#------------------------------------------------------------------------------ #$Date: 2020-08-18 05:02:47 +0300 (Tue, 18 Aug 2020) $ #$Revision: 255416 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/51/7705189.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_7705189 loop_ _publ_author_name 'Liang, Qiuming' 'Lin, Jack H.' 'DeMuth, Joshua C.' 'Neidig, Michael L.' 'Song, Datong' _publ_section_title ; Syntheses and Characterizations of Iron Complexes of Bulky o-Phenylenediamide ligand ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D0DT02087G _journal_year 2020 _chemical_formula_moiety 'C40 H48 Fe N4, C4 H10 O' _chemical_formula_sum 'C44 H58 Fe N4 O' _chemical_formula_weight 714.79 _space_group_crystal_system orthorhombic _space_group_IT_number 61 _space_group_name_Hall '-P 2ac 2ab' _space_group_name_H-M_alt 'P b c a' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2016/6 _audit_update_record ; 2020-08-11 deposited with the CCDC. 2020-08-17 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 19.1247(8) _cell_length_b 19.4899(10) _cell_length_c 21.8687(12) _cell_measurement_reflns_used 70372 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 27.544 _cell_measurement_theta_min 2.372 _cell_volume 8151.3(7) _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker Kappa Apex II' _diffrn_measurement_method 'Phi and Omega Scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1246 _diffrn_reflns_av_unetI/netI 0.0847 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 70465 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.544 _diffrn_reflns_theta_min 2.288 _exptl_absorpt_coefficient_mu 0.407 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.6304 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour 'dark purple' _exptl_crystal_density_diffrn 1.165 _exptl_crystal_description plate _exptl_crystal_F_000 3072 _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.726 _refine_diff_density_min -0.607 _refine_diff_density_rms 0.063 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 450 _refine_ls_number_reflns 9380 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.007 _refine_ls_R_factor_all 0.1197 _refine_ls_R_factor_gt 0.0552 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0537P)^2^+4.7246P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1173 _refine_ls_wR_factor_ref 0.1437 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5432 _reflns_number_total 9380 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02087g2.cif _cod_data_source_block wl307 _cod_database_code 7705189 _shelx_shelxl_version_number 2016/6 _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_res_file ; TITL wl307 in Pbca wl307.res created by SHELXL-2016/6 at 00:37:08 on 08-Aug-2020 CELL 0.71073 19.1247 19.4899 21.8687 90.000 90.000 90.000 ZERR 8.00 0.0008 0.0010 0.0012 0.000 0.000 0.000 LATT 1 SYMM x+1/2, -y+1/2, -z SYMM -x, y+1/2, -z+1/2 SYMM -x+1/2, -y, z+1/2 SFAC C H N O FE UNIT 352 464 32 8 8 TEMP -123.000 ACTA L.S. 8 FMAP 2 EADP O1 O1A EADP C41 C41A EADP C42 C42A EADP C43 C43A EADP C44 C44A OMIT 0 2 0 OMIT 0 0 2 OMIT 2 0 0 OMIT 1 1 1 PLAN 10 0 0.00 HTAB BOND $H CONF WGHT 0.053700 4.724600 FVAR 0.05117 0.42261 FE1 5 0.732980 0.204258 0.447348 11.00000 0.01883 0.01804 = 0.03549 0.00092 0.00016 0.00040 C1 1 0.616360 0.122627 0.438066 11.00000 0.02196 0.02086 = 0.01997 -0.00055 0.00179 0.00050 N1 3 0.633056 0.192133 0.438909 11.00000 0.01973 0.01839 = 0.03078 0.00107 0.00265 0.00254 N2 3 0.737827 0.106237 0.462327 11.00000 0.01946 0.01619 = 0.03757 0.00045 -0.00102 0.00142 C2 1 0.550425 0.095483 0.427269 11.00000 0.02165 0.02518 = 0.03839 -0.00211 -0.00167 0.00037 AFIX 43 H2 2 0.512793 0.125576 0.418064 11.00000 -1.20000 AFIX 0 N3 3 0.791372 0.248853 0.375536 11.00000 0.02412 0.03455 = 0.03783 0.00386 -0.00090 -0.00102 C3 1 0.538183 0.024866 0.429638 11.00000 0.02469 0.02980 = 0.04357 -0.00323 -0.00327 -0.00952 AFIX 43 H3 2 0.492392 0.007467 0.423077 11.00000 -1.20000 AFIX 0 N4 3 0.772503 0.270351 0.512959 11.00000 0.02268 0.01989 = 0.04037 -0.00049 -0.00184 0.00160 C4 1 0.592157 -0.019162 0.441406 11.00000 0.03581 0.02169 = 0.04789 -0.00475 0.00129 -0.00526 AFIX 43 H4 2 0.583984 -0.067224 0.442541 11.00000 -1.20000 AFIX 0 C5 1 0.659159 0.006402 0.451740 11.00000 0.02594 0.01873 = 0.04470 -0.00281 0.00250 0.00192 