#------------------------------------------------------------------------------ #$Date: 2026-06-12 23:54:06 +0100 (Fri, 12 Jun 2026) $ #$Revision: 306560 $ #$URL: svn://www.crystallography.net/cod/cif/7/72/11/7721122.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_7721122 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 'C48 H36 Fe4 O4 P2 Se2, C H2 Cl2' _chemical_formula_sum 'C49 H38 Cl2 Fe4 O4 P2 Se2' _chemical_formula_weight 1204.95 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_date 2023-08-03 _audit_creation_method ; Olex2 1.5 (compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748) ; _audit_update_record ; 2026-04-22 deposited with the CCDC. 2026-06-11 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90.565(3) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 44.7746(16) _cell_length_b 9.8242(3) _cell_length_c 21.6955(8) _cell_measurement_reflns_used 10710 _cell_measurement_temperature 150(1) _cell_measurement_theta_max 73.1450 _cell_measurement_theta_min 4.5080 _cell_volume 9542.8(6) _computing_cell_refinement 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXS (Sheldrick, 2008)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 150(1) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.2031 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.967 _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 14.00 50.00 1.00 2.35 -- 42.62 57.00 120.00 36 2 \w 91.00 116.00 1.00 2.35 -- 42.62 57.00 120.00 25 3 \w 92.00 131.00 1.00 9.39 -- 106.36 45.00 150.00 39 4 \w 100.00 178.00 1.00 9.39 -- 106.36 125.00 120.00 78 5 \w 81.00 173.00 1.00 9.39 -- 106.36 61.00 -60.00 92 6 \w 137.00 166.00 1.00 9.39 -- 106.36 125.00 -90.00 29 7 \w 123.00 149.00 1.00 9.39 -- 106.36 125.00-180.00 26 8 \w 79.00 163.00 1.00 9.39 -- 106.36 61.00-180.00 84 9 \w 29.00 104.00 1.00 9.39 -- 106.36 -95.00 60.00 75 10 \w -56.00 24.00 1.00 2.35 -- -42.62 38.00-180.00 80 11 \w -67.00 32.00 1.00 2.35 -- -42.62 38.00 -60.00 99 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0274819000 _diffrn_orient_matrix_UB_12 -0.0829226000 _diffrn_orient_matrix_UB_13 0.0197543000 _diffrn_orient_matrix_UB_21 -0.0205297000 _diffrn_orient_matrix_UB_22 0.0994759000 _diffrn_orient_matrix_UB_23 -0.0353155000 _diffrn_orient_matrix_UB_31 0.0027263000 _diffrn_orient_matrix_UB_32 -0.0882773000 _diffrn_orient_matrix_UB_33 -0.0583760000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0379 _diffrn_reflns_av_unetI/netI 0.0427 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.967 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_h_min -54 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 18709 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.967 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 73.468 _diffrn_reflns_theta_min 4.075 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 13.320 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.23575 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear red' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.677 _exptl_crystal_description block _exptl_crystal_F_000 4800 _exptl_crystal_preparation 'Crystal cut from large 'block'' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.16 _refine_diff_density_max 2.245 _refine_diff_density_min -1.787 _refine_diff_density_rms 0.155 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 568 _refine_ls_number_reflns 9303 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.033 _refine_ls_R_factor_all 0.0606 _refine_ls_R_factor_gt 0.0576 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1160P)^2^+30.6842P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1605 _refine_ls_wR_factor_ref 0.1647 _reflns_Friedel_coverage 0.000 _reflns_number_gt 8637 _reflns_number_total 9303 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL XSTR0800 in C2/c #15 REM reset to C2/c #15 CELL 1.54184 44.77455 9.8242 21.69546 90 90.5648 90 ZERR 8 0.0016 0.00028 0.00076 0 0.003 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H Cl Fe O P Se UNIT 392 304 16 32 32 16 16 L.S. 20 PLAN 20 BOND fmap 2 acta ABIN OMIT 0 0 4 OMIT -2 0 4 REM REM REM WGHT 0.116000 30.684200 FVAR 0.97173 SE1 7 0.607054 0.372717 0.204041 11.00000 0.02977 0.01883 = 0.01676 0.00270 -0.00103 0.00576 SE2 7 0.634824 0.172979 0.314519 11.00000 0.02078 0.01454 = 0.01710 0.00079 -0.00084 0.00288 FE1 4 0.588194 0.285478 0.298689 11.00000 0.01969 0.01483 = 0.01737 0.00040 -0.00175 0.00367 FE2 4 0.641360 0.404925 0.287198 11.00000 0.02485 0.01481 = 0.01749 0.00149 0.00014 -0.00030 FE3 4 0.637557 0.053447 0.157703 11.00000 0.02327 0.02000 = 0.01869 -0.00177 -0.00008 0.00365 FE4 4 0.627541 0.387775 0.496602 11.00000 0.01357 0.01514 = 0.01771 -0.00167 -0.00207 0.00134 P1 6 0.570934 0.260410 0.395174 11.00000 0.01458 0.01196 = 0.01851 -0.00151 -0.00171 0.00218 P2 6 0.672755 0.435521 0.366736 11.00000 0.01891 0.01508 = 0.02158 0.00144 0.00254 