#------------------------------------------------------------------------------ #$Date: 2026-06-12 23:54:06 +0100 (Fri, 12 Jun 2026) $ #$Revision: 306560 $ #$URL: svn://www.crystallography.net/cod/cif/7/72/11/7721121.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_7721121 loop_ _publ_author_name 'Orton, Georgia' 'Cockcroft, Jeremy Karl' 'Ringenberg, Mark R.' 'Hartl, Frantisek' 'Hogarth, Graeme' _publ_section_title ; [FeFe]-hydrogenase biomimics incorporating redox-active ligands: Tuning the oxidation chemistry of ferrocene-dichalcogenolate-bridged centres via phosphine substitution ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D6DT00946H _journal_year 2026 _chemical_formula_moiety 'C40 H30 Fe3 O4 P2 Se2' _chemical_formula_sum 'C40 H30 Fe3 O4 P2 Se2' _chemical_formula_weight 962.05 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary dual _audit_creation_date 2019-07-30 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2026-04-22 deposited with the CCDC. 2026-06-11 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 97.0411(11) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.92991(14) _cell_length_b 17.9632(2) _cell_length_c 17.2334(2) _cell_measurement_reflns_used 23058 _cell_measurement_temperature 150 _cell_measurement_theta_max 73.1870 _cell_measurement_theta_min 4.2350 _cell_volume 3665.25(7) _computing_cell_refinement 'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 150 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.2031 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.996 _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 -115.00 -14.00 1.00 1.25 -- -42.62 -57.00-180.00 101 2 \w -93.00 -17.00 1.00 1.25 -- -42.62 -57.00 -90.00 76 3 \w -66.00 -14.00 1.00 1.25 -- -42.62 -57.00 -30.00 52 4 \w -67.00 20.00 1.00 1.25 -- -42.62 38.00 120.00 87 5 \w -115.00 -15.00 1.00 1.25 -- -42.62 -57.00 60.00 100 6 \w -78.00 -6.00 1.00 1.25 -- -42.62 125.00 -90.00 72 7 \w -36.00 -6.00 1.00 1.25 -- -42.62 125.00-180.00 30 8 \w -103.00 -21.00 1.00 1.25 -- -42.62 -38.00 90.00 82 9 \w -61.00 30.00 1.00 1.25 -- -42.62 38.00-150.00 91 10 \w 8.00 33.00 1.00 1.25 -- 42.62 83.00 -84.75 25 11 \w 9.00 36.00 1.00 1.25 -- 42.62 82.00 85.44 27 12 \w 10.00 35.00 1.00 1.25 -- 42.62 75.00 -39.42 25 13 \w 11.00 36.00 1.00 1.25 -- 42.62 75.00 28.57 25 14 \w 10.00 35.00 1.00 1.25 -- 42.62 76.00-129.97 25 15 \w 12.00 42.00 1.00 1.25 -- 42.62 76.00 164.57 30 16 \w 76.00 102.00 1.00 5.00 -- 106.06 68.00-110.56 26 17 \w 79.00 178.00 1.00 5.00 -- 106.06 50.00 152.10 99 18 \w 77.00 122.00 1.00 5.00 -- 106.06 61.00 -64.38 45 19 \w 142.00 171.00 1.00 5.00 -- 106.06 62.00 94.74 29 20 \w 75.00 177.00 1.00 5.00 -- 106.06 72.00 6.34 102 21 \w 77.00 103.00 1.00 5.00 -- 106.06 62.00 94.74 26 22 \w 146.00 173.00 1.00 5.00 -- 106.06 73.00-178.35 27 23 \w 75.00 175.00 1.00 5.00 -- 106.06 72.00-150.00 100 24 \w 74.00 101.00 1.00 5.00 -- 106.06 74.00 -48.30 27 25 \w 77.00 103.00 1.00 5.00 -- 106.06 63.00 103.13 26 26 \w 76.00 136.00 1.00 5.00 -- 106.06 68.00 -58.99 60 27 \w 79.00 106.00 1.00 5.00 -- 106.06 -95.00 60.00 27 28 \w 142.00 169.00 1.00 5.00 -- 106.06 60.00 13.68 27 29 \w 75.00 101.00 1.00 5.00 -- 106.06 72.00 31.22 26 30 \w 128.00 178.00 1.00 5.00 -- 106.06 66.00 82.49 50 31 \w 76.00 102.00 1.00 5.00 -- 106.06 66.00 -77.78 26 32 \w 76.00 102.00 1.00 5.00 -- 106.06 66.00 82.49 26 33 \w 121.00 146.00 1.00 5.00 -- 106.06 65.00 144.06 25 34 \w 77.00 103.00 1.00 5.00 -- 106.06 63.00 -24.45 26 35 \w 74.00 100.00 1.00 5.00 -- 106.06 73.00-178.35 26 36 \w 76.00 102.00 1.00 5.00 -- 106.06 65.00 144.06 26 37 \w 25.00 100.00 1.00 5.00 -- 106.06 -95.00 150.00 75 38 \w 75.00 178.00 1.00 5.00 -- 106.06 69.00 68.29 103 39 \w 24.00 101.00 1.00 5.00 -- 106.06 -95.00-150.00 77 40 \w 77.00 106.00 1.00 5.00 -- 106.06 61.00 120.00 29 41 \w 75.00 106.00 1.00 5.00 -- 106.06 72.00 -24.38 31 42 \w 77.00 103.00 1.00 5.00 -- 106.06 61.00 30.00 26 43 \w 30.00 139.00 1.00 5.00 -- 106.06 -77.00 -30.00 109 44 \w 77.00 137.00 1.00 5.00 -- 106.06 61.00 60.00 60 45 \w 75.00 101.00 1.00 5.00 -- 106.06 69.00-161.13 26 46 \w 25.00 106.00 1.00 5.00 -- 106.06 -95.00 -90.00 81 47 \w 80.00 168.00 1.00 5.00 -- 106.06 45.00-180.00 88 48 \w 113.00 177.00 1.00 5.00 -- 106.06 68.00-110.56 64 49 \w 77.00 134.00 1.00 5.00 -- 106.06 61.00 0.00 57 50 \w 77.00 111.00 1.00 5.00 -- 106.06 61.00 -90.00 34 51 \w 81.00 107.00 1.00 5.00 -- 106.06 61.00-180.00 26 52 \w 77.00 103.00 1.00 5.00 -- 106.06 61.00-120.00 26 53 \w 75.00 178.00 1.00 5.00 -- 106.06 69.00 -50.78 103 54 \w 75.00 101.00 1.00 5.00 -- 106.06 71.00 161.79 26 55 \w 52.00 79.00 1.00 5.00 -- 106.06-125.00 60.00 27 56 \w 87.00 112.00 1.00 5.00 -- 106.06-125.00 60.00 25 57 \w 77.00 104.00 1.00 5.00 -- 106.06 60.00 13.68 27 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.1038221000 _diffrn_orient_matrix_UB_12 0.0228773000 _diffrn_orient_matrix_UB_13 0.0571321000 _diffrn_orient_matrix_UB_21 0.0693856000 _diffrn_orient_matrix_UB_22 0.0091811000 _diffrn_orient_matrix_UB_23 -0.0691587000 _diffrn_orient_matrix_UB_31 -0.0366957000 _diffrn_orient_matrix_UB_32 0.0821074000 _diffrn_orient_matrix_UB_33 -0.0082055000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0640 _diffrn_reflns_av_unetI/netI 0.0325 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 63682 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 73.387 _diffrn_reflns_theta_min 3.568 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 12.833 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.114 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details 'CrysAlisPro 1.171.40.57a (Rigaku Oxford Diffraction, 2019) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.' _exptl_crystal_colour 'clear dark orange' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier dark _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 1.743 _exptl_crystal_description plank _exptl_crystal_F_000 1912 _exptl_crystal_size_max 0.59 _exptl_crystal_size_mid 0.094 _exptl_crystal_size_min 0.057 _refine_diff_density_max 0.945 _refine_diff_density_min -0.509 _refine_diff_density_rms 0.079 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 580 _refine_ls_number_reflns 7338 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.025 _refine_ls_R_factor_all 0.0435 _refine_ls_R_factor_gt 0.0324 _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^)+(0.0454P)^2^+1.0319P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0753 _refine_ls_wR_factor_ref 0.0801 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6123 _reflns_number_total 7338 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6dt00946h2.cif _cod_data_source_block exp_1709 _cod_original_cell_volume 3665.27(8) _cod_database_code 7721121 _shelx_shelxl_version_number 2014/7 _chemical_oxdiff_formula 'C40 H30 Fe3 O4 P2 Se2' _chemical_oxdiff_usercomment 'Georgia Orton crystal' _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 0.528 _shelx_estimated_absorpt_t_min 0.049 _reflns_odcompleteness_completeness 99.97 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _olex2_refinement_description ; ; _shelx_res_file ; exp_1709.res created by SHELXL-2014/7 TITL exp_1709_a.res in P2(1)/n REM Old TITL exp_1709_a.res in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.092, Rweak 0.006, Alpha 0.041, Orientation as input REM Formula found by SHELXT: C40 Fe3 O4 P2 Se2 CELL 1.54184 11.929914 17.963228 17.233424 90 97.0411 90 ZERR 4 0.000141 0.000216 0.000206 0 0.0011 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H Fe O P Se UNIT 160 120 12 16 8 8 L.S. 10 PLAN 2 SIZE 0.057 0.094 0.59 TEMP -123.15 BOND $H CONF list 4 fmap 2 acta OMIT -4 20 0 OMIT -4 21 4 OMIT -4 20 1 OMIT 1 17 2 REM REM REM WGHT 0.045400 1.031900 FVAR 2.23663 SE1 6 0.709060 0.632648 0.679424 11.00000 0.03035 0.01720 = 0.03258 -0.00040 0.01027 -0.00021 SE2 6 0.880625 0.740200 0.585145 11.00000 0.02821 0.01768 = 0.03571 0.00066 0.00736 0.00069 FE1 3 0.709869 0.757940 0.638655 11.00000 0.02833 0.01477 = 0.03045 -0.00122 0.00727 0.00220 FE2 3 0.889299 0.686718 0.713703 11.00000 0.03044 0.02038 = 0.03289 -0.00020 0.00518 0.00200 FE3 3 0.787049 0.567544 0.496889 11.00000 0.03414 0.01889 = 0.03048 -0.00145 0.00730 0.00220 P1 5 0.592594 0.784657 0.723642 11.00000 0.03065 0.02078 = 0.03157 -0.00432 0.00776 0.00221 P2 5 0.736323 0.879210 0.629611 11.00000 0.03303 0.01543 = 0.03571 -0.00114 0.00542 0.00250 O1 4 0.533182 0.745658 0.507329 11.00000 0.04276 0.04820 = 0.04282 -0.00181 -0.00710 0.00046 O2 4 1.055152 0.568975 0.699113 11.00000 0.05250 0.03602 = 0.05175 -0.00940 -0.00339 0.01736 O3 4 1.030679 0.807621 0.785012 11.00000 0.05562 0.04065 = 0.06311 -0.01293 -0.00155 -0.00987 O4 4 0.871924 0.645120 0.875655 11.00000 0.07455 0.05385 = 0.04164 0.01095 0.00957 0.00699 C1 1 0.603591 0.752040 0.558050 11.00000 0.03831 0.01954 = 0.04029 0.00092 0.01174 0.00260 C2 1 0.989218 0.614887 0.702902 11.00000 0.03987 0.02121 = 0.03441 -0.00149 0.00194 0.00219 C3 1 0.972871 0.762803 0.753482 11.00000 0.04221 0.02985 = 0.03991 -0.00223 0.00340 0.00331 C4 1 0.873988 0.662592 0.812280 11.00000 0.04474 0.02942 = 0.04061 0.00261 0.00563 0.00066 C5 1 0.712173 0.563243 0.595289 11.00000 0.03354 