#------------------------------------------------------------------------------ #$Date: 2024-06-25 01:18:42 +0300 (Tue, 25 Jun 2024) $ #$Revision: 292547 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/19/1571976.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_1571976 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 'C32 H16 Fe5 O13 P, C8 H20 N' _chemical_formula_sum 'C40 H36 Fe5 N O13 P' _chemical_formula_weight 1048.92 _chemical_name_systematic '[NEt4][Fe5(mu5-C)(CO)13(PPh3)]' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary iterative _audit_creation_date 2023-01-16 _audit_creation_method ; Olex2 1.5 (compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498) ; _audit_update_record ; 2023-06-06 deposited with the CCDC. 2024-06-03 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 103.2791(16) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 17.1733(3) _cell_length_b 12.1213(2) _cell_length_c 20.6329(3) _cell_measurement_reflns_used 40338 _cell_measurement_temperature 100.0(5) _cell_measurement_theta_max 75.958 _cell_measurement_theta_min 2.637 _cell_volume 4180.16(12) _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 'olex2.solve 1.5 (Bourhis et al., 2015)' _diffrn_ambient_temperature 100.0(5) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.974 _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 -119.00 -50.00 0.50 4.00 -- -48.29-160.00-124.00 138 2 \w -91.00 -8.00 0.50 4.00 -- -48.29 118.00 113.00 166 3 \w 31.00 118.00 0.50 4.00 -- 48.29-160.00-124.00 174 4 \w 8.00 91.00 0.50 4.00 -- 48.29-118.00 27.00 166 5 \w 50.00 120.00 0.50 4.00 -- 48.29 160.00 -94.00 140 6 \w -109.00 -32.00 0.50 16.00 -- -104.52 118.00 113.00 154 7 \w -135.00 -32.00 0.50 16.00 -- -104.52 160.00 -94.00 206 8 \w -177.00 -78.00 0.50 16.00 -- -104.52-118.00 27.00 198 9 \w -158.00 -50.00 0.50 16.00 -- -104.52-160.00-124.00 216 10 \w 32.00 110.00 0.50 16.00 -- 104.52-118.00 27.00 156 11 \w 78.00 177.00 0.50 16.00 -- 104.52 118.00 113.00 198 12 \w 50.00 158.00 0.50 16.00 -- 104.52 160.00 -94.00 216 13 \w -119.00 -82.00 0.50 4.00 -- -48.29 -57.00 -60.00 74 14 \w -119.00 -87.00 0.50 4.00 -- -48.29-125.00-120.00 64 15 \w -119.00 -82.00 0.50 4.00 -- -48.29 -57.00 30.00 74 16 \w -119.00 -82.00 0.50 4.00 -- -48.29 -57.00-120.00 74 17 \w -119.00 -82.00 0.50 4.00 -- -48.29 -57.00 -90.00 74 18 \w 82.00 120.00 0.50 4.00 -- 48.29 57.00 120.00 76 19 \w -75.00 -32.00 0.50 16.00 -- -104.52 61.00 120.00 86 20 \w -177.00 -91.00 0.50 16.00 -- -104.52 -61.00 -60.00 172 21 \w 94.00 177.00 0.50 16.00 -- 104.52 45.00 -90.00 166 22 \w 32.00 105.00 0.50 16.00 -- 104.52 -95.00 60.00 146 23 \w 94.00 178.00 0.50 16.00 -- 104.52 15.00 -60.00 168 24 \w 32.00 105.00 0.50 16.00 -- 104.52 -95.00 30.00 146 25 \w 32.00 69.00 0.50 16.00 -- 104.52 -61.00 -60.00 74 26 \w 32.00 105.00 0.50 16.00 -- 104.52 -95.00-150.00 146 27 \w 32.00 69.00 0.50 16.00 -- 104.52 -61.00 -90.00 74 28 \w 32.00 69.00 0.50 16.00 -- 104.52 -61.00-180.00 74 29 \w 38.00 121.00 0.50 4.00 -- 48.29 38.00 0.00 166 30 \w 38.00 121.00 0.50 4.00 -- 48.29 38.00-180.00 166 31 \w 38.00 107.00 0.50 4.00 -- 48.29 38.00 -90.00 138 32 \w 38.00 121.00 0.50 4.00 -- 48.29 38.00 90.00 166 ; _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 -0.0841739000 _diffrn_orient_matrix_UB_12 -0.0423285000 _diffrn_orient_matrix_UB_13 -0.0336879000 _diffrn_orient_matrix_UB_21 0.0261144000 _diffrn_orient_matrix_UB_22 -0.1187681000 _diffrn_orient_matrix_UB_23 0.0213658000 _diffrn_orient_matrix_UB_31 -0.0268210000 _diffrn_orient_matrix_UB_32 0.0166038000 _diffrn_orient_matrix_UB_33 0.0655736000 _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 0.0709 _diffrn_reflns_av_unetI/netI 0.0279 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.974 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 63765 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.974 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 76.490 _diffrn_reflns_theta_min 2.644 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 14.509 _exptl_absorpt_correction_T_max 0.968 _exptl_absorpt_correction_T_min 0.090 _exptl_absorpt_correction_type 'gaussian and multi-scan' _exptl_absorpt_process_details ; CrysAlisPro 1.171.41.120a (Rigaku Oxford Diffraction, 2021) 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 'dark red' _exptl_crystal_colour_modifier dark _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.667 _exptl_crystal_description plate _exptl_crystal_F_000 2128 _exptl_crystal_preparation 'reaction of Fe6^0 with PPh3' _exptl_crystal_recrystallization_method 'grown from vapor diffusion of diethylether into fluorobenzene' _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.055 _refine_diff_density_max 0.841 _refine_diff_density_min -0.941 _refine_diff_density_rms 0.105 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.137 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 549 _refine_ls_number_reflns 8562 _refine_ls_number_restraints 6 _refine_ls_restrained_S_all 1.136 _refine_ls_R_factor_all 0.0484 _refine_ls_R_factor_gt 0.0459 _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^)+(0.0947P)^2^+2.0813P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1375 _refine_ls_wR_factor_ref 0.1401 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7910 _reflns_number_total 8562 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc01370k3.cif _cod_data_source_block compound4 _cod_original_cell_volume 4180.17(13) _cod_database_code 1571976 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.502 _shelx_estimated_absorpt_t_min 0.090 _olex2_refinement_description ; 1. Uiso/Uaniso restraints and constraints Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 2.a Secondary CH2 refined with riding coordinates: C33(H33A,H33B), C35(H35A,H35B), C37(H37A,H37B), C39(H39A,H39B) 2.b Aromatic/amide H refined with riding coordinates: 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) 2.c Idealised Me refined as rotating group: C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C), C40(H40A,H40B, H40C) ; _shelx_res_file ; TITL rjd102721-2nfphe1longerrun_auto_a.res in P2(1)/c rjd-102721.res created by SHELXL-2018/3 at 10:41:19 on 07-Jul-2022 REM Old TITL rjd102721-2nfphe1longerrun_auto_a.res in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.086, Rweak 0.005, Alpha 0.055 REM 0.354 for 428 systematic absences, Orientation as input REM Formula found by SHELXT: C40 Fe5 N O13 P CELL 1.54184 17.173308 12.121319 20.632899 90 103.2791 90 ZERR 4 0.000267 0.000237 0.000332 0 0.0016 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Fe N O P UNIT 160 144 20 4 52 4 ISOR 0.01 0.02 C1 L.S. 8 PLAN 1 SIZE 0.32 0.26 0.055 TEMP -173.1(5) CONF BOND LIST 4 MORE -1 BOND $H fmap 2 acta OMIT -20 4 9 OMIT -18 8 8 OMIT 12 5 15 OMIT -19 7 8 OMIT 12 4 16 OMIT -15 10 8 OMIT 15 5 10 REM REM REM WGHT 0.094700 2.081300 FVAR 2.32045 FE1 3 0.221155 0.174277 0.690290 11.00000 0.02465 0.01919 = 0.02204 0.00024 0.00268 -0.00029 H 2 0.249579 0.174781 0.610367 11.00000 0.05479 FE2 3 0.346519 0.242185 0.641851 11.00000 0.02937 0.01949 = 0.02013 0.00106 0.00676 0.00060 FE3 3 0.423761 0.288928 0.759904 11.00000 0.02510 0.02044 = 0.02545 -0.00080 0.00420 -0.00140 FE4 3 0.305012 0.232479 0.809520 11.00000 0.02959 0.01992 = 0.02090 0.00102 0.00702 0.00137 FE5 3 0.362510 0.093096 0.737278 11.00000 0.02646 0.01758 = 0.02157 0.00041 0.00430 0.00139 P1 6 0.119988 0.279708 0.638221 11.00000 0.02563 0.02227 = 0.02255 0.00230 0.00384 0.00117 O2 5 0.162536 -0.034658 0.626661 11.00000 0.04959 0.02661 = 0.04483 -0.00676 -0.00205 -0.00482 O3 5 0.345569 0.143720 0.511003 11.00000 0.07257 0.04784 = 0.02917 -0.00490 0.01709 0.00765 O4 5 0.322758 0.460039 0.580692 11.00000 0.04353 0.02562 = 0.03541 0.00959 0.00929 0.00206 O5 5 0.517624 0.278355 0.653086 11.00000 0.03409 0.05021 = 0.03830 0.00216 0.01388 0.00064 O6 5 0.596463 0.255737 0.814234 11.00000 0.02520 0.03966 = 0.04472 -0.00529 0.00249 0.00032 O7 5 0.409996 0.529074 0.767391 11.00000 0.04155 0.02144 = 0.04726 -0.00188 0.00967 -0.00214 O8 5 0.448150 0.304870 0.907832 11.00000 0.03514 0.04456 = 0.02702 -0.00832 0.00168 -0.00157 O9 5 0.298482 0.090138 0.922863 11.00000 0.05942 0.04717 = 0.03391 0.01595 0.01123 0.00252 O10 5 0.221196 0.425599 0.844270 11.00000 0.05754 0.03149 = 0.04048 -0.00490 0.01771 0.01345 O11 5 0.136311 0.120689 0.794183 11.00000 0.03235 0.04803 = 0.02778 0.00373 0.00857 -0.00898 O12 5 0.276598 -0.097877 0.773357 11.00000 0.04449 0.03081 = 0.04979 0.01225 0.01030 -0.00556 O13 5 0.498816 0.041417 0.847648 11.00000 0.03755 0.03249 = 0.03241 0.00086 -0.00290 0.00735 O14 5 0.418904 -0.020508 0.630854 11.00000 0.04963 0.02985 = 0.02790 -0.00021 0.00929 0.01298 C1 1 0.317514 0.247045 0.722887 11.00000 0.02671 0.01400 = 0.02564 -0.00113 0.00461 0.00279 C2 1 0.183305 0.049135 0.650964 11.00000 0.03568 0.02738 = 0.02737 0.00086 0.00479 0.00064 C3 1 0.348795 0.180462 0.562712 11.00000 0.04340 0.03110 = 0.03466 0.00582 0.01002 0.00431 C4 1 0.329045 0.374779 0.604519 11.00000 0.02879 0.03138 = 0.02585 -0.00154 0.00680 -0.00109 C5 1 0.457872 0.271521 0.670239 11.00000 0.03432 0.02858 = 0.03089 0.00321 0.00864 0.00217 C6 1 0.530412 0.269289 0.794420 11.00000 0.03808 0.02518 = 0.03036 -0.00361 0.00636 -0.00180 C7 1 0.419393 0.435398 0.763640 11.00000 0.02951 0.03036 = 0.03048 -0.00153 0.00632 -0.00518 C8 1 0.408524 0.283971 0.855738 11.00000 0.03271 0.02539 = 0.02270 -0.00384 0.00429 0.00141 C9 1 0.300965 0.144660 0.878308 11.00000 0.03492 0.03069 = 0.02315 0.00207 0.00125 -0.00034 C10 1 0.254318 0.349494 0.831702 11.00000 0.03669 0.03020 = 0.02273 -0.00123 0.00865 -0.00159 C11 1 0.180015 0.150747 0.762970 11.00000 0.03110 0.02701 = 0.02797 0.00169 0.00291 0.00161 C12 1 0.308103 -0.021741 0.758086 11.00000 0.03240 0.02659 = 0.02837 0.00310 0.00576 0.00581 C13 1 0.447812 0.066957 0.803277 11.00000 0.03211 0.02441 = 0.02685 -0.00411 0.00687 -0.00046 C14 1 0.395881 0.029778 0.670068 11.00000 0.03252 0.02513 = 0.02645 0.00323 0.00150 0.00266 C15 1 0.029076 0.268319 0.670059 11.00000 0.02909 0.03728 = 0.02346 0.00700 0.00556 0.00233 C16 1 -0.001910 0.163876 0.678328 11.00000 0.03305 0.03677 = 0.03200 0.00789 0.00663 0.00115 AFIX 43 H16 2 0.023026 0.100116 0.665523 11.00000 -1.20000 AFIX 0 C17 1 -0.068988 0.152213 0.705153 11.00000 0.03514 0.05398 = 0.03901 0.01809 0.00427 -0.00494 AFIX 43 H17 2 -0.090187 0.080999 0.709747 11.00000 -1.20000 