#------------------------------------------------------------------------------ #$Date: 2024-06-25 01:18:42 +0300 (Tue, 25 Jun 2024) $ #$Revision: 292547 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/19/1571975.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_1571975 loop_ _publ_author_name 'Cobb, Caitlyn R.' 'Ngo, Ren K.' 'Dick, Emily J.' 'Lynch, Vincent M.' 'Rose, Michael J.' _publ_section_title ; Multi-phosphine-chelated iron-carbide clusters via redox-promoted ligand exchange on an inert hexa-iron-carbide carbonyl cluster, [Fe6(\m6-C)(\m2-CO)4(CO)12]2− ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC01370K _journal_year 2024 _chemical_formula_moiety 'C56 H39 Fe5 O14 P3' _chemical_formula_sum 'C56 H39 Fe5 O14 P3' _chemical_formula_weight 1308.03 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2023-03-17 _audit_creation_method ; Olex2 1.5 (compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748) ; _audit_update_record ; 2023-06-02 deposited with the CCDC. 2024-06-03 downloaded from the CCDC. ; _cell_angle_alpha 85.773(5) _cell_angle_beta 76.692(7) _cell_angle_gamma 89.678(5) _cell_formula_units_Z 2 _cell_length_a 9.4782(8) _cell_length_b 15.6679(7) _cell_length_c 18.6940(10) _cell_measurement_reflns_used 5090 _cell_measurement_temperature 100.0(6) _cell_measurement_theta_max 76.3730 _cell_measurement_theta_min 2.8430 _cell_volume 2694.0(3) _computing_cell_refinement 'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)' _computing_data_collection 'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)' _computing_data_reduction 'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.0(6) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.980 _diffrn_measured_fraction_theta_max 0.980 _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 -89.00 -64.00 0.50 30.00 -- -48.57-158.00 91.00 50 2 \w -89.00 -26.00 0.50 30.00 -- -48.57 119.00 -29.00 126 3 \w -107.00 -72.00 0.50 30.00 -- -48.57 158.00 125.00 70 4 \w 73.00 98.00 0.50 30.00 -- 48.57-158.00 91.00 50 5 \w 26.00 51.00 0.50 30.00 -- 48.57-119.00-113.00 50 6 \w 51.00 119.00 0.50 30.00 -- 48.57 158.00 125.00 136 7 \w -108.00 -83.00 0.50 40.00 -- -105.12 158.00 125.00 50 8 \w -112.00 -87.00 0.50 40.00 -- -105.12-158.00 91.00 50 9 \w -138.00 -87.00 0.50 40.00 -- -105.12-119.00-113.00 102 10 \w -109.00 -73.00 0.50 40.00 -- -105.12 119.00 -29.00 72 11 \w 81.00 106.00 0.50 40.00 -- 105.12 158.00 125.00 50 12 \w 34.00 107.00 0.50 40.00 -- 105.12-119.00-113.00 146 13 \w 95.00 125.00 0.50 40.00 -- 105.12 119.00 -29.00 60 14 \w 34.00 133.00 0.50 40.00 -- 105.12-158.00 91.00 198 15 \w -26.00 20.00 0.50 30.00 -- -48.57 19.00-120.00 92 16 \w -120.00 -83.00 0.50 30.00 -- -48.57-125.00 90.00 74 17 \w -119.00 -28.00 0.50 30.00 -- -48.57 -77.00 -90.00 182 18 \w -42.00 24.00 0.50 30.00 -- -48.57 38.00 150.00 132 19 \w 78.00 118.00 0.50 30.00 -- 48.57 125.00-120.00 80 20 \w -155.00 -83.00 0.50 40.00 -- -105.12 -95.00-150.00 144 21 \w -68.00 -39.00 0.50 40.00 -- -105.12 61.00 -60.00 58 22 \w -177.00-100.00 0.50 40.00 -- -105.12 -62.00 98.99 154 23 \w -125.00 -89.00 0.50 40.00 -- -105.12 -64.00 -0.73 72 24 \w -104.00 -33.00 0.50 40.00 -- -105.12 77.00 0.00 142 25 \w -82.00 -35.00 0.50 40.00 -- -105.12 77.00 120.00 94 26 \w -109.00 -64.00 0.50 40.00 -- -105.12 125.00-150.00 90 27 \w -170.00-130.00 0.50 40.00 -- -105.12 -64.00 -0.73 80 28 \w -155.00-129.00 0.50 40.00 -- -105.12 -15.00-150.00 52 29 \w -108.00 -70.00 0.50 40.00 -- -105.12 115.00 101.98 76 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Single source at home/near, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.1280399000 _diffrn_orient_matrix_UB_12 -0.0375399000 _diffrn_orient_matrix_UB_13 -0.0258885000 _diffrn_orient_matrix_UB_21 -0.0711106000 _diffrn_orient_matrix_UB_22 -0.0316712000 _diffrn_orient_matrix_UB_23 0.0801216000 _diffrn_orient_matrix_UB_31 -0.0803091000 _diffrn_orient_matrix_UB_32 0.0854976000 _diffrn_orient_matrix_UB_33 0.0110248000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.1154 _diffrn_reflns_av_unetI/netI 0.1132 _diffrn_reflns_Laue_measured_fraction_full 0.980 _diffrn_reflns_Laue_measured_fraction_max 0.980 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 16464 _diffrn_reflns_point_group_measured_fraction_full 0.980 _diffrn_reflns_point_group_measured_fraction_max 0.980 _diffrn_reflns_theta_full 50.431 _diffrn_reflns_theta_max 50.431 _diffrn_reflns_theta_min 2.828 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 11.949 _exptl_absorpt_correction_T_max 0.835 _exptl_absorpt_correction_T_min 0.386 _exptl_absorpt_correction_type 'gaussian and multi-scan' _exptl_absorpt_process_details ; CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022) 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 black _exptl_crystal_colour_primary black _exptl_crystal_density_diffrn 1.612 _exptl_crystal_description needle _exptl_crystal_F_000 1324 _exptl_crystal_size_max 0.136 _exptl_crystal_size_mid 0.059 _exptl_crystal_size_min 0.045 _refine_diff_density_max 1.134 _refine_diff_density_min -0.715 _refine_diff_density_rms 0.116 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 704 _refine_ls_number_reflns 5542 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.066 _refine_ls_R_factor_all 0.0943 _refine_ls_R_factor_gt 0.0693 _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^)+(0.1036P)^2^+5.0159P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1823 _refine_ls_wR_factor_ref 0.1980 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4045 _reflns_number_total 5542 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc01370k3.cif _cod_data_source_block compound7_auto _cod_database_code 1571975 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'Fe5 C56 O14 P3 H37 ' _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Secondary CH2 refined with riding coordinates: C13(H13A,H13B), C15(H15A,H15B), C17(H17A,H17B) 2.b Aromatic/amide H refined with riding coordinates: C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C33(H33), C34(H34), C35(H35), C36(H36), C37(H37), C39(H39), C40(H40), C41(H41), C42(H42), C43(H43), C45(H45), C46(H46), C47(H47), C48(H48), C49(H49) 2.c Idealised Me refined as rotating group: C19(H19A,H19B,H19C) ; _smtbx_masks_void_probe_radius 1.2 _smtbx_masks_void_truncation_radius 1.2 _shelx_res_file ; TITL fe5ctriphosmonoboundfullexp_auto_a.res in P-1 fe5ctriphosmonoboundfullexp_auto.res created by SHELXL-2018/3 at 13:15:46 on 17-Mar-2023 REM Old TITL fe5Ctriphosmonoboundfullexp_auto in P-1 REM SHELXT solution in P-1: R1 0.175, Rweak 0.029, Alpha 0.098 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C56 O76 P12 Fe5 CELL 1.54184 9.478179 15.667891 18.693992 85.7728 76.6919 89.6779 ZERR 2 0.000767 0.000746 0.00103 0.0046 0.0065 0.005 LATT 1 SFAC C H Fe O P UNIT 112 78 10 