#------------------------------------------------------------------------------ #$Date: 2020-08-18 05:02:47 +0300 (Tue, 18 Aug 2020) $ #$Revision: 255416 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/51/7705182.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_7705182 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 'C60 H76 Cl2 Fe2 N4, C4 H10 O' _chemical_formula_sum 'C64 H86 Cl2 Fe2 N4 O' _chemical_formula_weight 1109.96 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _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 61.794(3) _cell_angle_beta 68.888(3) _cell_angle_gamma 79.987(4) _cell_formula_units_Z 1 _cell_length_a 10.1107(7) _cell_length_b 13.5638(9) _cell_length_c 13.8531(10) _cell_measurement_reflns_used 7092 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 27.562 _cell_measurement_theta_min 2.159 _cell_volume 1561.8(2) _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.983 _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 0.0397 _diffrn_reflns_av_unetI/netI 0.0514 _diffrn_reflns_Laue_measured_fraction_full 0.993 _diffrn_reflns_Laue_measured_fraction_max 0.983 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 24503 _diffrn_reflns_point_group_measured_fraction_full 0.993 _diffrn_reflns_point_group_measured_fraction_max 0.983 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.562 _diffrn_reflns_theta_min 2.159 _exptl_absorpt_coefficient_mu 0.591 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.6706 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour 'dark green' _exptl_crystal_density_diffrn 1.180 _exptl_crystal_description block _exptl_crystal_F_000 592 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.311 _refine_diff_density_min -0.254 _refine_diff_density_rms 0.050 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 352 _refine_ls_number_reflns 7092 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.027 _refine_ls_R_factor_all 0.0671 _refine_ls_R_factor_gt 0.0384 _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^)+(0.0357P)^2^+0.3940P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0810 _refine_ls_wR_factor_ref 0.0902 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5131 _reflns_number_total 7092 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02087g2.cif _cod_data_source_block wl152 _cod_original_cell_volume 1561.82(19) _cod_database_code 7705182 _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 wl152_0m in P-1 wl152.res created by SHELXL-2016/6 at 15:48:30 on 08-Aug-2020 CELL 0.71073 10.1107 13.5638 13.8531 61.794 68.888 79.987 ZERR 1.00 0.0007 0.0009 0.0010 0.003 0.003 0.004 LATT 1 SFAC C H N Cl Fe O UNIT 64 86 4 2 2 1 L.S. 5 ACTA BOND $H FMAP 2 PLAN -10 CONF HTAB TEMP -123.030 WGHT 0.035700 0.394000 FVAR 0.23177 FE1 5 0.871622 0.935408 0.597325 11.00000 0.02449 0.02851 = 0.02253 -0.01176 -0.00381 -0.00230 CL1 4 1.112075 0.891222 0.561283 11.00000 0.02646 0.03227 = 0.03218 -0.00760 -0.00678 0.00087 N1 3 0.746997 0.818987 0.628661 11.00000 0.02765 0.02414 = 0.02244 -0.01138 -0.00650 0.00105 C1 1 0.632741 0.799277 0.722815 11.00000 0.02524 0.02263 = 0.02462 -0.01024 -0.00733 0.00219 N2 3 0.749346 0.913218 0.754025 11.00000 0.02396 0.02964 = 0.02302 -0.01293 -0.00735 -0.00046 C2 1 0.517341 0.729413 