#------------------------------------------------------------------------------ #$Date: 2019-11-07 21:35:52 +0200 (Thu, 07 Nov 2019) $ #$Revision: 223554 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/23/45/7234532.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_7234532 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 101.152(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 19.9190(3) _cell_length_b 15.3887(3) _cell_length_c 18.5909(3) _cell_measurement_reflns_used 10030 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 73.79 _cell_measurement_theta_min 4.13 _cell_volume 5591.02(17) _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 150(2) _diffrn_detector_area_resol_mean 5.3095 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.988 _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 0.0330 _diffrn_reflns_av_unetI/netI 0.0284 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 19986 _diffrn_reflns_theta_full 72.00 _diffrn_reflns_theta_max 74.08 _diffrn_reflns_theta_min 3.66 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 5.280 _exptl_absorpt_correction_T_max 0.913 _exptl_absorpt_correction_T_min 0.089 _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 1.698 _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 0.784 _refine_diff_density_min -0.544 _refine_diff_density_rms 0.073 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 447 _refine_ls_number_reflns 5616 _refine_ls_number_restraints 63 _refine_ls_restrained_S_all 1.087 _refine_ls_R_factor_all 0.0639 _refine_ls_R_factor_gt 0.0620 _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^)+(0.0792P)^2^+19.0126P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1594 _refine_ls_wR_factor_ref 0.1611 _reflns_number_gt 5359 _reflns_number_total 5616 _reflns_threshold_expression >2sigma(I) _cod_data_source_file c9ce01496a2.cif _cod_data_source_block ig12c4fe _cod_depositor_comments 'Adding full bibliography for 7234530--7234535.cif.' _cod_original_cell_volume 5591.02(16) _cod_database_code 7234532 _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 1.38459 with sigma of 0.02 B36-F37B = B36-F38B = B36-F39B = B36-F40B 1.38459 with sigma of 0.02 B36-F37C = B36-F38C = B36-F39C = B36-F40C 1.38459 with sigma of 0.02 F37A-F38A = F37A-F39A = F37A-F40A = F38A-F39A = F38A-F40A = F39A-F40A 2.261035 with sigma of 0.02 F37B-F38B = F37B-F39B = F37B-F40B = F38B-F39B = F38B-F40B = F39B-F40B 2.261035 with sigma of 0.02 F37C-F38C = F37C-F39C = F37C-F40C = F38C-F39C = F38C-F40C = F39C-F40C 2.261035 with sigma of 0.02 B41-F42A = B41-F43A = B41-F44A = B41-F45A 1.38459 with sigma of 0.02 B41-F42B = B41-F43B = B41-F44B = B41-F45B 1.38459 with sigma of 0.02 B41-F42C = B41-F43C = B41-F44C = B41-F45C 1.38459 with sigma of 0.02 F42A-F43A = F42A-F44A = F42A-F45A = F43A-F44A = F43A-F45A = F44A-F45A 2.261035 with sigma of 0.02 F42B-F43B = F42B-F44B = F42B-F45B = F43B-F44B = F43B-F45B = F44B-F45B 2.261035 with sigma of 0.02 F42C-F43C = F42C-F44C = F42C-F45C = F43C-F44C = F43C-F45C = F44C-F45C 2.261035 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(0.62) C4A(0.62) C5A(0.62) H5A(0.62) C6A(0.62) H6A(0.62) C7A(0.62) H7A(0.62) C8A(0.62) N9A(0.62) N10A(0.62) C11A(0.62) H11A(0.62) C12A(0.62) H12A(0.62) C13A(0.62) H13A(0.62) N3B(0.38) C4B(0.38) C5B(0.38) H5B(0.38) C6B(0.38) H6B(0.38) C7B(0.38) H7B(0.38) C8B(0.38) N9B(0.38) N10B(0.38) C11B(0.38) H11B(0.38) C12B(0.38) H12B(0.38) C13B(0.38) H13B(0.38) 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 19.919 15.3887 18.5909 90 101.152 90 ZERR 4 0.0003 0.0003 0.0003 