#------------------------------------------------------------------------------ #$Date: 2023-06-29 17:44:28 +0200 (Thu, 29 Jun 2023) $ #$Revision: 284691 $ #$URL: svn://www.crystallography.net/cod/cif/2/02/27/2022784.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2022784 loop_ _publ_author_name 'B\"utikofer, Andr\'e' 'Chen, Peter' _publ_section_title ; Cyclopentadienone triisocyanide iron complexes: general synthesis and crystal structures of tris(2,6-dimethylphenyl isocyanide)(\h4-tetraphenylcyclopentadienone)iron and tris(naphthalen-2-yl isocyanide)(\h4-tetraphenylcyclopentadienone)iron acetone hemisolvate ; _journal_coeditor_code MW2197 _journal_issue 7 _journal_name_full 'Acta Crystallographica Section E Crystallographic Communications' _journal_paper_doi 10.1107/S205698902300498X _journal_volume 79 _journal_year 2023 _chemical_absolute_configuration ad _chemical_formula_iupac '[Fe (C9 H9 N)3 (C29 H20 O)]' _chemical_formula_moiety 'C56 H47 Fe N3 O' _chemical_formula_sum 'C56 H47 Fe N3 O' _chemical_formula_weight 833.81 _chemical_name_systematic ; Tris(2,6-dimethylphenyl isocyanide)(\h^4^-tetraphenylcyclopentadienone)iron ; _space_group_crystal_system orthorhombic _space_group_IT_number 29 _space_group_name_Hall 'P 2c -2ac' _space_group_name_H-M_alt 'P c a 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_method ; Olex2 1.5 (compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498) ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 16.7473(3) _cell_length_b 12.1998(2) _cell_length_c 20.9668(4) _cell_measurement_reflns_used 11706 _cell_measurement_temperature 100.00(10) _cell_measurement_theta_max 79.3330 _cell_measurement_theta_min 3.6120 _cell_volume 4283.80(13) _computing_cell_refinement ; CrysAlisPro 1.171.41.119a (Rigaku OD, 2021) ; _computing_data_collection ; CrysAlisPro 1.171.41.119a (Rigaku OD, 2021) ; _computing_data_reduction ; CrysAlisPro 1.171.41.119a (Rigaku OD, 2021) ; _computing_molecular_graphics ; Olex2 1.5 (Dolomanov et al., 2009) ; _computing_publication_material ; Mercury (Macrae et al., 2020) ; _computing_structure_refinement ; SHELXL2018/3 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 100.00(10) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 5.8140 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.985 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, Pilatus 300K' _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_R_equivalents 0.0810 _diffrn_reflns_av_unetI/netI 0.0602 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 33622 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 80.118 _diffrn_reflns_theta_min 3.623 _diffrn_source 'micro-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 3.164 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.697 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; (CrysAlisPro; Rigaku OD, 2021) ; _exptl_crystal_colour 'clear yellow' _exptl_crystal_density_diffrn 1.293 _exptl_crystal_description needle _exptl_crystal_F_000 1752 _exptl_crystal_size_max 0.141 _exptl_crystal_size_mid 0.032 _exptl_crystal_size_min 0.023 _refine_diff_density_max 0.362 _refine_diff_density_min -0.402 _refine_ls_abs_structure_details ; Flack x determined using 1989 quotients [(I^+^)-(I^-^)]/[(I^+^)+(I^-^)] (Parsons et al., 2013) ; _refine_ls_abs_structure_Flack -0.008(4) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 556 _refine_ls_number_reflns 7440 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.048 _refine_ls_R_factor_all 0.0514 _refine_ls_R_factor_gt 0.0422 _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^)+(0.0630P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1041 _refine_ls_wR_factor_ref 0.1093 _reflns_number_gt 6449 _reflns_number_total 7440 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL c130922_1_1_a.res in Pca2(1) c130922_1_1.res created by SHELXL-2018/3 at 15:08:09 on 14-Sep-2022 REM Old TITL c130922_1_1 in Pca2(1) REM SHELXT solution in Pca2(1) REM R1 0.088, Rweak 0.018, Alpha 0.004, Orientation as input REM Flack x = 0.016 ( 0.005 ) from Parsons' quotients REM Formula found by SHELXT: C55 N4 O Fe CELL 1.54184 16.7473 12.1998 20.9668 90 90 90 ZERR 4 0.0003 0.0002 0.0004 0 0 0 LATT -1 SYMM -X,-Y,0.5+Z SYMM 0.5+X,-Y,+Z SYMM 0.5-X,+Y,0.5+Z SFAC C H Fe N O UNIT 224 188 4 12 4 L.S. 9 PLAN 20 SIZE 0.02 0.03 0.14 TEMP -173 CONF BOND $H list 4 fmap 2 ACTA MORE -1 REM REM REM WGHT 0.063000 FVAR 0.41837 FE1 3 0.442119 0.297274 0.490250 11.00000 0.02225 0.01678 = 0.02004 0.00037 0.00030 -0.00091 O1 5 0.340977 0.178537 0.370471 11.00000 0.03100 0.02164 = 0.02148 -0.00117 -0.00228 0.00053 N1 4 0.546609 0.220813 0.382175 11.00000 0.02608 0.02585 = 0.02560 -0.00197 0.00449 -0.00007 N2 4 0.540083 0.220412 0.601279 11.00000 0.02519 0.02786 = 0.03028 0.00701 -0.00117 -0.00204 N3 4 0.518439 0.518345 0.486774 11.00000 0.02876 0.02033 = 0.02733 0.00106 -0.00065 -0.00422 C1 1 0.507230 0.248384 0.424916 11.00000 0.02494 0.01882 = 0.03409 0.00250 -0.00807 -0.00276 C2 1 0.503077 0.250357 0.557334 11.00000 0.02696 0.01810 = 0.02734 -0.00103 -0.00015 -0.00326 C3 1 0.488585 0.432543 0.489847 11.00000 0.02622 0.02593 = 0.01972 0.00067 -0.00095 0.00187 C4 1 0.341837 0.225041 0.423219 11.00000 0.01971 0.02074 = 0.02537 -0.00270 -0.00086 -0.00027 C5 1 0.353405 0.172428 0.485877 11.00000 0.01876 0.01718 = 0.02703 -0.00383 0.00101 -0.00260 C6 1 0.335502 0.250173 0.535393 11.00000 0.01771 0.01897 = 0.02293 0.00096 0.00097 -0.00170 C7 1 0.328186 0.356533 0.505427 11.00000 0.02187 0.01922 = 0.02143 -0.00095 -0.00088 0.00022 C8 1 0.338109 0.344227 0.437881 11.00000 0.01953 0.01792 = 0.02587 0.00023 -0.00521 0.00136 C9 1 0.360003 0.051577 0.493286 11.00000 0.02896 0.02016 = 0.02065 -0.00039 -0.00472 -0.00104 C10 1 0.415368 -0.008687 0.458730 11.00000 0.02960 0.02177 = 0.02956 -0.00440 -0.00227 -0.00138 AFIX 43 H10 2 0.451113 0.028206 0.430856 11.00000 -1.20000 AFIX 0 C11 1 0.419444 -0.122132 0.464187 11.00000 0.04094 0.02355 = 0.03655 -0.00794 -0.00898 0.00627 AFIX 43 H11 2 0.457570 -0.161958 0.439927 11.00000 -1.20000 AFIX 0 C12 1 0.368068 -0.177381 0.504909 11.00000 0.05339 0.01821 = 0.03507 0.00198 -0.01571 0.00183 AFIX 43 H12 2 0.371492 -0.254748 0.509268 11.00000 -1.20000 AFIX 0 C13 1 0.311631 -0.118618 0.539216 11.00000 0.05329 0.02308 = 0.02369 0.00260 -0.00362 -0.00799 AFIX 43 H13 2 0.275669 -0.155950 0.566711 11.00000 -1.20000 AFIX 0 C14 1 0.307587 -0.005487 0.533466 11.00000 0.03856 0.02483 = 0.02562 -0.00303 0.00005 -0.00595 AFIX 43 H14 2 0.268673 0.033951 0.557136 11.00000 -1.20000 AFIX 0 C15 1 0.317531 0.225753 0.603145 11.00000 0.02352 0.01849 = 0.02527 -0.00188 -0.00212 -0.00403 C16 1 0.363501 0.155473 0.640503 11.00000 0.02702 0.02224 = 0.02573 0.00078 0.00069 -0.00216 AFIX 43 H16 2 0.410074 0.122967 0.622858 11.00000 -1.20000 AFIX 0 C17 1 0.342362 0.132118 0.703161 11.00000 0.03501 0.02486 = 0.02669 0.00347 -0.00332 -0.00609 AFIX 43 H17 2 0.375556 0.086079 0.728307 11.00000 -1.20000 AFIX 0 C18 1 0.273342 0.175451 0.729130 11.00000 0.03848 0.02780 = 0.01963 -0.00189 0.00474 -0.00893 AFIX 43 H18 2 0.258942 0.159492 0.771960 11.00000 -1.20000 AFIX 0 C19 1 0.225281 0.242651 0.691801 11.00000 0.03036 0.02582 = 0.02889 -0.00470 0.00598 -0.00295 AFIX 43 H19 2 0.176829 0.270689 0.708802 11.00000 -1.20000 AFIX 0 C20 1 0.247485 0.269160 0.629864 11.00000 0.02442 0.02172 = 0.02627 0.00042 0.00180 -0.00172 AFIX 43 H20 2 0.214970 0.317101 0.605363 11.00000 -1.20000 AFIX 0 C21 1 0.301963 0.456005 0.541316 11.00000 0.02548 0.01696 = 0.02627 0.00065 0.00033 -0.00300 C22 1 0.343152 0.493136 0.595016 11.00000 0.03234 0.02302 = 0.02367 0.00154 0.00029 -0.00083 AFIX 43 H22 2 0.392299 0.459712 0.606579 11.00000 -1.20000 AFIX 0 C23 1 0.313033 0.578465 0.631738 11.00000 0.04402 0.01978 = 0.02496 -0.00161 0.00551 -0.00574 AFIX 43 H23 2 0.341359 0.602888 0.668332 11.00000 -1.20000 AFIX 0 C24 1 0.241056 0.628212 0.614730 11.00000 0.04636 0.01876 = 0.03165 -0.00391 0.01601 -0.00065 AFIX 43 H24 2 0.219540 0.685330 0.640286 11.00000 -1.20000 AFIX 0 C25 1 0.201126 0.593881 0.560380 11.00000 0.03062 0.02547 = 0.03801 0.00410 0.00824 0.00199 AFIX 43 H25 2 0.153037 0.629211 0.547934 11.00000 -1.20000 AFIX 0 C26 1 0.231083 0.508119 0.524058 11.00000 0.02715 0.02084 = 0.03258 0.00173 0.00050 0.00172 AFIX 43 H26 2 0.203041 0.484711 0.487102 11.00000 -1.20000 AFIX 0 C27 1 0.328615 0.431840 0.389819 11.00000 0.02311 0.02345 = 0.02580 -0.00016 0.00330 -0.00059 C28 1 0.341998 0.543382 0.404616 11.00000 0.03422 0.02192 = 0.02802 0.00105 0.00007 0.00010 AFIX 43 H28 2 0.363307 0.562470 0.445112 11.00000 -1.20000 AFIX 0 C29 1 0.324561 0.625302 0.361057 11.00000 0.04491 0.01888 = 0.02874 0.00295 -0.00172 0.00084 AFIX 43 H29 2 0.332359 0.699903 0.372456 11.00000 -1.20000 AFIX 0 C30 1 0.295882 0.599280 0.301090 11.00000 0.05659 0.02602 = 0.03171 0.00893 -0.00459 0.00505 AFIX 43 H30 2 0.283663 0.655662 0.271401 11.00000 -1.20000 AFIX 0 C31 1 0.285085 0.489873 0.284625 11.00000 0.05237 0.03038 = 0.02298 0.00324 -0.00529 0.00191 AFIX 43 H31 2 0.266627 0.471371 0.243156 11.00000 -1.20000 AFIX 0 C32 1 0.301139 0.407613 0.328464 11.00000 0.03401 0.02271 = 0.02486 -0.00261 -0.00063 0.00288 AFIX 43 H32 2 0.293296 0.333263 0.316540 11.00000 -1.20000 AFIX 0 C33 1 0.593276 0.190104 0.330202 11.00000 0.02789 0.02097 = 0.02480 -0.00223 0.00506 -0.00306 C34 1 0.566494 0.214837 0.268780 11.00000 0.03576 0.02277 = 0.02497 -0.00350 -0.00006 -0.00295 C35 1 0.488224 0.271649 0.259186 11.00000 0.04315 0.03910 = 0.03601 0.00129 -0.00667 0.00510 AFIX 137 H35A 2 0.446900 0.234730 0.284361 11.00000 -1.50000 H35B 2 0.473743 0.269284 0.213920 11.00000 -1.50000 H35C 2 0.492766 0.348139 0.272994 11.00000 -1.50000 AFIX 0 C36 1 0.615421 0.183198 0.218033 11.00000 0.05174 0.02858 = 0.02845 -0.00406 0.00635 -0.01154 AFIX 43 H36 2 0.598949 0.197116 0.175438 11.00000 -1.20000 AFIX 0 C37 1 0.687825 0.131645 0.229369 11.00000 0.04788 0.03128 = 0.04254 -0.00979 0.02213 -0.00507 AFIX 43 H37 2 0.721016 0.112063 0.194436 11.00000 -1.20000 AFIX 0 C38 1 0.712200 0.108501 0.290525 11.00000 0.03150 0.02830 = 0.05110 -0.00830 0.00856 -0.00119 AFIX 43 H38 2 0.761845 0.072581 0.297136 11.00000 -1.20000 AFIX 0 C39 1 0.665769 0.136554 0.342631 11.00000 0.02815 0.02341 = 0.03793 -0.00369 0.00270 0.00021 C40 1 0.690938 0.112744 0.409943 11.00000 0.04332 0.04318 = 0.04538 -0.00202 -0.01017 0.00837 AFIX 137 H40A 2 0.697759 0.181828 0.433163 11.00000 -1.50000 H40B 2 0.741584 0.072510 0.409616 11.00000 -1.50000 H40C 2 0.649900 0.068351 0.430990 11.00000 -1.50000 AFIX 0 C41 1 0.556821 0.177745 0.661976 11.00000 0.02357 0.02890 = 0.02638 0.00228 -0.00381 -0.00148 C42 1 0.580499 0.068158 0.665803 11.00000 0.02342 0.02964 = 0.03484 0.00509 -0.00504 0.00010 C43 1 0.593492 0.000910 0.607388 11.00000 0.05014 0.03172 = 0.04762 -0.00646 -0.00336 0.00781 AFIX 137 H43A 2 0.541778 -0.021491 0.589824 11.00000 -1.50000 H43B 2 0.624754 -0.064352 0.618305 11.00000 -1.50000 H43C 2 0.622491 0.044347 0.575618 11.00000 -1.50000 AFIX 0 C44 1 0.588829 0.022830 0.726356 11.00000 0.03309 0.03671 = 0.04931 0.01607 -0.00903 -0.00574 AFIX 43 H44 2 0.604670 -0.051553 0.730785 11.00000 -1.20000 AFIX 0 C45 1 0.574163 0.085501 0.780242 11.00000 0.03409 0.07459 = 0.02923 0.01433 -0.00692 -0.00892 AFIX 43 H45 2 0.579116 0.053327 0.821313 11.00000 -1.20000 AFIX 0 C46 1 0.552385 0.194443 0.774756 11.00000 0.03752 0.06911 = 0.02911 -0.01239 -0.00549 0.00349 AFIX 43 H46 2 0.543125 0.236364 0.812217 11.00000 -1.20000 AFIX 0 C47 1 0.543863 0.243379 0.715643 11.00000 0.03179 0.04217 = 0.03162 -0.00838 -0.00667 0.00190 C48 1 0.518130 0.360867 0.707377 11.00000 0.06822 0.04964 = 0.06235 -0.02579 -0.02351 0.02085 AFIX 137 H48A 2 0.549030 0.394599 0.672876 11.00000 -1.50000 H48B 2 0.527450 0.401122 0.747135 11.00000 -1.50000 H48C 2 0.461175 0.363298 0.696745 11.00000 -1.50000 AFIX 0 C49 1 0.559033 0.611834 0.465130 11.00000 0.02529 0.02075 = 0.02916 0.00625 -0.00288 -0.00118 C50 1 0.574784 0.695569 0.508399 11.00000 0.02632 0.02217 = 0.03313 0.00128 -0.00224 0.00145 C51 1 0.546798 0.686186 0.576057 11.00000 0.03549 0.03120 = 0.03389 -0.00639 0.00238 -0.00505 AFIX 137 H51A 2 0.488492 0.679505 0.576812 11.00000 -1.50000 H51B 2 0.562872 0.751732 0.599833 11.00000 -1.50000 H51C 2 0.570728 0.621185 0.595776 11.00000 -1.50000 AFIX 0 C52 1 0.618525 0.785155 0.486191 11.00000 0.03098 0.02119 = 0.04466 -0.00236 0.00162 -0.00272 AFIX 43 H52 2 0.632142 0.842696 0.514717 11.00000 -1.20000 AFIX 0 C53 1 0.642326 0.791083 0.422925 11.00000 0.02574 0.02432 = 0.04898 0.00938 0.00305 -0.00216 AFIX 43 H53 2 0.670757 0.853558 0.408235 11.00000 -1.20000 AFIX 0 C54 1 0.625079 0.707142 0.381233 11.00000 0.03133 0.03335 = 0.03448 0.01086 0.00365 -0.00340 AFIX 43 H54 2 0.641741 0.712719 0.338044 11.00000 -1.20000 AFIX 0 C55 1 0.583670 0.614195 0.401151 11.00000 0.03299 0.02879 = 0.03084 0.00399 -0.00213 -0.00197 C56 1 0.569459 0.518377 0.358345 11.00000 0.05724 0.04477 = 0.02941 -0.00162 0.00354 -0.01206 AFIX 137 H56A 2 0.596322 0.453630 0.375809 11.00000 -1.50000 H56B 2 0.590747 0.534355 0.315812 11.00000 -1.50000 H56C 2 0.511980 0.504244 0.355315 11.00000 -1.50000 AFIX 0 HKLF 4 REM c130922_1_1_a.res in Pca2(1) REM wR2 = 0.1093, GooF = S = 1.048, Restrained GooF = 1.048 for all data REM R1 = 0.0422 for 6449 Fo > 4sig(Fo) and 0.0514 for all 7440 data REM 556 parameters refined using 1 restraints END WGHT 0.0630 0.0000 REM Highest difference peak 0.362, deepest hole -0.402, 1-sigma level 0.055 Q1 1 0.3681 0.3413 0.4907 11.00000 0.05 0.36 Q2 1 0.5024 0.3596 0.4911 11.00000 0.05 0.30 Q3 1 0.4364 0.3825 0.4505 11.00000 0.05 0.29 Q4 1 0.4459 0.3737 0.4933 11.00000 0.05 0.26 Q5 1 0.5096 0.3386 0.4841 11.00000 0.05 0.26 Q6 1 0.2710 0.1961 0.3944 11.00000 0.05 0.24 Q7 1 0.4536 0.2249 0.4496 11.00000 0.05 0.23 Q8 1 0.3573 0.5009 0.3941 11.00000 0.05 0.23 Q9 1 0.5134 0.2780 0.5144 11.00000 0.05 0.23 Q10 1 0.4333 0.2228 0.5796 11.00000 0.05 0.22 Q11 1 0.4270 0.4616 0.5130 11.00000 0.05 0.22 Q12 1 0.4401 0.3813 0.5321 11.00000 0.05 0.22 Q13 1 0.6070 0.1587 0.6525 11.00000 0.05 0.22 Q14 1 0.3348 0.2868 0.4222 11.00000 0.05 0.22 Q15 1 0.4389 0.2805 0.5921 11.00000 0.05 0.21 Q16 1 0.4436 0.2843 0.3869 11.00000 0.05 0.21 Q17 1 0.5105 0.2606 0.4833 11.00000 0.05 0.20 Q18 1 0.5685 0.3008 0.5179 11.00000 0.05 0.20 Q19 1 0.4451 0.4478 0.4204 11.00000 0.05 0.20 Q20 1 0.4983 0.3430 0.2558 11.00000 0.05 0.19 REM The information below was added by Olex2. REM REM R1 = 0.0422 for 6449 Fo > 4sig(Fo) and 0.0514 for all 35279 data REM 556 parameters refined using n/a restraints REM Highest difference peak 0.36, deepest hole -0.40 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0514 REM R1_gt = 0.0422 REM wR_ref = 0.1093 REM GOOF = 1.048 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 35279 REM Reflections_gt = 6449 REM Parameters = 556 REM Hole = -0.40 REM Peak = 0.36 REM Flack = -0.008(4) ; _cod_data_source_file mw2197sup1.cif _cod_data_source_block I _cod_original_cell_volume 4283.81(13) _cod_database_code 2022784 _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 0.666 _shelx_estimated_absorpt_t_max 0.939 _shelx_hkl_file ; 0 0 -25 -3.25 12.06 0 0 -24 148.45 19.57 0 0 -23 1.96 18.07 0 0 -23 12.59 16.34 0 0 -22 94.13 20.99 0 0 -22 106.50 19.38 0 0 -21 -10.88 19.44 0 0 -21 6.62 13.67 0 0 -21 4.66 19.46 0 0 -20 361.21 29.24 0 0 -20 319.31 33.41 0 0 -20 317.37 33.08 0 0 -20 323.28 24.41 0 0 -20 334.54 26.04 0 0 -19 -2.67 19.79 0 0 -19 -2.72 14.43 0 0 -19 -11.73 9.63 0 0 -19 -3.27 19.01 0 0 -19 -3.50 6.67 0 0 -18 1380.47 96.04 0 0 -18 1206.62 98.31 0 0 -18 1374.17 93.68 0 0 -18 1284.18 97.76 0 0 -18 1445.10 95.23 0 0 -17 -28.65 28.39 0 0 -17 4.66 13.18 0 0 -17 -27.60 18.74 0 0 -17 -0.45 9.28 0 0 -17 -4.87 6.59 0 0 -17 10.00 17.51 0 0 -16 918.45 68.61 0 0 -16 805.30 70.67 0 0 -16 1017.40 68.02 0 0 -16 990.72 66.48 0 0 -16 928.17 70.71 0 0 -15 -4.78 23.90 0 0 -15 -0.91 12.01 0 0 -15 0.72 15.64 0 0 -15 -1.12 5.26 0 0 -15 -8.92 9.16 0 0 -15 23.35 15.34 0 0 -14 1233.14 91.60 0 0 -14 1252.84 93.37 0 0 -14 1391.41 93.22 0 0 -13 -21.72 22.78 0 0 -12 336.15 34.59 0 0 -11 -2.94 19.52 0 0 -10 3857.29 263.41 0 0 -9 3.62 16.60 0 0 -9 0.93 3.27 0 0 -8 5194.97 350.54 0 0 -8 5633.85 354.25 0 0 -7 -1.02 15.78 0 0 -7 1.95 3.51 0 0 -6 269.26 22.75 0 0 -6 244.46 17.97 0 0 -6 246.32 17.37 0 0 -5 17.35 13.03 0 0 -5 2.07 4.57 0 0 -4 3765.17 254.79 0 0 -4 3963.18 256.18 0 0 -3 5.57 8.05 0 0 -3 2.04 3.20 0 0 -2 8523.14 575.82 0 0 -2 8949.04 576.40 0 0 -1 3.92 2.38 0 -1 -25 8.50 11.85 0 -1 -24 28.50 15.29 0 1 -24 41.40 14.78 0 1 -23 -22.63 18.06 0 -1 -23 19.79 16.49 0 1 -23 21.51 16.78 0 1 -22 104.56 16.07 0 1 -22 96.50 19.94 0 -1 -22 91.90 19.78 0 1 -22 117.25 20.61 0 1 -21 3.09 14.37 0 -1 -21 0.50 14.23 0 1 -21 -2.51 19.61 0 1 -21 18.57 17.98 0 -1 -21 3.88 9.28 0 -1 -21 4.57 18.74 0 1 -20 73.78 21.22 0 -1 -20 110.64 16.65 0 1 -20 78.54 16.89 0 1 -20 86.11 21.04 0 -1 -20 89.80 13.32 0 -1 -20 99.38 21.39 0 1 -20 84.63 9.26 0 1 -19 29.03 28.70 0 -1 -19 1.60 14.67 0 1 -19 -0.55 14.83 0 1 -19 21.29 20.57 0 1 -19 -4.94 18.53 0 -1 -19 -6.42 18.64 0 -1 -19 -13.80 10.81 0 1 -19 1.74 6.13 0 -1 -19 0.29 7.44 0 1 -18 14.10 28.41 0 -1 -18 46.62 14.66 0 -1 -18 33.25 11.39 0 1 -18 6.09 19.11 0 1 -18 31.59 14.14 0 -1 -18 38.71 11.30 0 1 -18 28.36 17.97 0 1 -18 35.51 7.00 0 -1 -18 41.31 7.75 0 -1 -18 13.40 18.23 0 1 -17 -1.90 26.70 0 -1 -17 7.68 27.58 0 1 -17 3.16 13.53 0 1 -17 4.14 18.30 0 -1 -17 1.02 13.16 0 -1 -17 -8.77 11.39 0 1 -17 0.78 16.72 0 1 -17 4.72 5.99 0 1 -17 6.87 8.48 0 -1 -17 -5.36 6.63 0 -1 -17 -10.70 10.79 0 -1 -17 -2.27 17.62 0 -1 -16 241.29 33.40 0 1 -16 229.90 33.35 0 -1 -16 162.58 19.02 0 1 -16 202.87 19.95 0 1 -16 195.05 24.10 0 -1 -16 198.68 21.82 0 1 -16 220.26 17.09 0 -1 -16 190.55 15.66 0 1 -16 179.33 23.49 0 -1 -16 183.24 17.99 0 1 -16 181.26 14.85 0 1 -15 -1.58 23.62 0 -1 -15 26.27 25.16 0 1 -15 -1.86 11.33 0 1 -15 -2.11 15.20 0 -1 -15 -3.17 11.63 0 -1 -15 4.61 14.25 0 -1 -15 -2.70 5.81 0 -1 -15 -3.51 9.31 0 1 -15 -0.68 15.95 0 1 -15 -1.04 4.89 0 1 -14 166.35 27.21 0 1 -14 152.34 18.99 0 1 -14 152.37 16.71 0 -1 -14 168.02 16.65 0 1 -14 153.68 19.07 0 -1 -14 144.00 18.69 0 -1 -13 6.54 24.27 0 1 -13 7.59 23.44 0 1 -12 114.04 22.19 0 -1 -12 138.79 23.43 0 -1 -12 88.92 9.01 0 -1 -11 -14.11 21.32 0 1 -11 -13.41 18.86 0 -1 -11 -3.70 5.38 0 -1 -10 804.10 57.40 0 -1 -10 718.96 49.86 0 1 -10 676.38 55.74 0 1 -9 1.37 4.37 0 -1 -9 1.21 2.70 0 -1 -9 -7.52 17.46 0 -1 -9 0.19 5.77 0 1 -9 -9.86 17.51 0 1 -8 368.19 26.85 0 -1 -8 404.42 27.28 0 -1 -8 440.23 34.83 0 1 -8 449.07 33.99 0 -1 -8 375.51 26.98 0 1 -7 3.55 14.31 0 -1 -7 -10.65 15.70 0 1 -7 2.36 4.27 0 -1 -7 2.74 4.97 0 -1 -7 1.99 3.68 0 -1 -6 307.93 25.30 0 -1 -6 250.58 18.62 0 -1 -6 263.07 18.10 0 -1 -6 260.48 18.45 0 1 -6 279.49 24.16 0 -1 -5 -0.35 13.40 0 1 -5 3.71 12.89 0 1 -5 -3.22 4.48 0 -1 -5 2.16 3.59 0 -1 -5 4.04 3.21 0 -1 -4 1743.87 119.88 0 1 -4 1785.78 119.80 0 -1 -4 1814.05 121.49 0 1 -4 1888.47 121.42 0 -1 -3 -0.60 9.31 0 1 -3 9.64 9.51 0 -1 -3 -0.37 3.69 0 1 -3 -5.31 3.87 0 -1 -2 3690.07 242.54 0 -1 -2 3466.22 243.01 0 1 -2 3497.98 242.57 0 1 -2 3924.87 243.09 0 1 -1 -2.95 3.57 0 1 -1 -1.82 2.78 0 -1 -1 -0.66 2.57 0 -1 0 396.95 26.89 0 -2 -25 -21.27 11.35 0 2 -24 28.06 15.54 0 -2 -24 34.33 14.10 0 2 -23 3.29 17.25 0 2 -23 0.57 15.48 0 -2 -23 0.59 15.46 0 2 -22 32.72 13.70 0 2 -22 12.09 17.90 0 2 -22 17.40 17.77 0 -2 -22 30.84 16.38 0 2 -21 8.26 20.07 0 2 -21 24.17 14.26 0 -2 -21 3.66 17.24 0 2 -21 5.96 17.49 0 -2 -21 -7.98 10.91 0 2 -20 169.42 31.23 0 -2 -20 67.62 21.64 0 2 -20 92.86 22.12 0 2 -20 138.14 17.60 0 -2 -20 93.79 20.95 0 2 -20 115.71 21.07 0 -2 -20 101.24 14.77 0 2 -19 -12.44 29.89 0 2 -19 -6.67 15.65 0 2 -19 6.15 20.04 0 -2 -19 -11.26 20.48 0 -2 -19 -9.31 12.06 0 -2 -19 10.14 17.52 0 2 -19 -0.67 5.50 0 2 -19 -18.66 18.63 0 -2 -19 -9.05 11.43 0 -2 -18 743.16 64.70 0 -2 -18 912.81 61.27 0 2 -18 810.65 62.19 0 2 -18 730.63 64.68 0 2 -18 857.12 64.48 0 -2 -18 934.30 61.96 0 2 -18 864.70 59.10 0 -2 -18 849.44 64.17 0 2 -17 3.80 27.22 0 -2 -17 -13.31 12.60 0 -2 -17 12.59 19.52 0 2 -17 6.57 18.59 0 2 -17 -5.37 14.17 0 2 -17 3.51 5.53 0 -2 -17 -4.73 11.41 0 -2 -17 8.17 16.88 0 2 -17 -16.34 19.57 0 2 -16 472.91 41.17 0 2 -16 466.28 38.63 0 2 -16 530.06 35.27 0 -2 -16 483.17 41.78 0 2 -16 488.31 40.80 0 -2 -16 517.41 38.20 0 -2 -16 491.14 40.88 0 2 -16 485.97 35.23 0 2 -15 -11.19 22.21 0 -2 -15 13.24 23.77 0 2 -15 1.40 14.62 0 2 -15 15.32 11.53 0 -2 -15 -1.47 16.81 0 -2 -15 4.05 11.93 0 2 -15 -2.74 4.71 0 -2 -15 -0.65 13.81 0 2 -15 0.74 5.26 0 -2 -14 932.95 57.14 0 2 -14 1049.84 69.40 0 -2 -14 1092.62 70.22 0 -2 -14 814.10 58.58 0 -2 -14 665.54 60.39 0 2 -14 790.54 60.30 0 2 -14 706.92 58.55 0 -2 -14 790.36 60.10 0 -2 -13 13.45 20.88 0 2 -13 -1.27 20.47 0 -2 -13 5.39 5.94 0 2 -12 399.15 37.83 0 -2 -12 420.59 37.32 0 -2 -12 382.88 27.16 0 -2 -12 359.62 26.56 0 -2 -11 -6.17 21.06 0 2 -11 -7.67 18.07 0 -2 -11 2.19 6.33 0 -2 -10 382.24 28.80 0 2 -10 498.12 37.19 0 -2 -10 449.78 36.97 0 -2 -10 403.53 28.69 0 -2 -9 0.18 5.29 0 2 -9 2.87 16.45 0 -2 -9 -19.10 16.96 0 -2 -9 -2.58 5.85 0 -2 -9 2.07 4.25 0 -2 -8 836.50 62.47 0 2 -8 855.03 61.98 0 -2 -8 861.72 57.45 0 -2 -8 831.71 57.75 0 2 -7 8.23 14.01 0 -2 -7 -1.07 16.18 0 -2 -7 5.24 4.92 0 -2 -7 -0.85 3.72 0 2 -6 46.23 14.61 0 -2 -6 49.80 7.20 0 -2 -6 27.74 14.60 0 2 -6 30.15 6.78 0 -2 -6 45.43 5.14 0 -2 -6 42.79 5.58 0 -2 -5 3.40 5.88 0 2 -5 0.15 6.25 0 -2 -5 7.72 12.57 0 2 -5 3.58 12.15 0 -2 -5 -0.68 3.88 0 -2 -4 1645.91 113.52 0 2 -4 1674.42 113.67 0 -2 -4 1607.48 114.73 0 2 -4 1869.49 115.13 0 -2 -4 1697.70 113.15 0 2 -3 -1.29 9.43 0 2 -3 0.88 5.72 0 -2 -3 -0.61 4.59 0 -2 -3 1.82 3.04 0 -2 -2 5.86 5.75 0 2 -2 7.75 6.79 0 -2 -2 6.31 4.29 0 -2 -1 -7.53 4.91 0 -2 0 7257.74 485.65 0 -2 1 5.31 3.85 0 -2 2 47.45 4.98 0 -3 -25 6.01 9.84 0 3 -24 42.67 15.22 0 -3 -24 45.65 12.91 0 3 -23 -0.63 15.85 0 -3 -23 3.25 15.33 0 3 -22 236.50 21.55 0 3 -22 201.22 26.24 0 3 -22 262.86 24.66 0 -3 -22 202.94 23.60 0 3 -21 -2.02 14.58 0 3 -21 -4.03 17.83 0 -3 -21 0.49 11.08 0 3 -21 -3.42 17.07 0 -3 -21 -24.14 17.07 0 3 -20 23.73 14.77 0 -3 -20 28.68 12.63 0 3 -20 14.51 18.98 0 -3 -20 27.10 17.73 0 3 -19 -16.57 28.61 0 3 -19 3.48 19.79 0 3 -19 13.39 15.17 0 -3 -19 13.40 12.94 0 -3 -19 4.50 17.39 0 3 -18 6.07 26.08 0 -3 -18 1.50 14.03 0 3 -18 17.94 14.72 0 -3 -18 -0.87 13.67 0 -3 -18 36.19 19.62 0 3 -18 6.82 18.32 0 3 -18 -0.78 18.44 0 -3 -18 5.98 17.49 0 3 -18 8.74 5.04 0 3 -17 -15.36 27.31 0 3 -17 19.62 18.63 0 -3 -17 8.07 18.38 0 -3 -17 -4.43 12.76 0 3 -17 -4.94 14.41 0 -3 -17 -11.86 12.00 0 3 -17 -5.35 17.29 0 -3 -17 4.98 7.58 0 3 -17 0.61 5.35 0 -3 -17 10.90 16.95 0 3 -17 4.85 5.05 0 -3 -16 590.95 38.23 0 3 -16 633.57 52.76 0 3 -16 515.00 42.92 0 -3 -16 395.02 42.68 0 -3 -16 528.18 40.18 0 3 -16 519.97 40.61 0 -3 -16 543.04 38.37 0 3 -16 542.80 43.34 0 -3 -16 522.50 42.05 0 3 -16 566.28 37.40 0 3 -16 496.62 37.13 0 -3 -16 558.31 40.70 0 -3 -15 1.60 7.01 0 3 -15 8.20 24.54 0 3 -15 3.97 12.89 0 3 -15 -10.54 15.44 0 -3 -15 2.65 11.72 0 -3 -15 4.29 16.71 0 -3 -15 8.87 10.54 0 3 -15 2.13 5.32 0 3 -15 12.27 16.44 0 -3 -15 0.65 14.57 0 -3 -15 -2.42 7.07 0 -3 -14 30.58 7.24 0 3 -14 32.33 23.29 0 3 -14 43.36 12.76 0 -3 -14 11.10 15.82 0 -3 -14 41.14 11.57 0 3 -14 31.77 14.13 0 3 -14 33.74 5.92 0 -3 -14 31.80 11.14 0 -3 -14 38.35 7.82 0 3 -14 48.35 15.64 0 -3 -14 34.76 14.84 0 -3 -13 -5.34 5.75 0 3 -13 -13.07 22.31 0 -3 -13 -3.33 5.83 0 3 -13 13.17 10.50 0 3 -13 -3.98 12.57 0 -3 -13 -0.46 10.00 0 -3 -13 2.30 6.33 0 -3 -13 1.65 12.44 0 -3 -12 139.05 23.61 0 -3 -12 129.10 12.30 0 3 -12 172.60 25.55 0 -3 -12 145.35 12.90 0 -3 -11 -8.22 17.71 0 3 -11 3.00 19.40 0 -3 -11 -1.28 5.80 0 -3 -11 6.91 7.09 0 3 -10 47.05 18.19 0 -3 -10 73.46 19.83 0 -3 -10 81.06 8.57 0 -3 -10 86.45 9.11 0 -3 -10 88.28 7.72 0 3 -9 -15.07 15.78 0 -3 -9 6.02 16.53 0 -3 -9 -0.34 5.88 0 -3 -9 3.01 4.07 0 -3 -8 417.99 29.86 0 -3 -8 375.53 34.06 0 3 -8 376.15 34.08 0 -3 -8 451.71 28.74 0 -3 -8 381.12 28.73 0 3 -7 6.57 13.89 0 -3 -7 0.23 6.96 0 -3 -7 12.50 13.86 0 -3 -7 2.41 4.98 0 -3 -6 491.02 35.03 0 -3 -6 505.53 34.17 0 3 -6 472.94 37.98 0 -3 -5 -7.22 6.43 0 3 -5 -1.17 12.06 0 -3 -5 0.09 3.98 0 -3 -4 348.38 25.04 0 3 -4 345.21 27.71 0 -3 -4 355.88 24.31 0 3 -3 -10.88 9.57 0 -3 -3 -10.23 7.20 0 -3 -3 -0.41 5.25 0 -3 -2 2463.83 173.36 0 -3 -2 2577.55 173.08 0 3 -2 2716.01 173.63 0 -3 -1 4.39 6.73 0 -3 0 3002.15 201.57 0 -3 1 2.45 5.51 0 -3 2 3097.64 207.81 0 -3 3 3.96 4.48 0 -3 8 184.69 13.44 0 -3 9 2.89 3.23 0 -3 10 126.25 9.24 0 -4 -25 7.06 8.43 0 4 -24 7.01 13.41 0 -4 -24 35.80 12.08 0 4 -23 28.18 15.96 0 -4 -23 -19.07 13.94 0 4 -22 15.17 12.66 0 4 -22 35.90 17.54 0 -4 -22 9.01 15.62 0 4 -21 -6.23 13.74 0 -4 -21 15.17 12.32 0 4 -21 0.77 18.00 0 4 -21 12.84 15.58 0 -4 -21 -8.24 15.24 0 -4 -20 127.72 16.00 0 4 -20 77.86 21.71 0 4 -20 119.20 16.92 0 4 -20 107.48 19.67 0 -4 -20 104.66 16.04 0 -4 -20 122.44 19.51 0 4 -19 -2.75 14.58 0 -4 -19 5.70 13.67 0 4 -19 -2.57 19.51 0 4 -19 -18.39 17.03 0 -4 -19 8.55 17.17 0 -4 -19 7.75 13.31 0 4 -18 552.34 37.56 0 4 -18 463.42 44.40 0 4 -18 569.47 41.76 0 4 -18 580.50 43.99 0 -4 -18 490.82 43.08 0 -4 -18 507.08 41.30 0 4 -17 5.85 26.07 0 4 -17 -25.48 17.33 0 4 -17 -10.57 14.46 0 -4 -17 7.80 15.88 0 4 -17 -7.48 5.67 0 -4 -17 -7.31 12.74 0 4 -17 -7.98 17.23 0 -4 -16 190.92 16.01 0 4 -16 242.10 35.17 0 4 -16 175.73 24.36 0 4 -16 172.19 20.66 0 4 -16 168.60 22.35 0 -4 -16 169.24 22.18 0 -4 -16 170.08 19.67 0 4 -16 197.04 14.68 0 -4 -15 1.35 6.79 0 4 -15 25.53 26.04 0 4 -15 -1.03 13.69 0 -4 -15 -7.54 11.44 0 4 -15 -3.60 15.79 0 4 -15 -4.09 5.30 0 -4 -15 -2.85 12.24 0 4 -15 1.33 15.35 0 -4 -14 75.91 8.81 0 4 -14 70.66 25.98 0 4 -14 80.04 13.91 0 4 -14 54.52 15.13 0 -4 -14 59.12 12.12 0 -4 -14 62.70 9.65 0 4 -14 74.35 7.93 0 -4 -14 90.26 13.49 0 4 -14 58.59 15.62 0 -4 -13 -5.46 8.15 0 -4 -13 -1.33 6.09 0 4 -13 2.75 20.78 0 4 -13 -0.59 12.76 0 -4 -13 2.02 10.96 0 -4 -13 1.13 6.89 0 -4 -12 254.72 19.91 0 -4 -12 256.27 19.54 0 4 -12 242.44 22.77 0 -4 -12 273.51 21.85 0 -4 -12 218.37 18.90 0 -4 -11 -2.51 7.23 0 -4 -11 1.84 4.97 0 4 -11 -10.65 17.81 0 -4 -11 1.15 5.89 0 -4 -10 288.59 20.77 0 -4 -10 280.97 21.57 0 4 -10 326.86 30.13 0 -4 -9 0.75 5.95 0 -4 -9 -4.88 5.24 0 4 -9 -9.75 17.24 0 -4 -8 429.27 