AFIX 43 H5 2 0.696379 -0.024675 0.459523 11.00000 -1.20000 AFIX 0 C6 1 0.672605 0.076434 0.450886 11.00000 0.02274 0.01938 = 0.02361 -0.00392 0.00252 0.00067 C7 1 0.578940 0.241906 0.434804 11.00000 0.01649 0.01660 = 0.03857 0.00159 0.00083 -0.00175 C8 1 0.551000 0.270930 0.488752 11.00000 0.01954 0.02096 = 0.03825 -0.00302 0.00497 -0.00247 C9 1 0.503321 0.324609 0.483444 11.00000 0.02482 0.02306 = 0.04980 -0.00923 0.00908 -0.00056 AFIX 43 H9 2 0.485171 0.345245 0.519457 11.00000 -1.20000 AFIX 0 C10 1 0.481835 0.348513 0.427157 11.00000 0.02353 0.01919 = 0.06652 0.00044 0.00111 0.00195 AFIX 43 H10 2 0.449535 0.385427 0.424540 11.00000 -1.20000 AFIX 0 C11 1 0.507485 0.318548 0.374834 11.00000 0.02690 0.02630 = 0.04898 0.00748 -0.00595 0.00098 AFIX 43 H11 2 0.491900 0.334691 0.336177 11.00000 -1.20000 AFIX 0 C12 1 0.555919 0.264930 0.377149 11.00000 0.02003 0.02272 = 0.03801 0.00267 -0.00290 -0.00141 C13 1 0.570265 0.243024 0.550854 11.00000 0.03466 0.03604 = 0.03684 -0.00250 0.00799 0.00483 AFIX 13 H13 2 0.616966 0.220406 0.546776 11.00000 -1.20000 AFIX 0 C14 1 0.576886 0.297594 0.600479 11.00000 0.06296 0.05632 = 0.03921 -0.00468 0.00467 -0.00998 AFIX 137 H14A 2 0.606109 0.335334 0.585521 11.00000 -1.50000 H14B 2 0.598441 0.277378 0.636924 11.00000 -1.50000 H14C 2 0.530364 0.315143 0.610887 11.00000 -1.50000 AFIX 0 C15 1 0.518386 0.188014 0.570805 11.00000 0.08113 0.04901 = 0.04596 0.00894 0.00794 -0.01913 AFIX 137 H15A 2 0.471152 0.207483 0.571705 11.00000 -1.50000 H15B 2 0.530873 0.171518 0.611705 11.00000 -1.50000 H15C 2 0.519785 0.149680 0.541831 11.00000 -1.50000 AFIX 0 C16 1 0.583136 0.234013 0.318524 11.00000 0.03465 0.03344 = 0.03122 0.00486 -0.00438 0.00531 AFIX 13 H16 2 0.613523 0.194220 0.329801 11.00000 -1.20000 AFIX 0 C17 1 0.628073 0.284575 0.282616 11.00000 0.05124 0.05679 = 0.04153 0.00586 0.00635 -0.00387 AFIX 137 H17A 2 0.648845 0.261202 0.247342 11.00000 -1.50000 H17B 2 0.665313 0.302280 0.309047 11.00000 -1.50000 H17C 2 0.598934 0.322731 0.268388 11.00000 -1.50000 AFIX 0 C18 1 0.523618 0.206469 0.278626 11.00000 0.05111 0.05764 = 0.04099 -0.00541 -0.00866 -0.00020 AFIX 137 H18A 2 0.493901 0.244641 0.265381 11.00000 -1.50000 H18B 2 0.495639 0.173748 0.302272 11.00000 -1.50000 H18C 2 0.543225 0.183391 0.242694 11.00000 -1.50000 AFIX 0 C31 1 0.816298 0.313805 0.376714 11.00000 0.04532 0.03543 = 0.04764 0.00721 0.00282 -0.01079 AFIX 43 H31 2 0.811763 0.339222 0.413569 11.00000 -1.20000 AFIX 0 C30 1 0.843606 -0.047365 0.371400 11.00000 0.06089 0.05653 = 0.09687 -0.04067 0.00376 0.01127 AFIX 137 H30A 2 0.843292 -0.045710 0.326612 11.00000 -1.50000 H30B 2 0.802536 -0.072710 0.385822 11.00000 -1.50000 H30C 2 0.886184 -0.070487 0.385439 11.00000 -1.50000 AFIX 0 C29 1 0.903729 0.068426 0.373432 11.00000 0.04187 0.07969 = 0.06952 -0.01219 0.00732 -0.00375 AFIX 137 H29A 2 0.902086 0.070373 0.328676 11.00000 -1.50000 H29B 2 0.947537 0.046786 0.386411 11.00000 -1.50000 H29C 2 0.901223 0.115049 0.390070 11.00000 -1.50000 AFIX 0 C28 1 0.841726 0.026324 0.397100 11.00000 0.02853 0.03881 = 0.06577 -0.01910 0.00101 0.00742 AFIX 13 H28 2 0.798134 0.048536 0.381422 11.00000 -1.20000 AFIX 0 C27 1 0.668928 0.057837 0.615205 11.00000 0.04821 0.06217 = 0.05948 -0.00627 0.00980 -0.00200 AFIX 137 H27A 2 0.648113 0.035780 0.579283 11.00000 -1.50000 H27B 2 0.633146 0.084622 0.636634 11.00000 -1.50000 H27C 2 0.687586 0.022641 0.642737 11.00000 -1.50000 AFIX 0 C26 1 0.755688 0.145298 0.649550 11.00000 0.09873 0.05380 = 0.04619 -0.00701 0.01179 -0.02287 AFIX 137 H26A 2 0.795825 0.173142 0.636884 11.00000 -1.50000 H26B 2 0.770245 0.113174 0.681588 11.00000 -1.50000 H26C 2 0.718786 0.175320 0.665388 11.00000 -1.50000 AFIX 0 C25 1 0.728068 0.105334 0.594882 11.00000 0.05991 0.03221 = 0.03506 0.00387 0.00317 0.00313 AFIX 13 H25 2 0.707476 0.139419 0.565831 11.00000 -1.20000 AFIX 0 C24 1 0.838187 0.027614 0.465561 11.00000 0.02347 0.01987 = 0.06030 -0.00827 -0.00441 0.00143 C23 1 0.886688 -0.009316 0.500803 11.00000 0.02767 0.02211 = 0.09019 -0.00090 -0.00851 0.00615 AFIX 43 H23 2 0.921695 -0.035586 0.480759 11.00000 -1.20000 AFIX 0 C22 1 0.884691 -0.008337 0.563211 11.00000 0.03131 0.02800 = 0.09302 0.02070 -0.02272 -0.00453 AFIX 43 H22 2 0.918158 -0.033580 0.586111 11.00000 -1.20000 AFIX 0 C21 1 0.834101 0.029288 0.592891 11.00000 0.04200 0.02892 = 0.05670 0.01861 -0.01534 -0.01524 AFIX 43 H21 2 0.833194 0.029766 0.636323 11.00000 -1.20000 AFIX 0 C20 1 0.784219 0.066670 0.560586 11.00000 0.03241 0.01812 = 0.04727 0.00380 -0.00533 -0.00583 C19 1 0.786954 0.066505 0.496265 11.00000 0.02220 0.01531 = 0.04677 0.00105 -0.00556 -0.00293 C32 1 0.847604 0.344878 0.327910 11.00000 0.05237 0.05373 = 0.06215 0.01541 0.00663 -0.01035 AFIX 43 H32 2 0.863174 0.391078 0.330450 11.00000 -1.20000 AFIX 0 C33 1 0.855933 0.308189 0.275721 11.00000 0.04163 0.07529 = 0.05480 0.02247 0.01006 -0.00514 AFIX 43 H33 2 0.878230 0.328401 0.241335 11.00000 -1.20000 AFIX 0 C34 1 0.832390 0.242555 0.272639 11.00000 0.06807 0.07492 = 0.04880 -0.00453 0.01550 0.00007 AFIX 43 H34 2 0.837977 0.216423 0.236296 11.00000 -1.20000 AFIX 0 C35 1 0.799946 0.214301 0.323673 11.00000 0.05186 0.05334 = 0.05182 -0.00460 0.00837 -0.00748 AFIX 43 H35 2 0.783240 0.168470 0.321377 11.00000 -1.20000 AFIX 0 C36 1 0.744165 0.331437 0.526737 11.00000 0.02913 0.02454 = 0.04451 -0.00085 -0.00264 0.00353 AFIX 43 H36 2 0.698940 0.341983 0.511421 11.00000 -1.20000 AFIX 0 C37 1 0.778047 0.379388 0.562174 11.00000 0.04203 0.02488 = 0.06257 -0.00785 -0.00070 0.00325 AFIX 43 H37 2 0.756672 0.422331 0.570715 11.00000 -1.20000 AFIX 0 C38 1 0.843117 0.364377 0.585020 11.00000 0.04258 0.03059 = 0.06240 -0.00977 -0.01136 -0.00526 AFIX 43 H38 2 0.867438 0.396794 0.609517 11.00000 -1.20000 AFIX 0 C39 1 0.872743 0.301375 0.571852 11.00000 0.02927 0.03235 = 0.06326 -0.00197 -0.01324 0.00026 AFIX 43 H39 2 0.917625 0.289535 0.587188 11.00000 -1.20000 AFIX 0 C40 1 0.835804 0.256501 0.536177 11.00000 0.02520 0.02237 = 0.05431 -0.00125 -0.00414 0.00178 AFIX 43 H40 2 0.856151 0.213143 0.527384 11.00000 -1.20000 AFIX 0 PART 1 O1 4 0.630666 -0.008696 0.251578 10.50000 0.06673 C42 1 0.511106 -0.030719 0.247926 10.50000 0.07252 AFIX 33 H42A 2 0.466072 -0.008330 0.255606 10.50000 -1.50000 H42B 2 0.513528 -0.045157 0.205053 10.50000 -1.50000 H42C 2 0.515690 -0.070956 0.274500 10.50000 -1.50000 AFIX 0 C41 1 0.572939 0.021776 0.261944 10.50000 0.07015 AFIX 23 H41A 2 0.568647 0.062737 0.235437 10.50000 -1.20000 H41B 2 0.570818 0.036844 0.305137 10.50000 -1.20000 AFIX 0 C44 1 0.728028 0.053465 0.244146 10.50000 0.12545 AFIX 33 H44A 2 0.772762 0.062915 0.264315 10.50000 -1.50000 H44B 2 0.736668 0.035791 0.202879 10.50000 -1.50000 H44C 2 0.700680 0.095888 0.241558 10.50000 -1.50000 AFIX 0 C43 1 0.698982 0.015295 0.270582 10.50000 0.08844 AFIX 23 H43A 2 0.693627 0.033991 0.312413 10.50000 -1.20000 H43B 2 0.729348 -0.025661 0.274020 10.50000 -1.20000 AFIX 0 PART 2 O1A 4 0.614529 -0.016705 0.249102 10.50000 0.06673 C42A 1 0.494025 -0.035074 0.268667 10.50000 0.07252 AFIX 33 H42D 2 0.449086 -0.012038 0.275167 10.50000 -1.50000 H42E 2 0.490773 -0.065018 0.232779 10.50000 -1.50000 H42F 2 0.505671 -0.062604 0.304757 10.50000 -1.50000 AFIX 0 C41A 1 0.546687 0.014553 0.259009 10.50000 0.07015 AFIX 23 H41C 2 0.549193 0.045249 0.295011 10.50000 -1.20000 H41D 2 0.534288 0.042834 0.223001 10.50000 -1.20000 AFIX 0 C44A 1 0.692288 0.089965 0.228811 10.50000 0.12545 AFIX 33 H44D 2 0.722989 0.121611 0.250989 10.50000 -1.50000 H44E 2 0.719037 0.066660 0.196723 10.50000 -1.50000 H44F 2 0.653745 0.115726 0.210238 10.50000 -1.50000 AFIX 0 C43A 1 0.664856 0.040486 0.270135 10.50000 0.08844 AFIX 23 H43C 2 0.640593 0.066218 0.302896 10.50000 -1.20000 H43D 2 0.705386 0.017527 0.289484 10.50000 -1.20000 PART 0 AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM wl307 in Pbca REM R1 = 0.0552 for 5432 Fo > 4sig(Fo) and 0.1197 for all 9380 data REM 450 parameters refined using 0 restraints END WGHT 0.0537 4.7241 REM Instructions for potential hydrogen bonds HTAB C31 N4 EQIV $1 -x+3/2, y+1/2, z HTAB C32 O1_$1 HTAB C32 O1A_$1 REM Highest difference peak 0.726, deepest hole -0.607, 1-sigma level 0.063 Q1 1 0.5388 -0.0148 0.2193 11.00000 0.05 0.70 Q2 1 0.7407 0.0193 0.2612 11.00000 0.05 0.59 Q3 1 0.6339 0.0246 0.2861 11.00000 0.05 0.40 Q4 1 0.6901 0.0571 0.2620 11.00000 0.05 0.35 Q5 1 0.4989 -0.0111 0.2722 11.00000 0.05 0.32 Q6 1 0.7736 0.2410 0.4221 11.00000 0.05 0.30 Q7 1 0.7793 0.0471 0.5271 11.00000 0.05 0.30 Q8 1 0.8019 0.2048 0.4495 11.00000 0.05 0.29 Q9 1 0.7679 0.2411 0.4603 11.00000 0.05 0.26 Q10 1 0.6799 0.0057 0.2679 11.00000 0.05 0.24 ; _shelx_res_checksum 23954 loop_ _space_group_symop_operation_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' 'x-1/2, y, -z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.73298(2) 0.20426(2) 0.44735(2) 0.02412(11) Uani 1 1 d . . . . . C1 C 0.61636(13) 0.12263(13) 0.43807(11) 0.0209(6) Uani 1 1 d . . . . . N1 N 0.63306(11) 0.19213(10) 0.43891(10) 0.0230(5) Uani 1 1 d . . . . . N2 N 0.73783(11) 0.10624(10) 0.46233(10) 0.0244(5) Uani 1 1 d . . . . . C2 C 0.55043(14) 0.09548(14) 0.42727(13) 0.0284(6) Uani 1 1 d . . . . . H2 H 0.512793 0.125576 0.418064 0.034 Uiso 1 1 calc R U . . . N3 N 0.79137(12) 0.24885(12) 0.37554(12) 0.0322(6) Uani 1 1 d . . . . . C3 C 0.53818(14) 0.02487(14) 0.42964(14) 0.0327(7) Uani 1 1 d . . . . . H3 H 0.492392 0.007467 0.423077 0.039 Uiso 1 1 calc R U . . . N4 N 0.77250(11) 0.27035(11) 0.51296(11) 0.0276(5) Uani 1 1 d . . . . . C4 C 0.59216(15) -0.01916(14) 0.44141(14) 0.0351(7) Uani 1 1 d . . . . . H4 H 0.583984 -0.067224 0.442541 0.042 Uiso 1 1 calc R U . . . C5 C 0.65916(14) 0.00640(13) 0.45174(13) 0.0298(6) Uani 1 1 d . . . . . H5 H 0.696379 -0.024675 0.459523 0.036 Uiso 1 1 calc R U . . . C6 C 0.67260(13) 0.07643(12) 0.45089(12) 0.0219(6) Uani 1 1 d . . . . . C7 C 0.57894(13) 0.24191(13) 0.43480(13) 0.0239(6) Uani 1 1 d . . . . . C8 C 0.55100(13) 0.27093(13) 0.48875(13) 0.0263(6) Uani 1 1 d . . . . . C9 C 0.50332(14) 0.32461(14) 0.48344(15) 0.0326(7) Uani 1 1 d . . . . . H9 H 0.485171 0.345245 0.519457 0.039 Uiso 1 1 calc R U . . . C10 C 0.48184(15) 0.34851(14) 0.42716(16) 0.0364(8) Uani 1 1 d . . . . . H10 H 0.449535 0.385427 0.424540 0.044 Uiso 1 1 calc R U . . . C11 C 0.50749(14) 0.31855(14) 0.37483(15) 0.0341(7) Uani 1 1 d . . . . . H11 H 0.491900 0.334691 0.336177 0.041 Uiso 1 1 calc R U . . . C12 C 0.55592(13) 0.26493(13) 0.37715(13) 0.0269(6) Uani 1 1 d . . . . . C13 C 0.57026(15) 0.24302(15) 0.55085(14) 0.0358(7) Uani 1 1 d . . . . . H13 H 0.616966 0.220406 0.546776 0.043 Uiso 1 1 calc R U . . . C14 C 0.57689(19) 0.29759(18) 0.60048(16) 0.0528(9) Uani 1 1 d . . . . . H14A H 0.606109 0.335334 0.585521 0.079 Uiso 1 1 calc R U . . . H14B H 0.598441 0.277378 0.636924 0.079 Uiso 1 1 calc R U . . . H14C H 0.530364 0.315143 0.610887 0.079 Uiso 1 1 calc R U . . . C15 C 0.5184(2) 0.18801(18) 0.57081(17) 0.0587(10) Uani 1 1 d . . . . . H15A H 0.471152 0.207483 0.571705 0.088 Uiso 1 1 calc R U . . . H15B H 0.530873 0.171518 0.611705 0.088 Uiso 1 1 calc R U . . . H15C H 0.519785 0.149680 0.541831 0.088 Uiso 1 1 calc R U . . . C16 C 0.58314(15) 0.23401(15) 0.31852(13) 0.0331(7) Uani 1 1 d . . . . . H16 H 0.613523 0.194220 0.329801 0.040 Uiso 1 1 calc R U . . . C17 C 0.62807(18) 0.28458(17) 0.28262(16) 0.0499(9) Uani 1 1 d . . . . . H17A H 0.648845 0.261202 0.247342 0.075 Uiso 1 1 calc R U . . . H17B H 0.665313 0.302280 0.309047 0.075 Uiso 1 1 calc R U . . . H17C H 0.598934 0.322731 0.268388 0.075 Uiso 1 1 calc R U . . . C18 C 0.52362(18) 0.20647(18) 0.27863(16) 0.0499(9) Uani 1 1 d . . . . . H18A H 0.493901 0.244641 0.265381 0.075 Uiso 1 1 calc R U . . . H18B H 0.495639 0.173748 0.302272 0.075 Uiso 1 1 calc R U . . . H18C H 0.543225 0.183391 0.242694 0.075 Uiso 1 1 calc R U . . . C31 C 0.81630(16) 0.31380(16) 0.37671(16) 0.0428(8) Uani 1 1 d . . . . . H31 H 0.811763 0.339222 0.413569 0.051 Uiso 1 1 calc R U . . . C30 C 0.8436(2) -0.04736(19) 0.3714(2) 0.0714(13) Uani 1 1 d . . . . . H30A H 0.843292 -0.045710 0.326612 0.107 Uiso 1 1 calc R U . . . H30B H 0.802536 -0.072710 0.385822 0.107 Uiso 1 1 calc R U . . . H30C H 0.886184 -0.070487 0.385439 0.107 Uiso 1 1 calc R U . . . C29 C 0.90373(18) 0.0684(2) 0.37343(19) 0.0637(11) Uani 1 1 d . . . . . H29A H 0.902086 0.070373 0.328676 0.096 Uiso 1 1 calc R U . . . H29B H 0.947537 0.046786 0.386411 0.096 Uiso 1 1 calc R U . . . H29C H 0.901223 0.115049 0.390070 0.096 Uiso 1 1 calc R U . . . C28 C 0.84173(16) 0.02632(16) 0.39710(16) 0.0444(9) Uani 1 1 d . . . . . H28 H 0.798134 0.048536 0.381422 0.053 Uiso 1 1 calc R U . . . C27 C 0.66893(18) 0.05784(19) 0.61521(17) 0.0566(10) Uani 1 1 d . . . . . H27A H 0.648113 0.035780 0.579283 0.085 Uiso 1 1 calc R U . . . H27B H 0.633146 0.084622 0.636634 0.085 Uiso 1 1 calc R U . . . H27C H 0.687586 0.022641 0.642737 0.085 Uiso 1 1 calc R U . . . C26 C 0.7557(2) 0.1453(2) 0.64955(17) 0.0662(11) Uani 1 1 d . . . . . H26A H 0.795825 0.173142 0.636884 0.099 