0.01619 = 0.03534 -0.00105 0.00730 -0.00172 C6 1 0.629042 0.556933 0.528745 11.00000 0.03018 0.02651 = 0.04557 -0.00124 0.00423 -0.00164 H6 2 0.573070 0.590043 0.514930 11.00000 0.02796 C7 1 0.656109 0.492874 0.485863 11.00000 0.04149 0.03139 = 0.04192 -0.00963 0.00455 -0.00712 H7 2 0.616675 0.476480 0.439527 11.00000 0.04123 C8 1 0.754780 0.459414 0.525852 11.00000 0.04881 0.01893 = 0.04173 -0.00474 0.01305 -0.00255 H8 2 0.792104 0.419195 0.511912 11.00000 0.03983 C9 1 0.788906 0.502627 0.593825 11.00000 0.03553 0.01761 = 0.03598 0.00147 0.00736 0.00232 H9 2 0.850834 0.495874 0.627809 11.00000 0.03175 C10 1 0.866590 0.666509 0.503853 11.00000 0.03567 0.02171 = 0.03558 0.00197 0.01376 0.00094 C11 1 0.783422 0.665124 0.437167 11.00000 0.04720 0.02540 = 0.03493 0.00463 0.00869 0.00055 H11 2 0.721621 0.693795 0.428326 11.00000 0.03720 C12 1 0.810686 0.605659 0.388246 11.00000 0.06899 0.03224 = 0.02952 -0.00081 0.01338 -0.00086 H12 2 0.770386 0.593049 0.344514 11.00000 0.06082 C13 1 0.910775 0.571294 0.423885 11.00000 0.05754 0.02633 = 0.04649 -0.00348 0.02784 0.00249 H13 2 0.944003 0.530693 0.409858 11.00000 0.05744 C14 1 0.946113 0.609023 0.495279 11.00000 0.03592 0.02513 = 0.04504 0.00111 0.01911 0.00198 H14 2 1.009557 0.599457 0.531686 11.00000 0.02632 C15 1 0.588844 0.885275 0.736342 11.00000 0.03703 0.02429 = 0.03765 -0.00808 0.00628 0.00614 H15 2 0.543991 0.903214 0.771504 11.00000 0.04517 C16 1 0.648224 0.927119 0.693523 11.00000 0.03985 0.02099 = 0.04455 -0.00795 0.00559 0.00592 H16 2 0.650218 0.982170 0.698982 11.00000 0.04978 C17 1 0.443801 0.761218 0.696783 11.00000 0.03223 0.02876 = 0.03062 -0.00218 0.01050 0.00303 C18 1 0.358158 0.812599 0.704556 11.00000 0.03863 0.02996 = 0.05544 -0.00036 0.01439 0.00551 H18 2 0.376917 0.856933 0.724341 11.00000 0.03546 C19 1 0.246532 0.793452 0.685769 11.00000 0.03659 0.04103 = 0.07518 0.00566 0.01490 0.00866 H19 2 0.183589 0.834311 0.693026 11.00000 0.06867 C20 1 0.216680 0.722160 0.661429 11.00000 0.03140 0.05355 = 0.05275 0.00503 0.00880 0.00035 H20 2 0.136779 0.709720 0.649191 11.00000 0.05982 C21 1 0.300134 0.669994 0.653462 11.00000 0.03639 0.04349 = 0.04538 -0.00818 0.00847 -0.00460 H21 2 0.280017 0.620551 0.636423 11.00000 0.04136 C22 1 0.412275 0.690171 0.669176 11.00000 0.03534 0.03389 = 0.04865 -0.01134 0.00750 0.00358 H22 2 0.459447 0.659100 0.663783 11.00000 0.04981 C23 1 0.616929 0.750345 0.824530 11.00000 0.04463 0.03089 = 0.03390 -0.00599 0.00801 0.00488 C24 1 0.562068 0.687595 0.847770 11.00000 0.06545 0.05030 = 0.04393 0.00169 0.00974 -0.01366 H24 2 0.501978 0.665019 0.807677 11.00000 0.07009 C25 1 0.587155 0.660056 0.922887 11.00000 0.10004 0.06009 = 0.04659 0.01202 0.01707 -0.01917 H25 2 0.556478 0.621015 0.940103 11.00000 0.07639 C26 1 0.665108 0.695406 0.975514 11.00000 0.10456 0.04712 = 0.03612 0.00441 0.01011 0.00737 H26 2 0.680700 0.674126 1.024539 11.00000 0.06978 C27 1 0.720593 0.756920 0.952863 11.00000 0.08261 0.04354 = 0.04048 -0.00722 -0.00840 0.00478 H27 2 0.775439 0.779505 0.980540 11.00000 0.05584 C28 1 0.698156 0.784350 0.876947 11.00000 0.06077 0.02957 = 0.04061 -0.00258 0.00217 0.00314 H28 2 0.744673 0.822288 0.862942 11.00000 0.03482 C29 1 0.697855 0.921577 0.533115 11.00000 0.03222 0.01848 = 0.04358 0.00417 0.00308 -0.00093 C30 1 0.706077 0.880982 0.465832 11.00000 0.05640 0.02247 = 0.04283 0.00392 0.00327 -0.00122 H30 2 0.729539 0.825908 0.470358 11.00000 0.04999 C31 1 0.678535 0.912994 0.392298 11.00000 0.06301 0.03481 = 0.04136 0.00597 -0.00143 -0.00866 H31 2 0.678522 0.887130 0.345602 11.00000 0.06027 C32 1 0.641663 0.985233 0.385994 11.00000 0.04513 0.04251 = 0.05357 0.01742 -0.00354 -0.00348 H32 2 0.621215 1.003090 0.335239 11.00000 0.05290 C33 1 0.634178 1.026378 0.451874 11.00000 0.06034 0.03027 = 0.07066 0.01841 0.00741 0.01396 H33 2 0.610745 1.073728 0.453171 11.00000 0.06617 C34 1 0.662611 0.995111 0.525111 11.00000 0.06071 0.02832 = 0.05536 0.00011 0.00651 0.00639 H34 2 0.665077 1.022206 0.567126 11.00000 0.04635 C35 1 0.873157 0.924407 0.658845 11.00000 0.03868 0.01515 = 0.04703 -0.00257 0.00228 0.00076 C36 1 0.900976 0.951562 0.734283 11.00000 0.04758 0.03430 = 0.05314 -0.00885 0.00482 0.00084 H36 2 0.854001 0.942112 0.772018 11.00000 0.03795 C37 1 1.004225 0.985340 0.755511 11.00000 0.05849 0.04322 = 0.06493 -0.01734 -0.00990 -0.00385 H37 2 1.020157 1.006558 0.806643 11.00000 0.06960 C38 1 1.080786 0.993128 0.702912 11.00000 0.04129 0.03354 = 0.07983 -0.00676 -0.00557 -0.00644 H38 2 1.148536 1.013698 0.716799 11.00000 0.05392 C39 1 1.054517 0.966941 0.627423 11.00000 0.04162 