C 0.0824(3) -0.0467(4) 0.7650(3) 0.0422(13) Uani 1 1 d . . . . . H44 H 0.1044 -0.0297 0.8163 0.051 Uiso 1 1 calc R U . . . C40 C 0.1168(3) -0.0100(3) 0.7175(3) 0.0330(11) Uani 1 1 d . . . . . O4 O 0.1795(2) 0.0483(3) 0.74557(17) 0.0418(9) Uani 1 1 d . . . . . Cl1 Cl 0.91925(6) 0.28879(9) 0.07002(6) 0.0303(3) Uani 1 1 d . . . . . Cl2 Cl 0.93563(6) 0.20633(9) 0.58331(6) 0.0275(2) Uani 1 1 d . . . . . O5 O 0.9620(3) 0.2964(4) 0.6273(3) 0.103(2) Uani 1 1 d . . . . . O6 O 0.8674(2) 0.2290(5) 0.5237(2) 0.0880(18) Uani 1 1 d . . . . . O7 O 0.9197(2) 0.1257(4) 0.6265(3) 0.0689(13) Uani 1 1 d . . . . . O8 O 0.99276(19) 0.1730(3) 0.55596(19) 0.0391(8) Uani 1 1 d . . . . . O9 O 0.8668(3) 0.2090(4) 0.0684(3) 0.0795(15) Uani 1 1 d . . . . . O10 O 0.9391(2) 0.2834(3) 0.00622(19) 0.0488(10) Uani 1 1 d . . . . . O11 O 0.9862(2) 0.2830(4) 0.1349(2) 0.0720(14) Uani 1 1 d . . . . . O12 O 0.8866(3) 0.3904(4) 0.0717(3) 0.0746(14) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0168(3) 0.0199(3) 0.0190(3) -0.0014(2) 0.0056(2) -0.0002(2) O1 0.0198(15) 0.0285(16) 0.0278(16) 0.0044(13) 0.0092(13) 0.0003(12) C1 0.028(2) 0.015(2) 0.026(2) -0.0038(18) 0.0129(19) 0.0029(17) C2 0.030(2) 0.026(2) 0.030(2) 0.000(2) 0.013(2) -0.0037(19) C3 0.045(3) 0.026(2) 0.023(2) -0.002(2) 0.015(2) -0.009(2) C4 0.036(3) 0.025(2) 0.021(2) -0.005(2) -0.003(2) -0.006(2) C5 0.026(2) 0.022(2) 0.027(2) -0.0061(19) 0.0046(19) -0.0060(18) F1 0.0452(17) 0.0530(19) 0.0305(15) 0.0077(14) -0.0068(13) -0.0177(15) C6 0.026(2) 0.016(2) 0.022(2) -0.0037(17) 0.0104(18) 0.0003(17) C7 0.018(2) 0.017(2) 0.030(2) -0.0069(18) 0.0087(18) -0.0037(16) N1 0.0204(17) 0.0171(17) 0.0271(19) 0.0009(15) 0.0112(15) -0.0015(14) C8 0.027(2) 0.025(2) 0.029(2) 0.0027(19) 0.0139(19) -0.0028(18) C9 0.030(2) 0.024(2) 0.031(2) 0.004(2) 0.018(2) -0.0006(18) N2 0.0258(19) 0.0166(17) 0.0213(19) 0.0002(15) 0.0085(15) -0.0007(14) C10 0.031(2) 0.020(2) 0.028(2) 0.0056(19) 0.011(2) 0.0029(18) C11 0.032(2) 0.017(2) 0.031(2) 0.0005(19) 0.010(2) 0.0033(18) N3 0.030(2) 0.025(2) 0.020(2) -0.0008(17) 0.0121(16) 0.0046(16) C12 0.028(2) 0.029(2) 0.040(3) 0.003(2) 0.017(2) 0.0087(19) C13 0.021(2) 0.036(3) 0.023(2) 0.006(2) 0.0110(18) 0.0056(18) N4 0.0200(17) 0.0225(19) 0.0207(18) 0.0064(16) 0.0047(14) 0.0034(14) C14 