data_jmd16 _vrf_PLAT410_jmd16 ; PROBLEM: Short Intra H...H Contact H40A .. H41A .. 1.63 Ang. RESPONSE: The diallyl tert-butyl amine group has been modeled in two orientations. Hydrogen atoms have been located using a riding model. As such, their positions are not optimized and this leads to a spurious close contact between two disordered positions on the amine ligand. ; # end validation reply form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H60 Fe N6' _chemical_formula_sum 'C45 H60 Fe N6' _chemical_formula_weight 740.84 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' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.1532(10) _cell_length_b 14.2472(14) _cell_length_c 13.6316(14) _cell_angle_alpha 90.00 _cell_angle_beta 95.4920(10) _cell_angle_gamma 90.00 _cell_volume 1962.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9990 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 27.44 _exptl_crystal_description Shard _exptl_crystal_colour Brown _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.253 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 796 _exptl_absorpt_coefficient_mu 0.424 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.9314 _exptl_absorpt_correction_T_max 0.9791 _exptl_absorpt_process_details sadabs _exptl_special_details ; Collected, solved and refined by Dr. Zoe R. Turner PLAT230_ALERT_2_B Hirshfeld Test Diff for C42 -- C44A .. 8.00 su PLAT230_ALERT_2_B Hirshfeld Test Diff for C42 -- C43A .. 11.25 su PLAT230_ALERT_2_B Hirshfeld Test Diff for C42 -- C45 .. 12.50 su PLAT230_ALERT_2_C Hirshfeld Test Diff for C42 -- C44 .. 7.00 su The tert butyl group of C42 is disorded and has been modelled as best as possible as a two component disorder. The above alerts are a result of this disorder. PLAT411_ALERT_2_C Short Inter H...H Contact H2 .. H41B .. 2.10 Ang. This is a result of crystal packing. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method 'PHI AND OMEGA SCANS' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22273 _diffrn_reflns_av_R_equivalents 0.0271 _diffrn_reflns_av_sigmaI/netI 0.0457 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 27.51 _reflns_number_total 8668 _reflns_number_gt 7679 _reflns_threshold_expression >2\s(I) _computing_data_collection 'BRUKER, APEX II SOFTWARE SUITE' _computing_cell_refinement 'BRUKER, APEX II SOFTWARE SUITE' _computing_data_reduction 'BRUKER, APEX II SOFTWARE SUITE' _computing_structure_solution 'SIR-92 (Giacovazzo, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0429P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.004(10) _refine_ls_number_reflns 8668 _refine_ls_number_parameters 559 _refine_ls_number_restraints 37 _refine_ls_R_factor_all 0.0428 _refine_ls_R_factor_gt 0.0345 _refine_ls_wR_factor_ref 0.0806 _refine_ls_wR_factor_gt 0.0774 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6690(2) 1.03048(14) 0.05946(14) 0.0243(4) Uani 1 1 d . . . C2 C 0.5502(2) 1.14424(16) -0.03188(16) 0.0319(5) Uani 1 1 d . . . C3 C 0.6227(2) 1.10205(16) -0.09398(16) 0.0327(5) Uani 1 1 d . . . C4 C 0.7798(2) 0.96677(14) -0.07164(15) 0.0279(5) Uani 1 1 d . B . C5 C 0.8132(2) 0.95327(16) -0.16715(15) 0.0363(6) Uani 1 1 d . . . H5 H 0.7766 0.9917 -0.2198 0.044 Uiso 1 1 calc R . . C6 C 0.9015(2) 0.88203(18) -0.18319(16) 0.0401(6) Uani 1 1 d . . . H6 H 0.9261 0.8711 -0.2477 0.048 Uiso 1 1 calc R . . C7 C 0.9544(2) 0.82655(16) -0.10521(16) 0.0348(5) Uani 1 1 d . . . H7 H 1.0152 0.7776 -0.1150 0.042 Uiso 1 1 calc R . . C8 C 0.9150(2) 0.84533(15) -0.01328(15) 0.0284(4) Uani 1 1 d . B . C9 C 1.0413(2) 0.72310(15) 0.08747(18) 0.0335(5) Uani 1 1 d . B . C10 C 1.0483(2) 0.70386(16) 0.18378(18) 0.0351(5) Uani 1 1 d . B . C11 C 0.9049(2) 0.83003(16) 0.15992(16) 0.0275(5) Uani 1 1 d . B . C12 C 0.4958(2) 1.12895(15) 0.13913(15) 0.0262(4) Uani 1 1 d . . . C13 C 0.5367(2) 1.20429(14) 0.20104(15) 0.0304(5) Uani 1 1 d . . . C14 C 0.4543(2) 1.22977(16) 0.27286(17) 0.0386(5) Uani 1 1 d . . . H14 H 0.4801 1.2795 0.3170 0.046 Uiso 1 1 calc R . . C15 C 0.3361(2) 1.18411(18) 0.28107(18) 0.0417(6) Uani 1 1 d . . . H15 H 0.2827 1.2015 0.3317 0.050 Uiso 1 1 calc R . . C16 C 0.2949(2) 1.11324(17) 0.21607(17) 0.0378(5) Uani 1 1 d . . . H16 H 0.2122 1.0834 0.2214 0.045 Uiso 1 1 calc R . . C17 C 0.3729(2) 1.08491(15) 0.14290(15) 0.0300(5) Uani 1 1 d . . . C18 C 0.6569(2) 1.26255(15) 0.18519(16) 0.0361(5) Uani 1 1 d . . . H18 H 0.7142 1.2254 0.1437 0.043 Uiso 1 1 calc R . . C19 C 0.6121(3) 1.35190(19) 0.1280(2) 0.0578(8) Uani 1 1 d . . . H19A H 0.5574 1.3346 0.0676 0.087 Uiso 1 1 calc R . . H19B H 0.6900 1.3867 0.1109 0.087 Uiso 1 1 calc R . . H19C H 0.5605 1.3913 0.1691 0.087 Uiso 1 1 calc R . . C20 C 0.7398(3) 1.28960(18) 0.28054(18) 0.0445(6) Uani 1 1 d . . . H20A H 0.6887 1.3320 0.3190 0.067 Uiso 1 1 calc R . . H20B H 0.8208 1.3212 0.2647 0.067 Uiso 1 1 calc R . . H20C H 0.7630 1.2329 0.3191 0.067 Uiso 1 1 calc R . . C21 C 0.3186(2) 1.01500(16) 0.06566(16) 0.0327(5) Uani 1 1 d . . . H21 H 0.3927 0.9954 0.0268 0.039 Uiso 1 1 calc R . . C22 C 0.2133(2) 1.06278(19) -0.00464(18) 0.0424(6) Uani 1 1 d . . . H22A H 0.1413 1.0850 0.0324 0.064 Uiso 1 1 calc R . . H22B H 0.1783 1.0178 -0.0550 0.064 Uiso 1 1 calc R . . H22C H 0.2527 1.1162 -0.0365 0.064 Uiso 1 1 calc R . . C23 C 0.2619(2) 0.9273(2) 0.10916(17) 0.0427(6) Uani 1 1 d . . . H23A H 0.3281 0.8997 0.1578 0.064 Uiso 1 1 calc R . . H23B H 0.2384 0.8817 0.0565 0.064 Uiso 1 1 calc R . . H23C H 0.1828 0.9438 0.1412 0.064 Uiso 1 1 calc R . . C24 C 0.9580(2) 0.75959(14) 0.33317(15) 0.0279(4) Uani 1 1 d . B . C25 C 1.0517(2) 0.80738(15) 0.39707(16) 0.0311(5) Uani 1 1 d . . . C26 C 1.0472(2) 0.79249(18) 0.49744(17) 0.0417(6) Uani 1 1 d . . . H26 H 1.1083 0.8246 0.5428 0.050 Uiso 1 1 calc R . . C27 C 0.9570(3) 0.7328(2) 0.53282(18) 0.0477(7) Uani 1 1 d . . . H27 H 0.9557 0.7247 0.6019 0.057 Uiso 1 1 calc R . . C28 C 0.8685(2) 0.68465(18) 0.46876(18) 0.0404(6) Uani 1 1 d . . . H28 H 0.8072 0.6429 0.4941 0.049 Uiso 1 1 calc R . . C29 C 0.8676(2) 0.69635(15) 0.36717(16) 0.0310(5) Uani 1 1 d . . . C30 C 1.1590(2) 0.86705(17) 0.35892(18) 0.0380(5) Uani 1 1 d . . . H30 H 1.1288 0.8856 0.2897 0.046 Uiso 1 1 calc R . . C31 C 1.2861(2) 0.8095(2) 0.3567(2) 0.0511(7) Uani 1 1 d . . . H31A H 1.3215 0.7944 0.4243 0.077 Uiso 1 1 calc R . . H31B H 1.3516 0.8460 0.3246 0.077 Uiso 1 1 calc R . . H31C H 1.2665 0.7512 0.3199 0.077 Uiso 1 1 calc R . . C32 C 1.1868(3) 0.95683(17) 0.4187(2) 0.0494(7) Uani 1 1 d . . . H32A H 1.1036 0.9904 0.4244 0.074 Uiso 1 1 calc R . . H32B H 1.2471 0.9970 0.3855 0.074 Uiso 1 1 calc R . . H32C H 1.2275 0.9407 0.4847 0.074 Uiso 1 1 calc R . . C33 C 0.7769(2) 0.63706(17) 0.29762(17) 0.0407(6) Uani 1 1 d . . . H33 H 0.7729 0.6668 0.2309 0.049 Uiso 1 1 calc R . . C34 C 0.8368(3) 0.53893(18) 0.2894(2) 0.0567(8) Uani 1 1 d . . . H34A H 0.9246 0.5443 0.2656 0.085 Uiso 1 1 calc R . . H34B H 0.7793 0.5010 0.2431 0.085 Uiso 1 1 calc R . . H34C H 0.8449 0.5088 0.3544 0.085 Uiso 1 1 calc R . . C35 C 0.6366(3) 0.6315(2) 0.3268(2) 0.0571(8) Uani 1 1 d . . . H35A H 0.6365 0.5978 0.3894 0.086 Uiso 1 1 calc R . . H35B H 0.5807 0.5981 0.2756 0.086 Uiso 1 1 calc R . . H35C H 0.6020 0.6951 0.3341 0.086 Uiso 1 1 calc R . . C36 C 0.9131(2) 1.03893(16) 0.18584(17) 0.0294(5) Uani 1 1 d . . . H36A H 1.0066 1.0271 0.1748 0.035 Uiso 1 1 calc R A 1 H36B H 0.8854 