28 6 L.S. 4 PLAN 5 TEMP -173 CONF MORE -1 BOND $H ABIN fmap 2 acta SHEL 20 1 REM REM REM WGHT 0.103600 5.015900 FVAR 0.40386 FE1 3 0.677599 0.432196 0.842354 11.00000 0.02212 0.02629 = 0.03538 -0.00106 -0.00636 -0.00065 FE2 3 0.954941 0.458747 0.846018 11.00000 0.02593 0.03065 = 0.04046 0.00216 -0.01492 -0.00248 FE3 3 0.782139 0.586527 0.831116 11.00000 0.02562 0.02879 = 0.04657 -0.00193 -0.00924 -0.00056 FE4 3 1.000047 0.558378 0.723645 11.00000 0.02361 0.03660 = 0.03977 0.00184 -0.00793 0.00089 FE5 3 0.734961 0.527896 0.710747 11.00000 0.02619 0.03435 = 0.04469 0.00180 -0.01402 0.00055 P12 5 0.803216 0.246058 0.594269 11.00000 0.02585 0.03774 = 0.04154 0.00002 -0.00459 -0.00336 P16 5 0.447534 0.020667 0.734302 11.00000 0.02970 0.03245 = 0.03670 -0.00351 -0.00999 -0.00682 P18 5 0.638747 0.292577 0.829100 11.00000 0.02153 0.02901 = 0.03519 -0.00613 -0.00992 0.00017 O50 4 1.258163 0.624173 0.764262 11.00000 0.02993 0.05447 = 0.06331 0.01316 -0.01805 -0.01476 O52 4 0.898875 0.314753 0.956064 11.00000 0.04016 0.04177 = 0.04385 0.00594 -0.01406 -0.00062 O54 4 0.596479 0.413913 1.003675 11.00000 0.04307 0.04425 = 0.03914 -0.01396 -0.01706 0.00276 O56 4 0.748282 0.589238 0.991286 11.00000 0.04822 0.03468 = 0.04254 0.00059 0.00166 0.00115 O58 4 1.106596 0.561628 0.931516 11.00000 0.04080 0.03943 = 0.05339 -0.00517 -0.02324 0.00205 O60 4 1.206484 0.362384 0.773834 11.00000 0.03211 0.04051 = 0.05344 0.00102 -0.01216 0.00158 O62 4 0.956442 0.743006 0.813134 11.00000 0.03544 0.03828 = 0.06406 -0.00319 -0.01247 0.00049 O64 4 0.372417 0.473519 0.854938 11.00000 0.02214 0.05193 = 0.05769 0.00029 -0.00791 0.00294 O66 4 0.454378 0.477301 0.687546 11.00000 0.03891 0.05030 = 0.05264 0.00534 -0.01485 -0.00597 O68 4 1.002812 0.707521 0.618021 11.00000 0.02855 0.05314 = 0.04693 0.00835 -0.00309 -0.00343 O70 4 0.506517 0.674669 0.835536 11.00000 0.03599 0.06029 = 0.07706 -0.01496 -0.02942 0.00928 O72 4 0.673139 0.702235 0.658735 11.00000 0.04418 0.04490 = 0.09086 0.01333 -0.03147 0.00099 O74 4 1.165250 0.448173 0.615286 11.00000 0.05038 0.06543 = 0.06193 -0.01870 -0.01449 0.01843 O76 4 0.864302 0.473152 0.564543 11.00000 0.04840 0.07618 = 0.05525 -0.01185 -0.01637 -0.00116 C6 1 0.977810 0.190708 0.569937 11.00000 0.03359 0.04869 = 0.03847 -0.01469 -0.01539 0.00492 C7 1 1.101545 0.243233 0.537529 11.00000 0.02341 0.07017 = 0.04043 0.00581 -0.00657 -0.00934 AFIX 43 H7 2 1.090134 0.302497 0.525680 11.00000 -1.20000 AFIX 0 C8 1 1.237006 0.208182 0.523471 11.00000 0.02020 0.10430 = 0.03936 -0.01225 -0.00485 -0.00814 AFIX 43 H8 2 1.319773 0.243086 0.502088 11.00000 -1.20000 AFIX 0 C9 1 1.253010 0.120396 0.540809 11.00000 0.03153 0.11419 = 0.04386 -0.03416 -0.01510 0.02047 AFIX 43 H9 2 1.346722 0.095820 0.532042 11.00000 -1.20000 AFIX 0 C10 1 1.133498 0.070880 0.570210 11.00000 0.03252 0.05953 = 0.05704 -0.01069 -0.01045 0.00373 AFIX 43 H10 2 1.144088 0.011280 0.580868 11.00000 -1.20000 AFIX 0 C11 1 0.998327 0.105718 0.584632 11.00000 0.01681 0.05715 = 0.05953 -0.01715 -0.00333 0.00101 AFIX 43 H11 2 0.916619 0.069750 0.605432 11.00000 -1.20000 AFIX 0 C13 1 0.697914 0.166384 0.663847 11.00000 0.02122 0.03154 = 0.03344 0.00190 -0.00548 0.00798 AFIX 23 H13A 2 0.678427 0.116232 0.638167 11.00000 -1.20000 H13B 2 0.759288 0.146751 0.697980 11.00000 -1.20000 AFIX 0 C14 1 0.552681 0.196291 0.710039 11.00000 0.02005 0.03057 = 0.01935 0.00225 -0.00556 0.00164 C15 1 0.487424 0.123563 0.769226 11.00000 0.02134 0.03182 = 0.02889 0.00233 -0.00784 -0.00278 AFIX 23 H15A 2 0.396338 0.144408 0.800083 11.00000 -1.20000 H15B 2 0.555711 0.112295 0.801616 11.00000 -1.20000 AFIX 0 C17 1 0.569799 0.280889 0.745973 11.00000 0.02588 0.03045 = 0.03236 -0.00395 -0.00890 0.00440 AFIX 23 H17A 2 0.472497 0.306968 0.755963 11.00000 -1.20000 H17B 2 0.631882 0.318767 0.706612 11.00000 -1.20000 AFIX 0 C19 1 0.449399 0.217656 0.658720 11.00000 0.01990 0.03192 = 0.03166 0.00305 -0.00631 -0.00192 AFIX 137 H19A 2 0.489204 0.265976 0.623705 11.00000 -1.50000 H19B 2 0.354312 0.232876 0.688146 11.00000 -1.50000 H19C 2 0.438964 0.167713 0.631654 11.00000 -1.50000 AFIX 0 C20 1 0.621483 -0.035641 0.722072 11.00000 0.03435 0.02384 = 0.03824 -0.00166 -0.00734 0.00273 C21 1 0.680305 -0.068021 0.655281 11.00000 0.03927 0.03226 = 0.04727 -0.01323 -0.01678 0.00047 AFIX 43 H21 2 0.627523 -0.063802 0.617710 11.00000 -1.20000 AFIX 0 C22 1 0.813513 -0.106251 0.641819 11.00000 0.05203 0.03276 = 0.04551 -0.00685 -0.00664 0.01146 AFIX 43 H22 2 0.851457 -0.128945 0.595620 11.00000 -1.20000 AFIX 0 C23 1 0.892698 -0.111676 0.695907 11.00000 0.03821 0.04204 = 0.06766 -0.00125 -0.01522 0.01157 AFIX 43 H23 2 0.986139 -0.136613 0.686351 11.00000 -1.20000 AFIX 0 C24 1 0.833957 -0.080092 0.764895 11.00000 0.04487 0.03997 = 0.04112 -0.00041 -0.01856 0.01138 AFIX 43 H24 2 0.886476 -0.084499 0.802573 11.00000 -1.20000 AFIX 0 C25 1 0.702262 -0.043481 0.776983 11.00000 0.03770 0.03408 = 0.03317 -0.00085 -0.01150 0.00068 AFIX 43 H25 2 0.662727 -0.022388 0.823689 11.00000 -1.20000 AFIX 0 C26 1 0.504629 0.246355 0.908313 11.00000 0.02789 0.02602 = 0.04461 -0.00470 -0.01020 0.00752 C27 1 0.541539 0.219849 0.973907 11.00000 0.04185 0.02550 = 0.05194 -0.01548 -0.01728 -0.00254 AFIX 43 H27 2 0.640426 0.222730 0.976291 11.00000 -1.20000 AFIX 0 C28 1 0.441655 0.189852 1.035041 11.00000 0.05301 0.02736 = 0.05106 0.00575 -0.00932 -0.00815 AFIX 43 H28 2 0.471230 0.171393 1.078841 11.00000 -1.20000 AFIX 0 C29 1 0.298027 0.186401 1.033100 11.00000 0.04664 0.03841 = 0.05304 0.00007 0.00964 -0.00867 AFIX 43 H29 2 0.227949 0.164082 1.075123 11.00000 -1.20000 AFIX 0 C30 1 0.255584 0.215667 0.969466 11.00000 0.03320 0.03181 = 0.06977 -0.01817 -0.00555 -0.00282 AFIX 43 H30 2 0.155660 0.215376 0.968817 11.00000 -1.20000 AFIX 0 C31 1 0.357741 0.245457 0.906545 11.00000 0.03322 0.02844 = 0.03156 -0.00558 -0.00055 0.00670 AFIX 43 H31 2 0.328173 0.264924 0.862974 11.00000 -1.20000 AFIX 0 C32 1 0.344022 -0.034753 0.820226 11.00000 0.02346 0.03825 = 0.04831 0.00745 -0.00735 -0.00748 C33 1 0.301707 0.002981 0.886385 11.00000 0.06559 0.04061 = 0.08066 0.02311 0.02693 0.00178 AFIX 43 H33 2 0.335608 0.059311 0.889164 11.00000 -1.20000 AFIX 0 C34 1 0.209770 -0.038567 0.950517 11.00000 0.08203 0.04077 = 0.07686 0.02462 0.02366 0.01340 AFIX 43 H34 2 0.179728 -0.010969 0.995011 11.00000 -1.20000 AFIX 0 C35 1 0.167211 -0.120546 0.944339 11.00000 0.02261 0.08513 = 0.07614 0.03478 -0.01236 -0.01129 AFIX 43 H35 2 0.104383 -0.149986 0.985644 11.00000 -1.20000 AFIX 0 C36 1 0.210771 -0.161146 0.882104 11.00000 0.07412 0.06194 = 0.08911 0.02171 -0.03880 -0.04201 AFIX 43 H36 2 0.182472 -0.218895 0.880405 11.00000 -1.20000 AFIX 0 C37 1 0.300027 -0.116222 0.818746 11.00000 0.10663 0.05027 = 0.06255 0.00076 -0.02938 -0.03522 AFIX 43 H37 2 0.329161 -0.144345 0.774475 11.00000 -1.20000 AFIX 0 C38 1 0.800378 