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 REM Highest difference peak 0.892, deepest hole -0.730, 1-sigma level 0.099 GRID fmap 2 acta 144 MERG 2 REM C:/Users/chmmah/Desktop/150%20K/ig12c4fe.hkl WGHT 0.079200 19.012602 FVAR 1.65317 1.38459 FE1 5 0.500000 0.286711 0.250000 10.50000 0.04025 0.02660 = 0.02425 0.00000 0.00881 0.00000 FE2 5 0.500000 0.000000 0.500000 10.50000 0.02634 0.03193 = 0.02270 -0.00074 0.00774 0.00368 PART 1 N3A 6 0.591176 0.296742 0.282195 10.62000 0.03186 C4A 1 0.626361 0.356822 0.252193 10.62000 0.02947 C5A 1 0.696655 0.370588 0.278713 10.62000 0.03939 AFIX 43 H5A 2 0.721607 0.411938 0.256466 10.62000 -1.20000 AFIX 0 C6A 1 0.728369 0.321538 0.338660 10.62000 0.04617 AFIX 43 H6A 2 0.775579 0.330470 0.358119 10.62000 -1.20000 AFIX 0 C7A 1 0.692548 0.259882 0.370624 10.62000 0.03832 AFIX 43 H7A 2 0.713700 0.226525 0.411809 10.62000 -1.20000 AFIX 0 C8A 1 0.623557 0.249810 0.338627 10.62000 0.03074 N9A 6 0.585066 0.401180 0.196501 10.62000 0.03209 N10A 6 0.516574 0.377269 0.180618 10.62000 0.03365 C11A 1 0.487968 0.426807 0.126794 10.62000 0.03842 AFIX 43 H11A 2 0.440835 0.424529 0.104667 10.62000 -1.20000 AFIX 0 C12A 1 0.535637 0.484578 0.105172 10.62000 0.04143 AFIX 43 H12A 2 0.527001 0.526825 0.067245 10.62000 -1.20000 AFIX 0 C13A 1 0.597014 0.466670 0.150592 10.62000 0.03559 AFIX 43 H13A 2 0.639588 0.494342 0.150273 10.62000 -1.20000 AFIX 0 PART 0 PART 2 N3B 6 0.603349 0.287803 0.288512 10.38000 0.02280 C4B 1 0.643460 0.346447 0.263232 10.38000 0.02855 C5B 1 0.710724 0.355037 0.289700 10.38000 0.04775 AFIX 43 H5B 2 0.737053 0.398493 0.271675 10.38000 -1.20000 AFIX 0 C6B 1 0.738350 0.301606 0.340897 10.38000 0.04879 AFIX 43 H6B 2 0.786490 0.304057 0.357676 10.38000 -1.20000 AFIX 0 C7B 1 0.700120 0.239165 0.373428 10.38000 0.03992 AFIX 43 H7B 2 0.720363 0.202224 0.412601 10.38000 -1.20000 AFIX 0 C8B 1 0.633574 0.237406 0.343906 10.38000 0.02995 N9B 6 0.603415 0.394540 0.205231 10.38000 0.03232 N10B 6 0.534556 0.376705 0.187317 10.38000 0.02830 C11B 1 0.508806 0.430949 0.132421 10.38000 0.03690 AFIX 43 H11B 2 0.462146 0.432971 0.108516 10.38000 -1.20000 AFIX 0 C12B 1 0.559429 0.482984 0.115788 10.38000 0.03413 AFIX 43 H12B 2 0.554382 0.526610 0.078978 10.38000 -1.20000 AFIX 0 C13B 1 0.619262 0.459859 0.162821 10.38000 0.03945 AFIX 43 H13B 2 0.663149 0.485038 0.164956 10.38000 -1.20000 AFIX 0 PART 0 N14 6 0.579558 0.188386 0.363764 11.00000 0.02734 0.03731 = 0.02929 -0.00150 0.00553 -0.00321 N15 6 0.511884 0.195934 0.329453 11.00000 0.02931 0.03429 = 0.02686 -0.00271 0.00556 0.00052 C16 1 0.481007 0.138116 0.363846 11.00000 0.02819 0.03540 = 0.02666 -0.00133 0.00801 0.00069 AFIX 43 H16 2 0.433075 0.127972 0.352516 11.00000 -1.20000 AFIX 0 N17 6 0.524373 0.094122 0.417323 11.00000 0.03006 0.03543 = 0.02761 0.00103 0.00803 0.00223 C18 1 0.585178 0.126939 0.415199 11.00000 0.02957 0.03996 = 0.02719 0.00050 0.00465 0.00226 AFIX 43 H18 2 0.626830 0.109381 0.445805 11.00000 -1.20000 AFIX 0 N19 6 0.250042 0.163204 0.551848 11.00000 0.02930 0.03731 = 0.03392 0.00296 0.01084 0.00541 C20 1 0.200588 0.206719 0.575201 11.00000 0.03447 0.03687 = 0.03475 0.00587 0.01311 0.00741 C21 1 0.132216 0.202970 0.541038 11.00000 0.03100 0.04519 = 0.04613 0.00504 0.01431 0.00756 AFIX 43 H21 2 0.098289 0.234916 0.559306 11.00000 -1.20000 AFIX 0 C22 1 0.115348 0.151405 0.479850 11.00000 0.02659 0.05431 = 0.05040 0.00369 0.00800 0.00164 AFIX 43 H22 2 0.069015 0.147542 0.455124 11.00000 -1.20000 AFIX 0 C23 1 0.165579 0.104787 0.453798 11.00000 0.03027 0.05047 = 0.04489 -0.00164 