# Supplementary Material (ESI) for Organic & Biomolecular Chemistry # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Org.Biomol.Chem. # SUBMISSION DETAILS _journal_coden_Cambridge 0177 _audit_creation_method 'manual editing of SHELXL template' _publ_contact_author_name 'Dr Heinz-Bernard Kraatz' _publ_contact_author_address ; Department of Chemistry University of Saskatchewan Saskatoon, Saskatchewan S7N 5C9 Canada ; _publ_contact_author_email kraatz@skyway.usask.ca _publ_contact_author_fax '001 306 966 4730' _publ_contact_author_phone '001 306 966 4660' _publ_contact_letter ; To: Cambridge Crystallographic Data Centre Please accept the following CIF file which is being submitted in support of an upcoming communication to be published in Organic and Biomolecular Chemistry. Please forward any questions concerning this CIF to Dr. Gabriele Schatte (gabriele.schatte@usask.ca). ; # TITLE AND AUTHOR LIST _publ_section_title ; Amino acid conjugates of 1,1'-diaminoferrocene. Synthesis and chiral organisation ; loop_ _publ_author_name _publ_author_address H.-B.Kraatz ; Department of Chemistry University of Saskatchewan Saskatoon, Saskatchewan S7N 5C9 Canada ; G.Schatte ; Saskatchewan Structural Sciences Centre University of Saskatchewan Saskatoon, Saskatchewan S7N 5C9 Canada ; S.Chowdhury ; Department of Chemistry University of Saskatchewan Saskatoon, Saskatchewan S7N 5C9 Canada ; K.A.Mahmoud ; Department of Chemistry University of Saskatchewan Saskatoon, Saskatchewan S7N 5C9 Canada ; _publ_section_acknowledgements ; NSERC, CFI ; #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 265455' # originally saved as bksc0406 # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H28 Fe N2 O4' _chemical_formula_sum 'C20 H28 Fe N2 O4' _chemical_formula_weight 416.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' # Crystal Data _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall '-P 2yn' 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 10.81160(10) _cell_length_b 11.80650(10) _cell_length_c 40.9023(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.0490(4) _cell_angle_gamma 90.00 _cell_volume 5220.19(8) _cell_formula_units_Z 10 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 11860 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 30.03 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.324 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2200 _exptl_absorpt_coefficient_mu 0.748 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8647 _exptl_absorpt_correction_T_max 0.8647 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski & Minor 1997)' _exptl_special_details ; ? ; # EXPERIMENTAL DETAIL _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR590D, fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type 'KappaCCD (BruKer AXS-Nonius, FR540C)' _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'no decay' _diffrn_reflns_number 17111 _diffrn_reflns_av_R_equivalents 0.0418 _diffrn_reflns_av_sigmaI/netI 0.0684 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -51 _diffrn_reflns_limit_l_max 51 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 26.37 _reflns_number_total 10080 _reflns_number_gt 7236 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution ; 'SHELXS-97 (Sheldrick, 1997)' ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; Cameron (WinGX v1.64-05), Ortep (SHELXTL-NT v6.14, Bruker AXS) ; _computing_publication_material 'WinGX v1.70.01 (L. J. Farrugia)' # REFINEMENT DATA _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^ > 2sigma(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^)+(0.0427P)^2^+3.1301P] 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 10080 _refine_ls_number_parameters 625 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0767 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.1136 _refine_ls_wR_factor_gt 0.1013 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 Fe1 Fe 0.66185(4) -0.08479(4) 0.213341(10) 0.02405(12) Uani 1 1 d . . . Fe2 Fe 0.62424(3) 0.37751(4) 0.127963(10) 0.02336(12) Uani 1 1 d . . . Fe3 Fe 0.5000 0.5000 0.0000 0.01961(14) Uani 1 2 d S . . O11 O 0.34182(17) -0.0418(2) 0.22345(5) 0.0338(5) Uani 1 1 d . . . O12 O 0.27896(18) 0.07086(19) 0.17943(5) 0.0340(5) Uani 1 1 d . . . O21 O 0.57496(17) 0.10283(19) 0.31705(5) 0.0324(5) Uani 1 1 d . . . O22 O 0.39027(17) 0.05609(19) 0.30449(5) 0.0329(5) Uani 1 1 d . . . O31 O 0.78304(18) 0.64876(19) 0.06938(5) 0.0316(5) Uani 1 1 d . . . O32 O 0.86864(18) 0.76117(18) 0.10998(5) 0.0294(5) Uani 1 1 d . . . O41 O 0.47238(18) 0.08099(18) 0.11474(5) 0.0303(5) Uani 1 1 d . . . O42 O 0.34391(18) 0.10641(18) 0.07294(5) 0.0309(5) Uani 1 1 d . . . O51 O 0.26782(17) 0.38059(18) 0.05042(5) 0.0270(5) Uani 1 1 d . . . O52 O 0.12034(17) 0.3156(2) 0.01797(5) 0.0347(6) Uani 1 1 d . . . N11 N 0.4323(2) -0.0424(2) 0.17456(6) 0.0281(6) Uani 1 1 d . . . H11 H 0.4289 -0.0162 0.1544 0.034 Uiso 1 1 calc . . . N21 N 0.5214(2) 0.0058(3) 0.27002(6) 0.0400(8) Uani 1 1 d . . . H21 H 0.4603 -0.0337 0.2612 0.048 Uiso 1 1 calc . . . N31 N 0.8225(2) 0.5685(2) 0.11987(6) 0.0242(6) Uani 1 1 d . . . H31 H 0.8527 0.5852 0.1394 0.029 Uiso 1 1 calc . . . N41 N 0.3912(2) 0.2677(2) 0.10265(6) 0.0230(5) Uani 1 1 d . . . H41 H 0.3350 0.2991 0.0897 0.028 Uiso 1 1 calc . . . N51 N 0.29030(19) 0.3213(2) -0.00278(6) 0.0250(6) Uani 1 1 d . . . H51 H 0.2491 0.2941 -0.0198 0.030 Uiso 1 1 calc . . . C10 C 0.5247(2) -0.1194(3) 0.18278(7) 0.0241(7) Uani 1 1 d . . . C11 C 0.6274(3) -0.1181(3) 0.16482(7) 0.0287(7) Uani 1 1 d . . . H11A H 0.6477 -0.0679 0.1476 0.034 Uiso 1 1 calc . . . C12 C 0.6997(3) -0.2107(3) 0.17795(8) 0.0356(8) Uani 1 1 d . . . H12 H 0.7783 -0.2314 0.1699 0.043 Uiso 1 1 calc . . . C13 C 0.6423(3) -0.2680(3) 0.20404(8) 0.0323(8) Uani 1 1 d . . . H13 H 0.6722 -0.3309 0.2163 0.039 Uiso 1 1 calc . . . C14 C 0.5351(3) -0.2117(3) 0.20717(7) 0.0275(7) Uani 1 1 d . . . H14 H 0.4743 -0.2288 0.2229 0.033 Uiso 1 1 calc . . . C15 C 0.3497(2) -0.0069(3) 0.19528(7) 0.0255(7) Uani 1 1 d . . . C16 C 0.2006(3) 0.1507(3) 0.19788(9) 0.0395(9) Uani 1 1 d . . . C17 C 0.1487(4) 0.2292(4) 0.17062(10) 0.0612(12) Uani 1 1 d . . . H17A H 0.2169 0.2703 0.1606 0.073 Uiso 1 1 calc R . . H17B H 0.0907 0.2834 0.1801 0.073 Uiso 1 1 calc R . . H17C H 0.1055 0.1836 0.1540 0.073 Uiso 1 1 calc R . . C18 C 0.2680(3) 0.2298(3) 0.22203(9) 0.0516(10) Uani 1 1 d . . . H18A H 0.3019 0.1854 0.2404 0.062 Uiso 1 1 calc R . . H18B H 0.2097 0.2861 0.2303 0.062 Uiso 1 1 calc R . . H18C H 0.3355 0.2684 0.2109 0.062 Uiso 1 1 calc R . . C19 C 0.1101(3) 0.0743(3) 0.21416(10) 0.0537(11) Uani 1 1 d . . . H19A H 0.0748 0.0216 0.1980 0.064 Uiso 1 1 calc R . . H19B H 0.0438 0.1198 0.2236 0.064 Uiso 1 1 calc R . . H19C H 0.1525 0.0316 0.2316 0.064 Uiso 1 1 calc R . . C20 C 0.6289(3) 0.0107(3) 0.25452(7) 0.0308(8) Uani 1 1 d . . . C21 C 0.7216(3) -0.0693(3) 0.26025(7) 0.0332(8) Uani 1 1 d . . . H21A H 0.7246 -0.1301 0.2754 0.040 Uiso 1 1 calc . . . C22 C 0.8069(3) -0.0359(3) 0.23795(8) 0.0377(9) Uani 1 1 d . . . H22 H 0.8838 -0.0732 0.2351 0.045 Uiso 1 1 calc . . . C23 C 0.7674(3) 0.0640(3) 0.21879(8) 0.0387(9) Uani 1 1 d . . . H23 H 0.8130 0.1001 0.2021 0.046 Uiso 1 1 calc . . . C24 C 0.6564(3) 0.0943(3) 0.22908(8) 0.0347(8) Uani 1 1 d . . . H24 H 0.6065 0.1557 0.2217 0.042 Uiso 1 1 calc . . . C25 C 0.5028(3) 0.0600(3) 0.29905(7) 0.0254(7) Uani 1 1 d . . . C26 C 0.3382(3) 0.1327(3) 0.33010(7) 0.0315(8) Uani 1 1 d . . . C27 C 0.3683(3) 0.0826(4) 0.36360(8) 0.0514(11) Uani 1 1 d . . . H27A H 0.3173 0.1193 0.3801 0.062 Uiso 1 1 calc R . . H27B H 0.4560 0.0952 0.3690 0.062 Uiso 1 1 calc R . . H27C H 0.3512 0.0011 0.3633 0.062 Uiso 1 1 calc R . . C28 C 0.3713(3) 0.2661(3) 0.32552(10) 0.0544(11) Uani 1 1 d . . . H28A H 0.3537 0.2887 0.3029 0.065 Uiso 1 1 calc R . . H28B H 0.4591 0.2784 0.3307 0.065 Uiso 1 1 calc R . . H28C H 0.3209 0.3116 0.3403 0.065 Uiso 1 1 calc R . . C29 C 0.2131(3) 0.1160(4) 0.32223(9) 0.0526(11) Uani 1 1 d . . . H29A H 0.1965 0.1407 0.2997 0.063 Uiso 1 1 calc R . . H29B H 0.1622 0.1601 0.3372 0.063 Uiso 1 1 calc R . . H29C H 0.1929 0.0354 0.3243 0.063 Uiso 1 1 calc R . . C30 C 0.7802(2) 0.4477(3) 0.11533(7) 0.0231(7) Uani 1 1 d . . . C31 C 0.7227(2) 0.3962(3) 0.08768(7) 0.0247(7) Uani 1 1 d . . . H31A H 0.7005 0.4341 0.0680 0.030 Uiso 1 1 calc . . . C32 C 0.7017(3) 0.2697(3) 0.09440(8) 0.0301(7) Uani 1 1 d . . . H32 H 0.6656 0.2174 0.0794 0.036 Uiso 1 1 calc . . . C33 C 0.7442(3) 0.2434(3) 0.12635(8) 0.0333(8) Uani 1 1 d . . . H33 H 0.7428 0.1720 0.1371 0.040 Uiso 1 1 calc . . . C34 C 0.7923(3) 0.3539(3) 0.13945(7) 0.0300(7) Uani 1 1 d . . . H34 H 0.8268 0.3630 0.1608 0.036 Uiso 1 1 calc . . . C35 C 0.8207(2) 0.6590(3) 0.09709(7) 0.0241(7) Uani 1 1 d . . . C36 C 0.8878(3) 0.8722(3) 0.08979(8) 0.0312(7) Uani 1 1 d . . . C37 C 0.9405(4) 0.9600(3) 0.11475(9) 0.0490(10) Uani 1 1 d . . . H37A H 0.9503 1.0334 0.1039 0.059 Uiso 1 1 calc R . . H37B H 1.0211 0.9340 0.1231 0.059 Uiso 1 1 calc R . . H37C H 0.8834 0.9679 0.1329 0.059 Uiso 1 1 calc R . . C38 C 0.7767(3) 0.9235(3) 0.07661(9) 0.0426(9) Uani 1 1 d . . . H38A H 0.7975 0.9950 0.0659 0.051 Uiso 1 1 calc R . . H38B H 0.7192 0.9382 0.0944 0.051 Uiso 1 1 calc R . . H38C H 0.7378 0.8721 0.0606 0.051 Uiso 1 1 calc R . . C39 C 0.9706(3) 0.8405(3) 0.06275(9) 0.0492(10) Uani 1 1 d . . . H39A H 0.9263 0.7903 0.0475 0.059 Uiso 1 1 calc R . . H39B H 1.0436 0.8013 0.0717 0.059 Uiso 1 1 calc R . . H39C H 0.9965 0.9090 0.0512 0.059 Uiso 1 1 calc R . . C40 C 0.4528(2) 0.3425(3) 0.12483(7) 0.0242(7) Uani 1 1 d . . . C41 C 0.4960(3) 0.3142(3) 0.15661(7) 0.0326(8) Uani 1 1 d . . . H41A H 0.4943 0.2423 0.1670 0.039 Uiso 1 1 calc . . . C42 C 0.5445(3) 0.4227(3) 0.16995(7) 0.0370(9) Uani 1 1 d . . . H42 H 0.5798 0.4299 0.1913 0.044 Uiso 1 1 calc . . . C43 C 0.5323(3) 0.5187(3) 0.14679(8) 0.0343(8) Uani 1 1 d . . . H43 H 0.5566 0.5952 0.1501 0.041 Uiso 1 1 calc . . . C44 C 0.4760(3) 0.4695(3) 0.11860(7) 0.0280(7) Uani 1 1 d . . . H44 H 0.4557 0.5087 0.0989 0.034 Uiso 1 1 calc . . . C45 C 0.4084(2) 0.1450(3) 0.09841(7) 0.0249(7) Uani 1 1 d . . . C46 C 0.3573(3) -0.0194(3) 0.05943(8) 