#------------------------------------------------------------------------------ #$Date: 2024-08-05 20:57:08 +0300 (Mon, 05 Aug 2024) $ #$Revision: 293740 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/19/1571974.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_1571974 loop_ _publ_author_name 'Cobb, Caitlyn R.' 'Ngo, Ren K.' 'Dick, Emily J.' 'Lynch, Vincent M.' 'Rose, Michael J.' _publ_section_title ; Multi-phosphine-chelated iron-carbide clusters via redox-promoted ligand exchange on an inert hexa-iron-carbide carbonyl cluster, [Fe66-C)(μ2-CO)4(CO)12]2. ; _journal_issue 29 _journal_name_full 'Chemical science' _journal_page_first 11455 _journal_page_last 11471 _journal_paper_doi 10.1039/d4sc01370k _journal_volume 15 _journal_year 2024 _chemical_formula_moiety 'C32 H27 Fe0.5 N P2, C11 H Fe3 O10, 0.5(C4 H10 O)' _chemical_formula_sum 'C45 H33 Fe3.5 N O10.5 P2' _chemical_formula_weight 1013.14 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _audit_creation_date 2023-01-18 _audit_creation_method ; Olex2 1.5 (compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498) ; _audit_update_record ; 2023-06-02 deposited with the CCDC. 2024-06-03 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 94.5540(8) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.61041(12) _cell_length_b 15.93666(13) _cell_length_c 21.4660(2) _cell_measurement_reflns_used 31980 _cell_measurement_temperature 100.15 _cell_measurement_theta_max 76.9780 _cell_measurement_theta_min 3.4400 _cell_volume 4300.36(7) _computing_cell_refinement 'CrysAlisPro 1.171.42.25a (Rigaku OD, 2021)' _computing_data_collection 'CrysAlisPro 1.171.42.25a (Rigaku OD, 2021)' _computing_data_reduction 'CrysAlisPro 1.171.42.25a (Rigaku OD, 2021)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _diffrn_ambient_temperature 100.02(13) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0622 _diffrn_reflns_av_unetI/netI 0.0287 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 76437 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 68.251 _diffrn_reflns_theta_min 3.458 _diffrn_source 'micro-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 10.529 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.49557 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrysAlisPro 1.171.42.25a (Rigaku Oxford Diffraction, 2021) Empirical absorption correction using spherical harmonics, implemented in SCALES3 ABSPACK scaling algorithm.'' _exptl_crystal_colour 'clear red' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.565 _exptl_crystal_description prism _exptl_crystal_F_000 2060 _exptl_crystal_preparation 'From the reaction of 2 with 1,2-bis(diphenylphosphino)benzene in MeCN.' _exptl_crystal_recrystallization_method 'Fractional distillation by repeated slow evaporation from diethyl ether at -20 degrees C.' _exptl_crystal_size_max 0.243 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.09 _refine_diff_density_max 0.474 _refine_diff_density_min -0.312 _refine_diff_density_rms 0.062 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 590 _refine_ls_number_reflns 7871 _refine_ls_number_restraints 37 _refine_ls_restrained_S_all 1.098 _refine_ls_R_factor_all 0.0413 _refine_ls_R_factor_gt 0.0376 _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^)+(0.0361P)^2^+3.7934P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0800 _refine_ls_wR_factor_ref 0.0815 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7344 _reflns_number_total 7871 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc01370k3.cif _cod_data_source_block compound5 _cod_depositor_comments 'Adding full bibliography for 1571968--1571976.cif.' _cod_original_formula_sum 'C45 H33 Fe3.50 N O10.50 P2' _cod_database_code 1571974 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _olex2_refinement_description ; 1. Restrained distances C2A-C1A 1.5 with sigma of 0.02 C2A-C3A 2.4 with sigma of 0.04 O1A-C1A 2.4 with sigma of 0.04 C4A-C3A 1.5 with sigma of 0.02 O1A-C4A 2.4 with sigma of 0.04 O1A-C2A 1.45 with sigma of 0.02 O1A-C3A 1.45 with sigma of 0.02 2. Uiso/Uaniso restraints and constraints Uanis(C1A) \\sim Ueq, Uanis(C2A) \\sim Ueq, Uanis(O1A) \\sim Ueq, Uanis(C3A) \\sim Ueq, Uanis(C4A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 3. Others Fixed Sof: O1A(0.5) C1A(0.5) H1AA(0.5) H1AB(0.5) H1AC(0.5) C2A(0.5) H2AA(0.5) H2AB(0.5) C3A(0.5) H3AA(0.5) H3AB(0.5) C4A(0.5) H4AA(0.5) H4AB(0.5) H4AC(0.5) 4.a Secondary CH2 refined with riding coordinates: C2A(H2AA,H2AB), C3A(H3AA,H3AB) 4.b Aromatic/amide H refined with riding coordinates: C14(H14), C15(H15), C16(H16), C17(H17), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42) 4.c Idealised Me refined as rotating group: C12(H12A,H12B,H12C), C1A(H1AA,H1AB,H1AC), C4A(H4AA,H4AB,H4AC) ; _shelx_res_file ; TITL fe3methylidene_redixtal_auto_a.res in P2(1)/c fe3methylidene_redixtal_auto.res created by SHELXL-2018/3 at 14:49:24 on 30-Sep-2022 REM Old TITL fe3methylidene_redixtal_auto_a.res in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.085, Rweak 0.007, Alpha 0.054 REM 0.397 for 132 systematic absences, Orientation as input REM Formula found by SHELXT: C89 N4 O18 Fe7 P4 CELL 1.54184 12.610413 15.936661 21.466001 90 94.554 90 ZERR 4 0.000116 0.000126 0.000196 0 0.0008 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Fe N O P UNIT 180 132 14 4 42 8 DFIX 1.5 C2A C1A DFIX 2.4 0.04 C2A C3A DFIX 2.4 0.04 O1A C1A DFIX 1.5 C4A C3A DFIX 2.4 0.04 O1A C4A DFIX 1.45 O1A C2A DFIX 1.45 O1A C3A ISOR 0.01 0.02 C1A C2A O1A C3A C4A L.S. 4 0 0 PLAN 1 TEMP -173 CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta SHEL 20 0.83 OMIT 13 5 6 OMIT 12 6 3 REM REM REM WGHT 0.036100 3.793400 FVAR 0.84591 FE1 3 0.000000 0.500000 0.500000 10.50000 0.00901 0.01107 = 0.01206 0.00122 0.00093 0.00001 P1 6 0.164079 0.518933 0.459235 11.00000 0.01038 0.01407 = 0.01453 0.00108 0.00188 -0.00082 P2 6 0.072011 0.369156 0.525810 11.00000 0.01080 0.01182 = 0.01597 0.00180 0.00140 0.00045 N1 4 -0.054863 0.457957 0.420916 11.00000 0.00960 0.01339 = 0.01840 0.00156 0.00290 0.00053 C11 1 -0.079428 0.429720 0.373345 11.00000 0.01223 0.01857 = 0.01943 0.00184 0.00119 0.00287 C12 1 -0.109344 0.392743 0.312613 11.00000 0.03083 0.03619 = 0.02281 -0.00986 -0.00621 0.01250 AFIX 137 H12A 2 -0.054665 0.405392 0.284006 11.00000 -1.50000 H12B 2 -0.177634 0.416100 0.295853 11.00000 -1.50000 H12C 2 -0.115910 0.331797 0.317016 11.00000 -1.50000 AFIX 0 C13 1 0.256800 0.440508 0.493165 11.00000 0.01402 0.01574 = 0.01606 -0.00161 0.00100 0.00048 C14 1 0.365796 0.442022 0.484529 11.00000 0.01506 0.02072 = 0.02157 -0.00075 0.00239 -0.00205 AFIX 43 H14 2 0.393719 0.483962 0.458967 11.00000 -1.20000 AFIX 0 C15 1 0.432629 0.382354 0.513285 11.00000 0.00932 0.02513 = 0.02749 -0.00310 0.00125 0.00178 AFIX 43 H15 2 0.506399 0.383107 0.507132 11.00000 -1.20000 AFIX 0 C16 1 0.392298 0.321296 0.551146 11.00000 0.01466 0.02400 = 0.02708 0.00182 -0.00252 0.00523 AFIX 43 H16 2 0.438964 0.281370 0.571576 11.00000 -1.20000 AFIX 0 C17 1 0.284437 0.318288 0.559286 11.00000 0.01711 0.01718 = 0.02342 0.00343 0.00239 0.00166 AFIX 43 H17 2 0.256883 0.276173 0.584845 11.00000 -1.20000 AFIX 0 C18 1 0.216486 0.377917 0.529475 11.00000 0.01257 0.01545 = 0.01548 -0.00179 0.00124 0.00073 C19 1 0.239887 0.613772 0.481409 11.00000 0.01068 0.01578 = 0.02185 0.00044 0.00376 -0.00037 C20 1 0.281869 0.618631 0.543707 11.00000 0.01052 0.01868 = 0.02354 -0.00055 0.00367 0.00092 AFIX 43 H20 2 0.275430 0.572067 0.570781 11.00000 -1.20000 AFIX 0 C21 1 0.332900 0.691149 0.566184 11.00000 0.01230 0.02545 = 0.02747 -0.00591 -0.00128 0.00102 AFIX 43 H21 2 0.360478 0.694197 0.608613 11.00000 -1.20000 AFIX 0 C22 1 0.343555 0.758761 0.526915 11.00000 0.01592 0.02082 = 0.04213 -0.00575 0.00093 -0.00392 AFIX 43 H22 2 0.377129 0.808661 0.542608 11.00000 -1.20000 AFIX 0 C23 1 0.305642 0.754008 0.465096 11.00000 0.01871 0.01915 = 0.03778 0.00427 0.00495 -0.00425 AFIX 43 H23 2 0.314498 0.800256 0.438072 11.00000 -1.20000 AFIX 0 C24 1 0.254259 0.681608 0.441905 11.00000 0.01430 0.02217 = 0.02504 0.00328 0.00263 -0.00128 AFIX 43 H24 2 0.228996 0.678524 0.399080 11.00000 -1.20000 AFIX 0 C25 1 0.169237 0.502720 0.375026 11.00000 0.00919 0.02437 = 0.01915 -0.00104 0.00382 -0.00302 C26 1 0.132997 0.563693 0.331497 11.00000 0.01438 0.02906 = 0.02158 0.00255 0.00076 0.00399 AFIX 43 H26 2 0.106741 0.615684 0.345514 11.00000 -1.20000 AFIX 0 C27 1 0.135239 0.548544 0.267883 11.00000 0.02475 0.04137 = 0.02083 0.00578 -0.00046 0.00561 AFIX 43 H27 2 0.113220 0.591159 0.238724 11.00000 -1.20000 AFIX 0 C28 1 0.169262 0.471936 0.246634 11.00000 0.02493 0.04954 = 0.01744 -0.00507 0.00049 0.00144 AFIX 43 H28 2 0.169537 0.461635 0.203056 11.00000 -1.20000 AFIX 0 C29 1 0.202920 0.410338 0.289226 11.00000 0.02139 0.03076 = 0.02464 -0.00715 0.00395 -0.00169 AFIX 43 H29 2 0.225639 0.357437 0.274822 11.00000 -1.20000 AFIX 0 C30 1 0.203548 0.425738 0.353094 11.00000 0.01839 0.02289 = 0.02158 0.00010 0.00254 -0.00344 AFIX 43 H30 2 0.227576 0.383414 0.382023 11.00000 -1.20000 AFIX 0 C31 1 0.054604 0.320089 0.601334 11.00000 0.01110 0.01755 = 0.02019 0.00484 0.00206 0.00255 C32 1 0.106639 0.357091 0.654274 11.00000 0.01555 0.01916 = 0.02162 0.00385 0.00124 0.00186 AFIX 43 H32 2 0.150007 0.405133 0.649856 11.00000 -1.20000 AFIX 0 C33 1 0.095537 0.324370 0.713030 11.00000 0.01805 0.02857 = 0.02073 0.00407 -0.00136 0.00277 AFIX 43 H33 2 0.130772 0.350080 0.748857 11.00000 -1.20000 AFIX 0 C34 1 0.032842 