0.023(2) 0.021(2) 0.020(2) 0.0065(18) 0.0051(17) -0.0021(17) C15 0.025(2) 0.018(2) 0.022(2) 0.0063(18) 0.0074(18) 0.0023(17) C16 0.028(2) 0.019(2) 0.026(2) 0.0023(19) 0.0042(19) -0.0017(18) C17 0.040(3) 0.017(2) 0.023(2) 0.0027(19) 0.010(2) 0.0020(19) F2 0.0555(18) 0.0322(15) 0.0283(14) -0.0100(12) 0.0133(13) 0.0001(13) C18 0.038(3) 0.025(2) 0.028(2) 0.006(2) 0.018(2) 0.007(2) C19 0.024(2) 0.025(2) 0.024(2) 0.0050(19) 0.0088(18) 0.0047(18) C20 0.028(2) 0.016(2) 0.019(2) 0.0072(17) 0.0082(18) 0.0043(17) O2 0.0204(15) 0.0252(16) 0.0227(15) -0.0032(13) 0.0074(12) 0.0052(12) O3 0.0292(17) 0.0414(19) 0.0254(17) -0.0074(15) -0.0005(14) 0.0138(15) C21 0.024(2) 0.021(2) 0.024(2) 0.0012(18) 0.0038(18) -0.0012(17) C22 0.032(2) 0.022(2) 0.030(2) -0.004(2) 0.015(2) -0.0006(18) C23 0.022(2) 0.028(2) 0.048(3) -0.008(2) 0.010(2) 0.0000(19) Fe2 0.0222(3) 0.0207(3) 0.0252(3) -0.0026(3) 0.0000(3) 0.0007(2) C24 0.028(3) 0.035(3) 0.045(3) -0.013(2) -0.005(2) 0.005(2) C25 0.036(3) 0.037(3) 0.029(3) -0.015(2) 0.002(2) 0.004(2) C26 0.023(2) 0.024(2) 0.031(2) -0.007(2) 0.0060(19) -0.0012(18) C27 0.031(3) 0.052(3) 0.040(3) -0.030(3) 0.008(2) -0.002(2) F3 0.0393(18) 0.081(3) 0.055(2) -0.0334(19) -0.0230(15) 0.0274(17) N5 0.026(2) 0.064(3) 0.058(3) -0.045(3) -0.004(2) 0.010(2) C28 0.068(4) 0.111(4) 0.100(4) -0.063(4) 0.017(3) 0.028(3) C29 0.116(4) 0.139(5) 0.072(4) 0.016(3) 0.052(3) 0.081(4) N6 0.032(2) 0.052(3) 0.047(3) 0.022(2) 0.025(2) 0.015(2) C30 0.028(2) 0.021(2) 0.032(2) 0.002(2) 0.009(2) 0.0042(18) C31 0.028(2) 0.025(2) 0.030(2) 0.002(2) 0.008(2) -0.0040(19) N7 0.0139(18) 0.033(2) 0.033(2) -0.0014(17) 0.0086(16) -0.0024(15) C32 0.032(2) 0.043(3) 0.026(2) -0.004(2) 0.016(2) -0.007(2) C33 0.027(2) 0.041(3) 0.036(3) -0.011(2) 0.017(2) -0.002(2) N8 0.0220(18) 0.0227(19) 0.028(2) -0.0056(16) 0.0063(15) 0.0032(15) C34 0.025(2) 0.023(2) 0.026(2) -0.0073(19) 0.0032(18) 0.0018(18) C35 0.029(2) 0.018(2) 0.024(2) 0.0011(18) 0.0047(19) 0.0015(18) C36 0.033(3) 0.032(3) 0.029(2) 0.000(2) 0.007(2) 0.000(2) C37 0.031(2) 0.033(3) 0.040(3) 0.003(2) 0.014(2) 0.000(2) F4 0.0398(17) 0.060(2) 0.0537(19) 0.0052(16) 0.0188(15) -0.0129(15) C38 0.055(3) 0.037(3) 0.041(3) 0.007(3) 0.022(3) 0.003(3) C39 0.062(4) 0.030(3) 0.028(3) 0.007(2) 0.009(2) 0.004(2) C40 