0.0317(8) Uani 1 1 d . . . C47 C 0.3216(4) -0.1140(3) 0.08455(9) 0.0525(11) Uani 1 1 d . . . H47A H 0.3142 -0.1869 0.0732 0.063 Uiso 1 1 calc R . . H47B H 0.2424 -0.0949 0.0944 0.063 Uiso 1 1 calc R . . H47C H 0.3859 -0.1193 0.1017 0.063 Uiso 1 1 calc R . . C48 C 0.4780(3) -0.0366(3) 0.04827(9) 0.0449(9) Uani 1 1 d . . . H48A H 0.4817 -0.1084 0.0363 0.054 Uiso 1 1 calc R . . H48B H 0.5358 -0.0389 0.0670 0.054 Uiso 1 1 calc R . . H48C H 0.5007 0.0257 0.0337 0.054 Uiso 1 1 calc R . . C49 C 0.2761(3) -0.0168(3) 0.03021(9) 0.0530(11) Uani 1 1 d . . . H49A H 0.3046 0.0421 0.0152 0.064 Uiso 1 1 calc R . . H49B H 0.1912 -0.0001 0.0367 0.064 Uiso 1 1 calc R . . H49C H 0.2784 -0.0905 0.0192 0.064 Uiso 1 1 calc R . . C50 C 0.4086(2) 0.3395(2) -0.00505(7) 0.0221(6) Uani 1 1 d . . . C51 C 0.4620(2) 0.3697(2) -0.03482(7) 0.0222(6) Uani 1 1 d . . . H51A H 0.4207 0.3839 -0.0551 0.027 Uiso 1 1 calc . . . C52 C 0.5805(2) 0.3741(3) -0.02862(7) 0.0247(7) Uani 1 1 d . . . H52 H 0.6427 0.3923 -0.0438 0.030 Uiso 1 1 calc . . . C53 C 0.6004(2) 0.3468(3) 0.00500(7) 0.0258(7) Uani 1 1 d . . . H53 H 0.6795 0.3439 0.0155 0.031 Uiso 1 1 calc . . . C54 C 0.4936(2) 0.3258(3) 0.01997(7) 0.0242(7) Uani 1 1 d . . . H54 H 0.4801 0.3064 0.0422 0.029 Uiso 1 1 calc . . . C55 C 0.2299(2) 0.3428(3) 0.02462(7) 0.0236(7) Uani 1 1 d . . . C56 C 0.0330(3) 0.3318(3) 0.04326(8) 0.0347(8) Uani 1 1 d . . . C57 C 0.0200(3) 0.4669(3) 0.05105(9) 0.0470(10) Uani 1 1 d . . . H57A H 0.0996 0.4964 0.0591 0.056 Uiso 1 1 calc R . . H57B H -0.0428 0.4783 0.0677 0.056 Uiso 1 1 calc R . . H57C H -0.0048 0.5071 0.0310 0.056 Uiso 1 1 calc R . . C58 C 0.0617(3) 0.2572(3) 0.07352(9) 0.0491(10) Uani 1 1 d . . . H58A H 0.0828 0.1805 0.0664 0.059 Uiso 1 1 calc R . . H58B H -0.0112 0.2542 0.0874 0.059 Uiso 1 1 calc R . . H58C H 0.1315 0.2897 0.0859 0.059 Uiso 1 1 calc R . . C59 C -0.0714(3) 0.2797(4) 0.02605(10) 0.0658(13) Uani 1 1 d . . . H59A H -0.0883 0.3208 0.0056 0.079 Uiso 1 1 calc R . . H59B H -0.1446 0.2827 0.0398 0.079 Uiso 1 1 calc R . . H59C H -0.0518 0.2006 0.0211 0.079 Uiso 1 1 calc R . . 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 0.0176(2) 0.0339(3) 0.0206(2) -0.00479(19) 0.00022(17) -0.00038(18) Fe2 0.0147(2) 0.0324(3) 0.0230(2) -0.00355(19) 0.00245(16) -0.00283(18) Fe3 0.0116(3) 0.0272(3) 0.0201(3) -0.0030(2) 0.0032(2) 0.0006(2) O11 0.0159(10) 0.0626(16) 0.0231(12) 0.0023(11) 0.0007(9) -0.0023(10) O12 0.0219(11) 0.0480(15) 0.0320(12) -0.0035(11) 0.0011(9) 0.0116(10) O21 0.0170(10) 0.0601(16) 0.0201(11) -0.0075(10) -0.0017(9) -0.0032(10) O22 0.0158(10) 0.0544(15) 0.0285(12) -0.0094(10) 0.0043(9) -0.0012(10) O31 0.0240(11) 0.0482(15) 0.0224(12) 0.0017(10) -0.0053(9) -0.0046(10) O32 0.0264(11) 0.0335(13) 0.0283(12) 0.0020(10) -0.0018(9) -0.0076(9) O41 0.0246(11) 0.0392(14) 0.0272(12) 0.0098(10) -0.0012(9) 0.0016(10) O42 0.0223(10) 0.0360(14) 0.0342(13) -0.0093(10) -0.0061(9) 0.0003(9) O51 0.0162(10) 0.0474(14) 0.0176(11) 0.0006(10) -0.0006(8) 0.0009(9) O52 0.0124(10) 0.0662(17) 0.0258(12) -0.0077(11) 0.0070(9) -0.0046(10) N11 0.0203(12) 0.0445(16) 0.0196(13) 0.0047(12) 0.0005(10) 0.0057(12) N21 0.0139(12) 0.075(2) 0.0307(16) -0.0245(15) 0.0005(11) -0.0074(13) N31 0.0164(12) 0.0353(16) 0.0207(13) -0.0009(11) -0.0009(10) -0.0053(11) N41 0.0133(11) 0.0312(15) 0.0243(13) -0.0017(11) -0.0050(10) -0.0025(10) N51 0.0103(11) 0.0446(17) 0.0201(13) -0.0034(11) 0.0008(9) -0.0065(11) C10 0.0201(14) 0.0325(18) 0.0196(15) -0.0028(13) -0.0016(12) -0.0004(13) C11 0.0255(15) 0.045(2) 0.0162(15) -0.0051(14) 0.0022(12) 0.0028(14) C12 0.0261(16) 0.048(2) 0.0326(19) -0.0152(16) -0.0020(14) 0.0076(15) C13 0.0342(18) 0.0281(19) 0.0342(19) -0.0032(14) -0.0121(14) 0.0047(14) C14 0.0248(15) 0.0334(19) 0.0243(16) -0.0004(14) -0.0030(13) -0.0050(14) C15 0.0170(14) 0.0338(19) 0.0257(17) -0.0038(14) -0.0016(12) -0.0025(13) C16 0.0273(17) 0.043(2) 0.048(2) -0.0102(17) 0.0064(16) 0.0082(15) C17 0.046(2) 0.065(3) 0.072(3) -0.001(2) 0.001(2) 0.028(2) C18 0.041(2) 0.058(3) 0.057(3) -0.018(2) 0.0098(19) -0.0006(19) C19 0.0262(18) 0.069(3) 0.067(3) -0.012(2) 0.0113(18) 0.0024(18) C20 0.0194(15) 0.050(2) 0.0227(16) -0.0122(15) -0.0003(12) -0.0029(14) C21 0.0219(15) 0.053(2) 0.0243(17) -0.0038(15) -0.0052(13) 0.0016(15) C22 0.0192(15) 0.063(2) 0.0310(19) -0.0180(17) -0.0009(13) -0.0007(16) C23 0.0276(17) 0.053(2) 0.0357(19) -0.0138(17) 0.0053(15) -0.0154(16) C24 0.0283(17) 0.034(2) 0.042(2) -0.0115(16) -0.0011(14) -0.0024(14) C25 0.0159(14) 0.0360(19) 0.0243(16) 0.0024(14) 0.0016(12) 0.0015(13) C26 0.0185(14) 0.047(2) 0.0289(18) -0.0030(15) 0.0054(13) 0.0045(14) C27 0.0342(19) 0.091(3) 0.030(2) -0.002(2) 0.0082(16) 0.006(2) C28 0.040(2) 0.055(3) 0.069(3) -0.009(2) 0.012(2) 0.0077(19) C29 0.0171(16) 0.093(3) 0.048(2) 0.001(2) 0.0054(16) 0.0035(18) C30 0.0113(13) 0.0328(18) 0.0252(16) -0.0017(13) 0.0006(11) -0.0003(12) C31 0.0146(13) 0.0372(19) 0.0222(16) -0.0039(13) 0.0031(12) -0.0028(13) C32 0.0193(15) 0.036(2) 0.0356(19) -0.0087(15) 0.0051(13) -0.0004(14) C33 0.0201(15) 0.0321(19) 0.048(2) 0.0058(16) 0.0049(14) 0.0052(14) C34 0.0199(14) 0.040(2) 0.0299(18) 0.0030(15) -0.0038(13) -0.0007(14) C35 0.0142(13) 0.0370(19) 0.0213(16) 0.0002(14) 0.0028(12) 0.0012(13) C36 0.0268(16) 0.0333(19) 0.0336(19) 0.0061(15) 0.0023(14) -0.0028(14) C37 0.050(2) 0.041(2) 0.055(3) 0.0053(19) -0.0053(19) -0.0153(18) C38 0.042(2) 0.047(2) 0.039(2) 0.0070(17) 0.0015(16) 0.0076(17) C39 0.0293(18) 0.065(3) 0.054(2) 0.009(2) 0.0134(17) -0.0101(18) C40 0.0151(13) 0.0377(19) 0.0200(16) -0.0049(13) 0.0036(11) -0.0044(13) C41 0.0188(15) 0.055(2) 0.0240(17) 0.0042(15) 0.0022(12) -0.0073(15) C42 0.0215(16) 0.068(3) 0.0219(17) -0.0129(17) 0.0034(13) -0.0064(16) C43 0.0171(15) 0.042(2) 0.044(2) -0.0196(17) 0.0064(14) -0.0012(14) C44 0.0164(14) 0.0378(19) 0.0298(17) -0.0064(14) 0.0043(12) 0.0000(13) C45 0.0149(13) 0.037(2) 0.0228(16) 0.0011(14) 0.0041(12) -0.0052(13) C46 0.0240(16) 0.032(2) 0.039(2) -0.0086(15) -0.0011(14) -0.0037(14) C47 0.058(2) 0.041(2) 0.059(3) -0.0083(19) 0.014(2) -0.0189(19) C48 0.0320(18) 0.055(2) 0.048(2) -0.0123(19) 0.0036(16) 0.0016(17) C49 0.042(2) 0.062(3) 0.054(3) -0.024(2) -0.0130(19) -0.0050(19) C50 0.0141(13) 0.0283(17) 0.0239(16) -0.0015(13) 0.0023(11) -0.0017(12) C51 0.0169(13) 0.0297(17) 0.0201(15) -0.0047(13) 0.0032(11) -0.0017(12) C52 0.0168(14) 0.0305(18) 0.0269(17) -0.0070(13) 0.0062(12) 0.0010(13) C53 0.0128(13) 0.0317(18) 0.0329(18) -0.0076(14) -0.0026(12) 0.0038(12) C54 0.0178(14) 0.0312(18) 0.0237(16) 0.0013(13) 0.0018(12) 0.0006(13) C55 0.0151(14) 0.0295(18) 0.0264(17) 0.0040(13) 0.0043(12) -0.0004(12) C56 0.0139(14) 0.059(2) 0.0315(18) -0.0008(16) 0.0127(13) 0.0006(15) C57 0.0314(18) 0.066(3) 0.044(2) 0.0047(19) 0.0117(16) 0.0139(18) C58 0.0342(19) 0.064(3) 0.050(2) 0.018(2) 0.0181(17) 0.0019(18) C59 0.0166(17) 0.125(4) 0.056(3) -0.017(3) 0.0111(17) -0.014(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; # MOLECULAR GEOMETRY 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 C22 1.936(3) . ? Fe1 C10 1.965(3) . ? Fe1 C21 2.021(3) . ? Fe1 C14 2.043(3) . ? Fe1 C11 2.051(3) . ? Fe1 C20 2.063(3) . ? Fe1 C23 2.104(3) . ? Fe1 C12 2.120(3) . ? Fe1 C13 2.206(3) . ? Fe1 C24 2.211(3) . ? Fe2 C34 1.890(3) . ? Fe2 C40 1.901(3) . ? Fe2 C30 1.956(3) . ? Fe2 C44 1.968(3) . ? Fe2 C41 1.979(3) . ? Fe2 C31 1.990(3) . ? Fe2 C42 2.008(3) . ? Fe2 C33 2.049(3) . ? Fe2 C32 2.061(3) . ? Fe2 C43 2.094(3) . ? Fe3 C52 2.091(3) . ? Fe3 C52 2.091(3) 3_665 ? Fe3 C53 2.117(3) 3_665 ? Fe3 C53 2.117(3) . ? Fe3 C51 2.131(3) . ? Fe3 C51 2.131(3) 3_665 ? Fe3 C50 2.146(3) 3_665 ? Fe3 C50 2.146(3) . ? Fe3 C54 2.215(3) 3_665 ? Fe3 C54 2.215(3) . ? O11 C15 1.228(3) . ? O12 C15 1.353(4) . ? O12 C16 1.483(4) . ? O21 C25 1.177(3) . ? O22 C25 1.242(3) . ? O22 C26 1.501(3) . ? O31 C35 1.203(3) . ? O32 C35 1.411(4) . ? O32 C36 1.565(4) . ? O41 C45 1.217(3) . ? O42 C45 1.324(3) . ? O42 C46 1.592(4) . ? O51 C55 1.210(3) . ? O52 C55 1.253(3) . ? O52 C56 1.426(3) . ? N11 C15 1.312(3) . ? N11 C10 1.387(4) . ? N11 H11 0.8800 . ? N21 C20 1.336(3) . ? N21 C25 1.367(4) . ? N21 H21 0.8800 . ? N31 C35 1.417(4) . ? N31 C30 1.509(4) . ? N31 H31 0.8800 . ? N41 C40 1.423(4) . ? N41 C45 1.471(4) . ? N41 H41 0.8800 . ? N51 C50 1.302(3) . ? N51 C55 1.332(3) . ? N51 H51 0.8800 . ? C10 C11 1.343(4) . ? C10 C14 1.481(4) . ? C11 C12 1.442(5) . ? C11 H11A 0.9500 . ? C12 C13 1.417(4) . ? C12 H12 0.9500 . ? C13 C14 1.345(4) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C16 C19 1.495(5) . ? C16 C18 1.534(5) . ? C16 C17 1.548(5) . ? 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 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.393(4) . ? C20 C24 1.469(5) . ? C21 C22 1.367(4) . ? C21 H21A 0.9500 . ? C22 C23 1.475(5) . ? C22 H22 0.9500 . ? C23 C24 1.327(4) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C26 C29 1.399(4) . ? C26 C27 1.522(4) . ? C26 C28 1.627(5) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.418(4) . ? C30 C34 1.487(4) . ? C31 C32 1.535(4) . ? C31 H31A 0.9500 . ? C32 C33 1.412(4) . ? C32 H32 0.9500 . ? C33 C34 1.500(4) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C36 C38 1.442(4) . ? C36 C39 1.483(4) . ? C36 C37 1.556(5) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.413(4) . ? C40 C44 1.542(4) . ? C41 C42 1.485(5) . ? C41 H41A 0.9500 . ? C42 C43 1.481(5) . ? C42 H42 0.9500 . ? C43 C44 1.418(4) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C46 C48 1.406(4) . ? C46 C49 1.470(5) . ? C46 C47 1.571(5) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 C54 1.372(4) . ? C50 C51 1.403(4) . ? C51 C52 1.302(4) . ? C51 H51A 0.9500 . ? C52 C53 1.425(4) . ? C52 H52 0.9500 . ? C53 C54 1.341(4) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C56 C59 1.456(5) . ? C56 C58 1.546(5) . ? C56 C57 1.633(5) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 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 C22 Fe1 C10 170.92(14) . . ? C22 Fe1 C21 40.34(12) . . ? C10 Fe1 C21 147.89(11) . . ? C22 Fe1 C14 144.90(15) . . ? C10 Fe1 C14 43.31(12) . . ? C21 Fe1 C14 112.68(12) . . ? C22 Fe1 C11 133.73(12) . . ? C10 Fe1 C11 39.00(11) . . ? C21 Fe1 C11 170.11(12) . . ? C14 