# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Ivan Salitros' _publ_contact_author_email ivan.salitros@kit.edu loop_ _publ_author_name M.Ruben I.Salitros O.Fuhr A.Eichhoefer R.Kruk J.Pavlik R.Boca L.Dlhan data_c:\alle\is018pma\abscorr\is-018_a _database_code_depnum_ccdc_archive 'CCDC 846470' #TrackingRef '1A_180 K.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H18 B2 F8 Fe N10' _chemical_formula_weight 699.97 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 orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 15.379(3) _cell_length_b 16.291(3) _cell_length_c 23.329(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5845(2) _cell_formula_units_Z 8 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 3252 _cell_measurement_theta_min 1.34 _cell_measurement_theta_max 26.00 _exptl_crystal_description rod _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.591 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2816 _exptl_absorpt_coefficient_mu 0.605 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8535 _exptl_absorpt_correction_T_max 0.9748 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 -1 -2 0.0350 0 1 2 0.0340 0 -1 2 0.0360 0 1 -2 0.0430 -1 0 1 0.1690 1 0 1 0.1940 1 1 -1 0.1760 _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 ; 157 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 24642 _diffrn_reflns_av_R_equivalents 0.0636 _diffrn_reflns_av_sigmaI/netI 0.1022 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 25.65 _reflns_number_total 10914 _reflns_number_gt 6135 _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^)+(0.0243P)^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 0.00014(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.019(18) _refine_ls_number_reflns 10914 _refine_ls_number_parameters 849 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1072 _refine_ls_R_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.0820 _refine_ls_wR_factor_gt 0.0709 _refine_ls_goodness_of_fit_ref 0.874 _refine_ls_restrained_S_all 0.874 _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 0.22781(4) 0.50118(6) 0.94395(4) 0.0333(2) Uani 1 1 d . . . Fe2 Fe 0.26893(5) 0.00059(6) 0.69456(4) 0.0319(2) Uani 1 1 d . . . N1 N 0.1357(2) 0.5061(4) 0.8855(2) 0.0386(12) Uani 1 1 d . . . N2 N 0.1079(3) 0.5856(3) 0.8767(2) 0.0352(12) Uani 1 1 d . . . N3 N 0.2032(2) 0.6157(3) 0.9456(3) 0.0324(12) Uani 1 1 d . . . N4 N 0.3047(2) 0.6194(3) 1.0163(3) 0.0376(13) Uani 1 1 d . . . N5 N 0.3079(2) 0.5358(3) 1.0044(2) 0.0332(12) Uani 1 1 d . . . N6 N 0.1484(2) 0.4602(3) 1.0030(2) 0.0326(12) Uani 1 1 d . . . N7 N 0.1551(2) 0.3760(3) 1.0103(2) 0.0344(12) Uani 1 1 d . . . N8 N 0.2530(2) 0.3883(3) 0.9392(3) 0.0316(13) Uani 1 1 d . . . N9 N 0.3439(3) 0.4240(3) 0.8685(2) 0.0371(12) Uani 1 1 d . . . N10 N 0.3169(2) 0.5028(4) 0.8837(2) 0.0396(11) Uani 1 1 d . . . N11 N 0.1865(3) 0.0401(3) 0.7518(2) 0.0346(12) Uani 1 1 d . . . N12 N 0.1860(3) 0.1248(3) 0.7574(2) 0.0358(13) Uani 1 1 d . . . N13 N 0.2900(3) 0.1154(3) 0.6907(2) 0.0332(12) Uani 1 1 d . . . N14 N 0.3899(3) 0.0807(3) 0.6230(2) 0.0363(13) Uani 1 1 d . . . N15 N 0.3629(2) 0.0016(3) 0.6373(2) 0.0357(11) Uani 1 1 d . . . N16 N 0.3466(2) -0.0342(3) 0.7560(2) 0.0309(12) Uani 1 1 d . . . N17 N 0.3367(2) -0.1167(3) 0.7707(2) 0.0342(12) Uani 1 1 d . . . N18 N 0.2419(2) -0.1140(3) 0.6972(3) 0.0323(13) Uani 1 1 d . . . N19 N 0.1530(3) -0.0840(3) 0.6225(2) 0.0392(13) Uani 1 1 d . . . N20 N 0.1818(2) -0.0055(4) 0.6324(2) 0.0361(11) Uani 1 1 d . . . C1 C 0.0915(3) 0.4616(4) 0.8493(3) 0.0438(17) Uani 1 1 d . . . H1A H 0.0979 0.4038 0.8456 0.053 Uiso 1 1 calc R . . C2 C 0.0337(3) 0.5081(5) 0.8166(3) 0.0524(17) Uani 1 1 d . . . H2A H -0.0052 0.4892 0.7878 0.063 Uiso 1 1 calc R . . C3 C 0.0451(3) 0.5861(4) 0.8348(3) 0.0454(17) Uani 1 1 d . . . H3A H 0.0149 0.6330 0.8211 0.055 Uiso 1 1 calc R . . C4 C 0.1450(3) 0.6459(4) 0.9092(3) 0.0357(14) Uani 1 1 d . . . C5 C 0.1275(3) 0.7304(4) 0.9072(3) 0.0399(16) Uani 1 1 d . . . H5A H 0.0862 0.7522 0.8810 0.048 Uiso 1 1 calc R . . C6 C 0.1734(3) 0.7816(4) 0.9451(3) 0.0419(16) Uani 1 1 d . . . C7 C 0.2344(3) 0.7490(4) 0.9841(3) 0.0352(16) Uani 1 1 d . . . H7A H 0.2656 0.7827 1.0102 0.042 Uiso 1 1 calc R . . C8 C 0.2461(3) 0.6652(4) 0.9820(3) 0.0366(18) Uani 1 1 d . . . C9 C 0.3586(3) 0.6379(4) 1.0604(3) 0.0435(17) Uani 1 1 d . . . H9A H 0.3683 0.6911 1.0759 0.052 Uiso 1 1 calc R . . C10 C 0.3962(3) 0.5676(4) 1.0786(3) 0.0460(17) Uani 1 1 d . . . H10A H 0.4365 0.5612 1.1091 0.055 Uiso 1 1 calc R . . C11 C 0.3628(3) 0.5057(5) 1.0427(3) 0.0409(15) Uani 1 1 d . . . H11A H 0.3779 0.4493 1.0455 0.049 Uiso 1 1 calc R . . C12 C 0.1557(3) 0.8681(4) 0.9446(3) 0.0477(18) Uani 1 1 d . . . C13 C 0.1408(4) 0.9386(4) 0.9453(4) 0.058(2) Uani 1 1 d . . . H13A H 0.1288 0.9958 0.9457 0.070 Uiso 1 1 calc R . . C14 C 0.0900(3) 0.4853(4) 1.0406(3) 0.0405(16) Uani 1 1 d . . . H14A H 0.0716 0.5406 1.0451 0.049 Uiso 1 1 calc R . . C15 C 0.0589(3) 0.4188(4) 1.0732(3) 0.0422(16) Uani 1 1 d . . . H15A H 0.0170 0.4205 1.1031 0.051 Uiso 1 1 calc R . . C16 C 0.1018(3) 0.3508(4) 1.0525(3) 0.0476(18) Uani 1 1 d . . . H16A H 0.0951 0.2960 1.0657 0.057 Uiso 1 1 calc R . . C17 C 0.2117(3) 0.3344(4) 0.9736(3) 0.0328(15) Uani 1 1 d . . . C18 C 0.2250(3) 0.2514(4) 0.9709(3) 0.0366(15) Uani 1 1 d . . . H18A H 0.1945 0.2149 0.9955 0.044 Uiso 1 1 calc R . . C19 C 0.2844(3) 0.2223(4) 0.9310(3) 0.0365(14) Uani 1 1 d . . . C20 C 0.3276(3) 0.2767(4) 0.8940(3) 0.0370(15) Uani 1 1 d . . . H20A H 0.3669 0.2579 0.8654 0.044 Uiso 1 1 calc R . . C21 C 0.3097(3) 0.3588(4) 0.9013(3) 0.0373(15) Uani 1 1 d . . . C22 C 0.3993(4) 0.4261(4) 0.8231(3) 0.0504(18) Uani 1 1 d . . . H22A H 0.4273 0.3806 0.8056 0.060 Uiso 1 1 calc R . . C23 C 0.4069(4) 0.5071(5) 0.8077(3) 0.0553(19) Uani 1 1 d . . . H23A H 0.4404 0.5286 0.7769 0.066 Uiso 1 1 calc R . . C24 C 0.3558(4) 0.5516(4) 0.8460(3) 0.0484(18) Uani 1 1 d . . . H24A H 0.3496 0.6097 0.8453 0.058 Uiso 1 1 calc R . . C25 C 0.3009(3) 0.1347(4) 0.9262(3) 0.0453(18) Uani 1 1 d . . . C26 C 0.3129(4) 0.0637(4) 0.9253(4) 0.059(2) Uani 1 1 d . . . H26A H 0.3225 0.0061 0.9246 0.071 Uiso 1 1 calc R . . C27 C 0.1305(3) 0.0134(4) 0.7921(3) 0.0392(16) Uani 1 1 d . . . H27A H 0.1172 -0.0427 0.7990 0.047 Uiso 1 1 calc R . . C28 C 0.0947(3) 0.0796(5) 0.8224(3) 0.0451(18) Uani 1 1 d . . . H28A H 0.0533 0.0767 0.8526 0.054 Uiso 1 1 calc R . . C29 C 0.1306(3) 0.1484(4) 0.8001(3) 0.0404(16) Uani 1 1 d . . . H29A H 0.1194 0.2032 0.8121 0.048 Uiso 1 1 calc R . . C30 C 0.2433(3) 0.1667(4) 0.7221(3) 0.0350(17) Uani 1 1 d . . . C31 C 0.2505(3) 0.2525(4) 0.7165(3) 0.0377(18) Uani 1 1 d . . . H31A H 0.2148 0.2891 0.7378 0.045 Uiso 1 1 calc R . . C32 C 0.3123(3) 0.2806(4) 0.6784(3) 0.0381(16) Uani 1 1 d . . . C33 C 0.3613(3) 0.2275(4) 0.6445(3) 0.0382(16) Uani 1 1 d . . . H33A H 0.4019 0.2476 0.6172 0.046 Uiso 1 1 calc R . . C34 C 0.3483(3) 0.1462(4) 0.6522(3) 0.0370(15) Uani 1 1 d . . . C35 C 0.4516(3) 0.0796(4) 0.5820(3) 0.0484(18) Uani 1 1 d . . . H35A H 0.4805 0.1257 0.5659 0.058 Uiso 1 1 calc R . . C36 C 0.4642(3) -0.0003(5) 0.5683(3) 0.0492(15) Uani 1 1 d . . . H36A H 0.5031 -0.0207 0.5401 0.059 Uiso 1 1 calc R . . C37 C 0.4089(3) -0.0479(4) 0.6035(3) 0.0410(16) Uani 1 1 d . . . H37A H 0.4053 -0.1061 0.6031 0.049 Uiso 1 1 calc R . . C38 C 0.3226(3) 0.3697(4) 0.6728(3) 0.0478(19) Uani 1 1 d . . . C39 C 0.3302(4) 0.4399(5) 0.6689(3) 0.057(2) Uani 1 1 d . . . H39A H 0.3365 0.4978 0.6658 0.068 Uiso 1 1 calc R . . C40 C 0.4046(3) -0.0079(4) 0.7933(3) 0.0372(14) Uani 1 1 d . . . H40A H 0.4259 0.0468 0.7943 0.045 Uiso 1 1 calc R . . C41 C 