#------------------------------------------------------------------------------ #$Date: 2020-10-06 11:58:48 +0300 (Tue, 06 Oct 2020) $ #$Revision: 257555 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/51/7705188.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_7705188 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_issue 35 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 12287 _journal_page_last 12297 _journal_paper_doi 10.1039/d0dt02087g _journal_volume 49 _journal_year 2020 _chemical_formula_moiety 'C30 H38 Cl2 Fe N2, C16 H36 N' _chemical_formula_sum 'C46 H74 Cl2 Fe N3' _chemical_formula_weight 795.83 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _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 102.358(5) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 24.511(3) _cell_length_b 11.9033(11) _cell_length_c 32.937(3) _cell_measurement_reflns_used 78311 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 27.538 _cell_measurement_theta_min 2.391 _cell_volume 9387.1(17) _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 0.995 _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 0.1440 _diffrn_reflns_av_unetI/netI 0.1034 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_number 78310 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.538 _diffrn_reflns_theta_min 2.532 _exptl_absorpt_coefficient_mu 0.467 _exptl_absorpt_correction_T_max 0.7394 _exptl_absorpt_correction_T_min 0.6620 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour 'pale blue purple' _exptl_crystal_density_diffrn 1.126 _exptl_crystal_description plate _exptl_crystal_F_000 3448 _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.315 _refine_diff_density_min -0.365 _refine_diff_density_rms 0.069 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 481 _refine_ls_number_reflns 10788 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.001 _refine_ls_R_factor_all 0.1209 _refine_ls_R_factor_gt 0.0543 _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^)+(0.0274P)^2^+9.8425P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0864 _refine_ls_wR_factor_ref 0.1051 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6424 _reflns_number_total 10788 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02087g2.cif _cod_data_source_block wl308 _cod_depositor_comments 'Adding full bibliography for 7705182--7705191.cif.' _cod_original_cell_volume 9387.0(16) _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 7705188 _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 wl308_0m in C2/c wl308.res created by SHELXL-2016/6 at 12:44:44 on 03-Mar-2020 CELL 0.71073 24.5109 11.9033 32.9369 90.000 102.358 90.000 ZERR 8.00 0.0025 0.0011 0.0032 0.000 0.005 0.000 LATT 7 SYMM -x, y, -z+1/2 SFAC C CL FE N H UNIT 368 16 8 24 592 LIST 6 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP -123.000 ACTA L.S. 8 FMAP 2 OMIT 1 1 1 OMIT -2 0 2 OMIT 2 0 0 OMIT 1 1 0 OMIT -1 1 1 OMIT 0 0 2 OMIT 1 1 2 PLAN 5 0 0.00 HTAB BOND $H CONF WGHT 0.027400 9.842500 FVAR 0.05650 FE1 3 0.175672 0.609101 0.138552 11.00000 0.01694 0.01711 = 0.01836 -0.00185 0.00094 0.00009 CL1 2 0.184648 0.777792 0.170389 11.00000 0.04756 0.02103 = 0.02678 -0.00567 0.00710 0.00297 N1 4 0.207049 0.588100 0.087183 11.00000 0.01335 0.01885 = 0.01812 -0.00062 -0.00057 -0.00065 C1 1 0.169286 0.544919 0.055005 11.00000 0.01672 0.01218 = 0.01941 0.00093 -0.00130 0.00004 CL2 2 0.201094 0.471734 0.186583 11.00000 0.03231 0.01840 = 0.02652 0.00230 -0.00320 -0.00361 N2 4 0.104143 0.582472 0.097155 11.00000 0.01662 0.02043 = 0.01868 -0.00223 0.00205 0.00133 C2 1 0.180321 0.506845 0.016729 11.00000 0.01865 0.02080 = 0.01979 -0.00221 0.00331 0.00055 AFIX 43 H2 5 0.217356 0.509757 0.012330 11.00000 -1.20000 AFIX 0 N3 4 -0.166648 0.119383 0.297370 11.00000 0.02445 0.01472 = 0.01721 0.00082 0.00228 -0.00176 C3 1 0.138337 0.466050 -0.013875 11.00000 0.02501 0.02745 = 0.01990 -0.00418 0.00501 0.00252 AFIX 43 H3 5 0.146495 0.440950 -0.039305 11.00000 -1.20000 AFIX 0 C4 1 0.083098 0.460823 -0.008113 11.00000 0.02103 0.02969 = 0.02532 -0.00906 -0.00449 -0.00123 AFIX 43 H4 5 0.054440 0.430968 -0.029456 11.00000 -1.20000 AFIX 0 C5 1 0.070444 0.498440 0.028004 11.00000 0.01379 0.02726 = 0.02572 -0.00404 0.00114 0.00017 AFIX 43 H5 5 0.032890 0.495548 0.031274 11.00000 -1.20000 AFIX 0 C6 1 0.112391 0.541561 0.060545 11.00000 0.01435 0.01552 = 0.01896 -0.00084 -0.00045 0.00081 