#------------------------------------------------------------------------------ #$Date: 2019-11-07 21:35:52 +0200 (Thu, 07 Nov 2019) $ #$Revision: 223554 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/23/45/7234534.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_7234534 loop_ _publ_author_name 'Galadzhun, Iurii' 'Capel Berdiell, Izar' 'Shahid, Namrah' 'Halcrow, Malcolm A.' _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_issue 42 _journal_name_full CrystEngComm _journal_page_first 6330 _journal_paper_doi 10.1039/C9CE01496A _journal_volume 21 _journal_year 2019 _chemical_formula_moiety 'C40 H36 Fe2 N24 O2, 4(B F4), 1.34(H2 O), C H3 N O2' _chemical_formula_sum 'C41 H41.68 B4 F16 Fe2 N25 O5.34' _chemical_formula_weight 1429.05 _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 (2/1.34) 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 100.512(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 19.9235(5) _cell_length_b 15.5984(5) _cell_length_c 18.6533(4) _cell_measurement_reflns_used 8702 _cell_measurement_temperature 200(2) _cell_measurement_theta_max 73.57 _cell_measurement_theta_min 4.71 _cell_volume 5699.7(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 200(2) _diffrn_detector_area_resol_mean 5.3095 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.990 _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 0.0412 _diffrn_reflns_av_unetI/netI 0.0345 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 19798 _diffrn_reflns_theta_full 72.00 _diffrn_reflns_theta_max 73.72 _diffrn_reflns_theta_min 3.62 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 5.179 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.090 _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 1.665 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 2886 _exptl_crystal_size_max 0.90 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.28 _refine_diff_density_max 0.892 _refine_diff_density_min -0.730 _refine_diff_density_rms 0.099 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 447 _refine_ls_number_reflns 5714 _refine_ls_number_restraints 63 _refine_ls_restrained_S_all 1.063 _refine_ls_R_factor_all 0.0850 _refine_ls_R_factor_gt 0.0820 _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^)+(0.1611P)^2^+9.8584P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2271 _refine_ls_wR_factor_ref 0.2314 _reflns_number_gt 5316 _reflns_number_total 5714 _reflns_threshold_expression >2sigma(I) _cod_data_source_file c9ce01496a2.cif _cod_data_source_block ig12c4mt _cod_depositor_comments 'Adding full bibliography for 7234530--7234535.cif.' _cod_database_code 7234534 _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 1.38055 with sigma of 0.02 B36-F37B = B36-F38B = B36-F39B = B36-F40B 1.38055 with sigma of 0.02 B36-F37C = B36-F38C = B36-F39C = B36-F40C 1.38055 with sigma of 0.02 F37A-F38A = F37A-F39A = F37A-F40A = F38A-F39A = F38A-F40A = F39A-F40A 2.254438 with sigma of 0.02 F37B-F38B = F37B-F39B = F37B-F40B = F38B-F39B = F38B-F40B = F39B-F40B 2.254438 with sigma of 0.02 F37C-F38C = F37C-F39C = F37C-F40C = F38C-F39C = F38C-F40C = F39C-F40C 2.254438 with sigma of 0.02 B41-F42A = B41-F43A = B41-F44A = B41-F45A 1.38055 with sigma of 0.02 B41-F42B = B41-F43B = B41-F44B = B41-F45B 1.38055 with sigma of 0.02 B41-F42C = B41-F43C = B41-F44C = B41-F45C 1.38055 with sigma of 0.02 F42A-F43A = F42A-F44A = F42A-F45A = F43A-F44A = F43A-F45A = F44A-F45A 2.254438 with sigma of 0.02 F42B-F43B = F42B-F44B = F42B-F45B = F43B-F44B = F43B-F45B = F44B-F45B 2.254438 with sigma of 0.02 F42C-F43C = F42C-F44C = F42C-F45C = F43C-F44C = F43C-F45C = F44C-F45C 2.254438 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 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(0.6) C4A(0.6) C5A(0.6) H5A(0.6) C6A(0.6) H6A(0.6) C7A(0.6) H7A(0.6) C8A(0.6) N9A(0.6) N10A(0.6) C11A(0.6) H11A(0.6) C12A(0.6) H12A(0.6) C13A(0.6) H13A(0.6) N3B(0.4) C4B(0.4) C5B(0.4) H5B(0.4) C6B(0.4) H6B(0.4) C7B(0.4) H7B(0.4) C8B(0.4) N9B(0.4) N10B(0.4) C11B(0.4) H11B(0.4) C12B(0.4) H12B(0.4) C13B(0.4) H13B(0.4) 