1.1047 0.1724 0.035 Uiso 1 1 calc R A 1 C37 C 0.8718(5) 1.0004(3) 0.2650(3) 0.0248(10) Uani 0.479(4) 1 d P B 1 H37 H 0.9403 0.9590 0.3004 0.030 Uiso 0.479(4) 1 calc PR B 1 C38 C 0.7885(6) 1.0482(4) 0.3332(4) 0.0267(12) Uani 0.479(4) 1 d P B 1 H38A H 0.7300 1.0936 0.2952 0.032 Uiso 0.479(4) 1 calc PR B 1 H38B H 0.8466 1.0842 0.3821 0.032 Uiso 0.479(4) 1 calc PR B 1 C39 C 0.6144(5) 0.9387(5) 0.3205(4) 0.0279(11) Uani 0.479(4) 1 d P B 1 H39A H 0.5599 0.9874 0.2841 0.033 Uiso 0.479(4) 1 calc PR B 1 H39B H 0.5545 0.8993 0.3563 0.033 Uiso 0.479(4) 1 calc PR B 1 C40 C 0.6777(5) 0.8779(4) 0.2470(3) 0.0262(10) Uani 0.479(4) 1 d P B 1 H40 H 0.7294 0.8254 0.2808 0.031 Uiso 0.479(4) 1 calc PR B 1 C37A C 0.8056(5) 1.0384(3) 0.2489(3) 0.0221(9) Uani 0.521(4) 1 d P B 2 H37A H 0.7452 1.0934 0.2362 0.027 Uiso 0.521(4) 1 calc PR B 2 C38A C 0.8187(5) 1.0099(4) 0.3554(4) 0.0249(10) Uani 0.521(4) 1 d P B 2 H38C H 0.8837 0.9581 0.3648 0.030 Uiso 0.521(4) 1 calc PR B 2 H38D H 0.8538 1.0637 0.3958 0.030 Uiso 0.521(4) 1 calc PR B 2 C39A C 0.6474(5) 0.8983(4) 0.3348(3) 0.0241(10) Uani 0.521(4) 1 d P B 2 H39C H 0.5648 0.8798 0.3629 0.029 Uiso 0.521(4) 1 calc PR B 2 H39D H 0.7107 0.8455 0.3451 0.029 Uiso 0.521(4) 1 calc PR B 2 C40A C 0.6176(5) 0.9151(3) 0.2257(3) 0.0221(10) Uani 0.521(4) 1 d P B 2 H40A H 0.5454 0.9623 0.2113 0.027 Uiso 0.521(4) 1 calc PR B 2 C41 C 0.6179(2) 0.84963(15) 0.15382(15) 0.0287(5) Uani 1 1 d . . . H41A H 0.5291 0.8757 0.1334 0.034 Uiso 1 1 calc R B 1 H41B H 0.6273 0.7826 0.1365 0.034 Uiso 1 1 calc R B 1 C42 C 0.6800(3) 0.9985(2) 0.49024(18) 0.0528(8) Uani 1 1 d D . . N1 N 0.57615(17) 1.10277(12) 0.06120(12) 0.0253(4) Uani 1 1 d . . . N2 N 0.69318(17) 1.03263(12) -0.04037(12) 0.0268(4) Uani 1 1 d . . . N3 N 0.82866(17) 0.91392(11) 0.00625(12) 0.0266(4) Uani 1 1 d . . . N4 N 0.95585(17) 0.79855(12) 0.07358(12) 0.0287(4) Uani 1 1 d . . . N5 N 0.96748(17) 0.76690(12) 0.22801(12) 0.0284(4) Uani 1 1 d . . . N6 N 0.7037(2) 0.98193(13) 0.38775(13) 0.0353(5) Uani 1 1 d . B . Fe1 Fe 0.77835(3) 0.93592(2) 0.135037(18) 0.02491(8) Uani 1 1 d . B . C43 C 0.5415(6) 0.9571(6) 0.5152(4) 0.057(2) Uani 0.521(4) 1 d PDU B 1 H43A H 0.5280 0.9716 0.5838 0.086 Uiso 0.521(4) 1 calc PR B 1 H43B H 0.5410 0.8889 0.5058 0.086 Uiso 0.521(4) 1 calc PR B 1 H43C H 0.4703 0.9854 0.4713 0.086 Uiso 0.521(4) 1 calc PR B 1 C44 C 0.7051(6) 1.0843(4) 0.5342(4) 0.0471(15) Uani 0.479(4) 1 d PDU B 1 H44A H 0.6569 1.1332 0.4951 0.071 Uiso 0.479(4) 1 calc PR B 1 H44B H 0.8002 1.0974 0.5381 0.071 Uiso 0.479(4) 1 calc PR B 1 H44C H 0.6762 1.0834 0.6008 0.071 Uiso 0.479(4) 1 calc PR B 1 C45 C 0.7759(6) 0.9168(4) 0.5498(3) 0.0540(19) Uani 0.479(4) 1 d PDU B 1 H45A H 0.8682 0.9269 0.5369 0.081 Uiso 0.479(4) 1 calc PR B 1 H45B H 0.7473 0.8543 0.5264 0.081 Uiso 0.479(4) 1 calc PR B 1 H45C H 0.7683 0.9215 0.6207 0.081 Uiso 0.479(4) 1 calc PR B 1 C43A C 0.6094(7) 0.9306(5) 0.5362(4) 0.0467(16) Uani 0.479(4) 1 d PDU B 2 H43D H 0.6562 0.8704 0.5355 0.070 Uiso 0.479(4) 1 calc PR B 2 H43E H 0.5211 0.9240 0.5010 0.070 Uiso 0.479(4) 1 calc PR B 2 H43F H 0.6012 0.9493 0.6045 0.070 Uiso 0.479(4) 1 calc PR B 2 C44A C 0.5858(5) 1.0961(4) 0.4753(4) 0.0503(14) Uani 0.521(4) 1 d PDU B 2 H44D H 0.5637 1.1183 0.5397 0.075 Uiso 0.521(4) 1 calc PR B 2 H44E H 0.5043 1.0815 0.4337 0.075 Uiso 0.521(4) 1 calc PR B 2 H44F H 0.6349 1.1451 0.4438 0.075 Uiso 0.521(4) 1 calc PR B 2 C45A C 0.8017(6) 1.0383(4) 0.5519(3) 0.0494(15) Uani 0.521(4) 1 d PDU B 2 H45D H 0.8361 1.0922 0.5176 0.074 Uiso 0.521(4) 1 calc PR B 2 H45E H 0.8702 0.9898 0.5612 0.074 Uiso 0.521(4) 1 calc PR B 2 H45F H 0.7766 1.0585 0.6163 0.074 Uiso 0.521(4) 1 calc PR B 2 H2 H 0.486(3) 1.189(2) -0.044(2) 0.059 Uiso 1 1 d . . . H3 H 0.638(3) 1.114(2) -0.164(2) 0.059 Uiso 1 1 d . . . H9 H 1.083(3) 0.698(2) 0.035(2) 0.059 Uiso 1 1 d . . . H10 H 1.095(3) 0.659(2) 0.220(2) 0.059 Uiso 1 1 d . . . 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 C1 0.0273(10) 0.0233(10) 0.0218(9) 0.0011(8) -0.0008(8) -0.0043(8) C2 0.0336(12) 0.0300(12) 0.0303(11) 0.0092(9) -0.0063(9) -0.0003(10) C3 0.0368(12) 0.0367(12) 0.0232(11) 0.0074(9) -0.0038(9) -0.0050(10) C4 0.0308(11) 0.0299(11) 0.0228(10) -0.0001(8) 0.0012(8) -0.0036(8) C5 0.0486(13) 0.0390(15) 0.0211(9) 0.0015(9) 0.0030(9) -0.0036(11) C6 0.0529(15) 0.0432(14) 0.0254(11) -0.0049(10) 0.0094(10) -0.0054(12) C7 0.0389(13) 0.0328(12) 0.0337(12) -0.0058(10) 0.0079(10) -0.0008(10) C8 0.0294(11) 0.0273(11) 0.0283(10) -0.0039(9) 0.0015(8) -0.0028(9) C9 0.0339(12) 0.0257(11) 0.0406(13) -0.0044(10) 0.0013(10) -0.0003(9) C10 0.0377(13) 0.0271(11) 0.0393(13) -0.0014(10) -0.0023(10) 0.0076(10) C11 0.0266(11) 0.0267(11) 0.0281(11) 0.0002(9) -0.0035(8) -0.0061(9) C12 0.0273(11) 0.0247(10) 0.0255(10) 0.0029(8) -0.0032(8) 0.0056(8) C13 0.0384(12) 0.0235(10) 0.0273(11) 0.0041(8) -0.0068(9) 0.0052(9) C14 0.0510(15) 0.0302(12) 0.0330(12) -0.0076(10) -0.0039(10) 0.0074(11) C15 0.0418(14) 0.0501(15) 0.0339(12) -0.0047(11) 0.0064(10) 0.0131(12) C16 0.0288(12) 0.0461(14) 0.0383(13) 0.0030(11) 0.0027(10) 0.0024(10) C17 0.0289(11) 0.0312(11) 0.0288(11) 0.0011(9) -0.0023(9) 0.0055(9) C18 0.0491(14) 0.0274(11) 0.0301(11) -0.0005(9) -0.0052(10) -0.0049(10) C19 0.084(2) 0.0360(14) 0.0481(16) 0.0156(12) -0.0207(14) -0.0203(14) C20 0.0542(16) 0.0361(13) 0.0401(13) 0.0023(11) -0.0121(11) -0.0079(12) C21 0.0283(11) 0.0359(12) 0.0336(12) -0.0038(10) 0.0020(9) -0.0022(9) C22 0.0376(13) 0.0508(15) 0.0369(13) -0.0029(11) -0.0055(10) -0.0011(11) C23 0.0336(11) 0.0474(15) 0.0473(13) 0.0001(14) 0.0041(9) -0.0064(13) C24 0.0316(11) 0.0240(10) 0.0270(10) 0.0025(8) -0.0033(9) 0.0069(9) C25 0.0303(11) 0.0275(11) 0.0340(11) 0.0006(9) -0.0049(9) 0.0039(9) C26 0.0443(14) 0.0476(14) 0.0307(12) -0.0031(11) -0.0095(10) -0.0032(12) C27 0.0553(16) 0.0621(18) 0.0251(12) -0.0013(11) 0.0007(11) -0.0120(14) C28 0.0421(14) 0.0431(14) 0.0364(13) 0.0036(11) 0.0055(11) -0.0052(11) C29 0.0358(12) 0.0255(11) 0.0302(11) 0.0002(9) -0.0049(9) 0.0031(9) C30 0.0335(12) 0.0395(13) 0.0391(13) 0.0058(11) -0.0063(10) -0.0027(10) C31 0.0319(13) 0.0611(18) 0.0600(17) 0.0025(14) 0.0018(12) -0.0063(12) C32 0.0442(14) 0.0418(17) 0.0585(16) 0.0041(12) -0.0147(12) -0.0117(11) C33 0.0524(15) 0.0324(12) 0.0344(12) 0.0038(10) -0.0110(11) -0.0113(11) C34 0.090(2) 0.0294(13) 0.0483(16) -0.0045(12) -0.0060(15) -0.0070(14) C35 0.0516(17) 0.0592(18) 0.0572(17) 0.0127(15) -0.0123(13) -0.0237(14) C36 0.0263(11) 0.0248(11) 0.0365(13) -0.0077(10) 0.0004(9) -0.0033(9) C37 0.025(2) 0.023(2) 0.026(2) -0.0052(18) -0.0043(19) -0.005(2) C38 0.032(3) 0.023(3) 0.024(3) 0.007(2) -0.006(2) -0.006(2) C39 0.021(3) 0.031(3) 0.029(2) 0.009(3) -0.0064(18) 0.002(3) C40 0.022(3) 0.022(2) 0.034(3) 0.0066(19) -0.003(2) -0.009(2) C37A 0.025(2) 0.020(2) 0.021(2) 0.0001(16) -0.0034(16) -0.0001(18) C38A 0.030(3) 0.027(3) 0.016(2) -0.002(2) -0.0054(18) -0.003(2) C39A 0.022(3) 0.030(3) 0.020(2) 0.005(2) -0.0021(18) 0.004(2) C40A 0.0181(19) 0.026(3) 0.0220(19) 0.0070(16) -0.0021(14) -0.0023(17) C41 0.0272(11) 0.0287(11) 0.0290(11) 0.0004(9) -0.0033(8) -0.0052(9) C42 0.0372(14) 0.092(2) 0.0293(13) -0.0173(14) 0.0040(11) -0.0029(14) N1 0.0274(9) 0.0261(9) 0.0214(8) 0.0023(7) -0.0025(7) -0.0013(7) N2 0.0316(9) 0.0292(9) 0.0191(8) 0.0026(7) -0.0007(7) -0.0022(7) N3 0.0321(9) 0.0275(11) 0.0204(8) -0.0014(7) 0.0022(7) -0.0044(7) N4 0.0318(10) 