# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 1350 loop_ _publ_author_name 'Mario Ruben' 'Roman Boca' 'Olaf Fuhr' 'Jan Pavlik' 'Chandrasekar Rajadurai' 'Ivan Salitros' _publ_contact_author_name 'Mario Ruben' _publ_contact_author_email MARIO.RUBEN@INT.FZK.DE _publ_section_title ; Supramolecular lattice-solvent control of iron(II) spin transition parameters ; # Attachment 'comp1.CIF' data_c:\alle\m-pyfe2\pyfe2 _database_code_depnum_ccdc_archive 'CCDC 764304' #TrackingRef 'comp1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H24 Cl2 Fe N12 O8' _chemical_formula_weight 831.38 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 41.327(8) _cell_length_b 9.790(2) _cell_length_c 16.801(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.67(3) _cell_angle_gamma 90.00 _cell_volume 6605(2) _cell_formula_units_Z 8 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.672 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3392 _exptl_absorpt_coefficient_mu 0.693 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11023 _diffrn_reflns_av_R_equivalents 0.0728 _diffrn_reflns_av_sigmaI/netI 0.1148 _diffrn_reflns_limit_h_min -49 _diffrn_reflns_limit_h_max 50 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 25.66 _reflns_number_total 6055 _reflns_number_gt 3363 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.0765P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00169(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6055 _refine_ls_number_parameters 493 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1265 _refine_ls_R_factor_gt 0.0647 _refine_ls_wR_factor_ref 0.1617 _refine_ls_wR_factor_gt 0.1375 _refine_ls_goodness_of_fit_ref 0.930 _refine_ls_restrained_S_all 0.930 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.381803(16) 0.63646(8) 0.51046(5) 0.0324(2) Uani 1 1 d . . . N1 N 0.38984(10) 0.4997(5) 0.5993(3) 0.0369(11) Uani 1 1 d . . . N2 N 0.36034(10) 0.4442(5) 0.6112(3) 0.0374(11) Uani 1 1 d . . . N3 N 0.33775(10) 0.5795(5) 0.5045(3) 0.0345(11) Uani 1 1 d . . . N4 N 0.32400(9) 0.7265(5) 0.3987(3) 0.0353(11) Uani 1 1 d . . . N5 N 0.35786(10) 0.7496(5) 0.4178(3) 0.0363(11) Uani 1 1 d . . . N6 N 0.18453(10) 0.4041(5) 0.4043(3) 0.0425(12) Uani 1 1 d . . . N7 N 0.38552(9) 0.7828(4) 0.5919(3) 0.0342(11) Uani 1 1 d . . . N8 N 0.41707(10) 0.8407(5) 0.6129(3) 0.0350(10) Uani 1 1 d . . . N9 N 0.42621(10) 0.6920(5) 0.5182(3) 0.0344(10) Uani 1 1 d . . . N10 N 0.42602(10) 0.5327(5) 0.4220(3) 0.0367(11) Uani 1 1 d . . . N11 N 0.39402(10) 0.5102(5) 0.4314(3) 0.0385(11) Uani 1 1 d . . . N12 N 0.57182(11) 0.9700(5) 0.5920(4) 0.0447(13) Uani 1 1 d . . . C1 C 0.41359(13) 0.4384(6) 0.6547(4) 0.0400(14) Uani 1 1 d . . . H1A H 0.4367 0.4555 0.6617 0.048 Uiso 1 1 calc R . . C2 C 0.40025(13) 0.3456(6) 0.7015(4) 0.0432(14) Uani 1 1 d . . . H2A H 0.4123 0.2900 0.7449 0.052 Uiso 1 1 calc R . . C3 C 0.36685(14) 0.3505(6) 0.6728(4) 0.0446(14) Uani 1 1 d . . . H3A H 0.3509 0.2983 0.6921 0.054 Uiso 1 1 calc R . . C4 C 0.33122(12) 0.4864(5) 0.5578(4) 0.0347(13) Uani 1 1 d . . . C5 C 0.29936(12) 0.4424(6) 0.5575(4) 0.0362(13) Uani 1 1 d . . . H5A H 0.2953 0.3779 0.5962 0.043 Uiso 1 1 calc R . . C6 C 0.27325(12) 0.4982(6) 0.4968(4) 0.0376(13) Uani 1 1 d . . . C7 C 0.27964(12) 0.5957(6) 0.4412(4) 0.0370(13) Uani 1 1 d . . . H7A H 0.2622 0.6354 0.4007 0.044 Uiso 1 1 calc R . . C8 C 0.31242(12) 0.6312(6) 0.4480(4) 0.0362(12) Uani 1 1 d . . . C9 C 0.30847(13) 0.7974(6) 0.3313(4) 0.0400(14) Uani 1 1 d . . . H9A H 0.2853 0.7974 0.3063 0.048 Uiso 1 1 calc R . . C10 C 0.33281(13) 0.8695(6) 0.3060(4) 0.0427(14) Uani 1 1 d . . . H10A H 0.3299 0.9296 0.2604 0.051 Uiso 1 1 calc R . . C11 C 0.36272(12) 0.8363(5) 0.3610(4) 0.0345(12) Uani 1 1 d . . . H11A H 0.3839 0.8713 0.3582 0.041 Uiso 1 1 calc R . . C12 C 0.23844(12) 0.4551(6) 0.4910(4) 0.0352(13) Uani 1 1 d . . . C13 C 0.21687(12) 0.4408(6) 0.4154(4) 0.0393(13) Uani 1 1 d . . . H13A H 0.2252 0.4576 0.3682 0.047 Uiso 1 1 calc R . . C14 C 0.17388(13) 0.3815(6) 0.4723(4) 0.0454(15) Uani 1 1 d . . . H14A H 0.1512 0.3568 0.4663 0.054 Uiso 1 1 calc R . . C15 C 0.19334(13) 0.3915(7) 0.5495(4) 0.0461(15) Uani 1 1 d . . . H15A H 0.1842 0.3742 0.5954 0.055 Uiso 1 1 calc R . . C16 C 0.22669(13) 0.4272(6) 0.5607(4) 0.0445(15) Uani 1 1 d . . . H16A H 0.2410 0.4325 0.6140 0.053 Uiso 1 1 calc R . . C17 C 0.36887(12) 0.8444(6) 0.6408(4) 0.0393(13) Uani 1 1 d . . . H17A H 0.3462 0.8276 0.6403 0.047 Uiso 1 1 calc R . . C18 C 0.38942(12) 0.9374(6) 0.6932(4) 0.0412(14) Uani 1 1 d . . . H18A H 0.3835 0.9921 0.7343 0.049 Uiso 1 1 calc R . . C19 C 0.41963(13) 0.9335(6) 0.6730(4) 0.0395(13) Uani 1 1 d . . . H19A H 0.4387 0.9863 0.6970 0.047 Uiso 1 1 calc R . . C20 C 0.43979(12) 0.7920(5) 0.5696(4) 0.0342(12) Uani 1 1 d . . . C21 C 0.47193(11) 0.8385(6) 0.5770(4) 0.0345(12) Uani 1 1 d . . . H21A H 0.4809 0.9099 0.6139 0.041 Uiso 1 1 calc R . . C22 C 0.49081(12) 0.7760(6) 0.5277(4) 0.0349(13) Uani 1 1 d . . . C23 C 0.47679(11) 0.6714(6) 0.4727(4) 0.0351(12) Uani 1 1 d . . . H23A H 0.4890 0.6291 0.4382 0.042 Uiso 1 1 calc R . . C24 C 0.44449(11) 0.6332(6) 0.4713(3) 0.0348(12) Uani 1 1 d . . . C25 C 0.43286(14) 0.4490(6) 0.3627(4) 0.0441(15) Uani 1 1 d . . . H25A H 0.4532 0.4447 0.3459 0.053 Uiso 1 1 calc R . . C26 C 0.40531(14) 0.3737(7) 0.3327(4) 0.0495(15) Uani 1 1 d . . . H26A H 0.4025 0.3065 0.2908 0.059 Uiso 1 1 calc R . . C27 C 0.38168(13) 0.4148(6) 0.3760(4) 0.0408(14) Uani 1 1 d . . . H27A H 0.3597 0.3791 0.3668 0.049 Uiso 1 1 calc R . . C28 C 0.52546(12) 0.8226(6) 0.5314(4) 0.0350(12) Uani 1 1 d . . . C29 C 0.54073(13) 0.9211(6) 0.5865(4) 0.0414(14) Uani 1 1 d . . . H29A H 0.5285 0.9570 0.6231 0.050 Uiso 1 1 calc R . . C30 C 0.58850(13) 0.9158(6) 0.5403(5) 0.0486(16) Uani 1 1 d . . . H30A H 0.6104 0.9480 0.5426 0.058 Uiso 1 1 calc R . . C31 C 0.57577(15) 0.8171(7) 0.4845(5) 0.064(2) Uani 1 1 d . . . H31A H 0.5887 0.7813 0.4495 0.077 Uiso 1 1 calc R . . C32 C 0.54382(15) 0.7695(7) 0.4793(5) 0.059(2) Uani 1 1 d . . . H32A H 0.5345 0.7012 0.4404 0.071 Uiso 1 1 calc R . . Cl1 Cl 0.29431(4) 0.6838(2) 0.73718(13) 0.0686(6) Uani 1 1 d . . . Cl2 Cl 0.5000 0.6245(2) 0.7500 0.0392(5) Uani 1 2 d S . . Cl3 Cl 0.5000 0.8298(2) 0.2500 0.0423(5) Uani 1 2 d S . . O1A O 0.2683(2) 0.6833(11) 0.7846(7) 0.062(3) Uiso 0.50 1 d P A 1 O2A O 0.3223(4) 0.7818(16) 0.7668(10) 0.056(5) Uiso 0.50 1 d P A 1 O3A O 0.2987(4) 0.5432(18) 0.7568(12) 0.098(6) Uiso 0.50 1 d P A 1 O4A O 0.2889(2) 0.7217(10) 0.6452(7) 0.054(2) Uiso 0.50 1 d P A 1 O1B O 0.2676(3) 0.7633(16) 0.7588(10) 0.095(4) Uiso 0.50 1 d P A 2 O2B O 0.3218(4) 0.7545(17) 0.7764(12) 0.065(6) Uiso 0.50 1 d P A 2 O3B O 0.3091(3) 0.5439(14) 0.7433(9) 0.071(4) Uiso 0.50 1 d P A 2 O4B O 0.2763(3) 0.6895(12) 0.6582(8) 0.066(3) Uiso 0.50 1 d P A 2 O5 O 0.47166(9) 0.7088(4) 0.7525(3) 0.0473(11) Uani 1 1 d . . . O6 O 0.49201(9) 0.5401(4) 0.6772(3) 0.0480(11) Uani 1 1 d . . . O7 O 0.5000 0.9754(6) 0.2500 0.074(2) Uani 1 2 d S . . O8 O 0.4699(2) 0.7662(9) 0.2304(7) 0.054(2) Uiso 0.50 1 d P . . O9 O 0.5187(3) 0.8090(13) 0.3325(9) 0.088(3) Uiso 0.50 1 d P . . O10 O 0.5217(3) 0.7745(11) 0.2002(8) 0.072(3) Uiso 0.50 1 d P . . 