0.00063 O1 5 0.546344 0.511845 0.283047 11.00000 0.04897 0.04253 = 0.05050 0.01905 0.01144 0.02638 O2 5 0.550757 0.065769 0.250276 11.00000 0.03987 0.03698 = 0.03832 -0.00882 -0.00578 -0.00896 O3 5 0.611403 0.666018 0.306913 11.00000 0.05468 0.01838 = 0.03961 0.00027 -0.00624 0.01011 O4 5 0.686628 0.493730 0.200352 11.00000 0.06606 0.07071 = 0.03352 0.00922 0.01460 -0.03235 C1 1 0.562444 0.423921 0.290793 11.00000 0.03131 0.02812 = 0.02445 0.00632 0.00222 0.00832 C2 1 0.565454 0.151587 0.269815 11.00000 0.02935 0.02765 = 0.01713 0.00097 -0.00012 0.00407 C3 1 0.623131 0.563188 0.300473 11.00000 0.03649 0.02222 = 0.02779 0.00296 -0.00357 0.00095 C4 1 0.669851 0.454725 0.236269 11.00000 0.04663 0.03373 = 0.02524 0.00198 0.00119 -0.01355 C5 1 0.619240 0.237666 0.146046 11.00000 0.03218 0.02051 = 0.01771 0.00266 -0.00364 0.00866 C6 1 0.600140 0.137231 0.119485 11.00000 0.02579 0.02997 = 0.02483 0.00002 -0.00590 0.00623 AFIX 43 H6 2 0.580486 0.119927 0.130532 11.00000 -1.20000 AFIX 0 C7 1 0.616526 0.067666 0.072811 11.00000 0.04176 0.03173 = 0.01900 -0.00351 -0.00789 0.00900 AFIX 43 H7 2 0.609492 -0.003315 0.048301 11.00000 -1.20000 AFIX 0 C8 1 0.645431 0.126406 0.070629 11.00000 0.03731 0.03287 = 0.01760 0.00288 0.00316 0.00595 AFIX 43 H8 2 0.660658 0.100378 0.044272 11.00000 -1.20000 AFIX 0 C9 1 0.647243 0.231552 0.115387 11.00000 0.03627 0.02401 = 0.02139 0.00159 0.00403 -0.00004 AFIX 43 H9 2 0.663737 0.286604 0.123304 11.00000 -1.20000 AFIX 0 C10 1 0.623526 -0.062845 0.230146 11.00000 0.04647 0.01810 = 0.02154 0.00138 0.00241 -0.00012 AFIX 43 H10 2 0.603987 -0.076060 0.243006 11.00000 -1.20000 AFIX 0 C11 1 0.639171 -0.145284 0.188044 11.00000 0.05516 0.02064 = 0.02739 -0.00355 -0.00187 0.00820 AFIX 43 H11 2 0.631648 -0.221731 0.167937 11.00000 -1.20000 AFIX 0 C12 1 0.668401 -0.091153 0.181737 11.00000 0.04007 0.03658 = 0.02867 -0.00451 -0.00492 0.02154 AFIX 43 H12 2 0.683278 -0.125673 0.156534 11.00000 -1.20000 AFIX 0 C13 1 0.670991 0.024570 0.220481 11.00000 0.02985 0.02841 = 0.03568 -0.00314 -0.00179 0.01435 AFIX 43 H13 2 0.687968 0.077939 0.225931 11.00000 -1.20000 AFIX 0 C14 1 0.643001 0.044429 0.249503 11.00000 0.03274 0.01833 = 0.01848 0.00101 0.00072 0.00803 C15 1 0.566334 0.089621 0.427824 11.00000 0.02091 0.01458 = 0.02083 0.00273 -0.00309 0.00089 C16 1 0.580807 -0.022373 0.403496 11.00000 0.02912 0.01855 = 0.03128 0.00071 0.00548 0.00451 AFIX 43 H16 2 0.594265 -0.010900 0.371534 11.00000 -1.20000 AFIX 0 C17 1 0.575314 -0.152486 0.426676 11.00000 0.03972 0.01702 = 0.04018 0.00248 0.00337 0.00783 AFIX 43 H17 2 0.584871 -0.227441 0.409652 11.00000 -1.20000 AFIX 0 C18 1 0.555656 -0.170285 0.474993 11.00000 0.03483 0.01981 = 0.04069 0.01012 -0.00012 0.00063 AFIX 43 H18 2 0.552219 -0.256911 0.490687 11.00000 -1.20000 AFIX 0 C19 1 0.541164 -0.059005 0.499816 11.00000 0.02150 0.02799 = 0.03045 0.00611 0.00136 0.00083 AFIX 43 H19 2 0.528047 -0.070826 0.532353 11.00000 -1.20000 AFIX 0 C20 1 0.546163 0.070328 0.476251 11.00000 0.02114 0.02175 = 0.02379 0.00246 0.00188 0.00072 AFIX 43 H20 2 0.536101 0.144617 0.492618 11.00000 -1.20000 AFIX 0 C21 1 0.531754 0.317447 0.396179 11.00000 0.01793 0.02282 = 0.02168 0.00186 -0.00145 0.00053 C22 1 0.510451 0.239153 0.364424 11.00000 0.02384 0.03543 = 0.02629 -0.00399 0.00024 -0.00387 AFIX 43 H22 2 0.515959 0.156965 0.346557 11.00000 -1.20000 AFIX 0 C23 1 0.481222 0.284000 0.359620 11.00000 0.01862 0.06291 = 0.03353 -0.00720 -0.00354 -0.00673 AFIX 43 H23 2 0.467183 0.231282 0.338641 11.00000 -1.20000 AFIX 0 C24 1 0.472627 0.406221 0.385622 11.00000 0.01911 0.07123 = 0.04156 0.00554 0.00009 0.01537 AFIX 43 H24 2 0.452967 0.435858 0.381854 11.00000 -1.20000 AFIX 0 C25 1 0.493305 0.483615 0.417060 11.00000 0.02793 0.04106 = 0.04245 -0.00837 -0.00059 0.01553 AFIX 43 H25 2 0.487548 0.565684 0.434699 11.00000 -1.20000 AFIX 0 C26 1 0.523004 0.439905 0.422768 11.00000 0.02268 0.03009 = 0.03268 -0.00665 -0.00260 0.00734 AFIX 43 H26 2 0.536846 0.492645 0.444291 11.00000 -1.20000 AFIX 0 C27 1 0.586246 0.359062 0.458706 11.00000 0.01242 0.01964 = 0.02163 -0.00520 -0.00095 0.00344 C28 1 0.585666 0.330410 0.523212 11.00000 0.01598 0.02531 = 0.02571 -0.00549 -0.00078 0.00051 AFIX 43 H28 2 0.580281 0.248159 0.541182 11.00000 -1.20000 AFIX 0 C29 1 0.594807 0.450310 0.555108 11.00000 0.01987 0.03616 = 0.02535 -0.01175 0.00121 0.00307 AFIX 43 H29 2 0.596513 0.459566 0.597657 11.00000 -1.20000 AFIX 0 C30 1 0.600887 0.553480 0.511033 11.00000 0.01817 0.02187 = 0.03452 -0.01249 -0.00532 0.00580 AFIX 43 H30 2 0.607173 0.641657 0.519820 11.00000 -1.20000 AFIX 0 C31 1 0.595743 0.499073 0.451591 11.00000 0.01699 0.01493 = 0.03016 -0.00125 -0.00459 0.00492 AFIX 43 H31 2 0.598046 0.545026 0.414464 11.00000 -1.20000 AFIX 0 C32 1 0.657351 0.248707 0.463623 11.00000 0.01734 0.01677 = 0.02338 -0.00064 0.00248 0.00357 AFIX 43 H32 2 0.653236 0.176562 0.437117 11.00000 -1.20000 