0.225960 0.814875 11.00000 0.03062 0.03306 = 0.03989 -0.01857 -0.01834 0.00376 C39 1 0.914937 0.255599 0.757326 11.00000 0.01836 0.03802 = 0.04843 0.00091 -0.01246 -0.00811 AFIX 43 H39 2 0.909315 0.309478 0.731334 11.00000 -1.20000 AFIX 0 C40 1 1.037240 0.205480 0.738467 11.00000 0.01545 0.05774 = 0.05391 -0.02445 -0.01236 0.00641 AFIX 43 H40 2 1.113388 0.223851 0.697646 11.00000 -1.20000 AFIX 0 C41 1 1.049297 0.129291 0.778398 11.00000 0.03024 0.04788 = 0.06693 -0.01603 -0.02108 0.01345 AFIX 43 H41 2 1.134212 0.096109 0.764993 11.00000 -1.20000 AFIX 0 C42 1 0.940574 0.100678 0.837175 11.00000 0.04151 0.03442 = 0.06242 -0.00540 -0.02307 0.00599 AFIX 43 H42 2 0.951720 0.049665 0.866020 11.00000 -1.20000 AFIX 0 C43 1 0.811625 0.148394 0.854106 11.00000 0.03626 0.04231 = 0.05485 -0.00458 -0.01450 0.00405 AFIX 43 H43 2 0.732586 0.127375 0.892360 11.00000 -1.20000 AFIX 0 C44 1 0.730485 0.230314 0.512736 11.00000 0.01766 0.04693 = 0.02426 0.01151 0.00329 0.00038 C45 1 0.678051 0.303723 0.479729 11.00000 0.03028 0.06887 = 0.04750 0.00524 -0.00152 -0.01132 AFIX 43 H45 2 0.679915 0.357252 0.500304 11.00000 -1.20000 AFIX 0 C46 1 0.624290 0.298473 0.418062 11.00000 0.03289 0.05835 = 0.05129 0.01228 -0.00754 0.00419 AFIX 43 H46 2 0.591888 0.349083 0.395877 11.00000 -1.20000 AFIX 0 C47 1 0.615951 0.222343 0.387514 11.00000 0.02447 0.08879 = 0.04501 0.00181 -0.00860 0.00535 AFIX 43 H47 2 0.576024 0.219165 0.345588 11.00000 -1.20000 AFIX 0 C48 1 0.668963 0.148638 0.420676 11.00000 0.03784 0.05692 = 0.05159 -0.01017 -0.01227 0.01453 AFIX 43 H48 2 0.666245 0.094722 0.400846 11.00000 -1.20000 AFIX 0 C49 1 0.724078 0.155567 0.481411 11.00000 0.04077 0.03709 = 0.04761 -0.00364 -0.01822 0.00074 AFIX 43 H49 2 0.759711 0.105468 0.502767 11.00000 -1.20000 AFIX 0 C51 1 1.158920 0.596939 0.750497 11.00000 0.02774 0.04167 = 0.03993 0.00128 -0.00131 0.00336 C53 1 0.910472 0.373437 0.913367 11.00000 0.03096 0.04131 = 0.03280 -0.00294 -0.00515 -0.00018 C55 1 0.630725 0.417315 0.940150 11.00000 0.03824 0.03245 = 0.05581 -0.01582 -0.01571 -0.00136 C57 1 0.765113 0.584060 0.929732 11.00000 0.04029 0.03611 = 0.05346 -0.00203 -0.00761 -0.00312 C59 1 1.050361 0.521456 0.897753 11.00000 0.02488 0.03734 = 0.03188 -0.00613 -0.00141 0.00072 C61 1 1.107184 0.400460 0.801270 11.00000 0.02714 0.02725 = 0.05280 -0.00454 -0.00927 -0.00173 C63 1 0.892231 0.680279 0.815145 11.00000 0.03720 0.02312 = 0.04085 -0.00207 -0.01381 0.00758 C65 1 0.492415 0.456527 0.847937 11.00000 0.05132 0.02112 = 0.03408 -0.00238 -0.01801 -0.00062 C67 1 0.561417 0.494845 0.702336 11.00000 0.02999 0.03662 = 0.04048 0.00532 -0.01564 -0.00391 C69 1 0.999624 0.648423 0.658968 11.00000 0.01949 0.05122 = 0.04868 0.01125 -0.00249 -0.00155 C71 1 0.613339 0.639661 0.832456 11.00000 0.03635 0.05242 = 0.05915 0.00338 -0.02147 -0.01617 C73 1 0.697908 0.633552 0.680365 11.00000 0.03045 0.04870 = 0.05980 -0.00110 -0.02415 -0.00730 C75 1 1.100258 0.489888 0.655701 11.00000 0.02368 0.05022 = 0.03585 -0.00169 -0.00631 -0.00347 C77 1 0.815151 0.490183 0.621980 11.00000 0.04478 0.02861 = 0.03706 0.00870 -0.01944 0.00075 C78 1 0.842980 0.483971 0.776668 11.00000 0.03721 0.03401 = 0.03374 -0.00058 -0.01179 0.01152 HKLF 4 REM fe5ctriphosmonoboundfullexp_auto_a.res in P-1 REM wR2 = 0.1980, GooF = S = 1.066, Restrained GooF = 1.066 for all data REM R1 = 0.0693 for 4045 Fo > 4sig(Fo) and 0.0943 for all 5542 data REM 704 parameters refined using 0 restraints END WGHT 0.1045 4.9014 REM Highest difference peak 1.134, deepest hole -0.715, 1-sigma level 0.116 Q1 1 0.7971 0.4169 0.6846 11.00000 0.05 1.13 Q2 1 1.0531 0.4591 0.7263 11.00000 0.05 1.12 Q3 1 0.8027 0.5571 0.7683 11.00000 0.05 0.85 Q4 1 0.8570 0.5363 0.7273 11.00000 0.05 0.84 Q5 1 0.8029 0.2946 0.6345 11.00000 0.05 0.74 ; _shelx_res_checksum 34425 _shelx_fab_file ; -11 -5 1 0.1052 0.5977 -11 -4 1 -0.3143 -0.4881 -11 -4 2 0.1408 0.4592 -11 -3 1 0.4004 0.3736 -11 -3 2 0.0091 -0.3905 -11 -3 3 -0.3907 0.3837 -11 -2 1 -0.3972 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-4 3 0.7350 -0.3135 10 -4 4 -1.0709 0.2882 10 -4 5 1.2635 -0.2790 10 -4 6 -1.3184 0.2812 10 -4 7 1.2610 -0.2802 10 -4 8 -1.1275 0.2588 10 -4 9 0.9561 -0.2044 10 -4 10 -0.7806 0.1151 10 -4 11 0.6274 -0.0018 10 -4 12 -0.5136 -0.1149 10 -4 13 0.4475 0.2105 10 -4 14 -0.4279 -0.2651 10 -4 15 0.4451 0.2694 10 -3 0 -0.4757 -0.5329 10 -3 1 0.1778 0.4960 10 -3 2 0.1203 -0.4353 10 -3 3 -0.3772 0.3718 10 -3 4 0.5702 -0.3211 10 -3 5 -0.6975 0.2876 10 -3 6 0.7740 -0.2636 10 -3 7 -0.8215 0.2342 10 -3 8 0.8594 -0.1845 10 -3 9 -0.8977 0.1072 10 -3 10 0.9351 -0.0071 10 -3 11 -0.9627 -0.0994 10 -3 12 0.9698 0.1894 10 -3 13 -0.9495 -0.2414 10 -3 14 0.9021 0.2431 10 -3 15 -0.8337 -0.1957 10 -3 16 0.7531 0.1139 10 -2 0 -0.0098 0.5205 10 -2 1 -0.0371 -0.4670 10 -2 2 0.0850 0.3987 10 -2 3 -0.1359 -0.3330 10 -2 4 0.1775 0.2795 10 -2 5 -0.1870 -0.2370 10 -2 6 0.1403 0.1957 10 -2 7 -0.0243 -0.1431 10 -2 8 -0.1557 0.0714 10 -2 9 0.3731 0.0170 10 -2 10 -0.5864 -0.1089 10 -2 11 0.7510 0.1833 10 -2 12 -0.8326 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3 -0.3838 0.2207 10 1 4 0.0402 -0.1671 10 1 5 0.3225 0.1007 10 1 6 -0.6294 -0.0199 10 1 7 0.8265 -0.0668 10 1 8 -0.8952 0.1415 10 1 9 0.8549 -0.1811 10 1 10 -0.7541 0.1663 10 1 11 0.6517 -0.0895 10 1 12 -0.5960 -0.0396 10 1 13 0.6090 0.1942 10 1 14 -0.6803 -0.3375 10 1 15 0.7723 0.4324 10 1 16 -0.8356 -0.4537 10 1 17 0.8274 0.3962 10 2 0 -0.7405 0.4129 10 2 1 1.0564 -0.3631 10 2 2 -1.1569 0.3137 10 2 3 1.0411 -0.2611 10 2 4 -0.7558 0.1982 10 2 5 0.3812 -0.1206 10 2 6 -0.0077 0.0318 10 2 7 -0.2881 0.0552 10 2 8 0.4622 -0.1195 10 2 9 -0.5101 0.1396 10 2 10 0.4616 -0.1017 10 2 11 -0.3660 0.0064 10 2 12 0.2731 0.1278 10 2 13 -0.2169 -0.2684 10 2 14 0.2074 0.3775 10 2 15 -0.2310 -0.4233 10 2 16 0.2605 0.3904 10 2 17 -0.2678 -0.2855 10 3 0 0.7830 -0.4589 10 3 1 -1.1610 0.4202 10 3 2 1.3242 -0.3739 10 3 3 -1.2681 0.3168 10 3 4 1.0355 -0.2450 10 3 5 -0.7031 0.1583 10 3 6 0.3592 -0.0640 10 3 7 -0.0807 -0.0225 10 3 8 -0.0842 0.0813 10 3 9 0.1244 -0.0942 10 3 10 -0.0614 0.0525 10 3 11 -0.0618 0.0378 10 3 12 0.1974 -0.1554 10 3 13 -0.3066 0.2683 10 3 14 0.3685 -0.3427 10 3 15 -0.3811 0.3540 10 3 16 0.3559 -0.2948 10 3 17 -0.3100 0.1784 10 4 0 -0.7064 0.5220 10 4 1 0.9171 -0.4978 10 4 2 -0.9793 0.4542 10 4 3 0.8984 -0.3908 10 4 4 -0.7124 0.3082 10 4 5 0.4797 -0.2106 10 4 6 -0.2622 0.1083 10 4 7 0.1089 -0.0165 10 4 8 -0.0449 -0.0471 10 4 9 0.0687 0.0681 10 4 10 -0.1572 -0.0409 10 4 11 0.2761 -0.0279 10 4 12 -0.3912 0.1194 10 4 13 0.4777 -0.2069 10 4 14 -0.5239 0.2634 10 4 15 0.5300 -0.2700 10 4 16 -0.5037 0.2221 10 5 0 0.4445 -0.6341 10 5 1 -0.4050 0.6189 10 5 2 0.3221 -0.5700 10 5 3 -0.2129 0.4916 10 5 4 0.1034 -0.3901 10 5 5 -0.0201 0.2746 10 5 6 -0.0190 -0.1570 10 5 7 0.0100 0.0516 10 5 8 0.0357 0.0275 10 