C7 1 0.263105 0.607092 0.082501 11.00000 0.01413 0.02594 = 0.01183 -0.00015 -0.00149 -0.00311 C8 1 0.279767 0.719103 0.077776 11.00000 0.02154 0.02597 = 0.01265 -0.00136 0.00084 -0.00409 C9 1 0.334650 0.738891 0.074587 11.00000 0.03211 0.02828 = 0.01857 -0.00037 0.00528 -0.00837 AFIX 43 H9 5 0.346393 0.813765 0.071276 11.00000 -1.20000 AFIX 0 C10 1 0.372500 0.651903 0.076134 11.00000 0.01674 0.04467 = 0.02579 -0.00062 0.00605 -0.00709 AFIX 43 H10 5 0.409768 0.667085 0.073832 11.00000 -1.20000 AFIX 0 C11 1 0.355723 0.542739 0.081051 11.00000 0.01723 0.03178 = 0.02610 -0.00285 0.00193 0.00337 AFIX 43 H11 5 0.381967 0.483370 0.082469 11.00000 -1.20000 AFIX 0 C12 1 0.301096 0.517985 0.083971 11.00000 0.01455 0.02597 = 0.01782 -0.00128 0.00064 0.00044 C13 1 0.238169 0.814805 0.075467 11.00000 0.03046 0.02207 = 0.02339 -0.00074 0.00988 -0.00017 AFIX 13 H13 5 0.211863 0.794146 0.093647 11.00000 -1.20000 AFIX 0 C14 1 0.265391 0.927191 0.091445 11.00000 0.05235 0.02451 = 0.03861 -0.00488 0.01329 -0.00216 AFIX 137 H14A 5 0.288545 0.953915 0.072578 11.00000 -1.50000 H14B 5 0.288757 0.916677 0.119299 11.00000 -1.50000 H14C 5 0.236231 0.982654 0.092649 11.00000 -1.50000 AFIX 0 C15 1 0.203476 0.828538 0.031311 11.00000 0.03471 0.02696 = 0.03129 0.00757 0.00340 0.00542 AFIX 137 H15A 5 0.228111 0.847937 0.012532 11.00000 -1.50000 H15B 5 0.175974 0.888540 0.030856 11.00000 -1.50000 H15C 5 0.184095 0.757943 0.022232 11.00000 -1.50000 AFIX 0 C16 1 0.285311 0.396391 0.090158 11.00000 0.02039 0.02374 = 0.03388 0.00104 0.00426 0.00431 AFIX 13 H16 5 0.244029 0.393402 0.088061 11.00000 -1.20000 AFIX 0 C17 1 0.313863 0.356264 0.133661 11.00000 0.03417 0.03035 = 0.03878 0.00910 0.01156 0.00707 AFIX 137 H17A 5 0.302770 0.278587 0.137569 11.00000 -1.50000 H17B 5 0.302621 0.404532 0.154547 11.00000 -1.50000 H17C 5 0.354483 0.359977 0.136726 11.00000 -1.50000 AFIX 0 C18 1 0.299245 0.318765 0.056606 11.00000 0.03700 0.02880 = 0.04314 -0.00755 0.00142 0.00386 AFIX 137 H18A 5 0.278911 0.343779 0.029179 11.00000 -1.50000 H18B 5 0.288234 0.241652 0.061528 11.00000 -1.50000 H18C 5 0.339492 0.321275 0.057675 11.00000 -1.50000 AFIX 0 C19 1 0.048637 0.612928 0.100593 11.00000 0.01367 0.02495 = 0.01510 -0.00491 0.00071 -0.00098 C20 1 0.026289 0.715768 0.082958 11.00000 0.02337 0.02122 = 0.01979 -0.00470 -0.00152 -0.00269 C21 1 -0.026085 0.747769 0.089005 11.00000 0.02271 0.02023 = 0.03370 -0.00306 0.00198 0.00704 AFIX 43 H21 5 -0.041646 0.816817 0.077511 11.00000 -1.20000 AFIX 0 C22 1 -0.056032 0.682720 0.111068 11.00000 0.02052 0.03500 = 0.03593 -0.00483 0.00757 0.00995 AFIX 43 H22 5 -0.091443 0.707017 0.115030 11.00000 -1.20000 AFIX 0 C23 1 -0.033874 0.581768 0.127334 11.00000 0.02036 0.03324 = 0.03064 0.00186 0.00846 0.00167 AFIX 43 H23 5 -0.054772 0.536160 0.142157 11.00000 -1.20000 AFIX 0 C24 1 0.018329 0.544913 0.122606 11.00000 0.01781 0.02582 = 0.02194 -0.00257 0.00294 0.00169 C25 1 0.057038 0.791100 0.058243 11.00000 0.02503 0.02414 = 0.03267 0.00526 0.00310 0.00079 AFIX 13 H25 5 0.094679 0.757223 0.059422 11.00000 -1.20000 AFIX 0 C26 1 0.066012 0.907865 0.076927 11.00000 0.07204 0.03335 = 0.04150 -0.00015 0.00755 -0.02189 AFIX 137 H26A 5 0.086799 0.953538 0.060629 11.00000 -1.50000 H26B 5 0.087290 0.902525 0.105660 11.00000 -1.50000 H26C 5 0.029745 0.942970 0.076563 11.00000 -1.50000 AFIX 0 C27 1 0.027409 0.798065 0.012642 11.00000 0.06972 0.04887 = 0.03018 0.00108 0.00915 -0.01626 AFIX 137 H27A 5 0.048919 0.846189 -0.002326 11.00000 -1.50000 H27B 5 -0.009983 0.829857 0.010487 11.00000 -1.50000 H27C 5 0.024241 0.722627 0.000445 11.00000 -1.50000 AFIX 0 C28 1 0.039364 0.430824 0.139482 11.00000 0.01843 0.02859 = 0.03287 0.00581 0.00622 0.00229 AFIX 13 H28 5 0.077961 0.420440 0.134653 11.00000 -1.20000 AFIX 0 C29 1 0.042201 0.422720 0.186218 11.00000 0.03591 0.04603 = 0.04008 0.01461 0.00572 0.00677 AFIX 137 H29A 5 0.005232 0.438100 0.191827 11.00000 -1.50000 H29B 5 0.069061 0.477865 0.200834 11.00000 -1.50000 H29C 5 0.054129 0.347002 0.195948 11.00000 -1.50000 AFIX 0 C30 1 0.002165 0.338190 0.115955 11.00000 0.03234 0.03023 = 0.04741 0.00269 0.00656 -0.00122 AFIX 137 H30A 5 0.002807 0.342263 0.086343 11.00000 -1.50000 H30B 5 -0.036211 0.348349 0.119518 11.00000 -1.50000 H30C 5 0.016093 0.264679 0.126948 11.00000 -1.50000 AFIX 0 C31 1 -0.159561 0.192241 0.260989 11.00000 0.02526 0.02363 = 0.02293 0.00711 0.00210 -0.00345 AFIX 23 H31A 5 -0.188800 0.251038 0.256757 11.00000 -1.20000 H31B 5 -0.122967 0.230632 0.268638 11.00000 -1.20000 AFIX 0 C32 1 -0.162536 0.132294 0.220160 11.00000 0.03012 0.04434 = 0.02245 -0.00265 0.00250 -0.01349 AFIX 23 H32A 5 -0.198062 0.090041 0.212682 11.00000 -1.20000 H32B 5 -0.131405 0.077851 0.223067 11.00000 -1.20000 AFIX 0 C33 1 -0.158996 0.215676 0.185852 11.00000 0.03809 0.06507 = 0.02338 0.00564 0.00420 -0.01031 AFIX 23 H33A 5 -0.163837 0.174362 0.159232 11.00000 -1.20000 H33B 5 -0.190362 0.269451 0.183280 11.00000 -1.20000 AFIX 0 C34 1 -0.104862 0.281351 0.192462 11.00000 0.05697 0.06153 = 0.03654 0.00437 0.01325 -0.02308 AFIX 137 H34A 5 -0.073313 0.229022 0.196192 11.00000 -1.50000 H34B 5 -0.101347 0.328505 0.217278 11.00000 -1.50000 H34C 5 -0.104910 0.329009 0.168192 11.00000 -1.50000 AFIX 0 C35 1 -0.225443 0.072712 0.290808 11.00000 0.02416 0.02063 = 0.02308 -0.00290 0.00236 -0.00585 AFIX 23 H35A 5 -0.228602 0.029770 0.315944 11.00000 -1.20000 H35B 5 -0.230838 0.018987 0.267342 11.00000 -1.20000 AFIX 0 C36 1 -0.272705 0.157879 0.281953 11.00000 0.02698 0.03204 = 0.02436 -0.00254 0.00213 0.00282 AFIX 23 H36A 5 -0.276090 0.188801 0.253619 11.00000 -1.20000 H36B 5 -0.264334 0.220748 0.301999 11.00000 -1.20000 AFIX 0 C37 1 -0.327455 0.102719 0.285494 11.00000 0.02935 0.05619 = 0.03210 -0.00462 0.00669 -0.00031 AFIX 23 H37A 5 -0.325607 0.081837 0.314852 11.00000 -1.20000 H37B 5 -0.332469 0.032864 0.268795 11.00000 -1.20000 AFIX 0 C38 1 -0.377685 0.178866 0.270713 11.00000 0.02471 0.08377 = 0.05297 -0.01120 0.00169 0.00960 AFIX 137 H38A 5 -0.381101 0.196075 0.241178 11.00000 -1.50000 H38B 5 -0.372668 0.248774 0.286799 11.00000 -1.50000 H38C 5 -0.411618 0.140764 0.274646 11.00000 -1.50000 AFIX 0 C39 1 -0.152915 0.194458 0.335589 11.00000 0.02971 0.01473 = 0.02123 -0.00128 0.00219 -0.00229 AFIX 23 H39A 5 -0.112719 0.213590 0.340632 11.00000 -1.20000 H39B 5 -0.174086 0.265384 0.329123 11.00000 -1.20000 AFIX 0 C40 1 -0.164935 0.147605 0.375654 11.00000 0.02859 0.01861 = 0.02300 0.00155 0.00482 0.00151 AFIX 23 H40A 5 -0.149827 0.070420 0.380235 11.00000 -1.20000 H40B 5 -0.205790 0.144208 0.373611 11.00000 -1.20000 AFIX 0 C41 1 -0.138188 0.222084 0.411902 11.00000 0.04067 0.03284 = 0.03007 -0.00678 0.01010 -0.00389 AFIX 23 H41A 5 -0.097218 0.221630 0.414377 11.00000 -1.20000 H41B 5 -0.151367 0.300136 0.405804 11.00000 -1.20000 AFIX 0 C42 1 -0.150712 0.186913 0.453212 11.00000 0.05048 0.03795 = 0.02596 -0.00336 0.00922 0.00009 AFIX 137 H42A 5 -0.191232 0.184978 0.450905 11.00000 -1.50000 H42B 5 -0.133919 0.240940 0.474729 11.00000 -1.50000 H42C 5 -0.135080 0.112091 0.460698 11.00000 -1.50000 AFIX 0 C43 1 -0.128127 0.018269 0.302336 11.00000 0.02553 0.01619 = 0.02686 -0.00078 0.00319 0.00219 AFIX 23 H43A 5 -0.139058 -0.028947 0.277161 11.00000 -1.20000 H43B 5 -0.134727 -0.026549 0.326146 11.00000 -1.20000 AFIX 0 C44 1 -0.065892 0.041312 0.309149 11.00000 0.02589 0.02667 = 0.03345 0.00003 -0.00027 -0.00007 AFIX 23 H44A 5 -0.058623 0.093612 0.287541 11.00000 -1.20000 H44B 5 -0.052574 0.077053 0.336626 11.00000 -1.20000 AFIX 0 C45 1 -0.034606 -0.067901 0.307146 11.00000 0.03104 0.03515 = 0.03803 0.00092 0.00509 0.00962 AFIX 23 H45A 5 -0.047869 -0.102553 0.279466 11.00000 -1.20000 H45B 5 -0.043056 -0.120498 0.328259 11.00000 -1.20000 AFIX 0 C46 1 0.028236 -0.050735 0.314664 11.00000 0.03307 0.06710 = 0.05810 -0.00171 0.00155 0.01295 AFIX 137 H46A 5 0.046440 -0.122661 0.311690 11.00000 -1.50000 H46B 5 0.041994 -0.021456 0.342803 11.00000 -1.50000 H46C 5 0.036772 0.002974 0.294344 11.00000 -1.50000 AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM wl308_0m in C2/c REM R1 = 0.0543 for 6424 Fo > 4sig(Fo) and 0.1209 for all 10788 data REM 481 parameters refined using 0 restraints END WGHT 0.0274 9.8425 REM Instructions for potential hydrogen bonds EQIV $1 x-1/2, y-1/2, z HTAB C32 Cl2_$1 HTAB C35 Cl2_$1 HTAB C36 Cl1_$1 EQIV $2 -x, y, -z+1/2 HTAB C39 Cl2_$2 EQIV $3 -x, y-1, -z+1/2 HTAB C43 Cl1_$3 REM Highest difference peak 0.315, deepest hole -0.365, 1-sigma level 0.069 Q1 1 0.2033 0.5761 0.1090 11.00000 0.05 0.31 Q2 1 -0.3273 0.1191 0.2214 11.00000 0.05 0.29 Q3 1 -0.1533 0.1661 0.2388 11.00000 0.05 0.29 Q4 1 0.1806 0.6055 0.1825 11.00000 0.05 0.27 Q5 1 -0.1274 0.0249 0.2281 11.00000 0.05 0.27 ; _shelx_res_checksum 88276 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.17567(2) 0.60910(3) 0.13855(2) 0.01790(10) Uani 1 1 d . . . . . Cl1 Cl 0.18465(3) 0.77779(6) 0.17039(2) 0.03192(18) Uani 1 1 d . . . . . N1 N 0.20705(8) 0.58810(16) 0.08718(6) 0.0174(5) Uani 1 1 d . . . . . C1 C 0.16929(10) 0.54492(19) 0.05501(8) 0.0169(6) Uani 1 1 d . . . . . Cl2 Cl 0.20109(3) 0.47173(5) 0.18658(2) 0.02716(17) Uani 1 1 d . . . . . N2 N 0.10414(8) 0.58247(17) 0.09715(7) 0.0188(5) Uani 1 1 d . . . . . C2 C 0.18032(11) 0.5068(2) 0.01673(8) 0.0199(6) Uani 1 1 d . . . . . H2 H 0.217356 0.509757 0.012330 0.024 Uiso 1 1 calc R U . . . N3 N -0.16665(9) 0.11938(17) 0.29737(6) 0.0191(5) Uani 1 1 d . . . . . C3 C 0.13834(11) 0.4660(2) -0.01387(8) 0.0241(6) Uani 1 1 d . . . . . H3 H 0.146495 0.440950 -0.039305 0.029 Uiso 1 1 calc R U . . . C4 C 0.08310(11) 0.4608(2) -0.00811(9) 0.0268(7) Uani 1 1 d . . . . . H4 H 0.054440 0.430968 -0.029456 0.032 Uiso 1 1 calc R U . . . C5 C 0.07044(11) 0.4984(2) 0.02800(8) 0.0227(6) Uani 1 1 d . . . . . H5 H 0.032890 0.495548 0.031274 0.027 Uiso 1 1 calc R U . . . C6 C 0.11239(10) 0.5416(2) 0.06055(8) 0.0169(6) Uani 1 1 d . . . . . C7 C 0.26310(10) 0.6071(2) 0.08250(7) 0.0179(6) Uani 1 1 d . . . . . C8 C 0.27977(11) 0.7191(2) 0.07778(8) 0.0205(6) Uani 1 1 d . . . . . C9 C 0.33465(12) 0.7389(2) 0.07459(8) 0.0263(7) Uani 1 1 d . . . . . H9 H 0.346393 0.813765 0.071276 0.032 Uiso 1 1 calc R U . . . C10 C 0.37250(11) 0.6519(2) 0.07613(9) 0.0288(7) Uani 1 1 d . . . . . H10 H 0.409768 0.667085 0.073832 0.035 Uiso 1 1 calc R U . . . C11 C 0.35572(11) 0.5427(2) 0.08105(8) 0.0254(6) Uani 1 1 d . . . . . H11 H 0.381967 0.483370 0.082469 0.031 Uiso 1 1 calc R U . . . C12 C 0.30110(10) 0.5180(2) 0.08397(8) 0.0199(6) Uani 1 1 d . . . . . C13 C 0.23817(12) 0.8148(2) 0.07547(8) 0.0247(6) Uani 1 1 d . . . . . H13 H 0.211863 0.794146 0.093647 0.030 Uiso 1 1 calc R U . . . C14 C 0.26539(14) 0.9272(2) 0.09145(10) 0.0380(8) Uani 1 1 d . . . . . H14A H 0.288545 0.953915 0.072578 0.057 Uiso 1 1 calc R U . . . H14B H 0.288757 0.916677 0.119299 0.057 Uiso 1 1 calc R U . . . H14C H 0.236231 0.982654 0.092649 0.057 Uiso 1 1 calc R U . . . C15 C 0.20348(12) 0.8285(2) 0.03131(9) 0.0315(7) Uani 1 1 d . . . . . H15A H 0.228111 0.847937 0.012532 0.047 Uiso 1 1 calc R U . . . H15B H 0.175974 0.888540 0.030856 0.047 Uiso 1 1 calc R U . . . H15C H 0.184095 0.757943 0.022232 0.047 Uiso 1 1 calc R U . . . C16 C 0.28531(11) 0.3964(2) 0.09016(9) 0.0262(6) Uani 1 1 d . . . . . H16 H 0.244029 0.393402 0.088061 0.031 Uiso 1 1 calc R U . . . C17 C 0.31386(12) 0.3563(2) 0.13366(9) 0.0339(8) Uani 1 1 d . . . . . H17A H 0.302770 0.278587 0.137569 0.051 Uiso 1 1 calc R U . . . H17B H 0.302621 0.404532 0.154547 0.051 Uiso 1 1 calc R U . . . H17C H 0.354483 0.359977 0.136726 0.051 Uiso 1 1 calc R U . . . C18 C 0.29925(13) 0.3188(2) 0.05661(10) 0.0374(8) Uani 1 1 d . . . . . H18A H 0.278911 0.343779 0.029179 0.056 Uiso 1 1 calc R U . . . H18B H 0.288234 0.241652 0.061528 0.056 Uiso 1 1 calc R U . . . H18C H 0.339492 0.321275 0.057675 0.056 Uiso 1 1 calc R U . . . C19 C 0.04864(10) 0.6129(2) 0.10059(8) 0.0183(6) Uani 1 1 d . . . . . C20 C 0.02629(11) 0.7158(2) 0.08296(8) 0.0224(6) Uani 1 1 d . . . . . C21 C -0.02609(11) 0.7478(2) 0.08901(9) 0.0262(7) Uani 1 1 d . . . . . H21 H -0.041646 0.816817 0.077511 0.031 Uiso 1 1 calc R U . . . C22 C -0.05603(12) 0.6827(2) 0.11107(9) 0.0303(7) Uani 1 1 d . . . . . H22 H -0.091443 0.707017 0.115030 0.036 Uiso 1 1 calc R U . . . C23 C -0.03387(11) 0.5818(2) 0.12733(9) 0.0276(7) Uani 1 1 d . . . . . H23 H -0.054772 0.536160 0.142157 0.033 Uiso 1 1 calc R U . . . C24 C 0.01833(11) 0.5449(2) 0.12261(8) 0.0221(6) Uani 1 1 d . . . . . C25 C 0.05704(12) 0.7911(2) 0.05824(9) 0.0277(7) Uani 1 1 d . . . . . H25 H 0.094679 0.757223 0.059422 0.033 Uiso 1 1 calc R U . . . C26 C 0.06601(15) 0.9079(2) 0.07693(10) 0.0497(10) Uani 1 1 d . . . . . H26A H 0.086799 0.953538 0.060629 0.074 Uiso 1 1 calc R U . . . H26B H 0.087290 0.902525 0.105660 0.074 Uiso 1 1 calc R U . . . H26C H 0.029745 0.942970 0.076563 0.074 Uiso 1 1 calc R U . . . C27 C 0.02741(15) 0.7981(3) 0.01264(10) 0.0498(10) Uani 1 1 d . . . . . H27A H 0.048919 0.846189 -0.002326 0.075 Uiso 1 1 calc R U . . . H27B H -0.009983 0.829857 0.010487 0.075 Uiso 1 1 calc R U . . . H27C H 0.024241 0.722627 0.000445 0.075 Uiso 1 1 calc R U . . . C28 C 0.03936(11) 0.4308(2) 0.13948(9) 0.0265(7) Uani 1 1 d . . . . . H28 H 0.077961 0.420440 0.134653 0.032 Uiso 1 1 calc R U . . . C29 C 0.04220(13) 0.4227(3) 