#------------------------------------------------------------------------------ #$Date: 2024-09-06 01:48:15 +0300 (Fri, 06 Sep 2024) $ #$Revision: 294398 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/20/1572064.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_1572064 loop_ _publ_author_name 'K\"orner, Lukas' 'Bockfeld, Dirk' 'Bannenberg, Thomas' 'Tamm, Matthias' _publ_section_title ; 2,3-Diamino-4,5-diarylcyclopentadienone iron carbonyl complexes as catalysts for reductive amination reactions ; _journal_issue 16 _journal_name_full 'Catalysis Science & Technology' _journal_page_first 4522 _journal_page_last 4532 _journal_paper_doi 10.1039/D4CY00372A _journal_volume 14 _journal_year 2024 _chemical_formula_moiety 'C33 H31 F6 Fe N3 O3 [0.5 (C2 H3 N1)]' _chemical_formula_sum 'C34 H32.5 F6 Fe N3.5 O3' _chemical_formula_weight 707.98 _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 iterative _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2024-03-06 deposited with the CCDC. 2024-07-05 downloaded from the CCDC. ; _cell_angle_alpha 106.515(3) _cell_angle_beta 110.781(4) _cell_angle_gamma 94.220(3) _cell_formula_units_Z 2 _cell_length_a 10.7552(4) _cell_length_b 11.5325(3) _cell_length_c 14.6781(6) _cell_measurement_reflns_used 31930 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 78.3480 _cell_measurement_theta_min 3.3540 _cell_volume 1600.72(12) _computing_cell_refinement 'CrysAlisPro 1.171.42.64a (Rigaku OD, 2022)' _computing_data_collection 'CrysAlisPro 1.171.42.64a (Rigaku OD, 2022)' _computing_data_reduction 'CrysAlisPro 1.171.42.64a (Rigaku OD, 2022)' _computing_publication_material 'OLEX2 v1.3 (O. V. Dolomanov et al., J. Appl. Cryst., 2009, 42, 339-341)' _computing_structure_refinement 'SHELXL-2018/3 (G. M. Sheldrick, Acta Cryst., 2015, C71, 3-8)' _computing_structure_solution 'SHELXT 2018/2 (G. M. Sheldrick, Acta Cryst., 2015, A71, 3-8)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100(2) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.969 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Single source at home/near, HyPix' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_unetI/netI 0.0042 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.969 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 6848 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.969 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 80.574 _diffrn_reflns_theta_min 3.415 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 4.446 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.358 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.42.64a (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 orange _exptl_crystal_density_diffrn 1.469 _exptl_crystal_description irregular _exptl_crystal_F_000 730 _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.160 _exptl_crystal_size_min 0.060 _refine_diff_density_max 1.052 _refine_diff_density_min -0.814 _refine_diff_density_rms 0.084 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 474 _refine_ls_number_reflns 6848 _refine_ls_number_restraints 127 _refine_ls_restrained_S_all 1.127 _refine_ls_R_factor_all 0.0619 _refine_ls_R_factor_gt 0.0606 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1010P)^2^+2.0608P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1657 _refine_ls_wR_factor_ref 0.1675 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6677 _reflns_number_total 6848 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4cy00372a3.cif _cod_data_source_block lk42db _cod_depositor_comments 'Adding full bibliography for 1572060--1572070.cif.' _cod_original_cell_volume 1600.72(11) _cod_original_formula_sum 'C34 H32.50 F6 Fe N3.50 O3' _cod_database_code 1572064 _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_min 0.470 _shelx_estimated_absorpt_t_max 0.776 _oxdiff_exptl_absorpt_empirical_full_min 0.574 _oxdiff_exptl_absorpt_empirical_full_max 1.782 _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling - Detector area scaling ; _smtbx_masks_void_probe_radius 1.2 _smtbx_masks_void_truncation_radius 1.2 _smtbx_masks_special_details ; 0.5 molecules of acetonitrile per Asymmetric unit have been identified but could not be refined satisfactorily. Therefore, a solvent mask, the Olex2 implementation of the program SQUEEZE (Spek, A. L. (2015). Acta Cryst. C71, 9-18.) has been used to mathematically remove the electron density of these molecules. 