Uiso 1 1 calc R U . . . H26B H 0.770245 0.113174 0.681588 0.099 Uiso 1 1 calc R U . . . H26C H 0.718786 0.175320 0.665388 0.099 Uiso 1 1 calc R U . . . C25 C 0.72807(18) 0.10533(15) 0.59488(14) 0.0424(8) Uani 1 1 d . . . . . H25 H 0.707476 0.139419 0.565831 0.051 Uiso 1 1 calc R U . . . C24 C 0.83819(14) 0.02761(14) 0.46556(15) 0.0345(7) Uani 1 1 d . . . . . C23 C 0.88669(15) -0.00932(15) 0.50080(19) 0.0467(9) Uani 1 1 d . . . . . H23 H 0.921695 -0.035586 0.480759 0.056 Uiso 1 1 calc R U . . . C22 C 0.88469(16) -0.00834(16) 0.56321(19) 0.0508(10) Uani 1 1 d . . . . . H22 H 0.918158 -0.033580 0.586111 0.061 Uiso 1 1 calc R U . . . C21 C 0.83410(16) 0.02929(15) 0.59289(16) 0.0425(8) Uani 1 1 d . . . . . H21 H 0.833194 0.029766 0.636323 0.051 Uiso 1 1 calc R U . . . C20 C 0.78422(14) 0.06667(14) 0.56059(14) 0.0326(7) Uani 1 1 d . . . . . C19 C 0.78695(13) 0.06651(13) 0.49626(14) 0.0281(7) Uani 1 1 d . . . . . C32 C 0.84760(18) 0.3449(2) 0.32791(18) 0.0561(10) Uani 1 1 d . . . . . H32 H 0.863174 0.391078 0.330450 0.067 Uiso 1 1 calc R U . . . C33 C 0.85593(18) 0.3082(2) 0.27572(18) 0.0572(10) Uani 1 1 d . . . . . H33 H 0.878230 0.328401 0.241335 0.069 Uiso 1 1 calc R U . . . C34 C 0.8324(2) 0.2426(2) 0.27264(18) 0.0639(11) Uani 1 1 d . . . . . H34 H 0.837977 0.216423 0.236296 0.077 Uiso 1 1 calc R U . . . C35 C 0.79995(18) 0.21430(19) 0.32367(17) 0.0523(9) Uani 1 1 d . . . . . H35 H 0.783240 0.168470 0.321377 0.063 Uiso 1 1 calc R U . . . C36 C 0.74416(15) 0.33144(14) 0.52674(14) 0.0327(7) Uani 1 1 d . . . . . H36 H 0.698940 0.341983 0.511421 0.039 Uiso 1 1 calc R U . . . C37 C 0.77805(16) 0.37939(15) 0.56217(15) 0.0432(8) Uani 1 1 d . . . . . H37 H 0.756672 0.422331 0.570715 0.052 Uiso 1 1 calc R U . . . C38 C 0.84312(17) 0.36438(16) 0.58502(17) 0.0452(8) Uani 1 1 d . . . . . H38 H 0.867438 0.396794 0.609517 0.054 Uiso 1 1 calc R U . . . C39 C 0.87274(16) 0.30138(15) 0.57185(15) 0.0416(8) Uani 1 1 d . . . . . H39 H 0.917625 0.289535 0.587188 0.050 Uiso 1 1 calc R U . . . C40 C 0.83580(14) 0.25650(14) 0.53618(14) 0.0340(7) Uani 1 1 d . . . . . H40 H 0.856151 0.213143 0.527384 0.041 Uiso 1 1 calc R U . . . O1 O 0.6307(4) -0.0087(5) 0.2516(4) 0.0667(11) Uiso 0.5 1 d . . P A 1 C42 C 0.5111(5) -0.0307(5) 0.2479(5) 0.0725(19) Uiso 0.5 1 d . . P A 1 H42A H 0.466072 -0.008330 0.255606 0.109 Uiso 0.5 1 calc R U P A 1 H42B H 0.513528 -0.045157 0.205053 0.109 Uiso 0.5 1 calc R U P A 1 H42C H 0.515690 -0.070956 0.274500 0.109 Uiso 0.5 1 calc R U P A 1 C41 C 0.5729(5) 0.0218(6) 0.2619(5) 0.0701(18) Uiso 0.5 1 d . . P A 1 H41A H 0.568647 0.062737 0.235437 0.084 Uiso 0.5 1 calc R U P A 1 H41B H 0.570818 0.036844 0.305137 0.084 Uiso 0.5 1 calc R U P A 1 C44 C 0.7280(7) 0.0535(7) 0.2441(6) 0.125(3) Uiso 0.5 1 d . . P A 1 H44A H 0.772762 0.062915 0.264315 0.188 Uiso 0.5 1 calc R U P A 1 H44B H 0.736668 0.035791 0.202879 0.188 Uiso 0.5 1 calc R U P A 1 H44C H 0.700680 0.095888 0.241558 0.188 Uiso 0.5 1 calc R U P A 1 C43 C 0.6990(6) 0.0153(6) 0.2706(5) 0.088(2) Uiso 0.5 1 d . . P A 1 H43A H 0.693627 0.033991 0.312413 0.106 Uiso 0.5 1 calc R U P A 1 H43B H 0.729348 -0.025661 0.274020 0.106 Uiso 0.5 1 calc R U P A 1 O1A O 0.6145(4) -0.0167(5) 0.2491(4) 0.0667(11) Uiso 0.5 1 d . . P B 2 C42A C 0.4940(5) -0.0351(5) 0.2687(5) 0.0725(19) Uiso 0.5 1 d . . P B 2 H42D H 0.449086 -0.012038 0.275167 0.109 Uiso 0.5 1 calc R U P B 2 H42E H 0.490773 -0.065018 0.232779 0.109 Uiso 0.5 1 calc R U P B 2 H42F H 0.505671 -0.062604 0.304757 0.109 Uiso 0.5 1 calc R U P B 2 C41A C 0.5467(5) 0.0146(6) 0.2590(5) 0.0701(18) Uiso 0.5 1 d . . P B 2 H41C H 0.549193 0.045249 0.295011 0.084 Uiso 0.5 1 calc R U P B 2 H41D H 0.534288 0.042834 0.223001 0.084 Uiso 0.5 1 calc R U P B 2 C44A C 0.6923(7) 0.0900(7) 0.2288(6) 0.125(3) Uiso 0.5 1 d . . P B 2 H44D H 0.722989 0.121611 0.250989 0.188 Uiso 0.5 1 calc R U P B 2 H44E H 0.719037 0.066660 0.196723 0.188 Uiso 0.5 1 calc R U P B 2 H44F H 0.653745 0.115726 0.210238 0.188 Uiso 0.5 1 calc R U P B 2 C43A C 0.6649(6) 0.0405(6) 0.2701(5) 0.088(2) Uiso 0.5 1 d . . P B 2 H43C H 0.640593 0.066218 0.302896 0.106 Uiso 0.5 1 calc R U P B 2 H43D H 0.705386 0.017527 0.289484 0.106 Uiso 0.5 1 calc R U P B 2 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 0.01883(19) 0.01804(18) 0.0355(2) 0.00092(17) 0.00016(17) 0.00040(16) C1 0.0220(13) 0.0209(13) 