29.27 0 4 -8 417.82 34.85 0 -4 -8 392.69 30.36 0 -4 -7 1.79 4.65 0 4 -7 0.60 14.40 0 -4 -7 2.46 7.53 0 -4 -6 366.72 25.31 0 -4 -6 352.78 26.57 0 -4 -5 -2.26 4.49 0 -4 -5 0.87 6.55 0 -4 -4 337.86 23.76 0 -4 -4 351.42 24.86 0 -4 -3 -16.29 7.63 0 -4 -3 2.34 5.87 0 -4 -2 2004.18 132.99 0 -4 -2 1930.45 133.41 0 -4 -1 2.58 6.57 0 -4 0 1222.22 83.12 0 -4 1 -9.91 6.13 0 -4 2 2284.60 153.84 0 -4 3 -1.33 5.46 0 -4 5 2.67 4.66 0 -4 6 329.79 23.36 0 -4 7 -3.01 4.69 0 -4 8 523.39 36.05 0 -4 9 5.01 4.05 0 5 -24 79.74 13.94 0 5 -23 -6.25 15.09 0 5 -22 178.04 21.73 0 5 -21 7.23 16.14 0 -5 -21 -14.43 11.95 0 5 -21 -1.30 13.03 0 5 -20 383.82 29.64 0 -5 -20 371.66 29.54 0 5 -19 -1.05 14.16 0 5 -19 -8.33 18.44 0 5 -19 3.51 5.53 0 -5 -19 7.96 13.53 0 5 -18 105.09 30.51 0 5 -18 79.49 8.81 0 5 -18 103.17 16.69 0 -5 -18 101.68 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324.71 25.71 -10 5 -6 310.68 28.07 10 5 -6 370.81 28.87 -10 5 -6 323.04 26.01 -10 -5 -6 353.89 26.95 10 -5 -6 378.53 30.02 -10 -5 -6 349.11 26.31 10 5 -6 344.59 25.06 10 -5 -6 237.82 26.46 -10 5 -6 322.04 26.94 10 5 -6 342.65 23.98 10 5 -5 364.40 24.20 10 -5 -5 337.26 25.16 -10 5 -5 332.71 28.03 10 5 -5 409.59 28.19 -10 5 -5 352.42 26.53 10 -5 -5 356.81 29.16 -10 -5 -5 313.63 25.95 10 -5 -5 231.05 25.27 10 5 -5 355.16 24.39 -10 5 -5 310.94 26.12 10 5 -5 307.75 23.32 10 -5 -4 129.81 12.19 -10 5 -4 120.71 14.91 10 5 -4 153.98 16.14 -10 -5 -4 122.77 14.07 -10 5 -4 91.11 15.61 10 -5 -4 132.13 16.74 -10 -5 -4 125.21 14.64 10 -5 -4 85.95 12.74 10 5 -4 131.30 11.82 10 5 -3 172.06 16.66 -10 -5 -3 180.29 16.33 10 -5 -3 166.91 17.88 10 5 -3 171.23 13.05 10 -5 -3 159.25 13.52 -10 5 -3 156.65 16.08 10 5 -2 297.69 20.47 10 -5 -2 284.60 20.75 -10 5 -2 306.11 25.64 10 5 -2 316.17 23.92 -10 -5 -2 293.82 23.54 -10 5 -2 277.54 22.73 10 5 -1 53.35 7.15 10 -5 -1 54.47 7.48 -10 5 -1 69.06 15.26 10 5 -1 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36.91 7.21 13 7 -14 28.00 11.76 13 -7 -14 38.79 11.99 13 -7 -14 36.57 7.22 13 7 -13 7.29 10.44 -13 -7 -13 6.77 7.52 13 7 -13 13.17 11.20 13 -7 -13 5.38 7.40 13 -7 -13 8.03 12.61 -13 -7 -12 78.65 10.65 -13 7 -12 93.22 11.55 13 7 -12 72.02 12.84 13 -7 -12 60.65 15.89 13 -7 -12 58.23 9.71 -13 -7 -11 31.84 9.65 -13 7 -11 22.17 10.45 13 7 -11 36.61 12.98 13 -7 -11 29.74 15.92 13 7 -11 24.96 7.25 13 -7 -11 13.41 8.18 -13 -7 -10 32.60 10.93 13 7 -10 48.00 13.97 -13 7 -10 50.35 11.75 13 7 -10 35.16 8.33 13 -7 -10 20.80 17.60 13 -7 -10 38.68 8.67 -13 7 -9 193.17 17.92 -13 -7 -9 203.62 16.91 13 7 -9 232.94 20.18 13 -7 -9 124.85 14.28 13 -7 -9 124.28 22.12 13 7 -8 14.29 7.89 -13 -7 -8 4.68 11.10 -13 7 -8 16.24 12.50 13 7 -8 16.38 8.11 13 -7 -8 23.11 19.24 13 7 -7 41.22 8.52 -13 -7 -7 37.33 5.89 -13 -7 -7 25.86 10.45 -13 -7 -7 26.76 11.76 -13 7 -7 28.00 12.48 13 7 -7 20.34 8.84 -13 -7 -6 8.37 5.46 -13 -7 -6 1.67 10.99 -13 7 -6 -16.28 13.48 -13 -7 -6 0.39 11.46 13 7 -6 8.37 8.25 -13 -7 -5 6.49 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7.28 -13 -7 8 22.93 13.31 -13 -7 10 68.05 12.28 -13 -7 11 19.16 9.84 -13 -7 12 35.53 8.76 -13 -7 13 13.67 6.45 13 7 13 10.48 4.86 13 8 -16 5.80 5.29 13 8 -15 -3.42 3.99 13 8 -15 -0.27 7.36 13 -8 -15 13.94 5.87 13 8 -14 19.78 6.76 13 8 -14 19.62 9.51 -13 -8 -14 18.41 5.45 -13 -8 -13 22.68 6.55 13 8 -13 5.37 9.80 -13 -8 -12 37.31 8.03 13 8 -12 46.48 12.00 -13 -8 -11 15.79 8.54 13 8 -11 22.09 11.52 -13 -8 -10 64.42 10.74 -13 8 -10 74.51 12.05 13 8 -10 67.06 13.59 13 8 -10 73.89 8.49 -13 -8 -9 117.55 13.03 -13 8 -9 102.52 14.18 13 8 -9 137.13 15.69 13 8 -9 109.82 11.08 13 8 -8 222.25 18.28 -13 8 -8 220.09 20.99 -13 -8 -8 261.72 20.09 13 8 -8 232.71 22.01 13 8 -7 11.88 7.53 -13 -8 -7 9.46 5.08 -13 8 -7 6.20 11.73 -13 -8 -7 12.60 10.48 13 8 -7 7.09 7.43 -13 -8 -6 178.43 14.28 13 8 -6 197.82 15.63 -13 -8 -6 198.23 17.83 -13 8 -6 162.02 18.96 -13 -8 -6 166.27 16.82 13 8 -6 196.17 15.89 -13 -8 -5 32.95 11.31 -13 -8 -5 19.16 10.67 -13 8 -5 37.01 12.87 13 8 -5 42.20 8.71 -13 8 -4 125.55 17.31 13 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6.93 19 -4 -8 15.88 7.96 19 4 -8 0.70 5.29 -19 -4 -7 30.78 6.44 -19 4 -7 34.62 6.33 19 4 -7 38.02 7.01 -19 -4 -6 6.85 6.74 -19 4 -6 25.08 7.32 19 4 -6 20.60 6.51 19 -4 -6 6.51 10.71 -19 4 -5 83.85 9.68 19 4 -5 78.57 8.90 -19 4 -5 94.56 10.54 -19 4 -4 44.31 9.16 -19 4 -4 62.37 9.40 19 4 -4 65.31 7.82 19 4 -3 55.38 7.86 -19 4 -3 51.00 9.21 19 4 -2 17.68 7.13 -19 4 -1 60.67 9.29 -19 -4 0 3.77 11.68 -19 4 0 8.59 7.43 -19 -4 1 19.27 11.94 19 4 1 33.67 6.88 -19 -4 2 1.92 11.99 19 4 2 21.13 6.16 -19 -4 3 81.12 13.07 19 4 3 80.20 8.10 -19 -4 4 50.72 11.40 19 4 4 38.08 5.06 19 -5 -8 11.62 5.98 19 5 -8 23.23 4.51 -19 5 -7 3.62 4.55 19 -5 -7 -1.92 7.05 19 5 -7 1.97 4.54 -19 -5 -6 13.78 5.32 -19 5 -6 11.02 5.63 19 5 -6 23.36 5.69 19 -5 -6 1.40 8.96 -19 5 -5 4.52 6.92 19 5 -5 -3.84 5.59 19 -5 -5 -3.45 9.87 19 5 -4 8.23 5.06 -19 5 -4 2.29 7.04 19 5 -4 12.42 6.02 19 -5 -4 0.69 11.07 -19 5 -3 24.86 8.02 19 5 -3 15.32 6.20 19 5 -3 22.49 6.56 -19 5 -2 11.38 7.84 19 5 -2 1.70 6.07 -19 5 -1 2.04 7.61 19 5 -1 0.37 5.81 -19 5 0 22.52 7.95 -19 -5 0 5.04 10.04 -19 5 1 -4.61 7.37 -19 -5 1 -3.03 10.22 -19 5 2 12.41 6.84 -19 -5 2 -3.34 10.57 19 5 2 7.15 4.95 -19 -5 3 21.74 10.20 19 5 3 22.87 4.92 -19 5 4 0.44 5.19 -19 -5 4 -5.53 8.97 -19 5 5 3.44 4.15 -19 6 -6 2.74 3.69 19 -6 -6 5.96 5.65 19 6 -6 4.12 3.67 -19 6 -5 152.26 9.61 19 6 -5 168.30 9.45 -19 6 -4 77.07 7.11 19 6 -4 65.72 6.50 -19 6 -3 22.97 5.97 19 6 -3 4.49 4.65 19 6 -3 23.63 5.10 19 -6 -3 -3.83 8.41 -19 6 -2 66.10 6.97 19 6 -2 57.07 5.74 19 -6 -2 18.16 10.50 -19 6 -1 46.40 6.92 19 6 -1 49.34 6.13 -19 6 0 -3.55 5.56 -19 -6 0 2.15 7.25 19 6 0 5.93 4.81 -19 -6 1 64.03 9.28 -19 6 2 20.57 5.01 -19 -6 2 25.28 8.08 19 6 2 28.59 4.48 -19 -6 3 50.97 8.27 -19 -6 4 42.39 7.38 19 7 -1 2.60 2.84 19 -7 -1 -2.19 5.03 19 -7 0 6.09 5.50 19 -7 1 4.31 5.35 -20 0 -8 20.45 5.37 -20 0 -7 8.59 6.19 20 0 -7 1.08 4.79 -20 0 -6 42.13 7.45 20 0 -6 23.34 5.87 -20 0 -5 1.05 7.56 20 0 -5 8.87 5.45 -20 0 -4 7.06 7.83 20 0 -4 0.99 5.42 -20 0 -3 73.05 9.44 20 0 -3 53.27 7.01 -20 0 -2 33.51 8.79 -20 0 -1 95.10 11.06 -20 0 0 72.67 9.75 -20 0 2 45.89 7.48 -20 0 3 15.39 5.89 20 1 -8 23.76 5.05 -20 1 -8 34.49 5.61 -20 -1 -8 24.42 5.11 -20 -1 -7 0.39 5.49 -20 1 -7 7.13 5.94 -20 -1 -6 23.00 6.84 -20 1 -6 18.20 4.31 20 -1 -6 11.96 4.71 -20 1 -6 31.12 7.28 -20 1 -5 20.58 7.69 -20 -1 -5 23.10 7.46 20 1 -5 21.41 5.88 -20 1 -4 12.21 7.80 -20 -1 -4 12.69 7.70 20 1 -4 8.24 5.96 -20 1 -3 45.93 8.72 -20 -1 -3 27.85 8.48 20 1 -3 31.45 6.47 -20 1 -2 18.63 8.30 -20 -1 -2 16.59 8.15 20 1 -2 2.07 5.35 -20 1 -1 84.29 9.77 -20 -1 -1 67.99 9.70 20 1 -1 62.79 7.04 -20 -1 0 -0.18 7.87 -20 1 1 69.88 8.76 -20 1 2 7.06 6.19 -20 -1 2 20.83 6.97 -20 -1 3 48.23 6.81 -20 1 3 24.43 5.58 -20 -1 4 -0.74 4.81 20 2 -8 0.14 4.16 -20 -2 -8 2.37 3.66 -20 -2 -7 33.96 5.67 20 2 -7 26.40 5.64 -20 2 -7 26.12 6.34 -20 -2 -6 25.19 6.35 20 2 -6 17.24 5.63 -20 2 -6 32.15 6.95 -20 -2 -5 29.18 7.10 -20 2 -5 18.31 6.07 -20 -2 -4 10.97 7.09 20 -2 -4 -5.38 8.96 -20 -2 -3 56.13 8.97 20 2 -3 62.55 7.45 -20 2 -3 74.73 8.93 -20 -2 -2 40.72 8.36 20 2 -2 32.40 6.34 -20 2 -2 39.17 8.25 -20 -2 -1 72.56 9.75 20 2 -1 73.71 7.79 -20 -2 0 59.69 8.84 20 2 0 39.06 5.90 -20 2 0 53.52 7.91 -20 -2 1 70.41 8.99 -20 2 1 55.61 7.74 -20 2 2 13.81 5.28 -20 -2 3 51.24 7.28 -20 -2 4 11.25 5.06 -20 -3 -7 47.94 5.65 20 3 -7 69.98 6.37 -20 -3 -6 14.64 5.10 20 3 -6 18.16 5.38 -20 -3 -5 54.61 7.38 -20 3 -5 65.72 7.09 20 3 -5 63.01 7.31 -20 -3 -4 16.30 6.61 -20 3 -4 27.72 6.28 -20 3 -4 32.42 7.06 -20 -3 -3 15.53 6.96 -20 3 -3 2.98 6.35 -20 3 -3 7.81 6.80 20 -3 -3 7.59 10.36 -20 -3 -2 13.94 7.21 20 3 -2 -0.16 5.14 -20 3 -1 31.75 6.84 20 3 -1 29.95 5.76 20 3 0 5.04 4.52 -20 -3 3 25.15 6.04 -20 -3 4 24.99 5.00 20 4 -6 7.76 3.71 -20 -4 -5 4.76 4.47 -20 4 -5 13.89 4.33 20 4 -5 7.88 4.21 20 -4 -5 0.81 6.40 -20 -4 -4 1.89 5.23 -20 4 -4 9.82 5.01 20 4 -4 -2.94 4.56 20 -4 -4 3.56 7.56 -20 -4 -3 1.72 5.72 -20 4 -3 9.92 5.40 20 -4 -3 9.04 8.75 -20 4 -2 7.97 5.93 20 -4 -2 11.00 9.43 -20 4 -1 10.56 5.94 20 4 -1 9.28 4.54 -20 4 0 15.42 6.16 20 4 0 11.15 4.03 -20 4 1 23.45 6.18 -20 4 2 5.61 5.39 -20 4 3 11.37 4.96 20 -5 -4 0.16 4.95 -20 -5 -3 36.76 5.11 -20 5 -3 62.39 5.26 -20 -5 -2 6.70 4.43 -20 5 -2 -4.31 4.24 20 -5 -2 1.08 6.77 -20 5 -1 35.47 4.99 20 -5 -1 -2.54 7.16 -20 5 0 4.73 4.25 -20 5 1 42.07 5.13 -21 0 -5 2.84 3.56 -21 0 -4 -5.07 4.33 -21 0 -3 -3.19 4.77 -21 0 -2 3.21 4.75 -21 0 0 -4.81 4.28 -21 -1 -4 40.39 5.30 -21 1 -4 45.05 5.22 -21 -1 -3 -2.20 4.59 -21 1 -3 12.64 4.40 -21 -1 -2 81.39 7.76 -21 -1 -1 10.84 4.88 -21 -2 -3 0.28 3.90 -21 -2 -2 3.07 4.31 -21 2 -2 4.74 3.74 -21 -2 -1 -1.78 4.39 -21 2 -1 8.91 4.06 TITL c130922_1_1 in Pca2(1) REM Pca2(1) (#29, found as Pbc2(1) in