AFIX 0 C18 1 -0.104678 0.245177 0.725129 11.00000 0.03124 0.06931 = 0.03819 0.01744 0.01178 0.00788 AFIX 43 H18 2 -0.150431 0.237561 0.743332 11.00000 -1.20000 AFIX 0 C19 1 -0.073870 0.348007 0.718580 11.00000 0.03963 0.05552 = 0.03341 0.00824 0.01263 0.01028 AFIX 43 H19 2 -0.098209 0.411247 0.732659 11.00000 -1.20000 AFIX 0 C20 1 -0.007116 0.360392 0.691419 11.00000 0.03471 0.04143 = 0.02861 0.00383 0.00804 0.00569 AFIX 43 H20 2 0.013881 0.431933 0.687417 11.00000 -1.20000 AFIX 0 C21 1 0.089215 0.243953 0.549387 11.00000 0.02772 0.02232 = 0.02573 0.00076 0.00173 0.00404 C22 1 0.029582 0.167136 0.524689 11.00000 0.03469 0.02725 = 0.03122 0.00304 0.00147 0.00055 AFIX 43 H22 2 -0.001201 0.137157 0.553271 11.00000 -1.20000 AFIX 0 C23 1 0.014623 0.133724 0.458071 11.00000 0.04233 0.02949 = 0.03434 -0.00323 -0.00423 0.00327 AFIX 43 H23 2 -0.025783 0.080533 0.441855 11.00000 -1.20000 AFIX 0 C24 1 0.057973 0.177327 0.415994 11.00000 0.04735 0.04018 = 0.02822 -0.00606 0.00086 0.00674 AFIX 43 H24 2 0.047585 0.154648 0.370746 11.00000 -1.20000 AFIX 0 C25 1 0.116836 0.254451 0.439908 11.00000 0.04180 0.05224 = 0.02790 -0.00195 0.00982 -0.00147 AFIX 43 H25 2 0.146596 0.285226 0.410785 11.00000 -1.20000 AFIX 0 C26 1 0.132781 0.287171 0.505716 11.00000 0.03492 0.03999 = 0.02547 0.00244 0.00485 -0.00224 AFIX 43 H26 2 0.173829 0.339660 0.521529 11.00000 -1.20000 AFIX 0 C27 1 0.134592 0.428525 0.634453 11.00000 0.03124 0.02334 = 0.02538 0.00206 0.00973 0.00451 C28 1 0.200335 0.479291 0.675066 11.00000 0.03804 0.02581 = 0.02685 -0.00104 0.01296 0.00154 AFIX 43 H28 2 0.238367 0.436703 0.705678 11.00000 -1.20000 AFIX 0 C29 1 0.210612 0.593587 0.670892 11.00000 0.04557 0.02738 = 0.03215 -0.00106 0.01351 -0.00014 AFIX 43 H29 2 0.256310 0.628132 0.698004 11.00000 -1.20000 AFIX 0 C30 1 0.154372 0.656369 0.627375 11.00000 0.05709 0.02246 = 0.03589 0.00206 0.02212 0.00423 AFIX 43 H30 2 0.161211 0.733944 0.625176 11.00000 -1.20000 AFIX 0 C31 1 0.088107 0.606146 0.587019 11.00000 0.04621 0.02959 = 0.03231 0.00780 0.01161 0.01057 AFIX 43 H31 2 0.049514 0.649483 0.557406 11.00000 -1.20000 AFIX 0 C32 1 0.078043 0.493262 0.589750 11.00000 0.03890 0.02764 = 0.02986 0.00423 0.00799 0.00535 AFIX 43 H32 2 0.033001 0.459079 0.561509 11.00000 -1.20000 AFIX 0 N1 4 0.688951 0.232177 0.532193 11.00000 0.03526 0.03046 = 0.02038 0.00131 0.00479 0.00092 C33 1 0.651319 0.165765 0.580238 11.00000 0.04181 0.03603 = 0.02428 0.00577 0.01035 0.00173 AFIX 23 H33A 2 0.693443 0.119631 0.608373 11.00000 -1.20000 H33B 2 0.632066 0.217964 0.610002 11.00000 -1.20000 AFIX 0 C34 1 0.582108 0.091313 0.547483 11.00000 0.05436 0.03482 = 0.04026 0.00463 0.01227 -0.00744 AFIX 137 H34A 2 0.599903 0.040117 0.517069 11.00000 -1.50000 H34B 2 0.537990 0.136462 0.522460 11.00000 -1.50000 H34C 2 0.563851 0.049405 0.581823 11.00000 -1.50000 AFIX 0 C35 1 0.625858 0.296484 0.483006 11.00000 0.03505 0.03426 = 0.02447 0.00674 0.00224 -0.00129 AFIX 23 H35A 2 0.653048 0.341678 0.454855 11.00000 -1.20000 H35B 2 0.590903 0.243271 0.453451 11.00000 -1.20000 AFIX 0 C36 1 0.573858 0.371399 0.513510 11.00000 0.04273 0.03783 = 0.03393 0.00544 0.00318 0.00708 AFIX 137 H36A 2 0.533591 0.406409 0.478082 11.00000 -1.50000 H36B 2 0.607108 0.428368 0.540125 11.00000 -1.50000 H36C 2 0.547100 0.328080 0.542135 11.00000 -1.50000 AFIX 0 C37 1 0.728619 0.157346 0.490812 11.00000 0.04457 0.03889 = 0.02921 0.00072 0.01221 0.00652 AFIX 23 H37A 2 0.748642 0.203272 0.458430 11.00000 -1.20000 H37B 2 0.687559 0.106967 0.465074 11.00000 -1.20000 AFIX 0 C38 1 0.797355 0.088493 0.529426 11.00000 0.05953 0.05306 = 0.04313 0.00836 0.02185 0.02143 AFIX 137 H38A 2 0.821031 0.046289 0.498268 11.00000 -1.50000 H38B 2 0.777533 0.037586 0.558858 11.00000 -1.50000 H38C 2 0.837989 0.137041 0.556143 11.00000 -1.50000 AFIX 0 C39 1 0.749111 0.309018 0.575818 11.00000 0.03689 0.04329 = 0.02555 -0.00082 -0.00110 -0.00249 AFIX 23 H39A 2 0.719461 0.361604 0.597916 11.00000 -1.20000 H39B 2 0.783960 0.264505 0.611141 11.00000 -1.20000 AFIX 0 C40 1 0.802031 0.374631 0.539970 11.00000 0.04186 0.04903 = 0.03910 0.00620 0.00328 -0.00796 AFIX 137 H40A 2 0.768471 0.414375 0.502382 11.00000 -1.50000 H40B 2 0.837718 0.324191 0.523508 11.00000 -1.50000 H40C 2 0.833996 0.427595 0.570927 11.00000 -1.50000 AFIX 0 HKLF 4 REM rjd102721-2nfphe1longerrun_auto_a.res in P2(1)/c REM wR2 = 0.1401, GooF = S = 1.137, Restrained GooF = 1.136 for all data REM R1 = 0.0459 for 7910 Fo > 4sig(Fo) and 0.0484 for all 8562 data REM 549 parameters refined using 6 restraints END WGHT 0.0947 2.0818 REM Highest difference peak 0.841, deepest hole -0.941, 1-sigma level 0.105 Q1 1 0.2369 0.1139 0.5399 11.00000 0.05 0.84 ; _shelx_res_checksum 41043 _olex2_exptl_crystal_mounting_method mounted _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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 Fe1 Fe 0.22116(2) 0.17428(4) 0.69029(2) 0.02240(12) Uani 1 1 d . . . . . H H 0.250(3) 0.175(4) 0.610(2) 0.055(13) Uiso 1 1 d . . . . . Fe2 Fe 0.34652(3) 0.24219(4) 0.64185(2) 0.02282(12) Uani 1 1 d . . . . . Fe3 Fe 0.42376(3) 0.28893(4) 0.75990(2) 0.02392(12) Uani 1 1 d . . . . . Fe4 Fe 0.30501(3) 0.23248(4) 0.80952(2) 0.02327(12) Uani 1 1 d . . . . . Fe5 Fe 0.36251(3) 0.09310(4) 0.73728(2) 0.02207(12) Uani 1 1 d . . . . . P1 P 0.11999(4) 0.27971(6) 0.63822(4) 0.02376(16) Uani 1 1 d . . . . . O1 O 0.16254(16) -0.0347(2) 0.62666(13) 0.0424(6) Uani 1 1 d . . . . . O2 O 0.34557(19) 0.1437(2) 0.51100(13) 0.0490(7) Uani 1 1 d . . . . . O3 O 0.32276(14) 0.46004(19) 0.58069(12) 0.0348(5) Uani 1 1 d . . . . . O4 O 0.51762(14) 0.2784(2) 0.65309(13) 0.0400(6) Uani 1 1 d . . . . . O5 O 0.59646(13) 0.2557(2) 0.81423(13) 0.0374(5) Uani 1 1 d . . . . . O6 O 0.41000(14) 0.52907(19) 0.76739(13) 0.0368(5) Uani 1 1 d . . . . . O7 O 0.44815(14) 0.3049(2) 0.90783(11) 0.0365(5) Uani 1 1 d . . . . . O8 O 0.29848(17) 0.0901(2) 0.92286(13) 0.0467(6) Uani 1 1 d . . . . . O9 O 0.22120(16) 0.4256(2) 0.84427(13) 0.0421(6) Uani 1 1 d . . . . . O10 O 0.13631(13) 0.1207(2) 0.79418(11) 0.0358(5) Uani 1 1 d . . . . . O11 O 0.27660(16) -0.0979(2) 0.77336(14) 0.0418(6) Uani 1 1 d . . . . . O12 O 0.49882(14) 0.0414(2) 0.84765(11) 0.0359(5) Uani 1 1 d . . . . . O13 O 0.41890(15) -0.0205(2) 0.63085(11) 0.0357(5) Uani 1 1 d . . . . . C1 C 0.31751(17) 0.2470(2) 0.72289(14) 0.0223(6) Uani 1 1 d . U . . . C2 C 0.18331(19) 0.0491(3) 0.65096(15) 0.0305(6) Uani 1 1 d . . . . . C3 C 0.3488(2) 0.1805(3) 0.56271(17) 0.0362(7) Uani 1 1 d . . . . . C4 C 0.32905(18) 0.3748(3) 0.60452(15) 0.0286(6) Uani 1 1 d . . . . . C5 C 0.4579(2) 0.2715(3) 0.67024(16) 0.0311(6) Uani 1 1 d . . . . . C6 C 0.5304(2) 0.2693(3) 0.79442(16) 0.0315(7) Uani 1 1 d . . . . . C7 C 0.41939(18) 0.4354(3) 0.76364(16) 0.0302(6) Uani 1 1 d . . . . . C8 C 0.40852(19) 0.2840(3) 0.85574(15) 0.0273(6) Uani 1 1 d . . . . . C9 C 0.30096(19) 0.1447(3) 0.87831(15) 0.0305(6) Uani 1 1 d . . . . . C10 C 0.25432(19) 0.3495(3) 0.83170(15) 0.0296(6) Uani 1 1 d . . . . . C11 C 0.18002(18) 0.1507(3) 0.76297(16) 0.0293(6) Uani 1 1 d . . . . . C12 C 0.30810(18) -0.0217(3) 0.75809(15) 0.0293(6) Uani 1 1 d . . . . . C13 C 0.44781(18) 0.0670(3) 0.80328(15) 0.0278(6) Uani 1 1 d . . . . . C14 C 0.39588(18) 0.0298(3) 0.67007(15) 0.0289(6) Uani 1 1 d . . . . . C15 C 0.02908(18) 0.2683(3) 0.67006(15) 0.0300(6) Uani 1 1 d . . . . . C16 C -0.0019(2) 0.1639(3) 0.67833(16) 0.0341(7) Uani 1 1 d . . . . . H16 H 0.023026 0.100116 0.665523 0.041 Uiso 1 1 calc R U . . . C17 C -0.0690(2) 0.1522(4) 0.70515(19) 0.0434(9) Uani 1 1 d . . . . . H17 H -0.090187 0.080999 0.709747 0.052 Uiso 1 1 calc R U . . . C18 C -0.1047(2) 0.2452(4) 0.72513(19) 0.0456(9) Uani 1 1 d . . . . . H18 H -0.150431 0.237561 0.743332 0.055 Uiso 1 1 calc R U . . . C19 C -0.0739(2) 0.3480(4) 0.71858(18) 0.0422(8) Uani 1 1 d . . . . . H19 H -0.098209 0.411247 0.732659 0.051 Uiso 1 1 calc R U . . . C20 C -0.0071(2) 0.3604(3) 0.69142(16) 0.0348(7) Uani 1 1 d . . . . . H20 H 0.013881 0.431933 0.687417 0.042 Uiso 1 1 calc R U . . . C21 C 0.08921(18) 0.2440(2) 0.54939(15) 0.0260(6) Uani 1 1 d . . . . . C22 C 0.02958(19) 0.1671(3) 0.52469(16) 0.0320(7) Uani 1 1 d . . . . . H22 H -0.001201 0.137157 0.553271 0.038 Uiso 1 1 calc R U . . . C23 C 0.0146(2) 0.1337(3) 0.45807(17) 0.0375(7) Uani 1 1 d . . . . . H23 H -0.025783 0.080533 0.441855 0.045 Uiso 1 1 calc R U . . . C24 C 0.0580(2) 0.1773(3) 0.41599(17) 0.0398(8) Uani 1 1 d . . . . . H24 H 0.047585 0.154648 0.370746 0.048 Uiso 1 1 calc R U . . . C25 C 0.1168(2) 0.2545(3) 0.43991(18) 0.0404(8) Uani 1 1 d . . . . . H25 H 0.146596 0.285226 0.410785 0.048 Uiso 1 1 calc R U . . . C26 C 0.1328(2) 0.2872(3) 0.50572(16) 0.0338(7) Uani 1 1 d . . . . . H26 H 0.173829 0.339660 0.521529 0.041 Uiso 1 1 calc R U . . . C27 C 0.13459(18) 0.4285(3) 0.63445(15) 0.0261(6) Uani 1 1 d . . . . . C28 C 0.20034(19) 0.4793(3) 0.67507(15) 0.0293(6) Uani 1 1 d . . . . . H28 H 0.238367 0.436703 0.705678 0.035 Uiso 1 1 calc R U . . . C29 C 0.2106(2) 0.5936(3) 0.67089(17) 0.0343(7) Uani 1 1 d . . . . . H29 H 0.256310 0.628132 0.698004 0.041 Uiso 1 1 calc R U . . . C30 C 0.1544(2) 0.6564(3) 0.62737(17) 0.0366(7) Uani 1 1 d . . . . . H30 H 0.161211 0.733944 0.625176 0.044 Uiso 1 1 calc R U . . . C31 C 0.0881(2) 0.6061(3) 0.58702(17) 0.0356(7) Uani 1 1 d . . . . . H31 H 0.049514 0.649483 0.557406 0.043 Uiso 1 1 calc R U . . . C32 C 0.0780(2) 0.4933(3) 0.58975(16) 0.0321(6) Uani 1 1 d . . . . . H32 H 0.033001 0.459079 0.561509 0.039 Uiso 1 1 calc R U . . . N1 N 0.68895(16) 0.2322(2) 0.53219(12) 0.0290(5) Uani 1 1 d . . . . . C33 C 0.6513(2) 0.1658(3) 0.58024(16) 0.0336(7) Uani 1 1 d . . . . . H33A H 0.693443 0.119631 0.608373 0.040 Uiso 1 1 calc R U . . . H33B H 0.632066 0.217964 0.610002 0.040 Uiso 1 1 calc R U . . . C34 C 0.5821(2) 0.0913(3) 0.54748(19) 0.0429(8) Uani 1 1 d . . . . . H34A H 0.599903 0.040117 0.517069 0.064 Uiso 1 1 calc R U . . . H34B H 0.537990 0.136462 0.522460 0.064 Uiso 1 1 calc R U . . . H34C H 0.563851 0.049405 0.581823 0.064 Uiso 1 1 calc R U . . . C35 C 0.62586(19) 0.2965(3) 0.48301(15) 0.0320(7) Uani 1 1 d . . . . . H35A H 0.653048 0.341678 0.454855 0.038 Uiso 1 1 calc R U . . . H35B H 0.590903 0.243271 0.453451 0.038 Uiso 1 1 calc R U . . . C36 C 0.5739(2) 0.3714(3) 0.51351(18) 0.0391(8) Uani 1 1 d . . . . . H36A H 0.533591 0.406409 0.478082 0.059 Uiso 1 1 calc R U . . . H36B H 0.607108 0.428368 0.540125 0.059 Uiso 1 1 calc