#------------------------------------------------------------------------------ #$Date: 2024-07-10 01:19:24 +0300 (Wed, 10 Jul 2024) $ #$Revision: 293343 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/21/1572121.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_1572121 loop_ _publ_author_name 'Lundahl, Maike' 'Greiner, Maria B.' 'Piquette, Marc C.' 'Gannon, Paige M.' 'Kaminsky, Werner' 'Kovacs, Julie A.' _publ_section_title ; Exploring the Influence of H-Bonding and Ligand Constraints on Thiolate Ligated Non-Heme Iron Mediated Dioxygen Activation ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC02787F _journal_year 2024 _chemical_absolute_configuration ad _chemical_formula_moiety 'C16 H31 Fe N3 S2, C H4 O' _chemical_formula_sum 'C17 H35 Fe N3 O S2' _chemical_formula_weight 417.45 _space_group_IT_number 29 _space_group_name_Hall 'P 2c -2ac' _space_group_name_H-M_alt 'P c a 21' _symmetry_cell_setting orthorhombic _symmetry_Int_Tables_number 29 _symmetry_space_group_name_Hall 'P 2c -2ac' _symmetry_space_group_name_H-M 'P c a 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4.5 _audit_creation_date 2022-05-09T13:57:35-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_update_record ; 2022-10-11 deposited with the CCDC. 2024-07-05 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 19.3307(8) _cell_length_b 12.1908(5) _cell_length_c 9.1228(3) _cell_measurement_reflns_used 9962 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 28.24 _cell_measurement_theta_min 2.69 _cell_measurement_wavelength 0.71073 _cell_volume 2149.85(14) _computing_cell_refinement 'SAINT V8.34A integration software' _computing_data_collection 'Bruker APEX2 software' _computing_data_reduction 'SORTAV (Blessing, 1995)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 2012)' _computing_publication_material 'WinGX publication routines (Farrugia, 2012)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXS-2013 (Sheldrick, 2008)' _diffrn_ambient_temperature 100(2) _diffrn_detector 'APEX-II CCD' _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Bruker APEX-II' _diffrn_measurement_method '\f or \w oscillation scans' _diffrn_orient_matrix_UB_11 -0.002994 _diffrn_orient_matrix_UB_12 -0.068519 _diffrn_orient_matrix_UB_13 0.028397 _diffrn_orient_matrix_UB_21 0.000198 _diffrn_orient_matrix_UB_22 0.045056 _diffrn_orient_matrix_UB_23 0.043235 _diffrn_orient_matrix_UB_31 -0.109574 _diffrn_orient_matrix_UB_32 0.001967 _diffrn_orient_matrix_UB_33 -0.000709 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0595 _diffrn_reflns_av_unetI/netI 0.0416 _diffrn_reflns_Laue_measured_fraction_full 1 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 20760 _diffrn_reflns_point_group_measured_fraction_full 1 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_theta_full 25 _diffrn_reflns_theta_max 28.581 _diffrn_reflns_theta_min 1.67 _diffrn_source 'sealed x-ray tube' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.905 _exptl_absorpt_correction_T_max 0.746 _exptl_absorpt_correction_T_min 0.705 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2012/1 - Bruker AXS area detector scaling and absorption correcti ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.29 _exptl_crystal_density_method 'not measured' _exptl_crystal_description needle _exptl_crystal_F_000 896 _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _refine_diff_density_max 0.239 _refine_diff_density_min -0.427 _refine_diff_density_rms 0.054 _refine_ls_abs_structure_details ; Flack x determined using 2103 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.010(6) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_constraints 0 _refine_ls_number_parameters 225 _refine_ls_number_reflns 5450 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.037 _refine_ls_R_factor_all 0.0365 _refine_ls_R_factor_gt 0.0278 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0227P)^2^+0.2412P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0541 _refine_ls_wR_factor_ref 0.0574 _reflns_Friedel_coverage 0.87 _reflns_Friedel_fraction_full 0.999 _reflns_Friedel_fraction_max 0.984 _reflns_number_gt 4909 _reflns_number_total 5450 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc02787f2.cif _cod_data_source_block