0.253925 0.719551 11.00000 0.02722 0.03509 = 0.02133 0.01319 0.00083 0.00067 AFIX 43 H34 2 0.024585 0.231717 0.759950 11.00000 -1.20000 AFIX 0 C35 1 -0.017688 0.215910 0.667437 11.00000 0.02606 0.02773 = 0.03498 0.01341 0.00350 -0.00698 AFIX 43 H35 2 -0.059995 0.167335 0.672114 11.00000 -1.20000 AFIX 0 C36 1 -0.006809 0.248520 0.608193 11.00000 0.01975 0.01967 = 0.02431 0.00437 -0.00194 -0.00216 AFIX 43 H36 2 -0.041215 0.222024 0.572446 11.00000 -1.20000 AFIX 0 C37 1 0.048795 0.284254 0.468442 11.00000 0.01818 0.01194 = 0.01851 0.00232 -0.00088 0.00028 C38 1 0.133064 0.246313 0.440587 11.00000 0.01821 0.01945 = 0.02485 -0.00081 0.00253 0.00139 AFIX 43 H38 2 0.203932 0.264517 0.451218 11.00000 -1.20000 AFIX 0 C39 1 0.113671 0.182183 0.397481 11.00000 0.02414 0.02699 = 0.02999 -0.00791 0.00210 0.00443 AFIX 43 H39 2 0.171437 0.157169 0.378509 11.00000 -1.20000 AFIX 0 C40 1 0.011175 0.154267 0.381823 11.00000 0.03284 0.02150 = 0.02542 -0.00709 -0.00316 0.00345 AFIX 43 H40 2 -0.001445 0.109631 0.352848 11.00000 -1.20000 AFIX 0 C41 1 -0.072793 0.191957 0.408755 11.00000 0.02176 0.02254 = 0.02767 -0.00137 -0.00649 -0.00205 AFIX 43 H41 2 -0.143437 0.173394 0.397893 11.00000 -1.20000 AFIX 0 C42 1 -0.054579 0.256807 0.451604 11.00000 0.01621 0.01560 = 0.02282 0.00140 -0.00106 0.00099 AFIX 43 H42 2 -0.112892 0.282588 0.469528 11.00000 -1.20000 AFIX 0 FE2 3 0.494662 0.571270 0.780644 11.00000 0.02483 0.01523 = 0.02525 0.00124 0.00142 -0.00173 FE3 3 0.503671 0.414907 0.761775 11.00000 0.01638 0.01615 = 0.02210 0.00003 0.00161 -0.00015 FE4 3 0.404880 0.471492 0.854041 11.00000 0.02488 0.01899 = 0.02203 0.00252 0.00383 0.00348 O1 5 0.321234 0.501376 0.693121 11.00000 0.02166 0.02851 = 0.03246 0.00089 -0.00291 0.00258 O2 5 0.586719 0.418995 0.637965 11.00000 0.03103 0.05276 = 0.02625 0.00089 0.00664 0.00433 O3 5 0.686718 0.315367 0.812375 11.00000 0.03162 0.03604 = 0.03822 0.00679 -0.00339 0.01179 O4 5 0.338460 0.285010 0.749941 11.00000 0.02485 0.02292 = 0.07608 -0.00167 -0.00049 -0.00478 O5 5 0.398370 0.310802 0.919859 11.00000 0.03543 0.02973 = 0.05158 0.01877 0.00870 0.00376 O6 5 0.175471 0.499879 0.819308 11.00000 0.02762 0.03951 = 0.03930 0.01250 0.00667 0.00529 O7 5 0.441858 0.572661 0.966983 11.00000 0.09077 0.03871 = 0.03230 -0.01174 -0.01324 0.03530 O8 5 0.320528 0.685329 0.805794 11.00000 0.05553 0.03057 = 0.05516 0.00757 0.01870 0.01736 O9 5 0.675272 0.649944 0.853801 11.00000 0.05698 0.03422 = 0.04499 -0.00941 -0.01025 -0.01940 O10 5 0.550295 0.639714 0.660449 11.00000 0.03265 0.04152 = 0.03473 0.01445 0.00117 -0.00368 C1 1 0.547198 0.479266 0.837167 11.00000 0.02367 0.01823 = 0.02690 -0.00171 -0.00251 -0.00062 H1 2 0.615789 0.474532 0.863918 11.00000 0.02483 C2 1 0.554249 0.416671 0.686122 11.00000 0.01671 0.02664 = 0.03049 -0.00053 -0.00316 0.00145 C3 1 0.614867 0.354023 0.793401 11.00000 0.02541 0.02246 = 0.02586 -0.00043 0.00302 -0.00127 C4 1 0.402729 0.335905 0.754805 11.00000 0.02225 0.01882 = 0.03739 0.00009 0.00141 0.00380 C5 1 0.400839 0.373625 0.893679 11.00000 0.02136 0.03094 = 0.03216 0.00086 0.00649 0.00486 C6 1 0.264169 0.487169 0.832548 11.00000 0.03102 0.02337 = 0.02583 0.00593 0.00753 0.00174 C7 1 0.424183 0.533446 0.922446 11.00000 0.04596 0.02603 = 0.03051 0.00547 0.00467 0.01848 C8 1 0.388110 0.639791 0.796569 11.00000 0.04412 0.02116 = 0.03293 0.00555 0.00753 0.00040 C9 1 0.604558 0.619793 0.825497 11.00000 0.04519 0.01932 = 0.03308 -0.00098 0.00335 -0.00370 C10 1 0.530295 0.613861 0.707698 11.00000 0.02343 0.02100 = 0.03426 0.00108 -0.00302 -0.00159 C43 1 0.396023 0.497023 0.729777 11.00000 0.02243 0.01739 = 0.02933 0.00093 0.00551 0.00081 PART -1 O1A 5 -0.001421 0.012972 0.506751 10.50000 0.06752 0.03283 = 0.03971 0.00375 0.00789 0.00290 C1A 1 -0.189019 -0.001816 0.488464 10.50000 0.07059 0.05707 = 0.05843 0.01298 0.01463 0.00997 AFIX 137 H1AA 2 -0.245245 -0.028306 0.461075 10.50000 -1.50000 H1AB 2 -0.194934 0.059330 0.484798 10.50000 -1.50000 H1AC 2 -0.196526 -0.018484 0.531838 10.50000 -1.50000 AFIX 0 C2A 1 -0.082484 -0.029332 0.469619 10.50000 0.06582 0.04519 = 0.03436 0.00694 0.00428 0.00230 AFIX 23 H2AA 2 -0.074570 -0.090708 0.475389 10.50000 -1.20000 H2AB 2 -0.076526 -0.016339 0.424933 10.50000 -1.20000 AFIX 0 C3A 1 0.103026 -0.008631 0.491135 10.50000 0.06649 0.04448 = 0.04108 0.01393 0.00827 0.00639 AFIX 23 H3AA 2 0.112843 0.008056 0.447542 10.50000 -1.20000 H3AB 2 0.113990 -0.069985 0.494957 10.50000 -1.20000 AFIX 0 C4A 1 0.181562 0.037106 0.535685 10.50000 0.07867 0.06779 = 0.05866 0.01087 -0.00646 -0.00466 AFIX 137 H4AA 2 0.254063 0.025258 0.524774 10.50000 -1.50000 H4AB 2 0.173463 0.018163 0.578481 10.50000 -1.50000 H4AC 2 0.168174 0.097605 0.532738 10.50000 -1.50000 AFIX 0 HKLF 4 REM