0.00668 0.00028 AFIX 43 H23 2 0.155136 0.068777 0.411606 11.00000 -1.20000 AFIX 0 C24 1 0.231259 0.114047 0.492878 11.00000 0.02795 0.03981 = 0.03747 0.00407 0.01100 0.00427 N25 6 0.223498 0.258127 0.637396 11.00000 0.03160 0.04229 = 0.03755 0.00409 0.01144 0.01035 N26 6 0.179486 0.310938 0.665274 11.00000 0.04069 0.04434 = 0.04200 0.00338 0.01650 0.01580 C27 1 0.218755 0.351888 0.719794 11.00000 0.05063 0.04812 = 0.04218 -0.00291 0.01288 0.01480 AFIX 43 H27 2 0.202319 0.393877 0.749624 11.00000 -1.20000 AFIX 0 C28 1 0.287634 0.326719 0.729056 11.00000 0.04828 0.05408 = 0.04301 -0.00594 0.00678 0.01049 AFIX 43 H28 2 0.325035 0.347069 0.764766 11.00000 -1.20000 AFIX 0 C29 1 0.288993 0.266497 0.675369 11.00000 0.03568 0.05084 = 0.04176 0.00038 0.00875 0.01108 AFIX 43 H29 2 0.328066 0.236243 0.666231 11.00000 -1.20000 AFIX 0 N30 6 0.287711 0.070764 0.471307 11.00000 0.02694 0.03842 = 0.03509 -0.00252 0.00777 0.00161 N31 6 0.279383 0.013145 0.414588 11.00000 0.03356 0.04517 = 0.03830 -0.00922 0.00724 -0.00095 C32 1 0.342281 -0.010939 0.414403 11.00000 0.03288 0.03813 = 0.03383 -0.00513 0.00713 0.00062 AFIX 43 H32 2 0.353565 -0.051682 0.380229 11.00000 -1.20000 AFIX 0 N33 6 0.390648 0.027257 0.467425 11.00000 0.02877 0.03469 = 0.02652 0.00126 0.00710 0.00259 C34 1 0.353849 0.078339 0.502125 11.00000 0.02807 0.03536 = 0.02894 0.00044 0.00723 0.00354 AFIX 43 H34 2 0.371696 0.114696 0.542614 11.00000 -1.20000 AFIX 0 O35 7 0.507218 0.100700 0.577398 11.00000 0.03939 0.04722 = 0.03940 -0.01432 0.01469 -0.00480 H35A 2 0.534356 0.146414 0.581963 11.00000 -1.50000 H35B 2 0.499577 0.092519 0.621723 11.00000 -1.50000 B36 3 0.383470 0.050760 0.718087 11.00000 0.06193 0.05401 = 0.04264 0.01347 0.02460 0.00862 PART 1 F37A 4 0.413553 0.083845 0.666252 10.34000 0.03868 F38A 4 0.310408 0.040302 0.686950 10.34000 0.04134 F39A 4 0.381268 0.109795 0.777416 10.34000 0.03987 F40A 4 0.410512 -0.028502 0.739032 10.34000 0.03470 PART 0 PART 2 F37B 4 0.422608 0.104326 0.677525 10.33000 0.03605 F38B 4 0.334614 0.003850 0.658429 10.33000 0.10063 F39B 4 0.347502 0.088390 0.757677 10.33000 0.06504 F40B 4 0.425921 -0.011267 0.752926 10.33000 0.09224 PART 0 PART 3 F37C 4 0.404572 0.106161 0.667276 10.33000 0.03647 F38C 4 0.316894 0.052633 0.709558 10.33000 0.05475 F39C 4 0.410772 0.094576 0.787889 10.33000 0.05620 F40C 4 0.409922 -0.032019 0.720755 10.33000 0.05676 PART 0 B41 3 0.601447 0.293873 0.550425 11.00000 0.06184 0.04166 = 0.03887 -0.00121 -0.00579 0.00265 PART 1 F42A 4 0.619799 0.363680 0.509866 10.34000 0.11221 F43A 4 0.645192 0.224150 0.541030 10.34000 0.05109 F44A 4 0.604856 0.319760 0.618939 10.34000 0.13021 F45A 4 0.536177 0.270246 0.513268 10.34000 0.08966 PART 0 PART 2 F42B 4 0.546342 0.298853 0.490908 10.33000 0.06686 F43B 4 0.641480 0.358222 0.567079 10.33000 0.09925 F44B 4 0.553484 0.300369 0.607054 10.33000 0.09746 F45B 4 0.613995 0.207615 0.563267 10.33000 0.04690 PART 0 PART 3 F42C 4 0.558356 0.328631 0.497324 10.33000 0.09001 F43C 4 0.642856 0.357858 0.595240 10.33000 0.04618 F44C 4 0.582385 0.243689 0.603274 10.33000 0.09075 F45C 4 0.655807 0.250099 0.521883 10.33000 0.05989 PART 0 O46 7 0.264722 -0.064233 0.574570 10.67000 0.06392 0.07161 = 0.10145 0.01979 0.03197 0.00388 C47 1 0.500000 0.723169 0.250000 10.50000 0.12003 0.05125 = 0.10526 0.00000 0.04290 0.00000 AFIX 33 H47A 2 0.457470 0.744396 0.219480 10.50000 -1.50000 H47B 2 0.539148 0.744396 0.230248 10.50000 -1.50000 H47C 2 0.503382 0.744396 0.300273 10.50000 -1.50000 AFIX 0 N48 6 0.500000 0.628462 0.250000 10.50000 0.04657 0.06025 = 0.04264 