shelx _cod_database_code 1572121 _shelx_estimated_absorpt_t_min 0.737 _shelx_estimated_absorpt_t_max 0.973 _shelx_shelxl_version_number 2014/7 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL MG2156_0ma in Pca2(1) CELL 0.71073 19.3307 12.1908 9.1228 90.000 90.000 90.000 ZERR 4.00 0.0008 0.0005 0.0003 0.000 0.000 0.000 LATT -1 SYMM - X, - Y, 1/2 + Z SYMM 1/2 - X, Y, 1/2 + Z SYMM 1/2 + X, - Y, Z SFAC C H N S FE O UNIT 68 140 12 8 4 4 MERG 2 FMAP 2 PLAN 20 SIZE 0.030 0.040 0.360 ACTA 50.00 BOND $H L.S. 16 TEMP -173.00 WGHT 0.022700 0.241200 FVAR 0.15740 FE1 5 0.377500 0.302208 0.452111 11.00000 0.01204 0.01174 = 0.01103 -0.00015 0.00023 0.00040 S1 4 0.476294 0.252943 0.584327 11.00000 0.01584 0.01676 = 0.02134 0.00007 -0.00472 0.00102 S2 4 0.280948 0.379061 0.560420 11.00000 0.01292 0.01576 = 0.01808 -0.00285 0.00356 -0.00256 C3 1 0.513050 0.042910 0.660232 11.00000 0.02323 0.02413 = 0.02630 0.00329 0.00013 0.00723 AFIX 137 H3A 2 0.500338 -0.025898 0.708809 11.00000 -1.50000 H3B 2 0.549064 0.080040 0.717281 11.00000 -1.50000 H3C 2 0.530528 0.027114 0.561629 11.00000 -1.50000 AFIX 0 C2 1 0.416243 0.130971 0.801350 11.00000 0.02418 0.02841 = 0.01589 0.00007 -0.00081 0.00149 AFIX 137 H2A 2 0.378293 0.184093 0.795503 11.00000 -1.50000 H2B 2 0.451174 0.157440 0.870705 11.00000 -1.50000 H2C 2 0.398234 0.060139 0.834884 11.00000 -1.50000 AFIX 0 C16 1 0.260458 0.595268 0.624937 11.00000 0.01651 0.01966 = 0.03469 -0.00994 -0.00073 0.00436 AFIX 137 H16A 2 0.279249 0.665472 0.658896 11.00000 -1.50000 H16B 2 0.226428 0.568260 0.695915 11.00000 -1.50000 H16C 2 0.238080 0.605492 0.529519 11.00000 -1.50000 AFIX 0 N2 3 0.365331 0.299626 0.217436 11.00000 0.01212 0.01590 = 0.01208 0.00033 0.00022 0.00168 AFIX 13 H2 2 0.326334 0.351582 0.198282 11.00000 -1.20000 AFIX 0 N3 3 0.403015 0.472565 0.421578 11.00000 0.01183 0.01685 = 0.01267 0.00238 0.00066 -0.00232 C8 1 0.341415 0.194428 0.155125 11.00000 0.01790 0.01776 = 0.01362 -0.00342 -0.00055 0.00101 AFIX 23 H8A 2 0.380438 0.141892 0.151888 11.00000 -1.20000 H8B 2 0.324966 0.206215 0.053569 11.00000 -1.20000 AFIX 0 C7 1 0.283079 0.146875 0.247348 11.00000 0.01836 0.01865 = 0.01627 -0.00312 -0.00365 -0.00038 AFIX 23 H7A 2 0.256711 0.207798 0.292369 11.00000 -1.20000 H7B 2 0.251129 0.105846 0.182640 11.00000 -1.20000 AFIX 0 C6 1 0.308443 0.071268 0.366997 11.00000 0.01911 0.01476 = 0.01830 -0.00216 -0.00056 -0.00423 AFIX 23 H6A 2 0.268935 0.048907 0.429250 11.00000 -1.20000 H6B 2 0.328380 0.004333 0.322374 11.00000 -1.20000 AFIX 0 C4 1 0.394421 0.066155 0.551056 11.00000 0.02070 0.01513 = 0.01393 -0.00079 0.00268 0.00183 C5 1 0.380448 -0.054262 0.570207 11.00000 0.04123 0.01474 = 0.02393 0.00450 -0.00573 0.00042 AFIX 137 H5A 2 0.330442 -0.067336 0.567606 11.00000 -1.50000 H5B 2 0.399027 -0.078702 0.664671 11.00000 -1.50000 H5C 2 0.402764 -0.095274 0.490833 11.00000 -1.50000 AFIX 0 C1 1 0.449203 0.117240 0.649239 11.00000 0.01891 0.01597 = 0.01569 0.00133 0.00074 0.00470 C9 1 0.423860 0.344974 0.131592 11.00000 0.01759 0.02481 = 0.01549 -0.00025 0.00488 -0.00144 AFIX 23 H9A 2 0.414376 0.334596 0.025855 11.00000 -1.20000 H9B 2 0.466391 0.303504 0.155756 11.00000 -1.20000 AFIX 0 C10 1 0.436235 0.465720 0.160951 11.00000 0.01899 0.02406 = 0.01572 0.00472 0.00473 -0.00349 AFIX 23 H10A 2 0.393117 0.506227 0.138616 11.00000 -1.20000 H10B 2 0.472253 0.492133 0.092352 11.00000 -1.20000 AFIX 0 C11 1 0.458400 0.494247 0.315665 11.00000 0.01561 0.02237 = 0.01846 0.00188 0.00404 -0.00508 AFIX 23 H11A 2 0.499692 0.450465 0.342094 11.00000 -1.20000 H11B 2 0.471281 0.572775 0.320098 11.00000 -1.20000 AFIX 0 C12 1 0.373237 0.546906 0.496972 11.00000 0.01319 0.01333 = 0.01757 0.00094 -0.00333 -0.00200 C13 1 0.389210 0.667881 0.489493 11.00000 0.02857 0.01457 = 0.03638 -0.00009 0.00323 -0.00342 AFIX 137 H13A 2 0.432808 0.678985 0.436716 11.00000 -1.50000 H13B 2 0.393417 0.697337 0.589047 11.00000 -1.50000 H13C 2 0.351784 0.705923 0.437856 11.00000 -1.50000 AFIX 0 C14 1 0.319144 0.511924 0.610089 11.00000 0.01362 0.01384 = 0.01871 -0.00224 -0.00010 0.00032 C15 1 0.356718 0.500639 0.758277 11.00000 0.01919 0.02277 = 0.01702 -0.00305 -0.00031 -0.00250 AFIX 137 H15A 2 0.376505 0.571637 0.786216 11.00000 -1.50000 H15B 2 0.393815 0.446247 0.749460 