0.4312(4) -0.0687(4) 0.8309(3) 0.0464(18) Uani 1 1 d . . . H41A H 0.4717 -0.0631 0.8614 0.056 Uiso 1 1 calc R . . C42 C 0.3883(3) -0.1372(4) 0.8157(3) 0.0395(16) Uani 1 1 d . . . H42A H 0.3932 -0.1898 0.8331 0.047 Uiso 1 1 calc R . . C43 C 0.2793(3) -0.1613(4) 0.7353(3) 0.0290(14) Uani 1 1 d . . . C44 C 0.2624(3) -0.2448(4) 0.7386(3) 0.0370(16) Uani 1 1 d . . . H44A H 0.2904 -0.2784 0.7663 0.044 Uiso 1 1 calc R . . C45 C 0.2026(3) -0.2775(4) 0.6995(3) 0.0387(16) Uani 1 1 d . . . C46 C 0.1630(3) -0.2274(4) 0.6588(3) 0.0423(17) Uani 1 1 d . . . H46A H 0.1226 -0.2490 0.6319 0.051 Uiso 1 1 calc R . . C47 C 0.1849(3) -0.1451(4) 0.6590(3) 0.0360(15) Uani 1 1 d . . . C48 C 0.0983(4) -0.0856(4) 0.5770(3) 0.0480(17) Uani 1 1 d . . . H48A H 0.0697 -0.1327 0.5620 0.058 Uiso 1 1 calc R . . C49 C 0.0919(4) -0.0087(5) 0.5570(3) 0.0596(19) Uani 1 1 d . . . H49A H 0.0586 0.0092 0.5251 0.071 Uiso 1 1 calc R . . C50 C 0.1447(3) 0.0405(4) 0.5928(3) 0.0429(16) Uani 1 1 d . . . H50A H 0.1523 0.0981 0.5888 0.052 Uiso 1 1 calc R . . C51 C 0.1822(3) -0.3637(4) 0.7011(3) 0.0445(17) Uani 1 1 d . . . C52 C 0.1616(4) -0.4330(4) 0.7023(4) 0.057(2) Uani 1 1 d . . . H52A H 0.1449 -0.4892 0.7033 0.069 Uiso 1 1 calc R . . B1 B 0.9799(4) 0.8234(4) 0.7786(4) 0.0404(19) Uani 1 1 d . . . B2 B 0.4825(4) 0.7008(5) 0.7223(4) 0.0412(19) Uani 1 1 d . . . B3 B -0.0458(4) 0.6894(4) 1.0275(4) 0.0439(19) Uani 1 1 d . . . B4 B -0.0061(4) 0.1888(5) 0.9701(4) 0.049(2) Uani 1 1 d . . . F1 F 1.0683(3) 0.8247(3) 0.7872(3) 0.105(2) Uani 1 1 d . . . F2 F 0.9447(4) 0.8938(3) 0.7934(3) 0.130(3) Uani 1 1 d . . . F3 F 0.9465(2) 0.7572(2) 0.8108(2) 0.0688(14) Uani 1 1 d . . . F4 F 0.9657(3) 0.8101(3) 0.7212(3) 0.0874(16) Uani 1 1 d . . . F5 F 0.4585(2) 0.7756(3) 0.6984(2) 0.0709(14) Uani 1 1 d . . . F6 F 0.4628(2) 0.6997(3) 0.7798(2) 0.0606(12) Uani 1 1 d . . . F7 F 0.4381(2) 0.6381(2) 0.6975(2) 0.0685(11) Uani 1 1 d . . . F8 F 0.5707(2) 0.6901(3) 0.7140(2) 0.0775(15) Uani 1 1 d . . . F9 F 0.0426(2) 0.6748(3) 1.0367(2) 0.0727(14) Uani 1 1 d . . . F10 F -0.0708(2) 0.7597(2) 1.0555(2) 0.0633(12) Uani 1 1 d . . . F11 F -0.0946(3) 0.6234(3) 1.0465(2) 0.0763(13) Uani 1 1 d . . . F12 F -0.0586(2) 0.6969(3) 0.9684(2) 0.0575(11) Uani 1 1 d . . . F13 F 0.0275(2) 0.2568(3) 0.9426(2) 0.0640(12) Uani 1 1 d . . . F14 F 0.0166(3) 0.1880(3) 1.0282(3) 0.0808(14) Uani 1 1 d . . . F15 F -0.09458(19) 0.1882(3) 0.9665(2) 0.0644(13) Uani 1 1 d . . . F16 F 0.0260(2) 0.1164(2) 0.9457(2) 0.0766(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0385(3) 0.0240(4) 0.0375(6) 0.0004(5) -0.0004(4) 0.0037(4) Fe2 0.0385(3) 0.0236(4) 0.0336(5) 0.0005(5) 0.0013(4) -0.0024(4) N1 0.042(2) 0.030(3) 0.044(3) -0.003(3) -0.002(2) 0.003(3) N2 0.041(2) 0.028(3) 0.036(4) 0.002(2) 0.000(2) 0.007(2) N3 0.029(2) 0.027(3) 0.042(4) -0.004(3) -0.002(2) 0.0020(19) N4 0.040(2) 0.024(3) 0.049(4) 0.006(3) -0.002(2) 0.0004(19) N5 0.033(2) 0.027(3) 0.039(3) 0.000(2) 0.000(2) 0.0029(18) N6 0.038(2) 0.021(2) 0.039(3) -0.004(2) 0.002(2) 0.0016(18) N7 0.039(2) 0.026(3) 0.038(3) 0.000(2) 0.005(2) 0.000(2) N8 0.034(2) 0.028(3) 0.033(4) 0.005(3) -0.002(2) 0.0045(19) N9 0.049(2) 0.033(3) 0.029(3) 0.003(2) 0.015(2) 0.000(2) N10 0.045(2) 0.031(3) 0.043(3) 0.004(3) -0.003(2) 0.006(3) N11 0.042(2) 0.023(3) 0.040(3) -0.001(2) 0.006(2) 0.0004(19) N12 0.036(2) 0.038(3) 0.034(3) -0.004(3) 0.006(2) 0.003(2) N13 0.044(2) 0.019(3) 0.037(4) 0.001(2) -0.002(2) -0.006(2) N14 0.044(2) 0.032(3) 0.034(3) -0.003(2) 0.009(2) 0.004(2) N15 0.047(2) 0.022(2) 0.038(3) -0.003(3) 0.003(2) -0.002(3) N16 0.037(2) 0.024(2) 0.032(3) 0.000(2) 0.001(2) -0.0026(18) N17 0.039(2) 0.022(3) 0.041(4) -0.001(2) -0.001(2) -0.002(2) N18 0.034(2) 0.027(3) 0.037(3) -0.007(3) -0.005(2) -0.003(2) N19 0.054(3) 0.025(3) 0.039(4) 0.003(2) -0.004(2) -0.009(2) N20 0.046(2) 0.025(3) 0.037(3) 0.002(3) -0.007(2) -0.002(2) C1 0.050(3) 0.036(3) 0.045(5) -0.013(3) -0.004(3) 0.005(3) C2 0.056(3) 0.053(4) 0.048(4) -0.003(4) -0.017(3) 0.000(3) C3 0.052(3) 0.048(4) 0.036(4) 0.007(3) -0.010(3) 0.014(3) C4 0.043(3) 0.031(3) 0.033(4) 0.007(3) 0.000(3) 0.001(3) C5 0.048(3) 0.024(3) 0.048(4) 0.008(3) -0.001(3) 0.010(2) C6 0.042(3) 0.031(3) 0.053(5) -0.005(3) 0.010(3) 0.002(3) C7 0.040(3) 0.022(3) 0.043(5) 0.000(3) 0.003(3) 0.000(2) C8 0.029(3) 0.033(4) 0.048(5) -0.002(3) -0.001(2) -0.002(2) C9 0.042(3) 0.042(4) 0.047(5) -0.004(3) -0.007(3) -0.014(3) C10 0.043(3) 0.047(4) 0.048(5) -0.001(4) -0.011(3) 0.009(3) C11 0.037(2) 0.039(3) 0.047(4) -0.006(4) 0.001(3) 0.002(3) C12 0.045(3) 0.033(4) 0.065(5) 0.002(4) 0.003(3) -0.005(3) C13 0.069(4) 0.022(3) 0.084(6) -0.001(4) 0.006(4) 0.003(3) C14 0.042(3) 0.036(4) 0.043(4) -0.006(3) 0.007(3) 0.003(3) C15 0.049(3) 0.041(4) 0.037(4) -0.003(3) 0.004(3) 0.002(3) C16 0.045(3) 0.044(4) 0.054(5) 0.002(4) 0.009(3) 0.002(3) C17 0.030(3) 0.026(3) 0.042(4) 0.002(3) -0.001(3) -0.001(2) C18 0.041(3) 0.028(3) 0.041(4) 0.007(3) -0.002(3) 0.003(3) C19 0.043(3) 0.029(3) 0.038(4) -0.002(3) -0.004(3) 0.003(3) C20 0.041(3) 0.033(3) 0.037(4) -0.007(3) -0.001(3) 0.006(2) C21 0.040(3) 0.029(3) 0.043(4) -0.004(3) -0.002(3) 0.008(2) C22 0.054(3) 0.051(4) 0.046(5) -0.009(4) 0.019(3) 0.000(3) C23 0.068(3) 0.045(4) 0.053(5) 0.021(4) 0.023(3) 0.011(4) C24 0.055(4) 0.049(4) 0.041(5) 0.018(4) 0.014(3) 0.002(3) C25 0.040(3) 0.032(4) 0.063(5) -0.008(3) 0.004(3) 0.000(2) C26 0.061(4) 0.031(4) 0.086(7) -0.006(4) 0.015(4) 0.001(3) C27 0.045(3) 0.029(4) 0.043(4) 0.008(3) 0.001(3) -0.011(3) C28 0.041(3) 0.057(4) 0.037(4) 0.011(4) 0.009(3) 0.006(3) C29 0.041(3) 0.033(3) 0.047(5) 0.000(3) 0.012(3) 0.002(2) C30 0.036(3) 0.024(3) 0.045(5) 0.002(3) 0.005(3) 0.001(2) C31 0.041(3) 0.027(3) 0.045(5) -0.001(3) 0.001(3) 0.001(2) C32 0.037(3) 0.025(3) 0.053(5) -0.001(3) -0.007(3) -0.006(2) C33 0.040(3) 0.033(3) 0.042(4) -0.001(3) 0.000(3) -0.001(2) C34 0.040(3) 0.031(3) 0.040(4) 0.000(3) 0.003(3) -0.010(2) C35 0.047(3) 0.051(4) 0.048(5) -0.002(3) 0.017(3) -0.004(3) C36 0.061(3) 0.046(4) 0.041(4) -0.010(4) 0.016(3) 0.000(4) C37 0.047(3) 0.033(3) 0.042(5) -0.009(3) 0.011(3) -0.006(3) C38 0.045(3) 0.029(4) 0.069(6) 0.006(3) -0.001(3) 0.003(2) C39 0.067(4) 0.031(4) 0.072(6) -0.003(4) 0.020(4) -0.003(3) C40 0.041(3) 0.030(3) 0.040(4) -0.001(3) 0.001(3) -0.006(3) C41 0.047(3) 0.045(4) 0.047(5) -0.004(3) -0.010(3) 0.001(3) C42 0.058(3) 0.033(3) 0.028(4) 0.002(3) -0.020(3) 0.011(3) C43 0.029(3) 0.027(3) 0.031(4) -0.002(3) 0.000(2) 0.004(2) C44 0.036(3) 0.027(3) 0.047(5) 0.003(3) -0.005(3) -0.005(2) C45 0.043(3) 0.024(3) 0.049(5) -0.001(3) 0.008(3) -0.001(2) C46 0.045(3) 0.029(3) 0.054(5) -0.005(3) -0.001(3) -0.010(3) C47 0.037(3) 0.028(3) 0.043(4) 0.006(3) -0.001(3) 0.001(2) C48 0.058(3) 0.044(4) 0.043(5) 0.002(3) -0.022(3) -0.008(3) C49 0.080(4) 0.059(5) 0.039(5) -0.001(4) -0.021(3) 0.000(4) C50 0.051(3) 0.038(3) 0.040(4) 0.010(3) -0.005(3) -0.004(3) C51 0.050(3) 0.030(4) 0.053(5) -0.003(3) -0.003(3) -0.003(3) C52 0.057(3) 0.036(4) 0.079(6) 0.003(4) -0.003(4) -0.008(3) B1 0.049(4) 0.028(4) 0.044(5) 0.009(4) -0.012(3) -0.007(3) B2 0.042(3) 0.035(4) 0.046(5) -0.007(4) 0.007(3) 0.003(3) B3 0.056(4) 0.020(3) 0.055(6) 0.004(4) -0.009(4) 0.004(3) B4 0.049(4) 0.035(4) 0.062(7) 0.009(4) 0.003(4) 0.014(3) F1 0.078(3) 0.093(4) 0.145(6) 0.041(4) -0.026(3) -0.022(3) F2 0.225(5) 0.064(3) 0.103(5) 0.039(3) 0.094(4) 0.068(3) F3 0.058(2) 0.052(2) 0.096(4) 0.032(3) -0.010(2) -0.0011(16) F4 0.146(4) 0.050(3) 0.066(4) 0.004(3) -0.026(3) -0.018(3) F5 0.074(2) 0.046(2) 0.093(4) 0.023(2) 0.026(2) 0.0139(18) F6 0.071(2) 0.060(3) 0.051(3) -0.003(2) 0.0095(19) 0.0029(19) F7 0.097(2) 0.047(2) 0.062(3) -0.006(2) -0.006(2) -0.0034(19) F8 