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(0.67) H47A(0.5) H47B(0.5) H47C(0.5) 4.a Me refined with riding coordinates: C47(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) ; _shelx_res_file ; TITL ig12c4+fe-meno2_a.res in C2/c CELL 1.54184 19.9235 15.5984 18.6533 90 100.512 90 ZERR 4 0.0005 0.0005 0.0004 0 0.002 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H B F Fe N O UNIT 164 166.72 16 64 8 100 21.36 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 L.S. 8 PLAN 20 TEMP -73 HTAB O35 F37A HTAB O35 F37B HTAB O35 F37C HTAB O35 F45A HTAB O35 F45B HTAB O35 F44C BOND $H REM Old TITL IG12C4+Fe-MeNO2 in C2/m REM SHELXT solution in C2/c REM R1 0.247, Rweak 0.205, Alpha 0.127, Orientation as input REM Formula found by SHELXT: C30 N8 O7 Br REM ig12c4+fe-meno2_a.res in C2/c REM 450 parameters refined using 0 restraints REM Highest difference peak 0.733, deepest hole -0.934, 1-sigma level 0.091 REM 289 parameters refined using 30 restraints REM Highest difference peak 1.949, deepest hole -0.929, 1-sigma level 0.184 REM 351 parameters refined using 63 restraints REM Highest difference peak 1.352, deepest hole -0.760, 1-sigma level 0.113 REM Highest difference peak 1.346, deepest hole -0.806, 1-sigma level 0.113 REM Highest difference peak 1.866, deepest hole -0.851, 1-sigma level 0.124 REM 458 parameters refined using 63 restraints REM Highest difference peak 1.807, deepest hole -0.495, 1-sigma level 0.101 REM Highest difference peak 1.238, deepest hole -0.554, 1-sigma level 0.081 REM Highest difference peak 0.762, deepest hole -0.587, 1-sigma level 0.076 REM 448 parameters refined using 63 restraints REM Highest difference peak 0.879, deepest hole -0.716, 1-sigma level 0.107 REM Highest difference peak 0.884, deepest hole -0.722, 1-sigma level 0.102 REM 464 parameters refined using 73 restraints REM Highest difference peak 0.886, deepest hole -0.721, 1-sigma level 0.097 REM Highest difference peak 0.898, deepest hole -0.723, 1-sigma level 0.097 REM Highest difference peak 0.897, deepest hole -0.722, 1-sigma level 0.097 REM Highest difference peak 0.893, deepest hole -0.715, 1-sigma level 0.098 REM Highest difference peak 0.909, deepest hole -0.723, 1-sigma level 0.100 GRID fmap 2 acta 144 MERG 2 REM C:/Users/chmmah/Desktop/200%20K/ig12c4mt.hkl WGHT 0.161100 9.858400 FVAR 2.48861 1.38055 FE1 5 0.500000 0.286640 0.250000 10.50000 0.04819 0.03985 = 0.03727 0.00000 0.01236 0.00000 FE2 5 0.500000 0.000000 0.500000 10.50000 0.03086 0.04816 = 0.03526 -0.00530 0.01206 0.00177 PART 1 N3A 6 0.594134 0.296941 0.283244 10.60000 0.03710 C4A 1 0.629292 0.355879 0.253952 10.60000 0.04092 C5A 1 0.698583 0.368684 0.278778 10.60000 0.05581 AFIX 43 H5A 2 0.723484 0.409947 0.256809 10.60000 -1.20000 AFIX 0 C6A 1 0.729791 0.319308 0.336420 10.60000 0.06035 AFIX 43 H6A 2 0.777350 0.325777 0.354060 10.60000 -1.20000 AFIX 0 C7A 1 0.692536 0.259444 0.369679 10.60000 0.05373 AFIX 43 H7A 2 0.713137 0.227354 0.411186 10.60000 -1.20000 AFIX 0 C8A 1 0.624942 0.249705 0.339178 10.60000 0.04093 N9A 6 0.588639 0.400307 0.198020 10.60000 0.04424 N10A 6 0.521047 0.376597 0.181415 10.60000 0.04585 C11A 1 0.494675 0.426771 0.128486 10.60000 0.05475 AFIX 43 H11A 2 0.447861 0.425531 0.106107 10.60000 -1.20000 AFIX 0 C12A 1 0.542349 0.483064 0.107658 10.60000 0.05994 AFIX 43 H12A 2 0.534399 0.524742 0.069923 10.60000 -1.20000 AFIX 0 C13A 1 0.604553 0.464938 0.154385 10.60000 0.05311 AFIX 43 H13A 2 0.647645 0.491449 0.155401 10.60000 -1.20000 AFIX 0 PART 0 PART 2 N3B 6 0.607066 0.285531 0.298386 10.40000 0.04192 C4B 1 0.648182 0.343324 0.273729 10.40000 0.04253 C5B 1 0.713799 0.354563 0.302419 10.40000 0.05805 AFIX 43 H5B 2 0.741008 0.397577 0.285731 10.40000 -1.20000 