11.00000 -1.50000 H15C 2 0.323733 0.476857 0.833407 11.00000 -1.50000 AFIX 0 C18 1 0.653612 0.181749 0.448566 11.00000 0.04335 0.05883 = 0.07167 -0.02349 0.02188 -0.02487 AFIX 137 H18A 2 0.651852 0.230488 0.533912 11.00000 -1.50000 H18B 2 0.695675 0.196778 0.392065 11.00000 -1.50000 H18C 2 0.653982 0.105245 0.481546 11.00000 -1.50000 AFIX 0 O1 6 0.595445 0.199964 0.360149 11.00000 0.05992 0.04865 = 0.03939 -0.01311 0.02354 -0.00408 AFIX 147 H1 2 0.560340 0.207801 0.413397 11.00000 -1.50000 AFIX 0 N1 3 0.361178 0.125315 0.458442 11.00000 0.01625 0.01373 = 0.01276 -0.00033 0.00093 -0.00145 HKLF 4 1.0 1.00 0.00 0.00 0.00 1.00 0.00 0.00 0.00 1.00 REM MG2156_0ma in Pca2(1) REM R1 = 0.0278 for 4909 Fo > 4sig(Fo) and 0.0365 for all 5450 data REM 225 parameters refined using 1 restraints END WGHT 0.0227 0.2411 REM Highest difference peak 0.239, deepest hole -0.427, 1-sigma level 0.054 Q1 1 0.4295 0.4874 0.3772 11.00000 0.05 0.24 Q2 1 0.3960 0.3220 0.1802 11.00000 0.05 0.23 Q3 1 0.2786 -0.1207 0.6537 11.00000 0.05 0.23 Q4 1 0.3456 0.5199 0.5442 11.00000 0.05 0.22 Q5 1 0.3719 0.5781 0.4601 11.00000 0.05 0.22 Q6 1 0.2945 0.5459 0.6384 11.00000 0.05 0.21 Q7 1 0.4546 0.4625 0.2414 11.00000 0.05 0.21 Q8 1 0.3689 -0.1606 0.4472 11.00000 0.05 0.20 Q9 1 0.3719 0.6988 0.3727 11.00000 0.05 0.20 Q10 1 0.3880 0.3155 0.2882 11.00000 0.05 0.20 Q11 1 0.3527 0.7162 0.6227 11.00000 0.05 0.19 Q12 1 0.3628 0.3989 0.3896 11.00000 0.05 0.19 Q13 1 0.4212 0.1040 0.6022 11.00000 0.05 0.19 Q14 1 0.2991 0.4636 0.5934 11.00000 0.05 0.19 Q15 1 0.3060 0.3277 0.4194 11.00000 0.05 0.19 Q16 1 0.4744 0.3690 0.5596 11.00000 0.05 0.19 Q17 1 0.3497 0.2508 0.1745 11.00000 0.05 0.18 Q18 1 0.4357 0.1133 0.7074 11.00000 0.05 0.18 Q19 1 0.4418 0.3246 0.5097 11.00000 0.05 0.18 Q20 1 0.3484 0.3284 0.2320 11.00000 0.05 0.18 ; _shelx_res_checksum 8672 _shelx_hkl_file ; 0 0 1 -0.65 0.32 0 0 -1 -0.66 0.33 0 0 2 595.43 14.39 0 0 -2 552.25 13.41 0 0 3 0.19 0.84 0 0 -3 0.12 0.70 0 0 4 30.22 2.00 0 0 -4 36.37 2.06 0 0 5 -0.58 0.76 0 0 -5 -0.35 0.85 0 0 6 138.09 4.36 0 0 -6 139.91 5.00 0 0 7 -0.23 0.79 0 0 -7 -2.11 0.92 0 0 8 122.35 4.34 0 0 -8 122.93 5.15 0 0 9 -0.34 1.00 0 0 -9 0.71 1.39 0 0 10 115.81 6.80 0 0 -10 110.46 5.38 0 0 -11 0.01 2.21 0 0 -12 10.34 3.56 0 -1 -11 -2.55 2.22 0 1 11 1.75 2.09 0 -1 -10 4.14 1.75 0 1 10 2.00 1.23 0 -1 -9 2.24 1.40 0 1 9 -1.60 0.94 0 -1 -8 2.82 1.42 0 1 8 4.08 1.21 0 -1 -7 -0.17 1.11 0 1 7 -0.52 0.81 0 -1 -6 34.73 2.39 0 1 6 32.53 1.98 0 -1 -5 0.83 0.93 0 1 5 0.22 0.73 0 -1 -4 4.33 1.01 0 1 4 5.77 0.39 0 -1 -3 0.06 0.22 0 1 3 -0.25 0.17 0 -1 -2 45.03 0.93 0 1 2 50.25 0.93 0 -1 -1 -0.11 0.10 0 1 1 -0.18 0.09 0 -1 0 185.84 2.38 0 1 0 187.50 2.61 0 -1 1 -0.28 0.11 0 1 -1 -0.21 0.12 0 -1 2 48.45 0.80 0 1 -2 44.57 1.05 0 -1 3 -0.15 0.19 0 1 -3 -0.04 0.26 0 -1 4 6.20 0.31 0 1 -4 5.04 1.10 0 -1 5 0.02 0.27 0 1 -5 0.59 0.96 0 -1 6 36.85 1.86 0 1 -6 34.91 2.53 0 -1 7 1.08 0.80 0 1 -7 -1.03 1.06 0 -1 8 3.31 1.06 0 1 -8 1.84 1.32 0 -1 9 -0.64 0.91 0 1 -9 -0.39 1.76 0 1 -10 7.20 2.89 0 1 -11 4.22 2.53 0 1 -12 -0.93 2.40 0 -2 -11 2.28 2.43 0 2 11 -2.64 1.97 0 -2 -10 6.36 2.71 0 2 10 10.98 1.95 0 -2 -9 -3.75 1.81 0 2 9 0.76 1.27 0 -2 -8 94.60 4.29 0 2 8 98.18 4.12 0 -2 -7 0.06 1.06 0 2 7 0.11 0.40 0 -2 -6 55.63 2.88 0 2 6 51.81 1.39 0 -2 -5 0.15 0.25 0 2 5 0.05 0.22 0 -2 -4 71.92 1.62 0 2 4 72.95 1.07 0 -2 -3 0.05 0.11 0 2 3 0.12 0.21 0 -2 -2 161.76 1.74 0 2 2 158.71 1.76 0 -2 -1 -0.14 0.16 0 2 1 0.20 0.21 0 -2 0 16.22 0.44 0 2 0 16.39 0.46 0 -2 1 0.00 0.15 0 2 -1 -0.04 0.11 0 -2 2 159.07 2.05 0 2 -2 161.49 1.96 0 -2 3 0.24 0.22 0 2 -3 -0.08 0.21 0 -2 4 74.66 1.25 0 2 -4 71.05 1.17 0 -2 5 0.22 0.20 0 2 -5 -0.04 0.19 0 -2 6 48.95 0.96 0 2 -6 54.47 4.16 0 -2 7 -0.20 0.33 0 2 -7 -0.72 1.58 0 -2 8 104.14 2.66 0 2 -8 85.46 2.16 0 -2 9 -1.54 1.16 0 2 -9 -0.63 0.41 0 2 -10 9.68 0.76 0 2 -11 -0.48 0.50 0 2 -12 9.69 0.89 0 -3 -12 24.90 1.90 0 3 12 31.82 5.09 0 -3 -11 -0.52 0.50 0 3 11 -1.09 1.49 0 -3 -10 19.15 1.11 0 3 10 20.42 2.53 0 -3 -9 -0.20 0.44 0 3 9 -0.15 1.27 0 -3 -8 67.95 1.96 0 3 8 72.15 2.37 0 -3 -7 -0.81 0.34 0 3 7 -0.24 0.37 0 -3 -6 14.57 0.56 0 3 6 11.23 0.51 0 -3 -5 -0.11 0.17 0 3 5 0.01 0.23 0 -3 -4 36.75 0.84 0 3 4 39.29 0.84 0 -3 -3 0.08 0.19 0 3 3 -0.07 0.30 0 -3 -2 351.52 3.70 