#------------------------------------------------------------------------------ #$Date: 2019-10-11 03:39:57 +0300 (Fri, 11 Oct 2019) $ #$Revision: 219265 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/23/45/7234533.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_7234533 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), H2 O, C H3 N O2' _chemical_formula_sum 'C41 H41 B4 F16 Fe2 N25 O5' _chemical_formula_weight 1422.93 _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) 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 99.528(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 19.9189(6) _cell_length_b 15.8603(5) _cell_length_c 18.7484(4) _cell_measurement_reflns_used 4863 _cell_measurement_temperature 250(2) _cell_measurement_theta_max 72.85 _cell_measurement_theta_min 4.72 _cell_volume 5841.3(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 250(2) _diffrn_detector_area_resol_mean 5.3095 _diffrn_measured_fraction_theta_full 0.984 _diffrn_measured_fraction_theta_max 0.970 _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 0.0521 _diffrn_reflns_av_unetI/netI 0.0651 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 11206 _diffrn_reflns_theta_full 72.00 _diffrn_reflns_theta_max 73.60 _diffrn_reflns_theta_min 4.10 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 5.046 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.075 _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 1.618 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 2872 _exptl_crystal_size_max 0.90 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.28 _refine_diff_density_max 0.471 _refine_diff_density_min -0.394 _refine_diff_density_rms 0.074 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 452 _refine_ls_number_reflns 5722 _refine_ls_number_restraints 75 _refine_ls_restrained_S_all 1.060 _refine_ls_R_factor_all 0.1236 _refine_ls_R_factor_gt 0.0848 _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^)+(0.1168P)^2^+20.4895P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2212 _refine_ls_wR_factor_ref 0.2496 _reflns_number_gt 3749 _reflns_number_total 5722 _reflns_threshold_expression >2sigma(I) _cod_data_source_file c9ce01496a2.cif _cod_data_source_block ig12c4ht _cod_database_code 7234533 _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 1.38428 with sigma of 0.02 B36-F37B = B36-F38B = B36-F39B = B36-F40B 1.38428 with sigma of 0.02 B36-F37C = B36-F38C = B36-F39C = B36-F40C 1.38428 with sigma of 0.02 F37A-F38A = F37A-F39A = F37A-F40A = F38A-F39A = F38A-F40A = F39A-F40A 2.260529 with sigma of 0.02 F37B-F38B = F37B-F39B = F37B-F40B = F38B-F39B = F38B-F40B = F39B-F40B 2.260529 with sigma of 0.02 F37C-F38C = F37C-F39C = F37C-F40C = F38C-F39C = F38C-F40C = F39C-F40C 2.260529 with sigma of 0.02 B41-F42A = B41-F43A = B41-F44A = B41-F45A 1.38428 with sigma of 0.02 B41-F42B = B41-F43B = B41-F44B = B41-F45B 1.38428 with sigma of 0.02 B41-F42C = B41-F43C = B41-F44C = B41-F45C 1.38428 with sigma of 0.02 F42A-F43A = F42A-F44A = F42A-F45A = F43A-F44A = F43A-F45A = F44A-F45A 2.260529 with sigma of 0.02 F42B-F43B = F42B-F44B = F42B-F45B = F43B-F44B = F43B-F45B = F44B-F45B 2.260529 with sigma of 0.02 F42C-F43C = F42C-F44C = F42C-F45C = F43C-F44C = F43C-F45C = F44C-F45C 2.260529 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(0.55) C4A(0.55) C5A(0.55) H5A(0.55) C6A(0.55) H6A(0.55) C7A(0.55) H7A(0.55) C8A(0.55) N9A(0.55) N10A(0.55) C11A(0.55) H11A(0.55) C12A(0.55) H12A(0.55) C13A(0.55) H13A(0.55) N3B(0.45) C4B(0.45) C5B(0.45) H5B(0.45) C6B(0.45) H6B(0.45) C7B(0.45) H7B(0.45) C8B(0.45) N9B(0.45) N10B(0.45) C11B(0.45) H11B(0.45) C12B(0.45) H12B(0.45) C13B(0.45) H13B(0.45) 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(0.5) 