#------------------------------------------------------------------------------ #$Date: 2021-10-03 23:32:55 +0300 (Sun, 03 Oct 2021) $ #$Revision: 269495 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/90/4519073.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_4519073 loop_ _publ_author_name 'Khade, Rahul L.' 'Abucayon, Erwin G.' 'Powell, Douglas R.' 'Richter-Addo, George B.' 'Zhang, Yong' _publ_section_title ; Insights into the Observed trans-Bond Length Variations upon NO Binding to Ferric and Ferrous Porphyrins with Neutral Axial Ligands ; _journal_issue 38 _journal_name_full 'ACS Omega' _journal_page_first 24777 _journal_page_last 24787 _journal_paper_doi 10.1021/acsomega.1c03610 _journal_volume 6 _journal_year 2021 _chemical_formula_moiety 'C40 H50 Fe N7 O, F6 Sb' _chemical_formula_sum 'C40 H50 F6 Fe N7 O Sb' _chemical_formula_weight 936.47 _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 mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 63.727(2) _cell_angle_beta 74.453(2) _cell_angle_gamma 78.923(2) _cell_formula_units_Z 2 _cell_length_a 10.5327(13) _cell_length_b 13.9466(18) _cell_length_c 15.712(2) _cell_measurement_reflns_used 4020 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 29.88 _cell_measurement_theta_min 2.48 _cell_volume 1986.6(4) _computing_cell_refinement 'SAINT (Bruker, 2007)' _computing_data_collection 'APEX2 (Bruker, 2007)' _computing_data_reduction 'SAINT (Bruker, 2007)' _computing_molecular_graphics 'Mercury (CCDC, 2018)' _computing_publication_material 'SHELXL-2014/7 (Sheldrick, 2015b)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2015b)' _computing_structure_solution 'SHELXT (Sheldrick, 2015a)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measurement_device_type 'Bruker APEX CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0486 _diffrn_reflns_av_unetI/netI 0.0588 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 22523 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.911 _diffrn_reflns_theta_min 1.478 _exptl_absorpt_coefficient_mu 1.115 _exptl_absorpt_correction_T_max 0.564 _exptl_absorpt_correction_T_min 0.377 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS 2012/1 Krause, L., Herbst-Irmer, R., Sheldrick, G. M. & Stalke, D. (2015), J. Appl.Cryst. 48, 3-10. ; _exptl_crystal_colour red _exptl_crystal_density_diffrn 1.565 _exptl_crystal_description block _exptl_crystal_F_000 956 _exptl_crystal_size_max 0.180 _exptl_crystal_size_mid 0.180 _exptl_crystal_size_min 0.110 _refine_diff_density_max 1.565 _refine_diff_density_min -0.862 _refine_diff_density_rms 0.139 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 638 _refine_ls_number_reflns 22523 _refine_ls_number_restraints 1240 _refine_ls_restrained_S_all 7.876 _refine_ls_R_factor_all 0.0771 _refine_ls_R_factor_gt 0.0489 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0840P)^2^+0.2000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1284 _refine_ls_wR_factor_ref 0.1473 _reflns_Friedel_coverage 0.000 _reflns_number_gt 15942 _reflns_number_total 22523 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ao1c03610_si_003.cif _cod_data_source_block 15070b _cod_database_code 4519073 _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 0.824 _shelx_estimated_absorpt_t_max 0.887 _shelx_res_file ; TITL 15070b in P-1 15070b.res created by SHELXL-2018/3 at 10:23:48 on 15-Apr-2021 CELL 0.71073 10.5327 13.9466 15.712 63.727 74.453 78.923 ZERR 2.00 0.0013 0.0018 0.002 0.002 0.002 0.002 LATT 1 SFAC C H N O F FE SB UNIT 80 100 14 2 12 2 2 TEMP -173.15 SIZE 0.11 0.18 0.18 ACTA CONF WPDB -2 EQIV $1 x, y-1, z EQIV $2 -x+1, -y+1, -z+2 EQIV $3 -x+2, -y+1, -z+2 HTAB N6 F1_$1 HTAB C5 F5_$2 HTAB C5 F2'_$2 HTAB C10 F6'_$1 HTAB C37 F1_$1 HTAB C37 F1'_$1 HTAB C37 F1"_$1 HTAB C40 F2_$3 HTAB C40 F2"_$3 HTAB C40 F6"_$3 HTAB sadi 0.004 sb1 f1 sb1 f2 sb1 f3 sb1 f4 sb1 f5 sb1 f6 sadi 0.004 sb1' f1' sb1' f2' sb1' f3' sb1' f4' sb1' f5' sb1' f6' sb1 f1 sadi 0.004 sb1" f1" sb1' f2' sb1' f3' sb1' f4' sb1' f5' sb1' f6' sb1 f1 sadi 0.007 f1 f2 f1 f3 f1 f5 f1 f6 f2 f3 f2 f4 sadi 0.007 f2 f6 f3 f4 f3 f5 f4 f5 f4 f6 f5 f6 f1 f2 sadi 0.007 f1' f2' f1' f3' f1' f5' f1' f6' f2' f3' f2' f4' f1 f2 sadi 0.007 f2' f6' f3' f4' f3' f5' f4' f5' f4' f6' f5' f6' f1 f2 sadi 0.007 f1" f2" f1" f3" f1" f5" f1" f6" f2" f3" f2" f4" f1 f2 sadi 0.007 f2" f6" f3" f4" f3" f5" f4" f5" f4" f6" f5" f6" f1 f2 rigu 0.004 sb1 f1 f2 f3 f4 f5 f6 rigu 0.004 sb1' f1' f2' f3' f4' f5' f6' rigu 0.004 sb1" f1" f2" f3" f4" f5" f6" simu 0.004 sb1 > f6" isor 0.003 f3' sump 1 0.00001 1 2 1 3 1 4 L.S. 10 4 BOND $H FMAP 2 PLAN 20 WGHT 0.084000 0.200000 BASF 0.20200 FVAR 0.25137 0.95947 0.02298 0.01749 FE1 6 0.601504 0.383696 0.696685 11.00000 0.01933 0.00975 = 0.01377 -0.00393 -0.00278 -0.00287 O1 4 0.405447 0.444093 0.589985 11.00000 0.03269 0.06192 = 0.03760 -0.00953 -0.01833 -0.00533 N1 3 0.484964 0.431699 0.797394 11.00000 0.02115 0.01088 = 0.01559 -0.00497 -0.00238 -0.00301 N2 3 0.536764 0.236597 0.773817 11.00000 0.01996 0.01073 = 0.01374 -0.00405 -0.00054 -0.00407 N3 3 0.725416 0.333202 0.600024 11.00000 0.02037 0.01163 = 0.01499 -0.00452 -0.00138 -0.00336 N4 3 0.675426 0.527554 0.624182 11.00000 0.02265 0.00984 = 0.01516 -0.00317 -0.00241 -0.00421 N5 3 0.742056 0.334693 0.771553 11.00000 0.02288 0.01144 = 0.01727 -0.00478 -0.00248 -0.00438 N6 3 0.891805 0.228610 0.850432 11.00000 0.02897 0.01338 = 0.03775 -0.00582 -0.01669 0.00021 H6 2 0.937834 0.174940 0.872551 11.00000 -1.20000 N7 3 0.485953 0.421182 0.633604 11.00000 0.01895 0.01770 = 0.01925 -0.00567 -0.00032 -0.00523 C1 1 0.463724 0.534813 0.791238 11.00000 0.02345 0.01228 = 0.02040 -0.00771 -0.00609 -0.00023 C2 1 0.357253 0.541512 0.869570 11.00000 0.02451 0.01637 = 0.01932 -0.00946 -0.00419 -0.00001 C3 1 0.313939 0.441531 0.922525 11.00000 0.02259 0.01577 = 0.01806 -0.00869 -0.00507 -0.00130 C4 1 0.394092 0.373936 0.876896 11.00000 0.01956 0.01476 = 0.01597 -0.00695 -0.00376 -0.00139 C5 1 0.377091 0.266457 0.907098 11.00000 0.02342 0.01507 = 0.01343 -0.00423 -0.00192 -0.00405 AFIX 43 H5 2 0.314906 0.233958 0.965639 11.00000 -1.20000 AFIX 0 C6 1 0.443244 0.202651 0.858989 11.00000 0.02175 0.01178 = 0.01440 -0.00313 -0.00375 -0.00365 C7 1 0.421256 0.091653 0.890457 11.00000 0.02082 0.01252 = 0.01665 -0.00422 -0.00483 -0.00305 C8 1 0.503411 0.058748 0.822531 11.00000 0.02391 0.01218 = 0.01823 -0.00492 -0.00386 -0.00406 C9 1 0.572868 0.149757 0.749967 11.00000 0.02274 0.01312 = 0.01880 -0.00586 -0.00415 -0.00389 C10 1 0.660948 0.150481 0.666824 11.00000 0.02477 0.01320 = 0.01900 -0.00777 -0.00172 -0.00345 AFIX 43 H10 2 0.676284 0.086029 0.657573 11.00000 -1.20000 AFIX 0 C11 1 0.728546 0.236267 0.596117 11.00000 0.02057 0.01529 = 0.01832 -0.00814 -0.00312 -0.00194 C12 1 0.814999 0.235678 0.507532 11.00000 0.02196 0.01810 = 0.01737 -0.00923 -0.00186 -0.00240 C13 1 0.866790 0.332848 0.458389 11.00000 0.02079 0.01796 = 0.01716 -0.00730 -0.00291 -0.00115 C14 1 0.810972 0.393158 0.517168 11.00000 0.01900 0.01536 = 0.01434 -0.00389 -0.00197 -0.00180 C15 1 0.836355 0.497057 0.491212 11.00000 0.01793 0.01639 = 0.01572 -0.00293 -0.00244 -0.00445 AFIX 43 H15 2 0.904419 0.527382 0.436077 11.00000 -1.20000 AFIX 0 C16 1 0.769952 0.560457 0.539585 11.00000 0.01978 0.01455 = 0.01568 -0.00289 -0.00535 -0.00431 C17 1 0.783193 0.673989 0.502937 11.00000 0.02216 0.01359 = 0.01829 -0.00363 -0.00574 -0.00383 C18 1 0.694098 0.710130 0.565433 11.00000 0.02616 0.01178 = 0.02029 -0.00357 -0.00669 -0.00460 C19 1 0.628259 0.618335 0.640924 11.00000 0.02288 0.01282 = 0.01764 -0.00353 -0.00467 -0.00417 C20 1 0.530136 0.620899 0.719210 11.00000 0.02517 0.01194 = 0.02054 -0.00624 -0.00571 -0.00001 AFIX 43 H20 2 0.506481 0.688029 0.723661 11.00000 -1.20000 AFIX 0 C21 1 0.304765 0.642015 0.884716 11.00000 0.02559 0.01651 = 0.02886 -0.01227 -0.00020 -0.00268 AFIX 23 H21A 2 0.210634 0.636232 0.918239 11.00000 -1.20000 H21B 2 0.308926 0.703656 0.820590 11.00000 -1.20000 AFIX 0 C22 1 0.380124 0.664578 0.944043 11.00000 0.03934 0.02670 = 0.03414 -0.02042 -0.00227 -0.00615 AFIX 3 H22A 2 0.382105 0.601928 1.005893 11.00000 -1.50000 H22B 2 0.335794 0.727018 