ba-c setting) CELL 1.54184 16.747269 12.199808 20.966807 90.0000 90.0000 90.0000 ZERR 4.00 0.000328 0.000203 0.000442 0.0000 0.0000 0.0000 LATT -1 SYMM -x,-y, z+1/2 SYMM x+1/2,-y, z SYMM -x+1/2, y, z+1/2 SFAC C H N O Fe UNIT 224.00 188.00 12.00 4.00 4.00 REM CrysAlisPro recorded range (K): Min=99.9; max=100.1; aver:100.0 TEMP -173 SIZE 0.02 0.03 0.14 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 369 _shelx_res_file ; TITL c130922_1_1_a.res in Pca2(1) c130922_1_1.res created by SHELXL-2018/3 at 15:08:09 on 14-Sep-2022 REM Old TITL c130922_1_1 in Pca2(1) REM SHELXT solution in Pca2(1) REM R1 0.088, Rweak 0.018, Alpha 0.004, Orientation as input REM Flack x = 0.016 ( 0.005 ) from Parsons' quotients REM Formula found by SHELXT: C55 N4 O Fe CELL 1.54184 16.7473 12.1998 20.9668 90 90 90 ZERR 4 0.0003 0.0002 0.0004 0 0 0 LATT -1 SYMM -X,-Y,0.5+Z SYMM 0.5+X,-Y,+Z SYMM 0.5-X,+Y,0.5+Z SFAC C H Fe N O UNIT 224 188 4 12 4 L.S. 9 PLAN 20 SIZE 0.02 0.03 0.14 TEMP -173 CONF BOND $H list 4 fmap 2 ACTA MORE -1 REM REM REM WGHT 0.063000 FVAR 0.41837 FE1 3 0.442119 0.297274 0.490250 11.00000 0.02225 0.01678 = 0.02004 0.00037 0.00030 -0.00091 O1 5 0.340977 0.178537 0.370471 11.00000 0.03100 0.02164 = 0.02148 -0.00117 -0.00228 0.00053 N1 4 0.546609 0.220813 0.382175 11.00000 0.02608 0.02585 = 0.02560 -0.00197 0.00449 -0.00007 N2 4 0.540083 0.220412 0.601279 11.00000 0.02519 0.02786 = 0.03028 0.00701 -0.00117 -0.00204 N3 4 0.518439 0.518345 0.486774 11.00000 0.02876 0.02033 = 0.02733 0.00106 -0.00065 -0.00422 C1 1 0.507230 0.248384 0.424916 11.00000 0.02494 0.01882 = 0.03409 0.00250 -0.00807 -0.00276 C2 1 0.503077 0.250357 0.557334 11.00000 0.02696 0.01810 = 0.02734 -0.00103 -0.00015 -0.00326 C3 1 0.488585 0.432543 0.489847 11.00000 0.02622 0.02593 = 0.01972 0.00067 -0.00095 0.00187 C4 1 0.341837 0.225041 0.423219 11.00000 0.01971 0.02074 = 0.02537 -0.00270 -0.00086 -0.00027 C5 1 0.353405 0.172428 0.485877 11.00000 0.01876 0.01718 = 0.02703 -0.00383 0.00101 -0.00260 C6 1 0.335502 0.250173 0.535393 11.00000 0.01771 0.01897 = 0.02293 0.00096 0.00097 -0.00170 C7 1 0.328186 0.356533 0.505427 11.00000 0.02187 0.01922 = 0.02143 -0.00095 -0.00088 0.00022 C8 1 0.338109 0.344227 0.437881 11.00000 0.01953 0.01792 = 0.02587 0.00023 -0.00521 0.00136 C9 1 0.360003 0.051577 0.493286 11.00000 0.02896 0.02016 = 0.02065 -0.00039 -0.00472 -0.00104 C10 1 0.415368 -0.008687 0.458730 11.00000 0.02960 0.02177 = 0.02956 -0.00440 -0.00227 -0.00138 AFIX 43 H10 2 0.451113 0.028206 0.430856 11.00000 -1.20000 AFIX 0 C11 1 0.419444 -0.122132 0.464187 11.00000 0.04094 0.02355 = 0.03655 -0.00794 -0.00898 0.00627 AFIX 43 H11 2 0.457570 -0.161958 0.439927 11.00000 -1.20000 AFIX 0 C12 1 0.368068 -0.177381 0.504909 11.00000 0.05339 0.01821 = 0.03507 0.00198 -0.01571 0.00183 AFIX 43 H12 2 0.371492 -0.254748 0.509268 11.00000 -1.20000 AFIX 0 C13 1 0.311631 -0.118618 0.539216 11.00000 0.05329 0.02308 = 0.02369 0.00260 -0.00362 -0.00799 AFIX 43 H13 2 0.275669 -0.155950 0.566711 11.00000 -1.20000 AFIX 0 C14 1 0.307587 -0.005487 0.533466 11.00000 0.03856 0.02483 = 0.02562 -0.00303 0.00005 -0.00595 AFIX 43 H14 2 0.268673 0.033951 0.557136 11.00000 -1.20000 AFIX 0 C15 1 0.317531 0.225753 0.603145 11.00000 0.02352 0.01849 = 0.02527 -0.00188 -0.00212 -0.00403 C16 1 0.363501 0.155473 0.640503 11.00000 0.02702 0.02224 = 0.02573 0.00078 0.00069 -0.00216 AFIX 43 H16 2 0.410074 0.122967 0.622858 11.00000 -1.20000 AFIX 0 C17 1 0.342362 0.132118 0.703161 11.00000 0.03501 0.02486 = 0.02669 0.00347 -0.00332 -0.00609 AFIX 43 H17 2 0.375556 0.086079 0.728307 11.00000 -1.20000 AFIX 0 C18 1 0.273342 0.175451 0.729130 11.00000 0.03848 0.02780 = 0.01963 -0.00189 0.00474 -0.00893 AFIX 43 H18 2 0.258942 0.159492 0.771960 11.00000 -1.20000 AFIX 0 C19 1 0.225281 0.242651 0.691801 11.00000 0.03036 0.02582 = 0.02889 -0.00470 0.00598 -0.00295 AFIX 43 H19 2 0.176829 0.270689 0.708802 11.00000 -1.20000 AFIX 0 C20 1 0.247485 0.269160 0.629864 11.00000 0.02442 0.02172 = 0.02627 0.00042 0.00180 -0.00172 AFIX 43 H20 2 0.214970 0.317101 0.605363 11.00000 -1.20000 AFIX 0 C21 1 0.301963 0.456005 0.541316 11.00000 0.02548 0.01696 = 0.02627 0.00065 0.00033 -0.00300 C22 1 0.343152 0.493136 0.595016 11.00000 0.03234 0.02302 = 0.02367 0.00154 0.00029 -0.00083 AFIX 43 H22 2 0.392299 0.459712 0.606579 11.00000 -1.20000 AFIX 0 C23 1 0.313033 0.578465 0.631738 11.00000 0.04402 0.01978 = 0.02496 -0.00161 0.00551 -0.00574 AFIX 43 H23 2 0.341359 0.602888 0.668332 11.00000 -1.20000 AFIX 0 C24 1 0.241056 0.628212 0.614730 11.00000 0.04636 0.01876 = 0.03165 -0.00391 0.01601 -0.00065 AFIX 43 H24 2 0.219540 0.685330 0.640286 11.00000 -1.20000 AFIX 0 C25 1 0.201126 0.593881 0.560380 11.00000 0.03062 0.02547 = 0.03801 0.00410 0.00824 0.00199 AFIX 43 H25 2 0.153037 0.629211 0.547934 11.00000 -1.20000 AFIX 0 C26 1 0.231083 0.508119 0.524058 11.00000 0.02715 0.02084 = 0.03258 0.00173 0.00050 0.00172 AFIX 43 H26 2 0.203041 0.484711 0.487102 11.00000 -1.20000 AFIX 0 C27 1 0.328615 0.431840 0.389819 11.00000 0.02311 0.02345 = 0.02580 -0.00016 0.00330 -0.00059 C28 1 0.341998 0.543382 0.404616 11.00000 0.03422 0.02192 = 0.02802 0.00105 0.00007 0.00010 AFIX 43 H28 2 0.363307 0.562470 0.445112 11.00000 -1.20000 AFIX 0 C29 1 0.324561 0.625302 0.361057 11.00000 0.04491 0.01888 = 0.02874 0.00295 -0.00172 0.00084 AFIX 43 H29 2 0.332359 0.699903 0.372456 11.00000 -1.20000 AFIX 0 C30 1 0.295882 0.599280 0.301090 11.00000 0.05659 0.02602 = 0.03171 0.00893 -0.00459 0.00505 AFIX 43 H30 2 0.283663 0.655662 0.271401 11.00000 -1.20000 AFIX 0 C31 1 0.285085 0.489873 0.284625 11.00000 0.05237 0.03038 = 0.02298 0.00324 -0.00529 0.00191 AFIX 43 H31 2 0.266627 0.471371 0.243156 11.00000 -1.20000 AFIX 0 C32 1 0.301139 0.407613 0.328464 11.00000 0.03401 0.02271 = 0.02486 -0.00261 -0.00063 0.00288 AFIX 43 H32 2 0.293296 0.333263 0.316540 11.00000 -1.20000 AFIX 0 C33 1 0.593276 0.190104 0.330202 11.00000 0.02789 0.02097 = 0.02480 -0.00223 0.00506 -0.00306 C34 1 0.566494 0.214837 0.268780 11.00000 0.03576 0.02277 = 0.02497 -0.00350 -0.00006 -0.00295 C35 1 0.488224 0.271649 0.259186 11.00000 0.04315 0.03910 = 0.03601 0.00129 -0.00667 0.00510 AFIX 137 H35A 2 0.446900 0.234730 0.284361 11.00000 -1.50000 H35B 2 0.473743 0.269284 0.213920 11.00000 -1.50000 H35C 2 0.492766 0.348139 0.272994 11.00000 -1.50000 AFIX 0 C36 1 0.615421 0.183198 0.218033 11.00000 0.05174 0.02858 = 0.02845 -0.00406 0.00635 -0.01154 AFIX 43 H36 2 0.598949 0.197116 0.175438 11.00000 -1.20000 AFIX 0 C37 1 0.687825 0.131645 0.229369 11.00000 0.04788 0.03128 = 0.04254 -0.00979 0.02213 -0.00507 AFIX 43 H37 2 0.721016 0.112063 0.194436 11.00000 -1.20000 AFIX 0 C38 1 0.712200 0.108501 0.290525 11.00000 0.03150 0.02830 = 0.05110 -0.00830 0.00856 -0.00119 AFIX 43 H38 2 0.761845 0.072581 0.297136 11.00000 -1.20000 AFIX 0 C39 1 0.665769 0.136554 0.342631 11.00000 0.02815 0.02341 = 0.03793 -0.00369 0.00270 0.00021 C40 1 0.690938 0.112744 0.409943 11.00000 0.04332 0.04318 = 0.04538 -0.00202 -0.01017 0.00837 AFIX 137 H40A 2 0.697759 0.181828 0.433163 11.00000 -1.50000 H40B 2 0.741584 0.072510 0.409616 11.00000 -1.50000 H40C 2 0.649900 0.068351 0.430990 11.00000 -1.50000 AFIX 0 C41 1 0.556821 0.177745 0.661976 11.00000 0.02357 0.02890 = 0.02638 0.00228 -0.00381 -0.00148 C42 1 0.580499 0.068158 0.665803 11.00000 0.02342 0.02964 = 0.03484 0.00509 -0.00504 0.00010 C43 1 0.593492 0.000910 0.607388 11.00000 0.05014 0.03172 = 0.04762 -0.00646 -0.00336 0.00781 AFIX 137 H43A 2 0.541778 -0.021491 0.589824 11.00000 -1.50000 H43B 2 0.624754 -0.064352 0.618305 11.00000 -1.50000 H43C 2 0.622491 0.044347 0.575618 11.00000 -1.50000 AFIX 0 C44 1 0.588829 0.022830 0.726356 11.00000 0.03309 0.03671 = 0.04931 0.01607 -0.00903 -0.00574 AFIX 43 H44 2 0.604670 -0.051553 0.730785 11.00000 -1.20000 AFIX 0 C45 1 0.574163 0.085501 0.780242 11.00000 0.03409 0.07459 = 0.02923 0.01433 -0.00692 -0.00892 AFIX 43 H45 2 0.579116 0.053327 0.821313 11.00000 -1.20000 AFIX 0 C46 1 0.552385 0.194443 0.774756 11.00000 0.03752 0.06911 = 0.02911 -0.01239 -0.00549 0.00349 AFIX 43 H46 2 0.543125 0.236364 0.812217 11.00000 -1.20000 AFIX 0 C47 1 0.543863 0.243379 0.715643 11.00000 0.03179 0.04217 = 0.03162 -0.00838 -0.00667 0.00190 C48 1 0.518130 0.360867 0.707377 11.00000 0.06822 0.04964 = 0.06235 -0.02579 -0.02351 0.02085 AFIX 137 H48A 2 0.549030 0.394599 0.672876 11.00000 -1.50000 H48B 2 0.527450 0.401122 0.747135 11.00000 -1.50000 H48C 2 0.461175 0.363298 0.696745 11.00000 -1.50000 AFIX 0 C49 1 0.559033 0.611834 0.465130 11.00000 0.02529 0.02075 = 0.02916 0.00625 -0.00288 -0.00118 C50 1 0.574784 0.695569 0.508399 11.00000 0.02632 0.02217 = 0.03313 0.00128 -0.00224 0.00145 C51 1 0.546798 0.686186 0.576057 11.00000 0.03549 0.03120 = 0.03389 -0.00639 0.00238 -0.00505 AFIX 137 H51A 2 0.488492 0.679505 0.576812 11.00000 -1.50000 H51B 2 0.562872 0.751732 0.599833 11.00000 -1.50000 H51C 2 0.570728 0.621185 0.595776 11.00000 -1.50000 AFIX 0 C52 1 0.618525 0.785155 0.486191 11.00000 0.03098 0.02119 = 0.04466 -0.00236 0.00162 -0.00272 AFIX 43 H52 2 0.632142 0.842696 0.514717 11.00000 -1.20000 AFIX 0 C53 1 0.642326 0.791083 0.422925 11.00000 0.02574 0.02432 = 0.04898 0.00938 0.00305 -0.00216 AFIX 43 H53 2 0.670757 0.853558 0.408235 11.00000 -1.20000 AFIX 0 C54 1 0.625079 0.707142 0.381233 11.00000 0.03133 0.03335 = 0.03448 0.01086 0.00365 -0.00340 AFIX 43 H54 2 0.641741 0.712719 0.338044 11.00000 -1.20000 AFIX 0 C55 1 0.583670 0.614195 0.401151 11.00000 0.03299 0.02879 = 0.03084 0.00399 -0.00213 -0.00197 C56 1 0.569459 0.518377 0.358345 11.00000 0.05724 0.04477 = 0.02941 -0.00162 0.00354 -0.01206 AFIX 137 H56A 2 0.596322 0.453630 0.375809 11.00000 -1.50000 H56B 2 0.590747 0.534355 0.315812 11.00000 -1.50000 H56C 2 0.511980 0.504244 0.355315 11.00000 -1.50000 AFIX 0 HKLF 4 REM c130922_1_1_a.res in Pca2(1) REM wR2 = 0.1093, GooF = S = 1.048, Restrained GooF = 1.048 for all data REM R1 = 0.0422 for 6449 Fo > 4sig(Fo) and 0.0514 for all 7440 data REM 556 parameters refined using 1 restraints END WGHT 0.0630 0.0000 REM Highest difference peak 0.362, deepest hole -0.402, 1-sigma level 0.055 Q1 1 0.3681 0.3413 0.4907 11.00000 0.05 0.36 Q2 1 0.5024 0.3596 0.4911 11.00000 0.05 0.30 Q3 1 0.4364 0.3825 0.4505 11.00000 0.05 0.29 Q4 1 0.4459 0.3737 0.4933 11.00000 0.05 0.26 Q5 1 0.5096 0.3386 0.4841 11.00000 0.05 0.26 Q6 1 0.2710 0.1961 0.3944 11.00000 0.05 0.24 Q7 1 0.4536 0.2249 0.4496 11.00000 0.05 0.23 Q8 1 0.3573 0.5009 0.3941 11.00000 0.05 0.23 Q9 1 0.5134 0.2780 0.5144 11.00000 0.05 0.23 Q10 1 0.4333 0.2228 0.5796 11.00000 0.05 0.22 Q11 1 0.4270 0.4616 0.5130 11.00000 0.05 0.22 Q12 1 0.4401 0.3813 0.5321 11.00000 0.05 0.22 Q13 1 0.6070 0.1587 0.6525 11.00000 0.05 0.22 Q14 1 0.3348 0.2868 0.4222 11.00000 0.05 0.22 Q15 1 0.4389 0.2805 0.5921 11.00000 0.05 0.21 Q16 1 0.4436 0.2843 0.3869 11.00000 0.05 0.21 Q17 1 0.5105 0.2606 0.4833 11.00000 0.05 0.20 Q18 1 0.5685 0.3008 0.5179 11.00000 0.05 0.20 Q19 1 0.4451 0.4478 0.4204 11.00000 0.05 0.20 Q20 1 0.4983 0.3430 0.2558 11.00000 0.05 0.19 ; _shelx_res_checksum 6890 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe1 0.44212(3) 0.29727(4) 0.49025(3) 0.01969(13) Uani d 1 . . O O1 0.34098(16) 0.1785(2) 0.37047(13) 0.0247(6) Uani d 1 . . N N1 0.5466(2) 0.2208(3) 0.38217(18) 0.0258(7) Uani d 1 . . N N2 0.5401(2) 0.2204(3) 0.60128(19) 0.0278(7) Uani d 1 . . N N3 0.51844(17) 0.5183(2) 0.48677(19) 0.0255(6) Uani d 1 . . C C1 0.5072(2) 0.2484(3) 0.4249(2) 0.0259(9) Uani d 1 . . C C2 0.5031(2) 0.2504(3) 0.55733(19) 0.0241(8) Uani d 1 . . C C3 0.4886(2) 0.4325(3) 0.4898(2) 0.0240(7) Uani d 1 . . C C4 0.3418(2) 0.2250(3) 0.4232(2) 0.0219(8) Uani d 1 . . C C5 0.35340(18) 0.1724(2) 0.4859(2) 0.0210(6) Uani d 1 . . C C6 0.3355(2) 0.2502(3) 0.53539(19) 0.0199(7) Uani d 1 . . C C7 0.3282(2) 0.3565(3) 0.50543(18) 0.0208(7) Uani d 1 . . C C8 0.3381(2) 0.3442(3) 0.43788(18) 0.0211(7) Uani d 1 . . C C9 0.3600(2) 0.0516(2) 0.4933(2) 0.0233(7) Uani d 1 . . C C10 0.4154(2) -0.0087(3) 0.4587(2) 0.0270(8) Uani d 1 . . H H10 0.451113 0.028206 0.430856 0.032 Uiso calc 1 . . C C11 0.4194(3) -0.1221(3) 0.4642(2) 0.0337(9) Uani d 1 . . H H11 0.457570 -0.161958 0.439927 0.040 Uiso calc 1 . . C C12 0.3681(3) -0.1774(3) 0.5049(2) 0.0356(10) Uani d 1 . . H H12 0.371492 -0.254748 0.509268 0.043 Uiso calc 1 . . C C13 0.3116(3) -0.1186(3) 0.5392(2) 0.0334(9) Uani d 1 . . H H13 0.275669 -0.155950 0.566711 0.040 Uiso calc 1 . . C C14 0.3076(3) -0.0055(3) 0.5335(2) 0.0297(8) Uani d 1 . . H H14 0.268673 0.033951 0.557136 0.036 Uiso calc 1 . . C C15 0.3175(2) 0.2258(3) 0.6031(2) 0.0224(7) Uani d 1 . . C C16 0.3635(2) 0.1555(3) 0.64050(19) 0.0250(8) Uani d 1 . . H H16 0.410074 0.122967 0.622858 0.030 Uiso calc 1 . . C C17 0.3424(2) 0.1321(3) 0.7032(2) 0.0289(8) Uani d 1 . . H H17 0.375556 0.086079 0.728307 0.035 Uiso calc 1 . . C C18 0.2733(2) 0.1755(3) 0.7291(2) 0.0286(8) Uani d 1 . . H H18 0.258942 0.159492 0.771960 0.034 Uiso calc 1 . . C C19 0.2253(2) 0.2427(3) 0.6918(2) 0.0284(8) Uani d 1 . . H H19 0.176829 0.270689 0.708802 0.034 Uiso calc 1 . . C C20 0.2475(2) 0.2692(3) 0.62986(19) 0.0241(8) Uani d 1 . . H H20 0.214970 0.317101 0.605363 0.029 Uiso calc 1 . . C C21 0.3020(2) 0.4560(3) 0.54132(19) 0.0229(7) Uani d 1 . . C C22 0.3432(2) 0.4931(3) 0.59502(19) 0.0263(8) Uani d 1 . . H H22 0.392299 0.459712 0.606579 0.032 Uiso calc 1 . . C C23 0.3130(3) 0.5785(3) 0.6317(2) 0.0296(8) Uani d 1 . . H H23 0.341359 0.602888 0.668332 0.036 Uiso calc 1 . . C C24 0.2411(3) 0.6282(3) 0.6147(2) 0.0323(9) Uani d 1 . . H H24 0.219540 0.685330 0.640286 0.039 Uiso calc 1 . . C C25 0.2011(2) 0.5939(3) 0.5604(2) 0.0314(9) Uani d 1 . . H H25 0.153037 0.629211 0.547934 0.038 Uiso calc 1 . . C C26 0.2311(2) 0.5081(3) 0.5241(2) 0.0269(8) Uani d 1 . . H H26 0.203041 0.484711 0.487102 0.032 Uiso calc 1 . . C C27 0.3286(2) 0.4318(3) 0.38982(19) 0.0241(8) Uani d 1 . . C C28 0.3420(2) 0.5434(3) 0.4046(2) 0.0281(8) Uani d 1 . . H H28 0.363307 0.562470 0.445112 0.034 Uiso calc 1 . . C C29 0.3246(3) 0.6253(3) 0.3611(2) 0.0308(9) Uani d 1 . . H H29 0.332359 0.699903 0.372456 0.037 Uiso calc 1 . . C C30 0.2959(3) 0.5993(3) 0.3011(2) 0.0381(10) Uani d 1 . . H H30 0.283663 0.655662 0.271401 0.046 Uiso calc 1 . . C C31 0.2851(3) 0.4899(3) 0.2846(2) 0.0352(9) Uani d 1 . . H H31 0.266627 0.471371 0.243156 0.042 Uiso calc 1 . . C C32 0.3011(2) 0.4076(3) 0.3285(2) 0.0272(8) Uani d 1 . . H H32 0.293296 0.333263 0.316540 0.033 Uiso calc 1 . . C C33 0.5933(2) 0.1901(3) 0.33020(19) 0.0245(8) Uani d 1 . . C C34 0.5665(2) 0.2148(3) 0.2688(2) 0.0278(9) Uani d 1 . . C C35 0.4882(3) 0.2716(4) 0.2592(2) 0.0394(10) Uani d 1 . . H H35A 0.446900 0.234730 0.284361 0.059 Uiso calc 1 . . H H35B 0.473743 0.269284 0.213920 0.059 Uiso calc 1 . . H H35C 0.492766 0.348139 0.272994 0.059 Uiso calc 1 . . C C36 0.6154(3) 0.1832(3) 0.2180(2) 0.0363(10) Uani d 1 . . H H36 0.598949 0.197116 0.175438 0.044 Uiso calc 1 . . C C37 0.6878(3) 0.1316(3) 0.2294(2) 0.0406(11) Uani d 1 . . H H37 0.721016 0.112063 0.194436 0.049 Uiso calc 1 . . C C38 0.7122(3) 0.1085(3) 0.2905(2) 0.0370(10) Uani d 1 . . H H38 0.761845 0.072581 0.297136 0.044 Uiso calc 1 . . C C39 0.6658(2) 0.1366(3) 0.3426(2) 0.0298(9) Uani d 1 . . C C40 0.6909(3) 0.1127(4) 0.4099(3) 0.0440(11) Uani d 1 . . H H40A 0.697759 0.181828 0.433163 0.066 Uiso calc 1 . . H H40B 0.741584 0.072510 0.409616 0.066 Uiso calc 1 . . H H40C 0.649900 0.068351 0.430990 0.066 Uiso calc 1 . . C C41 0.5568(2) 0.1777(3) 0.6620(2) 0.0263(8) Uani d 1 . . C C42 0.5805(2) 0.0682(3) 0.6658(2) 0.0293(8) Uani d 1 . . C C43 0.5935(3) 0.0009(3) 0.6074(3) 0.0432(11) Uani d 1 . . H H43A 0.541778 -0.021491 0.589824 0.065 Uiso calc 1 . . H H43B 0.624754 -0.064352 0.618305 0.065 Uiso calc 1 . . H H43C 0.622491 0.044347 0.575618 0.065 Uiso calc 1 . . C C44 0.5888(3) 0.0228(4) 0.7264(3) 0.0397(11) Uani d 1 . . H H44 0.604670 -0.051553 0.730785 0.048 Uiso calc 1 . . C C45 0.5742(3) 0.0855(5) 0.7802(3) 0.0460(12) Uani d 1 . . H H45 0.579116 0.053327 0.821313 0.055 Uiso calc 1 . . C C46 0.5524(3) 0.1944(4) 0.7748(3) 0.0452(12) Uani d 1 . . H H46 0.543125 0.236364 0.812217 0.054 Uiso calc 1 . . C C47 0.5439(3) 0.2434(4) 0.7156(2) 0.0352(10) Uani d 1 . . C C48 0.5181(4) 0.3609(4) 0.7074(3) 0.0601(16) Uani d 1 . . H H48A 0.549030 0.394599 0.672876 0.090 Uiso calc 1 . . H H48B 0.527450 0.401122 0.747135 0.090 Uiso calc 1 . . H H48C 0.461175 0.363298 0.696745 0.090 Uiso calc 1 . . C C49 0.5590(2) 0.6118(3) 0.46513(19) 0.0251(8) Uani d 1 . . C C50 0.5748(2) 0.6956(3) 0.5084(2) 0.0272(8) Uani d 1 . . C C51 0.5468(3) 0.6862(3) 0.5761(2) 0.0335(9) Uani d 1 . . H H51A 0.488492 0.679505 0.576812 0.050 Uiso calc 1 . . H H51B 0.562872 0.751732 0.599833 0.050 Uiso calc 1 . . H H51C 0.570728 0.621185 0.595776 0.050 Uiso calc 1 . . C C52 0.6185(2) 0.7852(3) 0.4862(3) 0.0323(8) Uani d 1 . . H H52 0.632142 0.842696 0.514717 0.039 Uiso calc 1 . . C C53 0.6423(2) 0.7911(3) 0.4229(2) 0.0330(9) Uani d 1 . . H H53 0.670757 0.853558 0.408235 0.040 Uiso calc 1 . . C C54 0.6251(2) 0.7071(3) 0.3812(2) 0.0331(9) Uani d 1 . . H H54 0.641741 0.712719 0.338044 0.040 Uiso calc 1 . . C C55 0.5837(2) 0.6142(3) 0.4012(2) 0.0309(9) Uani d 1 . . C C56 0.5695(3) 0.5184(4) 0.3583(2) 0.0438(11) Uani d 1 . . H H56A 0.596322 0.453630 0.375809 0.066 Uiso calc 1 . . H H56B 0.590747 0.534355 0.315812 0.066 Uiso calc 1 . . H H56C 0.511980 0.504244 0.355315 0.066 Uiso calc 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Fe1 0.0222(2) 0.0168(2) 0.0200(3) -0.00091(18) 0.0003(3) 