0.760403 11.00000 0.03390 0.03291 = 0.03643 -0.01909 -0.00592 -0.00504 AFIX 43 H2A 2 0.516189 0.692933 0.716669 11.00000 -1.20000 AFIX 0 C3 1 0.408008 0.714419 0.859124 11.00000 0.03337 0.04380 = 0.04623 -0.02190 -0.00008 -0.01332 AFIX 43 H3A 2 0.331015 0.667694 0.883361 11.00000 -1.20000 AFIX 0 C4 1 0.407670 0.767129 0.925487 11.00000 0.03380 0.04848 = 0.03238 -0.01938 0.00617 -0.01055 AFIX 43 H4A 2 0.329913 0.755888 0.993572 11.00000 -1.20000 AFIX 0 C5 1 0.516583 0.834007 0.894149 11.00000 0.03144 0.03749 = 0.02569 -0.01522 -0.00388 -0.00347 AFIX 43 H5A 2 0.514543 0.868306 0.940661 11.00000 -1.20000 AFIX 0 C6 1 0.633174 0.852618 0.792162 11.00000 0.02381 0.02627 = 0.02085 -0.00918 -0.00710 0.00186 C7 1 0.770234 0.751825 0.569030 11.00000 0.02622 0.02824 = 0.03072 -0.01703 -0.00327 -0.00149 C8 1 0.818937 0.640592 0.619504 11.00000 0.04132 0.03237 = 0.04462 -0.02067 -0.00782 0.00467 C9 1 0.846159 0.579053 0.558162 11.00000 0.05995 0.03708 = 0.07281 -0.03567 -0.01627 0.01146 AFIX 43 H9A 2 0.879500 0.504263 0.590001 11.00000 -1.20000 AFIX 0 C10 1 0.826165 0.623434 0.452428 11.00000 0.06368 0.06615 = 0.08417 -0.06246 -0.02175 0.01339 AFIX 43 H10A 2 0.844589 0.579030 0.412620 11.00000 -1.20000 AFIX 0 C11 1 0.779212 0.732753 0.403615 11.00000 0.04890 0.06300 = 0.05351 -0.04292 -0.01956 0.00738 AFIX 43 H11A 2 0.766384 0.762835 0.330179 11.00000 -1.20000 AFIX 0 C12 1 0.750618 0.799020 0.460723 11.00000 0.02871 0.03811 = 0.03557 -0.02324 -0.00724 -0.00074 C13 1 0.846122 0.589275 0.734141 11.00000 0.07232 0.03373 = 0.04364 -0.01308 -0.01836 0.01700 AFIX 13 H13A 2 0.806557 0.641923 0.769496 11.00000 -1.20000 AFIX 0 C14 1 1.004128 0.577161 0.718467 11.00000 0.08142 0.05827 = 0.06610 -0.03295 -0.03596 0.01403 AFIX 33 H14A 2 1.017913 0.543736 0.794241 11.00000 -1.50000 H14B 2 1.047448 0.528917 0.680287 11.00000 -1.50000 H14C 2 1.048709 0.651033 0.670786 11.00000 -1.50000 AFIX 0 C15 1 0.771323 0.477906 0.818426 11.00000 0.11311 0.07508 = 0.07921 0.01978 -0.03527 -0.01878 AFIX 33 H15A 2 0.792146 0.448148 0.891123 11.00000 -1.50000 H15B 2 0.668787 0.488819 0.833419 11.00000 -1.50000 H15C 2 0.804817 0.424958 0.785069 11.00000 -1.50000 AFIX 0 C16 1 0.692270 0.916249 0.409152 11.00000 0.04469 0.04086 = 0.03316 -0.02067 -0.01829 0.00212 AFIX 13 H16A 2 0.701943 0.955836 0.451525 11.00000 -1.20000 AFIX 0 C17 1 0.772974 0.983664 0.281362 11.00000 0.09727 0.06473 = 0.03519 -0.01571 -0.01136 -0.00279 AFIX 33 H17A 2 0.730997 1.058558 0.252453 11.00000 -1.50000 H17B 2 0.872517 0.989995 0.271704 11.00000 -1.50000 H17C 2 0.767283 0.945772 0.237788 11.00000 -1.50000 AFIX 0 C18 1 0.533591 0.911641 0.428286 11.00000 0.05585 0.05869 = 0.08228 -0.04126 -0.04345 0.01680 AFIX 33 H18A 2 0.496766 0.987864 0.394636 11.00000 -1.50000 H18B 2 0.520420 0.869725 0.391036 11.00000 -1.50000 H18C 2 0.482382 0.874396 0.511387 11.00000 -1.50000 AFIX 0 C19 1 0.775089 0.945518 0.830615 11.00000 0.02194 0.04472 = 0.02472 -0.01841 -0.00470 -0.00341 C20 1 0.828838 0.864948 0.918114 11.00000 0.03326 0.05158 = 0.02854 -0.01293 -0.01071 -0.00498 C21 1 0.856279 0.898809 0.989763 11.00000 0.04028 0.08292 = 0.02943 -0.01779 -0.01792 -0.00541 AFIX 43 H21A 2 0.891167 0.845518 1.050351 11.00000 -1.20000 AFIX 0 C22 1 0.834153 1.007280 0.974980 11.00000 0.04720 