#------------------------------------------------------------------------------ #$Date: 2025-02-07 04:48:03 +0200 (Fri, 07 Feb 2025) $ #$Revision: 297630 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/38/1573863.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_1573863 loop_ _publ_author_name 'Valverde-Mu\~noz, Francisco Javier' 'Torres Ram\'irez, Ricardo Guillermo' 'Trzop, Elzbieta' 'Bataille, Thierry' 'Daro, Nathalie' 'Denux, Dominique' 'Guionneau, Philippe' 'Cailleau, Herv\'e' 'Chastanet, Guillaume' 'Le Guennic, Boris' 'Collet, Eric' _publ_section_title ; Stabilizing low symmetry-based functions of materials at room temperature through isosymmetric electronic bistability ; _journal_name_full 'Materials Horizons' _journal_paper_doi 10.1039/D4MH01318B _journal_year 2025 _chemical_formula_moiety 'C42 H28 Fe N6 S2' _chemical_formula_sum 'C42 H28 Fe N6 S2' _chemical_formula_weight 736.67 _chemical_melting_point ? _space_group_crystal_system orthorhombic _space_group_IT_number 56 _space_group_name_Hall '-P 2ab 2ac' _space_group_name_H-M_alt 'P c c n' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_method ; Olex2 1.5-ac5-024 (compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498) ; _audit_update_record ; 2023-11-22 deposited with the CCDC. 2025-02-06 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.2537(4) _cell_length_b 14.2713(5) _cell_length_c 17.4543(5) _cell_measurement_reflns_used 3981 _cell_measurement_temperature 91(5) _cell_measurement_theta_max 27.2590 _cell_measurement_theta_min 3.1270 _cell_volume 3550.53(19) _computing_cell_refinement 'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)' _computing_data_collection 'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)' _computing_data_reduction 'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)' _computing_molecular_graphics 'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2014/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 91(5) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.1852 _diffrn_detector_type Sapphire3 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -116.00 -91.00 1.00 90.00 -- -33.50 178.00 120.00 25 2 \w 60.00 111.00 1.00 90.00 -- 35.69 178.00 0.00 51 3 \w 60.00 87.00 1.00 90.00 -- 35.69 178.00 150.00 27 4 \w 64.00 97.00 1.00 90.00 -- 35.69 178.00 -60.00 33 5 \w 17.00 90.00 1.00 90.00 -- 35.69 57.00 0.00 73 6 \w 40.00 75.00 1.00 90.00 -- 35.69 -99.00 0.00 35 7 \w 5.00 71.00 1.00 90.00 -- 35.69 -99.00 120.00 66 8 \w -4.00 91.00 1.00 90.00 -- 35.69 19.00-120.00 95 9 \w -6.00 101.00 1.00 90.00 -- 35.69 0.00 150.00 107 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0378347000 _diffrn_orient_matrix_UB_12 -0.0287011000 _diffrn_orient_matrix_UB_13 -0.0122376000 _diffrn_orient_matrix_UB_21 