21 electrons were found in a volume of 129\%A^3^ in 1 void per unit cell. This is consistent with the presence of 0.5[C2H3N] per Asymmetric Unit which account for 22 electrons per unit cell. The sum formula and derived parameters are based on 0.5 molecules of C2H3N per Asymmetric unit. ; _shelx_res_file ; TITL lk42db_a.res in P-1 lk42db.res created by SHELXL-2018/3 at 13:46:31 on 05-Apr-2023 REM Old TITL lk42db_twin1_hklf4 in P-1 REM SHELXT solution in P-1: R1 0.259, Rweak 0.027, 0.084 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C35 N5 O2 F4 Fe CELL 1.54184 10.7552 11.5325 14.6781 106.515 110.781 94.22 ZERR 2 0.0004 0.0003 0.0006 0.003 0.004 0.003 LATT 1 SFAC C H F Fe N O UNIT 68 65 12 2 7 6 SADI C19 F4 C19 F5 C19 F6 C19 F4A C19 F5A C19 F6A C19 F4B C19 F5B C19 F6B SADI F4 F5 F5 F6 F6 F4 F4A F5A F5A F6A F6A F4A F4B F5B F5B F6B F6B F4B ISOR 0.001 0.002 F4 F5 F6 F4A F5A F6A F4B F5B F6B SUMP 1 0 1 2 1 3 1 4 L.S. 10 0 0 PLAN 10 SIZE 0.2 0.16 0.06 TEMP -173 CONF list 4 ABIN fmap 2 53 acta MERG 0 REM REM REM WGHT 0.101000 2.060800 BASF 0.45447 FVAR 5.27938 0.38714 0.30416 0.30871 FE1 4 0.427805 0.367581 0.152873 11.00000 0.02118 0.02364 = 0.03033 0.01335 0.00770 0.00581 F1 3 -0.070491 0.027189 0.343473 11.00000 0.04309 0.07198 = 0.07176 0.04161 0.02363 -0.00066 F2 3 -0.077912 -0.085104 0.198360 11.00000 0.05970 0.03106 = 0.14402 0.00419 0.06644 -0.00516 F3 3 -0.203933 0.050923 0.205622 11.00000 0.02795 0.05417 = 0.07540 0.03009 0.01743 -0.00006 O1 6 0.201676 0.530495 0.209341 11.00000 0.02353 0.03798 = 0.05367 0.02743 0.01386 0.01258 O2 6 0.671313 0.386471 0.107980 11.00000 0.03048 0.04537 = 0.04441 0.01473 0.01850 0.00899 O3 6 0.363503 0.096864 0.066022 11.00000 0.05840 0.02476 = 0.05061 0.01161 0.01297 0.00507 N1 5 0.685838 0.555576 0.344308 11.00000 0.02076 0.02209 = 0.03438 0.01237 0.00772 0.00686 N2 5 0.467081 0.665575 0.224002 11.00000 0.02479 0.02431 = 0.03750 0.01757 0.01138 0.00805 N3 5 0.284547 0.388649 0.035614 11.00000 0.02905 0.03271 = 0.03431 0.01553 0.00957 0.00810 C1 1 0.312124 0.498035 0.239163 11.00000 0.02136 0.02840 = 0.03559 0.01688 0.00990 0.00719 C2 1 0.339138 0.384719 0.262699 11.00000 0.02364 0.02571 = 0.03593 0.01634 0.01171 0.00645 C3 1 0.484328 0.390918 0.305188 11.00000 0.02275 0.02508 = 0.02915 0.01349 0.00904 0.00701 C4 1 0.549061 0.503604 0.302509 11.00000 0.02240 0.02411 = 0.02611 0.01077 0.00889 0.00695 C5 1 0.444403 0.558724 0.247306 11.00000 0.02268 0.02225 = 0.03227 0.01334 0.00937 0.00682 C6 1 0.233940 0.293604 0.261835 11.00000 0.02315 0.02887 = 0.03627 0.01495 0.01025 0.00583 C7 1 0.110215 0.324174 0.260047 11.00000 0.03030 0.02895 = 0.05259 0.01708 0.02003 0.00695 AFIX 43 H7 2 0.095301 0.404661 0.261199 11.00000 -1.20000 AFIX 0 C8 1 0.008626 0.239963 0.256633 11.00000 0.02984 0.03367 = 0.06270 0.01628 0.02548 0.00721 AFIX 43 H8 2 -0.075491 0.262392 0.254053 11.00000 -1.20000 AFIX 0 C9 1 0.029788 0.122307 0.256981 11.00000 0.02874 0.03207 = 0.04577 0.01349 0.01671 0.00026 C10 1 0.152698 0.090443 0.261346 11.00000 0.02834 0.03158 = 0.04760 0.01993 0.01397 0.00541 AFIX 43 H10 2 0.168125 0.010865 0.262991 11.00000 -1.20000 AFIX 0 C11 1 0.253820 0.174799 0.263332 11.00000 0.02651 0.03182 = 0.04930 0.02172 0.01442 0.00612 AFIX 43 H11 2 0.337661 0.151818 0.265738 11.00000 -1.20000 AFIX 0 C12 1 -0.079547 0.029854 0.251333 11.00000 0.03007 0.03651 = 0.06283 0.01641 0.02267 0.00492 C13 1 0.549874 0.313219 0.367198 11.00000 0.02041 0.02187 = 0.03330 0.01478 0.00926 0.00533 C14 1 0.609261 0.216629 0.329792 11.00000 0.02413 0.02703 = 0.03252 0.01455 0.01109 0.00727 AFIX 43 H14 2 0.612629 0.201460 0.263697 11.00000 -1.20000 AFIX 0 C15 1 0.663324 0.142639 0.387743 11.00000 0.02477 0.02414 = 0.04124 0.01499 0.01229 0.00929 AFIX 43 H15 2 0.703918 0.077655 0.361657 11.00000 -1.20000 AFIX 0 C16 1 0.657797 0.163983 0.483554 11.00000 0.03314 0.02528 = 0.04028 0.01810 0.01415 0.00986 C17 1 0.598804 0.258529 0.522331 11.00000 0.04042 0.03290 = 0.03499 0.01926 0.01743 0.01530 AFIX 43 H17 2 0.594868 0.272454 0.588141 11.00000 -1.20000 AFIX 0 C18 1 0.545381 0.332910 0.464142 11.00000 0.03249 0.02615 = 0.03867 0.01670 0.01514 0.01181 AFIX 43 H18 2 0.505304 0.397984 0.490807 11.00000 -1.20000 AFIX 0 C19 1 0.716947 0.084834 0.546540 11.00000 0.04477 0.03764 = 0.05007 0.02765 0.02314 0.01890 C20 1 0.787770 0.481104 0.373256 11.00000 0.02106 0.02618 = 0.03635 0.01491 0.00821 0.00728 AFIX 23 H20A 2 0.757731 0.397203 0.321458 11.00000 -1.20000 H20B 2 0.798683 0.473776 0.441140 11.00000 -1.20000 AFIX 0 C21 1 0.922603 0.540744 0.379201 11.00000 0.02335 0.03240 = 0.04118 0.01805 0.01122 0.00747 AFIX 23 H21A 2 0.991922 0.491896 0.402435 11.00000 -1.20000 H21B 2 0.913289 0.539753 0.309403 11.00000 -1.20000 AFIX 0 C22 1 0.970033 0.672962 0.452959 11.00000 0.02331 0.03201 = 0.05061 0.01696 0.00732 0.00266 AFIX 23 H22A 2 1.053846 0.710835 0.450404 11.00000 -1.20000 H22B 2 0.990464 0.674079 0.524528 11.00000 -1.20000 AFIX 0 C23 1 0.858894 0.746485 0.421964 11.00000 0.02762 0.02527 = 0.05473 0.01500 0.00915 0.00414 AFIX 23 H23A 2 0.886577 0.830750 0.473060 11.00000 -1.20000 H23B 2 0.846469 0.753487 0.353728 11.00000 -1.20000 AFIX 0 C24 1 0.725328 0.683908 0.416572 11.00000 0.02727 0.02319 = 0.03973 0.00714 0.00893 0.00582 AFIX 23 H24A 2 0.735206 0.683773 0.486215 11.00000 -1.20000 H24B 2 0.653589 0.730406 0.392914 11.00000 -1.20000 AFIX 0 C25 1 0.560504 0.666772 0.171294 11.00000 0.02603 0.02655 = 0.03956 0.01694 0.01338 0.00764 AFIX 23 H25A 2 0.513006 0.615852 0.097524 11.00000 -1.20000 H25B 2 0.638134 0.629794 0.202410 11.00000 -1.20000 AFIX 0 C26 1 0.612817 0.796831 0.179377 11.00000 0.03130 0.02726 = 0.04545 0.01748 0.01581 0.00567 AFIX 23 H26A 2 0.669720 0.793420 0.138783 11.00000 -1.20000 H26B 2 0.670277 0.844783 