0.956502 11.00000 -1.50000 H22C 2 0.470805 0.679228 0.907553 11.00000 -1.50000 AFIX 0 C23 1 0.201739 0.407471 1.009252 11.00000 0.02602 0.01795 = 0.01951 -0.00975 0.00039 -0.00412 AFIX 23 H23A 2 0.158242 0.351500 1.007698 11.00000 -1.20000 H23B 2 0.135763 0.469825 1.003759 11.00000 -1.20000 AFIX 0 C24 1 0.241220 0.363952 1.107161 11.00000 0.03456 0.03510 = 0.02173 -0.01220 -0.00118 -0.01136 AFIX 3 H24A 2 0.300320 0.298252 1.116242 11.00000 -1.50000 H24B 2 0.161810 0.347952 1.159131 11.00000 -1.50000 H24C 2 0.286870 0.417762 1.108991 11.00000 -1.50000 AFIX 0 C25 1 0.320241 0.030317 0.975889 11.00000 0.02832 0.01329 = 0.01596 -0.00418 -0.00143 -0.00530 AFIX 23 H25A 2 0.314381 0.051224 1.029469 11.00000 -1.20000 H25B 2 0.348336 -0.047374 0.998537 11.00000 -1.20000 AFIX 0 C26 1 0.184273 0.051339 0.950824 11.00000 0.02785 0.02537 = 0.02408 -0.00965 -0.00207 -0.00820 AFIX 3 H26A 2 0.159653 0.128809 0.923164 11.00000 -1.50000 H26B 2 0.118713 0.016059 1.009724 11.00000 -1.50000 H26C 2 0.187243 0.022759 0.903424 11.00000 -1.50000 AFIX 0 C27 1 0.521011 -0.049514 0.819964 11.00000 0.03171 0.01277 = 0.02367 -0.00791 -0.00013 -0.00606 AFIX 23 H27A 2 0.491435 -0.104106 0.886427 11.00000 -1.20000 H27B 2 0.616203 -0.067600 0.798394 11.00000 -1.20000 AFIX 0 C28 1 0.443908 -0.054573 0.752325 11.00000 0.03560 0.02215 = 0.03445 -0.01661 -0.00315 -0.00821 AFIX 3 H28A 2 0.349088 -0.040303 0.775125 11.00000 -1.50000 H28B 2 0.460888 -0.126162 0.752295 11.00000 -1.50000 H28C 2 0.472428 -0.000653 0.686335 11.00000 -1.50000 AFIX 0 C29 1 0.829501 0.147031 0.475882 11.00000 0.02848 0.01930 = 0.02015 -0.01139 -0.00031 -0.00282 AFIX 23 H29A 2 0.848067 0.077711 0.529694 11.00000 -1.20000 H29B 2 0.905571 0.157638 0.420434 11.00000 -1.20000 AFIX 0 C30 1 0.704039 0.142875 0.445727 11.00000 0.03676 0.02637 = 0.02347 -0.01326 -0.00472 -0.00560 AFIX 3 H30A 2 0.628539 0.132675 0.500437 11.00000 -1.50000 H30B 2 0.716009 0.083065 0.426737 11.00000 -1.50000 H30C 2 0.687499 0.210396 0.390777 11.00000 -1.50000 AFIX 0 C31 1 0.951238 0.375751 0.358363 11.00000 0.02709 0.01853 = 0.01895 -0.00606 0.00316 -0.00344 AFIX 23 H31A 2 1.011843 0.316604 0.347576 11.00000 -1.20000 H31B 2 1.005623 0.429910 0.352226 11.00000 -1.20000 AFIX 0 C32 1 0.866512 0.427002 0.281339 11.00000 0.04690 0.03038 = 0.01652 -0.00324 -0.00377 -0.00021 AFIX 3 H32A 2 0.805471 0.376062 0.291819 11.00000 -1.50000 H32B 2 0.923952 0.446052 0.216749 11.00000 -1.50000 H32C 2 0.815901 0.491832 0.286059 11.00000 -1.50000 AFIX 0 C33 1 0.868715 0.739392 0.408396 11.00000 0.02705 0.01634 = 0.02036 -0.00313 -0.00213 -0.00917 AFIX 23 H33A 2 0.953222 0.696724 0.397591 11.00000 -1.20000 H33B 2 0.889135 0.804063 0.411428 11.00000 -1.20000 AFIX 0 C34 1 0.800332 0.773722 0.323027 11.00000 0.04109 0.02838 = 0.01985 -0.00222 -0.00590 -0.00908 AFIX 3 H34A 2 0.788213 0.710042 0.315697 11.00000 -1.50000 H34B 2 0.855323 0.821232 0.263317 11.00000 -1.50000 H34C 2 0.713953 0.811842 0.335607 11.00000 -1.50000 AFIX 0 C35 1 0.666094 0.822780 0.558989 11.00000 0.02891 0.01112 = 0.02345 -0.00342 -0.00541 -0.00503 AFIX 23 H35A 2 0.570892 0.835025 0.585310 11.00000 -1.20000 H35B 2 0.685421 0.873893 0.489905 11.00000 -1.20000 AFIX 0 C36 1 0.747241 0.845638 0.614206 11.00000 0.03862 0.01947 = 0.04085 -0.01411 -0.01356 -0.00336 AFIX 3 H36A 2 0.732871 0.792527 0.681816 11.00000 -1.50000 H36B 2 0.719691 0.917708 0.612206 11.00000 -1.50000 H36C 2 0.841281 0.841317 0.583996 11.00000 -1.50000 AFIX 0 C37 1 0.802383 0.236639 0.800694 11.00000 0.03000 0.01637 = 0.03820 -0.01128 -0.01449 0.00040 AFIX 43 H37 2 0.784766 0.180345 0.788137 11.00000 -1.20000 AFIX 0 C38 1 0.798053 0.391017 0.804088 11.00000 0.02623 0.01353 = 0.01964 -0.00753 -0.00523 -0.00174 AFIX 43 H38 2 0.774570 0.464171 0.793190 11.00000 -1.20000 AFIX 0 C39 1 0.891739 0.325846 0.853996 11.00000 0.02523 0.01815 = 0.01810 -0.00677 -0.00299 -0.00435 C40 1 0.978940 0.341325 0.906022 11.00000 0.03419 0.02659 = 0.02617 -0.01078 -0.00979 -0.00408 AFIX 3 H40A 2 0.966160 0.286695 0.973032 11.00000 -1.50000 H40B 2 0.957041 0.412825 0.906102 11.00000 -1.50000 H40C 2 1.071390 0.334855 0.873202 11.00000 -1.50000 AFIX 0 PART 1 SB1 7 1.003665 0.912716 0.788890 21.00000 0.02126 0.01197 = 0.01727 -0.00574 -0.00201 -0.00173 F1 5 0.952480 1.039417 0.811485 21.00000 0.04165 0.01482 = 0.03261 -0.01194 0.00095 -0.00109 F2 5 1.111980 0.865677 0.877507 21.00000 0.04565 0.02588 = 0.04237 -0.01031 -0.02589 0.00086 F3 5 1.138727 0.981660 0.689519 21.00000 0.04373 0.02940 = 0.03560 -0.01371 0.01497 -0.01342 F4 5 1.055454 0.785526 0.768969 21.00000 0.04120 0.02031 = 0.03421 -0.01638 -0.00257 -0.00075 F5 5 0.867808 0.846456 0.889891 21.00000 0.03679 0.02836 = 0.03369 -0.01571 0.01202 -0.01415 F6 5 0.893826 0.960407 0.702175 21.00000 0.05103 0.03931 = 0.04085 -0.01475 -0.02808 0.00621 PART 2 SB1' 7 0.943986 0.926096 0.777444 31.00000 0.03406 0.02312 = 0.02670 -0.00946 0.00288 -0.00206 F1' 5 0.865398 1.054727 0.790932 31.00000 0.03567 0.01890 = 0.02914 -0.01051 0.00164 -0.00147 F2' 5 0.825097 0.845371 0.892118 31.00000 0.03051 0.02074 = 0.02780 -0.01482 0.00878 -0.01035 F3' 5 1.066683 0.910500 0.853173 31.00000 0.03446 0.02141 = 0.02921 -0.01045 -0.00485 -0.00074 F4' 5 1.022734 0.797572 0.764006 31.00000 0.03403 0.01886 = 0.02685 -0.01258 0.00146 0.00049 F5' 5 1.062866 1.006973 0.662812 31.00000 0.03736 0.02482 = 0.02853 -0.01166 -0.00185 -0.00311 F6' 5 0.821288 0.941911 0.701743 31.00000 0.04177 0.02829 = 0.03347 -0.01236 -0.00808 0.00212 PART 3 SB1" 7 1.072049 0.900550 0.801066 41.00000 0.03414 0.02269 = 0.02497 -0.01216 0.00220 -0.00241 F1" 5 0.951102 1.016074 0.809299 41.00000 0.03274 0.01638 = 0.02553 -0.01214 0.00027 -0.00084 F2" 5 1.148872 0.872186 0.883997 41.00000 0.03617 0.02088 = 0.02818 -0.01436 -0.01171 -0.00074 F3" 5 1.174401 0.980200 0.688828 41.00000 0.03354 0.02365 = 0.02703 -0.01443 0.00594 -0.00959 F4" 5 1.141410 0.767093 0.775911 41.00000 0.03497 0.01942 = 0.03024 -0.01601 -0.00235 -0.00227 F5" 5 0.943531 0.910864 0.701232 41.00000 0.03747 0.02355 = 0.02953 -0.01265 -0.00512 0.00021 F6" 5 0.917986 0.802998 0.896374 41.00000 0.03252 0.02057 = 0.02800 -0.01041 0.00544 -0.00625 PART 0 HKLF 5 REM 15070b in P-1 REM wR2 = 0.1473, GooF = S = 1.008, Restrained GooF = 7.876 for all data REM R1 = 0.0489 for 15942 Fo > 4sig(Fo) and 0.0771 for all 22523 data REM 638 parameters refined using 1240 restraints END WGHT 0.0830 0.0000 REM Instructions for potential hydrogen bonds HTAB N6 F1_$1 HTAB C5 F5_$2 HTAB C5 F2'_$2 HTAB C10 F6'_$1 HTAB C37 F1_$1 HTAB C37 F1'_$1 HTAB C37 F1"_$1 HTAB C40 F2_$3 HTAB C40 F2"_$3 HTAB C40 F6"_$3 REM Highest difference peak 1.565, deepest hole -0.862, 1-sigma level 0.139 Q1 1 1.0468 0.9060 0.7861 11.00000 0.05 1.56 Q2 1 0.6813 0.3562 0.7208 11.00000 0.05 1.32 Q3 1 0.5214 0.3935 0.6850 11.00000 0.05 1.30 Q4 1 0.4024 0.4381 0.8804 11.00000 0.05 1.15 Q5 1 0.3959 0.7931 0.7242 11.00000 0.05 1.05 Q6 1 0.8648 0.9302 0.7657 11.00000 0.05 0.91 Q7 1 0.8997 0.9358 0.8476 11.00000 0.05 0.83 Q8 1 1.0899 0.8550 0.8281 11.00000 0.05 0.80 Q9 1 0.9381 1.0045 0.7374 11.00000 0.05 0.80 Q10 1 1.0439 0.8097 0.7748 11.00000 0.05 0.79 Q11 1 0.4672 0.4141 0.6677 11.00000 0.05 0.78 Q12 1 1.0179 0.8432 0.8176 11.00000 0.05 0.74 Q13 1 1.1398 0.8911 0.8079 11.00000 0.05 0.72 Q14 1 0.3326 0.4892 0.9087 11.00000 0.05 0.70 Q15 1 1.0166 0.7366 0.3662 11.00000 0.05 0.65 Q16 1 0.4402 0.3997 0.8296 11.00000 0.05 0.64 Q17 1 1.1387 0.9112 0.7241 11.00000 0.05 0.63 Q18 1 0.2528 0.0418 0.9609 11.00000 0.05 0.63 Q19 1 0.9978 0.8046 0.7525 11.00000 0.05 0.62 Q20 1 0.5908 0.4559 0.6791 11.00000 0.05 0.60 ; _shelx_res_checksum 75148 _shelx_hkl_file ; 1 0 0 54.8953 1.25281 -2 1 0 0 54.8953 1.25281 1 1 0 0 12.9122 0.28905 2 1 0 0 37.5918 0.60032 1 2 0 0 46.8495 0.93211 2 2 0 0 215.367 5.42287 -2 2 0 0 215.367 5.42287 1 2 0 0 143.754 2.29245 1 3 0 0 4.14645 0.37670 2 3 0 0 22.4974 1.54182 -2 3 0 0 22.4974 1.54182 1 3 0 0 14.8583 0.61790 1 4 0 0 3.53462 0.40643 2 4 0 0 18.8779 1.32017 -2 4 0 0 18.8779 1.32017 1 4 0 0 13.9999 0.68262 1 5 0 0 187.580 3.34380 1 5 0 0 261.567 5.92903 -2 5 0 0 261.567 5.92903 1 5 0 0 49.9429 1.30215 2 6 0 0 168.121 