0.045(3) 0.018(2) 0.028(2) 0.004(2) 0.006(2) 0.003(2) O4 0.062(2) 0.0270(18) 0.0212(17) 0.0033(14) -0.0017(16) -0.0141(16) Cl1 0.0205(5) 0.0396(6) 0.0307(6) 0.0048(5) 0.0095(4) 0.0007(4) Cl2 0.0284(5) 0.0318(6) 0.0243(5) -0.0040(5) 0.0123(4) -0.0034(4) O5 0.101(4) 0.101(4) 0.153(5) -0.090(4) 0.099(4) -0.058(3) O6 0.040(2) 0.172(6) 0.053(3) 0.043(3) 0.019(2) 0.021(3) O7 0.066(3) 0.072(3) 0.087(3) 0.034(3) 0.050(3) 0.015(2) O8 0.0386(19) 0.040(2) 0.046(2) -0.0116(17) 0.0243(16) -0.0013(15) O9 0.066(3) 0.063(3) 0.138(5) -0.022(3) 0.070(3) -0.030(2) O10 0.040(2) 0.075(3) 0.0333(19) -0.0176(19) 0.0161(16) -0.0165(19) O11 0.041(2) 0.130(4) 0.045(2) 0.023(3) 0.0154(19) 0.008(2) O12 0.091(3) 0.053(3) 0.096(4) 0.018(3) 0.053(3) 0.031(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 99.18(13) . . ? O1 Fe1 N4 88.22(13) . . ? O2 Fe1 N4 91.19(14) . . ? O1 Fe1 N1 92.48(13) . . ? O2 Fe1 N1 85.18(13) . . ? N4 Fe1 N1 176.37(14) . . ? O1 Fe1 N2 169.02(14) . . ? O2 Fe1 N2 89.92(13) . . ? N4 Fe1 N2 97.78(14) . . ? N1 Fe1 N2 82.11(14) . . ? O1 Fe1 N3 89.73(14) . . ? O2 Fe1 N3 169.11(14) . . ? N4 Fe1 N3 82.78(15) . . ? N1 Fe1 N3 100.77(15) . . ? N2 Fe1 N3 81.96(15) . . ? C1 O1 Fe1 127.0(3) . . ? O1 C1 C2 118.0(4) . . ? O1 C1 C6 123.8(4) . . ? C2 C1 C6 118.2(4) . . ? C3 C2 C1 121.1(4) . . ? C3 C2 H1 119.4 . . ? C1 C2 H1 119.4 . . ? C2 C3 C4 119.4(4) . . ? C2 C3 H2 120.3 . . ? C4 C3 H2 120.3 . . ? F1 C4 C5 118.6(4) . . ? F1 C4 C3 119.0(4) . . ? C5 C4 C3 122.4(4) . . ? C4 C5 C6 118.8(4) . . ? C4 C5 H3 120.6 . . ? C6 C5 H3 120.6 . . ? C5 C6 C1 119.9(4) . . ? C5 C6 C7 117.1(4) . . ? C1 C6 C7 122.8(4) . . ? N1 C7 C6 124.7(4) . . ? N1 C7 H4 117.7 . . ? C6 C7 H4 117.7 . . ? C7 N1 C8 118.3(3) . . ? C7 N1 Fe1 124.4(3) . . ? C8 N1 Fe1 115.8(3) . . ? N1 C8 C9 106.0(3) . . ? N1 C8 H5 110.5 . . ? C9 C8 H5 110.5 . . ? N1 C8 H6 110.5 . . ? C9 C8 H6 110.5 . . ? H5 C8 H6 108.7 . . ? N2 C9 C8 108.6(3) . . ? N2 C9 H7 110.0 . . ? C8 C9 H7 110.0 . . ? N2 C9 H8 110.0 . . ? C8 C9 H8 110.0 . . ? H7 C9 H8 108.4 . . ? C9 N2 C10 113.6(3) . . ? C9 N2 Fe1 106.7(3) . . ? C10 N2 Fe1 112.3(3) . . ? C9 N2 H9 107(3) . . ? C10 N2 H9 108(3) . . ? Fe1 N2 H9 109(3) . . ? N2 C10 C11 110.1(3) . . ? N2 C10 H10 109.6 . . ? C11 C10 H10 109.6 . . ? N2 C10 H11 109.6 . . ? C11 