0.03227 = 0.07075 0.00453 0.00646 -0.00342 H39 2 1.100664 0.976620 0.592899 11.00000 0.04908 C40 1 0.950612 0.933255 0.605383 11.00000 0.03903 0.02904 = 0.04965 -0.00054 0.00473 -0.00033 H40 2 0.932343 0.917799 0.555019 11.00000 0.04033 HKLF 4 REM exp_1709_a.res in P2(1)/n REM R1 = 0.0324 for 6123 Fo > 4sig(Fo) and 0.0435 for all 7338 data REM 580 parameters refined using 0 restraints END WGHT 0.0454 1.0319 REM Highest difference peak 0.945, deepest hole -0.509, 1-sigma level 0.079 Q1 1 0.7772 0.6340 0.7064 11.00000 0.05 0.94 Q2 1 0.9455 0.7413 0.6183 11.00000 0.05 0.71 ; _shelx_res_checksum 68931 _olex2_date_sample_data_collection 2019-07-12 _olex2_exptl_crystal_mounting_method '0.3mm loop from 20um nylon from Hampton Research' _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 1.526 _oxdiff_exptl_absorpt_empirical_full_min 0.554 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' '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_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 Se1 Se 0.70906(3) 0.63265(2) 0.67942(2) 0.02618(8) Uani 1 1 d . . . . . Se2 Se 0.88063(3) 0.74020(2) 0.58515(2) 0.02692(8) Uani 1 1 d . . . . . Fe1 Fe 0.70987(4) 0.75794(3) 0.63865(3) 0.02421(10) Uani 1 1 d . . . . . Fe2 Fe 0.88930(4) 0.68672(3) 0.71370(3) 0.02779(11) Uani 1 1 d . . . . . Fe3 Fe 0.78705(4) 0.56754(3) 0.49689(3) 0.02756(11) Uani 1 1 d . . . . . P1 P 0.59259(6) 0.78466(4) 0.72364(4) 0.02734(16) Uani 1 1 d . . . . . P2 P 0.73632(7) 0.87921(4) 0.62961(5) 0.02795(16) Uani 1 1 d . . . . . O1 O 0.5332(2) 0.74566(15) 0.50733(15) 0.0456(6) Uani 1 1 d . . . . . O2 O 1.0552(2) 0.56898(15) 0.69911(15) 0.0476(6) Uani 1 1 d . . . . . O3 O 1.0307(2) 0.80762(16) 0.78501(17) 0.0539(7) Uani 1 1 d . . . . . O4 O 0.8719(3) 0.64512(17) 0.87565(16) 0.0565(7) Uani 1 1 d . . . . . C1 C 0.6036(3) 0.75204(17) 0.55805(19) 0.0321(7) Uani 1 1 d . . . . . C2 C 0.9892(3) 0.61489(18) 0.70290(18) 0.0320(7) Uani 1 1 d . . . . . C3 C 0.9729(3) 0.7628(2) 0.7535(2) 0.0375(7) Uani 1 1 d . . . . . C4 C 0.8740(3) 0.6626(2) 0.8123(2) 0.0382(7) Uani 1 1 d . . . . . C5 C 0.7122(3) 0.56324(17) 0.59529(18) 0.0281(6) Uani 1 1 d . . . . . C6 C 0.6290(3) 0.55693(19) 0.5287(2) 0.0341(7) Uani 1 1 d . . . . . H6 H 0.573(3) 0.590(2) 0.515(2) 0.028(9) Uiso 1 1 d . . . . . C7 C 0.6561(3) 0.4929(2) 0.4859(2) 0.0383(7) Uani 1 1 d . . . . . H7 H 0.617(3) 0.476(2) 0.440(2) 0.041(10) Uiso 1 1 d . . . . . C8 C 0.7548(3) 0.45941(19) 0.5259(2) 0.0359(7) Uani 1 1 d . . . . . H8 H 0.792(3) 0.419(2) 0.512(2) 0.040(10) Uiso 1 1 d . . . . . C9 C 0.7889(3) 0.50263(17) 0.59383(19) 0.0295(6) Uani 1 1 d . . . . . H9 H 0.851(3) 0.496(2) 0.628(2) 0.032(9) Uiso 1 1 d . . . . . C10 C 0.8666(3) 0.66651(18) 0.50385(18) 0.0302(6) Uani 1 1 d . . . . . C11 C 0.7834(3) 0.6651(2) 0.43717(19) 0.0355(7) Uani 1 1 d . . . . . H11 H 0.722(3) 0.694(2) 0.428(2) 0.037(10) Uiso 1 1 d . . . . . C12 C 0.8107(4) 0.6057(2) 0.3882(2) 0.0430(8) Uani 1 1 d . . . . . H12 H 0.770(4) 0.593(3) 0.345(3) 0.061(14) Uiso 1 1 d . . . . . C13 C 0.9108(3) 0.5713(2) 0.4239(2) 0.0417(8) Uani 1 1 d . . . . . H13 H 0.944(4) 0.531(3) 0.410(3) 0.057(13) Uiso 1 1 d . . . . . C14 C 0.9461(3) 0.60902(19) 0.4953(2) 0.0342(7) Uani 1 1 d . . . . . H14 H 1.010(3) 0.599(2) 0.5317(19) 0.026(8) Uiso 1 1 d . . . . . C15 C 0.5888(3) 0.88528(18) 0.73634(19) 0.0329(7) Uani 1 1 d . . . . . H15 H 0.544(3) 0.903(2) 0.772(2) 0.045(11) Uiso 1 1 d . . . . . C16 C 0.6482(3) 0.92712(19) 0.6935(2) 0.0351(7) Uani 1 1 d . . . . . H16 H 0.650(3) 0.982(3) 0.699(2) 0.050(12) Uiso 1 1 d . . . . . C17 C 0.4438(3) 0.76122(18) 0.69678(18) 0.0300(6) Uani 1 1 d . . . . . C18 C 0.3582(3) 0.8126(2) 0.7046(2) 0.0406(8) Uani 1 1 d . . . . . H18 H 0.377(3) 0.857(2) 0.724(2) 0.035(10) Uiso 1 1 d . . . . . C19 C 0.2465(3) 0.7935(2) 0.6858(3) 0.0503(10) Uani 1 1 d . . . . . H19 H 0.184(4) 0.834(3) 0.693(3) 0.069(14) Uiso 1 1 d . . . . . C20 C 0.2167(3) 0.7222(2) 0.6614(2) 0.0456(9) Uani 1 1 d . . . . . H20 H 0.137(4) 0.710(3) 0.649(3) 0.060(13) Uiso 1 1 d . . . . . C21 C 0.3001(3) 0.6700(2) 0.6535(2) 0.0415(8) Uani 1 1 d . . . . . H21 H 0.280(3) 0.621(2) 0.636(2) 0.041(10) Uiso 1 1 d . . . . . C22 C 0.4123(3) 0.6902(2) 0.6692(2) 0.0391(8) Uani 1 1 d . . . . . H22 H 0.459(4) 0.659(3) 0.664(2) 0.050(12) Uiso 1 1 d . . . . . C23 C 0.6169(3) 0.75035(19) 0.82453(19) 0.0362(7) Uani 1 1 d . . . . . C24 C 0.5621(4) 0.6876(3) 0.8478(2) 0.0530(10) Uani 1 1 d . . . . . H24 H 0.502(4) 0.665(3) 0.808(3) 0.070(15) Uiso 1 1 d . . . . . C25 C 0.5872(5) 0.6601(3) 0.9229(3) 0.0682(14) Uani 1 1 d . . . . . H25 H 0.556(5) 0.621(3) 0.940(3) 