fe3methylidene_redixtal_auto_a.res in P2(1)/c REM wR2 = 0.0815, GooF = S = 1.099, Restrained GooF = 1.098 for all data REM R1 = 0.0376 for 7344 Fo > 4sig(Fo) and 0.0413 for all 7871 data REM 590 parameters refined using 37 restraints END WGHT 0.0362 3.7788 REM Highest difference peak 0.474, deepest hole -0.312, 1-sigma level 0.062 Q1 1 0.5830 0.4212 0.7837 11.00000 0.05 0.47 ; _shelx_res_checksum 15628 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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 0.000000 0.500000 0.500000 0.01071(11) Uani 1 2 d S . P . . P1 P 0.16408(4) 0.51893(3) 0.45924(3) 0.01295(12) Uani 1 1 d . . . . . P2 P 0.07201(4) 0.36916(3) 0.52581(3) 0.01285(12) Uani 1 1 d . . . . . N1 N -0.05486(14) 0.45796(11) 0.42092(9) 0.0137(4) Uani 1 1 d . . . . . C11 C -0.07943(18) 0.42972(14) 0.37335(11) 0.0167(5) Uani 1 1 d . . . . . C12 C -0.1093(2) 0.39274(18) 0.31261(12) 0.0304(6) Uani 1 1 d . . . . . H12A H -0.054665 0.405392 0.284006 0.046 Uiso 1 1 calc R U . . . H12B H -0.177634 0.416100 0.295853 0.046 Uiso 1 1 calc R U . . . H12C H -0.115910 0.331797 0.317016 0.046 Uiso 1 1 calc R U . . . C13 C 0.25680(18) 0.44051(14) 0.49316(10) 0.0153(5) Uani 1 1 d . . . . . C14 C 0.36580(19) 0.44202(15) 0.48453(11) 0.0191(5) Uani 1 1 d . . . . . H14 H 0.393719 0.483962 0.458967 0.023 Uiso 1 1 calc R U . . . C15 C 0.43263(19) 0.38235(15) 0.51328(12) 0.0207(5) Uani 1 1 d . . . . . H15 H 0.506399 0.383107 0.507132 0.025 Uiso 1 1 calc R U . . . C16 C 0.39230(19) 0.32130(16) 0.55115(12) 0.0221(5) Uani 1 1 d . . . . . H16 H 0.438964 0.281370 0.571576 0.027 Uiso 1 1 calc R U . . . C17 C 0.28444(19) 0.31829(15) 0.55929(11) 0.0192(5) Uani 1 1 d . . . . . H17 H 0.256883 0.276173 0.584845 0.023 Uiso 1 1 calc R U . . . C18 C 0.21649(18) 0.37792(14) 0.52948(10) 0.0145(5) Uani 1 1 d . . . . . C19 C 0.23989(18) 0.61377(14) 0.48141(11) 0.0160(5) Uani 1 1 d . . . . . C20 C 0.28187(18) 0.61863(15) 0.54371(11) 0.0175(5) Uani 1 1 d . . . . . H20 H 0.275430 0.572067 0.570781 0.021 Uiso 1 1 calc R U . . . C21 C 0.33290(18) 0.69115(16) 0.56618(12) 0.0219(5) Uani 1 1 d . . . . . H21 H 0.360478 0.694197 0.608613 0.026 Uiso 1 1 calc R U . . . C22 C 0.3436(2) 0.75876(16) 0.52691(13) 0.0264(6) Uani 1 1 d . . . . . H22 H 0.377129 0.808661 0.542608 0.032 Uiso 1 1 calc R U . . . C23 C 0.3056(2) 0.75401(16) 0.46510(13) 0.0251(6) Uani 1 1 d . . . . . H23 H 0.314498 0.800256 0.438072 0.030 Uiso 1 1 calc R U . . . C24 C 0.25426(19) 0.68161(15) 0.44191(12) 0.0204(5) Uani 1 1 d . . . . . H24 H 0.228996 0.678524 0.399080 0.025 Uiso 1 1 calc R U . . . C25 C 0.16924(18) 0.50272(15) 0.37503(11) 0.0174(5) Uani 1 1 d . . . . . C26 C 0.13300(19) 0.56369(16) 0.33150(11) 0.0217(5) Uani 1 1 d . . . . . H26 H 0.106741 0.615684 0.345514 0.026 Uiso 1 1 calc R U . . . C27 C 0.1352(2) 0.54854(19) 0.26788(12) 0.0291(6) Uani 1 1 d . . . . . H27 H 0.113220 0.591159 0.238724 0.035 Uiso 1 1 calc R U . . . C28 C 0.1693(2) 0.47194(19) 0.24663(12) 0.0307(6) Uani 1 1 d . . . . . H28 H 0.169537 0.461635 0.203056 0.037 Uiso 1 1 calc R U . . . C29 C 0.2029(2) 0.41034(17) 0.28923(12) 0.0255(6) Uani 1 1 d . . . . . H29 H 0.225639 0.357437 0.274822 0.031 Uiso 1 1 calc R U . . . C30 C 0.20355(19) 0.42574(15) 0.35309(12) 0.0209(5) Uani 1 1 d . . . . . H30 H 0.227576 0.383414 0.382023 0.025 Uiso 1 1 calc R U . . . C31 C 0.05460(18) 0.32009(14) 0.60133(11) 0.0162(5) Uani 1 1 d . . . . . C32 C 0.10664(19) 0.35709(15) 0.65427(11) 0.0188(5) Uani 1 1 d . . . . . H32 H 0.150007 0.405133 0.649856 0.023 Uiso 1 1 calc R U . . . C33 C 0.0955(2) 0.32437(16) 0.71303(12) 0.0226(5) Uani 1 1 d . . . . . H33 H 0.130772 0.350080 0.748857 0.027 Uiso 1 1 calc R U . . . C34 C 0.0328(2) 0.25393(17) 0.71955(12) 0.0279(6) Uani 1 1 d . . . . . H34 H 0.024585 0.231717 0.759950 0.034 Uiso 1 1 calc R U . . . C35 C -0.0177(2) 0.21591(17) 0.66744(13) 0.0295(6) Uani 1 1 d . . . . . H35 H -0.059995 0.167335 0.672114 0.035 Uiso 1 1 calc R U . . . C36 C -0.0068(2) 0.24852(15) 0.60819(12) 0.0214(5) Uani 1 1 d . . . . . H36 H -0.041215 0.222024 0.572446 0.026 Uiso 1 1 calc R U . . . C37 C 0.04879(18) 0.28425(14) 0.46844(11) 0.0163(5) Uani 1 1 d . . . . . C38 C 0.1331(2) 0.24631(15) 0.44059(11) 0.0208(5) Uani 1 1 d . . . . . H38 H 0.203932 0.264517 0.451218 0.025 Uiso 1 1 calc R U . . . C39 C 0.1137(2) 0.18218(17) 0.39748(13) 0.0270(6) Uani 1 1 d . . . . . H39 H 0.171437 0.157169 0.378509 0.032 Uiso 1 1 calc R U . . . C40 C 0.0112(2) 0.15427(16) 0.38182(12) 0.0269(6) Uani 1 1 d . . . . . H40 H -0.001445 0.109631 0.352848 0.032 Uiso 1 1 calc R U . . . C41 C -0.0728(2) 0.19196(16) 0.40875(12) 0.0244(6) Uani 1 1 d . . . . . H41 H -0.143437 0.173394 0.397893 0.029 Uiso 1 1 calc R U . . . C42 C -0.05458(19) 0.25681(14) 0.45160(11) 