#------------------------------------------------------------------------------ #$Date: 2019-10-11 03:39:57 +0300 (Fri, 11 Oct 2019) $ #$Revision: 219265 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/23/45/7234535.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_7234535 loop_ _publ_author_name 'Galadzhun, Iurii' 'Capel Berdiell, Izar' 'Shahid, Namrah' 'Halcrow, Malcolm' _publ_section_title ; An Iron(II) Coordination Polymer of a Triazolyl Tris-Heterocycle Showing a Spin State Conversion Triggered by Loss of Lattice Solvent ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/C9CE01496A _journal_year 2019 _chemical_formula_moiety 'C40 H36 Fe2 N24 O2, 4(B F4), 0.66(H2 O), C H3 N O2' _chemical_formula_sum 'C41 H40.32 B4 F16 Fe2 N25 O4.66' _chemical_formula_weight 1416.80 _chemical_name_systematic ; catena-Bis-[/m-{2-(pyrazol-1-yl)-6-(1,2,4-triazol-1-yl)pyridine}]- bis [2-(pyrazol-1-yl)-6-(1,2,4-triazol-1-yl)pyridine]diaqua-di-iron(II) tetrakis-tetrafluoroborate hydrate (2/0.66) nitromethane solvate ; _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_date 2019-07-03 _audit_creation_method ; Olex2 1.2 (compiled Apr 23 2013 17:54:37, GUI svn.r4466) ; _audit_update_record ; 2019-09-04 deposited with the CCDC. 2019-10-10 downloaded from the CCDC. ; _cell_angle_alpha 90.00 _cell_angle_beta 99.397(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 19.9010(5) _cell_length_b 15.9683(4) _cell_length_c 18.7282(6) _cell_measurement_reflns_used 7325 _cell_measurement_temperature 290(2) _cell_measurement_theta_max 73.40 _cell_measurement_theta_min 4.43 _cell_volume 5871.7(3) _computing_cell_refinement 'CrysAlisPro, Agilent Technologies' _computing_data_collection 'CrysAlisPro, Agilent Technologies' _computing_data_reduction 'CrysAlisPro, Agilent Technologies' _computing_molecular_graphics 'XSEED (Barbour, 2001)' _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 290(2) _diffrn_detector_area_resol_mean 5.3095 _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.979 _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator mirror _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0451 _diffrn_reflns_av_unetI/netI 0.0429 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 19128 _diffrn_reflns_theta_full 72.00 _diffrn_reflns_theta_max 73.87 _diffrn_reflns_theta_min 4.09 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 5.013 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.074 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.603 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 2858 _exptl_crystal_size_max 0.90 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.28 _refine_diff_density_max 0.510 _refine_diff_density_min -0.530 _refine_diff_density_rms 0.074 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 453 _refine_ls_number_reflns 5822 _refine_ls_number_restraints 75 _refine_ls_restrained_S_all 1.077 _refine_ls_R_factor_all 0.0899 _refine_ls_R_factor_gt 0.0834 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1571P)^2^+6.4738P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2363 _refine_ls_wR_factor_ref 0.2454 _reflns_number_gt 5051 _reflns_number_total 5822 _reflns_threshold_expression >2sigma(I) _cod_data_source_file c9ce01496a2.cif _cod_data_source_block ig12c4rt _cod_database_code 7234535 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups, All O(H,H) groups 2. Restrained distances B36-F37A = B36-F38A = B36-F39A = B36-F40A 1.37971 with sigma of 0.02 B36-F37B = B36-F38B = B36-F39B = B36-F40B 1.37971 with sigma of 0.02 B36-F37C = B36-F38C = B36-F39C = B36-F40C 1.37971 with sigma of 0.02 F37A-F38A = F37A-F39A = F37A-F40A = F38A-F39A = F38A-F40A = F39A-F40A 2.253066 with sigma of 0.02 F37B-F38B = F37B-F39B = F37B-F40B = F38B-F39B = F38B-F40B = F39B-F40B 2.253066 with sigma of 0.02 F37C-F38C = F37C-F39C = F37C-F40C = F38C-F39C = F38C-F40C = F39C-F40C 2.253066 with sigma of 0.02 B41-F42A = B41-F43A = B41-F44A = B41-F45A 1.37971 with sigma of 0.02 B41-F42B = B41-F43B = B41-F44B = B41-F45B 1.37971 with sigma of 0.02 B41-F42C = B41-F43C = B41-F44C = B41-F45C 1.37971 with sigma of 0.02 F42A-F43A = F42A-F44A = F42A-F45A = F43A-F44A = F43A-F45A = F44A-F45A 2.253066 with sigma of 0.02 F42B-F43B = F42B-F44B = F42B-F45B = F43B-F44B = F43B-F45B = F44B-F45B 2.253066 with sigma of 0.02 F42C-F43C = F42C-F44C = F42C-F45C = F43C-F44C = F43C-F45C = F44C-F45C 2.253066 with sigma of 0.02 O35-H35A = O35-H35B 0.9 with sigma of 0.02 H35A-H35B 1.37 with sigma of 0.02 C47A-N48 = C47B-N48 1.45 with sigma of 0.02 N48-O49A = N48-O50A = N48-O49B = N48-O50B 1.22 with sigma of 0.02 O49A-O50A = O49B-O50B 2.09 with sigma of 0.02 C47A-O49A = C47A-O50A = C47B-O49B = C47B-O50B 2.3 with sigma of 0.02 3. Others 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=FVAR(1) 1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1(DFIX)=1.633*FVAR(2) Fixed Sof: N3A(0.51) C4A(0.51) C5A(0.51) H5A(0.51) C6A(0.51) H6A(0.51) C7A(0.51) H7A(0.51) C8A(0.51) N9A(0.51) N10A(0.51) C11A(0.51) H11A(0.51) C12A(0.51) H12A(0.51) C13A(0.51) H13A(0.51) N3B(0.49) C4B(0.49) C5B(0.49) H5B(0.49) C6B(0.49) H6B(0.49) C7B(0.49) H7B(0.49) C8B(0.49) N9B(0.49) N10B(0.49) C11B(0.49) H11B(0.49) C12B(0.49) H12B(0.49) C13B(0.49) H13B(0.49) F37A(0.34) F38A(0.34) F39A(0.34) F40A(0.34) F37B(0.33) F38B(0.33) F39B(0.33) F40B(0.33) F37C(0.33) F38C(0.33) F39C(0.33) F40C(0.33) F42A(0.34) F43A(0.34) F44A(0.34) F45A(0.34) F42B(0.33) F43B(0.33) F44B(0.33) F45B(0.33) F42C(0.33) F43C(0.33) F44C(0.33) F45C(0.33) O46(0.33) C47A(0.3) H47A(0.3) H47B(0.3) H47C(0.3) O49A(0.3) O50A(0.3) C47B(0.2) H47D(0.2) H47E(0.2) H47F(0.2) O49B(0.2) O50B(0.2) 4.a Me refined with riding coordinates: C47A(H47A,H47B,H47C) 4.b Aromatic/amide H refined with riding coordinates: C5A(H5A), C6A(H6A), C7A(H7A), C11A(H11A), C12A(H12A), C13A(H13A), C5B(H5B), C6B(H6B), C7B(H7B), C11B(H11B), C12B(H12B), C13B(H13B), C16(H16), C18(H18), C21(H21), C22(H22), C23(H23), C27(H27), C28(H28), C29(H29), C32(H32), C34(H34) 4.c Idealised Me refined as rotating group: C47B(H47D,H47E,H47F) ; _shelx_res_file ; TITL ig12c4+fe-meno2_a.res in C2/c CELL 1.54184 19.901 15.9683 18.7282 90 99.397 90 ZERR 4 0.0005 0.0004 0.0006 0 0.003 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H B F Fe N O UNIT 164 161.28 16 64 8 100 18.64 EQIV $1 1-X,+Y,0.5-Z DFIX 21 B36 F37A B36 F38A B36 F39A B36 F40A DFIX 21 B36 F37B B36 F38B B36 F39B B36 F40B DFIX 21 B36 F37C B36 F38C B36 F39C B36 F40C DFIX 21.633 F37A F38A F37A F39A F37A F40A F38A F39A F38A F40A F39A F40A DFIX 21.633 F37B F38B F37B F39B F37B F40B F38B F39B F38B F40B F39B F40B DFIX 21.633 F37C F38C F37C F39C F37C F40C F38C F39C F38C F40C F39C F40C DFIX 21 B41 F42A B41 F43A B41 F44A B41 F45A DFIX 21 B41 F42B B41 F43B B41 F44B B41 F45B DFIX 21 B41 F42C B41 F43C B41 F44C B41 F45C DFIX 21.633 F42A F43A F42A F44A F42A F45A F43A F44A F43A F45A F44A F45A DFIX 21.633 F42B F43B F42B F44B F42B F45B F43B F44B F43B F45B F44B F45B DFIX 21.633 F42C F43C F42C F44C F42C F45C F43C F44C F43C F45C F44C F45C DFIX 0.9 O35 H35a O35 H35b DFIX 1.37 H35a H35b DFIX 1.45 C47A N48 C47B N48 DFIX 1.22 N48 O49A N48 O50A N48 O49B N48 O50B DFIX 2.09 O49A O50A O49B O50B DFIX 2.3 C47A O49A C47A O50A C47B O49B C47B O50B L.S. 8 PLAN 20 TEMP 17 HTAB O35 F37A HTAB O35 F37B HTAB O35 F37C HTAB O35 F45A HTAB O35 F45B HTAB O35 F44C FREE C47A C47A_$1 FREE C47B C47B_$1 FREE C47B O50B_$1 BOND $H REM Old TITL IG12C4+Fe-MeNO2 in C2/m REM ig12c4+fe-meno2_a.res in C2/c REM 448 parameters refined using 63 restraints REM Highest difference peak 0.892, deepest hole -0.730, 1-sigma level 0.099 REM 457 parameters refined using 75 restraints REM Highest difference peak 0.515, deepest hole -0.533, 1-sigma level 0.075 REM 453 parameters refined using 75 restraints REM Highest difference peak 0.514, deepest hole -0.530, 1-sigma level 0.074 REM Highest difference peak 0.509, deepest hole -0.530, 1-sigma level 0.074 GRID fmap 2 acta 144 MERG 2 REM C:/Users/chmmah/Desktop/290%20K/ig12c4rt.hkl WGHT 0.157100 6.465900 FVAR 3.11067 1.37971 FE1 5 0.500000 0.286952 0.250000 10.50000 0.07857 0.04901 = 0.06409 0.00000 0.01805 0.00000 FE2 5 0.500000 0.000000 0.500000 10.50000 0.05200 0.05182 = 0.04968 -0.00151 0.01371 0.00814 PART 1 N3A 6 0.595794 0.298958 0.289827 10.51000 0.05480 C4A 1 0.634408 0.355376 0.263632 10.51000 0.06233 C5A 1 0.702508 0.369331 0.294005 10.51000 0.07994 AFIX 43 H5A 2 0.729251 0.407975 0.274267 10.51000 -1.20000 AFIX 0 C6A 1 0.728631 0.322212 0.355754 10.51000 0.09666 AFIX 43 H6A 