3.20891 1 6 0 0 242.057 5.88796 -2 6 0 0 242.057 5.88796 1 6 0 0 45.2998 1.14496 2 7 0 0 211.887 5.66617 -2 7 0 0 211.887 5.66617 1 7 0 0 41.0677 1.38541 2 7 0 0 156.062 2.78802 1 8 0 0 30.7760 2.33215 2 8 0 0 157.575 3.92966 -2 8 0 0 157.575 3.92966 1 8 0 0 130.711 4.65082 1 9 0 0 27.6772 3.26823 -2 9 0 0 27.6772 3.26823 1 9 0 0 6.37215 1.24870 2 9 0 0 27.3172 2.07530 1 10 0 0 158.945 4.97206 1 10 0 0 29.5383 2.20475 2 10 0 0 191.129 7.57704 -2 10 0 0 191.129 7.57704 1 11 0 0 4.22741 1.63832 1 11 0 0 0.14851 0.90738 2 12 0 0 15.4705 2.43765 1 12 0 0 -0.0461 1.54681 2 13 0 0 1.55825 1.85184 2 13 0 0 14.1843 3.16282 1 14 0 0 -1.1534 1.99130 1 14 0 0 -4.0198 1.53859 2 -14 1 0 9.12192 2.40764 2 -14 1 0 54.2382 5.59486 1 -13 1 0 -0.2748 1.63171 2 -13 1 0 -1.0254 1.63027 1 -12 1 0 9.36409 2.48369 1 -12 1 0 2.03685 1.65612 2 -11 1 0 4.97768 1.18036 2 -11 1 0 27.7024 2.48116 1 -10 1 0 8.93053 1.32008 1 -10 1 0 6.41688 4.37167 -2 -10 1 0 6.41688 4.37167 1 -10 1 0 2.26389 0.87928 2 -9 1 0 193.129 5.97512 -2 -9 1 0 193.129 5.97512 1 -9 1 0 149.459 5.16213 1 -9 1 0 30.7089 2.39156 2 -8 1 0 0.05493 0.55028 2 -8 1 0 0.40817 1.21144 -2 -8 1 0 0.40817 1.21144 1 -8 1 0 2.17289 0.69862 1 -7 1 0 177.697 3.49872 1 -7 1 0 45.5898 1.46505 2 -7 1 0 229.205 4.73059 -2 -7 1 0 229.205 4.73059 1 -6 1 0 126.058 3.32486 -2 -6 1 0 126.058 3.32486 1 -6 1 0 24.9429 1.04642 2 -6 1 0 102.075 2.66186 1 -5 1 0 26.0482 1.65954 -2 -5 1 0 26.0482 1.65954 1 -5 1 0 4.10565 0.46866 2 -5 1 0 18.7723 0.79692 1 -4 1 0 9.66150 0.57055 2 -4 1 0 59.6339 2.11211 -2 -4 1 0 59.6339 2.11211 1 -4 1 0 43.0351 1.09611 1 -3 1 0 0.63283 0.49776 -2 -3 1 0 0.63283 0.49776 1 -3 1 0 0.37104 0.26517 2 -3 1 0 0.09367 0.29077 1 -2 1 0 333.747 5.33726 -2 -2 1 0 333.747 5.33726 1 -2 1 0 74.0840 1.97988 2 -2 1 0 246.016 5.39183 1 -1 1 0 160.261 3.27441 2 -1 1 0 465.130 9.13295 1 -1 1 0 622.464 8.42577 -2 -1 1 0 622.464 8.42577 1 0 1 0 1.44846 0.17739 -2 0 1 0 1.44846 0.17739 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215.562 6.42313 1 3 6 12 44.1644 1.87991 -2 3 6 12 44.1644 1.87991 1 3 6 12 36.2308 4.58104 1 3 6 12 10.8337 2.73063 2 4 6 12 303.052 8.30116 1 4 6 12 100.490 4.00981 2 4 6 12 423.842 8.02239 -2 4 6 12 423.842 8.02239 1 5 6 12 56.2759 2.97188 -2 5 6 12 56.2759 2.97188 1 5 6 12 13.0025 1.75741 2 5 6 12 44.7021 2.71672 1 6 6 12 74.3279 3.39948 -2 6 6 12 74.3279 3.39948 1 6 6 12 18.6269 2.25230 2 6 6 12 48.4961 2.95360 1 7 6 12 14.3608 2.05483 2 7 6 12 56.3107 3.21630 1 7 6 12 71.2104 3.50455 -2 7 6 12 71.2104 3.50455 1 8 6 12 3.81292 2.17785 -2 8 6 12 3.81292 2.17785 1 8 6 12 1.82804 1.06858 2 8 6 12 2.91423 1.21674 1 9 6 12 19.1240 1.74281 2 9 6 12 77.1784 3.01237 1 9 6 12 90.8386 6.66369 -2 9 6 12 90.8386 6.66369 1 10 6 12 8.08273 1.77117 2 10 6 12 39.8091 3.54639 -2 10 6 12 39.8091 3.54639 1 10 6 12 31.6150 2.91339 1 11 6 12 16.5343 2.35255 1 11 6 12 3.18346 1.39744 2 11 6 12 20.2201 4.40263 -2 11 6 12 20.2201 4.40263 1 12 6 12 91.2330 4.44316 1 12 6 12 21.8715 2.57454 2 13 6 12 0.86726 1.69677 1 13 6 12 -0.6840 1.47755 2 14 6 12 11.0279 2.13856 2 14 6 12 62.3288 4.28915 1 -9 7 12 -0.1477 1.22143 1 -9 7 12 -1.9276 1.04651 2 -8 7 12 0.93817 1.13272 2 -8 7 12 4.42557 1.54419 1 -7 7 12 7.72129 1.64701 1 -7 7 12 1.00932 1.16412 2 -6 7 12 -0.1268 1.05093 2 -6 7 12 0.35055 1.19791 1 -5 7 12 13.9290 1.65670 2 -5 7 12 60.6698 3.01006 1 -4 7 12 -0.1679 1.46207 1 -4 7 12 -0.5120 2.34515 -2 -4 7 12 -0.5120 2.34515 1 -4 7 12 -2.1231 1.12255 2 -3 7 12 103.965 4.42795 -2 -3 7 12 103.965 4.42795 1 -3 7 12 83.5387 4.43317 1 -3 7 12 23.6907 2.53610 2 -2 7 12 99.6860 3.59386 -2 -2 7 12 99.6860 3.59386 1 -2 7 12 25.6753 3.57535 2 -2 7 12 62.1415 5.11184 1 -1 7 12 4.73605 1.66372 -2 -1 7 12 4.73605 1.66372 1 -1 7 12 4.45537 1.99691 1 -1 7 12 2.08323 1.73290 2 0 7 12 280.229 6.13005 -2 0 7 12 280.229 6.13005 1 0 7 12 186.730 9.01220 1 0 7 12 76.2761 5.38846 2 1 7 12 13.7271 1.27498 -2 1 7 12 13.7271 1.27498 1 1 7 12 1.88444 1.69666 2 1 7 12 11.6331 2.84610 1 2 7 12 103.170 2.58047 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12 13.9670 5.35130 -2 12 7 12 13.9670 5.35130 1 12 7 12 2.41493 1.39548 2 12 7 12 9.68623 2.80252 1 13 7 12 43.7019 4.57993 1 13 7 12 50.7595 7.33655 -2 13 7 12 50.7595 7.33655 1 13 7 12 9.31026 2.36165 2 14 7 12 -1.1043 1.65491 1 14 7 12 -0.9793 1.53686 2 -9 8 12 0.65793 1.21722 1 -9 8 12 -0.2147 1.13289 2 -8 8 12 0.45410 1.18317 2 -8 8 12 -0.0849 1.16550 1 -7 8 12 0.62717 1.00673 2 -7 8 12 3.24589 1.33931 1 -6 8 12 1.14597 1.03768 2 -6 8 12 0.35146 1.21134 1 -5 8 12 4.87218 1.25384 2 -5 8 12 30.7934 2.55956 1 -4 8 12 21.0250 3.53026 -2 -4 8 12 21.0250 3.53026 1 -4 8 12 16.2207 2.09602 1 -4 8 12 3.01363 1.16346 2 -3 8 12 81.2674 4.04155 -2 -3 8 12 81.2674 4.04155 1 -3 8 12 60.2629 3.78617 1 -3 8 12 15.4536 2.14860 2 -2 8 12 15.7405 2.16437 -2 -2 8 12 15.7405 2.16437 1 -2 8 12 11.3553 3.01376 1 -2 8 12 1.35547 1.58964 2 -1 8 12 17.6393 1.95686 -2 -1 8 12 17.6393 1.95686 1 -1 8 12 7.30954 2.32320 2 -1 8 12 12.2603 2.86679 1 0 8 12 1.84728 1.57263 -2 0 8 12 1.84728 1.57263 1 0 8 12 0.47138 1.53637 2 0 8 12 2.47065 1.80557 1 1 8 12 111.709 3.13475 -2 1 8 12 111.709 3.13475 1 2 8 12 92.9091 2.48387 -2 2 8 12 92.9091 2.48387 1 2 8 12 73.2262 4.88375 1 2 8 12 19.0551 2.88082 2 3 8 12 1.13772 1.01322 -2 3 8 12 1.13772 1.01322 1 4 8 12 65.2182 2.66128 -2 4 8 12 65.2182 2.66128 1 4 8 12 57.9443 4.43192 1 4 8 12 14.5742 2.74025 2 5 8 12 6.25277 1.57152 -2 5 8 12 6.25277 1.57152 1 5 8 12 10.1555 2.53175 1 5 8 12 2.02460 1.66012 2 6 8 12 37.5909 4.36037 1 6 8 12 45.2772 2.51162 -2 6 8 12 45.2772 2.51162 1 6 8 12 10.5716 2.54669 2 7 8 12 4.41310 1.55399 -2 7 8 12 4.41310 1.55399 1 7 8 12 5.36245 2.27284 1 7 8 12 0.81691 1.81277 2 8 8 12 10.2083 2.10396 1 8 8 12 14.2784 2.21651 -2 8 8 12 14.2784 2.21651 1 8 8 12 5.41736 1.69613 2 9 8 12 0.10473 1.51381 2 9 8 12 10.2160 2.16250 -2 9 8 12 10.2160 2.16250 1 9 8 12 6.32334 2.01656 1 10 8 12 3.53583 1.87103 2 10 8 12 19.8551 2.59749 -2 10 8 12 19.8551 2.59749 1 10 8 12 15.9120 2.85094 1 11 8 12 51.8787 3.67339 1 11 8 12 12.2635 1.94881 2 11 8 12 62.8678 6.97322 -2 11 8 12 62.8678 6.97322 1 12 8 12 4.01857 2.03792 1 12 8 12 6.48517 3.07777 -2 12 8 12 6.48517 3.07777 1 12 8 12 1.73696 2.04454 2 13 8 12 -0.5336 1.35783 2 13 8 12 1.24275 2.05421 1 13 8 12 -1.2968 4.88914 -2 13 8 12 -1.2968 4.88914 1 -8 9 12 4.69359 1.54779 1 -8 9 12 -0.3356 1.08818 2 -7 9 12 3.09005 1.16781 2 -7 9 12 23.1705 2.49678 1 -6 9 12 -0.5219 0.89892 2 -6 9 12 0.16315 1.12056 1 -5 9 12 0.31866 0.82919 2 -5 9 12 -0.2076 1.01076 1 -4 9 12 12.8128 1.75587 2 -4 9 12 72.5703 4.99191 -2 -4 9 12 72.5703 4.99191 1 -4 9 12 55.4822 3.24113 1 -3 9 12 5.09663 1.42268 2 -3 9 12 27.1235 3.51766 -2 -3 9 12 27.1235 3.51766 1 -3 9 12 20.1047 2.17041 1 -2 9 12 41.2983 3.99571 2 -2 9 12 166.765 4.72656 -2 -2 9 12 166.765 4.72656 1 -2 9 12 123.568 7.21899 1 -1 9 12 11.3050 1.61462 -2 -1 9 12 11.3050 1.61462 1 0 9 12 13.2703 1.58480 -2 0 9 12 13.2703 1.58480 1 1 9 12 2.37508 1.29858 -2 1 9 12 2.37508 1.29858 1 2 9 12 0.78297 1.42898 2 2 9 12 5.85384 1.54825 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13 9 12 -4.2315 4.38992 -2 13 9 12 -4.2315 4.38992 1 13 9 12 1.27768 1.31898 2 -8 10 12 52.3000 3.58454 1 -8 10 12 6.69598 1.42557 2 -7 10 12 28.1574 2.64351 1 -7 10 12 4.06680 1.23002 2 -6 10 12 5.37123 1.37071 2 -6 10 12 52.3343 3.41499 1 -5 10 12 5.00076 1.12908 2 -5 10 12 27.5447 2.11245 1 -4 10 12 40.0210 4.17072 -2 -4 10 12 40.0210 4.17072 1 -4 10 12 5.65525 1.35524 2 -4 10 12 39.3076 3.11034 1 -3 10 12 149.212 4.50371 -2 -3 10 12 149.212 4.50371 1 -3 10 12 118.565 7.74992 1 -3 10 12 28.6089 4.17364 2 -2 10 12 27.8807 2.03800 -2 -2 10 12 27.8807 2.03800 1 -1 10 12 21.3970 1.82856 -2 -1 10 12 21.3970 1.82856 1 0 10 12 18.7209 1.89492 -2 0 10 12 18.7209 1.89492 1 1 10 12 44.4391 2.15487 -2 1 10 12 44.4391 2.15487 1 2 10 12 169.868 4.00702 -2 2 10 12 169.868 4.00702 1 3 10 12 -0.6835 1.11975 -2 3 10 12 -0.6835 1.11975 1 4 10 12 227.191 4.75686 -2 4 10 12 227.191 4.75686 1 5 10 12 39.9232 2.72818 -2 5 10 12 39.9232 2.72818 1 5 10 12 47.2649 4.93692 -2 5 10 12 47.2649 4.93692 -2 5 10 12 