5 9 -0.0968 -0.0690 10 5 10 0.1497 0.0682 10 5 11 -0.1771 -0.0293 10 5 12 0.1737 -0.0349 10 5 13 -0.1467 0.1057 10 5 14 0.1119 -0.1627 10 5 15 -0.0859 0.1905 10 5 16 0.0795 -0.1823 10 6 0 -0.0934 0.7941 10 6 1 -0.0830 -0.7723 10 6 2 0.2100 0.7027 10 6 3 -0.2708 -0.5960 10 6 4 0.2595 0.4655 10 6 5 -0.1846 -0.3251 10 6 6 0.0702 0.1879 10 6 7 0.0484 -0.0659 10 6 8 -0.1327 -0.0308 10 6 9 0.1511 0.0948 10 6 10 -0.0890 -0.1221 10 6 11 -0.0460 0.1133 10 6 12 0.2244 -0.0743 10 6 13 -0.4031 0.0156 10 6 14 0.5368 0.0492 10 6 15 -0.5916 -0.1066 10 7 0 -0.1349 -0.9359 10 7 1 0.2445 0.8884 10 7 2 -0.2694 -0.7836 10 7 3 0.2074 0.6397 10 7 4 -0.0733 -0.4772 10 7 5 -0.1014 0.3143 10 7 6 0.2732 -0.1647 10 7 7 -0.3947 0.0368 10 7 8 0.4250 0.0650 10 7 9 -0.3408 -0.1386 10 7 10 0.1438 0.1824 10 7 11 0.1366 -0.1956 10 7 12 -0.4484 0.1784 10 7 13 0.7287 -0.1337 10 7 14 -0.9187 0.0681 10 8 0 0.0961 0.9614 10 8 1 -0.0074 -0.8771 10 8 2 -0.1344 0.7339 10 8 3 0.3114 -0.5570 10 8 4 -0.4977 0.3731 10 8 5 0.6626 -0.2042 10 8 6 -0.7740 0.0630 10 8 7 0.8039 0.0467 10 8 8 -0.7338 -0.1277 10 8 9 0.5606 0.1856 10 8 10 -0.2995 -0.2242 10 8 11 -0.0150 0.2440 10 8 12 0.3343 -0.2424 10 8 13 -0.6045 0.2160 10 8 14 0.7779 -0.1644 10 9 0 0.1493 -0.8168 10 9 1 -0.4112 0.6997 10 9 2 0.6576 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-0.3064 -0.7225 11 -5 2 -0.0808 0.5684 11 -5 3 0.4075 -0.4023 11 -5 4 -0.6393 0.2562 11 -5 5 0.7660 -0.1504 11 -5 6 -0.8000 0.0884 11 -5 7 0.7682 -0.0582 11 -5 8 -0.7025 0.0393 11 -5 9 0.6307 -0.0115 11 -5 10 -0.5706 -0.0366 11 -5 11 0.5290 0.1035 11 -4 0 -0.6541 -0.6738 11 -4 1 0.4346 0.5399 11 -4 2 -0.2079 -0.3789 11 -4 3 0.0061 0.2268 11 -4 4 0.1554 -0.1119 11 -4 5 -0.2797 0.0463 11 -4 6 0.3836 -0.0242 11 -4 7 -0.4873 0.0258 11 -4 8 0.6045 -0.0266 11 -4 9 -0.7354 0.0072 11 -4 10 0.8656 0.0394 11 -4 11 -0.9712 -0.1054 11 -4 12 1.0275 0.1719 11 -3 0 0.4243 0.3697 11 -3 1 -0.4761 -0.2389 11 -3 2 0.5127 0.1067 11 -3 3 -0.5334 -0.0023 11 -3 4 0.5254 -0.0571 11 -3 5 -0.4674 0.0708 11 -3 6 0.3385 -0.0531 11 -3 7 -0.1297 0.0270 11 -3 8 -0.1473 -0.0145 11 -3 9 0.4579 0.0278 11 -3 10 -0.7511 -0.0653 11 -3 11 0.9723 0.1125 11 -3 12 -1.0787 -0.1482 11 -3 13 1.0525 0.1532 11 -2 0 -0.1082 -0.0637 11 -2 1 0.3544 -0.0456 11 -2 2 -0.6004 0.1337 11 -2 3 0.8200 -0.1830 11 -2 4 -0.9761 0.1892 11 -2 5 1.0294 -0.1618 11 -2 6 -0.9511 0.1197 11 -2 7 0.7367 -0.0834 11 -2 8 -0.4134 0.0667 11 -2 9 0.0380 -0.0717 11 -2 10 0.3145 0.0880 11 -2 11 -0.5704 -0.0978 11 -2 12 0.6780 0.0830 11 -2 13 -0.6228 -0.0336 11 -1 0 -0.2092 -0.1096 11 -1 1 -0.0280 0.1950 11 -1 2 0.3109 -0.2468 11 -1 3 -0.6075 0.2583 11 -1 4 0.8684 -0.2355 11 -1 5 -1.0389 0.1934 11 -1 6 1.0760 -0.1502 11 -1 7 -0.9641 0.1193 11 -1 8 0.7248 -0.1045 11 -1 9 -0.4146 0.0982 11 -1 10 0.1111 -0.0852 11 -1 11 0.1084 0.0494 11 -1 12 -0.1901 0.0188 11 -1 13 0.1200 -0.1169 11 0 0 0.4963 0.1072 11 0 1 -0.4559 -0.1770 11 0 2 0.3032 0.2123 11 0 3 -0.0591 -0.2142 11 0 4 -0.2262 0.1932 11 0 5 0.4859 -0.1645 11 0 6 -0.6572 0.1410 11 0 7 0.7011 -0.1275 11 0 8 -0.6155 0.1186 11 0 9 0.4372 -0.1011 11 0 10 -0.2300 0.0596 11 0 11 0.0648 0.0157 11 0 12 0.0038 -0.1235 11 0 13 0.0450 0.2491 11 0 14 -0.1915 -0.3679 11 1 0 -0.7320 0.0183 11 1 1 0.9298 0.0440 11 1 2 -0.9578 -0.0810 11 1 3 0.8206 0.0965 11 1 4 -0.5645 -0.1006 11 1 5 0.2631 0.1039 11 1 6 0.0036 -0.1120 11 1 7 -0.1734 0.1218 11 1 8 0.2183 -0.1220 11 1 9 -0.1506 0.0976 11 1 10 0.0163 -0.0369 11 1 11 0.1230 -0.0624 11 1 12 -0.2108 0.1890 11 1 13 0.2145 -0.3199 11 1 14 -0.1343 0.4259 11 2 0 0.8501 -0.1830 11 2 1 -1.1651 0.1265 11 2 2 1.2944 -0.0791 11 2 3 -1.2345 0.0383 11 2 4 1.0261 0.0016 11 2 5 -0.7410 -0.0441 11 2 6 0.4615 0.0875 11 2 7 -0.2573 -0.1226 11 2 8 0.1679 0.1355 11 2 9 -0.1944 -0.1123 11 2 10 0.3041 0.0456 11 2 11 -0.4441 0.0605 11 2 12 0.5596 -0.1891 11 2 13 -0.6107 0.3137 11 2 14 0.5830 -0.4050 11 3 0 -0.7641 0.3383 11 3 1 1.0190 -0.2894 11 3 2 -1.1288 0.2296 11 3 3 1.0924 -0.1602 11 3 4 -0.9426 0.0825 11 3 5 0.7358 -0.0002 11 3 6 -0.5355 -0.0781 11 3 7 0.3945 0.1397 11 3 8 -0.3421 -0.1699 11 3 9 0.3786 0.1571 11 3 10 -0.4783 -0.0972 11 3 11 0.6004 -0.0030 11 3 12 -0.7024 0.1251 11 3 13 0.7523 -0.2436 11 4 0 0.4639 -0.4802 11 4 1 -0.5625 0.4368 11 4 2 0.5972 -0.3620 11 4 3 -0.5721 0.2626 11 4 4 0.5064 -0.1475 11 4 5 -0.4280 0.0278 11 4 6 0.3644 0.0829 11 4 7 -0.3343 -0.1701 11 4 8 0.3434 0.2201 11 4 9 -0.3830 -0.2237 11 4 10 0.4352 0.1786 11 4 11 -0.4790 -0.0919 11 4 12 0.4976 -0.0207 11 4 13 -0.4831 0.1369 11 5 0 -0.0780 0.6058 11 5 1 0.0636 -0.5582 11 5 2 -0.0667 0.4624 11 5 3 0.0903 -0.3315 11 5 4 -0.1346 0.1821 11 5 5 0.1947 -0.0317 11 5 6 -0.2603 -0.1030 11 5 7 0.3171 0.2079 11 5 8 -0.3492 -0.2722 11 5 9 0.3441 0.2897 11 5 10 -0.2963 -0.2599 11 5 11 0.2109 0.1888 11 5 12 -0.1025 -0.0884 11 6 0 -0.1880 -0.6766 11 6 1 0.1923 0.6122 11 6 2 -0.1372 -0.4905 11 6 3 0.0290 0.3314 11 6 4 0.1137 -0.1582 11 6 5 -0.2634 -0.0070 11 6 6 0.3884 0.1469 11 6 7 -0.4590 -0.2501 11 6 8 0.4545 0.3109 11 6 9 -0.3686 -0.3286 11 6 10 0.2118 0.3059 11 6 11 -0.0107 -0.2483 11 7 2 -0.0336 0.4048 11 7 3 0.2064 -0.2308 11 7 4 -0.3816 0.0545 11 7 5 0.5289 0.1002 11 7 6 -0.6198 -0.2174 11 7 7 0.6339 0.2908 11 7 8 -0.5631 -0.3225 11 7 9 0.4141 0.3192 11 7 10 -0.2082 -0.2892 11 8 5 -0.6862 -0.2273 11 8 6 0.6813 0.2956 0 0 0 0.0 0.0 ; _shelx_fab_checksum 55725 _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 2.930 _oxdiff_exptl_absorpt_empirical_full_min 0.390 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -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 0.67760(15) 0.43220(8) 0.84235(8) 0.0280(4) Uani 1 1 d . . . . . Fe2 Fe 0.95494(16) 0.45875(9) 0.84602(9) 0.0314(5) Uani 1 1 d . . . . . Fe3 Fe 0.78214(16) 0.58653(9) 0.83112(9) 0.0335(5) Uani 1 1 d . . . . . Fe4 Fe 1.00005(16) 0.55838(9) 0.72364(9) 0.0335(5) Uani 1 1 d . . . . . Fe5 Fe 0.73496(16) 0.52790(9) 0.71075(9) 0.0344(5) Uani 1 1 d . . . . . P12 P 0.8032(3) 0.24606(16) 0.59427(15) 0.0357(7) Uani 1 1 d . . . . . P16 P 0.4475(3) 0.02067(15) 0.73430(15) 0.0325(7) Uani 1 1 d . . . . . P18 P 0.6387(3) 0.29258(14) 0.82910(14) 0.0278(6) Uani 1 1 d . . . . . O50 O 1.2582(8) 0.6242(4) 0.7643(4) 0.049(2) Uani 1 1 d . . . . . O52 O 0.8989(7) 0.3148(5) 0.9561(4) 0.0417(18) Uani 1 1 d . . . . . O54 O 0.5965(8) 0.4139(4) 1.0037(5) 0.0404(18) Uani 1 1 d . . . . . O56 O 0.7483(8) 0.5892(4) 0.9913(5) 0.0440(19) Uani 1 1 d . . . . . O58 O 1.1066(8) 0.5616(4) 0.9315(4) 0.0424(18) Uani 1 1 d . . . . . O60 O 1.2065(8) 0.3624(4) 0.7738(4) 0.0419(18) Uani 1 1 d . . . . . O62 O 0.9564(8) 0.7430(5) 0.8131(4) 0.0458(19) Uani 1 1 d . . . . . O64 O 0.3724(8) 0.4735(4) 0.8549(4) 0.0444(19) Uani 1 1 d . . . . . O66 O 0.4544(9) 0.4773(4) 0.6875(4) 0.0470(19) Uani 1 1 d . . . . . O68 O 1.0028(7) 0.7075(5) 0.6180(4) 0.0444(19) Uani 1 1 d . . . . . O70 O 