0.0295323000 _diffrn_orient_matrix_UB_22 -0.0398753000 _diffrn_orient_matrix_UB_23 0.0016727000 _diffrn_orient_matrix_UB_31 -0.0131886000 _diffrn_orient_matrix_UB_32 -0.0073354000 _diffrn_orient_matrix_UB_33 0.0387276000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1006 _diffrn_reflns_av_unetI/netI 0.0572 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 28015 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.999 _diffrn_reflns_theta_min 3.400 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.583 _exptl_absorpt_correction_T_max 0.972 _exptl_absorpt_correction_T_min 0.936 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro 1.171.41.115a (Rigaku Oxford Diffraction, 2021) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour black _exptl_crystal_colour_primary black _exptl_crystal_density_diffrn 1.378 _exptl_crystal_density_meas ? _exptl_crystal_density_method none _exptl_crystal_description prism _exptl_crystal_F_000 1520 _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.07 _refine_diff_density_max 0.316 _refine_diff_density_min -0.327 _refine_diff_density_rms 0.065 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 231 _refine_ls_number_reflns 3489 _refine_ls_number_restraints 7 _refine_ls_restrained_S_all 1.049 _refine_ls_R_factor_all 0.0726 _refine_ls_R_factor_gt 0.0425 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0310P)^2^+1.1675P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0793 _refine_ls_wR_factor_ref 0.0891 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2553 _reflns_number_total 3489 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4mh01318b3.cif _cod_data_source_block Fe_PM_PEA_NCS_90K _cod_depositor_comments ; The following automatic conversions were performed: data item '_chemical_melting_point' value 'not measured' was changed to '?' -- the value is undefined or not given. data item '_exptl_crystal_density_meas' value 'not measured' was changed to '?' -- the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas ; _cod_database_code 1573863 _shelxl_version_number 2014-3 _chemical_oxdiff_formula 'C42 H28 Fe1 N6 S2' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.960 _shelx_estimated_absorpt_t_min 0.897 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups 2. Restrained distances C9-C10 = C20-C19 = C21-C20 = C18-C17 1.39 with sigma of 0.01 C9-C10 1.39 with sigma of 0.005 C20-C19 = C21-C20 1.39 with sigma of 0.005 3.a Aromatic/amide H refined with riding coordinates: C7(H7), C13(H13), C9(H9), C2(H2), C5(H5), C21(H21), C12(H12), C19(H19), C10(H10), C3(H3), C20(H20), C4(H4), C18(H18), C17(H17) ; _shelx_res_file ; TITL Fe_PM_PEA_NCS_90K in Pccn CELL 0.71073 14.2537 14.2713 17.4543 90 90 90 ZERR 4 0.0004 0.0005 0.0005 0 0 0 LATT 1 SYMM 