Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_I _database_code_depnum_ccdc_archive 'CCDC 634174' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H30 B2 F8 Fe N14' _chemical_formula_weight 936.25 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 P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 10.691(2) _cell_length_b 13.868(3) _cell_length_c 28.711(6) _cell_angle_alpha 90.00 _cell_angle_beta 97.64(3) _cell_angle_gamma 90.00 _cell_volume 4219.2(15) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.474 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 0.443 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.4907 _exptl_absorpt_correction_T_max 0.8846 _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 22314 _diffrn_reflns_av_R_equivalents 0.0578 _diffrn_reflns_av_sigmaI/netI 0.0434 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.43 _diffrn_reflns_theta_max 25.71 _reflns_number_total 7918 _reflns_number_gt 6173 _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^)+(0.1163P)^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 0.0178(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7918 _refine_ls_number_parameters 626 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0679 _refine_ls_R_factor_gt 0.0564 _refine_ls_wR_factor_ref 0.1607 _refine_ls_wR_factor_gt 0.1528 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _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 0.38570(3) 0.72937(2) 0.624842(11) 0.04757(15) Uani 1 1 d . . . N1 N 0.3515(2) 0.65707(15) 0.68145(8) 0.0562(5) Uani 1 1 d . . . N2 N 0.3898(2) 0.56200(15) 0.68206(7) 0.0525(5) Uani 1 1 d . . . N3 N 0.4633(2) 0.60532(16) 0.61532(7) 0.0518(5) Uani 1 1 d . . . N4 N 0.5225(2) 0.67509(17) 0.55125(7) 0.0598(5) Uani 1 1 d . . . N5 N 0.4613(3) 0.75425(16) 0.56603(8) 0.0605(6) Uani 1 1 d . . . N6 N 0.8218(3) -0.0174(2) 0.56643(11) 0.0887(9) Uani 1 1 d . . . N7 N 0.5218(2) 0.80905(17) 0.66157(8) 0.0587(5) Uani 1 1 d . . . N8 N 0.4785(2) 0.89715(16) 0.67528(7) 0.0556(5) Uani 1 1 d . . . N9 N 0.2936(2) 0.84516(15) 0.63750(7) 0.0508(5) Uani 1 1 d . . . N10 N 0.1259(2) 0.77097(15) 0.59634(8) 0.0550(5) Uani 1 1 d . . . N11 N 0.2133(2) 0.70179(15) 0.58973(7) 0.0552(5) Uani 1 1 d . . . N12 N -0.2042(4) 1.3883(2) 0.70854(12) 0.0946(9) Uani 1 1 d . . . C1 C 0.2959(3) 0.6677(2) 0.71983(10) 