0.252442 11.00000 -1.20000 AFIX 0 C27 1 0.496978 0.861742 0.139697 11.00000 0.03524 0.02524 = 0.04618 0.01915 0.01221 0.00660 AFIX 23 H27A 2 0.533615 0.949069 0.153410 11.00000 -1.20000 H27B 2 0.447530 0.821823 0.064131 11.00000 -1.20000 AFIX 0 C28 1 0.401046 0.854774 0.193575 11.00000 0.03294 0.02539 = 0.04925 0.02025 0.01401 0.01192 AFIX 23 H28A 2 0.322633 0.891908 0.164273 11.00000 -1.20000 H28B 2 0.448347 0.903070 0.267986 11.00000 -1.20000 AFIX 0 C29 1 0.350255 0.721691 0.181322 11.00000 0.02697 0.02663 = 0.04454 0.02005 0.01092 0.00980 AFIX 23 H29A 2 0.289315 0.720144 0.218274 11.00000 -1.20000 H29B 2 0.298330 0.673927 0.107282 11.00000 -1.20000 AFIX 0 C30 1 0.571698 0.378962 0.120307 11.00000 0.03177 0.02784 = 0.02966 0.01181 0.00891 0.00619 C31 1 0.388711 0.202264 0.100183 11.00000 0.03388 0.03364 = 0.03191 0.01480 0.00797 0.00653 C32 1 0.192597 0.399573 -0.027717 11.00000 0.03309 0.05440 = 0.04247 0.02491 0.01237 0.01342 C33 1 0.074097 0.412173 -0.109582 11.00000 0.03737 0.12555 = 0.07246 0.06456 0.01029 0.02810 AFIX 137 H33A 2 0.079410 0.374512 -0.176608 11.00000 -1.50000 H33B 2 0.071625 0.499784 -0.098135 11.00000 -1.50000 H33C 2 -0.008332 0.370684 -0.108987 11.00000 -1.50000 AFIX 0 PART 1 F4 3 0.827131 0.152170 0.634996 21.00000 0.03486 0.04230 = 0.04294 0.02690 0.00534 0.00676 F5 3 0.754107 -0.009231 0.499916 21.00000 0.05567 0.04539 = 0.05068 0.01834 0.01708 0.02432 F6 3 0.629794 0.044583 0.584586 21.00000 0.03285 0.03190 = 0.03353 0.02159 0.01030 0.00072 PART 2 F4A 3 0.825066 0.042941 0.526500 31.00000 0.03322 0.03279 = 0.03398 0.01504 0.00879 0.01817 F5A 3 0.635253 -0.005846 0.537076 31.00000 0.06914 0.06188 = 0.06898 0.03211 0.02081 0.01023 F6A 3 0.782299 0.151810 0.649674 31.00000 0.05713 0.05282 = 0.04776 0.02011 0.01946 0.02121 PART 3 F4B 3 0.672655 0.087631 0.620281 41.00000 0.05516 0.04672 = 0.04430 0.01823 0.01680 0.01634 F5B 3 0.843795 0.096765 0.580627 41.00000 0.06138 0.05946 = 0.06528 0.02921 0.01676 0.01064 F6B 3 0.670211 -0.040021 0.482281 41.00000 0.04808 0.02829 = 0.04300 0.01907 0.00876 0.01195 HKLF 5 REM lk42db_a.res in P-1 REM wR2 = 0.1675, GooF = S = 1.054, Restrained GooF = 1.127 for all data REM R1 = 0.0606 for 6677 Fo > 4sig(Fo) and 0.0619 for all 6848 data REM 474 parameters refined using 127 restraints END WGHT 0.1010 2.0608 REM Highest difference peak 1.052, deepest hole -0.814, 1-sigma level 0.084 Q1 1 0.4348 0.3830 0.2273 11.00000 0.05 1.05 Q2 1 0.4138 0.3450 0.0817 11.00000 0.05 0.93 Q3 1 0.5201 0.3841 0.1678 11.00000 0.05 0.85 Q4 1 0.7318 0.1177 0.6379 11.00000 0.05 0.69 Q5 1 0.3389 0.3566 0.1332 11.00000 0.05 0.68 Q6 1 0.6117 -0.0453 0.4789 11.00000 0.05 0.67 Q7 1 0.8748 0.0803 0.5390 11.00000 0.05 0.59 Q8 1 0.3562 0.3639 0.2010 11.00000 0.05 0.50 Q9 1 0.4059 0.3801 0.2814 11.00000 0.05 0.45 Q10 1 0.2586 0.3991 -0.0366 11.00000 0.05 0.40 ; _shelx_res_checksum 1385 _shelx_hkl_file ; 0 0 1 20101.0 15.0517 -2 0 0 1 20101.0 15.0517 1 0 0 2 269060. 75.7116 -2 0 0 2 269060. 75.7116 1 0 0 -3 128701. 64.1023 -2 0 0 -3 128701. 64.1023 1 0 0 -4 9548.50 29.3224 -2 0 0 -4 9548.50 29.3224 1 0 0 -5 8626.52 38.7533 -2 0 0 -5 8626.52 38.7533 1 0 0 6 4771.51 47.7273 -2 0 0 6 4771.51 47.7273 1 0 0 7 888.479 57.8354 -2 0 0 7 888.479 57.8354 1 0 0 -8 30019.7 57.8311 -2 0 0 -8 30019.7 57.8311 1 0 0 -9 3302.95 33.9175 -2 0 0 -9 3302.95 33.9175 1 0 0 10 17878.2 41.1241 -2 0 0 10 17878.2 41.1241 1 0 0 11 1672.50 40.2529 -2 0 0 11 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-12 0 0.1502 -0.2872 8 -12 1 0.0336 -0.1494 8 -12 2 -0.0066 0.0695 8 -12 3 0.0341 0.2975 8 -12 4 0.1191 0.4569 8 -11 0 0.1675 -0.1892 8 -11 1 0.1831 -0.1354 8 -11 2 0.2553 -0.0664 8 -11 3 0.3475 -0.0289 8 -11 4 0.4022 -0.0549 8 -11 5 0.3731 -0.1435 8 -11 6 0.2532 -0.2592 8 -10 0 0.2349 0.1423 8 -10 1 0.3859 0.0881 8 -10 2 0.4727 -0.0109 8 -10 3 0.4822 -0.1303 8 -10 4 0.4247 -0.2348 8 -10 5 0.3252 -0.2902 8 -10 6 0.2121 -0.2770 8 -10 7 0.1099 -0.1993 8 -10 8 0.0337 -0.0850 8 -9 0 0.0173 0.0501 8 -9 1 0.0881 0.0039 8 -9 2 0.0576 -0.0438 8 -9 3 -0.0250 -0.0613 8 -9 4 -0.0836 -0.0315 8 -9 5 -0.0621 0.0389 8 -9 6 0.0427 0.1237 8 -9 7 0.1809 0.1914 8 -9 8 0.2798 0.2193 8 -9 9 0.2864 0.2003 8 -8 0 -0.0397 -0.0879 8 -8 1 -0.1103 -0.0976 8 -8 2 -0.2242 -0.0881 8 -8 3 -0.3205 -0.0601 8 -8 4 -0.3337 -0.0234 8 -8 5 -0.2319 0.0069 8 -8 6 -0.0406 0.0200 8 -8 7 0.1662 0.0175 8 -8 8 0.3051 0.0124 8 -8 9 0.3284 0.0184 8 -7 0 -0.0037 0.0076 8 -7 1 -0.1519 0.0044 8 -7 2 -0.2543 -0.0039 8 -7 3 -0.2780 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-3 5 0.1564 -0.0306 8 -3 6 -0.0000 -0.0195 8 -3 7 -0.1719 -0.0243 8 -3 8 -0.2896 -0.0419 8 -3 9 -0.3102 -0.0608 8 -3 10 -0.2403 -0.0707 8 -2 0 0.0058 0.0237 8 -2 1 0.0301 0.0141 8 -2 2 0.0690 0.0050 8 -2 3 0.1551 0.0091 8 -2 4 0.2778 0.0306 8 -2 5 0.3837 0.0573 8 -2 6 0.4117 0.0650 8 -2 7 0.3363 0.0351 8 -2 8 0.1877 -0.0288 8 -2 9 0.0337 -0.0999 8 -2 10 -0.0619 -0.1431 8 -1 0 -0.2148 0.0940 8 -1 1 -0.2300 0.1048 8 -1 2 -0.2960 0.0969 8 -1 3 -0.2999 0.0752 8 -1 4 -0.1639 0.0572 8 -1 5 0.0939 0.0596 8 -1 6 0.3696 0.0839 8 -1 7 0.5415 0.1138 8 -1 