AFIX 0 C6B 1 0.739328 0.298749 0.358439 10.40000 0.07382 AFIX 43 H6B 2 0.786062 0.303160 0.380639 10.40000 -1.20000 AFIX 0 C7B 1 0.700408 0.238090 0.382911 10.40000 0.05907 AFIX 43 H7B 2 0.719114 0.198846 0.420186 10.40000 -1.20000 AFIX 0 C8B 1 0.634021 0.236140 0.351873 10.40000 0.04498 N9B 6 0.612441 0.393252 0.213886 10.40000 0.04902 N10B 6 0.546088 0.377265 0.189976 10.40000 0.04688 C11B 1 0.527660 0.432028 0.132972 10.40000 0.06798 AFIX 43 H11B 2 0.483361 0.434271 0.103701 10.40000 -1.20000 AFIX 0 C12B 1 0.576264 0.479010 0.123912 10.40000 0.06275 AFIX 43 H12B 2 0.573784 0.522406 0.087790 10.40000 -1.20000 AFIX 0 C13B 1 0.635277 0.458292 0.175035 10.40000 0.06760 AFIX 43 H13B 2 0.679522 0.483031 0.181044 10.40000 -1.20000 AFIX 0 PART 0 N14 6 0.580239 0.187943 0.365759 11.00000 0.03115 0.05309 = 0.05040 -0.00790 0.01341 -0.00421 N15 6 0.513270 0.194170 0.331897 11.00000 0.03610 0.05150 = 0.04342 -0.00629 0.01135 -0.00111 C16 1 0.482692 0.136374 0.365495 11.00000 0.03045 0.05480 = 0.04324 -0.00410 0.01429 -0.00447 AFIX 43 H16 2 0.435034 0.125480 0.353783 11.00000 -1.20000 AFIX 0 N17 6 0.525232 0.093558 0.418465 11.00000 0.03715 0.05456 = 0.04086 -0.00369 0.01405 -0.00060 C18 1 0.585540 0.127048 0.416687 11.00000 0.03344 0.05845 = 0.04326 -0.00297 0.00932 0.00023 AFIX 43 H18 2 0.626920 0.110256 0.447292 11.00000 -1.20000 AFIX 0 N19 6 0.249837 0.163140 0.551809 11.00000 0.03531 0.05282 = 0.04445 0.00624 0.01345 0.00824 C20 1 0.200591 0.206339 0.574673 11.00000 0.04249 0.05341 = 0.04973 0.01080 0.01816 0.00937 C21 1 0.132096 0.202968 0.540438 11.00000 0.03803 0.06774 = 0.06460 0.00812 0.01996 0.00923 AFIX 43 H21 2 0.098032 0.234756 0.558448 11.00000 -1.20000 AFIX 0 C22 1 0.116007 0.151964 0.479827 11.00000 0.03343 0.07687 = 0.07086 0.00338 0.01172 0.00033 AFIX 43 H22 2 0.069996 0.148435 0.455041 11.00000 -1.20000 AFIX 0 C23 1 0.166280 0.105376 0.454261 11.00000 0.03622 0.07081 = 0.06097 0.00145 0.01040 -0.00072 AFIX 43 H23 2 0.156175 0.069467 0.412549 11.00000 -1.20000 AFIX 0 C24 1 0.231779 0.114514 0.493222 11.00000 0.03353 0.05530 = 0.04997 0.00600 0.01392 0.00330 N25 6 0.222279 0.257020 0.636280 11.00000 0.04068 0.05813 = 0.05160 0.00495 0.01652 0.01307 N26 6 0.178240 0.309330 0.664014 11.00000 0.05247 0.06164 = 0.06024 0.00675 0.02284 0.02258 C27 1 0.216905 0.349480 0.718374 11.00000 0.07081 0.06543 = 0.05877 -0.00281 0.02082 0.02077 AFIX 43 H27 2 0.200200 0.390820 0.748149 11.00000 -1.20000 AFIX 0 C28 1 0.285328 0.324557 0.727472 11.00000 0.06478 0.07867 = 0.05741 -0.00727 0.00920 0.01654 AFIX 43 H28 2 0.322334 0.344622 0.763002 11.00000 -1.20000 AFIX 0 C29 1 0.287416 0.265229 0.674306 11.00000 0.04853 0.07141 = 0.05660 -0.00178 0.00995 0.01633 AFIX 43 H29 2 0.326611 0.235324 0.665387 11.00000 -1.20000 AFIX 0 N30 6 0.288136 0.071244 0.471949 11.00000 0.03310 0.05494 = 0.04367 -0.00061 0.00988 0.00166 N31 6 0.280809 0.014465 0.415649 11.00000 0.03843 0.06273 = 0.05128 -0.00831 0.00787 -0.00047 C32 1 0.343213 -0.009770 0.415008 11.00000 0.04123 0.05627 = 0.04350 -0.00663 0.00956 0.00253 AFIX 43 H32 2 0.354719 -0.049878 0.380879 11.00000 -1.20000 AFIX 0 N33 6 0.390805 0.027776 0.467991 11.00000 0.03367 0.05107 = 0.03924 -0.00092 0.01079 0.00189 C34 1 0.354039 0.078172 0.502266 11.00000 0.03738 0.05053 = 0.04051 -0.00037 0.01078 0.00308 AFIX 43 H34 2 0.371706 0.114023 0.542462 11.00000 -1.20000 AFIX 0 O35 7 0.507233 0.098376 0.578115 11.00000 0.04983 0.06479 = 0.05111 -0.01994 0.01983 -0.00869 H35A 2 0.535510 0.142203 0.584360 11.00000 -1.50000 H35B 2 0.493532 0.092381 0.620003 11.00000 -1.50000 B36 3 0.383042 0.050336 0.718617 11.00000 0.06427 0.07567 = 0.05505 0.01403 0.02914 0.01240 PART 1 F37A 4 0.415716 0.080638 0.668296 10.34000 0.05373 F38A 4 0.311332 0.039384 0.688264 10.34000 0.05470 F39A 4 0.380902 0.109901 0.777163 10.34000 0.05477 F40A 4 0.410133 -0.026792 0.742389 10.34000 0.05576 PART 0 PART 