47.2649 4.93692 1 6 10 12 0.79438 1.39264 -2 6 10 12 0.79438 1.39264 1 7 10 12 171.791 4.27360 -2 7 10 12 171.791 4.27360 1 8 10 12 1.54723 1.45532 -2 8 10 12 1.54723 1.45532 1 9 10 12 51.0486 2.82563 -2 9 10 12 51.0486 2.82563 1 9 10 12 11.8149 3.75554 2 9 10 12 42.7474 6.25722 1 10 10 12 9.43248 3.74074 2 10 10 12 38.3015 2.66286 -2 10 10 12 38.3015 2.66286 1 10 10 12 31.9254 5.65091 1 11 10 12 25.1879 3.61439 1 11 10 12 8.33878 2.17153 2 11 10 12 28.5440 3.79547 -2 11 10 12 28.5440 3.79547 1 12 10 12 11.1702 2.57759 2 12 10 12 39.2498 4.54684 1 12 10 12 38.5224 4.46932 -2 12 10 12 38.5224 4.46932 1 13 10 12 18.6107 5.34467 -2 13 10 12 18.6107 5.34467 1 13 10 12 3.50945 1.70566 2 13 10 12 11.4067 2.28462 1 -8 11 12 3.85076 1.51205 2 -8 11 12 32.3298 3.46603 1 -7 11 12 3.63431 1.47579 2 -7 11 12 28.2219 3.15056 1 -6 11 12 8.41020 1.44051 2 -6 11 12 48.3778 3.27896 1 -5 11 12 22.6680 2.00731 2 -5 11 12 122.514 4.32248 1 -5 11 12 156.989 9.30504 -2 -5 11 12 156.989 9.30504 1 -4 11 12 55.3932 3.43171 1 -4 11 12 80.5805 4.72323 -2 -4 11 12 80.5805 4.72323 1 -4 11 12 11.4613 1.79616 2 -3 11 12 110.869 4.56237 -2 -3 11 12 110.869 4.56237 1 -3 11 12 17.0936 2.30610 2 -3 11 12 78.1648 4.45460 1 -2 11 12 243.626 5.32726 -2 -2 11 12 243.626 5.32726 1 -1 11 12 6.52375 1.50501 -2 -1 11 12 6.52375 1.50501 1 0 11 12 231.467 5.00262 -2 0 11 12 231.467 5.00262 1 1 11 12 6.72096 1.52293 -2 1 11 12 6.72096 1.52293 1 2 11 12 121.618 3.35927 -2 2 11 12 121.618 3.35927 1 3 11 12 121.921 3.37617 -2 3 11 12 121.921 3.37617 1 4 11 12 101.380 3.38732 -2 4 11 12 101.380 3.38732 1 5 11 12 514.191 8.60736 -2 5 11 12 514.191 8.60736 1 6 11 12 14.2013 1.69493 -2 6 11 12 14.2013 1.69493 1 7 11 12 0.54508 1.45537 -2 7 11 12 0.54508 1.45537 1 8 11 12 25.0389 2.07566 -2 8 11 12 25.0389 2.07566 1 9 11 12 23.9532 4.76208 1 9 11 12 7.84595 3.43322 2 9 11 12 30.6490 2.56366 -2 9 11 12 30.6490 2.56366 1 10 11 12 77.9614 3.51474 -2 10 11 12 77.9614 3.51474 1 10 11 12 56.1595 6.29972 1 10 11 12 19.6004 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43.0963 3.50604 1 7 3 20 5.40112 1.73556 1 7 3 20 -0.0703 1.22003 2 -1 4 20 -0.0457 1.75702 2 -1 4 20 3.90303 2.45112 1 0 4 20 91.9122 9.97873 -2 0 4 20 91.9122 9.97873 1 0 4 20 15.3513 2.99868 2 0 4 20 60.2999 7.77682 1 1 4 20 8.54165 2.96131 1 1 4 20 -0.0529 1.83616 2 2 4 20 36.9835 4.51669 1 2 4 20 10.4089 2.71324 2 3 4 20 42.2673 4.77453 1 3 4 20 10.1974 2.68745 2 4 4 20 13.2177 3.11368 1 4 4 20 3.03752 1.95274 2 5 4 20 11.9679 2.36769 2 5 4 20 48.1125 4.20877 1 6 4 20 15.5631 2.33075 1 6 4 20 1.35591 1.33838 2 7 4 20 3.49995 1.41757 2 7 4 20 19.3887 2.52557 1 8 4 20 22.2429 2.62990 1 8 4 20 5.60652 1.51329 2 -1 5 20 3.34634 2.04845 2 -1 5 20 6.08265 2.55325 1 0 5 20 0.28026 5.67910 -2 0 5 20 0.28026 5.67910 1 0 5 20 -0.2888 1.67958 2 0 5 20 -0.7782 2.37399 1 1 5 20 3.75868 2.03261 2 1 5 20 20.1985 3.51227 1 2 5 20 -2.1228 1.54704 2 2 5 20 0.02155 2.09603 1 3 5 20 39.5065 4.67080 1 3 5 20 15.3629 2.77344 2 4 5 20 14.5585 3.26780 1 4 5 20 4.10103 2.09652 2 5 5 20 4.31091 1.74948 2 5 5 20 17.3458 2.92571 1 6 5 20 5.35014 1.56616 2 6 5 20 20.8861 2.59218 1 7 5 20 3.45714 1.56453 1 7 5 20 0.63195 1.16039 2 8 5 20 2.50399 1.34788 2 8 5 20 14.0647 2.31408 1 -2 6 20 4.38055 2.18646 2 -2 6 20 20.6414 3.83339 1 -1 6 20 8.06725 3.48081 1 -1 6 20 5.19605 2.88832 2 0 6 20 0.39332 1.86001 1 0 6 20 -4.8176 5.25590 -2 0 6 20 -4.8176 5.25590 1 0 6 20 -0.8782 1.61492 2 1 6 20 2.06406 1.78820 2 1 6 20 5.34293 2.23369 1 2 6 20 2.25604 1.94234 1 2 6 20 -1.6374 1.64884 2 3 6 20 -1.4204 1.61797 2 3 6 20 2.82527 2.20844 1 4 6 20 1.96243 2.22106 1 4 6 20 0.90433 1.69399 2 5 6 20 2.91663 1.60441 2 5 6 20 10.7720 2.86992 1 6 6 20 0.03958 1.20141 2 6 6 20 7.00068 1.82926 1 7 6 20 23.6752 2.66522 1 7 6 20 5.16527 1.55055 2 8 6 20 2.32034 1.19934 2 8 6 20 4.57500 1.59299 1 9 6 20 2.10079 1.41375 1 9 6 20 -0.6926 1.21567 2 -2 7 20 0.56488 1.94077 2 -2 7 20 5.75241 2.58713 1 -1 7 20 12.7761 4.39973 1 -1 7 20 16.4616 6.84378 -2 -1 7 20 16.4616 6.84378 1 -1 7 20 -0.8825 2.15637 2 0 7 20 -0.9705 1.61745 2 0 7 20 -4.0933 2.24612 1 1 7 20 -0.4509 1.71351 2 1 7 20 -1.3043 1.71617 1 2 7 20 0.41061 1.80808 2 2 7 20 5.53836 2.40743 1 3 7 20 4.96926 2.40717 1 3 7 20 -0.2501 1.62857 2 4 7 20 7.88343 2.32646 2 4 7 20 49.2619 5.13981 1 5 7 20 0.84617 1.71547 2 5 7 20 0.63357 1.94732 1 6 7 20 0.37117 1.52811 1 6 7 20 0.31561 1.36937 2 7 7 20 0.62117 1.14496 2 7 7 20 0.52143 1.70547 1 8 7 20 0.14082 1.03909 2 8 7 20 0.60178 1.25066 1 9 7 20 2.29634 1.19021 2 9 7 20 9.05396 1.71030 1 -2 8 20 27.3649 4.15427 1 -2 8 20 8.44613 2.45530 2 -1 8 20 8.58421 3.68511 1 -1 8 20 3.30550 1.92382 2 -1 8 20 16.8448 6.74034 -2 -1 8 20 16.8448 6.74034 1 0 8 20 43.4836 4.58362 1 0 8 20 9.07848 2.54747 2 1 8 20 -0.4197 1.76680 2 1 8 20 1.11389 1.90882 1 2 8 20 11.7077 2.76626 1 2 8 20 2.85959 2.05612 2 3 8 20 6.88800 2.20149 2 3 8 20 35.1561 4.29064 1 4 8 20 8.45146 2.61525 1 4 8 20 0.96619 2.07964 2 5 8 20 54.1893 5.32651 1 5 8 20 14.3975 2.75868 2 6 8 20 1.63741 1.41709 2 6 8 20 5.86261 2.44837 1 7 8 20 12.5567 1.67703 2 7 8 20 48.1731 4.10492 1 8 8 20 25.4682 2.45745 1 8 8 20 4.27053 1.26825 2 9 8 20 0.86156 1.37423 1 9 8 20 0.14448 1.12273 2 -2 9 20 32.8619 6.65207 1 -2 9 20 7.60381 2.58491 2 -1 9 20 4.51912 2.05694 2 -1 9 20 20.0846 7.08828 -2 -1 9 20 20.0846 7.08828 1 -1 9 20 16.0802 4.29299 1 0 9 20 3.49521 1.99589 1 0 9 20 1.49400 1.75721 2 1 9 20 20.1298 3.26123 2 1 9 20 70.8162 5.08075 1 2 9 20 1.52661 1.93194 1 2 9 20 0.03737 1.70885 2 3 9 20 7.99436 2.50586 2 3 9 20 34.4265 4.22794 1 4 9 20 29.8588 4.09582 1 4 9 20 5.37446 2.09475 2 5 9 20 5.54463 2.48333 1 5 9 20 -0.7952 1.66545 2 6 9 20 50.6019 5.08235 1 6 9 20 16.3978 2.97044 2 7 9 20 9.67082 2.28101 1 7 9 20 0.40856 1.40450 2 8 9 20 72.1828 4.76127 1 8 9 20 19.2149 2.25745 2 9 9 20 11.6714 2.10686 1 9 9 20 2.97644 1.35320 2 -1 10 20 9.47165 2.38883 1 -1 10 20 7.42107 6.30316 -2 -1 10 20 7.42107 6.30316 1 -1 10 20 4.36763 2.14205 2 0 10 20 4.35329 2.23034 2 0 10 20 13.9472 2.91101 1 1 10 20 1.29523 1.84168 1 1 10 20 0.69595 1.98584 2 2 10 20 16.9498 3.17063 2 2 10 20 57.9486 5.23926 1 3 10 20 -0.9445 1.63408 1 3 10 20 -2.2394 1.51554 2 4 10 20 56.5741 7.19259 1 4 10 20 71.9389 7.94610 -2 4 10 20 71.9389 7.94610 1 4 10 20 16.8946 4.49673 2 5 10 20 1.06800 4.70762 -2 5 10 20 1.06800 4.70762 1 5 10 20 2.56256 2.62350 2 5 10 20 6.89185 3.29957 1 6 10 20 15.6750 3.23716 1 6 10 20 4.62175 2.07824 2 7 10 20 4.10879 2.06851 2 7 10 20 7.26176 2.65976 1 8 10 20 3.65539 1.70428 2 8 10 20 7.19076 2.16291 1 9 10 20 0.82528 1.23832 2 9 10 20 3.70874 1.55802 1 -1 11 20 -0.8440 1.52980 2 -1 11 20 0.90448 1.88079 1 0 11 20 1.01348 1.95998 2 0 11 20 5.03361 2.30270 1 1 11 20 3.87984 2.15410 1 1 11 20 1.47376 1.99864 2 2 11 20 3.96502 4.89026 -2 2 11 20 3.96502 4.89026 1 2 11 20 4.94209 2.92421 1 2 11 20 -2.7262 2.33057 2 3 11 20 41.1579 6.73864 -2 3 11 20 41.1579 6.73864 1 3 11 20 23.8545 4.79214 1 3 11 20 7.66405 3.84290 2 4 11 20 0.29450 2.51226 1 4 11 20 0.53631 2.55154 2 4 11 20 -0.7210 4.59836 -2 4 11 20 -0.7210 4.59836 1 5 11 20 1.20059 2.79412 2 5 11 20 9.26701 3.47228 1 5 11 20 1.55120 4.51217 -2 5 11 20 1.55120 4.51217 1 6 11 20 3.89156 4.56816 -2 6 11 20 3.89156 4.56816 1 6 11 20 5.38837 3.11385 1 6 11 20 -2.1930 2.25862 2 7 11 20 3.60425 3.25607 1 7 11 20 2.03618 2.60087 2 7 11 20 5.08010 4.68785 -2 7 11 20 5.08010 4.68785 1 8 11 20 60.1506 7.08270 -2 8 11 20 60.1506 7.08270 1 8 11 20 8.55473 3.20539 2 8 11 20 43.2815 6.95840 1 9 11 20 -2.4731 2.48182 1 9 11 20 2.89674 1.86110 2 -1 12 20 0.72294 3.92080 -2 -1 12 20 0.72294 3.92080 1 0 12 20 -0.9846 3.70380 -2 0 12 20 -0.9846 3.70380 1 0 12 20 -0.6330 2.48020 1 0 12 20 2.65709 2.94833 2 1 12 20 -0.8200 2.43742 2 1 12 20 2.53368 2.77601 1 1 12 20 -2.0830 4.12525 -2 1 12 20 -2.0830 4.12525 1 2 12 20 -4.1387 4.77327 -2 2 12 20 -4.1387 4.77327 1 2 12 20 -0.0127 2.65961 1 2 12 20 -1.3932 2.24760 2 3 12 20 1.67988 2.78096 2 3 12 20 5.33637 2.90885 1 3 12 20 1.56494 4.51435 -2 3 12 20 1.56494 4.51435 1 4 12 20 -7.2350 4.27228 -2 4 12 20 -7.2350 4.27228 1 4 12 20 1.96258 2.84926 1 4 12 20 