0.09088 = 0.04078 -0.04201 -0.01130 -0.01016 AFIX 43 H22A 2 0.853211 1.028160 1.025175 11.00000 -1.20000 AFIX 0 C23 1 0.784209 1.085650 0.887053 11.00000 0.04135 0.06581 = 0.04487 -0.03954 -0.01041 -0.00338 AFIX 43 H23A 2 0.770577 1.160726 0.876524 11.00000 -1.20000 AFIX 0 C24 1 0.753335 1.056846 0.813318 11.00000 0.02580 0.04947 = 0.03107 -0.02610 -0.00509 -0.00296 C25 1 0.860601 0.746127 0.934009 11.00000 0.05145 0.05281 = 0.04833 -0.00954 -0.03085 0.00159 AFIX 13 H25A 2 0.836003 0.739749 0.873432 11.00000 -1.20000 AFIX 0 C26 1 1.018991 0.717695 0.915949 11.00000 0.05768 0.06748 = 0.07005 -0.02408 -0.02837 0.00938 AFIX 33 H26A 2 1.035676 0.640281 0.926886 11.00000 -1.50000 H26B 2 1.074755 0.768359 0.837381 11.00000 -1.50000 H26C 2 1.047505 0.726323 0.972069 11.00000 -1.50000 AFIX 0 C27 1 0.771126 0.660431 1.051826 11.00000 0.06911 0.06267 = 0.09441 0.00634 -0.02102 -0.00546 AFIX 33 H27A 2 0.795365 0.584930 1.058087 11.00000 -1.50000 H27B 2 0.790357 0.666381 1.113343 11.00000 -1.50000 H27C 2 0.670360 0.675106 1.059495 11.00000 -1.50000 AFIX 0 C28 1 0.695576 1.145322 0.720216 11.00000 0.04077 0.04261 = 0.04418 -0.03016 -0.01626 0.00560 AFIX 13 H28A 2 0.686772 1.111058 0.672818 11.00000 -1.20000 AFIX 0 C29 1 0.796160 1.245534 0.639156 11.00000 0.07059 0.05288 = 0.05595 -0.02150 -0.02045 -0.00952 AFIX 33 H29A 2 0.755414 1.301106 0.580022 11.00000 -1.50000 H29B 2 0.809215 1.279297 0.683931 11.00000 -1.50000 H29C 2 0.888045 1.220154 0.601783 11.00000 -1.50000 AFIX 0 C30 1 0.546793 1.182443 0.774349 11.00000 0.04929 0.06952 = 0.06716 -0.04443 -0.02167 0.01927 AFIX 33 H30A 2 0.510789 1.239787 0.712937 11.00000 -1.50000 H30B 2 0.483037 1.117932 0.820393 11.00000 -1.50000 H30C 2 0.551636 1.213294 0.824254 11.00000 -1.50000 AFIX 0 PART -1 O1 6 0.474697 0.529204 0.489223 10.50000 0.05584 0.04339 = 0.06530 -0.02791 -0.01723 -0.00236 C31 1 0.445733 0.497344 0.603216 10.50000 0.08480 0.05811 = 0.06669 -0.00461 -0.01365 -0.01250 AFIX 3 H31A 2 0.533674 0.474984 0.619696 10.50000 -1.20000 H31B 2 0.382864 0.434414 0.649896 10.50000 -1.20000 AFIX 0 C32 1 0.543326 0.446561 0.450175 10.50000 0.06124 0.04451 = 0.12271 -0.03149 0.00668 0.00475 AFIX 3 H32A 2 0.490965 0.377871 0.496446 10.50000 -1.20000 H32B 2 0.635015 0.431941 0.460276 10.50000 -1.20000 AFIX 0 C33 1 0.385979 0.593131 0.631776 10.50000 0.12459 0.09120 = 0.08310 -0.04328 -0.03792 -0.03160 AFIX 3 H33A 2 0.369869 0.569721 0.712206 10.50000 -1.50000 H33B 2 0.449558 0.655631 0.585686 10.50000 -1.50000 H33C 2 0.297499 0.614721 0.616136 10.50000 -1.50000 AFIX 0 C34 1 0.566283 0.483622 0.331088 10.50000 0.10232 0.12018 = 0.10205 -0.08217 -0.00095 -0.02384 AFIX 3 H34A 2 0.615204 0.426852 0.308338 10.50000 -1.50000 H34B 2 0.474774 0.496882 0.320818 10.50000 -1.50000 H34C 2 0.620284 0.551502 0.284278 10.50000 -1.50000 PART 0 AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM wl152_0m in P-1 REM R1 = 0.0384 for 5131 Fo > 4sig(Fo) and 0.0671 for all 7092 data REM 352 parameters refined using 0 restraints END WGHT 0.0357 0.3940 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 0.311, deepest hole -0.254, 1-sigma level 0.050 Q1 1 0.8243 0.9222 0.7003 11.00000 0.05 0.31 Q2 1 0.5799 0.8488 0.8413 11.00000 0.05 0.30 Q3 1 0.9984 1.0583 0.4328 11.00000 0.05 0.30 Q4 