0.5065(9) 0.6747(5) 0.8355(5) 0.055(2) Uani 1 1 d . . . . . O72 O 0.6731(8) 0.7022(5) 0.6587(5) 0.058(2) Uani 1 1 d . . . . . O74 O 1.1653(9) 0.4482(5) 0.6153(5) 0.058(2) Uani 1 1 d . . . . . O76 O 0.8643(9) 0.4732(5) 0.5645(5) 0.059(2) Uani 1 1 d . . . . . C6 C 0.9778(11) 0.1907(7) 0.5699(6) 0.039(3) Uani 1 1 d . . . . . C7 C 1.1015(11) 0.2432(8) 0.5375(6) 0.045(3) Uani 1 1 d . . . . . H7 H 1.090134 0.302497 0.525680 0.054 Uiso 1 1 calc R U . . . C8 C 1.2370(12) 0.2082(9) 0.5235(6) 0.055(3) Uani 1 1 d . . . . . H8 H 1.319773 0.243086 0.502088 0.065 Uiso 1 1 calc R U . . . C9 C 1.2530(13) 0.1204(10) 0.5408(7) 0.061(4) Uani 1 1 d . . . . . H9 H 1.346722 0.095820 0.532042 0.073 Uiso 1 1 calc R U . . . C10 C 1.1335(12) 0.0709(7) 0.5702(6) 0.049(3) Uani 1 1 d . . . . . H10 H 1.144088 0.011280 0.580868 0.059 Uiso 1 1 calc R U . . . C11 C 0.9983(11) 0.1057(7) 0.5846(6) 0.045(3) Uani 1 1 d . . . . . H11 H 0.916619 0.069750 0.605432 0.054 Uiso 1 1 calc R U . . . C13 C 0.6979(10) 0.1664(6) 0.6638(5) 0.029(2) Uani 1 1 d . . . . . H13A H 0.678427 0.116232 0.638167 0.035 Uiso 1 1 calc R U . . . H13B H 0.759288 0.146751 0.697980 0.035 Uiso 1 1 calc R U . . . C14 C 0.5527(9) 0.1963(5) 0.7100(5) 0.023(2) Uani 1 1 d . . . . . C15 C 0.4874(10) 0.1236(5) 0.7692(5) 0.027(2) Uani 1 1 d . . . . . H15A H 0.396338 0.144408 0.800083 0.033 Uiso 1 1 calc R U . . . H15B H 0.555711 0.112295 0.801616 0.033 Uiso 1 1 calc R U . . . C17 C 0.5698(10) 0.2809(6) 0.7460(5) 0.029(2) Uani 1 1 d . . . . . H17A H 0.472497 0.306968 0.755963 0.035 Uiso 1 1 calc R U . . . H17B H 0.631882 0.318767 0.706612 0.035 Uiso 1 1 calc R U . . . C19 C 0.4494(10) 0.2177(6) 0.6587(5) 0.028(2) Uani 1 1 d . . . . . H19A H 0.489204 0.265976 0.623705 0.042 Uiso 1 1 calc R U . . . H19B H 0.354312 0.232876 0.688146 0.042 Uiso 1 1 calc R U . . . H19C H 0.438964 0.167713 0.631654 0.042 Uiso 1 1 calc R U . . . C20 C 0.6215(11) -0.0356(5) 0.7221(6) 0.032(3) Uani 1 1 d . . . . . C21 C 0.6803(12) -0.0680(6) 0.6553(6) 0.038(3) Uani 1 1 d . . . . . H21 H 0.627523 -0.063802 0.617710 0.046 Uiso 1 1 calc R U . . . C22 C 0.8135(13) -0.1063(6) 0.6418(7) 0.044(3) Uani 1 1 d . . . . . H22 H 0.851457 -0.128945 0.595620 0.053 Uiso 1 1 calc R U . . . C23 C 0.8927(12) -0.1117(7) 0.6959(7) 0.049(3) Uani 1 1 d . . . . . H23 H 0.986139 -0.136613 0.686351 0.059 Uiso 1 1 calc R U . . . C24 C 0.8340(12) -0.0801(6) 0.7649(6) 0.041(3) Uani 1 1 d . . . . . H24 H 0.886476 -0.084499 0.802573 0.049 Uiso 1 1 calc R U . . . C25 C 0.7023(11) -0.0435(6) 0.7770(6) 0.035(3) Uani 1 1 d . . . . . H25 H 0.662727 -0.022388 0.823689 0.041 Uiso 1 1 calc R U . . . C26 C 0.5046(10) 0.2464(5) 0.9083(6) 0.032(3) Uani 1 1 d . . . . . C27 C 0.5415(12) 0.2198(6) 0.9739(6) 0.038(3) Uani 1 1 d . . . . . H27 H 0.640426 0.222730 0.976291 0.046 Uiso 1 1 calc R U . . . C28 C 0.4417(13) 0.1899(6) 1.0350(7) 0.045(3) Uani 1 1 d . . . . . H28 H 0.471230 0.171393 1.078841 0.054 Uiso 1 1 calc R U . . . C29 C 0.2980(13) 0.1864(6) 1.0331(7) 0.050(3) Uani 1 1 d . . . . . H29 H 0.227949 0.164082 1.075123 0.060 Uiso 1 1 calc R U . . . C30 C 0.2556(12) 0.2157(6) 0.9695(7) 0.045(3) Uani 1 1 d . . . . . H30 H 0.155660 0.215376 0.968817 0.054 Uiso 1 1 calc R U . . . C31 C 0.3577(11) 0.2455(6) 0.9065(6) 0.032(3) Uani 1 1 d . . . . . H31 H 0.328173 0.264924 0.862974 0.038 Uiso 1 1 calc R U . . . C32 C 0.3440(11) -0.0348(6) 0.8202(6) 0.037(3) Uani 1 1 d . . . . . C33 C 0.3017(14) 0.0030(7) 0.8864(8) 0.071(4) Uani 1 1 d . . . . . H33 H 0.335608 0.059311 0.889164 0.085 Uiso 1 1 calc R U . . . C34 C 0.2098(15) -0.0386(8) 0.9505(8) 0.075(5) Uani 1 1 d . . . . . H34 H 0.179728 -0.010969 0.995011 0.090 Uiso 1 1 calc R U . . . C35 C 0.1672(12) -0.1205(9) 0.9443(9) 0.063(4) Uani 1 1 d . . . . . H35 H 0.104383 -0.149986 0.985644 0.076 Uiso 1 1 calc R U . . . C36 C 0.2108(16) -0.1611(9) 0.8821(9) 0.073(4) Uani 1 1 d . . . . . H36 H 0.182472 -0.218895 0.880405 0.088 Uiso 1 1 calc R U . . . C37 C 0.3000(16) -0.1162(8) 0.8187(8) 0.072(4) Uani 1 1 d . . . . . H37 H 0.329161 -0.144345 0.774475 0.086 Uiso 1 1 calc R U . . . C38 C 0.8004(11) 0.2260(6) 0.8149(6) 0.032(3) Uani 1 1 d . . . . . C39 C 0.9149(10) 0.2556(6) 0.7573(6) 0.034(3) Uani 1 1 d . . . . . H39 H 0.909315 0.309478 0.731334 0.041 Uiso 1 1 calc R U . . . C40 C 1.0372(11) 0.2055(7) 0.7385(6) 0.041(3) Uani 1 1 d . . . . . H40 H 1.113388 0.223851 0.697646 0.049 Uiso 1 1 calc R U . . . C41 C 1.0493(12) 0.1293(7) 0.7784(7) 0.046(3) Uani 1 1 d . . . . . H41 H 1.134212 0.096109 0.764993 0.055 Uiso 1 1 calc R U . . . C42 C 0.9406(12) 0.1007(6) 0.8372(7) 0.044(3) Uani 1 1 d . . . . . H42 H 0.951720 0.049665 0.866020 0.053 Uiso 1 1 calc R U . . . C43 C 0.8116(12) 0.1484(6) 0.8541(6) 0.044(3) Uani 1 1 d . . . . . H43 H 0.732586 0.127375 0.892360 0.053 Uiso 1 1 calc R U . . . C44 C 0.7305(10) 0.2303(6) 0.5127(5) 0.032(3) Uani 1 1 d . . . . . C45 C 0.6781(12) 0.3037(8) 0.4797(7) 0.051(3) Uani 1 1 d . . . . . H45 H 0.679915 0.357252 0.500304 0.061 Uiso 1 1 calc R U . . . C46 C 0.6243(12) 0.2985(8) 0.4181(7) 0.049(3) Uani 1 1 d . . . . . H46 H 0.591888 0.349083 0.395877 0.058 Uiso 1 1 calc R U . . . C47 C 0.6160(11) 0.2223(9) 0.3875(7) 0.053(3) Uani 1 1 d . . . . . H47 H 0.576024 0.219165 0.345588 0.064 Uiso 1 1 calc R U . . . C48 C 0.6690(12) 0.1486(7) 0.4207(7) 0.048(3) Uani 1 1 d . . . . . H48 H 0.666245 0.094722 0.400846 0.058 Uiso 1 1 calc R U . . . C49 C 0.7241(11) 0.1556(7) 0.4814(6) 0.040(3) Uani 1 1 d . . . . . H49 H 0.759711 0.105468 0.502767 0.049 Uiso 1 1 calc R U . . . C51 C 1.1589(12) 0.5969(6) 0.7505(6) 0.038(3) Uani 1 1 d . . . . . C53 C 0.9105(11) 0.3734(7) 0.9134(6) 0.035(3) Uani 1 1 d . . . . . C55 C 0.6307(12) 0.4173(6) 0.9402(8) 0.041(3) Uani 1 1 d . . . . . C57 C 0.7651(12) 0.5841(6) 0.9297(8) 0.044(3) Uani 1 1 d . . . . . C59 C 1.0504(11) 0.5215(6) 0.8978(6) 0.032(2) Uani 1 1 d . . . . . C61 C 1.1072(12) 0.4005(6) 0.8013(6) 0.036(3) Uani 1 1 d . . . . . C63 C 0.8922(11) 0.6803(6) 0.8151(6) 0.033(3) Uani 1 1 d . . . . . C65 C 0.4924(14) 0.4565(6) 0.8479(6) 0.034(3) Uani 1 1 d . . . . . C67 C 0.5614(12) 0.4948(6) 0.7023(6) 0.035(3) Uani 1 1 d . . . . . C69 C 0.9996(10) 0.6484(7) 0.6590(6) 0.041(3) Uani 1 1 d . . . . . C71 C 0.6133(14) 0.6397(7) 0.8325(7) 0.048(3) Uani 1 1 d . . . . . C73 C 0.6979(11) 0.6336(8) 0.6804(7) 0.044(3) Uani 1 1 d . . . . . C75 C 1.1003(12) 0.4899(7) 0.6557(6) 0.037(3) Uani 1 1 d . . . . . C77 C 0.8152(12) 0.4902(6) 0.6220(7) 0.036(3) Uani 1 1 d . . . . . C78 C 0.8430(11) 0.4840(6) 0.7767(5) 0.035(3) 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 0.0221(9) 0.0263(8) 0.0354(10) -0.0011(7) -0.0064(7) -0.0007(6) Fe2 0.0259(9) 0.0306(8) 0.0405(10) 0.0022(7) -0.0149(8) -0.0025(7) Fe3 0.0256(9) 0.0288(8) 0.0466(11) -0.0019(7) -0.0092(8) -0.0006(7) Fe4 0.0236(9) 0.0366(9) 0.0398(11) 0.0018(7) -0.0079(8) 0.0009(7) Fe5 