AFIX 0 C33 1 0.657097 0.243058 0.528843 11.00000 0.01667 0.01909 = 0.02868 0.00421 -0.00171 0.00409 AFIX 43 H33 2 0.652652 0.166865 0.552480 11.00000 -1.20000 AFIX 0 C34 1 0.664855 0.374761 0.552081 11.00000 0.01733 0.03080 = 0.02809 0.00030 -0.00479 0.00201 AFIX 43 H34 2 0.666205 0.398996 0.593452 11.00000 -1.20000 AFIX 0 C35 1 0.670156 0.462394 0.501138 11.00000 0.01584 0.02409 = 0.02879 -0.00120 -0.00397 -0.00436 AFIX 43 H35 2 0.675884 0.553267 0.503384 11.00000 -1.20000 AFIX 0 C36 1 0.665068 0.385237 0.445254 11.00000 0.01704 0.01690 = 0.02455 -0.00043 0.00265 0.00231 C37 1 0.709339 0.349132 0.361065 11.00000 0.02155 0.02381 = 0.03542 0.00121 0.00862 0.00133 C38 1 0.729557 0.358157 0.410209 11.00000 0.02917 0.07366 = 0.04478 -0.01125 0.00101 0.01752 AFIX 43 H38 2 0.725066 0.412342 0.444023 11.00000 -1.20000 AFIX 0 C39 1 0.756372 0.286841 0.409087 11.00000 0.02941 0.09539 = 0.06601 -0.00285 0.00377 0.02549 AFIX 43 H39 2 0.769839 0.294196 0.441827 11.00000 -1.20000 AFIX 0 C40 1 0.762933 0.205498 0.359524 11.00000 0.02107 0.04914 = 0.08746 0.00344 0.01746 0.00892 AFIX 43 H40 2 0.780736 0.156774 0.358917 11.00000 -1.20000 AFIX 0 C41 1 0.743440 0.196316 0.311517 11.00000 0.02828 0.04023 = 0.07719 -0.01948 0.02123 0.00020 AFIX 43 H41 2 0.748019 0.140840 0.278186 11.00000 -1.20000 AFIX 0 C42 1 0.716472 0.269057 0.311233 11.00000 0.02669 0.03318 = 0.04744 -0.00721 0.01047 0.00000 AFIX 43 H42 2 0.703495 0.263232 0.277602 11.00000 -1.20000 AFIX 0 C43 1 0.682698 0.616275 0.372482 11.00000 0.02902 0.01726 = 0.02779 0.00261 -0.00175 -0.00402 C44 1 0.706666 0.667199 0.340225 11.00000 0.04037 0.03128 = 0.04814 -0.00051 0.01387 -0.00944 AFIX 43 H44 2 0.719598 0.607761 0.320469 11.00000 -1.20000 AFIX 0 C45 1 0.711590 0.806609 0.337087 11.00000 0.05954 0.03745 = 0.06051 0.00805 0.01717 -0.01974 AFIX 43 H45 2 0.727673 0.839810 0.314834 11.00000 -1.20000 AFIX 0 C46 1 0.692963 0.895705 0.366486 11.00000 0.06121 0.02175 = 0.04887 0.00555 0.00395 -0.01245 AFIX 43 H46 2 0.696467 0.988872 0.364231 11.00000 -1.20000 AFIX 0 C47 1 0.668795 0.846656 0.399726 11.00000 0.04536 0.02010 = 0.03698 0.00100 -0.00516 -0.00073 AFIX 43 H47 2 0.656220 0.906600 0.420141 11.00000 -1.20000 AFIX 0 C48 1 0.663632 0.706963 0.402111 11.00000 0.02860 0.02376 = 0.02942 0.00104 -0.00071 0.00057 AFIX 43 H48 2 0.647318 0.673816 0.423661 11.00000 -1.20000 AFIX 0 CL1 3 0.500053 0.154135 0.644628 11.00000 0.16927 0.09998 = 0.12176 -0.00537 -0.04894 -0.05218 CL2 3 0.561880 0.234956 0.665861 11.00000 0.10238 0.12578 = 0.08706 0.03575 0.00864 0.00602 C49 1 0.524899 0.236309 0.694990 11.00000 0.09918 0.06293 = 0.06696 0.00685 -0.01670 -0.01715 AFIX 23 H49A 2 0.524647 0.191183 0.734748 11.00000 -1.20000 H49B 2 0.518490 0.329682 0.700883 11.00000 -1.20000 AFIX 0 HKLF 4 REM XSTR0800 in C2/c #15 REM R1 = 0.0576 for 8637 Fo > 4sig(Fo) and 0.0606 for all 9303 data REM 568 parameters refined using 0 restraints END WGHT 0.1164 30.1746 REM Highest difference peak 2.245, deepest hole -1.787, 1-sigma level 0.155 Q1 1 0.5104 0.1990 0.7819 11.00000 0.05 2.25 Q2 1 0.6264 0.3770 0.2094 11.00000 0.05 1.47 Q3 1 0.6547 0.1721 0.3200 11.00000 0.05 1.41 Q4 1 0.6398 0.1262 0.2812 11.00000 0.05 1.25 Q5 1 0.5999 0.3382 0.2489 11.00000 0.05 1.12 Q6 1 0.6296 0.1297 0.3491 11.00000 0.05 1.10 Q7 1 0.6127 0.3245 0.1709 11.00000 0.05 1.10 Q8 1 0.6124 0.1786 0.3117 11.00000 0.05 1.07 Q9 1 0.5845 0.3743 0.2031 11.00000 0.05 1.00 Q10 1 0.6063 0.3006 0.3038 11.00000 0.05 0.99 Q11 1 0.6450 0.3841 0.2473 11.00000 0.05 0.97 Q12 1 0.6034 0.4149 0.2412 11.00000 0.05 0.94 Q13 1 0.6115 0.4189 0.1724 11.00000 0.05 0.91 Q14 1 0.6312 0.2042 0.3490 11.00000 0.05 0.91 Q15 1 0.6601 0.4102 0.2915 11.00000 0.05 0.89 Q16 1 0.6562 0.0723 0.1627 11.00000 0.05 0.89 Q17 1 0.6235 0.3569 0.5310 11.00000 0.05 0.88 Q18 1 0.6076 0.3994 0.4915 11.00000 0.05 0.88 Q19 1 0.5490 0.2370 0.7007 11.00000 0.05 0.86 Q20 1 0.5943 0.2226 0.2716 11.00000 0.05 0.86 REM The information below was added by Olex2. REM REM R1 = 0.0576 for 8637 Fo > 4sig(Fo) and 0.0606 for all 19502 data REM n/a parameters refined using n/a restraints REM Highest difference peak 2.25, deepest hole -1.79 REM Mean Shift 0, Max Shift 0.002. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0606 REM R1_gt = 0.0576 REM wR_ref = 0.1647 REM GOOF = 1.033 REM Shift_max = 0.002 REM Shift_mean = 0 REM Reflections_all = 19502 REM Reflections_gt = 8637 REM Parameters = n/a REM Hole = -1.79 REM Peak = 2.25 REM Flack = n/a ; _cod_data_source_file d6dt00946h2.cif _cod_data_source_block xstr0800 _cod_original_cell_volume 9542.8(5) _cod_database_code 7721122 _shelxl_version_number 2013-4 _chemical_oxdiff_formula 'Fe2 Se2 P2 C50H40 O4' _chemical_oxdiff_usercomment 'GH sample' _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. ; _reflns_odcompleteness_completeness 99.68 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.49 _olex2_refinement_description ; 1.a Secondary CH2 refined with riding coordinates: C49(H49A,H49B) 1.b Aromatic/amide H refined with riding coordinates: C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48) ; _shelx_fab_file ; -54 2 1 2.2524 -0.3680 -54 2 2 -3.4065 0.0466 -54 2 3 0.7223 -0.5583 -54 2 4 -1.0811 -2.0117 -53 1 1 1.9276 1.9514 -53 1 2 -3.4426 2.1100 -53 1 3 3.3463 0.2459 -53 1 4 -0.6130 0.2192 -53 1 5 -0.2358 0.4333 -53 1 6 2.6183 -1.4975 -53 3 1 -2.8144 2.7925 -53 3 2 -1.1042 0.9039 -53 3 3 -3.3300 0.7029 -53 3 4 -2.7264 1.4254 -53 3 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-0.7068 46 6 3 -3.0136 2.2829 47 1 0 1.8521 0.4021 47 1 1 -7.5122 0.0198 47 1 2 0.4525 -0.5616 47 1 3 -10.9958 0.8613 47 1 4 -1.3912 -0.6530 47 1 5 -8.2006 -0.1339 47 1 6 -2.4003 0.5447 47 1 7 -3.1898 -1.2553 47 1 8 -3.1829 0.1442 47 1 9 0.3720 -0.8393 47 1 10 -2.0003 0.7210 47 1 11 2.6798 -0.2706 47 1 12 1.1192 -0.1706 47 1 13 2.5006 0.1448 47 1 14 0.8709 -0.9816 47 3 0 -6.8259 0.2023 47 3 1 6.0687 -0.3754 47 3 2 -5.4045 -0.8754 47 3 3 5.3348 2.0175 47 3 4 -3.2796 -0.5156 47 3 5 4.3497 -0.6710 47 3 6 -0.3111 0.7955 47 3 7 1.0649 -2.4902 47 3 8 5.2055 1.4967 47 3 9 -2.2540 -0.5354 47 3 10 5.5720 0.7277 47 3 11 -2.0535 -0.2639 47 3 12 3.0035 -0.9717 47 5 0 0.3074 0.6967 47 5 1 0.2906 0.6858 47 5 2 3.2671 1.1947 47 5 3 -0.2867 -0.2394 47 5 4 4.1229 -0.9097 47 5 5 -0.4264 -1.5170 47 5 6 2.7262 1.2406 47 5 7 -1.8220 -0.5058 47 5 8 2.1390 3.1321 48 0 0 4.1308 0.8967 48 0 2 9.6224 0.6121 48 0 4 12.7271 -0.1430 48 0 6 8.1872 -0.9912 48 0 8 4.9913 -0.9872 48 0 10 1.2120 -1.7573 48 0 12 -1.6480 0.0475 48 2 0 -3.9294 0.2902 48 2 1 4.1613 0.6089 48 2 2 -6.2078 1.2128 48 2 3 3.1154 -1.2752 48 2 4 -6.1809 -0.1260 48 2 5 1.1609 0.2235 48 2 6 -3.7233 1.3973 48 2 7 -1.2564 -0.6564 48 2 8 0.4088 1.1853 48 2 9 -4.4492 0.0200 48 2 10 2.2984 -0.1947 48 2 11 -2.0161 0.7742 48 2 12 0.9208 0.6490 48 4 0 2.1646 0.3210 48 4 1 -5.3660 -1.7979 48 4 2 2.2913 1.1800 48 4 3 -4.3483 -2.2144 48 4 4 2.8556 2.1993 48 4 5 -3.6284 -0.3006 48 4 6 1.9670 -0.0260 48 4 7 -0.3382 -0.8743 48 4 8 1.5908 -0.1408 48 4 9 1.7518 0.7454 48 4 10 0.2166 -0.0099 49 1 0 -1.8996 -0.6541 49 1 1 4.5369 -0.0270 49 1 2 -1.3138 0.3255 49 1 3 8.7300 -1.1400 49 1 4 0.3689 0.8182 49 1 5 8.0461 -0.3590 49 1 6 1.5837 -0.6951 49 1 7 3.8475 1.1079 49 1 8 2.2813 -0.2221 49 1 9 1.1937 0.8977 49 1 10 2.2726 -0.7975 49 1 11 -0.8752 0.5178 49 1 12 -0.3654 -0.2851 49 3 0 4.9523 -0.2743 49 3 1 -3.8123 0.3780 49 3 2 4.4914 1.0136 49 3 3 -3.8228 -2.1164 49 3 4 3.3114 0.9966 49 3 5 -3.9838 -0.2375 49 3 6 1.6273 -0.5268 49 3 7 -2.3641 2.8654 49 3 8 -2.9170 -1.4633 49 3 9 0.5272 1.2176 49 3 10 -3.7096 -1.4014 49 5 0 0.3854 -0.4456 49 5 1 -0.2925 -0.2980 49 5 2 -2.1846 -1.8326 49 5 3 0.0362 0.0407 49 5 4 -3.2355 0.4395 49 5 5 -0.1912 1.8485 50 0 0 -1.5141 -1.3872 50 0 2 -6.1295 -1.4976 50 0 4 -11.2245 -0.5508 50 0 6 -8.2184 0.9733 50 0 8 -5.4192 1.0719 50 2 0 1.4566 0.1399 50 2 1 -3.4513 -1.1896 50 2 2 3.9016 -1.6600 50 2 3 -3.4179 1.2976 50 2 4 4.5384 -0.2007 50 2 5 -1.7515 -0.2822 50 2 6 3.7368 -1.3861 50 2 7 -0.0429 0.3618 50 2 8 0.6909 -1.7739 50 2 9 3.1450 -0.0683 50 2 10 -1.1865 0.0845 50 4 0 -0.9820 -0.1694 50 4 1 4.0033 1.5756 50 4 2 -1.2933 -0.8214 50 4 3 3.2373 3.1036 50 4 4 -1.8840 -2.3667 50 4 5 3.1234 0.7398 50 4 6 -1.1442 -0.3313 50 4 7 0.8510 1.1133 51 1 0 1.9957 0.6132 51 1 1 -1.7950 0.0665 51 1 2 1.8094 0.0651 51 1 3 -5.6121 1.2547 51 1 4 0.5461 -0.9077 51 1 5 -6.5701 0.8329 51 1 6 -0.8154 0.7660 51 1 7 -3.2773 -0.8247 51 1 8 -1.2188 0.3250 51 1 9 -1.4494 -0.7603 51 1 10 -1.9428 0.7168 51 3 0 -2.9860 0.2393 51 3 1 1.7297 -0.2565 51 3 2 -3.0774 -1.0133 51 3 3 2.1462 1.8494 51 3 4 -2.5756 -1.4141 51 3 5 2.7747 1.1538 51 3 6 -1.9836 0.1738 51 3 7 2.5014 -2.6802 51 3 8 1.2937 1.1468 52 0 0 -0.4597 1.3787 52 0 2 2.5364 2.2379 52 0 4 8.3691 1.5055 52 0 6 6.9760 -0.6069 52 2 0 0.2163 -0.6681 52 2 1 2.4987 1.5356 52 2 2 -2.0617 1.9037 52 2 3 2.9881 -1.3114 52 2 4 -2.6015 0.6602 52 2 5 1.5733 0.1596 52 2 6 -2.8054 1.2168 52 2 7 0.5058 -0.0931 52 4 0 -0.0315 -0.0444 52 4 1 -2.6005 -1.0281 52 4 2 0.3256 0.3313 52 4 3 -2.0629 -3.5297 53 1 0 -1.9937 -0.1679 53 1 1 -0.1292 -0.1655 53 1 2 -1.8076 -0.4525 53 1 3 2.5885 -1.1649 53 1 4 -1.0997 0.8748 53 1 5 4.4892 -1.1728 53 1 6 0.3014 -0.7361 53 3 0 1.3878 -0.0987 53 3 1 -0.2901 -0.0208 53 3 2 1.6428 0.8373 53 3 3 -0.8213 -1.3156 53 3 4 1.5547 1.6163 54 0 0 1.4970 -0.8886 54 0 2 0.2850 -2.5417 54 2 0 -0.9259 1.0918 54 2 1 -1.5321 -1.5241 54 2 2 1.0875 -1.8888 54 2 3 -2.0733 1.3544 54 2 4 1.0694 -1.1626 0 0 0 0.0 0.0 ; _olex2_date_sample_data_collection 2017-12-12 _olex2_exptl_crystal_mounting_method 'Nylon Loop' _olex2_submission_original_sample_id xstr0800 _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 2.194 _oxdiff_exptl_absorpt_empirical_full_min 0.535 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -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 