Fe1 C11 68.32(12) . . ? C22 Fe1 C20 64.07(12) . . ? C10 Fe1 C20 119.58(12) . . ? C21 Fe1 C20 39.88(12) . . ? C14 Fe1 C20 112.10(11) . . ? C11 Fe1 C20 149.76(13) . . ? C22 Fe1 C23 42.56(15) . . ? C10 Fe1 C23 129.96(14) . . ? C21 Fe1 C23 70.17(14) . . ? C14 Fe1 C23 170.56(13) . . ? C11 Fe1 C23 110.53(13) . . ? C20 Fe1 C23 63.81(12) . . ? C22 Fe1 C12 113.56(13) . . ? C10 Fe1 C12 64.69(12) . . ? C21 Fe1 C12 130.49(13) . . ? C14 Fe1 C12 62.53(12) . . ? C11 Fe1 C12 40.41(12) . . ? C20 Fe1 C12 168.22(14) . . ? C23 Fe1 C12 123.14(12) . . ? C22 Fe1 C13 117.15(14) . . ? C10 Fe1 C13 67.52(12) . . ? C21 Fe1 C13 106.28(13) . . ? C14 Fe1 C13 36.64(11) . . ? C11 Fe1 C13 68.29(12) . . ? C20 Fe1 C13 131.24(12) . . ? C23 Fe1 C13 152.50(13) . . ? C12 Fe1 C13 38.16(12) . . ? C22 Fe1 C24 65.73(14) . . ? C10 Fe1 C24 111.12(13) . . ? C21 Fe1 C24 69.32(13) . . ? C14 Fe1 C24 135.72(12) . . ? C11 Fe1 C24 117.36(13) . . ? C20 Fe1 C24 40.00(12) . . ? C23 Fe1 C24 35.72(11) . . ? C12 Fe1 C24 151.13(13) . . ? C13 Fe1 C24 170.04(12) . . ? C34 Fe2 C40 156.46(14) . . ? C34 Fe2 C30 45.46(12) . . ? C40 Fe2 C30 156.66(13) . . ? C34 Fe2 C44 154.98(14) . . ? C40 Fe2 C44 46.94(13) . . ? C30 Fe2 C44 114.70(12) . . ? C34 Fe2 C41 118.58(13) . . ? C40 Fe2 C41 42.66(12) . . ? C30 Fe2 C41 158.94(13) . . ? C44 Fe2 C41 75.31(13) . . ? C34 Fe2 C31 72.28(12) . . ? C40 Fe2 C31 120.25(12) . . ? C30 Fe2 C31 42.09(11) . . ? C44 Fe2 C31 102.94(12) . . ? C41 Fe2 C31 157.43(13) . . ? C34 Fe2 C42 104.65(13) . . ? C40 Fe2 C42 71.45(12) . . ? C30 Fe2 C42 119.94(13) . . ? C44 Fe2 C42 70.04(13) . . ? C41 Fe2 C42 43.72(13) . . ? C31 Fe2 C42 157.42(14) . . ? C34 Fe2 C33 44.54(13) . . ? C40 Fe2 C33 116.53(13) . . ? C30 Fe2 C33 76.68(12) . . ? C44 Fe2 C33 159.09(14) . . ? C41 Fe2 C33 100.26(13) . . ? C31 Fe2 C33 73.16(12) . . ? C42 Fe2 C33 121.00(14) . . ? C34 Fe2 C32 70.97(13) . . ? C40 Fe2 C32 103.18(12) . . ? C30 Fe2 C32 73.92(12) . . ? C44 Fe2 C32 123.40(13) . . ? C41 Fe2 C32 117.31(13) . . ? C31 Fe2 C32 44.51(12) . . ? C42 Fe2 C32 156.91(14) . . ? C33 Fe2 C32 40.20(13) . . ? C34 Fe2 C43 119.13(13) . . ? C40 Fe2 C43 74.30(12) . . ? C30 Fe2 C43 100.21(12) . . ? C44 Fe2 C43 40.73(12) . . ? C41 Fe2 C43 74.96(13) . . ? C31 Fe2 C43 118.75(13) . . ? C42 Fe2 C43 42.26(14) . . ? C33 Fe2 C43 158.72(14) . . ? C32 Fe2 C43 159.66(14) . . ? C52 Fe3 C52 180.0 . 3_665 ? C52 Fe3 C53 140.43(11) . 3_665 ? C52 Fe3 C53 39.57(11) 3_665 3_665 ? C52 Fe3 C53 39.57(11) . . ? C52 Fe3 C53 140.43(11) 3_665 . ? C53 Fe3 C53 180.0 3_665 . ? C52 Fe3 C51 35.91(10) . . ? C52 Fe3 C51 144.09(10) 3_665 . ? C53 Fe3 C51 117.37(11) 3_665 . ? C53 Fe3 C51 62.63(11) . . ? C52 Fe3 C51 144.09(10) . 3_665 ? C52 Fe3 C51 35.91(10) 3_665 3_665 ? C53 Fe3 C51 62.63(11) 3_665 3_665 ? C53 Fe3 C51 117.37(11) . 3_665 ? C51 Fe3 C51 180.0 . 3_665 ? C52 Fe3 C50 119.09(10) . 3_665 ? C52 Fe3 C50 60.91(10) 3_665 3_665 ? C53 Fe3 C50 59.29(11) 3_665 3_665 ? C53 Fe3 C50 120.71(11) . 3_665 ? C51 Fe3 C50 141.70(10) . 3_665 ? C51 Fe3 C50 38.31(10) 3_665 3_665 ? C52 Fe3 C50 60.92(10) . . ? C52 Fe3 C50 119.08(10) 3_665 . ? C53 Fe3 C50 120.71(11) 3_665 . ? C53 Fe3 C50 59.29(11) . . ? C51 Fe3 C50 38.31(10) . . ? C51 Fe3 C50 141.69(10) 3_665 . ? C50 Fe3 C50 180.0 3_665 . ? C52 Fe3 C54 115.95(10) . 3_665 ? C52 Fe3 C54 64.06(10) 3_665 3_665 ? C53 Fe3 C54 35.97(10) 3_665 3_665 ? C53 Fe3 C54 144.04(10) . 3_665 ? C51 Fe3 C54 115.53(11) . 3_665 ? C51 Fe3 C54 64.48(11) 3_665 3_665 ? C50 Fe3 C54 36.64(10) 3_665 3_665 ? C50 Fe3 C54 143.36(10) . 3_665 ? C52 Fe3 C54 64.06(10) . . ? C52 Fe3 C54 115.94(10) 3_665 . ? C53 Fe3 C54 144.03(10) 3_665 . ? C53 Fe3 C54 35.97(10) . . ? C51 Fe3 C54 64.47(11) . . ? C51 Fe3 C54 115.52(11) 3_665 . ? C50 Fe3 C54 143.36(10) 3_665 . ? C50 Fe3 C54 36.64(10) . . ? C54 Fe3 C54 180.0 3_665 . ? C15 O12 C16 120.7(2) . . ? C25 O22 C26 118.9(2) . . ? C35 O32 C36 124.8(2) . . ? C45 O42 C46 123.0(2) . . ? C55 O52 C56 116.4(2) . . ? C15 N11 C10 123.3(3) . . ? C15 N11 H11 118.4 . . ? C10 N11 H11 118.4 . . ? C20 N21 C25 122.4(3) . . ? C20 N21 H21 118.8 . . ? C25 N21 H21 118.8 . . ? C35 N31 C30 129.1(2) . . ? C35 N31 H31 115.4 . . ? C30 N31 H31 115.4 . . ? C40 N41 C45 128.9(2) . . ? C40 N41 H41 115.6 . . ? C45 N41 H41 115.6 . . ? C50 N51 C55 121.7(2) . . ? C50 N51 H51 119.1 . . ? C55 N51 H51 119.1 . . ? C11 C10 N11 117.3(3) . . ? C11 C10 C14 108.9(3) . . ? N11 C10 C14 133.7(2) . . ? C11 C10 Fe1 73.96(18) . . ? N11 C10 Fe1 123.4(2) . . ? C14 C10 Fe1 71.16(17) . . ? C10 C11 C12 103.6(3) . . ? C10 C11 Fe1 67.04(17) . . ? C12 C11 Fe1 72.39(18) . . ? C10 C11 H11A 128.2 . . ? C12 C11 H11A 128.2 . . ? Fe1 C11 H11A 124.1 . . ? C13 C12 C11 113.7(3) . . ? C13 C12 Fe1 74.22(18) . . ? C11 C12 Fe1 67.20(17) . . ? C13 C12 H12 123.2 . . ? C11 C12 H12 123.2 . . ? Fe1 C12 H12 127.1 . . ? C14 C13 C12 103.0(3) . . ? C14 C13 Fe1 65.06(18) . . ? C12 C13 Fe1 67.63(18) . . ? C14 C13 H13 128.5 . . ? C12 C13 H13 128.5 . . ? Fe1 C13 H13 130.1 . . ? C13 C14 C10 110.8(3) . . ? C13 C14 Fe1 78.30(19) . . ? C10 C14 Fe1 65.53(16) . . ? C13 C14 H14 124.6 . . ? C10 C14 H14 124.6 . . ? Fe1 C14 H14 122.9 . . ? O11 C15 N11 124.0(3) . . ? O11 C15 O12 129.0(3) . . ? N11 C15 O12 107.1(3) . . ? O12 C16 C19 103.2(3) . . ? O12 C16 C18 116.4(3) . . ? C19 C16 C18 112.8(3) . . ? O12 C16 C17 102.5(3) . . ? C19 C16 C17 116.8(3) . . ? C18 C16 C17 105.1(3) . . ? 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 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N21 C20 C21 121.4(3) . . ? N21 C20 C24 123.7(3) . . ? C21 C20 C24 114.9(3) . . ? N21 C20 Fe1 121.9(2) . . ? C21 C20 Fe1 68.45(17) . . ? C24 C20 Fe1 75.45(17) . . ? C22 C21 C20 100.6(3) . . ? C22 C21 Fe1 66.46(18) . . ? C20 C21 Fe1 71.67(18) . . ? C22 C21 H21A 129.7 . . ? C20 C21 H21A 129.7 . . ? Fe1 C21 H21A 124.0 . . ? C21 C22 C23 113.1(3) . . ? C21 C22 Fe1 73.19(19) . . ? C23 C22 Fe1 74.82(19) . . ? C21 C22 H22 123.4 . . ? C23 C22 H22 123.4 . . ? Fe1 C22 H22 120.0 . . ? C24 C23 C22 107.6(3) . . ? C24 C23 Fe1 76.5(2) . . ? C22 C23 Fe1 62.62(18) . . ? C24 C23 H23 126.2 . . ? C22 C23 H23 126.2 . . ? Fe1 C23 H23 125.9 . . ? C23 C24 C20 103.9(3) . . ? C23 C24 Fe1 67.7(2) . . ? C20 C24 Fe1 64.55(17) . . ? C23 C24 H24 128.1 . . ? C20 C24 H24 128.1 . . ? Fe1 C24 H24 131.0 . . ? O21 C25 O22 123.0(3) . . ? O21 C25 N21 129.7(3) . . ? O22 C25 N21 107.3(3) . . ? C29 C26 O22 97.4(3) . . ? C29 C26 C27 110.0(3) . . ? O22 C26 C27 108.5(3) . . ? C29 C26 C28 108.9(3) . . ? O22 C26 C28 114.6(2) . . ? C27 C26 C28 115.8(3) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31 C30 C34 104.0(3) . . ? C31 C30 N31 129.2(3) . . ? C34 C30 N31 126.8(3) . . ? C31 C30 Fe2 70.23(15) . . ? C34 C30 Fe2 64.90(15) . . ? N31 C30 Fe2 128.97(18) . . ? C30 C31 C32 109.8(3) . . ? C30 C31 Fe2 67.67(15) . . ? C32 C31 Fe2 70.18(15) . . ? C30 C31 H31A 125.1 . . ? C32 C31 H31A 125.1 . . ? Fe2 C31 H31A 128.7 . . ? C33 C32 C31 109.5(3) . . ? C33 C32 Fe2 69.46(17) . . ? C31 C32 Fe2 65.31(14) . . ? C33 C32 H32 125.3 . . ? C31 C32 H32 125.3 . . ? Fe2 C32 H32 131.7 . . ? C32 C33 C34 104.1(3) . . ? C32 C33 Fe2 70.34(17) . . ? C34 C33 Fe2 62.08(16) . . ? C32 C33 H33 127.9 . . ? C34 C33 H33 127.9 . . ? Fe2 C33 H33 130.9 . . ? C30 C34 C33 112.6(3) . . ? C30 C34 Fe2 69.64(16) . . ? C33 C34 Fe2 73.38(17) . . ? C30 C34 H34 123.7 . . ? C33 C34 H34 123.7 . . ? Fe2 C34 H34 124.9 . . ? O31 C35 O32 123.6(3) . . ? O31 C35 N31 123.0(3) . . ? O32 C35 N31 113.4(2) . . ? C38 C36 C39 109.7(3) . . ? C38 C36 C37 105.0(3) . . ? C39 C36 C37 116.0(3) . . ? C38 C36 O32 115.6(2) . . ? C39 C36 O32 105.7(3) . . ? C37 C36 O32 105.2(2) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C41 C40 N41 125.6(3) . . ? C41 C40 C44 109.3(3) . . ? N41 C40 C44 125.0(3) . . ? C41 C40 Fe2 71.61(16) . . ? N41 C40 Fe2 128.52(18) . . ? C44 C40 Fe2 68.80(15) . . ? C40 C41 C42 104.0(3) . . ? C40 C41 Fe2 65.73(15) . . ? C42 C41 Fe2 69.19(16) . . ? C40 C41 H41A 128.0 . . ? C42 C41 H41A 128.0 . . ? Fe2 C41 H41A 128.5 . . ? C43 C42 C41 113.5(3) . . ? C43 C42 Fe2 71.98(16) . . ? C41 C42 Fe2 67.09(16) . . ? C43 C42 H42 123.3 . . ? C41 C42 H42 123.3 . . ? Fe2 C42 H42 129.6 . . ? C44 C43 C42 103.8(3) . . ? C44 C43 Fe2 64.84(16) . . ? C42 C43 Fe2 65.77(16) . . ? C44 C43 H43 128.1 . . ? C42 C43 H43 128.1 . . ? Fe2 C43 H43 132.6 . . ? C43 C44 C40 109.4(3) . . ? C43 C44 Fe2 74.44(18) . . ? C40 C44 Fe2 64.26(15) . . ? C43 C44 H44 125.3 . . ? C40 C44 H44 125.3 . . ? Fe2 C44 H44 127.5 . . ? O41 C45 O42 120.3(3) . . ? O41 C45 N41 128.3(3) . . ? O42 C45 N41 111.5(3) . . ? C48 C46 C49 106.4(3) . . ? C48 C46 C47 110.5(3) . . ? C49 C46 C47 113.4(3) . . ? C48 C46 O42 109.8(3) . . ? C49 C46 O42 101.9(3) . . ? C47 C46 O42 114.3(2) . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C46 C48 H48A 109.5 . . ? C46 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C46 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C46 C49 H49A 109.5 . . ? C46 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C46 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? N51 C50 C54 124.9(3) . . ? N51 C50 C51 121.6(3) . . ? C54 C50 C51 113.4(2) . . ? N51 C50 Fe3 126.2(2) . . ? C54 C50 Fe3 74.41(18) . . ? C51 C50 Fe3 70.28(16) . . ? C52 C51 C50 105.1(3) . . ? C52 C51 Fe3 70.37(18) . . ? C50 C51 Fe3 71.42(16) . . ? C52 C51 H51A 127.5 . . ? C50 C51 H51A 127.5 . . ? Fe3 C51 H51A 122.6 . . ? C51 C52 C53 108.1(2) . . ? C51 C52 Fe3 73.72(17) . . ? C53 C52 Fe3 71.20(16) . . ? C51 C52 H52 126.0 . . ? C53 C52 H52 126.0 . . ? Fe3 C52 H52 120.9 . . ? C54 C53 C52 111.5(3) . . ? C54 C53 Fe3 75.98(18) . . ? C52 C53 Fe3 69.23(16) . . ? C54 C53 H53 124.3 . . ? C52 C53 H53 124.3 . . ? Fe3 C53 H53 122.0 . . ? C53 C54 C50 102.0(3) . . ? C53 C54 Fe3 68.06(18) . . ? C50 C54 Fe3 68.96(17) . . ? C53 C54 H54 129.0 . . ? C50 C54 H54 129.0 . . ? Fe3 C54 H54 125.6 . . ? O51 C55 O52 126.0(2) . . ? O51 C55 N51 129.9(3) . . ? O52 C55 N51 104.1(3) . . ? O52 C56 C59 96.3(2) . . ? O52 C56 C58 112.2(3) . . ? C59 C56 C58 106.8(3) . . ? O52 C56 C57 109.5(2) . . ? C59 C56 C57 116.0(3) . . ? C58 C56 C57 114.7(3) . . ? C56 C57 H57A 109.5 . . ? C56 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C56 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C56 C58 H58A 109.5 . . ? C56 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C56 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C56 C59 H59A 109.5 . . ? C56 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C56 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 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 C15 N11 C10 C11 -155.9(3) . . . . ? C15 N11 C10 C14 27.7(5) . . . . ? C15 N11 C10 Fe1 -67.7(4) . . . . ? C21 Fe1 C10 C11 -167.7(2) . . . . ? C14 Fe1 C10 C11 -117.0(2) . . . . ? C20 Fe1 C10 C11 151.35(19) . . . . ? C23 Fe1 C10 C11 72.1(2) . . . . ? C12 Fe1 C10 C11 -41.04(19) . . . . ? C13 Fe1 C10 C11 -82.8(2) . . . . ? C24 Fe1 C10 C11 107.8(2) . . . . ? C21 Fe1 C10 N11 79.8(3) . . . . ? C14 Fe1 C10 N11 130.5(3) . . . . ? C11 Fe1 C10 N11 -112.5(3) . . . . ? C20 Fe1 C10 N11 38.9(3) . . . . ? C23 Fe1 C10 N11 -40.4(3) . . . . ? C12 Fe1 C10 N11 -153.5(3) . . . . ? C13 Fe1 C10 N11 164.7(3) . . . . ? C24 Fe1 C10 N11 -4.7(3) . . . . ? C21 Fe1 C10 C14 -50.7(3) . . . . ? C11 Fe1 C10 C14 117.0(2) . . . . ? C20 Fe1 C10 C14 -91.63(19) . . . . ? C23 Fe1 C10 C14 -170.88(16) . . . . ? C12 Fe1 C10 C14 75.99(18) . . . . ? C13 Fe1 C10 C14 34.20(16) . . . . ? C24 Fe1 C10 C14 -135.16(16) . . . . ? N11 C10 C11 C12 -176.4(3) . . . . ? C14 C10 C11 C12 0.8(3) . . . . ? Fe1 C10 C11 C12 63.9(2) . . . . ? N11 C10 C11 Fe1 119.7(3) . . . . ? C14 C10 C11 Fe1 -63.0(2) . . . . ? C22 Fe1 C11 C10 -172.0(2) . . . . ? C14 Fe1 C11 C10 41.11(19) . . . . ? C20 Fe1 C11 C10 -55.9(3) . . . . ? C23 Fe1 C11 C10 -128.8(2) . . . . ? C12 Fe1 C11 C10 113.7(3) . . . . ? C13 Fe1 C11 C10 80.7(2) . . . . ? C24 Fe1 C11 C10 -90.3(2) . . . . ? C22 Fe1 C11 C12 74.3(3) . . . . ? C10 Fe1 C11 C12 -113.7(3) . . . . ? C14 Fe1 C11 C12 -72.61(19) . . . . ? C20 Fe1 C11 C12 -169.6(2) . . . . ? C23 Fe1 C11 C12 117.43(19) . . . . ? C13 Fe1 C11 C12 -33.07(17) . . . . ? C24 Fe1 C11 C12 155.96(17) . . . . ? C10 C11 C12 C13 -0.6(4) . . . . ? Fe1 C11 C12 C13 59.6(3) . . . . ? C10 C11 C12 Fe1 -60.1(2) . . . . ? C22 Fe1 C12 C13 104.5(2) . . . . ? C10 Fe1 C12 C13 -85.3(2) . . . . ? C21 Fe1 C12 C13 60.7(2) . . . . ? C14 Fe1 C12 C13 -36.66(18) . . . . ? C11 Fe1 C12 C13 -124.9(3) . . . . ? C20 Fe1 C12 C13 28.7(7) . . . . ? C23 Fe1 C12 C13 152.1(2) . . . . ? C24 Fe1 C12 C13 -173.4(2) . . . . ? C22 Fe1 C12 C11 -130.62(19) . . . . ? C10 Fe1 C12 C11 39.60(17) . . . . ? C21 Fe1 C12 C11 -174.48(17) . . . . ? C14 Fe1 C12 C11 88.19(19) . . . . ? C20 Fe1 C12 C11 153.6(5) . . . . ? C23 Fe1 C12 C11 -83.1(2) . . . . ? C13 Fe1 C12 C11 124.9(3) . . . . ? C24 Fe1 C12 C11 -48.5(3) . . . . ? C11 C12 C13 C14 0.0(4) . . . . ? Fe1 C12 C13 C14 55.7(2) . . . . ? C11 C12 C13 Fe1 -55.7(2) . . . . ? C22 Fe1 C13 C14 148.33(19) . . . . ? C10 Fe1 C13 C14 -40.25(18) . . . . ? C21 Fe1 C13 C14 106.28(19) . . . . ? C11 Fe1 C13 C14 -82.5(2) . . . . ? C20 Fe1 C13 C14 70.1(2) . . . . ? C23 Fe1 C13 C14 -175.5(3) . . . . ? C12 Fe1 C13 C14 -117.4(3) . . . . ? C22 Fe1 C13 C12 -94.3(2) . . . . ? C10 Fe1 C13 C12 77.16(19) . . . . ? C21 Fe1 C13 C12 -136.32(19) . . . . ? C14 Fe1 C13 C12 117.4(3) . . . . ? C11 Fe1 C13 C12 34.93(18) . . . . ? C20 Fe1 C13 C12 -172.50(18) . . . . ? C23 Fe1 C13 C12 -58.1(3) . . . . ? C12 C13 C14 C10 0.5(4) . . . . ? Fe1 C13 C14 C10 57.9(2) . . . . ? C12 C13 C14 Fe1 -57.4(2) . . . . ? C11 C10 C14 C13 -0.9(4) . . . . ? N11 C10 C14 C13 175.7(3) . . . . ? Fe1 C10 C14 C13 -65.7(2) . . . . ? C11 C10 C14 Fe1 64.8(2) . . . . ? N11 C10 C14 Fe1 -118.5(4) . . . . ? C22 Fe1 C14 C13 -54.3(3) . . . . ? C10 Fe1 C14 C13 119.5(2) . . . . ? C21 Fe1 C14 C13 -87.0(2) . . . . ? C11 Fe1 C14 C13 82.4(2) . . . . ? C20 Fe1 C14 C13 -130.26(19) . . . . ? C12 Fe1 C14 C13 38.18(19) . . . . ? C24 Fe1 C14 C13 -170.1(2) . . . . ? C22 Fe1 C14 C10 -173.83(19) . . . . ? C21 Fe1 C14 C10 153.52(16) . . . . ? C11 Fe1 C14 C10 -37.11(16) . . . . ? C20 Fe1 C14 C10 110.24(17) . . . . ? C12 Fe1 C14 C10 -81.31(18) . . . . ? C13 Fe1 C14 C10 -119.5(2) . . . . ? C24 Fe1 C14 C10 70.4(2) . . . . ? C10 N11 C15 O11 -3.7(5) . . . . ? C10 N11 C15 O12 177.0(3) . . . . ? C16 O12 C15 O11 18.0(5) . . . . ? C16 O12 C15 N11 -162.7(3) . . . . ? C15 O12 C16 C19 -63.7(4) . . . . ? C15 O12 C16 C18 60.4(4) . . . . ? C15 O12 C16 C17 174.5(3) . . . . ? C25 N21 C20 C21 90.7(4) . . . . ? C25 N21 C20 C24 -93.2(4) . . . . ? C25 N21 C20 Fe1 173.4(2) . . . . ? C22 Fe1 C20 N21 -156.7(3) . . . . ? C10 Fe1 C20 N21 32.7(3) . . . . ? C21 Fe1 C20 N21 -114.4(4) . . . . ? C14 Fe1 C20 N21 -15.0(3) . . . . ? C11 Fe1 C20 N21 69.5(4) . . . . ? C23 Fe1 C20 N21 155.7(3) . . . . ? C12 Fe1 C20 N21 -75.5(7) . . . . ? C13 Fe1 C20 N21 -52.3(3) . . . . ? C24 Fe1 C20 N21 120.9(4) . . . . ? C22 Fe1 C20 C21 -42.3(2) . . . . ? C10 Fe1 C20 C21 147.12(19) . . . . ? C14 Fe1 C20 C21 99.4(2) . . . . ? C11 Fe1 C20 C21 -176.1(2) . . . . ? C23 Fe1 C20 C21 -89.9(2) . . . . ? C12 Fe1 C20 C21 38.9(6) . . . . ? C13 Fe1 C20 C21 62.1(2) . . . . ? C24 Fe1 C20 C21 -124.7(3) . . . . ? C22 Fe1 C20 C24 82.4(2) . . . . ? C10 Fe1 C20 C24 -88.2(2) . . . . ? C21 Fe1 C20 C24 124.7(3) . . . . ? C14 Fe1 C20 C24 -135.91(18) . . . . ? C11 Fe1 C20 C24 -51.4(3) . . . . ? C23 Fe1 C20 C24 34.77(19) . . . . ? C12 Fe1 C20 C24 163.6(5) . . . . ? C13 Fe1 C20 C24 -173.18(17) . . . . ? N21 C20 C21 C22 175.8(3) . . . . ? C24 C20 C21 C22 -0.6(4) . . . . ? Fe1 C20 C21 C22 60.7(2) . . . . ? N21 C20 C21 Fe1 115.2(3) . . . . ? C24 C20 C21 Fe1 -61.3(2) . . . . ? C10 Fe1 C21 C22 -173.5(2) . . . . ? C14 Fe1 C21 C22 151.4(2) . . . . ? C20 Fe1 C21 C22 -110.8(3) . . . . ? C23 Fe1 C21 C22 -38.3(2) . . . . ? C12 Fe1 C21 C22 78.9(3) . . . . ? C13 Fe1 C21 C22 113.0(2) . . . . ? C24 Fe1 C21 C22 -76.4(2) . . . . ? C22 Fe1 C21 C20 110.8(3) . . . . ? C10 Fe1 C21 C20 -62.7(3) . . . . ? C14 Fe1 C21 C20 -97.8(2) . . . . ? C23 Fe1 C21 C20 72.54(19) . . . . ? C12 Fe1 C21 C20 -170.31(18) . . . . ? C13 Fe1 C21 C20 -136.18(18) . . . . ? C24 Fe1 C21 C20 34.39(18) . . . . ? C20 C21 C22 C23 0.3(4) . . . . ? Fe1 C21 C22 C23 64.8(2) . . . . ? C20 C21 C22 Fe1 -64.5(2) . . . . ? C14 Fe1 C22 C21 -50.3(3) . . . . ? C11 Fe1 C22 C21 -168.4(2) . . . . ? C20 Fe1 C22 C21 41.8(2) . . . . ? C23 Fe1 C22 C21 120.5(3) . . . . ? C12 Fe1 C22 C21 -125.5(2) . . . . ? C13 Fe1 C22 C21 -83.3(2) . . . . ? C24 Fe1 C22 C21 86.1(2) . . . . ? C21 Fe1 C22 C23 -120.5(3) . . . . ? C14 Fe1 C22 C23 -170.74(19) . . . . ? C11 Fe1 C22 C23 71.1(2) . . . . ? C20 Fe1 C22 C23 -78.69(19) . . . . ? C12 Fe1 C22 C23 114.02(19) . . . . ? C13 Fe1 C22 C23 156.25(17) . . . . ? C24 Fe1 C22 C23 -34.35(17) . . . . ? C21 C22 C23 C24 0.2(4) . . . . ? Fe1 C22 C23 C24 64.0(2) . . . . ? C21 C22 C23 Fe1 -63.8(3) . . . . ? C22 Fe1 C23 C24 -118.2(3) . . . . ? C10 Fe1 C23 C24 68.9(3) . . . . ? C21 Fe1 C23 C24 -81.9(2) . . . . ? C11 Fe1 C23 C24 108.7(2) . . . . ? C20 Fe1 C23 C24 -38.9(2) . . . . ? C12 Fe1 C23 C24 152.1(2) . . . . ? C13 Fe1 C23 C24 -169.2(2) . . . . ? C10 Fe1 C23 C22 -172.86(16) . . . . ? C21 Fe1 C23 C22 36.38(17) . . . . ? C11 Fe1 C23 C22 -133.11(17) . . . . ? C20 Fe1 C23 C22 79.35(19) . . . . ? C12 Fe1 C23 C22 -89.7(2) . . . . ? C13 Fe1 C23 C22 -50.9(3) . . . . ? C24 Fe1 C23 C22 118.2(3) . . . . ? C22 C23 C24 C20 -0.5(4) . . . . ? Fe1 C23 C24 C20 54.6(2) . . . . ? C22 C23 C24 Fe1 -55.1(2) . . . . ? N21 C20 C24 C23 -175.6(3) . . . . ? C21 C20 C24 C23 0.8(4) . . . . ? Fe1 C20 C24 C23 -56.7(2) . . . . ? N21 C20 C24 Fe1 -118.9(3) . . . . ? C21 C20 C24 Fe1 57.4(2) . . . . ? C22 Fe1 C24 C23 40.8(2) . . . . ? C10 Fe1 C24 C23 -130.0(2) . . . . ? C21 Fe1 C24 C23 84.5(2) . . . . ? C14 Fe1 C24 C23 -173.8(2) . . . . ? C11 Fe1 C24 C23 -87.5(2) . . . . ? C20 Fe1 C24 C23 118.8(3) . . . . ? C12 Fe1 C24 C23 -54.4(4) . . . . ? C22 Fe1 C24 C20 -78.0(2) . . . . ? C10 Fe1 C24 C20 111.27(18) . . . . ? C21 Fe1 C24 C20 -34.29(17) . . . . ? C14 Fe1 C24 C20 67.4(2) . . . . ? C11 Fe1 C24 C20 153.70(17) . . . . ? C23 Fe1 C24 C20 -118.8(3) . . . . ? C12 Fe1 C24 C20 -173.1(2) . . . . ? C26 O22 C25 O21 16.0(5) . . . . ? C26 O22 C25 N21 -165.0(3) . . . . ? C20 N21 C25 O21 -12.1(6) . . . . ? C20 N21 C25 O22 169.0(3) . . . . ? C25 O22 C26 C29 167.9(3) . . . . ? C25 O22 C26 C27 -78.0(3) . . . . ? C25 O22 C26 C28 53.2(4) . . . . ? C35 N31 C30 C31 -3.3(4) . . . . ? C35 N31 C30 C34 175.4(3) . . . . ? C35 N31 C30 Fe2 -99.0(3) . . . . ? C34 Fe2 C30 C31 116.9(2) . . . . ? C40 Fe2 C30 C31 -48.1(4) . . . . ? C44 Fe2 C30 C31 -81.9(2) . . . . ? C41 Fe2 C30 C31 163.4(3) . . . . ? C42 Fe2 C30 C31 -162.16(19) . . . . ? C33 Fe2 C30 C31 79.52(19) . . . . ? C32 Fe2 C30 C31 37.99(18) . . . . ? C43 Fe2 C30 C31 -121.99(19) . . . . ? C40 Fe2 C30 C34 -165.0(3) . . . . ? C44 Fe2 C30 C34 161.23(18) . . . . ? C41 Fe2 C30 C34 46.6(4) . . . . ? C31 Fe2 C30 C34 -116.9(2) . . . . ? C42 Fe2 C30 C34 80.9(2) . . . . ? C33 Fe2 C30 C34 -37.38(18) . . . . ? C32 Fe2 C30 C34 -78.90(19) . . . . ? C43 Fe2 C30 C34 121.11(19) . . . . ? C34 Fe2 C30 N31 -118.2(3) . . . . ? C40 Fe2 C30 N31 76.9(4) . . . . ? C44 Fe2 C30 N31 43.1(3) . . . . ? C41 Fe2 C30 N31 -71.6(5) . . . . ? C31 Fe2 C30 N31 124.9(3) . . . . ? C42 Fe2 C30 N31 -37.2(3) . . . . ? C33 Fe2 C30 N31 -155.6(3) . . . . ? C32 Fe2 C30 N31 162.9(3) . . . . ? C43 Fe2 C30 N31 2.9(3) . . . . ? C34 C30 C31 C32 -1.2(3) . . . . ? N31 C30 C31 C32 177.8(2) . . . . ? Fe2 C30 C31 C32 -57.51(17) . . . . ? C34 C30 C31 Fe2 56.34(17) . . . . ? N31 C30 C31 Fe2 -124.7(3) . . . . ? C34 Fe2 C31 C30 -41.86(18) . . . . ? C40 Fe2 C31 C30 160.05(18) . . . . ? C44 Fe2 C31 C30 112.65(18) . . . . ? C41 Fe2 C31 C30 -164.5(3) . . . . ? C42 Fe2 C31 C30 43.7(4) . . . . ? C33 Fe2 C31 C30 -88.62(19) . . . . ? C32 Fe2 C31 C30 -122.5(2) . . . . ? C43 Fe2 C31 C30 72.2(2) . . . . ? C34 Fe2 C31 C32 80.61(18) . . . . ? C40 Fe2 C31 C32 -77.5(2) . . . . ? C30 Fe2 C31 C32 122.5(2) . . . . ? C44 Fe2 C31 C32 -124.88(18) . . . . ? C41 Fe2 C31 C32 -42.1(4) . . . . ? C42 Fe2 C31 C32 166.2(3) . . . . ? C33 Fe2 C31 C32 33.85(17) . . . . ? C43 Fe2 C31 C32 -165.34(17) . . . . ? C30 C31 C32 C33 0.9(3) . . . . ? Fe2 C31 C32 C33 -55.11(19) . . . . ? C30 C31 C32 Fe2 56.04(18) . . . . ? C34 Fe2 C32 C33 40.54(18) . . . . ? C40 Fe2 C32 C33 -115.70(19) . . . . ? C30 Fe2 C32 C33 88.26(19) . . . . ? C44 Fe2 C32 C33 -162.43(18) . . . . ? C41 Fe2 C32 C33 -72.5(2) . . . . ? C31 Fe2 C32 C33 124.3(2) . . . . ? C42 Fe2 C32 C33 -42.2(4) . . . . ? C43 Fe2 C32 C33 164.0(3) . . . . ? C34 Fe2 C32 C31 -83.77(18) . . . . ? C40 Fe2 C32 C31 119.99(17) . . . . ? C30 Fe2 C32 C31 -36.06(16) . . . . ? C44 Fe2 C32 C31 73.3(2) . . . . ? C41 Fe2 C32 C31 163.18(17) . . . . ? C42 Fe2 C32 C31 -166.5(3) . . . . ? C33 Fe2 C32 C31 -124.3(2) . . . . ? C43 Fe2 C32 C31 39.7(4) . . . . ? C31 C32 C33 C34 -0.2(3) . . . . ? Fe2 C32 C33 C34 -52.95(18) . . . . ? C31 C32 C33 Fe2 52.74(18) . . . . ? C34 Fe2 C33 C32 -118.8(2) . . . . ? C40 Fe2 C33 C32 78.70(19) . . . . ? C30 Fe2 C33 C32 -80.75(18) . . . . ? C44 Fe2 C33 C32 44.9(4) . . . . ? C41 Fe2 C33 C32 120.54(19) . . . . ? C31 Fe2 C33 C32 -37.22(17) . . . . ? C42 Fe2 C33 C32 162.11(18) . . . . ? C43 Fe2 C33 C32 -164.7(3) . . . . ? C40 Fe2 C33 C34 -162.47(17) . . . . ? C30 Fe2 C33 C34 38.09(17) . . . . ? C44 Fe2 C33 C34 163.8(3) . . . . ? C41 Fe2 C33 C34 -120.62(18) . . . . ? C31 Fe2 C33 C34 81.61(18) . . . . ? C42 Fe2 C33 C34 -79.1(2) . . . . ? C32 Fe2 C33 C34 118.8(2) . . . . ? C43 Fe2 C33 C34 -45.8(4) . . . . ? C31 C30 C34 C33 1.1(3) . . . . ? N31 C30 C34 C33 -177.9(2) . . . . ? Fe2 C30 C34 C33 61.0(2) . . . . ? C31 C30 C34 Fe2 -59.88(17) . . . . ? N31 C30 C34 Fe2 121.1(2) . . . . ? C32 C33 C34 C30 -0.5(3) . . . . ? Fe2 C33 C34 C30 -58.81(19) . . . . ? C32 C33 C34 Fe2 58.28(19) . . . . ? C40 Fe2 C34 C30 165.1(3) . . . . ? C44 Fe2 C34 C30 -43.7(4) . . . . ? C41 Fe2 C34 C30 -162.72(17) . . . . ? C31 Fe2 C34 C30 38.87(17) . . . . ? C42 Fe2 C34 C30 -117.81(19) . . . . ? C33 Fe2 C34 C30 122.6(2) . . . . ? C32 Fe2 C34 C30 85.89(18) . . . . ? C43 Fe2 C34 C30 -74.7(2) . . . . ? C40 Fe2 C34 C33 42.4(4) . . . . ? C30 Fe2 C34 C33 -122.6(2) . . . . ? C44 Fe2 C34 C33 -166.4(3) . . . . ? C41 Fe2 C34 C33 74.7(2) . . . . ? C31 Fe2 C34 C33 -83.76(18) . . . . ? C42 Fe2 C34 C33 119.56(19) . . . . ? C32 Fe2 C34 C33 -36.74(17) . . . . ? C43 Fe2 C34 C33 162.66(18) . . . . ? C36 O32 C35 O31 -4.2(4) . . . . ? C36 O32 C35 N31 174.9(2) . . . . ? C30 N31 C35 O31 -0.6(4) . . . . ? C30 N31 C35 O32 -179.8(2) . . . . ? C35 O32 C36 C38 64.0(4) . . . . ? C35 O32 C36 C39 -57.5(3) . . . . ? C35 O32 C36 C37 179.3(2) . . . . ? C45 N41 C40 C41 -33.1(4) . . . . ? C45 N41 C40 C44 150.8(2) . . . . ? C45 N41 C40 Fe2 61.2(4) . . . . ? C34 Fe2 C40 C41 43.7(4) . . . . ? C30 Fe2 C40 C41 -163.9(3) . . . . ? C44 Fe2 C40 C41 -120.1(2) . . . . ? C31 Fe2 C40 C41 160.84(19) . . . . ? C42 Fe2 C40 C41 -40.5(2) . . . . ? C33 Fe2 C40 C41 75.6(2) . . . . ? C32 Fe2 C40 C41 116.2(2) . . . . ? C43 Fe2 C40 C41 -84.7(2) . . . . ? C34 Fe2 C40 N41 -77.6(4) . . . . ? C30 Fe2 C40 N41 74.7(4) . . . . ? C44 Fe2 C40 N41 118.5(3) . . . . ? C41 Fe2 C40 N41 -121.3(4) . . . . ? C31 Fe2 C40 N41 39.5(3) . . . . ? C42 Fe2 C40 N41 -161.8(3) . . . . ? C33 Fe2 C40 N41 -45.7(3) . . . . ? C32 Fe2 C40 N41 -5.2(3) . . . . ? C43 Fe2 C40 N41 154.0(3) . . . . ? C34 Fe2 C40 C44 163.8(3) . . . . ? C30 Fe2 C40 C44 -43.8(4) . . . . ? C41 Fe2 C40 C44 120.1(2) . . . . ? C31 Fe2 C40 C44 -79.04(18) . . . . ? C42 Fe2 C40 C44 79.67(18) . . . . ? C33 Fe2 C40 C44 -164.25(16) . . . . ? C32 Fe2 C40 C44 -123.70(17) . . . . ? C43 Fe2 C40 C44 35.45(16) . . . . ? N41 C40 C41 C42 -176.3(2) . . . . ? C44 C40 C41 C42 0.4(3) . . . . ? Fe2 C40 C41 C42 59.05(18) . . . . ? N41 C40 C41 Fe2 124.7(3) . . . . ? C44 C40 C41 Fe2 -58.67(17) . . . . ? C34 Fe2 C41 C40 -161.69(19) . . . . ? C30 Fe2 C41 C40 162.2(3) . . . . ? C44 Fe2 C41 C40 40.80(18) . . . . ? C31 Fe2 C41 C40 -47.6(4) . . . . ? C42 Fe2 C41 C40 117.1(3) . . . . ? C33 Fe2 C41 C40 -118.3(2) . . . . ? C32 Fe2 C41 C40 -79.5(2) . . . . ? C43 Fe2 C41 C40 83.0(2) . . . . ? C34 Fe2 C41 C42 81.2(2) . . . . ? C40 Fe2 C41 C42 -117.1(3) . . . . ? C30 Fe2 C41 C42 45.1(4) . . . . ? C44 Fe2 C41 C42 -76.3(2) . . . . ? C31 Fe2 C41 C42 -164.7(3) . . . . ? C33 Fe2 C41 C42 124.6(2) . . . . ? C32 Fe2 C41 C42 163.35(19) . . . . ? C43 Fe2 C41 C42 -34.12(19) . . . . ? C40 C41 C42 C43 -0.1(3) . . . . ? Fe2 C41 C42 C43 56.6(2) . . . . ? C40 C41 C42 Fe2 -56.76(17) . . . . ? C34 Fe2 C42 C43 117.42(18) . . . . ? C40 Fe2 C42 C43 -86.83(19) . . . . ? C30 Fe2 C42 C43 70.7(2) . . . . ? C44 Fe2 C42 C43 -36.94(17) . . . . ? C41 Fe2 C42 C43 -126.3(3) . . . . ? C31 Fe2 C42 C43 38.4(4) . . . . ? C33 Fe2 C42 C43 162.80(17) . . . . ? C32 Fe2 C42 C43 -166.8(3) . . . . ? C34 Fe2 C42 C41 -116.2(2) . . . . ? C40 Fe2 C42 C41 39.51(18) . . . . ? C30 Fe2 C42 C41 -162.92(18) . . . . ? C44 Fe2 C42 C41 89.4(2) . . . . ? C31 Fe2 C42 C41 164.8(3) . . . . ? C33 Fe2 C42 C41 -70.9(2) . . . . ? C32 Fe2 C42 C41 -40.5(4) . . . . ? C43 Fe2 C42 C41 126.3(3) . . . . ? C41 C42 C43 C44 -0.2(3) . . . . ? Fe2 C42 C43 C44 53.80(18) . . . . ? C41 C42 C43 Fe2 -54.0(2) . . . . ? C34 Fe2 C43 C44 160.51(18) . . . . ? C40 Fe2 C43 C44 -40.50(18) . . . . ? C30 Fe2 C43 C44 116.20(19) . . . . ? C41 Fe2 C43 C44 -84.82(19) . . . . ? C31 Fe2 C43 C44 75.8(2) . . . . ? C42 Fe2 C43 C44 -120.0(2) . . . . ? C33 Fe2 C43 C44 -164.3(3) . . . . ? C32 Fe2 C43 C44 45.1(4) . . . . ? C34 Fe2 C43 C42 -79.5(2) . . . . ? C40 Fe2 C43 C42 79.52(19) . . . . ? C30 Fe2 C43 C42 -123.78(18) . . . . ? C44 Fe2 C43 C42 120.0(2) . . . . ? C41 Fe2 C43 C42 35.20(18) . . . . ? C31 Fe2 C43 C42 -164.21(17) . . . . ? C33 Fe2 C43 C42 -44.3(4) . . . . ? C32 Fe2 C43 C42 165.1(3) . . . . ? C42 C43 C44 C40 0.4(3) . . . . ? Fe2 C43 C44 C40 54.81(17) . . . . ? C42 C43 C44 Fe2 -54.39(18) . . . . ? C41 C40 C44 C43 -0.5(3) . . . . ? N41 C40 C44 C43 176.1(2) . . . . ? Fe2 C40 C44 C43 -60.93(19) . . . . ? C41 C40 C44 Fe2 60.39(19) . . . . ? N41 C40 C44 Fe2 -122.9(2) . . . . ? C34 Fe2 C44 C43 -43.6(4) . . . . ? C40 Fe2 C44 C43 121.2(2) . . . . ? C30 Fe2 C44 C43 -76.4(2) . . . . ? C41 Fe2 C44 C43 83.9(2) . . . . ? C31 Fe2 C44 C43 -119.31(19) . . . . ? C42 Fe2 C44 C43 38.28(18) . . . . ? C33 Fe2 C44 C43 164.1(3) . . . . ? C32 Fe2 C44 C43 -162.85(18) . . . . ? C34 Fe2 C44 C40 -164.7(3) . . . . ? C30 Fe2 C44 C40 162.43(15) . . . . ? C41 Fe2 C44 C40 -37.30(16) . . . . ? C31 Fe2 C44 C40 119.52(16) . . . . ? C42 Fe2 C44 C40 -82.89(17) . . . . ? C33 Fe2 C44 C40 42.9(4) . . . . ? C32 Fe2 C44 C40 75.99(18) . . . . ? C43 Fe2 C44 C40 -121.2(2) . . . . ? C46 O42 C45 O41 -7.5(4) . . . . ? C46 O42 C45 N41 171.8(2) . . . . ? C40 N41 C45 O41 6.1(4) . . . . ? C40 N41 C45 O42 -173.2(2) . . . . ? C45 O42 C46 C48 -63.1(4) . . . . ? C45 O42 C46 C49 -175.6(3) . . . . ? C45 O42 C46 C47 61.7(3) . . . . ? C55 N51 C50 C54 34.5(5) . . . . ? C55 N51 C50 C51 -149.2(3) . . . . ? C55 N51 C50 Fe3 -61.5(4) . . . . ? C52 Fe3 C50 N51 -153.0(3) . . . . ? C52 Fe3 C50 N51 27.0(3) 3_665 . . . ? C53 Fe3 C50 N51 -19.0(3) 3_665 . . . ? C53 Fe3 C50 N51 161.0(3) . . . . ? C51 Fe3 C50 N51 -115.3(3) . . . . ? C51 Fe3 C50 N51 64.7(3) 3_665 . . . ? C54 Fe3 C50 N51 -57.8(3) 3_665 . . . ? C54 Fe3 C50 N51 122.2(3) . . . . ? C52 Fe3 C50 C54 84.78(18) . . . . ? C52 Fe3 C50 C54 -95.22(18) 3_665 . . . ? C53 Fe3 C50 C54 -141.14(16) 3_665 . . . ? C53 Fe3 C50 C54 38.85(16) . . . . ? C51 Fe3 C50 C54 122.5(2) . . . . ? C51 Fe3 C50 C54 -57.5(2) 3_665 . . . ? C54 Fe3 C50 C54 180.0 3_665 . . . ? C52 Fe3 C50 C51 -37.72(17) . . . . ? C52 Fe3 C50 C51 142.29(17) 3_665 . . . ? C53 Fe3 C50 C51 96.36(18) 3_665 . . . ? C53 Fe3 C50 C51 -83.65(18) . . . . ? C51 Fe3 C50 C51 180.0 3_665 . . . ? C54 Fe3 C50 C51 57.5(2) 3_665 . . . ? C54 Fe3 C50 C51 -122.5(2) . . . . ? N51 C50 C51 C52 -176.2(3) . . . . ? C54 C50 C51 C52 0.5(4) . . . . ? Fe3 C50 C51 C52 62.8(2) . . . . ? N51 C50 C51 Fe3 121.0(3) . . . . ? C54 C50 C51 Fe3 -62.2(2) . . . . ? C52 Fe3 C51 C52 -180.0 3_665 . . . ? C53 Fe3 C51 C52 139.92(18) 3_665 . . . ? C53 Fe3 C51 C52 -40.09(18) . . . . ? C50 Fe3 C51 C52 65.7(3) 3_665 . . . ? C50 Fe3 C51 C52 -114.3(3) . . . . ? C54 Fe3 C51 C52 99.62(19) 3_665 . . . ? C54 Fe3 C51 C52 -80.38(19) . . . . ? C52 Fe3 C51 C50 114.3(3) . . . . ? C52 Fe3 C51 C50 -65.7(3) 3_665 . . . ? C53 Fe3 C51 C50 -105.81(18) 3_665 . . . ? C53 Fe3 C51 C50 74.19(18) . . . . ? C50 Fe3 C51 C50 180.0 3_665 . . . ? C54 Fe3 C51 C50 -146.10(16) 3_665 . . . ? C54 Fe3 C51 C50 33.90(16) . . . . ? C50 C51 C52 C53 -0.1(3) . . . . ? Fe3 C51 C52 C53 63.4(2) . . . . ? C50 C51 C52 Fe3 -63.5(2) . . . . ? C53 Fe3 C52 C51 -63.9(2) 3_665 . . . ? C53 Fe3 C52 C51 116.1(2) . . . . ? C51 Fe3 C52 C51 180.0 3_665 . . . ? C50 Fe3 C52 C51 -139.72(18) 3_665 . . . ? C50 Fe3 C52 C51 40.28(18) . . . . ? C54 Fe3 C52 C51 -98.35(19) 3_665 . . . ? C54 Fe3 C52 C51 81.65(19) . . . . ? C53 Fe3 C52 C53 180.0 3_665 . . . ? C51 Fe3 C52 C53 -116.1(2) . . . . ? C51 Fe3 C52 C53 63.9(2) 3_665 . . . ? C50 Fe3 C52 C53 104.14(17) 3_665 . . . ? C50 Fe3 C52 C53 -75.86(17) . . . . ? C54 Fe3 C52 C53 145.51(16) 3_665 . . . ? C54 Fe3 C52 C53 -34.49(16) . . . . ? C51 C52 C53 C54 -0.3(4) . . . . ? Fe3 C52 C53 C54 64.7(2) . . . . ? C51 C52 C53 Fe3 -65.0(2) . . . . ? C52 Fe3 C53 C54 -119.9(3) . . . . ? C52 Fe3 C53 C54 60.1(3) 3_665 . . . ? C51 Fe3 C53 C54 -83.52(19) . . . . ? C51 Fe3 C53 C54 96.47(19) 3_665 . . . ? C50 Fe3 C53 C54 140.40(17) 3_665 . . . ? C50 Fe3 C53 C54 -39.60(17) . . . . ? C54 Fe3 C53 C54 180.0 3_665 . . . ? C52 Fe3 C53 C52 180.0 3_665 . . . ? C51 Fe3 C53 C52 36.36(15) . . . . ? C51 Fe3 C53 C52 -143.64(15) 3_665 . . . ? C50 Fe3 C53 C52 -99.72(17) 3_665 . . . ? C50 Fe3 C53 C52 80.29(17) . . . . ? C54 Fe3 C53 C52 -60.1(3) 3_665 . . . ? C54 Fe3 C53 C52 119.9(3) . . . . ? C52 C53 C54 C50 0.6(3) . . . . ? Fe3 C53 C54 C50 61.2(2) . . . . ? C52 C53 C54 Fe3 -60.6(2) . . . . ? N51 C50 C54 C53 175.9(3) . . . . ? C51 C50 C54 C53 -0.7(4) . . . . ? Fe3 C50 C54 C53 -60.6(2) . . . . ? N51 C50 C54 Fe3 -123.5(3) . . . . ? C51 C50 C54 Fe3 59.9(2) . . . . ? C52 Fe3 C54 C53 37.89(18) . . . . ? C52 Fe3 C54 C53 -142.10(18) 3_665 . . . ? C53 Fe3 C54 C53 -180.0 3_665 . . . ? C51 Fe3 C54 C53 77.91(19) . . . . ? C51 Fe3 C54 C53 -102.09(19) 3_665 . . . ? C50 Fe3 C54 C53 -66.7(2) 3_665 . . . ? C50 Fe3 C54 C53 113.3(2) . . . . ? C52 Fe3 C54 C50 -75.43(17) . . . . ? C52 Fe3 C54 C50 104.58(17) 3_665 . . . ? C53 Fe3 C54 C50 66.7(2) 3_665 . . . ? C53 Fe3 C54 C50 -113.3(2) . . . . ? C51 Fe3 C54 C50 -35.41(15) . . . . ? C51 Fe3 C54 C50 