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 0.0281(3) 0.0350(4) 0.0340(5) -0.0010(4) 0.0071(3) -0.0018(3) N1 0.027(2) 0.041(3) 0.044(3) -0.004(2) 0.0095(19) -0.0040(18) N2 0.029(2) 0.044(3) 0.037(3) 0.007(2) 0.0049(19) -0.0034(19) N3 0.033(2) 0.037(2) 0.034(3) 0.006(2) 0.0083(19) 0.0031(18) N4 0.027(2) 0.039(3) 0.039(3) 0.002(2) 0.0065(19) -0.0062(18) N5 0.027(2) 0.038(2) 0.043(3) -0.006(2) 0.0061(19) -0.0061(17) N6 0.031(2) 0.050(3) 0.048(3) -0.003(2) 0.012(2) -0.0052(19) N7 0.0260(19) 0.036(2) 0.041(3) 0.003(2) 0.0090(19) -0.0050(17) N8 0.0299(19) 0.037(3) 0.039(3) 0.000(2) 0.0106(18) -0.0008(18) N9 0.035(2) 0.036(2) 0.033(3) -0.003(2) 0.0105(19) 0.0027(18) N10 0.029(2) 0.043(3) 0.039(3) -0.007(2) 0.0080(19) -0.0053(18) N11 0.028(2) 0.046(3) 0.042(3) -0.002(2) 0.011(2) -0.0053(19) N12 0.034(2) 0.048(3) 0.053(4) -0.008(3) 0.012(2) -0.011(2) C1 0.036(3) 0.041(3) 0.041(4) 0.000(3) 0.005(2) 0.002(2) C2 0.042(3) 0.042(3) 0.042(4) 0.005(3) 0.004(3) 0.000(3) C3 0.046(3) 0.040(3) 0.044(4) 0.009(3) 0.003(3) -0.005(3) C4 0.029(2) 0.038(3) 0.033(3) -0.001(3) 0.001(2) 0.002(2) C5 0.034(2) 0.035(3) 0.040(3) 0.004(3) 0.010(2) -0.006(2) C6 0.030(2) 0.039(3) 0.043(4) -0.001(3) 0.008(2) -0.002(2) C7 0.029(2) 0.039(3) 0.042(4) 0.004(3) 0.005(2) -0.002(2) C8 0.034(2) 0.035(3) 0.040(3) 0.002(3) 0.010(2) -0.002(2) C9 0.032(2) 0.044(3) 0.041(4) 0.009(3) 0.002(2) 0.004(2) C10 0.041(3) 0.048(3) 0.038(3) 0.008(3) 0.008(2) -0.002(3) C11 0.037(2) 0.033(3) 0.034(3) 0.003(2) 0.010(2) -0.003(2) C12 0.032(2) 0.036(3) 0.038(3) 0.002(2) 0.009(2) -0.001(2) C13 0.038(3) 0.042(3) 0.039(4) -0.003(3) 0.011(2) -0.007(2) C14 0.036(3) 0.049(4) 0.054(4) -0.002(3) 0.016(3) -0.007(2) C15 0.041(3) 0.056(4) 0.046(4) -0.001(3) 0.019(3) -0.009(3) C16 0.042(3) 0.050(4) 0.043(4) -0.007(3) 0.013(3) -0.006(3) C17 0.033(2) 0.037(3) 0.047(4) -0.005(3) 0.008(2) -0.001(2) C18 0.037(3) 0.046(3) 0.045(4) -0.011(3) 0.018(3) 0.001(2) C19 0.043(3) 0.036(3) 0.041(4) -0.008(3) 0.013(3) -0.006(2) C20 0.032(2) 0.035(3) 0.037(3) -0.002(2) 0.011(2) 0.000(2) C21 0.030(2) 0.037(3) 0.037(3) -0.003(2) 0.009(2) -0.005(2) C22 0.029(2) 0.040(3) 0.036(3) 0.004(3) 0.010(2) 0.000(2) C23 0.028(2) 0.042(3) 0.036(3) -0.002(3) 0.009(2) -0.001(2) C24 0.031(2) 0.039(3) 0.034(3) -0.008(3) 0.005(2) -0.004(2) C25 0.040(3) 0.046(3) 0.045(4) -0.011(3) 0.007(3) 0.000(2) C26 0.053(3) 0.050(4) 0.044(4) -0.014(3) 0.008(3) -0.003(3) C27 0.040(3) 0.040(3) 0.040(4) -0.010(3) 0.005(2) -0.005(2) C28 0.030(2) 0.038(3) 0.036(3) 0.002(2) 0.006(2) -0.003(2) C29 0.033(3) 0.053(4) 0.039(4) -0.003(3) 0.010(2) -0.005(2) C30 0.034(3) 0.050(4) 0.065(5) -0.010(3) 0.019(3) -0.008(2) C31 0.045(3) 0.066(5) 0.093(6) -0.032(4) 0.039(4) -0.020(3) C32 0.049(3) 0.056(4) 0.083(6) -0.027(4) 0.036(4) -0.019(3) Cl1 0.0471(8) 0.0954(15) 0.0569(12) -0.0158(10) -0.0006(8) 0.0150(9) Cl2 0.0345(8) 0.0414(10) 0.0438(12) 0.000 0.0132(8) 0.000 Cl3 0.0434(9) 0.0396(11) 0.0406(12) 0.000 0.0034(8) 0.000 O5 0.040(2) 0.051(2) 0.057(3) 0.009(2) 0.0224(19) 0.0186(18) O6 0.045(2) 0.054(3) 0.046(3) -0.012(2) 0.0126(19) -0.0110(19) O7 0.065(4) 0.032(3) 0.123(8) 0.000 0.019(4) 0.000 _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. ; 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 N3 1.884(4) . ? Fe1 N9 1.889(4) . ? Fe1 N7 1.962(5) . ? Fe1 N11 1.966(5) . ? Fe1 N1 1.974(5) . ? Fe1 N5 1.976(5) . ? N1 C1 1.325(7) . ? N1 N2 1.391(6) . ? N2 C3 1.362(8) . ? N2 C4 1.383(6) . ? N3 C8 1.336(7) . ? N3 C4 1.349(7) . ? N4 C9 1.355(7) . ? N4 N5 1.378(5) . ? N4 C8 1.403(7) . ? N5 C11 1.327(7) . ? N6 C14 1.335(8) . ? N6 C13 1.354(6) . ? N7 C17 1.334(8) . ? N7 N8 1.389(5) . ? N8 C19 1.344(8) . ? N8 C20 1.400(7) . ? N9 C20 1.338(7) . ? N9 C24 1.344(7) . ? N10 C25 1.369(8) . ? N10 N11 1.386(6) . ? N10 C24 1.392(7) . ? N11 C27 1.333(7) . ? N12 C30 1.340(9) . ? N12 C29 1.354(7) . ? C1 C2 1.398(9) . ? C2 C3 1.351(7) . ? C4 C5 1.383(7) . ? C5 C6 1.407(8) . ? C6 C7 1.405(8) . ? C6 C12 1.480(7) . ? C7 C8 1.377(7) . ? C9 C10 1.376(8) . ? C10 C11 1.396(7) . ? C12 C13 1.375(8) . ? C12 C16 1.398(9) . ? C14 C15 1.358(9) . ? C15 C16 1.391(7) . ? C17 C18 1.404(8) . ? C18 C19 1.369(8) . ? C20 C21 1.382(7) . ? C21 C22 1.405(8) . ? C22 C23 1.409(8) . ? C22 C28 1.490(7) . ? C23 C24 1.381(7) . ? C25 C26 1.350(8) . ? C26 C27 1.407(9) . ? C28 C29 1.382(8) . ? C28 C32 1.388(9) . ? C30 C31 1.362(9) . ? C31 C32 1.383(8) . ? Cl1 O2B 1.360(17) . ? Cl1 O4B 1.361(12) . ? Cl1 O3A 1.417(18) . ? Cl1 O1B 1.465(14) . ? Cl1 O1A 1.481(11) . ? Cl1 O3B 1.494(14) . ? Cl1 O2A 1.496(16) . ? Cl1 O4A 1.553(11) . ? Cl2 O5 1.442(4) 2_656 ? Cl2 O5 1.442(4) . ? Cl2 O6 1.449(4) 2_656 ? Cl2 O6 1.449(4) . ? Cl3 O8 1.361(9) 2_655 ? Cl3 O8 1.361(9) . ? Cl3 O7 1.425(7) . ? Cl3 O9 1.434(14) . ? Cl3 O9 1.434(14) 2_655 ? Cl3 O10 1.468(12) . ? Cl3 O10 1.468(12) 2_655 ? O8 O10 1.138(15) 2_655 ? O8 O9 1.323(16) 2_655 ? O9 O8 1.323(16) 2_655 ? O9 O10 1.665(15) 2_655 ? O10 O8 1.138(15) 2_655 ? O10 O9 1.665(15) 2_655 ? 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 N3 Fe1 N9 179.0(2) . . ? N3 Fe1 N7 99.72(19) . . ? N9 Fe1 N7 80.02(19) . . ? N3 Fe1 N11 100.21(19) . . ? N9 Fe1 N11 80.05(19) . . ? N7 Fe1 N11 160.08(17) . . ? N3 Fe1 N1 80.04(18) . . ? N9 Fe1 N1 98.96(19) . . ? N7 Fe1 N1 89.8(2) . . ? N11 Fe1 N1 93.5(2) . . ? N3 Fe1 N5 80.02(19) . . ? N9 Fe1 N5 100.99(19) . . ? N7 Fe1 N5 94.7(2) . . ? N11 Fe1 N5 88.9(2) . . ? N1 Fe1 N5 160.02(17) . . ? C1 N1 N2 104.6(5) . . ? C1 N1 Fe1 143.3(4) . . ? N2 N1 Fe1 112.1(3) . . ? C3 N2 C4 132.8(5) . . ? C3 N2 N1 110.4(4) . . ? C4 N2 N1 116.7(5) . . ? C8 N3 C4 118.8(4) . . ? C8 N3 Fe1 120.7(4) . . ? C4 N3 Fe1 120.5(3) . . ? C9 N4 N5 111.3(5) . . ? C9 N4 C8 132.3(4) . . ? N5 N4 C8 116.2(4) . . ? C11 N5 N4 104.9(4) . . ? C11 N5 Fe1 142.4(3) . . ? N4 N5 Fe1 112.5(4) . . ? C14 N6 C13 116.1(5) . . ? C17 N7 N8 104.4(4) . . ? C17 N7 Fe1 142.5(3) . . ? N8 N7 Fe1 113.0(3) . . ? C19 N8 N7 111.7(4) . . ? C19 N8 C20 132.6(4) . . ? N7 N8 C20 115.7(4) . . ? C20 N9 C24 118.9(4) . . ? C20 N9 Fe1 120.5(4) . . ? C24 N9 Fe1 120.5(4) . . ? C25 N10 N11 110.8(4) . . ? C25 N10 C24 