0.0639(7) Uani 1 1 d . . . H1A H 0.2595 0.7260 0.7290 0.077 Uiso 1 1 calc R . . C2 C 0.2984(3) 0.5808(2) 0.74485(10) 0.0665(7) Uani 1 1 d . . . H2A H 0.2655 0.5699 0.7736 0.080 Uiso 1 1 calc R . . C3 C 0.3570(3) 0.5152(2) 0.72006(9) 0.0592(6) Uani 1 1 d . . . H3A H 0.3721 0.4493 0.7279 0.071 Uiso 1 1 calc R . . C4 C 0.4556(2) 0.53294(18) 0.64556(8) 0.0509(5) Uani 1 1 d . . . C5 C 0.5076(3) 0.4437(2) 0.64059(9) 0.0559(6) Uani 1 1 d . . . H5A H 0.5024 0.3943 0.6632 0.067 Uiso 1 1 calc R . . C6 C 0.5688(3) 0.4276(2) 0.60094(9) 0.0572(6) Uani 1 1 d . . . C7 C 0.5736(3) 0.5026(2) 0.56869(9) 0.0582(6) Uani 1 1 d . . . H7A H 0.6118 0.4932 0.5410 0.070 Uiso 1 1 calc R . . C8 C 0.5220(3) 0.58994(19) 0.57782(9) 0.0545(6) Uani 1 1 d . . . C9 C 0.5843(3) 0.6979(3) 0.51418(10) 0.0719(8) Uani 1 1 d . . . H9A H 0.6343 0.6563 0.4980 0.086 Uiso 1 1 calc R . . C10 C 0.5589(4) 0.7941(3) 0.50506(12) 0.0794(9) Uani 1 1 d . . . H10A H 0.5875 0.8316 0.4809 0.095 Uiso 1 1 calc R . . C11 C 0.4838(3) 0.8258(2) 0.53792(10) 0.0724(8) Uani 1 1 d . . . H11A H 0.4531 0.8898 0.5399 0.087 Uiso 1 1 calc R . . C12 C 0.6254(3) 0.3321(2) 0.59388(10) 0.0608(6) Uani 1 1 d . . . C13 C 0.5712(3) 0.2487(2) 0.60916(11) 0.0668(7) Uani 1 1 d . . . H13A H 0.4986 0.2535 0.6248 0.080 Uiso 1 1 calc R . . C14 C 0.6217(3) 0.1585(2) 0.60187(11) 0.0692(7) Uani 1 1 d . . . H14A H 0.5836 0.1019 0.6122 0.083 Uiso 1 1 calc R . . C15 C 0.7282(3) 0.1522(2) 0.57946(11) 0.0695(8) Uani 1 1 d . . . C16 C 0.7855(3) 0.2350(2) 0.56493(13) 0.0756(8) Uani 1 1 d . . . H16A H 0.8599 0.2302 0.5503 0.091 Uiso 1 1 calc R . . C17 C 0.7339(3) 0.3243(2) 0.57178(11) 0.0716(8) Uani 1 1 d . . . H17A H 0.7723 0.3808 0.5614 0.086 Uiso 1 1 calc R . . C18 C 0.7803(3) 0.0576(3) 0.57209(11) 0.0757(8) Uani 1 1 d . . . C19 C 0.6449(3) 0.8080(3) 0.67688(10) 0.0688(7) Uani 1 1 d . . . H19A H 0.7003 0.7560 0.6727 0.083 Uiso 1 1 calc R . . C20 C 0.6809(3) 0.8945(3) 0.69999(12) 0.0774(9) Uani 1 1 d . . . H20A H 0.7635 0.9114 0.7141 0.093 Uiso 1 1 calc R . . C21 C 0.5752(3) 0.9500(2) 0.69852(10) 0.0694(8) Uani 1 1 d . . . H21A H 0.5697 1.0129 0.7112 0.083 Uiso 1 1 calc R . . C22 C 0.3501(2) 0.91716(18) 0.66331(8) 0.0507(5) Uani 1 1 d . . . C23 C 0.2873(3) 0.99745(18) 0.67588(9) 0.0547(6) Uani 1 1 d . . . H23A H 0.3306 1.0477 0.6938 0.066 Uiso 1 1 calc R . . C24 C 0.1569(3) 1.00270(18) 