0.0579(19) 0.074(3) 0.101(4) 0.028(3) 0.025(2) 0.015(2) F9 0.065(2) 0.068(3) 0.085(4) -0.010(3) -0.040(2) 0.023(2) F10 0.0653(19) 0.042(2) 0.082(4) -0.019(2) -0.009(2) 0.0037(16) F11 0.121(3) 0.050(2) 0.057(3) 0.000(2) 0.011(2) -0.037(2) F12 0.070(2) 0.050(2) 0.052(3) 0.010(2) -0.010(2) 0.0007(18) F13 0.0616(19) 0.050(2) 0.080(4) 0.022(2) -0.004(2) -0.0060(17) F14 0.136(3) 0.051(3) 0.055(4) 0.005(3) -0.018(3) -0.006(3) F15 0.0543(19) 0.064(3) 0.075(4) -0.005(3) 0.0126(19) 0.0031(17) F16 0.111(3) 0.043(2) 0.075(3) -0.012(2) 0.039(2) 0.004(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. ; 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 N8 1.883(5) . ? Fe1 N3 1.904(5) . ? Fe1 N5 1.956(5) . ? Fe1 N6 1.958(5) . ? Fe1 N10 1.963(5) . ? Fe1 N1 1.968(5) . ? Fe2 N13 1.901(5) . ? Fe2 N18 1.913(5) . ? Fe2 N16 1.950(5) . ? Fe2 N11 1.950(5) . ? Fe2 N15 1.967(4) . ? Fe2 N20 1.976(4) . ? N1 C1 1.305(8) . ? N1 N2 1.380(7) . ? N2 C4 1.366(8) . ? N2 C3 1.374(8) . ? N3 C4 1.328(8) . ? N3 C8 1.344(8) . ? N4 C9 1.356(8) . ? N4 N5 1.390(7) . ? N4 C8 1.417(8) . ? N5 C11 1.323(8) . ? N6 C14 1.321(7) . ? N6 N7 1.385(7) . ? N7 C16 1.346(9) . ? N7 C17 1.396(8) . ? N8 C21 1.332(8) . ? N8 C17 1.349(8) . ? N9 C22 1.361(8) . ? N9 N10 1.395(8) . ? N9 C21 1.410(8) . ? N10 C24 1.328(8) . ? N11 C27 1.347(8) . ? N11 N12 1.386(7) . ? N12 C29 1.366(8) . ? N12 C30 1.386(8) . ? N13 C30 1.323(8) . ? N13 C34 1.366(8) . ? N14 C35 1.346(8) . ? N14 N15 1.395(7) . ? N14 C34 1.420(8) . ? N15 C37 1.331(8) . ? N16 C40 1.318(7) . ? N16 N17 1.396(7) . ? N17 C42 1.359(8) . ? N17 C43 1.410(7) . ? N18 C43 1.308(8) . ? N18 C47 1.350(8) . ? N19 C48 1.356(8) . ? N19 N20 1.372(7) . ? N19 C47 1.398(8) . ? N20 C50 1.321(8) . ? C1 C2 1.396(9) . ? C2 C3 1.351(10) . ? C4 C5 1.403(8) . ? C5 C6 1.407(9) . ? C6 C7 1.410(9) . ? C6 C12 1.435(9) . ? C7 C8 1.377(9) . ? C9 C10 1.352(9) . ? C10 C11 1.408(10) . ? C12 C13 1.172(9) . ? C14 C15 1.406(9) . ? C15 C16 1.377(9) . ? C17 C18 1.369(8) . ? C18 C19 1.388(9) . ? C19 C20 1.405(9) . ? C19 C25 1.454(9) . ? C20 C21 1.375(9) . ? C22 C23 1.373(10) . ? C23 C24 1.394(9) . ? C25 C26 1.172(9) . ? C27 C28 1.403(10) . ? C28 C29 1.354(9) . ? C30 C31 1.408(9) . ? C31 C32 1.377(9) . ? C32 C33 1.394(9) . ? C32 C38 1.466(9) . ? C33 C34 1.351(9) . ? C35 C36 1.354(10) . ? C36 C37 1.413(9) . ? C38 C39 1.154(9) . ? C40 C41 1.385(9) . ? C41 C42 1.344(9) . ? C43 C44 1.387(8) . ? C44 C45 1.402(9) . ? C45 C46 1.393(9) . ? C45 C51 1.438(9) . ? C46 C47 1.383(9) . ? C48 C49 1.341(10) . ? C49 C50 1.413(9) . ? C51 C52 1.175(9) . ? B1 F2 1.314(9) . ? B1 F1 1.374(7) . ? B1 F4 1.374(10) . ? B1 F3 1.411(8) . ? B2 F7 1.358(8) . ? B2 F6 1.376(9) . ? B2 F8 1.381(7) . ? B2 F5 1.390(9) . ? B3 F10 1.373(8) . ? B3 F11 1.384(8) . ? B3 F9 1.397(7) . ? B3 F12 1.398(10) . ? B4 F15 1.364(7) . ? B4 F13 1.378(9) . ? B4 F16 1.399(9) . ? B4 F14 1.401(11) . ? 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 N8 Fe1 N3 177.7(3) . . ? N8 Fe1 N5 101.2(2) . . ? N3 Fe1 N5 80.1(2) . . ? N8 Fe1 N6 80.6(2) . . ? N3 Fe1 N6 101.3(2) . . ? N5 Fe1 N6 89.1(2) . . ? N8 Fe1 N10 80.0(2) . . ? N3 Fe1 N10 98.0(2) . . ? N5 Fe1 N10 94.19(19) . . ? N6 Fe1 N10 160.6(2) . . ? N8 Fe1 N1 98.5(2) . . ? N3 Fe1 N1 80.3(2) . . ? N5 Fe1 N1 160.3(2) . . ? N6 Fe1 N1 93.0(2) . . ? N10 Fe1 N1 90.32(18) . . ? N13 Fe2 N18 177.2(2) . . ? N13 Fe2 N16 102.5(2) . . ? N18 Fe2 N16 79.9(2) . . ? N13 Fe2 N11 79.5(2) . . ? N18 Fe2 N11 99.1(2) . . ? N16 Fe2 N11 89.5(2) . . ? N13 Fe2 N15 80.5(2) . . ? N18 Fe2 N15 100.9(2) . . ? N16 Fe2 N15 92.96(19) . . ? N11 Fe2 N15 159.9(2) . . ? N13 Fe2 N20 97.5(2) . . ? N18 Fe2 N20 80.1(2) . . ? N16 Fe2 N20 160.0(2) . . ? N11 Fe2 N20 94.5(2) . . ? N15 Fe2 N20 90.02(17) . . ? C1 N1 N2 105.3(5) . . ? C1 N1 Fe1 143.2(5) . . ? N2 N1 Fe1 111.4(4) . . ? C4 N2 C3 133.2(5) . . ? C4 N2 N1 117.6(5) . . ? C3 N2 N1 109.2(5) . . ? C4 N3 C8 120.8(6) . . ? C4 N3 Fe1 119.0(4) . . ? C8 N3 Fe1 120.2(4) . . ? C9 N4 N5 110.3(5) . . ? C9 N4 C8 134.4(6) . . ? N5 N4 C8 115.2(5) . . ? C11 N5 N4 104.6(5) . . ? C11 N5 Fe1 141.3(5) . . ? N4 N5 Fe1 113.8(4) . . ? C14 N6 N7 106.0(5) . . ? C14 N6 Fe1 141.8(4) . . ? N7 N6 Fe1 112.2(4) . . ? C16 N7 N6 110.3(5) . . ? C16 N7 C17 132.9(5) . . ? N6 N7 C17 116.8(5) . . ? C21 N8 C17 117.9(6) . . ? C21 N8 Fe1 121.8(4) . . ? C17 N8 Fe1 120.2(4) . . ? C22 N9 N10 111.1(5) . . ? C22 N9 C21 132.4(5) . . ? N10 N9 C21 116.4(5) . . ? C24 N10 N9 104.5(5) . . ? C24 N10 Fe1 142.8(5) . . ? N9 N10 Fe1 112.1(4) . . ? C27 N11 N12 104.6(5) . . ? C27 N11 Fe2 141.8(4) . . ? N12 N11 Fe2 113.4(4) . . ? C29 N12 N11 110.7(5) . . ? C29 N12 C30 133.7(6) . . ? N11 N12 C30 115.5(5) . . ? C30 N13 C34 119.3(5) . . ? C30 N13 Fe2 120.2(4) . . ? C34 N13 Fe2 120.3(4) . . ? C35 N14 N15 111.6(5) . . ? C35 N14 C34 132.0(5) . . ? N15 N14 C34 116.4(4) . . ? C37 N15 N14 104.9(5) . . ? C37 N15 Fe2 142.0(5) . . ? N14 N15 Fe2 112.9(4) . . ? C40 N16 N17 103.0(5) . . ? C40 N16 Fe2 143.7(5) . . ? N17 N16 Fe2 113.2(4) . . ? C42 N17 N16 111.3(5) . . ? C42 N17 C43 133.8(5) . . ? N16 N17 C43 114.9(5) . . ? C43 N18 C47 120.9(6) . . ? C43 N18 Fe2 120.1(4) . . ? C47 N18 Fe2 119.0(5) . . ? C48 N19 N20 110.5(5) . . ? C48 N19 C47 132.8(5) . . ? N20 N19 C47 116.6(5) . . ? C50 N20 N19 105.7(5) . . ? C50 N20 Fe2 141.1(5) . . ? N19 N20 Fe2 112.9(4) . . ? N1 C1 C2 112.5(6) . . ? C3 C2 C1 104.8(6) . . ? C2 C3 N2 108.1(6) . . ? N3 C4 N2 111.7(5) . . ? N3 C4 C5 120.9(6) . . ? N2 C4 C5 127.3(6) . . ? C4 C5 C6 117.7(6) . . ? C5 C6 C7 121.1(6) . . ? C5 C6 C12 118.8(6) . . ? C7 C6 C12 120.1(6) . . ? C8 C7 C6 115.9(6) . . ? N3 C8 C7 123.5(6) . . ? N3 C8 N4 110.6(6) . . ? C7 C8 N4 125.8(6) . . ? C10 C9 N4 108.1(6) . . ? C9 C10 C11 105.3(6) . . ? N5 C11 C10 111.6(6) . . ? C13 C12 C6 178.8(9) . . ? N6 C14 C15 110.6(6) . . ? C16 C15 C14 105.5(6) . . ? N7 C16 C15 107.6(6) . . ? N8 C17 C18 123.1(6) . . ? N8 C17 N7 110.0(5) . . ? C18 C17 N7 126.9(6) . . ? C17 C18 C19 117.8(6) . . ? C18 C19 C20 120.6(5) . . ? C18 C19 C25 120.1(6) . . ? C20 C19 C25 119.3(6) . . ? C21 C20 C19 116.3(6) . . ? N8 C21 C20 124.4(6) . . ? N8 C21 N9 109.4(5) . . ? C20 C21 N9 126.2(6) . . ? N9 C22 C23 106.4(6) . . ? C22 C23 C24 106.5(6) . . ? N10 C24 C23 111.5(6) . . ? C26 C25 C19 176.4(9) . . ? N11 C27 C28 110.8(6) . . ? C29 C28 C27 106.4(6) . . ? C28 C29 N12 107.5(6) . . ? N13 C30 N12 111.3(6) . . ? N13 C30 C31 122.2(6) . . ? N12 C30 C31 126.5(6) . . ? C32 C31 C30 116.4(6) . . ? C31 C32 C33 122.2(6) . . ? C31 C32 C38 117.4(6) . . ? C33 C32 C38 120.3(6) . . ? C34 C33 C32 116.9(6) . . ? C33 C34 N13 123.0(6) . . ? C33 C34 N14 127.4(6) . . ? N13 C34 N14 109.6(5) . . ? N14 C35 C36 106.3(6) . . ? C35 C36 C37 107.7(5) . . ? N15 C37 C36 109.4(6) . . ? C39 C38 C32 179.2(9) . . ? N16 C40 C41 112.7(6) . . ? C42 C41 C40 106.4(6) . . ? C41 C42 N17 106.6(6) . . ? N18 C43 C44 122.2(6) . . ? N18 C43 N17 111.7(5) . . ? C44 C43 N17 126.1(6) . . ? C43 C44 C45 117.4(6) . . ? C46 C45 C44 120.5(6) . . ? C46 C45 C51 119.6(6) . . ? C44 C45 C51 119.9(6) . . ? C47 C46 C45 117.4(6) . . ? N18 C47 C46 121.6(6) . . ? N18 C47 N19 111.3(6) . . ? C46 C47 N19 127.1(6) . . ? C49 C48 N19 107.4(6) . . ? C48 C49 C50 106.4(6) . . ? N20 C50 C49 109.9(6) . . ? C52 C51 C45 176.9(6) . . ? F2 B1 F1 110.9(7) . . ? F2 B1 F4 109.1(6) . . ? F1 B1 F4 107.6(7) . . ? F2 B1 F3 112.2(6) . . ? F1 B1 F3 107.1(6) . . ? F4 B1 F3 109.9(6) . . ? F7 B2 F6 107.1(6) . . ? F7 B2 F8 109.9(6) . . ? F6 B2 F8 110.6(6) . . ? F7 B2 F5 110.8(6) . . ? F6 B2 F5 110.1(6) . . ? F8 B2 F5 108.4(6) . . ? F10 B3 F11 110.1(6) . . ? F10 B3 F9 110.0(6) . . ? F11 B3 F9 110.3(6) . . ? F10 B3 F12 110.9(6) . . ? F11 B3 F12 107.9(6) . . ? F9 B3 F12 107.6(6) . . ? F15 B4 F13 110.5(6) . . ? F15 B4 F16 108.7(7) . . ? F13 B4 F16 110.9(6) . . ? F15 B4 F14 108.0(6) . . ? F13 B4 F14 111.3(7) . . ? F16 B4 F14 107.3(6) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.65 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.346 _refine_diff_density_min -0.240 _refine_diff_density_rms 0.047 # Attachment '1A_350 K.CIF' data_c:\alle\is018rta\abskorr\is18a_ht _database_code_depnum_ccdc_archive 'CCDC 846471' #TrackingRef '1A_350 K.