0 3 2 369.40 4.91 0 -3 -1 -0.13 0.23 0 3 1 0.02 0.30 0 -3 0 3.47 0.30 0 3 0 3.71 0.34 0 -3 1 0.19 0.22 0 3 -1 -0.13 0.25 0 -3 2 378.37 4.63 0 3 -2 350.72 4.39 0 -3 3 -0.11 0.26 0 3 -3 -0.19 0.24 0 -3 4 39.31 0.79 0 3 -4 35.20 0.79 0 -3 5 -0.21 0.24 0 3 -5 -0.15 0.21 0 -3 6 11.54 0.49 0 3 -6 15.60 0.64 0 -3 7 0.40 0.26 0 3 -7 -0.82 0.45 0 -3 8 71.48 2.10 0 3 -8 71.24 2.15 0 -3 9 -0.29 0.65 0 3 -9 -1.32 0.54 0 3 -10 19.35 1.24 0 3 -11 -1.24 0.61 0 3 -12 23.89 2.06 0 -4 -11 0.11 0.65 0 4 11 0.78 1.63 0 -4 -10 9.95 0.96 0 4 10 10.94 2.20 0 -4 -9 -0.83 0.50 0 4 9 -1.10 0.63 0 -4 -8 16.62 1.09 0 4 8 18.76 1.17 0 -4 -7 0.08 0.31 0 4 7 0.48 0.54 0 -4 -6 22.89 0.96 0 4 6 19.88 0.84 0 -4 -5 0.03 0.19 0 4 5 -0.03 0.37 0 -4 -4 18.15 0.70 0 4 4 15.06 0.74 0 -4 -3 0.19 0.25 0 4 3 -0.15 0.39 0 -4 -2 8.44 0.41 0 4 2 7.17 0.47 0 -4 -1 -0.13 0.25 0 4 1 -0.52 0.32 0 -4 0 16.77 0.60 0 4 0 16.27 0.60 0 -4 1 -0.39 0.26 0 4 -1 -0.40 0.28 0 -4 2 7.84 0.36 0 4 -2 7.84 0.57 0 -4 3 0.12 0.33 0 4 -3 -0.39 0.35 0 -4 4 17.28 0.77 0 4 -4 20.15 0.65 0 -4 5 -0.03 0.27 0 4 -5 -0.23 0.32 0 -4 6 20.09 0.73 0 4 -6 22.34 0.84 0 -4 7 -0.29 0.30 0 4 -7 0.20 0.36 0 -4 8 18.66 1.42 0 4 -8 17.80 1.22 0 -4 9 0.45 0.66 0 4 -9 -0.19 0.63 0 -4 10 10.10 1.67 0 4 -10 11.82 1.15 0 4 -11 -1.19 0.98 0 -5 -11 0.91 1.13 0 5 11 -0.21 1.70 0 -5 -10 7.31 1.42 0 5 10 4.21 1.23 0 -5 -9 0.01 0.64 0 5 9 -0.44 0.65 0 -5 -8 39.31 1.33 0 5 8 44.76 1.82 0 -5 -7 -0.19 0.43 0 5 7 -0.05 0.63 0 -5 -6 138.72 2.43 0 5 6 135.97 2.59 0 -5 -5 0.13 0.32 0 5 5 -0.29 0.44 0 -5 -4 240.18 3.16 0 5 4 238.79 3.92 0 -5 -3 -0.47 0.26 0 5 3 -0.35 0.43 0 -5 -2 81.19 1.50 0 5 2 70.67 1.45 0 -5 -1 0.17 0.31 0 5 1 -0.60 0.39 0 -5 0 419.70 5.70 0 5 0 415.68 5.31 0 -5 1 -0.11 0.34 0 5 -1 -0.29 0.33 0 -5 2 76.89 1.60 0 5 -2 75.25 1.44 0 -5 3 -0.60 0.35 0 5 -3 0.36 0.46 0 -5 4 243.66 4.24 0 5 -4 232.30 3.73 0 -5 5 -0.12 0.36 0 5 -5 -0.69 0.37 0 -5 6 138.15 2.71 0 5 -6 132.53 2.40 0 -5 7 0.03 0.52 0 5 -7 -0.51 0.49 0 -5 8 42.36 2.20 0 5 -8 38.86 1.44 0 -5 9 0.62 0.74 0 5 -9 0.39 0.77 0 -5 10 4.90 1.10 0 5 -10 9.29 1.62 0 -5 11 -0.25 0.87 0 5 -11 1.23 1.26 0 -6 -11 -1.12 1.08 0 6 11 -2.04 1.12 0 -6 -10 17.85 2.06 0 6 10 15.21 1.81 0 -6 -9 0.66 1.03 0 6 9 -1.39 0.74 0 -6 -8 1.36 0.57 0 6 8 2.38 0.85 0 -6 -7 0.02 0.48 0 6 7 0.06 0.70 0 -6 -6 57.17 1.42 0 6 6 57.71 1.79 0 -6 -5 -0.24 0.35 0 6 5 -0.50 0.47 0 -6 -4 136.28 2.26 0 6 4 130.76 2.58 0 -6 -3 -0.18 0.31 0 6 3 0.07 0.48 0 -6 -2 91.19 1.72 0 6 2 82.16 1.68 0 -6 -1 -0.09 0.33 0 6 1 -0.02 0.45 0 -6 0 46.87 1.41 0 6 0 43.48 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233.11 2.59 2 1 3 96.66 1.46 -2 -1 -3 96.29 1.53 2 1 4 16.68 0.53 -2 -1 -4 18.06 0.66 2 1 5 3.82 0.30 -2 -1 -5 4.40 1.11 2 1 6 6.42 0.47 -2 -1 -6 3.90 1.15 2 1 7 28.17 2.20 -2 -1 -7 27.19 2.38 2 1 8 5.24 1.28 -2 -1 -8 2.93 1.31 2 1 9 1.56 1.17 -2 -1 -9 1.67 1.40 2 1 10 0.61 1.20 -2 -1 -10 5.74 2.47 -2 -1 -11 6.26 2.87 2 0 -11 6.63 2.18 2 0 -10 12.32 2.38 -2 0 10 9.66 2.49 2 0 -9 81.16 4.39 -2 0 9 77.06 3.44 2 0 -8 4.64 1.46 -2 0 8 2.19 1.31 2 0 -7 131.63 5.08 -2 0 7 130.25 5.94 2 0 -6 30.59 2.42 -2 0 6 32.47 1.00 2 0 -5 77.17 3.23 -2 0 5 65.57 1.62 2 0 -4 44.39 1.08 -2 0 4 43.98 0.88 2 0 -3 670.56 8.48 -2 0 3 687.10 9.35 2 0 -2 12.92 0.32 -2 0 2 13.75 0.32 2 0 -1 981.80 8.97 -2 0 1 978.22 9.72 2 0 0 25.33 0.43 -2 0 0 26.63 0.51 2 0 1 996.48 10.98 -2 0 -1 1000.00 10.47 2 0 2 14.33 0.37 -2 0 -2 15.17 0.48 2 0 3 710.08 9.70 -2 0 -3 682.21 11.48 2 0 4 45.50 0.88 -2 0 -4 47.44 2.31 2 0 5 66.59 1.63 -2 0 -5 72.95 3.06 2 0 6 37.04 2.88 -2 0 -6 32.15 2.47 2 0 7 150.54 7.04 -2 0 -7 130.63 5.07 2 0 8 2.81 1.00 -2 0 -8 4.11 1.95 2 0 9 73.88 3.39 -2 0 -9 69.66 5.50 2 0 10 8.48 2.26 -2 0 -10 9.15 2.85 -2 0 -11 11.30 3.30 -2 0 -12 9.65 3.47 2 -1 -12 0.62 2.71 2 -1 -11 6.49 2.96 -2 1 11 -0.85 2.02 2 -1 -10 2.53 2.32 -2 1 10 0.75 1.28 2 -1 -9 3.29 1.59 -2 1 9 1.50 1.14 2 -1 -8 2.04 1.31 -2 1 8 2.98 1.17 2 -1 -7 23.46 2.26 -2 1 7 27.18 2.76 2 -1 -6 6.62 1.41 -2 1 6 5.98 0.50 2 -1 -5 3.58 1.11 -2 1 5 3.61 0.27 2 -1 -4 16.17 0.65 -2 1 4 17.99 0.56 2 -1 -3 98.35 1.63 -2 1 3 94.81 1.13 2 -1 -2 223.69 2.48 -2 1 2 223.67 2.48 2 -1 -1 89.28 1.02 -2 1 1 86.54 1.00 2 -1 0 35.37 0.60 -2 1 0 35.10 0.54 2 -1 1 89.58 1.14 -2 1 -1 91.05 1.16 2 -1 2 228.80 