0.00000 0.01126 0.00000 O49 7 0.450441 0.590220 0.216382 11.00000 0.05971 0.08859 = 0.07852 -0.02522 0.00926 -0.00924 HKLF 4 REM ig12c4+fe-meno2_a.res in C2/c REM R1 = 0.0620 for 5359 Fo > 4sig(Fo) and 0.0639 for all 5616 data REM 447 parameters refined using 63 restraints END WGHT 0.0792 19.0130 REM Highest difference peak 0.784, deepest hole -0.544, 1-sigma level 0.073 Q1 1 0.6490 0.3015 0.4983 11.00000 0.05 0.78 Q2 1 0.5833 0.3224 0.4753 11.00000 0.05 0.72 Q3 1 0.6080 0.2134 0.6005 11.00000 0.05 0.71 Q4 1 0.5483 0.2615 0.5877 11.00000 0.05 0.70 Q5 1 0.4428 0.0406 0.7890 11.00000 0.05 0.67 Q6 1 0.5370 0.3240 0.5238 11.00000 0.05 0.63 Q7 1 0.3761 -0.0252 0.6890 11.00000 0.05 0.53 Q8 1 0.6213 0.3810 0.5663 11.00000 0.05 0.48 Q9 1 0.6162 0.3802 0.5340 11.00000 0.05 0.47 Q10 1 0.4013 0.1399 0.7823 11.00000 0.05 0.47 Q11 1 0.3287 0.0543 0.7457 11.00000 0.05 0.44 Q12 1 0.6638 0.3329 0.5982 11.00000 0.05 0.39 Q13 1 0.5581 0.3288 0.6168 11.00000 0.05 0.38 Q14 1 0.6347 0.3401 0.6146 11.00000 0.05 0.38 Q15 1 0.3167 0.0046 0.6497 11.00000 0.05 0.35 Q16 1 0.5494 0.4358 0.1507 11.00000 0.05 0.35 Q17 1 0.5384 0.2654 0.4899 11.00000 0.05 0.34 Q18 1 0.7292 0.3189 0.3721 11.00000 0.05 0.34 Q19 1 0.3743 0.0765 0.7788 11.00000 0.05 0.34 Q20 1 0.4515 0.6406 0.1890 11.00000 0.05 0.33 REM The information below was added by Olex2. REM REM R1 = 0.0620 for 5359 Fo > 4sig(Fo) and 0.0639 for all 20460 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.78, deepest hole -0.54 REM Mean Shift 0, Max Shift 0. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0639 REM R1_gt = 0.0620 REM wR_ref = 0.1611 REM GOOF = 1.035 REM Shift_max = 0 REM Shift_mean = 0 REM Reflections_all = 20460 REM Reflections_gt = 5359 REM Parameters = n/a REM Hole = 0.78 REM Peak = -0.54 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 0.28671(4) 0.2500 0.03002(19) Uani 1 2 d S . . Fe2 Fe 0.5000 0.0000 0.5000 0.02659(19) Uani 1 2 d S . . N3A N 0.5912(4) 0.2967(4) 0.2822(4) 0.032(2) Uiso 0.62 1 d P A 1 C4A C 0.6264(4) 0.3568(4) 0.2522(4) 0.0295(16) Uiso 0.62 1 d P A 1 C5A C 0.6967(4) 0.3706(5) 0.2787(4) 0.0394(19) Uiso 0.62 1 d P A 1 H5A H 0.7216 0.4119 0.2565 0.047 Uiso 0.62 1 calc PR A 1 C6A C 0.7284(5) 0.3215(6) 0.3387(5) 0.046(2) Uiso 0.62 1 d P A 1 H6A H 0.7756 0.3305 0.3581 0.055 Uiso 0.62 1 calc PR A 1 C7A C 0.6925(4) 0.2599(6) 0.3706(4) 0.038(2) Uiso 0.62 1 d P A 1 H7A H 0.7137 0.2265 0.4118 0.046 Uiso 0.62 1 calc PR A 1 C8A C 0.6236(4) 0.2498(6) 0.3386(4) 0.031(2) Uiso 0.62 1 d P A 1 N9A N 0.5851(4) 0.4012(4) 0.1965(3) 0.0321(15) Uiso 0.62 1 d P A 1 N10A N 0.5166(4) 0.3773(4) 0.1806(3) 0.0336(17) Uiso 0.62 1 d P A 1 C11A C 0.4880(5) 0.4268(5) 0.1268(4) 0.0384(18) Uiso 0.62 1 d P A 1 H11A H 0.4408 0.4245 0.1047 0.046 Uiso 0.62 1 calc PR A 1 C12A C 0.5356(4) 0.4846(5) 0.1052(4) 0.0414(17) Uiso 0.62 1 d P A 1 H12A H 0.5270 0.5268 0.0672 0.050 Uiso 0.62 1 calc PR A 1 C13A C 0.5970(4) 0.4667(4) 0.1506(4) 0.0356(15) Uiso 0.62 1 d P A 1 H13A H 0.6396 0.4943 0.1503 0.043 Uiso 0.62 1 calc PR A 1 N3B N 0.6033(5) 0.2878(6) 0.2885(5) 0.023(3) Uiso 0.38 1 d P A 2 C4B C 0.6435(6) 0.3464(7) 0.2632(6) 0.029(3) Uiso 0.38 1 d P A 2 C5B C 0.7107(7) 0.3550(10) 0.2897(8) 0.048(4) Uiso 0.38 1 d P A 2 H5B H 0.7371 0.3985 0.2717 0.057 Uiso 0.38 1 calc PR A 2 C6B C 0.7383(8) 0.3016(10) 0.3409(8) 0.049(4) Uiso 0.38 1 d P A 2 H6B H 0.7865 0.3041 0.3577 0.059 Uiso 0.38 1 calc PR A 2 C7B C 0.7001(7) 0.2392(10) 0.3734(7) 0.040(3) Uiso 0.38 1 d P A 2 H7B H 0.7204 0.2022 0.4126 0.048 Uiso 0.38 1 calc PR A 2 C8B C 0.6336(7) 0.2374(9) 0.3439(7) 0.030(4) Uiso 