0.5-X,0.5-Y,+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,-Y,0.5-Z SFAC C H Fe N S UNIT 168 112 4 24 8 DFIX 1.39 0.01 C9 C10 C20 C19 C21 C20 C18 C17 DFIX 1.39 0.005 C9 C10 DFIX 1.39 0.005 C20 C19 C21 C20 L.S. 10 PLAN 10 SIZE 0.07 0.13 0.19 TEMP -182 CONF LIST 4 MORE -1 BOND $H fmap 2 53 acta OMIT -4 52 OMIT 1 1 2 WGHT 0.031000 1.167500 FVAR 0.22290 FE1 3 0.750000 0.750000 0.548976 10.50000 0.01297 0.01699 = 0.01230 0.00000 0.00000 0.00142 S1 5 0.778546 0.514663 0.362480 11.00000 0.02263 0.02401 = 0.01844 -0.00489 -0.00343 0.00369 N2 4 0.872083 0.812662 0.553117 11.00000 0.01372 0.01687 = 0.01382 0.00286 -0.00041 0.00174 N3 4 0.725094 0.839421 0.632048 11.00000 0.01337 0.01803 = 0.01384 0.00319 0.00003 0.00293 N1 4 0.785530 0.659964 0.470002 11.00000 0.01366 0.02152 = 0.01844 -0.00080 -0.00099 0.00065 C7 1 0.796398 0.887063 0.654987 11.00000 0.02108 0.01635 = 0.01367 -0.00009 -0.00023 -0.00043 AFIX 43 H7 2 0.793401 0.926805 0.698582 11.00000 -1.20000 AFIX 0 C8 1 0.638969 0.844825 0.673269 11.00000 0.01619 0.01419 = 0.01785 -0.00312 0.00490 0.00192 C13 1 0.636121 0.834106 0.752199 11.00000 0.01957 0.02353 = 0.01780 -0.00166 -0.00230 0.00141 AFIX 43 H13 2 0.692333 0.823420 0.780106 11.00000 -1.20000 AFIX 0 C6 1 0.881510 0.876560 0.610456 11.00000 0.01748 0.01869 = 0.01585 0.00125 -0.00155 0.00117 C9 1 0.556445 0.859106 0.632595 11.00000 0.01965 0.02147 = 0.01408 0.00097 0.00269 0.00570 AFIX 43 H9 2 0.558412 0.866493 0.578527 11.00000 -1.20000 AFIX 0 C15 1 0.303561 0.870087 0.816884 11.00000 0.02236 0.02048 = 0.02038 -0.00085 0.00155 -0.00020 C11 1 0.468107 0.853270 0.749798 11.00000 0.01926 0.01593 = 0.02134 -0.00268 0.00616 0.00006 C2 1 0.944962 0.800764 0.505718 11.00000 0.01951 0.02237 = 0.01789 0.00322 0.00231 0.00300 AFIX 43 H2 2 0.938718 0.757949 0.464354 11.00000 -1.20000 AFIX 0 C1 1 0.781700 0.599470 0.425534 11.00000 0.01167 0.02287 = 0.01653 0.00395 -0.00031 0.00175 C16 1 0.211768 0.883133 0.849289 11.00000 0.01872 0.01713 = 0.02168 0.00153 0.00617 0.00030 C5 1 0.963836 0.925648 0.622878 11.00000 0.02226 0.02579 = 0.02077 0.00034 -0.00170 -0.00351 AFIX 43 H5 2 0.968678 0.968881 0.664075 11.00000 -1.20000 AFIX 0 C21 1 0.200144 0.900770 0.927174 11.00000 0.01605 0.03095 = 0.02196 0.00195 -0.00112 -0.00109 AFIX 43 H21 2 0.253487 0.903847 0.959708 11.00000 -1.20000 AFIX 0 C12 1 0.551223 0.839036 0.790020 11.00000 0.02529 0.02629 = 0.01499 -0.00176 0.00414 0.00171 AFIX 43 H12 2 0.549493 0.832636 0.844177 11.00000 -1.20000 AFIX 0 C19 1 0.033667 0.909218 0.910793 11.00000 0.01429 0.02694 = 0.02769 0.00322 0.00700 0.00126 AFIX 43 H19 2 -0.027135 0.918080 0.931877 11.00000 -1.20000 AFIX 0 C10 1 0.471886 0.862573 0.670442 11.00000 0.01695 0.02375 = 0.02258 -0.00016 0.00128 0.00474 AFIX 43 H10 2 0.415590 