0.0235(9) 0.0299(9) -0.0028(7) -0.0010(7) -0.0022(7) N5 0.0324(10) 0.0236(9) 0.0281(9) -0.0014(7) -0.0028(7) 0.0014(8) N6 0.0549(13) 0.0299(10) 0.0213(9) -0.0019(8) 0.0044(8) -0.0043(9) Fe1 0.03298(15) 0.02327(13) 0.01820(12) -0.00096(14) 0.00096(10) -0.00571(15) C43 0.069(4) 0.078(6) 0.026(3) -0.003(3) 0.017(3) 0.004(4) C44 0.067(4) 0.046(3) 0.029(3) -0.008(2) 0.008(3) 0.000(3) C45 0.075(4) 0.070(5) 0.017(2) 0.008(2) 0.003(2) 0.041(3) C43A 0.067(4) 0.047(4) 0.027(3) 0.002(3) 0.009(3) -0.023(4) C44A 0.052(3) 0.058(3) 0.042(3) -0.008(2) 0.011(2) 0.003(3) C45A 0.059(3) 0.065(4) 0.024(2) 0.000(2) 0.002(2) -0.014(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; 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 C1 N1 1.398(3) . ? C1 N2 1.406(2) . ? C1 Fe1 1.972(2) . ? C2 C3 1.319(3) . ? C2 N1 1.402(3) . ? C2 H2 0.92(3) . ? C3 N2 1.387(3) . ? C3 H3 1.00(3) . ? C4 N3 1.356(3) . ? C4 N2 1.381(3) . ? C4 C5 1.390(3) . ? C5 C6 1.385(3) . ? C5 H5 0.9500 . ? C6 C7 1.390(3) . ? C6 H6 0.9500 . ? C7 C8 1.377(3) . ? C7 H7 0.9500 . ? C8 N3 1.356(3) . ? C8 N4 1.387(3) . ? C9 C10 1.336(3) . ? C9 N4 1.383(3) . ? C9 H9 0.94(3) . ? C10 N5 1.392(3) . ? C10 H10 0.91(3) . ? C11 N5 1.400(3) . ? C11 N4 1.404(3) . ? C11 Fe1 1.990(2) . ? C12 C17 1.402(3) . ? C12 C13 1.403(3) . ? C12 N1 1.449(3) . ? C13 C14 1.395(3) . ? C13 C18 1.509(3) . ? C14 C15 1.379(4) . ? C14 H14 0.9500 . ? C15 C16 1.382(3) . ? C15 H15 0.9500 . ? C16 C17 1.391(3) . ? C16 H16 0.9500 . ? C17 C21 1.514(3) . ? C18 C20 1.529(3) . ? C18 C19 1.538(3) . ? C18 H18 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C23 1.520(4) . ? C21 C22 1.526(3) . ? C21 H21 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C29 1.397(3) . ? C24 C25 1.403(3) . ? C24 N5 1.450(3) . ? C25 C26 1.390(3) . ? C25 C30 1.513(3) . ? C26 C27 1.370(4) . ? C26 H26 0.9500 . ? C27 C28 1.375(3) . ? C27 H27 0.9500 . ? C28 C29 1.394(3) . ? C28 H28 0.9500 . ? C29 C33 1.514(3) . ? C30 C32 1.529(3) . ? C30 C31 1.531(4) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C35 1.517(4) . ? C33 C34 1.533(4) . ? C33 H33 1.0000 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C37 1.315(5) . ? C36 C37A 1.452(5) . ? C36 Fe1 2.079(2) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.482(8) . ? C37 Fe1 2.135(4) . ? C37 H37 1.0000 . ? C38 N6 1.519(6) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 N6 1.373(6) . ? C39 C40 1.513(8) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.413(5) . ? C40 Fe1 2.087(4) . ? C40 H40 1.0000 . ? C37A C38A 1.501(6) . ? C37A Fe1 2.129(4) . ? C37A H37A 1.0000 . ? C38A N6 1.348(5) . ? C38A H38C 0.9900 . ? C38A H38D 0.9900 . ? C39A N6 1.480(6) . ? C39A C40A 1.508(6) . ? C39A H39C 0.9900 . ? C39A H39D 0.9900 . ? C40A C41 1.353(4) . ? C40A Fe1 2.161(4) . ? C40A H40A 1.0000 . ? C41 Fe1 2.076(2) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C44 1.374(5) . ? C42 C43A 1.389(6) . ? C42 N6 1.459(3) . ? C42 C45A 1.535(5) . ? C42 C43 1.591(6) . ? C42 C45 1.676(5) . ? C42 C44A 1.689(6) . ? N3 Fe1 1.9008(16) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C43A H43D 0.9800 . ? C43A H43E 0.9800 . ? C43A H43F 0.9800 . ? C44A H44D 0.9800 . ? C44A H44E 0.9800 . ? C44A H44F 0.9800 . ? C45A H45D 0.9800 . ? C45A H45E 0.9800 . ? C45A H45F 0.9800 . ? 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 C1 N2 100.43(16) . . ? N1 C1 Fe1 147.27(15) . . ? N2 C1 Fe1 112.24(14) . . ? C3 C2 N1 108.7(2) . . ? C3 C2 H2 129.0(18) . . ? N1 C2 H2 122.0(18) . . ? C2 C3 N2 106.16(19) . . ? C2 C3 H3 133.1(17) . . ? N2 C3 H3 120.6(17) . . ? N3 C4 N2 109.37(17) . . ? N3 C4 C5 123.6(2) . . ? N2 C4 C5 127.08(19) . . ? C6 C5 C4 118.0(2) . . ? C6 C5 H5 121.0 . . ? C4 C5 H5 121.0 . . ? C5 C6 C7 120.3(2) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? C8 C7 C6 117.5(2) . . ? C8 C7 H7 121.3 . . ? C6 C7 H7 121.3 . . ? N3 C8 C7 124.6(2) . . ? N3 C8 N4 108.94(17) . . ? C7 C8 N4 126.5(2) . . ? C10 C9 N4 105.5(2) . . ? C10 C9 H9 133.6(18) . . ? N4 C9 H9 120.9(18) . . ? C9 C10 N5 108.4(2) . . ? C9 C10 H10 131.1(19) . . ? N5 C10 H10 120.6(19) . . ? N5 C11 N4 99.81(18) . . ? N5 C11 Fe1 147.62(17) . . ? N4 C11 Fe1 112.53(15) . . ? C17 C12 C13 122.2(2) . . ? C17 C12 N1 118.51(18) . . ? C13 C12 N1 118.86(19) . . ? C14 C13 C12 117.3(2) . . ? C14 C13 C18 120.3(2) . . ? C12 C13 C18 122.1(2) . . ? C15 C14 C13 121.3(2) . . ? C15 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? C14 C15 C16 120.4(2) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C15 C16 C17 120.9(2) . . ? C15 C16 H16 119.6 . . ? C17 C16 H16 119.6 . . ? C16 C17 C12 117.8(2) . . ? C16 C17 C21 119.7(2) . . ? C12 C17 C21 122.33(19) . . ? C13 C18 C20 113.83(19) . . ? C13 C18 C19 108.9(2) . . ? C20 C18 C19 109.51(19) . . ? C13 C18 H18 108.2 . . ? C20 C18 H18 108.2 . . ? C19 C18 H18 108.2 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C17 C21 C23 113.32(19) . . ? C17 C21 C22 109.24(19) . . ? C23 C21 C22 110.07(19) . . ? C17 C21 H21 108.0 . . ? C23 C21 H21 108.0 . . ? C22 C21 H21 108.0 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C29 C24 C25 122.36(19) . . ? C29 C24 N5 118.83(18) . . ? C25 C24 N5 118.29(19) . . ? C26 C25 C24 116.9(2) . . ? C26 C25 C30 121.1(2) . . ? C24 C25 C30 121.8(2) . . ? C27 C26 C25 121.8(2) . . ? C27 C26 H26 119.1 . . ? C25 C26 H26 119.1 . . ? C26 C27 C28 120.3(2) . . ? C26 C27 H27 119.9 . . ? C28 C27 H27 119.9 . . ? C27 C28 C29 120.9(2) . . ? C27 C28 H28 119.6 . . ? C29 C28 H28 119.6 . . ? C28 C29 C24 117.7(2) . . ? C28 C29 C33 120.1(2) . . ? C24 C29 C33 122.12(19) . . ? C25 C30 C32 112.9(2) . . ? C25 C30 C31 110.0(2) . . ? C32 C30 C31 110.2(2) . . ? C25 C30 H30 107.9 . . ? C32 C30 H30 107.9 . . ? C31 C30 H30 107.9 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C29 C33 C35 113.3(2) . . ? C29 C33 C34 109.4(2) . . ? C35 C33 C34 111.1(2) . . ? C29 C33 H33 107.6 . . ? C35 C33 H33 107.6 . . ? C34 C33 H33 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 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C37 C36 Fe1 74.2(2) . . ? C37A C36 Fe1 71.68(17) . . ? C37 C36 H36A 116.1 . . ? C37A C36 H36A 151.1 . . ? Fe1 C36 H36A 116.1 . . ? C37 C36 H36B 116.1 . . ? C37A C36 H36B 84.2 . . ? Fe1 C36 H36B 116.1 . . ? H36A C36 H36B 113.1 . . ? C36 C37 C38 124.7(5) . . ? C36 C37 Fe1 69.5(2) . . ? C38 C37 Fe1 118.9(4) . . ? C36 C37 H37 112.4 . . ? C38 C37 H37 112.4 . . ? Fe1 C37 H37 112.4 . . ? C37 C38 N6 113.9(4) . . ? C37 C38 H38A 108.8 . . ? N6 C38 H38A 108.8 . . ? C37 C38 H38B 108.8 . . ? N6 C38 H38B 108.8 . . ? H38A C38 H38B 107.7 . . ? N6 C39 C40 113.8(4) . . ? N6 C39 H39A 108.8 . . ? C40 C39 H39A 108.8 . . ? N6 C39 H39B 108.8 . . ? C40 C39 H39B 108.8 . . ? H39A C39 H39B 107.7 . . ? C41 C40 C39 125.8(5) . . ? C41 C40 Fe1 69.7(2) . . ? C39 C40 Fe1 121.8(4) . . ? C41 C40 H40 111.2 . . ? C39 C40 H40 111.2 . . ? Fe1 C40 H40 111.2 . . ? C36 C37A C38A 124.9(4) . . ? C36 C37A Fe1 67.97(17) . . ? C38A C37A Fe1 120.9(3) . . ? C36 C37A H37A 112.1 . . ? C38A C37A H37A 112.1 . . ? Fe1 C37A H37A 112.1 . . ? N6 C38A C37A 113.4(4) . . ? N6 C38A H38C 108.9 . . ? C37A C38A H38C 108.9 . . ? N6 C38A H38D 108.9 . . ? C37A C38A H38D 108.9 . . ? H38C C38A H38D 107.7 . . ? N6 C39A C40A 112.6(4) . . ? N6 C39A H39C 109.1 . . ? C40A C39A H39C 109.1 . . ? N6 C39A H39D 109.1 . . ? C40A C39A H39D 109.1 . . ? H39C C39A H39D 107.8 . . ? C41 C40A C39A 126.2(4) . . ? C41 C40A Fe1 