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), C47B(H47D,H47E,H47F) 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 19.9189 15.8603 18.7484 90 99.528 90 ZERR 4 0.0006 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 164 164 16 64 8 100 20 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 -23 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 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 0.472, deepest hole -0.394, 1-sigma level 0.074 GRID BOND $H fmap 2 acta 144 MERG 2 REM C:/Users/chmmah/Desktop/250%20K/ig12c4ht.hkl WGHT 0.116800 20.489500 FVAR 2.96807 1.38428 FE1 5 0.500000 0.287852 0.250000 10.50000 0.09026 0.04182 = 0.04457 0.00000 0.01968 0.00000 FE2 5 0.500000 0.000000 0.500000 10.50000 0.04600 0.04523 = 0.03118 -0.00246 0.00668 0.00881 PART 1 N3A 6 0.594194 0.300625 0.290213 10.55000 0.04231 C4A 1 0.632620 0.359805 0.263820 10.55000 0.05231 C5A 1 0.701544 0.372329 0.292654 10.55000 0.06759 AFIX 43 H5A 2 0.728945 0.409994 0.271506 10.55000 -1.20000 AFIX 0 C6A 1 0.727002 0.326279 0.353867 10.55000 0.08062 AFIX 43 H6A 2 0.771562 0.337534 0.377301 10.55000 -1.20000 AFIX 0 C7A 1 0.690300 0.264832 0.382114 10.55000 0.06341 AFIX 43 H7A 2 0.708455 0.232260 0.422625 10.55000 -1.20000 AFIX 0 C8A 1 0.623988 0.254991 0.345603 10.55000 0.04607 N9A 6 0.596382 0.402984 0.205663 10.55000 0.05133 N10A 6 0.528340 0.379513 0.180716 10.55000 0.05234 C11A 1 0.508448 0.427830 0.124793 10.55000 0.07279 AFIX 43 H11A 2 0.464911 0.425217 0.096448 10.55000 -1.20000 AFIX 0 C12A 1 0.559148 0.483744 0.111912 10.55000 0.08583 AFIX 43 H12A 2 0.554985 0.525011 0.075459 10.55000 -1.20000 AFIX 0 C13A 1 0.618922 0.466982 0.164362 10.55000 0.06147 AFIX 43 H13A 2 0.662034 0.492535 0.169495 10.55000 -1.20000 AFIX 0 PART 0 PART 2 N3B 6 0.614523 0.282205 0.300771 10.45000 0.04468 C4B 1 0.657445 0.337262 0.277259 10.45000 0.04916 C5B 1 0.725538 0.337666 0.309228 10.45000 0.07274 AFIX 43 H5B 2 0.755944 0.377207 0.295083 10.45000 -1.20000 AFIX 0 C6B 1 0.745915 0.283473 0.358011 10.45000 0.09366 AFIX 43 H6B 2 0.792557 0.281231 0.377251 10.45000 -1.20000 AFIX 0 C7B 1 0.703805 0.229594 0.383061 10.45000 0.06746 AFIX 43 H7B 2 0.719780 0.191856 0.420720 10.45000 -1.20000 AFIX 0 C8B 1 0.638861 0.231173 0.353052 10.45000 0.05109 N9B 6 0.626508 0.387359 0.219541 10.45000 0.05550 N10B 6 0.560204 0.379085 0.193238 10.45000 0.04791 C11B 1 0.544632 0.433979 0.140498 10.45000 0.07010 AFIX 43 H11B 2 0.501157 0.439814 0.112495 10.45000 -1.20000 AFIX 0 C12B 1 0.596282 0.478242 0.132359 10.45000 0.07372 AFIX 43 H12B 2 0.596585 0.521758 0.098376 10.45000 -1.20000 AFIX 0 C13B 1 0.653936 0.450807 0.183559 10.45000 0.08215 AFIX 43 H13B 2 0.698896 0.471071 0.190629 10.45000 -1.20000 AFIX 0 PART 0 N14 6 0.581567 0.187624 0.369133 11.00000 0.04464 0.06752 = 0.04294 -0.00389 0.01020 -0.01255 N15 6 0.515577 0.191859 0.335538 11.00000 0.04929 0.05045 = 0.04500 0.00131 0.00784 -0.00181 C16 1 0.484730 0.133494 0.367853 11.00000 0.04050 0.05034 = 0.04941 0.00028 0.00613 -0.00296 AFIX 43 H16 2 0.438079 0.121240 0.355513 11.00000 -1.20000 AFIX 0 N17 6 0.527099 0.092676 0.420895 11.00000 0.04536 0.05244 = 0.04526 0.00223 0.00686 0.00388 C18 1 0.586214 0.127149 0.419254 11.00000 0.04417 0.07973 = 0.04062 -0.00005 0.00386 0.00086 AFIX 43 H18 2 0.626804 0.111492 0.449404 11.00000 -1.20000 AFIX 0 N19 6 0.249632 0.163018 0.551774 11.00000 0.05361 0.06515 = 0.04956 0.01487 0.01542 0.01910 C20 1 0.199492 0.206065 0.574280 11.00000 0.05937 0.06936 = 0.05648 0.02348 0.02400 0.02657 C21 1 0.132527 0.203856 0.540507 11.00000 0.05711 0.08797 = 0.07677 0.01414 0.02485 0.02354 AFIX 43 H21 2 0.098739 0.235726 0.557664 11.00000 -1.20000 AFIX 0 C22 1 0.117335 0.152864 