132.6(5) . . ? N11 N10 C24 116.6(5) . . ? C27 N11 N10 104.4(5) . . ? C27 N11 Fe1 142.8(4) . . ? N10 N11 Fe1 112.4(3) . . ? C30 N12 C29 116.2(5) . . ? N1 C1 C2 111.3(5) . . ? C3 C2 C1 106.3(5) . . ? C2 C3 N2 107.3(5) . . ? N3 C4 N2 110.6(4) . . ? N3 C4 C5 123.1(5) . . ? N2 C4 C5 126.3(5) . . ? C4 C5 C6 116.7(5) . . ? C7 C6 C5 120.9(5) . . ? C7 C6 C12 118.8(5) . . ? C5 C6 C12 120.3(5) . . ? C8 C7 C6 116.9(5) . . ? N3 C8 C7 123.6(5) . . ? N3 C8 N4 110.6(4) . . ? C7 C8 N4 125.8(5) . . ? N4 C9 C10 106.6(4) . . ? C9 C10 C11 105.9(5) . . ? N5 C11 C10 111.3(5) . . ? C13 C12 C16 118.4(5) . . ? C13 C12 C6 119.9(6) . . ? C16 C12 C6 121.7(5) . . ? N6 C13 C12 123.9(6) . . ? N6 C14 C15 124.3(5) . . ? C14 C15 C16 119.5(6) . . ? C15 C16 C12 117.7(6) . . ? N7 C17 C18 110.8(5) . . ? C19 C18 C17 106.2(5) . . ? N8 C19 C18 106.9(5) . . ? N9 C20 C21 123.1(5) . . ? N9 C20 N8 110.7(4) . . ? C21 C20 N8 126.1(5) . . ? C20 C21 C22 117.4(5) . . ? C21 C22 C23 120.2(5) . . ? C21 C22 C28 120.3(5) . . ? C23 C22 C28 119.4(5) . . ? C24 C23 C22 117.0(5) . . ? N9 C24 C23 123.3(5) . . ? N9 C24 N10 110.3(4) . . ? C23 C24 N10 126.4(5) . . ? C26 C25 N10 107.3(5) . . ? C25 C26 C27 106.2(6) . . ? N11 C27 C26 111.3(5) . . ? C29 C28 C32 116.9(5) . . ? C29 C28 C22 121.6(6) . . ? C32 C28 C22 121.5(5) . . ? N12 C29 C28 124.7(6) . . ? N12 C30 C31 123.6(5) . . ? C30 C31 C32 119.3(7) . . ? C31 C32 C28 119.3(6) . . ? O2B Cl1 O4B 130.8(10) . . ? O2B Cl1 O3A 109.5(10) . . ? O4B Cl1 O3A 106.1(9) . . ? O2B Cl1 O1B 101.6(9) . . ? O4B Cl1 O1B 87.1(8) . . ? O3A Cl1 O1B 121.5(10) . . ? O2B Cl1 O1A 111.7(9) . . ? O4B Cl1 O1A 103.0(7) . . ? O3A Cl1 O1A 86.7(9) . . ? O1B Cl1 O1A 35.3(6) . . ? O2B Cl1 O3B 98.7(9) . . ? O4B Cl1 O3B 103.1(7) . . ? O3A Cl1 O3B 20.8(8) . . ? O1B Cl1 O3B 142.3(9) . . ? O1A Cl1 O3B 107.3(8) . . ? O2B Cl1 O2A 11.5(11) . . ? O4B Cl1 O2A 120.0(9) . . ? O3A Cl1 O2A 119.9(9) . . ? O1B Cl1 O2A 98.4(8) . . ? O1A Cl1 O2A 115.2(8) . . ? O3B Cl1 O2A 107.0(8) . . ? O2B Cl1 O4A 105.6(9) . . ? O4B Cl1 O4A 26.2(5) . . ? O3A Cl1 O4A 116.4(9) . . ? O1B Cl1 O4A 100.3(7) . . ? O1A Cl1 O4A 125.7(6) . . ? O3B Cl1 O4A 104.4(7) . . ? O2A Cl1 O4A 95.5(8) . . ? O5 Cl2 O5 110.2(4) 2_656 . ? O5 Cl2 O6 109.1(2) 2_656 2_656 ? O5 Cl2 O6 109.0(2) . 2_656 ? O5 Cl2 O6 109.0(2) 2_656 . ? O5 Cl2 O6 109.1(2) . . ? O6 Cl2 O6 110.4(4) 2_656 . ? O8 Cl3 O8 125.5(8) 2_655 . ? O8 Cl3 O7 117.2(4) 2_655 . ? O8 Cl3 O7 117.2(4) . . ? O8 Cl3 O9 56.5(6) 2_655 . ? O8 Cl3 O9 115.0(7) . . ? O7 Cl3 O9 98.2(5) . . ? O8 Cl3 O9 115.0(7) 2_655 2_655 ? O8 Cl3 O9 56.5(6) . 2_655 ? O7 Cl3 O9 98.2(5) . 2_655 ? O9 Cl3 O9 163.6(10) . 2_655 ? O8 Cl3 O10 47.3(6) 2_655 . ? O8 Cl3 O10 109.9(6) . . ? O7 Cl3 O10 111.7(4) . . ? O9 Cl3 O10 103.7(7) . . ? O9 Cl3 O10 70.0(7) 2_655 . ? O8 Cl3 O10 109.9(6) 2_655 2_655 ? O8 Cl3 O10 47.3(6) . 2_655 ? O7 Cl3 O10 111.7(4) . 2_655 ? O9 Cl3 O10 70.0(7) . 2_655 ? O9 Cl3 O10 103.7(7) 2_655 2_655 ? O10 Cl3 O10 136.7(9) . 2_655 ? O10 O8 O9 135.8(11) 2_655 2_655 ? O10 O8 Cl3 71.3(8) 2_655 . ? O9 O8 Cl3 64.6(7) 2_655 . ? O8 O9 Cl3 59.0(7) 2_655 . ? O8 O9 O10 101.0(10) 2_655 2_655 ? Cl3 O9 O10 56.0(6) . 2_655 ? O8 O10 Cl3 61.4(8) 2_655 . ? O8 O10 O9 113.0(11) 2_655 2_655 ? Cl3 O10 O9 54.0(6) . 2_655 ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 25.66 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.561 _refine_diff_density_min -0.453 _refine_diff_density_rms 0.090 # Attachment 'comp2.CIF' data_c:\alle\m-pyfe\pyfe_abs _database_code_depnum_ccdc_archive 'CCDC 764305' #TrackingRef 'comp2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H24 B2 F8 Fe N12' _chemical_formula_weight 806.10 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 41.196(8) _cell_length_b 9.874(2) _cell_length_c 16.528(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.03(3) _cell_angle_gamma 90.00 _cell_volume 6523(2) _cell_formula_units_Z 8 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod _exptl_crystal_colour red _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.642 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3264 _exptl_absorpt_coefficient_mu 0.556 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8737 _exptl_absorpt_correction_T_max 0.9573 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15085 _diffrn_reflns_av_R_equivalents 0.0424 _diffrn_reflns_av_sigmaI/netI 0.0345 _diffrn_reflns_limit_h_min -48 _diffrn_reflns_limit_h_max 48 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5688 _reflns_number_gt 4666 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.1338P)^2^+4.3758P] 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 SHELXL _refine_ls_extinction_coef 0.0062(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5688 _refine_ls_number_parameters 508 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0744 _refine_ls_R_factor_gt 0.0639 _refine_ls_wR_factor_ref 0.1857 _refine_ls_wR_factor_gt 0.1774 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.382115(10) 0.63487(5) 0.51055(3) 0.0385(2) Uani 1 1 d . . . N1 N 0.39062(6) 0.5010(3) 0.60175(18) 0.0425(6) Uani 1 1 d . . . N2 N 0.36142(6) 0.4443(3) 0.61437(18) 0.0436(7) Uani 1 1 d . . . N3 N 0.33763(6) 0.5796(3) 0.50546(18) 0.0405(6) Uani 1 1 d . . . N4 N 0.32365(6) 0.7247(3) 0.39828(18) 0.0426(6) Uani 1 1 d . . . N5 N 0.35778(6) 0.7478(3) 0.41686(18) 0.0419(6) Uani 1 1 d . . . N6 N 0.18429(7) 0.3986(4) 0.4055(2) 0.0509(7) Uani 1 1 d . . . N7 N 0.38628(6) 0.7831(3) 0.59187(18) 0.0413(6) Uani 1 1 d . . . N8 N 0.41799(6) 0.8395(3) 0.61185(18) 0.0403(6) Uani 1 1 d . . . N9 N 0.42673(6) 0.6891(3) 0.51704(17) 0.0384(6) Uani 1 1 d . . . N10 N 0.42588(6) 0.5267(3) 0.42120(18) 0.0429(6) Uani 1 1 d . . . N11 N 0.39373(7) 0.5080(3) 0.43020(19) 0.0433(6) Uani 1 1 d . . . N12 N 0.57285(7) 0.9635(3) 0.5901(2) 0.0517(8) Uani 1 1 d . . . C1 C 0.41491(8) 0.4407(4) 0.6585(2) 0.0440(8) Uani 1 1 d . . . H1A H 0.4381 0.4588 0.6655 0.053 Uiso 1 1 calc R . . C2 C 0.40199(9) 0.3472(4) 0.7064(2) 0.0476(8) Uani 1 1 d . . . H2A H 0.4143 0.2918 0.7502 0.057 Uiso 1 1 calc R . . C3 C 0.36789(9) 0.3524(4) 0.6768(2) 0.0482(8) Uani 1 1 d . . . H3A H 0.3519 0.3010 0.6965 0.058 Uiso 1 1 calc R . . C4 C 0.33137(8) 0.4885(4) 0.5597(2) 0.0424(7) Uani 1 1 d . . . C5 C 0.29970(8) 0.4443(4) 0.5589(2) 0.0444(8) Uani 1 1 d . . . H5A H 0.2959 0.3794 0.5981 0.053 Uiso 1 1 calc R . . C6 C 0.27317(8) 0.4986(4) 0.4982(2) 0.0438(8) Uani 1 1 d . . . C7 C 0.27937(8) 0.5951(4) 0.4417(2) 0.0458(8) Uani 1 1 d . . . H7A H 0.2616 0.6339 0.4006 0.055 Uiso 1 1 calc R . . C8 C 0.31211(8) 0.6315(3) 0.4478(2) 0.0431(8) Uani 1 1 d . . . C9 C 0.30742(8) 0.7992(4) 0.3305(2) 0.0476(8) Uani 