0.0183(5) Uani 1 1 d . . . . . H42 H -0.112892 0.282588 0.469528 0.022 Uiso 1 1 calc R U . . . Fe2 Fe 0.49466(3) 0.57127(2) 0.78064(2) 0.02180(10) Uani 1 1 d . . . . . Fe3 Fe 0.50367(3) 0.41491(2) 0.76177(2) 0.01821(9) Uani 1 1 d . . . . . Fe4 Fe 0.40488(3) 0.47149(2) 0.85404(2) 0.02186(10) Uani 1 1 d . . . . . O1 O 0.32123(14) 0.50138(11) 0.69312(9) 0.0278(4) Uani 1 1 d . . . . . O2 O 0.58672(16) 0.41899(14) 0.63797(9) 0.0364(5) Uani 1 1 d . . . . . O3 O 0.68672(16) 0.31537(13) 0.81237(10) 0.0356(5) Uani 1 1 d . . . . . O4 O 0.33846(16) 0.28501(12) 0.74994(11) 0.0415(5) Uani 1 1 d . . . . . O5 O 0.39837(16) 0.31080(12) 0.91986(10) 0.0386(5) Uani 1 1 d . . . . . O6 O 0.17547(16) 0.49988(13) 0.81931(10) 0.0353(5) Uani 1 1 d . . . . . O7 O 0.4419(2) 0.57266(14) 0.96698(10) 0.0549(7) Uani 1 1 d . . . . . O8 O 0.32053(19) 0.68533(13) 0.80579(11) 0.0463(6) Uani 1 1 d . . . . . O9 O 0.67527(19) 0.64994(13) 0.85380(11) 0.0462(6) Uani 1 1 d . . . . . O10 O 0.55030(16) 0.63971(13) 0.66045(10) 0.0364(5) Uani 1 1 d . . . . . C1 C 0.5472(2) 0.47927(15) 0.83717(12) 0.0232(5) Uani 1 1 d . . . . . H1 H 0.616(2) 0.4745(17) 0.8639(13) 0.025(7) Uiso 1 1 d . . . . . C2 C 0.5542(2) 0.41667(16) 0.68612(13) 0.0249(6) Uani 1 1 d . . . . . C3 C 0.6149(2) 0.35402(16) 0.79340(12) 0.0245(6) Uani 1 1 d . . . . . C4 C 0.4027(2) 0.33591(16) 0.75481(13) 0.0262(6) Uani 1 1 d . . . . . C5 C 0.4008(2) 0.37362(18) 0.89368(13) 0.0279(6) Uani 1 1 d . . . . . C6 C 0.2642(2) 0.48717(16) 0.83255(13) 0.0265(6) Uani 1 1 d . . . . . C7 C 0.4242(3) 0.53345(18) 0.92245(14) 0.0341(7) Uani 1 1 d . . . . . C8 C 0.3881(2) 0.63979(17) 0.79657(14) 0.0325(6) Uani 1 1 d . . . . . C9 C 0.6046(2) 0.61979(17) 0.82550(14) 0.0325(6) Uani 1 1 d . . . . . C10 C 0.5303(2) 0.61386(16) 0.70770(13) 0.0265(6) Uani 1 1 d . . . . . C43 C 0.3960(2) 0.49702(15) 0.72978(13) 0.0229(5) Uani 1 1 d . . . . . O1A O -0.0014(10) 0.0130(6) 0.5068(6) 0.046(2) Uani 0.5 1 d D U P A -1 C1A C -0.1890(8) -0.0018(6) 0.4885(5) 0.062(3) Uani 0.5 1 d D U P A -1 H1AA H -0.245245 -0.028306 0.461075 0.092 Uiso 0.5 1 calc R U P A -1 H1AB H -0.194934 0.059330 0.484798 0.092 Uiso 0.5 1 calc R U P A -1 H1AC H -0.196526 -0.018484 0.531838 0.092 Uiso 0.5 1 calc R U P A -1 C2A C -0.0825(6) -0.0293(5) 0.4696(3) 0.0484(17) Uani 0.5 1 d D U P A -1 H2AA H -0.074570 -0.090708 0.475389 0.058 Uiso 0.5 1 calc R U P A -1 H2AB H -0.076526 -0.016339 0.424933 0.058 Uiso 0.5 1 calc R U P A -1 C3A C 0.1030(7) -0.0086(5) 0.4911(3) 0.0505(18) Uani 0.5 1 d D U P A -1 H3AA H 0.112843 0.008056 0.447542 0.061 Uiso 0.5 1 calc R U P A -1 H3AB H 0.113990 -0.069985 0.494957 0.061 Uiso 0.5 1 calc R U P A -1 C4A C 0.1816(9) 0.0371(7) 0.5357(5) 0.069(3) Uani 0.5 1 d D U P A -1 H4AA H 0.254063 0.025258 0.524774 0.104 Uiso 0.5 1 calc R U P A -1 H4AB H 0.173463 0.018163 0.578481 0.104 Uiso 0.5 1 calc R U P A -1 H4AC H 0.168174 0.097605 0.532738 0.104 Uiso 0.5 1 calc R U P A -1 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 0.0090(2) 0.0111(2) 0.0121(2) 0.00122(18) 0.00093(18) 0.00001(18) P1 0.0104(3) 0.0141(3) 0.0145(3) 0.0011(2) 0.0019(2) -0.0008(2) P2 0.0108(3) 0.0118(3) 0.0160(3) 0.0018(2) 0.0014(2) 0.0005(2) N1 0.0096(9) 0.0134(9) 0.0184(10) 0.0016(8) 0.0029(7) 0.0005(7) C11 0.0122(11) 0.0186(11) 0.0194(12) 0.0018(9) 0.0012(9) 0.0029(9) C12 0.0308(15) 0.0362(15) 0.0228(14) -0.0099(11) -0.0062(11) 0.0125(12) C13 0.0140(11) 0.0157(11) 0.0161(11) -0.0016(9) 0.0010(9) 0.0005(9) C14 0.0151(12) 0.0207(12) 0.0216(12) -0.0008(10) 0.0024(9) -0.0020(9) C15 0.0093(11) 0.0251(13) 0.0275(13) -0.0031(10) 0.0012(10) 0.0018(10) C16 0.0147(12) 0.0240(12) 0.0271(13) 0.0018(10) -0.0025(10) 0.0052(10) C17 0.0171(12) 0.0172(11) 0.0234(13) 0.0034(9) 0.0024(10) 0.0017(9) C18 0.0126(11) 0.0155(11) 0.0155(11) -0.0018(9) 0.0012(9) 0.0007(9) C19 0.0107(11) 0.0158(11) 0.0218(12) 0.0004(9) 0.0038(9) -0.0004(9) C20 0.0105(11) 0.0187(11) 0.0235(12) -0.0005(10) 0.0037(9) 0.0009(9) C21 0.0123(12) 0.0255(13) 0.0275(13) -0.0059(10) -0.0013(10) 0.0010(10) C22 0.0159(12) 0.0208(12) 0.0421(16) -0.0057(11) 0.0009(11) -0.0039(10) C23 0.0187(13) 0.0192(12) 0.0378(15) 0.0043(11) 0.0049(11) -0.0043(10) C24 0.0143(12) 0.0222(12) 0.0250(13) 0.0033(10) 0.0026(10) -0.0013(9) C25 0.0092(11) 0.0244(12) 0.0192(12) -0.0010(9) 0.0038(9) -0.0030(9) C26 0.0144(12) 0.0291(13) 0.0216(12) 0.0026(10) 0.0008(10) 0.0040(10) C27 0.0248(14) 0.0414(16) 0.0208(13) 0.0058(12) -0.0005(11) 0.0056(12) C28 0.0249(14) 0.0495(17) 0.0174(13) -0.0051(12) 0.0005(11) 0.0014(13) C29 0.0214(13) 0.0308(14) 0.0246(13) -0.0072(11) 0.0040(11) -0.0017(11) C30 0.0184(12) 0.0229(12) 0.0216(12) 0.0001(10) 0.0025(10) -0.0034(10) C31 0.0111(11) 0.0176(11) 0.0202(12) 0.0048(9) 0.0021(9) 0.0025(9) C32 0.0155(12) 0.0192(12) 0.0216(12) 