0.480498 11.00000 0.04688 0.11122 = 0.09673 0.01196 0.01466 0.01190 AFIX 43 H22 2 0.072149 0.149418 0.456310 11.00000 -1.20000 AFIX 0 C23 1 0.168169 0.105977 0.454862 11.00000 0.05283 0.09408 = 0.07841 -0.00161 0.01636 0.00925 AFIX 43 H23 2 0.158844 0.070986 0.413953 11.00000 -1.20000 AFIX 0 C24 1 0.232274 0.114858 0.493695 11.00000 0.04278 0.07462 = 0.06273 0.01784 0.01610 0.01468 N25 6 0.220323 0.255276 0.635294 11.00000 0.07205 0.07668 = 0.05596 0.01266 0.02222 0.03308 N26 6 0.175249 0.307907 0.662098 11.00000 0.08405 0.07922 = 0.07688 0.01347 0.03551 0.04137 C27 1 0.212834 0.347575 0.715707 11.00000 0.11589 0.09567 = 0.07899 0.00416 0.02823 0.05632 AFIX 43 H27 2 0.196113 0.388974 0.744077 11.00000 -1.20000 AFIX 0 C28 1 0.281074 0.320991 0.725834 11.00000 0.10736 0.11674 = 0.07125 -0.01175 0.01076 0.03949 AFIX 43 H28 2 0.316872 0.339365 0.761545 11.00000 -1.20000 AFIX 0 C29 1 0.284347 0.263024 0.672999 11.00000 0.07337 0.10480 = 0.06439 -0.00036 0.01292 0.04070 AFIX 43 H29 2 0.323343 0.234005 0.664309 11.00000 -1.20000 AFIX 0 N30 6 0.289190 0.072064 0.473134 11.00000 0.04776 0.06844 = 0.04186 0.00498 0.01029 0.00880 N31 6 0.282176 0.016820 0.416573 11.00000 0.05041 0.08325 = 0.05674 -0.00928 0.00899 -0.00137 C32 1 0.344523 -0.007252 0.416194 11.00000 0.05799 0.07008 = 0.04145 -0.00518 0.01212 0.00348 AFIX 43 H32 2 0.356182 -0.045876 0.382231 11.00000 -1.20000 AFIX 0 N33 6 0.391491 0.027675 0.468609 11.00000 0.04617 0.05648 = 0.03454 0.00146 0.00798 0.01166 C34 1 0.353613 0.077517 0.503020 11.00000 0.04948 0.05999 = 0.04074 0.00121 0.00831 0.01492 AFIX 43 H34 2 0.370477 0.111699 0.542938 11.00000 -1.20000 AFIX 0 O35 7 0.507028 0.094851 0.579202 11.00000 0.06360 0.06117 = 0.05541 -0.01835 0.01652 -0.00299 H35A 2 0.532591 0.140067 0.584720 11.00000 -1.50000 H35B 2 0.496846 0.085677 0.622506 11.00000 -1.50000 B36 3 0.381596 0.047408 0.717076 11.00000 0.09193 0.08057 = 0.06833 0.02322 0.02821 0.02234 PART 1 F37A 4 0.411899 0.077796 0.664776 10.34000 0.07481 F38A 4 0.310759 0.036123 0.686306 10.34000 0.07470 F39A 4 0.380870 0.104959 0.775564 10.34000 0.06417 F40A 4 0.407968 -0.030715 0.737574 10.34000 0.05864 PART 0 PART 2 F37B 4 0.423505 0.100916 0.680456 10.33000 0.06653 F38B 4 0.337808 0.004861 0.659098 10.33000 0.14453 F39B 4 0.347068 0.085289 0.760151 10.33000 0.08954 F40B 4 0.423992 -0.010209 0.756502 10.33000 0.11489 PART 0 PART 3 F37C 4 0.400069 0.105255 0.668462 10.33000 0.06528 F38C 4 0.315346 0.048899 0.717916 10.33000 0.09903 F39C 4 0.412327 0.080036 0.787534 10.33000 0.13255 F40C 4 0.406448 -0.031411 0.710978 10.33000 0.10914 PART 0 B41 3 0.593151 0.293114 0.549583 11.00000 0.15281 0.09306 = 0.07937 -0.02102 0.03303 -0.03057 PART 1 F42A 4 0.613139 0.346131 0.501515 10.34000 0.13536 F43A 4 0.634915 0.216441 0.548278 10.34000 0.10329 F44A 4 0.600816 0.319951 0.618759 10.34000 0.14941 F45A 4 0.529104 0.260477 0.524711 10.34000 0.14357 PART 0 PART 2 F42B 4 0.544627 0.298905 0.482871 10.33000 0.11182 F43B 4 0.643212 0.343530 0.548532 10.33000 0.10867 F44B 4 0.548063 0.328126 0.597710 10.33000 0.11821 F45B 4 0.599273 0.210532 0.565615 10.33000 0.08123 PART 0 PART 3 F42C 4 0.563500 0.344605 0.496317 10.33000 0.16031 F43C 4 0.640572 0.345580 0.600145 10.33000 0.08177 F44C 4 0.554295 0.253030 0.588192 10.33000 0.15187 F45C 4 0.644731 0.245861 0.523084 10.33000 0.15387 PART 0 O46 7 0.262236 -0.070395 0.572297 10.50000 0.10812 PART 1 C47A 1 0.482955 0.716666 0.250205 10.30000 0.14491 AFIX 33 H47A 2 0.473126 0.732329 0.297416 10.30000 -1.50000 H47B 2 0.443332 0.727565 0.213772 10.30000 -1.50000 H47C 2 0.521128 0.749592 0.239562 10.30000 -1.50000 AFIX 0 PART 0 N48 6 0.500000 0.626779 0.250000 10.50000 0.09363 0.13623 = 0.10261 0.00000 