2 0.772701 0.332129 0.379518 10.51000 -1.20000 AFIX 0 C7A 1 0.690521 0.263050 0.380700 10.51000 0.08122 AFIX 43 H7A 2 0.707879 0.230298 0.420521 10.51000 -1.20000 AFIX 0 C8A 1 0.625299 0.252665 0.345489 10.51000 0.06066 N9A 6 0.598803 0.400006 0.205383 10.51000 0.06197 N10A 6 0.530471 0.377299 0.180483 10.51000 0.07073 C11A 1 0.511164 0.426513 0.126153 10.51000 0.08303 AFIX 43 H11A 2 0.467976 0.425369 0.098290 10.51000 -1.20000 AFIX 0 C12A 1 0.564066 0.483019 0.113880 10.51000 0.09539 AFIX 43 H12A 2 0.561260 0.523959 0.078197 10.51000 -1.20000 AFIX 0 C13A 1 0.619870 0.464771 0.165315 10.51000 0.07652 AFIX 43 H13A 2 0.662395 0.490396 0.171693 10.51000 -1.20000 AFIX 0 PART 0 PART 2 N3B 6 0.611645 0.284347 0.300397 10.49000 0.05306 C4B 1 0.654772 0.337996 0.278297 10.49000 0.05744 C5B 1 0.721959 0.340894 0.307518 10.49000 0.08335 AFIX 43 H5B 2 0.751134 0.379879 0.291953 10.49000 -1.20000 AFIX 0 C6B 1 0.743450 0.287850 0.357283 10.49000 0.08996 AFIX 43 H6B 2 0.789492 0.287669 0.376932 10.49000 -1.20000 AFIX 0 C7B 1 0.701743 0.231994 0.382423 10.49000 0.07288 AFIX 43 H7B 2 0.718249 0.194710 0.419285 10.49000 -1.20000 AFIX 0 C8B 1 0.635816 0.232322 0.352311 10.49000 0.05653 N9B 6 0.623167 0.388851 0.219429 10.49000 0.06452 N10B 6 0.555361 0.377638 0.192206 10.49000 0.06080 C11B 1 0.540334 0.434091 0.139815 10.49000 0.07383 AFIX 43 H11B 2 0.497091 0.442068 0.113222 10.49000 -1.20000 AFIX 0 C12B 1 0.595892 0.478232 0.130261 10.49000 0.08582 AFIX 43 H12B 2 0.598450 0.518913 0.095271 10.49000 -1.20000 AFIX 0 C13B 1 0.648207 0.451085 0.182690 10.49000 0.08266 AFIX 43 H13B 2 0.692471 0.471797 0.191146 10.49000 -1.20000 AFIX 0 PART 0 N14 6 0.581450 0.186061 0.369402 11.00000 0.05341 0.07115 = 0.05816 -0.00284 0.01203 -0.00527 N15 6 0.515881 0.190658 0.335736 11.00000 0.05430 0.05871 = 0.05948 0.00419 0.01080 -0.00087 C16 1 0.484856 0.133448 0.368203 11.00000 0.04937 0.06010 = 0.06522 0.00536 0.01264 0.00011 AFIX 43 H16 2 0.438551 0.122058 0.356297 11.00000 -1.20000 AFIX 0 N17 6 0.527037 0.092264 0.421110 11.00000 0.05599 0.06147 = 0.05734 0.00376 0.01407 0.00382 C18 1 0.586651 0.126579 0.419207 11.00000 0.05747 0.07955 = 0.05722 0.00475 0.00895 0.00389 AFIX 43 H18 2 0.626956 0.111222 0.448760 11.00000 -1.20000 AFIX 0 N19 6 0.249434 0.162606 0.551506 11.00000 0.05960 0.07340 = 0.06844 0.01159 0.02228 0.01780 C20 1 0.199980 0.206115 0.573924 11.00000 0.06655 0.07226 = 0.07874 0.01792 0.02826 0.02086 C21 1 0.132748 0.203560 0.539849 11.00000 0.06537 0.09476 = 0.09430 0.01370 0.03137 0.02034 AFIX 43 H21 2 0.099428 0.235701 0.556309 11.00000 -1.20000 AFIX 0 C22 1 0.117203 0.152139 0.481231 11.00000 0.05074 0.12197 = 0.12033 0.00473 0.01546 0.01119 AFIX 43 H22 2 0.072403 0.148314 0.457666 11.00000 -1.20000 AFIX 0 C23 1 0.168047 0.105078 0.456217 11.00000 0.05870 0.11613 = 0.09054 0.00074 0.01829 0.00776 AFIX 43 H23 2 0.158750 0.070064 0.416139 11.00000 -1.20000 AFIX 0 C24 1 0.232387 0.114043 0.494705 11.00000 0.05471 0.07757 = 0.07510 0.01192 0.02157 0.01170 N25 6 0.220808 0.256429 0.634104 11.00000 0.07419 0.08217 = 0.07758 0.01076 0.02876 0.02856 N26 6 0.176140 0.308626 0.660676 11.00000 0.08822 0.08622 = 0.09545 0.01307 0.04000 0.03698 C27 1 0.213344 0.347475 0.714367 11.00000 0.11441 0.09952 = 0.09585 -0.00277 0.03173 0.04375 AFIX 43 H27 2 0.196401 0.387342 0.742970 11.00000 -1.20000 AFIX 0 C28 1 0.282076 0.322268 0.724171 11.00000 0.10363 0.12594 = 0.09667 -0.01532 0.01384 0.03700 AFIX 43 H28 2 0.317730 0.341320 0.758727 11.00000 -1.20000 AFIX 0 C29 1 0.284612 0.265079 0.672926 11.00000 0.08548 0.11020 = 0.08547 -0.00247 0.01772 0.03799 AFIX 43 H29 2 0.323234 0.236056 0.664994 11.00000 -1.20000 AFIX 0 N30 6 0.288915 0.070435 0.474191 11.00000 0.05517 0.07767 = 0.06320 0.00268 0.01614 0.00769 N31 6 0.282073 0.015014 0.418349 11.00000 0.05956 0.08978 = 0.07877 -0.01097 0.01176 0.00377 C32 1 0.344344 -0.008633 0.417387 11.00000 0.06356 0.07770 = 0.06195 -0.00737 0.01290 0.00467 AFIX 43 H32 2 0.355870 -0.046970 0.384011 11.00000 -1.20000 AFIX 0 N33 6 0.391195 0.027217 0.469100 11.00000 0.05533 0.06406 = 0.05506 0.00295 0.01242 0.01078 C34 1 0.353791 0.077294 0.503521 11.00000 0.05765 0.06734 = 0.05934 0.00059 0.01288 0.01316 AFIX 43 H34 2 0.370648 0.111863 0.542290 