0.60705(2) 0.37272(5) 0.20404(2) 0.02179(14) Uani 1 1 d . . . . . Se2 Se 0.63482(2) 0.17298(4) 0.31452(2) 0.01748(13) Uani 1 1 d . . . . . Fe1 Fe 0.58819(2) 0.28548(7) 0.29869(3) 0.01731(16) Uani 1 1 d . . . . . Fe2 Fe 0.64136(2) 0.40493(7) 0.28720(3) 0.01905(17) Uani 1 1 d . . . . . Fe3 Fe 0.63756(2) 0.05345(7) 0.15770(3) 0.02066(17) Uani 1 1 d . . . . . Fe4 Fe 0.62754(2) 0.38777(7) 0.49660(3) 0.01549(16) Uani 1 1 d . . . . . P1 P 0.57093(2) 0.26041(10) 0.39517(5) 0.0150(2) Uani 1 1 d . . . . . P2 P 0.67275(2) 0.43552(11) 0.36674(5) 0.0185(2) Uani 1 1 d . . . . . O1 O 0.54634(10) 0.5118(5) 0.2830(2) 0.0473(11) Uani 1 1 d . . . . . O2 O 0.55076(9) 0.0658(4) 0.25028(18) 0.0384(9) Uani 1 1 d . . . . . O3 O 0.61140(10) 0.6660(4) 0.30691(18) 0.0376(9) Uani 1 1 d . . . . . O4 O 0.68663(12) 0.4937(6) 0.2004(2) 0.0567(13) Uani 1 1 d . . . . . C1 C 0.56244(11) 0.4239(5) 0.2908(2) 0.0279(10) Uani 1 1 d . . . . . C2 C 0.56545(11) 0.1516(5) 0.2698(2) 0.0247(9) Uani 1 1 d . . . . . C3 C 0.62313(12) 0.5632(5) 0.3005(2) 0.0289(10) Uani 1 1 d . . . . . C4 C 0.66985(13) 0.4547(6) 0.2363(2) 0.0352(12) Uani 1 1 d . . . . . C5 C 0.61924(11) 0.2377(5) 0.1460(2) 0.0235(9) Uani 1 1 d . . . . . C6 C 0.60014(11) 0.1372(5) 0.1195(2) 0.0269(10) Uani 1 1 d . . . . . H6 H 0.5805 0.1199 0.1305 0.032 Uiso 1 1 calc R . . . . C7 C 0.61653(12) 0.0677(6) 0.0728(2) 0.0309(11) Uani 1 1 d . . . . . H7 H 0.6095 -0.0033 0.0483 0.037 Uiso 1 1 calc R . . . . C8 C 0.64543(12) 0.1264(5) 0.0706(2) 0.0292(10) Uani 1 1 d . . . . . H8 H 0.6607 0.1004 0.0443 0.035 Uiso 1 1 calc R . . . . C9 C 0.64724(12) 0.2316(5) 0.1154(2) 0.0272(10) Uani 1 1 d . . . . . H9 H 0.6637 0.2866 0.1233 0.033 Uiso 1 1 calc R . . . . C10 C 0.62353(13) -0.0628(5) 0.2301(2) 0.0287(10) Uani 1 1 d . . . . . H10 H 0.6040 -0.0761 0.2430 0.034 Uiso 1 1 calc R . . . . C11 C 0.63917(14) -0.1453(5) 0.1880(2) 0.0344(12) Uani 1 1 d . . . . . H11 H 0.6316 -0.2217 0.1679 0.041 Uiso 1 1 calc R . . . . C12 C 0.66840(13) -0.0912(6) 0.1817(2) 0.0351(12) Uani 1 1 d . . . . . H12 H 0.6833 -0.1257 0.1565 0.042 Uiso 1 1 calc R . . . . C13 C 0.67099(12) 0.0246(5) 0.2205(2) 0.0313(11) Uani 1 1 d . . . . . H13 H 0.6880 0.0779 0.2259 0.038 Uiso 1 1 calc R . . . . C14 C 0.64300(11) 0.0444(5) 0.2495(2) 0.0232(9) Uani 1 1 d . . . . . C15 C 0.56633(10) 0.0896(4) 0.4278(2) 0.0188(8) Uani 1 1 d . . . . . C16 C 0.58081(11) -0.0224(5) 0.4035(2) 0.0263(9) Uani 1 1 d . . . . . H16 H 0.5943 -0.0109 0.3715 0.032 Uiso 1 1 calc R . . . . C17 C 0.57531(12) -0.1525(5) 0.4267(3) 0.0323(11) Uani 1 1 d . . . . . H17 H 0.5849 -0.2274 0.4097 0.039 Uiso 1 1 calc R . . . . C18 C 0.55566(12) -0.1703(5) 0.4750(3) 0.0318(11) Uani 1 1 d . . . . . H18 H 0.5522 -0.2569 0.4907 0.038 Uiso 1 1 calc R . . . . C19 C 0.54116(10) -0.0590(5) 0.4998(2) 0.0266(10) Uani 1 1 d . . . . . H19 H 0.5280 -0.0708 0.5324 0.032 Uiso 1 1 calc R . . . . C20 C 0.54616(10) 0.0703(5) 0.4763(2) 0.0222(9) Uani 1 1 d . . . . . H20 H 0.5361 0.1446 0.4926 0.027 Uiso 1 1 calc R . . . . C21 C 0.53175(9) 0.3174(5) 0.3962(2) 0.0208(9) Uani 1 1 d . . . . . C22 C 0.51045(11) 0.2392(6) 0.3644(2) 0.0285(10) Uani 1 1 d . . . . . H22 H 0.5160 0.1570 0.3466 0.034 Uiso 1 1 calc R . . . . C23 C 0.48122(11) 0.2840(7) 0.3596(3) 0.0384(13) Uani 1 1 d . . . . . H23 H 0.4672 0.2313 0.3386 0.046 Uiso 1 1 calc R . . . . C24 C 0.47263(12) 0.4062(7) 0.3856(3) 0.0440(15) Uani 1 1 d . . . . . H24 H 0.4530 0.4359 0.3819 0.053 Uiso 1 1 calc R . . . . C25 C 0.49331(12) 0.4836(6) 0.4171(3) 0.0372(12) Uani 1 1 d . . . . . H25 H 0.4875 0.5657 0.4347 0.045 Uiso 1 1 calc R . . . . C26 C 0.52300(11) 0.4399(5) 0.4228(2) 0.0285(10) Uani 1 1 d . . . . . H26 H 0.5368 0.4926 0.4443 0.034 Uiso 1 1 calc R . . . . C27 C 0.58625(9) 0.3591(4) 0.4587(2) 0.0179(8) Uani 1 1 d . . . . . C28 C 0.58567(9) 0.3304(5) 0.5232(2) 0.0223(9) Uani 1 1 d . . . . . H28 H 0.5803 0.2482 0.5412 0.027 Uiso 1 1 calc R . . . . C29 C 0.59481(10) 0.4503(5) 0.5551(2) 0.0271(10) Uani 1 1 d . . . . . H29 H 0.5965 0.4596 0.5977 0.033 Uiso 1 1 calc R . . . . C30 C 0.60089(10) 0.5535(5) 0.5110(2) 0.0249(9) Uani 1 1 d . . . . . H30 H 0.6072 0.6417 0.5198 0.030 Uiso 1 1 calc R . . . . C31 C 0.59574(9) 0.4991(4) 0.4516(2) 0.0207(8) Uani 1 1 d . . . . . H31 H 0.5980 0.5450 0.4145 0.025 Uiso 1 1 calc R . . . . C32 C 0.65735(9) 0.2487(5) 0.4636(2) 0.0191(8) Uani 1 1 d . . . . . H32 H 0.6532 0.1766 0.4371 0.023 Uiso 1 1 calc R . . . . C33 C 0.65710(9) 0.2431(5) 0.5288(2) 0.0215(9) Uani 1 1 d . . . . . H33 H 0.6527 0.1669 0.5525 0.026 Uiso 1 1 calc R . . . . C34 C 0.66485(10) 0.3748(5) 0.5521(2) 0.0254(9) Uani 1 1 d . . . . . H34 H 0.6662 0.3990 0.5935 0.031 Uiso 1 1 calc R . . . . C35 C 0.67016(9) 0.4624(5) 0.5011(2) 0.0229(9) Uani 1 1 d . . . . . H35 H 0.6759 0.5533 0.5034 0.028 Uiso 1 1 calc R . . . . C36 C 0.66507(9) 0.3852(4) 0.4453(2) 0.0195(8) Uani 1 1 d . . . . . C37 C 0.70934(10) 0.3491(5) 0.3611(2) 0.0269(10) Uani 1 1 d . . . . . C38 C 0.72956(13) 0.3582(8) 0.4102(3) 0.0492(16) Uani 1 1 d . . . . . H38 H 0.7251 0.4123 0.4440 0.059 Uiso 1 1 calc R . . . . C39 C 0.75637(15) 0.2868(10) 0.4091(4) 0.064(2) Uani 1 1 d . . . . . H39 H 0.7698 0.2942 0.4418 0.076 Uiso 1 1 calc R . . . . C40 C 0.76293(13) 0.2055(7) 0.3595(4) 0.0524(17) Uani 1 1 d . . . . . H40 H 0.7807 0.1568 0.3589 0.063 Uiso 1 1 calc R . . . . C41 C 0.74344(13) 0.1963(7) 0.3115(4) 0.0484(16) Uani 1 1 d . . . . . H41 H 0.7480 0.1408 0.2782 0.058 Uiso 1 1 calc R . . . . C42 C 0.71647(12) 0.2691(6) 0.3112(3) 0.0357(12) Uani 1 1 d . . . . . H42 H 0.7035 0.2632 0.2776 0.043 Uiso 1 1 calc R . . . . C43 C 0.68270(11) 0.6163(5) 0.3725(2) 0.0247(9) Uani 1 1 d . . . . . C44 C 0.70667(14) 0.6672(6) 0.3402(3) 0.0398(13) Uani 1 1 d . . . . . H44 H 0.7196 0.6078 0.3205 0.048 Uiso 1 1 calc R . . . . C45 C 0.71159(17) 0.8066(7) 0.3371(3) 0.0524(17) Uani 1 1 d . . . . . H45 H 0.7277 0.8398 0.3148 0.063 Uiso 1 1 calc R . . . . C46 C 0.69296(16) 0.8957(6) 0.3665(3) 0.0439(14) Uani 1 1 d . . . . . H46 H 0.6965 0.9889 0.3642 0.053 Uiso 1 1 calc R . . . . C47 C 0.66879(13) 0.8467(5) 0.3997(3) 0.0342(11) Uani 1 1 d . . . . . H47 H 0.6562 0.9066 0.4201 0.041 Uiso 1 1 calc R . . . . C48 C 0.66363(11) 0.7070(5) 0.4021(2) 0.0273(10) Uani 1 1 d . . . . . H48 H 0.6473 0.6738 0.4237 0.033 Uiso 1 1 calc R . . . . Cl1 Cl 0.50005(11) 0.1541(4) 0.64463(18) 0.1307(14) Uani 1 1 d . . . . . Cl2 Cl 0.56188(7) 0.2350(4) 0.66586(14) 0.1050(9) Uani 1 1 d . . . . . C49 C 0.5249(2) 0.2363(10) 0.6950(4) 0.076(3) Uani 1 1 d . . . . . H49A H 0.5246 0.1912 0.7347 0.092 Uiso 1 1 calc R . . . . H49B H 0.5185 0.3297 0.7009 0.092 Uiso 1 1 calc R . . . . 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 0.0298(3) 0.0188(2) 0.0168(2) 0.00270(17) -0.00103(17) 0.00576(18) Se2 0.0208(2) 0.0145(2) 0.0171(2) 0.00079(15) -0.00084(16) 0.00288(16) Fe1 0.0197(3) 0.0148(3) 0.0174(3) 0.0004(2) -0.0018(2) 0.0037(2) Fe2 0.0248(4) 0.0148(3) 0.0175(3) 0.0015(3) 0.0001(3) -0.0003(3) Fe3 0.0233(3) 0.0200(4) 0.0187(3) -0.0018(3) -0.0001(3) 0.0037(3) Fe4 0.0136(3) 0.0151(3) 0.0177(3) -0.0017(2) -0.0021(2) 0.0013(2) P1 0.0146(4) 0.0120(5) 0.0185(5) -0.0015(4) -0.0017(3) 0.0022(3) P2 0.0189(5) 0.0151(5) 0.0216(5) 0.0014(4) 0.0025(4) 0.0006(4) O1 0.049(2) 0.043(2) 0.050(2) 0.019(2) 0.0114(19) 0.026(2) O2 0.040(2) 0.037(2) 0.038(2) -0.0088(17) -0.0058(16) -0.0090(17) O3 0.055(2) 0.0184(18) 0.040(2) 0.0003(15) -0.0062(17) 0.0101(16) O4 0.066(3) 0.071(3) 0.034(2) 0.009(2) 0.015(2) -0.032(3) C1 0.031(2) 0.028(2) 0.024(2) 0.0063(19) 0.0022(18) 0.008(2) C2 0.029(2) 0.028(2) 0.017(2) 0.0010(18) -0.0001(17) 0.0041(19) C3 0.036(3) 0.022(2) 0.028(2) 0.0030(19) -0.0036(19) 0.001(2) C4 0.047(3) 0.034(3) 0.025(2) 0.002(2) 0.001(2) -0.014(2) C5 0.032(2) 0.021(2) 0.018(2) 0.0027(17) -0.0036(17) 0.0087(18) C6 0.026(2) 0.030(2) 0.025(2) 0.0000(19) -0.0059(17) 0.0062(19) C7 0.042(3) 0.032(3) 0.019(2) -0.0035(19) -0.0079(19) 0.009(2) C8 0.037(3) 0.033(3) 0.018(2) 0.0029(19) 0.0032(18) 0.006(2) C9 0.036(3) 0.024(2) 0.021(2) 0.0016(18) 0.0040(18) 0.0000(19) C10 0.046(3) 0.018(2) 0.022(2) 0.0014(18) 0.0024(19) 0.000(2) C11 0.055(3) 0.021(2) 0.027(3) -0.004(2) -0.002(2) 0.008(2) C12 0.040(3) 0.037(3) 0.029(3) -0.005(2) -0.005(2) 0.022(2) C13 0.030(2) 0.028(3) 0.036(3) -0.003(2) -0.002(2) 0.014(2) C14 0.033(2) 0.018(2) 0.018(2) 0.0010(17) 0.0007(17) 0.0080(18) C15 0.021(2) 0.0146(19) 0.021(2) 0.0027(16) -0.0031(16) 0.0009(16) C16 0.029(2) 0.019(2) 0.031(2) 0.0007(19) 0.0055(18) 0.0045(18) C17 0.040(3) 0.017(2) 0.040(3) 0.002(2) 0.003(2) 0.008(2) C18 0.035(3) 0.020(2) 0.041(3) 0.010(2) 0.000(2) 0.0006(19) C19 0.021(2) 0.028(2) 0.030(2) 0.006(2) 0.0014(17) 0.0008(18) C20 0.021(2) 0.022(2) 0.024(2) 0.0025(18) 0.0019(16) 0.0007(17) C21 0.0179(19) 0.023(2) 0.022(2) 0.0019(17) -0.0015(15) 0.0005(17) C22 0.024(2) 0.035(3) 0.026(2) -0.004(2) 0.0002(17) -0.004(2) C23 0.019(2) 0.063(4) 0.034(3) -0.007(3) -0.0035(19) -0.007(2) C24 0.019(2) 0.071(4) 0.042(3) 0.006(3) 0.000(2) 0.015(3) C25 0.028(2) 0.041(3) 0.042(3) -0.008(2) -0.001(2) 0.016(2) C26 0.023(2) 0.030(3) 0.033(3) -0.007(2) -0.0026(18) 0.0073(19) C27 0.0124(17) 0.020(2) 0.022(2) -0.0052(16) -0.0009(14) 0.0034(15) C28 0.0160(19) 0.025(2) 0.026(2) -0.0055(18) -0.0008(16) 0.0005(16) C29 0.020(2) 0.036(3) 0.025(2) -0.012(2) 0.0012(16) 0.0031(19) C30 0.018(2) 0.022(2) 0.035(2) -0.0125(19) -0.0053(17) 0.0058(17) C31 0.0170(19) 0.015(2) 0.030(2) -0.0013(17) -0.0046(16) 0.0049(16) C32 0.0173(18) 0.017(2) 0.023(2) -0.0006(16) 0.0025(15) 0.0036(15) C33 0.0167(18) 0.019(2) 0.029(2) 0.0042(17) -0.0017(16) 0.0041(16) C34 0.017(2) 0.031(3) 0.028(2) 0.0003(19) -0.0048(16) 0.0020(18) C35 0.0158(19) 0.024(2) 0.029(2) -0.0012(18) -0.0040(16) -0.0044(17) C36 0.0170(19) 0.017(2) 0.025(2) -0.0004(16) 0.0027(16) 0.0023(15) C37 0.022(2) 