1 1.1226 0.9805 0.4857 11.00000 0.05 0.29 Q5 1 0.8402 0.6245 0.6745 11.00000 0.05 0.25 Q6 1 0.5966 0.9278 0.3573 11.00000 0.05 0.25 Q7 1 0.8853 0.8772 0.6728 11.00000 0.05 0.24 Q8 1 0.7813 1.0252 0.9304 11.00000 0.05 0.24 Q9 1 0.8942 0.6258 0.7406 11.00000 0.05 0.23 Q10 1 0.7228 0.7632 0.5298 11.00000 0.05 0.23 ; _shelx_res_checksum 30632 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.87162(3) 0.93541(2) 0.59732(2) 0.02586(9) Uani 1 1 d . . . . . Cl1 Cl 1.11208(5) 0.89122(4) 0.56128(4) 0.03415(13) Uani 1 1 d . . . . . N1 N 0.74700(15) 0.81899(12) 0.62866(12) 0.0250(3) Uani 1 1 d . . . . . C1 C 0.63274(18) 0.79928(15) 0.72282(15) 0.0248(4) Uani 1 1 d . . . . . N2 N 0.74935(15) 0.91322(12) 0.75402(12) 0.0250(3) Uani 1 1 d . . . . . C2 C 0.5173(2) 0.72941(17) 0.76040(17) 0.0338(5) Uani 1 1 d . . . . . H2A H 0.516189 0.692933 0.716669 0.041 Uiso 1 1 calc R U . . . C3 C 0.4080(2) 0.71442(18) 0.85912(19) 0.0424(5) Uani 1 1 d . . . . . H3A H 0.331015 0.667694 0.883361 0.051 Uiso 1 1 calc R U . . . C4 C 0.4077(2) 0.76713(18) 0.92549(18) 0.0414(5) Uani 1 1 d . . . . . H4A H 0.329913 0.755888 0.993572 0.050 Uiso 1 1 calc R U . . . C5 C 0.51658(19) 0.83401(17) 0.89415(16) 0.0322(4) Uani 1 1 d . . . . . H5A H 0.514543 0.868306 0.940661 0.039 Uiso 1 1 calc R U . . . C6 C 0.63317(18) 0.85262(15) 0.79216(15) 0.0245(4) Uani 1 1 d . . . . . C7 C 0.77023(18) 0.75183(16) 0.56903(16) 0.0283(4) Uani 1 1 d . . . . . C8 C 0.8189(2) 0.64059(17) 0.61950(19) 0.0405(5) Uani 1 1 d . . . . . C9 C 0.8462(3) 0.5791(2) 0.5582(2) 0.0550(7) Uani 1 1 d . . . . . H9A H 0.879500 0.504263 0.590001 0.066 Uiso 1 1 calc R U . . . C10 C 0.8262(3) 0.6234(2) 0.4524(3) 0.0615(7) Uani 1 1 d . . . . . H10A H 0.844589 0.579030 0.412620 0.074 Uiso 1 1 calc R U . . . C11 C 0.7792(2) 0.7328(2) 0.4036(2) 0.0480(6) Uani 1 1 d . . . . . H11A H 0.766384 0.762835 0.330179 0.058 Uiso 1 1 calc R U . . . C12 C 0.75062(19) 0.79902(17) 0.46072(17) 0.0321(4) Uani 1 1 d . . . . . C13 C 0.8461(3) 0.58928(19) 0.7341(2) 0.0542(7) Uani 1 1 d . . . . . H13A H 0.806557 0.641923 0.769496 0.065 Uiso 1 1 calc R U . . . C14 C 1.0041(3) 0.5772(2) 0.7185(2) 0.0646(7) Uani 1 1 d . . . . . H14A H 1.017913 0.543736 0.794241 0.097 Uiso 1 1 calc R U . . . H14B H 1.047448 0.528917 0.680287 0.097 Uiso 1 1 calc R U . . . H14C H 1.048709 0.651033 0.670786 0.097 Uiso 1 1 calc R U . . . C15 C 0.7713(4) 0.4779(3) 0.8184(3) 0.1084(13) Uani 1 1 d . . . . . H15A H 0.792146 0.448148 0.891123 0.163 Uiso 1 1 calc R U . . . H15B H 0.668787 0.488819 0.833419 0.163 Uiso 1 1 calc R U . . . H15C H 0.804817 0.424958 0.785069 0.163 Uiso 1 1 calc R U . . . C16 C 0.6923(2) 0.91625(18) 0.40915(17) 0.0363(5) Uani 1 1 d . . . . . H16A H 0.701943 0.955836 0.451525 0.044 Uiso 1 1 calc R U . . . C17 C 0.7730(3) 0.9837(2) 0.2814(2) 0.0713(8) Uani 1 1 d . . . . . H17A H 0.730997 1.058558 0.252453 0.107 Uiso 1 1 calc R U . . . H17B H 0.872517 0.989995 0.271704 0.107 Uiso 1 1 calc R U . . . H17C H 0.767283 0.945772 0.237788 0.107 Uiso 1 1 calc R U . . . C18 C 0.5336(2) 0.9116(2) 0.4283(2) 0.0572(7) Uani 1 1 d . . . . . H18A H 0.496766 0.987864 0.394636 0.086 Uiso 1 1 calc R U . . . H18B H 0.520420 0.869725 0.391036 0.086 Uiso 1 1 calc R U . . . H18C H 0.482382 0.874396 0.511387 0.086 Uiso 1 1 calc R U . . . C19 C 0.77509(18) 0.94552(17) 0.83062(16) 0.0296(4) Uani 1 1 d . . . . . C20 C 0.8288(2) 0.86495(19) 0.91811(17) 0.0390(5) Uani 1 1 d . . . . . C21 C 0.8563(2) 0.8988(2) 0.98976(19) 0.0512(6) Uani 1 1 d . . . . . H21A H 0.891167 0.845518 1.050351 0.061 Uiso 1 1 calc R U . . . C22 C 0.8342(2) 1.0073(3) 0.9750(2) 0.0537(7) Uani 1 1 d . . . . . H22A H 0.853211 1.028160 1.025175 0.064 Uiso 1 1 calc R U . . . C23 C 0.7842(2) 1.0856(2) 0.88705(19) 0.0449(6) Uani 1 1 d . . . . . H23A H 0.770577 1.160726 0.876524 0.054 Uiso 1 1 calc R U . . . C24 C 0.75334(19) 1.05685(18) 0.81332(17) 0.0328(5) Uani 1 1 d . . . . . C25 C 0.8606(2) 0.7461(2) 0.9340(2) 0.0521(6) Uani 1 1 d . . . . . H25A H 0.836003 0.739749 0.873432 0.063 Uiso 1 1 calc R U . . . C26 C 1.0190(3) 0.7177(2) 0.9159(2) 0.0668(8) Uani 1 1 d . . . . . H26A H 1.035676 0.640281 0.926886 0.100 Uiso 1 1 calc R U . . . H26B H 1.074755 0.768359 0.837381 0.100 Uiso 1 1 calc R U . . . H26C H 1.047505 0.726323 0.972069 0.100 Uiso 1 1 calc R U . . . C27 C 0.7711(3) 0.6604(3) 1.0518(3) 0.0940(11) Uani 1 1 d . . . . . H27A H 0.795365 0.584930 1.058087 0.141 Uiso 1 1 calc R U . . . H27B H 0.790357 0.666381 1.113343 0.141 Uiso 1 1 calc R U . . . H27C H 0.670360 0.675106 1.059495 0.141 Uiso 1 1 calc R U . . . C28 C 0.6956(2) 1.14532(18) 0.72022(18) 0.0379(5) Uani 1 1 d . . . . . H28A H 0.686772 1.111058 0.672818 0.045 Uiso 1 1 calc R U . . . C29 C 0.7962(3) 1.2455(2) 0.6392(2) 0.0596(7) Uani 1 1 d . . . . . H29A H 0.755414 1.301106 0.580022 0.089 Uiso 1 1 calc R U . . . H29B H 0.809215 1.279297 0.683931 0.089 Uiso 1 1 calc R U . . . H29C H 0.888045 1.220154 0.601783 0.089 Uiso 1 1 calc R U . . . C30 C 0.5468(2) 1.1824(2) 0.7743(2) 0.0578(7) Uani 1 1 d . . . . . H30A H 0.510789 1.239787 0.712937 0.087 Uiso 1 1 calc R U . . . H30B H 0.483037 1.117932 0.820393 0.087 Uiso 1 1 calc R U . . . H30C H 0.551636 1.213294 0.824254 0.087 Uiso 1 1 calc R U . . . O1 O 0.4747(5) 0.5292(3) 0.4892(6) 0.0536(12) Uani 0.5 1 d . . P A -1 C31 C 0.4457(10) 0.4973(8) 0.6032(8) 0.081(3) Uani 0.5 1 d . . P A -1 H31A H 0.533674 0.474984 0.619696 0.098 Uiso 0.5 1 d R U P A -1 H31B H 0.382864 0.434414 0.649896 0.098 Uiso 0.5 1 d R U P A -1 C32 C 0.5433(9) 0.4466(8) 0.4502(12) 0.091(4) Uani 0.5 1 d . . P A -1 H32A H 0.490965 0.377871 0.496446 0.109 Uiso 0.5 1 d R U P A -1 H32B H 0.635015 0.431941 0.460276 0.109 Uiso 0.5 1 d R U P A -1 C33 C 0.3860(10) 0.5931(7) 0.6318(8) 0.092(3) Uani 0.5 1 d . . P A -1 H33A H 0.369869 0.569721 0.712206 0.138 Uiso 0.5 1 d R U P A -1 H33B H 0.449558 0.655631 0.585686 0.138 Uiso 0.5 1 d R U P A -1 H33C H 0.297499 0.614721 0.616136 0.138 Uiso 0.5 1 d R U P A -1 C34 C 0.5663(10) 0.4836(9) 0.3311(8) 0.101(3) Uani 0.5 1 d . . P A -1 H34A H 0.615204 0.426852 0.308338 0.151 Uiso 0.5 1 d R U P A -1 H34B H 0.474774 0.496882 0.320818 0.151 Uiso 0.5 1 d R U P A -1 H34C H 0.620284 0.551502 0.284278 0.151 Uiso 0.5 1 d R U P A -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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.02449(15) 0.02851(16) 0.02253(15) -0.01176(12) -0.00381(10) -0.00230(11) Cl1 0.0265(2) 0.0323(3) 0.0322(3) -0.0076(2) -0.0068(2) 0.0009(2) N1 0.0277(8) 0.0241(8) 0.0224(8) -0.0114(7) -0.0065(6) 0.0011(6) C1 0.0252(9) 0.0226(9) 