0.18622(10) 0.0410(8) Uani 1 1 d . . . . . H29A H 0.005232 0.438100 0.191827 0.062 Uiso 1 1 calc R U . . . H29B H 0.069061 0.477865 0.200834 0.062 Uiso 1 1 calc R U . . . H29C H 0.054129 0.347002 0.195948 0.062 Uiso 1 1 calc R U . . . C30 C 0.00216(12) 0.3382(2) 0.11595(10) 0.0370(8) Uani 1 1 d . . . . . H30A H 0.002807 0.342263 0.086343 0.055 Uiso 1 1 calc R U . . . H30B H -0.036211 0.348349 0.119518 0.055 Uiso 1 1 calc R U . . . H30C H 0.016093 0.264679 0.126948 0.055 Uiso 1 1 calc R U . . . C31 C -0.15956(11) 0.1922(2) 0.26099(8) 0.0244(6) Uani 1 1 d . . . . . H31A H -0.188800 0.251038 0.256757 0.029 Uiso 1 1 calc R U . . . H31B H -0.122967 0.230632 0.268638 0.029 Uiso 1 1 calc R U . . . C32 C -0.16254(13) 0.1323(2) 0.22016(9) 0.0328(7) Uani 1 1 d . . . . . H32A H -0.198062 0.090041 0.212682 0.039 Uiso 1 1 calc R U . . . H32B H -0.131405 0.077851 0.223067 0.039 Uiso 1 1 calc R U . . . C33 C -0.15900(13) 0.2157(3) 0.18585(9) 0.0425(9) Uani 1 1 d . . . . . H33A H -0.163837 0.174362 0.159232 0.051 Uiso 1 1 calc R U . . . H33B H -0.190362 0.269451 0.183280 0.051 Uiso 1 1 calc R U . . . C34 C -0.10486(14) 0.2814(3) 0.19246(10) 0.0512(10) Uani 1 1 d . . . . . H34A H -0.073313 0.229022 0.196192 0.077 Uiso 1 1 calc R U . . . H34B H -0.101347 0.328505 0.217278 0.077 Uiso 1 1 calc R U . . . H34C H -0.104910 0.329009 0.168192 0.077 Uiso 1 1 calc R U . . . C35 C -0.22544(11) 0.0727(2) 0.29081(9) 0.0230(6) Uani 1 1 d . . . . . H35A H -0.228602 0.029770 0.315944 0.028 Uiso 1 1 calc R U . . . H35B H -0.230838 0.018987 0.267342 0.028 Uiso 1 1 calc R U . . . C36 C -0.27271(11) 0.1579(2) 0.28195(9) 0.0283(7) Uani 1 1 d . . . . . H36A H -0.276090 0.188801 0.253619 0.034 Uiso 1 1 calc R U . . . H36B H -0.264334 0.220748 0.301999 0.034 Uiso 1 1 calc R U . . . C37 C -0.32746(12) 0.1027(3) 0.28549(10) 0.0392(8) Uani 1 1 d . . . . . H37A H -0.325607 0.081837 0.314852 0.047 Uiso 1 1 calc R U . . . H37B H -0.332469 0.032864 0.268795 0.047 Uiso 1 1 calc R U . . . C38 C -0.37768(13) 0.1789(3) 0.27071(11) 0.0548(10) Uani 1 1 d . . . . . H38A H -0.381101 0.196075 0.241178 0.082 Uiso 1 1 calc R U . . . H38B H -0.372668 0.248774 0.286799 0.082 Uiso 1 1 calc R U . . . H38C H -0.411618 0.140764 0.274646 0.082 Uiso 1 1 calc R U . . . C39 C -0.15291(12) 0.1945(2) 0.33559(8) 0.0224(6) Uani 1 1 d . . . . . H39A H -0.112719 0.213590 0.340632 0.027 Uiso 1 1 calc R U . . . H39B H -0.174086 0.265384 0.329123 0.027 Uiso 1 1 calc R U . . . C40 C -0.16494(12) 0.1476(2) 0.37565(8) 0.0235(6) Uani 1 1 d . . . . . H40A H -0.149827 0.070420 0.380235 0.028 Uiso 1 1 calc R U . . . H40B H -0.205790 0.144208 0.373611 0.028 Uiso 1 1 calc R U . . . C41 C -0.13819(13) 0.2221(2) 0.41190(9) 0.0341(7) Uani 1 1 d . . . . . H41A H -0.097218 0.221630 0.414377 0.041 Uiso 1 1 calc R U . . . H41B H -0.151367 0.300136 0.405804 0.041 Uiso 1 1 calc R U . . . C42 C -0.15071(14) 0.1869(3) 0.45321(9) 0.0380(8) Uani 1 1 d . . . . . H42A H -0.191232 0.184978 0.450905 0.057 Uiso 1 1 calc R U . . . H42B H -0.133919 0.240940 0.474729 0.057 Uiso 1 1 calc R U . . . H42C H -0.135080 0.112091 0.460698 0.057 Uiso 1 1 calc R U . . . C43 C -0.12813(11) 0.0183(2) 0.30234(9) 0.0232(6) Uani 1 1 d . . . . . H43A H -0.139058 -0.028947 0.277161 0.028 Uiso 1 1 calc R U . . . H43B H -0.134727 -0.026549 0.326146 0.028 Uiso 1 1 calc R U . . . C44 C -0.06589(11) 0.0413(2) 0.30915(9) 0.0297(7) Uani 1 1 d . . . . . H44A H -0.058623 0.093612 0.287541 0.036 Uiso 1 1 calc R U . . . H44B H -0.052574 0.077053 0.336626 0.036 Uiso 1 1 calc R U . . . C45 C -0.03461(12) -0.0679(2) 0.30715(10) 0.0351(8) Uani 1 1 d . . . . . H45A H -0.047869 -0.102553 0.279466 0.042 Uiso 1 1 calc R U . . . H45B H -0.043056 -0.120498 0.328259 0.042 Uiso 1 1 calc R U . . . C46 C 0.02824(13) -0.0507(3) 0.31466(11) 0.0540(10) Uani 1 1 d . . . . . H46A H 0.046440 -0.122661 0.311690 0.081 Uiso 1 1 calc R U . . . H46B H 0.041994 -0.021456 0.342803 0.081 Uiso 1 1 calc R U . . . H46C H 0.036772 0.002974 0.294344 0.081 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.01694(19) 0.01711(19) 0.0184(2) -0.00185(17) 0.00094(15) 0.00009(17) Cl1 0.0476(5) 0.0210(4) 0.0268(4) -0.0057(3) 0.0071(4) 0.0030(3) N1 0.0134(11) 0.0189(12) 0.0181(12) -0.0006(9) -0.0006(9) -0.0007(9) C1 0.0167(13) 0.0122(13) 0.0194(14) 0.0009(11) -0.0013(11) 0.0000(11) Cl2 0.0323(4) 0.0184(3) 0.0265(4) 0.0023(3) -0.0032(3) -0.0036(3) N2 0.0166(11) 0.0204(12) 0.0187(12) -0.0022(9) 