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H18 B2 F8 Fe N10' _chemical_formula_weight 699.97 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 orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 15.681(3) _cell_length_b 16.300(3) _cell_length_c 23.553(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6020(2) _cell_formula_units_Z 8 _cell_measurement_temperature 350(2) _cell_measurement_reflns_used 2059 _cell_measurement_theta_min 1.51 _cell_measurement_theta_max 24.84 _exptl_crystal_description rod _exptl_crystal_colour red _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.545 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2816 _exptl_absorpt_coefficient_mu 0.588 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8583 _exptl_absorpt_correction_T_max 0.9433 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 -1 -2 0.0680 0 1 2 0.0710 1 0 0 0.1840 -1 0 0 0.2020 0 -1 2 0.0990 0 1 -2 0.0780 _exptl_special_details ; ? ; _diffrn_ambient_temperature 350(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 ; 125 frames, detector distance = 140 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 20458 _diffrn_reflns_av_R_equivalents 0.0474 _diffrn_reflns_av_sigmaI/netI 0.0525 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 24.59 _reflns_number_total 10047 _reflns_number_gt 6320 _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^)+(0.1054P)^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 none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.06(2) _refine_ls_number_reflns 10047 _refine_ls_number_parameters 848 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0929 _refine_ls_R_factor_gt 0.0593 _refine_ls_wR_factor_ref 0.1713 _refine_ls_wR_factor_gt 0.1535 _refine_ls_goodness_of_fit_ref 0.954 _refine_ls_restrained_S_all 0.954 _refine_ls_shift/su_max 0.002 _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 0.22465(5) 0.50140(5) 0.94331(3) 0.0652(2) Uani 1 1 d . . . Fe2 Fe 0.27182(5) 0.00003(5) 0.69320(3) 0.0647(2) Uani 1 1 d . . . N1 N 0.1317(3) 0.5095(3) 0.8855(2) 0.0776(13) Uani 1 1 d . . . N2 N 0.1057(3) 0.5896(3) 0.8772(2) 0.0745(13) Uani 1 1 d . . . N3 N 0.2010(3) 0.6183(3) 0.9448(2) 0.0675(12) Uani 1 1 d . . . N4 N 0.3010(3) 0.6197(3) 1.0151(2) 0.0807(14) Uani 1 1 d . . . N5 N 0.3031(3) 0.5364(3) 1.0034(2) 0.0764(14) Uani 1 1 d . . . N6 N 0.1462(3) 0.4566(3) 1.0014(2) 0.0723(13) Uani 1 1 d . . . N7 N 0.1532(3) 0.3730(3) 1.0090(2) 0.0777(14) Uani 1 1 d . . . N8 N 0.2501(3) 0.3847(3) 0.9376(2) 0.0652(13) Uani 1 1 d . . . N9 N 0.3391(4) 0.4237(3) 0.8680(2) 0.0834(15) Uani 1 1 d . . . N10 N 0.3113(3) 0.5023(4) 0.8821(2) 0.0807(13) Uani 1 1 d . . . N11 N 0.1897(3) 0.0422(3) 0.7507(2) 0.0723(13) Uani 1 1 d . . . N12 N 0.1896(3) 0.1279(3) 0.7548(2) 0.0797(14) Uani 1 1 d . . . N13 N 0.2926(3) 0.1151(3) 0.6879(2) 0.0669(12) Uani 1 1 d . . . N14 N 0.3913(3) 0.0819(3) 0.6224(2) 0.0764(14) Uani 1 1 d . . . N15 N 0.3649(3) 0.0038(4) 0.6358(2) 0.0788(12) Uani 1 1 d . . . N16 N 0.3478(3) -0.0373(3) 0.7558(2) 0.0721(13) Uani 1 1 d . . . N17 N 0.3361(3) -0.1181(3) 0.7692(2) 0.0766(14) Uani 1 1 d . . . N18 N 0.2440(3) -0.1149(3) 0.6968(2) 0.0696(13) Uani 1 1 d . . . N19 N 0.1566(4) -0.0887(3) 0.6229(2) 0.0831(15) Uani 1 1 d . . . N20 N 0.1850(3) -0.0107(3) 0.63083(19) 0.0755(13) Uani 1 1 d . . . C1 C 0.0862(5) 0.4646(5) 0.8498(3) 0.099(2) Uani 1 1 d . . . H1A H 0.0899 0.4078 0.8468 0.119 Uiso 1 1 calc R . . C2 C 0.0314(6) 0.5141(5) 0.8168(3) 0.115(3) Uani 1 1 d . . . H2A H -0.0054 0.4975 0.7881 0.138 Uiso 1 1 calc R . . C3 C 0.0444(5) 0.5912(5) 0.8362(3) 0.099(2) Uani 1 1 d . . . H3A H 0.0160 0.6379 0.8237 0.118 Uiso 1 1 calc R . . C4 C 0.1431(4) 0.6498(4) 0.9112(3) 0.0753(16) Uani 1 1 d . . . C5 C 0.1282(5) 0.7327(4) 0.9077(3) 0.0859(19) Uani 1 1 d . . . H5A H 0.0902 0.7543 0.8813 0.103 Uiso 1 1 calc R . . C6 C 0.1719(4) 0.7822(4) 0.9449(3) 0.0830(19) Uani 1 1 d . . . C7 C 0.2314(5) 0.7495(4) 0.9818(3) 0.085(2) Uani 1 1 d . . . H7A H 0.2617 0.7828 1.0067 0.102 Uiso 1 1 calc R . . C8 C 0.2443(4) 0.6665(4) 0.9804(3) 0.0713(17) Uani 1 1 d . . . C9 C 0.3541(5) 0.6386(5) 1.0565(3) 0.095(2) Uani 1 1 d . . . H9A H 0.3633 0.6912 1.0706 0.114 Uiso 1 1 calc R . . C10 C 0.3938(5) 0.5684(5) 1.0758(3) 0.098(2) Uani 1 1 d . . . H10A H 0.4338 0.5628 1.1047 0.118 Uiso 1 1 calc R . . C11 C 0.3588(4) 0.5080(4) 1.0410(3) 0.0839(17) Uani 1 1 d . . . H11A H 0.3732 0.4528 1.0439 0.101 Uiso 1 1 calc R . . C12 C 0.1570(5) 0.8692(4) 0.9438(4) 0.106(2) Uani 1 1 d . . . C13 C 0.1426(6) 0.9389(5) 0.9454(4) 0.129(3) Uani 1 1 d . . . H13A H 0.1311 0.9948 0.9467 0.154 Uiso 1 1 calc R . . C14 C 0.0896(5) 0.4799(4) 1.0394(3) 0.091(2) Uani 1 1 d . . . H14A H 0.0720 0.5339 1.0443 0.109 Uiso 1 1 calc R . . C15 C 0.0593(5) 0.4148(5) 1.0713(3) 0.102(2) Uani 1 1 d . . . H15A H 0.0196 0.4160 1.1006 0.123 Uiso 1 1 calc R . . C16 C 0.1014(5) 0.3486(5) 1.0495(3) 0.095(2) Uani 1 1 d . . . H16A H 0.0944 0.2947 1.0615 0.114 Uiso 1 1 calc R . . C17 C 0.2100(4) 0.3336(3) 0.9714(3) 0.0671(15) Uani 1 1 d . . . C18 C 0.2253(5) 0.2513(4) 0.9692(3) 0.087(2) Uani 1 1 d . . . H18A H 0.1979 0.2154 0.9938 0.104 Uiso 1 1 calc R . . C19 C 0.2832(4) 0.2225(4) 0.9288(3) 0.0819(18) Uani 1 1 d . . . C20 C 0.3263(4) 0.2800(4) 0.8935(3) 0.0816(17) Uani 1 1 d . . . H20A H 0.3667 0.2638 0.8669 0.098 Uiso 1 1 calc R . . C21 C 0.3050(4) 0.3591(4) 0.9009(3) 0.0702(15) Uani 1 1 d . . . C22 C 0.3932(5) 0.4259(5) 0.8231(3) 0.104(2) Uani 1 1 d . . . H22A H 0.4192 0.3812 0.8057 0.125 Uiso 1 1 calc R . . C23 C 0.4023(6) 0.5071(6) 0.8082(3) 0.122(3) Uani 1 1 d . . . H23A H 0.4358 0.5281 0.7790 0.146 Uiso 1 1 calc R . . C24 C 0.3498(6) 0.5525(5) 0.8465(3) 0.100(2) Uani 1 1 d . . . H24A H 0.3437 0.6092 0.8464 0.121 Uiso 1 1 calc R . . C25 C 0.3007(5) 0.1361(4) 0.9245(4) 0.098(2) Uani 1 1 d . . . C26 C 0.3125(5) 0.0662(5) 0.9226(4) 0.121(3) Uani 1 1 d . . . H26A H 0.3220 0.0099 0.9211 0.145 Uiso 1 1 calc R . . C27 C 0.1355(5) 0.0175(4) 0.7894(3) 0.0867(19) Uani 1 1 d . . . H27A H 0.1224 -0.0371 0.7966 0.104 Uiso 1 1 calc R . . C28 C 0.1005(5) 0.0830(6) 0.8182(3) 0.103(2) Uani 1 1 d . . . H28A H 0.0610 0.0802 0.8476 0.124 Uiso 1 1 calc R . . C29 C 0.1339(5) 0.1520(5) 0.7958(3) 0.098(2) Uani 1 1 d . . . H29A H 0.1214 0.2057 0.8063 0.117 Uiso 1 1 calc R . . C30 C 0.2463(4) 0.1693(4) 0.7175(3) 0.0729(17) Uani 1 1 d . . . C31 C 0.2536(4) 0.2542(4) 0.7126(4) 0.087(2) Uani 1 1 d . . . H31A H 0.2201 0.2898 0.7339 0.105 Uiso 1 1 calc R . . C32 C 0.3122(4) 0.2815(4) 0.6752(3) 0.0771(17) Uani 1 1 d . . . C33 C 0.3619(4) 0.2287(4) 0.6418(3) 0.0789(17) Uani 1 1 d . . . H33A H 0.4015 0.2482 0.6157 0.095 Uiso 1 1 calc R . . C34 C 0.3481(4) 0.1461(3) 0.6503(2) 0.0639(14) Uani 1 1 d . . . C35 C 0.4522(5) 0.0804(5) 0.5814(3) 0.098(2) Uani 1 1 d . . . H35A H 0.4784 0.1255 0.5647 0.118 Uiso 1 1 calc R . . C36 C 0.4672(6) 0.0012(6) 0.5697(3) 0.115(2) Uani 1 1 d . . . H36A H 0.5070 -0.0192 0.5440 0.138 Uiso 1 1 calc R . . C37 C 0.4116(5) -0.0449(4) 0.6033(3) 0.091(2) Uani 1 1 d . . . H37A H 0.4079 -0.1018 0.6029 0.109 Uiso 1 1 calc R . . C38 C 0.3230(5) 0.3689(4) 0.6688(4) 0.102(2) Uani 