R U . . . H36C H 0.547100 0.328080 0.542135 0.059 Uiso 1 1 calc R U . . . C37 C 0.7286(2) 0.1573(3) 0.49081(17) 0.0370(7) Uani 1 1 d . . . . . H37A H 0.748642 0.203272 0.458430 0.044 Uiso 1 1 calc R U . . . H37B H 0.687559 0.106967 0.465074 0.044 Uiso 1 1 calc R U . . . C38 C 0.7974(3) 0.0885(4) 0.5294(2) 0.0503(10) Uani 1 1 d . . . . . H38A H 0.821031 0.046289 0.498268 0.075 Uiso 1 1 calc R U . . . H38B H 0.777533 0.037586 0.558858 0.075 Uiso 1 1 calc R U . . . H38C H 0.837989 0.137041 0.556143 0.075 Uiso 1 1 calc R U . . . C39 C 0.7491(2) 0.3090(3) 0.57582(16) 0.0366(7) Uani 1 1 d . . . . . H39A H 0.719461 0.361604 0.597916 0.044 Uiso 1 1 calc R U . . . H39B H 0.783960 0.264505 0.611141 0.044 Uiso 1 1 calc R U . . . C40 C 0.8020(2) 0.3746(4) 0.53997(19) 0.0443(8) Uani 1 1 d . . . . . H40A H 0.768471 0.414375 0.502382 0.066 Uiso 1 1 calc R U . . . H40B H 0.837718 0.324191 0.523508 0.066 Uiso 1 1 calc R U . . . H40C H 0.833996 0.427595 0.570927 0.066 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0247(2) 0.0192(2) 0.0220(2) 0.00024(16) 0.00268(17) -0.00029(16) Fe2 0.0294(2) 0.0195(2) 0.0201(2) 0.00106(16) 0.00676(18) 0.00060(17) Fe3 0.0251(2) 0.0204(2) 0.0255(2) -0.00080(17) 0.00420(17) -0.00140(17) Fe4 0.0296(2) 0.0199(2) 0.0209(2) 0.00102(16) 0.00702(18) 0.00137(17) Fe5 0.0265(2) 0.0176(2) 0.0216(2) 0.00041(16) 0.00430(17) 0.00139(16) P1 0.0256(3) 0.0223(4) 0.0226(3) 0.0023(3) 0.0038(3) 0.0012(3) O1 0.0496(14) 0.0266(13) 0.0448(13) -0.0068(11) -0.0020(11) -0.0048(11) O2 0.0726(18) 0.0478(16) 0.0292(13) -0.0049(11) 0.0171(12) 0.0076(14) O3 0.0435(12) 0.0256(12) 0.0354(12) 0.0096(9) 0.0093(10) 0.0021(10) O4 0.0341(12) 0.0502(15) 0.0383(13) 0.0022(11) 0.0139(10) 0.0006(11) O5 0.0252(11) 0.0397(14) 0.0447(14) -0.0053(11) 0.0025(10) 0.0003(9) O6 0.0415(12) 0.0214(12) 0.0473(13) -0.0019(10) 0.0097(10) -0.0021(9) O7 0.0351(11) 0.0446(14) 0.0270(11) -0.0083(10) 0.0017(9) -0.0016(10) O8 0.0594(16) 0.0472(16) 0.0339(13) 0.0159(11) 0.0112(11) 0.0025(13) O9 0.0575(15) 0.0315(13) 0.0405(13) -0.0049(10) 0.0177(12) 0.0134(12) O10 0.0324(11) 0.0480(14) 0.0278(11) 0.0037(10) 0.0086(9) -0.0090(10) O11 0.0445(13) 0.0308(13) 0.0498(15) 0.0122(11) 0.0103(11) -0.0056(11) O12 0.0376(11) 0.0325(12) 0.0324(11) 0.0009(9) -0.0029(9) 0.0074(10) O13 0.0496(13) 0.0299(12) 0.0279(11) -0.0002(9) 0.0093(10) 0.0130(10) C1 0.0267(13) 0.0140(12) 0.0256(14) -0.0011(10) 0.0046(11) 0.0028(10) C2 0.0357(15) 0.0274(16) 0.0274(14) 0.0009(12) 0.0048(12) 0.0006(13) C3 0.0434(17) 0.0311(17) 0.0347(17) 0.0058(14) 0.0100(14) 0.0043(14) C4 0.0288(13) 0.0314(17) 0.0258(14) -0.0015(12) 0.0068(11) -0.0011(12) C5 0.0343(16) 0.0286(16) 0.0309(15) 0.0032(12) 0.0086(13) 0.0022(13) C6 0.0381(17) 0.0252(16) 0.0304(15) -0.0036(12) 0.0064(13) -0.0018(12) C7 0.0295(14) 0.0304(17) 0.0305(15) -0.0015(12) 0.0063(12) -0.0052(12) C8 0.0327(14) 0.0254(15) 0.0227(14) -0.0038(11) 0.0043(12) 0.0014(12) C9 0.0349(15) 0.0307(16) 0.0231(14) 0.0021(12) 0.0012(11) -0.0003(13) C10 0.0367(15) 0.0302(16) 0.0227(14) -0.0012(12) 0.0087(12) -0.0016(13) C11 0.0311(14) 0.0270(15) 0.0280(15) 0.0017(12) 0.0029(12) 0.0016(12) C12 0.0324(14) 0.0266(15) 0.0284(14) 0.0031(12) 0.0058(11) 0.0058(12) C13 0.0321(14) 0.0244(14) 0.0268(14) -0.0041(12) 0.0069(12) -0.0005(12) C14 0.0325(14) 0.0251(15) 0.0264(14) 0.0032(12) 0.0015(11) 0.0027(12) C15 0.0291(14) 0.0373(18) 0.0235(14) 0.0070(12) 0.0056(12) 0.0023(13) C16 0.0330(15) 0.0368(18) 0.0320(16) 0.0079(14) 0.0066(13) 0.0011(13) C17 0.0351(16) 0.054(2) 0.0390(19) 0.0181(17) 0.0043(14) -0.0049(16) C18 0.0312(16) 0.069(3) 0.0382(19) 0.0174(18) 0.0118(14) 0.0079(17) C19 0.0396(17) 0.056(2) 0.0334(17) 0.0082(16) 0.0126(14) 0.0103(16) C20 0.0347(15) 0.0414(19) 0.0286(15) 0.0038(14) 0.0080(13) 0.0057(14) C21 0.0277(14) 0.0223(14) 0.0257(14) 0.0008(11) 0.0017(11) 0.0040(11) C22 0.0347(15) 0.0273(16) 0.0312(16) 0.0030(12) 0.0015(12) 0.0006(13) C23 0.0423(17) 0.0295(17) 0.0343(17) -0.0032(13) -0.0042(14) 0.0033(14) C24 0.0474(19) 0.040(2) 0.0282(16) -0.0061(14) 0.0009(14) 0.0067(16) C25 0.0418(18) 0.052(2) 0.0279(16) -0.0020(15) 0.0098(14) -0.0015(16) C26 0.0349(15) 0.0400(18) 0.0255(15) 0.0024(13) 0.0049(12) -0.0022(14) C27 0.0312(14) 0.0233(14) 0.0254(14) 0.0021(11) 0.0097(11) 0.0045(12) C28 0.0380(15) 0.0258(15) 0.0269(14) -0.0010(12) 0.0130(12) 0.0015(12) C29 0.0456(17) 0.0274(16) 0.0321(16) -0.0011(13) 0.0135(14) -0.0001(13) C30 0.057(2) 0.0225(15) 0.0359(17) 0.0021(13) 0.0221(15) 0.0042(14) C31 0.0462(18) 0.0296(17) 0.0323(16) 0.0078(13) 0.0116(14) 0.0106(14) C32 0.0389(16) 0.0276(16) 0.0299(15) 0.0042(12) 0.0080(12) 0.0054(13) N1 0.0353(13) 0.0305(13) 0.0204(11) 0.0013(10) 0.0048(10) 0.0009(11) C33 0.0418(17) 0.0360(18) 0.0243(14) 0.0058(13) 0.0104(13) 0.0017(14) C34 0.054(2) 0.0348(19) 0.0403(19) 0.0046(15) 0.0123(16) -0.0074(16) C35 0.0351(15) 0.0343(17) 0.0245(14) 0.0067(13) 0.0022(12) -0.0013(13) C36 0.0427(17) 0.0378(19) 0.0339(17) 0.0054(14) 0.0032(14) 0.0071(15) C37 0.0446(17) 0.0389(19) 0.0292(16) 0.0007(14) 0.0122(14) 0.0065(15) C38 0.060(2) 0.053(2) 0.043(2) 0.0084(18) 0.0218(18) 0.021(2) C39 0.0369(16) 0.043(2) 0.0255(15) -0.0008(14) -0.0011(13) -0.0025(15) C40 0.0419(18) 0.049(2) 0.0391(19) 0.0062(17) 