0.02676 0.00000 PART 1 O49A 7 0.455783 0.577874 0.221850 10.30000 0.08685 O50A 7 0.546261 0.600706 0.295044 10.30000 0.12927 PART 0 PART 2 C47B 1 0.488502 0.716933 0.236756 10.20000 0.06698 AFIX 33 H47D 2 0.509760 0.734235 0.196150 10.20000 -1.50000 H47E 2 0.508149 0.748462 0.279475 10.20000 -1.50000 H47F 2 0.439974 0.727884 0.225862 10.20000 -1.50000 AFIX 0 O49B 7 0.460822 0.576408 0.217685 10.20000 0.18274 O50B 7 0.554025 0.604060 0.284529 10.20000 0.11461 HKLF 4 REM ig12c4+fe-meno2_a.res in C2/c REM R1 = 0.0848 for 3749 Fo > 4sig(Fo) and 0.1236 for all 5722 data REM 452 parameters refined using 75 restraints END WGHT 0.1168 20.4722 REM Highest difference peak 0.471, deepest hole -0.394, 1-sigma level 0.074 Q1 1 0.4384 0.0250 0.7858 11.00000 0.05 0.47 Q2 1 0.3184 -0.0048 0.6445 11.00000 0.05 0.46 Q3 1 0.5939 0.2185 0.6041 11.00000 0.05 0.46 Q4 1 0.4064 0.1329 0.7866 11.00000 0.05 0.46 Q5 1 0.4469 0.0312 0.4884 11.00000 0.05 0.45 Q6 1 0.5884 0.3117 0.4787 11.00000 0.05 0.41 Q7 1 0.4504 0.0653 0.6904 11.00000 0.05 0.41 Q8 1 0.5369 0.3672 0.5761 11.00000 0.05 0.41 Q9 1 0.3750 0.1438 0.7766 11.00000 0.05 0.40 Q10 1 0.5379 0.2799 0.5784 11.00000 0.05 0.36 Q11 1 0.5178 0.2820 0.4801 11.00000 0.05 0.35 Q12 1 0.6623 0.3220 0.5892 11.00000 0.05 0.35 Q13 1 0.6505 0.2957 0.5020 11.00000 0.05 0.34 Q14 1 0.5620 0.2969 0.6205 11.00000 0.05 0.32 Q15 1 0.7410 0.3126 0.3329 11.00000 0.05 0.32 Q16 1 0.2774 -0.0621 0.6028 11.00000 0.05 0.31 Q17 1 0.3088 0.0025 0.7016 11.00000 0.05 0.30 Q18 1 0.4556 0.1083 0.5732 11.00000 0.05 0.30 Q19 1 0.2460 -0.0960 0.5415 11.00000 0.05 0.30 Q20 1 0.4504 0.2550 0.2363 11.00000 0.05 0.30 REM The information below was added by Olex2. REM REM R1 = 0.0848 for 3749 Fo > 4sig(Fo) and 0.1236 for all 11506 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.47, deepest hole -0.39 REM Mean Shift 0, Max Shift 0. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.1236 REM R1_gt = 0.0848 REM wR_ref = 0.2496 REM GOOF = 1.031 REM Shift_max = 0 REM Shift_mean = 0 REM Reflections_all = 11506 REM Reflections_gt = 3749 REM Parameters = n/a REM Hole = 0.47 REM Peak = -0.39 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 0.28785(8) 0.2500 0.0579(4) Uani 1 2 d S . . Fe2 Fe 0.5000 0.0000 0.5000 0.0408(3) Uani 1 2 d S . . N3A N 0.5942(5) 0.3006(6) 0.2902(5) 0.042(2) Uiso 0.55 1 d P A 1 C4A C 0.6326(6) 0.3598(8) 0.2638(7) 0.052(3) Uiso 0.55 1 d P A 1 C5A C 0.7015(7) 0.3723(9) 0.2927(7) 0.068(3) Uiso 0.55 1 d P A 1 H5A H 0.7289 0.4100 0.2715 0.081 Uiso 0.55 1 calc PR A 1 C6A C 0.7270(8) 0.3263(11) 0.3539(9) 0.081(4) Uiso 0.55 1 d P A 1 H6A H 0.7716 0.3375 0.3773 0.097 Uiso 0.55 1 calc PR A 1 C7A C 0.6903(7) 0.2648(9) 0.3821(7) 0.063(3) Uiso 0.55 1 d P A 1 H7A H 0.7085 0.2323 0.4226 0.076 Uiso 0.55 1 calc PR A 1 C8A C 0.6240(6) 0.2550(8) 0.3456(7) 0.046(3) Uiso 0.55 1 d P A 1 N9A N 0.5964(6) 0.4030(6) 0.2057(5) 0.051(2) Uiso 0.55 1 d P A 1 N10A N 0.5283(6) 0.3795(6) 0.1807(5) 0.052(2) Uiso 0.55 1 d P A 1 C11A C 0.5084(8) 0.4278(9) 0.1248(8) 0.073(3) Uiso 0.55 1 d P A 1 H11A H 0.4649 0.4252 0.0964 0.087 Uiso 0.55 1 calc PR A 1 C12A C 0.5591(9) 0.4837(11) 0.1119(9) 0.086(4) Uiso 0.55 1 d P A 1 H12A H 0.5550 0.5250 0.0755 0.103 Uiso 0.55 1 calc PR A 1 C13A C 0.6189(8) 0.4670(8) 0.1644(8) 0.061(3) Uiso 0.55 1 d P A 1 H13A H 0.6620 0.4925 0.1695 0.074 Uiso 0.55 1 calc PR A 1 N3B N 0.6145(6) 0.2822(7) 0.3008(7) 0.045(3) Uiso 0.45 1 d P A 2 C4B C 0.6574(8) 0.3373(9) 0.2773(7) 0.049(3) Uiso 0.45 1 d P A 2 C5B C 0.7255(9) 0.3377(12) 0.3092(10) 0.073(4) Uiso 0.45 1 d P A 2 H5B H 0.7559 0.3772 0.2951 0.087 Uiso 0.45 1 calc PR A 2 C6B C 0.7459(11) 0.2835(14) 0.3580(11) 0.094(6) Uiso 0.45 1 d P A 2 H6B H 0.7926 0.2812 0.3773 0.112 Uiso 0.45 