0.0200(15) -0.0006(11) 0.0018(11) 0.0005(10) N1 0.0197(11) 0.0184(11) 0.0308(13) 0.0011(9) 0.0026(9) 0.0025(9) N2 0.0195(11) 0.0162(10) 0.0376(14) 0.0004(9) -0.0010(10) 0.0014(9) C2 0.0217(14) 0.0252(14) 0.0384(18) -0.0021(12) -0.0017(12) 0.0004(11) N3 0.0241(12) 0.0346(14) 0.0378(15) 0.0039(12) -0.0009(11) -0.0010(11) C3 0.0247(15) 0.0298(15) 0.0436(19) -0.0032(13) -0.0033(13) -0.0095(13) N4 0.0227(12) 0.0199(11) 0.0404(14) -0.0005(10) -0.0018(10) 0.0016(10) C4 0.0358(16) 0.0217(14) 0.048(2) -0.0048(14) 0.0013(14) -0.0053(12) C5 0.0259(14) 0.0187(13) 0.0447(18) -0.0028(13) 0.0025(13) 0.0019(11) C6 0.0227(13) 0.0194(13) 0.0236(14) -0.0039(11) 0.0025(11) 0.0007(10) C7 0.0165(12) 0.0166(13) 0.0386(18) 0.0016(11) 0.0008(11) -0.0018(10) C8 0.0195(13) 0.0210(13) 0.0382(18) -0.0030(12) 0.0050(12) -0.0025(11) C9 0.0248(15) 0.0231(14) 0.050(2) -0.0092(14) 0.0091(14) -0.0006(12) C10 0.0235(15) 0.0192(14) 0.067(2) 0.0004(14) 0.0011(15) 0.0019(12) C11 0.0269(16) 0.0263(15) 0.049(2) 0.0075(14) -0.0060(14) 0.0010(12) C12 0.0200(13) 0.0227(14) 0.0380(18) 0.0027(13) -0.0029(12) -0.0014(11) C13 0.0347(16) 0.0360(17) 0.0368(18) -0.0025(15) 0.0080(14) 0.0048(13) C14 0.063(2) 0.056(2) 0.039(2) -0.0047(18) 0.0047(17) -0.0100(19) C15 0.081(3) 0.049(2) 0.046(2) 0.0089(17) 0.0079(19) -0.019(2) C16 0.0346(16) 0.0334(16) 0.0312(17) 0.0049(13) -0.0044(13) 0.0053(13) C17 0.051(2) 0.057(2) 0.042(2) 0.0059(17) 0.0064(17) -0.0039(17) C18 0.051(2) 0.058(2) 0.041(2) -0.0054(18) -0.0087(16) -0.0002(18) C31 0.045(2) 0.0354(18) 0.048(2) 0.0072(15) 0.0028(16) -0.0108(15) C30 0.061(2) 0.057(2) 0.097(3) -0.041(2) 0.004(2) 0.011(2) C29 0.042(2) 0.080(3) 0.070(3) -0.012(2) 0.0073(19) -0.004(2) C28 0.0285(16) 0.0388(18) 0.066(2) -0.0191(17) 0.0010(15) 0.0074(14) C27 0.048(2) 0.062(2) 0.059(3) -0.006(2) 0.0098(18) -0.0020(19) C26 0.099(3) 0.054(2) 0.046(2) -0.0070(18) 0.012(2) -0.023(2) C25 0.060(2) 0.0322(17) 0.0351(18) 0.0039(14) 0.0032(16) 0.0031(16) C24 0.0235(14) 0.0199(14) 0.060(2) -0.0083(14) -0.0044(14) 0.0014(12) C23 0.0277(17) 0.0221(16) 0.090(3) -0.0009(17) -0.0085(17) 0.0062(13) C22 0.0313(18) 0.0280(17) 0.093(3) 0.0207(19) -0.0227(19) -0.0045(14) C21 0.0420(19) 0.0289(16) 0.057(2) 0.0186(16) -0.0153(16) -0.0152(15) C20 0.0324(16) 0.0181(13) 0.047(2) 0.0038(13) -0.0053(13) -0.0058(11) C19 0.0222(14) 0.0153(13) 0.047(2) 0.0010(12) -0.0056(12) -0.0029(11) C32 0.052(2) 0.054(2) 0.062(3) 0.015(2) 0.0066(19) -0.0104(18) C33 0.042(2) 0.075(3) 0.055(3) 0.022(2) 0.0101(17) -0.0051(19) C34 0.068(3) 0.075(3) 0.049(3) -0.005(2) 0.015(2) 0.000(2) C35 0.052(2) 0.053(2) 0.052(2) -0.0046(19) 0.0084(18) -0.0075(18) C36 0.0291(16) 0.0245(15) 0.0445(18) -0.0008(13) -0.0026(13) 0.0035(12) C37 0.0420(19) 0.0249(15) 0.063(2) -0.0078(15) -0.0007(16) 0.0033(14) C38 0.0426(19) 0.0306(17) 0.062(2) -0.0098(16) -0.0114(17) -0.0053(15) C39 0.0293(16) 0.0323(17) 0.063(2) -0.0020(16) -0.0132(15) 0.0003(14) C40 0.0252(15) 0.0224(14) 0.054(2) -0.0013(14) -0.0041(14) 0.0018(12) 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' Fe Fe 0.3463 0.8444 '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 N1 Fe1 N2 86.73(9) . . ? N1 Fe1 N4 120.17(9) . . ? N2 Fe1 N4 118.55(9) . . ? N1 Fe1 N3 120.08(9) . . ? N2 Fe1 N3 120.33(9) . . ? N4 Fe1 N3 93.79(9) . . ? C2 C1 N1 125.6(2) . . ? C2 C1 C6 118.5(2) . . ? N1 C1 C6 115.9(2) . . ? C1 N1 C7 119.8(2) . . ? C1 N1 Fe1 110.29(15) . . ? C7 N1 Fe1 129.94(16) . . ? C6 N2 C19 117.1(2) . . ? C6 N2 Fe1 109.64(16) . . ? C19 N2 Fe1 130.84(16) . . ? C1 C2 C3 121.4(3) . . ? C1 C2 H2 119.3 . . ? C3 C2 H2 119.3 . . ? C35 N3 C31 116.5(3) . . ? C35 N3 Fe1 119.4(2) . . ? C31 N3 Fe1 123.8(2) . . ? C4 C3 C2 119.9(3) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C40 N4 C36 117.3(2) . . ? C40 N4 Fe1 117.83(18) . . ? C36 N4 Fe1 124.04(19) . . ? C3 C4 C5 120.0(3) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C6 C5 C4 121.3(3) . . ? C6 C5 H5 119.4 . . ? C4 C5 H5 119.4 . . ? C5 C6 N2 124.8(2) . . ? C5 C6 C1 118.8(2) . . ? N2 C6 C1 116.4(2) . . ? C12 C7 C8 120.1(2) . . ? C12 C7 N1 120.1(2) . . ? C8 C7 N1 119.7(2) . . ? C9 C8 C7 118.6(3) . . ? C9 C8 C13 120.4(3) . . ? C7 C8 C13 121.0(2) . . ? C10 C9 C8 121.6(3) . . ? C10 C9 H9 119.2 . . ? C8 C9 H9 119.2 . . ? C11 C10 C9 119.5(3) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? C10 C11 C12 121.6(3) . . ? C10 