68.00(19) . . ? C39A C40A Fe1 119.6(3) . . ? C41 C40A H40A 112.0 . . ? C39A C40A H40A 112.0 . . ? Fe1 C40A H40A 112.0 . . ? C40A C41 Fe1 74.80(19) . . ? C40 C41 Fe1 70.56(19) . . ? C40A C41 H41A 83.1 . . ? C40 C41 H41A 116.6 . . ? Fe1 C41 H41A 116.6 . . ? C40A C41 H41B 147.6 . . ? C40 C41 H41B 116.6 . . ? Fe1 C41 H41B 116.6 . . ? H41A C41 H41B 113.6 . . ? C44 C42 C43A 120.3(4) . . ? C44 C42 N6 121.4(3) . . ? C43A C42 N6 117.3(3) . . ? C44 C42 C45A 47.7(3) . . ? C43A C42 C45A 115.7(4) . . ? N6 C42 C45A 112.7(3) . . ? C44 C42 C43 111.5(4) . . ? N6 C42 C43 112.0(3) . . ? C45A C42 C43 134.5(3) . . ? C44 C42 C45 109.4(4) . . ? C43A C42 C45 66.3(4) . . ? N6 C42 C45 102.1(2) . . ? C45A C42 C45 65.9(3) . . ? C43 C42 C45 97.1(4) . . ? C44 C42 C44A 53.1(3) . . ? C43A C42 C44A 108.5(4) . . ? N6 C42 C44A 99.3(3) . . ? C45A C42 C44A 100.3(4) . . ? C43 C42 C44A 80.1(4) . . ? C45 C42 C44A 157.8(3) . . ? C1 N1 C2 111.34(18) . . ? C1 N1 C12 129.06(16) . . ? C2 N1 C12 119.01(18) . . ? C4 N2 C3 129.30(18) . . ? C4 N2 C1 117.34(17) . . ? C3 N2 C1 113.35(18) . . ? C8 N3 C4 116.18(17) . . ? C8 N3 Fe1 122.41(14) . . ? C4 N3 Fe1 121.40(14) . . ? C9 N4 C8 128.50(19) . . ? C9 N4 C11 114.22(19) . . ? C8 N4 C11 117.28(18) . . ? C10 N5 C11 112.09(18) . . ? C10 N5 C24 118.65(17) . . ? C11 N5 C24 129.26(18) . . ? C38A N6 C39 116.9(3) . . ? C38A N6 C42 119.5(3) . . ? C39 N6 C42 123.6(3) . . ? C38A N6 C39A 112.7(3) . . ? C42 N6 C39A 120.4(3) . . ? C39 N6 C38 108.7(3) . . ? C42 N6 C38 121.4(3) . . ? C39A N6 C38 118.2(3) . . ? N3 Fe1 C1 79.50(8) . . ? N3 Fe1 C11 78.82(8) . . ? C1 Fe1 C11 158.29(8) . . ? N3 Fe1 C41 107.44(8) . . ? C1 Fe1 C41 93.43(8) . . ? C11 Fe1 C41 91.80(9) . . ? N3 Fe1 C36 101.39(8) . . ? C1 Fe1 C36 90.65(9) . . ? C11 Fe1 C36 94.87(8) . . ? C41 Fe1 C36 151.15(8) . . ? N3 Fe1 C40 143.52(13) . . ? C1 Fe1 C40 111.22(18) . . ? C11 Fe1 C40 85.90(18) . . ? C41 Fe1 C40 39.70(13) . . ? C36 Fe1 C40 112.85(13) . . ? N3 Fe1 C37A 139.34(11) . . ? C1 Fe1 C37A 86.55(14) . . ? C11 Fe1 C37A 111.03(15) . . ? C41 Fe1 C37A 111.40(12) . . ? C36 Fe1 C37A 40.35(13) . . ? C40 Fe1 C37A 77.10(16) . . ? N3 Fe1 C37 134.42(14) . . ? C1 Fe1 C37 108.84(16) . . ? C11 Fe1 C37 87.49(17) . . ? C41 Fe1 C37 116.34(13) . . ? C36 Fe1 C37 36.33(13) . . ? C40 Fe1 C37 76.87(17) . . ? C37A Fe1 C37 23.66(14) . . ? N3 Fe1 C40A 142.23(12) . . ? C1 Fe1 C40A 88.52(15) . . ? C11 Fe1 C40A 108.02(15) . . ? C41 Fe1 C40A 37.19(11) . . ? C36 Fe1 C40A 114.55(11) . . ? C40 Fe1 C40A 22.70(14) . . ? C37A Fe1 C40A 74.32(15) . . ? C37 Fe1 C40A 83.35(16) . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? C42 C45 H45A 109.5 . . ? C42 C45 H45B 109.5 . . ? C42 C45 H45C 109.5 . . ? C42 C43A H43D 109.5 . . ? C42 C43A H43E 109.5 . . ? H43D C43A H43E 109.5 . . ? C42 C43A H43F 109.5 . . ? H43D C43A H43F 109.5 . . ? H43E C43A H43F 109.5 . . ? C42 C44A H44D 109.5 . . ? C42 C44A H44E 109.5 . . ? H44D C44A H44E 109.5 . . ? C42 C44A H44F 109.5 . . ? H44D C44A H44F 109.5 . . ? H44E C44A H44F 109.5 . . ? C42 C45A H45D 109.5 . . ? C42 C45A H45E 109.5 . . ? H45D C45A H45E 109.5 . . ? C42 C45A H45F 109.5 . . ? H45D C45A H45F 109.5 . . ? H45E C45A H45F 109.5 . . ? 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 N1 C2 C3 N2 1.0(2) . . . . ? N3 C4 C5 C6 -0.2(3) . . . . ? N2 C4 C5 C6 -179.2(2) . . . . ? C4 C5 C6 C7 -0.1(3) . . . . ? C5 C6 C7 C8 0.2(3) . . . . ? C6 C7 C8 N3 0.0(3) . . . . ? C6 C7 C8 N4 -180.0(2) . . . . ? N4 C9 C10 N5 0.2(3) . . . . ? C17 C12 C13 C14 4.9(3) . . . . ? N1 C12 C13 C14 177.64(18) . . . . ? C17 C12 C13 C18 -168.92(19) . . . . ? N1 C12 C13 C18 3.8(3) . . . . ? C12 C13 C14 C15 -1.5(3) . . . . ? C18 C13 C14 C15 172.5(2) . . . . ? C13 C14 C15 C16 -1.7(4) . . . . ? C14 C15 C16 C17 1.7(4) . . . . ? C15 C16 C17 C12 1.6(3) . . . . ? C15 C16 C17 C21 -173.1(2) . . . . ? C13 C12 C17 C16 -5.0(3) . . . . ? N1 C12 C17 C16 -177.76(19) . . . . ? C13 C12 C17 C21 169.56(19) . . . . ? N1 C12 C17 C21 -3.2(3) . . . . ? C14 C13 C18 C20 46.0(3) . . . . ? C12 C13 C18 C20 -140.3(2) . . . . ? C14 C13 C18 C19 -76.4(3) . . . . ? C12 C13 C18 C19 97.2(2) . . . . ? C16 C17 C21 C23 -51.2(3) . . . . ? C12 C17 C21 C23 134.3(2) . . . . ? C16 C17 C21 C22 71.9(3) . . . . ? C12 C17 C21 C22 -102.6(2) . . . . ? C29 C24 C25 C26 -2.9(3) . . . . ? N5 C24 C25 C26 -174.55(19) . . . . ? C29 C24 C25 C30 172.90(19) . . . . ? N5 C24 C25 C30 1.3(3) . . . . ? C24 C25 C26 C27 1.0(4) . . . . ? C30 C25 C26 C27 -174.8(2) . . . . ? C25 C26 C27 C28 0.8(4) . . . . ? C26 C27 C28 C29 -0.8(4) . . . . ? C27 C28 C29 C24 -1.0(4) . . . . ? C27 C28 C29 C33 175.1(2) . . . . ? C25 C24 C29 C28 2.9(3) . . . . ? N5 C24 C29 C28 174.50(19) . . . . ? C25 C24 C29 C33 -173.1(2) . . . . ? N5 C24 C29 C33 -1.5(3) . . . . ? C26 C25 C30 C32 -43.0(3) . . . . ? C24 C25 C30 C32 141.4(2) . . . . ? C26 C25 C30 C31 80.6(3) . . . . ? C24 C25 C30 C31 -95.1(2) . . . . ? C28 C29 C33 C35 46.5(3) . . . . ? C24 C29 C33 C35 -137.6(2) . . . . ? C28 C29 C33 C34 -78.1(3) . . . . ? C24 C29 C33 C34 97.9(3) . . . . ? C37A C36 C37 C38 -31.2(4) . . . . ? Fe1 C36 C37 C38 -111.7(5) . . . . ? C37A C36 C37 Fe1 80.5(4) . . . . ? C36 C37 C38 N6 153.2(4) . . . . ? Fe1 C37 C38 N6 69.1(6) . . . . ? N6 C39 C40 C41 -158.9(4) . . . . ? N6 C39 C40 Fe1 -72.1(6) . . . . ? C37 C36 C37A C38A 25.2(4) . . . . ? Fe1 C36 C37A C38A 113.1(4) . . . . ? C37 C36 C37A Fe1 -87.9(4) . . . . ? C36 C37A C38A N6 -156.8(3) . . . . ? Fe1 C37A C38A N6 -73.4(5) . . . . ? N6 C39A C40A C41 151.3(3) . . . . ? N6 C39A C40A Fe1 68.1(5) . . . . ? C39A C40A C41 C40 -33.7(5) . . . . ? Fe1 C40A C41 C40 77.7(4) . . . . ? C39A C40A C41 Fe1 -111.4(5) . . . . ? C39 C40 C41 C40A 24.2(4) . . . . ? Fe1 C40 C41 C40A -91.0(4) . . . . ? C39 C40 C41 Fe1 115.2(5) . . . . ? N2 C1 N1 C2 -0.6(2) . . . . ? Fe1 C1 N1 C2 175.9(2) . . . . ? N2 C1 N1 C12 170.28(19) . . . . ? Fe1 C1 N1 C12 -13.2(4) . . . . ? C3 C2 N1 C1 -0.2(2) . . . . ? C3 C2 N1 C12 -172.13(19) . . . . ? C17 C12 N1 C1 -87.8(2) . . . . ? C13 C12 N1 C1 99.2(2) . . . . ? C17 C12 N1 C2 82.5(2) . . . . ? C13 C12 N1 C2 -90.5(2) . . . . ? N3 C4 N2 C3 178.59(19) . . . . ? C5 C4 N2 C3 -2.3(4) . . . . ? N3 C4 N2 C1 -2.3(2) . . . . ? C5 C4 N2 C1 176.8(2) . . . . ? C2 C3 N2 C4 177.7(2) . . . . ? C2 C3 N2 C1 -1.4(3) . . . . ? N1 C1 N2 C4 -177.96(17) . . . . ? Fe1 C1 N2 C4 4.1(2) . . . . ? N1 C1 N2 C3 1.2(2) . . . . ? Fe1 C1 N2 C3 -176.69(14) . . . . ? C7 C8 N3 C4 -0.3(3) . . . . ? N4 C8 N3 C4 179.67(16) . . . . ? C7 C8 N3 Fe1 179.88(16) . . . . ? N4 C8 N3 Fe1 -0.1(2) . . . . ? N2 C4 N3 C8 179.56(17) . . . . ? C5 C4 N3 C8 0.4(3) . . . . ? N2 C4 N3 Fe1 -0.6(2) . . . . ? C5 C4 N3 Fe1 -179.80(16) . . . . ? C10 C9 N4 C8 -179.9(2) . . . . ? C10 C9 N4 C11 -0.2(3) . . . . ? N3 C8 N4 C9 178.74(18) . . . . ? C7 C8 N4 C9 -1.3(3) . . . . ? N3 C8 N4 C11 -0.9(2) . . . . ? C7 C8 N4 C11 179.1(2) . . . . ? N5 C11 N4 C9 0.1(2) . . . . ? Fe1 C11 N4 C9 -178.20(14) . . . . ? N5 C11 N4 C8 179.85(17) . . . . ? Fe1 C11 N4 C8 1.5(2) . . . . ? C9 C10 N5 C11 -0.1(3) . . . . ? C9 C10 N5 C24 179.64(19) . . . . ? N4 C11 N5 C10 0.0(2) . . . . ? Fe1 C11 N5 C10 177.1(2) . . . . ? N4 C11 N5 C24 -179.72(19) . . . . ? Fe1 C11 N5 C24 -2.6(4) . . . . ? C29 C24 N5 C10 -84.8(2) . . . . ? C25 C24 N5 C10 87.2(2) . . . . ? C29 C24 N5 C11 94.9(3) . . . . ? C25 C24 N5 C11 -93.2(3) . . . . ? C37A C38A N6 C39 31.7(7) . . . . ? C37A C38A N6 C42 -148.2(3) . . . . ? C37A C38A N6 