0.0004(2) O1 0.0310(14) 0.0216(11) 0.0215(15) 0.0005(10) -0.0023(11) -0.0012(10) N1 0.0261(17) 0.0258(15) 0.026(2) -0.0001(12) 0.0045(14) -0.0020(13) N2 0.0252(16) 0.0279(15) 0.030(2) -0.0020(13) -0.0012(15) 0.0070(15) N3 0.0288(14) 0.0203(12) 0.0273(16) -0.0042(10) -0.0006(15) 0.0011(14) C1 0.0249(19) 0.0188(15) 0.034(3) -0.0028(14) -0.0081(18) 0.0025(15) C2 0.0270(19) 0.0181(15) 0.027(2) -0.0033(13) -0.0001(17) -0.0010(14) C3 0.0262(16) 0.0259(15) 0.0197(18) 0.0019(12) -0.0009(17) 0.0007(16) C4 0.0197(17) 0.0207(15) 0.025(2) -0.0003(13) -0.0009(15) -0.0027(14) C5 0.0188(14) 0.0172(13) 0.0270(19) -0.0026(10) 0.0010(17) -0.0038(16) C6 0.0177(16) 0.0190(14) 0.023(2) -0.0017(12) 0.0010(14) 0.0010(14) C7 0.0219(16) 0.0192(14) 0.021(2) 0.0002(12) -0.0009(13) -0.0009(13) C8 0.0195(17) 0.0179(15) 0.026(2) 0.0014(12) -0.0052(14) 0.0002(14) C9 0.0290(16) 0.0202(14) 0.0206(19) -0.0010(12) -0.0047(17) -0.0004(16) C10 0.0296(19) 0.0218(16) 0.030(2) -0.0014(14) -0.0023(16) -0.0044(15) C11 0.041(2) 0.0235(17) 0.037(2) 0.0063(15) -0.0090(18) -0.0079(16) C12 0.053(3) 0.0182(15) 0.035(3) 0.0018(16) -0.0157(19) 0.0020(15) C13 0.053(3) 0.0231(16) 0.024(2) -0.0080(17) -0.0036(19) 0.0026(16) C14 0.039(2) 0.0248(17) 0.026(2) -0.0059(15) 0.0000(17) -0.0030(15) C15 0.0235(17) 0.0185(14) 0.025(2) -0.0040(12) -0.0021(16) -0.0019(14) C16 0.0270(18) 0.0222(15) 0.026(2) -0.0022(13) 0.0007(15) 0.0008(14) C17 0.035(2) 0.0249(16) 0.027(2) -0.0061(15) -0.0033(16) 0.0035(15) C18 0.038(2) 0.0278(17) 0.020(2) -0.0089(15) 0.0047(17) -0.0019(15) C19 0.0304(19) 0.0258(17) 0.029(2) -0.0030(15) 0.0060(16) -0.0047(15) C20 0.0244(18) 0.0217(15) 0.026(2) -0.0017(13) 0.0018(15) 0.0004(14) C21 0.0255(18) 0.0170(14) 0.026(2) -0.0030(13) 0.0003(15) 0.0006(14) C22 0.032(2) 0.0230(16) 0.024(2) -0.0008(14) 0.0003(16) 0.0015(14) C23 0.044(2) 0.0198(15) 0.025(2) -0.0057(15) 0.0055(17) -0.0016(15) C24 0.046(2) 0.0188(15) 0.032(2) -0.0007(15) 0.0160(19) -0.0039(15) C25 0.031(2) 0.0255(17) 0.038(3) 0.0020(15) 0.0082(18) 0.0041(16) C26 0.0271(18) 0.0208(15) 0.033(2) 0.0017(14) 0.0005(16) 0.0017(15) C27 0.0231(18) 0.0234(16) 0.026(2) -0.0006(13) 0.0033(15) -0.0002(14) C28 0.034(2) 0.0219(16) 0.028(2) 0.0001(15) 0.0001(17) 0.0010(15) C29 0.045(2) 0.0189(15) 0.029(2) 0.0008(15) -0.0017(18) 0.0030(15) C30 0.057(3) 0.0260(18) 0.032(3) 0.0050(18) -0.005(2) 0.0089(16) C31 0.052(3) 0.0304(18) 0.023(2) 0.0019(18) -0.005(2) 0.0032(17) C32 0.034(2) 0.0227(16) 0.025(2) 0.0029(14) -0.0006(16) -0.0026(15) C33 0.0279(19) 0.0210(15) 0.025(2) -0.0031(13) 0.0051(16) -0.0022(14) C34 0.036(2) 0.0228(16) 0.025(2) -0.0030(15) -0.0001(17) -0.0035(14) C35 0.043(3) 0.039(2) 0.036(3) 0.0051(19) -0.007(2) 0.0013(18) C36 0.052(3) 0.0286(19) 0.028(2) -0.0115(18) 0.006(2) -0.0041(17) C37 0.048(3) 0.031(2) 0.043(3) -0.0051(18) 0.022(2) -0.0098(19) C38 0.031(2) 0.0283(18) 0.051(3) -0.0012(16) 0.009(2) -0.0083(18) C39 0.0281(19) 0.0234(16) 0.038(3) 0.0002(14) 0.0027(17) -0.0037(16) C40 0.043(3) 0.043(2) 0.045(3) 0.008(2) -0.010(2) -0.002(2) C41 0.0236(19) 0.0289(17) 0.026(2) -0.0015(14) -0.0038(16) 0.0023(16) C42 0.0234(18) 0.0296(18) 0.035(2) 0.0001(14) -0.0050(17) 0.0051(17) C43 0.050(3) 0.032(2) 0.048(3) 0.0078(18) -0.003(2) -0.006(2) C44 0.033(2) 0.037(2) 0.049(3) -0.0057(17) -0.009(2) 0.016(2) C45 0.034(2) 0.075(3) 0.029(3) -0.009(2) -0.0069(19) 0.014(3) C46 0.038(2) 0.069(3) 0.029(3) 0.003(2) -0.005(2) -0.012(2) C47 0.032(2) 0.042(2) 0.032(3) 0.0019(18) -0.0067(19) -0.008(2) C48 0.068(4) 0.050(3) 0.062(4) 0.021(3) -0.024(3) -0.026(3) C49 0.0253(17) 0.0208(16) 0.029(2) -0.0012(13) -0.0029(15) 0.0063(14) C50 0.0263(18) 0.0222(16) 0.033(2) 0.0015(13) -0.0022(15) 0.0013(15) C51 0.035(2) 0.0312(19) 0.034(3) -0.0050(16) 0.0024(18) -0.0064(17) C52 0.0310(18) 0.0212(14) 0.045(2) -0.0027(12) 0.002(2) -0.0024(18) C53 0.0257(19) 0.0243(17) 0.049(3) -0.0022(15) 0.0031(18) 0.0094(17) C54 0.031(2) 0.0333(19) 0.034(3) -0.0034(15) 0.0037(17) 0.0109(18) C55 0.033(2) 0.0288(18) 0.031(2) -0.0020(15) -0.0021(17) 0.0040(16) C56 0.057(3) 0.045(2) 0.029(3) -0.012(2) 0.004(2) -0.002(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 1 -1 0.0158 1 1 2 0.0267 1 1 0 0.0389 0 0 1 0.0099 10 -2 4 0.0624 7 -1 -10 0.0561 -1 1 -13 0.0228 0 -2 -13 0.0156 8 -5 -4 0.0507 0 -6 -9 0.0153 4 -7 1 0.0268 0 -8 0 0.0074 0 -7 7 0.0066 -3 -8 -1 0.0166 -10 -3 0 0.0649 -6 6 3 0.0442 0 8 2 0.0138 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C1 Fe1 C4 . . 81.84(15) ? C1 Fe1 C5 . . 98.56(15) ? C1 Fe1 C6 . . 138.28(15) ? C1 Fe1 C7 . . 140.51(16) ? C1 Fe1 C8 . . 100.74(16) ? C2 Fe1 C1 . . 98.02(16) ? C2 Fe1 C4 . . 137.55(14) ? C2 Fe1 C5 . . 101.46(16) ? C2 Fe1 C6 . . 92.42(16) ? C2 Fe1 C7 . . 120.43(17) ? C2 Fe1 C8 . . 158.98(16) ? C3 Fe1 C1 . . 92.11(17) ? C3 Fe1 C2 . . 92.78(17) ? C3 Fe1 C4 . . 129.67(15) ? C3 Fe1 C5 . . 160.77(14) ? C3 Fe1 C6 . . 127.73(15) ? C3 Fe1 C7 . . 94.48(14) ? C3 Fe1 C8 . . 95.90(14) ? C5 Fe1 C4 . . 37.91(15) ? C5 Fe1 C8 . . 66.48(13) ? C6 Fe1 C4 . . 63.99(14) ? C6 Fe1 C5 . . 39.73(14) ? C6 Fe1 C8 . . 67.18(14) ? C7 Fe1 C4 . . 64.22(13) ? C7 Fe1 C5 . . 67.20(12) ? C7 Fe1 C6 . . 40.63(13) ? C7 Fe1 C8 . . 39.85(15) ? C8 Fe1 C4 . . 38.22(12) ? C1 N1 C33 . . 178.6(4) ? C2 N2 C41 . . 159.5(4) ? C3 N3 C49 . . 163.5(4) ? N1 C1 Fe1 . . 177.1(4) ? N2 C2 Fe1 . . 178.1(4) ? N3 C3 Fe1 . . 177.1(4) ? O1 C4 Fe1 . . 135.1(3) ? O1 C4 C5 . . 126.5(3) ? O1 C4 C8 . . 129.0(3) ? C5 C4 Fe1 . . 62.53(18) ? C5 C4 C8 . . 104.3(3) ? C8 C4 Fe1 . . 62.74(18) ? C4 C5 Fe1 . . 79.56(19) ? C4 C5 C9 . . 122.3(3) ? C6 C5 Fe1 . . 69.06(18) ? C6 C5 C4 . . 109.2(3) ? C6 C5 C9 . . 126.5(4) ? C9 C5 Fe1 . . 130.8(2) ? C5 C6 Fe1 . . 71.21(19) ? C5 C6 C7 . . 107.2(3) ? C5 C6 C15 . . 127.0(3) ? C7 C6 Fe1 . . 68.35(19) ? C7 C6 C15 . . 125.4(3) ? C15 C6 Fe1 . . 131.2(3) ? C6 C7 Fe1 . . 71.02(19) ? C6 C7 C21 . . 122.3(3) ? C8 C7 Fe1 . . 72.8(2) ? C8 C7 C6 . . 109.0(3) ? C8 C7 C21 . . 128.1(3) ? C21 C7 Fe1 . . 129.3(2) ? C4 C8 Fe1 . . 79.0(2) ? C7 C8 Fe1 . . 67.4(2) ? C7 C8 C4 . . 108.1(3) ? C7 C8 C27 . . 125.8(3) ? C27 C8 Fe1 . . 129.2(3) ? C27 C8 C4 . . 124.8(3) ? C10 C9 C5 . . 121.4(3) ? C10 C9 C14 . . 118.0(3) ? C14 C9 C5 . . 120.6(3) ? C9 C10 H10 . . 119.4 ? C9 C10 C11 . . 121.1(4) ? C11 C10 H10 . . 119.4 ? C10 C11 H11 . . 119.9 ? C12 C11 C10 . . 120.3(4) ? C12 C11 H11 . . 119.9 ? C11 C12 H12 . . 120.3 ? C11 C12 C13 . . 119.4(3) ? C13 C12 H12 . . 120.3 ? C12 C13 H13 . . 119.9 ? C14 C13 C12 . . 120.2(4) ? C14 C13 H13 . . 119.9 ? C9 C14 H14 . . 119.5 ? C13 C14 C9 . . 121.1(4) ? C13 C14 H14 . . 119.5 ? C16 C15 C6 . . 123.4(3) ? C16 C15 C20 . . 118.0(4) ? C20 C15 C6 . . 118.4(3) ? C15 C16 H16 . . 119.4 ? C17 C16 C15 . . 121.1(4) ? C17 C16 H16 . . 119.4 ? C16 C17 H17 . . 119.8 ? C18 C17 C16 . . 120.4(4) ? C18 C17 H17 . . 119.8 ? C17 C18 H18 . . 120.4 ? C17 C18 C19 . . 119.2(4) ? C19 C18 H18 . . 120.4 ? C18 C19 H19 . . 119.7 ? C20 C19 C18 . . 120.6(4) ? C20 C19 H19 . . 119.7 ? C15 C20 H20 . . 119.7 ? C19 C20 C15 . . 120.6(4) ? C19 C20 H20 . . 119.7 ? C22 C21 C7 . . 121.6(3) ? C26 C21 C7 . . 119.3(3) ? C26 C21 C22 . . 118.8(3) ? C21 C22 H22 . . 119.6 ? C23 C22 C21 . . 120.7(4) ? C23 C22 H22 . . 119.6 ? C22 C23 H23 . . 120.1 ? C22 C23 C24 . . 119.8(4) ? C24 C23 H23 . . 120.1 ? C23 C24 H24 . . 120.2 ? C25 C24 C23 . . 119.7(4) ? C25 C24 H24 . . 120.2 ? C24 C25 H25 . . 119.9 ? C24 C25 C26 . . 120.3(4) ? C26 C25 H25 . . 119.9 ? C21 C26 H26 . . 119.7 ? C25 C26 C21 . . 120.6(4) ? C25 C26 H26 . . 119.7 ? C28 C27 C8 . . 122.0(3) ? C32 C27 C8 . . 120.7(3) ? C32 C27 C28 . . 117.2(3) ? C27 C28 H28 . . 119.5 ? C29 C28 C27 . . 121.1(4) ? C29 C28 H28 . . 119.5 ? C28 C29 H29 . . 119.8 ? C30 C29 C28 . . 120.5(4) ? C30 C29 H29 . . 119.8 ? C29 C30 H30 . . 120.3 ? C29 C30 C31 . . 119.4(4) ? C31 C30 H30 . . 120.3 ? C30 C31 H31 . . 119.8 ? C32 C31 C30 . . 120.3(4) ? C32 C31 H31 . . 119.8 ? C27 C32 H32 . . 119.3 ? C31 C32 C27 . . 121.4(3) ? C31 C32 H32 . . 119.3 ? N1 C33 C34 . . 118.9(4) ? N1 C33 C39 . . 117.8(4) ? C34 C33 C39 . . 123.3(4) ? C33 C34 C35 . . 120.4(4) ? C33 C34 C36 . . 117.0(4) ? C36 C34 C35 . . 122.6(4) ? C34 C35 H35A . . 109.5 ? C34 C35 H35B . . 109.5 ? C34 C35 H35C . . 109.5 ? H35A C35 H35B . . 109.5 ? H35A C35 H35C . . 109.5 ? H35B C35 H35C . . 109.5 ? C34 C36 H36 . . 119.7 ? C37 C36 C34 . . 120.5(4) ? C37 C36 H36 . . 119.7 ? C36 C37 H37 . . 119.6 ? C38 C37 C36 . . 120.8(4) ? C38 C37 H37 . . 119.6 ? C37 C38 H38 . . 119.4 ? C37 C38 C39 . . 121.2(4) ? C39 C38 H38 . . 119.4 ? C33 C39 C40 . . 120.5(4) ? C38 C39 C33 . . 117.0(4) ? C38 C39 C40 . . 122.4(4) ? C39 C40 H40A . . 109.5 ? C39 C40 H40B . . 109.5 ? C39 C40 H40C . . 109.5 ? H40A C40 H40B . . 109.5 ? H40A C40 H40C . . 109.5 ? H40B C40 H40C . . 109.5 ? C42 C41 N2 . . 117.6(4) ? C42 C41 C47 . . 123.1(4) ? C47 C41 N2 . . 