2.57539 2.70956 2 5 12 20 1.71274 2.86970 2 5 12 20 13.2895 4.18497 1 5 12 20 10.5508 5.05475 -2 5 12 20 10.5508 5.05475 1 6 12 20 3.18884 3.01187 2 6 12 20 26.4928 5.94137 -2 6 12 20 26.4928 5.94137 1 6 12 20 21.0733 4.84571 1 7 12 20 -0.3077 2.12697 1 7 12 20 -3.3659 3.93479 -2 7 12 20 -3.3659 3.93479 1 7 12 20 -0.9424 2.21344 2 8 12 20 1.26062 2.55725 1 8 12 20 -1.5885 2.86121 2 8 12 20 2.28690 4.00642 -2 8 12 20 2.28690 4.00642 1 0 13 20 6.77763 3.10657 1 0 13 20 1.26053 2.73676 2 0 13 20 12.5691 4.84729 -2 0 13 20 12.5691 4.84729 1 1 13 20 18.5588 4.74670 1 1 13 20 15.5728 5.27755 -2 1 13 20 15.5728 5.27755 1 1 13 20 7.59715 3.56646 2 2 13 20 0.18831 2.49662 2 2 13 20 4.14993 2.84075 1 2 13 20 -0.1328 4.82657 -2 2 13 20 -0.1328 4.82657 1 3 13 20 8.51318 4.74775 -2 3 13 20 8.51318 4.74775 1 3 13 20 3.66112 2.92569 2 3 13 20 10.0201 3.73255 1 4 13 20 15.9052 4.36442 1 4 13 20 4.95095 3.28267 2 4 13 20 8.93353 4.81705 -2 4 13 20 8.93353 4.81705 1 5 13 20 2.25733 2.64215 1 5 13 20 -5.4687 4.08807 -2 5 13 20 -5.4687 4.08807 1 5 13 20 -1.4173 2.12504 2 6 13 20 10.9939 3.56651 2 6 13 20 45.7994 6.30916 -2 6 13 20 45.7994 6.30916 1 6 13 20 46.1290 6.84745 1 7 13 20 1.44757 2.77652 1 7 13 20 1.45712 2.64298 2 7 13 20 1.03520 4.60001 -2 7 13 20 1.03520 4.60001 1 8 13 20 11.5954 3.80205 1 8 13 20 14.9281 5.40190 -2 8 13 20 14.9281 5.40190 1 1 14 20 33.9634 6.05319 -2 1 14 20 33.9634 6.05319 1 1 14 20 8.58038 3.35690 2 1 14 20 31.0236 5.74252 1 2 14 20 14.3491 4.03305 2 2 14 20 49.5456 7.06704 1 2 14 20 61.2954 7.20108 -2 2 14 20 61.2954 7.20108 1 3 14 20 6.21873 3.26800 2 3 14 20 5.26038 3.16986 1 4 14 20 17.4169 4.45733 1 4 14 20 2.97924 2.58199 2 5 14 20 38.9231 6.13173 -2 5 14 20 38.9231 6.13173 1 5 14 20 6.04006 2.87050 2 5 14 20 28.2762 5.27324 1 6 14 20 2.12314 2.70937 2 6 14 20 1.63898 2.57230 1 6 14 20 4.06222 4.13125 -2 6 14 20 4.06222 4.13125 1 7 14 20 31.0288 5.46060 1 7 14 20 5.64362 2.91904 2 7 14 20 35.4059 5.91791 -2 7 14 20 35.4059 5.91791 1 3 15 20 62.1455 7.72050 1 3 15 20 13.7162 4.46643 2 4 15 20 7.10377 2.29595 1 4 15 20 0.15764 1.53849 2 5 15 20 30.9308 6.53956 1 5 15 20 6.91771 2.18136 2 3 3 21 1.79186 3.15975 2 3 3 21 16.1003 4.58294 1 1 4 21 -0.6983 2.66612 2 1 4 21 -2.1840 2.68402 1 2 4 21 0.11772 1.89032 2 2 4 21 -0.5406 1.97154 1 3 4 21 27.1028 4.10400 1 3 4 21 6.11064 2.37965 2 4 4 21 3.72927 2.17470 2 4 4 21 9.05212 2.92431 1 5 4 21 12.7382 3.21570 1 5 4 21 1.00757 1.51946 2 6 4 21 0.92666 2.94479 2 6 4 21 -2.9563 2.43270 1 1 5 21 15.3685 3.22319 1 1 5 21 2.33975 1.96299 2 2 5 21 1.83188 2.12360 1 2 5 21 1.47236 1.96808 2 3 5 21 -2.4271 1.91937 1 3 5 21 0.36308 1.92219 2 4 5 21 80.7979 5.83627 1 4 5 21 22.2141 3.63968 2 5 5 21 3.32636 2.68458 1 5 5 21 0.04792 1.93382 2 6 5 21 0.05331 1.70927 1 6 5 21 0.94666 1.32932 2 0 6 21 42.9623 7.74188 1 0 6 21 4.80200 3.36733 2 1 6 21 1.85385 1.95162 2 1 6 21 14.5354 3.28893 1 2 6 21 9.78521 2.62647 2 2 6 21 40.6007 4.77640 1 3 6 21 5.98775 2.17683 2 3 6 21 14.2533 3.18284 1 4 6 21 4.41467 2.33549 2 4 6 21 23.5377 3.87655 1 5 6 21 18.9136 3.77069 1 5 6 21 2.68432 1.89768 2 6 6 21 2.56350 1.63303 2 6 6 21 24.2447 3.21048 1 7 6 21 37.2827 3.33810 1 7 6 21 8.20110 1.74915 2 0 7 21 17.6423 4.34144 1 0 7 21 2.75927 1.90440 2 1 7 21 31.8863 4.15254 1 1 7 21 8.02716 2.37982 2 2 7 21 1.63484 1.99009 2 2 7 21 4.77734 2.36007 1 3 7 21 9.53574 2.60518 2 3 7 21 40.9959 4.85792 1 4 7 21 31.9250 4.37745 1 4 7 21 9.53405 2.62272 2 5 7 21 22.7910 3.91475 1 5 7 21 2.09266 1.91127 2 6 7 21 86.5257 5.92493 1 6 7 21 20.1436 2.67603 2 7 7 21 -1.0044 1.15766 2 7 7 21 -1.5220 1.53732 1 0 8 21 0.76466 1.99965 2 0 8 21 2.21423 1.88505 1 1 8 21 0.49634 2.12596 1 1 8 21 1.94937 2.02516 2 2 8 21 3.10775 2.99484 2 2 8 21 20.9479 3.50218 1 3 8 21 0.30581 3.07844 1 3 8 21 0.11406 2.49747 2 4 8 21 24.1216 3.50669 2 4 8 21 92.3542 8.41702 1 5 8 21 6.87891 2.49763 1 5 8 21 0.25129 1.87778 2 6 8 21 1.02204 1.73659 2 6 8 21 1.10794 1.92060 1 7 8 21 8.89680 1.70306 2 7 8 21 46.8141 4.09535 1 0 9 21 1.08042 1.72649 2 0 9 21 -1.8135 1.60506 1 1 9 21 -0.4861 1.62705 2 1 9 21 1.79974 1.89911 1 2 9 21 0.94184 2.00608 1 2 9 21 -1.9813 1.60119 2 3 9 21 15.9034 3.26303 1 3 9 21 5.55835 2.47379 2 4 9 21 8.88374 2.61111 1 4 9 21 0.75296 1.98916 2 5 9 21 11.8990 3.03659 1 5 9 21 2.82058 1.92850 2 6 9 21 1.84898 1.76913 2 6 9 21 5.82554 2.50232 1 7 9 21 -0.7140 1.61555 1 7 9 21 0.30086 1.64851 2 8 9 21 3.59458 3.41051 2 8 9 21 8.91334 3.68268 1 0 10 21 1.47680 2.03903 2 0 10 21 7.19762 2.27157 1 1 10 21 0.23693 1.61262 2 1 10 21 3.32785 2.17709 1 2 10 21 3.56224 1.97256 2 2 10 21 18.1400 3.30887 1 3 10 21 2.60348 1.95475 1 3 10 21 0.41672 1.72576 2 4 10 21 -0.2057 1.81979 2 4 10 21 3.09664 2.19219 1 5 10 21 9.90128 2.48806 2 5 10 21 48.8627 5.13376 1 6 10 21 -0.4839 1.71579 1 6 10 21 -2.4619 1.41411 2 7 10 21 0.19730 1.60141 2 7 10 21 -1.0669 1.63799 1 1 11 21 47.4197 4.89471 1 1 11 21 11.7798 2.79361 2 2 11 21 -0.4487 1.59851 1 2 11 21 -1.1820 1.59669 2 3 11 21 4.16973 3.41678 2 3 11 21 23.5992 5.07002 1 3 11 21 25.6222 6.09575 -2 3 11 21 25.6222 6.09575 1 4 11 21 7.93837 4.97633 -2 4 11 21 7.93837 4.97633 1 4 11 21 11.6640 3.89319 1 4 11 21 7.41782 3.94494 2 5 11 21 -1.1707 1.92037 2 5 11 21 6.82245 4.82193 -2 5 11 21 6.82245 4.82193 1 5 11 21 1.43620 2.88766 1 6 11 21 8.12154 3.60501 1 6 11 21 1.90936 2.68953 2 6 11 21 18.7767 5.20743 -2 6 11 21 18.7767 5.20743 1 7 11 21 6.15415 3.18468 1 7 11 21 -1.2607 2.18207 2 2 12 21 47.2629 6.82761 1 2 12 21 52.1806 7.41023 -2 2 12 21 52.1806 7.41023 1 2 12 21 13.2814 4.24443 2 3 12 21 5.06276 3.01658 1 3 12 21 2.92843 4.77413 -2 3 12 21 2.92843 4.77413 1 3 12 21 3.97907 3.05149 2 4 12 21 6.76192 3.46955 2 4 12 21 20.8746 5.10623 1 4 12 21 29.2369 6.22447 -2 4 12 21 29.2369 6.22447 1 5 12 21 4.21802 3.21486 2 5 12 21 13.6939 4.27468 1 5 12 21 7.56579 4.87917 -2 5 12 21 7.56579 4.87917 1 6 12 21 10.2563 3.75328 1 6 12 21 3.22607 2.68628 2 6 12 21 6.02679 4.61647 -2 6 12 21 6.02679 4.61647 1 7 12 21 64.2457 7.54855 -2 7 12 21 64.2457 7.54855 1 3 13 21 12.8365 3.96089 2 3 13 21 47.0128 6.54438 -2 3 13 21 47.0128 6.54438 1 3 13 21 34.4822 5.98523 1 4 13 21 2.51030 4.38429 -2 4 13 21 2.51030 4.38429 1 4 13 21 5.49330 3.25793 1 4 13 21 2.75081 3.14674 2 5 13 21 54.9760 7.26202 -2 5 13 21 54.9760 7.26202 1 5 13 21 11.9040 3.75115 2 5 13 21 44.1768 7.02215 1 4 9 22 -1.1841 2.64422 2 4 9 22 9.46702 4.54453 1 0 0 0 0.00 0.00 0 ; _shelx_hkl_checksum 46446 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 0.60150(4) 0.38370(4) 0.69669(3) 0.01454(12) Uani 1 1 d . . . . . O1 O 0.4054(3) 0.4441(3) 0.5900(2) 0.0457(9) Uani 1 1 d . . . . . N1 N 0.4850(3) 0.4317(2) 0.7974(2) 0.0161(5) Uani 1 1 d . . . . . N2 N 0.5368(3) 0.2366(2) 0.7738(2) 0.0154(5) Uani 1 1 d . . . . . N3 N 0.7254(3) 0.3332(2) 0.6000(2) 0.0162(5) Uani 1 1 d . . . . . N4 N 0.6754(3) 0.5276(2) 0.6242(2) 0.0165(5) Uani 1 1 d . . . . . N5 N 0.7421(3) 0.3347(2) 0.7716(2) 0.0176(6) Uani 1 1 d . . . . . N6 N 0.8918(3) 0.2286(3) 0.8504(3) 0.0267(7) Uani 1 1 d . . . . . H6 H 0.938(4) 0.175(4) 0.873(3) 0.032 Uiso 1 1 d . U . . . N7 N 0.4860(3) 0.4212(2) 0.6336(2) 0.0196(6) Uani 1 1 d . . . . . C1 C 0.4637(3) 0.5348(3) 0.7912(3) 0.0182(6) Uani 1 1 d . . . . . C2 C 0.3573(3) 0.5415(3) 0.8696(3) 0.0196(7) Uani 1 1 d . . . . . C3 C 0.3139(3) 0.4415(3) 0.9225(2) 0.0180(6) Uani 1 1 d . . . . . C4 C 0.3941(3) 0.3739(3) 0.8769(2) 0.0165(6) Uani 1 1 d . . . . . C5 C 0.3771(3) 0.2665(3) 0.9071(2) 0.0180(6) Uani 1 1 d . . . . . H5 H 0.314906 0.233958 0.965639 0.022 Uiso 1 1 calc R U . . . C6 C 0.4432(3) 0.2027(3) 0.8590(2) 0.0165(6) Uani 1 1 d . . . . . C7 C 0.4213(3) 0.0917(3) 0.8905(2) 0.0169(6) Uani 1 1 d . . . . . C8 C 0.5034(3) 0.0587(3) 0.8225(2) 0.0184(6) Uani 1 1 d . . . . . C9 C 0.5729(3) 0.1498(3) 0.7500(2) 0.0182(6) Uani 1 1 d . . . . . C10 C 0.6609(3) 0.1505(3) 0.6668(2) 0.0189(7) Uani 1 1 d . . . . . H10 H 0.676284 0.086029 0.657573 0.023 Uiso 1 1 calc R U . . . C11 C 0.7285(3) 0.2363(3) 0.5961(2) 0.0177(6) Uani 1 1 d . . . . . C12 C 0.8150(3) 0.2357(3) 0.5075(2) 0.0188(7) Uani 1 1 d . . . . . C13 C 0.8668(3) 0.3328(3) 0.4584(2) 0.0189(7) Uani 