0.0246(10) -0.0102(8) -0.0073(8) 0.0022(7) N2 0.0240(8) 0.0296(9) 0.0230(8) -0.0129(7) -0.0073(6) -0.0005(6) C2 0.0339(11) 0.0329(11) 0.0364(12) -0.0191(10) -0.0059(9) -0.0050(9) C3 0.0334(11) 0.0438(13) 0.0462(14) -0.0219(11) -0.0001(10) -0.0133(10) C4 0.0338(11) 0.0485(14) 0.0324(12) -0.0194(11) 0.0062(9) -0.0105(10) C5 0.0314(10) 0.0375(11) 0.0257(10) -0.0152(9) -0.0039(8) -0.0035(9) C6 0.0238(9) 0.0263(10) 0.0209(9) -0.0092(8) -0.0071(7) 0.0019(7) C7 0.0262(10) 0.0282(10) 0.0307(11) -0.0170(9) -0.0033(8) -0.0015(8) C8 0.0413(12) 0.0324(12) 0.0446(13) -0.0207(10) -0.0078(10) 0.0047(9) C9 0.0599(15) 0.0371(13) 0.0728(19) -0.0357(13) -0.0163(13) 0.0115(11) C10 0.0637(17) 0.0662(18) 0.084(2) -0.0625(17) -0.0218(15) 0.0134(14) C11 0.0489(13) 0.0630(16) 0.0535(15) -0.0429(13) -0.0196(11) 0.0074(12) C12 0.0287(10) 0.0381(12) 0.0356(12) -0.0232(10) -0.0072(8) -0.0007(9) C13 0.0723(17) 0.0337(13) 0.0436(14) -0.0131(11) -0.0184(12) 0.0170(12) C14 0.081(2) 0.0583(17) 0.0661(19) -0.0330(15) -0.0360(15) 0.0140(15) C15 0.113(3) 0.075(2) 0.079(2) 0.0198(19) -0.035(2) -0.019(2) C16 0.0447(12) 0.0409(12) 0.0332(11) -0.0207(10) -0.0183(9) 0.0021(10) C17 0.097(2) 0.0647(19) 0.0352(15) -0.0157(14) -0.0114(14) -0.0028(16) C18 0.0559(15) 0.0587(16) 0.082(2) -0.0413(15) -0.0435(14) 0.0168(12) C19 0.0219(9) 0.0447(12) 0.0247(10) -0.0184(9) -0.0047(8) -0.0034(8) C20 0.0333(11) 0.0516(14) 0.0285(11) -0.0129(10) -0.0107(9) -0.0050(10) C21 0.0403(13) 0.083(2) 0.0294(12) -0.0178(12) -0.0179(10) -0.0054(12) C22 0.0472(14) 0.091(2) 0.0408(14) -0.0420(15) -0.0113(11) -0.0102(13) C23 0.0414(12) 0.0658(16) 0.0449(14) -0.0395(13) -0.0104(10) -0.0034(11) C24 0.0258(10) 0.0495(13) 0.0311(11) -0.0261(10) -0.0051(8) -0.0030(9) C25 0.0514(14) 0.0528(15) 0.0483(15) -0.0095(12) -0.0309(12) 0.0016(12) C26 0.0577(16) 0.0675(19) 0.0701(19) -0.0241(16) -0.0284(14) 0.0094(14) C27 0.069(2) 0.063(2) 0.094(3) 0.0063(18) -0.0210(18) -0.0055(16) C28 0.0408(12) 0.0426(13) 0.0442(13) -0.0302(11) -0.0163(10) 0.0056(10) C29 0.0706(17) 0.0529(16) 0.0560(17) -0.0215(13) -0.0204(13) -0.0095(13) C30 0.0493(14) 0.0695(18) 0.0672(18) -0.0444(15) -0.0217(13) 0.0193(13) O1 0.056(3) 0.043(4) 0.065(3) -0.028(3) -0.017(2) -0.002(2) C31 0.085(5) 0.058(6) 0.067(7) -0.005(5) -0.014(5) -0.012(4) C32 0.061(4) 0.045(5) 0.123(11) -0.031(6) 0.007(5) 0.005(4) C33 0.125(7) 0.091(6) 0.083(6) -0.043(5) -0.038(5) -0.032(5) C34 0.102(6) 0.120(8) 0.102(8) -0.082(7) -0.001(5) -0.024(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' O O 0.0106 0.0060 '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 82.36(6) . . ? N2 Fe1 Cl1 121.03(5) . 2_776 ? N1 Fe1 Cl1 119.93(5) . 2_776 ? N2 Fe1 Cl1 120.38(4) . . ? N1 Fe1 Cl1 115.90(5) . . ? Cl1 Fe1 Cl1 98.749(18) 2_776 . ? Fe1 Cl1 Fe1 81.252(18) 2_776 . ? C1 N1 C7 119.07(15) . . ? C1 N1 Fe1 112.56(12) . . ? C7 N1 Fe1 128.23(11) . . ? N1 C1 C2 125.70(17) . . ? N1 C1 C6 115.42(15) . . ? C2 C1 C6 118.84(16) . . ? C6 N2 C19 118.88(14) . . ? C6 N2 Fe1 112.35(11) . . ? C19 N2 Fe1 128.58(11) . . ? C3 C2 C1 120.22(19) . . ? C3 C2 H2A 119.9 . . ? C1 C2 H2A 119.9 . . ? C2 C3 C4 120.91(19) . . ? C2 C3 H3A 119.5 . . ? C4 C3 H3A 119.5 . . ? C5 C4 C3 121.32(18) . . ? C5 C4 H4A 119.3 . . ? C3 C4 H4A 119.3 . . ? C4 C5 C6 120.19(18) . . ? C4 C5 H5A 119.9 . . ? C6 C5 H5A 119.9 . . ? N2 C6 C5 126.04(17) . . ? N2 C6 C1 115.42(15) . . ? C5 C6 C1 118.51(16) . . ? C12 C7 C8 121.67(18) . . ? C12 C7 N1 119.64(17) . . ? C8 C7 N1 118.63(17) . . ? C9 C8 C7 117.6(2) . . ? C9 C8 C13 119.8(2) . . ? C7 C8 C13 122.63(19) . . ? C10 C9 C8 121.6(2) . . ? C10 C9 H9A 119.2 . . ? C8 C9 H9A 119.2 . . ? C9 C10 C11 120.2(2) . . ? C9 C10 H10A 119.9 . . ? C11 C10 H10A 119.9 . . ? C10 C11 C12 120.9(2) . . ? C10 C11 H11A 119.6 . . ? C12 C11 H11A 119.6 . . ? C11 C12 C7 118.03(19) . . ? C11 C12 C16 120.23(19) . . ? C7 C12 C16 121.65(17) . . ? C8 C13 C15 112.6(2) . . ? C8 C13 C14 111.6(2) . . ? C15 C13 C14 110.6(2) . . ? C8 C13 H13A 107.2 . . ? C15 C13 H13A 107.2 . . ? C14 C13 H13A 107.2 . . ? 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 112.85(19) . . ? C12 C16 C18 110.05(18) . . ? C17 C16 C18 110.8(2) . . ? C12 C16 H16A 107.6 . . ? C17 C16 H16A 107.6 . . ? C18 C16 H16A 107.6 . . ? 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 121.51(18) . . ? C24 C19 N2 119.86(17) . . ? C20 C19 N2 118.56(18) . . ? C21 C20 C19 117.6(2) . . ? C21 C20 C25 120.1(2) . . ? C19 C20 C25 122.32(19) . . ? C22 C21 C20 121.7(2) . . ? C22 C21 H21A 119.1 . . ? C20 C21 H21A 119.1 . . ? C21 C22 C23 119.8(2) . . ? C21 C22 H22A 120.1 . . ? C23 C22 H22A 120.1 . . ? C22 C23 C24 121.3(2) . . ? C22 C23 H23A 119.4 . . ? C24 C23 H23A 119.4 . . ? C23 C24 C19 118.1(2) . . ? C23 C24 C28 119.1(2) . . ? C19 C24 C28 122.78(17) . . ? C20 C25 C27 112.5(2) . . ? C20 C25 C26 111.7(2) . . ? C27 C25 C26 110.1(2) . . ? C20 C25 H25A 107.4 . . ? C27 C25 H25A 107.4 . . ? C26 C25 H25A 107.4 . . ? 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 111.72(18) . . ? C24 C28 C30 110.44(18) . . ? C29 C28 C30 111.29(19) . . ? C24 C28 H28A 107.7 . . ? C29 C28 H28A 107.7 . . ? C30 C28 H28A 107.7 . . ? 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 . . ? C31 O1 C32 115.7(5) . . ? O1 C31 C33 110.9(8) . . ? O1 C31 H31A 107.4 . . ? C33 C31 H31A 108.1 . . ? O1 C31 H31B 111.1 . . ? C33 C31 H31B 111.0 . . ? H31A C31 H31B 108.1 . . ? C34 C32 O1 112.9(9) . . ? C34 C32 H32A 110.9 . . ? O1 C32 H32A 110.5 . . ? C34 C32 H32B 106.8 . . ? O1 C32 H32B 107.6 . . ? H32A C32 H32B 107.9 . . ? C31 C33 H33A 109.6 . . ? C31 C33 H33B 110.9 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 107.9 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 110.0 . . ? C32 C34 H34B 107.1 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 111.3 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 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 1.9773(15) . ? Fe1 N1 1.9798(15) . ? Fe1 Cl1 2.3183(5) 2_776 ? Fe1 Cl1 2.3282(5) . ? N1 C1 1.341(2) . ? N1 C7 1.437(2) . ? C1 C2 1.418(2) . ? C1 C6 1.452(2) . ? N2 C6 1.346(2) . ? N2 C19 1.436(2) . ? C2 C3 1.364(3) . ? C2 H2A 0.9500 . ? C3 C4 1.405(3) . ? C3 H3A 0.9500 . ? C4 C5 1.362(3) . ? C4 H4A 0.9500 . ? C5 C6 1.420(2) . ? C5 H5A 0.9500 . ? C7 C12 1.401(3) . ? C7 C8 1.414(3) . ? C8 C9 1.384(3) . ? C8 C13 1.512(3) . ? C9 C10 1.373(4) . ? C9 H9A 0.9500 . ? C10 C11 1.386(4) . ? C10 H10A 0.9500 . ? C11 C12 1.391(3) . ? C11 H11A 0.9500 . ? C12 C16 1.513(3) . ? C13 C15 1.520(4) . ? C13 C14 1.523(3) . ? C13 H13A 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(3) . ? C16 C18 1.537(3) . ? C16 H16A 