0.871387 0.642213 11.00000 -1.20000 AFIX 0 C3 1 1.028753 0.848017 0.514362 11.00000 0.01550 0.03312 = 0.02463 0.00252 0.00438 -0.00016 AFIX 43 H3 2 1.078836 0.837554 0.479485 11.00000 -1.20000 AFIX 0 C20 1 0.111757 0.913794 0.957376 11.00000 0.02410 0.03086 = 0.01624 -0.00062 0.00631 0.00055 AFIX 43 H20 2 0.104554 0.925989 1.010559 11.00000 -1.20000 AFIX 0 C14 1 0.379284 0.860760 0.788219 11.00000 0.02306 0.01905 = 0.02190 0.00094 0.00325 0.00060 C4 1 1.039286 0.910569 0.574016 11.00000 0.01609 0.02913 = 0.03015 0.00393 -0.00261 -0.00603 AFIX 43 H4 2 1.096946 0.942670 0.581525 11.00000 -1.20000 AFIX 0 C18 1 0.044128 0.891733 0.833494 11.00000 0.02042 0.02747 = 0.02557 -0.00020 -0.00534 -0.00109 AFIX 43 H18 2 -0.009675 0.888734 0.801465 11.00000 -1.20000 AFIX 0 C17 1 0.132176 0.878569 0.802370 11.00000 0.02459 0.02468 = 0.01890 -0.00281 0.00147 0.00092 AFIX 43 H17 2 0.138790 0.866414 0.749131 11.00000 -1.20000 AFIX 0 HKLF 4 REM Fe_PM_PEA_NCS_90K in Pccn REM R1 = 0.0425 for 2553 Fo > 4sig(Fo) and 0.0726 for all 3489 data REM 231 parameters refined using 7 restraints END WGHT 0.0310 1.1756 REM Highest difference peak 0.316, deepest hole -0.327, 1-sigma level 0.065 Q1 1 0.7013 0.7456 0.5018 11.00000 0.05 0.32 Q2 1 0.2500 0.7500 0.6592 10.50000 0.05 0.31 Q3 1 0.3350 0.8216 0.8175 11.00000 0.05 0.28 Q4 1 0.7352 0.7896 0.6086 11.00000 0.05 0.28 Q5 1 0.5031 0.8671 0.7751 11.00000 0.05 0.27 Q6 1 0.8011 0.8055 0.5594 11.00000 0.05 0.26 Q7 1 0.7019 0.5152 0.3575 11.00000 0.05 0.24 Q8 1 0.8462 0.4823 0.3759 11.00000 0.05 0.24 Q9 1 0.8204 0.6734 0.4225 11.00000 0.05 0.24 Q10 1 1.2134 0.7771 0.5607 11.00000 0.05 0.24 ; _shelx_res_checksum 26072 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.027 _oxdiff_exptl_absorpt_empirical_full_min 0.975 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.7500 0.7500 0.54898(2) 0.01409(14) Uani 1 2 d S T P . . S1 S 0.77855(5) 0.51466(5) 0.36248(3) 0.02169(17) Uani 1 1 d . . . . . N2 N 0.87208(13) 0.81266(15) 0.55312(10) 0.0148(5) Uani 1 1 d . . . . . N3 N 0.72509(14) 0.83942(15) 0.63205(10) 0.0151(5) Uani 1 1 d . . . . . N1 N 0.78553(14) 0.65996(16) 0.47000(11) 0.0179(5) Uani 1 1 d . . . . . C7 C 0.79640(17) 0.88706(18) 0.65499(13) 0.0170(6) Uani 1 1 d . . . . . H7 H 0.7934 0.9268 0.6986 0.020 Uiso 1 1 calc R U . . . C8 C 0.63897(17) 0.84483(18) 0.67327(13) 0.0161(6) Uani 1 1 d . . . . . C13 C 0.63612(18) 0.83411(19) 0.75220(13) 0.0203(6) Uani 1 1 d . . . . . H13 H 0.6923 0.8234 0.7801 0.024 Uiso 1 1 calc R U . . . C6 C 0.88151(18) 0.87656(19) 0.61046(13) 0.0173(6) Uani 1 1 d . . . . . C9 C 0.55644(16) 0.85911(19) 0.63259(13) 0.0184(6) Uani 1 1 d D . . . . H9 H 0.5584 0.8665 0.5785 0.022 Uiso 1 1 calc R U . . . C15 C 0.30356(19) 0.87009(19) 0.81688(14) 0.0211(6) Uani 1 1 d . . . . . C11 