1 calc PR A 2 C7B C 0.7038(9) 0.2296(12) 0.3831(9) 0.067(4) Uiso 0.45 1 d P A 2 H7B H 0.7198 0.1919 0.4207 0.081 Uiso 0.45 1 calc PR A 2 C8B C 0.6389(8) 0.2312(10) 0.3531(8) 0.051(4) Uiso 0.45 1 d P A 2 N9B N 0.6265(7) 0.3874(8) 0.2195(7) 0.055(3) Uiso 0.45 1 d P A 2 N10B N 0.5602(7) 0.3791(7) 0.1932(6) 0.048(2) Uiso 0.45 1 d P A 2 C11B C 0.5446(10) 0.4340(11) 0.1405(9) 0.070(4) Uiso 0.45 1 d P A 2 H11B H 0.5012 0.4398 0.1125 0.084 Uiso 0.45 1 calc PR A 2 C12B C 0.5963(11) 0.4782(12) 0.1324(12) 0.074(5) Uiso 0.45 1 d P A 2 H12B H 0.5966 0.5218 0.0984 0.088 Uiso 0.45 1 calc PR A 2 C13B C 0.6539(11) 0.4508(12) 0.1836(10) 0.082(5) Uiso 0.45 1 d P A 2 H13B H 0.6989 0.4711 0.1906 0.099 Uiso 0.45 1 calc PR A 2 N14 N 0.5816(2) 0.1876(3) 0.3691(2) 0.0514(11) Uani 1 1 d . . . N15 N 0.5156(2) 0.1919(3) 0.3355(2) 0.0482(10) Uani 1 1 d . A . C16 C 0.4847(3) 0.1335(3) 0.3679(3) 0.0469(12) Uani 1 1 d . . . H16 H 0.4381 0.1212 0.3555 0.056 Uiso 1 1 calc R A . N17 N 0.5271(2) 0.0927(3) 0.4209(2) 0.0478(10) Uani 1 1 d . A . C18 C 0.5862(3) 0.1271(4) 0.4193(3) 0.0552(14) Uani 1 1 d . A . H18 H 0.6268 0.1115 0.4494 0.066 Uiso 1 1 calc R . . N19 N 0.2496(2) 0.1630(3) 0.5518(3) 0.0553(12) Uani 1 1 d . . . C20 C 0.1995(3) 0.2061(4) 0.5743(3) 0.0601(16) Uani 1 1 d . . . C21 C 0.1325(3) 0.2039(5) 0.5405(4) 0.0724(19) Uani 1 1 d . . . H21 H 0.0987 0.2357 0.5577 0.087 Uiso 1 1 calc R . . C22 C 0.1173(4) 0.1529(6) 0.4805(5) 0.085(2) Uani 1 1 d . . . H22 H 0.0721 0.1494 0.4563 0.102 Uiso 1 1 calc R . . C23 C 0.1682(3) 0.1060(5) 0.4549(4) 0.0745(19) Uani 1 1 d . . . H23 H 0.1588 0.0710 0.4140 0.089 Uiso 1 1 calc R . . C24 C 0.2323(3) 0.1149(4) 0.4937(3) 0.0592(15) Uani 1 1 d . . . N25 N 0.2203(3) 0.2553(4) 0.6353(3) 0.0669(15) Uani 1 1 d . . . N26 N 0.1752(3) 0.3079(4) 0.6621(4) 0.0775(18) Uani 1 1 d . . . C27 C 0.2128(5) 0.3476(6) 0.7157(5) 0.095(3) Uani 1 1 d . . . H27 H 0.1961 0.3890 0.7441 0.115 Uiso 1 1 calc R . . C28 C 0.2811(5) 0.3210(6) 0.7258(5) 0.099(3) Uani 1 1 d . . . H28 H 0.3169 0.3394 0.7615 0.119 Uiso 1 1 calc R . . C29 C 0.2843(4) 0.2630(5) 0.6730(4) 0.081(2) Uani 1 1 d . . . H29 H 0.3233 0.2340 0.6643 0.097 Uiso 1 1 calc R . . N30 N 0.2892(2) 0.0721(3) 0.4731(2) 0.0524(11) Uani 1 1 d . . . N31 N 0.2822(3) 0.0168(4) 0.4166(3) 0.0635(14) Uani 1 1 d . . . C32 C 0.3445(3) -0.0073(4) 0.4162(3) 0.0561(14) Uani 1 1 d . . . H32 H 0.3562 -0.0459 0.3822 0.067 Uiso 1 1 calc R . . N33 N 0.3915(2) 0.0277(3) 0.4686(2) 0.0456(10) Uani 1 1 d . . . C34 C 0.3536(3) 0.0775(4) 0.5030(3) 0.0500(13) Uani 1 1 d . . . H34 H 0.3705 0.1117 0.5429 0.060 Uiso 1 1 calc R . . O35 O 0.5070(2) 0.0949(3) 0.5792(2) 0.0593(10) Uani 1 1 d D . . H35A H 0.533(3) 0.140(3) 0.585(3) 0.089 Uiso 1 1 d D . . H35B H 0.497(4) 0.086(4) 0.6225(19) 0.089 Uiso 1 1 d D . . B36 B 0.3816(4) 0.0474(5) 0.7171(4) 0.079(2) Uani 1 1 d D . . F37A F 0.4119(8) 0.0778(9) 0.6648(7) 0.075(4) Uiso 0.34 1 d PD B 1 F38A F 0.3108(5) 0.0361(8) 0.6863(8) 0.075(4) Uiso 0.34 1 d PD B 1 F39A F 0.3809(7) 0.1050(7) 0.7756(6) 0.064(3) Uiso 0.34 1 d PD B 1 F40A F 0.4080(6) -0.0307(7) 0.7376(9) 0.059(3) Uiso 0.34 1 d PD B 1 F37B F 0.4235(7) 0.1009(10) 0.6805(7) 0.067(4) Uiso 0.33 1 d PD B 2 F38B F 0.3378(10) 0.0049(12) 0.6591(9) 0.145(7) Uiso 0.33 1 d PD B 2 F39B F 0.3471(8) 0.0853(9) 0.7602(8) 0.090(4) Uiso 0.33 1 d PD B 2 F40B F 0.4240(9) -0.0102(11) 0.7565(9) 0.115(7) Uiso 0.33 1 d PD B 2 F37C F 0.4001(8) 0.1053(9) 0.6685(7) 0.065(4) Uiso 0.33 1 d PD B 3 F38C F 0.3153(6) 0.0489(11) 0.7179(11) 0.099(5) Uiso 0.33 1 d PD B 3 F39C F 0.4123(10) 0.0800(12) 0.7875(8) 0.133(7) Uiso 0.33 1 d PD B 3 F40C F 0.4064(9) -0.0314(8) 0.7110(10) 0.109(7) Uiso 0.33 1 d PD B 3 B41 B 0.5932(5) 0.2931(6) 0.5496(5) 0.107(4) Uani 1 1 d D . . F42A F 0.6131(11) 0.3461(11) 0.5015(10) 0.135(6) Uiso 0.34 1 d PD C 1 F43A F 0.6349(8) 0.2164(9) 0.5483(9) 0.103(5) Uiso 0.34 1 d PD C 1 F44A F 0.6008(12) 0.3200(12) 0.6188(8) 0.149(7) Uiso 0.34 1 d PD C 1 F45A F 0.5291(7) 0.2605(12) 0.5247(11) 0.144(7) Uiso 0.34 1 d PD C 1 F42B F 0.5446(8) 0.2989(12) 0.4829(7) 0.112(5) Uiso 0.33 1 d PD C 2 F43B F 0.6432(7) 0.3435(9) 0.5485(10) 0.109(5) Uiso 0.33 1 d PD C 2 F44B F 0.5481(8) 0.3281(10) 0.5977(8) 0.118(5) Uiso 0.33 1 d PD C 2 F45B F 0.5993(7) 0.2105(7) 0.5656(7) 0.081(4) Uiso 0.33 1 d PD C 2 F42C F 0.5635(12) 0.3446(14) 0.4963(10) 0.160(9) Uiso 0.33 1 d PD C 3 F43C F 0.6406(6) 0.3456(8) 0.6001(7) 0.082(3) Uiso 0.33 1 d PD C 3 F44C F 0.5543(10) 0.2530(13) 0.5882(11) 0.152(7) Uiso 0.33 1 d PD C 3 F45C F 0.6447(9) 0.2459(13) 0.5231(12) 0.154(9) Uiso 0.33 1 d PD C 3 O46 O 0.2622(7) -0.0704(9) 0.5723(7) 0.108(4) Uiso 0.50 1 d P . . C47A C 0.483(3) 0.7167(13) 0.250(4) 0.14(3) Uiso 0.30 1 d PD D 1 H47A H 0.4731 0.7323 0.2974 0.217 Uiso 0.30 1 calc PR D 1 H47B H 0.4433 0.7276 0.2138 0.217 Uiso 0.30 1 calc PR D 1 H47C H 0.5211 0.7496 0.2396 0.217 Uiso 0.30 1 calc PR D 1 N48 N 0.5000 0.6268(8) 0.2500 0.110(4) Uani 1 2 d SD . . O49A O 0.4558(18) 0.578(2) 0.222(2) 0.087(11) Uiso 0.30 1 d PD . 1 O50A O 0.546(2) 0.601(3) 0.295(3) 0.13(3) Uiso 0.30 1 d PD . 1 C47B C 0.489(3) 0.7169(12) 0.237(3) 0.067(14) Uiso 0.20 1 d PD D 2 H47D H 0.5098 0.7342 0.1961 0.100 Uiso 0.20 1 calc PR D 2 H47E H 0.5081 0.7485 0.2795 0.100 Uiso 0.20 1 calc PR D 2 H47F H 0.4400 0.7279 0.2259 0.100 Uiso 0.20 1 calc PR D 2 O49B O 0.461(4) 0.576(3) 0.218(8) 0.18(6) Uiso 0.20 1 d PD . 2 O50B O 0.554(2) 0.604(4) 0.285(4) 0.11(3) 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 0.0903(10) 0.0418(7) 0.0446(7) 0.000 0.0197(6) 0.000 Fe2 0.0460(6) 0.0452(6) 0.0312(5) -0.0025(5) 0.0067(4) 0.0088(5) N14 0.045(2) 0.068(3) 0.043(2) -0.004(2) 0.0102(19) -0.013(2) N15 0.049(3) 0.050(3) 0.045(2) 0.001(2) 0.0078(19) -0.002(2) C16 0.040(3) 0.050(3) 0.049(3) 0.000(2) 0.006(2) -0.003(2) N17 0.045(2) 0.052(3) 0.045(2) 0.002(2) 0.0069(19) 0.004(2) C18 0.044(3) 0.080(4) 0.041(3) 0.000(3) 0.004(2) 0.001(3) N19 0.054(3) 0.065(3) 0.050(3) 0.015(2) 0.015(2) 0.019(2) C20 0.059(4) 0.069(4) 0.056(3) 0.023(3) 0.024(3) 0.027(3) C21 0.057(4) 0.088(5) 0.077(5) 0.014(4) 0.025(3) 0.024(4) C22 0.047(4) 0.111(6) 0.097(6) 0.012(5) 0.015(4) 0.012(4) C23 0.053(4) 0.094(5) 0.078(5) -0.002(4) 0.016(3) 0.009(4) C24 0.043(3) 0.075(4) 0.063(4) 0.018(3) 0.016(3) 0.015(3) N25 0.072(4) 0.077(4) 0.056(3) 0.013(3) 0.022(3) 0.033(3) N26 0.084(4) 0.079(4) 0.077(4) 0.013(3) 0.036(3) 0.041(3) C27 0.116(7) 0.096(6) 0.079(5) 0.004(5) 0.028(5) 0.056(5) C28 0.107(6) 0.117(7) 0.071(5) -0.012(5) 0.011(4) 0.039(6) C29 0.073(5) 0.105(6) 0.064(4) 0.000(4) 0.013(3) 0.041(4) N30 0.048(3) 0.068(3) 0.042(2) 0.005(2) 0.0103(19) 0.009(2) N31 0.050(3) 0.083(4) 0.057(3) -0.009(3) 0.009(2) -0.001(3) C32 0.058(3) 0.070(4) 0.041(3) -0.005(3) 0.012(2) 0.003(3) N33 0.046(2) 0.056(3) 0.035(2) 0.0015(18) 0.0080(18) 0.012(2) C34 0.049(3) 0.060(3) 0.041(3) 0.001(2) 0.008(2) 0.015(3) O35 0.064(3) 0.061(3) 0.055(2) -0.018(2) 0.0165(19) -0.003(2) B36 0.092(6) 0.081(6) 0.068(5) 0.023(4) 0.028(4) 0.022(5) B41 0.153(11) 0.093(8) 0.079(7) -0.021(6) 0.033(7) -0.031(8) N48 0.094(8) 0.136(11) 0.103(8) 0.000 0.027(7) 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 167.8(6) 2_655 . N3A Fe1 N3B 176.0(4) . 2_655 N3A Fe1 N10A 79.8(4) . . N3A Fe1 N10A 91.7(4) . 2_655 N3A Fe1 N15 111.8(3) . 2_655 N3A Fe1 N15 77.0(3) . . N10A Fe1 N10A 91.8(5) 2_655 . N10A Fe1 N10B 93.8(3) 2_655 . N10A Fe1 N15 92.8(3) . 