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 1.402(3) . ? C19 C20 1.405(3) . ? C20 C21 1.395(3) . ? C20 C25 1.511(3) . ? C21 C22 1.375(4) . ? C21 H21A 0.9500 . ? C22 C23 1.379(3) . ? C22 H22A 0.9500 . ? C23 C24 1.394(3) . ? C23 H23A 0.9500 . ? C24 C28 1.510(3) . ? C25 C27 1.530(4) . ? C25 C26 1.537(3) . ? C25 H25A 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 1.536(3) . ? C28 C30 1.536(3) . ? C28 H28A 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 . ? O1 C31 1.354(13) . ? O1 C32 1.436(12) . ? C31 C33 1.500(13) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C32 C34 1.417(16) . ? C32 H32A 0.9601 . ? C32 H32B 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9601 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9599 . ? C34 H34C 0.9600 . ? 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 -11.0(3) . . . . ? Fe1 N1 C1 C2 173.13(15) . . . . ? C7 N1 C1 C6 166.91(15) . . . . ? Fe1 N1 C1 C6 -8.99(19) . . . . ? N1 C1 C2 C3 178.83(19) . . . . ? C6 C1 C2 C3 1.0(3) . . . . ? C1 C2 C3 C4 -0.3(3) . . . . ? C2 C3 C4 C5 -0.5(3) . . . . ? C3 C4 C5 C6 0.5(3) . . . . ? C19 N2 C6 C5 12.9(3) . . . . ? Fe1 N2 C6 C5 -171.62(15) . . . . ? C19 N2 C6 C1 -164.81(16) . . . . ? Fe1 N2 C6 C1 10.69(19) . . . . ? C4 C5 C6 N2 -177.40(19) . . . . ? C4 C5 C6 C1 0.2(3) . . . . ? N1 C1 C6 N2 -1.2(2) . . . . ? C2 C1 C6 N2 176.89(16) . . . . ? N1 C1 C6 C5 -179.02(16) . . . . ? C2 C1 C6 C5 -1.0(3) . . . . ? C1 N1 C7 C12 108.4(2) . . . . ? Fe1 N1 C7 C12 -76.4(2) . . . . ? C1 N1 C7 C8 -74.5(2) . . . . ? Fe1 N1 C7 C8 100.72(19) . . . . ? C12 C7 C8 C9 -0.3(3) . . . . ? N1 C7 C8 C9 -177.38(18) . . . . ? C12 C7 C8 C13 177.66(19) . . . . ? N1 C7 C8 C13 0.6(3) . . . . ? C7 C8 C9 C10 -0.4(4) . . . . ? C13 C8 C9 C10 -178.4(2) . . . . ? C8 C9 C10 C11 0.8(4) . . . . ? C9 C10 C11 C12 -0.5(4) . . . . ? C10 C11 C12 C7 -0.2(3) . . . . ? C10 C11 C12 C16 -176.9(2) . . . . ? C8 C7 C12 C11 0.6(3) . . . . ? N1 C7 C12 C11 177.63(17) . . . . ? C8 C7 C12 C16 177.21(18) . . . . ? N1 C7 C12 C16 -5.8(3) . . . . ? C9 C8 C13 C15 -53.9(3) . . . . ? C7 C8 C13 C15 128.1(3) . . . . ? C9 C8 C13 C14 71.2(3) . . . . ? C7 C8 C13 C14 -106.8(2) . . . . ? C11 C12 C16 C17 -47.5(3) . . . . ? C7 C12 C16 C17 136.0(2) . . . . ? C11 C12 C16 C18 76.8(2) . . . . ? C7 C12 C16 C18 -99.7(2) . . . . ? C6 N2 C19 C24 -106.3(2) . . . . ? Fe1 N2 C19 C24 79.0(2) . . . . ? C6 N2 C19 C20 76.9(2) . . . . ? Fe1 N2 C19 C20 -97.77(19) . . . . ? C24 C19 C20 C21 1.8(3) . . . . ? N2 C19 C20 C21 178.49(17) . . . . ? C24 C19 C20 C25 -176.57(19) . . . . ? N2 C19 C20 C25 0.1(3) . . . . ? C19 C20 C21 C22 -1.0(3) . . . . ? C25 C20 C21 C22 177.3(2) . . . . ? C20 C21 C22 C23 -0.3(3) . . . . ? C21 C22 C23 C24 1.0(3) . . . . ? C22 C23 C24 C19 -0.3(3) . . . . ? C22 C23 C24 C28 178.5(2) . . . . ? C20 C19 C24 C23 -1.1(3) . . . . ? N2 C19 C24 C23 -177.81(16) . . . . ? C20 C19 C24 C28 -179.91(18) . . . . ? N2 C19 C24 C28 3.4(3) . . . . ? C21 C20 C25 C27 63.4(3) . . . . ? C19 C20 C25 C27 -118.3(2) . . . . ? C21 C20 C25 C26 -61.0(3) . . . . ? C19 C20 C25 C26 117.3(2) . . . . ? C23 C24 C28 C29 57.8(2) . . . . ? C19 C24 C28 C29 -123.5(2) . . . . ? C23 C24 C28 C30 -66.7(2) . . . . ? C19 C24 C28 C30 112.1(2) . . . . ? C32 O1 C31 C33 175.1(6) . . . . ? C31 O1 C32 C34 177.9(7) . . . . ?