2 F37B 4 0.419346 0.107192 0.677773 10.33000 0.04819 F38B 4 0.335448 0.004196 0.660622 10.33000 0.13280 F39B 4 0.348201 0.086572 0.759543 10.33000 0.08751 F40B 4 0.427991 -0.009106 0.751244 10.33000 0.12363 PART 0 PART 3 F37C 4 0.402049 0.102877 0.665861 10.33000 0.05422 F38C 4 0.316211 0.051582 0.713622 10.33000 0.07343 F39C 4 0.409307 0.091326 0.787457 10.33000 0.08323 F40C 4 0.408373 -0.031945 0.719720 10.33000 0.06677 PART 0 B41 3 0.598737 0.293315 0.550383 11.00000 0.06985 0.06237 = 0.06033 -0.00124 0.00387 -0.00213 PART 1 F42A 4 0.614530 0.353273 0.502405 10.34000 0.14396 F43A 4 0.641145 0.221108 0.545508 10.34000 0.08088 F44A 4 0.606541 0.324717 0.618182 10.34000 0.13603 F45A 4 0.533512 0.263967 0.522045 10.34000 0.12367 PART 0 PART 2 F42B 4 0.546014 0.296681 0.489238 10.33000 0.09618 F43B 4 0.646954 0.345932 0.557480 10.33000 0.13718 F44B 4 0.553779 0.313361 0.605545 10.33000 0.10535 F45B 4 0.609134 0.207663 0.563996 10.33000 0.05685 PART 0 PART 3 F42C 4 0.561606 0.334286 0.495765 10.33000 0.10381 F43C 4 0.642134 0.354203 0.596559 10.33000 0.06080 F44C 4 0.569319 0.247518 0.596331 10.33000 0.15494 F45C 4 0.651456 0.247982 0.523127 10.33000 0.09830 PART 0 O46 7 0.264141 -0.064678 0.574647 10.67000 0.08364 0.09834 = 0.14597 0.02833 0.05452 0.00518 C47 1 0.500000 0.719826 0.250000 10.50000 0.12949 0.07739 = 0.13581 0.00000 0.04635 0.00000 AFIX 33 H47A 2 0.457774 0.740768 0.219702 10.50000 -1.50000 H47B 2 0.539313 0.740768 0.230291 10.50000 -1.50000 H47C 2 0.502914 0.740768 0.300006 10.50000 -1.50000 AFIX 0 N48 6 0.500000 0.627051 0.250000 10.50000 0.05840 0.08927 = 0.06303 0.00000 0.01222 0.00000 O49 7 0.451233 0.589539 0.215588 11.00000 0.08619 0.12033 = 0.10989 -0.02596 0.01098 -0.01085 HKLF 4 REM ig12c4+fe-meno2_a.res in C2/c REM R1 = 0.0820 for 5316 Fo > 4sig(Fo) and 0.0850 for all 5714 data REM 447 parameters refined using 63 restraints END WGHT 0.1611 9.8584 REM Highest difference peak 0.892, deepest hole -0.730, 1-sigma level 0.099 Q1 1 0.5470 0.0006 0.5011 11.00000 0.05 0.89 Q2 1 0.5479 0.2824 0.2487 11.00000 0.05 0.88 Q3 1 0.5410 0.2747 0.5813 11.00000 0.05 0.75 Q4 1 0.6499 0.2990 0.5019 11.00000 0.05 0.74 Q5 1 0.6028 0.2177 0.5985 11.00000 0.05 0.67 Q6 1 0.4439 0.0354 0.7880 11.00000 0.05 0.59 Q7 1 0.5861 0.3175 0.4769 11.00000 0.05 0.52 Q8 1 0.3971 0.1424 0.7811 11.00000 0.05 0.48 Q9 1 0.5365 0.3266 0.5263 11.00000 0.05 0.45 Q10 1 0.6281 0.3785 0.5742 11.00000 0.05 0.45 Q11 1 0.4545 0.0783 0.6925 11.00000 0.05 0.45 Q12 1 0.3324 0.0573 0.7426 11.00000 0.05 0.42 Q13 1 0.5286 0.2699 0.4922 11.00000 0.05 0.41 Q14 1 0.6895 0.2687 0.4032 11.00000 0.05 0.39 Q15 1 0.6612 0.3289 0.6041 11.00000 0.05 0.39 Q16 1 0.6711 0.4493 0.1870 11.00000 0.05 0.38 Q17 1 0.7273 0.3321 0.3708 11.00000 0.05 0.38 Q18 1 0.3783 -0.0306 0.6910 11.00000 0.05 0.37 Q19 1 0.6129 0.3775 0.5220 11.00000 0.05 0.37 Q20 1 0.5598 0.4374 0.1540 11.00000 0.05 0.35 REM The information below was added by Olex2. REM REM R1 = 0.0820 for 5316 Fo > 4sig(Fo) and 0.0850 for all 20260 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.89, deepest hole -0.73 REM Mean Shift 0, Max Shift 0. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0850 REM R1_gt = 0.0820 REM wR_ref = 0.2314 REM GOOF = 1.029 REM Shift_max = 0 REM Shift_mean = 0 REM Reflections_all = 20260 REM Reflections_gt = 5316 REM Parameters = n/a REM Hole = 0.89 REM Peak = -0.73 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 0.28664(5) 0.2500 0.0412(3) Uani 1 2 d S . . Fe2 Fe 0.5000 0.0000 0.5000 0.0373(2) Uani 1 2 d S . . N3A N 0.5941(3) 0.2969(4) 0.2832(4) 0.0371(17) Uiso 0.60 1 d P A 1 C4A C 0.6293(4) 0.3559(5) 0.2540(4) 0.0409(15) Uiso 0.60 1 d P A 1 C5A C 0.6986(5) 0.3687(6) 0.2788(6) 0.056(2) Uiso 0.60 1 d P A 1 H5A H 0.7235 0.4099 0.2568 0.067 Uiso 0.60 1 calc PR A 1 C6A C 0.7298(5) 0.3193(7) 0.3364(7) 0.060(2) Uiso 0.60 1 d P A 1 H6A H 0.7773 0.3258 0.3541 0.072 Uiso 