1 1 d . . . H9A H 0.2841 0.7996 0.3055 0.057 Uiso 1 1 calc R . . C10 C 0.33162(9) 0.8732(4) 0.3059(2) 0.0492(8) Uani 1 1 d . . . H10A H 0.3284 0.9356 0.2608 0.059 Uiso 1 1 calc R . . C11 C 0.36222(8) 0.8380(4) 0.3609(2) 0.0430(8) Uani 1 1 d . . . H11A H 0.3833 0.8741 0.3584 0.052 Uiso 1 1 calc R . . C12 C 0.23848(8) 0.4537(4) 0.4935(2) 0.0447(8) Uani 1 1 d . . . C13 C 0.21588(8) 0.4380(4) 0.4160(2) 0.0486(8) Uani 1 1 d . . . H13A H 0.2236 0.4568 0.3675 0.058 Uiso 1 1 calc R . . C14 C 0.17408(9) 0.3733(4) 0.4747(3) 0.0540(9) Uani 1 1 d . . . H14A H 0.1515 0.3457 0.4688 0.065 Uiso 1 1 calc R . . C15 C 0.19425(9) 0.3847(4) 0.5542(3) 0.0539(9) Uani 1 1 d . . . H15A H 0.1858 0.3645 0.6014 0.065 Uiso 1 1 calc R . . C16 C 0.22686(9) 0.4257(4) 0.5640(2) 0.0517(9) Uani 1 1 d . . . H16A H 0.2412 0.4348 0.6181 0.062 Uiso 1 1 calc R . . C17 C 0.36993(9) 0.8485(4) 0.6398(2) 0.0467(8) Uani 1 1 d . . . H17A H 0.3471 0.8329 0.6394 0.056 Uiso 1 1 calc R . . C18 C 0.39036(9) 0.9432(4) 0.6908(2) 0.0498(8) Uani 1 1 d . . . H18A H 0.3844 1.0011 0.7308 0.060 Uiso 1 1 calc R . . C19 C 0.42089(9) 0.9356(4) 0.6714(2) 0.0458(8) Uani 1 1 d . . . H19A H 0.4403 0.9876 0.6952 0.055 Uiso 1 1 calc R . . C20 C 0.44070(8) 0.7899(3) 0.5681(2) 0.0391(7) Uani 1 1 d . . . C21 C 0.47276(8) 0.8350(4) 0.5741(2) 0.0415(7) Uani 1 1 d . . . H21A H 0.4820 0.9063 0.6112 0.050 Uiso 1 1 calc R . . C22 C 0.49148(8) 0.7730(3) 0.5240(2) 0.0401(7) Uani 1 1 d . . . C23 C 0.47698(8) 0.6673(4) 0.4708(2) 0.0420(7) Uani 1 1 d . . . H23A H 0.4891 0.6233 0.4361 0.050 Uiso 1 1 calc R . . C24 C 0.44480(8) 0.6289(3) 0.4701(2) 0.0406(7) Uani 1 1 d . . . C25 C 0.43251(9) 0.4412(4) 0.3629(2) 0.0477(8) Uani 1 1 d . . . H25A H 0.4529 0.4351 0.3461 0.057 Uiso 1 1 calc R . . C26 C 0.40464(10) 0.3663(4) 0.3331(2) 0.0525(9) Uani 1 1 d . . . H26A H 0.4017 0.2976 0.2918 0.063 Uiso 1 1 calc R . . C27 C 0.38088(9) 0.4105(4) 0.3756(2) 0.0479(8) Uani 1 1 d . . . H27A H 0.3588 0.3759 0.3668 0.057 Uiso 1 1 calc R . . C28 C 0.52599(8) 0.8198(4) 0.5272(2) 0.0432(8) Uani 1 1 d . . . C29 C 0.54197(8) 0.9158(4) 0.5853(2) 0.0478(8) Uani 1 1 d . . . H29A H 0.5302 0.9495 0.6240 0.057 Uiso 1 1 calc R . . C30 C 0.58889(9) 0.9142(4) 0.5361(3) 0.0517(9) Uani 1 1 d . . . H30A H 0.6109 0.9465 0.5388 0.062 Uiso 1 1 calc R . . C31 C 0.57563(9) 0.8191(5) 0.4765(3) 0.0577(10) Uani 1 1 d . . . H31A H 0.5882 0.7869 0.4392 0.069 Uiso 1 1 calc R . . C32 C 0.54361(9) 0.7714(4) 0.4719(3) 0.0535(9) Uani 1 1 d . . . H32A H 0.5338 0.7060 0.4311 0.064 Uiso 1 1 calc R . . B1 B 0.29566(14) 0.7022(8) 0.7291(4) 0.0801(17) Uani 1 1 d . . . B2 B 0.5000 0.6270(6) 0.7500 0.0470(13) Uani 1 2 d S . . B3 B 0.5000 0.8281(6) 0.2500 0.0422(12) Uani 1 2 d S . . F1A F 0.3242(2) 0.787(2) 0.7675(6) 0.041(2) Uiso 0.34 1 d P A 1 F2A F 0.3024(3) 0.5551(11) 0.7464(7) 0.068(2) Uiso 0.34 1 d P A 1 F3A F 0.2950(3) 0.7434(12) 0.6386(7) 0.066(4) Uiso 0.34 1 d P A 1 F4A F 0.2699(2) 0.8079(13) 0.7447(6) 0.081(3) Uiso 0.34 1 d P A 1 F1B F 0.2892(3) 0.7210(12) 0.6455(7) 0.059(3) Uiso 0.33 1 d P A 2 F2B F 0.2685(2) 0.7435(12) 0.7521(6) 0.064(2) Uiso 0.33 1 d P A 2 F3B F 0.3221(3) 0.7499(19) 0.7710(7) 0.062(5) Uiso 0.33 1 d P A 2 F4B F 0.2923(5) 0.597(3) 0.7572(13) 0.156(8) Uiso 0.33 1 d P A 2 F1C F 0.3119(4) 0.5658(17) 0.7328(10) 0.112(6) Uiso 0.33 1 d P A 3 F2C F 0.2693(3) 0.6854(14) 0.7804(8) 0.096(3) Uiso 0.33 1 d P A 3 F3C F 0.2750(3) 0.6869(12) 0.6582(7) 0.093(3) Uiso 0.33 1 d P A 3 F4C F 0.3213(8) 0.787(5) 0.767(2) 0.161(14) Uiso 0.33 1 d P A 3 F5A F 0.47250(6) 0.7071(3) 0.75110(16) 0.0646(7) Uani 1 1 d . . . F6A F 0.49270(5) 0.5463(3) 0.67843(14) 0.0593(6) Uani 1 1 d . . . F7A F 0.5021(2) 0.9578(10) 0.2847(5) 0.128(3) Uiso 0.50 1 d P . 1 F8A F 0.52886(13) 0.7602(6) 0.2713(4) 0.0669(14) Uiso 0.50 1 d P . 1 F7B F 0.5049(2) 0.8894(9) 0.3273(6) 0.110(2) Uiso 0.50 1 d P . 2 F8B F 0.5246(2) 0.7530(11) 0.2301(7) 0.131(3) Uiso 0.50 1 d P . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0315(3) 0.0423(3) 0.0407(3) -0.00007(19) 0.0066(2) -0.00162(17) N1 0.0314(13) 0.0478(16) 0.0466(16) -0.0034(13) 0.0062(11) -0.0025(11) N2 0.0350(13) 0.0467(16) 0.0462(16) 0.0036(13) 0.0041(11) -0.0049(11) N3 0.0345(13) 0.0430(15) 0.0423(15) 0.0030(12) 0.0058(11) -0.0004(11) N4 0.0349(13) 0.0486(16) 0.0424(15) 0.0057(13) 0.0057(11) -0.0027(11) N5 0.0351(13) 0.0456(16) 0.0448(15) -0.0014(13) 0.0092(11) -0.0063(11) N6 0.0365(14) 0.064(2) 0.0509(18) -0.0005(15) 0.0089(12) -0.0063(13) N7 0.0305(12) 0.0479(16) 0.0452(15) 0.0056(13) 0.0085(11) 0.0003(11) N8 0.0334(13) 0.0464(16) 0.0402(15) -0.0007(12) 0.0069(11) -0.0022(11) N9 0.0363(13) 0.0415(15) 0.0366(14) -0.0018(12) 0.0075(11) -0.0008(11) N10 0.0366(13) 0.0479(16) 0.0437(15) -0.0052(13) 0.0086(11) -0.0032(12) N11 0.0366(13) 0.0438(16) 0.0470(15) 0.0002(13) 0.0053(11) -0.0036(11) N12 0.0388(15) 0.0592(19) 0.0572(18) -0.0043(15) 0.0120(13) -0.0089(13) C1 0.0372(15) 0.0473(19) 0.0435(18) -0.0045(15) 0.0018(13) 0.0010(13) C2 0.0428(18) 0.049(2) 0.0452(19) 0.0039(16) 0.0000(14) 0.0005(14) C3 0.0459(19) 0.050(2) 0.047(2) 0.0076(16) 0.0088(15) -0.0040(15) C4 0.0341(15) 0.0494(19) 0.0416(17) -0.0002(15) 0.0053(13) 0.0006(13) C5 0.0381(16) 0.0481(19) 0.0453(18) 0.0021(15) 0.0067(13) -0.0061(14) C6 0.0364(16) 0.0474(19) 0.0467(19) -0.0007(15) 0.0084(14) -0.0009(13) C7 0.0329(15) 0.054(2) 0.0472(19) 0.0060(16) 0.0034(13) -0.0024(14) C8 0.0382(17) 0.0443(19) 0.0459(19) 0.0021(15) 0.0085(14) -0.0007(13) C9 0.0380(16) 0.054(2) 0.048(2) 0.0055(16) 0.0054(14) 0.0017(14) C10 0.0453(18) 0.055(2) 0.046(2) 0.0086(16) 0.0089(15) -0.0025(15) C11 0.0398(16) 0.0470(19) 0.0427(18) -0.0023(15) 0.0109(14) -0.0045(13) C12 0.0366(16) 0.049(2) 0.0483(19) 0.0010(16) 0.0093(14) -0.0031(14) C13 0.0401(17) 0.058(2) 0.0461(19) 0.0006(17) 0.0076(14) -0.0052(15) C14 0.0380(18) 0.061(2) 0.064(2) -0.0049(19) 0.0130(16) -0.0043(15) C15 0.0419(18) 0.068(3) 0.055(2) 0.0001(19) 0.0173(16) -0.0057(16) C16 0.0435(18) 0.064(2) 0.047(2) 0.0012(18) 0.0092(15) -0.0060(16) C17 0.0420(17) 0.052(2) 0.048(2) 0.0031(16) 0.0153(15) 0.0049(14) C18 0.0498(19) 0.051(2) 0.050(2) -0.0072(16) 0.0151(15) 0.0039(15) C19 0.0442(17) 0.0459(19) 0.0467(19) -0.0072(15) 0.0097(14) -0.0004(14) C20 0.0367(15) 0.0418(17) 0.0387(17) -0.0007(14) 0.0092(13) 0.0014(13) C21 0.0351(16) 0.0442(18) 0.0441(18) -0.0005(14) 0.0075(13) -0.0027(13) C22 0.0343(15) 0.0430(17) 0.0416(17) 0.0035(14) 0.0066(13) -0.0016(13) C23 0.0361(16) 0.0477(18) 0.0436(18) 0.0006(15) 0.0122(13) 0.0005(13) C24 0.0387(16) 0.0402(18) 0.0412(18) -0.0017(14) 0.0066(13) -0.0005(13) C25 0.0478(18) 0.051(2) 0.0439(19) -0.0050(16) 0.0106(15) 0.0039(15) C26 