1 1 d . . . C39 C 0.3309(6) 0.4387(5) 0.6660(4) 0.123(3) Uani 1 1 d . . . H39A H 0.3373 0.4954 0.6638 0.147 Uiso 1 1 calc R . . C40 C 0.4056(4) -0.0092(5) 0.7917(3) 0.0916(19) Uani 1 1 d . . . H40A H 0.4264 0.0442 0.7923 0.110 Uiso 1 1 calc R . . C41 C 0.4306(6) -0.0714(6) 0.8287(4) 0.119(3) Uani 1 1 d . . . H41A H 0.4707 -0.0670 0.8577 0.143 Uiso 1 1 calc R . . C42 C 0.3868(5) -0.1380(5) 0.8149(3) 0.100(2) Uani 1 1 d . . . H42A H 0.3897 -0.1888 0.8328 0.120 Uiso 1 1 calc R . . C43 C 0.2808(4) -0.1638(3) 0.7365(3) 0.0720(16) Uani 1 1 d . . . C44 C 0.2612(5) -0.2448(4) 0.7397(3) 0.082(2) Uani 1 1 d . . . H44A H 0.2854 -0.2773 0.7678 0.099 Uiso 1 1 calc R . . C45 C 0.2034(5) -0.2797(4) 0.6999(4) 0.087(2) Uani 1 1 d . . . C46 C 0.1673(5) -0.2295(4) 0.6603(3) 0.0855(19) Uani 1 1 d . . . H46A H 0.1287 -0.2507 0.6341 0.103 Uiso 1 1 calc R . . C47 C 0.1879(4) -0.1481(4) 0.6592(3) 0.0751(17) Uani 1 1 d . . . C48 C 0.1030(6) -0.0912(5) 0.5784(3) 0.108(2) Uani 1 1 d . . . H48A H 0.0743 -0.1373 0.5652 0.129 Uiso 1 1 calc R . . C49 C 0.0983(6) -0.0175(6) 0.5571(4) 0.123(3) Uani 1 1 d . . . H49A H 0.0676 -0.0020 0.5251 0.147 Uiso 1 1 calc R . . C50 C 0.1475(5) 0.0336(4) 0.5910(3) 0.093(2) Uani 1 1 d . . . H50A H 0.1533 0.0899 0.5864 0.112 Uiso 1 1 calc R . . C51 C 0.1828(5) -0.3633(4) 0.7046(4) 0.097(2) Uani 1 1 d . . . C52 C 0.1646(6) -0.4343(4) 0.7046(4) 0.124(3) Uani 1 1 d . . . H52A H 0.1504 -0.4897 0.7047 0.149 Uiso 1 1 calc R . . B1 B 0.9747(7) 0.8286(5) 0.7825(4) 0.094(2) Uani 1 1 d . . . B2 B 0.4850(7) 0.7049(7) 0.7188(5) 0.109(3) Uani 1 1 d . . . B3 B -0.0468(6) 0.6862(5) 1.0260(4) 0.092(2) Uani 1 1 d . . . B4 B -0.0061(6) 0.1852(6) 0.9651(5) 0.098(3) Uani 1 1 d . . . F1 F 1.0520(7) 0.8400(7) 0.7951(6) 0.336(8) Uani 1 1 d . . . F2 F 0.9422(8) 0.8928(4) 0.7914(4) 0.303(7) Uani 1 1 d . . . F3 F 0.9479(4) 0.7646(3) 0.8129(3) 0.155(2) Uani 1 1 d . . . F4 F 0.9587(8) 0.8169(4) 0.7284(3) 0.244(5) Uani 1 1 d . . . F5 F 0.4596(5) 0.7711(4) 0.6948(4) 0.204(4) Uani 1 1 d . . . F6 F 0.4617(4) 0.6980(3) 0.7740(2) 0.1423(18) Uani 1 1 d . . . F7 F 0.4413(6) 0.6377(4) 0.7012(3) 0.199(3) Uani 1 1 d . . . F8 F 0.5662(4) 0.6857(4) 0.7051(4) 0.221(4) Uani 1 1 d . . . F9 F 0.0377(4) 0.6711(3) 1.0367(3) 0.166(2) Uani 1 1 d . . . F10 F -0.0703(4) 0.7533(3) 1.0573(3) 0.147(2) Uani 1 1 d . . . F11 F -0.0934(5) 0.6202(3) 1.0446(3) 0.176(3) Uani 1 1 d . . . F12 F -0.0612(4) 0.6927(3) 0.9698(3) 0.152(2) Uani 1 1 d . . . F13 F 0.0277(4) 0.2521(3) 0.9376(3) 0.147(2) Uani 1 1 d . . . F14 F 0.0210(7) 0.1784(4) 1.0180(4) 0.250(5) Uani 1 1 d . . . F15 F -0.0865(4) 0.1872(4) 0.9703(4) 0.202(3) Uani 1 1 d . . . F16 F 0.0199(6) 0.1169(4) 0.9418(3) 0.235(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0783(5) 0.0465(4) 0.0709(5) 0.0018(4) -0.0025(4) 0.0090(5) Fe2 0.0798(5) 0.0448(4) 0.0693(5) 0.0000(4) 0.0016(4) -0.0068(5) N1 0.090(3) 0.065(3) 0.078(3) -0.002(3) -0.010(3) 0.003(3) N2 0.084(3) 0.069(3) 0.070(3) 0.001(2) -0.012(3) 0.012(3) N3 0.070(3) 0.052(2) 0.080(3) -0.005(2) -0.006(3) 0.008(2) N4 0.093(4) 0.059(3) 0.090(4) 0.005(3) -0.003(3) -0.007(3) N5 0.078(3) 0.064(3) 0.087(4) 0.012(3) -0.002(3) 0.009(2) N6 0.082(3) 0.058(3) 0.076(3) -0.007(2) -0.004(3) -0.001(2) N7 0.082(3) 0.057(3) 0.094(4) 0.000(3) 0.009(3) -0.002(2) N8 0.070(3) 0.059(3) 0.067(3) 0.007(3) -0.006(2) 0.000(2) N9 0.112(4) 0.066(3) 0.072(3) 0.000(2) 0.022(3) 0.000(3) N10 0.096(3) 0.064(3) 0.083(3) 0.017(3) 0.004(3) 0.001(3) N11 0.082(3) 0.058(3) 0.076(3) 0.007(2) 0.006(3) -0.005(2) N12 0.086(3) 0.080(3) 0.073(3) -0.002(3) 0.017(3) 0.012(3) N13 0.069(3) 0.054(2) 0.079(3) -0.003(2) 0.002(3) 0.000(2) N14 0.085(3) 0.068(3) 0.075(3) -0.004(2) 0.016(3) 0.002(3) N15 0.092(3) 0.066(3) 0.077(3) -0.007(3) 0.005(3) -0.013(3) N16 0.079(3) 0.059(3) 0.079(3) -0.007(2) -0.004(3) -0.011(2) N17 0.083(3) 0.069(3) 0.077(3) 0.004(3) -0.010(3) 0.004(3) N18 0.082(3) 0.060(3) 0.068(3) -0.010(3) -0.012(3) -0.003(2) N19 0.105(4) 0.070(3) 0.075(3) 0.004(3) -0.017(3) -0.004(3) N20 0.096(3) 0.059(3) 0.072(3) 0.005(2) -0.008(3) -0.004(3) C1 0.095(5) 0.106(5) 0.096(5) -0.039(4) -0.012(4) -0.008(4) C2 0.120(6) 0.120(6) 0.106(6) -0.030(5) -0.044(5) 0.010(5) C3 0.116(6) 0.100(5) 0.081(5) 0.005(4) -0.018(4) 0.028(4) C4 0.081(4) 0.066(3) 0.078(4) 0.005(3) 0.010(3) 0.015(3) C5 0.094(5) 0.063(4) 0.101(5) 0.017(3) -0.003(4) 0.013(3) C6 0.086(4) 0.053(3) 0.110(5) -0.001(3) 0.024(4) 0.002(3) C7 0.087(4) 0.057(4) 0.110(6) 0.002(3) -0.009(4) -0.006(3) C8 0.077(4) 0.066(4) 0.072(4) 0.000(3) -0.005(3) -0.006(3) C9 0.107(5) 0.104(5) 0.074(4) 0.004(4) -0.017(4) -0.036(4) C10 0.099(5) 0.103(5) 0.093(5) 0.013(4) -0.010(4) -0.004(4) C11 0.078(4) 0.073(4) 0.101(5) 0.014(4) -0.005(4) 0.010(4) C12 0.111(6) 0.056(4) 0.151(7) 0.007(4) 0.012(5) 0.005(4) C13 0.148(8) 0.059(4) 0.179(9) 0.011(5) 0.011(7) 0.008(4) C14 0.105(5) 0.087(5) 0.080(4) -0.018(4) 0.005(4) 0.015(4) C15 0.118(6) 0.104(5) 0.085(5) -0.011(4) 0.032(5) 0.001(5) C16 0.104(5) 0.088(5) 0.094(5) -0.008(4) 0.023(4) -0.014(4) C17 0.073(4) 0.049(3) 0.079(4) -0.007(3) 0.001(3) -0.002(3) C18 0.086(4) 0.065(4) 0.111(6) 0.009(4) -0.012(5) -0.004(3) C19 0.073(4) 0.061(3) 0.111(5) -0.013(3) 0.004(4) 0.009(3) C20 0.079(4) 0.073(4) 0.093(4) -0.009(3) 0.004(4) 0.007(3) C21 0.067(4) 0.065(3) 0.078(4) -0.002(3) -0.001(3) 0.005(3) C22 0.117(6) 0.104(5) 0.090(5) -0.004(4) 0.023(5) 0.002(5) C23 0.154(7) 0.113(6) 0.098(6) 0.037(5) 0.031(5) 0.007(7) C24 0.121(6) 0.080(4) 0.101(5) 0.024(4) 0.009(5) -0.001(4) C25 0.089(5) 0.063(4) 0.141(6) -0.024(4) -0.009(5) 0.008(3) C26 0.103(6) 0.078(5) 0.181(9) -0.003(5) 0.018(6) 0.021(4) C27 0.091(4) 0.087(5) 0.083(4) 0.017(4) 0.007(4) -0.012(4) C28 0.092(5) 0.127(6) 0.091(5) 0.025(5) 0.033(4) -0.007(5) C29 0.089(5) 0.103(5) 0.101(5) -0.020(4) 0.021(4) 0.024(4) C30 0.071(4) 0.060(3) 0.088(4) 0.007(3) 0.004(3) -0.006(3) C31 0.083(5) 0.056(4) 0.122(6) -0.008(4) 0.007(4) 0.004(3) C32 0.079(4) 0.058(3) 0.094(5) 0.004(3) 0.001(4) -0.009(3) C33 0.078(4) 0.070(4) 0.089(4) 0.005(3) 0.004(3) -0.013(3) C34 0.071(4) 0.062(3) 0.059(3) -0.005(3) 0.017(3) -0.004(3) C35 0.109(6) 0.104(5) 0.082(5) 0.011(4) 0.024(4) 0.002(4) C36 0.130(6) 0.115(6) 0.099(5) -0.023(6) 0.024(5) 0.007(6) C37 0.119(6) 0.073(4) 0.081(4) -0.010(4) 0.015(4) -0.005(4) C38 0.106(5) 0.064(4) 0.135(7) -0.004(4) 0.010(5) -0.005(4) C39 0.143(8) 0.068(5) 0.157(8) 0.014(5) 0.031(6) 0.003(5) C40 0.095(4) 0.097(5) 0.083(4) -0.028(4) -0.010(4) -0.003(5) C41 0.125(7) 0.114(6) 0.119(7) -0.031(6) -0.025(6) 0.014(6) C42 0.120(6) 0.091(5) 0.088(5) 0.016(4) -0.030(5) 0.017(4) C43 0.077(4) 0.056(3) 0.083(4) 0.001(3) 0.001(3) 0.007(3) C44 0.089(5) 0.056(4) 0.102(5) 0.009(3) 0.003(4) 0.005(3) C45 0.087(5) 0.046(3) 0.128(6) -0.013(4) 0.011(4) -0.006(3) C46 0.095(5) 0.057(3) 0.104(5) -0.004(3) -0.005(4) -0.017(3) C47 0.085(4) 0.067(3) 0.073(4) -0.014(3) 0.007(3) -0.011(3) C48 0.132(7) 0.095(5) 0.097(5) -0.006(4) -0.034(5) -0.011(5) C49 0.149(7) 0.123(7) 0.096(5) 0.009(5) -0.050(5) -0.004(6) C50 0.118(6) 0.080(4) 0.082(4) 0.028(3) -0.015(4) -0.002(4) C51 0.091(5) 0.066(4) 0.134(6) -0.001(4) 0.003(5) -0.002(3) C52 0.134(7) 0.049(4) 0.191(9) 0.004(5) 0.029(7) -0.009(4) B1 0.112(7) 0.075(5) 0.095(6) 0.008(5) -0.004(5) -0.012(5) B2 0.103(7) 0.100(7) 0.124(8) 0.003(6) 0.026(6) 0.022(6) B3 0.117(7) 0.073(5) 0.087(6) 0.017(4) -0.005(5) 0.022(5) B4 0.078(6) 0.085(6) 0.132(8) 0.008(6) -0.004(6) 0.014(4) F1 0.249(10) 0.278(11) 0.481(18) 0.174(12) -0.158(12) -0.169(9) F2 0.496(16) 0.151(5) 0.263(8) 0.119(6) 0.230(10) 0.186(8) F3 0.159(5) 0.105(3) 0.202(6) 0.067(4) -0.025(4) -0.002(3) F4 0.451(15) 0.146(5) 0.136(5) 