C 0.46811(18) 0.85327(19) 0.74980(14) 0.0188(6) Uani 1 1 d . . . . . C2 C 0.94496(18) 0.80076(19) 0.50572(13) 0.0199(6) Uani 1 1 d . . . . . H2 H 0.9387 0.7579 0.4644 0.024 Uiso 1 1 calc R U . . . C1 C 0.78170(17) 0.59947(19) 0.42553(13) 0.0170(6) Uani 1 1 d . . . . . C16 C 0.21177(18) 0.88313(19) 0.84929(13) 0.0192(6) Uani 1 1 d . . . . . C5 C 0.96384(18) 0.9256(2) 0.62288(14) 0.0229(6) Uani 1 1 d . . . . . H5 H 0.9687 0.9689 0.6641 0.028 Uiso 1 1 calc R U . . . C21 C 0.20014(17) 0.9008(2) 0.92717(14) 0.0230(6) Uani 1 1 d D . . . . H21 H 0.2535 0.9038 0.9597 0.028 Uiso 1 1 calc R U . . . C12 C 0.55122(18) 0.8390(2) 0.79002(14) 0.0222(6) Uani 1 1 d . . . . . H12 H 0.5495 0.8326 0.8442 0.027 Uiso 1 1 calc R U . . . C19 C 0.03367(17) 0.9092(2) 0.91079(14) 0.0230(6) Uani 1 1 d D . . . . H19 H -0.0271 0.9181 0.9319 0.028 Uiso 1 1 calc R U . . . C10 C 0.47189(17) 0.86257(19) 0.67044(14) 0.0211(6) Uani 1 1 d D . . . . H10 H 0.4156 0.8714 0.6422 0.025 Uiso 1 1 calc R U . . . C3 C 1.02875(18) 0.8480(2) 0.51436(14) 0.0244(6) Uani 1 1 d . . . . . H3 H 1.0788 0.8376 0.4795 0.029 Uiso 1 1 calc R U . . . C20 C 0.11176(16) 0.9138(2) 0.95738(13) 0.0237(6) Uani 1 1 d D . . . . H20 H 0.1046 0.9260 1.0106 0.028 Uiso 1 1 calc R U . . . C14 C 0.37928(19) 0.86076(19) 0.78822(14) 0.0213(6) Uani 1 1 d . . . . . C4 C 1.03929(19) 0.9106(2) 0.57402(15) 0.0251(7) Uani 1 1 d . . . . . H4 H 1.0969 0.9427 0.5815 0.030 Uiso 1 1 calc R U . . . C18 C 0.04413(18) 0.8917(2) 0.83349(14) 0.0245(6) Uani 1 1 d D . . . . H18 H -0.0097 0.8887 0.8015 0.029 Uiso 1 1 calc R U . . . C17 C 0.13218(18) 0.8786(2) 0.80237(14) 0.0227(6) Uani 1 1 d D . . . . H17 H 0.1388 0.8664 0.7491 0.027 Uiso 1 1 calc R U . . . 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 0.0130(3) 0.0170(3) 0.0123(2) 0.000 0.000 0.0014(2) S1 0.0226(4) 0.0240(4) 0.0184(3) -0.0049(3) -0.0034(3) 0.0037(3) N2 0.0137(11) 0.0169(12) 0.0138(10) 0.0029(9) -0.0004(9) 0.0017(9) N3 0.0134(11) 0.0180(12) 0.0138(10) 0.0032(8) 0.0000(8) 0.0029(9) N1 0.0137(11) 0.0215(13) 0.0184(11) -0.0008(9) -0.0010(8) 0.0007(10) C7 0.0211(15) 0.0164(14) 0.0137(12) -0.0001(10) -0.0002(10) -0.0004(12) C8 0.0162(14) 0.0142(15) 0.0178(12) -0.0031(11) 0.0049(10) 0.0019(11) C13 0.0196(15) 0.0235(17) 0.0178(13) -0.0017(11) -0.0023(11) 0.0014(12) C6 0.0175(14) 0.0187(16) 0.0158(12) 0.0012(11) -0.0015(10) 0.0012(12) C9 0.0196(14) 0.0215(16) 0.0141(12) 0.0010(11) 0.0027(10) 0.0057(12) C15 0.0224(16) 0.0205(17) 0.0204(13) -0.0009(11) 0.0015(11) -0.0002(12) C11 0.0193(14) 0.0159(15) 0.0213(13) -0.0027(11) 0.0062(11) 0.0001(12) C2 0.0195(15) 0.0224(16) 0.0179(13) 0.0032(11) 0.0023(11) 0.0030(13) C1 0.0117(13) 0.0229(16) 0.0165(12) 0.0039(11) -0.0003(10) 0.0017(12) C16 0.0187(14) 0.0171(15) 0.0217(13) 0.0015(11) 