C11 H11 119.2 . . ? C12 C11 H11 119.2 . . ? C11 C12 C7 118.5(3) . . ? C11 C12 C16 119.8(3) . . ? C7 C12 C16 121.7(2) . . ? C8 C13 C15 110.6(3) . . ? C8 C13 C14 114.2(3) . . ? C15 C13 C14 109.9(3) . . ? C8 C13 H13 107.3 . . ? C15 C13 H13 107.3 . . ? C14 C13 H13 107.3 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C12 C16 C17 111.9(2) . . ? C12 C16 C18 111.6(2) . . ? C17 C16 C18 110.6(3) . . ? C12 C16 H16 107.5 . . ? C17 C16 H16 107.5 . . ? C18 C16 H16 107.5 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N3 C31 C32 123.7(3) . . ? N3 C31 H31 118.2 . . ? C32 C31 H31 118.2 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C24 C28 C29 111.3(3) . . ? C24 C28 C30 112.4(3) . . ? C29 C28 C30 110.9(3) . . ? C24 C28 H28 107.3 . . ? C29 C28 H28 107.3 . . ? C30 C28 H28 107.3 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C26 H26A 109.5 . . ? 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 . . ? C20 C25 C26 113.5(3) . . ? C20 C25 C27 111.6(3) . . ? C26 C25 C27 109.8(3) . . ? C20 C25 H25 107.2 . . ? C26 C25 H25 107.2 . . ? C27 C25 H25 107.2 . . ? C23 C24 C19 118.3(3) . . ? C23 C24 C28 120.6(3) . . ? C19 C24 C28 121.1(3) . . ? C22 C23 C24 121.5(3) . . ? C22 C23 H23 119.2 . . ? C24 C23 H23 119.2 . . ? C23 C22 C21 119.9(3) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C22 C21 C20 121.4(3) . . ? C22 C21 H21 119.3 . . ? C20 C21 H21 119.3 . . ? C21 C20 C19 118.7(3) . . ? C21 C20 C25 119.7(3) . . ? C19 C20 C25 121.6(3) . . ? C20 C19 C24 120.2(3) . . ? C20 C19 N2 119.6(2) . . ? C24 C19 N2 120.2(3) . . ? C33 C32 C31 118.4(4) . . ? C33 C32 H32 120.8 . . ? C31 C32 H32 120.8 . . ? C32 C33 C34 120.0(3) . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C33 C34 C35 118.8(4) . . ? C33 C34 H34 120.6 . . ? C35 C34 H34 120.6 . . ? N3 C35 C34 122.6(4) . . ? N3 C35 H35 118.7 . . ? C34 C35 H35 118.7 . . ? N4 C36 C37 122.6(3) . . ? N4 C36 H36 118.7 . . ? C37 C36 H36 118.7 . . ? C38 C37 C36 119.2(3) . . ? C38 C37 H37 120.4 . . ? C36 C37 H37 120.4 . . ? C37 C38 C39 119.0(3) . . ? C37 C38 H38 120.5 . . ? C39 C38 H38 120.5 . . ? C40 C39 C38 118.3(3) . . ? C40 C39 H39 120.8 . . ? C38 C39 H39 120.8 . . ? N4 C40 C39 123.6(3) . . ? N4 C40 H40 118.2 . . ? C39 C40 H40 118.2 . . ? C41 O1 C43 125.5(10) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O1 C41 C42 108.0(10) . . ? O1 C41 H41A 110.1 . . ? C42 C41 H41A 110.1 . . ? O1 C41 H41B 110.1 . . ? C42 C41 H41B 110.1 . . ? H41A C41 H41B 108.4 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C44 C43 O1 121.7(13) . . ? C44 C43 H43A 106.9 . . ? O1 C43 H43A 106.9 . . ? C44 C43 H43B 106.9 . . ? O1 C43 H43B 106.9 . . ? H43A C43 H43B 106.7 . . ? C41A O1A C43A 102.1(9) . . ? C41A C42A H42D 109.5 . . ? C41A C42A H42E 109.5 . . ? H42D C42A H42E 109.5 . . ? C41A C42A H42F 109.5 . . ? H42D C42A H42F 109.5 . . ? H42E C42A H42F 109.5 . . ? C42A C41A O1A 111.9(10) . . ? C42A C41A H41C 109.2 . . ? O1A C41A H41C 109.2 . . ? C42A C41A H41D 109.2 . . ? O1A C41A H41D 109.2 . . ? H41C C41A H41D 107.9 . . ? C43A C44A H44D 109.5 . . ? C43A C44A H44E 109.5 . . ? H44D C44A H44E 109.5 . . ? C43A C44A H44F 109.5 . . ? H44D C44A H44F 109.5 . . ? H44E C44A H44F 109.5 . . ? C44A C43A O1A 122.1(10) . . ? C44A C43A H43C 106.8 . . ? O1A C43A H43C 106.8 . . ? C44A C43A H43D 106.8 . . ? O1A C43A H43D 106.8 . . ? H43C C43A H43D 106.7 . . ? 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 N1 1.934(2) . ? Fe1 N2 1.941(2) . ? Fe1 N4 2.071(2) . ? Fe1 N3 2.114(2) . ? C1 C2 1.388(3) . ? C1 N1 1.392(3) . ? C1 C6 1.430(3) . ? N1 C7 1.421(3) . ? N2 C6 1.399(3) . ? N2 C19 1.426(3) . ? C2 C3 1.397(4) . ? C2 H2 0.9500 . ? N3 C35 1.329(4) . ? N3 C31 1.353(4) . ? C3 C4 1.367(4) . ? C3 H3 0.9500 . ? N4 C40 1.340(3) . ? N4 C36 1.342(3) . ? C4 C5 1.393(4) . ? C4 H4 0.9500 . ? C5 C6 1.389(3) . ? C5 H5 0.9500 . ? C7 C12 1.409(4) . ? C7 C8 1.413(4) . ? C8 C9 1.393(4) . ? C8 C13 1.509(4) . ? C9 C10 1.379(4) . ? C9 H9 0.9500 . ? C10 C11 1.375(4) . ? C10 H10 0.9500 . ? C11 C12 1.397(4) . ? C11 H11 0.9500 . ? C12 C16 1.509(4) . ? C13 C15 1.525(4) . ? C13 C14 1.525(4) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.525(4) . ? C16 C18 1.531(4) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C31 C32 1.365(4) . ? C31 H31 0.9500 . ? C30 C28 1.543(4) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C29 C28 