C39A 61.7(6) . . . . ? C37A C38A N6 C38 -46.4(6) . . . . ? C40 C39 N6 C38A 35.3(7) . . . . ? C40 C39 N6 C42 -144.7(4) . . . . ? C40 C39 N6 C39A -52.5(7) . . . . ? C40 C39 N6 C38 63.0(6) . . . . ? C44 C42 N6 C38A 46.9(5) . . . . ? C43A C42 N6 C38A -144.4(5) . . . . ? C45A C42 N6 C38A -6.3(5) . . . . ? C43 C42 N6 C38A -177.9(4) . . . . ? C45 C42 N6 C38A -75.0(4) . . . . ? C44A C42 N6 C38A 99.1(4) . . . . ? C44 C42 N6 C39 -133.0(5) . . . . ? C43A C42 N6 C39 35.7(6) . . . . ? C45A C42 N6 C39 173.8(5) . . . . ? C43 C42 N6 C39 2.2(6) . . . . ? C45 C42 N6 C39 105.1(5) . . . . ? C44A C42 N6 C39 -80.8(4) . . . . ? C44 C42 N6 C39A -165.3(5) . . . . ? C43A C42 N6 C39A 3.3(6) . . . . ? C45A C42 N6 C39A 141.5(4) . . . . ? C43 C42 N6 C39A -30.1(5) . . . . ? C45 C42 N6 C39A 72.8(4) . . . . ? C44A C42 N6 C39A -113.1(3) . . . . ? C44 C42 N6 C38 15.9(5) . . . . ? C43A C42 N6 C38 -175.4(5) . . . . ? C45A C42 N6 C38 -37.2(5) . . . . ? C43 C42 N6 C38 151.2(4) . . . . ? C45 C42 N6 C38 -105.9(4) . . . . ? C44A C42 N6 C38 68.1(4) . . . . ? C40A C39A N6 C38A -60.5(6) . . . . ? C40A C39A N6 C39 44.5(6) . . . . ? C40A C39A N6 C42 149.7(3) . . . . ? C40A C39A N6 C38 -31.5(6) . . . . ? C37 C38 N6 C38A 48.6(7) . . . . ? C37 C38 N6 C39 -64.3(6) . . . . ? C37 C38 N6 C42 142.7(4) . . . . ? C37 C38 N6 C39A -36.1(6) . . . . ? C8 N3 Fe1 C1 -177.94(16) . . . . ? C4 N3 Fe1 C1 2.27(15) . . . . ? C8 N3 Fe1 C11 0.75(16) . . . . ? C4 N3 Fe1 C11 -179.05(16) . . . . ? C8 N3 Fe1 C41 -87.61(16) . . . . ? C4 N3 Fe1 C41 92.59(16) . . . . ? C8 N3 Fe1 C36 93.53(16) . . . . ? C4 N3 Fe1 C36 -86.27(16) . . . . ? C8 N3 Fe1 C40 -66.3(3) . . . . ? C4 N3 Fe1 C40 113.9(3) . . . . ? C8 N3 Fe1 C37A 110.1(2) . . . . ? C4 N3 Fe1 C37A -69.7(3) . . . . ? C8 N3 Fe1 C37 75.9(3) . . . . ? C4 N3 Fe1 C37 -103.9(3) . . . . ? C8 N3 Fe1 C40A -104.3(3) . . . . ? C4 N3 Fe1 C40A 75.9(3) . . . . ? N1 C1 Fe1 N3 -179.5(3) . . . . ? N2 C1 Fe1 N3 -3.25(13) . . . . ? N1 C1 Fe1 C11 177.0(2) . . . . ? N2 C1 Fe1 C11 -6.7(3) . . . . ? N1 C1 Fe1 C41 73.4(3) . . . . ? N2 C1 Fe1 C41 -110.36(14) . . . . ? N1 C1 Fe1 C36 -78.0(3) . . . . ? N2 C1 Fe1 C36 98.22(15) . . . . ? N1 C1 Fe1 C40 36.9(3) . . . . ? N2 C1 Fe1 C40 -146.89(17) . . . . ? N1 C1 Fe1 C37A -37.9(3) . . . . ? N2 C1 Fe1 C37A 138.38(17) . . . . ? N1 C1 Fe1 C37 -46.0(3) . . . . ? N2 C1 Fe1 C37 130.29(18) . . . . ? N1 C1 Fe1 C40A 36.5(3) . . . . ? N2 C1 Fe1 C40A -147.24(16) . . . . ? N5 C11 Fe1 N3 -178.1(3) . . . . ? N4 C11 Fe1 N3 -1.15(14) . . . . ? N5 C11 Fe1 C1 -174.6(2) . . . . ? N4 C11 Fe1 C1 2.3(3) . . . . ? N5 C11 Fe1 C41 -70.7(3) . . . . ? N4 C11 Fe1 C41 106.27(15) . . . . ? N5 C11 Fe1 C36 81.2(3) . . . . ? N4 C11 Fe1 C36 -101.83(16) . . . . ? N5 C11 Fe1 C40 -31.4(3) . . . . ? N4 C11 Fe1 C40 145.55(18) . . . . ? N5 C11 Fe1 C37A 43.1(3) . . . . ? N4 C11 Fe1 C37A -139.95(17) . . . . ? N5 C11 Fe1 C37 45.6(3) . . . . ? N4 C11 Fe1 C37 -137.43(18) . . . . ? N5 C11 Fe1 C40A -36.6(3) . . . . ? N4 C11 Fe1 C40A 140.39(16) . . . . ? C40A C41 Fe1 N3 -163.1(2) . . . . ? C40 C41 Fe1 N3 160.2(3) . . . . ? C40A C41 Fe1 C1 -83.0(2) . . . . ? C40 C41 Fe1 C1 -119.7(3) . . . . ? C40A C41 Fe1 C11 118.1(2) . . . . ? C40 C41 Fe1 C11 81.4(3) . . . . ? C40A C41 Fe1 C36 14.6(3) . . . . ? C40 C41 Fe1 C36 -22.1(3) . . . . ? C40A C41 Fe1 C40 36.7(2) . . . . ? C40A C41 Fe1 C37A 4.6(3) . . . . ? C40 C41 Fe1 C37A -32.1(3) . . . . ? C40A C41 Fe1 C37 30.0(3) . . . . ? C40 C41 Fe1 C37 -6.7(3) . . . . ? C40 C41 Fe1 C40A -36.7(2) . . . . ? C37 C36 Fe1 N3 -158.6(3) . . . . ? C37A C36 Fe1 N3 163.3(2) . . . . ? C37 C36 Fe1 C1 122.0(3) . . . . ? C37A C36 Fe1 C1 83.9(2) . . . . ? C37 C36 Fe1 C11 -79.1(3) . . . . ? C37A C36 Fe1 C11 -117.1(2) . . . . ? C37 C36 Fe1 C41 23.6(4) . . . . ? C37A C36 Fe1 C41 -14.4(3) . . . . ? C37 C36 Fe1 C40 8.5(3) . . . . ? C37A C36 Fe1 C40 -29.5(3) . . . . ? C37 C36 Fe1 C37A 38.1(2) . . . . ? C37A C36 Fe1 C37 -38.1(2) . . . . ? C37 C36 Fe1 C40A 33.3(3) . . . . ? C37A C36 Fe1 C40A -4.8(3) . . . . ? C41 C40 Fe1 N3 -32.9(4) . . . . ? C39 C40 Fe1 N3 -153.2(3) . . . . ? C41 C40 Fe1 C1 68.5(2) . . . . ? C39 C40 Fe1 C1 -51.8(4) . . . . ? C41 C40 Fe1 C11 -97.8(2) . . . . ? C39 C40 Fe1 C11 141.9(4) . . . . ? C39 C40 Fe1 C41 -120.3(6) . . . . ? C41 C40 Fe1 C36 168.65(18) . . . . ? C39 C40 Fe1 C36 48.3(5) . . . . ? C41 C40 Fe1 C37A 149.5(3) . . . . ? C39 C40 Fe1 C37A 29.2(4) . . . . ? C41 C40 Fe1 C37 173.8(3) . . . . ? C39 C40 Fe1 C37 53.5(4) . . . . ? C41 C40 Fe1 C40A 69.4(4) . . . . ? C39 C40 Fe1 C40A -50.9(5) . . . . ? C36 C37A Fe1 N3 -25.6(3) . . . . ? C38A C37A Fe1 N3 -144.1(3) . . . . ? C36 C37A Fe1 C1 -95.08(19) . . . . ? C38A C37A Fe1 C1 146.4(4) . . . . ? C36 C37A Fe1 C11 71.8(2) . . . . ? C38A C37A Fe1 C11 -46.7(4) . . . . ? C36 C37A Fe1 C41 172.58(16) . . . . ? C38A C37A Fe1 C41 54.1(4) . . . . ? C38A C37A Fe1 C36 -118.5(5) . . . . ? C36 C37A Fe1 C40 152.2(2) . . . . ? C38A C37A Fe1 C40 33.7(4) . . . . ? C36 C37A Fe1 C37 65.5(4) . . . . ? C38A C37A Fe1 C37 -52.9(5) . . . . ? C36 C37A Fe1 C40A 175.5(2) . . . . ? C38A C37A Fe1 C40A 57.0(4) . . . . ? C36 C37 Fe1 N3 30.0(4) . . . . ? C38 C37 Fe1 N3 149.2(3) . . . . ? C36 C37 Fe1 C1 -63.7(3) . . . . ? C38 C37 Fe1 C1 55.5(4) . . . . ? C36 C37 Fe1 C11 101.7(2) . . . . ? C38 C37 Fe1 C11 -139.1(4) . . . . ? C36 C37 Fe1 C41 -167.53(19) . . . . ? C38 C37 Fe1 C41 -48.3(5) . . . . ? C38 C37 Fe1 C36 119.2(6) . . . . ? C36 C37 Fe1 C40 -171.9(3) . . . . ? C38 C37 Fe1 C40 -52.7(4) . . . . ? C36 C37 Fe1 C37A -84.2(4) . . . . ? C38 C37 Fe1 C37A 35.0(4) . . . . ? C36 C37 Fe1 C40A -149.8(3) . . . . ? C38 C37 Fe1 C40A -30.6(4) . . . . ? C41 C40A Fe1 N3 27.0(4) . . . . ? C39A C40A Fe1 N3 147.1(3) . . . . ? C41 C40A Fe1 C1 97.6(2) . . . . ? C39A C40A Fe1 C1 -142.2(4) . . . . ? C41 C40A Fe1 C11 -68.0(2) . . . . ? C39A C40A Fe1 C11 52.1(4) . . . . ? C39A C40A Fe1 C41 120.2(5) . . . . ? C41 C40A Fe1 C36 -172.31(17) . . . . ? C39A C40A Fe1 C36 -52.1(4) . . . . ? C41 C40A Fe1 C40 -81.5(4) . . . . ? C39A C40A Fe1 C40 38.7(4) . . . . ? C41 C40A Fe1 C37A -175.5(3) . . . . ? C39A C40A Fe1 C37A -55.4(4) . . . . ? C41 C40A Fe1 C37 -153.2(2) . . . . ? C39A C40A Fe1 C37 -33.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.353 _refine_diff_density_min -0.183 _refine_diff_density_rms 0.043 data_jmd20 _vrf_PLAT232_jmd20 ; PROBLEM: Hirshfeld Test Diff (M-X) Fe1 -- N6 .. 12.3 su PROBLEM: Hirshfeld Test Diff (M-X) Fe1 -- C10 .. 7.9 su PROBLEM: Hirshfeld Test Diff (M-X) Fe1 -- C11 .. 6.5 su RESPONSE: Along chemical bonds, the anisotropic displacement parameter components are always assumed to be equal in magnitude. In this case, the large difference associated with the Fe1-N6, Fe1-C10, and Fe1-C11 bonds can be attributed to the presence of a heavy atom. Here, charge deformation has a lesser importance with respect to the total charge density present. ; # end validation reply form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H61 Fe N9 O' _chemical_formula_weight 811.