0.0033(15) -0.0080(17) 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' N N 0.0311 0.0180 '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 -6 1 13 0.1070 3 7 -5 0.1185 5 5 -9 0.1266 3 -6 -9 0.0882 -2 -8 2 0.1105 11 0 -1 0.0320 -11 0 1 0.0230 -4 4 11 0.1286 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 H 42.5(15) . . ? Fe4 Fe1 H 129.7(15) . . ? Fe4 Fe1 Fe2 87.301(18) . . ? Fe5 Fe1 H 85.3(15) . . ? Fe5 Fe1 Fe2 59.781(16) . . ? Fe5 Fe1 Fe4 59.361(16) . . ? P1 Fe1 H 84.4(15) . . ? P1 Fe1 Fe2 104.28(3) . . ? P1 Fe1 Fe4 119.60(3) . . ? P1 Fe1 Fe5 163.56(3) . . ? C1 Fe1 H 85.7(15) . . ? C1 Fe1 Fe2 43.17(9) . . ? C1 Fe1 Fe4 44.59(9) . . ? C1 Fe1 Fe5 50.63(9) . . ? C1 Fe1 P1 115.70(9) . . ? C2 Fe1 H 74.6(16) . . ? C2 Fe1 Fe2 109.33(10) . . ? C2 Fe1 Fe4 135.92(10) . . ? C2 Fe1 Fe5 93.43(10) . . ? C2 Fe1 P1 96.14(11) . . ? C2 Fe1 C1 140.73(13) . . ? C2 Fe1 C11 94.14(15) . . ? C11 Fe1 H 168.5(16) . . ? C11 Fe1 Fe2 147.69(10) . . ? C11 Fe1 Fe4 60.47(10) . . ? C11 Fe1 Fe5 98.03(10) . . ? C11 Fe1 P1 94.59(10) . . ? C11 Fe1 C1 104.94(13) . . ? Fe1 Fe2 H 42.2(15) . . ? Fe3 Fe2 Fe1 89.899(19) . . ? Fe3 Fe2 H 131.8(15) . . ? Fe3 Fe2 Fe5 59.904(17) . . ? Fe5 Fe2 Fe1 58.048(16) . . ? Fe5 Fe2 H 83.7(15) . . ? C1 Fe2 Fe1 43.39(9) . . ? C1 Fe2 H 85.6(15) . . ? C1 Fe2 Fe3 47.21(9) . . ? C1 Fe2 Fe5 49.60(9) . . ? C1 Fe2 C5 100.14(13) . . ? C3 Fe2 Fe1 113.15(12) . . ? C3 Fe2 H 72.6(15) . . ? C3 Fe2 Fe3 147.14(11) . . ? C3 Fe2 Fe5 111.77(11) . . ? C3 Fe2 C1 153.67(15) . . ? C3 Fe2 C5 97.30(15) . . ? C4 Fe2 Fe1 111.48(10) . . ? C4 Fe2 H 101.5(15) . . ? C4 Fe2 Fe3 102.21(10) . . ? C4 Fe2 Fe5 156.97(10) . . ? C4 Fe2 C1 107.99(13) . . ? C4 Fe2 C3 91.11(15) . . ? C4 Fe2 C5 91.27(14) . . ? C5 Fe2 Fe1 140.70(10) . . ? C5 Fe2 H 163.7(15) . . ? C5 Fe2 Fe3 53.09(10) . . ? C5 Fe2 Fe5 88.47(10) . . ? Fe2 Fe3 Fe4 92.00(2) . . ? Fe2 Fe3 Fe5 61.669(17) . . ? Fe4 Fe3 Fe5 60.215(17) . . ? C1 Fe3 Fe2 46.33(9) . . ? C1 Fe3 Fe4 46.06(9) . . ? C1 Fe3 Fe5 50.51(9) . . ? C1 Fe3 C5 93.25(13) . . ? C1 Fe3 C8 93.26(12) . . ? C5 Fe3 Fe2 47.06(9) . . ? C5 Fe3 Fe4 137.61(10) . . ? C5 Fe3 Fe5 86.12(10) . . ? C6 Fe3 Fe2 126.78(10) . . ? C6 Fe3 Fe4 128.80(11) . . ? C6 Fe3 Fe5 106.28(11) . . ? C6 Fe3 C1 156.75(14) . . ? C6 Fe3 C5 82.58(14) . . ? C6 Fe3 C8 87.64(14) . . ? C7 Fe3 Fe2 104.16(10) . . ? C7 Fe3 Fe4 101.70(10) . . ? C7 Fe3 Fe5 154.31(10) . . ? C7 Fe3 C1 103.92(13) . . ? C7 Fe3 C5 99.40(14) . . ? C7 Fe3 C6 99.33(14) . . ? C7 Fe3 C8 88.37(13) . . ? C8 Fe3 Fe2 139.30(9) . . ? C8 Fe3 Fe4 47.32(9) . . ? C8 Fe3 Fe5 90.60(9) . . ? C8 Fe3 C5 168.36(13) . . ? Fe3 Fe4 Fe1 90.735(19) . . ? Fe3 Fe4 Fe5 60.260(17) . . ? Fe5 Fe4 Fe1 59.308(16) . . ? C1 Fe4 Fe1 44.66(9) . . ? C1 Fe4 Fe3 46.77(9) . . ? C1 Fe4 Fe5 50.60(9) . . ? C1 Fe4 C8 98.55(13) . . ? C1 Fe4 C11 86.77(12) . . ? C8 Fe4 Fe1 142.51(9) . . ? C8 Fe4 Fe3 51.92(9) . . ? C8 Fe4 Fe5 93.78(9) . . ? C8 Fe4 C11 172.61(12) . . ? C9 Fe4 Fe1 117.86(11) . . ? C9 Fe4 Fe3 130.71(11) . . ? C9 Fe4 Fe5 99.07(11) . . ? C9 Fe4 C1 148.73(14) . . ? C9 Fe4 C8 89.98(14) . . ? C9 Fe4 C11 82.85(13) . . ? C10 Fe4 Fe1 104.95(10) . . ? C10 Fe4 Fe3 111.69(11) . . ? C10 Fe4 Fe5 160.22(10) . . ? C10 Fe4 C1 110.09(13) . . ? C10 Fe4 C8 93.73(14) . . ? C10 Fe4 C9 99.20(15) . . ? C10 Fe4 C11 89.21(13) . . ? C11 Fe4 Fe1 42.20(8) . . ? C11 Fe4 Fe3 132.78(8) . . ? C11 Fe4 Fe5 85.61(8) . . ? Fe1 Fe5 Fe2 62.171(17) . . ? Fe1 Fe5 Fe3 91.50(2) . . ? Fe1 Fe5 Fe4 61.331(17) . . ? Fe3 Fe5 Fe2 58.426(17) . . ? Fe4 Fe5 Fe2 89.690(19) . . ? Fe4 Fe5 Fe3 59.525(17) . . ? C1 Fe5 Fe1 45.50(8) . . ? C1 Fe5 Fe2 44.41(8) . . ? C1 Fe5 Fe3 46.00(8) . . ? C1 Fe5 Fe4 45.40(8) . . ? C12 Fe5 Fe1 83.62(10) . . ? C12 Fe5 Fe2 138.03(10) . . ? C12 Fe5 Fe3 152.13(10) . . ? C12 Fe5 Fe4 94.61(10) . . ? C12 Fe5 C1 123.64(13) . . ? C12 Fe5 C13 93.52(14) . . ? C12 Fe5 C14 97.50(14) . . ? C13 Fe5 Fe1 152.48(10) . . ? C13 Fe5 Fe2 128.11(10) . . ? C13 Fe5 Fe3 78.31(10) . . ? C13 Fe5 Fe4 91.79(10) . . ? C13 Fe5 C1 119.77(13) . . ? C13 Fe5 C14 99.34(13) . . ? C14 Fe5 Fe1 108.17(10) . . ? C14 Fe5 Fe2 73.31(10) . . ? C14 Fe5 Fe3 110.05(10) . . ? C14 Fe5 Fe4 162.97(10) . . ? C14 Fe5 C1 117.57(13) . . ? C15 P1 Fe1 114.75(10) . . ? C15 P1 C21 105.43(14) . . ? C21 P1 Fe1 111.08(10) . . ? C27 P1 Fe1 119.25(10) . . ? C27 P1 C15 103.08(14) . . ? C27 P1 C21 101.61(14) . . ? Fe1 C1 Fe3 167.34(17) . . ? Fe1 C1 Fe5 83.88(11) . . ? Fe2 C1 Fe1 93.44(13) . . ? Fe2 C1 Fe3 86.45(12) . . ? Fe2 C1 Fe4 168.67(17) . . ? Fe2 C1 Fe5 85.99(11) . . ? Fe3 C1 Fe5 83.49(11) . . ? Fe4 C1 Fe1 90.75(12) . . ? Fe4 C1 Fe3 87.17(12) . . ? Fe4 C1 Fe5 83.99(11) . . ? O1 C2 Fe1 176.4(3) . . ? O2 C3 Fe2 175.8(3) . . ? O3 C4 Fe2 175.8(3) . . ? Fe2 C5 Fe3 79.85(12) . . ? O4 C5 Fe2 144.6(3) . . ? O4 C5 Fe3 135.5(3) . . ? O5 C6 Fe3 178.2(3) . . ? O6 C7 Fe3 173.9(3) . . ? Fe4 C8 Fe3 80.76(11) . . ? O7 C8 Fe3 135.1(3) . . ? O7 C8 Fe4 144.2(3) . . ? O8 C9 Fe4 178.9(3) . . ? O9 C10 Fe4 178.2(3) . . ? Fe1 C11 Fe4 77.33(11) . . ? O10 C11 Fe1 159.0(3) . . ? O10 C11 Fe4 123.6(2) . . ? O11 C12 Fe5 176.5(3) . . ? O12 C13 Fe5 173.3(3) . . ? O13 C14 Fe5 173.0(3) . . ? C16 C15 P1 119.4(3) . . ? C20 C15 P1 122.0(3) . . ? C20 C15 C16 118.4(3) . . ? C15 C16 H16 119.6 . . ? C17 C16 C15 