1.532(5) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C28 C24 1.499(5) . ? C28 H28 1.0000 . ? C27 C25 1.528(4) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C26 C25 1.522(5) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C25 C20 1.511(4) . ? C25 H25 1.0000 . ? C24 C23 1.404(4) . ? C24 C19 1.409(4) . ? C23 C22 1.365(5) . ? C23 H23 0.9500 . ? C22 C21 1.377(5) . ? C22 H22 0.9500 . ? C21 C20 1.393(4) . ? C21 H21 0.9500 . ? C20 C19 1.408(4) . ? C32 C33 1.356(5) . ? C32 H32 0.9500 . ? C33 C34 1.358(5) . ? C33 H33 0.9500 . ? C34 C35 1.391(5) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 C37 1.376(4) . ? C36 H36 0.9500 . ? C37 C38 1.373(4) . ? C37 H37 0.9500 . ? C38 C39 1.383(4) . ? C38 H38 0.9500 . ? C39 C40 1.368(4) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? O1 C41 1.274(14) . ? O1 C43 1.449(13) . ? C42 C41 1.593(14) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C44 C43 1.094(14) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? O1A C41A 1.450(13) . ? O1A C43A 1.543(15) . ? C42A C41A 1.412(14) . ? C42A H42D 0.9800 . ? C42A H42E 0.9800 . ? C42A H42F 0.9800 . ? C41A H41C 0.9900 . ? C41A H41D 0.9900 . ? C44A C43A 1.422(15) . ? C44A H44D 0.9800 . ? C44A H44E 0.9800 . ? C44A H44F 0.9800 . ? C43A H43C 0.9900 . ? C43A H43D 0.9900 . ? 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 C2 C1 N1 C7 6.9(4) . . . . ? C6 C1 N1 C7 -171.6(2) . . . . ? C2 C1 N1 Fe1 -174.0(2) . . . . ? C6 C1 N1 Fe1 7.4(3) . . . . ? N1 C1 C2 C3 -177.5(3) . . . . ? C6 C1 C2 C3 1.0(4) . . . . ? C1 C2 C3 C4 -1.5(4) . . . . ? C2 C3 C4 C5 0.8(5) . . . . ? C3 C4 C5 C6 0.5(5) . . . . ? C4 C5 C6 N2 178.3(3) . . . . ? C4 C5 C6 C1 -1.1(4) . . . . ? C19 N2 C6 C5 -21.9(4) . . . . ? Fe1 N2 C6 C5 173.9(2) . . . . ? C19 N2 C6 C1 157.5(2) . . . . ? Fe1 N2 C6 C1 -6.7(3) . . . . ? C2 C1 C6 C5 0.3(4) . . . . ? N1 C1 C6 C5 179.0(2) . . . . ? C2 C1 C6 N2 -179.1(2) . . . . ? N1 C1 C6 N2 -0.4(3) . . . . ? C1 N1 C7 C12 -88.3(3) . . . . ? Fe1 N1 C7 C12 92.9(3) . . . . ? C1 N1 C7 C8 95.2(3) . . . . ? Fe1 N1 C7 C8 -83.7(3) . . . . ? C12 C7 C8 C9 -3.2(4) . . . . ? N1 C7 C8 C9 173.4(2) . . . . ? C12 C7 C8 C13 174.8(2) . . . . ? N1 C7 C8 C13 -8.7(4) . . . . ? C7 C8 C9 C10 1.6(4) . . . . ? C13 C8 C9 C10 -176.3(3) . . . . ? C8 C9 C10 C11 0.5(4) . . . . ? C9 C10 C11 C12 -1.1(4) . . . . ? C10 C11 C12 C7 -0.5(4) . . . . ? C10 C11 C12 C16 -179.5(3) . . . . ? C8 C7 C12 C11 2.6(4) . . . . ? N1 C7 C12 C11 -173.9(2) . . . . ? C8 C7 C12 C16 -178.4(2) . . . . ? N1 C7 C12 C16 5.0(4) . . . . ? C9 C8 C13 C15 86.3(3) . . . . ? C7 C8 C13 C15 -91.6(3) . . . . ? C9 C8 C13 C14 -38.3(4) . . . . ? C7 C8 C13 C14 143.8(3) . . . . ? C11 C12 C16 C17 67.1(3) . . . . ? C7 C12 C16 C17 -111.9(3) . . . . ? C11 C12 C16 C18 -57.5(3) . . . . ? C7 C12 C16 C18 123.6(3) . . . . ? C35 N3 C31 C32 1.4(5) . . . . ? Fe1 N3 C31 C32 -172.9(3) . . . . ? C29 C28 C24 C23 -72.8(4) . . . . ? C30 C28 C24 C23 52.3(4) . . . . ? C29 C28 C24 C19 106.3(3) . . . . ? C30 C28 C24 C19 -128.6(3) . . . . ? C19 C24 C23 C22 0.3(4) . . . . ? C28 C24 C23 C22 179.4(3) . . . . ? C24 C23 C22 C21 0.2(5) . . . . ? C23 C22 C21 C20 0.2(4) . . . . ? C22 C21 C20 C19 -1.1(4) . . . . ? C22 C21 C20 C25 177.9(3) . . . . ? C26 C25 C20 C21 44.7(4) . . . . ? C27 C25 C20 C21 -80.0(4) . . . . ? C26 C25 C20 C19 -136.3(3) . . . . ? C27 C25 C20 C19 99.0(3) . . . . ? C21 C20 C19 C24 1.7(4) . . . . ? C25 C20 C19 C24 -177.3(3) . . . . ? C21 C20 C19 N2 -177.9(2) . . . . ? C25 C20 C19 N2 3.0(4) . . . . ? C23 C24 C19 C20 -1.3(4) . . . . ? C28 C24 C19 C20 179.6(3) . . . . ? C23 C24 C19 N2 178.3(2) . . . . ? C28 C24 C19 N2 -0.8(4) . . . . ? C6 N2 C19 C20 -84.2(3) . . . . ? Fe1 N2 C19 C20 76.0(3) . . . . ? C6 N2 C19 C24 96.2(3) . . . . ? Fe1 N2 C19 C24 -103.6(3) . . . . ? N3 C31 C32 C33 -1.8(5) . . . . ? C31 C32 C33 C34 1.0(6) . . . . ? C32 C33 C34 C35 0.0(6) . . . . ? C31 N3 C35 C34 -0.3(5) . . . . ? Fe1 N3 C35 C34 174.3(3) . . . . ? C33 C34 C35 N3 -0.4(6) . . . . ? C40 N4 C36 C37 1.2(4) . . . . ? Fe1 N4 C36 C37 -168.0(2) . . . . ? N4 C36 C37 C38 -0.6(5) . . . . ? C36 C37 C38 C39 -0.1(5) . . . . ? C37 C38 C39 C40 0.3(5) . . . . ? C36 N4 C40 C39 -1.1(5) . . . . ? Fe1 N4 C40 C39 168.8(3) . . . . ? C38 C39 C40 N4 0.4(5) . . . . ? C43 O1 C41 C42 -166.2(9) . . . . ? C41 O1 C43 C44 -82.7(18) . . . . ? C43A O1A C41A C42A -154.2(9) . . . . ? C41A O1A C43A C44A -92.0(12) . . . . ?