0.0262(9) 0.0344(9) 0.0447(11) 0.0018(8) -0.0140(8) 0.0005(7) P12 0.0258(15) 0.0377(14) 0.0415(18) 0.0000(13) -0.0046(13) -0.0034(12) P16 0.0297(15) 0.0325(13) 0.0367(17) -0.0035(12) -0.0100(13) -0.0068(11) P18 0.0215(14) 0.0290(13) 0.0352(16) -0.0061(11) -0.0099(12) 0.0002(10) O50 0.030(4) 0.054(4) 0.063(6) 0.013(4) -0.018(4) -0.015(4) O52 0.040(5) 0.042(4) 0.044(5) 0.006(4) -0.014(4) -0.001(3) O54 0.043(5) 0.044(4) 0.039(5) -0.014(4) -0.017(4) 0.003(3) O56 0.048(5) 0.035(4) 0.043(5) 0.001(4) 0.002(4) 0.001(3) O58 0.041(5) 0.039(4) 0.053(5) -0.005(4) -0.023(4) 0.002(3) O60 0.032(5) 0.041(4) 0.053(5) 0.001(4) -0.012(4) 0.002(4) O62 0.035(4) 0.038(4) 0.064(6) -0.003(4) -0.012(4) 0.000(4) O64 0.022(5) 0.052(4) 0.058(5) 0.000(4) -0.008(4) 0.003(4) O66 0.039(5) 0.050(4) 0.053(5) 0.005(4) -0.015(4) -0.006(4) O68 0.029(4) 0.053(5) 0.047(5) 0.008(4) -0.003(4) -0.003(3) O70 0.036(5) 0.060(5) 0.077(6) -0.015(4) -0.029(5) 0.009(4) O72 0.044(5) 0.045(5) 0.091(7) 0.013(5) -0.031(5) 0.001(4) O74 0.050(5) 0.065(5) 0.062(6) -0.019(5) -0.014(5) 0.018(4) O76 0.048(5) 0.076(6) 0.055(6) -0.012(5) -0.016(5) -0.001(4) C6 0.034(7) 0.049(7) 0.038(7) -0.015(5) -0.015(6) 0.005(5) C7 0.023(7) 0.070(7) 0.040(7) 0.006(6) -0.007(6) -0.009(6) C8 0.020(7) 0.104(11) 0.039(8) -0.012(7) -0.005(6) -0.008(7) C9 0.032(8) 0.114(12) 0.044(8) -0.034(8) -0.015(6) 0.020(8) C10 0.033(8) 0.060(7) 0.057(8) -0.011(6) -0.010(6) 0.004(6) C11 0.017(7) 0.057(8) 0.060(8) -0.017(6) -0.003(6) 0.001(5) C13 0.021(6) 0.032(5) 0.033(6) 0.002(5) -0.005(5) 0.008(4) C14 0.020(5) 0.031(5) 0.019(6) 0.002(4) -0.006(5) 0.002(4) C15 0.021(5) 0.032(5) 0.029(6) 0.002(5) -0.008(5) -0.003(4) C17 0.026(6) 0.030(5) 0.032(6) -0.004(5) -0.009(5) 0.004(4) C19 0.020(5) 0.032(5) 0.032(6) 0.003(4) -0.006(5) -0.002(4) C20 0.034(6) 0.024(5) 0.038(7) -0.002(5) -0.007(6) 0.003(4) C21 0.039(7) 0.032(5) 0.047(8) -0.013(5) -0.017(6) 0.000(5) C22 0.052(8) 0.033(6) 0.046(8) -0.007(5) -0.007(7) 0.011(6) C23 0.038(7) 0.042(6) 0.068(9) -0.001(6) -0.015(7) 0.012(5) C24 0.045(8) 0.040(6) 0.041(8) 0.000(6) -0.019(6) 0.011(5) C25 0.038(7) 0.034(5) 0.033(7) -0.001(5) -0.011(6) 0.001(5) C26 0.028(7) 0.026(5) 0.045(7) -0.005(5) -0.010(6) 0.008(4) C27 0.042(7) 0.025(5) 0.052(8) -0.015(5) -0.017(7) -0.003(5) C28 0.053(9) 0.027(5) 0.051(8) 0.006(5) -0.009(7) -0.008(5) C29 0.047(9) 0.038(6) 0.053(9) 0.000(6) 0.010(7) -0.009(5) C30 0.033(7) 0.032(6) 0.070(10) -0.018(6) -0.006(7) -0.003(5) C31 0.033(7) 0.028(5) 0.032(7) -0.006(5) -0.001(6) 0.007(5) C32 0.023(6) 0.038(6) 0.048(8) 0.007(6) -0.007(6) -0.007(5) C33 0.066(9) 0.041(7) 0.081(11) 0.023(8) 0.027(8) 0.002(6) C34 0.082(10) 0.041(8) 0.077(10) 0.025(7) 0.024(9) 0.013(7) C35 0.023(7) 0.085(11) 0.076(11) 0.035(9) -0.012(7) -0.011(6) C36 0.074(10) 0.062(8) 0.089(12) 0.022(9) -0.039(10) -0.042(8) C37 0.107(12) 0.050(8) 0.063(9) 0.001(7) -0.029(9) -0.035(8) C38 0.031(6) 0.033(6) 0.040(7) -0.019(5) -0.018(6) 0.004(5) C39 0.018(6) 0.038(6) 0.048(7) 0.001(5) -0.012(6) -0.008(5) C40 0.015(6) 0.058(7) 0.054(8) -0.024(6) -0.012(5) 0.006(5) C41 0.030(7) 0.048(7) 0.067(9) -0.016(7) -0.021(7) 0.013(6) C42 0.042(8) 0.034(6) 0.062(9) -0.005(6) -0.023(7) 0.006(6) C43 0.036(7) 0.042(6) 0.055(8) -0.005(6) -0.014(6) 0.004(5) C44 0.018(6) 0.047(7) 0.024(6) 0.012(5) 0.003(5) 0.000(5) C45 0.030(7) 0.069(8) 0.047(8) 0.005(6) -0.002(6) -0.011(6) C46 0.033(7) 0.058(8) 0.051(8) 0.012(7) -0.008(6) 0.004(5) C47 0.024(7) 0.089(10) 0.045(8) 0.002(7) -0.009(6) 0.005(6) C48 0.038(7) 0.057(7) 0.052(8) -0.010(6) -0.012(7) 0.015(6) C49 0.041(7) 0.037(6) 0.048(8) -0.004(6) -0.018(6) 0.001(5) C51 0.028(7) 0.042(6) 0.040(7) 0.001(5) -0.001(6) 0.003(5) C53 0.031(6) 0.041(6) 0.033(7) -0.003(6) -0.005(5) 0.000(5) C55 0.038(7) 0.032(6) 0.056(9) -0.016(6) -0.016(7) -0.001(5) C57 0.040(7) 0.036(6) 0.053(9) -0.002(6) -0.008(7) -0.003(5) C59 0.025(6) 0.037(6) 0.032(7) -0.006(5) -0.001(5) 0.001(5) C61 0.027(7) 0.027(5) 0.053(8) -0.005(5) -0.009(6) -0.002(5) C63 0.037(6) 0.023(6) 0.041(7) -0.002(5) -0.014(5) 0.008(5) C65 0.051(9) 0.021(5) 0.034(7) -0.002(4) -0.018(6) -0.001(5) C67 0.030(7) 0.037(6) 0.040(7) 0.005(5) -0.016(6) -0.004(5) C69 0.019(6) 0.051(7) 0.049(8) 0.011(7) -0.002(6) -0.002(5) C71 0.036(8) 0.052(7) 0.059(9) 0.003(6) -0.021(6) -0.016(6) C73 0.030(7) 0.049(7) 0.060(8) -0.001(6) -0.024(6) -0.007(5) C75 0.024(6) 0.050(7) 0.036(7) -0.002(6) -0.006(6) -0.003(5) C77 0.045(7) 0.029(5) 0.037(7) 0.009(5) -0.019(6) 0.001(5) C78 0.037(6) 0.034(5) 0.034(6) -0.001(5) -0.012(5) 0.012(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' 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' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 10 4 0.0143 1 -10 -3 0.0265 -6 1 -5 0.0402 0 -6 9 0.0268 0 6 -9 0.0268 -3 5 8 0.0225 3 -5 -8 0.0225 6 0 7 0.0806 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 Fe1 Fe5 87.18(6) . . ? Fe3 Fe1 Fe2 59.51(5) . . ? Fe3 Fe1 Fe5 58.98(6) . . ? P18 Fe1 Fe2 110.29(9) . . ? P18 Fe1 Fe3 165.10(10) . . ? P18 Fe1 Fe5 112.22(9) . . ? C55 Fe1 Fe2 89.9(3) . . ? C55 Fe1 Fe3 97.8(3) . . ? C55 Fe1 Fe5 154.3(3) . . ? C55 Fe1 P18 92.8(3) . . ? C55 Fe1 C78 131.1(5) . . ? C65 Fe1 Fe2 157.8(3) . . ? C65 Fe1 Fe3 99.2(3) . . ? C65 Fe1 Fe5 86.5(3) . . ? C65 Fe1 P18 91.8(3) . . ? C65 Fe1 C55 86.7(5) . . ? C65 Fe1 C78 127.9(4) . . ? C78 Fe1 Fe2 44.4(3) . . ? C78 Fe1 Fe3 49.3(3) . . ? C78 Fe1 Fe5 43.1(3) . . ? C78 Fe1 P18 115.8(3) . . ? Fe3 Fe2 Fe1 58.60(5) . . ? Fe3 Fe2 Fe4 59.20(6) . . ? Fe4 Fe2 Fe1 91.64(6) . . ? C53 Fe2 Fe1 80.0(3) . . ? C53 Fe2 Fe3 124.0(3) . . ? C53 Fe2 Fe4 165.1(3) . . ? C53 Fe2 C59 95.8(5) . . ? C53 Fe2 C61 89.1(5) . . ? C53 Fe2 C78 121.7(5) . . ? C59 Fe2 Fe1 136.3(3) . . ? C59 Fe2 Fe3 91.0(3) . . ? C59 Fe2 Fe4 98.7(3) . . ? C59 Fe2 C78 135.1(4) . . ? C61 Fe2 Fe1 126.5(3) . . ? C61 Fe2 Fe3 145.1(3) . . ? C61 Fe2 Fe4 85.9(3) . . ? C61 Fe2 C59 96.7(4) . . ? C61 Fe2 C78 106.8(5) . . ? C78 Fe2 Fe1 45.1(3) . . ? C78 Fe2 Fe3 48.8(3) . . ? C78 Fe2 Fe4 47.3(3) . . ? Fe1 Fe3 Fe2 61.89(5) . . ? Fe1 Fe3 Fe5 63.07(6) . . ? Fe2 Fe3 Fe5 90.73(7) . . ? Fe4 Fe3 Fe1 94.43(7) . . ? Fe4 Fe3 Fe2 60.49(6) . . ? Fe4 Fe3 Fe5 60.56(6) . . ? C57 Fe3 Fe1 91.4(3) . . ? C57 Fe3 Fe2 81.0(3) . . ? C57 Fe3 Fe4 131.8(4) . . ? C57 Fe3 Fe5 153.9(3) . . ? C57 Fe3 C78 120.9(4) . . ? C63 Fe3 Fe1 166.7(3) . . ? C63 Fe3 Fe2 106.1(3) . . ? C63 Fe3 Fe4 73.7(3) . . ? C63 Fe3 Fe5 113.9(3) . . ? C63 Fe3 C57 92.2(5) . . ? C63 Fe3 C71 96.5(4) . . ? C63 Fe3 C78 121.2(4) . . ? C71 Fe3 Fe1 95.9(3) . . ? C71 Fe3 Fe2 157.2(3) . . ? C71 Fe3 Fe4 131.5(4) . . ? C71 Fe3 Fe5 82.8(4) . . ? C71 Fe3 C57 95.2(5) . . ? C71 Fe3 C78 123.4(5) . . ? C78 Fe3 Fe1 46.7(3) . . ? C78 Fe3 Fe2 45.6(3) . . ? C78 Fe3 Fe4 47.7(3) . . ? C78 Fe3 Fe5 45.3(3) . . ? Fe2 Fe4 Fe5 90.51(6) . . ? Fe3 Fe4 Fe2 60.31(6) . . ? Fe3 Fe4 Fe5 60.35(6) . . ? C51 Fe4 Fe2 86.0(3) . . ? C51 Fe4 