119.1(4) ? C41 C42 C43 . . 121.4(4) ? C44 C42 C41 . . 117.5(4) ? C44 C42 C43 . . 121.1(4) ? C42 C43 H43A . . 109.5 ? C42 C43 H43B . . 109.5 ? C42 C43 H43C . . 109.5 ? H43A C43 H43B . . 109.5 ? H43A C43 H43C . . 109.5 ? H43B C43 H43C . . 109.5 ? C42 C44 H44 . . 119.8 ? C45 C44 C42 . . 120.4(4) ? C45 C44 H44 . . 119.8 ? C44 C45 H45 . . 119.7 ? C46 C45 C44 . . 120.6(5) ? C46 C45 H45 . . 119.7 ? C45 C46 H46 . . 119.4 ? C45 C46 C47 . . 121.1(5) ? C47 C46 H46 . . 119.4 ? C41 C47 C48 . . 119.8(4) ? C46 C47 C41 . . 117.3(4) ? C46 C47 C48 . . 122.9(5) ? C47 C48 H48A . . 109.5 ? C47 C48 H48B . . 109.5 ? C47 C48 H48C . . 109.5 ? H48A C48 H48B . . 109.5 ? H48A C48 H48C . . 109.5 ? H48B C48 H48C . . 109.5 ? N3 C49 C55 . . 117.9(3) ? C50 C49 N3 . . 118.5(4) ? C50 C49 C55 . . 123.5(3) ? C49 C50 C51 . . 120.1(3) ? C49 C50 C52 . . 117.2(4) ? C52 C50 C51 . . 122.7(4) ? C50 C51 H51A . . 109.5 ? C50 C51 H51B . . 109.5 ? C50 C51 H51C . . 109.5 ? H51A C51 H51B . . 109.5 ? H51A C51 H51C . . 109.5 ? H51B C51 H51C . . 109.5 ? C50 C52 H52 . . 119.6 ? C53 C52 C50 . . 120.7(4) ? C53 C52 H52 . . 119.6 ? C52 C53 H53 . . 119.7 ? C54 C53 C52 . . 120.5(4) ? C54 C53 H53 . . 119.7 ? C53 C54 H54 . . 119.4 ? C53 C54 C55 . . 121.3(4) ? C55 C54 H54 . . 119.4 ? C49 C55 C56 . . 120.8(4) ? C54 C55 C49 . . 116.7(4) ? C54 C55 C56 . . 122.4(4) ? C55 C56 H56A . . 109.5 ? C55 C56 H56B . . 109.5 ? C55 C56 H56C . . 109.5 ? H56A C56 H56B . . 109.5 ? H56A C56 H56C . . 109.5 ? H56B C56 H56C . . 109.5 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Fe1 C1 . 1.850(4) ? Fe1 C2 . 1.830(4) ? Fe1 C3 . 1.825(3) ? Fe1 C4 . 2.361(4) ? Fe1 C5 . 2.130(3) ? Fe1 C6 . 2.101(4) ? Fe1 C7 . 2.065(3) ? Fe1 C8 . 2.137(3) ? O1 C4 . 1.243(5) ? N1 C1 . 1.162(6) ? N1 C33 . 1.392(5) ? N2 C2 . 1.169(5) ? N2 C41 . 1.403(6) ? N3 C3 . 1.162(4) ? N3 C49 . 1.403(4) ? C4 C5 . 1.475(6) ? C4 C8 . 1.487(4) ? C5 C6 . 1.438(5) ? C5 C9 . 1.487(4) ? C6 C7 . 1.447(5) ? C6 C15 . 1.482(6) ? C7 C8 . 1.434(6) ? C7 C21 . 1.494(5) ? C8 C27 . 1.478(5) ? C9 C10 . 1.388(5) ? C9 C14 . 1.402(5) ? C10 H10 . 0.9500 ? C10 C11 . 1.390(5) ? C11 H11 . 0.9500 ? C11 C12 . 1.387(6) ? C12 H12 . 0.9500 ? C12 C13 . 1.387(6) ? C13 H13 . 0.9500 ? C13 C14 . 1.387(5) ? C14 H14 . 0.9500 ? C15 C16 . 1.393(5) ? C15 C20 . 1.404(5) ? C16 H16 . 0.9500 ? C16 C17 . 1.390(6) ? C17 H17 . 0.9500 ? C17 C18 . 1.383(6) ? C18 H18 . 0.9500 ? C18 C19 . 1.390(6) ? C19 H19 . 0.9500 ? C19 C20 . 1.389(6) ? C20 H20 . 0.9500 ? C21 C22 . 1.396(5) ? C21 C26 . 1.394(5) ? C22 H22 . 0.9500 ? C22 C23 . 1.390(5) ? C23 H23 . 0.9500 ? C23 C24 . 1.396(6) ? C24 H24 . 0.9500 ? C24 C25 . 1.386(6) ? C25 H25 . 0.9500 ? C25 C26 . 1.388(5) ? C26 H26 . 0.9500 ? C27 C28 . 1.414(5) ? C27 C32 . 1.398(6) ? C28 H28 . 0.9500 ? C28 C29 . 1.385(5) ? C29 H29 . 0.9500 ? C29 C30 . 1.383(6) ? C30 H30 . 0.9500 ? C30 C31 . 1.390(6) ? C31 H31 . 0.9500 ? C31 C32 . 1.387(6) ? C32 H32 . 0.9500 ? C33 C34 . 1.397(6) ? C33 C39 . 1.403(5) ? C34 C35 . 1.496(6) ? C34 C36 . 1.397(6) ? C35 H35A . 0.9800 ? C35 H35B . 0.9800 ? C35 H35C . 0.9800 ? C36 H36 . 0.9500 ? C36 C37 . 1.386(7) ? C37 H37 . 0.9500 ? C37 C38 . 1.375(7) ? C38 H38 . 0.9500 ? C38 C39 . 1.384(6) ? C39 C40 . 1.501(7) ? C40 H40A . 0.9800 ? C40 H40B . 0.9800 ? C40 H40C . 0.9800 ? C41 C42 . 1.397(5) ? C41 C47 . 1.398(6) ? C42 C43 . 1.490(6) ? C42 C44 . 1.392(6) ? C43 H43A . 0.9800 ? C43 H43B . 0.9800 ? C43 H43C . 0.9800 ? C44 H44 . 0.9500 ? C44 C45 . 1.386(8) ? C45 H45 . 0.9500 ? C45 C46 . 1.383(8) ? C46 H46 . 0.9500 ? C46 C47 . 1.383(7) ? C47 C48 . 1.507(7) ? C48 H48A . 0.9800 ? C48 H48B . 0.9800 ? C48 H48C . 0.9800 ? C49 C50 . 1.391(5) ? C49 C55 . 1.404(6) ? C50 C51 . 1.498(6) ? C50 C52 . 1.396(5) ? C51 H51A . 0.9800 ? C51 H51B . 0.9800 ? C51 H51C . 0.9800 ? C52 H52 . 0.9500 ? C52 C53 . 1.387(7) ? C53 H53 . 0.9500 ? C53 C54 . 1.377(6) ? C54 H54 . 0.9500 ? C54 C55 . 1.393(5) ? C55 C56 . 1.493(6) ? C56 H56A . 0.9800 ? C56 H56B . 0.9800 ? C56 H56C . 0.9800 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Fe1 C4 C5 C6 . . . . 63.3(2) ? Fe1 C4 C5 C9 . . . . -132.0(3) ? Fe1 C4 C8 C7 . . . . -61.6(2) ? Fe1 C4 C8 C27 . . . . 130.5(4) ? Fe1 C5 C6 C7 . . . . 59.1(2) ? Fe1 C5 C6 C15 . . . . -128.0(4) ? Fe1 C5 C9 C10 . . . . -51.3(6) ? Fe1 C5 C9 C14 . . . . 131.7(4) ? Fe1 C6 C7 C8 . . . . 63.3(2) ? Fe1 C6 C7 C21 . . . . -125.1(3) ? Fe1 C6 C15 C16 . . . . -49.1(5) ? Fe1 C6 C15 C20 . . . . 135.7(3) ? Fe1 C7 C8 C4 . . . . 69.3(2) ? Fe1 C7 C8 C27 . . . . -122.9(4) ? Fe1 C7 C21 C22 . . . . -33.2(5) ? Fe1 C7 C21 C26 . . . . 152.1(3) ? Fe1 C8 C27 C28 . . . . -61.0(5) ? Fe1 C8 C27 C32 . . . . 122.9(4) ? O1 C4 C5 Fe1 . . . . 127.5(4) ? O1 C4 C5 C6 . . . . -169.2(4) ? O1 C4 C5 C9 . . . . -4.5(5) ? O1 C4 C8 Fe1 . . . . -127.4(4) ? O1 C4 C8 C7 . . . . 171.0(4) ? O1 C4 C8 C27 . . . . 3.0(6) ? N1 C33 C34 C35 . . . . -1.1(5) ? N1 C33 C34 C36 . . . . 179.6(3) ? N1 C33 C39 C38 . . . . -178.8(3) ? N1 C33 C39 C40 . . . . 0.6(5) ? N2 C41 C42 C43 . . . . 4.5(6) ? N2 C41 C42 C44 . . . . -173.3(4) ? N2 C41 C47 C46 . . . . 172.8(4) ? N2 C41 C47 C48 . . . . -4.5(6) ? N3 C49 C50 C51 . . . . -1.5(5) ? N3 C49 C50 C52 . . . . 177.1(3) ? N3 C49 C55 C54 . . . . -178.9(4) ? N3 C49 C55 C56 . . . . -2.1(6) ? C2 N2 C41 C42 . . . . 101.2(11) ? C2 N2 C41 C47 . . . . -74.3(12) ? C3 N3 C49 C50 . . . . -175.2(11) ? C3 N3 C49 C55 . . . . 2.9(14) ? C4 C5 C6 Fe1 . . . . -70.2(2) ? C4 C5 C6 C7 . . . . -11.1(4) ? C4 C5 C6 C15 . . . . 161.8(3) ? C4 C5 C9 C10 . . . . 53.9(5) ? C4 C5 C9 C14 . . . . -123.1(4) ? C4 C8 C27 C28 . . . . -166.6(3) ? C4 C8 C27 C32 . . . . 17.3(6) ? C5 C4 C8 Fe1 . . . . 48.2(2) ? C5 C4 C8 C7 . . . . -13.4(4) ? C5 C4 C8 C27 . . . . 178.7(3) ? C5 C6 C7 Fe1 . . . . -60.9(2) ? C5 C6 C7 C8 . . . . 2.4(4) ? C5 C6 C7 C21 . . . . 173.9(3) ? C5 C6 C15 C16 . . . . 48.0(5) ? C5 C6 C15 C20 . . . . -127.2(4) ? C5 C9 C10 C11 . . . . -177.7(4) ? C5 C9 C14 C13 . . . . 178.0(4) ? C6 C5 C9 C10 . . . . -144.1(4) ? C6 C5 C9 C14 . . . . 38.8(5) ? C6 C7 C8 Fe1 . . . . -62.2(2) ? C6 C7 C8 C4 . . . . 7.1(4) ? C6 C7 C8 C27 . . . . 174.9(3) ? C6 C7 C21 C22 . . . . 58.0(5) ? C6 C7 C21 C26 . . . . -116.8(4) ? C6 C15 C16 C17 . . . . -177.6(3) ? C6 C15 C20 C19 . . . . 175.7(3) ? C7 C6 C15 C16 . . . . -140.3(4) ? C7 C6 C15 C20 . . . . 44.5(5) ? C7 C8 C27 C28 . . . . 27.6(6) ? C7 C8 C27 C32 . . . . -148.5(4) ? C7 C21 C22 C23 . . . . -173.0(3) ? C7 C21 C26 C25 . . . . 173.5(3) ? C8 C4 C5 Fe1 . . . . -48.3(2) ? C8 C4 C5 C6 . . . . 15.0(3) ? C8 C4 C5 C9 . . . . 179.7(3) ? C8 C7 C21 C22 . . . . -132.2(4) ? C8 C7 C21 C26 . . . . 53.1(5) ? C8 C27 C28 C29 . . . . -173.0(4) ? C8 C27 C32 C31 . . . . 174.1(4) ? C9 C5 C6 Fe1 . . . . 125.9(3) ? C9 C5 C6 C7 . . . . -175.0(3) ? C9 C5 C6 C15 . . . . -2.1(6) ? C9 C10 C11 C12 . . . . -0.4(6) ? C10 C9 C14 C13 . . . . 0.9(6) ? C10 C11 C12 C13 . . . . 1.2(6) ? C11 C12 C13 C14 . . . . -1.0(6) ? C12 C13 C14 C9 . . . . -0.1(6) ? C14 C9 C10 C11 . . . . -0.7(6) ? C15 C6 C7 Fe1 . . . . 126.0(3) ? C15 C6 C7 C8 . . . . -170.7(3) ? C15 C6 C7 C21 . . . . 0.9(5) ? C15 C16 C17 C18 . . . . 2.3(5) ? C16 C15 C20 C19 . . . . 0.2(5) ? C16 C17 C18 C19 . . . . 0.0(5) ? C17 C18 C19 C20 . . . . -2.2(6) ? C18 C19 C20 C15 . . . . 2.1(5) ? C20 C15 C16 C17 . . . . -2.3(5) ? C21 C7 C8 Fe1 . . . . 126.9(4) ? C21 C7 C8 C4 . . . . -163.8(3) ? C21 C7 C8 C27 . . . . 3.9(6) ? C21 C22 C23 C24 . . . . -0.3(6) ? C22 C21 C26 C25 . . . . -1.3(5) ? C22 C23 C24 C25 . . . . -1.6(6) ? C23 C24 C25 C26 . . . . 2.1(6) ? C24 C25 C26 C21 . . . . -0.6(6) ? C26 C21 C22 C23 . . . . 1.8(6) ? C27 C28 C29 C30 . . . . -2.1(6) ? C28 C27 C32 C31 . . . . -2.1(6) ? C28 C29 C30 C31 . . . . -0.4(7) ? C29 C30 C31 C32 . . . . 1.5(7) ? C30 C31 C32 C27 . . . . -0.2(7) ? C32 C27 C28 C29 . . . . 3.3(6) ? C33 C34 C36 C37 . . . . -1.3(5) ? C34 C33 C39 C38 . . . . 0.5(5) ? C34 C33 C39 C40 . . . . 179.9(4) ? C34 C36 C37 C38 . . . . 1.4(6) ? C35 C34 C36 C37 . . . . 179.4(4) ? C36 C37 C38 C39 . . . . -0.5(6) ? C37 C38 C39 C33 . . . . -0.4(5) ? C37 C38 C39 C40 . . . . -179.8(4) ? C39 C33 C34 C35 . . . . 179.7(4) ? C39 C33 C34 C36 . . . . 0.3(5) ? C41 C42 C44 C45 . . . . -0.2(6) ? C42 C41 C47 C46 . . . . -2.5(6) ? C42 C41 C47 C48 . . . . -179.8(4) ? C42 C44 C45 C46 . . . . -1.1(7) ? C43 C42 C44 C45 . . . . -178.0(4) ? C44 C45 C46 C47 . . . . 0.7(7) ? C45 C46 C47 C41 . . . . 1.1(7) ? C45 C46 C47 C48 . . . . 178.3(5) ? C47 C41 C42 C43 . . . . 179.8(4) ? C47 C41 C42 C44 . . . . 2.1(6) ? C49 C50 C52 C53 . . . . 2.3(5) ? C50 C49 C55 C54 . . . . -0.9(6) ? C50 C49 C55 C56 . . . . 176.0(4) ? C50 C52 C53 C54 . . . . -1.8(6) ? C51 C50 C52 C53 . . . . -179.2(4) ? C52 C53 C54 C55 . . . . -0.2(6) ? C53 C54 C55 C49 . . . . 1.4(6) ? C53 C54 C55 C56 . . . . -175.3(4) ? C55 C49 C50 C51 . . . . -179.6(4) ? C55 C49 C50 C52 . . . . -1.0(5) ? _cod_database_fobs_code 2022784