0.0021(9) 0.0013(9) C2 0.0186(14) 0.0208(14) 0.0198(15) -0.0022(11) 0.0033(12) 0.0005(12) N3 0.0245(12) 0.0147(11) 0.0172(12) 0.0008(9) 0.0023(10) -0.0018(10) C3 0.0250(15) 0.0274(16) 0.0199(15) -0.0042(12) 0.0050(12) 0.0025(13) C4 0.0210(15) 0.0297(16) 0.0253(16) -0.0091(13) -0.0045(12) -0.0012(13) C5 0.0138(13) 0.0273(15) 0.0257(16) -0.0040(12) 0.0011(12) 0.0002(12) C6 0.0144(13) 0.0155(13) 0.0190(14) -0.0008(11) -0.0005(11) 0.0008(11) C7 0.0141(13) 0.0259(14) 0.0118(13) -0.0001(12) -0.0015(10) -0.0031(12) C8 0.0215(14) 0.0260(15) 0.0127(13) -0.0014(11) 0.0008(11) -0.0041(12) C9 0.0321(17) 0.0283(16) 0.0186(15) -0.0004(12) 0.0053(13) -0.0084(14) C10 0.0167(14) 0.0447(19) 0.0258(17) -0.0006(14) 0.0060(13) -0.0071(14) C11 0.0172(14) 0.0318(17) 0.0261(16) -0.0029(13) 0.0019(12) 0.0034(13) C12 0.0145(13) 0.0260(15) 0.0178(14) -0.0013(12) 0.0006(11) 0.0004(12) C13 0.0305(16) 0.0221(15) 0.0234(16) -0.0007(12) 0.0099(13) -0.0002(13) C14 0.052(2) 0.0245(16) 0.0386(19) -0.0049(14) 0.0133(17) -0.0022(15) C15 0.0347(17) 0.0270(16) 0.0313(17) 0.0076(14) 0.0034(14) 0.0054(14) C16 0.0204(14) 0.0237(15) 0.0339(17) 0.0010(13) 0.0043(13) 0.0043(13) C17 0.0342(18) 0.0304(17) 0.0388(19) 0.0091(14) 0.0116(15) 0.0071(14) C18 0.0370(18) 0.0288(17) 0.043(2) -0.0075(15) 0.0014(16) 0.0039(15) C19 0.0137(13) 0.0249(14) 0.0151(13) -0.0049(12) 0.0007(10) -0.0010(12) C20 0.0234(15) 0.0212(15) 0.0198(15) -0.0047(12) -0.0015(12) -0.0027(12) C21 0.0227(15) 0.0202(15) 0.0337(17) -0.0031(13) 0.0020(13) 0.0070(12) C22 0.0205(15) 0.0350(18) 0.0359(18) -0.0048(14) 0.0076(14) 0.0099(14) C23 0.0204(15) 0.0332(17) 0.0306(17) 0.0019(13) 0.0085(13) 0.0017(13) C24 0.0178(14) 0.0258(15) 0.0219(15) -0.0026(12) 0.0029(12) 0.0017(12) C25 0.0250(16) 0.0241(15) 0.0327(17) 0.0053(13) 0.0031(13) 0.0008(13) C26 0.072(3) 0.033(2) 0.041(2) -0.0002(16) 0.0075(19) -0.0219(18) C27 0.070(3) 0.049(2) 0.0302(19) 0.0011(16) 0.0091(18) -0.0163(19) C28 0.0184(14) 0.0286(15) 0.0329(17) 0.0058(13) 0.0062(13) 0.0023(13) C29 0.0359(18) 0.046(2) 0.040(2) 0.0146(16) 0.0057(16) 0.0068(16) C30 0.0323(18) 0.0302(17) 0.047(2) 0.0027(15) 0.0066(16) -0.0012(15) C31 0.0253(15) 0.0236(15) 0.0229(15) 0.0071(12) 0.0021(13) -0.0034(12) C32 0.0301(17) 0.0443(19) 0.0224(17) -0.0026(14) 0.0025(13) -0.0135(15) C33 0.0381(19) 0.065(2) 0.0234(17) 0.0056(16) 0.0042(15) -0.0103(17) C34 0.057(2) 0.062(2) 0.037(2) 0.0044(18) 0.0133(18) -0.023(2) C35 0.0242(15) 0.0206(14) 0.0231(16) -0.0029(12) 0.0024(12) -0.0059(12) C36 0.0270(16) 0.0320(16) 0.0244(16) -0.0025(13) 0.0021(13) 0.0028(13) C37 0.0293(17) 0.056(2) 0.0321(18) -0.0046(16) 0.0067(14) -0.0003(17) C38 0.0247(18) 0.084(3) 0.053(2) -0.011(2) 0.0017(17) 0.0096(19) C39 0.0297(16) 0.0147(13) 0.0212(15) -0.0013(11) 0.0022(13) -0.0023(12) C40 0.0286(16) 0.0186(14) 0.0230(16) 0.0015(11) 0.0048(13) 0.0015(12) C41 0.0407(19) 0.0328(17) 0.0301(18) -0.0068(14) 0.0101(15) -0.0039(15) C42 0.050(2) 0.0379(19) 0.0260(17) -0.0034(14) 0.0092(16) 0.0001(16) C43 0.0255(15) 0.0162(14) 0.0269(16) -0.0008(12) 0.0032(13) 0.0022(12) C44 0.0259(16) 0.0267(16) 0.0334(18) 0.0000(13) -0.0003(13) -0.0001(13) C45 0.0310(17) 0.0352(17) 0.0380(19) 0.0009(15) 0.0051(15) 0.0096(15) C46 0.0331(19) 0.067(3) 0.058(3) -0.002(2) 0.0016(18) 0.0130(18) 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' Cl Cl 0.1484 0.1585 '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' N N 0.0061 0.0033 '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' 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 N2 Fe1 N1 81.07(8) . . ? N2 Fe1 Cl1 116.22(6) . . ? N1 Fe1 Cl1 118.92(6) . . ? N2 Fe1 Cl2 115.51(6) . . ? N1 Fe1 Cl2 113.48(6) . . ? Cl1 Fe1 Cl2 109.44(3) . . ? C1 N1 C7 119.2(2) . . ? C1 N1 Fe1 112.63(16) . . ? C7 N1 Fe1 128.09(16) . . ? N1 C1 C2 126.1(2) . . ? N1 C1 C6 115.4(2) . . ? C2 C1 C6 118.4(2) . . ? C6 N2 C19 119.0(2) . . ? C6 N2 Fe1 112.78(16) . . ? C19 N2 Fe1 127.78(16) . . ? C3 C2 C1 120.8(2) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? C35 N3 C43 105.98(18) . . ? C35 N3 C31 111.2(2) . . ? C43 N3 C31 111.4(2) . . ? C35 N3 C39 111.6(2) . . ? C43 N3 C39 110.76(19) . . ? C31 N3 C39 105.96(18) . . ? C2 C3 C4 120.7(3) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C5 C4 C3 120.4(3) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C4 C5 C6 121.0(2) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? N2 C6 C5 125.6(2) . . ? N2 C6 C1 115.7(2) . . ? C5 C6 C1 118.6(2) . . ? C12 C7 C8 120.7(2) . . ? C12 C7 N1 121.4(2) . . ? C8 C7 N1 117.9(2) . . ? C9 C8 C7 118.4(2) . . ? C9 C8 C13 121.2(2) . . ? C7 C8 C13 120.4(2) . . ? C10 C9 C8 121.5(3) . . ? C10 C9 H9 119.3 . . ? C8 C9 H9 119.3 . . ? C11 C10 C9 119.6(3) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? C10 C11 C12 121.4(3) . . ? C10 C11 H11 119.3 . . ? C12 C11 H11 119.3 . . ? C11 C12 C7 118.5(2) . . ? C11 C12 C16 119.0(2) . . ? C7 C12 C16 122.4(2) . . ? C8 C13 C15 111.0(2) . . ? C8 C13 C14 113.4(2) . . ? C15 C13 C14 110.2(2) . . ? 