Fe3 105.8(3) . . ? C51 Fe4 Fe5 165.2(3) . . ? C51 Fe4 C75 95.0(5) . . ? C51 Fe4 C78 130.9(4) . . ? C69 Fe4 Fe2 162.4(4) . . ? C69 Fe4 Fe3 103.4(3) . . ? C69 Fe4 Fe5 86.0(3) . . ? C69 Fe4 C51 93.0(5) . . ? C69 Fe4 C75 94.8(5) . . ? C69 Fe4 C78 130.2(4) . . ? C75 Fe4 Fe2 102.7(3) . . ? C75 Fe4 Fe3 151.3(3) . . ? C75 Fe4 Fe5 99.8(3) . . ? C75 Fe4 C78 102.1(4) . . ? C78 Fe4 Fe2 45.5(3) . . ? C78 Fe4 Fe3 49.3(3) . . ? C78 Fe4 Fe5 45.2(3) . . ? Fe3 Fe5 Fe1 57.95(5) . . ? Fe3 Fe5 Fe4 59.10(6) . . ? Fe4 Fe5 Fe1 90.47(6) . . ? C67 Fe5 Fe1 86.3(3) . . ? C67 Fe5 Fe3 123.1(4) . . ? C67 Fe5 Fe4 173.5(3) . . ? C67 Fe5 C77 90.2(5) . . ? C67 Fe5 C78 128.5(4) . . ? C73 Fe5 Fe1 135.7(4) . . ? C73 Fe5 Fe3 89.0(4) . . ? C73 Fe5 Fe4 96.7(3) . . ? C73 Fe5 C67 89.5(4) . . ? C73 Fe5 C77 97.9(5) . . ? C73 Fe5 C78 132.7(5) . . ? C77 Fe5 Fe1 126.2(3) . . ? C77 Fe5 Fe3 146.2(4) . . ? C77 Fe5 Fe4 87.2(4) . . ? C77 Fe5 C78 107.5(4) . . ? C78 Fe5 Fe1 44.0(3) . . ? C78 Fe5 Fe3 48.8(3) . . ? C78 Fe5 Fe4 47.2(3) . . ? C6 P12 C13 100.3(4) . . ? C6 P12 C44 100.8(5) . . ? C44 P12 C13 102.2(4) . . ? C20 P16 C15 103.1(4) . . ? C32 P16 C15 100.0(5) . . ? C32 P16 C20 101.1(5) . . ? C17 P18 Fe1 110.5(3) . . ? C26 P18 Fe1 110.2(3) . . ? C26 P18 C17 108.1(5) . . ? C26 P18 C38 109.0(5) . . ? C38 P18 Fe1 115.3(3) . . ? C38 P18 C17 103.4(4) . . ? C7 C6 P12 116.3(8) . . ? C11 C6 P12 125.3(8) . . ? C11 C6 C7 118.3(10) . . ? C6 C7 H7 120.0 . . ? C8 C7 C6 119.9(11) . . ? C8 C7 H7 120.0 . . ? C7 C8 H8 120.1 . . ? C7 C8 C9 119.7(11) . . ? C9 C8 H8 120.1 . . ? C8 C9 H9 120.2 . . ? C10 C9 C8 119.5(11) . . ? C10 C9 H9 120.2 . . ? C9 C10 H10 119.6 . . ? C9 C10 C11 120.9(11) . . ? C11 C10 H10 119.6 . . ? C6 C11 C10 121.6(10) . . ? C6 C11 H11 119.2 . . ? C10 C11 H11 119.2 . . ? P12 C13 H13A 108.1 . . ? P12 C13 H13B 108.1 . . ? H13A C13 H13B 107.3 . . ? C14 C13 P12 116.6(6) . . ? C14 C13 H13A 108.1 . . ? C14 C13 H13B 108.1 . . ? C13 C14 C15 108.9(7) . . ? C13 C14 C17 112.0(7) . . ? C13 C14 C19 108.9(8) . . ? C15 C14 C17 111.3(7) . . ? C19 C14 C15 110.5(7) . . ? C19 C14 C17 105.3(7) . . ? P16 C15 H15A 108.2 . . ? P16 C15 H15B 108.2 . . ? C14 C15 P16 116.3(6) . . ? C14 C15 H15A 108.2 . . ? C14 C15 H15B 108.2 . . ? H15A C15 H15B 107.4 . . ? P18 C17 H17A 105.6 . . ? P18 C17 H17B 105.6 . . ? C14 C17 P18 126.9(6) . . ? C14 C17 H17A 105.6 . . ? C14 C17 H17B 105.6 . . ? H17A C17 H17B 106.1 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 P16 119.1(8) . . ? C21 C20 C25 117.9(9) . . ? C25 C20 P16 123.0(8) . . ? C20 C21 H21 119.3 . . ? C22 C21 C20 121.4(11) . . ? C22 C21 H21 119.3 . . ? C21 C22 H22 120.1 . . ? C21 C22 C23 119.8(11) . . ? C23 C22 H22 120.1 . . ? C22 C23 H23 120.1 . . ? C22 C23 C24 119.7(10) . . ? C24 C23 H23 120.1 . . ? C23 C24 H24 120.4 . . ? C25 C24 C23 119.3(10) . . ? C25 C24 H24 120.4 . . ? C20 C25 H25 119.1 . . ? C24 C25 C20 121.8(10) . . ? C24 C25 H25 119.1 . . ? C27 C26 P18 121.6(8) . . ? C27 C26 C31 118.1(9) . . ? C31 C26 P18 119.9(8) . . ? C26 C27 H27 118.7 . . ? C28 C27 C26 122.5(10) . . ? C28 C27 H27 118.7 . . ? C27 C28 H28 120.2 . . ? C27 C28 C29 119.6(11) . . ? C29 C28 H28 120.2 . . ? C28 C29 H29 120.2 . . ? C28 C29 C30 119.7(10) . . ? C30 C29 H29 120.2 . . ? C29 C30 H30 119.6 . . ? C29 C30 C31 120.8(10) . . ? C31 C30 H30 119.6 . . ? C26 C31 H31 120.4 . . ? C30 C31 C26 119.2(10) . . ? C30 C31 H31 120.4 . . ? C33 C32 P16 124.2(8) . . ? C37 C32 P16 118.6(10) . . ? C37 C32 C33 117.2(11) . . ? C32 C33 H33 118.4 . . ? C32 C33 C34 123.2(12) . . ? C34 C33 H33 118.4 . . ? C33 C34 H34 121.9 . . ? C35 C34 C33 116.2(14) . . ? C35 C34 H34 121.9 . . ? C34 C35 H35 118.7 . . ? C36 C35 C34 122.7(12) . . ? C36 C35 H35 118.7 . . ? C35 C36 H36 120.5 . . ? C35 C36 C37 119.1(12) . . ? C37 C36 H36 120.5 . . ? C32 C37 C36 121.6(13) . . ? C32 C37 H37 119.2 . . ? C36 C37 H37 119.2 . . ? C39 C38 P18 115.3(7) . . ? C43 C38 P18 124.7(8) . . ? C43 C38 C39 119.9(9) . . ? C38 C39 H39 120.4 . . ? C40 C39 C38 119.3(10) . . ? C40 C39 H39 120.4 . . ? C39 C40 H40 119.7 . . ? C41 C40 C39 120.7(10) . . ? C41 C40 H40 119.7 . . ? C40 C41 H41 119.5 . . ? C42 C41 C40 121.0(10) . . ? C42 C41 H41 119.5 . . ? C41 C42 H42 120.6 . . ? C41 C42 C43 118.9(10) . . ? C43 C42 H42 120.6 . . ? C38 C43 C42 120.1(10) . . ? C38 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C45 C44 P12 116.3(8) . . ? C49 C44 P12 126.4(8) . . ? C49 C44 C45 117.3(10) . . ? C44 C45 H45 119.8 . . ? C46 C45 C44 120.4(11) . . ? C46 C45 H45 119.8 . . ? C45 C46 H46 119.0 . . ? C47 C46 C45 121.9(11) . . ? C47 C46 H46 119.0 . . ? C46 C47 H47 121.2 . . ? C46 C47 C48 117.6(11) . . ? C48 C47 H47 121.2 . . ? C47 C48 H48 120.2 . . ? C49 C48 C47 119.5(11) . . ? C49 C48 H48 120.2 . . ? C44 C49 C48 123.3(10) . . ? C44 C49 H49 118.4 . . ? C48 C49 H49 118.4 . . ? O50 C51 Fe4 176.4(9) . . ? O52 C53 Fe2 171.7(9) . . ? O54 C55 Fe1 174.8(9) . . ? O56 C57 Fe3 173.9(10) . . ? O58 C59 Fe2 178.0(9) . . ? O60 C61 Fe2 178.5(10) . . ? O62 C63 Fe3 172.0(9) . . ? O64 C65 Fe1 176.6(9) . . ? O66 C67 Fe5 171.2(9) . . ? O68 C69 Fe4 177.9(9) . . ? O70 C71 Fe3 177.6(11) . . ? O72 C73 Fe5 178.3(10) . . ? O74 C75 Fe4 177.7(10) . . ? O76 C77 Fe5 174.5(9) . . ? Fe1 C78 Fe3 84.0(4) . . ? Fe1 C78 Fe4 166.9(6) . . ? Fe2 C78 Fe1 90.5(4) . . ? Fe2 C78 Fe3 85.6(4) . . ? Fe2 C78 Fe4 87.1(4) . . ? Fe4 C78 Fe3 83.0(4) . . ? Fe5 C78 Fe1 92.9(4) . . ? Fe5 C78 Fe2 170.5(6) . . ? Fe5 C78 Fe3 86.0(4) . . ? Fe5 C78 Fe4 87.6(4) . . ? 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 Fe2 2.681(2) . ? Fe1 Fe3 2.5940(19) . ? Fe1 Fe5 2.729(2) . ? Fe1 P18 2.261(3) . ? Fe1 C55 1.777(14) . ? Fe1 C65 1.775(13) . ? Fe1 C78 1.898(10) . ? Fe2 Fe3 2.619(2) . ? Fe2 Fe4 2.624(2) . ? Fe2 C53 1.750(12) . ? Fe2 C59 1.809(12) . ? Fe2 C61 1.777(12) . ? Fe2 C78 1.875(10) . ? Fe3 Fe4 2.590(2) . ? Fe3 Fe5 2.623(2) . ? Fe3 C57 1.811(15) . ? Fe3 C63 1.773(11) . ? Fe3 C71 1.795(14) . ? Fe3 C78 1.978(9) . ? Fe4 Fe5 2.628(2) . ? Fe4 C51 1.813(13) . ? Fe4 C69 1.790(12) . ? Fe4 C75 1.817(13) . ? Fe4 C78 1.931(10) . ? Fe5 C67 1.772(11) . ? Fe5 C73 1.770(12) . ? Fe5 C77 1.800(14) . ? Fe5 C78 1.868(10) . ? P12 C6 1.842(11) . ? P12 C13 1.850(9) . ? P12 C44 1.844(11) . ? P16 C15 1.856(9) . ? P16 C20 1.841(10) . ? P16 C32 1.837(11) . ? P18 C17 1.840(10) . ? P18 C26 1.822(10) . ? P18 C38 1.828(10) . ? O50 C51 1.125(12) . ? O52 C53 1.161(11) . ? O54 C55 1.154(13) . ? O56 C57 1.134(13) . ? O58 C59 1.138(11) . ? O60 C61 1.149(11) . ? O62 C63 1.153(11) . ? O64 C65 1.147(12) . ? O66 C67 1.151(12) . ? O68 C69 1.153(11) . ? O70 C71 1.141(13) . ? O72 C73 1.163(12) . ? O74 C75 1.110(12) . ? O76 C77 1.119(12) . ? C6 C7 1.425(14) . ? C6 C11 1.362(15) . ? C7 H7 0.9500 . ? C7 C8 1.370(16) . ? C8 H8 0.9500 . ? C8 C9 1.405(18) . ? C9 H9 0.9500 . ? C9 C10 1.359(17) . ? C10 H10 0.9500 . ? C10 C11 1.366(15) . ? C11 H11 0.9500 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C13 