0.076(17) Uiso 1 1 d . . . . . C26 C 0.6651(5) 0.6954(3) 0.9755(2) 0.0625(13) Uani 1 1 d . . . . . H26 H 0.681(4) 0.674(3) 1.025(3) 0.070(15) Uiso 1 1 d . . . . . C27 C 0.7206(5) 0.7569(3) 0.9529(2) 0.0569(11) Uani 1 1 d . . . . . H27 H 0.775(4) 0.780(3) 0.981(3) 0.056(13) Uiso 1 1 d . . . . . C28 C 0.6982(4) 0.7844(2) 0.8769(2) 0.0440(8) Uani 1 1 d . . . . . H28 H 0.745(3) 0.822(2) 0.863(2) 0.035(10) Uiso 1 1 d . . . . . C29 C 0.6979(3) 0.92158(17) 0.53312(19) 0.0316(7) Uani 1 1 d . . . . . C30 C 0.7061(3) 0.8810(2) 0.4658(2) 0.0408(8) Uani 1 1 d . . . . . H30 H 0.730(4) 0.826(3) 0.470(2) 0.050(12) Uiso 1 1 d . . . . . C31 C 0.6785(4) 0.9130(2) 0.3923(2) 0.0470(9) Uani 1 1 d . . . . . H31 H 0.679(4) 0.887(3) 0.346(3) 0.060(14) Uiso 1 1 d . . . . . C32 C 0.6417(3) 0.9852(2) 0.3860(2) 0.0479(9) Uani 1 1 d . . . . . H32 H 0.621(4) 1.003(3) 0.335(3) 0.053(12) Uiso 1 1 d . . . . . C33 C 0.6342(4) 1.0264(2) 0.4519(3) 0.0538(10) Uani 1 1 d . . . . . H33 H 0.611(4) 1.074(3) 0.453(3) 0.066(15) Uiso 1 1 d . . . . . C34 C 0.6626(4) 0.9951(2) 0.5251(3) 0.0482(9) Uani 1 1 d . . . . . H34 H 0.665(4) 1.022(2) 0.567(2) 0.046(12) Uiso 1 1 d . . . . . C35 C 0.8732(3) 0.92441(17) 0.6588(2) 0.0339(7) Uani 1 1 d . . . . . C36 C 0.9010(3) 0.9516(2) 0.7343(2) 0.0451(9) Uani 1 1 d . . . . . H36 H 0.854(3) 0.942(2) 0.772(2) 0.038(10) Uiso 1 1 d . . . . . C37 C 1.0042(4) 0.9853(3) 0.7555(3) 0.0570(11) Uani 1 1 d . . . . . H37 H 1.020(4) 1.007(3) 0.807(3) 0.070(15) Uiso 1 1 d . . . . . C38 C 1.0808(3) 0.9931(2) 0.7029(3) 0.0526(10) Uani 1 1 d . . . . . H38 H 1.149(4) 1.014(3) 0.717(3) 0.054(12) Uiso 1 1 d . . . . . C39 C 1.0545(3) 0.9669(2) 0.6274(3) 0.0482(9) Uani 1 1 d . . . . . H39 H 1.101(4) 0.977(2) 0.593(2) 0.049(12) Uiso 1 1 d . . . . . C40 C 0.9506(3) 0.9333(2) 0.6054(2) 0.0393(8) Uani 1 1 d . . . . . H40 H 0.932(3) 0.918(2) 0.555(2) 0.040(10) Uiso 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 Se1 0.03035(15) 0.01720(16) 0.03258(16) -0.00040(11) 0.01027(11) -0.00021(12) Se2 0.02821(15) 0.01768(16) 0.03571(16) 0.00066(12) 0.00736(12) 0.00069(11) Fe1 0.0283(2) 0.0148(2) 0.0305(2) -0.00122(17) 0.00727(17) 0.00220(17) Fe2 0.0304(2) 0.0204(3) 0.0329(2) -0.00020(19) 0.00518(18) 0.00200(18) Fe3 0.0341(2) 0.0189(2) 0.0305(2) -0.00145(18) 0.00730(18) 0.00220(19) P1 0.0306(4) 0.0208(4) 0.0316(4) -0.0043(3) 0.0078(3) 0.0022(3) P2 0.0330(4) 0.0154(4) 0.0357(4) -0.0011(3) 0.0054(3) 0.0025(3) O1 0.0428(14) 0.0482(17) 0.0428(13) -0.0018(11) -0.0071(11) 0.0005(11) O2 0.0525(15) 0.0360(15) 0.0518(15) -0.0094(12) -0.0034(12) 0.0174(12) O3 0.0556(16) 0.0407(16) 0.0631(17) -0.0129(13) -0.0016(13) -0.0099(13) O4 0.0745(19) 0.0538(19) 0.0416(15) 0.0110(13) 0.0096(13) 0.0070(15) C1 0.0383(17) 0.0195(16) 0.0403(17) 0.0009(12) 0.0117(14) 0.0026(12) C2 0.0399(17) 0.0212(16) 0.0344(16) -0.0015(12) 0.0019(13) 0.0022(13) C3 0.0422(18) 0.0298(19) 0.0399(17) -0.0022(14) 0.0034(14) 0.0033(14) C4 0.0447(18) 0.0294(19) 0.0406(19) 0.0026(14) 0.0056(14) 0.0007(14) C5 0.0335(15) 0.0162(15) 0.0353(15) -0.0010(12) 0.0073(12) -0.0017(12) C6 0.0302(15) 0.0265(17) 0.0456(18) -0.0012(14) 0.0042(13) -0.0016(13) C7 0.0415(18) 0.0314(19) 0.0419(18) -0.0096(14) 0.0046(14) -0.0071(14) C8 0.0488(19) 0.0189(17) 0.0417(17) -0.0047(13) 0.0131(14) -0.0025(14) C9 0.0355(16) 0.0176(15) 0.0360(15) 0.0015(12) 0.0074(13) 0.0023(12) C10 0.0357(16) 0.0217(16) 0.0356(16) 0.0020(12) 0.0138(12) 0.0009(12) C11 0.0472(19) 0.0254(17) 0.0349(16) 0.0046(13) 0.0087(14) 0.0006(14) C12 0.069(2) 0.032(2) 0.0295(17) -0.0008(14) 0.0134(16) -0.0009(17) C13 0.058(2) 0.0263(19) 0.0465(19) -0.0035(15) 0.0278(17) 0.0025(16) C14 0.0359(17) 0.0251(18) 0.0450(18) 0.0011(13) 0.0191(14) 0.0020(13) C15 0.0370(16) 0.0243(17) 0.0377(16) -0.0081(13) 0.0063(13) 0.0061(13) C16 0.0398(17) 0.0210(17) 0.0445(18) -0.0079(13) 0.0056(14) 0.0059(13) C17 0.0322(15) 0.0288(17) 0.0306(14) -0.0022(12) 0.0105(12) 0.0030(12) C18 0.0386(18) 0.030(2) 0.055(2) -0.0004(16) 0.0144(15) 0.0055(15) C19 0.0366(18) 0.041(2) 0.075(3) 0.006(2) 0.0149(18) 0.0087(16) C20 0.0314(17) 0.054(3) 0.053(2) 0.0050(18) 0.0088(15) 0.0003(16) C21 0.0364(18) 0.043(2) 0.0454(19) -0.0082(16) 0.0085(14) -0.0046(15) C22 0.0353(17) 0.034(2) 0.0486(19) -0.0113(15) 0.0075(14) 0.0036(15) C23 0.0446(18) 0.0309(19) 0.0339(16) -0.0060(13) 0.0080(13) 0.0049(14) C24 0.065(3) 0.050(3) 0.044(2) 0.0017(18) 0.0097(18) -0.014(2) C25 0.100(4) 0.060(3) 0.047(2) 0.012(2) 0.017(2) -0.019(3) C26 0.105(4) 0.047(3) 0.036(2) 0.0044(18) 0.010(2) 0.007(2) C27 0.083(3) 0.044(3) 0.040(2) -0.0072(18) -0.008(2) 0.005(2) C28 0.061(2) 0.030(2) 