0.38 1 d P A 2 N9B N 0.6034(6) 0.3945(6) 0.2052(5) 0.032(3) Uiso 0.38 1 d P A 2 N10B N 0.5346(6) 0.3767(6) 0.1873(5) 0.028(2) Uiso 0.38 1 d P A 2 C11B C 0.5088(7) 0.4309(8) 0.1324(6) 0.037(3) Uiso 0.38 1 d P A 2 H11B H 0.4621 0.4330 0.1085 0.044 Uiso 0.38 1 calc PR A 2 C12B C 0.5594(7) 0.4830(7) 0.1158(6) 0.034(2) Uiso 0.38 1 d P A 2 H12B H 0.5544 0.5266 0.0790 0.041 Uiso 0.38 1 calc PR A 2 C13B C 0.6193(7) 0.4599(7) 0.1628(6) 0.039(3) Uiso 0.38 1 d P A 2 H13B H 0.6631 0.4850 0.1650 0.047 Uiso 0.38 1 calc PR A 2 N14 N 0.57956(13) 0.18839(19) 0.36376(14) 0.0313(6) Uani 1 1 d . . . N15 N 0.51188(13) 0.19593(18) 0.32945(14) 0.0301(5) Uani 1 1 d . A . C16 C 0.48101(16) 0.1381(2) 0.36385(17) 0.0297(6) Uani 1 1 d . . . H16 H 0.4331 0.1280 0.3525 0.036 Uiso 1 1 calc R A . N17 N 0.52437(14) 0.09412(18) 0.41732(14) 0.0307(6) Uani 1 1 d . A . C18 C 0.58518(17) 0.1269(2) 0.41520(17) 0.0324(7) Uani 1 1 d . A . H18 H 0.6268 0.1094 0.4458 0.039 Uiso 1 1 calc R . . N19 N 0.25004(14) 0.16320(19) 0.55185(15) 0.0329(6) Uani 1 1 d . . . C20 C 0.20059(17) 0.2067(2) 0.57520(19) 0.0345(7) Uani 1 1 d . . . C21 C 0.13222(18) 0.2030(2) 0.5410(2) 0.0399(8) Uani 1 1 d . . . H21 H 0.0983 0.2349 0.5593 0.048 Uiso 1 1 calc R . . C22 C 0.11535(18) 0.1514(3) 0.4799(2) 0.0437(8) Uani 1 1 d . . . H22 H 0.0690 0.1475 0.4551 0.052 Uiso 1 1 calc R . . C23 C 0.16558(18) 0.1048(3) 0.4538(2) 0.0420(8) Uani 1 1 d . . . H23 H 0.1551 0.0688 0.4116 0.050 Uiso 1 1 calc R . . C24 C 0.23126(16) 0.1140(2) 0.49288(19) 0.0345(7) Uani 1 1 d . . . N25 N 0.22350(14) 0.2581(2) 0.63740(16) 0.0365(6) Uani 1 1 d . . . N26 N 0.17949(16) 0.3109(2) 0.66527(17) 0.0412(7) Uani 1 1 d . . . C27 C 0.2188(2) 0.3519(3) 0.7198(2) 0.0465(9) Uani 1 1 d . . . H27 H 0.2023 0.3939 0.7496 0.056 Uiso 1 1 calc R . . C28 C 0.2876(2) 0.3267(3) 0.7291(2) 0.0487(9) Uani 1 1 d . . . H28 H 0.3250 0.3471 0.7648 0.058 Uiso 1 1 calc R . . C29 C 0.28899(19) 0.2665(3) 0.6754(2) 0.0426(8) Uani 1 1 d . . . H29 H 0.3281 0.2362 0.6662 0.051 Uiso 1 1 calc R . . N30 N 0.28771(14) 0.07076(19) 0.47131(15) 0.0332(6) Uani 1 1 d . . . N31 N 0.27938(15) 0.0131(2) 0.41459(17) 0.0390(7) Uani 1 1 d . . . C32 C 0.34228(17) -0.0109(2) 0.41440(19) 0.0349(7) Uani 1 1 d . . . H32 H 0.3536 -0.0517 0.3802 0.042 Uiso 1 1 calc R . . N33 N 0.39065(13) 0.02726(18) 0.46743(14) 0.0298(5) Uani 1 1 d . . . C34 C 0.35385(16) 0.0783(2) 0.50212(17) 0.0306(6) Uani 1 1 d . . . H34 H 0.3717 0.1147 0.5426 0.037 Uiso 1 1 calc R . . O35 O 0.50722(13) 0.10070(18) 0.57740(14) 0.0411(6) Uani 1 1 d D . . H35A H 0.534(2) 0.146(2) 0.582(2) 0.062 Uiso 1 1 d D . . H35B H 0.500(2) 0.093(3) 0.6217(15) 0.062 Uiso 1 1 d D . . B36 B 0.3835(3) 0.0508(3) 0.7181(2) 0.0509(11) Uani 1 1 d D . . F37A F 0.4136(5) 0.0838(6) 0.6663(5) 0.039(2) Uiso 0.34 1 d PD B 1 F38A F 0.3104(3) 0.0403(5) 0.6869(5) 0.0413(18) Uiso 0.34 1 d PD B 1 F39A F 0.3813(4) 0.1098(4) 0.7774(3) 0.0399(14) Uiso 0.34 1 d PD B 1 F40A F 0.4105(5) -0.0285(5) 0.7390(6) 0.035(2) Uiso 0.34 1 d PD B 1 F37B F 0.4226(5) 0.1043(7) 0.6775(4) 0.036(2) Uiso 0.33 1 d PD B 2 F38B F 0.3346(6) 0.0039(8) 0.6584(6) 0.101(4) Uiso 0.33 1 d PD B 2 F39B F 0.3475(5) 0.0884(6) 0.7577(5) 0.065(2) Uiso 0.33 1 d PD B 2 F40B F 0.4259(7) -0.0113(8) 0.7529(7) 0.092(5) Uiso 0.33 1 d PD B 2 F37C F 0.4046(5) 0.1062(7) 0.6673(5) 0.036(2) Uiso 0.33 1 d PD B 3 F38C F 0.3169(4) 0.0526(6) 0.7096(6) 0.055(2) Uiso 0.33 1 d PD B 3 F39C F 0.4108(5) 0.0946(5) 0.7879(4) 0.056(2) Uiso 0.33 1 d PD B 3 F40C F 0.4099(6) -0.0320(6) 0.7208(6) 0.057(4) Uiso 0.33 1 d PD B 3 B41 B 0.6014(3) 0.2939(3) 0.5504(2) 