8 0.5466 0.1268 8 -1 9 0.4117 0.1114 8 0 0 0.2263 0.0580 8 0 1 0.2190 0.0377 8 0 2 0.1038 0.0073 8 0 3 -0.0441 -0.0338 8 0 4 -0.1276 -0.0744 8 0 5 -0.0977 -0.0935 8 0 6 0.0163 -0.0741 8 0 7 0.1350 -0.0192 8 0 8 0.1874 0.0463 8 0 9 0.1551 0.0894 8 1 0 1.5942 0.0236 8 1 1 1.6251 0.0050 8 1 2 1.5494 0.0015 8 1 3 1.3262 0.0023 8 1 4 0.9963 -0.0095 8 1 5 0.6500 -0.0394 8 1 6 0.3706 -0.0748 8 1 7 0.1927 -0.0949 8 1 8 0.0995 -0.0872 8 2 0 1.9767 0.0977 8 2 1 2.1657 0.0815 8 2 2 2.2936 0.0763 8 2 3 2.2376 0.0894 8 2 4 1.9685 0.1085 8 2 5 1.5601 0.1124 8 2 6 1.1337 0.0885 8 2 7 0.7830 0.0430 8 2 8 0.5330 -0.0040 8 3 0 0.9643 0.0984 8 3 1 1.1336 0.0632 8 3 2 1.2598 0.0244 8 3 3 1.2588 0.0176 8 3 4 1.1057 0.0580 8 3 5 0.8519 0.1274 8 3 6 0.5897 0.1847 8 3 7 0.3918 0.1942 8 4 0 -0.2960 0.0395 8 4 1 -0.3118 0.0154 8 4 2 -0.2918 -0.0312 8 4 3 -0.2684 -0.0640 8 4 4 -0.2666 -0.0516 8 4 5 -0.2828 0.0083 8 4 6 -0.2878 0.0855 8 5 0 -0.5932 -0.0039 8 5 1 -0.4594 -0.0460 8 5 2 -0.2994 -0.1137 8 5 3 -0.1480 -0.1844 8 5 4 -0.0387 -0.2284 8 5 5 0.0097 -0.2243 8 6 0 0.1958 -0.0390 8 6 1 0.2689 -0.0793 8 6 2 0.2785 -0.1299 8 6 3 0.2630 -0.1889 8 6 4 0.2412 -0.2434 8 7 0 0.3989 0.0443 8 7 1 0.2176 0.0921 8 7 2 0.0551 0.1138 8 7 3 -0.0399 0.0899 8 8 0 0.0751 0.0782 8 8 1 0.1452 0.1987 8 8 2 0.2079 0.2624 8 9 0 0.2872 0.0268 9 -11 0 0.0531 -0.4745 9 -11 1 0.0358 -0.3992 9 -11 2 0.0549 -0.2691 9 -11 3 0.0871 -0.1523 9 -11 4 0.0981 -0.1014 9 -10 0 0.2848 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0 5 0.0526 -0.1677 9 0 6 0.1150 -0.1411 9 0 7 0.1579 -0.0686 9 1 0 1.4625 0.0184 9 1 1 1.4776 0.0108 9 1 2 1.2925 0.0149 9 1 3 0.9679 0.0137 9 1 4 0.6161 -0.0067 9 1 5 0.3315 -0.0422 9 1 6 0.1498 -0.0732 9 1 7 0.0560 -0.0804 9 2 0 2.1939 -0.0445 9 2 1 2.1935 -0.0423 9 2 2 1.9718 0.0195 9 2 3 1.5635 0.1166 9 2 4 1.0837 0.1983 9 2 5 0.6614 0.2217 9 2 6 0.3734 0.1790 9 3 0 1.2503 0.0079 9 3 1 1.1546 -0.0259 9 3 2 0.9477 -0.0302 9 3 3 0.6622 0.0125 9 3 4 0.3786 0.0888 9 3 5 0.1833 0.1614 9 4 0 -0.5077 0.0694 9 4 1 -0.6196 -0.0219 9 4 2 -0.6546 -0.1329 9 4 3 -0.6395 -0.2017 9 4 4 -0.5842 -0.1886 9 4 5 -0.4800 -0.1018 9 5 0 -0.9198 0.0005 9 5 1 -0.7204 -0.0948 9 5 2 -0.4674 -0.2055 9 5 3 -0.2494 -0.2855 9 5 4 -0.1143 -0.2990 9 6 0 0.2740 -0.0633 9 6 1 0.4210 -0.0823 9 6 2 0.4842 -0.1031 9 7 0 0.6372 0.0328 9 7 1 0.4116 0.1318 10 -10 0 0.2929 -0.1492 10 -10 1 0.2489 -0.1751 10 -10 2 0.1821 -0.1787 10 -10 3 0.1121 -0.1751 10 -9 0 0.0341 0.0812 10 -9 1 -0.0532 0.0812 10 -9 2 -0.1286 0.0749 10 -9 3 -0.1603 0.0667 10 -9 4 -0.1426 0.0634 10 -9 5 -0.0958 0.0704 10 -8 0 -0.3908 -0.0254 10 -8 1 -0.3456 0.0219 10 -8 2 -0.2652 0.0488 10 -8 3 -0.1630 0.0539 10 -8 4 -0.0612 0.0409 10 -8 5 0.0157 0.0160 10 -7 0 0.0736 0.0291 10 -7 1 0.2299 0.0141 10 -7 2 0.3784 -0.0187 10 -7 3 0.4751 -0.0522 10 -7 4 0.4892 -0.0730 10 -7 5 0.4161 -0.0771 10 -7 6 0.2806 -0.0676 10 -6 0 -0.0149 0.0334 10 -6 1 0.0816 -0.0164 10 -6 2 0.2074 -0.0367 10 -6 3 0.3220 -0.0100 10 -6 4 0.3848 0.0583 10 -6 5 0.3744 0.1420 10 -6 6 0.2971 0.2062 10 -5 0 -0.6306 -0.0779 10 -5 1 -0.5978 -0.0683 10 -5 2 -0.4986 -0.0204 10 -5 3 -0.3578 0.0496 10 -5 4 -0.2007 0.1184 10 -5 5 -0.0521 0.1658 10 -5 6 0.0631 0.1808 10 -5 7 0.1243 0.1622 10 -4 0 -0.3949 -0.0565 10 -4 1 -0.4160 -0.0264 10 -4 2 -0.4113 -0.0020 10 -4 3 -0.3834 -0.0062 10 -4 4 -0.3223 -0.0452 10 -4 5 -0.2233 -0.1014 10 -4 6 -0.1039 -0.1428 10 -4 7 -0.0030 -0.1440 10 -3 0 -0.2718 0.0451 10 -3 1 -0.2343 0.0573 10 -3 2 -0.1256 0.0533 10 -3 3 0.0070 0.0321 10 -3 4 0.1164 -0.0061 10 -3 5 0.1769 -0.0546 10 -3 6 0.1867 -0.0989 10 -3 7 0.1586 -0.1213 10 -2 0 -0.3654 0.0660 10 -2 1 -0.2112 0.0441 10 -2 2 0.0817 0.0333 10 -2 3 0.3946 0.0546 10 -2 4 0.5925 0.1028 10 -2 5 0.6023 0.1475 10 -2 6 0.4481 0.1548 10 -1 0 -0.0965 -0.0469 10 -1 1 0.0326 -0.0958 10 -1 2 0.2328 -0.1371 10 -1 3 0.4172 -0.1427 10 -1 4 0.4849 -0.0989 10 -1 5 0.3893 -0.0207 10 -1 6 0.1734 0.0551 10 0 0 0.3180 0.0258 10 0 1 0.3668 0.0216 10 0 2 0.3425 -0.0266 10 0 3 0.2686 -0.1073 10 0 4 0.1631 -0.1812 10 0 5 0.0410 -0.2074 10 0 6 -0.0733 -0.1718 10 1 0 1.1990 0.1575 10 1 1 1.1215 0.2032 10 1 2 0.8689 0.2143 10 1 3 0.5468 0.1710 10 1 4 0.2614 0.0842 10 1 5 0.0685 -0.0086 10 2 0 2.0243 -0.0564 10 2 1 1.8266 -0.0238 10 2 2 1.4120 0.0676 10 2 3 0.9175 0.1747 10 2 4 0.4885 0.2421 10 3 0 1.4499 -0.2186 10 3 1 1.1795 -0.2681 10 3 2 0.7576 -0.2321 10 3 3 0.3234 -0.1226 10 3 4 0.0136 0.0073 10 4 0 -0.2760 -0.1200 10 4 1 -0.4760 -0.2579 10 4 2 -0.6444 -0.3581 10 4 3 -0.7291 -0.3735 10 5 0 -0.9237 -0.0703 10 5 1 -0.8054 -0.1588 10 5 2 -0.6313 -0.2366 10 6 0 -0.0210 -0.0558 11 -9 0 0.1058 0.1875 11 -9 1 0.0420 0.1080 11 -8 0 -0.2049 -0.0885 11 -8 1 -0.2073 -0.0819 11 -8 2 -0.1935 -0.0551 11 -8 3 -0.1712 -0.0211 11 -7 0 0.1996 -0.1814 11 -7 1 0.2731 -0.1474 11 -7 2 0.3196 -0.1026 11 -7 3 0.3108 -0.0643 11 -7 4 0.2406 -0.0446 11 -6 0 0.1643 -0.0349 11 -6 1 0.2452 -0.0124 11 -6 2 0.3332 0.0208 11 -6 3 0.3826 0.0600 11 -6 4 0.3593 0.0966 11 -5 0 -0.8094 0.0965 11 -5 1 -0.6708 0.1130 11 -5 2 -0.4836 0.1238 11 -5 3 -0.3024 0.1334 11 -5 4 -0.1680 0.1454 11 -5 5 -0.0950 0.1583 11 -4 0 -0.7207 0.0092 11 -4 1 -0.5839 -0.0230 11 -4 2 -0.4942 -0.0576 11 -4 3 -0.4515 -0.0919 11 -4 4 -0.4200 -0.1200 11 -4 5 -0.3629 -0.1307 11 -3 0 -0.0448 -0.0895 11 -3 1 -0.0268 -0.0746 11 -3 2 -0.0593 -0.0428 11 -3 3 -0.1112 -0.0173 11 -3 4 -0.1345 -0.0185 11 -3 5 -0.0999 -0.0481 11 -2 0 -0.1259 0.0725 11 -2 1 -0.0942 0.1080 11 -2 2 0.0510 0.1450 11 -2 3 0.2353 0.1814 11 -2 4 0.3778 0.2024 11 -1 0 -0.1811 0.0118 11 -1 1 0.0163 -0.0792 11 -1 2 0.3290 -0.1634 11 -1 3 0.5925 -0.1921 11 -1 4 0.6720 -0.1489 11 0 0 0.2209 -0.0480 11 0 1 0.4089 -0.0938 11 0 2 0.5466 -0.1593 11 0 3 0.5604 -0.2179 11 0 4 0.4219 -0.2373 11 1 0 0.7094 0.2283 11 1 1 0.6130 0.3586 11 1 2 0.4310 0.4030 11 1 3 0.2277 0.3379 11 2 0 1.2046 0.1585 11 2 1 0.9306 0.2647 11 2 2 0.5930 0.3422 11 3 0 1.1898 -0.1552 11 3 1 0.9507 -0.2385 11 3 2 0.6102 -0.2340 11 4 0 0.2399 -0.2199 11 4 1 0.0964 -0.4145 12 -7 0 0.2016 -0.2486 12 -6 0 0.2336 -0.2167 12 -6 1 0.2632 -0.1259 12 -5 0 -0.5953 0.1635 12 -5 1 -0.4412 0.2351 12 -5 2 -0.2493 0.2510 12 -4 0 -0.5625 0.1919 12 -4 1 -0.3499 0.1106 12 -4 2 -0.2086 -0.0005 12 -3 0 0.3406 -0.1629 12 -3 1 0.3455 -0.1910 12 -3 2 0.2045 -0.1684 12 -2 0 0.1925 -0.0003 12 -2 1 0.0552 0.0864 12 -2 2 -0.0608 0.1785 12 -1 0 -0.3221 0.1330 12 -1 1 -0.2253 0.0222 12 -1 2 -0.0300 -0.0908 12 0 0 -0.0311 -0.0924 12 0 1 0.2210 -0.2327 12 1 0 0.2094 0.0461 12 1 1 0.2078 0.2022 12 2 0 0.2647 0.1751 0 0 0 0.0 0.0 ; _shelx_fab_checksum 73285 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 0.42780(4) 0.36758(3) 0.15287(3) 0.02468(14) Uani 1 1 d . . . . . F1 F -0.0705(2) 0.0272(2) 0.34347(19) 0.0586(6) Uani 1 1 d . . . . . F2 F -0.0779(3) -0.0851(2) 0.1984(3) 0.0770(9) Uani 1 1 d . . . . . F3 F -0.20393(19) 0.0509(2) 0.20562(19) 0.0519(5) Uani 1 1 d . . . . . O1 O 0.2017(2) 0.5305(2) 0.20934(18) 0.0356(5) Uani 1 1 d . . . . . O2 O 0.6713(2) 0.3865(2) 0.10798(18) 0.0389(5) Uani 1 1 d . . . . . O3 O 0.3635(3) 0.0969(2) 0.06602(19) 0.0474(6) Uani 1 1 d . . . . . N1 N 0.6858(2) 0.5556(2) 0.34431(18) 0.0258(4) Uani 1 1 d . . . . . N2 N 0.4671(2) 0.6656(2) 0.22400(18) 0.0273(5) Uani 1 1 d . . . . . N3 N 0.2845(2) 0.3886(2) 0.03561(19) 0.0317(5) Uani 1 1 d . . . . . C1 C 0.3121(3) 0.4980(2) 0.2392(2) 0.0273(5) Uani 1 1 d . . . . . C2 C 0.3391(3) 0.3847(2) 0.2627(2) 0.0269(5) Uani 1 1 d . . . . . C3 C 0.4843(3) 0.3909(2) 0.3052(2) 0.0248(5) Uani 1 1 d . . . . . C4 C 0.5491(3) 0.5036(2) 0.30251(19) 0.0237(5) Uani 1 1 d . . . . . C5 C 0.4444(3) 0.5587(2) 0.2473(2) 0.0250(5) Uani 1 1 d . . . . . C6 C 0.2339(3) 0.2936(3) 0.2618(2) 0.0289(5) Uani 1 1 d . . . . . C7 C 0.1102(3) 0.3242(3) 0.2600(3) 0.0353(6) Uani 1 1 d . . . . . H7 H 0.095301 0.404661 0.261199 0.042 Uiso 1 1 calc R U . . . C8 C 0.0086(3) 0.2400(3) 0.2566(3) 0.0398(7) Uani 1 1 d . . . . . H8 H -0.075491 0.262392 0.254053 0.048 Uiso 1 1 calc R U . . . C9 C 0.0298(3) 0.1223(3) 0.2570(2) 0.0351(6) Uani 1 1 d . . . . . C10 C 0.1527(3) 0.0904(3) 0.2613(2) 0.0346(6) Uani 1 1 d . . . . . H10 H 0.168125 0.010865 0.262991 0.042 Uiso 1 1 calc R U . . . C11 C 0.2538(3) 0.1748(3) 0.2633(2) 0.0341(6) Uani 1 1 d . . . . . H11 H 0.337661 0.151818 0.265738 0.041 Uiso 1 1 calc R U . . . C12 C -0.0795(3) 0.0299(3) 0.2513(3) 0.0420(7) Uani 1 1 d . . . . . C13 C 0.5499(3) 0.3132(2) 0.3672(2) 0.0242(5) Uani 1 1 d . . . . . C14 C 0.6093(3) 0.2166(2) 0.3298(2) 0.0267(5) Uani 1 1 d . . . . . H14 H 0.612629 0.201460 0.263697 0.032 Uiso 1 1 calc R U . . . C15 C 0.6633(3) 0.1426(2) 0.3877(2) 0.0291(5) Uani 1 1 d . . . . . H15 H 0.703918 0.077655 0.361657 0.035 Uiso 1 1 calc R U . . . C16 C 0.6578(3) 0.1640(3) 0.4836(2) 0.0311(6) Uani 1 1 d . . . . . C17 C 0.5988(3) 0.2585(3) 0.5223(2) 0.0331(6) Uani 1 1 d . . . . . H17 H 0.594868 0.272454 0.588141 0.040 Uiso 1 1 calc R U . . . C18 C 0.5454(3) 0.3329(3) 0.4641(2) 0.0304(6) Uani 1 1 d . . . . . H18 H 0.505304 0.397984 0.490807 0.036 Uiso 1 1 calc R U . . . C19 C 0.7169(3) 0.0848(3) 0.5465(3) 0.0392(7) Uani 1 1 d D . . . . C20 C 0.7878(3) 0.4811(2) 0.3733(2) 0.0276(5) Uani 1 1 d . . . . . H20A H 0.757731 0.397203 0.321458 0.033 Uiso 1 1 calc R U . . . H20B H 0.798683 0.473776 0.441140 0.033 Uiso 1 1 calc R U . . . C21 C 0.9226(3) 0.5407(3) 0.3792(2) 0.0313(6) Uani 1 1 d . . . . . H21A H 0.991922 0.491896 0.402435 0.038 Uiso 1 1 calc R U . . . H21B H 0.913289 0.539753 0.309403 0.038 Uiso 1 1 calc R U . . . C22 C 0.9700(3) 0.6730(3) 0.4530(3) 0.0368(6) Uani 1 1 d . . . . . H22A H 1.053846 0.710835 0.450404 0.044 Uiso 1 1 calc R U . . . H22B H 0.990464 0.674079 0.524528 0.044 Uiso 1 1 calc R U . . . C23 C 0.8589(3) 0.7465(3) 0.4220(3) 0.0376(7) Uani 1 1 d . . . . . H23A H 0.886577 0.830750 0.473060 0.045 Uiso 1 1 calc R U . . . H23B H 0.846469 0.753487 0.353728 0.045 Uiso 1 1 calc R U . . . C24 C 0.7253(3) 0.6839(2) 0.4166(2) 0.0320(6) Uani 1 1 d . . . . . H24A H 0.735206 0.683773 0.486215 0.038 Uiso 1 1 calc R U . . . H24B H 0.653589 0.730406 0.392914 0.038 Uiso 1 1 calc R U . . . C25 C 0.5605(3) 0.6668(2) 0.1713(2) 0.0291(5) Uani 1 1 d . . . . . H25A H 0.513006 0.615852 0.097524 0.035 Uiso 1 1 calc R U . . . H25B