0.60 1 calc PR A 1 C7A C 0.6925(5) 0.2594(7) 0.3697(5) 0.054(2) Uiso 0.60 1 d P A 1 H7A H 0.7131 0.2274 0.4112 0.064 Uiso 0.60 1 calc PR A 1 C8A C 0.6249(4) 0.2497(6) 0.3392(5) 0.041(2) Uiso 0.60 1 d P A 1 N9A N 0.5886(4) 0.4003(4) 0.1980(3) 0.0442(14) Uiso 0.60 1 d P A 1 N10A N 0.5210(4) 0.3766(4) 0.1814(3) 0.0459(15) Uiso 0.60 1 d P A 1 C11A C 0.4947(5) 0.4268(5) 0.1285(4) 0.0547(16) Uiso 0.60 1 d P A 1 H11A H 0.4479 0.4255 0.1061 0.066 Uiso 0.60 1 calc PR A 1 C12A C 0.5423(5) 0.4831(6) 0.1077(5) 0.0599(18) Uiso 0.60 1 d P A 1 H12A H 0.5344 0.5247 0.0699 0.072 Uiso 0.60 1 calc PR A 1 C13A C 0.6046(5) 0.4649(5) 0.1544(5) 0.0531(16) Uiso 0.60 1 d P A 1 H13A H 0.6476 0.4914 0.1554 0.064 Uiso 0.60 1 calc PR A 1 N3B N 0.6071(6) 0.2855(7) 0.2984(7) 0.042(3) Uiso 0.40 1 d P A 2 C4B C 0.6482(6) 0.3433(7) 0.2737(6) 0.043(2) Uiso 0.40 1 d P A 2 C5B C 0.7138(8) 0.3546(10) 0.3024(10) 0.058(3) Uiso 0.40 1 d P A 2 H5B H 0.7410 0.3976 0.2857 0.070 Uiso 0.40 1 calc PR A 2 C6B C 0.7393(9) 0.2987(11) 0.3584(11) 0.074(5) Uiso 0.40 1 d P A 2 H6B H 0.7861 0.3032 0.3806 0.089 Uiso 0.40 1 calc PR A 2 C7B C 0.7004(8) 0.2381(11) 0.3829(9) 0.059(4) Uiso 0.40 1 d P A 2 H7B H 0.7191 0.1988 0.4202 0.071 Uiso 0.40 1 calc PR A 2 C8B C 0.6340(7) 0.2361(9) 0.3519(8) 0.045(4) Uiso 0.40 1 d P A 2 N9B N 0.6124(6) 0.3933(7) 0.2139(6) 0.049(2) Uiso 0.40 1 d P A 2 N10B N 0.5461(7) 0.3773(6) 0.1900(5) 0.047(2) Uiso 0.40 1 d P A 2 C11B C 0.5277(9) 0.4320(10) 0.1330(8) 0.068(3) Uiso 0.40 1 d P A 2 H11B H 0.4834 0.4343 0.1037 0.082 Uiso 0.40 1 calc PR A 2 C12B C 0.5763(9) 0.4790(9) 0.1239(9) 0.063(3) Uiso 0.40 1 d P A 2 H12B H 0.5738 0.5224 0.0878 0.075 Uiso 0.40 1 calc PR A 2 C13B C 0.6353(9) 0.4583(9) 0.1750(8) 0.068(3) Uiso 0.40 1 d P A 2 H13B H 0.6795 0.4830 0.1810 0.081 Uiso 0.40 1 calc PR A 2 N14 N 0.58024(15) 0.1879(2) 0.36576(18) 0.0441(7) Uani 1 1 d . . . N15 N 0.51327(15) 0.1942(2) 0.33190(17) 0.0432(7) Uani 1 1 d . A . C16 C 0.48269(18) 0.1364(3) 0.3655(2) 0.0419(8) Uani 1 1 d . . . H16 H 0.4350 0.1255 0.3538 0.050 Uiso 1 1 calc R A . N17 N 0.52523(16) 0.0936(2) 0.41846(17) 0.0433(7) Uani 1 1 d . A . C18 C 0.58554(18) 0.1270(3) 0.4167(2) 0.0448(8) Uani 1 1 d . A . H18 H 0.6269 0.1103 0.4473 0.054 Uiso 1 1 calc R . . N19 N 0.24984(15) 0.1631(2) 0.55181(17) 0.0434(7) Uani 1 1 d . . . C20 C 0.2006(2) 0.2063(3) 0.5747(2) 0.0473(8) Uani 1 1 d . . . C21 C 0.1321(2) 0.2030(3) 0.5404(3) 0.0555(10) Uani 1 1 d . . . H21 H 0.0980 0.2348 0.5584 0.067 Uiso 1 1 calc R . . C22 C 0.1160(2) 0.1520(3) 0.4798(3) 0.0601(11) Uani 1 1 d . . . H22 H 0.0700 0.1484 0.4550 0.072 Uiso 1 1 calc R . . C23 C 0.1663(2) 0.1054(3) 0.4543(3) 0.0558(10) Uani 1 1 d . . . H23 H 0.1562 0.0695 0.4125 0.067 Uiso 1 1 calc R . . C24 C 0.23178(18) 0.1145(3) 0.4932(2) 0.0455(8) Uani 1 1 d . . . N25 N 0.22228(16) 0.2570(2) 0.63628(19) 0.0491(8) Uani 1 1 d . . . N26 N 0.17824(19) 0.3093(3) 0.6640(2) 0.0565(9) Uani 1 1 d . . . C27 C 0.2169(3) 0.3495(3) 0.7184(3) 0.0639(12) Uani 1 1 d . . . H27 H 0.2002 0.3908 0.7481 0.077 Uiso 1 1 calc R . . C28 C 0.2853(3) 0.3246(4) 0.7275(3) 0.0672(12) Uani 1 1 d . . . H28 H 0.3223 0.3446 0.7630 0.081 Uiso 1 1 calc R . . C29 C 0.2874(2) 0.2652(3) 0.6743(3) 0.0588(11) Uani 1 1 d . . . H29 H 0.3266 0.2353 0.6654 0.071 Uiso 1 1 calc R . . N30 N 0.28814(15) 0.0712(2) 0.47195(17) 0.0435(7) Uani 1 1 d . . . N31 N 0.28081(18) 0.0145(2) 0.4156(2) 0.0509(8) Uani 1 1 d . . . C32 C 0.3432(2) -0.0098(3) 0.4150(2) 0.0468(8) Uani 1 1 d . . . H32 H 0.3547 -0.0499 0.3809 0.056 Uiso 1 1 calc R . . N33 N 0.39080(15) 0.0278(2) 0.46799(16) 0.0408(6) Uani 1 1 d . . . C34 C 0.35404(18) 0.0782(2) 0.5023(2) 0.0423(8) Uani 1 1 d . . . H34 H 0.3717 0.1140 0.5425 0.051 Uiso 1 1 calc R . . O35 O 0.50723(16) 0.0984(2) 0.57812(16) 0.0539(7) Uani 1 1 d D . . H35A H 0.536(3) 0.142(3) 0.584(3) 0.081 Uiso 1 1 d D . . H35B H 0.494(3) 0.092(4) 0.6200(19) 0.081 Uiso 1 1 d D . . B36 