11.00000 -1.20000 AFIX 0 O35 7 0.507012 0.094266 0.579615 11.00000 0.07771 0.07326 = 0.06961 -0.01953 0.02596 -0.00408 H35A 2 0.529038 0.142619 0.586867 11.00000 -1.50000 H35B 2 0.494520 0.085942 0.622544 11.00000 -1.50000 B36 3 0.381243 0.046106 0.716456 11.00000 0.09134 0.10530 = 0.08270 0.02338 0.04475 0.02502 PART 1 F37A 4 0.408999 0.076430 0.663363 10.34000 0.08855 F38A 4 0.311026 0.035169 0.686292 10.34000 0.10127 F39A 4 0.380817 0.104425 0.775389 10.34000 0.08598 F40A 4 0.407945 -0.030799 0.736794 10.34000 0.07442 PART 0 PART 2 F37B 4 0.423890 0.097301 0.681418 10.33000 0.08309 F38B 4 0.337880 0.002240 0.658515 10.33000 0.15075 F39B 4 0.345785 0.081991 0.758631 10.33000 0.10283 F40B 4 0.421410 -0.010940 0.758831 10.33000 0.12914 PART 0 PART 3 F37C 4 0.401822 0.107621 0.670315 10.33000 0.07484 F38C 4 0.316126 0.048933 0.719112 10.33000 0.11191 F39C 4 0.413136 0.074903 0.788348 10.33000 0.18226 F40C 4 0.404548 -0.030780 0.706712 10.33000 0.13642 PART 0 B41 3 0.592704 0.292213 0.548891 11.00000 0.13711 0.08354 = 0.09066 -0.01357 0.02794 -0.02081 PART 1 F42A 4 0.606772 0.345282 0.497811 10.34000 0.17436 F43A 4 0.634258 0.218542 0.544842 10.34000 0.12287 F44A 4 0.599069 0.322183 0.616441 10.34000 0.14619 F45A 4 0.528009 0.256607 0.524616 10.34000 0.15132 PART 0 PART 2 F42B 4 0.546101 0.299714 0.483322 10.33000 0.13044 F43B 4 0.644695 0.341038 0.550494 10.33000 0.13286 F44B 4 0.549409 0.324878 0.599248 10.33000 0.12971 F45B 4 0.601297 0.209870 0.564448 10.33000 0.09119 PART 0 PART 3 F42C 4 0.562987 0.348462 0.498340 10.33000 0.17083 F43C 4 0.638686 0.342358 0.600790 10.33000 0.10946 F44C 4 0.551542 0.251442 0.584146 10.33000 0.17656 F45C 4 0.643261 0.249005 0.520135 10.33000 0.16197 PART 0 O46 7 0.261223 -0.071122 0.572485 10.33000 0.10439 N48 6 0.500000 0.627597 0.250000 10.50000 0.10932 0.18531 = 0.10261 0.00000 0.01575 0.00000 PART 1 C47A 1 0.486776 0.716565 0.246769 10.30000 0.10708 AFIX 33 H47A 2 0.470207 0.733879 0.289806 10.30000 -1.50000 H47B 2 0.453213 0.728878 0.205180 10.30000 -1.50000 H47C 2 0.528120 0.746072 0.243174 10.30000 -1.50000 AFIX 0 O49A 7 0.455887 0.578952 0.221516 10.30000 0.10787 O50A 7 0.545343 0.600285 0.296516 10.30000 0.14140 PART 0 PART 2 C47B 1 0.489231 0.713266 0.223465 10.20000 0.15667 AFIX 137 H47D 2 0.444842 0.717836 0.194627 10.20000 -1.50000 H47E 2 0.523233 0.727307 0.194528 10.20000 -1.50000 H47F 2 0.492535 0.751013 0.263784 10.20000 -1.50000 AFIX 0 O49B 7 0.466690 0.572011 0.215113 10.20000 0.24839 O50B 7 0.557615 0.609032 0.280683 10.20000 0.15013 HKLF 4 REM ig12c4+fe-meno2_a.res in C2/c REM R1 = 0.0834 for 5051 Fo > 4sig(Fo) and 0.0899 for all 5822 data REM 453 parameters refined using 75 restraints END WGHT 0.1571 6.4742 REM Highest difference peak 0.510, deepest hole -0.530, 1-sigma level 0.074 Q1 1 0.5917 0.2189 0.6039 11.00000 0.05 0.51 Q2 1 0.5364 0.2862 0.2254 11.00000 0.05 0.49 Q3 1 0.4410 0.0246 0.7855 11.00000 0.05 0.48 Q4 1 0.2463 -0.0925 0.5388 11.00000 0.05 0.45 Q5 1 0.5354 0.0013 0.4776 11.00000 0.05 0.45 Q6 1 0.5270 0.2665 0.4897 11.00000 0.05 0.44 Q7 1 0.5829 0.3163 0.4714 11.00000 0.05 0.43 Q8 1 0.6509 0.2999 0.5111 11.00000 0.05 0.41 Q9 1 0.2691 -0.0536 0.6038 11.00000 0.05 0.39 Q10 1 0.3833 0.1424 0.7777 11.00000 0.05 0.39 Q11 1 0.4585 0.0625 0.6954 11.00000 0.05 0.38 Q12 1 0.3167 -0.0040 0.6415 11.00000 0.05 0.36 Q13 1 0.5397 0.3587 0.5709 11.00000 0.05 0.33 Q14 1 0.5375 0.3261 0.5387 11.00000 0.05 0.31 Q15 1 0.3316 0.0435 0.7509 11.00000 0.05 0.30 Q16 1 0.5357 0.2799 0.5829 11.00000 0.05 0.30 Q17 1 0.4944 0.1006 0.4510 11.00000 0.05 0.28 Q18 1 0.7159 0.3458 0.2789 11.00000 0.05 0.27 Q19 1 0.7006 0.3786 0.3272 11.00000 0.05 0.27 Q20 1 0.7404 0.3068 0.3252 11.00000 0.05 0.27 REM The information below was added by Olex2. REM REM R1 = 0.0834 for 5051 Fo > 4sig(Fo) and 0.0899 for all 19490 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.51, deepest hole -0.53 REM Mean Shift 0, Max Shift 0. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0899 REM R1_gt = 0.0834 REM wR_ref = 0.2454 REM GOOF = 1.043 REM Shift_max = 0 REM Shift_mean = 0 REM Reflections_all = 19490 REM Reflections_gt = 5051 REM Parameters = n/a REM Hole = 0.51 REM Peak = -0.53 REM Flack = n/a ; loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, y, -z+1/2' 3 'x+1/2, y+1/2, z' 4 '-x+1/2, y+1/2, -z+1/2' 5 '-x, -y, -z' 6 'x, -y, z-1/2' 7 '-x+1/2, -y+1/2, -z' 8 '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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.5000 0.28695(5) 0.2500 0.0632(3) Uani 1 2 d S . . Fe2 Fe 0.5000 0.0000 0.5000 0.0506(3) Uani 1 2 d S . . N3A N 0.5958(4) 0.2990(5) 0.2898(4) 0.055(2) Uiso 0.51 1 d P A 1 C4A C 0.6344(5) 0.3554(6) 0.2636(6) 0.062(2) Uiso 0.51 1 d P A 1 C5A C 0.7025(6) 0.3693(8) 0.2940(6) 0.080(3) Uiso 0.51 1 d P A 1 H5A H 0.7293 0.4080 0.2743 0.096 Uiso 0.51 1 calc PR A 1 C6A C 0.7286(8) 0.3222(10) 0.3558(9) 0.097(4) Uiso 0.51 1 d P A 1 H6A H 0.7727 0.3321 0.3795 0.116 Uiso 0.51 1 calc PR A 1 C7A C 0.6905(6) 0.2630(9) 0.3807(7) 0.081(3) Uiso 0.51 1 d P A 1 H7A H 0.7079 0.2303 0.4205 0.097 Uiso 0.51 1 calc PR A 1 C8A C 0.6253(5) 0.2527(8) 0.3455(6) 0.061(3) Uiso 0.51 1 d P A 1 N9A N 0.5988(5) 0.4000(5) 0.2054(4) 0.0620(18) Uiso 0.51 1 d P A 1 N10A N 0.5305(5) 0.3773(5) 0.1805(5) 0.071(2) Uiso 0.51 1 d P A 1 C11A C 0.5112(7) 0.4265(7) 0.1262(7) 0.083(3) Uiso 0.51 1 d P A 1 H11A H 0.4680 0.4254 0.0983 0.100 Uiso 0.51 1 calc PR A 1 C12A C 0.5641(9) 0.4830(9) 0.1139(8) 0.095(3) Uiso 0.51 1 d P A 1 H12A H 0.5613 0.5240 0.0782 0.114 Uiso 0.51 1 calc PR A 1 C13A C 0.6199(7) 0.4648(7) 0.1653(8) 0.077(2) Uiso 0.51 1 d P A 1 H13A H 0.6624 0.4904 0.1717 0.092 Uiso 0.51 1 calc PR A 1 N3B N 0.6116(4) 0.2843(5) 0.3004(5) 0.053(2) Uiso 0.49 1 d P A 2 C4B C 0.6548(5) 0.3380(6) 0.2783(5) 0.057(2) Uiso 0.49 1 d P A 2 C5B C 0.7220(7) 0.3409(9) 0.3075(8) 0.083(3) Uiso 0.49 1 d P A 2 H5B H 0.7511 0.3799 0.2920 0.100 Uiso 0.49 1 calc PR A 2 C6B C 0.7434(7) 0.2878(9) 0.3573(8) 0.090(3) Uiso 0.49 1 d P A 2 H6B H 0.7895 0.2877 0.3769 0.108 Uiso 0.49 1 calc PR A 2 C7B C 0.7017(6) 0.2320(8) 0.3824(6) 0.073(3) Uiso 0.49 1 d P A 2 H7B H 0.7182 0.1947 0.4193 0.087 Uiso 0.49 1 calc PR A 2 C8B C 0.6358(5) 0.2323(7) 0.3523(5) 0.057(3) Uiso 0.49 1 d P A 2 N9B N 0.6232(5) 0.3889(6) 0.2194(5) 0.065(2) Uiso 0.49 1 d P A 2 N10B N 0.5554(5) 0.3776(5) 0.1922(5) 0.0608(19) Uiso 0.49 1 d P A 2 C11B C 0.5403(7) 0.4341(7) 0.1398(6) 0.074(3) Uiso 0.49 1 d P A 2 H11B H 0.4971 0.4421 0.1132 0.089 Uiso 0.49 1 calc PR A 2 C12B C 0.5959(8) 0.4782(9) 0.1303(9) 0.086(3) Uiso 0.49 1 d P A 2 H12B H 0.5985 0.5189 0.0953 0.103 Uiso 0.49 1 calc PR A 2 C13B C 0.6482(8) 0.4511(8) 0.1827(7) 0.083(3) Uiso 0.49 1 d P A 2 H13B H 0.6925 0.4718 0.1911 0.099 Uiso 0.49 1 calc PR A 2 N14 N 0.58145(16) 0.1861(2) 0.36940(19) 0.0606(8) Uani 1 1 d . . . N15 N 0.51588(16) 0.1907(2) 0.33574(18) 0.0573(7) Uani 1 1 d . A . C16 C 0.48486(19) 0.1334(2) 0.3682(2) 0.0579(8) Uani 1 1 d . . . H16 H 0.4386 0.1221 0.3563 0.069 Uiso 1 1 calc R A . N17 N 0.52704(16) 0.0923(2) 0.42111(18) 0.0577(7) Uani 1 1 d . A . C18 C 0.5867(2) 0.1266(3) 0.4192(2) 0.0648(10) Uani 1 1 d . A . H18 H 0.6270 0.1112 0.4488 0.078 Uiso 1 1 calc R . . N19 N 0.24943(18) 0.1626(2) 0.5515(2) 0.0658(9) Uani 1 1 d . . . C20 C 0.2000(2) 0.2061(3) 0.5739(3) 0.0707(11) Uani 1 1 d . . . C21 C 0.1327(3) 0.2036(4) 0.5398(3) 0.0828(14) Uani 1 1 d . . . H21 H 0.0994 0.2357 0.5563 0.099 Uiso 1 1 calc R . . C22 C 0.1172(3) 0.1521(5) 0.4812(4) 0.0975(18) Uani 1 1 d . . . H22 H 0.0724 0.1483 0.4577 0.117 Uiso 1 1 calc R . . C23 C 0.1680(2) 0.1051(4) 0.4562(3) 0.0878(15) Uani 1 1 d . . . H23 H 0.1587 0.0701 0.4161 0.105 Uiso 1 1 calc R . . C24 C 0.2324(2) 0.1140(3) 0.4947(3) 0.0679(10) Uani 1 1 d . . . N25 N 0.2208(2) 0.2564(3) 0.6341(2) 0.0761(11) Uani 1 1 d . . . N26 N 0.1761(2) 0.3086(3) 0.6607(3) 0.0872(13) Uani 1 1 d . . . C27 C 0.2133(4) 0.3475(4) 0.7144(4) 0.1016(19) Uani 1 1 d . . . H27 H 0.1964 0.3873 0.7430 0.122 Uiso 1 1 calc R . . C28 C 0.2821(4) 0.3223(5) 0.7242(4) 0.109(2) Uani 1 1 d . . . H28 H 0.3177 0.3413 0.7587 0.131 Uiso 1 1 calc R . . C29 C 0.2846(3) 0.2651(4) 0.6729(3) 0.0933(17) Uani 1 1 d . . . H29 H 0.3232 0.2361 0.6650 0.112 Uiso 1 1 calc R . . N30 N 0.28891(17) 0.0704(2) 0.4742(2) 0.0646(8) Uani 1 1 d . . . N31 N 0.2821(2) 0.0150(3) 0.4183(3) 0.0760(10) Uani 1 1 d . . . C32 C 0.3443(2) -0.0086(3) 0.4174(3) 0.0674(10) Uani 1 1 d . . . H32 H 0.3559 -0.0470 0.3840 0.081 Uiso 1 1 calc R . . N33 N 0.39120(16) 0.0272(2) 