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P2(1)/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.098(5) _cell_length_b 23.513(5) _cell_length_c 16.613(5) _cell_angle_alpha 90.000 _cell_angle_beta 92.883(5) _cell_angle_gamma 90.000 _cell_volume 4330(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9948 _cell_measurement_theta_min 4.61 _cell_measurement_theta_max 65.56 _exptl_crystal_description cube _exptl_crystal_colour black _exptl_crystal_size_max 0.083 _exptl_crystal_size_mid 0.073 _exptl_crystal_size_min 0.057 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.246 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1736 _exptl_absorpt_coefficient_mu 3.145 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6903 _exptl_absorpt_correction_T_max 0.7528 _exptl_absorpt_process_details 'SADABS V2008/1 (Bruker AXS)' _exptl_special_details ; Collected, solved and refined by Scott P. Semproni ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54187 _diffrn_radiation_type 'CuK\a' _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45763 _diffrn_reflns_av_R_equivalents 0.0326 _diffrn_reflns_av_sigmaI/netI 0.0203 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.26 _diffrn_reflns_theta_max 66.34 _reflns_number_total 7424 _reflns_number_gt 6845 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR92 (Giacavazzo 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0491P)^2^+1.7647P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7424 _refine_ls_number_parameters 526 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0351 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0858 _refine_ls_wR_factor_gt 0.0835 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.20320(15) 0.04598(7) 0.26809(10) 0.0256(4) Uani 1 1 d . . . H1 H 0.2126 0.0106 0.2953 0.031 Uiso 1 1 calc R . . C1S C 0.5188(2) 0.08183(10) 0.15311(15) 0.0517(6) Uani 1 1 d . . . H1S1 H 0.4849 0.0638 0.1038 0.078 Uiso 1 1 calc R . . H1S2 H 0.4743 0.1169 0.1634 0.078 Uiso 1 1 calc R . . H1S3 H 0.5121 0.0557 0.1986 0.078 Uiso 1 1 calc R . . C2 C 0.22185(15) 0.05541(7) 0.19013(10) 0.0270(4) Uani 1 1 d . . . H2 H 0.2463 0.0283 0.1518 0.032 Uiso 1 1 calc R . . C2S C 0.6487(2) 0.09570(9) 0.14313(14) 0.0474(5) Uani 1 1 d . . . H2S1 H 0.6554 0.1238 0.0992 0.057 Uiso 1 1 calc R . . H2S2 H 0.6839 0.1128 0.1935 0.057 Uiso 1 1 calc R . . C3 C 0.21083(14) 0.14663(7) 0.10946(9) 0.0225(3) Uani 1 1 d . . . C3S C 0.8396(2) 0.05631(11) 0.12118(13) 0.0513(6) Uani 1 1 d . . . H3S1 H 0.8746 0.0654 0.1757 0.062 Uiso 1 1 calc R . . H3S2 H 0.8533 0.0891 0.0855 0.062 Uiso 1 1 calc R . . C4 C 0.24301(15) 0.13077(8) 0.03347(10) 0.0283(4) Uani 1 1 d . . . H4 H 0.2571 0.0920 0.0208 0.034 Uiso 1 1 calc R . . C4S C 0.8987(2) 0.00452(13) 0.08941(19) 0.0687(7) Uani 1 1 d . . . H4S1 H 0.8859 -0.0276 0.1255 0.103 Uiso 1 1 calc R . . H4S2 H 0.9854 0.0114 0.0863 0.103 Uiso 1 1 calc R . . H4S3 H 0.8635 -0.0043 0.0356 0.103 Uiso 1 1 calc R . . C5 C 0.25424(15) 0.17347(8) -0.02422(10) 0.0305(4) Uani 1 1 d . . . H5 H 0.2757 0.1638 -0.0771 0.037 Uiso 1 1 calc R . . C6 C 0.23408(15) 0.23009(8) -0.00451(10) 0.0260(4) Uani 1 1 d . . . H6 H 0.2414 0.2594 -0.0433 0.031 Uiso 1 1 calc R . . C7 C 0.20319(13) 0.24248(7) 0.07298(9) 0.0218(3) Uani 1 1 d . . . C8 C 0.19375(14) 0.34981(7) 0.07610(10) 0.0249(4) Uani 1 1 d . . . H8 H 0.2091 0.3598 0.0222 0.030 Uiso 1 1 calc R . . C9 C 0.17416(15) 0.38539(7) 0.13675(10) 0.0246(4) Uani 1 1 d . . . H9 H 0.1727 0.4257 0.1335 0.030 Uiso 1 1 calc R . . C10 C 0.16299(13) 0.29533(7) 0.18989(9) 0.0192(3) Uani 1 1 d . . . C11 C 0.16609(13) 0.14108(7) 0.24690(9) 0.0191(3) Uani 1 1 d . . . C12 C 0.14560(14) 0.10441(6) 0.38641(9) 0.0199(3) Uani 1 1 d . . . C13 C 0.24194(15) 0.11971(7) 0.43953(10) 0.0234(3) Uani 1 1 d . . . C14 C 0.21832(15) 0.12773(7) 0.52032(10) 0.0260(4) Uani 1 1 d . . . H14 H 0.2821 0.1383 0.5576 0.031 Uiso 1 1 calc R . . C15 C 0.10310(16) 0.12044(8) 0.54685(10) 0.0282(4) Uani 1 1 d . . . H15 H 0.0883 0.1262 0.6021 0.034 Uiso 1 1 calc R . . C16 C 0.00917(15) 0.10485(8) 0.49332(10) 0.0269(4) Uani 1 1 d . . . H16 H -0.0694 0.0999 0.5124 0.032 Uiso 1 1 calc R . . C17 C 0.02805(14) 0.09637(7) 0.41205(10) 0.0216(3) Uani 1 1 d . . . C18 C 0.36960(15) 0.12575(8) 0.41175(11) 0.0319(4) Uani 1 1 d . . . H18 H 0.3656 0.1264 0.3515 0.038 Uiso 1 1 calc R . . C19 C 0.44549(18) 0.07407(9) 0.43960(16) 0.0507(6) Uani 1 1 d . . . H19A H 0.4557 0.0741 0.4985 0.076 Uiso 1 1 calc R . . H19B H 0.5248 0.0760 0.4163 0.076 Uiso 1 1 calc R . . H19C H 0.4044 0.0391 0.4217 0.076 Uiso 1 1 calc R . . C20 C 0.43049(16) 0.18040(8) 0.44176(13) 0.0372(4) Uani 1 1 d . . . H20A H 0.3811 0.2131 0.4244 0.056 Uiso 1 1 calc R . . H20B H 0.5103 0.1835 0.4195 0.056 Uiso 1 1 calc R . . H20C H 0.4392 0.1797 0.5007 0.056 Uiso 1 1 calc R . . C21 C -0.07311(15) 0.07716(7) 0.35327(10) 0.0256(4) Uani 1 1 d . . . H21 H -0.0594 0.0949 0.2998 0.031 Uiso 1 1 calc R . . C22 C -0.07106(17) 0.01253(8) 0.34262(13) 0.0392(5) Uani 1 1 d . . . H22A H 0.0074 0.0009 0.3235 0.059 Uiso 1 1 calc R . . H22B H -0.1351 0.0012 0.3031 0.059 Uiso 1 1 calc R . . H22C H -0.0841 -0.0059 0.3944 0.059 Uiso 1 1 calc R . . C23 C -0.19851(15) 0.09480(8) 0.37804(11) 0.0284(4) Uani 1 1 d . . . H23A H -0.2193 0.0733 0.4259 0.043 Uiso 1 1 calc R . . H23B H -0.2579 0.0869 0.3338 0.043 Uiso 1 1 calc R . . H23C H -0.1987 0.1356 0.3903 0.043 Uiso 1 1 calc R . . C24 C 0.13136(14) 0.37907(7) 0.28160(9) 0.0205(3) Uani 1 1 d . . . C25 C 0.22341(15) 0.38116(7) 0.34299(10) 0.0230(3) Uani 1 1 d . . . C26 C 0.19747(16) 0.40948(7) 0.41362(10) 0.0281(4) Uani 1 1 d . . . H26 H 0.2575 0.4116 0.4564 0.034 Uiso 1 1 calc R . . C27 C 0.08592(17) 0.43462(8) 0.42299(11) 0.0313(4) Uani 1 1 d . . . H27 H 0.0709 0.4542 0.4715 0.038 Uiso 1 1 calc R . . C28 C -0.00334(16) 0.43133(7) 0.36216(10) 0.0284(4) Uani 1 1 d . . . H28 H -0.0797 0.4483 0.3694 0.034 Uiso 1 1 calc R . . C29 C 0.01743(15) 0.40330(7) 0.29018(10) 0.0226(3) Uani 1 1 d . . . C30 C 0.34574(15) 0.35379(7) 0.33251(10) 0.0255(4) Uani 1 1 d . . . H30 H 0.3311 0.3159 0.3065 0.031 Uiso 1 1 calc R . . C31 C 0.41702(16) 0.34352(8) 0.41242(11) 0.0324(4) Uani 1 1 d . . . H31A H 0.4402 0.3801 0.4368 0.049 Uiso 1 1 calc R . . H31B H 0.4897 0.3214 0.4026 0.049 Uiso 1 1 calc R . . H31C H 0.3668 0.3225 0.4491 0.049 Uiso 1 1 calc R . . C32 C 0.42227(17) 0.38904(9) 0.27614(12) 0.0367(4) Uani 1 1 d . . . H32A H 0.3803 0.3918 0.2229 0.055 Uiso 1 1 calc R . . H32B H 0.5006 0.3705 0.2709 0.055 Uiso 1 1 calc R . . H32C H 0.4346 0.4273 0.2986 0.055 Uiso 1 1 calc R . . C33 C -0.08146(15) 0.40121(7) 0.22326(10) 0.0244(4) Uani 1 1 d . . . H33 H -0.0558 0.3741 0.1810 0.029 Uiso 1 1 calc R . . C34 C -0.20111(16) 0.38024(8) 0.25423(11) 0.0300(4) Uani 1 1 d . . . H34A H -0.1896 0.3426 0.2787 0.045 Uiso 1 1 calc R . . H34B H -0.2614 0.3778 0.2092 0.045 Uiso 1 1 calc R . . H34C H -0.2290 0.4069 0.2946 0.045 Uiso 1 1 calc R . . C35 C -0.09899(17) 0.45982(8) 0.18432(12) 0.0346(4) Uani 1 1 d . . . H35A H -0.1268 0.4868 0.2244 0.052 Uiso 1 1 calc R . . H35B H -0.1592 0.4572 0.1393 0.052 Uiso 1 1 calc R . . H35C H -0.0222 0.4730 0.1644 0.052 Uiso 1 1 calc R . . C36 C -0.09581(14) 0.22947(7) 0.14038(10) 0.0223(3) Uani 1 1 d . . . H36 H -0.0437 0.2304 0.0968 0.027 Uiso 1 1 calc R . . C37 C -0.21743(15) 0.23432(7) 0.12239(10) 0.0241(3) Uani 1 1 d . . . H37 H -0.2467 0.2387 0.0680 0.029 Uiso 1 1 calc R . . C38 C -0.29898(14) 0.23282(7) 0.18502(10) 0.0238(4) Uani 1 1 d . . . C39 C -0.24571(15) 0.22645(7) 0.26293(10) 0.0238(4) Uani 1 1 d . . . H39 H -0.2953 0.2248 0.3079 0.029 Uiso 1 1 calc R . . C40 C -0.12245(14) 0.22256(7) 0.27483(10) 0.0220(3) Uani 1 1 d . . . H40 H -0.0903 0.2190 0.3287 0.026 Uiso 1 1 calc R . . C41 C -0.47757(17) 0.23808(9) 0.09066(12) 