0.024(2) 0.035(3) 0.001(2) 0.0086(18) 0.0013(18) C38 0.029(3) 0.074(5) 0.045(3) -0.011(3) 0.001(2) 0.018(3) C39 0.029(3) 0.095(6) 0.066(4) -0.003(4) 0.004(3) 0.025(4) C40 0.021(3) 0.049(4) 0.087(5) 0.003(3) 0.017(3) 0.009(2) C41 0.028(3) 0.040(3) 0.077(5) -0.019(3) 0.021(3) 0.000(2) C42 0.027(2) 0.033(3) 0.047(3) -0.007(2) 0.010(2) 0.000(2) C43 0.029(2) 0.017(2) 0.028(2) 0.0026(18) -0.0017(18) -0.0040(18) C44 0.040(3) 0.031(3) 0.048(3) -0.001(2) 0.014(2) -0.009(2) C45 0.060(4) 0.037(3) 0.061(4) 0.008(3) 0.017(3) -0.020(3) C46 0.061(4) 0.022(3) 0.049(3) 0.006(2) 0.004(3) -0.012(3) C47 0.045(3) 0.020(2) 0.037(3) 0.001(2) -0.005(2) -0.001(2) C48 0.029(2) 0.024(2) 0.029(2) 0.0010(19) -0.0007(18) 0.0006(19) Cl1 0.169(4) 0.100(2) 0.122(3) -0.0054(19) -0.049(2) -0.052(2) Cl2 0.102(2) 0.126(2) 0.0871(17) 0.0357(17) 0.0086(14) 0.0060(18) C49 0.099(7) 0.063(5) 0.067(5) 0.007(4) -0.017(5) -0.017(5) 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' Cl Cl 0.3639 0.7018 '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_ _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 Fe2 Se1 Fe1 68.08(3) . . ? C5 Se1 Fe1 115.00(14) . . ? C5 Se1 Fe2 113.90(14) . . ? Fe2 Se2 Fe1 68.22(3) . . ? C14 Se2 Fe1 111.72(14) . . ? C14 Se2 Fe2 114.88(14) . . ? Se1 Fe1 Fe2 55.82(2) . . ? Se2 Fe1 Se1 88.49(3) . . ? Se2 Fe1 Fe2 55.70(2) . . ? P1 Fe1 Se1 165.10(4) . . ? P1 Fe1 Se2 97.09(4) . . ? P1 Fe1 Fe2 116.72(4) . . ? C1 Fe1 Se1 82.98(16) . . ? C1 Fe1 Se2 158.16(18) . . ? C1 Fe1 Fe2 103.37(17) . . ? C1 Fe1 P1 86.87(16) . . ? C2 Fe1 Se1 99.74(15) . . ? C2 Fe1 Se2 101.88(16) . . ? C2 Fe1 Fe2 143.39(15) . . ? C2 Fe1 P1 92.64(15) . . ? C2 Fe1 C1 99.4(2) . . ? Se1 Fe2 Fe1 56.11(2) . . ? Se2 Fe2 Se1 88.93(3) . . ? Se2 Fe2 Fe1 56.08(2) . . ? P2 Fe2 Se1 178.75(4) . . ? P2 Fe2 Se2 90.83(4) . . ? P2 Fe2 Fe1 122.82(4) . . ? C3 Fe2 Se1 86.86(17) . . ? C3 Fe2 Se2 137.74(17) . . ? C3 Fe2 Fe1 87.60(17) . . ? C3 Fe2 P2 92.49(17) . . ? C4 Fe2 Se1 91.57(18) . . ? C4 Fe2 Se2 120.9(2) . . ? C4 Fe2 Fe1 146.25(18) . . ? C4 Fe2 P2 89.61(19) . . ? C4 Fe2 C3 101.2(3) . . ? C5 Fe3 C6 41.3(2) . . ? C5 Fe3 C7 69.12(19) . . ? C5 Fe3 C8 69.04(19) . . ? C5 Fe3 C9 41.49(19) . . ? C5 Fe3 C10 118.2(2) . . ? C5 Fe3 C11 155.4(2) . . ? C5 Fe3 C12 159.2(2) . . ? C5 Fe3 C13 120.6(2) . . ? C5 Fe3 C14 102.18(18) . . ? C6 Fe3 C7 40.8(2) . . ? C6 Fe3 C8 68.4(2) . . ? C6 Fe3 C10 106.3(2) . . ? C6 Fe3 C11 122.6(2) . . ? C6 Fe3 C12 159.3(2) . . ? C8 Fe3 C7 40.3(2) . . ? C8 Fe3 C11 128.2(2) . . ? C9 Fe3 C6 69.2(2) . . ? C9 Fe3 C7 68.6(2) . . ? C9 Fe3 C8 40.7(2) . . ? C9 Fe3 C10 154.05(19) . . ? C9 Fe3 C11 163.0(2) . . ? C9 Fe3 C12 124.7(2) . . ? C9 Fe3 C13 105.3(2) . . ? C10 Fe3 C7 125.6(2) . . ? C10 Fe3 C8 163.3(2) . . ? C10 Fe3 C11 40.2(2) . . ? C11 Fe3 C7 111.3(2) . . ? C12 Fe3 C7 125.1(2) . . ? C12 Fe3 C8 110.8(2) . . ? C12 Fe3 C10 68.2(2) . . ? C12 Fe3 C11 40.5(2) . . ? C13 Fe3 C6 157.9(2) . . ? C13 Fe3 C7 158.9(2) . . ? C13 Fe3 C8 122.2(2) . . ? C13 Fe3 C10 68.7(2) . . ? C13 Fe3 C11 68.3(2) . . ? C13 Fe3 C12 40.7(2) . . ? C14 Fe3 C6 120.91(19) . . ? C14 Fe3 C7 159.8(2) . . ? C14 Fe3 C8 155.2(2) . . ? C14 Fe3 C9 117.6(2) . . ? C14 Fe3 C10 41.3(2) . . ? C14 Fe3 C11 68.8(2) . . ? C14 Fe3 C12 68.97(19) . . ? C14 Fe3 C13 41.20(19) . . ? C27 Fe4 C28 40.95(18) . . ? C27 Fe4 C29 68.79(18) . . ? C27 Fe4 C30 69.08(17) . . ? C27 Fe4 C31 41.67(17) . . ? C27 Fe4 C32 111.07(17) . . ? C27 Fe4 C33 128.27(18) . . ? C27 Fe4 C34 163.45(19) . . ? C27 Fe4 C35 155.81(19) . . ? C28 Fe4 C33 107.54(18) . . ? C28 Fe4 C34 124.05(19) . . ? C29 Fe4 C28 40.76(19) . . ? C29 Fe4 C30 40.7(2) . . ? C29 Fe4 C32 153.3(2) . . ? C29 Fe4 C33 117.3(2) . . ? C29 Fe4 C34 103.83(19) . . ? C29 Fe4 C35 122.48(19) . . ? C30 Fe4 C28 68.79(19) . . ? C30 Fe4 C33 150.64(19) . . ? C30 Fe4 C34 115.63(19) . . ? C30 Fe4 C35 104.65(19) . . ? C31 Fe4 C28 69.21(19) . . ? C31 Fe4 C29 68.5(2) . . ? C31 Fe4 C30 40.50(19) . . ? C31 Fe4 C32 130.29(18) . . ? C31 Fe4 C33 167.67(18) . . ? C31 Fe4 C34 151.08(19) . . ? C31 Fe4 C35 118.55(19) . . ? C32 Fe4 C28 121.19(18) . . ? C32 Fe4 C30 165.9(2) . . ? C32 Fe4 C33 40.37(18) . . ? C32 Fe4 C34 68.49(19) . . ? C32 Fe4 C35 69.17(18) . . ? C34 Fe4 C33 40.69(19) . . ? C35 Fe4 C28 160.38(19) . . ? C35 Fe4 C33 68.60(18) . . ? C35 Fe4 C34 40.62(19) . . ? C36 Fe4 C27 122.09(18) . . ? C36 Fe4 C28 156.81(18) . . ? C36 Fe4 C29 161.7(2) . . ? C36 Fe4 C30 125.64(19) . . ? C36 Fe4 C31 108.83(18) . . ? C36 Fe4 C32 41.51(17) . . ? C36 Fe4 C33 69.18(17) . . ? C36 Fe4 C34 69.33(19) . . ? C36 Fe4 C35 41.61(18) . . ? C15 P1 Fe1 120.00(15) . . ? C15 P1 C21 99.4(2) . . ? C21 P1 Fe1 108.26(14) . . ? C27 P1 Fe1 121.15(15) . . ? C27 P1 C15 103.8(2) . . ? C27 P1 C21 100.45(19) . . ? C36 P2 Fe2 124.47(15) . . ? C36 P2 C37 96.6(2) . . ? C36 P2 C43 104.4(2) . . ? C37 P2 Fe2 115.94(17) . . ? C43 P2 Fe2 109.45(16) . . ? C43 P2 C37 103.5(2) . . ? O1 C1 Fe1 177.0(5) . . ? O2 C2 Fe1 179.0(5) . . ? O3 