0.46910(18) 0.0578(7) Uani 1 1 d . . . C34 C 0.3538(2) 0.0773(3) 0.5035(2) 0.0611(9) Uani 1 1 d . . . H34 H 0.3706 0.1119 0.5423 0.073 Uiso 1 1 calc R . . O35 O 0.50701(17) 0.0943(2) 0.57961(18) 0.0720(8) Uani 1 1 d D . . H35A H 0.529(3) 0.143(2) 0.587(3) 0.108 Uiso 1 1 d D . . H35B H 0.495(3) 0.086(4) 0.6225(19) 0.108 Uiso 1 1 d D . . B36 B 0.3812(3) 0.0461(4) 0.7165(3) 0.0897(19) Uani 1 1 d D . . F37A F 0.4090(7) 0.0764(8) 0.6634(6) 0.089(3) Uiso 0.34 1 d PD B 1 F38A F 0.3110(5) 0.0352(8) 0.6863(8) 0.101(3) Uiso 0.34 1 d PD B 1 F39A F 0.3808(6) 0.1044(6) 0.7754(5) 0.086(2) Uiso 0.34 1 d PD B 1 F40A F 0.4079(5) -0.0308(5) 0.7368(7) 0.074(2) Uiso 0.34 1 d PD B 1 F37B F 0.4239(6) 0.0973(8) 0.6814(6) 0.083(3) Uiso 0.33 1 d PD B 2 F38B F 0.3379(9) 0.0022(10) 0.6585(8) 0.151(6) Uiso 0.33 1 d PD B 2 F39B F 0.3458(7) 0.0820(8) 0.7586(7) 0.103(3) Uiso 0.33 1 d PD B 2 F40B F 0.4214(8) -0.0109(10) 0.7588(9) 0.129(6) Uiso 0.33 1 d PD B 2 F37C F 0.4018(6) 0.1076(7) 0.6703(6) 0.075(3) Uiso 0.33 1 d PD B 3 F38C F 0.3161(6) 0.0489(9) 0.7191(9) 0.112(4) Uiso 0.33 1 d PD B 3 F39C F 0.4131(10) 0.0749(13) 0.7883(8) 0.182(8) Uiso 0.33 1 d PD B 3 F40C F 0.4045(9) -0.0308(8) 0.7067(10) 0.136(6) Uiso 0.33 1 d PD B 3 B41 B 0.5927(4) 0.2922(4) 0.5489(4) 0.103(2) Uani 1 1 d D . . F42A F 0.6068(11) 0.3453(11) 0.4978(10) 0.174(7) Uiso 0.34 1 d PD C 1 F43A F 0.6343(7) 0.2185(8) 0.5448(9) 0.123(4) Uiso 0.34 1 d PD C 1 F44A F 0.5991(10) 0.3222(10) 0.6164(7) 0.146(5) Uiso 0.34 1 d PD C 1 F45A F 0.5280(6) 0.2566(10) 0.5246(10) 0.151(5) Uiso 0.34 1 d PD C 1 F42B F 0.5461(7) 0.2997(10) 0.4833(7) 0.130(4) Uiso 0.33 1 d PD C 2 F43B F 0.6447(6) 0.3410(9) 0.5505(9) 0.133(4) Uiso 0.33 1 d PD C 2 F44B F 0.5494(7) 0.3249(9) 0.5992(7) 0.130(4) Uiso 0.33 1 d PD C 2 F45B F 0.6013(6) 0.2099(5) 0.5644(6) 0.091(3) Uiso 0.33 1 d PD C 2 F42C F 0.5630(10) 0.3485(12) 0.4983(9) 0.171(7) Uiso 0.33 1 d PD C 3 F43C F 0.6387(6) 0.3424(8) 0.6008(7) 0.109(3) Uiso 0.33 1 d PD C 3 F44C F 0.5515(9) 0.2514(12) 0.5841(11) 0.177(7) Uiso 0.33 1 d PD C 3 F45C F 0.6433(8) 0.2490(12) 0.5201(10) 0.162(7) Uiso 0.33 1 d PD C 3 O46 O 0.2612(7) -0.0711(9) 0.5725(8) 0.104(4) Uiso 0.33 1 d P . . N48 N 0.5000 0.6276(8) 0.2500 0.133(3) Uani 1 2 d SD . . C47A C 0.4868(17) 0.7166(10) 0.247(3) 0.107(9) Uiso 0.30 1 d PD D 1 H47A H 0.4702 0.7339 0.2898 0.161 Uiso 0.30 1 calc PR D 1 H47B H 0.4532 0.7289 0.2052 0.161 Uiso 0.30 1 calc PR D 1 H47C H 0.5281 0.7461 0.2432 0.161 Uiso 0.30 1 calc PR D 1 O49A O 0.4559(15) 0.5790(17) 0.2215(15) 0.108(7) Uiso 0.30 1 d PD . 1 O50A O 0.5453(17) 0.600(2) 0.2965(19) 0.141(13) Uiso 0.30 1 d PD . 1 C47B C 0.489(4) 0.7133(18) 0.223(4) 0.16(3) Uiso 0.20 1 d PD D 2 H47D H 0.4448 0.7178 0.1946 0.235 Uiso 0.20 1 calc PR D 2 H47E H 0.5232 0.7273 0.1945 0.235 Uiso 0.20 1 calc PR D 2 H47F H 0.4925 0.7510 0.2638 0.235 Uiso 0.20 1 calc PR D 2 O49B O 0.467(3) 0.572(3) 0.215(5) 0.25(5) Uiso 0.20 1 d PD . 2 O50B O 0.5576(15) 0.609(4) 0.281(3) 0.15(2) Uiso 0.20 1 d PD . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0786(6) 0.0490(5) 0.0641(5) 0.000 0.0180(4) 0.000 Fe2 0.0520(4) 0.0518(4) 0.0497(5) -0.0015(3) 0.0137(3) 0.0081(3) N14 0.0534(16) 0.071(2) 0.0582(18) -0.0028(15) 0.0120(13) -0.0053(14) N15 0.0543(16) 0.0587(17) 0.0595(18) 0.0042(13) 0.0108(13) -0.0009(13) C16 0.0494(17) 0.060(2) 0.065(2) 0.0054(16) 0.0126(15) 0.0001(15) N17 0.0560(16) 0.0615(17) 0.0573(17) 0.0038(13) 0.0141(13) 0.0038(13) C18 0.057(2) 0.080(3) 0.057(2) 0.0047(18) 0.0089(17) 0.0039(18) N19 0.0596(18) 0.073(2) 0.068(2) 0.0116(17) 0.0223(15) 0.0178(15) C20 0.067(2) 0.072(3) 0.079(3) 0.018(2) 0.028(2) 0.0209(19) C21 0.065(3) 0.095(3) 0.094(4) 0.014(3) 0.031(2) 0.020(2) C22 0.051(2) 0.122(5) 0.120(5) 0.005(4) 0.015(3) 0.011(3) C23 0.059(2) 0.116(4) 0.091(4) 0.001(3) 0.018(2) 0.008(3) C24 0.055(2) 0.078(3) 0.075(3) 0.012(2) 0.0216(19) 0.0117(18) N25 0.074(2) 0.082(2) 0.078(2) 0.0108(19) 0.0288(19) 0.0286(19) N26 0.088(3) 0.086(3) 0.095(3) 0.013(2) 0.040(2) 0.037(2) C27 0.114(5) 0.100(4) 0.096(4) -0.003(3) 0.032(4) 0.044(4) C28 0.104(4) 0.126(5) 0.097(4) -0.015(4) 0.014(3) 0.037(4) C29 0.085(3) 0.110(4) 0.085(4) -0.002(3) 0.018(3) 0.038(3) N30 0.0552(17) 0.078(2) 0.0632(19) 0.0027(16) 0.0161(15) 0.0077(15) N31 0.060(2) 0.090(3) 0.079(3) -0.011(2) 0.0118(18) 0.0038(18) C32 0.064(2) 0.078(3) 0.062(2) -0.0074(19) 0.0129(19) 0.0047(19) N33 0.0553(16) 0.0641(18) 0.0551(17) 0.0030(14) 0.0124(13) 0.0108(14) C34 0.058(2) 0.067(2) 0.059(2) 0.0006(17) 0.0129(16) 0.0132(16) O35 0.0777(19) 0.0733(18) 0.0696(18) -0.0195(14) 0.0260(15) -0.0041(14) B36 0.091(4) 0.105(5) 0.083(4) 0.023(3) 0.045(3) 0.025(3) B41 0.137(7) 0.084(4) 0.091(5) -0.014(3) 0.028(4) -0.021(4) N48 0.109(7) 0.185(11) 0.103(6) 0.000 0.016(5) 0.000 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' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 N3A Fe1 N3A 168.7(5) 2_655 . N3A Fe1 N3B 175.0(3) . 