2.84 -2 1 -2 225.16 2.63 2 -1 3 98.51 1.32 -2 1 -3 95.69 1.45 2 -1 4 18.07 0.55 -2 1 -4 15.88 0.70 2 -1 5 4.00 0.29 -2 1 -5 3.49 1.54 2 -1 6 6.65 0.52 -2 1 -6 5.55 1.82 2 -1 7 29.27 2.64 -2 1 -7 26.43 3.40 2 -1 8 2.77 1.03 -2 1 -8 4.25 2.04 2 -1 9 3.12 1.12 -2 1 -9 -0.03 1.97 -2 1 -10 3.32 2.35 -2 1 -11 6.76 2.96 -2 1 -12 1.52 2.43 2 -2 -12 1.64 0.58 2 -2 -11 6.11 0.69 -2 2 11 7.69 2.94 2 -2 -10 7.58 0.68 -2 2 10 7.94 1.82 2 -2 -9 30.74 1.13 -2 2 9 33.71 2.78 2 -2 -8 21.33 1.24 -2 2 8 23.93 2.22 2 -2 -7 28.96 1.35 -2 2 7 30.79 1.15 2 -2 -6 37.42 1.52 -2 2 6 35.89 0.77 2 -2 -5 136.49 2.28 -2 2 5 142.16 2.19 2 -2 -4 60.30 1.06 -2 2 4 61.74 0.99 2 -2 -3 79.67 1.19 -2 2 3 88.26 1.30 2 -2 -2 75.25 0.94 -2 2 2 73.90 1.06 2 -2 -1 44.82 0.67 -2 2 1 33.79 0.70 2 -2 0 11.63 0.36 -2 2 0 11.07 0.39 2 -2 1 35.54 0.69 -2 2 -1 45.08 0.80 2 -2 2 73.98 1.05 -2 2 -2 74.96 0.99 2 -2 3 89.02 1.30 -2 2 -3 77.26 1.16 2 -2 4 62.08 1.04 -2 2 -4 61.44 1.11 2 -2 5 144.77 2.06 -2 2 -5 141.99 2.41 2 -2 6 36.95 0.80 -2 2 -6 36.63 0.94 2 -2 7 34.41 1.03 -2 2 -7 31.27 1.10 2 -2 8 26.33 1.25 -2 2 -8 22.77 1.00 2 -2 9 36.12 3.27 -2 2 -9 31.54 1.25 -2 2 -10 6.73 0.72 -2 2 -11 6.67 0.76 -2 2 -12 2.67 0.66 2 -3 -12 3.16 1.11 -2 3 12 3.77 3.00 2 -3 -11 18.06 1.20 -2 3 11 22.29 4.21 2 -3 -10 -0.14 0.52 -2 3 10 0.36 1.43 2 -3 -9 57.40 1.90 -2 3 9 57.49 3.43 2 -3 -8 16.98 0.99 -2 3 8 16.84 1.21 2 -3 -7 15.12 0.90 -2 3 7 13.09 0.70 2 -3 -6 9.03 0.49 -2 3 6 8.31 0.46 2 -3 -5 32.97 0.78 -2 3 5 32.14 0.81 2 -3 -4 31.76 0.74 -2 3 4 34.02 0.77 2 -3 -3 27.78 0.56 -2 3 3 30.72 0.75 2 -3 -2 15.18 0.48 -2 3 2 13.90 0.48 2 -3 -1 343.15 3.84 -2 3 1 317.98 3.78 2 -3 0 6.30 0.34 -2 3 0 5.91 0.38 2 -3 1 326.32 3.86 -2 3 -1 333.82 4.48 2 -3 2 15.07 0.51 -2 3 -2 14.83 0.56 2 -3 3 32.09 0.84 -2 3 -3 26.50 0.66 2 -3 4 35.98 0.82 -2 3 -4 33.04 0.80 2 -3 5 33.44 0.85 -2 3 -5 30.80 0.74 2 -3 6 8.36 0.48 -2 3 -6 8.12 0.51 2 -3 7 13.79 0.63 -2 3 -7 15.50 0.60 2 -3 8 16.27 0.82 -2 3 -8 16.47 1.05 2 -3 9 61.39 3.00 -2 3 -9 55.37 1.93 -2 3 -10 0.24 0.61 -2 3 -11 21.31 1.37 -2 3 -12 4.17 1.21 2 -4 -11 5.85 1.26 -2 4 11 6.73 2.16 2 -4 -10 13.90 1.16 -2 4 10 13.70 2.27 2 -4 -9 5.10 0.78 -2 4 9 4.41 0.76 2 -4 -8 37.16 1.60 -2 4 8 35.54 1.34 2 -4 -7 29.01 0.92 -2 4 7 29.26 1.06 2 -4 -6 54.89 1.54 -2 4 6 54.32 1.19 2 -4 -5 5.86 0.45 -2 4 5 3.79 0.43 2 -4 -4 68.30 1.29 -2 4 4 69.90 1.37 2 -4 -3 4.07 0.35 -2 4 3 2.97 0.42 2 -4 -2 108.20 1.76 -2 4 2 109.54 1.72 2 -4 -1 7.17 0.40 -2 4 1 5.48 0.46 2 -4 0 327.72 3.77 -2 4 0 326.56 5.27 2 -4 1 5.51 0.38 -2 4 -1 5.74 0.48 2 -4 2 108.02 1.56 -2 4 -2 108.79 2.15 2 -4 3 3.33 0.45 -2 4 -3 3.71 0.47 2 -4 4 70.70 1.59 -2 4 -4 68.77 1.27 2 -4 5 4.27 0.44 -2 4 -5 5.61 0.48 2 -4 6 54.73 1.37 -2 4 -6 54.36 1.23 2 -4 7 30.70 1.02 -2 4 -7 28.58 0.99 2 -4 8 34.79 1.56 -2 4 -8 32.66 1.14 2 -4 9 5.15 0.77 -2 4 -9 5.47 0.87 2 -4 10 10.51 1.67 -2 4 -10 12.12 1.18 -2 4 -11 5.17 1.39 2 -5 -11 17.94 2.01 -2 5 11 16.01 2.76 2 -5 -10 1.99 1.16 -2 5 10 2.68 1.20 2 -5 -9 45.17 2.03 -2 5 9 42.25 1.83 2 -5 -8 17.91 0.99 -2 5 8 19.50 1.31 2 -5 -7 53.02 1.66 -2 5 7 61.27 2.11 2 -5 -6 1.08 0.42 -2 5 6 0.79 0.43 2 -5 -5 129.46 2.15 -2 5 5 122.98 2.35 2 -5 -4 13.80 0.56 -2 5 4 14.17 0.80 2 -5 -3 185.12 2.62 -2 5 3 184.83 3.16 2 -5 -2 52.93 1.15 -2 5 2 51.30 1.21 2 -5 -1 498.63 6.28 -2 5 1 492.14 7.20 2 -5 0 112.58 1.80 -2 5 0 110.68 2.10 2 -5 1 499.19 6.30 -2 5 -1 491.02 6.16 2 -5 2 55.44 1.12 -2 5 -2 52.28 1.20 2 -5 3 185.56 3.02 -2 5 -3 187.25 3.44 2 -5 4 14.09 0.66 -2 5 -4 13.74 0.75 2 -5 5 124.77 2.20 -2 5 -5 127.97 2.35 2 -5 6 0.05 0.35 -2 5 -6 0.45 0.39 2 -5 7 61.74 1.85 -2 5 -7 52.79 1.72 2 -5 8 17.92 1.30 -2 5 -8 17.47 1.04 2 -5 9 40.23 1.85 -2 5 -9 41.49 2.02 2 -5 10 2.77 1.05 -2 5 -10 4.35 1.31 2 -5 11 15.92 1.73 -2 5 -11 15.24 2.00 2 -6 -11 3.36 1.39 -2 6 11 1.39 1.32 2 -6 -10 3.92 1.34 -2 6 10 5.54 1.39 2 -6 -9 3.09 1.26 -2 6 9 2.05 0.87 2 -6 -8 8.41 0.86 -2 6 8 7.33 1.05 2 -6 -7 17.93 1.14 -2 6 7 18.56 1.37 2 -6 -6 24.17 1.11 -2 6 6 25.46 1.30 2 -6 -5 21.65 0.88 -2 6 5 19.98 1.02 2 -6 -4 5.96 0.51 -2 6 4 4.69 0.67 2 -6 -3 67.36 1.52 -2 6 3 68.93 1.83 2 -6 -2 29.50 1.02 -2 6 2 26.73 1.04 2 -6 -1 20.53 0.84 -2 6 1 15.96 0.94 2 -6 0 3.48 0.48 -2 6 0 4.02 0.57 2 -6 1 17.70 0.78 -2 6 -1 18.77 0.93 2 -6 2 29.90 