0.0383(5) Uani 1 1 d . . . H41A H -0.4282 0.2607 0.0554 0.057 Uiso 1 1 calc R . . H41B H -0.5579 0.2552 0.0925 0.057 Uiso 1 1 calc R . . H41C H -0.4850 0.1992 0.0697 0.057 Uiso 1 1 calc R . . C42 C -0.49918(16) 0.22985(10) 0.23846(12) 0.0386(5) Uani 1 1 d . . . H42A H -0.4861 0.1922 0.2627 0.058 Uiso 1 1 calc R . . H42B H -0.5836 0.2334 0.2188 0.058 Uiso 1 1 calc R . . H42C H -0.4807 0.2593 0.2790 0.058 Uiso 1 1 calc R . . N1 N 0.16766(11) 0.09704(6) 0.30248(8) 0.0200(3) Uani 1 1 d . . . N2 N 0.19829(12) 0.11271(6) 0.17667(8) 0.0218(3) Uani 1 1 d . . . N3 N 0.19073(11) 0.20187(6) 0.13106(8) 0.0194(3) Uani 1 1 d . . . N4 N 0.18710(11) 0.29517(6) 0.10768(8) 0.0206(3) Uani 1 1 d . . . N5 N 0.15626(11) 0.35316(6) 0.20561(8) 0.0203(3) Uani 1 1 d . . . N6 N 0.14409(11) 0.24034(6) 0.33803(8) 0.0194(3) Uani 1 1 d . . . N7 N 0.14601(13) 0.25287(6) 0.40389(8) 0.0265(3) Uani 1 1 d . . . N8 N -0.04452(11) 0.22347(5) 0.21565(8) 0.0191(3) Uani 1 1 d . . . N9 N -0.42067(13) 0.23677(7) 0.17143(9) 0.0322(3) Uani 1 1 d . . . Fe1 Fe 0.13913(2) 0.221220(10) 0.234263(14) 0.01591(8) Uani 1 1 d . . . O1S O 0.71374(13) 0.04575(6) 0.12467(9) 0.0458(4) Uani 1 1 d . . . 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 C1 0.0263(8) 0.0197(8) 0.0306(9) -0.0035(7) 0.0008(7) 0.0014(7) C1S 0.0571(14) 0.0390(12) 0.0594(15) 0.0035(11) 0.0048(11) 0.0045(10) C2 0.0293(9) 0.0258(9) 0.0262(9) -0.0085(7) 0.0034(7) 0.0006(7) C2S 0.0636(15) 0.0355(11) 0.0426(12) 0.0000(9) -0.0034(10) -0.0046(10) C3 0.0175(8) 0.0314(9) 0.0185(8) -0.0026(7) -0.0007(6) 0.0000(6) C3S 0.0543(14) 0.0655(15) 0.0326(11) 0.0062(11) -0.0120(10) -0.0152(12) C4 0.0268(9) 0.0368(10) 0.0213(9) -0.0088(7) 0.0008(7) 0.0022(7) C4S 0.0438(14) 0.0793(19) 0.083(2) 0.0143(16) 0.0008(13) 0.0046(13) C5 0.0263(9) 0.0496(11) 0.0156(8) -0.0065(8) 0.0012(7) 0.0016(8) C6 0.0203(8) 0.0410(10) 0.0167(8) 0.0006(7) 0.0008(6) -0.0003(7) C7 0.0129(7) 0.0339(9) 0.0184(8) 0.0005(7) -0.0006(6) -0.0001(6) C8 0.0211(8) 0.0333(9) 0.0201(8) 0.0073(7) 0.0002(6) -0.0029(7) C9 0.0242(8) 0.0271(9) 0.0224(8) 0.0069(7) -0.0010(7) -0.0031(7) C10 0.0121(7) 0.0293(8) 0.0158(8) -0.0003(6) -0.0011(6) 0.0002(6) C11 0.0132(7) 0.0266(8) 0.0173(8) -0.0022(6) -0.0009(6) -0.0008(6) C12 0.0220(8) 0.0187(8) 0.0191(8) 0.0010(6) 0.0003(6) 0.0019(6) C13 0.0233(8) 0.0247(8) 0.0221(8) 0.0017(7) -0.0013(6) -0.0008(6) C14 0.0261(9) 0.0304(9) 0.0209(8) 0.0005(7) -0.0045(7) -0.0016(7) C15 0.0304(9) 0.0358(10) 0.0183(8) 0.0012(7) 0.0011(7) 0.0025(7) C16 0.0223(8) 0.0354(9) 0.0231(8) 0.0023(7) 0.0028(7) 0.0014(7) C17 0.0211(8) 0.0208(8) 0.0228(8) 0.0028(6) 0.0000(6) 0.0019(6) C18 0.0221(9) 0.0506(11) 0.0228(9) -0.0059(8) -0.0003(7) -0.0072(8) C19 0.0261(10) 0.0403(12) 0.0863(18) -0.0222(12) 0.0095(10) 0.0012(9) C20 0.0221(9) 0.0378(10) 0.0515(12) 0.0074(9) -0.0022(8) -0.0043(8) C21 0.0211(8) 0.0334(9) 0.0222(8) -0.0010(7) 0.0009(6) -0.0032(7) C22 0.0274(10) 0.0381(11) 0.0524(12) -0.0143(9) 0.0042(9) -0.0047(8) C23 0.0213(8) 0.0356(10) 0.0282(9) 0.0016(8) 0.0007(7) -0.0012(7) C24 0.0238(8) 0.0191(8) 0.0186(8) 0.0015(6) -0.0003(6) -0.0017(6) C25 0.0240(8) 0.0199(8) 0.0247(8) 0.0030(7) -0.0034(7) -0.0028(6) C26 0.0335(10) 0.0275(9) 0.0225(9) -0.0017(7) -0.0074(7) -0.0008(7) C27 0.0403(10) 0.0300(9) 0.0233(9) -0.0061(7) -0.0002(7) 0.0046(8) C28 0.0292(9) 0.0288(9) 0.0273(9) 0.0005(7) 0.0012(7) 0.0059(7) C29 0.0243(8) 0.0218(8) 0.0216(8) 0.0031(7) -0.0004(6) 0.0006(6) C30 0.0219(8) 0.0272(9) 0.0268(9) 0.0000(7) -0.0043(7) -0.0010(7) C31 0.0257(9) 0.0366(10) 0.0337(10) -0.0008(8) -0.0091(7) 0.0022(8) C32 0.0240(9) 0.0445(11) 0.0413(11) 0.0077(9) -0.0013(8) -0.0046(8) C33 0.0229(8) 0.0296(9) 0.0206(8) 0.0017(7) -0.0008(6) 0.0032(7) C34 0.0268(9) 0.0385(10) 0.0246(9) 0.0024(8) -0.0003(7) -0.0028(7) C35 0.0299(9) 0.0384(10) 0.0350(10) 0.0122(8) -0.0038(8) 0.0014(8) C36 0.0190(8) 0.0300(9) 0.0181(8) 0.0015(7) 0.0015(6) -0.0022(6) C37 0.0202(8) 0.0320(9) 0.0199(8) 0.0039(7) -0.0022(6) -0.0018(7) C38 0.0174(8) 0.0265(8) 0.0275(9) 0.0015(7) 0.0000(7) -0.0002(6) C39 0.0184(8) 0.0327(9) 0.0208(8) -0.0001(7) 0.0039(6) -0.0001(7) C40 0.0198(8) 0.0291(9) 0.0169(8) -0.0001(6) 0.0002(6) 0.0000(6) C41 0.0226(9) 0.0529(12) 0.0383(11) 0.0116(9) -0.0082(8) -0.0037(8) C42 0.0167(9) 0.0601(13) 0.0394(11) -0.0050(9) 0.0051(8) 0.0005(8) N1 0.0191(7) 0.0215(7) 0.0194(7) -0.0024(5) 0.0007(5) 0.0002(5) N2 0.0214(7) 0.0257(7) 0.0183(7) -0.0053(6) 0.0013(5) 0.0006(5) N3 0.0144(6) 0.0281(7) 0.0156(6) -0.0020(6) -0.0005(5) 0.0004(5) N4 0.0164(6) 0.0291(7) 0.0163(7) 0.0018(6) 0.0001(5) -0.0010(5) N5 0.0187(6) 0.0247(7) 0.0172(7) 0.0015(6) -0.0002(5) -0.0007(5) N6 0.0169(6) 0.0207(7) 0.0205(8) 0.0026(6) -0.0008(5) 0.0011(5) N7 0.0319(8) 0.0293(8) 0.0180(8) -0.0009(6) -0.0005(6) 0.0011(6) N8 0.0158(7) 0.0235(7) 0.0179(7) 0.0000(5) 0.0000(5) -0.0011(5) N9 0.0149(7) 0.0511(9) 0.0304(8) 0.0037(7) -0.0010(6) 0.0006(6) Fe1 0.01274(13) 0.02185(14) 0.01312(13) -0.00089(9) 0.00026(9) 0.00026(9) O1S 0.0441(8) 0.0421(8) 0.0507(9) 0.0050(7) -0.0026(7) -0.0053(6) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; 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 C1 C2 1.340(2) . ? C1 N1 1.395(2) . ? C1S C2S 1.496(3) . ? C2 N2 1.388(2) . ? C2S O1S 1.420(3) . ? C3 N3 1.369(2) . ? C3 C4 1.380(2) . ? C3 N2 1.385(2) . ? C3S O1S 1.423(3) . ? C3S C4S 1.492(4) . ? C4 C5 1.398(3) . ? C5 C6 1.392(3) . ? C6 C7 1.380(2) . ? C7 N3 1.369(2) . ? C7 N4 1.382(2) . ? C8 C9 1.336(2) . ? C8 N4 1.391(2) . ? C9 N5 1.395(2) . ? C10 N5 1.387(2) . ? C10 N4 1.405(2) . ? C10 Fe1 1.9156(17) . ? C11 N1 1.387(2) . ? C11 N2 1.406(2) . ? C11 Fe1 1.9179(17) . ? C12 C13 1.399(2) . ? C12 C17 1.405(2) . ? C12 N1 1.438(2) . ? C13 C14 1.393(2) . ? C13 C18 1.519(2) . ? C14 C15 1.384(3) . ? C15 C16 1.385(2) . ? C16 C17 1.391(2) . ? C17 C21 1.519(2) . ? C18 C20 1.524(3) . ? C18 C19 1.537(3) . ? C21 C23 1.528(2) . ? C21 C22 1.530(3) . ? C24 C29 1.401(2) . ? C24 C25 1.408(2) . ? C24 N5 1.441(2) . ? C25 C26 1.392(2) . ? C25 C30 1.520(2) . ? C26 C27 1.388(3) . ? C27 C28 1.381(3) . ? C28 C29 1.395(2) . ? C29 C33 1.523(2) . ? C30 C31 1.530(2) . ? C30 C32 1.538(3) . ? C33 C34 1.530(2) . ? C33 C35 1.531(2) . ? C36 N8 1.355(2) . ? C36 C37 1.372(2) . ? C37 C38 1.413(2) . ? C38 N9 1.361(2) . ? C38 C39 1.404(2) . ? C39 C40 1.375(2) . ? C40 N8 1.342(2) . ? C41 N9 1.454(2) . ? C42 N9 1.457(2) . ? N3 Fe1 1.8903(14) . ? N6 N7 1.1323(19) . ? N6 Fe1 1.7797(14) . ? N8 Fe1 2.0467(16) . ? 