0.0495(11) Uani 1 1 d D . . F42A F 0.6198(7) 0.3637(7) 0.5099(7) 0.112(4) Uiso 0.34 1 d PD C 1 F43A F 0.6452(4) 0.2241(5) 0.5410(5) 0.0511(18) Uiso 0.34 1 d PD C 1 F44A F 0.6049(8) 0.3198(10) 0.6189(6) 0.130(5) Uiso 0.34 1 d PD C 1 F45A F 0.5362(5) 0.2702(8) 0.5133(7) 0.090(3) Uiso 0.34 1 d PD C 1 F42B F 0.5463(5) 0.2989(8) 0.4909(5) 0.067(3) Uiso 0.33 1 d PD C 2 F43B F 0.6415(6) 0.3582(8) 0.5671(9) 0.099(4) Uiso 0.33 1 d PD C 2 F44B F 0.5535(6) 0.3004(8) 0.6071(6) 0.097(3) Uiso 0.33 1 d PD C 2 F45B F 0.6140(4) 0.2076(4) 0.5633(4) 0.0469(15) Uiso 0.33 1 d PD C 2 F42C F 0.5584(6) 0.3286(9) 0.4973(6) 0.090(4) Uiso 0.33 1 d PD C 3 F43C F 0.6429(4) 0.3579(5) 0.5952(5) 0.0462(18) Uiso 0.33 1 d PD C 3 F44C F 0.5824(6) 0.2437(7) 0.6033(6) 0.091(3) Uiso 0.33 1 d PD C 3 F45C F 0.6558(4) 0.2501(6) 0.5219(5) 0.060(2) Uiso 0.33 1 d PD C 3 O46 O 0.2647(3) -0.0642(4) 0.5746(4) 0.0769(16) Uani 0.67 1 d P . . C47 C 0.5000 0.7232(5) 0.2500 0.089(3) Uani 1 2 d S . . H47A H 0.4575 0.7444 0.2195 0.134 Uiso 0.50 1 calc PR . . H47B H 0.5391 0.7444 0.2302 0.134 Uiso 0.50 1 calc PR . . H47C H 0.5034 0.7444 0.3003 0.134 Uiso 0.50 1 calc PR . . N48 N 0.5000 0.6285(4) 0.2500 0.0495(11) Uani 1 2 d S . . O49 O 0.45044(19) 0.5902(3) 0.2164(2) 0.0762(11) 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 0.0402(4) 0.0266(4) 0.0243(3) 0.000 0.0088(3) 0.000 Fe2 0.0263(3) 0.0319(4) 0.0227(3) -0.0007(3) 0.0077(2) 0.0037(3) N14 0.0273(12) 0.0373(14) 0.0293(13) -0.0015(11) 0.0055(10) -0.0032(11) N15 0.0293(13) 0.0343(14) 0.0269(12) -0.0027(11) 0.0056(10) 0.0005(11) C16 0.0282(14) 0.0354(16) 0.0267(14) -0.0013(12) 0.0080(11) 0.0007(12) N17 0.0301(13) 0.0354(14) 0.0276(13) 0.0010(11) 0.0080(10) 0.0022(11) C18 0.0296(15) 0.0400(17) 0.0272(15) 0.0005(13) 0.0047(12) 0.0023(13) N19 0.0293(13) 0.0373(14) 0.0339(14) 0.0030(11) 0.0108(11) 0.0054(11) C20 0.0345(16) 0.0369(17) 0.0347(17) 0.0059(13) 0.0131(13) 0.0074(13) C21 0.0310(16) 0.0452(19) 0.046(2) 0.0050(16) 0.0143(15) 0.0076(14) C22 0.0266(16) 0.054(2) 0.050(2) 0.0037(17) 0.0080(15) 0.0016(15) C23 0.0303(16) 0.050(2) 0.045(2) -0.0016(16) 0.0067(14) 0.0003(15) C24 0.0279(15) 0.0398(18) 0.0375(17) 0.0041(14) 0.0110(13) 0.0043(13) N25 0.0316(14) 0.0423(16) 0.0376(15) 0.0041(12) 0.0114(12) 0.0104(12) N26 0.0407(16) 0.0443(16) 0.0420(16) 0.0034(13) 0.0165(13) 0.0158(13) C27 0.051(2) 0.048(2) 0.042(2) -0.0029(17) 0.0129(17) 0.0148(17) C28 0.048(2) 0.054(2) 0.043(2) -0.0059(17) 0.0068(17) 0.0105(18) C29 0.0357(18) 0.051(2) 0.0418(19) 0.0004(16) 0.0087(15) 0.0111(16) N30 0.0269(13) 0.0384(15) 0.0351(14) -0.0025(12) 0.0078(11) 0.0016(11) N31 0.0336(15) 0.0452(16) 0.0383(16) -0.0092(13) 0.0072(12) -0.0010(12) C32 0.0329(16) 0.0381(17) 0.0338(16) -0.0051(13) 0.0071(13) 0.0006(13) N33 0.0288(13) 0.0347(14) 0.0265(12) 0.0013(10) 0.0071(10) 0.0026(11) C34 0.0281(15) 0.0354(16) 0.0289(15) 0.0004(12) 0.0072(12) 0.0035(12) O35 0.0394(13) 0.0472(14) 0.0394(13) -0.0143(11) 0.0147(11) -0.0048(11) B36 0.062(3) 0.054(3) 0.043(2) 0.013(2) 0.025(2) 0.009(2) B41 0.062(3) 0.042(2) 0.039(2) -0.0012(18) -0.006(2) 0.003(2) O46 0.064(3) 0.072(3) 0.101(4) 0.020(3) 0.032(3) 0.004(3) C47 0.120(8) 0.051(4) 0.105(7) 0.000 0.043(6) 0.000 N48 0.047(3) 0.060(3) 0.043(2) 0.000 0.011(2) 0.000 O49 0.060(2) 0.089(3) 0.079(2) -0.025(2) 0.0093(18) -0.0092(19) 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 174.5(3) 2_655 . N3A Fe1 N10A 82.6(3) . . N3A Fe1 N10A 90.4(3) . 2_655 N3A Fe1 N15 81.3(2) . . N3A Fe1 N15 105.7(2) . 2_655 N10A Fe1 N10A 89.9(4) 2_655 . N10A Fe1 N10B 90.7(2) 2_655 . N10A Fe1 N15 163.8(2) . . N10A Fe1 N15 91.22(19) . 