0.92 -2 6 -2 29.52 1.04 2 -6 3 69.40 1.34 -2 6 -3 66.92 1.79 2 -6 4 6.70 0.54 -2 6 -4 5.34 0.61 2 -6 5 21.19 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-24 0 1 -0.53 1.21 24 0 0 0.91 1.30 -24 0 0 1.33 1.16 24 0 1 1.34 1.31 -24 0 -1 1.49 1.29 24 0 2 21.10 2.43 -24 0 -2 18.31 2.01 24 0 3 8.29 1.81 -24 0 -3 7.70 1.88 24 0 4 28.09 3.16 -24 0 -4 19.98 2.47 24 -1 -4 2.26 1.47 -24 1 4 -0.64 1.24 24 -1 -3 3.10 1.37 -24 1 3 2.13 1.25 24 -1 -2 6.48 1.59 -24 1 2 4.68 1.42 24 -1 -1 7.06 1.66 -24 1 1 2.72 1.33 24 -1 0 1.08 1.30 -24 1 0 4.06 1.46 24 -1 1 1.94 1.38 -24 1 -1 4.87 1.47 24 -1 2 7.02 1.69 -24 1 -2 5.21 1.46 24 -1 3 3.73 1.48 -24 1 -3 1.98 1.43 24 -1 4 1.38 1.51 -24 1 -4 0.14 1.36 24 -2 -4 26.05 2.87 -24 2 4 17.92 2.14 24 -2 -3 4.13 1.41 -24 2 3 0.64 1.24 24 -2 -2 9.16 1.73 -24 2 2 4.96 1.40 24 -2 -1 6.94 1.68 -24 2 1 2.39 1.28 24 -2 0 5.51 1.55 -24 2 0 3.32 1.47 24 -2 1 8.33 1.77 -24 2 -1 3.06 1.37 24 -2 2 9.23 1.84 -24 2 -2 7.89 1.62 24 -2 3 2.75 1.47 -24 2 -3 0.78 1.50 24 -2 4 30.29 3.40 -24 2 -4 19.49 2.47 -24 3 4 10.16 3.47 24 -3 -3 12.49 2.30 -24 3 3 3.51 1.39 24 -3 -2 6.23 1.63 -24 3 2 6.70 1.60 24 -3 -1 4.31 1.45 -24 3 1 3.49 1.37 24 -3 0 8.52 1.74 -24 3 0 7.63 1.62 24 -3 1 4.11 1.41 -24 3 -1 4.47 1.49 24 -3 2 8.62 1.75 -24 3 -2 6.14 1.60 24 -3 3 9.86 1.87 -24 3 -3 4.81 1.76 24 -4 -3 9.08 2.00 -24 4 3 6.83 1.65 24 -4 -2 9.42 1.76 -24 4 2 7.52 1.60 24 -4 -1 13.59 2.03 -24 4 1 8.92 1.74 24 -4 0 2.96 1.46 -24 4 0 -0.43 1.21 24 -4 1 12.99 2.05 -24 4 -1 7.56 1.65 24 -4 2 9.34 1.91 -24 4 -2 7.89 1.67 24 -4 3 5.37 1.67 -24 4 -3 8.39 2.07 24 -5 -2 19.63 2.33 -24 5 2 9.12 1.69 24 -5 -1 6.93 1.65 -24 5 1 4.32 1.49 24 -5 0 7.83 1.81 -24 5 0 8.75 1.70 24 -5 1 4.33 1.53 -24 5 -1 2.98 1.41 24 -5 2 15.36 2.17 -24 5 -2 13.88 1.89 -24 6 1 -1.57 2.27 24 -6 0 15.02 2.11 -24 6 0 10.98 1.89 -24 6 -1 3.50 2.72 25 4 -1 9.49 2.89 -25 -4 1 8.43 2.86 25 4 0 0.29 1.30 -25 -4 0 -0.12 1.20 25 4 1 11.63 3.02 -25 -4 -1 19.06 3.86 25 3 -2 3.70 1.65 -25 -3 2 1.08 1.28 25 3 -1 11.78 1.99 -25 -3 1 11.66 1.84 25 3 0 -0.14 1.35 -25 -3 0 -0.71 1.13 25 3 1 11.89 1.99 -25 -3 -1 9.84 1.79 25 3 2 4.23 1.60 -25 -3 -2 0.91 1.20 -25 -2 3 11.47 3.40 25 2 -2 0.14 1.33 -25 -2 2 1.51 1.30 25 2 -1 4.47 1.54 -25 -2 1 2.73 1.44 25 2 0 -0.66 1.26 -25 -2 0 2.38 1.39 25 2 1 4.78 1.63 -25 -2 -1 3.35 1.36 25 2 2 3.00 1.54 -25 -2 -2 0.71 1.21 25 1 -3 55.91 5.59 -25 -1 3 32.45 2.71 25 1 -2 5.50 1.63 -25 -1 2 0.65 1.22 25 1 -1 8.98 1.85 -25 -1 1 2.81 1.36 25 1 0 0.13 1.22 -25 -1 0 2.42 1.32 25 1 1 4.23 1.58 -25 -1 -1 5.18 1.55 25 1 2 2.84 1.53 -25 -1 -2 0.90 1.20 25 1 3 61.65 4.05 -25 -1 -3 39.54 4.70 25 0 -3 -1.13 1.56 -25 0 3 0.58 1.24 25 0 -2 0.04 1.24 -25 0 2 -1.42 1.11 25 0 -1 1.40 1.40 -25 0 1 2.81 1.41 25 0 0 -1.38 1.17 -25 0 0 -1.78 1.09 25 0 1 -1.10 1.24 -25 0 -1 0.74 1.15 25 0 2 0.60 1.36 -25 0 -2 -0.10 1.19 25 0 3 0.74 1.39 -25 0 -3 -0.83 1.92 25 -1 -3 52.30 5.36 -25 1 3 38.87 3.70 25 -1 -2 3.48 1.42 -25 1 2 2.13 1.35 25 -1 -1 6.30 1.76 -25 1 1 1.85 1.37 25 -1 0 0.42 1.33 -25 1 0 1.22 1.30 25 -1 1 7.27 1.78 -25 1 -1 6.24 1.50 25 -1 2 1.03 1.34 -25 1 -2 2.15 1.34 25 -1 3 58.49 4.64 -25 1 -3 47.07 5.26 25 -2 -2 1.68 1.38 -25 2 2 -1.53 1.16 25 -2 -1 5.92 1.61 -25 2 1 3.34 1.45 25 -2 0 2.77 1.43 -25 2 0 2.70 1.35 25 -2 1 3.15 1.52 -25 2 -1 1.53 1.34 25 -2 2 1.98 1.43 -25 2 -2 0.59 1.26 25 -3 -2 1.79 1.40 -25 3 2 0.68 1.36 25 -3 -1 12.99 2.06 -25 3 1 7.45 1.71 25 -3 0 0.46 1.26 -25 3 0 -1.67 1.11 25 -3 1 12.63 1.99 -25 3 -1 7.82 1.74 25 -3 2 4.58 1.72 -25 3 -2 1.97 1.72 -25 4 1 21.03 4.00 25 -4 0 2.18 1.38 -25 4 0 2.00 1.33 -25 4 -1 7.36 3.03 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 35255 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y, z+1/2' 'x+1/2, -y, z' 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 0.37750(2) 0.30221(3) 0.45211(4) 0.01160(8) Uani 1 1 d . . . . . S1 S 0.47629(4) 0.25294(6) 0.58433(8) 0.01798(14) Uani 1 1 d . . . . . S2 S 0.28095(3) 0.37906(5) 0.56042(7) 0.01559(14) Uani 1 1 d . . . . . C3 C 0.51305(16) 0.0429(2) 0.6602(3) 0.0246(7) Uani 1 1 d . . . . . H3A H 0.5003 -0.0259 0.7088 0.037 Uiso 1 1 calc R U . . . H3B H 0.5491 0.08 0.7173 0.037 Uiso 1 1 calc R U . . . H3C H 0.5305 0.0271 0.5616 0.037 Uiso 1 1 calc R U . . . C2 C 0.41624(15) 0.1310(3) 