0.66132(9) 0.0539(6) Uani 1 1 d . . . C25 C 0.0959(3) 0.92730(17) 0.63457(9) 0.0532(6) Uani 1 1 d . . . H25A H 0.0077 0.9289 0.6245 0.064 Uiso 1 1 calc R . . C26 C 0.1689(3) 0.85142(17) 0.62366(8) 0.0518(6) Uani 1 1 d . . . C27 C 0.0122(3) 0.7499(2) 0.57101(11) 0.0681(8) Uani 1 1 d . . . H27A H -0.0628 0.7871 0.5697 0.082 Uiso 1 1 calc R . . C28 C 0.0260(3) 0.6664(2) 0.54809(11) 0.0751(8) Uani 1 1 d . . . H28A H -0.0370 0.6333 0.5277 0.090 Uiso 1 1 calc R . . C29 C 0.1518(3) 0.6385(2) 0.56038(10) 0.0642(7) Uani 1 1 d . . . H29A H 0.1883 0.5820 0.5492 0.077 Uiso 1 1 calc R . . C30 C 0.0810(3) 1.08705(19) 0.67310(9) 0.0560(6) Uani 1 1 d . . . C31 C 0.1276(3) 1.1803(2) 0.67039(10) 0.0632(7) Uani 1 1 d . . . H31A H 0.2099 1.1903 0.6623 0.076 Uiso 1 1 calc R . . C32 C 0.0542(3) 1.2585(2) 0.67946(11) 0.0686(8) Uani 1 1 d . . . H32A H 0.0855 1.3222 0.6773 0.082 Uiso 1 1 calc R . . C33 C -0.0652(3) 1.2433(2) 0.69180(10) 0.0644(7) Uani 1 1 d . . . C34 C -0.1116(3) 1.1505(2) 0.69548(10) 0.0639(7) Uani 1 1 d . . . H34A H -0.1930 1.1404 0.7045 0.077 Uiso 1 1 calc R . . C35 C -0.0379(3) 1.0728(2) 0.68590(10) 0.0618(6) Uani 1 1 d . . . H35A H -0.0692 1.0091 0.6881 0.074 Uiso 1 1 calc R . . C36 C -0.1431(4) 1.3243(2) 0.70105(11) 0.0765(9) Uani 1 1 d . . . B1 B 0.1938(4) 0.3738(3) 0.57594(13) 0.0698(9) Uani 1 1 d . . . F1 F 0.0684(2) 0.35007(19) 0.56504(8) 0.1043(7) Uani 1 1 d . . . F2 F 0.2101(2) 0.42755(16) 0.61631(7) 0.0901(6) Uani 1 1 d . . . F3 F 0.2315(3) 0.42706(15) 0.53912(9) 0.1059(8) Uani 1 1 d . . . F4 F 0.2661(2) 0.29045(15) 0.58162(9) 0.0948(6) Uani 1 1 d . . . B2 B 0.0000 0.7920(4) 0.7500 0.0726(13) Uani 1 2 d S . . F5 F -0.0668(10) 0.7236(6) 0.7315(3) 0.169(5) Uani 0.50 1 d P . . F6 F -0.0595(12) 0.8610(10) 0.7661(4) 0.235(9) Uani 0.50 1 d P . . F7 F 0.0703(6) 0.7622(8) 0.7910(4) 0.197(6) Uani 0.50 1 d P . . F8 F 0.0885(10) 0.8316(10) 0.7292(4) 0.152(4) Uani 0.50 1 d P . . B3 B 0.5000 0.7820(3) 0.2500 0.0659(11) Uani 1 2 d S . . F9 F 0.5612(9) 0.7605(9) 0.2934(3) 0.180(5) Uani 0.50 1 d P . . F10 F 0.4730(9) 0.7045(4) 0.2273(3) 0.171(5) Uani 0.50 1 d P . . F11 F 0.5857(13) 0.8353(9) 0.2303(4) 0.124(4) Uani 0.50 1 d P . . F12 F 0.3999(12) 0.8348(10) 0.2574(5) 0.129(5) Uani 0.50 1 d P . . N13 N 0.3233(4) 1.0223(3) 0.56315(13) 0.1044(11) Uani 1 1 d . . . C37 C 0.2286(4) 1.0592(3) 0.55217(13) 