B 0.3830(3) 0.0503(4) 0.7186(3) 0.0627(13) Uani 1 1 d D . . F37A F 0.4157(5) 0.0806(6) 0.6683(5) 0.054(2) Uiso 0.34 1 d PD B 1 F38A F 0.3113(4) 0.0394(5) 0.6883(5) 0.055(2) Uiso 0.34 1 d PD B 1 F39A F 0.3809(5) 0.1099(5) 0.7772(4) 0.0548(17) Uiso 0.34 1 d PD B 1 F40A F 0.4101(6) -0.0268(6) 0.7424(7) 0.056(2) Uiso 0.34 1 d PD B 1 F37B F 0.4193(5) 0.1072(7) 0.6778(5) 0.048(2) Uiso 0.33 1 d PD B 2 F38B F 0.3354(8) 0.0042(10) 0.6606(8) 0.133(6) Uiso 0.33 1 d PD B 2 F39B F 0.3482(6) 0.0866(7) 0.7595(6) 0.088(3) Uiso 0.33 1 d PD B 2 F40B F 0.4280(8) -0.0091(10) 0.7512(10) 0.124(7) Uiso 0.33 1 d PD B 2 F37C F 0.4020(6) 0.1029(8) 0.6659(6) 0.054(3) Uiso 0.33 1 d PD B 3 F38C F 0.3162(5) 0.0516(7) 0.7136(7) 0.073(3) Uiso 0.33 1 d PD B 3 F39C F 0.4093(6) 0.0913(7) 0.7875(5) 0.083(3) Uiso 0.33 1 d PD B 3 F40C F 0.4084(6) -0.0319(6) 0.7197(7) 0.067(3) Uiso 0.33 1 d PD B 3 B41 B 0.5987(3) 0.2933(3) 0.5504(3) 0.0652(13) Uani 1 1 d D . . F42A F 0.6145(10) 0.3533(10) 0.5024(9) 0.144(6) Uiso 0.34 1 d PD C 1 F43A F 0.6411(6) 0.2211(7) 0.5455(7) 0.081(3) Uiso 0.34 1 d PD C 1 F44A F 0.6065(9) 0.3247(11) 0.6182(7) 0.136(5) Uiso 0.34 1 d PD C 1 F45A F 0.5335(6) 0.2640(10) 0.5220(9) 0.124(5) Uiso 0.34 1 d PD C 1 F42B F 0.5460(6) 0.2967(10) 0.4892(6) 0.096(4) Uiso 0.33 1 d PD C 2 F43B F 0.6470(7) 0.3459(10) 0.5575(11) 0.137(6) Uiso 0.33 1 d PD C 2 F44B F 0.5538(7) 0.3134(9) 0.6055(7) 0.105(4) Uiso 0.33 1 d PD C 2 F45B F 0.6091(4) 0.2077(4) 0.5640(4) 0.0569(17) Uiso 0.33 1 d PD C 2 F42C F 0.5616(7) 0.3343(10) 0.4958(7) 0.104(4) Uiso 0.33 1 d PD C 3 F43C F 0.6421(4) 0.3542(5) 0.5966(5) 0.0608(18) Uiso 0.33 1 d PD C 3 F44C F 0.5693(9) 0.2475(12) 0.5963(9) 0.155(7) Uiso 0.33 1 d PD C 3 F45C F 0.6515(6) 0.2480(9) 0.5231(7) 0.098(4) Uiso 0.33 1 d PD C 3 O46 O 0.2641(4) -0.0647(5) 0.5746(5) 0.105(2) Uani 0.67 1 d P . . C47 C 0.5000 0.7198(7) 0.2500 0.111(4) Uani 1 2 d S . . H47A H 0.4578 0.7408 0.2197 0.167 Uiso 0.50 1 calc PR . . H47B H 0.5393 0.7408 0.2303 0.167 Uiso 0.50 1 calc PR . . H47C H 0.5029 0.7408 0.3000 0.167 Uiso 0.50 1 calc PR . . N48 N 0.5000 0.6271(5) 0.2500 0.0701(15) Uani 1 2 d S . . O49 O 0.4512(3) 0.5895(4) 0.2156(3) 0.1063(16) 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 0.0482(5) 0.0399(4) 0.0373(4) 0.000 0.0124(3) 0.000 Fe2 0.0309(4) 0.0482(5) 0.0353(4) -0.0053(3) 0.0121(3) 0.0018(3) N14 0.0312(14) 0.0531(17) 0.0504(17) -0.0079(14) 0.0134(12) -0.0042(12) N15 0.0361(15) 0.0515(17) 0.0434(15) -0.0063(13) 0.0113(12) -0.0011(13) C16 0.0305(15) 0.055(2) 0.0432(17) -0.0041(15) 0.0143(13) -0.0045(14) N17 0.0372(15) 0.0546(17) 0.0409(15) -0.0037(13) 0.0141(12) -0.0006(13) C18 0.0334(16) 0.058(2) 0.0433(18) -0.0030(15) 0.0093(14) 0.0002(15) N19 0.0353(15) 0.0528(17) 0.0444(16) 0.0062(13) 0.0134(12) 0.0082(12) C20 0.0425(19) 0.053(2) 0.050(2) 0.0108(16) 0.0182(16) 0.0094(16) C21 0.0380(19) 0.068(3) 0.065(3) 0.008(2) 0.0200(18) 0.0092(18) C22 0.0334(18) 0.077(3) 0.071(3) 0.003(2) 0.0117(18) 0.0003(18) C23 0.0362(19) 0.071(3) 0.061(2) 0.001(2) 0.0104(17) -0.0007(18) C24 0.0335(17) 0.055(2) 0.050(2) 0.0060(16) 0.0139(15) 0.0033(15) N25 0.0407(16) 0.0581(19) 0.0516(17) 0.0049(15) 0.0165(13) 0.0131(14) N26 0.0525(19) 0.062(2) 0.060(2) 0.0067(17) 0.0228(16) 0.0226(17) C27 0.071(3) 0.065(3) 0.059(3) -0.003(2) 0.021(2) 0.021(2) C28 0.065(3) 0.079(3) 0.057(2) -0.007(2) 0.009(2) 0.017(2) C29 0.049(2) 0.071(3) 0.057(2) -0.002(2) 0.0100(18) 0.016(2) N30 0.0331(14) 0.0549(17) 0.0437(15) -0.0006(13) 0.0099(12) 0.0017(13) N31 0.0384(17) 0.063(2) 0.0513(19) -0.0083(15) 0.0079(14) -0.0005(14) C32 0.0412(19) 0.056(2) 0.0435(19) -0.0066(15) 0.0096(15) 0.0025(15) N33 0.0337(14) 0.0511(16) 0.0392(14) -0.0009(12) 0.0108(11) 0.0019(12) C34 0.0374(17) 0.0505(19) 0.0405(17) -0.0004(14) 0.0108(14) 0.0031(14) O35 0.0498(15) 0.0648(18) 0.0511(15) -0.0199(13) 0.0198(12) -0.0087(13) B36 0.064(3) 0.076(3) 0.055(3) 0.014(2) 0.029(2) 0.012(3) B41 0.070(3) 0.062(3) 0.060(3) -0.001(2) 0.004(3) -0.002(3) O46 0.084(4) 0.098(5) 0.146(7) 0.028(5) 0.055(5) 0.005(4) C47 0.129(10) 0.077(6) 0.136(10) 0.000 0.046(8) 0.000 N48 0.058(3) 0.089(4) 0.063(3) 0.000 0.012(3) 0.000 O49 0.086(3) 0.120(4) 0.110(4) -0.026(3) 0.011(3) -0.011(3) 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 170.2(4) . 