0.061(2) 0.048(2) 0.046(2) -0.0102(16) 0.0088(17) -0.0029(16) C27 0.0470(18) 0.0451(19) 0.0469(19) -0.0058(16) 0.0022(15) -0.0029(15) C28 0.0346(16) 0.0478(19) 0.0469(19) 0.0057(15) 0.0093(13) -0.0001(13) C29 0.0374(17) 0.055(2) 0.051(2) -0.0030(17) 0.0107(14) -0.0023(15) C30 0.0385(17) 0.057(2) 0.061(2) 0.0005(19) 0.0155(16) -0.0050(15) C31 0.0459(19) 0.067(3) 0.066(3) -0.012(2) 0.0248(18) -0.0107(17) C32 0.0436(18) 0.061(2) 0.058(2) -0.0090(19) 0.0172(16) -0.0095(16) B1 0.059(3) 0.099(5) 0.074(4) -0.013(3) -0.001(3) 0.007(3) B2 0.038(3) 0.054(3) 0.049(3) 0.000 0.011(2) 0.000 B3 0.040(3) 0.037(3) 0.044(3) 0.000 -0.001(2) 0.000 F5A 0.0568(13) 0.0763(17) 0.0659(15) 0.0169(13) 0.0247(11) 0.0204(11) F6A 0.0531(12) 0.0693(15) 0.0551(13) -0.0062(11) 0.0121(9) -0.0118(10) _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. ; 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 N9 1.892(3) . ? Fe1 N3 1.894(3) . ? Fe1 N7 1.967(3) . ? Fe1 N11 1.967(3) . ? Fe1 N1 1.971(3) . ? Fe1 N5 1.973(3) . ? N1 C1 1.334(4) . ? N1 N2 1.388(4) . ? N2 C3 1.351(5) . ? N2 C4 1.413(4) . ? N3 C8 1.337(4) . ? N3 C4 1.339(5) . ? N4 C9 1.371(5) . ? N4 N5 1.383(4) . ? N4 C8 1.391(5) . ? N5 C11 1.328(5) . ? N6 C13 1.329(4) . ? N6 C14 1.334(5) . ? N7 C17 1.325(5) . ? N7 N8 1.384(4) . ? N8 C19 1.352(5) . ? N8 C20 1.402(4) . ? N9 C24 1.338(4) . ? N9 C20 1.341(4) . ? N10 C25 1.358(5) . ? N10 N11 1.381(4) . ? N10 C24 1.404(4) . ? N11 C27 1.338(5) . ? N12 C30 1.324(5) . ? N12 C29 1.341(4) . ? C1 C2 1.402(5) . ? C2 C3 1.372(5) . ? C4 C5 1.373(5) . ? C5 C6 1.398(5) . ? C6 C7 1.401(5) . ? C6 C12 1.480(5) . ? C7 C8 1.376(5) . ? C9 C10 1.375(5) . ? C10 C11 1.408(5) . ? C12 C16 1.391(5) . ? C12 C13 1.397(5) . ? C14 C15 1.379(6) . ? C15 C16 1.375(5) . ? C17 C18 1.397(5) . ? C18 C19 1.374(5) . ? C20 C21 1.375(5) . ? C21 C22 1.402(5) . ? C22 C23 1.402(5) . ? C22 C28 1.484(4) . ? C23 C24 1.376(5) . ? C25 C26 1.354(5) . ? C26 C27 1.405(6) . ? C28 C32 1.383(5) . ? C28 C29 1.396(5) . ? C30 C31 1.375(6) . ? C31 C32 1.385(5) . ? B1 F4B 1.16(2) . ? B1 F3B 1.234(17) . ? B1 F3C 1.280(12) . ? B1 F2B 1.331(10) . ? B1 F1B 1.355(13) . ? B1 F4C 1.38(4) . ? B1 F1A 1.454(16) . ? B1 F2A 1.493(14) . ? B1 F1C 1.497(17) . ? B1 F2C 1.541(14) . ? B1 F3A 1.544(14) . ? B1 F4A 1.554(12) . ? B2 F5A 1.385(4) 2_656 ? B2 F5A 1.385(4) . ? B2 F6A 1.398(4) . ? B2 F6A 1.398(4) 2_656 ? B3 F8A 1.336(6) 2_655 ? B3 F8A 1.336(6) . ? B3 F8B 1.358(11) 2_655 ? B3 F8B 1.358(11) . ? B3 F7B 1.384(9) . ? B3 F7B 1.384(9) 2_655 ? B3 F7A 1.397(10) . ? B3 F7A 1.397(10) 2_655 ? F2B F4B 1.74(3) . ? F7A F7A 1.117(17) 2_655 ? 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 N9 Fe1 N3 179.26(12) . . ? N9 Fe1 N7 80.10(11) . . ? N3 Fe1 N7 99.67(12) . . ? N9 Fe1 N11 80.02(12) . . ? N3 Fe1 N11 100.23(12) . . ? N7 Fe1 N11 160.09(11) . . ? N9 Fe1 N1 98.99(11) . . ? N3 Fe1 N1 80.31(11) . . ? N7 Fe1 N1 90.39(12) . . ? N11 Fe1 N1 93.55(12) . . ? N9 Fe1 N5 100.74(12) . . ? N3 Fe1 N5 79.96(12) . . ? N7 Fe1 N5 93.40(12) . . ? N11 Fe1 N5 89.45(12) . . ? N1 Fe1 N5 160.26(11) . . ? C1 N1 N2 104.1(3) . . ? C1 N1 Fe1 143.2(2) . . ? N2 N1 Fe1 112.7(2) . . ? C3 N2 N1 111.6(3) . . ? C3 N2 C4 132.5(3) . . ? N1 N2 C4 115.8(3) . . ? C8 N3 C4 119.2(3) . . ? C8 N3 Fe1 120.4(2) . . ? C4 N3 Fe1 120.3(2) . . ? C9 N4 N5 111.2(3) . . ? C9 N4 C8 131.9(3) . . ? N5 N4 C8 116.9(3) . . ? C11 N5 N4 105.1(3) . . ? C11 N5 Fe1 142.7(2) . . ? N4 N5 Fe1 112.1(2) . . ? C13 N6 C14 116.5(3) . . ? C17 N7 N8 104.4(3) . . ? C17 N7 Fe1 143.0(2) . . ? N8 N7 Fe1 112.5(2) . . ? C19 N8 N7 111.6(3) . . ? C19 N8 C20 132.0(3) . . ? N7 N8 C20 116.5(3) . . ? C24 N9 C20 118.7(3) . . ? C24 N9 Fe1 120.7(2) . . ? C20 N9 Fe1 120.6(2) . . ? C25 N10 N11 110.9(3) . . ? C25 N10 C24 132.5(3) . . ? N11 N10 C24 116.6(3) . . ? C27 N11 N10 104.9(3) . . ? C27 N11 Fe1 142.4(2) . . ? N10 N11 Fe1 112.6(2) . . ? C30 N12 C29 116.9(3) . . ? N1 C1 C2 111.6(3) . . ? C3 C2 C1 105.7(3) . . ? N2 C3 C2 107.0(3) . . ? N3 C4 C5 123.0(3) . . ? N3 C4 N2 110.8(3) . . ? C5 C4 N2 126.2(3) . . ? C4 C5 C6 117.5(3) . . ? C5 C6 C7 120.1(3) . . ? C5 C6 C12 120.0(3) . . ? C7 C6 C12 119.9(3) . . ? C8 C7 C6 117.5(3) . . ? N3 C8 C7 122.7(3) . . ? N3 C8 N4 110.5(3) . . ? C7 C8 N4 126.7(3) . . ? N4 C9 C10 106.4(3) . . ? C9 C10 C11 106.1(3) . . ? N5 C11 C10 111.3(3) . . ? C16 C12 C13 117.2(3) . . ? C16 C12 C6 122.6(3) . . ? C13 C12 C6 120.2(3) . . ? N6 C13 C12 124.5(3) . . ? N6 C14 C15 124.0(3) . . ? C16 C15 C14 118.8(4) . . ? C15 C16 C12 119.0(3) . . ? N7 C17 C18 111.6(3) . . ? C19 C18 C17 105.9(3) . . ? N8 C19 C18 106.5(3) . . ? N9 C20 C21 123.0(3) . . ? N9 C20 N8 110.2(3) . . ? C21 C20 N8 126.8(3) . . ? C20 C21 C22 118.2(3) . . ? C21 C22 C23 119.0(3) . . ? C21 C22 C28 120.2(3) . . ? C23 C22 C28 120.9(3) . . ? C24 C23 C22 118.3(3) . . ? N9 C24 C23 122.9(3) . . ? N9 C24 N10 110.1(3) . . ? C23 C24 N10 127.0(3) . . ? C26 C25 N10 107.4(3) . . ? C25 C26 C27 106.3(3) . . ? N11 C27 C26 110.5(3) . . ? C32 C28 C29 117.0(3) . . ? C32 C28 C22 121.4(3) . . ? C29 C28 C22 121.6(3) . . ? N12 C29 C28 124.2(3) . . ? N12 C30 C31 123.9(3) . . ? C30 C31 C32 118.6(4) . . ? C28 C32 C31 119.5(4) . . ? F4B B1 F3B 107.0(14) . . ? F4B B1 F3C 98.3(13) . . ? F3B B1 F3C 149.3(12) . . ? F4B B1 F2B 88.3(13) . . ? F3B B1 F2B 114.4(8) . . ? F3C B1 F2B 82.9(7) . . ? F4B B1 F1B 121.2(13) . . ? F3B B1 F1B 116.7(11) . . ? F3C B1 F1B 32.8(6) . . ? F2B B1 F1B 106.1(8) . . ? F4B B1 F4C 121(2) . . ? F3B B1 F4C 15(2) . . ? F3C B1 F4C 139.4(19) . . ? F2B B1 F4C 106.6(14) . . ? F1B B1 F4C 109.0(18) . . ? F4B B1 F1A 120.0(13) . . ? F3B B1 F1A 13.2(6) . . ? F3C B1 F1A 139.1(11) . . ? F2B B1 F1A 110.2(8) . . ? F1B B1 F1A 107.8(10) . . ? F4C B1 F1A 3.6(16) . . ? F4B B1 F2A 24.0(11) . . ? F3B B1 F2A 99.6(10) . . ? F3C B1 F2A 96.5(8) . . ? F2B B1 F2A 111.9(10) . . ? F1B B1 F2A 108.1(8) . . ? F4C B1 F2A 114.8(17) . . ? F1A B1 F2A 112.4(9) . . ? F4B B1 F1C 43.4(11) . . ? F3B B1 F1C 89.8(10) . . ? F3C B1 F1C 97.1(9) . . ? F2B B1 F1C 131.4(11) . . ? F1B B1 F1C 98.1(9) . . ? F4C B1 F1C 104.2(17) . . ? F1A B1 F1C 101.1(10) . . ? F2A B1 F1C 19.5(7) . . ? F4B B1 F2C 61.0(12) . . ? F3B B1 F2C 112.2(8) . . ? F3C B1 F2C 95.1(8) . . ? F2B B1 F2C 28.5(5) . . ? F1B B1 F2C 125.7(8) . . ? F4C B1 F2C 112.1(15) . . ? F1A B1 F2C 115.1(7) . . ? F2A B1 F2C 85.0(9) . . ? F1C B1 F2C 104.3(10) . . ? F4B B1 F3A 130.4(13) . . ? F3B B1 F3A 104.4(10) . . ? F3C B1 F3A 44.9(8) . . ? F2B B1 F3A 112.1(7) . . ? F1B B1 F3A 12.3(7) . . ? F4C B1 F3A 96.7(17) . . ? F1A B1 F3A 95.5(8) . . ? F2A B1 F3A 113.6(8) . . ? F1C B1 F3A 100.4(9) . . ? F2C B1 F3A 135.3(7) . . ? F4B B1 F4A 112.5(14) . . ? F3B B1 F4A 101.3(9) . . ? F3C B1 F4A 84.3(7) . . ? F2B B1 F4A 24.6(5) . . ? F1B B1 F4A 95.9(7) . . ? F4C B1 F4A 89.6(15) . . ? F1A B1 F4A 93.1(8) . . ? F2A B1 F4A 136.4(10) . . ? F1C B1 F4A 155.9(10) . . ? F2C B1 F4A 51.7(7) . . ? F3A B1 F4A 97.5(7) . . ? F5A B2 F5A 110.4(5) 2_656 . ? F5A B2 F6A 108.86(14) 2_656 . ? F5A B2 F6A 109.14(15) . . ? F5A B2 F6A 109.14(15) 2_656 2_656 ? F5A B2 F6A 108.86(14) . 