C10 H11 109.6 . . ? H10 C10 H11 108.2 . . ? N3 C11 C10 108.0(3) . . ? N3 C11 H12 110.1 . . ? C10 C11 H12 110.1 . . ? N3 C11 H13 110.1 . . ? C10 C11 H13 110.1 . . ? H12 C11 H13 108.4 . . ? C11 N3 C12 112.1(3) . . ? C11 N3 Fe1 109.2(3) . . ? C12 N3 Fe1 110.5(3) . . ? C11 N3 H14 107(4) . . ? C12 N3 H14 109(3) . . ? Fe1 N3 H14 109(3) . . ? N3 C12 C13 108.5(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 105.7(3) . . ? N4 C13 H17 110.6 . . ? C12 C13 H17 110.6 . . ? N4 C13 H18 110.6 . . ? C12 C13 H18 110.6 . . ? H17 C13 H18 108.7 . . ? C14 N4 C13 120.9(4) . . ? C14 N4 Fe1 127.6(3) . . ? C13 N4 Fe1 111.5(3) . . ? N4 C14 C15 123.8(4) . . ? N4 C14 H19 118.1 . . ? C15 C14 H19 118.1 . . ? C16 C15 C20 119.9(4) . . ? C16 C15 C14 118.3(4) . . ? C20 C15 C14 121.8(4) . . ? C17 C16 C15 119.0(4) . . ? C17 C16 H20 120.5 . . ? C15 C16 H20 120.5 . . ? C16 C17 F2 119.1(4) . . ? C16 C17 C18 123.0(4) . . ? F2 C17 C18 117.8(4) . . ? C17 C18 C19 118.4(4) . . ? C17 C18 H21 120.8 . . ? C19 C18 H21 120.8 . . ? C18 C19 C20 121.3(4) . . ? C18 C19 H22 119.4 . . ? C20 C19 H22 119.4 . . ? O2 C20 C19 117.8(4) . . ? O2 C20 C15 123.9(4) . . ? C19 C20 C15 118.3(4) . . ? C20 O2 Fe1 125.4(2) . . ? C21 O3 Fe2 134.4(3) . . ? O3 C21 C26 122.9(4) . . ? O3 C21 C22 119.0(4) . . ? C26 C21 C22 118.1(4) . . ? C23 C22 C21 121.3(4) . . ? C23 C22 H23 119.3 . . ? C21 C22 H23 119.3 . . ? C24 C23 C22 118.3(4) . . ? C24 C23 H24 120.9 . . ? C22 C23 H24 120.9 . . ? O3 Fe2 O4 109.06(16) . . ? O3 Fe2 N8 96.89(13) . . ? O4 Fe2 N8 85.07(14) . . ? O3 Fe2 N5 85.85(15) . . ? O4 Fe2 N5 87.39(19) . . ? N8 Fe2 N5 172.45(19) . . ? O3 Fe2 N7 87.63(14) . . ? O4 Fe2 N7 157.53(14) . . ? N8 Fe2 N7 77.89(14) . . ? N5 Fe2 N7 109.33(19) . . ? O3 Fe2 N6 152.29(17) . . ? O4 Fe2 N6 92.26(16) . . ? N8 Fe2 N6 102.56(16) . . ? N5 Fe2 N6 77.42(17) . . ? N7 Fe2 N6 77.50(15) . . ? C25 C24 F3 119.1(5) . . ? C25 C24 C23 123.1(4) . . ? F3 C24 C23 117.9(4) . . ? C24 C25 C26 119.3(5) . . ? C24 C25 H25 120.3 . . ? C26 C25 H25 120.3 . . ? C25 C26 C21 119.7(4) . . ? C25 C26 C27 118.2(4) . . ? C21 C26 C27 121.9(4) . . ? N5 C27 C26 125.4(5) . . ? N5 C27 H26 117.3 . . ? C26 C27 H26 117.3 . . ? C27 N5 C28 117.3(5) . . ? C27 N5 Fe2 126.5(3) . . ? C28 N5 Fe2 115.4(4) . . ? C29 C28 N5 113.1(6) . . ? C29 C28 H27 