2_655 N3A Fe1 N3B 173.2(3) . 2_655 N3A Fe1 N10A 92.4(3) . 2_655 N3A Fe1 N10A 80.6(3) . . N3A Fe1 N15 80.3(2) . . N3A Fe1 N15 106.7(2) . 2_655 N10A Fe1 N10A 90.6(4) . 2_655 N10A Fe1 N10B 91.8(3) 2_655 . N10A Fe1 N15 160.8(2) . . N10A Fe1 N15 91.7(2) . 2_655 N3B Fe1 N3B 179.1(6) . 2_655 N10A Fe1 N3B 88.1(4) . . N10A Fe1 N3B 92.6(3) 2_655 . N10B Fe1 N3B 74.7(5) . . N10B Fe1 N3B 106.0(4) . 2_655 N10B Fe1 N10B 96.1(5) . 2_655 N15 Fe1 N3B 106.5(3) . 2_655 N15 Fe1 N3B 72.8(3) . . N15 Fe1 N10B 147.4(4) . . N15 Fe1 N10B 94.8(3) . 2_655 N15 Fe1 N15 92.32(17) 2_655 . N17 Fe2 N17 180.00 5_656 . N33 Fe2 N17 88.80(12) . 5_656 N33 Fe2 N17 91.20(11) . . N33 Fe2 N33 180.00 5_656 . O35 Fe2 N17 89.97(12) . . O35 Fe2 N17 90.03(12) . 5_656 O35 Fe2 N33 90.94(12) . 5_656 O35 Fe2 N33 89.06(12) . . O35 Fe2 O35 180.00 . 5_656 C4A N3A Fe1 119.6(6) . . C4A N3A C8A 120.1(7) . . C8A N3A Fe1 120.2(5) . . N3A C4A C5A 121.9(9) . . N3A C4A N9A 112.1(7) . . N9A C4A C5A 126.1(8) . . C4A C5A H5A 121.3 . . C6A C5A C4A 117.4(8) . . C6A C5A H5A 121.3 . . C5A C6A H6A 119.4 . . C5A C6A C7A 121.1(9) . . C7A C6A H6A 119.4 . . C6A C7A H7A 121.7 . . C8A C7A C6A 116.6(10) . . C8A C7A H7A 121.7 . . N3A C8A C7A 122.7(9) . . N3A C8A N14 114.1(7) . . C7A C8A N14 123.1(9) . . N10A N9A C4A 116.7(6) . . C13A N9A C4A 130.5(8) . . C13A N9A N10A 112.8(7) . . N9A N10A Fe1 110.9(5) . . C11A N10A Fe1 144.2(7) . . C11A N10A N9A 104.7(7) . . N10A C11A H11A 123.5 . . N10A C11A C12A 112.9(9) . . C12A C11A H11A 123.5 . . C11A C12A H12A 127.2 . . C11A C12A C13A 105.5(8) . . C13A C12A H12A 127.2 . . N9A C13A C12A 104.1(8) . . N9A C13A H13A 128.0 . . C12A C13A H13A 128.0 . . C4B N3B Fe1 117.7(10) . . C8B N3B Fe1 124.4(9) . . C8B N3B C4B 117.8(12) . . N3B C4B N9B 112.3(11) . . C5B C4B N3B 124.2(14) . . C5B C4B N9B 123.5(12) . . C4B C5B H5B 122.6 . . C4B C5B C6B 114.8(14) . . C6B C5B H5B 122.6 . . C5B C6B H6B 118.7 . . C7B C6B C5B 122.7(16) . . C7B C6B H6B 118.7 . . C6B C7B H7B 121.6 . . C8B C7B C6B 116.7(17) . . C8B C7B H7B 121.6 . . N3B C8B C7B 123.7(13) . . N3B C8B N14 104.0(11) . . C7B C8B N14 132.2(14) . . N10B N9B C4B 118.5(10) . . N10B N9B C13B 111.4(13) . . C13B N9B C4B 130.2(12) . . N9B N10B Fe1 116.5(7) . . N9B N10B C11B 104.6(12) . . C11B N10B Fe1 138.8(11) . . N10B C11B H11B 124.2 . . C12B C11B N10B 111.6(16) . . C12B C11B H11B 124.2 . . C11B C12B H12B 124.9 . . C11B C12B C13B 110.2(16) . . C13B C12B H12B 124.9 . . N9B C13B C12B 102.2(13) . . N9B C13B H13B 128.9 . . C12B C13B H13B 128.9 . . N15 N14 C8A 113.6(5) . . N15 N14 C8B 127.0(7) . . C18 N14 C8A 137.6(5) . . C18 N14 C8B 124.2(7) . . C18 N14 N15 108.8(3) . . N14 N15 Fe1 111.7(2) . . C16 N15 Fe1 145.1(3) . . C16 N15 N14 103.3(3) . . N15 C16 H16 123.1 . . N15 C16 N17 113.9(3) . . N17 C16 H16 123.1 . . C16 N17 Fe2 129.1(2) . . C18 N17 Fe2 126.7(3) . . C18 N17 C16 103.8(3) . . N14 C18 H18 124.9 . . N17 C18 N14 110.3(3) . . N17 C18 H18 124.9 . . C20 N19 C24 116.8(3) . . N19 C20 C21 123.6(4) . . N19 C20 N25 114.6(4) . . N25 C20 C21 121.8(4) . . C20 C21 H21 121.3 . . C22 C21 C20 117.4(4) . . C22 C21 H21 121.3 . . C21 C22 H22 119.6 . . C21 C22 C23 120.7(4) . . C23 C22 H22 119.6 . . C22 C23 H23 122.1 . . C24 C23 C22 115.9(4) . . C24 C23 H23 122.1 . . N19 C24 C23 125.6(4) . . N19 C24 N30 113.0(3) . . C23 C24 N30 121.4(4) . . N26 N25 C20 121.7(3) . . C29 N25 C20 127.0(3) . . C29 N25 N26 111.2(4) . . C27 N26 N25 104.5(4) . . N26 C27 H27 123.8 . . N26 C27 C28 112.5(4) . . C28 C27 H27 123.8 . . C27 C28 H28 127.5 . . C29 C28 C27 105.0(5) . . C29 C28 H28 127.5 . . N25 C29 H29 126.6 . . C28 C29 