2_656 ? F6A B2 F6A 110.4(5) . 2_656 ? F8A B3 F8A 119.7(6) 2_655 . ? F8A B3 F8B 28.6(4) 2_655 2_655 ? F8A B3 F8B 109.3(6) . 2_655 ? F8A B3 F8B 109.3(6) 2_655 . ? F8A B3 F8B 28.6(4) . . ? F8B B3 F8B 113.9(10) 2_655 . ? F8A B3 F7B 112.6(4) 2_655 . ? F8A B3 F7B 93.2(4) . . ? F8B B3 F7B 88.0(6) 2_655 . ? F8B B3 F7B 120.8(6) . . ? F8A B3 F7B 93.2(4) 2_655 2_655 ? F8A B3 F7B 112.6(4) . 2_655 ? F8B B3 F7B 120.8(6) 2_655 2_655 ? F8B B3 F7B 88.0(6) . 2_655 ? F7B B3 F7B 128.1(9) . 2_655 ? F8A B3 F7A 122.0(5) 2_655 . ? F8A B3 F7A 112.9(5) . . ? F8B B3 F7A 112.1(6) 2_655 . ? F8B B3 F7A 128.6(6) . . ? F7B B3 F7A 40.5(4) . . ? F7B B3 F7A 87.6(7) 2_655 . ? F8A B3 F7A 112.9(5) 2_655 2_655 ? F8A B3 F7A 122.0(5) . 2_655 ? F8B B3 F7A 128.6(6) 2_655 2_655 ? F8B B3 F7A 112.1(6) . 2_655 ? F7B B3 F7A 87.6(7) . 2_655 ? F7B B3 F7A 40.5(4) 2_655 2_655 ? F7A B3 F7A 47.1(8) . 2_655 ? B1 F2B F4B 41.8(7) . . ? B1 F4B F2B 49.9(11) . . ? F7A F7A B3 66.4(4) 2_655 . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.838 _refine_diff_density_min -0.649 _refine_diff_density_rms 0.091 # Attachment 'comp3.CIF' data_c:\alle\iso34\abscorr\iso34a _database_code_depnum_ccdc_archive 'CCDC 764306' #TrackingRef 'comp3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H30 B3 F12 Fe N13 O' _chemical_formula_weight 952.99 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.177(3) _cell_length_b 17.0990(19) _cell_length_c 16.797(3) _cell_angle_alpha 90.00 _cell_angle_beta 111.742(14) _cell_angle_gamma 90.00 _cell_volume 4048.9(11) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 5632 _cell_measurement_theta_min 1.29 _cell_measurement_theta_max 26.12 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.563 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1928 _exptl_absorpt_coefficient_mu 0.477 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.7436 _exptl_absorpt_correction_T_max 0.9181 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -1 1 0 0.0920 1 -1 0 0.0870 -1 0 2 0.3230 1 0 -1 0.2300 1 1 0 0.0830 -1 -1 0 0.1400 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm, multiple pinhole' _diffrn_source_voltage 50 _diffrn_source_current 40 _diffrn_source_power 2.00 _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 180 frames, detector distance = 130 mm ; _diffrn_detector 'image plate ( 34 cm diameter )' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27402 _diffrn_reflns_av_R_equivalents 0.0348 _diffrn_reflns_av_sigmaI/netI 0.0256 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 25.63 _reflns_number_total 7596 _reflns_number_gt 6538 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.1233P)^2^+6.2026P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0024(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7596 _refine_ls_number_parameters 578 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0820 _refine_ls_R_factor_gt 0.0739 _refine_ls_wR_factor_ref 0.2111 _refine_ls_wR_factor_gt 0.2034 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.035 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.71992(3) 0.26851(3) 0.51817(3) 0.0359(2) Uani 1 1 d . . . N1 N 0.5992(2) 0.30685(18) 0.4323(2) 0.0404(7) Uani 1 1 d . . . N2 N 0.6021(2) 0.3852(2) 0.4154(2) 0.0477(8) Uani 1 1 d . . . N3 N 0.7484(2) 0.37601(18) 0.51710(19) 0.0393(7) Uani 1 1 d . . . N4 N 0.8908(2) 0.34236(19) 0.61497(19) 0.0401(7) Uani 1 1 d . . . N5 N 0.8493(2) 0.26960(18) 0.6065(2) 0.0394(7) Uani 1 1 d . . . N6 N 0.8262(3) 0.7101(2) 0.3895(2) 0.0492(8) Uani 1 1 d D . . H6N H 0.801(3) 0.733(3) 0.334(2) 0.059 Uiso 1 1 d D . . N7 N 0.6607(2) 0.25602(17) 0.60446(19) 0.0372(6) Uani 1 1 d . . . N8 N 0.6432(2) 0.17870(17) 0.61728(18) 0.0355(6) Uani 1 1 d . . . N9 N 0.7003(2) 0.15895(18) 0.51305(18) 0.0363(6) Uani 1 1 d . . . N10 N 0.7641(2) 0.1634(2) 0.41178(19) 0.0419(7) Uani 1 1 d . . . N11 N 0.7703(2) 0.24182(19) 0.4299(2) 0.0414(7) Uani 1 1 d . . . N12 N 0.6872(3) -0.2075(2) 0.5827(3) 0.0602(10) Uani 1 1 d . . . C1 C 0.5114(3) 0.2837(2) 0.3843(3) 0.0450(9) Uani 1 1 d . . . H1A H 0.4881 0.2319 0.3826 0.054 Uiso 1 1 calc R . . C2 C 0.4587(3) 0.3467(3) 0.3369(3) 0.0585(12) Uani 1 1 d . . . H2A H 0.3945 0.3455 0.2982 0.070 Uiso 1 1 calc R . . C3 C 0.5171(3) 0.4100(3) 0.3570(3) 0.0611(13) Uani 1 1 d . . . H3A H 0.5018 0.4614 0.3348 0.073 Uiso 1 1 calc R . . C4 C 0.6878(3) 0.4244(2) 0.4602(2) 0.0427(8) Uani 1 1 d . . . C5 C 0.7099(3) 0.4998(2) 0.4472(3) 0.0449(9) Uani 1 1 d . . . H5A H 0.6651 0.5329 0.4068 0.054 Uiso 1 1 calc R . . C6 C 0.8016(3) 0.5258(2) 0.4959(2) 0.0405(8) Uani 1 1 d . . . C7 C 0.8667(3) 0.4759(2) 0.5550(2) 0.0406(8) Uani 1 1 d . . . H7A H 0.9294 0.4927 0.5880 0.049 Uiso 1 1 calc R . . C8 C 0.8363(2) 0.4021(2) 0.5632(2) 0.0382(8) Uani 1 1 d . . . C9 C 0.9803(3) 0.3404(3) 0.6750(2) 0.0451(9) Uani 1 1 d . . . H9A H 1.0231 0.3832 0.6927 0.054 Uiso 1 1 calc R . . C10 C 0.9973(3) 0.2663(3) 0.7048(3) 0.0476(9) Uani 1 1 d . . . H10A H 1.0540 0.2469 0.7472 0.057 Uiso 1 1 calc R . . C11 C 0.9143(3) 0.2236(2) 0.6605(2) 0.0425(8) Uani 1 1 d . . . H11A H 0.9061 0.1695 0.6682 0.051 Uiso 1 1 calc R . . C12 C 0.8321(3) 0.6057(2) 0.4829(3) 0.0413(8) Uani 1 1 d . . . C13 C 0.7981(3) 0.6381(2) 0.4023(3) 0.0428(8) Uani 1 1 d . . . H13A H 0.7549 0.6096 0.3555 0.051 Uiso 1 1 calc R . . C14 C 0.8874(3) 0.7524(3) 0.4532(4) 0.0582(11) Uani 1 1 d . . . H14A H 0.9066 0.8027 0.4419 0.070 Uiso 1 1 calc R . . C15 C 0.9223(3) 0.7227(3) 0.5345(3) 0.0613(12) Uani 1 1 d . . . H15A H 0.9649 0.7527 0.5802 0.074 Uiso 1 1 calc R . . C16 C 0.8952(3) 0.6491(3) 0.5500(3) 0.0516(10) Uani 1 1 d . . . H16A H 0.9196 0.6280 0.6064 0.062 Uiso 1 1 calc R . . C17 C 0.6317(3) 0.2958(2) 0.6580(2) 0.0417(8) Uani 1 1 d . . . H17A H 0.6345 0.3511 0.6637 0.050 Uiso 1 1 calc R . . C18 C 0.5965(3) 0.2457(2) 0.7049(3) 0.0448(9) Uani 1 1 d . . . H18A H 0.5715 0.2603 0.7469 0.054 Uiso 1 1 calc R . . C19 C 0.6054(3) 0.1720(2) 0.6784(2) 0.0403(8) Uani 1 1 d . . . H19A H 0.5883 0.1248 0.6988 0.048 Uiso 1 1 calc R . . C20 C 0.6646(2) 0.1234(2) 0.5651(2) 0.0354(7) Uani 1 1 d . . . C21 C 0.6522(3) 0.0436(2) 0.5654(2) 0.0393(8) Uani 1 1 d . . . H21A H 0.6270 0.0195 0.6034 0.047 Uiso 1 1 calc R . . C22 C 0.6784(3) -0.0006(2) 0.5076(2) 0.0396(8) Uani 1 1 d . . . C23 C 0.7163(3) 0.0366(2) 0.4532(2) 0.0402(8) Uani 1 1 d . . . H23A H 0.7349 0.0075 0.4138 0.048 Uiso 1 1 calc R . . C24 C 0.7257(2) 0.1157(2) 0.4586(2) 0.0378(8) Uani 1 1 d . . . C25 C 0.8027(3) 0.1459(3) 0.3524(2) 0.0492(9) Uani 1 1 d . . . H25A H 0.8074 0.0956 0.3303 0.059 Uiso 1 1 calc R . . C26 C 0.8330(3) 0.2151(3) 0.3311(3) 0.0547(11) Uani 1 1 d . . . H26A H 0.8627 0.2225 0.2909 0.066 Uiso 1 1 calc R . . C27 C 0.8119(3) 0.2731(3) 0.3802(3) 0.0481(9) Uani 1 1 d . . . H27A H 0.8254 0.3272 0.3783 0.058 Uiso 1 1 calc R . . C28 C 0.6694(3) -0.0870(2) 0.5051(3) 0.0439(9) Uani 1 1 d . . . C29 C 0.6908(3) -0.1292(2) 0.5805(3) 0.0509(10) Uani 1 1 d . . . H29A H 0.7088 -0.1013 0.6330 0.061 Uiso 1 1 calc R . . C30 C 0.6597(4) -0.2461(3) 0.5080(4) 0.0629(13) Uani 1 1 d . . . H30A H 0.6557 -0.3015 0.5090 0.075 Uiso 1 1 calc R . . C31 C 0.6370(3) -0.2097(3) 0.4309(4) 0.0634(13) Uani 1 1 d . . . H31A H 0.6176 -0.2394 0.3794 0.076 Uiso 1 1 calc R . . C32 C 0.6427(3) -0.1284(3) 0.4284(3) 0.0538(10) Uani 1 1 d . . . H32A H 0.6288 -0.1018 0.3754 0.065 Uiso 1 1 calc R . . B1 B 0.7694(5) 0.5219(3) 0.7097(4) 0.0669(15) Uani 1 1 d . . . F1 F 0.6902(3) 0.4877(3) 0.6507(3) 0.1239(15) Uani 1 1 d . A . F2A F 0.8268(5) 0.4600(4) 0.7198(5) 0.0674(19) Uiso 0.50 1 d P A 1 F3A F 0.7388(5) 0.5403(4) 0.7729(4) 0.0600(15) Uiso 0.50 1 d P A 1 F4A F 0.8134(5) 0.5880(4) 0.6860(4) 0.0675(16) Uiso 0.50 1 d P A 1 F2B F 0.8557(5) 0.4743(4) 0.7390(4) 0.0624(17) Uiso 0.50 1 d P A 2 F3B F 0.7738(6) 0.5493(4) 0.7940(5) 0.076(2) Uiso 0.50 1 d P A 2 F4B F 0.7719(4) 0.5851(3) 0.6613(4) 0.0569(13) Uiso 0.50 1 d P A 2 B2 B 0.8636(4) 0.4645(3) 0.2889(3) 0.0561(12) Uani 1 1 d D . . F5 F 0.8432(2) 0.53998(17) 0.2592(2) 0.0758(8) Uani 1 1 d . B . F6A F 0.8993(4) 0.4576(4) 0.3764(4) 0.0752(15) Uiso 0.70 1 d P B 1 F7A F 0.9497(4) 0.4427(3) 0.2725(3) 0.0814(12) Uiso 0.70 1 d P B 1 F8A F 0.8013(4) 0.4089(3) 0.2492(3) 0.0853(13) Uiso 0.70 1 d P B 1 F6B F 0.9125(14) 0.4838(12) 0.3692(12) 0.118(7) Uiso 0.30 1 d PD B 2 F7B F 0.8640(11) 0.4215(9) 0.2284(9) 0.106(4) Uiso 0.30 1 d P B 2 F8B F 0.7646(6) 0.4458(5) 0.2888(6) 0.059(2) Uiso 0.30 1 d PD B 2 B3 B 0.4627(4) 0.0847(3) 0.2803(4) 0.0642(15) Uani 1 1 d D . . F9A F 0.4099(5) 0.0164(3) 0.2658(4) 0.0645(14) Uiso 0.50 1 d P C 1 F10A F 0.4910(4) 0.0968(3) 0.3740(3) 0.0582(12) Uiso 0.50 1 d P C 1 F11A F 0.5441(5) 0.0793(4) 0.2663(5) 0.0848(18) Uiso 0.50 1 d P C 1 F12A F 0.4033(6) 0.1422(5) 0.2384(6) 0.094(2) Uiso 0.50 1 d P C 1 F9B F 0.4626(6) 0.0061(5) 0.2961(5) 0.089(2) Uiso 0.50 1 d PD C 2 F10B F 0.5441(5) 0.1215(4) 0.3256(5) 0.0905(19) Uiso 0.50 1 d P C 2 F11B F 0.4668(5) 0.0928(4) 0.1912(4) 0.0826(17) Uiso 0.50 1 d PD C 2 F12B F 0.3847(6) 0.1360(5) 0.2672(5) 0.087(2) Uiso 0.50 1 d P C 2 N13 N 0.9782(4) 0.0926(3) 0.5493(4) 0.0818(14) Uani 1 1 d . . . C33 C 0.9675(4) 0.0352(3) 0.5774(3) 0.0627(12) Uani 1 1 d . . . C34 C 0.9509(4) -0.0395(3) 0.6107(4) 0.0724(14) Uani 1 1 d . . . H34A H 0.8868 -0.0402 0.6117 0.109 Uiso 1 1 calc R . . H34B H 0.9974 -0.0468 0.6690 0.109 Uiso 1 1 calc R . . H34C H 0.9573 -0.0818 0.5738 0.109 Uiso 1 1 calc R . . O1 O 0.7664(3) 0.77501(19) 0.2397(2) 0.0663(9) Uani 1 1 d D . . H1O H 0.742(4) 0.750(3) 0.187(2) 0.080 Uiso 1 1 d D . . H2O H 0.778(4) 0.8292(18) 0.237(4) 0.080 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0351(3) 0.0333(3) 0.0373(3) 0.00119(19) 0.0111(2) -0.0024(2) N1 0.0397(16) 0.0361(16) 0.0433(16) 0.0011(13) 0.0131(13) -0.0078(13) N2 0.0353(16) 0.0398(17) 0.0554(19) 0.0113(15) 0.0019(14) -0.0083(13) N3 0.0346(15) 0.0376(16) 0.0412(16) 0.0011(12) 0.0087(12) -0.0027(12) N4 0.0340(15) 0.0397(17) 0.0414(16) -0.0005(13) 0.0078(12) 0.0000(13) N5 0.0412(16) 0.0361(16) 0.0415(16) 0.0006(12) 0.0159(13) 0.0020(13) N6 0.0496(19) 0.0375(18) 0.066(2) 0.0042(16) 0.0276(17) -0.0011(15) N7 0.0391(16) 0.0297(15) 0.0401(16) -0.0009(12) 0.0116(13) 0.0004(12) N8 0.0371(15) 0.0320(15) 0.0385(15) -0.0007(12) 0.0152(12) -0.0001(12) N9 0.0361(15) 0.0369(16) 0.0358(15) -0.0015(12) 0.0130(12) 0.0000(12) N10 0.0410(16) 0.0479(19) 0.0386(16) 0.0003(13) 0.0169(13) -0.0012(14) N11 0.0393(16) 0.0438(18) 0.0386(16) 0.0033(13) 0.0117(13) -0.0044(13) N12 0.066(2) 0.0364(19) 0.089(3) -0.0024(18) 0.042(2) -0.0041(17) C1 0.0386(19) 0.047(2) 0.046(2) -0.0014(16) 0.0125(16) -0.0118(16) C2 0.039(2) 0.062(3) 0.059(3) 0.013(2) 0.0004(18) -0.0124(19) C3 0.036(2) 0.054(3) 0.073(3) 0.022(2) -0.0037(19) -0.0075(18) C4 0.0339(18) 0.038(2) 0.046(2) 0.0051(16) 0.0038(15) -0.0044(15) C5 0.0362(19) 0.039(2) 0.052(2) 0.0064(16) 0.0064(16) -0.0040(15) C6 0.0383(18) 0.0363(19) 0.0453(19) -0.0021(15) 0.0135(15) -0.0047(15) C7 0.0334(17) 0.0379(19) 0.046(2) -0.0053(15) 0.0090(15) -0.0047(15) C8 0.0322(17) 0.0384(19) 0.0399(18) 0.0003(14) 0.0088(14) 0.0002(14) C9 0.0330(18) 0.054(2) 0.043(2) -0.0024(17) 0.0078(15) 0.0006(16) C10 0.040(2) 0.057(2) 0.043(2) 0.0042(17) 0.0126(16) 0.0116(18) C11 0.046(2) 0.044(2) 0.0389(19) 0.0037(15) 0.0175(16) 0.0108(16) C12 0.0375(18) 0.0335(19) 0.053(2) -0.0040(16) 0.0170(16) -0.0031(15) C13 0.0378(18) 0.0341(19) 0.058(2) -0.0003(16) 0.0188(17) -0.0031(15) C14 0.055(3) 0.036(2) 0.089(3) -0.006(2) 0.034(2) -0.0099(19) C15 0.054(3) 0.044(2) 0.078(3) -0.012(2) 0.015(2) -0.014(2) C16 0.043(2) 0.045(2) 0.059(2) -0.0059(18) 0.0093(18) -0.0076(17) C17 0.0383(18) 0.0390(19) 0.0432(19) -0.0056(15) 0.0097(15) 0.0049(15) C18 0.042(2) 0.051(2) 0.043(2) -0.0060(17) 0.0185(16) 0.0042(17) C19 0.0379(18) 0.043(2) 0.0426(19) 0.0001(15) 0.0181(15) 0.0000(15) C20 0.0339(17) 0.0354(18) 0.0365(17) -0.0007(14) 0.0124(14) 0.0009(14) C21 0.0400(18) 0.0346(19) 0.0451(19) -0.0013(15) 0.0178(16) -0.0017(15) C22 0.0355(18) 0.0375(19) 0.0433(19) -0.0055(15) 0.0117(15) -0.0014(14) C23 0.0383(18) 0.043(2) 0.0393(18) -0.0068(15) 0.0138(15) 0.0005(15) C24 0.0351(17) 0.044(2) 0.0349(17) -0.0016(14) 0.0133(14) -0.0005(15) C25 0.046(2) 0.066(3) 0.0389(19) -0.0028(18) 0.0189(17) 0.0005(19) C26 0.045(2) 0.079(3) 0.041(2) 0.008(2) 0.0163(18) -0.003(2) C27 0.041(2) 0.059(3) 0.043(2) 0.0092(17) 0.0139(16) -0.0050(18) C28 0.0360(18) 0.036(2) 0.059(2) -0.0086(17) 0.0171(17) -0.0027(15) C29 0.055(2) 0.037(2) 0.068(3) -0.0091(18) 0.030(2) -0.0054(18) C30 0.060(3) 0.038(2) 0.100(4) -0.020(2) 0.041(3) -0.008(2) C31 0.048(2) 0.051(3) 0.085(3) -0.030(3) 0.016(2) -0.006(2) C32 0.046(2) 0.048(2) 0.060(3) -0.0156(19) 0.0119(19) 0.0012(18) B1 0.101(5) 0.038(3) 0.074(4) 0.001(2) 0.047(3) 0.008(3) F1 0.118(3) 0.105(3) 0.140(4) -0.018(3) 0.037(3) -0.006(3) B2 0.070(3) 0.050(3) 0.046(2) -0.009(2) 0.018(2) -0.022(2) F5 0.0756(19) 0.0566(17) 0.097(2) 0.0057(15) 0.0341(17) -0.0007(14) B3 