120.8(3) . . ? C17 C16 H16 119.6 . . ? C16 C17 H17 120.1 . . ? C18 C17 C16 119.7(4) . . ? C18 C17 H17 120.1 . . ? C17 C18 H18 120.0 . . ? C19 C18 C17 120.1(3) . . ? C19 C18 H18 120.0 . . ? C18 C19 H19 119.7 . . ? C18 C19 C20 120.5(4) . . ? C20 C19 H19 119.7 . . ? C15 C20 H20 119.8 . . ? C19 C20 C15 120.5(4) . . ? C19 C20 H20 119.8 . . ? C22 C21 P1 122.8(2) . . ? C22 C21 C26 118.2(3) . . ? C26 C21 P1 118.7(2) . . ? C21 C22 H22 119.8 . . ? C21 C22 C23 120.5(3) . . ? C23 C22 H22 119.8 . . ? C22 C23 H23 119.8 . . ? C24 C23 C22 120.4(3) . . ? C24 C23 H23 119.8 . . ? C23 C24 H24 120.2 . . ? C23 C24 C25 119.5(3) . . ? C25 C24 H24 120.2 . . ? C24 C25 H25 119.7 . . ? C26 C25 C24 120.6(3) . . ? C26 C25 H25 119.7 . . ? C21 C26 H26 119.6 . . ? C25 C26 C21 120.8(3) . . ? C25 C26 H26 119.6 . . ? C28 C27 P1 120.9(2) . . ? C28 C27 C32 119.4(3) . . ? C32 C27 P1 119.7(2) . . ? C27 C28 H28 120.1 . . ? C27 C28 C29 119.9(3) . . ? C29 C28 H28 120.1 . . ? C28 C29 H29 119.9 . . ? C30 C29 C28 120.3(3) . . ? C30 C29 H29 119.9 . . ? C29 C30 H30 119.9 . . ? C29 C30 C31 120.1(3) . . ? C31 C30 H30 119.9 . . ? C30 C31 H31 119.9 . . ? C32 C31 C30 120.2(3) . . ? C32 C31 H31 119.9 . . ? C27 C32 H32 119.9 . . ? C31 C32 C27 120.2(3) . . ? C31 C32 H32 119.9 . . ? C35 N1 C33 111.1(2) . . ? C35 N1 C39 111.4(3) . . ? C37 N1 C33 111.3(3) . . ? C37 N1 C35 106.0(2) . . ? C37 N1 C39 111.6(3) . . ? C39 N1 C33 105.6(2) . . ? N1 C33 H33A 108.5 . . ? N1 C33 H33B 108.5 . . ? H33A C33 H33B 107.5 . . ? C34 C33 N1 115.3(3) . . ? C34 C33 H33A 108.5 . . ? C34 C33 H33B 108.5 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34B 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N1 C35 H35A 108.4 . . ? N1 C35 H35B 108.4 . . ? H35A C35 H35B 107.5 . . ? C36 C35 N1 115.5(3) . . ? C36 C35 H35A 108.4 . . ? C36 C35 H35B 108.4 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36B 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N1 C37 H37A 108.4 . . ? N1 C37 H37B 108.4 . . ? N1 C37 C38 115.6(3) . . ? H37A C37 H37B 107.4 . . ? C38 C37 H37A 108.4 . . ? C38 C37 H37B 108.4 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38B 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N1 C39 H39A 108.4 . . ? N1 C39 H39B 108.4 . . ? H39A C39 H39B 107.4 . . ? C40 C39 N1 115.6(3) . . ? C40 C39 H39A 108.4 . . ? C40 C39 H39B 108.4 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40B 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? 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 H 1.82(5) . ? Fe1 Fe2 2.7018(6) . ? Fe1 Fe4 2.6450(6) . ? Fe1 Fe5 2.5923(6) . ? Fe1 P1 2.2245(8) . ? Fe1 C1 1.859(3) . ? Fe1 C2 1.772(3) . ? Fe1 C11 1.821(3) . ? Fe2 H 1.83(5) . ? Fe2 Fe3 2.5552(6) . ? Fe2 Fe5 2.6400(6) . ? Fe2 C1 1.852(3) . ? Fe2 C3 1.805(4) . ? Fe2 C4 1.778(3) . ? Fe2 C5 1.900(3) . ? Fe3 Fe4 2.5757(6) . ? Fe3 Fe5 2.5949(6) . ? Fe3 C1 1.879(3) . ? Fe3 C5 2.076(3) . ? Fe3 C6 1.822(3) . ? Fe3 C7 1.779(3) . ? Fe3 C8 2.054(3) . ? Fe4 Fe5 2.5937(6) . ? Fe4 C1 1.857(3) . ? Fe4 C8 1.918(3) . ? Fe4 C9 1.788(3) . ? Fe4 C10 1.778(3) . ? Fe4 C11 2.359(3) . ? Fe5 C1 2.015(3) . ? Fe5 C12 1.783(3) . ? Fe5 C13 1.784(3) . ? Fe5 C14 1.790(3) . ? P1 C15 1.833(3) . ? P1 C21 1.839(3) . ? P1 C27 1.825(3) . ? O1 C2 1.152(4) . ? O2 C3 1.146(4) . ? O3 C4 1.139(4) . ? O4 C5 1.163(4) . ? O5 C6 1.126(4) . ? O6 C7 1.152(4) . ? O7 C8 1.160(4) . ? O8 C9 1.141(4) . ? O9 C10 1.144(4) . ? O10 C11 1.155(4) . ? O11 C12 1.150(4) . ? O12 C13 1.154(4) . ? O13 C14 1.153(4) . ? C15 C16 1.399(5) . ? C15 C20 1.397(5) . ? C16 H16 0.9500 . ? C16 C17 1.395(5) . ? C17 H17 0.9500 . ? C17 C18 1.390(6) . ? C18 H18 0.9500 . ? C18 C19 1.373(6) . ? C19 H19 0.9500 . ? C19 C20 1.395(5) . ? C20 H20 0.9500 . ? C21 C22 1.391(4) . ? C21 C26 1.398(5) . ? C22 H22 0.9500 . ? C22 C23 1.399(5) . ? C23 H23 0.9500 . ? C23 C24 1.373(6) . ? C24 H24 0.9500 . ? C24 C25 1.382(5) . ? C25 H25 0.9500 . ? C25 C26 1.380(5) . ? C26 H26 0.9500 . ? C27 C28 1.386(4) . ? C27 C32 1.414(4) . ? C28 H28 0.9500 . ? C28 C29 1.402(5) . ? C29 H29 0.9500 . ? C29 C30 1.386(5) . ? C30 H30 0.9500 . ? C30 C31 1.387(5) . ? C31 H31 0.9500 . ? C31 C32 1.382(5) . ? C32 H32 0.9500 . ? N1 C33 1.531(4) . ? N1 C35 1.519(4) . ? N1 C37 1.511(4) . ? N1 C39 1.522(4) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C33 C34 1.521(5) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C35 C36 1.509(5) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C37 C38 1.514(5) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C39 C40 1.521(5) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? 