2_655 N10A Fe1 N15 156.5(3) . . N3B Fe1 N3B 175.6(6) 2_655 . N10A Fe1 N3B 96.9(4) 2_655 . N10A Fe1 N3B 86.2(4) . . N10B Fe1 N3B 69.8(5) . . N10B Fe1 N3B 113.2(4) 2_655 . N10B Fe1 N10B 100.2(6) 2_655 . N15 Fe1 N3B 70.3(3) . . N15 Fe1 N3B 106.4(3) . 2_655 N15 Fe1 N10B 97.0(3) . 2_655 N15 Fe1 N10B 140.1(4) . . N15 Fe1 N15 92.2(2) 2_655 . N17 Fe2 N17 180.00 . 5_656 N33 Fe2 N17 91.50(16) . . N33 Fe2 N17 88.50(16) . 5_656 N33 Fe2 N33 180.00 . 5_656 O35 Fe2 N17 90.17(17) . . O35 Fe2 N17 89.83(17) . 5_656 O35 Fe2 N33 89.64(17) . . O35 Fe2 N33 90.36(17) . 5_656 O35 Fe2 O35 180.00 5_656 . C4A N3A Fe1 120.4(9) . . C8A N3A Fe1 122.3(8) . . C8A N3A C4A 117.3(11) . . N3A C4A C5A 122.2(13) . . N3A C4A N9A 112.2(11) . . N9A C4A C5A 125.6(12) . . C4A C5A H5A 121.8 . . C6A C5A C4A 116.5(13) . . C6A C5A H5A 121.8 . . C5A C6A H6A 118.4 . . C7A C6A C5A 123.2(15) . . C7A C6A H6A 118.4 . . C6A C7A H7A 122.9 . . C6A C7A C8A 114.3(14) . . C8A C7A H7A 122.9 . . N3A C8A C7A 126.2(12) . . N3A C8A N14 115.2(9) . . C7A C8A N14 118.6(11) . . C4A N9A N10A 118.6(10) . . C4A N9A C13A 128.5(13) . . C13A N9A N10A 112.8(11) . . N9A N10A Fe1 108.8(7) . . C11A N10A Fe1 146.1(10) . . C11A N10A N9A 105.0(10) . . N10A C11A H11A 123.8 . . N10A C11A C12A 112.3(15) . . C12A C11A H11A 123.8 . . C11A C12A H12A 126.1 . . C11A C12A C13A 107.8(15) . . C13A C12A H12A 126.1 . . N9A C13A C12A 102.0(12) . . N9A C13A H13A 129.0 . . C12A C13A H13A 129.0 . . C4B N3B Fe1 118.3(10) . . C8B N3B Fe1 123.4(10) . . C8B N3B C4B 118.2(13) . . N3B C4B C5B 119.3(15) . . N3B C4B N9B 113.5(13) . . C5B C4B N9B 127.2(14) . . C4B C5B H5B 120.7 . . C6B C5B C4B 118.7(18) . . C6B C5B H5B 120.7 . . C5B C6B H6B 118.6 . . C5B C6B C7B 123(2) . . C7B C6B H6B 118.6 . . C6B C7B H7B 121.1 . . C8B C7B C6B 117.7(19) . . C8B C7B H7B 121.1 . . N3B C8B C7B 123.3(15) . . N3B C8B N14 104.6(12) . . C7B C8B N14 132.0(15) . . N10B N9B C4B 120.7(12) . . N10B N9B C13B 109.8(15) . . C13B N9B C4B 129.4(14) . . N9B N10B Fe1 117.3(8) . . C11B N10B Fe1 134.6(13) . . C11B N10B N9B 107.9(15) . . N10B C11B H11B 124.5 . . C12B C11B N10B 111.1(19) . . C12B C11B H11B 124.5 . . C11B C12B H12B 125.5 . . C11B C12B C13B 109(2) . . C13B C12B H12B 125.5 . . N9B C13B C12B 102.2(17) . . N9B C13B H13B 128.9 . . C12B C13B H13B 128.9 . . N15 N14 C8A 112.5(7) . . N15 N14 C8B 129.1(8) . . C18 N14 C8A 139.0(7) . . C18 N14 C8B 122.6(8) . . C18 N14 N15 108.1(4) . . N14 N15 Fe1 112.4(3) . . C16 N15 Fe1 143.6(4) . . C16 N15 N14 104.0(4) . . N15 C16 H16 123.4 . . N15 C16 N17 113.1(5) . . N17 C16 H16 123.4 . . C16 N17 Fe2 128.0(4) . . C18 N17 Fe2 127.9(4) . . C18 N17 C16 103.7(5) . . N14 C18 H18 124.4 . . N17 C18 N14 111.1(5) . . N17 C18 H18 124.4 . . C24 N19 C20 116.5(5) . . N19 C20 C21 124.0(7) . . N19 C20 N25 114.2(6) . . C21 C20 N25 121.8(6) . . C20 C21 H21 121.5 . . C22 C21 C20 117.1(6) . . C22 C21 H21 121.5 . . C21 C22 H22 119.4 . . C21 C22 C23 121.1(7) . . C23 C22 H22 119.4 . . C22 C23 H23 122.4 . . C24 C23 C22 115.2(7) . . C24 C23 H23 122.4 . . N19 C24 C23 126.1(6) . . N19 C24 N30 112.6(5) . . C23 C24 N30 121.3(6) . . N26 N25 C20 121.0(6) . . C29 N25 C20 127.3(5) . . C29 N25 N26 111.6(6) . . C27 N26 N25 104.2(6) . . N26 C27 H27 123.9 . . N26 C27 C28 112.1(7) . . C28 C27 H27 123.9 . . C27 C28 H28 127.3 . . C29 C28 C27 105.4(8) . . C29 C28 H28 127.3 . . N25 C29 C28 106.6(6) . . N25 C29 H29 126.7 . . C28 C29 H29 126.7 . . N31 N30 C24 122.1(5) . . C34 N30 C24 128.0(5) . . C34 N30 N31 109.9(5) . . C32 N31 N30 102.6(5) . . N31 C32 H32 122.6 . . N31 C32 N33 114.9(5) . . N33 C32 H32 122.6 . . C32 N33 Fe2 130.1(4) . . C34 N33 Fe2 127.1(4) . . C34 N33 C32 102.4(5) . . N30 C34 N33 110.2(5) . . N30 C34 H34 124.9 . . N33 C34 H34 124.9 . . Fe2 O35 H35A 130(4) . . Fe2 O35 H35B 122(4) . . H35A O35 H35B 104(3) . . F37A B36 F38A 106.5(10) . . F37A B36 F39A 113.5(9) . . F37A