144.59(15) 3_665 . . . ? C50 Fe3 C54 C50 180.0 3_665 . . . ? C56 O52 C55 O51 0.5(5) . . . . ? C56 O52 C55 N51 -179.0(3) . . . . ? C50 N51 C55 O51 0.6(5) . . . . ? C50 N51 C55 O52 -179.9(3) . . . . ? C55 O52 C56 C59 -174.5(3) . . . . ? C55 O52 C56 C58 -63.4(4) . . . . ? C55 O52 C56 C57 65.1(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N11 H11 O41 0.88 2.05 2.887(3) 158.8 . N21 H21 O11 0.88 1.99 2.753(3) 144.1 . N31 H31 O21 0.88 1.94 2.818(3) 173.1 2_655 N41 H41 O51 0.88 2.00 2.831(3) 157.5 . N51 H51 O31 0.88 2.16 2.845(3) 134.4 3_665 _diffrn_measured_fraction_theta_max 0.944 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.944 _refine_diff_density_max 0.326 _refine_diff_density_min -0.378 _refine_diff_density_rms 0.068 #===END data_7 _database_code_depnum_ccdc_archive 'CCDC 265456' # Original saved as bksc0503 # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H38 Fe N4 O6' _chemical_formula_sum 'C26 H38 Fe N4 O6' _chemical_formula_weight 558.45 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' # Crystal Data _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2 _symmetry_space_group_name_Hall 'C 2y' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 15.4790(3) _cell_length_b 9.3420(3) _cell_length_c 11.0400(3) _cell_angle_alpha 90.00 _cell_angle_beta 117.071(2) _cell_angle_gamma 90.00 _cell_volume 1421.53(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3809 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 30.03 _exptl_crystal_description square _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.305 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 592 _exptl_absorpt_coefficient_mu 0.575 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8696 _exptl_absorpt_correction_T_max 0.9187 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski & Minor 1997)' _exptl_special_details ; ? ; # EXPERIMENTAL DETAIL _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR590D, fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type 'KappaCCD (BruKer AXS-Nonius, FR540C)' _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'no decay' _diffrn_reflns_number 7467 _diffrn_reflns_av_R_equivalents 0.0312 _diffrn_reflns_av_sigmaI/netI 0.0435 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 30.08 _reflns_number_total 4039 _reflns_number_gt 3656 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution ; 'SIR-97 (A. Altomare, G. Cascarano et al.)' ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; Cameron (WinGX v1.70.01, 2005), Ortep (SHELXTL-NT v6.14, Bruker AXS) ; _computing_publication_material 'WinGX v1.70.01 (L. J. Farrugia)' # REFINEMENT DATA _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^ > 2sigma(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^)+(0.0279P)^2^+0.6901P] 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 ? _chemical_absolute_configuration . _refine_ls_abs_structure_details 'Flack H D (1983), 1843 Friedel pairs' _refine_ls_abs_structure_Flack -0.002(12) _refine_ls_number_reflns 4039 _refine_ls_number_parameters 172 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0432 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.0753 _refine_ls_wR_factor_gt 0.0717 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 Fe1 Fe 0.0000 0.29193(2) 0.0000 0.02145(8) Uani 1 2 d S . . O11 O 0.18569(9) 0.55835(14) -0.02474(14) 0.0288(3) Uani 1 1 d . . . O12 O 0.13540(10) 0.74324(14) 0.17325(14) 0.0313(3) Uani 1 1 d . . . O13 O 0.25441(10) 0.91279(14) 0.24656(13) 0.0280(3) Uani 1 1 d . . . N11 N 0.02054(10) 0.56661(14) -0.14226(14) 0.0200(3) Uani 1 1 d . . . H11 H -0.0284 0.6265 -0.1811 0.024 Uiso 1 1 calc . . . N12 N 0.18035(11) 0.85584(16) 0.02912(15) 0.0232(3) Uani 1 1 d . . . H12 H 0.2221 0.9153 0.0225 0.028 Uiso 1 1 calc . . . C10 C -0.00352(15) 0.41951(19) -0.15196(19) 0.0200(4) Uani 1 1 d . . . C11 C 0.05515(12) 0.2969(3) -0.13749(16) 0.0261(3) Uani 1 1 d . . . H11A H 0.1218 0.2970 -0.1170 0.031 Uiso 1 1 calc . . . C12 C -0.00472(18) 0.1745(2) -0.1595(2) 0.0305(5) Uani 1 1 d . . . H12A H 0.0152 0.0778 -0.1564 0.037 Uiso 1 1 calc . . . C13 C -0.09902(17) 0.2208(2) -0.1868(2) 0.0295(5) Uani 1 1 d . . . H13 H -0.1531 0.1606 -0.2051 0.035 Uiso 1 1 calc . . . C14 C -0.09864(15) 0.3734(2) -0.1819(2) 0.0234(4) Uani 1 1 d . . . H14 H -0.1521 0.4331 -0.1960 0.028 Uiso 1 1 calc . . . C15 C 0.10941(12) 0.62563(18) -0.08062(16) 0.0195(3) Uani 1 1 d . . . C16 C 0.10767(10) 0.7894(2) -0.09278(14) 0.0208(3) Uani 1 1 d . . . H16 H 0.0421 0.8254 -0.1105 0.025 Uiso 1 1 calc R . . C17 C 0.12695(16) 0.8297(2) -0.2125(2) 0.0356(5) Uani 1 1 d . . . H17A H 0.1271 0.9341 -0.2205 0.043 Uiso 1 1 calc R . . H17B H 0.0760 0.7891 -0.2965 0.043 Uiso 1 1 calc R . . H17C H 0.1901 0.7916 -0.1971 0.043 Uiso 1 1 calc R . . C18 C 0.18621(12) 0.82982(17) 0.15184(18) 0.0218(3) Uani 1 1 d . . . C19 C 0.29240(16) 0.8806(2) 0.3927(2) 0.0336(4) Uani 1 1 d . . . C110 C 0.34269(19) 0.7374(3) 0.4214(3) 0.0506(6) Uani 1 1 d . . . H11B H 0.2947 0.6618 0.3768 0.061 Uiso 1 1 calc R . . H11C H 0.3755 0.7206 0.5198 0.061 Uiso 1 1 calc R . . H11D H 0.3905 0.7368 0.3863 0.061 Uiso 1 1 calc R . . C111 C 0.2133(2) 0.8875(3) 0.4364(2) 0.0476(6) Uani 1 1 d . . . H11E H 0.1749 0.9746 0.3999 0.057 Uiso 1 1 calc R . . H11F H 0.2424 0.8889 0.5360 0.057 Uiso 1 1 calc R . . H11G H 0.1712 0.8035 0.4018 0.057 Uiso 1 1 calc R . . C112 C 0.3637(2) 1.0022(3) 0.4560(2) 0.0619(8) Uani 1 1 d . . . H11H H 0.4121 1.0004 0.4219 0.074 Uiso 1 1 calc R . . H11I H 0.3962 0.9913 0.5552 0.074 Uiso 1 1 calc R . . H11J H 0.3289 1.0937 0.4320 0.074 Uiso 1 1 calc R . . 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 0.02360(16) 0.01397(14) 0.02541(16) 0.000 0.00995(13) 0.000 O11 0.0201(6) 0.0228(6) 0.0406(7) -0.0029(5) 0.0111(6) 0.0056(5) O12 0.0310(7) 0.0319(7) 0.0351(7) -0.0037(5) 0.0186(6) -0.0128(5) O13 0.0308(7) 0.0237(6) 0.0249(6) -0.0017(5) 0.0085(6) -0.0101(5) N11 0.0187(7) 0.0153(6) 0.0240(7) -0.0009(5) 0.0080(6) 0.0007(5) N12 0.0230(7) 0.0202(7) 0.0280(7) -0.0031(6) 0.0131(6) -0.0067(6) C10 0.0246(9) 0.0131(8) 0.0214(8) -0.0023(7) 0.0098(7) -0.0002(7) C11 0.0320(8) 0.0182(7) 0.0307(7) -0.0051(9) 0.0167(7) -0.0008(9) C12 0.0418(13) 0.0172(10) 0.0328(11) -0.0080(8) 0.0174(10) -0.0019(9) C13 0.0321(11) 0.0225(10) 0.0282(11) -0.0055(8) 0.0088(9) -0.0083(8) C14 0.0231(10) 0.0199(9) 0.0235(9) -0.0013(7) 0.0075(8) -0.0008(7) C15 0.0212(8) 0.0185(7) 0.0213(7) -0.0004(6) 0.0117(7) 0.0025(6) C16 0.0207(7) 0.0159(6) 0.0255(7) -0.0014(9) 0.0103(6) -0.0022(9) C17 0.0484(12) 0.0310(11) 0.0303(9) 0.0012(7) 0.0204(9) -0.0073(8) C18 0.0188(8) 0.0182(8) 0.0284(8) -0.0036(6) 0.0108(7) -0.0038(6) C19 0.0369(11) 0.0330(10) 0.0232(9) 0.0023(7) 0.0068(8) -0.0045(8) C110 0.0494(14) 0.0495(13) 0.0447(13) 0.0149(11) 0.0144(12) 0.0119(12) C111 0.0561(15) 0.0582(15) 0.0322(11) -0.0033(10) 0.0232(11) -0.0016(12) C112 0.0680(18) 0.0653(17) 0.0278(11) -0.0047(11) 0.0003(11) -0.0323(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; # MOLECULAR GEOMETRY 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 C14 2.038(2) 2 ? Fe1 C14 2.038(2) . ? Fe1 C10 2.0383(18) 2 ? Fe1 C10 2.0384(18) . ? Fe1 C13 2.041(2) 2 ? Fe1 C13 2.041(2) . ? Fe1 C12 2.048(2) 2 ? Fe1 C12 2.048(2) . ? Fe1 C11 2.0528(15) 2 ? Fe1 C11 2.0528(15) . ? O11 C15 1.227(2) . ? O12 C18 1.224(2) . ? O13 C18 1.343(2) . ? O13 C19 1.475(2) . ? N11 C15 1.344(2) . ? N11 C10 1.415(2) . ? N11 H11 0.8800 . ? N12 C18 1.338(2) . ? N12 C16 1.444(2) . ? N12 H12 0.8800 . ? C10 C14 1.421(3) . ? C10 C11 1.425(3) . ? C11 C12 1.421(3) . ? C11 H11A 0.9500 . ? C12 C13 1.417(3) . ? C12 H12A 0.9500 . ? C13 C14 1.426(2) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.535(3) . ? C16 C17 1.528(2) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C19 C110 1.507(3) . ? C19 C111 1.508(3) . ? C19 C112 1.515(3) . ? C110 H11B 0.9800 . ? C110 H11C 0.9800 . ? C110 H11D 0.9800 . ? C111 H11E 0.9800 . ? C111 H11F 0.9800 . ? C111 H11G 0.9800 . ? C112 H11H 0.9800 . ? C112 H11I 0.9800 . ? C112 H11J 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 C14 Fe1 C14 136.15(11) 2 . ? C14 Fe1 C10 40.82(8) 2 2 ? C14 Fe1 C10 108.67(7) . 2 ? C14 Fe1 C10 108.67(7) 2 . ? C14 Fe1 C10 40.82(8) . . ? C10 Fe1 C10 108.43(10) 2 . ? C14 Fe1 C13 40.94(6) 2 2 ? C14 Fe1 C13 176.94(10) . 2 ? C10 Fe1 C13 68.44(9) 2 2 ? C10 Fe1 C13 138.44(9) . 2 ? C14 Fe1 C13 176.94(10) 2 . ? C14 Fe1 C13 40.94(6) . . ? C10 Fe1 C13 138.45(9) 2 . ? C10 Fe1 C13 68.44(9) . . ? C13 Fe1 C13 141.98(12) 2 . ? C14 Fe1 C12 68.60(9) 2 2 ? C14 Fe1 C12 139.91(9) . 2 ? C10 Fe1 C12 68.18(6) 2 2 ? C10 Fe1 C12 176.59(9) . 2 ? C13 Fe1 C12 40.56(10) 2 2 ? C13 Fe1 C12 114.25(9) . 2 ? C14 Fe1 C12 139.91(9) 2 . ? C14 Fe1 C12 68.60(9) . . ? C10 Fe1 C12 176.59(9) 2 . ? C10 Fe1 C12 68.18(6) . . ? C13 Fe1 C12 114.25(9) 2 . ? C13 Fe1 C12 40.56(10) . . ? C12 Fe1 C12 115.21(12) 2 . ? C14 Fe1 C11 68.91(8) 2 2 ? C14 Fe1 C11 110.06(8) . 2 ? C10 Fe1 C11 40.76(8) 2 2 ? C10 Fe1 C11 136.97(8) . 2 ? C13 Fe1 C11 68.55(8) 2 2 ? C13 Fe1 C11 112.37(8) . 2 ? C12 Fe1 C11 40.56(9) 2 2 ? C12 Fe1 C11 141.62(9) . 2 ? C14 Fe1 C11 110.06(8) 2 . ? C14 Fe1 C11 68.91(8) . . ? C10 Fe1 C11 136.97(8) 2 . ? C10 Fe1 C11 40.76(8) . . ? C13 Fe1 C11 112.36(8) 2 . ? C13 Fe1 C11 68.55(8) . . ? C12 Fe1 C11 141.62(9) 2 . ? C12 Fe1 C11 40.57(9) . . ? C11 Fe1 C11 177.40(14) 2 . ? C18 O13 C19 120.98(14) . . ? C15 N11 C10 127.59(15) . . ? C15 N11 H11 116.2 . . ? C10 N11 H11 116.2 . . ? C18 N12 C16 122.06(14) . . ? C18 N12 H12 119.0 . . ? C16 N12 H12 119.0 . . ? N11 C10 C14 121.42(17) . . ? N11 C10 C11 129.79(18) . . ? C14 C10 C11 108.79(17) . . ? N11 C10 Fe1 126.73(13) . . ? C14 C10 Fe1 69.56(11) . . ? C11 C10 Fe1 70.17(10) . . ? C12 C11 C10 107.15(14) . . ? C12 C11 Fe1 69.52(11) . . ? C10 C11 Fe1 69.08(10) . . ? C12 C11 H11A 126.4 . . ? C10 C11 H11A 126.4 . . ? Fe1 C11 H11A 126.5 . . ? C13 C12 C11 108.62(19) . . ? C13 C12 Fe1 69.47(12) . . ? C11 C12 Fe1 69.92(10) . . ? C13 C12 H12A 125.7 . . ? C11 C12 H12A 125.7 . . ? Fe1 C12 H12A 126.5 . . ? C12 C13 C14 108.1(2) . . ? C12 C13 Fe1 69.97(12) . . ? C14 C13 Fe1 69.40(14) . . ? C12 C13 H13 126.0 . . ? C14 C13 H13 126.0 . . ? Fe1 C13 H13 126.3 . . ? C10 C14 C13 107.3(2) . . ? C10 C14 Fe1 69.62(11) . . ? C13 C14 Fe1 69.66(14) . . ? C10 C14 H14 126.3 . . ? C13 C14 H14 126.3 . . ? Fe1 C14 H14 126.0 . . ? O11 C15 N11 124.97(16) . . ? O11 C15 C16 121.93(15) . . ? N11 C15 C16 113.03(13) . . ? N12 C16 C17 108.92(14) . . ? N12 C16 C15 111.82(13) . . ? C17 C16 C15 108.56(14) . . ? N12 C16 H16 109.2 . . ? C17 C16 H16 109.2 . . ? C15 C16 H16 109.2 . . ? 