0.0062(11) 0.0003(12) C5 0.0223(15) 0.0258(18) 0.0208(13) 0.0003(12) -0.0017(11) -0.0035(13) C21 0.0161(15) 0.0309(18) 0.0220(13) 0.0020(12) -0.0011(11) -0.0011(13) C12 0.0253(15) 0.0263(17) 0.0150(13) -0.0018(11) 0.0041(11) 0.0017(13) C19 0.0143(14) 0.0269(18) 0.0277(14) 0.0032(12) 0.0070(11) 0.0013(12) C10 0.0169(14) 0.0238(17) 0.0226(13) -0.0002(11) 0.0013(11) 0.0047(12) C3 0.0155(14) 0.0331(18) 0.0246(14) 0.0025(13) 0.0044(11) -0.0002(13) C20 0.0241(15) 0.0309(18) 0.0162(13) -0.0006(12) 0.0063(11) 0.0005(13) C14 0.0231(15) 0.0191(16) 0.0219(13) 0.0009(11) 0.0033(12) 0.0006(12) C4 0.0161(15) 0.0291(18) 0.0302(14) 0.0039(13) -0.0026(11) -0.0060(13) C18 0.0204(15) 0.0275(17) 0.0256(14) -0.0002(12) -0.0053(11) -0.0011(13) C17 0.0246(16) 0.0247(17) 0.0189(13) -0.0028(12) 0.0015(12) 0.0009(13) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 15 13 2 0.0636 -15 -13 1 0.0155 5 3 -24 0.0787 -2 0 25 0.0640 -1 20 -1 0.0383 1 -20 1 0.0216 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Fe1 N2 175.77(11) 2_665 . ? N2 Fe1 N3 96.25(8) 2_665 . ? N2 Fe1 N3 80.60(8) . . ? N2 Fe1 N3 96.25(8) . 2_665 ? N2 Fe1 N3 80.59(8) 2_665 2_665 ? N3 Fe1 N3 84.83(11) 2_665 . ? N1 Fe1 N2 95.52(8) 2_665 2_665 ? N1 Fe1 N2 95.52(8) . . ? N1 Fe1 N2 87.48(8) 2_665 . ? N1 Fe1 N2 87.48(8) . 2_665 ? N1 Fe1 N3 175.10(8) 2_665 2_665 ? N1 Fe1 N3 92.68(8) . 2_665 ? N1 Fe1 N3 175.10(8) . . ? N1 Fe1 N3 92.68(8) 2_665 . ? N1 Fe1 N1 90.11(12) . 2_665 ? C6 N2 Fe1 114.90(16) . . ? C2 N2 Fe1 127.51(17) . . ? C2 N2 C6 117.6(2) . . ? C7 N3 Fe1 115.49(16) . . ? C7 N3 C8 119.7(2) . . ? C8 N3 Fe1 124.31(16) . . ? C1 N1 Fe1 161.6(2) . . ? N3 C7 H7 122.0 . . ? N3 C7 C6 116.1(2) . . ? C6 C7 H7 122.0 . . ? C13 C8 N3 121.4(2) . . ? C13 C8 C9 119.9(2) . . ? C9 C8 N3 118.6(2) . . ? C8 C13 H13 120.2 . . ? C12 C13 C8 119.7(2) . . ? C12 C13 H13 120.2 . . ? N2 C6 C7 112.4(2) . . ? N2 C6 C5 122.6(2) . . ? C5 C6 C7 125.0(2) . . ? C8 C9 H9 119.9 . . ? C10 C9 C8 120.1(2) . . ? C10 C9 H9 119.9 . . ? C14 C15 C16 178.2(3) . . ? C12 C11 C10 118.9(2) . . ? C12 C11 C14 121.7(2) . . ? C10 C11 C14 119.4(2) . . ? N2 C2 H2 118.6 . . ? N2 C2 C3 122.8(2) . . ? C3 C2 H2 118.6 . . ? N1 C1 S1 178.8(2) . . ? C21 C16 C15 121.1(2) . . ? C21 C16 C17 118.9(2) . . ? C17 C16 C15 120.1(2) . . ? C6 C5 H5 120.6 . . ? C6 C5 C4 118.8(2) . . ? C4 C5 H5 120.6 . . ? C16 C21 H21 119.8 . . ? C20 C21 C16 120.4(2) . . ? C20 C21 H21 119.8 . . ? C13 C12 C11 120.8(2) . . ? C13 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? C20 C19 H19 120.1 . . ? C20 C19 C18 119.8(2) . . ? C18 C19 H19 120.1 . . ? C9 C10 C11 120.5(2) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C2 C3 H3 120.2 . . ? C4 C3 C2 119.5(2) . . ? C4 C3 H3 120.2 . . ? C21 C20 C19 120.4(2) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C15 