0.065(3) 0.042(3) 0.095(4) -0.020(3) 0.041(3) -0.017(2) N13 0.107(4) 0.059(3) 0.097(4) -0.016(2) 0.058(3) -0.014(3) C33 0.071(3) 0.058(3) 0.071(3) -0.014(2) 0.040(3) -0.006(2) C34 0.082(4) 0.070(3) 0.078(3) 0.005(3) 0.045(3) -0.001(3) O1 0.063(2) 0.0417(17) 0.080(2) 0.0158(15) 0.0092(18) -0.0021(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. ; 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 N3 1.890(3) . ? Fe1 N9 1.894(3) . ? Fe1 N11 1.957(3) . ? Fe1 N5 1.975(3) . ? Fe1 N1 1.977(3) . ? Fe1 N7 1.980(3) . ? N1 C1 1.337(5) . ? N1 N2 1.373(4) . ? N2 C3 1.368(5) . ? N2 C4 1.407(5) . ? N3 C4 1.339(5) . ? N3 C8 1.346(5) . ? N4 C9 1.359(5) . ? N4 N5 1.378(4) . ? N4 C8 1.396(5) . ? N5 C11 1.323(5) . ? N6 C14 1.339(6) . ? N6 C13 1.346(5) . ? N7 C17 1.325(5) . ? N7 N8 1.381(4) . ? N8 C19 1.354(5) . ? N8 C20 1.407(4) . ? N9 C20 1.333(5) . ? N9 C24 1.339(5) . ? N10 C25 1.363(5) . ? N10 N11 1.371(5) . ? N10 C24 1.401(5) . ? N11 C27 1.331(5) . ? N12 C29 1.340(5) . ? N12 C30 1.340(7) . ? C1 C2 1.402(6) . ? C2 C3 1.359(6) . ? C4 C5 1.370(5) . ? C5 C6 1.400(5) . ? C6 C7 1.401(5) . ? C6 C12 1.483(5) . ? C7 C8 1.369(5) . ? C9 C10 1.352(6) . ? C10 C11 1.406(6) . ? C12 C13 1.374(6) . ? C12 C16 1.394(5) . ? C14 C15 1.367(7) . ? C15 C16 1.379(6) . ? C17 C18 1.398(6) . ? C18 C19 1.361(6) . ? C20 C21 1.378(5) . ? C21 C22 1.398(5) . ? C22 C23 1.400(5) . ? C22 C28 1.483(5) . ? C23 C24 1.360(5) . ? C25 C26 1.365(7) . ? C26 C27 1.401(7) . ? C28 C29 1.387(6) . ? C28 C32 1.394(6) . ? C30 C31 1.362(8) . ? C31 C32 1.395(7) . ? B1 F2A 1.339(9) . ? B1 F3A 1.344(8) . ? B1 F4B 1.362(8) . ? B1 F1 1.374(8) . ? B1 F4A 1.442(9) . ? B1 F2B 1.463(9) . ? B1 F3B 1.469(9) . ? B2 F7B 1.257(15) . ? B2 F6B 1.317(19) . ? B2 F8A 1.333(7) . ? B2 F6A 1.369(8) . ? B2 F5 1.376(6) . ? B2 F7A 1.479(8) . ? B2 F8B 1.535(10) . ? B3 F10B 1.344(9) . ? B3 F12A 1.343(10) . ? B3 F11A 1.344(9) . ? B3 F9B 1.369(9) . ? B3 F9A 1.385(8) . ? B3 F12B 1.424(10) . ? B3 F10A 1.485(8) . ? B3 F11B 1.527(9) . ? N13 C33 1.126(7) . ? C33 C34 1.453(7) . ? 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 N3 Fe1 N9 173.92(13) . . ? N3 Fe1 N11 93.71(14) . . ? N9 Fe1 N11 80.45(13) . . ? N3 Fe1 N5 80.25(13) . . ? N9 Fe1 N5 98.02(13) . . ? N11 Fe1 N5 90.68(13) . . ? N3 Fe1 N1 79.85(13) . . ? N9 Fe1 N1 101.96(13) . . ? N11 Fe1 N1 92.38(13) . . ? N5 Fe1 N1 160.02(13) . . ? N3 Fe1 N7 106.21(13) . . ? N9 Fe1 N7 79.64(12) . . ? N11 Fe1 N7 160.08(14) . . ? N5 Fe1 N7 92.66(13) . . ? N1 Fe1 N7 91.16(13) . . ? C1 N1 N2 105.4(3) . . ? C1 N1 Fe1 142.1(3) . . ? N2 N1 Fe1 112.5(2) . . ? C3 N2 N1 110.9(3) . . ? C3 N2 C4 132.5(3) . . ? N1 N2 C4 116.6(3) . . ? C4 N3 C8 118.6(3) . . ? C4 N3 Fe1 120.6(3) . . ? C8 N3 Fe1 119.8(3) . . ? C9 N4 N5 110.3(3) . . ? C9 N4 C8 132.7(3) . . ? N5 N4 C8 116.9(3) . . ? C11 N5 N4 105.6(3) . . ? C11 N5 Fe1 142.3(3) . . ? N4 N5 Fe1 112.1(2) . . ? C14 N6 C13 122.2(4) . . ? C17 N7 N8 104.8(3) . . ? C17 N7 Fe1 142.7(3) . . ? N8 N7 Fe1 112.5(2) . . ? C19 N8 N7 111.1(3) . . ? C19 N8 C20 132.5(3) . . ? N7 N8 C20 116.4(3) . . ? C20 N9 C24 119.0(3) . . ? C20 N9 Fe1 121.1(2) . . ? C24 N9 Fe1 119.8(2) . . ? C25 N10 N11 111.4(3) . . ? C25 N10 C24 131.6(4) . . ? N11 N10 C24 116.9(3) . . ? C27 N11 N10 105.3(3) . . ? C27 N11 Fe1 142.2(3) . . ? N10 N11 Fe1 112.5(2) . . ? C29 N12 C30 117.9(5) . . ? N1 C1 C2 110.3(4) . . ? C3 C2 C1 106.7(4) . . ? C2 C3 N2 106.7(4) . . ? N3 C4 C5 123.4(3) . . ? N3 C4 N2 110.0(3) . . ? C5 C4 N2 126.5(3) . . ? C4 C5 C6 117.1(4) . . ? C5 C6 C7 120.5(3) . . ? C5 C6 C12 120.2(3) . . ? C7 C6 C12 119.2(3) . . ? C8 C7 C6 117.2(3) . . ? N3 C8 C7 123.2(3) . . ? N3 C8 N4 110.4(3) . . ? C7 C8 N4 126.4(3) . . ? C10 C9 N4 107.4(4) . . ? C9 C10 C11 106.2(3) . . ? N5 C11 C10 110.4(4) . . ? C13 C12 C16 118.5(4) . . ? C13 C12 C6 119.5(3) . . ? C16 C12 C6 122.0(4) . . ? N6 C13 C12 120.1(4) . . ? N6 C14 C15 119.7(4) . . ? C14 C15 C16 119.7(4) . . ? C15 C16 C12 119.8(4) . . ? N7 C17 C18 111.1(3) . . ? C19 C18 C17 106.1(3) . . ? N8 C19 C18 106.9(3) . . ? N9 C20 C21 122.9(3) . . ? N9 C20 N8 110.2(3) . . ? C21 C20 N8 126.8(3) . . ? C20 C21 C22 117.2(3) . . ? C21 C22 C23 119.9(3) . . ? C21 C22 C28 120.7(3) . . ? C23 C22 C28 119.3(3) . . ? C24 C23 C22 117.8(3) . . ? N9 C24 C23 123.1(3) . . ? N9 C24 N10 110.3(3) . . ? C23 C24 N10 126.6(3) . . ? N10 C25 C26 106.2(4) . . ? C25 C26 C27 106.7(4) . . ? N11 C27 C26 110.5(4) . . ? C29 C28 C32 118.0(4) . . ? C29 C28 C22 120.3(4) . . ? C32 C28 C22 121.6(4) . . ? N12 C29 C28 123.2(4) . . ? N12 C30 C31 123.1(4) . . ? C30 C31 C32 119.2(4) . . ? C28 C32 C31 118.6(5) . . ? F2A B1 F3A 118.9(6) . . ? F2A B1 F4B 122.8(6) . . ? F3A B1 F4B 112.3(5) . . ? F2A B1 F1 96.3(5) . . ? F3A B1 F1 101.8(6) . . ? F4B B1 F1 96.7(6) . . ? F2A B1 F4A 108.0(6) . . ? F3A B1 F4A 111.4(5) . . ? F4B B1 F4A 25.1(3) . . ? F1 B1 F4A 120.3(6) . . ? F2A B1 F2B 20.0(4) . . ? F3A B1 F2B 113.2(6) . . ? F4B B1 F2B 115.0(6) . . ? F1 B1 F2B 116.2(5) . . ? F4A B1 F2B 94.6(6) . . ? F2A B1 F3B 109.6(6) . . ? F3A B1 F3B 21.5(4) . . ? F4B B1 F3B 108.7(5) . . ? F1 B1 F3B 123.1(6) . . ? F4A B1 F3B 98.9(5) . . ? F2B B1 F3B 98.0(6) . . ? F7B B2 F6B 143.6(12) . . ? F7B B2 F8A 52.6(7) . . ? F6B B2 F8A 135.8(10) . . ? F7B B2 F6A 134.4(9) . . ? F6B B2 F6A 22.3(9) . . ? F8A B2 F6A 113.6(5) . . ? F7B B2 F5 108.8(8) . . ? F6B B2 F5 95.9(9) . . ? F8A B2 F5 117.7(5) . . ? F6A B2 F5 114.6(5) . . ? F7B B2 F7A 55.4(7) . . ? F6B B2 F7A 93.0(9) . . ? F8A B2 F7A 103.8(5) . . ? F6A B2 F7A 98.8(5) . . ? F5 B2 F7A 105.4(4) . . ? F7B B2 F8B 100.1(8) . . ? F6B B2 F8B 103.5(10) . . ? F8A B2 F8B 48.5(4) . . ? F6A B2 F8B 88.9(5) . . ? F5 B2 F8B 96.1(5) . . ? F7A B2 F8B 151.4(5) . . ? F10B B3 F12A 104.6(6) . . ? F10B B3 F11A 54.4(5) . . ? F12A B3 F11A 116.1(7) . . ? F10B B3 F9B 114.6(7) . . ? F12A B3 F9B 140.4(7) . . ? F11A B3 F9B 91.9(6) . . ? F10B B3 F9A 147.6(7) . . ? F12A B3 F9A 107.0(6) . . ? F11A B3 F9A 114.9(6) . . ? F9B B3 F9A 33.4(4) . . ? F10B B3 F12B 109.6(6) . . ? F12A B3 F12B 27.1(4) . . ? F11A B3 F12B 141.3(7) . . ? F9B B3 F12B 125.1(6) . . ? F9A B3 F12B 95.7(5) . . ? F10B B3 F10A 59.4(4) . . ? F12A B3 F10A 109.2(6) . . ? F11A B3 F10A 105.7(6) . . ? F9B B3 F10A 87.3(5) . . ? F9A B3 F10A 103.0(5) . . ? F12B B3 F10A 88.6(5) . . ? F10B B3 F11B 98.6(5) . . ? F12A B3 F11B 71.5(6) . . ? F11A B3 F11B 57.3(5) . . ? F9B B3 F11B 106.4(5) . . ? F9A B3 F11B 97.8(5) . . ? F12B B3 F11B 97.2(6) . . ? F10A B3 F11B 157.7(5) . . ? N13 C33 C34 177.9(7) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.63 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.425 _refine_diff_density_min -0.779 _refine_diff_density_rms 0.081