1 1 d . . . . . C14 C 0.8110(3) 0.3932(3) 0.5172(2) 0.0173(6) Uani 1 1 d . . . . . C15 C 0.8364(3) 0.4971(3) 0.4912(2) 0.0179(6) Uani 1 1 d . . . . . H15 H 0.904419 0.527382 0.436077 0.021 Uiso 1 1 calc R U . . . C16 C 0.7700(3) 0.5605(3) 0.5396(2) 0.0172(6) Uani 1 1 d . . . . . C17 C 0.7832(3) 0.6740(3) 0.5029(2) 0.0185(6) Uani 1 1 d . . . . . C18 C 0.6941(3) 0.7101(3) 0.5654(3) 0.0197(7) Uani 1 1 d . . . . . C19 C 0.6283(3) 0.6183(3) 0.6409(2) 0.0183(6) Uani 1 1 d . . . . . C20 C 0.5301(3) 0.6209(3) 0.7192(2) 0.0194(7) Uani 1 1 d . . . . . H20 H 0.506481 0.688029 0.723661 0.023 Uiso 1 1 calc R U . . . C21 C 0.3048(3) 0.6420(3) 0.8847(3) 0.0236(7) Uani 1 1 d . . . . . H21A H 0.210634 0.636232 0.918239 0.028 Uiso 1 1 calc R U . . . H21B H 0.308926 0.703656 0.820590 0.028 Uiso 1 1 calc R U . . . C22 C 0.3801(4) 0.6646(3) 0.9440(3) 0.0311(9) Uani 1 1 d . . . . . H22A H 0.382105 0.601928 1.005893 0.047 Uiso 1 1 d R U . . . H22B H 0.335794 0.727018 0.956502 0.047 Uiso 1 1 d R U . . . H22C H 0.470805 0.679228 0.907553 0.047 Uiso 1 1 d R U . . . C23 C 0.2017(3) 0.4075(3) 1.0093(3) 0.0212(7) Uani 1 1 d . . . . . H23A H 0.158242 0.351500 1.007698 0.025 Uiso 1 1 calc R U . . . H23B H 0.135763 0.469825 1.003759 0.025 Uiso 1 1 calc R U . . . C24 C 0.2412(4) 0.3640(4) 1.1072(3) 0.0300(8) Uani 1 1 d . . . . . H24A H 0.300320 0.298252 1.116242 0.045 Uiso 1 1 d R U . . . H24B H 0.161810 0.347952 1.159131 0.045 Uiso 1 1 d R U . . . H24C H 0.286870 0.417762 1.108991 0.045 Uiso 1 1 d R U . . . C25 C 0.3202(3) 0.0303(3) 0.9759(2) 0.0200(7) Uani 1 1 d . . . . . H25A H 0.314381 0.051224 1.029469 0.024 Uiso 1 1 calc R U . . . H25B H 0.348336 -0.047374 0.998537 0.024 Uiso 1 1 calc R U . . . C26 C 0.1843(3) 0.0513(3) 0.9508(3) 0.0258(8) Uani 1 1 d . . . . . H26A H 0.159653 0.128809 0.923164 0.039 Uiso 1 1 d R U . . . H26B H 0.118713 0.016059 1.009724 0.039 Uiso 1 1 d R U . . . H26C H 0.187243 0.022759 0.903424 0.039 Uiso 1 1 d R U . . . C27 C 0.5210(4) -0.0495(3) 0.8200(3) 0.0231(7) Uani 1 1 d . . . . . H27A H 0.491435 -0.104106 0.886427 0.028 Uiso 1 1 calc R U . . . H27B H 0.616203 -0.067600 0.798394 0.028 Uiso 1 1 calc R U . . . C28 C 0.4439(4) -0.0546(3) 0.7523(3) 0.0289(8) Uani 1 1 d . . . . . H28A H 0.349088 -0.040303 0.775125 0.043 Uiso 1 1 d R U . . . H28B H 0.460888 -0.126162 0.752295 0.043 Uiso 1 1 d R U . . . H28C H 0.472428 -0.000653 0.686335 0.043 Uiso 1 1 d R U . . . C29 C 0.8295(3) 0.1470(3) 0.4759(3) 0.0223(7) Uani 1 1 d . . . . . H29A H 0.848067 0.077711 0.529694 0.027 Uiso 1 1 calc R U . . . H29B H 0.905571 0.157638 0.420434 0.027 Uiso 1 1 calc R U . . . C30 C 0.7040(4) 0.1429(3) 0.4457(3) 0.0276(8) Uani 1 1 d . . . . . H30A H 0.628539 0.132675 0.500437 0.041 Uiso 1 1 d R U . . . H30B H 0.716009 0.083065 0.426737 0.041 Uiso 1 1 d R U . . . H30C H 0.687499 0.210396 0.390777 0.041 Uiso 1 1 d R U . . . C31 C 0.9512(3) 0.3758(3) 0.3584(3) 0.0236(7) Uani 1 1 d . . . . . H31A H 1.011843 0.316604 0.347576 0.028 Uiso 1 1 calc R U . . . H31B H 1.005623 0.429910 0.352226 0.028 Uiso 1 1 calc R U . . . C32 C 0.8665(4) 0.4270(4) 0.2813(3) 0.0348(10) Uani 1 1 d . . . . . H32A H 0.805471 0.376062 0.291819 0.052 Uiso 1 1 d R U . . . H32B H 0.923952 0.446052 0.216749 0.052 Uiso 1 1 d R U . . . H32C H 0.815901 0.491832 0.286059 0.052 Uiso 1 1 d R U . . . C33 C 0.8687(3) 0.7394(3) 0.4084(3) 0.0224(7) Uani 1 1 d . . . . . H33A H 0.953222 0.696724 0.397591 0.027 Uiso 1 1 calc R U . . . H33B H 0.889135 0.804063 0.411428 0.027 Uiso 1 1 calc R U . . . C34 C 0.8003(4) 0.7737(4) 0.3230(3) 0.0319(9) Uani 1 1 d . . . . . H34A H 0.788213 0.710042 0.315697 0.048 Uiso 1 1 d R U . . . H34B H 0.855323 0.821232 0.263317 0.048 Uiso 1 1 d R U . . . H34C H 0.713953 0.811842 0.335607 0.048 Uiso 1 1 d R U . . . C35 C 0.6661(3) 0.8228(3) 0.5590(3) 0.0221(7) Uani 1 1 d . . . . . H35A H 0.570892 0.835025 0.585310 0.026 Uiso 1 1 calc R U . . . H35B H 0.685421 0.873893 0.489905 0.026 Uiso 1 1 calc R U . . . C36 C 0.7472(4) 0.8456(3) 0.6142(3) 0.0311(9) Uani 1 1 d . . . . . H36A H 0.732871 0.792527 0.681816 0.047 Uiso 1 1 d R U . . . H36B H 0.719691 0.917708 0.612206 0.047 Uiso 1 1 d R U . . . H36C H 0.841281 0.841317 0.583996 0.047 Uiso 1 1 d R U . . . C37 C 0.8024(4) 0.2366(3) 0.8007(3) 0.0270(8) Uani 1 1 d . . . . . H37 H 0.784766 0.180345 0.788137 0.032 Uiso 1 1 calc R U . . . C38 C 0.7981(3) 0.3910(3) 0.8041(2) 0.0194(7) Uani 1 1 d . . . . . H38 H 0.774570 0.464171 0.793190 0.023 Uiso 1 1 calc R U . . . C39 C 0.8917(3) 0.3258(3) 0.8540(3) 0.0207(7) Uani 1 1 d . . . . . C40 C 0.9789(4) 0.3413(3) 0.9060(3) 0.0281(8) Uani 1 1 d . . . . . H40A H 0.966160 0.286695 0.973032 0.042 Uiso 1 1 d R U . . . H40B H 0.957041 0.412825 0.906102 0.042 Uiso 1 1 d R U . . . H40C H 1.071390 0.334855 0.873202 0.042 Uiso 1 1 d R U . . . Sb1 Sb 1.00367(4) 0.91272(2) 0.78889(2) 0.01733(11) Uani 0.9595(19) 1 d D U P A 1 F1 F 0.9525(2) 1.03942(18) 0.81148(19) 0.0309(6) Uani 0.9595(19) 1 d D U P A 1 F2 F 1.1120(3) 0.8657(2) 0.87751(19) 0.0364(6) Uani 0.9595(19) 1 d D U P A 1 F3 F 1.1387(2) 0.9817(2) 0.68952(19) 0.0395(7) Uani 0.9595(19) 1 d D U P A 1 F4 F 1.0555(2) 0.78553(18) 0.76897(18) 0.0314(6) Uani 0.9595(19) 1 d D U P A 1 F5 F 0.8678(2) 0.8465(2) 0.88989(17) 0.0343(6) Uani 0.9595(19) 1 d D U P A 1 F6 F 0.8938(3) 0.9604(2) 0.70218(19) 0.0420(7) Uani 0.9595(19) 1 d D U P A 1 Sb1' Sb 0.944(2) 0.9261(11) 0.7774(10) 0.0303(19) Uani 0.0230(13) 1 d D U P B 2 F1' F 0.865(5) 1.055(2) 0.791(4) 0.030(5) Uani 0.0230(13) 1 d D U P B 2 F2' F 0.825(4) 0.845(4) 0.892(2) 0.026(5) Uani 0.0230(13) 1 d D U P B 2 F3' F 1.067(4) 0.910(4) 0.853(3) 0.029(3) Uani 0.0230(13) 1 d D U P B 2 F4' F 1.023(5) 0.798(2) 0.764(4) 0.027(4) Uani 0.0230(13) 1 d D U P B 2 F5' F 1.063(4) 1.007(4) 0.663(2) 0.031(4) Uani 0.0230(13) 1 d D U P B 2 F6' F 0.821(4) 0.942(4) 0.702(3) 0.035(5) Uani 0.0230(13) 1 d D U P B 2 Sb1" Sb 1.072(2) 0.9006(13) 0.8011(12) 0.028(2) Uani 0.0175(10) 1 d D U P C 3 F1" F 0.951(7) 1.016(4) 0.809(6) 0.025(4) Uani 0.0175(10) 1 d D U P C 3 F2" F 1.149(7) 0.872(6) 0.884(6) 0.026(5) Uani 0.0175(10) 1 d D U P C 3 F3" F 1.174(6) 0.980(5) 0.689(6) 0.028(5) Uani 0.0175(10) 1 d D U P C 3 F4" F 1.141(7) 0.767(4) 0.776(6) 0.027(5) Uani 0.0175(10) 1 d D U P C 3 F5" F 0.944(7) 0.911(7) 0.701(5) 0.030(3) Uani 0.0175(10) 1 d D U P C 3 F6" F 0.918(6) 0.803(5) 0.896(5) 0.029(5) Uani 0.0175(10) 1 d D U P C 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 0.0193(2) 0.0098(2) 0.0138(2) -0.00393(18) -0.00278(17) -0.00287(17) O1 0.0327(15) 0.062(2) 0.0376(18) -0.0095(17) -0.0183(14) -0.0053(15) N1 0.0212(13) 0.0109(13) 0.0156(13) -0.0050(11) -0.0024(10) -0.0030(10) N2 0.0200(13) 0.0107(13) 0.0137(13) -0.0041(11) -0.0005(10) -0.0041(10) N3 0.0204(13) 0.0116(13) 0.0150(13) -0.0045(11) -0.0014(10) -0.0034(10) N4 0.0227(13) 0.0098(13) 0.0152(13) -0.0032(11) -0.0024(10) -0.0042(10) N5 0.0229(13) 0.0114(13) 0.0173(14) -0.0048(11) -0.0025(11) -0.0044(11) N6 0.0290(16) 0.0134(15) 0.0377(19) -0.0058(14) -0.0167(14) 0.0002(12) N7 0.0190(13) 0.0177(15) 0.0192(14) -0.0057(12) -0.0003(11) -0.0052(11) C1 0.0235(16) 0.0123(15) 0.0204(17) -0.0077(13) -0.0061(13) -0.0002(12) C2 0.0245(16) 0.0164(16) 0.0193(17) -0.0095(14) -0.0042(13) 0.0000(13) C3 0.0226(15) 0.0158(16) 0.0181(16) -0.0087(13) -0.0051(12) -0.0013(13) C4 0.0196(15) 0.0148(16) 0.0160(15) -0.0070(13) -0.0038(12) -0.0014(12) C5 0.0234(16) 0.0151(16) 0.0134(15) -0.0042(13) -0.0019(12) -0.0041(13) C6 0.0217(15) 0.0118(15) 0.0144(15) -0.0031(12) -0.0037(12) -0.0037(12) C7 0.0208(15) 0.0125(15) 0.0166(16) -0.0042(13) -0.0048(12) -0.0031(12) C8 0.0239(16) 0.0122(15) 0.0182(16) -0.0049(13) -0.0039(12) -0.0041(12) C9 0.0227(15) 0.0131(15) 0.0188(16) -0.0059(13) -0.0042(12) -0.0039(12) C10 0.0248(16) 0.0132(15) 0.0190(16) -0.0078(13) -0.0017(13) -0.0034(13) C11 0.0206(15) 0.0153(16) 0.0183(16) -0.0081(13) -0.0031(12) -0.0019(12) C12 0.0220(15) 0.0181(17) 0.0174(16) -0.0092(14) -0.0019(12) -0.0024(13) C13 0.0208(15) 0.0180(17) 0.0172(16) -0.0073(14) -0.0029(12) -0.0011(13) C14 0.0190(15) 0.0154(16) 0.0143(15) -0.0039(13) -0.0020(11) -0.0018(12) C15 0.0179(15) 0.0164(16) 0.0157(15) -0.0029(13) -0.0024(12) -0.0045(12) C16 