H 0.638134 0.629794 0.202410 0.035 Uiso 1 1 calc R U . . . C26 C 0.6128(3) 0.7968(3) 0.1794(2) 0.0332(6) Uani 1 1 d . . . . . H26A H 0.669720 0.793420 0.138783 0.040 Uiso 1 1 calc R U . . . H26B H 0.670277 0.844783 0.252442 0.040 Uiso 1 1 calc R U . . . C27 C 0.4970(3) 0.8617(3) 0.1397(3) 0.0350(6) Uani 1 1 d . . . . . H27A H 0.533615 0.949069 0.153410 0.042 Uiso 1 1 calc R U . . . H27B H 0.447530 0.821823 0.064131 0.042 Uiso 1 1 calc R U . . . C28 C 0.4010(3) 0.8548(3) 0.1936(3) 0.0343(6) Uani 1 1 d . . . . . H28A H 0.322633 0.891908 0.164273 0.041 Uiso 1 1 calc R U . . . H28B H 0.448347 0.903070 0.267986 0.041 Uiso 1 1 calc R U . . . C29 C 0.3503(3) 0.7217(3) 0.1813(2) 0.0315(6) Uani 1 1 d . . . . . H29A H 0.289315 0.720144 0.218274 0.038 Uiso 1 1 calc R U . . . H29B H 0.298330 0.673927 0.107282 0.038 Uiso 1 1 calc R U . . . C30 C 0.5717(3) 0.3790(3) 0.1203(2) 0.0301(6) Uani 1 1 d . . . . . C31 C 0.3887(3) 0.2023(3) 0.1002(2) 0.0337(6) Uani 1 1 d . . . . . C32 C 0.1926(3) 0.3996(3) -0.0277(3) 0.0418(7) Uani 1 1 d . . . . . C33 C 0.0741(4) 0.4122(6) -0.1096(4) 0.0738(14) Uani 1 1 d . . . . . H33A H 0.079410 0.374512 -0.176608 0.111 Uiso 1 1 calc R U . . . H33B H 0.071625 0.499784 -0.098135 0.111 Uiso 1 1 calc R U . . . H33C H -0.008332 0.370684 -0.108987 0.111 Uiso 1 1 calc R U . . . F4 F 0.8271(6) 0.1522(5) 0.6350(4) 0.0401(13) Uani 0.387(3) 1 d D U P A 1 F5 F 0.7541(8) -0.0092(6) 0.4999(5) 0.0503(14) Uani 0.387(3) 1 d D U P A 1 F6 F 0.6298(5) 0.0446(5) 0.5846(5) 0.0314(10) Uani 0.387(3) 1 d D U P A 1 F4A F 0.8251(6) 0.0429(6) 0.5265(5) 0.0331(13) Uani 0.304(3) 1 d D U P A 2 F5A F 0.6353(8) -0.0058(8) 0.5371(8) 0.066(2) Uani 0.304(3) 1 d D U P A 2 F6A F 0.7823(9) 0.1518(8) 0.6497(5) 0.052(2) Uani 0.304(3) 1 d D U P A 2 F4B F 0.6727(9) 0.0876(8) 0.6203(6) 0.0485(19) Uani 0.309(3) 1 d D U P A 3 F5B F 0.8438(7) 0.0968(9) 0.5806(8) 0.063(2) Uani 0.309(3) 1 d D U P A 3 F6B F 0.6702(8) -0.0400(5) 0.4823(5) 0.0406(14) Uani 0.309(3) 1 d D U P A 3 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 0.0212(2) 0.0236(2) 0.0303(2) 0.01335(16) 0.00770(17) 0.00581(15) F1 0.0431(12) 0.0720(15) 0.0718(15) 0.0416(12) 0.0236(11) -0.0007(10) F2 0.0597(15) 0.0311(10) 0.144(3) 0.0042(13) 0.0664(17) -0.0052(9) F3 0.0279(9) 0.0542(12) 0.0754(14) 0.0301(11) 0.0174(9) -0.0001(8) O1 0.0235(10) 0.0380(11) 0.0537(13) 0.0274(10) 0.0139(9) 0.0126(8) O2 0.0305(11) 0.0454(12) 0.0444(12) 0.0147(10) 0.0185(9) 0.0090(9) O3 0.0584(15) 0.0248(11) 0.0506(14) 0.0116(9) 0.0130(12) 0.0051(10) N1 0.0208(10) 0.0221(10) 0.0344(11) 0.0124(9) 0.0077(9) 0.0069(8) N2 0.0248(11) 0.0243(10) 0.0375(12) 0.0176(9) 0.0114(9) 0.0080(8) N3 0.0291(12) 0.0327(12) 0.0343(12) 0.0155(10) 0.0096(10) 0.0081(9) C1 0.0214(12) 0.0284(13) 0.0356(13) 0.0169(11) 0.0099(10) 0.0072(10) C2 0.0236(13) 0.0257(12) 0.0359(14) 0.0163(10) 0.0117(11) 0.0064(10) C3 0.0227(12) 0.0251(12) 0.0291(12) 0.0135(10) 0.0090(10) 0.0070(9) C4 0.0224(12) 0.0241(12) 0.0261(12) 0.0108(9) 0.0089(10) 0.0070(9) C5 0.0227(12) 0.0222(11) 0.0323(13) 0.0133(10) 0.0094(10) 0.0068(9) C6 0.0232(13) 0.0289(13) 0.0363(14) 0.0150(11) 0.0103(11) 0.0058(10) C7 0.0303(15) 0.0289(13) 0.0526(17) 0.0171(12) 0.0200(13) 0.0069(11) C8 0.0298(15) 0.0337(15) 0.063(2) 0.0163(14) 0.0255(14) 0.0072(12) C9 0.0287(15) 0.0321(14) 0.0458(16) 0.0135(12) 0.0167(13) 0.0003(11) C10 0.0283(14) 0.0316(14) 0.0476(16) 0.0199(12) 0.0140(12) 0.0054(11) C11 0.0265(14) 0.0318(14) 0.0493(17) 0.0217(12) 0.0144(12) 0.0061(11) C12 0.0301(16) 0.0365(16) 0.063(2) 0.0164(15) 0.0227(15) 0.0049(12) C13 0.0204(12) 0.0219(11) 0.0333(13) 0.0148(10) 0.0093(10) 0.0053(9) C14 0.0241(12) 0.0270(12) 0.0325(13) 0.0146(10) 0.0111(10) 0.0073(10) C15 0.0248(13) 0.0241(12) 0.0412(15) 0.0150(11) 0.0123(11) 0.0093(10) C16 0.0331(14) 0.0253(12) 0.0403(15) 0.0181(11) 0.0142(12) 0.0099(11) C17 0.0404(16) 0.0329(14) 0.0350(14) 0.0193(12) 0.0174(12) 0.0153(12) C18 0.0325(14) 0.0262(13) 0.0387(14) 0.0167(11) 0.0151(12) 0.0118(11) C19 0.0448(18) 0.0376(16) 0.0501(18) 0.0276(14) 0.0231(15) 0.0189(13) C20 0.0211(12) 0.0262(12) 0.0363(14) 0.0149(10) 0.0082(10) 0.0073(10) C21 0.0233(13) 0.0324(14) 0.0412(15) 0.0181(12) 0.0112(11) 0.0075(10) C22 0.0233(14) 0.0320(14) 0.0506(17) 0.0170(13) 0.0073(12) 0.0027(11) C23 0.0276(15) 0.0253(13) 0.0547(18) 0.0150(12) 0.0092(13) 0.0041(11) C24 0.0273(14) 0.0232(12) 0.0397(15) 0.0071(11) 0.0089(11) 0.0058(10) C25 0.0260(13) 0.0266(12) 0.0396(14) 0.0169(11) 0.0134(11) 0.0076(10) C26 0.0313(14) 0.0273(13) 0.0455(16) 0.0175(12) 0.0158(12) 0.0057(11) C27 0.0352(15) 0.0252(13) 0.0462(16) 0.0191(12) 0.0122(13) 0.0066(11) C28 0.0329(15) 0.0254(13) 0.0492(17) 0.0202(12) 0.0140(13) 0.0119(11) C29 0.0270(14) 0.0266(13) 0.0445(15) 0.0200(11) 0.0109(12) 0.0098(10) C30 0.0318(14) 0.0278(13) 0.0297(13) 0.0118(10) 0.0089(11) 0.0062(10) C31 0.0339(15) 0.0336(15) 0.0319(14) 0.0148(11) 0.0080(12) 0.0065(11) C32 0.0331(16) 0.0544(19) 0.0425(17) 0.0249(15) 0.0124(14) 0.0134(14) C33 0.037(2) 0.126(4) 0.072(3) 0.065(3) 0.010(2) 0.028(2) F4 0.0349(19) 0.0423(19) 0.043(2) 0.0269(16) 0.0053(15) 0.0068(15) F5 0.056(2) 0.045(2) 