0.8013(3) 0.0228(6) Uani 1 1 d . . . . . H2A H 0.3783 0.1841 0.7955 0.034 Uiso 1 1 calc R U . . . H2B H 0.4512 0.1574 0.8707 0.034 Uiso 1 1 calc R U . . . H2C H 0.3982 0.0601 0.8349 0.034 Uiso 1 1 calc R U . . . C16 C 0.26046(16) 0.5953(2) 0.6249(3) 0.0236(7) Uani 1 1 d . . . . . H16A H 0.2792 0.6655 0.6589 0.035 Uiso 1 1 calc R U . . . H16B H 0.2264 0.5683 0.6959 0.035 Uiso 1 1 calc R U . . . H16C H 0.2381 0.6055 0.5295 0.035 Uiso 1 1 calc R U . . . N2 N 0.36533(11) 0.29963(18) 0.2174(2) 0.0134(5) Uani 1 1 d . . . . . H2 H 0.3263 0.3516 0.1983 0.016 Uiso 1 1 calc R U . . . N3 N 0.40301(11) 0.47257(18) 0.4216(2) 0.0138(5) Uani 1 1 d . . . . . C8 C 0.34141(15) 0.1944(2) 0.1551(3) 0.0164(6) Uani 1 1 d . . . . . H8A H 0.3804 0.1419 0.1519 0.02 Uiso 1 1 calc R U . . . H8B H 0.325 0.2062 0.0536 0.02 Uiso 1 1 calc R U . . . C7 C 0.28308(14) 0.1469(2) 0.2473(3) 0.0178(6) Uani 1 1 d . . . . . H7A H 0.2567 0.2078 0.2924 0.021 Uiso 1 1 calc R U . . . H7B H 0.2511 0.1058 0.1826 0.021 Uiso 1 1 calc R U . . . C6 C 0.30844(14) 0.0713(2) 0.3670(3) 0.0174(6) Uani 1 1 d . . . . . H6A H 0.2689 0.0489 0.4292 0.021 Uiso 1 1 calc R U . . . H6B H 0.3284 0.0043 0.3224 0.021 Uiso 1 1 calc R U . . . C4 C 0.39442(15) 0.0662(2) 0.5511(3) 0.0166(5) Uani 1 1 d . . . . . C5 C 0.38045(16) -0.0543(2) 0.5702(3) 0.0266(7) Uani 1 1 d . . . . . H5A H 0.3304 -0.0673 0.5676 0.04 Uiso 1 1 calc R U . . . H5B H 0.399 -0.0787 0.6647 0.04 Uiso 1 1 calc R U . . . H5C H 0.4028 -0.0953 0.4908 0.04 Uiso 1 1 calc R U . . . C1 C 0.44920(15) 0.1172(2) 0.6492(3) 0.0169(6) Uani 1 1 d . . . . . C9 C 0.42386(15) 0.3450(2) 0.1316(3) 0.0193(6) Uani 1 1 d . . . . . H9A H 0.4144 0.3346 0.0259 0.023 Uiso 1 1 calc R U . . . H9B H 0.4664 0.3035 0.1558 0.023 Uiso 1 1 calc R U . . . C10 C 0.43624(15) 0.4657(2) 0.1610(3) 0.0196(6) Uani 1 1 d . . . . . H10A H 0.3931 0.5062 0.1386 0.024 Uiso 1 1 calc R U . . . H10B H 0.4723 0.4921 0.0924 0.024 Uiso 1 1 calc R U . . . C11 C 0.45840(14) 0.4942(2) 0.3157(3) 0.0188(6) Uani 1 1 d . . . . . H11A H 0.4997 0.4505 0.3421 0.023 Uiso 1 1 calc R U . . . H11B H 0.4713 0.5728 0.3201 0.023 Uiso 1 1 calc R U . . . C12 C 0.37324(14) 0.5469(2) 0.4970(3) 0.0147(5) Uani 1 1 d . . . . . C13 C 0.38921(17) 0.6679(2) 0.4895(3) 0.0265(7) Uani 1 1 d . . . . . H13A H 0.4328 0.679 0.4367 0.04 Uiso 1 1 calc R U . . . H13B H 0.3934 0.6973 0.589 0.04 Uiso 1 1 calc R U . . . H13C H 0.3518 0.7059 0.4379 0.04 Uiso 1 1 calc R U . . . C14 C 0.31914(14) 0.5119(2) 0.6101(3) 0.0154(6) Uani 1 1 d . . . . . C15 C 0.35672(15) 0.5006(2) 0.7583(3) 0.0197(6) Uani 1 1 d . . . . . H15A H 0.3765 0.5716 0.7862 0.029 Uiso 1 1 calc R U . . . H15B H 0.3938 0.4462 0.7495 0.029 Uiso 1 1 calc R U . . . H15C H 0.3237 0.4769 0.8334 0.029 Uiso 1 1 calc R U . . . C18 C 0.6536(2) 0.1817(3) 0.4486(6) 0.0580(11) Uani 1 1 d . . . . . H18A H 0.6519 0.2305 0.5339 0.087 Uiso 1 1 calc R U . . . H18B H 0.6957 0.1968 0.3921 0.087 Uiso 1 1 calc R U . . . H18C H 0.654 0.1052 0.4815 0.087 Uiso 1 1 calc R U . . . O1 O 0.59545(16) 0.2000(2) 0.3601(3) 0.0493(7) Uani 1 1 d . . . . . H1 H 0.5603 0.2078 0.4134 0.074 Uiso 1 1 calc R U . . . N1 N 0.36118(11) 0.12531(16) 0.4584(3) 0.0142(4) 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 0.01204(17) 0.01174(16) 0.01103(14) -0.00015(16) 0.00023(16) 0.00040(14) S1 0.0158(3) 0.0168(3) 0.0213(3) 0.0001(3) -0.0047(3) 0.0010(3) S2 0.0129(3) 0.0158(3) 0.0181(3) -0.0029(3) 0.0036(3) -0.0026(3) C3 0.0232(17) 0.0241(16) 0.0263(15) 0.0033(12) 0.0001(12) 0.0072(13) C2 0.0242(16) 0.0284(17) 0.0159(13) 0.0001(11) -0.0008(12) 0.0015(13) C16 0.0165(16) 0.0197(15) 0.0347(17) -0.0099(12) -0.0007(12) 0.0044(12) N2 0.0121(11) 0.0159(11) 0.0121(10) 0.0003(8) 0.0002(8) 0.0017(9) N3 0.0118(11) 0.0169(11) 0.0127(11) 0.0024(8) 0.0007(8) -0.0023(9) C8 0.0179(15) 0.0178(14) 0.0136(12) -0.0034(10) -0.0005(10) 0.0010(12) C7 0.0184(15) 0.0187(14) 0.0163(13) -0.0031(10) -0.0037(11) -0.0004(12) C6 0.0191(15) 0.0148(13) 0.0183(13) -0.0022(10) -0.0006(11) -0.0042(11) C4 0.0207(14) 0.0151(13) 0.0139(12) -0.0008(10) 0.0027(11) 0.0018(11) C5 0.041(2) 0.0147(13) 0.0239(15) 0.0045(12) -0.0057(14) 0.0004(13) C1 0.0189(15) 0.0160(14) 0.0157(12) 0.0013(10) 0.0007(11) 0.0047(12) C9 0.0176(15) 0.0248(15) 0.0155(13) -0.0003(11) 