0.0406(18) -0.0026(15) 0.0022(16) 0.0031(17) C29 0.0322(15) 0.0185(15) 0.0436(17) 0.0042(13) 0.0031(13) -0.0009(12) C30 0.056(2) 0.0225(18) 0.0428(19) 0.0039(14) 0.0033(15) -0.0012(15) C31 0.063(2) 0.035(2) 0.041(2) 0.0060(16) -0.0014(17) -0.0087(17) C32 0.045(2) 0.043(2) 0.054(2) 0.0174(18) -0.0035(16) -0.0035(17) C33 0.060(2) 0.030(2) 0.071(3) 0.018(2) 0.007(2) 0.0140(18) C34 0.061(2) 0.028(2) 0.055(2) 0.0001(17) 0.0065(18) 0.0064(17) C35 0.0387(17) 0.0151(15) 0.0470(18) -0.0026(13) 0.0023(14) 0.0008(12) C36 0.048(2) 0.034(2) 0.053(2) -0.0089(17) 0.0048(17) 0.0008(16) C37 0.058(3) 0.043(3) 0.065(3) -0.017(2) -0.010(2) -0.0038(19) C38 0.041(2) 0.034(2) 0.080(3) -0.007(2) -0.0056(19) -0.0064(16) C39 0.042(2) 0.032(2) 0.071(3) 0.0045(19) 0.0065(19) -0.0034(16) C40 0.0390(18) 0.0290(19) 0.050(2) -0.0005(15) 0.0047(15) -0.0003(14) 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' Fe Fe -1.1336 3.1974 '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' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.7943 1.1372 '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 0 1 0 0.2747 0 -1 0 0.3137 -5 0 9 0.0512 5 0 -9 0.0230 -2 11 -1 0.2656 2 -11 0 0.3087 7 1 5 0.0338 -4 -5 9 0.1479 0 0 11 0.0411 2 -4 9 0.1204 -2 -1 -10 0.0329 4 1 9 0.0283 -4 -1 -9 0.0283 -6 0 -5 0.0187 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 Fe1 Se1 Fe2 69.268(19) . . ? C5 Se1 Fe1 113.23(9) . . ? C5 Se1 Fe2 110.76(9) . . ? Fe1 Se2 Fe2 68.625(18) . . ? C10 Se2 Fe1 112.10(9) . . ? C10 Se2 Fe2 112.76(9) . . ? Se1 Fe1 Se2 91.307(18) . . ? Se1 Fe1 Fe2 55.528(16) . . ? Se2 Fe1 Fe2 56.515(16) . . ? P1 Fe1 Se1 89.06(3) . . ? P1 Fe1 Se2 160.14(3) . . ? P1 Fe1 Fe2 108.53(3) . . ? P1 Fe1 P2 86.55(3) . . ? P2 Fe1 Se1 165.44(3) . . ? P2 Fe1 Se2 88.16(3) . . ? P2 Fe1 Fe2 113.04(3) . . ? C1 Fe1 Se1 98.53(10) . . ? C1 Fe1 Se2 104.81(10) . . ? C1 Fe1 Fe2 143.46(10) . . ? C1 Fe1 P1 94.76(11) . . ? C1 Fe1 P2 95.67(11) . . ? Se1 Fe2 Se2 89.932(19) . . ? Se1 Fe2 Fe1 55.204(16) . . ? Se2 Fe2 Fe1 54.860(16) . . ? C2 Fe2 Se1 106.00(11) . . ? C2 Fe2 Se2 98.44(10) . . ? C2 Fe2 Fe1 143.00(10) . . ? C2 Fe2 C4 94.10(16) . . ? C3 Fe2 Se1 149.36(12) . . ? C3 Fe2 Se2 90.39(11) . . ? C3 Fe2 Fe1 101.28(11) . . ? C3 Fe2 C2 104.25(16) . . ? C3 Fe2 C4 86.43(16) . . ? C4 Fe2 Se1 86.68(12) . . ? C4 Fe2 Se2 167.46(12) . . ? C4 Fe2 Fe1 113.93(12) . . ? C5 Fe3 C6 41.23(13) . . ? C5 Fe3 C7 68.97(13) . . ? C5 Fe3 C8 69.09(13) . . ? C5 Fe3 C9 41.21(12) . . ? C5 Fe3 C11 118.43(13) . . ? C5 Fe3 C12 155.42(15) . . ? C5 Fe3 C13 160.65(15) . . ? C5 Fe3 C14 122.32(13) . . ? C6 Fe3 C7 40.85(14) . . ? C6 Fe3 C8 68.81(14) . . ? C6 Fe3 C12 120.95(16) . . ? C6 Fe3 C13 157.91(16) . . ? C6 Fe3 C14 158.52(14) . . ? C7 Fe3 C8 40.56(15) . . ? C7 Fe3 C13 124.14(15) . . ? C8 Fe3 C13 110.49(14) . . ? C9 Fe3 C6 69.04(13) . . ? C9 Fe3 C7 68.45(14) . . ? C9 Fe3 C8 40.72(13) . . ? C9 Fe3 C12 162.62(14) . . ? C9 Fe3 C13 125.81(15) . . ? C9 Fe3 C14 107.67(14) . . ? C10 Fe3 C5 103.80(12) . . ? C10 Fe3 C6 120.81(13) . . ? C10 Fe3 C7 158.78(14) . . ? C10 Fe3 C8 157.28(14) . . ? C10 Fe3 C9 119.98(13) . . ? C10 Fe3 C11 41.23(14) . . ? C10 Fe3 C12 69.01(14) . . ? C10 Fe3 C13 68.81(13) . . ? C10 Fe3 C14 41.07(13) . . ? C11 Fe3 C6 104.75(15) . . ? C11 Fe3 C7 123.31(15) . . ? C11 Fe3 C8 161.22(14) . . ? C11 Fe3 C9 155.25(13) . . ? C11 Fe3 C12 40.87(14) . . ? C11 Fe3 C13 68.50(15) . . ? C11 Fe3 C14 68.91(14) . . ? C12 Fe3 C7 108.85(16) . . ? C12 Fe3 C8 126.16(14) . . ? C12 Fe3 C13 40.40(16) . . ? C14 Fe3 C7 159.44(14) . . ? C14 Fe3 C8 123.41(14) . . ? C14 Fe3 C12 68.46(16) . . ? C14 Fe3 C13 40.64(15) . . ? C15 P1 Fe1 108.88(11) . . ? C15 P1 C17 102.80(15) . . ? C15 P1 C23 102.88(15) . . ? C17 P1 Fe1 117.29(10) . . ? C17 P1 C23 101.46(16) . . ? C23 P1 Fe1 121.23(11) . . ? C16 P2 Fe1 108.91(12) . . ? C16 P2 C29 104.62(16) . . ? C16 P2 C35 100.59(16) . . ? C29 P2 Fe1 116.79(11) . . ? C29 P2 C35 100.39(15) . . ? C35 P2 Fe1 123.10(11) . . ? O1 C1 Fe1 177.1(3) . . ? O2 C2 Fe2 177.2(3) . . ? O3 C3 Fe2 173.5(3) . . ? O4 C4 Fe2 175.0(3) . . ? Se1 C5 Fe3 131.63(16) . . ? C6 C5 Se1 125.8(2) . . ? C6 C5 Fe3 70.26(18) . . ? C9 C5 Se1 125.6(2) . . ? C9 C5 Fe3 70.24(18) . . ? C9 C5 C6 108.1(3) . . ? Fe3 C6 H6 123(2) . . ? C5 C6 Fe3 68.51(18) . . ? C5 C6 H6 125(2) . . ? C5 C6 C7 107.6(3) . . ? C7 C6 Fe3 70.1(2) . . ? C7 C6 H6 127(2) . . ? Fe3 C7 H7 126(2) . . ? C6 C7 Fe3 69.04(19) . . ? C6 C7 H7 126(3) . . ? C8 C7 Fe3 69.9(2) . . ? C8 C7 C6 108.5(3) . . ? C8 C7 H7 126(2) . . ? Fe3 C8 H8 126(3) . . ? C7 C8 Fe3 69.6(2) . . ? C7 C8 H8 128(2) . . ? C7 C8 C9 107.7(3) . . ? C9 C8 Fe3 68.95(18) . . ? C9 