0.0813(9) Uani 1 1 d . . . C38 C 0.1098(4) 1.1069(3) 0.53939(14) 0.0894(10) Uani 1 1 d . . . H38A H 0.1151 1.1730 0.5515 0.134 Uiso 1 1 calc R . . H38B H 0.0435 1.0719 0.5529 0.134 Uiso 1 1 calc R . . H38C H 0.0898 1.1083 0.5051 0.134 Uiso 1 1 calc R . . N14 N -0.2142(3) 0.6210(3) 0.62990(14) 0.1097(12) Uani 1 1 d . . . C39 C -0.1186(4) 0.5923(3) 0.64505(14) 0.0809(9) Uani 1 1 d . . . C40 C 0.0040(4) 0.5570(3) 0.66463(16) 0.0954(11) Uani 1 1 d . . . H40A H 0.0619 0.6115 0.6715 0.143 Uiso 1 1 calc R . . H40B H 0.0365 0.5139 0.6420 0.143 Uiso 1 1 calc R . . H40C H -0.0031 0.5216 0.6937 0.143 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0530(2) 0.0411(2) 0.0487(2) 0.00034(13) 0.00684(15) 0.00372(14) N1 0.0618(13) 0.0497(11) 0.0584(11) -0.0089(9) 0.0128(10) -0.0034(10) N2 0.0545(12) 0.0532(11) 0.0501(10) 0.0001(9) 0.0083(9) -0.0012(9) N3 0.0495(11) 0.0572(12) 0.0491(10) 0.0018(9) 0.0075(8) -0.0014(9) N4 0.0650(14) 0.0636(13) 0.0514(11) 0.0039(10) 0.0096(10) -0.0063(11) N5 0.0732(16) 0.0499(11) 0.0571(12) 0.0048(9) 0.0035(11) -0.0024(10) N6 0.085(2) 0.084(2) 0.0928(19) -0.0153(16) -0.0053(16) 0.0267(16) N7 0.0547(13) 0.0632(13) 0.0589(12) 0.0033(10) 0.0100(10) 0.0085(10) N8 0.0512(12) 0.0589(12) 0.0558(11) -0.0018(9) 0.0034(9) -0.0031(10) N9 0.0523(12) 0.0458(10) 0.0527(10) 0.0037(8) 0.0012(9) -0.0023(9) N10 0.0575(13) 0.0466(11) 0.0591(12) -0.0023(9) 0.0004(10) -0.0008(9) N11 0.0668(14) 0.0446(10) 0.0539(11) -0.0027(9) 0.0074(10) -0.0003(10) N12 0.107(2) 0.0763(19) 0.102(2) -0.0088(16) 0.0198(18) 0.0294(18) C1 0.0728(18) 0.0630(16) 0.0595(14) -0.0094(12) 0.0229(13) -0.0100(13) C2 0.0707(18) 0.0748(18) 0.0567(14) -0.0044(13) 0.0187(13) -0.0121(15) C3 0.0566(15) 0.0651(16) 0.0553(13) 0.0096(12) 0.0057(11) -0.0069(12) C4 0.0482(13) 0.0530(13) 0.0507(12) 0.0007(10) 0.0038(10) -0.0009(10) C5 0.0531(14) 0.0570(14) 0.0574(13) 0.0026(11) 0.0068(11) 0.0025(11) C6 0.0529(14) 0.0580(15) 0.0601(14) -0.0055(11) 0.0058(11) 0.0011(12) C7 0.0552(15) 0.0651(16) 0.0553(13) -0.0033(12) 0.0109(11) -0.0027(12) C8 0.0519(14) 0.0592(14) 0.0521(12) 0.0004(11) 0.0062(11) -0.0032(11) C9 0.0725(19) 0.088(2) 0.0570(15) 0.0015(14) 0.0155(14) -0.0127(16) C10 0.091(2) 0.082(2) 0.0658(17) 0.0149(15) 0.0122(16) -0.0213(18) C11 0.090(2) 0.0634(17) 0.0625(16) 0.0125(13) 0.0051(15) -0.0127(16) C12 0.0575(16) 0.0638(16) 