C14 1.538(13) . ? C14 C15 1.553(12) . ? C14 C17 1.555(13) . ? C14 C19 1.540(13) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.377(14) . ? C20 C25 1.413(14) . ? C21 H21 0.9500 . ? C21 C22 1.372(15) . ? C22 H22 0.9500 . ? C22 C23 1.389(16) . ? C23 H23 0.9500 . ? C23 C24 1.407(15) . ? C24 H24 0.9500 . ? C24 C25 1.349(14) . ? C25 H25 0.9500 . ? C26 C27 1.385(14) . ? C26 C31 1.400(14) . ? C27 H27 0.9500 . ? C27 C28 1.361(15) . ? C28 H28 0.9500 . ? C28 C29 1.372(16) . ? C29 H29 0.9500 . ? C29 C30 1.387(16) . ? C30 H30 0.9500 . ? C30 C31 1.392(15) . ? C31 H31 0.9500 . ? C32 C33 1.384(17) . ? C32 C37 1.349(15) . ? C33 H33 0.9500 . ? C33 C34 1.425(17) . ? C34 H34 0.9500 . ? C34 C35 1.369(19) . ? C35 H35 0.9500 . ? C35 C36 1.347(19) . ? C36 H36 0.9500 . ? C36 C37 1.427(19) . ? C37 H37 0.9500 . ? C38 C39 1.395(14) . ? C38 C43 1.389(14) . ? C39 H39 0.9500 . ? C39 C40 1.388(14) . ? C40 H40 0.9500 . ? C40 C41 1.379(15) . ? C41 H41 0.9500 . ? C41 C42 1.372(15) . ? C42 H42 0.9500 . ? C42 C43 1.414(15) . ? C43 H43 0.9500 . ? C44 C45 1.407(15) . ? C44 C49 1.355(14) . ? C45 H45 0.9500 . ? C45 C46 1.371(16) . ? C46 H46 0.9500 . ? C46 C47 1.370(17) . ? C47 H47 0.9500 . ? C47 C48 1.415(16) . ? C48 H48 0.9500 . ? C48 C49 1.366(15) . ? C49 H49 0.9500 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Fe1 Fe2 C78 Fe3 83.9(4) . . . . ? Fe1 Fe2 C78 Fe4 167.1(5) . . . . ? Fe1 Fe5 C78 Fe3 -83.8(4) . . . . ? Fe1 Fe5 C78 Fe4 -166.9(6) . . . . ? Fe1 P18 C17 C14 169.4(7) . . . . ? Fe1 P18 C26 C27 -80.6(8) . . . . ? Fe1 P18 C26 C31 92.5(7) . . . . ? Fe1 P18 C38 C39 -53.2(8) . . . . ? Fe1 P18 C38 C43 130.3(8) . . . . ? Fe2 Fe1 C78 Fe3 -85.5(4) . . . . ? Fe2 Fe1 C78 Fe4 -80(3) . . . . ? Fe2 Fe1 C78 Fe5 -171.2(6) . . . . ? Fe3 Fe1 C78 Fe2 85.5(4) . . . . ? Fe3 Fe1 C78 Fe4 6(2) . . . . ? Fe3 Fe1 C78 Fe5 -85.6(4) . . . . ? Fe3 Fe2 C78 Fe1 -83.9(4) . . . . ? Fe3 Fe2 C78 Fe4 83.2(3) . . . . ? Fe3 Fe5 C78 Fe1 83.8(4) . . . . ? Fe3 Fe5 C78 Fe4 -83.1(4) . . . . ? Fe4 Fe2 C78 Fe1 -167.1(5) . . . . ? Fe4 Fe2 C78 Fe3 -83.2(3) . . . . ? Fe4 Fe5 C78 Fe1 166.9(6) . . . . ? Fe4 Fe5 C78 Fe3 83.1(4) . . . . ? Fe5 Fe1 C78 Fe2 171.2(6) . . . . ? Fe5 Fe1 C78 Fe3 85.6(4) . . . . ? Fe5 Fe1 C78 Fe4 91(3) . . . . ? P12 C6 C7 C8 174.6(9) . . . . ? P12 C6 C11 C10 -174.5(9) . . . . ? P12 C13 C14 C15 -175.3(6) . . . . ? P12 C13 C14 C17 -51.8(10) . . . . ? P12 C13 C14 C19 64.2(9) . . . . ? P12 C44 C45 C46 178.8(8) . . . . ? P12 C44 C49 C48 -179.8(8) . . . . ? P16 C20 C21 C22 176.3(8) . . . . ? P16 C20 C25 C24 -175.5(7) . . . . ? P16 C32 C33 C34 173.8(10) . . . . ? P16 C32 C37 C36 -175.6(10) . . . . ? P18 Fe1 C78 Fe2 -93.2(3) . . . . ? P18 Fe1 C78 Fe3 -178.75(16) . . . . ? P18 Fe1 C78 Fe4 -173(2) . . . . ? P18 Fe1 C78 Fe5 95.6(3) . . . . ? P18 C26 C27 C28 176.0(7) . . . . ? P18 C26 C31 C30 -175.3(7) . . . . ? P18 C38 C39 C40 -174.6(8) . . . . ? P18 C38 C43 C42 178.2(8) . . . . ? C6 P12 C13 C14 167.9(7) . . . . ? C6 P12 C44 C45 -130.9(7) . . . . ? C6 P12 C44 C49 48.5(10) . . . . ? C6 C7 C8 C9 0.3(17) . . . . ? C7 C6 C11 C10 1.1(17) . . . . ? C7 C8 C9 C10 1.1(18) . . . . ? C8 C9 C10 C11 -1.5(18) . . . . ? C9 C10 C11 C6 0.3(18) . . . . ? C11 C6 C7 C8 -1.4(16) . . . . ? C13 P12 C6 C7 -158.6(8) . . . . ? C13 P12 C6 C11 17.1(10) . . . . ? C13 P12 C44 C45 126.0(7) . . . . ? C13 P12 C44 C49 -54.7(10) . . . . ? C13 C14 C15 P16 -60.6(9) . . . . ? C13 C14 C17 P18 -78.9(10) . . . . ? C15 P16 C20 C21 -127.8(7) . . . . ? C15 P16 C20 C25 48.7(8) . . . . ? C15 P16 C32 C33 6.6(11) . . . . ? C15 P16 C32 C37 -176.6(10) . . . . ? C15 C14 C17 P18 43.2(11) . . . . ? C17 P18 C26 C27 158.6(7) . . . . ? C17 P18 C26 C31 -28.4(8) . . . . ? C17 P18 C38 C39 67.5(8) . . . . ? C17 P18 C38 C43 -109.0(9) . . . . ? C17 C14 C15 P16 175.6(6) . . . . ? C19 C14 C15 P16 59.0(9) . . . . ? C19 C14 C17 P18 162.9(7) . . . . ? C20 P16 C15 C14 86.3(7) . . . . ? C20 P16 C32 C33 112.2(11) . . . . ? C20 P16 C32 C37 -71.0(11) . . . . ? C20 C21 C22 C23 -1.0(15) . . . . ? C21 C20 C25 C24 1.0(14) . . . . ? C21 C22 C23 C24 1.8(15) . . . . ? C22 C23 C24 C25 -1.2(15) . . . . ? C23 C24 C25 C20 -0.2(14) . . . . ? C25 C20 C21 C22 -0.4(14) . . . . ? C26 P18 C17 C14 -69.9(9) . . . . ? C26 P18 C38 C39 -177.7(7) . . . . ? C26 P18 C38 C43 5.8(10) . . . . ? C26 C27 C28 C29 -1.0(15) . . . . ? C27 C26 C31 C30 -2.0(13) . . . . ? C27 C28 C29 C30 -1.7(15) . . . . ? C28 C29 C30 C31 2.5(15) . . . . ? C29 C30 C31 C26 -0.6(14) . . . . ? C31 C26 C27 C28 2.9(14) . . . . ? C32 P16 C15 C14 -169.8(7) . . . . ? C32 P16 C20 C21 129.1(8) . . . . ? C32 P16 C20 C25 -54.4(8) . . . . ? C32 C33 C34 C35 2(2) . . . . ? C33 C32 C37 C36 1(2) . . . . ? C33 C34 C35 C36 1(2) . . . . ? C34 C35 C36 C37 -3(2) . . . . ? C35 C36 C37 C32 1(2) . . . . ? C37 C32 C33 C34 -3(2) . . . . ? C38 P18 C17 C14 45.6(9) . . . . ? C38 P18 C26 C27 46.9(9) . . . . ? C38 P18 C26 C31 -140.1(7) . . . . ? C38 C39 C40 C41 -3.4(15) . . . . ? C39 C38 C43 C42 1.8(15) . . . . ? C39 C40 C41 C42 0.6(16) . . . . ? C40 C41 C42 C43 3.3(16) . . . . ? C41 C42 C43 C38 -4.5(16) . . . . ? C43 C38 C39 C40 2.1(14) . . . . ? C44 P12 C6 C7 96.8(8) . . . . ? C44 P12 C6 C11 -87.6(10) . . . . ? C44 P12 C13 C14 -88.5(8) . . . . ? C44 C45 C46 C47 1.7(16) . . . . ? C45 C44 C49 C48 -0.5(15) . . . . ? C45 C46 C47 C48 -1.8(16) . . . . ? C46 C47 C48 C49 0.7(15) . . . . ? C47 C48 C49 C44 0.4(16) . . . . ? C49 C44 C45 C46 -0.5(14) . . . . ? C53 Fe2 C78 Fe1 25.5(6) . . . . ? C53 Fe2 C78 Fe3 109.5(5) . . . . ? C53 Fe2 C78 Fe4 -167.4(4) . . . . ? C55 Fe1 C78 Fe2 26.4(7) . . . . ? C55 Fe1 C78 Fe3 -59.2(6) . . . . ? C55 Fe1 C78 Fe4 -53(3) . . . . ? C55 Fe1 C78 Fe5 -144.8(5) . . . . ? C59 Fe2 C78 Fe1 -116.4(5) . . . . ? C59 Fe2 C78 Fe3 -32.5(7) . . . . ? C59 Fe2 C78 Fe4 50.7(7) . . . . ? C61 Fe2 C78 Fe1 125.2(4) . . . . ? C61 Fe2 C78 Fe3 -150.9(4) . . . . ? C61 Fe2 C78 Fe4 -67.7(4) . . . . ? C65 Fe1 C78 Fe2 151.9(4) . . . . ? C65 Fe1 C78 Fe3 66.4(6) . . . . ? C65 Fe1 C78 Fe4 72(3) . . . . ? C65 Fe1 C78 Fe5 -19.3(7) . . . . ? C67 Fe5 C78 Fe1 -19.6(7) . . . . ? C67 Fe5 C78 Fe3 -103.4(5) . . . . ? C67 Fe5 C78 Fe4 173.5(4) . . . . ? C73 Fe5 C78 Fe1 116.5(6) . . . . ? C73 Fe5 C78 Fe3 32.7(7) . . . . ? C73 Fe5 C78 Fe4 -50.4(7) . . . . ? C77 Fe5 C78 Fe1 -124.4(4) . . . . ? C77 Fe5 C78 Fe3 151.9(4) . . . . ? C77 Fe5 C78 Fe4 68.7(5) . . . . ? 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 -0.4565 9.8227 3.5466 -0.4021 0.0055 0.9156 1.1279 -9.7410 -2.8839 0.2959 -0.0028 -0.9552 -5.9747 0.6181 -5.3540 0.8804 -0.0237 0.4736 0.3854 -5.8344 9.2848 -0.0707 0.9013 -0.4274 -0.3854 5.8344 -9.2848 0.0707 -0.9013 0.4274 -2.6745 5.1260 7.9999 -0.0571 0.6688 0.7412 2.6745 -5.1260 -7.9999 0.0571 -0.6688 -0.7412 6.0042 0.0002 6.9910 -0.9498 0.1332 -0.4051 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 0.500 0.500 0.500 60.0 1.1 ? 2 0.500 0.000 0.000 24.2 0.0 ?