0.051(2) 0.0183(15) 0.0171(15) 0.0243(17) F6 0.0329(17) 0.0319(17) 0.0335(18) 0.0216(14) 0.0103(14) 0.0007(13) F4A 0.033(2) 0.0328(19) 0.0340(19) 0.0150(15) 0.0088(15) 0.0182(16) F5A 0.069(3) 0.062(3) 0.069(3) 0.032(2) 0.0208(19) 0.0102(18) F6A 0.057(3) 0.053(3) 0.048(3) 0.0201(18) 0.0195(18) 0.0212(19) F4B 0.055(3) 0.047(2) 0.044(2) 0.0182(17) 0.0168(17) 0.0163(18) F5B 0.061(3) 0.059(3) 0.065(3) 0.0292(19) 0.0168(18) 0.0106(18) F6B 0.048(2) 0.0283(19) 0.043(2) 0.0191(16) 0.0088(16) 0.0120(16) 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' F F 0.0727 0.0534 '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' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -6 -2 2 0.0554 1 -7 3 0.0877 7 1 -1 0.0779 1 7 -3 0.0637 0 1 8 0.0343 -1 -1 -7 0.0255 1 -1 -8 0.0332 -7 -1 4 0.0674 -1 -5 -3 0.0528 2 -5 -4 0.0821 0 2 -9 0.0403 1 -2 9 0.0553 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 C30 Fe1 C31 93.35(13) . . ? C30 Fe1 N3 102.66(12) . . ? C31 Fe1 N3 94.12(12) . . ? C30 Fe1 C3 111.11(12) . . ? C31 Fe1 C3 100.02(12) . . ? N3 Fe1 C3 142.29(10) . . ? C30 Fe1 C2 151.49(12) . . ? C31 Fe1 C2 96.86(12) . . ? N3 Fe1 C2 103.06(10) . . ? C3 Fe1 C2 40.85(10) . . ? C30 Fe1 C4 88.08(11) . . ? C31 Fe1 C4 135.74(11) . . ? N3 Fe1 C4 128.67(10) . . ? C3 Fe1 C4 40.16(10) . . ? C2 Fe1 C4 66.18(10) . . ? C30 Fe1 C5 102.27(11) . . ? C31 Fe1 C5 162.38(12) . . ? N3 Fe1 C5 90.39(10) . . ? C3 Fe1 C5 66.89(10) . . ? C2 Fe1 C5 65.52(10) . . ? C4 Fe1 C5 38.55(9) . . ? C30 Fe1 C1 139.53(11) . . ? C31 Fe1 C1 127.05(12) . . ? N3 Fe1 C1 79.18(10) . . ? C3 Fe1 C1 64.37(10) . . ? C2 Fe1 C1 37.34(9) . . ? C4 Fe1 C1 62.45(9) . . ? C5 Fe1 C1 37.50(9) . . ? C4 N1 C20 120.3(2) . . ? C4 N1 C24 116.0(2) . . ? C20 N1 C24 113.0(2) . . ? C5 N2 C25 115.9(2) . . ? C5 N2 C29 118.7(2) . . ? C25 N2 C29 111.4(2) . . ? C32 N3 Fe1 173.0(3) . . ? O1 C1 C2 127.9(2) . . ? O1 C1 C5 127.2(2) . . ? C2 C1 C5 104.6(2) . . ? O1 C1 Fe1 133.7(2) . . ? C2 C1 Fe1 61.09(14) . . ? C5 C1 Fe1 64.21(14) . . ? C3 C2 C1 109.0(2) . . ? C3 C2 C6 126.6(2) . . ? C1 C2 C6 123.3(2) . . ? C3 C2 Fe1 66.22(14) . . ? C1 C2 Fe1 81.57(16) . . ? C6 C2 Fe1 127.7(2) . . ? C4 C3 C2 107.8(2) . . ? C4 C3 C13 126.8(2) . . ? C2 C3 C13 123.2(2) . . ? C4 C3 Fe1 75.10(15) . . ? C2 C3 Fe1 72.93(15) . . ? C13 C3 Fe1 131.17(19) . . ? N1 C4 C5 123.3(2) . . ? N1 C4 C3 128.8(2) . . ? C5 C4 C3 107.9(2) . . ? N1 C4 Fe1 129.28(18) . . ? C5 C4 Fe1 72.00(15) . . ? C3 C4 Fe1 64.73(14) . . ? N2 C5 C4 125.0(2) . . ? N2 C5 C1 125.8(2) . . ? C4 C5 C1 108.1(2) . . ? N2 C5 Fe1 127.27(19) . . ? C4 C5 Fe1 69.45(14) . . ? C1 C5 Fe1 78.29(15) . . ? C7 C6 C11 117.6(3) . . ? C7 C6 C2 120.2(2) . . ? C11 C6 C2 122.2(2) . . ? C8 C7 C6 121.5(3) . . ? C7 C8 C9 120.0(3) . . ? C10 C9 C8 119.7(3) . . ? C10 C9 C12 119.7(3) . . ? C8 C9 C12 120.6(3) . . ? C9 C10 C11 120.1(3) . . ? C10 C11 C6 121.1(3) . . ? F1 C12 F2 105.6(3) . . ? F1 C12 F3 105.7(3) . . ? F2 C12 F3 106.8(3) . . ? F1 C12 C9 113.4(3) . . ? F2 C12 C9 112.2(3) . . ? F3 C12 C9 112.6(3) . . ? C18 C13 C14 118.3(2) . . ? C18 C13 C3 118.9(2) . . ? C14 C13 C3 122.7(2) . . ? C15 C14 C13 121.0(3) . . ? C16 C15 C14 119.6(2) . . ? C15 C16 C17 120.7(2) . . ? C15 C16 C19 119.7(2) . . ? C17 C16 C19 119.6(3) . . ? C16 C17 C18 119.5(3) . . ? C17 C18 C13 120.9(3) . . ? F5B C19 F4B 110.7(6) . . ? F5 C19 F6 108.0(4) . . ? F5A C19 F6A 108.4(6) . . ? F5 C19 F4 107.5(5) . . ? F6 C19 F4 102.5(4) . . ? F5A C19 F4A 108.7(6) . . ? F6A C19 F4A 99.7(5) . . ? F5B C19 F6B 103.6(5) . . ? F4B C19 F6B 102.1(5) . . ? F5B C19 C16 116.0(4) . . ? F5A C19 C16 115.7(5) . . ? F5 C19 C16 115.3(4) . . ? F4B C19 C16 114.4(4) . . ? F6 C19 C16 111.6(3) . . ? F6A C19 C16 112.0(4) . . ? F4 C19 C16 111.1(3) . . ? F4A C19 C16 111.1(3) . . ? F6B C19 C16 108.4(3) . . ? N1 C20 C21 109.9(2) . . ? C22 C21 C20 112.2(2) . . ? C21 C22 C23 109.4(2) . . ? C24 C23 C22 110.8(2) . . ? N1 C24 C23 110.2(2) . . ? N2 C25 C26 111.6(2) . . ? C25 C26 C27 111.6(2) . . ? C28 C27 C26 109.4(2) . . ? C27 C28 C29 111.6(2) . . ? N2 C29 C28 109.5(2) . . ? O2 C30 Fe1 173.9(3) . . ? O3 C31 Fe1 179.6(3) . . ? N3 C32 C33 179.4(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 C30 1.781(3) . ? Fe1 C31 1.795(3) . ? Fe1 N3 1.951(2) . ? Fe1 C3 2.027(3) . ? Fe1 C2 2.118(3) . ? Fe1 C4 2.166(3) . ? Fe1 C5 2.200(3) . ? Fe1 C1 2.393(3) . ? F1 C12 1.330(4) . ? F2 C12 1.338(4) . ? F3 C12 1.343(4) . ? O1 C1 1.238(3) . ? O2 C30 1.149(4) . ? O3 C31 1.145(4) . ? N1 C4 1.386(3) . ? N1 C20 1.461(3) . ? N1 C24 1.480(3) . ? N2 C5 1.396(3) . ? N2 C25 1.471(4) . ? N2 C29 1.477(3) . ? N3 C32 1.136(4) . ? C1 C2 1.467(3) . ? C1 C5 1.488(4) . ? C2 C3 1.449(4) . ? C2 C6 1.480(4) . ? C3 C4 1.446(3) . ? C3 C13 1.493(3) . ? C4 C5 1.442(3) . ? C6 C7 1.395(4) . ? C6 C11 1.407(4) . ? C7 C8 1.384(4) . ? C8 C9 1.393(4) . ? C9 C10 1.383(4) . ? C9 C12 1.491(4) . ? C10 C11 1.391(4) . ? C13 C18 1.395(4) . ? C13 C14 1.399(4) . ? C14 C15 1.387(4) . ? C15 C16 1.381(4) . ? C16 C17 1.386(4) . ? C16 C19 1.497(4) . ? C17 C18 1.391(4) . ? C19 F5B 1.257(7) . ? C19 F5A 1.257(7) . ? C19 F5 1.281(6) . ? C19 F4B 1.322(7) . ? C19 F6 1.364(5) . ? C19 F6A 1.372(7) . ? C19 F4 1.376(6) . ? C19 F4A 1.384(6) . ? C19 F6B 1.414(6) . ? C20 C21 1.521(4) . ? C21 C22 1.521(4) . ? C22 C23 1.529(4) . ? C23 C24 1.525(4) . ? C25 C26 1.519(4) . ? C26 C27 1.524(4) . ? C27 C28 1.516(4) . ? C28 C29 1.528(4) . ? C32 C33 1.459(5) . ? 