0.0607(14) -0.0027(12) 0.0062(12) 0.0053(12) C13 0.0684(19) 0.0638(16) 0.0693(17) 0.0006(13) 0.0133(14) 0.0104(14) C14 0.0733(19) 0.0637(17) 0.0699(17) 0.0028(13) 0.0072(14) 0.0082(14) C15 0.0697(19) 0.0705(18) 0.0661(16) -0.0071(14) 0.0007(14) 0.0193(15) C16 0.0646(19) 0.080(2) 0.083(2) -0.0099(17) 0.0160(16) 0.0114(16) C17 0.0647(18) 0.0711(19) 0.0811(19) -0.0052(15) 0.0179(15) 0.0054(14) C18 0.075(2) 0.078(2) 0.0716(18) -0.0070(15) 0.0005(15) 0.0185(17) C19 0.0485(15) 0.091(2) 0.0664(16) 0.0047(15) 0.0066(13) 0.0015(14) C20 0.0512(16) 0.102(2) 0.0770(19) 0.0093(18) 0.0023(14) -0.0101(16) C21 0.0626(18) 0.0768(19) 0.0669(16) -0.0037(14) 0.0020(13) -0.0193(15) C22 0.0506(13) 0.0504(13) 0.0505(12) 0.0023(10) 0.0041(10) -0.0026(10) C23 0.0616(16) 0.0473(13) 0.0547(13) 0.0006(10) 0.0056(11) -0.0035(11) C24 0.0609(16) 0.0466(13) 0.0543(12) 0.0026(10) 0.0084(11) 0.0021(11) C25 0.0534(14) 0.0475(13) 0.0573(13) 0.0022(10) 0.0023(11) 0.0029(11) C26 0.0560(14) 0.0446(12) 0.0531(12) 0.0016(10) 0.0013(11) -0.0024(10) C27 0.0598(17) 0.0631(16) 0.0756(18) 0.0018(13) -0.0120(14) -0.0034(13) C28 0.081(2) 0.0645(17) 0.0746(18) -0.0067(14) -0.0098(16) -0.0130(15) C29 0.080(2) 0.0524(14) 0.0589(14) -0.0068(12) 0.0028(13) -0.0074(13) C30 0.0637(16) 0.0513(13) 0.0528(12) 0.0007(10) 0.0071(11) 0.0039(11) C31 0.0715(18) 0.0508(14) 0.0689(16) 0.0006(12) 0.0152(14) 0.0020(13) C32 0.083(2) 0.0505(15) 0.0726(17) -0.0023(13) 0.0118(16) 0.0042(14) C33 0.0739(19) 0.0597(15) 0.0589(15) -0.0040(12) 0.0059(13) 0.0162(14) C34 0.0643(17) 0.0656(16) 0.0621(14) -0.0020(12) 0.0098(13) 0.0063(13) C35 0.0661(17) 0.0556(15) 0.0648(15) 0.0003(12) 0.0126(13) 0.0018(13) C36 0.092(2) 0.0682(19) 0.0696(17) -0.0061(14) 0.0105(16) 0.0177(17) B1 0.075(2) 0.0614(19) 0.074(2) -0.0113(16) 0.0115(17) 0.0023(17) F1 0.0793(14) 0.1232(18) 0.1048(15) -0.0176(14) -0.0090(12) -0.0057(13) F2 0.0828(13) 0.0984(14) 0.0882(12) -0.0327(11) 0.0082(10) -0.0063(11) F3 0.149(2) 0.0668(12) 0.1126(16) 0.0054(11) 0.0564(15) 0.0218(13) F4 0.1046(16) 0.0688(11) 0.1129(16) 0.0015(11) 0.0212(13) 0.0146(11) B2 0.056(3) 0.063(3) 0.099(4) 0.000 0.010(3) 0.000 F5 0.233(11) 0.142(6) 0.150(8) -0.054(5) 0.095(7) -0.116(7) F6 0.263(17) 0.227(11) 0.179(11) -0.150(10) -0.099(9) 0.153(11) F7 0.080(4) 0.274(12) 0.213(9) 0.174(9) -0.066(5) -0.066(6) F8 0.124(6) 0.160(8) 0.192(9) 