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 . . ? O12 C18 N12 124.20(16) . . ? O12 C18 O13 125.27(17) . . ? N12 C18 O13 110.52(14) . . ? O13 C19 C110 108.76(19) . . ? O13 C19 C111 111.33(18) . . ? C110 C19 C111 112.8(2) . . ? O13 C19 C112 101.29(17) . . ? C110 C19 C112 111.8(2) . . ? C111 C19 C112 110.3(2) . . ? C19 C110 H11B 109.5 . . ? C19 C110 H11C 109.5 . . ? H11B C110 H11C 109.5 . . ? C19 C110 H11D 109.5 . . ? H11B C110 H11D 109.5 . . ? H11C C110 H11D 109.5 . . ? C19 C111 H11E 109.5 . . ? C19 C111 H11F 109.5 . . ? H11E C111 H11F 109.5 . . ? C19 C111 H11G 109.5 . . ? H11E C111 H11G 109.5 . . ? H11F C111 H11G 109.5 . . ? C19 C112 H11H 109.5 . . ? C19 C112 H11I 109.5 . . ? H11H C112 H11I 109.5 . . ? C19 C112 H11J 109.5 . . ? H11H C112 H11J 109.5 . . ? H11I C112 H11J 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 C15 N11 C10 C14 160.43(17) . . . . ? C15 N11 C10 C11 -20.5(3) . . . . ? C15 N11 C10 Fe1 73.6(2) . . . . ? C14 Fe1 C10 N11 -26.08(18) 2 . . . ? C14 Fe1 C10 N11 114.6(2) . . . . ? C10 Fe1 C10 N11 17.09(12) 2 . . . ? C13 Fe1 C10 N11 -60.9(2) 2 . . . ? C13 Fe1 C10 N11 152.85(19) . . . . ? C12 Fe1 C10 N11 -163.3(2) . . . . ? C11 Fe1 C10 N11 52.7(2) 2 . . . ? C11 Fe1 C10 N11 -125.4(2) . . . . ? C14 Fe1 C10 C14 -140.66(12) 2 . . . ? C10 Fe1 C10 C14 -97.49(12) 2 . . . ? C13 Fe1 C10 C14 -175.50(15) 2 . . . ? C13 Fe1 C10 C14 38.27(12) . . . . ? C12 Fe1 C10 C14 82.08(14) . . . . ? C11 Fe1 C10 C14 -61.88(15) 2 . . . ? C11 Fe1 C10 C14 120.00(16) . . . . ? C14 Fe1 C10 C11 99.35(12) 2 . . . ? C14 Fe1 C10 C11 -120.00(16) . . . . ? C10 Fe1 C10 C11 142.51(13) 2 . . . ? C13 Fe1 C10 C11 64.51(15) 2 . . . ? C13 Fe1 C10 C11 -81.72(12) . . . . ? C12 Fe1 C10 C11 -37.92(11) . . . . ? C11 Fe1 C10 C11 178.12(10) 2 . . . ? N11 C10 C11 C12 -178.9(2) . . . . ? C14 C10 C11 C12 0.33(18) . . . . ? Fe1 C10 C11 C12 59.33(11) . . . . ? N11 C10 C11 Fe1 121.8(2) . . . . ? C14 C10 C11 Fe1 -59.01(13) . . . . ? C14 Fe1 C11 C12 145.67(12) 2 . . . ? C14 Fe1 C11 C12 -81.32(13) . . . . ? C10 Fe1 C11 C12 -176.47(16) 2 . . . ? C10 Fe1 C11 C12 -118.68(13) . . . . ? C13 Fe1 C11 C12 101.67(13) 2 . . . ? C13 Fe1 C11 C12 -37.24(13) . . . . ? C12 Fe1 C11 C12 65.2(2) 2 . . . ? C14 Fe1 C11 C10 -95.65(11) 2 . . . ? C14 Fe1 C11 C10 37.36(11) . . . . ? C10 Fe1 C11 C10 -57.79(19) 2 . . . ? C13 Fe1 C11 C10 -139.65(11) 2 . . . ? C13 Fe1 C11 C10 81.44(12) . . . . ? C12 Fe1 C11 C10 -176.17(16) 2 . . . ? C12 Fe1 C11 C10 118.68(13) . . . . ? C10 C11 C12 C13 -0.19(19) . . . . ? Fe1 C11 C12 C13 58.86(15) . . . . ? C10 C11 C12 Fe1 -59.05(11) . . . . ? C14 Fe1 C12 C13 -175.33(15) 2 . . . ? C14 Fe1 C12 C13 -37.84(13) . . . . ? C10 Fe1 C12 C13 -81.90(14) . . . . ? C13 Fe1 C12 C13 143.38(14) 2 . . . ? C12 Fe1 C12 C13 98.52(13) 2 . . . ? C11 Fe1 C12 C13 57.81(19) 2 . . . ? C11 Fe1 C12 C13 -119.99(19) . . . . ? C14 Fe1 C12 C11 -55.34(17) 2 . . . ? C14 Fe1 C12 C11 82.15(13) . . . . ? C10 Fe1 C12 C11 38.10(11) . . . . ? C13 Fe1 C12 C11 -96.63(13) 2 . . . ? C13 Fe1 C12 C11 119.99(19) . . . . ? C12 Fe1 C12 C11 -141.49(14) 2 . . . ? C11 Fe1 C12 C11 177.80(12) 2 . . . ? C11 C12 C13 C14 0.0(3) . . . . ? Fe1 C12 C13 C14 59.12(17) . . . . ? C11 C12 C13 Fe1 -59.13(14) . . . . ? C14 Fe1 C13 C12 119.4(2) . . . . ? C10 Fe1 C13 C12 175.03(14) 2 . . . ? C10 Fe1 C13 C12 81.20(12) . . . . ? C13 Fe1 C13 C12 -62.02(12) 2 . . . ? C12 Fe1 C13 C12 -101.07(17) 2 . . . ? C11 Fe1 C13 C12 -145.38(13) 2 . . . ? C11 Fe1 C13 C12 37.24(13) . . . . ? C10 Fe1 C13 C14 55.7(2) 2 . . . ? C10 Fe1 C13 C14 -38.16(14) . . . . ? C13 Fe1 C13 C14 178.61(16) 2 . . . ? C12 Fe1 C13 C14 139.57(15) 2 . . . ? C12 Fe1 C13 C14 -119.4(2) . . . . ? C11 Fe1 C13 C14 95.26(16) 2 . . . ? C11 Fe1 C13 C14 -82.12(16) . . . . ? N11 C10 C14 C13 178.95(18) . . . . ? C11 C10 C14 C13 -0.3(3) . . . . ? Fe1 C10 C14 C13 -59.71(17) . . . . ? N11 C10 C14 Fe1 -121.34(17) . . . . ? C11 C10 C14 Fe1 59.38(13) . . . . ? C12 C13 C14 C10 0.2(3) . . . . ? Fe1 C13 C14 C10 59.69(15) . . . . ? C12 C13 C14 Fe1 -59.48(16) . . . . ? C14 Fe1 C14 C10 60.11(10) 2 . . . ? C10 Fe1 C14 C10 96.86(14) 2 . . . ? C13 Fe1 C14 C10 -118.5(2) . . . . ? C12 Fe1 C14 C10 174.87(14) 2 . . . ? C12 Fe1 C14 C10 -80.97(11) . . . . ? C11 Fe1 C14 C10 140.16(12) 2 . . . ? C11 Fe1 C14 C10 -37.30(12) . . . . ? C14 Fe1 C14 C13 178.58(17) 2 . . . ? C10 Fe1 C14 C13 -144.68(15) 2 . . . ? C10 Fe1 C14 C13 118.5(2) . . . . ? C12 Fe1 C14 C13 -66.7(2) 2 . . . ? C12 Fe1 C14 C13 37.50(15) . . . . ? C11 Fe1 C14 C13 -101.38(16) 2 . . . ? C11 Fe1 C14 C13 81.17(16) . . . . ? C10 N11 C15 O11 2.1(3) . . . . ? C10 N11 C15 C16 179.03(15) . . . . ? C18 N12 C16 C17 -174.45(17) . . . . ? C18 N12 C16 C15 -54.5(2) . . . . ? O11 C15 C16 N12 -39.5(2) . . . . ? N11 C15 C16 N12 143.48(14) . . . . ? O11 C15 C16 C17 80.73(19) . . . . ? N11 C15 C16 C17 -96.33(16) . . . . ? C16 N12 C18 O12 4.2(3) . . . . ? C16 N12 C18 O13 -175.07(15) . . . . ? C19 O13 C18 O12 16.3(3) . . . . ? C19 O13 C18 N12 -164.44(16) . . . . ? C18 O13 C19 C110 63.2(2) . . . . ? C18 O13 C19 C111 -61.7(2) . . . . ? C18 O13 C19 C112 -178.98(19) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 30.08 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.258 _refine_diff_density_min -0.444 _refine_diff_density_rms 0.078 #===END data_8 _database_code_depnum_ccdc_archive 'CCDC 265457' # originally saved as 160 # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H38 Fe N4 O6' _chemical_formula_sum 'C26 H38 Fe N4 O6' _chemical_formula_weight 558.45 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' # Crystal Data _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2 _symmetry_space_group_name_Hall 'C 2y' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 15.490(3) _cell_length_b 9.3390(19) _cell_length_c 11.036(2) _cell_angle_alpha 90.00 _cell_angle_beta 117.09(3) _cell_angle_gamma 90.00 _cell_volume 1421.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1625 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.305 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 592 _exptl_absorpt_coefficient_mu 0.575 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8839 _exptl_absorpt_correction_T_max 0.9718 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski & Minor 1997)' _exptl_special_details ; ? ; # EXPERIMENTAL DETAIL _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR590D, fine-focus sealed tube' _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type 'KappaCCD (BruKer AXS-Nonius, FR540C)' _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'no decay' _diffrn_reflns_number 2796 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0640 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 26.36 _reflns_number_total 2795 _reflns_number_gt 2529 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution ; SIR-97 (A. Altomare, G. Cascarano et al.) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; Cameron (WinGX v1.64-05), Ortep (SHELXTL-NT v6.14, Bruker AXS) ; _computing_publication_material 'WinGX v1.64-05 (L. J. Farrugia)' # REFINEMENT DATA _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^ > 2sigma(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^)+(0.0079P)^2^+1.0130P] 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_abs_structure_Flack 0.026(17) _chemical_absolute_configuration . _refine_ls_abs_structure_details 'Flack (1983), 1249 Friedel pairs' _refine_ls_number_reflns 2795 _refine_ls_number_parameters 172 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0488 _refine_ls_R_factor_gt 0.0393 _refine_ls_wR_factor_ref 0.0810 _refine_ls_wR_factor_gt 0.0755 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 Fe1 Fe 0.0000 1.20800(4) 0.0000 0.02425(15) Uani 1 2 d S . . O11 O 0.18547(15) 0.9411(2) -0.0253(2) 0.0330(5) Uani 1 1 d . . . O12 O 0.13521(14) 0.7568(2) 0.17303(19) 0.0338(5) Uani 1 1 d . . . O13 O 0.25443(15) 0.5876(2) 0.24617(18) 0.0309(5) Uani 1 1 d . . . N11 N 0.02026(16) 0.9333(2) -0.1425(2) 0.0220(5) Uani 1 1 d . . . H11 H -0.0286 0.8733 -0.1809 0.026 Uiso 1 1 calc . . . N12 N 0.18031(17) 0.6442(2) 0.0290(2) 0.0247(5) Uani 1 1 d . . . H12 H 0.2221 0.5849 0.0225 0.030 Uiso 1 1 calc . . . C10 C -0.0041(2) 1.0807(3) -0.1527(3) 0.0217(6) Uani 1 1 d . . . C11 C 0.05444(18) 1.2032(4) -0.1379(2) 0.0281(5) Uani 1 1 d . . . H11A H 0.1210 1.2032 -0.1174 0.034 Uiso 1 1 calc . . . C12 C -0.0050(3) 1.3250(3) -0.1592(3) 0.0339(8) Uani 1 1 d . . . H12A H 0.0149 1.4218 -0.1560 0.041 Uiso 1 1 calc . . . C13 C -0.0987(3) 1.2787(3) -0.1861(3) 0.0312(8) Uani 1 1 d . . . H13 H -0.1526 1.3390 -0.2040 0.037 Uiso 1 1 calc . . . C14 C -0.0990(2) 1.1263(3) -0.1820(3) 0.0261(7) Uani 1 1 d . . . H14 H -0.1525 1.0666 -0.1962 0.031 Uiso 1 1 calc . . . C15 C 0.1094(2) 0.8741(3) -0.0810(2) 0.0219(6) Uani 1 1 d . . . C16 C 0.10751(16) 0.7102(4) -0.0933(2) 0.0234(5) Uani 1 1 d . . . H16 H 0.0420 0.6741 -0.1111 0.028 Uiso 1 1 calc R . . C17 C 0.1270(2) 0.6701(3) -0.2125(3) 0.0384(8) Uani 1 1 d . . . H17A H 0.1261 0.5657 -0.2216 0.046 Uiso 1 1 calc R . . H17B H 0.1906 0.7069 -0.1962 0.046 Uiso 1 1 calc R . . H17C H 0.0767 0.7121 -0.2964 0.046 Uiso 1 1 calc R . . C18 C 0.1863(2) 0.6701(3) 0.1518(3) 0.0245(6) Uani 1 1 d . . . C19 C 0.2924(2) 0.6197(4) 0.3929(3) 0.0371(8) Uani 1 1 d . . . C110 C 0.3430(3) 0.7634(4) 0.4212(4) 0.0537(10) Uani 1 1 d . . . H11B H 0.2953 0.8389 0.3752 0.064 Uiso 1 1 calc R . . H11C H 0.3915 0.7629 0.3873 0.064 Uiso 1 1 calc R . . H11D H 0.3751 0.7812 0.5195 0.064 Uiso 1 1 calc R . . C111 C 0.2131(3) 0.6128(4) 0.4360(3) 0.0521(9) Uani 1 1 d . . . H11E H 0.1763 0.5239 0.4022 0.063 Uiso 1 1 calc R . . H11F H 0.1697 0.6950 0.3982 0.063 Uiso 1 1 calc R . . H11G H 0.2419 0.6150 0.5355 0.063 Uiso 1 1 calc R . . C112 C 0.3639(3) 0.4981(4) 0.4563(3) 0.0637(12) Uani 1 1 d . . . H11H H 0.4125 0.5006 0.4226 0.076 Uiso 1 1 calc R . . H11I H 0.3293 0.4065 0.4316 0.076 Uiso 1 1 calc R . . H11J H 0.3961 0.5085 0.5555 0.076 Uiso 1 1 calc R . . 