2_655 N3A Fe1 N10A 78.8(4) . . N3A Fe1 N10A 93.4(4) . 2_655 N3A Fe1 N15 77.0(3) . . N3A Fe1 N15 111.3(2) . 2_655 N10A Fe1 N10A 93.1(5) 2_655 . N10A Fe1 N10B 94.1(2) 2_655 . N10A Fe1 N15 155.3(3) . . N10A Fe1 N15 92.8(3) . 2_655 N3B Fe1 N3B 177.9(4) 2_655 . N10A Fe1 N3B 96.7(4) 2_655 . N10A Fe1 N3B 84.7(4) . . N10B Fe1 N3B 71.5(3) . . N10B Fe1 N3B 110.0(3) . 2_655 N10B Fe1 N10B 98.0(4) . 2_655 N10B Fe1 N15 97.1(2) . 2_655 N10B Fe1 N15 142.2(3) . . N15 Fe1 N3B 70.8(2) . . N15 Fe1 N3B 107.7(2) . 2_655 N15 Fe1 N15 91.74(18) . 2_655 N17 Fe2 N17 180.00 . 5_656 N33 Fe2 N17 91.67(12) . . N33 Fe2 N17 88.33(12) . 5_656 N33 Fe2 N33 180.00 . 5_656 O35 Fe2 N17 89.91(13) . 5_656 O35 Fe2 N17 90.09(13) . . O35 Fe2 N33 89.63(13) . . O35 Fe2 N33 90.36(13) . 5_656 O35 Fe2 O35 180.00 5_656 . C4A N3A Fe1 121.1(8) . . C4A N3A C8A 117.2(9) . . C8A N3A Fe1 121.7(7) . . N3A C4A C5A 122.5(11) . . N3A C4A N9A 112.6(9) . . N9A C4A C5A 124.8(10) . . C4A C5A H5A 121.5 . . C4A C5A C6A 116.9(11) . . C6A C5A H5A 121.5 . . C5A C6A H6A 119.7 . . C7A C6A C5A 120.6(13) . . C7A C6A H6A 119.7 . . C6A C7A H7A 121.2 . . C6A C7A C8A 117.6(13) . . C8A C7A H7A 121.2 . . N3A C8A C7A 124.9(11) . . N3A C8A N14 115.2(8) . . C7A C8A N14 119.9(11) . . C4A N9A N10A 117.8(8) . . C13A N9A C4A 130.2(11) . . C13A N9A N10A 112.0(10) . . N9A N10A Fe1 109.4(6) . . C11A N10A Fe1 145.8(10) . . C11A N10A N9A 104.5(9) . . N10A C11A H11A 123.9 . . N10A C11A C12A 112.1(13) . . C12A C11A H11A 123.9 . . C11A C12A H12A 126.7 . . C13A C12A C11A 106.5(13) . . C13A C12A H12A 126.7 . . N9A C13A H13A 127.6 . . C12A C13A N9A 104.9(11) . . C12A C13A H13A 127.6 . . C4B N3B Fe1 119.9(8) . . C8B N3B Fe1 122.5(7) . . C8B N3B C4B 117.6(9) . . N3B C4B C5B 122.7(11) . . N3B C4B N9B 112.5(9) . . C5B C4B N9B 124.8(10) . . C4B C5B H5B 121.3 . . C6B C5B C4B 117.4(12) . . C6B C5B H5B 121.3 . . C5B C6B H6B 118.7 . . C5B C6B C7B 122.6(14) . . C7B C6B H6B 118.7 . . C6B C7B H7B 121.2 . . C8B C7B C6B 117.7(12) . . C8B C7B H7B 121.2 . . N3B C8B C7B 122.0(10) . . N3B C8B N14 107.6(8) . . C7B C8B N14 130.2(10) . . N10B N9B C4B 119.6(8) . . C13B N9B C4B 131.2(10) . . C13B N9B N10B 109.2(11) . . N9B N10B Fe1 116.2(6) . . C11B N10B Fe1 137.4(9) . . C11B N10B N9B 105.9(10) . . N10B C11B H11B 124.4 . . N10B C11B C12B 111.2(13) . . C12B C11B H11B 124.4 . . C11B C12B H12B 126.8 . . C11B C12B C13B 106.3(13) . . C13B C12B H12B 126.8 . . N9B C13B C12B 107.2(12) . . N9B C13B H13B 126.4 . . C12B C13B H13B 126.4 . . N15 N14 C8A 112.8(6) . . N15 N14 C8B 126.2(6) . . C18 N14 C8A 137.9(6) . . C18 N14 C8B 124.7(6) . . C18 N14 N15 109.0(3) . . N14 N15 Fe1 112.9(2) . . C16 N15 Fe1 143.4(3) . . C16 N15 N14 103.8(3) . . N15 C16 H16 123.4 . . N15 C16 N17 113.3(4) . . N17 C16 H16 123.4 . . C16 N17 Fe2 128.3(3) . . C18 N17 Fe2 128.0(3) . . C18 N17 C16 103.4(3) . . N14 C18 H18 124.7 . . N17 C18 N14 110.6(4) . . N17 C18 H18 124.7 . . C24 N19 C20 117.2(4) . . N19 C20 C21 123.3(5) . . N19 C20 N25 114.9(4) . . C21 C20 N25 121.8(4) . . C20 C21 H21 121.2 . . C22 C21 C20 117.6(5) . . C22 C21 H21 121.2 . . C21 C22 H22 119.7 . . C21 C22 C23 120.7(5) . . C23 C22 H22 119.7 . . C22 C23 H23 122.2 . . C24 C23 C22 115.6(6) . . C24 C23 H23 122.2 . . N19 C24 C23 125.6(4) . . N19 C24 N30 113.2(4) . . C23 C24 N30 121.1(5) . . N26 N25 C20 121.4(4) . . C29 N25 C20 128.2(4) . . C29 N25 N26 110.3(5) . . C27 N26 N25 104.4(5) . . N26 C27 H27 123.8 . . N26 C27 C28 112.4(5) . . C28 C27 H27 123.8 . . C27 C28 H28 127.7 . . C29 C28 C27 104.6(7) . . C29 C28 H28 127.7 . . N25 C29 H29 125.9 . . C28 C29 N25 108.2(5) . . C28 C29 H29 125.9 . . N31 N30 C24 122.7(4) . . C34 N30 C24 