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 110.1(2) . . ? C12 C16 C18 112.0(2) . . ? C17 C16 C18 111.0(2) . . ? C12 C16 H16 107.9 . . ? C17 C16 H16 107.9 . . ? C18 C16 H16 107.9 . . ? 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 . . ? C24 C19 C20 120.7(2) . . ? C24 C19 N2 120.7(2) . . ? C20 C19 N2 118.5(2) . . ? C21 C20 C19 117.7(2) . . ? C21 C20 C25 119.6(2) . . ? C19 C20 C25 122.6(2) . . ? C22 C21 C20 122.2(3) . . ? C22 C21 H21 118.9 . . ? C20 C21 H21 118.9 . . ? C21 C22 C23 119.0(3) . . ? C21 C22 H22 120.5 . . ? C23 C22 H22 120.5 . . ? C22 C23 C24 121.7(3) . . ? C22 C23 H23 119.1 . . ? C24 C23 H23 119.1 . . ? C23 C24 C19 118.5(2) . . ? C23 C24 C28 119.3(2) . . ? C19 C24 C28 122.1(2) . . ? C20 C25 C26 111.7(2) . . ? C20 C25 C27 112.0(2) . . ? C26 C25 C27 110.3(2) . . ? C20 C25 H25 107.5 . . ? C26 C25 H25 107.5 . . ? C27 C25 H25 107.5 . . ? 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 . . ? 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 . . ? C24 C28 C29 111.4(2) . . ? C24 C28 C30 109.9(2) . . ? C29 C28 C30 111.0(2) . . ? C24 C28 H28 108.2 . . ? C29 C28 H28 108.2 . . ? C30 C28 H28 108.2 . . ? 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 . . ? 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 . . ? C32 C31 N3 116.2(2) . . ? C32 C31 H31A 108.2 . . ? N3 C31 H31A 108.2 . . ? C32 C31 H31B 108.2 . . ? N3 C31 H31B 108.2 . . ? H31A C31 H31B 107.4 . . ? C31 C32 C33 110.7(2) . . ? C31 C32 H32A 109.5 . . ? C33 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? C33 C32 H32B 109.5 . . ? H32A C32 H32B 108.1 . . ? C34 C33 C32 114.7(3) . . ? C34 C33 H33A 108.6 . . ? C32 C33 H33A 108.6 . . ? C34 C33 H33B 108.6 . . ? C32 C33 H33B 108.6 . . ? H33A C33 H33B 107.6 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N3 C35 C36 116.4(2) . . ? N3 C35 H35A 108.2 . . ? C36 C35 H35A 108.2 . . ? N3 C35 H35B 108.2 . . ? C36 C35 H35B 108.2 . . ? H35A C35 H35B 107.3 . . ? C35 C36 C37 110.3(2) . . ? C35 C36 H36A 109.6 . . ? C37 C36 H36A 109.6 . . ? C35 C36 H36B 109.6 . . ? C37 C36 H36B 109.6 . . ? H36A C36 H36B 108.1 . . ? C36 C37 C38 112.6(3) . . ? C36 C37 H37A 109.1 . . ? C38 C37 H37A 109.1 . . ? C36 C37 H37B 109.1 . . ? C38 C37 H37B 109.1 . . ? H37A C37 H37B 107.8 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C40 C39 N3 117.0(2) . . ? C40 C39 H39A 108.1 . . ? N3 C39 H39A 108.1 . . ? C40 C39 H39B 108.1 . . ? N3 C39 H39B 108.1 . . ? H39A C39 H39B 107.3 . . ? C39 C40 C41 109.7(2) . . ? C39 C40 H40A 109.7 . . ? C41 C40 H40A 109.7 . . ? C39 C40 H40B 109.7 . . ? C41 C40 H40B 109.7 . . ? H40A C40 H40B 108.2 . . ? C42 C41 C40 114.1(2) . . ? C42 C41 H41A 108.7 . . ? C40 C41 H41A 108.7 . . ? C42 C41 H41B 108.7 . . ? C40 C41 H41B 108.7 . . ? H41A C41 H41B 107.6 . . ? 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 . . ? N3 C43 C44 117.1(2) . . ? N3 C43 H43A 108.0 . . ? C44 C43 H43A 108.0 . . ? N3 C43 H43B 108.0 . . ? C44 C43 H43B 108.0 . . ? H43A C43 H43B 107.3 . . ? C45 C44 C43 109.9(2) . . ? C45 C44 H44A 109.7 . . ? C43 C44 H44A 109.7 . . ? C45 C44 H44B 109.7 . . ? C43 C44 H44B 109.7 . . ? H44A C44 H44B 108.2 . . ? C44 C45 C46 112.4(3) . . ? C44 C45 H45A 109.1 . . ? C46 C45 H45A 109.1 . . ? C44 C45 H45B 109.1 . . ? C46 C45 H45B 109.1 . . ? H45A C45 H45B 107.9 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N2 2.003(2) . ? Fe1 N1 2.018(2) . ? Fe1 Cl1 2.2541(8) . ? Fe1 Cl2 2.2677(8) . ? N1 C1 1.351(3) . ? N1 C7 1.433(3) . ? C1 C2 1.419(3) . ? C1 C6 1.445(3) . ? N2 C6 1.355(3) . ? N2 C19 1.436(3) . ? C2 C3 1.366(3) . ? C2 H2 0.9500 . ? N3 C35 1.516(3) . ? N3 C43 1.517(3) . ? N3 C31 1.519(3) . ? N3 C39 1.522(3) . ? C3 C4 1.408(4) . ? C3 H3 0.9500 . ? C4 C5 1.367(4) . ? C4 H4 0.9500 . ? C5 C6 1.413(3) . ? C5 H5 0.9500 . ? C7 C12 1.405(3) . ? C7 C8 1.413(3) . ? C8 C9 1.392(4) . ? C8 C13 1.520(4) . ? C9 C10 1.384(4) . ? C9 H9 0.9500 . ? C10 C11 1.383(4) . ? C10 