0.0198(15) 0.0146(16) 0.0157(15) -0.0029(13) -0.0053(12) -0.0043(12) C17 0.0222(15) 0.0136(15) 0.0183(16) -0.0036(13) -0.0057(12) -0.0038(12) C18 0.0262(16) 0.0118(15) 0.0203(17) -0.0036(13) -0.0067(13) -0.0046(13) C19 0.0229(16) 0.0128(15) 0.0176(16) -0.0035(13) -0.0047(12) -0.0042(12) C20 0.0252(16) 0.0119(15) 0.0205(17) -0.0062(13) -0.0057(13) 0.0000(13) C21 0.0256(17) 0.0165(17) 0.029(2) -0.0123(15) -0.0002(14) -0.0027(14) C22 0.039(2) 0.027(2) 0.034(2) -0.0204(19) -0.0023(17) -0.0061(17) C23 0.0260(17) 0.0179(17) 0.0195(17) -0.0097(14) 0.0004(13) -0.0041(13) C24 0.035(2) 0.035(2) 0.0217(19) -0.0122(17) -0.0012(15) -0.0114(17) C25 0.0283(17) 0.0133(16) 0.0160(16) -0.0042(13) -0.0014(13) -0.0053(13) C26 0.0278(18) 0.025(2) 0.0241(19) -0.0096(16) -0.0021(14) -0.0082(15) C27 0.0317(18) 0.0128(16) 0.0237(18) -0.0079(14) -0.0001(14) -0.0061(14) C28 0.036(2) 0.0222(19) 0.034(2) -0.0166(18) -0.0031(16) -0.0082(16) C29 0.0285(17) 0.0193(17) 0.0202(17) -0.0114(15) -0.0003(13) -0.0028(14) C30 0.037(2) 0.026(2) 0.0235(19) -0.0133(17) -0.0047(15) -0.0056(16) C31 0.0271(17) 0.0185(17) 0.0189(17) -0.0061(14) 0.0032(13) -0.0034(14) C32 0.047(2) 0.030(2) 0.0165(18) -0.0032(17) -0.0038(16) -0.0002(19) C33 0.0271(17) 0.0163(17) 0.0204(17) -0.0031(14) -0.0021(13) -0.0092(14) C34 0.041(2) 0.028(2) 0.0198(19) -0.0022(16) -0.0059(16) -0.0091(17) C35 0.0289(17) 0.0111(15) 0.0234(18) -0.0034(14) -0.0054(14) -0.0050(13) C36 0.039(2) 0.0195(19) 0.041(2) -0.0141(18) -0.0136(18) -0.0034(16) C37 0.0300(18) 0.0164(17) 0.038(2) -0.0113(17) -0.0145(16) 0.0004(14) C38 0.0262(16) 0.0135(15) 0.0196(17) -0.0075(13) -0.0052(13) -0.0017(13) C39 0.0252(16) 0.0182(17) 0.0181(17) -0.0068(14) -0.0030(13) -0.0044(13) C40 0.0342(19) 0.027(2) 0.026(2) -0.0108(17) -0.0098(16) -0.0041(16) Sb1 0.0213(2) 0.01197(13) 0.01727(13) -0.00574(9) -0.00201(10) -0.00173(11) F1 0.0417(13) 0.0148(11) 0.0326(13) -0.0119(10) 0.0010(10) -0.0011(10) F2 0.0456(15) 0.0259(13) 0.0424(15) -0.0103(12) -0.0259(12) 0.0009(11) F3 0.0437(15) 0.0294(14) 0.0356(14) -0.0137(12) 0.0150(12) -0.0134(12) F4 0.0412(14) 0.0203(12) 0.0342(13) -0.0164(11) -0.0026(11) -0.0007(10) F5 0.0368(13) 0.0284(13) 0.0337(14) -0.0157(11) 0.0120(11) -0.0141(11) F6 0.0510(15) 0.0393(16) 0.0408(15) -0.0147(13) -0.0281(13) 0.0062(13) Sb1' 0.034(3) 0.023(3) 0.027(3) -0.009(2) 0.003(3) -0.002(3) F1' 0.036(7) 0.019(6) 0.029(7) -0.011(6) 0.002(6) -0.001(6) F2' 0.031(7) 0.021(7) 0.028(6) -0.015(7) 0.009(6) -0.010(6) F3' 0.034(4) 0.021(4) 0.029(4) -0.010(4) -0.005(4) -0.001(4) F4' 0.034(5) 0.019(5) 0.027(5) -0.013(5) 0.001(5) 0.000(5) F5' 0.037(5) 0.025(5) 0.029(5) -0.012(5) -0.002(5) -0.003(5) F6' 0.042(6) 0.028(7) 0.033(6) -0.012(6) -0.008(6) 0.002(6) Sb1" 0.034(3) 0.023(3) 0.025(3) -0.012(3) 0.002(3) -0.002(3) F1" 0.033(5) 0.016(5) 0.026(5) -0.012(5) 0.000(5) -0.001(5) F2" 0.036(7) 0.021(7) 0.028(6) -0.014(6) -0.012(6) -0.001(6) F3" 0.034(7) 0.024(7) 0.027(6) -0.014(7) 0.006(6) -0.010(6) F4" 0.035(8) 0.019(7) 0.030(8) -0.016(7) -0.002(8) -0.002(7) F5" 0.037(5) 0.024(5) 0.030(4) -0.013(4) -0.005(4) 0.000(4) F6" 0.033(6) 0.021(6) 0.028(6) -0.010(6) 0.005(6) -0.006(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N7 Fe1 N5 178.21(13) . . ? N7 Fe1 N4 92.43(13) . . ? N5 Fe1 N4 88.66(12) . . ? N7 Fe1 N2 91.15(13) . . ? N5 Fe1 N2 87.75(11) . . ? N4 Fe1 N2 176.41(11) . . ? N7 Fe1 N3 90.86(13) . . ? N5 Fe1 N3 87.73(11) . . ? N4 Fe1 N3 89.69(12) . . ? N2 Fe1 N3 90.07(11) . . ? N7 Fe1 N1 92.12(13) . . ? N5 Fe1 N1 89.29(11) . . ? N4 Fe1 N1 90.22(12) . . ? N2 Fe1 N1 89.84(11) . . ? N3 Fe1 N1 177.02(11) . . ? C4 N1 C1 105.8(3) . . ? C4 N1 Fe1 127.1(2) . . ? C1 N1 Fe1 126.2(2) . . ? C6 N2 C9 105.6(3) . . ? C6 N2 Fe1 127.4(2) . . ? C9 N2 Fe1 126.9(2) . . ? C11 N3 C14 105.9(3) . . ? C11 N3 Fe1 126.4(2) . . ? C14 N3 Fe1 127.1(2) . . ? C16 N4 C19 105.6(3) . . ? C16 N4 Fe1 127.2(2) . . ? C19 N4 Fe1 126.7(2) . . ? C37 N5 C38 106.3(3) . . ? C37 N5 Fe1 124.4(2) . . ? C38 N5 Fe1 129.3(2) . . ? C37 N6 C39 109.5(3) . . ? C37 N6 H6 123(3) . . ? C39 N6 H6 128(3) . . ? O1 N7 Fe1 177.9(3) . . ? N1 C1 C20 125.4(3) . . ? N1 C1 C2 110.1(3) . . ? C20 C1 C2 124.5(3) . . ? C3 C2 C1 106.8(3) . . ? C3 C2 C21 128.1(3) . . ? C1 C2 C21 125.1(3) . . ? C2 C3 C4 106.6(3) . . ? C2 C3 C23 127.5(3) . . ? C4 C3 C23 125.9(3) . . ? N1 C4 C5 125.0(3) . . ? N1 C4 C3 110.7(3) . . ? C5 C4 C3 124.3(3) . . ? C6 C5 C4 125.5(3) . . ? C6 C5 H5 117.2 . . ? C4 C5 H5 117.2 . . ? N2 C6 C5 124.8(3) . . ? N2 C6 C7 110.6(3) . . ? C5 C6 C7 124.5(3) . . ? C8 C7 C6 106.3(3) . . ? C8 C7 C25 128.0(3) . . ? C6 C7 C25 125.6(3) . . ? C7 C8 C9 106.8(3) . . ? C7 C8 C27 128.6(3) . . ? C9 C8 C27 124.5(3) . . ? N2 C9 C10 124.8(3) . . ? N2 C9 C8 110.6(3) . . ? C10 C9 C8 124.6(3) . . ? C11 C10 C9 125.9(3) . . ? C11 C10 H10 117.1 . . ? C9 C10 H10 117.1 . . ? N3 C11 C10 125.2(3) . . ? N3 C11 C12 110.5(3) . . ? C10 C11 C12 124.3(3) . . ? C13 C12 C11 106.9(3) . . ? C13 C12 C29 128.8(3) . . ? C11 C12 C29 124.0(3) . . ? C12 C13 C14 106.5(3) . . ? C12 C13 C31 127.5(3) . . ? C14 C13 C31 125.6(3) . . ? N3 C14 C15 125.3(3) . . ? N3 C14 C13 110.2(3) . . ? C15 C14 C13 124.5(3) . . ? C14 C15 C16 124.9(3) . . ? C14 C15 H15 117.6 . . ? C16 C15 H15 117.6 . . ? N4 C16 C15 125.5(3) . . ? N4 C16 C17 110.4(3) . . ? C15 C16 C17 123.9(3) . . ? C18 C17 C16 106.8(3) . . ? C18 C17 C33 127.5(3) . . ? C16 C17 C33 125.4(3) . . ? C17 C18 C19 106.6(3) . . ? C17 C18 C35 128.1(3) . . ? C19 C18 C35 125.4(3) . . ? N4 C19 C20 124.5(3) . . ? N4 C19 C18 110.7(3) . . ? C20 C19 C18 124.8(3) . . ? C1 C20 C19 126.0(3) . . ? C1 C20 H20 117.0 . . ? C19 C20 H20 117.0 . . ? C2 C21 C22 113.8(3) . . ? C2 C21 H21A 108.8 . . ? C22 C21 H21A 108.8 . . ? C2 C21 H21B 108.8 . . ? C22 C21 H21B 108.8 . . ? H21A C21 H21B 107.7 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.4 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C3 C23 C24 115.0(3) . . ? C3 C23 H23A 108.5 . . ? C24 C23 H23A 108.5 . . ? C3 C23 H23B 108.5 . . ? C24 C23 H23B 108.5 . . ? H23A C23 H23B 107.5 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.4 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C7 C25 C26 111.6(3) . . ? C7 C25 H25A 109.3 . . ? C26 C25 H25A 109.3 . . ? C7 C25 H25B 109.3 . . ? C26 C25 H25B 109.3 . . ? H25A C25 H25B 108.0 . . ? C25 C26 H26A 109.4 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C8 C27 C28 113.0(3) . . ? C8 C27 H27A 109.0 . . ? C28 C27 H27A 109.0 . . ? C8 C27 H27B 109.0 . . ? C28 C27 H27B 109.0 . . ? H27A C27 H27B 107.8 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.4 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.6 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C12 C29 C30 111.6(3) . . ? C12 C29 H29A 109.3 . . ? C30 C29 H29A 109.3 . . ? C12 C29 H29B 109.3 . . ? C30 C29 H29B 109.3 . . ? H29A C29 H29B 108.0 . . ? C29 C30 H30A 109.4 . . ? C29 C30 H30B 109.6 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.4 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C13 C31 C32 111.1(3) . . ? C13 C31 H31A 109.4 . . ? C32 C31 H31A 109.4 . . ? C13 C31 H31B 109.4 . . ? C32 C31 H31B 109.4 . . ? H31A C31 H31B 108.0 . . ? C31 C32 H32A 109.6 . . ? C31 C32 H32B 109.4 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.4 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C17 C33 C34 111.5(3) . . ? C17 C33 H33A 109.3 . . ? C34 C33 H33A 109.3 . . ? C17 C33 H33B 109.3 . . ? C34 C33 H33B 109.3 . . ? H33A C33 H33B 108.0 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.4 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C18 C35 C36 113.0(3) . . ? C18 C35 H35A 109.0 . . ? C36 C35 H35A 109.0 . . ? C18 C35 H35B 109.0 . . ? C36 C35 H35B 109.0 . . ? H35A C35 H35B 107.8 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.4 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N5 C37 N6 109.9(3) . . ? N5 C37 H37 125.1 . . ? N6 C37 H37 125.1 . . ? C39 C38 N5 109.9(3) . . ? C39 C38 H38 125.1 . . ? N5 C38 H38 125.1 . . ? C38 C39 N6 104.4(3) . . ? C38 C39 C40 133.5(4) . . ? N6 C39 C40 122.1(3) . . ? C39 C40 H40A 109.6 . . ? C39 C40 H40B 109.4 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.4 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? F6 