127.3(4) . . C34 N30 N31 110.0(3) . . C32 N31 N30 102.9(4) . . N31 C32 H32 122.8 . . N31 C32 N33 114.4(4) . . N33 C32 H32 122.8 . . C32 N33 Fe2 129.7(3) . . C34 N33 Fe2 126.8(3) . . C34 N33 C32 103.1(3) . . N30 C34 N33 109.6(4) . . N30 C34 H34 125.2 . . N33 C34 H34 125.2 . . Fe2 O35 H35A 135(4) . . Fe2 O35 H35B 122(4) . . H35A O35 H35B 101(3) . . F37A B36 F38A 104.6(8) . . F37A B36 F39A 113.5(8) . . F37A B36 F40A 110.6(8) . . F38A B36 F39A 104.7(7) . . F40A B36 F38A 108.1(8) . . F40A B36 F39A 114.6(8) . . F37B B36 F38B 105.1(9) . . F39B B36 F37B 117.5(9) . . F39B B36 F38B 111.0(10) . . F39B B36 F40B 105.5(9) . . F40B B36 F37B 108.3(9) . . F40B B36 F38B 109.3(10) . . F37C B36 F39C 102.6(10) . . F38C B36 F37C 112.8(8) . . F38C B36 F39C 103.8(10) . . F38C B36 F40C 114.0(10) . . F40C B36 F37C 114.5(9) . . F40C B36 F39C 107.8(11) . . F42A B41 F43A 106.8(11) . . F42A B41 F45A 108.1(11) . . F44A B41 F42A 116.7(11) . . F44A B41 F43A 111.9(10) . . F44A B41 F45A 112.9(10) . . F45A B41 F43A 98.9(9) . . F42B B41 F44B 99.0(9) . . F43B B41 F42B 112.2(10) . . F43B B41 F44B 108.7(9) . . F43B B41 F45B 120.6(10) . . F45B B41 F42B 108.1(9) . . F45B B41 F44B 105.9(8) . . F42C B41 F43C 104.7(10) . . F42C B41 F45C 108.3(11) . . F44C B41 F42C 116.2(12) . . F44C B41 F43C 108.3(10) . . F44C B41 F45C 119.9(12) . . F45C B41 F43C 96.6(9) . . N48 C47A H47A 109.5 . . N48 C47A H47B 109.5 . . N48 C47A H47C 109.5 . . H47A C47A H47B 109.5 . . H47A C47A H47C 109.5 . . H47B C47A H47C 109.5 . . O49A N48 C47A 119.5(15) . . O49A N48 O50A 118.3(18) . . O50A N48 C47A 119.1(17) . . N48 C47B H47D 109.5 . . N48 C47B H47E 109.5 . . N48 C47B H47F 109.5 . . H47D C47B H47E 109.5 . . H47D C47B H47F 109.5 . . H47E C47B H47F 109.5 . . O49B N48 C47B 117(2) . . O49B N48 O50B 117(2) . . O50B N48 C47B 117(2) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Fe1 N3A 1.940(9) Fe1 N10A 2.098(9) Fe1 N3B 2.268(9) Fe1 N10B 2.207(9) Fe1 N15 2.208(3) Fe2 N17 2.214(3) Fe2 N33 2.192(3) Fe2 O35 2.107(3) N3A C4A 1.329(12) N3A C8A 1.333(15) C4A C5A 1.399(16) C4A N9A 1.396(14) C5A H5A 0.9300 C5A C6A 1.41(2) C6A H6A 0.9300 C6A C7A 1.342(19) C7A H7A 0.9300 C7A C8A 1.367(16) C8A N14 1.490(11) N9A N10A 1.411(13) N9A C13A 1.382(14) N10A C11A 1.293(15) C11A H11A 0.9300 C11A C12A 1.43(2) C12A H12A 0.9300 C12A C13A 1.38(2) C13A H13A 0.9300 N3B C4B 1.326(12) N3B C8B 1.309(15) C4B C5B 1.360(17) C4B N9B 1.430(13) C5B H5B 0.9300 C5B C6B 1.28(2) C6B H6B 0.9300 C6B C7B 1.354(18) C7B H7B 0.9300 C7B C8B 1.341(16) C8B N14 1.390(10) N9B N10B 1.374(13) N9B C13B 1.350(15) N10B C11B 1.330(14) C11B H11B 0.9300 C11B C12B 1.348(19) C12B H12B 0.9300 C12B C13B 1.38(2) C13B H13B 0.9300 N14 N15 1.355(5) N14 C18 1.323(6) N15 C16 1.307(5) C16 H16 0.9300 C16 N17 1.359(5) N17 C18 1.313(5) C18 H18 0.9300 N19 C20 1.328(5) N19 C24 1.315(6) C20 C21 1.386(8) C20 N25 1.391(7) C21 H21 0.9300 C21 C22 1.365(9) C22 H22 0.9300 C22 C23 1.401(8) C23 H23 0.9300 C23 C24 1.370(7) C24 N30 1.428(5) N25 N26 1.370(5) N25 C29 1.363(8) N26 C27 1.304(9) C27 H27 0.9300 C27 C28 1.409(9) C28 H28 0.9300 C28 C29 1.332(9) C29 H29 0.9300 N30 N31 1.360(6) N30 C34 1.323(6) N31 C32 1.298(6) C32 H32 0.9300 C32 N33 1.357(6) N33 C34 1.329(5) C34 H34 0.9300 O35 H35A 0.89(2) O35 H35B 0.89(2) B36 F37A 1.307(10) B36 F38A 1.430(11) B36 F39A 1.445(10) B36 F40A 1.367(10) B36 F37B 1.415(10) B36 F38B 1.452(13) B36 F39B 1.278(10) B36 F40B 1.375(12) B36 F37C 1.412(10) B36 F38C 1.306(11) B36 F39C 1.466(13) B36 F40C 1.335(12) B41 F42A 1.341(13) B41 F43A 1.447(12) B41 F44A 1.339(12) B41 F45A 1.413(13) B41 F42B 1.418(12) B41 F43B 1.292(12) B41 F44B 1.473(12) B41 F45B 1.352(10) B41 F42C 1.367(13) B41 F43C 1.460(12) B41 F44C 1.307(13) B41 F45C 1.398(13) C47A N48 1.444(15) C47A H47A 0.9600 C47A H47B 0.9600 C47A H47C 0.9600 N48 O49A 1.227(14) N48 O50A 1.227(16) C47B N48 1.459(19) C47B H47D 0.9600 C47B H47E 0.9600 C47B H47F 0.9600 N48 O49B 1.230(19) N48 O50B 1.232(18) loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA O35 H35A F45A 0.89(2) 2.16(5) 2.845(18) 134(5) O35 H35A F45B 0.89(2) 1.90(4) 2.680(11) 146(6) O35 H35A F44C 0.89(2) 1.80(3) 2.658(18) 163(7) O35 H35B F37A 0.89(2) 1.98(5) 2.710(10) 138(6) O35 H35B F37B 0.89(2) 1.93(4) 2.721(11) 147(6) O35 H35B F37C 0.89(2) 2.21(5) 2.911(10) 136(6)