0.042(4) -0.048(7) -0.100(7) F5 0.212(7) 0.111(4) 0.289(9) 0.080(5) 0.104(7) 0.046(4) F6 0.175(5) 0.125(4) 0.127(4) 0.014(3) 0.030(4) -0.003(4) F7 0.288(10) 0.132(5) 0.177(6) -0.001(4) -0.024(6) -0.043(6) F8 0.162(5) 0.153(5) 0.347(11) 0.103(6) 0.121(7) 0.042(4) F9 0.133(4) 0.143(4) 0.222(7) -0.006(4) -0.059(4) 0.027(4) F10 0.150(5) 0.099(3) 0.191(6) -0.048(3) -0.019(4) 0.004(3) F11 0.254(7) 0.114(4) 0.161(5) 0.003(3) 0.025(5) -0.064(5) F12 0.197(6) 0.123(4) 0.137(4) 0.008(3) -0.048(4) 0.000(4) F13 0.147(4) 0.102(3) 0.192(5) 0.059(4) -0.024(4) -0.010(3) F14 0.376(13) 0.143(5) 0.232(8) 0.054(6) -0.124(9) -0.051(7) F15 0.137(5) 0.187(6) 0.281(10) -0.015(6) 0.054(6) -0.001(5) F16 0.346(10) 0.121(4) 0.239(7) -0.037(5) 0.176(8) 0.003(6) _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 1.941(4) . ? Fe1 N8 1.948(5) . ? Fe1 N5 1.960(5) . ? Fe1 N6 1.980(5) . ? Fe1 N10 1.982(5) . ? Fe1 N1 1.999(5) . ? Fe2 N13 1.907(4) . ? Fe2 N18 1.925(5) . ? Fe2 N11 1.991(5) . ? Fe2 N16 1.990(5) . ? Fe2 N15 1.990(5) . ? Fe2 N20 2.011(5) . ? N1 C1 1.324(8) . ? N1 N2 1.383(7) . ? N2 C3 1.362(8) . ? N2 C4 1.396(8) . ? N3 C4 1.310(7) . ? N3 C8 1.336(7) . ? N4 C9 1.320(8) . ? N4 N5 1.386(7) . ? N4 C8 1.427(8) . ? N5 C11 1.327(7) . ? N6 C14 1.316(8) . ? N6 N7 1.379(6) . ? N7 C16 1.316(8) . ? N7 C17 1.411(8) . ? N8 C21 1.288(7) . ? N8 C17 1.313(7) . ? N9 C22 1.356(9) . ? N9 N10 1.393(7) . ? N9 C21 1.413(8) . ? N10 C24 1.318(8) . ? N11 C27 1.310(8) . ? N11 N12 1.400(7) . ? N12 C29 1.359(8) . ? N12 C30 1.421(8) . ? N13 C30 1.338(7) . ? N13 C34 1.341(7) . ? N14 C35 1.357(8) . ? N14 N15 1.376(7) . ? N14 C34 1.409(7) . ? N15 C37 1.323(8) . ? N16 C40 1.322(8) . ? N16 N17 1.368(7) . ? N17 C42 1.378(8) . ? N17 C43 1.377(8) . ? N18 C43 1.356(8) . ? N18 C47 1.361(8) . ? N19 C48 1.343(9) . ? N19 N20 1.360(7) . ? N19 C47 1.383(8) . ? N20 C50 1.320(8) . ? C1 C2 1.412(11) . ? C2 C3 1.353(10) . ? C4 C5 1.373(8) . ? C5 C6 1.375(10) . ? C6 C7 1.383(10) . ? C6 C12 1.436(9) . ? C7 C8 1.367(8) . ? C9 C10 1.380(10) . ? C10 C11 1.394(9) . ? C12 C13 1.159(9) . ? C14 C15 1.383(10) . ? C15 C16 1.365(9) . ? C17 C18 1.363(8) . ? C18 C19 1.396(10) . ? C19 C20 1.424(9) . ? C19 C25 1.438(9) . ? C20 C21 1.342(8) . ? C22 C23 1.376(11) . ? C23 C24 1.428(11) . ? C25 C26 1.155(9) . ? C27 C28 1.379(10) . ? C28 C29 1.349(10) . ? C30 C31 1.393(8) . ? C31 C32 1.349(10) . ? C32 C33 1.402(9) . ? C32 C38 1.443(9) . ? C33 C34 1.379(8) . ? C35 C36 1.341(11) . ? C36 C37 1.396(10) . ? C38 C39 1.146(9) . ? C40 C41 1.393(11) . ? C41 C42 1.325(11) . ? C43 C44 1.359(8) . ? C44 C45 1.422(10) . ? C45 C46 1.363(10) . ? C45 C51 1.405(9) . ? C46 C47 1.365(8) . ? C48 C49 1.303(10) . ? C49 C50 1.387(10) . ? C51 C52 1.191(9) . ? B1 F2 1.182(11) . ? B1 F1 1.262(12) . ? B1 F4 1.312(11) . ? B1 F3 1.333(10) . ? B2 F5 1.282(12) . ? B2 F6 1.355(12) . ? B2 F8 1.352(11) . ? B2 F7 1.357(13) . ? B3 F12 1.346(10) . ? B3 F11 1.372(10) . ? B3 F10 1.369(9) . ? B3 F9 1.372(11) . ? B4 F15 1.267(10) . ? B4 F16 1.306(10) . ? B4 F14 1.322(12) . ? B4 F13 1.375(10) . ? 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 N8 176.9(2) . . ? N3 Fe1 N5 79.7(2) . . ? N8 Fe1 N5 101.86(19) . . ? N3 Fe1 N6 103.3(2) . . ? N8 Fe1 N6 79.4(2) . . ? N5 Fe1 N6 89.9(2) . . ? N3 Fe1 N10 97.9(2) . . ? N8 Fe1 N10 79.4(2) . . ? N5 Fe1 N10 95.3(2) . . ? N6 Fe1 N10 158.7(2) . . ? N3 Fe1 N1 79.0(2) . . ? N8 Fe1 N1 99.6(2) . . ? N5 Fe1 N1 158.5(2) . . ? N6 Fe1 N1 92.4(2) . . ? N10 Fe1 N1 90.2(2) . . ? N13 Fe2 N18 176.6(2) . . ? N13 Fe2 N11 79.3(2) . . ? N18 Fe2 N11 99.2(2) . . ? N13 Fe2 N16 104.2(2) . . ? N18 Fe2 N16 78.8(2) . . ? N11 Fe2 N16 89.3(2) . . ? N13 Fe2 N15 78.5(2) . . ? N18 Fe2 N15 103.0(2) . . ? N11 Fe2 N15 157.8(2) . . ? N16 Fe2 N15 94.2(2) . . ? N13 Fe2 N20 98.9(2) . . ? N18 Fe2 N20 78.1(2) . . ? N11 Fe2 N20 95.1(2) . . ? N16 Fe2 N20 156.9(2) . . ? N15 Fe2 N20 90.2(2) . . ? C1 N1 N2 105.9(6) . . ? C1 N1 Fe1 142.1(5) . . ? N2 N1 Fe1 111.9(4) . . ? C3 N2 N1 109.0(5) . . ? C3 N2 C4 133.6(6) . . ? N1 N2 C4 117.3(5) . . ? C4 N3 C8 120.0(5) . . ? C4 N3 Fe1 120.5(4) . . ? C8 N3 Fe1 119.5(4) . . ? C9 N4 N5 111.1(6) . . ? C9 N4 C8 133.6(6) . . ? N5 N4 C8 115.2(5) . . ? C11 N5 N4 103.0(5) . . ? C11 N5 Fe1 142.5(5) . . ? N4 N5 Fe1 114.4(4) . . ? C14 N6 N7 104.5(5) . . ? C14 N6 Fe1 141.5(5) . . ? N7 N6 Fe1 113.8(4) . . ? C16 N7 N6 110.0(5) . . ? C16 N7 C17 135.1(5) . . ? N6 N7 C17 114.8(5) . . ? C21 N8 C17 121.3(5) . . ? C21 N8 Fe1 120.0(4) . . ? C17 N8 Fe1 118.7(4) . . ? C22 N9 N10 110.9(5) . . ? C22 N9 C21 133.2(6) . . ? N10 N9 C21 115.8(5) . . ? C24 N10 N9 106.0(6) . . ? C24 N10 Fe1 141.4(5) . . ? N9 N10 Fe1 112.4(4) . . ? C27 N11 N12 104.9(5) . . ? C27 N11 Fe2 141.9(5) . . ? N12 N11 Fe2 113.1(4) . . ? C29 N12 N11 109.8(6) . . ? C29 N12 C30 134.8(6) . . ? N11 N12 C30 115.5(5) . . ? C30 N13 C34 116.5(5) . . ? C30 N13 Fe2 121.5(4) . . ? C34 N13 Fe2 121.6(4) . . ? C35 N14 N15 110.9(6) . . ? C35 N14 C34 133.1(6) . . ? N15 N14 C34 115.8(5) . . ? C37 N15 N14 104.8(5) . . ? C37 N15 Fe2 141.3(5) . . ? N14 N15 Fe2 113.9(4) . . ? C40 N16 N17 106.2(6) . . ? C40 N16 Fe2 141.2(5) . . ? N17 N16 Fe2 112.6(4) . . ? N16 N17 C42 109.2(6) . . ? N16 N17 C43 118.4(5) . . ? C42 N17 C43 132.3(6) . . ? C43 N18 C47 119.3(5) . . ? C43 N18 Fe2 120.4(4) . . ? C47 N18 Fe2 120.3(4) . . ? C48 N19 N20 109.9(6) . . ? C48 N19 C47 133.1(6) . . ? N20 N19 C47 116.9(5) . . ? C50 N20 N19 105.5(5) . . ? C50 N20 Fe2 140.5(5) . . ? N19 N20 Fe2 113.8(4) . . ? N1 C1 C2 111.2(7) . . ? C3 C2 C1 104.7(7) . . ? C2 C3 N2 109.2(6) . . ? N3 C4 C5 122.8(7) . . ? N3 C4 N2 111.2(5) . . ? C5 C4 N2 125.8(6) . . ? C6 C5 C4 117.0(7) . . ? C5 C6 C7 120.7(6) . . ? C5 C6 C12 119.1(7) . . ? C7 C6 C12 120.1(7) . . ? C8 C7 C6 117.8(7) . . ? N3 C8 C7 121.4(6) . . ? N3 C8 N4 111.1(5) . . ? C7 C8 N4 127.4(6) . . ? N4 C9 C10 109.6(7) . . ? C9 C10 C11 102.4(6) . . ? N5 C11 C10 113.9(6) . . ? C13 C12 C6 176.5(10) . . ? N6 C14 C15 112.3(6) . . ? C16 C15 C14 103.7(6) . . ? N7 C16 C15 109.4(7) . . ? N8 C17 C18 121.2(6) . . ? N8 C17 N7 113.2(5) . . ? C18 C17 N7 125.6(6) . . ? C17 C18 C19 118.1(7) . . ? C18 C19 C20 119.0(6) . . ? C18 C19 C25 120.1(7) . . ? C20 C19 C25 120.9(7) . . ? C21 C20 C19 116.0(6) . . ? N8 C21 C20 124.4(6) . . ? N8 C21 N9 112.3(5) . . ? C20 C21 N9 123.3(6) . . ? N9 C22 C23 106.8(7) . . ? C22 C23 C24 106.1(7) . . ? N10 C24 C23 110.1(7) . . ? C26 C25 C19 177.4(10) . . ? N11 C27 C28 111.3(6) . . ? C29 C28 C27 107.3(6) . . ? C28 C29 N12 106.7(6) . . ? N13 C30 C31 124.7(6) . . ? N13 C30 N12 110.3(5) . . ? C31 C30 N12 125.0(6) . . ? C32 C31 C30 115.9(7) . . ? C31 C32 C33 122.8(6) . . ? C31 C32 C38 118.3(6) . . ? C33 C32 C38 118.9(6) . . ? C34 C33 C32 115.6(6) . . ? N13 C34 C33 124.4(5) . . ? N13 C34 N14 109.9(5) . . ? C33 C34 N14 125.6(5) . . ? C36 C35 N14 106.7(7) . . ? C35 C36 C37 106.9(7) . . ? N15 C37 C36 110.6(6) . . ? C39 C38 C32 177.3(10) . . ? N16 C40 C41 110.0(7) . . ? C42 C41 C40 107.3(8) . . ? C41 C42 N17 107.3(7) . . ? N18 C43 C44 120.9(6) . . ? N18 C43 N17 109.6(5) . . ? C44 C43 N17 129.5(6) . . ? C43 C44 C45 119.8(7) . . ? C46 C45 C51 122.7(7) . . ? C46 C45 C44 118.3(6) . . ? C51 C45 C44 118.9(7) . . ? C47 C46 C45 119.9(7) . . ? N18 C47 C46 121.8(7) . . ? N18 C47 N19 110.7(5) . . ? C46 C47 N19 127.5(6) . . ? C49 C48 N19 107.9(7) . . ? C48 C49 C50 107.5(7) . . ? N20 C50 C49 109.1(6) . . ? C52 C51 C45 175.6(10) . . ? F2 B1 F1 104.0(11) . . ? F2 B1 F4 102.7(10) . . ? F1 B1 F4 115.6(12) . . ? F2 B1 F3 117.5(9) . . ? F1 B1 F3 107.0(9) . . ? F4 B1 F3 110.3(8) . . ? F5 B2 F6 114.2(9) . . ? F5 B2 F8 112.4(9) . . ? F6 B2 F8 117.7(10) . . ? F5 B2 F7 112.8(10) . . ? F6 B2 F7 95.2(9) . . ? F8 B2 F7 102.4(9) . . ? F12 B3 F11 106.6(8) . . ? F12 B3 F10 115.0(7) . . ? F11 B3 F10 108.1(8) . . ? F12 B3 F9 110.9(8) . . ? F11 B3 F9 108.4(7) . . ? F10 B3 F9 107.7(8) . . ? F15 B4 F16 112.0(10) . . ? F15 B4 F14 103.4(11) . . ? F16 B4 F14 103.0(9) . . ? F15 B4 F13 114.1(8) . . ? F16 B4 F13 111.0(9) . . ? F14 B4 F13 112.7(9) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 24.59 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.480 _refine_diff_density_min -0.390 _refine_diff_density_rms 0.056 # Attachment '1B_180 K.CIF' data_c:\alle\is018\abskorr\is-018 _database_code_depnum_ccdc_archive 'CCDC 846472' #TrackingRef '1B_180 K.