Sb1 F3 89.76(13) . . ? F6 Sb1 F5 90.74(12) . . ? F3 Sb1 F5 178.38(11) . . ? F6 Sb1 F2 179.00(12) . . ? F3 Sb1 F2 90.85(12) . . ? F5 Sb1 F2 88.63(12) . . ? F6 Sb1 F4 90.74(11) . . ? F3 Sb1 F4 91.32(11) . . ? F5 Sb1 F4 90.22(10) . . ? F2 Sb1 F4 90.03(11) . . ? F6 Sb1 F1 90.34(11) . . ? F3 Sb1 F1 89.15(10) . . ? F5 Sb1 F1 89.31(11) . . ? F2 Sb1 F1 88.88(10) . . ? F4 Sb1 F1 178.83(11) . . ? F4' Sb1' F6' 90.1(3) . . ? F4' Sb1' F2' 90.0(3) . . ? F6' Sb1' F2' 90.0(3) . . ? F4' Sb1' F5' 90.0(3) . . ? F6' Sb1' F5' 90.0(3) . . ? F2' Sb1' F5' 179.9(4) . . ? F4' Sb1' F1' 179.9(4) . . ? F6' Sb1' F1' 90.0(3) . . ? F2' Sb1' F1' 90.0(3) . . ? F5' Sb1' F1' 89.9(3) . . ? F4' Sb1' F3' 90.0(3) . . ? F6' Sb1' F3' 179.9(4) . . ? F2' Sb1' F3' 90.0(3) . . ? F5' Sb1' F3' 90.0(3) . . ? F1' Sb1' F3' 89.9(3) . . ? F2" Sb1" F3" 107(3) . . ? F2" Sb1" F1" 103(2) . . ? F3" Sb1" F1" 95.2(19) . . ? F2" Sb1" F4" 96.6(13) . . ? F3" Sb1" F4" 90.2(17) . . ? F1" Sb1" F4" 157(4) . . ? F2" Sb1" F6" 93(3) . . ? F3" Sb1" F6" 159(4) . . ? F1" Sb1" F6" 85.4(16) . . ? F4" Sb1" F6" 81.8(18) . . ? F2" Sb1" F5" 169(3) . . ? F3" Sb1" F5" 83(2) . . ? F1" Sb1" F5" 80.9(17) . . ? F4" Sb1" F5" 77.9(19) . . ? F6" Sb1" F5" 76.3(19) . . ? 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 N7 1.637(3) . ? Fe1 N5 1.969(3) . ? Fe1 N4 2.008(3) . ? Fe1 N2 2.009(3) . ? Fe1 N3 2.009(3) . ? Fe1 N1 2.010(3) . ? O1 N7 1.142(4) . ? N1 C4 1.375(4) . ? N1 C1 1.376(4) . ? N2 C6 1.377(4) . ? N2 C9 1.379(4) . ? N3 C11 1.374(4) . ? N3 C14 1.379(4) . ? N4 C16 1.376(4) . ? N4 C19 1.379(4) . ? N5 C37 1.323(4) . ? N5 C38 1.386(4) . ? N6 C37 1.337(5) . ? N6 C39 1.382(5) . ? N6 H6 0.80(5) . ? C1 C20 1.381(5) . ? C1 C2 1.450(5) . ? C2 C3 1.363(5) . ? C2 C21 1.501(5) . ? C3 C4 1.443(4) . ? C3 C23 1.503(5) . ? C4 C5 1.390(5) . ? C5 C6 1.387(5) . ? C5 H5 0.9500 . ? C6 C7 1.447(5) . ? C7 C8 1.373(5) . ? C7 C25 1.494(5) . ? C8 C9 1.440(5) . ? C8 C27 1.503(5) . ? C9 C10 1.382(5) . ? C10 C11 1.378(5) . ? C10 H10 0.9500 . ? C11 C12 1.447(4) . ? C12 C13 1.365(5) . ? C12 C29 1.493(5) . ? C13 C14 1.454(5) . ? C13 C31 1.497(5) . ? C14 C15 1.380(5) . ? C15 C16 1.386(5) . ? C15 H15 0.9500 . ? C16 C17 1.447(5) . ? C17 C18 1.364(5) . ? C17 C33 1.500(5) . ? C18 C19 1.443(5) . ? C18 C35 1.504(5) . ? C19 C20 1.388(5) . ? C20 H20 0.9500 . ? C21 C22 1.533(5) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.526(5) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9799 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.527(5) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9801 . ? C26 H26B 0.9799 . ? C26 H26C 0.9798 . ? C27 C28 1.531(5) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9800 . ? C28 H28B 0.9801 . ? C28 H28C 0.9800 . ? C29 C30 1.537(5) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.530(5) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9799 . ? C33 C34 1.538(5) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9801 . ? C34 H34C 0.9799 . ? C35 C36 1.527(5) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37 0.9500 . ? C38 C39 1.362(5) . ? C38 H38 0.9500 . ? C39 C40 1.481(5) . ? C40 H40A 0.9800 . ? C40 H40B 0.9799 . ? C40 H40C 0.9801 . ? Sb1 F6 1.840(2) . ? Sb1 F3 1.842(2) . ? Sb1 F5 1.847(2) . ? Sb1 F2 1.851(2) . ? Sb1 F4 1.890(2) . ? Sb1 F1 1.904(2) . ? Sb1' F4' 1.901(4) . ? Sb1' F6' 1.902(4) . ? Sb1' F2' 1.902(4) . ? Sb1' F5' 1.902(4) . ? Sb1' F1' 1.903(4) . ? Sb1' F3' 1.903(4) . ? Sb1" F2" 1.58(6) . ? Sb1" F3" 1.79(6) . ? Sb1" F1" 1.882(4) . ? Sb1" F4" 2.03(3) . ? Sb1" F6" 2.11(6) . ? Sb1" F5" 2.28(6) . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag N6 H6 F1^a 0.80(5) 2.44(5) 2.884(4) 117(4) 1_545 yes C5 H5 F5^a 0.95 2.52 3.466(4) 174.0 2_667 yes C5 H5 F2'^b 0.95 2.25 3.200(16) 177.5 2_667 yes C10 H10 F6'^b 0.95 2.24 2.97(5) 133.0 1_545 yes C37 H37 F1^a 0.95 2.34 2.855(4) 113.3 1_545 yes C37 H37 F1'^b 0.95 1.78 2.558(17) 136.8 1_545 yes C37 H37 F1"^c 0.95 2.55 3.14(2) 119.7 1_545 yes C40 H40A F2^a 0.98 2.43 3.383(5) 162.8 2_767 yes C40 H40A F2"^c 0.98 2.57 3.47(9) 152.8 2_767 yes C40 H40A F6"^c 0.98 2.40 3.21(7) 139.9 2_767 yes 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 C4 N1 C1 C20 -177.3(3) . . . . ? Fe1 N1 C1 C20 -7.4(5) . . . . ? C4 N1 C1 C2 0.5(3) . . . . ? Fe1 N1 C1 C2 170.3(2) . . . . ? N1 C1 C2 C3 -0.5(4) . . . . ? C20 C1 C2 C3 177.3(3) . . . . ? N1 C1 C2 C21 -178.6(3) . . . . ? C20 C1 C2 C21 -0.8(5) . . . . ? C1 C2 C3 C4 0.2(4) . . . . ? C21 C2 C3 C4 178.3(3) . . . . ? C1 C2 C3 C23 -177.6(3) . . . . ? C21 C2 C3 C23 0.4(6) . . . . ? C1 N1 C4 C5 177.0(3) . . . . ? Fe1 N1 C4 C5 7.2(5) . . . . ? C1 N1 C4 C3 -0.3(3) . . . . ? Fe1 N1 C4 C3 -170.1(2) . . . . ? C2 C3 C4 N1 0.0(4) . . . . ? C23 C3 C4 N1 178.0(3) . . . . ? C2 C3 C4 C5 -177.3(3) . . . . ? C23 C3 C4 C5 0.6(5) . . . . ? N1 C4 C5 C6 -4.0(5) . . . . ? C3 C4 C5 C6 173.0(3) . . . . ? C9 N2 C6 C5 -177.9(3) . . . . ? Fe1 N2 C6 C5 -0.4(5) . . . . ? C9 N2 C6 C7 0.9(3) . . . . ? Fe1 N2 C6 C7 178.4(2) . . . . ? C4 C5 C6 N2 0.4(5) . . . . ? C4 C5 C6 C7 -178.2(3) . . . . ? N2 C6 C7 C8 0.0(4) . . . . ? C5 C6 C7 C8 178.7(3) . . . . ? N2 C6 C7 C25 -175.5(3) . . . . ? C5 C6 C7 C25 3.3(5) . . . . ? C6 C7 C8 C9 -0.8(3) . . . . ? C25 C7 C8 C9 174.5(3) . . . . ? C6 C7 C8 C27 179.6(3) . . . . ? C25 C7 C8 C27 -5.1(6) . . . . ? C6 N2 C9 C10 177.1(3) . . . . ? Fe1 N2 C9 C10 -0.4(5) . . . . ? C6 N2 C9 C8 -1.5(3) . . . . ? Fe1 N2 C9 C8 -178.9(2) . . . . ? C7 C8 C9 N2 1.5(4) . . . . ? C27 C8 C9 N2 -179.0(3) . . . . ? C7 C8 C9 C10 -177.0(3) . . . . ? C27 C8 C9 C10 2.5(5) . . . . ? N2 C9 C10 C11 1.6(5) . . . . ? C8 C9 C10 C11 179.9(3) . . . . ? C14 N3 C11 C10 177.4(3) . . . . ? Fe1 N3 C11 C10 -10.7(5) . . . . ? C14 N3 C11 C12 -1.7(4) . . . . ? Fe1 N3 C11 C12 170.2(2) . . . . ? C9 C10 C11 N3 4.3(6) . . . . ? C9 C10 C11 C12 -176.7(3) . . . . ? N3 C11 C12 C13 1.3(4) . . . . ? C10 C11 C12 C13 -177.8(3) . . . . ? N3 C11 C12 C29 -173.3(3) . . . . ? C10 C11 C12 C29 7.6(5) . . . . ? C11 C12 C13 C14 -0.3(4) . . . . ? C29 C12 C13 C14 173.9(3) . . . . ? C11 C12 C13 C31 -173.5(3) . . . . ? C29 C12 C13 C31 0.7(6) . . . . ? C11 N3 C14 C15 179.0(3) . . . . ? Fe1 N3 C14 C15 7.1(5) . . . . ? C11 N3 C14 C13 1.5(3) . . . . ? Fe1 N3 C14 C13 -170.4(2) . . . . ? C12 C13 C14 N3 -0.7(4) . . . . ? C31 C13 C14 N3 172.6(3) . . . . ? C12 C13 C14 C15 -178.3(3) . . . . ? C31 C13 C14 C15 -4.9(5) . . . . ? N3 C14 C15 C16 -6.7(5) . . . . ? C13 C14 C15 C16 170.4(3) . . . . ? C19 N4 C16 C15 -174.7(3) . . . . ? Fe1 N4 C16 C15 -3.3(5) . . . . ? C19 N4 C16 C17 0.5(3) . . . . ? Fe1 N4 C16 C17 171.9(2) . . . . ? C14 C15 C16 N4 4.7(5) . . . . ? C14 C15 C16 C17 -169.8(3) . . . . ? N4 C16 C17 C18 -0.9(4) . . . . ? C15 C16 C17 C18 174.3(3) . . . . ? N4 C16 C17 C33 -174.9(3) . . . . ? C15 C16 C17 C33 0.4(5) . . . . ? C16 C17 C18 C19 0.9(4) . . . . ? C33 C17 C18 C19 174.7(3) . . . . ? C16 C17 C18 C35 -178.5(3) . . . . ? C33 C17 C18 C35 -4.7(6) . . . . ? C16 N4 C19 C20 179.6(3) . . . . ? Fe1 N4 C19 C20 8.1(5) . . . . ? C16 N4 C19 C18 0.1(3) . . . . ? Fe1 N4 C19 C18 -171.4(2) . . . . ? C17 C18 C19 N4 -0.7(4) . . . . ? C35 C18 C19 N4 178.8(3) . . . . ? C17 C18 C19 C20 179.9(3) . . . . ? C35 C18 C19 C20 -0.7(5) . . . . ? N1 C1 C20 C19 0.5(6) . . . . ? C2 C1 C20 C19 -176.9(3) . . . . ? N4 C19 C20 C1 -0.8(5) . . . . ? C18 C19 C20 C1 178.6(3) . . . . ? C3 C2 C21 C22 95.4(4) . . . . ? C1 C2 C21 C22 -86.9(4) . . . . ? C2 C3 C23 C24 -92.9(4) . . . . ? C4 C3 C23 C24 89.6(4) . . . . ? C8 C7 C25 C26 -91.6(4) . . . . ? C6 C7 C25 C26 82.8(4) . . . . ? C7 C8 C27 C28 99.4(4) . . . . ? C9 C8 C27 C28 -80.1(4) . . . . ? C13 C12 C29 C30 -103.7(4) . . . . ? C11 C12 C29 C30 69.7(4) . . . . ? C12 C13 C31 C32 84.0(4) . . . . ? C14 C13 C31 C32 -87.9(4) . . . . ? C18 C17 C33 C34 -91.2(4) . . . . ? C16 C17 C33 C34 81.5(4) . . . . ? C17 C18 C35 C36 -92.7(4) . . . . ? C19 C18 C35 C36 87.9(4) . . . . ? C38 N5 C37 N6 0.7(4) . . . . ? Fe1 N5 C37 N6 -179.5(2) . . . . ? C39 N6 C37 N5 -0.4(5) . . . . ? C37 N5 C38 C39 -0.6(4) . . . . ? Fe1 N5 C38 C39 179.5(2) . . . . ? N5 C38 C39 N6 0.4(4) . . . . ? N5 C38 C39 C40 -178.2(4) . . . . ? C37 N6 C39 C38 0.0(4) . . . . ? C37 N6 C39 C40 178.8(4) . . . . ?