2_655 N3B Fe1 N3B 179.1(6) 2_655 . N10A Fe1 N3B 92.9(3) 2_655 . N10A Fe1 N3B 86.5(3) . . N10B Fe1 N3B 103.0(4) . 2_655 N10B Fe1 N3B 76.3(4) . . N10B Fe1 N10B 93.2(5) . 2_655 N15 Fe1 N3B 77.4(3) . . N15 Fe1 N3B 103.3(3) . 2_655 N15 Fe1 N10B 153.7(3) . . N15 Fe1 N10B 93.3(3) . 2_655 N15 Fe1 N15 92.14(15) 2_655 . N17 Fe2 N17 180.00 5_656 . N33 Fe2 N17 88.71(10) . 5_656 N33 Fe2 N17 91.29(10) . . N33 Fe2 N33 180.00 . 5_656 O35 Fe2 N17 89.87(10) . . O35 Fe2 N17 90.13(10) . 5_656 O35 Fe2 N33 88.90(10) . . O35 Fe2 N33 91.10(10) . 5_656 O35 Fe2 O35 180.00 5_656 . C4A N3A Fe1 119.5(6) . . C8A N3A Fe1 121.1(6) . . C8A N3A C4A 119.2(7) . . N3A C4A C5A 121.4(7) . . N3A C4A N9A 111.7(6) . . N9A C4A C5A 126.8(6) . . C4A C5A H5A 121.1 . . C6A C5A C4A 117.7(7) . . C6A C5A H5A 121.1 . . C5A C6A H6A 119.3 . . C7A C6A C5A 121.5(8) . . C7A C6A H6A 119.3 . . C6A C7A H7A 122.0 . . C6A C7A C8A 116.0(8) . . C8A C7A H7A 122.0 . . N3A C8A C7A 124.2(8) . . N3A C8A N14 112.5(6) . . C7A C8A N14 123.4(7) . . C4A N9A N10A 116.7(6) . . C13A N9A C4A 133.2(7) . . C13A N9A N10A 110.1(6) . . N9A N10A Fe1 109.3(5) . . C11A N10A Fe1 144.7(6) . . C11A N10A N9A 106.0(6) . . N10A C11A H11A 124.2 . . N10A C11A C12A 111.7(8) . . C12A C11A H11A 124.2 . . C11A C12A H12A 127.3 . . C13A C12A C11A 105.4(6) . . C13A C12A H12A 127.3 . . N9A C13A C12A 106.8(6) . . N9A C13A H13A 126.6 . . C12A C13A H13A 126.6 . . C4B N3B Fe1 120.5(9) . . C8B N3B Fe1 122.6(8) . . C8B N3B C4B 116.6(11) . . N3B C4B N9B 109.3(10) . . C5B C4B N3B 123.7(12) . . C5B C4B N9B 127.0(11) . . C4B C5B H5B 121.4 . . C6B C5B C4B 117.3(14) . . C6B C5B H5B 121.4 . . C5B C6B H6B 118.3 . . C5B C6B C7B 123.4(14) . . C7B C6B H6B 118.3 . . C6B C7B H7B 123.0 . . C8B C7B C6B 114.1(13) . . C8B C7B H7B 123.0 . . N3B C8B N14 104.9(10) . . C7B C8B N3B 124.7(12) . . C7B C8B N14 130.3(12) . . N10B N9B C4B 117.9(9) . . C13B N9B C4B 132.1(11) . . C13B N9B N10B 110.0(11) . . N9B N10B Fe1 115.7(7) . . C11B N10B Fe1 138.1(10) . . C11B N10B N9B 106.1(10) . . N10B C11B H11B 124.9 . . N10B C11B C12B 110.2(12) . . C12B C11B H11B 124.9 . . C11B C12B H12B 126.6 . . C11B C12B C13B 106.8(11) . . C13B C12B H12B 126.6 . . N9B C13B C12B 106.9(11) . . N9B C13B H13B 126.6 . . C12B C13B H13B 126.6 . . N15 N14 C8A 113.5(4) . . N15 N14 C8B 123.8(6) . . C18 N14 C8A 137.1(4) . . C18 N14 C8B 126.9(6) . . C18 N14 N15 109.3(3) . . N14 N15 Fe1 111.3(2) . . C16 N15 Fe1 145.7(2) . . C16 N15 N14 103.0(3) . . N15 C16 H16 123.2 . . N15 C16 N17 113.6(3) . . N17 C16 H16 123.2 . . C16 N17 Fe2 129.2(2) . . C18 N17 Fe2 126.3(2) . . C18 N17 C16 104.1(3) . . N14 C18 H18 125.0 . . N17 C18 N14 110.0(3) . . N17 C18 H18 125.0 . . C24 N19 C20 116.7(3) . . N19 C20 C21 123.5(3) . . N19 C20 N25 114.2(3) . . C21 C20 N25 122.3(3) . . C20 C21 H21 121.2 . . C22 C21 C20 117.6(3) . . C22 C21 H21 121.2 . . C21 C22 H22 119.7 . . C21 C22 C23 120.6(3) . . C23 C22 H22 119.7 . . C22 C23 H23 122.0 . . C24 C23 C22 115.9(4) . . C24 C23 H23 122.0 . . N19 C24 C23 125.7(3) . . N19 C24 N30 112.7(3) . . C23 C24 N30 121.5(3) . . N26 N25 C20 121.1(3) . . C29 N25 C20 127.3(3) . . C29 N25 N26 111.5(3) . . C27 N26 N25 104.3(3) . . N26 C27 H27 123.7 . . N26 C27 C28 112.6(3) . . C28 C27 H27 123.7 . . C27 C28 H28 127.6 . . C29 C28 C27 104.7(4) . . C29 C28 H28 127.6 . . N25 C29 C28 106.9(3) . . N25 C29 H29 126.6 . . C28 C29 H29 126.6 . . N31 N30 C24 122.4(3) . . C34 N30 C24 127.1(3) . . C34 N30 N31 110.5(3) . . C32 N31 N30 102.3(3) . . N31 C32 H32 122.7 . . N31 C32 N33 114.7(3) . . N33 C32 H32 122.7 . . C32 N33 Fe2 129.9(2) . . C34 