C8 H8 124(2) . . ? Fe3 C9 H9 123(2) . . ? C5 C9 Fe3 68.55(18) . . ? C5 C9 H9 125(2) . . ? C8 C9 Fe3 70.34(19) . . ? C8 C9 C5 108.2(3) . . ? C8 C9 H9 127(2) . . ? Se2 C10 Fe3 130.63(16) . . ? C11 C10 Se2 126.2(2) . . ? C11 C10 Fe3 70.09(19) . . ? C14 C10 Se2 125.2(3) . . ? C14 C10 Fe3 70.61(19) . . ? C14 C10 C11 108.1(3) . . ? Fe3 C11 H11 123(3) . . ? C10 C11 Fe3 68.68(19) . . ? C10 C11 H11 127(2) . . ? C12 C11 Fe3 70.1(2) . . ? C12 C11 C10 107.7(3) . . ? C12 C11 H11 125(2) . . ? Fe3 C12 H12 125(3) . . ? C11 C12 Fe3 69.01(19) . . ? C11 C12 H12 124(3) . . ? C13 C12 Fe3 70.2(2) . . ? C13 C12 C11 108.2(3) . . ? C13 C12 H12 127(3) . . ? Fe3 C13 H13 122(3) . . ? C12 C13 Fe3 69.4(2) . . ? C12 C13 H13 129(3) . . ? C12 C13 C14 108.2(3) . . ? C14 C13 Fe3 69.21(19) . . ? C14 C13 H13 123(3) . . ? Fe3 C14 H14 127(2) . . ? C10 C14 Fe3 68.33(18) . . ? C10 C14 C13 107.8(3) . . ? C10 C14 H14 124(2) . . ? C13 C14 Fe3 70.2(2) . . ? C13 C14 H14 128(2) . . ? P1 C15 H15 117(3) . . ? C16 C15 P1 118.4(2) . . ? C16 C15 H15 125(3) . . ? P2 C16 H16 121(2) . . ? C15 C16 P2 117.2(3) . . ? C15 C16 H16 122(2) . . ? C18 C17 P1 121.5(3) . . ? C18 C17 C22 117.8(3) . . ? C22 C17 P1 120.6(2) . . ? C17 C18 H18 119(3) . . ? C19 C18 C17 120.8(4) . . ? C19 C18 H18 121(2) . . ? C18 C19 H19 118(3) . . ? C18 C19 C20 120.7(4) . . ? C20 C19 H19 121(3) . . ? C19 C20 H20 119(3) . . ? C19 C20 C21 119.7(4) . . ? C21 C20 H20 121(3) . . ? C20 C21 H21 120(2) . . ? C22 C21 C20 119.6(4) . . ? C22 C21 H21 120(2) . . ? C17 C22 H22 121(3) . . ? C21 C22 C17 121.4(3) . . ? C21 C22 H22 118(3) . . ? C24 C23 P1 121.4(3) . . ? C28 C23 P1 119.2(3) . . ? C28 C23 C24 119.2(3) . . ? C23 C24 H24 116(3) . . ? C25 C24 C23 120.3(4) . . ? C25 C24 H24 123(3) . . ? C24 C25 H25 124(4) . . ? C26 C25 C24 120.3(5) . . ? C26 C25 H25 116(4) . . ? C25 C26 H26 117(3) . . ? C27 C26 C25 119.8(4) . . ? C27 C26 H26 123(3) . . ? C26 C27 H27 126(3) . . ? C26 C27 C28 120.6(4) . . ? C28 C27 H27 113(3) . . ? C23 C28 C27 119.7(4) . . ? C23 C28 H28 123(2) . . ? C27 C28 H28 117(2) . . ? C30 C29 P2 120.4(2) . . ? C30 C29 C34 118.0(3) . . ? C34 C29 P2 121.6(3) . . ? C29 C30 H30 119(2) . . ? C29 C30 C31 120.8(3) . . ? C31 C30 H30 120(2) . . ? C30 C31 H31 124(3) . . ? C32 C31 C30 120.0(4) . . ? C32 C31 H31 116(3) . . ? C31 C32 H32 116(3) . . ? C33 C32 C31 120.0(4) . . ? C33 C32 H32 124(3) . . ? C32 C33 H33 126(3) . . ? C32 C33 C34 120.3(4) . . ? C34 C33 H33 114(3) . . ? C29 C34 H34 118(3) . . ? C33 C34 C29 120.9(4) . . ? C33 C34 H34 121(3) . . ? C36 C35 P2 120.9(3) . . ? C36 C35 C40 118.5(3) . . ? C40 C35 P2 120.6(3) . . ? C35 C36 H36 120(2) . . ? C37 C36 C35 120.3(4) . . ? C37 C36 H36 119(2) . . ? C36 C37 H37 119(3) . . ? C38 C37 C36 121.0(4) . . ? C38 C37 H37 120(3) . . ? C37 C38 H38 121(3) . . ? C37 C38 C39 119.7(4) . . ? C39 C38 H38 119(3) . . ? C38 C39 H39 119(3) . . ? C38 C39 C40 119.8(4) . . ? C40 C39 H39 121(3) . . ? C35 C40 H40 120(3) . . ? C39 C40 C35 120.7(4) . . ? C39 C40 H40 120(3) . . ? 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 Se1 Fe1 2.3581(5) . ? Se1 Fe2 2.3674(6) . ? Se1 C5 1.916(3) . ? Se2 Fe1 2.3584(5) . ? Se2 Fe2 2.4054(6) . ? Se2 C10 1.920(3) . ? Fe1 Fe2 2.6857(7) . ? Fe1 P1 2.1989(9) . ? Fe1 P2 2.2094(9) . ? Fe1 C1 1.765(3) . ? Fe2 C2 1.782(3) . ? Fe2 C3 1.779(4) . ? Fe2 C4 1.784(4) . ? Fe3 C5 2.013(3) . ? Fe3 C6 2.036(3) . ? Fe3 C7 2.050(3) . ? Fe3 C8 2.054(3) . ? Fe3 C9 2.035(3) . ? Fe3 C10 2.012(3) . ? Fe3 C11 2.030(3) . ? Fe3 C12 2.045(3) . ? Fe3 C13 2.055(3) . ? Fe3 C14 2.042(3) . ? P1 C15 1.822(3) . ? P1 C17 1.828(3) . ? P1 C23 1.834(3) . ? P2 C16 1.828(3) . ? P2 C29 1.835(3) . ? P2 C35 1.837(3) . ? O1 C1 1.141(4) . ? O2 C2 1.147(4) . ? O3 C3 1.152(4) . ? O4 C4 1.140(4) . ? C5 C6 1.426(5) . ? C5 C9 1.425(4) . ? C6 H6 0.90(4) . ? C6 C7 1.426(5) . ? C7 H7 0.92(4) . ? C7 C8 1.422(5) . ? C8 H8 0.90(4) . ? C8 C9 1.423(5) . ? C9 H9 0.89(4) . ? C10 C11 1.423(5) . ? C10 C14 1.422(4) . ? C11 H11 0.90(4) . ? C11 C12 1.423(5) . ? C12 H12 0.87(5) . ? C12 C13 1.416(6) . ? C13 H13 0.88(5) . ? C13 C14 1.423(5) . ? C14 H14 0.94(3) . ? C15 H15 0.91(4) . ? C15 C16 1.319(5) . ? C16 H16 0.99(4) . ? C17 C18 1.395(5) . ? C17 C22 1.397(5) . ? C18 H18 0.88(4) . ? C18 C19 1.375(6) . ? C19 H19 1.07(5) . ? C19 C20 1.381(6) . ? C20 H20 0.98(5) . ? C20 C21 1.386(5) . ? C21 H21 0.96(4) . ? C21 C22 1.380(5) . ? C22 H22 0.81(5) . ? C23 C24 1.387(6) . ? C23 C28 1.383(5) . ? C24 H24 1.02(5) . ? C24 C25 1.384(6) . ? C25 H25 0.86(6) . ? C25 C26 1.373(7) . ? C26 H26 0.93(5) . ? C26 C27 1.369(7) . ? C27 H27 0.86(5) . ? C27 C28 1.393(6) . ? C28 H28 0.93(4) . ? C29 C30 1.383(5) . ? C29 C34 1.388(5) . ? C30 H30 1.03(4) . ? C30 C31 1.394(5) . ? C31 H31 0.93(5) . ? C31 C32 1.370(6) . ? C32 H32 0.94(4) . ? C32 C33 1.367(7) . ? C33 H33 0.90(5) . ? C33 C34 1.385(6) . ? C34 H34 0.87(4) . ? C35 C36 1.390(5) . ? C35 C40 1.392(5) . ? C36 H36 0.92(4) . ? C36 C37 1.382(6) . ? C37 H37 0.96(5) . ? C37 C38 1.371(7) . ? C38 H38 0.89(5) . ? C38 C39 1.383(6) . ? C39 H39 0.88(4) . ? C39 C40 1.390(5) . ? C40 H40 0.91(4) . ? 