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H18 B2 F8 Fe N10' _chemical_formula_weight 699.97 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 tetragonal _symmetry_space_group_name_H-M I4(1)/a _symmetry_Int_Tables_number 88 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 9.5513(14) _cell_length_b 9.5513(14) _cell_length_c 29.315(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2674.4(8) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 3184 _cell_measurement_theta_min 1.37 _cell_measurement_theta_max 26.09 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.738 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 0.661 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8170 _exptl_absorpt_correction_T_max 0.9113 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 0 -1 0.0880 1 0 1 0.1030 -1 0 1 0.1580 -1 0 -1 0.1680 0 -1 -1 0.1010 0 1 1 0.1210 0 -1 1 0.0840 0 1 -1 0.1100 _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 ; 460 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 11566 _diffrn_reflns_av_R_equivalents 0.0558 _diffrn_reflns_av_sigmaI/netI 0.0197 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 25.63 _reflns_number_total 1267 _reflns_number_gt 1223 _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^)+(0.0369P)^2^+2.5885P] 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 refall _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0026(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1267 _refine_ls_number_parameters 128 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0298 _refine_ls_R_factor_gt 0.0289 _refine_ls_wR_factor_ref 0.0756 _refine_ls_wR_factor_gt 0.0749 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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 0.0000 0.2500 0.1250 0.02773(18) Uani 1 4 d S . . N1 N 0.14271(14) 0.39560(14) 0.11365(4) 0.0306(3) Uani 1 1 d . . . N2 N 0.17747(14) 0.40349(14) 0.06800(4) 0.0315(3) Uani 1 1 d . . . N3 N 0.0000 0.2500 0.06083(6) 0.0286(4) Uani 1 2 d S . . C1 C 0.22539(18) 0.48785(18) 0.13382(6) 0.0353(4) Uani 1 1 d . . . H1 H 0.216(2) 0.502(2) 0.1663(8) 0.041(5) Uiso 1 1 d . . . C2 C 0.31378(19) 0.55357(19) 0.10235(6) 0.0389(4) Uani 1 1 d . . . H2 H 0.383(2) 0.622(2) 0.1075(7) 0.046(6) Uiso 1 1 d . . . C3 C 0.28171(18) 0.49877(18) 0.06089(6) 0.0352(4) Uani 1 1 d . . . H3 H 0.318(2) 0.515(2) 0.0312(7) 0.042(5) Uiso 1 1 d . . . C4 C 0.09358(16) 0.32720(17) 0.03794(5) 0.0299(3) Uani 1 1 d . . . C5 C 0.09999(18) 0.32879(18) -0.00889(6) 0.0330(4) Uani 1 1 d . . . H5 H 0.172(2) 0.379(2) -0.0236(6) 0.035(5) Uiso 1 1 d . . . C6 C 0.0000 0.2500 -0.03248(8) 0.0319(5) Uani 1 2 d S . . C7 C 0.0000 0.2500 -0.08139(8) 0.0354(5) Uani 1 2 d S . . C8 C 0.0000 0.2500 -0.12176(9) 0.0396(6) Uani 1 2 d S . . H8 H 0.0000 0.2500 -0.1530(13) 0.066(11) Uiso 1 2 d S . . B1 B 0.0000 0.7500 0.25572(9) 0.0346(6) Uani 1 2 d S . . F1 F -0.06520(11) 0.84951(12) 0.22800(4) 0.0454(3) Uani 1 1 d . . . F2 F -0.09826(12) 0.68357(12) 0.28297(4) 0.0484(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0284(2) 0.0284(2) 0.0264(3) 0.000 0.000 0.000 N1 0.0323(7) 0.0332(7) 0.0262(6) -0.0006(5) -0.0013(5) 0.0023(6) N2 0.0313(7) 0.0346(7) 0.0286(7) -0.0010(5) 0.0006(5) -0.0039(6) N3 0.0266(9) 0.0310(10) 0.0281(9) 0.000 0.000 -0.0021(7) C1 0.0354(9) 0.0333(9) 0.0371(9) -0.0042(7) -0.0062(7) 0.0007(7) C2 0.0345(9) 0.0341(9) 0.0482(10) -0.0039(8) -0.0044(7) -0.0043(7) C3 0.0320(8) 0.0339(9) 0.0399(10) 0.0016(7) 0.0016(7) -0.0053(7) C4 0.0280(8) 0.0315(8) 0.0302(8) -0.0002(6) -0.0005(6) -0.0003(6) C5 0.0315(8) 0.0379(9) 0.0297(8) 0.0027(7) 0.0029(6) -0.0007(7) C6 0.0315(11) 0.0362(12) 0.0280(11) 0.000 0.000 0.0051(9) C7 0.0322(12) 0.0414(13) 0.0328(13) 0.000 0.000 0.0013(10) C8 0.0408(14) 0.0502(15) 0.0277(13) 0.000 0.000 -0.0022(11) B1 0.0337(14) 0.0366(14) 0.0335(13) 0.000 0.000 0.0035(11) F1 0.0462(6) 0.0494(6) 0.0407(6) 0.0075(5) -0.0029(5) 0.0086(5) F2 0.0495(6) 0.0460(6) 0.0498(6) 0.0046(5) 0.0138(5) -0.0020(5) _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 1.8813(19) . ? Fe1 N3 1.8813(19) 15 ? Fe1 N1 1.9755(14) 6_454 ? Fe1 N1 1.9755(14) . ? Fe1 N1 1.9755(14) 15 ? Fe1 N1 1.9755(14) 12_666 ? N1 C1 1.323(2) . ? N1 N2 1.3810(19) . ? N2 C3 1.365(2) . ? N2 C4 1.396(2) . ? N3 C4 1.3388(18) 6_454 ? N3 C4 1.3388(18) . ? C1 C2 1.399(3) . ? C2 C3 1.358(3) . ? C4 C5 1.374(2) . ? C5 C6 1.399(2) . ? C6 C5 1.399(2) 6_454 ? C6 C7 1.434(3) . ? C7 C8 1.183(4) . ? B1 F2 1.3861(19) 6_464 ? B1 F2 1.3861(19) . ? B1 F1 1.3970(19) 6_464 ? B1 F1 1.3970(19) . ? 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 N3 180.0 . 15 ? N3 Fe1 N1 80.30(4) . 6_454 ? N3 Fe1 N1 99.70(4) 15 6_454 ? N3 Fe1 N1 80.31(4) . . ? N3 Fe1 N1 99.69(4) 15 . ? N1 Fe1 N1 160.61(8) 6_454 . ? N3 Fe1 N1 99.69(4) . 15 ? N3 Fe1 N1 80.31(4) 15 15 ? N1 Fe1 N1 91.625(13) 6_454 15 ? N1 Fe1 N1 91.625(13) . 15 ? N3 Fe1 N1 99.70(4) . 12_666 ? N3 Fe1 N1 80.31(4) 15 12_666 ? N1 Fe1 N1 91.625(13) 6_454 12_666 ? N1 Fe1 N1 91.625(13) . 12_666 ? N1 Fe1 N1 160.61(8) 15 12_666 ? C1 N1 N2 104.67(14) . . ? C1 N1 Fe1 143.67(12) . . ? N2 N1 Fe1 111.56(10) . . ? C3 N2 N1 111.09(13) . . ? C3 N2 C4 132.09(14) . . ? N1 N2 C4 116.43(13) . . ? C4 N3 C4 119.9(2) 6_454 . ? C4 N3 Fe1 120.07(10) 6_454 . ? C4 N3 Fe1 120.07(10) . . ? N1 C1 C2 111.36(16) . . ? C3 C2 C1 106.32(16) . . ? C2 C3 N2 106.55(16) . . ? N3 C4 C5 122.44(15) . . ? N3 C4 N2 110.76(14) . . ? C5 C4 N2 126.80(15) . . ? C4 C5 C6 117.22(16) . . ? C5 C6 C5 120.8(2) . 6_454 ? C5 C6 C7 119.62(11) . . ? C5 C6 C7 119.62(11) 6_454 . ? C8 C7 C6 180.0 . . ? F2 B1 F2 109.6(2) 6_464 . ? F2 B1 F1 110.17(7) 6_464 6_464 ? F2 B1 F1 109.00(7) . 6_464 ? F2 B1 F1 109.00(7) 6_464 . ? F2 B1 F1 110.17(7) . . ? F1 B1 F1 108.8(2) 6_464 . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.63 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.271 _refine_diff_density_min -0.373 _refine_diff_density_rms 0.042 # Attachment '1C_370 K.cif' data_d:\alle\is18_370\abskorr\is18-370 _database_code_depnum_ccdc_archive 'CCDC 846473' #TrackingRef '1C_370 K.