H10 0.9500 . ? C11 C12 1.394(4) . ? C11 H11 0.9500 . ? C12 C16 1.523(4) . ? C13 C15 1.528(4) . ? C13 C14 1.537(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 1.530(4) . ? C16 C18 1.534(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 . ? C19 C24 1.401(4) . ? C19 C20 1.414(4) . ? C20 C21 1.394(4) . ? C20 C25 1.516(4) . ? C21 C22 1.376(4) . ? C21 H21 0.9500 . ? C22 C23 1.379(4) . ? C22 H22 0.9500 . ? C23 C24 1.393(4) . ? C23 H23 0.9500 . ? C24 C28 1.515(4) . ? C25 C26 1.517(4) . ? C25 C27 1.524(4) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.529(4) . ? C28 C30 1.531(4) . ? C28 H28 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.510(4) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.520(4) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.515(4) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.520(4) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.521(4) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.522(4) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.518(3) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.519(4) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.516(4) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.519(4) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.518(4) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.521(4) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C7 N1 C1 C2 5.3(4) . . . . ? Fe1 N1 C1 C2 -171.2(2) . . . . ? C7 N1 C1 C6 -172.6(2) . . . . ? Fe1 N1 C1 C6 10.9(3) . . . . ? N1 C1 C2 C3 -179.1(2) . . . . ? C6 C1 C2 C3 -1.2(4) . . . . ? C1 C2 C3 C4 0.0(4) . . . . ? C2 C3 C4 C5 1.2(4) . . . . ? C3 C4 C5 C6 -1.0(4) . . . . ? C19 N2 C6 C5 -17.2(4) . . . . ? Fe1 N2 C6 C5 169.6(2) . . . . ? C19 N2 C6 C1 161.9(2) . . . . ? Fe1 N2 C6 C1 -11.3(3) . . . . ? C4 C5 C6 N2 178.9(2) . . . . ? C4 C5 C6 C1 -0.2(4) . . . . ? N1 C1 C6 N2 0.3(3) . . . . ? C2 C1 C6 N2 -177.9(2) . . . . ? N1 C1 C6 C5 179.4(2) . . . . ? C2 C1 C6 C5 1.3(3) . . . . ? C1 N1 C7 C12 -76.3(3) . . . . ? Fe1 N1 C7 C12 99.6(3) . . . . ? C1 N1 C7 C8 105.8(3) . . . . ? Fe1 N1 C7 C8 -78.2(3) . . . . ? C12 C7 C8 C9 0.1(4) . . . . ? N1 C7 C8 C9 177.9(2) . . . . ? C12 C7 C8 C13 178.9(2) . . . . ? N1 C7 C8 C13 -3.2(3) . . . . ? C7 C8 C9 C10 -0.3(4) . . . . ? C13 C8 C9 C10 -179.2(2) . . . . ? C8 C9 C10 C11 -0.2(4) . . . . ? C9 C10 C11 C12 0.8(4) . . . . ? C10 C11 C12 C7 -1.0(4) . . . . ? C10 C11 C12 C16 -178.9(2) . . . . ? C8 C7 C12 C11 0.6(4) . . . . ? N1 C7 C12 C11 -177.2(2) . . . . ? C8 C7 C12 C16 178.4(2) . . . . ? N1 C7 C12 C16 0.6(4) . . . . ? C9 C8 C13 C15 95.3(3) . . . . ? C7 C8 C13 C15 -83.5(3) . . . . ? C9 C8 C13 C14 -29.4(4) . . . . ? C7 C8 C13 C14 151.8(2) . . . . ? C11 C12 C16 C17 69.3(3) . . . . ? C7 C12 C16 C17 -108.4(3) . . . . ? C11 C12 C16 C18 -54.7(3) . . . . ? C7 C12 C16 C18 127.6(3) . . . . ? C6 N2 C19 C24 105.5(3) . . . . ? Fe1 N2 C19 C24 -82.4(3) . . . . ? C6 N2 C19 C20 -77.4(3) . . . . ? Fe1 N2 C19 C20 94.7(3) . . . . ? C24 C19 C20 C21 1.3(4) . . . . ? N2 C19 C20 C21 -175.7(2) . . . . ? C24 C19 C20 C25 -178.9(2) . . . . ? N2 C19 C20 C25 4.1(4) . . . . ? C19 C20 C21 C22 -0.4(4) . . . . ? C25 C20 C21 C22 179.8(3) . . . . ? C20 C21 C22 C23 -0.8(4) . . . . ? C21 C22 C23 C24 1.1(4) . . . . ? C22 C23 C24 C19 -0.1(4) . . . . ? C22 C23 C24 C28 -177.3(3) . . . . ? C20 C19 C24 C23 -1.1(4) . . . . ? N2 C19 C24 C23 175.9(2) . . . . ? C20 C19 C24 C28 175.9(2) . . . . ? N2 C19 C24 C28 -7.1(4) . . . . ? C21 C20 C25 C26 57.6(3) . . . . ? C19 C20 C25 C26 -122.2(3) . . . . ? C21 C20 C25 C27 -66.7(3) . . . . ? C19 C20 C25 C27 113.5(3) . . . . ? C23 C24 C28 C29 -58.3(3) . . . . ? C19 C24 C28 C29 124.7(3) . . . . ? C23 C24 C28 C30 65.1(3) . . . . ? C19 C24 C28 C30 -111.9(3) . . . . ? C35 N3 C31 C32 -67.3(3) . . . . ? C43 N3 C31 C32 50.7(3) . . . . ? C39 N3 C31 C32 171.2(2) . . . . ? N3 C31 C32 C33 175.9(2) . . . . ? C31 C32 C33 C34 62.4(4) . . . . ? C43 N3 C35 C36 -175.9(2) . . . . ? C31 N3 C35 C36 -54.7(3) . . . . ? C39 N3 C35 C36 63.4(3) . . . . ? N3 C35 C36 C37 -167.6(2) . . . . ? C35 C36 C37 C38 -171.4(3) . . . . ? C35 N3 C39 C40 50.0(3) . . . . ? C43 N3 C39 C40 -67.9(3) . . . . ? C31 N3 C39 C40 171.2(2) . . . . ? N3 C39 C40 C41 168.5(2) . . . . ? C39 C40 C41 C42 176.3(3) . . . . ? C35 N3 C43 C44 179.6(2) . . . . ? C31 N3 C43 C44 58.5(3) . . . . ? C39 N3 C43 C44 -59.1(3) . . . . ? N3 C43 C44 C45 -171.8(2) . . . . ? C43 C44 C45 C46 -178.8(3) . . . . ?