109.0 . . ? N5 C28 H27 109.0 . . ? C29 C28 H28 109.0 . . ? N5 C28 H28 109.0 . . ? H27 C28 H28 107.8 . . ? C28 C29 N6 122.2(6) . . ? C28 C29 H29 106.8 . . ? N6 C29 H29 106.8 . . ? C28 C29 H30 106.8 . . ? N6 C29 H30 106.8 . . ? H29 C29 H30 106.6 . . ? C29 N6 C30 113.2(6) . . ? C29 N6 Fe2 109.2(4) . . ? C30 N6 Fe2 113.2(3) . . ? C29 N6 H31 108(4) . . ? C30 N6 H31 107(4) . . ? Fe2 N6 H31 106(4) . . ? N6 C30 C31 109.8(4) . . ? N6 C30 H32 109.7 . . ? C31 C30 H32 109.7 . . ? N6 C30 H33 109.7 . . ? C31 C30 H33 109.7 . . ? H32 C30 H33 108.2 . . ? N7 C31 C30 108.7(3) . . ? N7 C31 H34 109.9 . . ? C30 C31 H34 109.9 . . ? N7 C31 H35 109.9 . . ? C30 C31 H35 109.9 . . ? H34 C31 H35 108.3 . . ? C31 N7 C32 114.1(4) . . ? C31 N7 Fe2 109.1(3) . . ? C32 N7 Fe2 111.1(3) . . ? C31 N7 H36 112(3) . . ? C32 N7 H36 106(3) . . ? Fe2 N7 H36 103(3) . . ? N7 C32 C33 108.8(4) . . ? N7 C32 H37 109.9 . . ? C33 C32 H37 109.9 . . ? N7 C32 H38 109.9 . . ? C33 C32 H38 109.9 . . ? H37 C32 H38 108.3 . . ? N8 C33 C32 106.5(4) . . ? N8 C33 H39 110.4 . . ? C32 C33 H39 110.4 . . ? N8 C33 H40 110.4 . . ? C32 C33 H40 110.4 . . ? H39 C33 H40 108.6 . . ? C34 N8 C33 120.2(4) . . ? C34 N8 Fe2 127.1(3) . . ? C33 N8 Fe2 112.2(3) . . ? N8 C34 C35 125.7(4) . . ? N8 C34 H41 117.2 . . ? C35 C34 H41 117.2 . . ? C36 C35 C40 119.4(4) . . ? C36 C35 C34 118.8(4) . . ? C40 C35 C34 121.8(4) . . ? C37 C36 C35 120.2(4) . . ? C37 C36 H42 119.9 . . ? C35 C36 H42 119.9 . . ? C36 C37 F4 119.6(4) . . ? C36 C37 C38 122.1(5) . . ? F4 C37 C38 118.3(4) . . ? C37 C38 C39 118.5(5) . . ? C37 C38 H43 120.7 . . ? C39 C38 H43 120.7 . . ? C38 C39 C40 121.4(5) . . ? C38 C39 H44 119.3 . . ? C40 C39 H44 119.3 . . ? O4 C40 C39 118.9(4) . . ? O4 C40 C35 122.7(4) . . ? C39 C40 C35 118.4(4) . . ? C40 O4 Fe2 132.1(3) . . ? O11 Cl1 O9 111.7(3) . . ? O11 Cl1 O10 109.1(2) . . ? O9 Cl1 O10 111.3(3) . . ? O11 Cl1 O12 106.0(3) . . ? O9 Cl1 O12 109.7(3) . . ? O10 Cl1 O12 108.7(3) . . ? O5 Cl2 O6 109.9(4) . . ? O5 Cl2 O7 109.4(3) . . ? O6 Cl2 O7 107.3(3) . . ? O5 Cl2 O8 108.7(2) . . ? O6 Cl2 O8 110.1(2) . . ? O7 Cl2 O8 111.4(2) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O1 1.873(3) . ? Fe1 O2 1.897(3) . ? Fe1 N4 1.955(3) . ? Fe1 N1 1.974(3) . ? Fe1 N2 2.042(3) . ? Fe1 N3 2.048(4) . ? O1 C1 1.329(5) . ? C1 