0.034(6) 0.099(6) -0.011(5) B3 0.074(3) 0.054(2) 0.070(3) 0.000 0.012(2) 0.000 F9 0.100(5) 0.341(14) 0.091(4) 0.075(7) -0.014(3) -0.004(8) F10 0.191(11) 0.106(4) 0.244(12) -0.120(6) 0.132(10) -0.092(6) F11 0.168(11) 0.078(5) 0.141(6) 0.038(5) 0.083(7) -0.013(5) F12 0.081(4) 0.096(7) 0.207(11) 0.025(6) 0.005(6) 0.032(4) N13 0.116(3) 0.097(2) 0.108(2) 0.033(2) 0.043(2) 0.013(2) C37 0.094(3) 0.071(2) 0.083(2) 0.0143(17) 0.0283(19) 0.0008(19) C38 0.094(3) 0.084(2) 0.089(2) -0.0037(19) 0.007(2) 0.003(2) N14 0.069(2) 0.125(3) 0.131(3) -0.034(2) -0.003(2) -0.001(2) C39 0.072(2) 0.077(2) 0.096(2) -0.0193(18) 0.0181(18) -0.0094(17) C40 0.075(2) 0.086(2) 0.126(3) 0.005(2) 0.020(2) 0.0118(19) _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 1.943(2) . ? Fe1 N3 1.945(2) . ? Fe1 N1 1.985(2) . ? Fe1 N5 1.996(2) . ? Fe1 N7 2.011(3) . ? Fe1 N11 2.017(2) . ? N1 C1 1.328(3) . ? N1 N2 1.380(3) . ? N2 C3 1.355(3) . ? N2 C4 1.397(3) . ? N3 C8 1.333(3) . ? N3 C4 1.337(3) . ? N4 C9 1.362(4) . ? N4 N5 1.374(3) . ? N4 C8 1.406(3) . ? N5 C11 1.322(4) . ? N6 C18 1.150(4) . ? N7 C19 1.331(4) . ? N7 N8 1.382(3) . ? N8 C21 1.366(4) . ? N8 C22 1.398(3) . ? N9 C22 1.339(3) . ? N9 C26 1.342(3) . ? N10 C27 1.362(4) . ? N10 N11 1.370(3) . ? N10 C26 1.406(3) . ? N11 C29 1.328(3) . ? N12 C36 1.140(4) . ? C1 C2 1.401(4) . ? C2 C3 1.359(4) . ? C4 C5 1.373(4) . ? C5 C6 1.404(4) . ? C6 C7 1.397(4) . ? C6 C12 1.481(4) . ? C7 C8 1.371(4) . ? C9 C10 1.379(5) . ? C10 C11 1.389(5) . ? C12 C13 1.391(4) . ? C12 C17 1.398(4) . ? C13 C14 1.389(4) . ? C14 C15 1.383(5) . ? C15 C16 1.392(5) . ? C15 C18 1.451(4) . ? C16 C17 1.380(4) . ? C19 C20 1.400(5) . ? C20 C21 1.364(5) . ? C22 C23 1.373(4) . ? C23 C24 1.403(4) . ? C24 C25 1.405(4) . ? C24 C30 1.488(4) . ? C25 C26 1.371(4) . ? C27 C28 1.350(4) . ? C28 C29 1.398(5) . ? C30 C35 1.384(4) . ? C30 C31 1.392(4) . ? C31 C32 1.382(4) . ? C32 C33 1.386(5) . ? C33 C34 1.388(4) . ? C33 C36 1.444(4) . ? C34 C35 1.384(4) . ? B1 F2 1.370(4) . ? B1 F1 1.375(4) . ? B1 F4 1.388(4) . ? B1 F3 1.393(4) . ? B2 F5 1.262(9) . ? B2 F5 1.262(8) 2_556 ? B2 F6 1.270(11) . ? B2 F6 1.270(11) 2_556 ? B2 F8 1.305(8) . ? B2 F8 1.305(8) 2_556 ? B2 F7 1.374(7) 2_556 ? B2 F7 1.374(7) . ? F5 F7 0.837(16) 2_556 ? F5 F5 1.66(2) 2_556 ? F6 F8 0.54(2) 2_556 ? F6 F6 1.67(3) 2_556 ? F7 F5 0.837(16) 2_556 ? F8 F6 0.54(2) 