0.0049(11) -0.0014(13) C10 0.0190(15) 0.0241(15) 0.0157(13) 0.0047(11) 0.0047(11) -0.0035(12) C11 0.0156(15) 0.0224(15) 0.0185(13) 0.0019(11) 0.0040(11) -0.0051(11) C12 0.0132(14) 0.0133(13) 0.0176(12) 0.0009(9) -0.0033(10) -0.0020(11) C13 0.0286(18) 0.0146(14) 0.0364(19) -0.0001(11) 0.0032(13) -0.0034(13) C14 0.0136(14) 0.0138(13) 0.0187(13) -0.0022(10) -0.0001(10) 0.0003(11) C15 0.0192(15) 0.0228(15) 0.0170(13) -0.0030(11) -0.0003(11) -0.0025(12) C18 0.043(2) 0.059(3) 0.072(2) -0.023(3) 0.022(3) -0.025(2) O1 0.060(2) 0.0486(17) 0.0394(15) -0.0131(12) 0.0235(13) -0.0041(14) N1 0.0163(11) 0.0137(10) 0.0128(9) -0.0003(11) 0.0009(10) -0.0014(8) 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 0 '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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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 _geom_angle_publ_flag N3 Fe1 N2 84.87(8) . . ? N3 Fe1 N1 172.24(8) . . ? N2 Fe1 N1 89.77(8) . . ? N3 Fe1 S2 81.33(6) . . ? N2 Fe1 S2 110.05(6) . . ? N1 Fe1 S2 105.83(6) . . ? N3 Fe1 S1 97.32(6) . . ? N2 Fe1 S1 126.76(6) . . ? N1 Fe1 S1 81.40(6) . . ? S2 Fe1 S1 122.93(3) . . ? C1 S1 Fe1 99.51(9) . . ? C14 S2 Fe1 97.95(9) . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C8 N2 C9 111.1(2) . . ? C8 N2 Fe1 115.43(16) . . ? C9 N2 Fe1 115.86(16) . . ? C8 N2 H2 104.3 . . ? C9 N2 H2 104.3 . . ? Fe1 N2 H2 104.3 . . ? C12 N3 C11 123.8(2) . . ? C12 N3 Fe1 120.83(18) . . ? C11 N3 Fe1 115.25(17) . . ? N2 C8 C7 110.5(2) . . ? N2 C8 H8A 109.6 . . ? C7 C8 H8A 109.6 . . ? N2 C8 H8B 109.6 . . ? C7 C8 H8B 109.6 . . ? H8A C8 H8B 108.1 . . ? C6 C7 C8 113.0(2) . . ? C6 C7 H7A 109 . . ? C8 C7 H7A 109 . . ? C6 C7 H7B 109 . . ? C8 C7 H7B 109 . . ? H7A C7 H7B 107.8 . . ? N1 C6 C7 111.2(2) . . ? N1 C6 H6A 109.4 . . ? C7 C6 H6A 109.4 . . ? N1 C6 H6B 109.4 . . ? C7 C6 H6B 109.4 . . ? H6A C6 H6B 108 . . ? N1 C4 C5 122.4(2) . . ? N1 C4 C1 120.4(2) . . ? C5 C4 C1 117.2(2) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C1 C3 110.9(2) . . ? C4 C1 C2 106.7(2) . . ? C3 C1 C2 109.8(2) . . ? C4 C1 S1 112.23(18) . . ? C3 C1 S1 108.9(2) . . ? C2 C1 S1 108.17(19) . . ? N2 C9 C10 112.9(2) . . ? N2 C9 H9A 109 . . ? C10 C9 H9A 109 . . ? N2 C9 H9B 109 . . ? C10 C9 H9B 109 . . ? H9A C9 H9B 107.8 . . ? C9 C10 C11 115.6(2) . . ? C9 C10 H10A 108.4 . . ? C11 C10 H10A 108.4 . . ? C9 C10 H10B 108.4 . . ? C11 C10 H10B 108.4 . . ? H10A C10 H10B 107.4 . . ? N3 C11 C10 111.5(2) . . ? N3 C11 H11A 109.3 . . ? C10 C11 H11A 109.3 . . ? N3 C11 H11B 109.3 . . ? C10 C11 H11B 109.3 . . ? H11A C11 H11B 108 . . ? N3 C12 C13 125.3(2) . . ? N3 C12 C14 118.3(2) . . ? C13 C12 C14 116.3(2) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C16 C14 C12 112.4(2) . . ? C16 C14 C15 109.4(2) . . ? C12 C14 C15 107.1(2) . . ? C16 C14 S2 108.03(19) . . ? C12 C14 S2 110.74(18) . . ? C15 C14 S2 109.10(18) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O1 C18 H18A 109.5 . . ? O1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C18 O1 H1 109.5 . . ? C4 N1 C6 117.9(2) . . ? C4 N1 Fe1 120.06(18) . . ? C6 N1 Fe1 121.85(16) . . ? 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 N3 2.153(2) . ? Fe1 N2 2.154(2) . ? Fe1 N1 2.1802(19) . ? Fe1 S2 2.3103(7) . ? Fe1 S1 2.3372(8) . ? S1 C1 1.833(3) . ? S2 C14 1.837(3) . ? C3 C1 1.534(4) . ? C3 H3A 0.98 . ? C3 H3B 0.98 . ? C3 H3C 0.98 . ? C2 C1 1.536(4) . ? C2 H2A 0.98 . ? C2 H2B 0.98 . ? C2 H2C 0.98 . ? C16 C14 1.529(4) . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? N2 C8 1.477(3) . ? N2 C9 1.483(3) . ? N2 H2 1 . ? N3 C12 1.275(3) . ? N3 C11 1.466(3) . ? C8 C7 1.522(4) . ? C8 H8A 0.99 . ? C8 H8B 0.99 . ? C7 C6 1.510(4) . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? C6 N1 1.473(3) . ? C6 H6A 0.99 . ? C6 H6B 0.99 . ? C4 N1 1.283(3) . ? C4 C5 1.503(4) . ? C4 C1 1.520(4) . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C9 C10 1.515(4) . ? C9 H9A 0.99 . ? C9 H9B 0.99 . ? C10 C11 1.515(4) . ? C10 H10A 0.99 . ? C10 H10B 0.99 . ? C11 H11A 0.99 . ? C11 H11B 0.99 . ? C12 C13 1.508(4) . ? C12 C14 1.530(4) . ? C13 H13A 0.98 . ? C13 H13B 0.98 . ? C13 H13C 0.98 . ? C14 C15 1.541(4) . ? C15 H15A 0.98 . ? C15 H15B 0.98 . ? C15 H15C 0.98 . ? C18 O1 1.401(5) . ? C18 H18A 0.98 . ? C18 H18B 0.98 . ? C18 H18C 0.98 . ? O1 H1 0.84 . ?