0.0038(9) 0.0012(9) 0.0019(9) C33 0.0181(12) 0.0286(13) 0.0207(13) 0.0041(10) -0.0014(10) 0.0028(10) C34 0.0272(14) 0.0351(15) 0.0213(13) 0.0132(11) 0.0008(11) 0.0007(12) C35 0.0261(14) 0.0277(14) 0.0350(15) 0.0134(12) 0.0035(12) -0.0070(11) C36 0.0198(13) 0.0197(12) 0.0243(13) 0.0044(10) -0.0019(10) -0.0022(10) C37 0.0182(12) 0.0119(10) 0.0185(12) 0.0023(9) -0.0009(9) 0.0003(9) C38 0.0182(12) 0.0194(12) 0.0249(13) -0.0008(10) 0.0025(10) 0.0014(10) C39 0.0241(14) 0.0270(13) 0.0300(14) -0.0079(11) 0.0021(11) 0.0044(11) C40 0.0328(15) 0.0215(12) 0.0254(13) -0.0071(10) -0.0032(11) 0.0035(11) C41 0.0218(13) 0.0225(12) 0.0277(14) -0.0014(10) -0.0065(11) -0.0021(10) C42 0.0162(12) 0.0156(11) 0.0228(12) 0.0014(10) -0.0011(9) 0.0010(9) Fe2 0.0248(2) 0.01523(19) 0.0252(2) 0.00124(15) 0.00142(16) -0.00173(15) Fe3 0.0164(2) 0.01615(18) 0.0221(2) 0.00003(15) 0.00161(15) -0.00015(14) Fe4 0.0249(2) 0.01899(19) 0.0220(2) 0.00252(15) 0.00383(16) 0.00348(16) O1 0.0217(10) 0.0285(10) 0.0325(10) 0.0009(8) -0.0029(8) 0.0026(8) O2 0.0310(11) 0.0528(13) 0.0262(11) 0.0009(9) 0.0066(9) 0.0043(9) O3 0.0316(11) 0.0360(11) 0.0382(12) 0.0068(9) -0.0034(9) 0.0118(9) O4 0.0248(11) 0.0229(10) 0.0761(16) -0.0017(10) -0.0005(10) -0.0048(9) O5 0.0354(12) 0.0297(11) 0.0516(13) 0.0188(10) 0.0087(10) 0.0038(9) O6 0.0276(12) 0.0395(11) 0.0393(12) 0.0125(9) 0.0067(9) 0.0053(9) O7 0.091(2) 0.0387(12) 0.0323(12) -0.0117(10) -0.0132(12) 0.0353(13) O8 0.0555(15) 0.0306(11) 0.0552(14) 0.0076(10) 0.0187(11) 0.0174(11) O9 0.0570(15) 0.0342(11) 0.0450(13) -0.0094(10) -0.0102(11) -0.0194(11) O10 0.0326(11) 0.0415(12) 0.0347(11) 0.0144(9) 0.0012(9) -0.0037(9) C1 0.0237(14) 0.0182(12) 0.0269(13) -0.0017(10) -0.0025(11) -0.0006(10) C2 0.0167(13) 0.0266(13) 0.0305(15) -0.0005(11) -0.0032(11) 0.0015(10) C3 0.0254(14) 0.0225(12) 0.0259(14) -0.0004(10) 0.0030(11) -0.0013(11) C4 0.0223(14) 0.0188(12) 0.0374(15) 0.0001(11) 0.0014(11) 0.0038(11) C5 0.0214(13) 0.0309(15) 0.0322(15) 0.0009(12) 0.0065(11) 0.0049(11) C6 0.0310(16) 0.0234(13) 0.0258(14) 0.0059(11) 0.0075(11) 0.0017(11) C7 0.0460(18) 0.0260(14) 0.0305(16) 0.0055(12) 0.0047(13) 0.0185(13) C8 0.0441(18) 0.0212(13) 0.0329(15) 0.0056(11) 0.0075(13) 0.0004(13) C9 0.0452(18) 0.0193(13) 0.0331(16) -0.0010(11) 0.0033(14) -0.0037(12) C10 0.0234(14) 0.0210(13) 0.0343(16) 0.0011(11) -0.0030(11) -0.0016(11) C43 0.0224(14) 0.0174(12) 0.0293(14) 0.0009(10) 0.0055(11) 0.0008(10) O1A 0.068(3) 0.033(6) 0.040(5) 0.004(4) 0.008(3) 0.003(4) C1A 0.071(7) 0.057(6) 0.058(6) 0.013(4) 0.015(5) 0.010(5) C2A 0.066(5) 0.045(4) 0.034(4) 0.007(3) 0.004(3) 0.002(4) C3A 0.066(5) 0.044(4) 0.041(4) 0.014(3) 0.008(4) 0.006(4) C4A 0.079(7) 0.068(7) 0.059(6) 0.011(5) -0.006(5) -0.005(6) 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' 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' P P 0.2955 0.4335 '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 P1 Fe1 P1 180.0 3_566 . ? P2 Fe1 P1 97.827(19) . 3_566 ? P2 Fe1 P1 82.174(19) . . ? P2 Fe1 P1 82.174(19) 3_566 3_566 ? P2 Fe1 P1 97.825(19) 3_566 . ? P2 Fe1 P2 180.0 3_566 . ? N1 Fe1 P1 88.93(6) 3_566 3_566 ? N1 Fe1 P1 91.07(6) 3_566 . ? N1 Fe1 P1 88.93(6) . . ? N1 Fe1 P1 91.07(6) . 3_566 ? N1 Fe1 P2 90.25(6) 3_566 3_566 ? N1 Fe1 P2 89.75(6) 3_566 . ? N1 Fe1 P2 90.24(6) . . ? N1 Fe1 P2 89.76(6) . 3_566 ? N1 Fe1 N1 180.0 3_566 . ? C13 P1 Fe1 108.77(8) . . ? C13 P1 C19 99.03(10) . . ? C13 P1 C25 103.03(11) . . ? C19 P1 Fe1 118.05(8) . . ? C19 P1 C25 108.31(11) . . ? C25 P1 Fe1 117.03(8) . . ? C18 P2 Fe1 108.17(7) . . ? C18 P2 C31 100.63(10) . . ? C18 P2 C37 101.00(10) . . ? C31 P2 Fe1 121.53(8) . . ? C31 P2 C37 104.79(11) . . ? C37 P2 Fe1 117.55(7) . . ? C11 N1 Fe1 174.17(19) . . ? N1 C11 C12 179.1(3) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 P1 122.67(18) . . ? C18 C13 P1 117.74(17) . . ? C18 C13 C14 119.6(2) . . ? C13 C14 H14 120.1 . . ? C15 C14 C13 119.9(2) . . ? C15 C14 H14 120.1 . . ? C14 C15 H15 119.9 . . ? C14 C15 C16 120.3(2) . . ? C16 C15 H15 119.9 . . ? C15 C16 H16 119.8 . . ? C17 C16 C15 120.4(2) . . ? C17 C16 H16 119.8 . . ? C16 C17 H17 120.3 . . ? C16 C17 C18 119.4(2) . . ? C18 C17 H17 120.3 . . ? C13 C18 P2 116.14(17) . . ? C13 C18 C17 120.4(2) . . ? C17 C18 P2 122.77(18) . . ? C20 C19 P1 116.34(17) . . ? C24 C19 P1 124.90(18) . . ? C24 C19 C20 118.7(2) . . ? C19 C20 H20 119.8 . . ? C21 C20 C19 120.4(2) . . ? C21 C20 H20 119.8 . . ? C20 C21 H21 120.0 . . ? C22 C21 C20 120.1(2) . . ? C22 C21 H21 120.0 . . ? C21 C22 H22 119.9 . . ? C23 C22 C21 120.2(2) . . ? C23 C22 H22 119.9 . . ? C22 C23 H23 119.8 . . ? C22 C23 C24 120.3(2) . . ? C24 C23 H23 119.8 . . ? C19 C24 C23 120.2(2) . . ? C19 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C26 C25 P1 121.70(19) . . ? C30 C25 