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 C1 Fe3 167.32(17) . . . . ? Fe1 Fe2 C1 Fe4 111.5(9) . . . . ? Fe1 Fe2 C1 Fe5 83.61(11) . . . . ? Fe1 Fe4 C1 Fe2 -111.7(9) . . . . ? Fe1 Fe4 C1 Fe3 -167.51(16) . . . . ? Fe1 Fe4 C1 Fe5 -83.76(11) . . . . ? Fe1 P1 C15 C16 -50.1(3) . . . . ? Fe1 P1 C15 C20 124.8(2) . . . . ? Fe1 P1 C21 C22 91.8(3) . . . . ? Fe1 P1 C21 C26 -81.5(3) . . . . ? Fe1 P1 C27 C28 -14.3(3) . . . . ? Fe1 P1 C27 C32 166.0(2) . . . . ? Fe2 Fe1 C1 Fe3 -89.1(8) . . . . ? Fe2 Fe1 C1 Fe4 -169.46(18) . . . . ? Fe2 Fe1 C1 Fe5 -85.59(11) . . . . ? Fe2 Fe1 C11 Fe4 4.5(2) . . . . ? Fe2 Fe1 C11 O10 -170.4(7) . . . . ? Fe2 Fe3 C1 Fe1 89.9(8) . . . . ? Fe2 Fe3 C1 Fe4 170.63(16) . . . . ? Fe2 Fe3 C1 Fe5 86.36(10) . . . . ? Fe3 Fe2 C1 Fe1 -167.32(17) . . . . ? Fe3 Fe2 C1 Fe4 -55.9(9) . . . . ? Fe3 Fe2 C1 Fe5 -83.71(10) . . . . ? Fe3 Fe4 C1 Fe1 167.51(17) . . . . ? Fe3 Fe4 C1 Fe2 55.8(8) . . . . ? Fe3 Fe4 C1 Fe5 83.75(10) . . . . ? Fe4 Fe1 C1 Fe2 169.46(18) . . . . ? Fe4 Fe1 C1 Fe3 80.4(8) . . . . ? Fe4 Fe1 C1 Fe5 83.88(11) . . . . ? Fe4 Fe1 C11 O10 -175.0(8) . . . . ? Fe4 Fe3 C1 Fe1 -80.8(8) . . . . ? Fe4 Fe3 C1 Fe2 -170.63(16) . . . . ? Fe4 Fe3 C1 Fe5 -84.27(10) . . . . ? Fe5 Fe1 C1 Fe2 85.59(11) . . . . ? Fe5 Fe1 C1 Fe3 -3.5(7) . . . . ? Fe5 Fe1 C1 Fe4 -83.88(11) . . . . ? Fe5 Fe1 C11 Fe4 47.83(7) . . . . ? Fe5 Fe1 C11 O10 -127.1(8) . . . . ? Fe5 Fe2 C1 Fe1 -83.61(11) . . . . ? Fe5 Fe2 C1 Fe3 83.71(10) . . . . ? Fe5 Fe2 C1 Fe4 27.9(8) . . . . ? Fe5 Fe3 C1 Fe1 3.5(7) . . . . ? Fe5 Fe3 C1 Fe2 -86.36(10) . . . . ? Fe5 Fe3 C1 Fe4 84.27(10) . . . . ? Fe5 Fe4 C1 Fe1 83.76(11) . . . . ? Fe5 Fe4 C1 Fe2 -28.0(8) . . . . ? Fe5 Fe4 C1 Fe3 -83.75(10) . . . . ? P1 Fe1 C1 Fe2 -83.52(11) . . . . ? P1 Fe1 C1 Fe3 -172.6(7) . . . . ? P1 Fe1 C1 Fe4 107.02(9) . . . . ? P1 Fe1 C1 Fe5 -169.11(4) . . . . ? P1 Fe1 C11 Fe4 -121.60(6) . . . . ? P1 Fe1 C11 O10 63.4(8) . . . . ? P1 C15 C16 C17 177.2(3) . . . . ? P1 C15 C20 C19 -176.7(3) . . . . ? P1 C21 C22 C23 -172.8(3) . . . . ? P1 C21 C26 C25 173.8(3) . . . . ? P1 C27 C28 C29 179.5(2) . . . . ? P1 C27 C32 C31 179.3(2) . . . . ? C1 Fe1 C11 Fe4 -3.46(12) . . . . ? C1 Fe1 C11 O10 -178.4(8) . . . . ? C2 Fe1 C1 Fe2 57.4(2) . . . . ? C2 Fe1 C1 Fe3 -31.7(9) . . . . ? C2 Fe1 C1 Fe4 -112.08(19) . . . . ? C2 Fe1 C1 Fe5 -28.2(2) . . . . ? C2 Fe1 C11 Fe4 141.88(12) . . . . ? C2 Fe1 C11 O10 -33.1(8) . . . . ? C3 Fe2 C1 Fe1 -32.1(4) . . . . ? C3 Fe2 C1 Fe3 135.3(3) . . . . ? C3 Fe2 C1 Fe4 79.4(10) . . . . ? C3 Fe2 C1 Fe5 51.6(3) . . . . ? C4 Fe2 C1 Fe1 102.53(14) . . . . ? C4 Fe2 C1 Fe3 -90.15(13) . . . . ? C4 Fe2 C1 Fe4 -146.0(9) . . . . ? C4 Fe2 C1 Fe5 -173.86(11) . . . . ? C5 Fe2 C1 Fe1 -162.78(13) . . . . ? C5 Fe2 C1 Fe3 4.54(14) . . . . ? C5 Fe2 C1 Fe4 -51.3(9) . . . . ? C5 Fe2 C1 Fe5 -79.17(13) . . . . ? C5 Fe3 C1 Fe1 85.8(8) . . . . ? C5 Fe3 C1 Fe2 -4.10(12) . . . . ? C5 Fe3 C1 Fe4 166.54(12) . . . . ? C5 Fe3 C1 Fe5 82.26(12) . . . . ? C6 Fe3 C1 Fe1 7.0(10) . . . . ? C6 Fe3 C1 Fe2 -82.8(4) . . . . ? C6 Fe3 C1 Fe4 87.8(3) . . . . ? C6 Fe3 C1 Fe5 3.5(4) . . . . ? C7 Fe3 C1 Fe1 -173.7(8) . . . . ? C7 Fe3 C1 Fe2 96.43(13) . . . . ? C7 Fe3 C1 Fe4 -92.94(13) . . . . ? C7 Fe3 C1 Fe5 -177.21(12) . . . . ? C8 Fe3 C1 Fe1 -84.6(8) . . . . ? C8 Fe3 C1 Fe2 -174.45(12) . . . . ? C8 Fe3 C1 Fe4 -3.81(12) . . . . ? C8 Fe3 C1 Fe5 -88.09(11) . . . . ? C8 Fe4 C1 Fe1 171.63(12) . . . . ? C8 Fe4 C1 Fe2 59.9(9) . . . . ? C8 Fe4 C1 Fe3 4.12(13) . . . . ? C8 Fe4 C1 Fe5 87.87(12) . . . . ? C9 Fe4 C1 Fe1 67.3(3) . . . . ? C9 Fe4 C1 Fe2 -44.4(10) . . . . ? C9 Fe4 C1 Fe3 -100.2(3) . . . . ? C9 Fe4 C1 Fe5 -16.4(3) . . . . ? C10 Fe4 C1 Fe1 -91.18(14) . . . . ? C10 Fe4 C1 Fe2 157.1(9) . . . . ? C10 Fe4 C1 Fe3 101.31(14) . . . . ? C10 Fe4 C1 Fe5 -174.94(12) . . . . ? C11 Fe1 C1 Fe2 173.76(13) . . . . ? C11 Fe1 C1 Fe3 84.7(8) . . . . ? C11 Fe1 C1 Fe4 4.29(15) . . . . ? C11 Fe1 C1 Fe5 88.17(13) . . . . ? C11 Fe4 C1 Fe1 -3.20(11) . . . . ? C11 Fe4 C1 Fe2 -114.9(9) . . . . ? C11 Fe4 C1 Fe3 -170.71(12) . . . . ? C11 Fe4 C1 Fe5 -86.97(11) . . . . ? C15 P1 C21 C22 -33.1(3) . . . . ? C15 P1 C21 C26 153.6(3) . . . . ? C15 P1 C27 C28 114.2(2) . . . . ? C15 P1 C27 C32 -65.5(3) . . . . ? C15 C16 C17 C18 -1.2(5) . . . . ? C16 C15 C20 C19 -1.7(5) . . . . ? C16 C17 C18 C19 -0.1(6) . . . . ? C17 C18 C19 C20 0.5(6) . . . . ? C18 C19 C20 C15 0.4(5) . . . . ? C20 C15 C16 C17 2.2(5) . . . . ? C21 P1 C15 C16 72.5(3) . . . . ? C21 P1 C15 C20 -112.7(3) . . . . ? C21 P1 C27 C28 -136.7(2) . . . . ? C21 P1 C27 C32 43.6(3) . . . . ? C21 C22 C23 C24 -0.8(5) . . . . ? C22 C21 C26 C25 0.1(5) . . . . ? C22 C23 C24 C25 0.2(5) . . . . ? C23 C24 C25 C26 0.6(6) . . . . ? C24 C25 C26 C21 -0.7(6) . . . . ? C26 C21 C22 C23 0.6(5) . . . . ? C27 P1 C15 C16 178.7(3) . . . . ? C27 P1 C15 C20 -6.5(3) . . . . ? C27 P1 C21 C22 -140.3(3) . . . . ? C27 P1 C21 C26 46.3(3) . . . . ? C27 C28 C29 C30 1.4(5) . . . . ? C28 C27 C32 C31 -0.4(5) . . . . ? C28 C29 C30 C31 -0.9(5) . . . . ? C29 C30 C31 C32 -0.3(5) . . . . ? C30 C31 C32 C27 1.0(5) . . . . ? C32 C27 C28 C29 -0.8(4) . . . . ? C33 N1 C35 C36 54.7(4) . . . . ? C33 N1 C37 C38 -62.1(4) . . . . ? C33 N1 C39 C40 172.9(3) . . . . ? C35 N1 C33 C34 52.7(4) . . . . ? C35 N1 C37 C38 177.0(3) . . . . ? C35 N1 C39 C40 -66.4(4) . . . . ? C37 N1 C33 C34 -65.1(4) . . . . ? C37 N1 C35 C36 175.7(3) . . . . ? C37 N1 C39 C40 51.9(4) . . . . ? C39 N1 C33 C34 173.6(3) . . . . ? C39 N1 C35 C36 -62.7(4) . . . . ? C39 N1 C37 C38 55.6(4) . . . . ? loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -5.7454 0.5798 12.7248 0.0304 0.0530 0.9981 3.2042 7.1567 -4.7294 -0.4133 -0.8674 -0.2772 4.8765 5.3700 -8.9452 -0.3364 -0.7016 -0.6282 3.0750 -5.9559 -8.5970 0.2829 0.6040 -0.7451 -1.9455 -7.7003 1.8097 0.4287 0.9024 0.0430 10.9921 -0.3665 -0.8941 -0.8796 0.3115 -0.3595 -10.9921 0.3665 0.8941 0.8796 -0.3115 0.3595 -4.0117 3.9988 11.0030 -0.2022 -0.3446 0.8955