C2 1.410(6) . ? C1 C6 1.422(6) . ? C2 C3 1.377(6) . ? C2 H1 0.9500 . ? C3 C4 1.383(7) . ? C3 H2 0.9500 . ? C4 F1 1.369(5) . ? C4 C5 1.372(7) . ? C5 C6 1.412(6) . ? C5 H3 0.9500 . ? C6 C7 1.441(6) . ? C7 N1 1.283(5) . ? C7 H4 0.9500 . ? N1 C8 1.482(5) . ? C8 C9 1.508(6) . ? C8 H5 0.9900 . ? C8 H6 0.9900 . ? C9 N2 1.496(5) . ? C9 H7 0.9900 . ? C9 H8 0.9900 . ? N2 C10 1.497(5) . ? N2 H9 0.89(5) . ? C10 C11 1.508(6) . ? C10 H10 0.9900 . ? C10 H11 0.9900 . ? C11 N3 1.473(6) . ? C11 H12 0.9900 . ? C11 H13 0.9900 . ? N3 C12 1.488(6) . ? N3 H14 0.79(5) . ? C12 C13 1.523(6) . ? C12 H15 0.9900 . ? C12 H16 0.9900 . ? C13 N4 1.473(5) . ? C13 H17 0.9900 . ? C13 H18 0.9900 . ? N4 C14 1.283(5) . ? C14 C15 1.450(6) . ? C14 H19 0.9500 . ? C15 C16 1.408(6) . ? C15 C20 1.424(6) . ? C16 C17 1.367(6) . ? C16 H20 0.9500 . ? C17 F2 1.369(5) . ? C17 C18 1.388(6) . ? C18 C19 1.390(6) . ? C18 H21 0.9500 . ? C19 C20 1.412(6) . ? C19 H22 0.9500 . ? C20 O2 1.331(5) . ? O3 C21 1.311(5) . ? O3 Fe2 1.910(3) . ? C21 C26 1.410(6) . ? C21 C22 1.415(6) . ? C22 C23 1.379(6) . ? C22 H23 0.9500 . ? C23 C24 1.379(7) . ? C23 H24 0.9500 . ? Fe2 O4 1.928(3) . ? Fe2 N8 2.104(4) . ? Fe2 N5 2.105(4) . ? Fe2 N7 2.196(4) . ? Fe2 N6 2.202(4) . ? C24 C25 1.357(7) . ? C24 F3 1.373(5) . ? C25 C26 1.404(6) . ? C25 H25 0.9500 . ? C26 C27 1.441(6) . ? C27 N5 1.274(6) . ? C27 H26 0.9500 . ? N5 C28 1.450(7) . ? C28 C29 1.368(7) . ? C28 H27 0.9900 . ? C28 H28 0.9900 . ? C29 N6 1.417(8) . ? C29 H29 0.9900 . ? C29 H30 0.9900 . ? N6 C30 1.471(6) . ? N6 H31 0.90(6) . ? C30 C31 1.523(6) . ? C30 H32 0.9900 . ? C30 H33 0.9900 . ? C31 N7 1.476(6) . ? C31 H34 0.9900 . ? C31 H35 0.9900 . ? N7 C32 1.484(6) . ? N7 H36 0.84(4) . ? C32 C33 1.521(7) . ? C32 H37 0.9900 . ? C32 H38 0.9900 . ? C33 N8 1.460(6) . ? C33 H39 0.9900 . ? C33 H40 0.9900 . ? N8 C34 1.287(6) . ? C34 C35 1.440(6) . ? C34 H41 0.9500 . ? C35 C36 1.410(6) . ? C35 C40 1.411(6) . ? C36 C37 1.354(7) . ? C36 H42 0.9500 . ? C37 F4 1.375(5) . ? C37 C38 1.385(7) . ? C38 C39 1.392(8) . ? C38 H43 0.9500 . ? C39 C40 1.404(7) . ? C39 H44 0.9500 . ? C40 O4 1.334(6) . ? Cl1 O11 1.415(4) . ? Cl1 O9 1.417(4) . ? Cl1 O10 1.434(4) . ? Cl1 O12 1.440(4) . ? Cl2 O5 1.405(4) . ? Cl2 O6 1.405(4) . ? Cl2 O7 1.432(4) . ? Cl2 O8 1.446(3) . ?