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 0.0274(3) 0.0156(2) 0.0281(3) 0.000 0.0111(2) 0.000 O11 0.0260(11) 0.0266(11) 0.0449(12) 0.0015(9) 0.0150(10) -0.0077(9) O12 0.0330(12) 0.0350(12) 0.0372(11) 0.0022(8) 0.0191(10) 0.0126(9) O13 0.0344(13) 0.0275(10) 0.0257(10) 0.0003(8) 0.0092(10) 0.0093(9) N11 0.0223(13) 0.0157(11) 0.0258(12) -0.0012(9) 0.0092(10) -0.0007(10) N12 0.0248(13) 0.0217(11) 0.0283(12) 0.0025(9) 0.0128(11) 0.0074(10) C10 0.0248(17) 0.0157(15) 0.0205(14) 0.0021(12) 0.0067(13) -0.0019(13) C11 0.0341(15) 0.0207(12) 0.0318(12) 0.0045(16) 0.0171(12) 0.0000(17) C12 0.048(2) 0.0171(17) 0.0385(18) 0.0051(14) 0.0215(18) 0.0014(15) C13 0.036(2) 0.0233(17) 0.0295(18) 0.0062(13) 0.0110(16) 0.0080(14) C14 0.0250(18) 0.0218(17) 0.0280(17) 0.0014(13) 0.0090(15) 0.0004(13) C15 0.0253(16) 0.0207(13) 0.0214(13) -0.0017(11) 0.0121(12) -0.0045(12) C16 0.0216(13) 0.0186(11) 0.0285(12) 0.0008(16) 0.0102(10) 0.0009(16) C17 0.050(2) 0.035(2) 0.0325(15) -0.0012(12) 0.0214(15) 0.0061(14) C18 0.0206(15) 0.0200(16) 0.0323(15) 0.0034(10) 0.0116(13) 0.0029(11) C19 0.040(2) 0.0366(19) 0.0265(16) -0.0023(13) 0.0084(15) 0.0065(15) C110 0.054(2) 0.055(2) 0.045(2) -0.0164(16) 0.0161(19) -0.0123(19) C111 0.061(3) 0.062(2) 0.0362(18) 0.0018(16) 0.0249(18) -0.0001(19) C112 0.070(3) 0.068(3) 0.0278(17) 0.0050(17) 0.0006(18) 0.030(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; # MOLECULAR GEOMETRY 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 C13 2.033(3) 2 ? Fe1 C13 2.033(3) . ? Fe1 C10 2.039(3) . ? Fe1 C10 2.039(3) 2 ? Fe1 C14 2.041(3) 2 ? Fe1 C14 2.041(3) . ? Fe1 C12 2.041(3) 2 ? Fe1 C12 2.041(3) . ? Fe1 C11 2.048(2) . ? Fe1 C11 2.048(2) 2 ? O11 C15 1.224(3) . ? O12 C18 1.228(3) . ? O13 C18 1.338(3) . ? O13 C19 1.480(3) . ? N11 C15 1.349(3) . ? N11 C10 1.419(4) . ? N11 H11 0.8800 . ? N12 C18 1.337(3) . ? N12 C16 1.445(3) . ? N12 H12 0.8800 . ? C10 C14 1.419(5) . ? C10 C11 1.422(4) . ? C11 C12 1.414(5) . ? C11 H11A 0.9500 . ? C12 C13 1.411(5) . ? C12 H12A 0.9500 . ? C13 C14 1.424(3) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.536(4) . ? C16 C17 1.524(3) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C19 C111 1.506(5) . ? C19 C110 1.513(4) . ? C19 C112 1.517(5) . ? C110 H11B 0.9800 . ? C110 H11C 0.9800 . ? C110 H11D 0.9800 . ? C111 H11E 0.9800 . ? C111 H11F 0.9800 . ? C111 H11G 0.9800 . ? C112 H11H 0.9800 . ? C112 H11I 0.9800 . ? C112 H11J 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 C13 Fe1 C13 142.12(19) 2 . ? C13 Fe1 C10 138.61(14) 2 . ? C13 Fe1 C10 68.17(13) . . ? C13 Fe1 C10 68.17(13) 2 2 ? C13 Fe1 C10 138.61(14) . 2 ? C10 Fe1 C10 108.69(16) . 2 ? C13 Fe1 C14 40.92(10) 2 2 ? C13 Fe1 C14 176.81(15) . 2 ? C10 Fe1 C14 108.79(12) . 2 ? C10 Fe1 C14 40.70(13) 2 2 ? C13 Fe1 C14 176.81(15) 2 . ? C13 Fe1 C14 40.92(10) . . ? C10 Fe1 C14 40.70(13) . . ? C10 Fe1 C14 108.79(12) 2 . ? C14 Fe1 C14 136.08(17) 2 . ? C13 Fe1 C12 40.54(15) 2 2 ? C13 Fe1 C12 114.35(14) . 2 ? C10 Fe1 C12 176.71(14) . 2 ? C10 Fe1 C12 68.03(9) 2 2 ? C14 Fe1 C12 68.64(14) 2 2 ? C14 Fe1 C12 139.88(14) . 2 ? C13 Fe1 C12 114.36(14) 2 . ? C13 Fe1 C12 40.53(15) . . ? C10 Fe1 C12 68.03(9) . . ? C10 Fe1 C12 176.71(14) 2 . ? C14 Fe1 C12 139.88(14) 2 . ? C14 Fe1 C12 68.64(14) . . ? C12 Fe1 C12 115.24(18) 2 . ? C13 Fe1 C11 112.51(13) 2 . ? C13 Fe1 C11 68.36(12) . . ? C10 Fe1 C11 40.73(13) . . ? C10 Fe1 C11 137.10(13) 2 . ? C14 Fe1 C11 110.12(12) 2 . ? C14 Fe1 C11 68.88(12) . . ? C12 Fe1 C11 141.65(14) 2 . ? C12 Fe1 C11 40.45(13) . . ? C13 Fe1 C11 68.36(12) 2 2 ? C13 Fe1 C11 112.51(13) . 2 ? C10 Fe1 C11 137.10(13) . 2 ? C10 Fe1 C11 40.73(13) 2 2 ? C14 Fe1 C11 68.88(12) 2 2 ? C14 Fe1 C11 110.12(12) . 2 ? C12 Fe1 C11 40.45(13) 2 2 ? C12 Fe1 C11 141.65(14) . 2 ? C11 Fe1 C11 177.5(2) . 2 ? C18 O13 C19 120.9(2) . . ? C15 N11 C10 127.7(2) . . ? C15 N11 H11 116.1 . . ? C10 N11 H11 116.1 . . ? C18 N12 C16 122.3(2) . . ? C18 N12 H12 118.8 . . ? C16 N12 H12 118.8 . . ? N11 C10 C14 121.3(3) . . ? N11 C10 C11 129.7(3) . . ? C14 C10 C11 109.0(3) . . ? N11 C10 Fe1 126.39(19) . . ? C14 C10 Fe1 69.70(18) . . ? C11 C10 Fe1 69.99(16) . . ? C12 C11 C10 107.2(2) . . ? C12 C11 Fe1 69.48(16) . . ? C10 C11 Fe1 69.29(15) . . ? C12 C11 H11A 126.4 . . ? C10 C11 H11A 126.4 . . ? Fe1 C11 H11A 126.4 . . ? C13 C12 C11 108.5(3) . . ? C13 C12 Fe1 69.43(19) . . ? C11 C12 Fe1 70.07(16) . . ? C13 C12 H12A 125.7 . . ? C11 C12 H12A 125.7 . . ? Fe1 C12 H12A 126.3 . . ? C12 C13 C14 108.5(3) . . ? C12 C13 Fe1 70.03(19) . . ? C14 C13 Fe1 69.8(2) . . ? C12 C13 H13 125.7 . . ? C14 C13 H13 125.7 . . ? Fe1 C13 H13 126.0 . . ? C10 C14 C13 106.8(3) . . ? C10 C14 Fe1 69.60(18) . . ? C13 C14 Fe1 69.3(2) . . ? C10 C14 H14 126.6 . . ? C13 C14 H14 126.6 . . ? Fe1 C14 H14 126.1 . . ? O11 C15 N11 125.0(3) . . ? O11 C15 C16 121.9(2) . . ? N11 C15 C16 113.0(2) . . ? N12 C16 C17 109.0(2) . . ? N12 C16 C15 111.5(2) . . ? C17 C16 C15 108.5(2) . . ? N12 C16 H16 109.3 . . ? C17 C16 H16 109.3 . . ? C15 C16 H16 109.3 . . ? 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 . . ? O12 C18 N12 124.0(3) . . ? O12 C18 O13 125.4(3) . . ? N12 C18 O13 110.6(2) . . ? O13 C19 C111 111.2(3) . . ? O13 C19 C110 108.4(3) . . ? C111 C19 C110 113.2(3) . . ? O13 C19 C112 101.3(2) . . ? C111 C19 C112 110.6(3) . . ? C110 C19 C112 111.6(3) . . ? C19 C110 H11B 109.5 . . ? C19 C110 H11C 109.5 . . ? H11B C110 H11C 109.5 . . ? C19 C110 H11D 109.5 . . ? H11B C110 H11D 109.5 . . ? H11C C110 H11D 109.5 . . ? C19 C111 H11E 109.5 . . ? C19 C111 H11F 109.5 . . ? H11E C111 H11F 109.5 . . ? C19 C111 H11G 109.5 . . ? H11E C111 H11G 109.5 . . ? H11F C111 H11G 109.5 . . ? C19 C112 H11H 109.5 . . ? C19 C112 H11I 109.5 . . ? H11H C112 H11I 109.5 . . ? C19 C112 H11J 109.5 . . ? H11H C112 H11J 109.5 . . ? H11I C112 H11J 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 C15 N11 C10 C14 -160.4(3) . . . . ? C15 N11 C10 C11 19.8(4) . . . . ? C15 N11 C10 Fe1 -73.6(4) . . . . ? C13 Fe1 C10 N11 60.7(3) 2 . . . ? C13 Fe1 C10 N11 -153.1(3) . . . . ? C10 Fe1 C10 N11 -17.2(2) 2 . . . ? C14 Fe1 C10 N11 25.9(3) 2 . . . ? C14 Fe1 C10 N11 -114.6(3) . . . . ? C12 Fe1 C10 N11 163.1(3) . . . . ? C11 Fe1 C10 N11 125.2(3) . . . . ? C11 Fe1 C10 N11 -53.0(3) 2 . . . ? C13 Fe1 C10 C14 175.3(2) 2 . . . ? C13 Fe1 C10 C14 -38.50(19) . . . . ? C10 Fe1 C10 C14 97.36(19) 2 . . . ? C14 Fe1 C10 C14 140.46(19) 2 . . . ? C12 Fe1 C10 C14 -82.3(2) . . . . ? C11 Fe1 C10 C14 -120.2(3) . . . . ? C11 Fe1 C10 C14 61.6(2) 2 . . . ? C13 Fe1 C10 C11 -64.5(2) 2 . . . ? C13 Fe1 C10 C11 81.74(19) . . . . ? C10 Fe1 C10 C11 -142.4(2) 2 . . . ? C14 Fe1 C10 C11 -99.31(18) 2 . . . ? C14 Fe1 C10 C11 120.2(3) . . . . ? C12 Fe1 C10 C11 37.90(16) . . . . ? C11 Fe1 C10 C11 -178.19(16) 2 . . . ? N11 C10 C11 C12 179.4(3) . . . . ? C14 C10 C11 C12 -0.4(3) . . . . ? Fe1 C10 C11 C12 -59.40(17) . . . . ? N11 C10 C11 Fe1 -121.2(3) . . . . ? C14 C10 C11 Fe1 59.0(2) . . . . ? C13 Fe1 C11 C12 -101.6(2) 2 . . . ? C13 Fe1 C11 C12 37.4(2) . . . . ? C10 Fe1 C11 C12 118.6(2) . . . . ? C10 Fe1 C11 C12 176.7(2) 2 . . . ? C14 Fe1 C11 C12 -145.65(19) 2 . . . ? C14 Fe1 C11 C12 81.4(2) . . . . ? C12 Fe1 C11 C12 -65.0(3) 2 . . . ? C13 Fe1 C11 C10 139.76(17) 2 . . . ? C13 Fe1 C11 C10 -81.24(19) . . . . ? C10 Fe1 C11 C10 58.1(3) 2 . . . ? C14 Fe1 C11 C10 95.76(18) 2 . . . ? C14 Fe1 C11 C10 -37.15(18) . . . . ? C12 Fe1 C11 C10 176.4(3) 2 . . . ? C12 Fe1 C11 C10 -118.6(2) . . . . ? C10 C11 C12 C13 0.3(3) . . . . ? Fe1 C11 C12 C13 -59.0(2) . . . . ? C10 C11 C12 Fe1 59.27(16) . . . . ? C13 Fe1 C12 C13 -143.5(2) 2 . . . ? C14 Fe1 C12 C13 175.1(2) 2 . . . ? C14 Fe1 C12 C13 37.7(2) . . . . ? C12 Fe1 C12 C13 -98.6(2) 2 . . . ? C11 Fe1 C12 C13 119.8(3) . . . . ? C11 Fe1 C12 C13 -58.1(3) 2 . . . ? C13 Fe1 C12 C11 96.7(2) 2 . . . ? C13 Fe1 C12 C11 -119.8(3) . . . . ? C14 Fe1 C12 C11 55.3(3) 2 . . . ? C14 Fe1 C12 C11 -82.1(2) . . . . ? C12 Fe1 C12 C11 141.6(2) 2 . . . ? C11 Fe1 C12 C11 -177.90(18) 2 . . . ? C11 C12 C13 C14 -0.1(4) . . . . ? Fe1 C12 C13 C14 -59.4(3) . . . . ? C11 C12 C13 Fe1 59.4(2) . . . . ? C10 Fe1 C13 C12 -81.28(19) . . . . ? C10 Fe1 C13 C12 -175.2(2) 2 . . . ? C14 Fe1 C13 C12 -119.6(3) . . . . ? C12 Fe1 C13 C12 101.0(3) 2 . . . ? C11 Fe1 C13 C12 -37.3(2) . . . . ? C11 Fe1 C13 C12 145.2(2) 2 . . . ? C13 Fe1 C13 C14 -178.4(3) 2 . . . ? C10 Fe1 C13 C14 38.3(2) . . . . ? C10 Fe1 C13 C14 -55.6(3) 2 . . . ? C12 Fe1 C13 C14 -139.4(2) 2 . . . ? C12 Fe1 C13 C14 119.6(3) . . . . ? C11 Fe1 C13 C14 82.3(2) . . . . ? C11 Fe1 C13 C14 -95.2(2) 2 . . . ? N11 C10 C14 C13 -179.4(3) . . . . ? C11 C10 C14 C13 0.4(4) . . . . ? Fe1 C10 C14 C13 59.5(3) . . . . ? N11 C10 C14 Fe1 121.0(3) . . . . ? C11 C10 C14 Fe1 -59.14(19) . . . . ? C12 C13 C14 C10 -0.2(4) . . . . ? Fe1 C13 C14 C10 -59.8(2) . . . . ? C12 C13 C14 Fe1 59.5(2) . . . . ? C13 Fe1 C14 C10 118.1(3) . . . . ? C10 Fe1 C14 C10 -97.1(2) 2 . . . ? C14 Fe1 C14 C10 -60.33(16) 2 . . . ? C12 Fe1 C14 C10 -175.0(2) 2 . . . ? C12 Fe1 C14 C10 80.72(18) . . . . ? C11 Fe1 C14 C10 37.17(19) . . . . ? C11 Fe1 C14 C10 -140.39(19) 2 . . . ? C10 Fe1 C14 C13 -118.1(3) . . . . ? C10 Fe1 C14 C13 144.8(2) 2 . . . ? C14 Fe1 C14 C13 -178.4(3) 2 . . . ? C12 Fe1 C14 C13 66.9(3) 2 . . . ? C12 Fe1 C14 C13 -37.4(2) . . . . ? C11 Fe1 C14 C13 -80.9(2) . . . . ? C11 Fe1 C14 C13 101.5(2) 2 . . . ? C10 N11 C15 O11 -1.8(4) . . . . ? C10 N11 C15 C16 -178.8(2) . . . . ? C18 N12 C16 C17 174.3(3) . . . . ? C18 N12 C16 C15 54.5(3) . . . . ? O11 C15 C16 N12 39.6(3) . . . . ? N11 C15 C16 N12 -143.3(2) . . . . ? O11 C15 C16 C17 -80.5(3) . . . . ? N11 C15 C16 C17 96.7(3) . . . . ? C16 N12 C18 O12 -4.2(4) . . . . ? C16 N12 C18 O13 175.0(2) . . . . ? C19 O13 C18 O12 -16.1(4) . . . . ? C19 O13 C18 N12 164.7(2) . . . . ? C18 O13 C19 C111 61.4(4) . . . . ? C18 O13 C19 C110 -63.6(3) . . . . ? C18 O13 C19 C112 178.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.36 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.204 _refine_diff_density_min -0.327 _refine_diff_density_rms 0.054 #===END