C3 Fe2 177.7(5) . . ? O4 C4 Fe2 174.1(6) . . ? Se1 C5 Fe3 131.6(2) . . ? C6 C5 Se1 125.0(4) . . ? C6 C5 Fe3 70.6(3) . . ? C6 C5 C9 108.0(4) . . ? C9 C5 Se1 126.4(4) . . ? C9 C5 Fe3 70.1(3) . . ? C5 C6 Fe3 68.1(3) . . ? C5 C6 C7 107.9(4) . . ? C7 C6 Fe3 70.7(3) . . ? C6 C7 Fe3 68.5(3) . . ? C8 C7 Fe3 69.5(3) . . ? C8 C7 C6 107.7(4) . . ? C7 C8 Fe3 70.3(3) . . ? C7 C8 C9 108.6(4) . . ? C9 C8 Fe3 68.5(3) . . ? C5 C9 Fe3 68.4(3) . . ? C8 C9 Fe3 70.7(3) . . ? C8 C9 C5 107.8(4) . . ? C11 C10 Fe3 70.5(3) . . ? C11 C10 C14 107.9(5) . . ? C14 C10 Fe3 67.8(3) . . ? C10 C11 Fe3 69.3(3) . . ? C10 C11 C12 108.1(5) . . ? C12 C11 Fe3 69.2(3) . . ? C11 C12 Fe3 70.4(3) . . ? C13 C12 Fe3 69.2(3) . . ? C13 C12 C11 108.2(5) . . ? C12 C13 Fe3 70.1(3) . . ? C12 C13 C14 107.8(5) . . ? C14 C13 Fe3 68.4(3) . . ? Se2 C14 Fe3 132.4(2) . . ? C10 C14 Se2 125.3(4) . . ? C10 C14 Fe3 70.9(3) . . ? C13 C14 Se2 126.0(4) . . ? C13 C14 Fe3 70.4(3) . . ? C13 C14 C10 107.9(4) . . ? C16 C15 P1 121.7(3) . . ? C16 C15 C20 119.0(4) . . ? C20 C15 P1 119.2(3) . . ? C15 C16 C17 120.4(4) . . ? C18 C17 C16 120.2(5) . . ? C19 C18 C17 119.9(5) . . ? C18 C19 C20 120.1(4) . . ? C19 C20 C15 120.4(4) . . ? C22 C21 P1 118.1(4) . . ? C26 C21 P1 122.7(3) . . ? C26 C21 C22 119.0(4) . . ? C23 C22 C21 120.1(5) . . ? C24 C23 C22 120.8(5) . . ? C25 C24 C23 119.6(5) . . ? C24 C25 C26 120.6(5) . . ? C21 C26 C25 119.9(5) . . ? P1 C27 Fe4 135.7(2) . . ? C28 C27 Fe4 69.9(2) . . ? C28 C27 P1 129.0(3) . . ? C28 C27 C31 107.4(4) . . ? C31 C27 Fe4 69.2(2) . . ? C31 C27 P1 122.4(3) . . ? C27 C28 Fe4 69.1(2) . . ? C29 C28 Fe4 69.5(3) . . ? C29 C28 C27 107.8(4) . . ? C28 C29 Fe4 69.7(3) . . ? C30 C29 Fe4 69.7(3) . . ? C30 C29 C28 108.6(4) . . ? C29 C30 Fe4 69.6(3) . . ? C31 C30 Fe4 69.5(2) . . ? C31 C30 C29 108.3(4) . . ? C27 C31 Fe4 69.1(2) . . ? C30 C31 Fe4 70.0(3) . . ? C30 C31 C27 107.9(4) . . ? C33 C32 Fe4 70.4(2) . . ? C33 C32 C36 108.5(4) . . ? C36 C32 Fe4 68.5(2) . . ? C32 C33 Fe4 69.2(2) . . ? C32 C33 C34 108.2(4) . . ? C34 C33 Fe4 69.4(3) . . ? C33 C34 Fe4 69.9(3) . . ? C35 C34 Fe4 69.4(3) . . ? C35 C34 C33 108.4(4) . . ? C34 C35 Fe4 70.0(3) . . ? C34 C35 C36 107.9(4) . . ? C36 C35 Fe4 68.4(2) . . ? P2 C36 Fe4 132.9(2) . . ? C32 C36 Fe4 69.9(2) . . ? C32 C36 P2 124.2(3) . . ? C32 C36 C35 107.0(4) . . ? C35 C36 Fe4 69.9(2) . . ? C35 C36 P2 128.0(3) . . ? C38 C37 P2 119.2(4) . . ? C42 C37 P2 121.8(4) . . ? C42 C37 C38 118.9(5) . . ? C39 C38 C37 120.6(6) . . ? C40 C39 C38 119.9(7) . . ? C41 C40 C39 119.9(6) . . ? C40 C41 C42 121.1(6) . . ? C37 C42 C41 119.6(6) . . ? C44 C43 P2 120.4(4) . . ? C44 C43 C48 119.0(5) . . ? C48 C43 P2 120.0(4) . . ? C43 C44 C45 120.4(6) . . ? C46 C45 C44 120.6(6) . . ? C45 C46 C47 120.0(5) . . ? C46 C47 C48 119.4(5) . . ? C47 C48 C43 120.6(5) . . ? Cl1 C49 Cl2 111.3(6) . . ? 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 2.3871(8) . ? Se1 Fe2 2.3790(8) . ? Se1 C5 1.912(5) . ? Se2 Fe1 2.3842(8) . ? Se2 Fe2 2.3733(8) . ? Se2 C14 1.931(4) . ? Fe1 Fe2 2.6679(10) . ? Fe1 P1 2.2520(12) . ? Fe1 C1 1.790(5) . ? Fe1 C2 1.774(5) . ? Fe2 P2 2.2352(13) . ? Fe2 C3 1.781(5) . ? Fe2 C4 1.765(5) . ? Fe3 C5 2.002(5) . ? Fe3 C6 2.036(5) . ? Fe3 C7 2.065(5) . ? Fe3 C8 2.054(5) . ? Fe3 C9 2.025(5) . ? Fe3 C10 2.047(5) . ? Fe3 C11 2.061(5) . ? Fe3 C12 2.045(5) . ? Fe3 C13 2.034(5) . ? Fe3 C14 2.006(4) . ? Fe4 C27 2.036(4) . ? Fe4 C28 2.046(4) . ? Fe4 C29 2.043(4) . ? Fe4 C30 2.044(4) . ? Fe4 C31 2.037(4) . ? Fe4 C32 2.044(4) . ? Fe4 C33 2.060(4) . ? Fe4 C34 2.053(5) . ? Fe4 C35 2.046(4) . ? Fe4 C36 2.025(4) . ? P1 C15 1.834(4) . ? P1 C21 1.842(4) . ? P1 C27 1.814(4) . ? P2 C36 1.810(5) . ? P2 C37 1.850(5) . ? P2 C43 1.835(5) . ? O1 C1 1.136(6) . ? O2 C2 1.148(6) . ? O3 C3 1.148(6) . ? O4 C4 1.153(7) . ? C5 C6 1.424(7) . ? C5 C9 1.426(7) . ? C6 C7 1.430(7) . ? C7 C8 1.418(8) . ? C8 C9 1.420(7) . ? C10 C11 1.412(7) . ? C10 C14 1.428(7) . ? C11 C12 1.421(9) . ? C12 C13 1.418(8) . ? C13 C14 1.422(7) . ? C15 C16 1.384(6) . ? C15 C20 1.405(6) . ? C16 C17 1.396(7) . ? C17 C18 1.386(8) . ? C18 C19 1.383(7) . ? C19 C20 1.389(7) . ? C21 C22 1.401(7) . ? C21 C26 1.392(7) . ? C22 C23 1.384(7) . ? C23 C24 1.383(9) . ? C24 C25 1.374(9) . ? C25 C26 1.402(7) . ? C27 C28 1.428(6) . ? C27 C31 1.448(6) . ? C28 C29 1.424(7) . ? C29 C30 1.422(8) . ? C30 C31 1.413(7) . ? C32 C33 1.416(6) . ? C32 C36 1.442(6) . ? C33 C34 1.430(7) . ? C34 C35 1.423(7) . ? C35 C36 1.446(6) . ? C37 C38 1.395(8) . ? C37 C42 1.377(8) . ? C38 C39 1.391(8) . ? C39 C40 1.374(11) . ? C40 C41 1.355(11) . ? C41 C42 1.403(8) . ? C43 C44 1.381(7) . ? C43 C48 1.395(7) . ? C44 C45 1.389(8) . ? C45 C46 1.371(10) . ? C46 C47 1.392(9) . ? C47 C48 1.393(7) . ? Cl1 C49 1.749(10) . ? Cl2 C49 1.778(11) . ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 0.250 0.250 0.500 223.9 62.0 ? 2 0.250 0.750 0.000 223.9 62.0 ? 3 0.750 0.250 0.000 223.9 62.0 ? 4 0.750 -0.250 0.500 223.9 62.0 ?