N33 Fe2 126.5(2) . . C34 N33 C32 103.1(3) . . N30 C34 H34 125.3 . . N33 C34 N30 109.4(3) . . N33 C34 H34 125.3 . . Fe2 O35 H35A 128(3) . . Fe2 O35 H35B 123(3) . . H35A O35 H35B 104(3) . . F37A B36 F38A 107.9(6) . . F37A B36 F39A 113.5(6) . . F37A B36 F40A 110.0(6) . . F39A B36 F38A 101.4(5) . . F40A B36 F38A 108.8(6) . . F40A B36 F39A 114.6(7) . . F37B B36 F38B 103.0(6) . . F39B B36 F37B 117.9(7) . . F39B B36 F38B 106.8(7) . . F39B B36 F40B 114.6(8) . . F40B B36 F37B 107.6(8) . . F40B B36 F38B 105.6(8) . . F37C B36 F39C 102.0(6) . . F38C B36 F37C 109.6(6) . . F38C B36 F39C 106.9(6) . . F38C B36 F40C 113.4(7) . . F40C B36 F37C 115.2(7) . . F40C B36 F39C 108.6(6) . . F42A B41 F43A 106.5(7) . . F44A B41 F42A 108.5(9) . . F44A B41 F43A 115.4(8) . . F44A B41 F45A 115.1(9) . . F45A B41 F42A 104.4(8) . . F45A B41 F43A 106.1(6) . . F42B B41 F44B 92.4(7) . . F43B B41 F42B 120.5(9) . . F43B B41 F44B 102.9(8) . . F43B B41 F45B 129.1(8) . . F45B B41 F42B 106.3(7) . . F45B B41 F44B 93.4(6) . . F42C B41 F43C 112.3(8) . . F42C B41 F44C 123.4(8) . . F42C B41 F45C 110.1(7) . . F43C B41 F45C 98.3(5) . . F44C B41 F43C 100.3(6) . . F44C B41 F45C 109.3(7) . . N48 C47 H47A 109.5 . . N48 C47 H47B 109.5 . . N48 C47 H47C 109.5 . . O49 N48 C47 119.0(3) . . O49 N48 O49 122.0(6) . 2_655 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Fe1 N3A 1.806(7) Fe1 N10A 1.970(6) Fe1 N3B 2.045(11) Fe1 N10B 2.015(9) Fe1 N15 2.013(3) Fe2 N17 2.233(3) Fe2 N33 2.186(3) Fe2 O35 2.101(2) N3A C4A 1.345(9) N3A C8A 1.333(11) C4A C5A 1.408(10) C4A N9A 1.373(10) C5A H5A 0.9500 C5A C6A 1.392(12) C6A H6A 0.9500 C6A C7A 1.388(12) C7A H7A 0.9500 C7A C8A 1.396(11) C8A N14 1.428(8) N9A N10A 1.389(9) N9A C13A 1.371(9) N10A C11A 1.299(10) C11A H11A 0.9500 C11A C12A 1.415(11) C12A H12A 0.9500 C12A C13A 1.373(11) C13A H13A 0.9500 N3B C4B 1.349(14) N3B C8B 1.336(17) C4B C5B 1.342(18) C4B N9B 1.419(15) C5B H5B 0.9500 C5B C6B 1.30(2) C6B H6B 0.9500 C6B C7B 1.43(2) C7B H7B 0.9500 C7B C8B 1.333(19) C8B N14 1.420(13) N9B N10B 1.375(14) N9B C13B 1.352(15) N10B C11B 1.341(15) C11B H11B 0.9500 C11B C12B 1.369(17) C12B H12B 0.9500 C12B C13B 1.381(16) C13B H13B 0.9500 N14 N15 1.380(4) N14 C18 1.334(4) N15 C16 1.316(4) C16 H16 0.9500 C16 N17 1.364(4) N17 C18 1.320(4) C18 H18 0.9500 N19 C20 1.331(4) N19 C24 1.325(5) C20 C21 1.388(5) C20 N25 1.402(5) C21 H21 0.9500 C21 C22 1.374(6) C22 H22 0.9500 C22 C23 1.392(5) C23 H23 0.9500 C23 C24 1.376(5) C24 N30 1.429(4) N25 N26 1.369(4) N25 C29 1.364(5) N26 C27 1.315(5) C27 H27 0.9500 C27 C28 1.404(6) C28 H28 0.9500 C28 C29 1.366(6) C29 H29 0.9500 N30 N31 1.363(4) N30 C34 1.336(4) N31 C32 1.307(5) C32 H32 0.9500 C32 N33 1.370(4) N33 C34 1.324(4) C34 H34 0.9500 O35 H35A 0.88(2) O35 H35B 0.88(2) B36 F37A 1.331(8) B36 F38A 1.467(8) B36 F39A 1.436(7) B36 F40A 1.360(8) B36 F37B 1.443(8) B36 F38B 1.510(10) B36 F39B 1.263(9) B36 F40B 1.354(10) B36 F37C 1.396(8) B36 F38C 1.305(9) B36 F39C 1.470(8) B36 F40C 1.376(9) B41 F42A 1.401(11) B41 F43A 1.414(8) B41 F44A 1.324(11) B41 F45A 1.397(10) B41 F42B 1.402(9) B41 F43B 1.272(11) B41 F44B 1.556(10) B41 F45B 1.363(8) B41 F42C 1.292(10) B41 F43C 1.442(8) B41 F44C 1.360(10) B41 F45C 1.459(9) C47 H47A 0.9800 C47 H47B 0.9800 C47 H47C 0.9800 C47 N48 1.457(9) N48 O49 1.214(4) 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) 2.30(4) 2.971(13) 133(4) O35 H35A F45B 0.88(2) 1.93(3) 2.742(8) 152(4) O35 H35A F44C 0.88(2) 1.78(2) 2.653(11) 171(4) O35 H35B F37A 0.88(2) 2.05(4) 2.733(8) 135(4) O35 H35B F37B 0.88(2) 2.02(4) 2.743(8) 139(5) O35 H35B F37C 0.88(2) 2.23(4) 2.881(8) 131(4)