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 C2 C1 N1 108.29(15) . . ? C1 C2 N2 106.22(14) . . ? O1S C2S C1S 110.27(18) . . ? N3 C3 C4 123.31(15) . . ? N3 C3 N2 108.11(13) . . ? C4 C3 N2 128.52(16) . . ? O1S C3S C4S 108.76(19) . . ? C3 C4 C5 117.98(16) . . ? C6 C5 C4 120.31(15) . . ? C7 C6 C5 118.15(16) . . ? N3 C7 C6 123.29(16) . . ? N3 C7 N4 108.15(13) . . ? C6 C7 N4 128.44(15) . . ? C9 C8 N4 106.28(14) . . ? C8 C9 N5 108.27(15) . . ? N5 C10 N4 101.55(13) . . ? N5 C10 Fe1 144.03(12) . . ? N4 C10 Fe1 114.10(11) . . ? N1 C11 N2 101.73(13) . . ? N1 C11 Fe1 143.42(12) . . ? N2 C11 Fe1 114.84(11) . . ? C13 C12 C17 122.36(15) . . ? C13 C12 N1 118.72(14) . . ? C17 C12 N1 118.92(14) . . ? C14 C13 C12 117.88(15) . . ? C14 C13 C18 120.25(15) . . ? C12 C13 C18 121.84(15) . . ? C15 C14 C13 120.77(15) . . ? C14 C15 C16 120.39(16) . . ? C15 C16 C17 121.05(16) . . ? C16 C17 C12 117.54(15) . . ? C16 C17 C21 121.60(15) . . ? C12 C17 C21 120.83(14) . . ? C13 C18 C20 112.61(15) . . ? C13 C18 C19 109.89(16) . . ? C20 C18 C19 109.94(15) . . ? C17 C21 C23 113.56(14) . . ? C17 C21 C22 110.78(15) . . ? C23 C21 C22 108.64(14) . . ? C29 C24 C25 122.55(15) . . ? C29 C24 N5 118.36(14) . . ? C25 C24 N5 119.03(14) . . ? C26 C25 C24 117.01(15) . . ? C26 C25 C30 121.53(15) . . ? C24 C25 C30 121.46(15) . . ? C27 C26 C25 121.46(16) . . ? C28 C27 C26 120.35(16) . . ? C27 C28 C29 120.68(16) . . ? C28 C29 C24 117.93(15) . . ? C28 C29 C33 119.80(15) . . ? C24 C29 C33 122.25(15) . . ? C25 C30 C31 113.15(14) . . ? C25 C30 C32 111.42(14) . . ? C31 C30 C32 109.64(15) . . ? C29 C33 C34 111.76(14) . . ? C29 C33 C35 110.55(14) . . ? C34 C33 C35 109.77(14) . . ? N8 C36 C37 124.93(15) . . ? C36 C37 C38 119.78(15) . . ? N9 C38 C39 121.90(15) . . ? N9 C38 C37 122.88(15) . . ? C39 C38 C37 115.21(15) . . ? C40 C39 C38 120.62(15) . . ? N8 C40 C39 124.51(16) . . ? C11 N1 C1 111.36(13) . . ? C11 N1 C12 123.95(13) . . ? C1 N1 C12 124.48(13) . . ? C3 N2 C2 131.53(14) . . ? C3 N2 C11 115.85(14) . . ? C2 N2 C11 112.35(13) . . ? C3 N3 C7 116.96(13) . . ? C3 N3 Fe1 121.80(11) . . ? C7 N3 Fe1 121.14(11) . . ? C7 N4 C8 131.32(14) . . ? C7 N4 C10 116.29(13) . . ? C8 N4 C10 112.36(13) . . ? C10 N5 C9 111.53(13) . . ? C10 N5 C24 126.43(13) . . ? C9 N5 C24 122.02(14) . . ? N7 N6 Fe1 179.17(14) . . ? C40 N8 C36 114.93(14) . . ? C40 N8 Fe1 124.23(11) . . ? C36 N8 Fe1 120.74(11) . . ? C38 N9 C41 122.38(15) . . ? C38 N9 C42 119.48(15) . . ? C41 N9 C42 117.32(15) . . ? N6 Fe1 N3 160.62(6) . . ? N6 Fe1 C10 98.33(6) . . ? N3 Fe1 C10 79.39(6) . . ? N6 Fe1 C11 98.34(6) . . ? N3 Fe1 C11 79.05(6) . . ? C10 Fe1 C11 155.79(7) . . ? N6 Fe1 N8 97.00(6) . . ? N3 Fe1 N8 102.36(6) . . ? C10 Fe1 N8 94.26(6) . . ? C11 Fe1 N8 100.99(6) . . ? C2S O1S C3S 112.01(17) . . ? 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 N1 C1 C2 N2 0.34(18) . . . . ? N3 C3 C4 C5 -0.7(2) . . . . ? N2 C3 C4 C5 -177.57(15) . . . . ? C3 C4 C5 C6 0.4(2) . . . . ? C4 C5 C6 C7 0.1(2) . . . . ? C5 C6 C7 N3 -0.4(2) . . . . ? C5 C6 C7 N4 175.18(15) . . . . ? N4 C8 C9 N5 0.38(18) . . . . ? C17 C12 C13 C14 -0.8(2) . . . . ? N1 C12 C13 C14 178.78(14) . . . . ? C17 C12 C13 C18 177.27(16) . . . . ? N1 C12 C13 C18 -3.2(2) . . . . ? C12 C13 C14 C15 0.3(2) . . . . ? C18 C13 C14 C15 -177.77(16) . . . . ? C13 C14 C15 C16 0.2(3) . . . . ? C14 C15 C16 C17 -0.2(3) . . . . ? C15 C16 C17 C12 -0.2(2) . . . . ? C15 C16 C17 C21 177.72(16) . . . . ? C13 C12 C17 C16 0.7(2) . . . . ? N1 C12 C17 C16 -178.83(14) . . . . ? C13 C12 C17 C21 -177.21(15) . . . . ? N1 C12 C17 C21 3.2(2) . . . . ? C14 C13 C18 C20 -49.2(2) . . . . ? C12 C13 C18 C20 132.79(17) . . . . ? C14 C13 C18 C19 73.7(2) . . . . ? C12 C13 C18 C19 -104.29(19) . . . . ? C16 C17 C21 C23 27.4(2) . . . . ? C12 C17 C21 C23 -154.76(15) . . . . ? C16 C17 C21 C22 -95.22(19) . . . . ? C12 C17 C21 C22 82.65(19) . . . . ? C29 C24 C25 C26 -1.0(2) . . . . ? N5 C24 C25 C26 176.38(14) . . . . ? C29 C24 C25 C30 179.14(15) . . . . ? N5 C24 C25 C30 -3.5(2) . . . . ? C24 C25 C26 C27 -0.1(2) . . . . ? C30 C25 C26 C27 179.77(16) . . . . ? C25 C26 C27 C28 0.9(3) . . . . ? C26 C27 C28 C29 -0.7(3) . . . . ? C27 C28 C29 C24 -0.4(3) . . . . ? C27 C28 C29 C33 -178.79(16) . . . . ? C25 C24 C29 C28 1.2(2) . . . . ? N5 C24 C29 C28 -176.14(14) . . . . ? C25 C24 C29 C33 179.58(15) . . . . ? N5 C24 C29 C33 2.2(2) . . . . ? C26 C25 C30 C31 18.8(2) . . . . ? C24 C25 C30 C31 -161.26(15) . . . . ? C26 C25 C30 C32 -105.24(19) . . . . ? C24 C25 C30 C32 74.7(2) . . . . ? C28 C29 C33 C34 -51.3(2) . . . . ? C24 C29 C33 C34 130.37(17) . . . . ? C28 C29 C33 C35 71.3(2) . . . . ? C24 C29 C33 C35 -107.04(18) . . . . ? N8 C36 C37 C38 -0.4(3) . . . . ? C36 C37 C38 N9 -179.27(16) . . . . ? C36 C37 C38 C39 0.2(2) . . . . ? N9 C38 C39 C40 179.99(16) . . . . ? C37 C38 C39 C40 0.5(2) . . . . ? C38 C39 C40 N8 -1.1(3) . . . . ? N2 C11 N1 C1 2.17(16) . . . . ? Fe1 C11 N1 C1 -176.80(15) . . . . ? N2 C11 N1 C12 177.14(13) . . . . ? Fe1 C11 N1 C12 -1.8(3) . . . . ? C2 C1 N1 C11 -1.67(19) . . . . ? C2 C1 N1 C12 -176.61(14) . . . . ? C13 C12 N1 C11 -85.53(19) . . . . ? C17 C12 N1 C11 94.06(18) . . . . ? C13 C12 N1 C1 88.79(19) . . . . ? C17 C12 N1 C1 -91.62(19) . . . . ? N3 C3 N2 C2 -171.84(15) . . . . ? C4 C3 N2 C2 5.4(3) . . . . ? N3 C3 N2 C11 1.73(18) . . . . ? C4 C3 N2 C11 179.00(16) . . . . ? C1 C2 N2 C3 174.83(16) . . . . ? C1 C2 N2 C11 1.09(19) . . . . ? N1 C11 N2 C3 -176.79(12) . . . . ? Fe1 C11 N2 C3 2.53(17) . . . . ? N1 C11 N2 C2 -1.99(16) . . . . ? Fe1 C11 N2 C2 177.34(11) . . . . ? C4 C3 N3 C7 0.4(2) . . . . ? N2 C3 N3 C7 177.81(12) . . . . ? C4 C3 N3 Fe1 176.84(12) . . . . ? N2 C3 N3 Fe1 -5.72(17) . . . . ? C6 C7 N3 C3 0.2(2) . . . . ? N4 C7 N3 C3 -176.17(13) . . . . ? C6 C7 N3 Fe1 -176.30(12) . . . . ? N4 C7 N3 Fe1 7.33(16) . . . . ? N3 C7 N4 C8 177.92(15) . . . . ? C6 C7 N4 C8 1.8(3) . . . . ? N3 C7 N4 C10 0.01(18) . . . . ? C6 C7 N4 C10 -176.12(15) . . . . ? C9 C8 N4 C7 -178.03(15) . . . . ? C9 C8 N4 C10 -0.05(18) . . . . ? N5 C10 N4 C7 178.01(12) . . . . ? Fe1 C10 N4 C7 -6.79(16) . . . . ? N5 C10 N4 C8 -0.29(16) . . . . ? Fe1 C10 N4 C8 174.91(10) . . . . ? N4 C10 N5 C9 0.52(16) . . . . ? Fe1 C10 N5 C9 -172.00(15) . . . . ? N4 C10 N5 C24 179.11(13) . . . . ? Fe1 C10 N5 C24 6.6(3) . . . . ? C8 C9 N5 C10 -0.60(18) . . . . ? C8 C9 N5 C24 -179.25(14) . . . . ? C29 C24 N5 C10 -105.83(18) . . . . ? C25 C24 N5 C10 76.7(2) . . . . ? C29 C24 N5 C9 72.62(19) . . . . ? C25 C24 N5 C9 -104.83(17) . . . . ? C39 C40 N8 C36 0.9(2) . . . . ? C39 C40 N8 Fe1 177.15(12) . . . . ? C37 C36 N8 C40 -0.1(2) . . . . ? C37 C36 N8 Fe1 -176.51(13) . . . . ? C39 C38 N9 C41 -174.17(17) . . . . ? C37 C38 N9 C41 5.3(3) . . . . ? C39 C38 N9 C42 -4.8(3) . . . . ? C37 C38 N9 C42 174.62(17) . . . . ? N7 N6 Fe1 N3 147(74) . . . . ? N7 N6 Fe1 C10 65(11) . . . . ? N7 N6 Fe1 C11 -132(11) . . . . ? N7 N6 Fe1 N8 -30(11) . . . . ? C3 N3 Fe1 N6 89.8(2) . . . . ? C7 N3 Fe1 N6 -93.9(2) . . . . ? C3 N3 Fe1 C10 174.72(13) . . . . ? C7 N3 Fe1 C10 -8.96(11) . . . . ? C3 N3 Fe1 C11 5.80(12) . . . . ? C7 N3 Fe1 C11 -177.88(12) . . . . ? C3 N3 Fe1 N8 -93.20(12) . . . . ? C7 N3 Fe1 N8 83.12(12) . . . . ? N5 C10 Fe1 N6 -19.5(2) . . . . ? N4 C10 Fe1 N6 168.51(10) . . . . ? N5 C10 Fe1 N3 -180.0(2) . . . . ? N4 C10 Fe1 N3 8.03(10) . . . . ? N5 C10 Fe1 C11 -152.60(17) . . . . ? N4 C10 Fe1 C11 35.4(2) . . . . ? N5 C10 Fe1 N8 78.21(19) . . . . ? N4 C10 Fe1 N8 -93.76(11) . . . . ? N1 C11 Fe1 N6 14.16(19) . . . . ? N2 C11 Fe1 N6 -164.73(11) . . . . ? N1 C11 Fe1 N3 174.68(19) . . . . ? N2 C11 Fe1 N3 -4.21(10) . . . . ? N1 C11 Fe1 C10 147.25(17) . . . . ? N2 C11 Fe1 C10 -31.6(2) . . . . ? N1 C11 Fe1 N8 -84.69(19) . . . . ? N2 C11 Fe1 N8 96.41(11) . . . . ? C40 N8 Fe1 N6 -17.06(13) . . . . ? C36 N8 Fe1 N6 158.99(12) . . . . ? C40 N8 Fe1 N3 163.95(13) . . . . ? C36 N8 Fe1 N3 -20.01(13) . . . . ? C40 N8 Fe1 C10 -116.00(13) . . . . ? C36 N8 Fe1 C10 60.05(13) . . . . ? C40 N8 Fe1 C11 82.90(13) . . . . ? C36 N8 Fe1 C11 -101.06(12) . . . . ? C1S C2S O1S C3S -175.20(18) . . . . ? C4S C3S O1S C2S -171.43(19) . . . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 'ACTA 50' _diffrn_measured_fraction_theta_full 'ACTA 50' _refine_diff_density_max 0.286 _refine_diff_density_min -0.280 _refine_diff_density_rms 0.039