C14 C11 176.3(3) . . ? C5 C4 H4 120.7 . . ? C3 C4 C5 118.6(2) . . ? C3 C4 H4 120.7 . . ? C19 C18 H18 119.7 . . ? C19 C18 C17 120.5(2) . . ? C17 C18 H18 119.7 . . ? C16 C17 H17 120.0 . . ? C18 C17 C16 120.0(2) . . ? C18 C17 H17 120.0 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N2 1.958(2) 2_665 ? Fe1 N2 1.958(2) . ? Fe1 N3 1.964(2) . ? Fe1 N3 1.964(2) 2_665 ? Fe1 N1 1.951(2) . ? Fe1 N1 1.951(2) 2_665 ? S1 C1 1.636(3) . ? N2 C6 1.361(3) . ? N2 C2 1.339(3) . ? N3 C7 1.287(3) . ? N3 C8 1.425(3) . ? N1 C1 1.162(3) . ? C7 H7 0.9500 . ? C7 C6 1.449(3) . ? C8 C13 1.387(3) . ? C8 C9 1.389(3) . ? C13 H13 0.9500 . ? C13 C12 1.380(3) . ? C6 C5 1.384(4) . ? C9 H9 0.9500 . ? C9 C10 1.375(3) . ? C15 C16 1.438(4) . ? C15 C14 1.197(3) . ? C11 C12 1.392(4) . ? C11 C10 1.392(3) . ? C11 C14 1.437(3) . ? C2 H2 0.9500 . ? C2 C3 1.380(4) . ? C16 C21 1.392(3) . ? C16 C17 1.401(3) . ? C5 H5 0.9500 . ? C5 C4 1.389(4) . ? C21 H21 0.9500 . ? C21 C20 1.378(3) . ? C12 H12 0.9500 . ? C19 H19 0.9500 . ? C19 C20 1.380(3) . ? C19 C18 1.380(3) . ? C10 H10 0.9500 . ? C3 H3 0.9500 . ? C3 C4 1.380(4) . ? C20 H20 0.9500 . ? C4 H4 0.9500 . ? C18 H18 0.9500 . ? C18 C17 1.380(3) . ? C17 H17 0.9500 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Fe1 N2 C6 C7 -2.2(3) . . . . ? Fe1 N2 C6 C5 178.4(2) . . . . ? Fe1 N2 C2 C3 -179.23(19) . . . . ? Fe1 N3 C7 C6 7.3(3) . . . . ? Fe1 N3 C8 C13 122.0(2) . . . . ? Fe1 N3 C8 C9 -56.6(3) . . . . ? N2 C6 C5 C4 1.3(4) . . . . ? N2 C2 C3 C4 0.0(4) . . . . ? N3 C7 C6 N2 -3.3(3) . . . . ? N3 C7 C6 C5 176.0(2) . . . . ? N3 C8 C13 C12 -179.5(2) . . . . ? N3 C8 C9 C10 178.5(2) . . . . ? C7 N3 C8 C13 -49.1(4) . . . . ? C7 N3 C8 C9 132.3(3) . . . . ? C7 C6 C5 C4 -178.0(2) . . . . ? C8 N3 C7 C6 179.2(2) . . . . ? C8 C13 C12 C11 1.0(4) . . . . ? C8 C9 C10 C11 1.0(4) . . . . ? C13 C8 C9 C10 0.0(4) . . . . ? C6 N2 C2 C3 2.1(4) . . . . ? C6 C5 C4 C3 0.8(4) . . . . ? C9 C8 C13 C12 -0.9(4) . . . . ? C15 C16 C21 C20 179.5(3) . . . . ? C15 C16 C17 C18 -179.6(3) . . . . ? C2 N2 C6 C7 176.6(2) . . . . ? C2 N2 C6 C5 -2.7(4) . . . . ? C2 C3 C4 C5 -1.4(4) . . . . ? C16 C21 C20 C19 0.2(4) . . . . ? C21 C16 C17 C18 0.2(4) . . . . ? C12 C11 C10 C9 -0.9(4) . . . . ? C19 C18 C17 C16 -0.2(4) . . . . ? C10 C11 C12 C13 0.0(4) . . . . ? C20 C19 C18 C17 0.1(4) . . . . ? C14 C11 C12 C13 -178.6(3) . . . . ? C14 C11 C10 C9 177.6(3) . . . . ? C18 C19 C20 C21 -0.2(4) . . . . ? C17 C16 C21 C20 -0.2(4) . . . . ? loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 15.0663 13.1759 2.0729 -0.9736 -0.0770 -0.2151 -15.2156 -13.1016 0.7290 0.9428 0.0743 0.3250 4.9299 2.5451 -23.6487 0.0298 0.0045 -0.9995 -1.7934 0.2285 24.5025 -0.2386 -0.0211 0.9709 -1.2376 20.0681 -1.2773 -0.5135 -0.8389 -0.1804 1.3485 -20.0772 0.8161 0.5152 0.8418 0.1611