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 Se1 C5 C6 Fe3 127.7(2) . . . . ? Se1 C5 C6 C7 -172.8(2) . . . . ? Se1 C5 C9 Fe3 -127.7(2) . . . . ? Se1 C5 C9 C8 173.0(2) . . . . ? Se2 C10 C11 Fe3 -126.4(2) . . . . ? Se2 C10 C11 C12 174.1(2) . . . . ? Se2 C10 C14 Fe3 126.6(2) . . . . ? Se2 C10 C14 C13 -174.1(2) . . . . ? Fe1 P1 C15 C16 3.0(3) . . . . ? Fe1 P1 C17 C18 -131.5(3) . . . . ? Fe1 P1 C17 C22 49.9(3) . . . . ? Fe1 P1 C23 C24 -98.3(3) . . . . ? Fe1 P1 C23 C28 76.6(3) . . . . ? Fe1 P2 C16 C15 3.0(3) . . . . ? Fe1 P2 C29 C30 -30.6(3) . . . . ? Fe1 P2 C29 C34 151.0(3) . . . . ? Fe1 P2 C35 C36 -91.5(3) . . . . ? Fe1 P2 C35 C40 89.5(3) . . . . ? Fe3 C5 C6 C7 59.5(2) . . . . ? Fe3 C5 C9 C8 -59.4(2) . . . . ? Fe3 C6 C7 C8 58.9(2) . . . . ? Fe3 C7 C8 C9 58.6(2) . . . . ? Fe3 C8 C9 C5 58.3(2) . . . . ? Fe3 C10 C11 C12 -59.5(2) . . . . ? Fe3 C10 C14 C13 59.3(2) . . . . ? Fe3 C11 C12 C13 -59.4(3) . . . . ? Fe3 C12 C13 C14 -58.5(2) . . . . ? Fe3 C13 C14 C10 -58.1(2) . . . . ? P1 C15 C16 P2 -3.8(4) . . . . ? P1 C17 C18 C19 -178.5(3) . . . . ? P1 C17 C22 C21 175.7(3) . . . . ? P1 C23 C24 C25 175.9(4) . . . . ? P1 C23 C28 C27 -177.4(3) . . . . ? P2 C29 C30 C31 -179.1(3) . . . . ? P2 C29 C34 C33 179.8(3) . . . . ? P2 C35 C36 C37 179.9(3) . . . . ? P2 C35 C40 C39 -179.5(3) . . . . ? C5 C6 C7 Fe3 -58.5(2) . . . . ? C5 C6 C7 C8 0.4(4) . . . . ? C6 C5 C9 Fe3 60.3(2) . . . . ? C6 C5 C9 C8 1.0(4) . . . . ? C6 C7 C8 Fe3 -58.4(2) . . . . ? C6 C7 C8 C9 0.2(4) . . . . ? C7 C8 C9 Fe3 -59.0(2) . . . . ? C7 C8 C9 C5 -0.7(4) . . . . ? C9 C5 C6 Fe3 -60.3(2) . . . . ? C9 C5 C6 C7 -0.9(4) . . . . ? C10 C11 C12 Fe3 58.6(2) . . . . ? C10 C11 C12 C13 -0.8(4) . . . . ? C11 C10 C14 Fe3 -60.3(2) . . . . ? C11 C10 C14 C13 -1.0(4) . . . . ? C11 C12 C13 Fe3 58.7(3) . . . . ? C11 C12 C13 C14 0.2(4) . . . . ? C12 C13 C14 Fe3 58.7(3) . . . . ? C12 C13 C14 C10 0.5(4) . . . . ? C14 C10 C11 Fe3 60.6(2) . . . . ? C14 C10 C11 C12 1.1(4) . . . . ? C15 P1 C17 C18 -12.1(3) . . . . ? C15 P1 C17 C22 169.3(3) . . . . ? C15 P1 C23 C24 139.9(3) . . . . ? C15 P1 C23 C28 -45.2(3) . . . . ? C16 P2 C29 C30 -151.1(3) . . . . ? C16 P2 C29 C34 30.6(3) . . . . ? C16 P2 C35 C36 29.5(3) . . . . ? C16 P2 C35 C40 -149.5(3) . . . . ? C17 P1 C15 C16 -122.1(3) . . . . ? C17 P1 C23 C24 33.7(4) . . . . ? C17 P1 C23 C28 -151.4(3) . . . . ? C17 C18 C19 C20 2.3(6) . . . . ? C18 C17 C22 C21 -3.0(5) . . . . ? C18 C19 C20 C21 -2.1(6) . . . . ? C19 C20 C21 C22 -0.7(6) . . . . ? C20 C21 C22 C17 3.2(6) . . . . ? C22 C17 C18 C19 0.2(5) . . . . ? C23 P1 C15 C16 132.8(3) . . . . ? C23 P1 C17 C18 94.1(3) . . . . ? C23 P1 C17 C22 -84.5(3) . . . . ? C23 C24 C25 C26 1.2(8) . . . . ? C24 C23 C28 C27 -2.4(6) . . . . ? C24 C25 C26 C27 -1.9(9) . . . . ? C25 C26 C27 C28 0.4(8) . . . . ? C26 C27 C28 C23 1.7(7) . . . . ? C28 C23 C24 C25 1.0(7) . . . . ? C29 P2 C16 C15 128.5(3) . . . . ? C29 P2 C35 C36 136.7(3) . . . . ? C29 P2 C35 C40 -42.3(3) . . . . ? C29 C30 C31 C32 -0.7(6) . . . . ? C30 C29 C34 C33 1.4(6) . . . . ? C30 C31 C32 C33 1.4(6) . . . . ? C31 C32 C33 C34 -0.7(7) . . . . ? C32 C33 C34 C29 -0.7(7) . . . . ? C34 C29 C30 C31 -0.7(6) . . . . ? C35 P2 C16 C15 -127.7(3) . . . . ? C35 P2 C29 C30 105.0(3) . . . . ? C35 P2 C29 C34 -73.4(3) . . . . ? C35 C36 C37 C38 0.3(7) . . . . ? C36 C35 C40 C39 1.5(5) . . . . ? C36 C37 C38 C39 0.1(7) . . . . ? C37 C38 C39 C40 0.3(6) . . . . ? C38 C39 C40 C35 -1.1(6) . . . . ? C40 C35 C36 C37 -1.1(6) . . . . ? 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 0.0000 1.0000 0.0000 0.0229 0.0092 0.0821 -0.0000 -1.0000 -0.0000 -0.0229 -0.0092 -0.0821 -5.3687 0.1631 8.9453 -0.0426 -0.9897 0.1370 5.2802 0.4783 -9.0385 0.0428 0.9959 -0.0803 -1.9796 11.1999 -0.8994 -0.0007 0.0277 0.9996 2.3722 -11.0844 0.1972 0.0040 0.0492 -0.9988 6.5343 0.5503 4.7750 0.9638 0.1282 -0.2338 -4.0303 -5.2767 8.7498 -0.0393 -0.9332 -0.3572 -0.3027 0.1173 11.1458 0.6080 -0.7908 -0.0707 2.4379 -3.8409 9.4504 0.7052 -0.5197 -0.4824 -1.7983 -0.7463 -10.4566 -0.8012 0.5915 0.0905 4.1888 0.7203 8.5704 0.9410 -0.2955 -0.1649 -4.1888 -0.7203 -8.5704 -0.9410 0.2955 0.1649 -6.4035 -0.2732 -5.1011 -0.9625 -0.0940 0.2544