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 O1 C1 C2 C3 -174.1(3) . . . . ? C5 C1 C2 C3 12.2(3) . . . . ? Fe1 C1 C2 C3 61.16(18) . . . . ? O1 C1 C2 C6 -5.3(5) . . . . ? C5 C1 C2 C6 -178.9(2) . . . . ? Fe1 C1 C2 C6 -130.0(3) . . . . ? O1 C1 C2 Fe1 124.7(3) . . . . ? C5 C1 C2 Fe1 -48.93(19) . . . . ? C1 C2 C3 C4 -3.6(3) . . . . ? C6 C2 C3 C4 -172.0(3) . . . . ? Fe1 C2 C3 C4 67.60(18) . . . . ? C1 C2 C3 C13 160.3(2) . . . . ? C6 C2 C3 C13 -8.1(4) . . . . ? Fe1 C2 C3 C13 -128.5(3) . . . . ? C1 C2 C3 Fe1 -71.2(2) . . . . ? C6 C2 C3 Fe1 120.4(3) . . . . ? C20 N1 C4 C5 -162.9(2) . . . . ? C24 N1 C4 C5 55.3(3) . . . . ? C20 N1 C4 C3 17.7(4) . . . . ? C24 N1 C4 C3 -124.2(3) . . . . ? C20 N1 C4 Fe1 -69.5(3) . . . . ? C24 N1 C4 Fe1 148.7(2) . . . . ? C2 C3 C4 N1 172.6(3) . . . . ? C13 C3 C4 N1 9.4(4) . . . . ? Fe1 C3 C4 N1 -121.3(3) . . . . ? C2 C3 C4 C5 -6.9(3) . . . . ? C13 C3 C4 C5 -170.1(2) . . . . ? Fe1 C3 C4 C5 59.25(18) . . . . ? C2 C3 C4 Fe1 -66.14(18) . . . . ? C13 C3 C4 Fe1 130.7(3) . . . . ? C25 N2 C5 C4 52.6(4) . . . . ? C29 N2 C5 C4 -170.7(3) . . . . ? C25 N2 C5 C1 -140.7(3) . . . . ? C29 N2 C5 C1 -4.0(4) . . . . ? C25 N2 C5 Fe1 -37.2(3) . . . . ? C29 N2 C5 Fe1 99.6(3) . . . . ? N1 C4 C5 N2 3.9(4) . . . . ? C3 C4 C5 N2 -176.6(2) . . . . ? Fe1 C4 C5 N2 -121.8(3) . . . . ? N1 C4 C5 C1 -164.8(2) . . . . ? C3 C4 C5 C1 14.7(3) . . . . ? Fe1 C4 C5 C1 69.49(18) . . . . ? N1 C4 C5 Fe1 125.7(2) . . . . ? C3 C4 C5 Fe1 -54.80(17) . . . . ? O1 C1 C5 N2 1.2(5) . . . . ? C2 C1 C5 N2 174.9(3) . . . . ? Fe1 C1 C5 N2 127.8(3) . . . . ? O1 C1 C5 C4 169.8(3) . . . . ? C2 C1 C5 C4 -16.5(3) . . . . ? Fe1 C1 C5 C4 -63.59(17) . . . . ? O1 C1 C5 Fe1 -126.6(3) . . . . ? C2 C1 C5 Fe1 47.14(19) . . . . ? C3 C2 C6 C7 153.0(3) . . . . ? C1 C2 C6 C7 -13.8(4) . . . . ? Fe1 C2 C6 C7 -120.5(3) . . . . ? C3 C2 C6 C11 -26.6(4) . . . . ? C1 C2 C6 C11 166.5(3) . . . . ? Fe1 C2 C6 C11 59.9(4) . . . . ? C11 C6 C7 C8 -2.0(5) . . . . ? C2 C6 C7 C8 178.4(3) . . . . ? C6 C7 C8 C9 1.3(5) . . . . ? C7 C8 C9 C10 0.4(5) . . . . ? C7 C8 C9 C12 -178.8(3) . . . . ? C8 C9 C10 C11 -1.3(5) . . . . ? C12 C9 C10 C11 178.0(3) . . . . ? C9 C10 C11 C6 0.5(5) . . . . ? C7 C6 C11 C10 1.1(5) . . . . ? C2 C6 C11 C10 -179.3(3) . . . . ? C10 C9 C12 F1 86.1(4) . . . . ? C8 C9 C12 F1 -94.6(4) . . . . ? C10 C9 C12 F2 -33.4(5) . . . . ? C8 C9 C12 F2 145.8(4) . . . . ? C10 C9 C12 F3 -153.9(3) . . . . ? C8 C9 C12 F3 25.3(5) . . . . ? C4 C3 C13 C18 93.8(3) . . . . ? C2 C3 C13 C18 -67.0(4) . . . . ? Fe1 C3 C13 C18 -163.1(2) . . . . ? C4 C3 C13 C14 -89.9(3) . . . . ? C2 C3 C13 C14 109.3(3) . . . . ? Fe1 C3 C13 C14 13.3(4) . . . . ? C18 C13 C14 C15 -0.5(4) . . . . ? C3 C13 C14 C15 -176.8(2) . . . . ? C13 C14 C15 C16 0.4(4) . . . . ? C14 C15 C16 C17 0.0(4) . . . . ? C14 C15 C16 C19 -179.6(3) . . . . ? C15 C16 C17 C18 -0.4(5) . . . . ? C19 C16 C17 C18 179.2(3) . . . . ? C16 C17 C18 C13 0.3(5) . . . . ? C14 C13 C18 C17 0.1(4) . . . . ? C3 C13 C18 C17 176.6(3) . . . . ? C15 C16 C19 F5B 68.2(7) . . . . ? C17 C16 C19 F5B -111.4(6) . . . . ? C15 C16 C19 F5A -94.3(7) . . . . ? C17 C16 C19 F5A 86.2(7) . . . . ? C15 C16 C19 F5 -8.7(6) . . . . ? C17 C16 C19 F5 171.8(5) . . . . ? C15 C16 C19 F4B -161.0(5) . . . . ? C17 C16 C19 F4B 19.4(6) . . . . ? C15 C16 C19 F6 -132.3(4) . . . . ? C17 C16 C19 F6 48.1(5) . . . . ? C15 C16 C19 F6A 140.8(5) . . . . ? C17 C16 C19 F6A -38.8(6) . . . . ? C15 C16 C19 F4 114.0(4) . . . . ? C17 C16 C19 F4 -65.6(5) . . . . ? C15 C16 C19 F4A 30.2(5) . . . . ? C17 C16 C19 F4A -149.3(4) . . . . ? C15 C16 C19 F6B -47.8(5) . . . . ? C17 C16 C19 F6B 132.6(4) . . . . ? C4 N1 C20 C21 159.4(2) . . . . ? C24 N1 C20 C21 -57.6(3) . . . . ? N1 C20 C21 C22 55.9(3) . . . . ? C20 C21 C22 C23 -54.8(3) . . . . ? C21 C22 C23 C24 54.7(4) . . . . ? C4 N1 C24 C23 -156.9(2) . . . . ? C20 N1 C24 C23 58.5(3) . . . . ? C22 C23 C24 N1 -56.4(3) . . . . ? C5 N2 C25 C26 -162.1(2) . . . . ? C29 N2 C25 C26 58.1(3) . . . . ? N2 C25 C26 C27 -54.8(3) . . . . ? C25 C26 C27 C28 52.8(3) . . . . ? C26 C27 C28 C29 -55.1(3) . . . . ? C5 N2 C29 C28 162.3(2) . . . . ? C25 N2 C29 C28 -59.1(3) . . . . ? C27 C28 C29 N2 58.4(3) . . . . ? 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 -6.4191 -1.6544 1.7315 -0.0208 0.1100 0.9937 0.6140 -7.4678 3.2212 -0.1822 0.9802 0.0776 6.5454 1.0765 -1.4944 0.0065 -0.0328 -0.9994 0.8275 7.3476 -3.3917 0.1750 -0.9410 -0.2896 0.2200 0.7022 7.9643 -0.9301 -0.1731 -0.3239 -1.0723 -0.7762 -7.3824 0.8834 0.1645 0.4388 0.5249 -0.6289 -8.3708 0.9591 0.1784 0.2199 -6.8730 -0.6147 4.4792 -0.3518 -0.0648 0.9338 -1.3047 -5.0220 -3.2356 0.5281 0.6894 0.4958 1.7011 -5.3592 -4.3883 0.6062 0.7909 0.0834 0.3836 2.4497 -9.0802 0.9614 -0.2304 0.1502 0.5338 -2.2629 8.6174 -0.9326 0.2236 -0.2832 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 0.000 0.000 0.000 128.7 20.0 '1 MeCN'