B36 F40A 109.6(10) . . F39A B36 F38A 104.6(8) . . F40A B36 F38A 107.6(9) . . F40A B36 F39A 114.4(9) . . F37B B36 F38B 104.0(10) . . F39B B36 F37B 115.7(10) . . F39B B36 F38B 111.7(11) . . F39B B36 F40B 108.4(10) . . F40B B36 F37B 107.2(10) . . F40B B36 F38B 109.6(11) . . F37C B36 F39C 104.1(10) . . F38C B36 F37C 111.7(10) . . F38C B36 F39C 104.7(10) . . F38C B36 F40C 113.3(11) . . F40C B36 F37C 114.5(11) . . F40C B36 F39C 107.4(11) . . F42A B41 F43A 105.9(11) . . F42A B41 F44A 116.7(12) . . F42A B41 F45A 111.6(12) . . F44A B41 F43A 107.5(11) . . F44A B41 F45A 113.1(12) . . F45A B41 F43A 100.2(10) . . F42B B41 F44B 96.7(10) . . F43B B41 F42B 110.9(11) . . F43B B41 F44B 109.1(11) . . F43B B41 F45B 124.7(12) . . F45B B41 F42B 106.1(10) . . F45B B41 F44B 105.7(10) . . F42C B41 F43C 106.8(12) . . F42C B41 F45C 108.2(12) . . F44C B41 F42C 118.5(13) . . F44C B41 F43C 107.0(11) . . F44C B41 F45C 117.6(13) . . F45C B41 F43C 95.7(10) . . H47A C47A H47B 109.5 . . H47A C47A H47C 109.5 . . H47B C47A H47C 109.5 . . N48 C47A H47A 109.5 . . N48 C47A H47B 109.5 . . N48 C47A H47C 109.5 . . O49A N48 C47A 117.8(17) . . O50A N48 C47A 118.6(19) . . O50A N48 O49A 119.5(19) . . 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 119(2) . . O49B N48 O50B 121(2) . . O50B N48 C47B 118.7(18) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Fe1 N3A 1.913(9) Fe1 N10A 2.089(9) Fe1 N3B 2.324(12) Fe1 N10B 2.255(12) Fe1 N15 2.196(5) Fe2 N17 2.217(4) Fe2 N33 2.188(4) Fe2 O35 2.102(4) N3A C4A 1.355(15) N3A C8A 1.323(16) C4A C5A 1.404(18) C4A N9A 1.385(16) C5A H5A 0.9400 C5A C6A 1.38(2) C6A H6A 0.9400 C6A C7A 1.38(2) C7A H7A 0.9400 C7A C8A 1.392(18) C8A N14 1.474(13) N9A N10A 1.409(14) N9A C13A 1.395(16) N10A C11A 1.306(17) C11A H11A 0.9400 C11A C12A 1.39(2) C12A H12A 0.9400 C12A C13A 1.44(2) C13A H13A 0.9400 N3B C4B 1.346(17) N3B C8B 1.30(2) C4B C5B 1.39(2) C4B N9B 1.400(19) C5B H5B 0.9400 C5B C6B 1.27(3) C6B H6B 0.9400 C6B C7B 1.34(3) C7B H7B 0.9400 C7B C8B 1.32(2) C8B N14 1.409(15) N9B N10B 1.338(18) N9B C13B 1.37(2) N10B C11B 1.32(2) C11B H11B 0.9400 C11B C12B 1.28(3) C12B H12B 0.9400 C12B C13B 1.44(3) C13B H13B 0.9400 N14 N15 1.362(6) N14 C18 1.335(8) N15 C16 1.313(7) C16 H16 0.9400 C16 N17 1.357(7) N17 C18 1.303(7) C18 H18 0.9400 N19 C20 1.335(7) N19 C24 1.328(8) C20 C21 1.379(9) C20 N25 1.390(9) C21 H21 0.9400 C21 C22 1.378(11) C22 H22 0.9400 C22 C23 1.404(10) C23 H23 0.9400 C23 C24 1.368(9) C24 N30 1.428(7) N25 N26 1.380(7) N25 C29 1.357(9) N26 C27 1.310(11) C27 H27 0.9400 C27 C28 1.406(11) C28 H28 0.9400 C28 C29 1.361(11) C29 H29 0.9400 N30 N31 1.365(7) N30 C34 1.315(7) N31 C32 1.300(8) C32 H32 0.9400 C32 N33 1.358(7) N33 C34 1.331(7) C34 H34 0.9400 O35 H35A 0.88(2) O35 H35B 0.88(2) B36 F37A 1.324(12) B36 F38A 1.444(12) B36 F39A 1.429(11) B36 F40A 1.376(11) B36 F37B 1.442(12) B36 F38B 1.444(13) B36 F39B 1.292(12) B36 F40B 1.374(13) B36 F37C 1.385(12) B36 F38C 1.323(12) B36 F39C 1.456(13) B36 F40C 1.356(13) B41 F42A 1.340(13) B41 F43A 1.476(13) B41 F44A 1.349(13) B41 F45A 1.384(14) B41 F42B 1.451(13) B41 F43B 1.281(13) B41 F44B 1.482(13) B41 F45B 1.345(12) B41 F42C 1.348(14) B41 F43C 1.479(12) B41 F44C 1.309(14) B41 F45C 1.426(14) C47A N48 1.466(17) C47A H47A 0.9700 C47A H47B 0.9700 C47A H47C 0.9700 N48 O49A 1.226(15) N48 O50A 1.215(17) C47B N48 1.463(17) C47B H47D 0.9700 C47B H47E 0.9700 C47B H47F 0.9700 N48 O49B 1.207(18) N48 O50B 1.215(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 0.88(2) 2.21(6) 2.88(2) 133(6) O35 H35A F45B 0.88(2) 1.82(3) 2.639(14) 156(6) O35 H35A F44C 0.88(2) 1.84(4) 2.675(19) 158(7) O35 H35B F37A 0.88(2) 1.99(5) 2.691(12) 136(6) O35 H35B F37B 0.88(2) 1.97(5) 2.725(13) 142(7) O35 H35B F37C 0.88(2) 2.26(6) 2.924(13) 132(6)