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H18 B2 F8 Fe N10' _chemical_formula_weight 699.97 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 orthorhombic _symmetry_space_group_name_H-M Pbcn _symmetry_Int_Tables_number 60 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 16.726(3) _cell_length_b 12.202(2) _cell_length_c 15.212(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3104.6(11) _cell_formula_units_Z 4 _cell_measurement_temperature 370(2) _cell_measurement_reflns_used 1621 _cell_measurement_theta_min 2.07 _cell_measurement_theta_max 24.68 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.498 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 0.570 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8801 _exptl_absorpt_correction_T_max 0.9400 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -3 1 -1 0.1094 3 -1 1 0.1094 1 3 1 0.1272 -1 -3 -1 0.1272 -1 -1 3 0.0966 1 1 -3 0.0966 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 370(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 diameter, monocapillary' _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 2T' _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 100 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 7733 _diffrn_reflns_av_R_equivalents 0.0846 _diffrn_reflns_av_sigmaI/netI 0.0794 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 25.77 _reflns_number_total 2743 _reflns_number_gt 1166 _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^)+(0.1127P)^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 0.0063(18) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2743 _refine_ls_number_parameters 221 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1529 _refine_ls_R_factor_gt 0.0652 _refine_ls_wR_factor_ref 0.2137 _refine_ls_wR_factor_gt 0.1646 _refine_ls_goodness_of_fit_ref 0.937 _refine_ls_restrained_S_all 0.937 _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 0.5000 0.36312(9) 0.2500 0.0972(5) Uani 1 2 d S . . N1 N 0.5563(3) 0.2383(4) 0.3273(3) 0.1045(13) Uani 1 1 d . . . N2 N 0.6374(2) 0.2321(4) 0.3214(3) 0.1027(13) Uani 1 1 d . . . N3 N 0.6252(2) 0.3751(4) 0.2268(3) 0.0929(12) Uani 1 1 d . . . N4 N 0.5950(3) 0.5121(4) 0.1317(3) 0.1072(14) Uani 1 1 d . . . N5 N 0.5173(3) 0.4894(4) 0.1522(3) 0.1078(14) Uani 1 1 d . . . C1 C 0.5371(5) 0.1557(6) 0.3798(5) 0.127(2) Uani 1 1 d . . . H1A H 0.4849 0.1394 0.3963 0.153 Uiso 1 1 calc R . . C2 C 0.6026(5) 0.0967(6) 0.4072(5) 0.137(2) Uani 1 1 d . . . H2A H 0.6031 0.0352 0.4433 0.165 Uiso 1 1 calc R . . C3 C 0.6664(5) 0.1478(6) 0.3701(5) 0.130(2) Uani 1 1 d . . . H3A H 0.7199 0.1286 0.3769 0.156 Uiso 1 1 calc R . . C4 C 0.6759(3) 0.3077(5) 0.2663(3) 0.0961(15) Uani 1 1 d . . . C5 C 0.7575(3) 0.3114(6) 0.2541(4) 0.1107(17) Uani 1 1 d . . . H5A H 0.7916 0.2641 0.2840 0.133 Uiso 1 1 calc R . . C6 C 0.7867(3) 0.3887(6) 0.1955(4) 0.1110(18) Uani 1 1 d . . . C7 C 0.7343(3) 0.4606(5) 0.1526(4) 0.1083(17) Uani 1 1 d . . . H7A H 0.7527 0.5137 0.1137 0.130 Uiso 1 1 calc R . . C8 C 0.6552(3) 0.4490(5) 0.1708(3) 0.0953(15) Uani 1 1 d . . . C9 C 0.6008(5) 0.5994(6) 0.0752(5) 0.133(2) Uani 1 1 d . . . H9A H 0.6473 0.6298 0.0523 0.160 Uiso 1 1 calc R . . C10 C 0.5245(5) 0.6323(7) 0.0598(6) 0.149(3) Uani 1 1 d . . . H10A H 0.5085 0.6894 0.0235 0.179 Uiso 1 1 calc R . . C11 C 0.4754(4) 0.5645(7) 0.1087(5) 0.135(2) Uani 1 1 d . . . H11A H 0.4200 0.5707 0.1108 0.162 Uiso 1 1 calc R . . C12 C 0.8708(4) 0.3939(7) 0.1772(4) 0.137(3) Uani 1 1 d . . . C13 C 0.9380(4) 0.3924(8) 0.1599(5) 0.169(3) Uani 1 1 d . . . H13A H 0.9921 0.3912 0.1459 0.203 Uiso 1 1 calc R . . B1 B 0.8314(7) 0.7048(10) -0.0077(7) 0.143(3) Uiso 1 1 d . . . F1A F 0.7743(7) 0.6189(10) -0.0331(8) 0.132(4) Uiso 0.40 1 d P A 1 F2A F 0.8279(7) 0.6919(10) 0.0849(6) 0.122(3) Uiso 0.40 1 d P A 1 F3A F 0.8956(7) 0.6624(10) -0.0548(10) 0.111(3) Uiso 0.40 1 d P A 1 F4A F 0.8218(7) 0.8185(9) -0.0270(12) 0.112(3) Uiso 0.40 1 d P A 1 F1B F 0.7583(7) 0.6605(11) -0.0484(8) 0.099(4) Uiso 0.30 1 d P A 2 F2B F 0.8665(14) 0.728(2) 0.0716(13) 0.194(8) Uiso 0.30 1 d P A 2 F3B F 0.9018(8) 0.6399(11) -0.0141(11) 0.124(5) Uiso 0.30 1 d P A 2 F4B F 0.8317(10) 0.7891(16) -0.0658(12) 0.147(6) Uiso 0.30 1 d P A 2 F1C F 0.8522(15) 0.633(2) 0.0558(16) 0.207(8) Uiso 0.30 1 d P A 3 F2C F 0.8745(13) 0.6976(19) -0.0868(12) 0.173(8) Uiso 0.30 1 d P A 3 F3C F 0.7595(10) 0.6735(13) 0.0011(11) 0.143(5) Uiso 0.30 1 d P A 3 F4C F 0.8299(16) 0.809(2) 0.0102(18) 0.211(13) Uiso 0.30 1 d P A 3 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 0.0642(6) 0.1045(8) 0.1230(9) 0.000 0.0123(6) 0.000 N1 0.082(3) 0.119(4) 0.112(3) 0.012(3) 0.012(3) -0.004(3) N2 0.078(3) 0.113(4) 0.117(3) 0.015(3) -0.004(2) 0.000(2) N3 0.071(2) 0.108(3) 0.100(3) 0.006(2) 0.005(2) -0.005(2) N4 0.082(3) 0.106(4) 0.133(3) 0.019(3) 0.009(3) -0.002(2) N5 0.075(3) 0.107(3) 0.142(4) 0.017(3) 0.005(3) 0.011(2) C1 0.118(5) 0.126(6) 0.138(5) 0.011(4) 0.018(4) -0.014(4) C2 0.142(6) 0.115(5) 0.154(6) 0.033(4) -0.021(5) -0.012(5) C3 0.116(5) 0.126(5) 0.149(5) 0.027(4) -0.028(4) -0.001(4) C4 0.069(3) 0.115(4) 0.105(4) 0.002(3) -0.005(3) 0.000(3) C5 0.077(3) 0.137(5) 0.118(4) 0.007(4) -0.008(3) 0.003(3) C6 0.065(3) 0.152(6) 0.116(4) -0.002(4) 0.007(3) -0.009(3) C7 0.087(4) 0.117(4) 0.121(4) 0.007(3) 0.015(3) -0.008(3) C8 0.075(3) 0.108(4) 0.104(4) 0.001(3) 0.005(3) -0.005(3) C9 0.120(6) 0.111(5) 0.169(6) 0.037(4) 0.016(5) 0.002(4) C10 0.125(6) 0.125(6) 0.198(7) 0.043(5) 0.009(5) 0.019(5) C11 0.095(4) 0.143(6) 0.168(6) 0.035(5) 0.010(4) 0.017(4) C12 0.068(4) 0.211(8) 0.133(5) 0.006(4) 0.010(4) -0.014(4) C13 0.075(4) 0.237(9) 0.195(7) 0.028(6) 0.019(5) -0.007(5) _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 2.129(4) 4_655 ? Fe1 N3 2.129(4) . ? Fe1 N1 2.142(5) 4_655 ? Fe1 N1 2.142(5) . ? Fe1 N5 2.161(5) 4_655 ? Fe1 N5 2.161(5) . ? N1 C1 1.326(8) . ? N1 N2 1.362(5) . ? N2 C3 1.358(7) . ? N2 C4 1.402(7) . ? N3 C4 1.326(7) . ? N3 C8 1.337(6) . ? N4 N5 1.366(6) . ? N4 C9 1.371(8) . ? N4 C8 1.400(7) . ? N5 C11 1.331(8) . ? C1 C2 1.377(10) . ? C2 C3 1.359(10) . ? C4 C5 1.379(7) . ? C5 C6 1.388(8) . ? C6 C7 1.400(8) . ? C6 C12 1.436(8) . ? C7 C8 1.359(7) . ? C9 C10 1.358(10) . ? C10 C11 1.382(10) . ? C12 C13 1.155(9) . ? B1 F3C 1.268(15) . ? B1 F4C 1.30(3) . ? B1 F1C 1.35(2) . ? B1 F4B 1.356(17) . ? B1 F2B 1.37(2) . ? B1 F3A 1.390(14) . ? B1 F2C 1.405(19) . ? B1 F2A 1.418(14) . ? B1 F3B 1.423(17) . ? B1 F4A 1.427(16) . ? B1 F1A 1.469(16) . ? B1 F1B 1.472(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Fe1 N3 172.1(3) 4_655 . ? N3 Fe1 N1 72.99(17) 4_655 4_655 ? N3 Fe1 N1 112.99(17) . 4_655 ? N3 Fe1 N1 112.99(17) 4_655 . ? N3 Fe1 N1 72.99(17) . . ? N1 Fe1 N1 89.4(3) 4_655 . ? N3 Fe1 N5 72.82(17) 4_655 4_655 ? N3 Fe1 N5 101.37(16) . 4_655 ? N1 Fe1 N5 145.64(17) 4_655 4_655 ? N1 Fe1 N5 100.84(18) . 4_655 ? N3 Fe1 N5 101.37(16) 4_655 . ? N3 Fe1 N5 72.82(17) . . ? N1 Fe1 N5 100.84(18) 4_655 . ? N1 Fe1 N5 145.64(17) . . ? N5 Fe1 N5 89.1(3) 4_655 . ? C1 N1 N2 103.8(5) . . ? C1 N1 Fe1 139.8(5) . . ? N2 N1 Fe1 116.2(3) . . ? C3 N2 N1 111.3(5) . . ? C3 N2 C4 131.4(5) . . ? N1 N2 C4 117.3(4) . . ? C4 N3 C8 117.8(5) . . ? C4 N3 Fe1 120.7(4) . . ? C8 N3 Fe1 121.4(4) . . ? N5 N4 C9 111.6(5) . . ? N5 N4 C8 118.3(5) . . ? C9 N4 C8 130.0(5) . . ? C11 N5 N4 104.3(5) . . ? C11 N5 Fe1 139.7(4) . . ? N4 N5 Fe1 115.5(3) . . ? N1 C1 C2 112.8(7) . . ? C3 C2 C1 105.1(7) . . ? N2 C3 C2 107.1(7) . . ? N3 C4 C5 123.5(5) . . ? N3 C4 N2 112.7(4) . . ? C5 C4 N2 123.8(5) . . ? C4 C5 C6 117.2(5) . . ? C5 C6 C7 120.4(5) . . ? C5 C6 C12 119.9(6) . . ? C7 C6 C12 119.7(6) . . ? C8 C7 C6 116.7(5) . . ? N3 C8 C7 124.4(5) . . ? N3 C8 N4 111.8(5) . . ? C7 C8 N4 123.7(5) . . ? C10 C9 N4 105.7(6) . . ? C9 C10 C11 106.8(7) . . ? N5 C11 C10 111.5(7) . . ? C13 C12 C6 176.0(9) . . ? F3C B1 F4C 104.7(17) . . ? F3C B1 F1C 88.5(15) . . ? F4C B1 F1C 119.2(19) . . ? F4B B1 F2B 114.7(15) . . ? F3C B1 F2C 124.0(14) . . ? F4C B1 F2C 104.5(17) . . ? F1C B1 F2C 116.1(18) . . ? F3A B1 F2A 120.1(12) . . ? F4B B1 F3B 112.0(14) . . ? F2B B1 F3B 79.5(13) . . ? F3A B1 F4A 110.0(11) . . ? F2A B1 F4A 107.9(12) . . ? F3A B1 F1A 95.8(9) . . ? F2A B1 F1A 98.9(10) . . ? F4A B1 F1A 124.5(11) . . ? F4B B1 F1B 90.5(10) . . ? F2B B1 F1B 143.1(14) . . ? F3B B1 F1B 117.0(11) . . ? F4A B1 F1B 100.2(10) . . ? _diffrn_measured_fraction_theta_max 0.919 _diffrn_reflns_theta_full 25.77 _diffrn_measured_fraction_theta_full 0.919 _refine_diff_density_max 0.305 _refine_diff_density_min -0.213 _refine_diff_density_rms 0.046