N25 106.8(4) . . C28 C29 H29 126.6 . . N31 N30 C24 122.9(3) . . C34 N30 C24 127.3(3) . . C34 N30 N31 109.8(3) . . C32 N31 N30 103.2(3) . . N31 C32 H32 123.0 . . N31 C32 N33 113.9(4) . . N33 C32 H32 123.0 . . C32 N33 Fe2 129.3(3) . . C34 N33 Fe2 126.7(3) . . C34 N33 C32 103.4(3) . . N30 C34 H34 125.2 . . N33 C34 N30 109.7(3) . . N33 C34 H34 125.2 . . Fe2 O35 H35A 128(4) . . Fe2 O35 H35B 123(4) . . H35A O35 H35B 105(3) . . F37A B36 F38A 110.0(7) . . F37A B36 F39A 113.2(7) . . F37A B36 F40A 109.3(7) . . F39A B36 F38A 102.1(6) . . F40A B36 F38A 109.1(7) . . F40A B36 F39A 112.9(7) . . F37B B36 F38B 103.1(8) . . F39B B36 F37B 115.4(8) . . F39B B36 F38B 108.1(9) . . F39B B36 F40B 115.4(10) . . F40B B36 F37B 107.7(9) . . F40B B36 F38B 106.1(10) . . F37C B36 F39C 105.5(8) . . F38C B36 F37C 110.2(7) . . F38C B36 F39C 104.7(7) . . F38C B36 F40C 112.2(8) . . F40C B36 F37C 114.5(8) . . F40C B36 F39C 109.1(7) . . F42A B41 F43A 106.8(9) . . F42A B41 F45A 106.7(10) . . F44A B41 F42A 111.5(10) . . F44A B41 F43A 112.5(9) . . F44A B41 F45A 114.8(10) . . F45A B41 F43A 103.9(8) . . F42B B41 F44B 95.5(8) . . F43B B41 F42B 120.5(11) . . F43B B41 F44B 109.3(10) . . F43B B41 F45B 122.2(9) . . F45B B41 F42B 104.6(8) . . F45B B41 F44B 99.4(7) . . F42C B41 F43C 109.4(8) . . F42C B41 F44C 120.6(11) . . F42C B41 F45C 108.1(9) . . F44C B41 F43C 104.6(9) . . F44C B41 F45C 113.6(10) . . F45C B41 F43C 97.9(7) . . H47A C47 H47B 109.5 . . H47A C47 H47C 109.5 . . H47B C47 H47C 109.5 . . N48 C47 H47A 109.5 . . N48 C47 H47B 109.5 . . N48 C47 H47C 109.5 . . O49 N48 C47 118.8(4) . . O49 N48 O49 122.3(9) . 2_655 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Fe1 N3A 1.872(7) Fe1 N10A 1.994(6) Fe1 N3B 2.159(12) Fe1 N10B 2.114(11) Fe1 N15 2.082(3) Fe2 N17 2.230(3) Fe2 N33 2.192(3) Fe2 O35 2.103(3) N3A C4A 1.332(9) N3A C8A 1.332(12) C4A C5A 1.388(12) C4A N9A 1.384(10) C5A H5A 0.9500 C5A C6A 1.375(14) C6A H6A 0.9500 C6A C7A 1.406(15) C7A H7A 0.9500 C7A C8A 1.371(13) C8A N14 1.459(9) N9A N10A 1.376(9) N9A C13A 1.369(10) N10A C11A 1.294(11) C11A H11A 0.9500 C11A C12A 1.400(13) C12A H12A 0.9500 C12A C13A 1.408(12) C13A H13A 0.9500 N3B C4B 1.354(15) N3B C8B 1.297(18) C4B C5B 1.331(19) C4B N9B 1.439(15) C5B H5B 0.9500 C5B C6B 1.38(2) C6B H6B 0.9500 C6B C7B 1.35(2) C7B H7B 0.9500 C7B C8B 1.34(2) C8B N14 1.372(13) N9B N10B 1.339(16) N9B C13B 1.372(18) N10B C11B 1.361(18) C11B H11B 0.9500 C11B C12B 1.25(2) C12B H12B 0.9500 C12B C13B 1.41(2) C13B H13B 0.9500 N14 N15 1.372(4) N14 C18 1.334(5) N15 C16 1.310(5) C16 H16 0.9500 C16 N17 1.355(5) N17 C18 1.316(5) C18 H18 0.9500 N19 C20 1.323(5) N19 C24 1.325(5) C20 C21 1.398(6) C20 N25 1.397(6) C21 H21 0.9500 C21 C22 1.372(7) C22 H22 0.9500 C22 C23 1.390(7) C23 H23 0.9500 C23 C24 1.380(6) C24 N30 1.427(5) N25 N26 1.367(5) N25 C29 1.367(6) N26 C27 1.315(7) C27 H27 0.9500 C27 C28 1.398(7) C28 H28 0.9500 C28 C29 1.363(7) C29 H29 0.9500 N30 N31 1.361(5) N30 C34 1.336(5) N31 C32 1.302(5) C32 H32 0.9500 C32 N33 1.370(5) N33 C34 1.317(5) C34 H34 0.9500 O35 H35A 0.88(2) O35 H35B 0.88(2) B36 F37A 1.323(9) B36 F38A 1.448(9) B36 F39A 1.440(9) B36 F40A 1.359(9) B36 F37B 1.446(9) B36 F38B 1.488(12) B36 F39B 1.256(10) B36 F40B 1.354(12) B36 F37C 1.385(10) B36 F38C 1.318(10) B36 F39C 1.444(10) B36 F40C 1.378(10) B41 F42A 1.370(13) B41 F43A 1.421(10) B41 F44A 1.339(12) B41 F45A 1.388(12) B41 F42B 1.404(11) B41 F43B 1.252(12) B41 F44B 1.515(11) B41 F45B 1.369(9) B41 F42C 1.311(11) B41 F43C 1.456(9) B41 F44C 1.331(12) B41 F45C 1.434(11) C47 H47A 0.9800 C47 H47B 0.9800 C47 H47C 0.9800 C47 N48 1.447(12) N48 O49 1.213(6) 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 0.88(2) 2.22(5) 2.870(17) 130(5) O35 H35A F45B 0.88(2) 1.88(3) 2.700(9) 154(5) O35 H35A F44C 0.88(2) 1.77(3) 2.628(17) 163(6) O35 H35B F37A 0.88(2) 1.94(4) 2.711(8) 146(5) O35 H35B F37B 0.88(2) 2.00(4) 2.780(9) 148(6) O35 H35B F37C 0.88(2) 2.16(4) 2.886(10) 140(5)