P1 119.55(18) . . ? C30 C25 C26 118.6(2) . . ? C25 C26 H26 119.8 . . ? C27 C26 C25 120.3(2) . . ? C27 C26 H26 119.8 . . ? C26 C27 H27 119.7 . . ? C28 C27 C26 120.6(3) . . ? C28 C27 H27 119.7 . . ? C27 C28 H28 120.2 . . ? C27 C28 C29 119.6(2) . . ? C29 C28 H28 120.2 . . ? C28 C29 H29 119.9 . . ? C28 C29 C30 120.2(2) . . ? C30 C29 H29 119.9 . . ? C25 C30 H30 119.7 . . ? C29 C30 C25 120.6(2) . . ? C29 C30 H30 119.7 . . ? C32 C31 P2 117.32(18) . . ? C36 C31 P2 123.41(18) . . ? C36 C31 C32 119.3(2) . . ? C31 C32 H32 119.7 . . ? C33 C32 C31 120.5(2) . . ? C33 C32 H32 119.7 . . ? C32 C33 H33 120.1 . . ? C32 C33 C34 119.8(2) . . ? C34 C33 H33 120.1 . . ? C33 C34 H34 119.9 . . ? C35 C34 C33 120.2(2) . . ? C35 C34 H34 119.9 . . ? C34 C35 H35 119.9 . . ? C34 C35 C36 120.2(2) . . ? C36 C35 H35 119.9 . . ? C31 C36 H36 120.0 . . ? C35 C36 C31 119.9(2) . . ? C35 C36 H36 120.0 . . ? C38 C37 P2 121.28(18) . . ? C42 C37 P2 120.03(18) . . ? C42 C37 C38 118.7(2) . . ? C37 C38 H38 119.9 . . ? C39 C38 C37 120.3(2) . . ? C39 C38 H38 119.9 . . ? C38 C39 H39 119.6 . . ? C40 C39 C38 120.7(2) . . ? C40 C39 H39 119.6 . . ? C39 C40 H40 120.3 . . ? C39 C40 C41 119.4(2) . . ? C41 C40 H40 120.3 . . ? C40 C41 H41 119.8 . . ? C40 C41 C42 120.5(2) . . ? C42 C41 H41 119.8 . . ? C37 C42 H42 119.8 . . ? C41 C42 C37 120.4(2) . . ? C41 C42 H42 119.8 . . ? Fe3 Fe2 Fe4 60.986(15) . . ? C1 Fe2 Fe3 49.63(7) . . ? C1 Fe2 Fe4 46.21(8) . . ? C8 Fe2 Fe3 132.65(10) . . ? C8 Fe2 Fe4 83.45(9) . . ? C8 Fe2 C1 123.71(12) . . ? C8 Fe2 C9 101.20(14) . . ? C8 Fe2 C10 100.37(12) . . ? C8 Fe2 C43 91.24(12) . . ? C9 Fe2 Fe3 117.84(9) . . ? C9 Fe2 Fe4 107.26(9) . . ? C9 Fe2 C1 77.56(11) . . ? C9 Fe2 C43 167.30(12) . . ? C10 Fe2 Fe3 102.43(9) . . ? C10 Fe2 Fe4 157.39(9) . . ? C10 Fe2 C1 135.90(12) . . ? C10 Fe2 C9 93.94(13) . . ? C10 Fe2 C43 86.26(11) . . ? C43 Fe2 Fe3 50.00(7) . . ? C43 Fe2 Fe4 71.32(8) . . ? C43 Fe2 C1 93.45(10) . . ? Fe2 Fe3 Fe4 60.190(15) . . ? C1 Fe3 Fe2 50.53(8) . . ? C1 Fe3 Fe4 45.91(8) . . ? C1 Fe3 C43 94.61(11) . . ? C2 Fe3 Fe2 98.83(8) . . ? C2 Fe3 Fe4 156.52(8) . . ? C2 Fe3 C1 130.14(12) . . ? C2 Fe3 C3 91.59(12) . . ? C2 Fe3 C43 87.63(11) . . ? C3 Fe3 Fe2 121.08(8) . . ? C3 Fe3 Fe4 107.97(9) . . ? C3 Fe3 C1 79.11(11) . . ? C3 Fe3 C43 171.07(11) . . ? C4 Fe3 Fe2 131.80(8) . . ? C4 Fe3 Fe4 85.79(9) . . ? C4 Fe3 C1 126.10(12) . . ? C4 Fe3 C2 103.74(12) . . ? C4 Fe3 C3 100.41(12) . . ? C4 Fe3 C43 88.41(11) . . ? C43 Fe3 Fe2 50.40(8) . . ? C43 Fe3 Fe4 71.01(8) . . ? Fe2 Fe4 Fe3 58.824(15) . . ? C1 Fe4 Fe2 50.22(8) . . ? C1 Fe4 Fe3 48.99(8) . . ? C5 Fe4 Fe2 150.24(9) . . ? C5 Fe4 Fe3 95.42(9) . . ? C5 Fe4 C1 102.47(12) . . ? C5 Fe4 C6 100.24(12) . . ? C6 Fe4 Fe2 103.23(8) . . ? C6 Fe4 Fe3 111.98(9) . . ? C6 Fe4 C1 151.51(12) . . ? C7 Fe4 Fe2 97.21(10) . . ? C7 Fe4 Fe3 141.94(11) . . ? C7 Fe4 C1 93.04(13) . . ? C7 Fe4 C5 95.71(13) . . ? C7 Fe4 C6 101.62(13) . . ? Fe2 C1 H1 129.6(16) . . ? Fe3 C1 Fe2 79.83(10) . . ? Fe3 C1 H1 127.4(16) . . ? Fe4 C1 Fe2 83.57(11) . . ? Fe4 C1 Fe3 85.11(11) . . ? Fe4 C1 H1 133.2(17) . . ? O2 C2 Fe3 179.0(2) . . ? O3 C3 Fe3 178.5(2) . . ? O4 C4 Fe3 179.4(3) . . ? O5 C5 Fe4 179.3(3) . . ? O6 C6 Fe4 177.7(2) . . ? O7 C7 Fe4 176.7(3) . . ? O8 C8 Fe2 178.3(3) . . ? O9 C9 Fe2 179.2(3) . . ? O10 C10 Fe2 177.9(2) . . ? Fe3 C43 Fe2 79.60(10) . . ? O1 C43 Fe2 139.9(2) . . ? O1 C43 Fe3 139.7(2) . . ? C2A O1A C3A 113.0(7) . . ? H1AA C1A H1AB 109.5 . . ? H1AA C1A H1AC 109.5 . . ? H1AB C1A H1AC 109.5 . . ? C2A C1A H1AA 109.5 . . ? C2A C1A H1AB 109.5 . . ? C2A C1A H1AC 109.5 . . ? O1A C2A C1A 109.3(8) . . ? O1A C2A H2AA 109.8 . . ? O1A C2A H2AB 109.8 . . ? C1A C2A H2AA 109.8 . . ? C1A C2A H2AB 109.8 . . ? H2AA C2A H2AB 108.3 . . ? O1A C3A H3AA 110.1 . . ? O1A C3A H3AB 110.1 . . ? O1A C3A C4A 107.8(8) . . ? H3AA C3A H3AB 108.5 . . ? C4A C3A H3AA 110.1 . . ? C4A C3A H3AB 110.1 . . ? C3A C4A H4AA 109.5 . . ? C3A C4A H4AB 109.5 . . ? C3A C4A H4AC 109.5 . . ? H4AA C4A H4AB 109.5 . . ? H4AA C4A H4AC 109.5 . . ? H4AB C4A H4AC 109.5 . . ? 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 P1 2.3293(6) . ? Fe1 P1 2.3292(6) 3_566 ? Fe1 P2 2.3237(5) 3_566 ? Fe1 P2 2.3238(5) . ? Fe1 N1 1.9034(19) 3_566 ? Fe1 N1 1.9034(19) . ? P1 C13 1.823(2) . ? P1 C19 1.831(2) . ? P1 C25 1.832(2) . ? P2 C18 1.823(2) . ? P2 C31 1.829(2) . ? P2 C37 1.837(2) . ? N1 C11 1.136(3) . ? C11 C12 1.453(3) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.402(3) . ? C13 C18 1.387(3) . ? C14 H14 0.9500 . ? C14 C15 1.383(3) . ? C15 H15 0.9500 . ? C15 C16 1.390(4) . ? C16 H16 0.9500 . ? C16 C17 1.386(3) . ? C17 H17 0.9500 . ? C17 C18 1.400(3) . ? C19 C20 1.401(3) . ? C19 C24 1.395(3) . ? C20 H20 0.9500 . ? C20 C21 1.390(3) . ? C21 H21 0.9500 . ? C21 C22 1.381(4) . ? C22 H22 0.9500 . ? C22 C23 1.376(4) . ? C23 H23 0.9500 . ? C23 C24 1.396(3) . ? C24 H24 0.9500 . ? C25 C26 1.399(3) . ? C25 C30 1.395(3) . ? C26 H26 0.9500 . ? C26 C27 1.389(4) . ? C27 H27 0.9500 . ? C27 C28 1.383(4) . ? C28 H28 0.9500 . ? C28 C29 1.385(4) . ? C29 H29 0.9500 . ? C29 C30 1.392(4) . ? C30 H30 0.9500 . ? C31 C32 1.397(3) . ? C31 C36 1.393(3) . ? C32 H32 0.9500 . ? C32 C33 1.382(3) . ? C33 H33 0.9500 . ? C33 C34 1.387(4) . ? C34 H34 0.9500 . ? C34 C35 1.383(4) . ? C35 H35 0.9500 . ? C35 C36 1.391(4) . ? C36 H36 0.9500 . ? C37 C38 1.398(3) . ? C37 C42 1.395(3) . ? C38 H38 0.9500 . ? C38 C39 1.387(4) . ? C39 H39 0.9500 . ? C39 C40 1.383(4) . ? C40 H40 0.9500 . ? C40 C41 1.383(4) . ? C41 H41 0.9500 . ? C41 C42 1.390(3) . ? C42 H42 0.9500 . ? Fe2 Fe3 2.5286(5) . ? Fe2 Fe4 2.5644(6) . ? Fe2 C1 1.983(3) . ? Fe2 C8 1.785(3) . ? Fe2 C9 1.798(3) . ? Fe2 C10 1.796(3) . ? Fe2 C43 1.981(3) . ? Fe3 Fe4 2.5845(5) . ? Fe3 C1 1.957(3) . ? Fe3 C2 1.791(3) . ? Fe3 C3 1.794(3) . ? Fe3 C4 1.788(3) . ? Fe3 C43 1.970(3) . ? Fe4 C1 1.863(3) . ? Fe4 C5 1.779(3) . ? Fe4 C6 1.815(3) . ? Fe4 C7 1.770(3) . ? O1 C43 1.181(3) . ? O2 C2 1.142(3) . ? O3 C3 1.144(3) . ? O4 C4 1.146(3) . ? O5 C5 1.150(3) . ? O6 C6 1.150(3) . ? O7 C7 1.149(4) . ? O8 C8 1.148(4) . ? O9 C9 1.144(4) . ? O10 C10 1.141(3) . ? C1 H1 1.00(3) . ? O1A C2A 1.416(12) . ? O1A C3A 1.427(13) . ? C1A H1AA 0.9800 . ? C1A H1AB 0.9800 . ? C1A H1AC 0.9800 . ? C1A C2A 1.499(11) . ? C2A H2AA 0.9900 . ? C2A H2AB 0.9900 . ? C3A H3AA 0.9900 . ? C3A H3AB 0.9900 . ? C3A C4A 1.509(11) . ? C4A H4AA 0.9800 . ? C4A H4AB 0.9800 . ? C4A H4AC 0.9800 . ? 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 P1 C13 C14 -171.33(17) . . . . ? Fe1 P1 C13 C18 7.9(2) . . . . ? Fe1 P1 C19 C20 69.22(19) . . . . ? Fe1 P1 C19 C24 -107.9(2) . . . . ? Fe1 P1 C25 C26 78.5(2) . . . . ? Fe1 P1 C25 C30 -97.21(19) . . . . ? Fe1 P2 C18 C13 -26.55(19) . . . . ? Fe1 P2 C18 C17 162.69(18) . . . . ? Fe1 P2 C31 C32 -68.67(19) . . . . ? Fe1 P2 C31 C36 111.6(2) . . . . ? Fe1 P2 C37 C38 116.84(18) . . . . ? Fe1 P2 C37 C42 -62.8(2) . . . . ? P1 C13 C14 C15 177.78(18) . . . . ? P1 C13 C18 P2 12.1(2) . . . . ? P1 C13 C18 C17 -176.89(18) . . . . ? P1 C19 C20 C21 -174.61(18) . . . . ? P1 C19 C24 C23 174.36(19) . . . . ? P1 C25 C26 C27 -178.2(2) . . . . ? P1 C25 C30 C29 176.63(19) . . . . ? P2 C31 C32 C33 178.79(19) . . . . ? P2 C31 C36 C35 -178.8(2) . . . . ? P2 C37 C38 C39 179.86(19) . . . . ? P2 C37 C42 C41 -179.28(18) . . . . ? C13 P1 C19 C20 -47.77(19) . . . . ? C13 P1 C19 C24 135.2(2) . . . . ? C13 P1 C25 C26 -162.2(2) . . . . ? C13 P1 C25 C30 22.1(2) . . . . ? C13 C14 C15 C16 -0.5(4) . . . . ? C14 C13 C18 P2 -168.65(17) . . . . ? C14 C13 C18 C17 2.3(3) . . . . ? C14 C15 C16 C17 1.6(4) . . . . ? C15 C16 C17 C18 -0.6(4) . . . . ? C16 C17 C18 P2 169.05(19) . . . . ? C16 C17 C18 C13 -1.3(3) . . . . ? C18 P2 C31 C32 50.5(2) . . . . ? C18 P2 C31 C36 -129.2(2) . . . . ? C18 P2 C37 C38 -0.5(2) . . . . ? C18 P2 C37 C42 179.86(19) . . . . ? C18 C13 C14 C15 -1.4(3) . . . . ? C19 P1 C13 C14 -47.5(2) . . . . ? C19 P1 C13 C18 131.71(19) . . . . ? C19 P1 C25 C26 -57.9(2) . . . . ? C19 P1 C25 C30 126.32(19) . . . . ? C19 C20 C21 C22 -0.7(4) . . . . ? C20 C19 C24 C23 -2.7(3) . . . . ? C20 C21 C22 C23 -1.3(4) . . . . ? C21 C22 C23 C24 1.3(4) . . . . ? C22 C23 C24 C19 0.7(4) . . . . ? C24 C19 C20 C21 2.7(3) . . . . ? C25 P1 C13 C14 63.8(2) . . . . ? C25 P1 C13 C18 -116.99(19) . . . . ? C25 P1 C19 C20 -154.81(17) . . . . ? C25 P1 C19 C24 28.1(2) . . . . ? C25 C26 C27 C28 2.6(4) . . . . ? C26 C25 C30 C29 0.8(4) . . . . ? C26 C27 C28 C29 -1.0(4) . . . . ? C27 C28 C29 C30 -0.7(4) . . . . ? C28 C29 C30 C25 0.8(4) . . . . ? C30 C25 C26 C27 -2.4(4) . . . . ? C31 P2 C18 C13 -154.98(18) . . . . ? C31 P2 C18 C17 34.3(2) . . . . ? C31 P2 C37 C38 -104.8(2) . . . . ? C31 P2 C37 C42 75.6(2) . . . . ? C31 C32 C33 C34 0.4(4) . . . . ? C32 C31 C36 C35 1.5(4) . . . . ? C32 C33 C34 C35 0.6(4) . . . . ? C33 C34 C35 C36 -0.6(4) . . . . ? C34 C35 C36 C31 -0.5(4) . . . . ? C36 C31 C32 C33 -1.5(3) . . . . ? C37 P2 C18 C13 97.49(18) . . . . ? C37 P2 C18 C17 -73.3(2) . . . . ? C37 P2 C31 C32 155.00(18) . . . . ? C37 P2 C31 C36 -24.7(2) . . . . ? C37 C38 C39 C40 -0.6(4) . . . . ? C38 C37 C42 C41 1.1(3) . . . . ? C38 C39 C40 C41 1.2(4) . . . . ? C39 C40 C41 C42 -0.6(4) . . . . ? C40 C41 C42 C37 -0.6(4) . . . . ? C42 C37 C38 C39 -0.5(4) . . . . ? Fe2 Fe4 C1 Fe3 -80.29(9) . . . . ? Fe3 Fe4 C1 Fe2 80.29(9) . . . . ? C5 Fe4 C1 Fe2 166.62(11) . . . . ? C5 Fe4 C1 Fe3 86.33(12) . . . . ? C6 Fe4 C1 Fe2 24.5(3) . . . . ? C6 Fe4 C1 Fe3 -55.8(3) . . . . ? C7 Fe4 C1 Fe2 -96.85(11) . . . . ? C7 Fe4 C1 Fe3 -177.14(11) . . . . ? C2A O1A C3A C4A -177.4(9) . . . . ? C3A O1A C2A C1A -179.0(9) . . . . ?