2_556 ? B3 F10 1.269(6) . ? B3 F10 1.269(6) 2_655 ? B3 F12 1.338(10) . ? B3 F12 1.338(10) 2_655 ? B3 F11 1.358(9) . ? B3 F11 1.358(9) 2_655 ? B3 F9 1.362(7) 2_655 ? B3 F9 1.362(7) . ? F9 F10 1.017(12) 2_655 ? F10 F9 1.017(12) 2_655 ? F10 F10 1.351(19) 2_655 ? F11 F12 0.37(2) 2_655 ? F12 F11 0.37(2) 2_655 ? N13 C37 1.140(5) . ? C37 C38 1.435(6) . ? N14 C39 1.129(5) . ? C39 C40 1.441(6) . ? 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 173.47(9) . . ? N9 Fe1 N1 96.39(9) . . ? N3 Fe1 N1 78.26(9) . . ? N9 Fe1 N5 106.71(9) . . ? N3 Fe1 N5 78.81(9) . . ? N1 Fe1 N5 156.82(9) . . ? N9 Fe1 N7 78.30(9) . . ? N3 Fe1 N7 105.51(9) . . ? N1 Fe1 N7 92.71(9) . . ? N5 Fe1 N7 90.15(10) . . ? N9 Fe1 N11 78.34(9) . . ? N3 Fe1 N11 98.08(9) . . ? N1 Fe1 N11 93.32(9) . . ? N5 Fe1 N11 93.20(10) . . ? N7 Fe1 N11 156.37(9) . . ? C1 N1 N2 105.1(2) . . ? C1 N1 Fe1 140.8(2) . . ? N2 N1 Fe1 113.98(15) . . ? C3 N2 N1 111.1(2) . . ? C3 N2 C4 132.5(2) . . ? N1 N2 C4 116.4(2) . . ? C8 N3 C4 118.7(2) . . ? C8 N3 Fe1 120.68(18) . . ? C4 N3 Fe1 120.58(17) . . ? C9 N4 N5 110.9(2) . . ? C9 N4 C8 131.0(3) . . ? N5 N4 C8 117.8(2) . . ? C11 N5 N4 106.2(2) . . ? C11 N5 Fe1 140.7(2) . . ? N4 N5 Fe1 112.72(16) . . ? C19 N7 N8 105.7(2) . . ? C19 N7 Fe1 141.4(2) . . ? N8 N7 Fe1 112.88(16) . . ? C21 N8 N7 110.7(2) . . ? C21 N8 C22 131.9(3) . . ? N7 N8 C22 117.4(2) . . ? C22 N9 C26 118.2(2) . . ? C22 N9 Fe1 121.16(18) . . ? C26 N9 Fe1 120.41(16) . . ? C27 N10 N11 110.6(2) . . ? C27 N10 C26 132.1(2) . . ? N11 N10 C26 117.1(2) . . ? C29 N11 N10 105.1(2) . . ? C29 N11 Fe1 141.7(2) . . ? N10 N11 Fe1 113.13(16) . . ? N1 C1 C2 110.5(3) . . ? C3 C2 C1 106.6(2) . . ? N2 C3 C2 106.7(3) . . ? N3 C4 C5 123.3(2) . . ? N3 C4 N2 110.5(2) . . ? C5 C4 N2 126.1(2) . . ? C4 C5 C6 117.8(2) . . ? C7 C6 C5 118.8(2) . . ? C7 C6 C12 121.5(2) . . ? C5 C6 C12 119.7(2) . . ? C8 C7 C6 118.7(2) . . ? N3 C8 C7 122.7(2) . . ? N3 C8 N4 109.9(2) . . ? C7 C8 N4 127.4(2) . . ? N4 C9 C10 105.6(3) . . ? C9 C10 C11 107.1(3) . . ? N5 C11 C10 110.2(3) . . ? C13 C12 C17 118.9(3) . . ? C13 C12 C6 120.4(3) . . ? C17 C12 C6 120.7(3) . . ? C14 C13 C12 121.0(3) . . ? C15 C14 C13 119.2(3) . . ? C14 C15 C16 120.6(3) . . ? C14 C15 C18 118.7(3) . . ? C16 C15 C18 120.7(3) . . ? C17 C16 C15 119.9(3) . . ? C16 C17 C12 120.4(3) . . ? N6 C18 C15 179.7(4) . . ? N7 C19 C20 110.1(3) . . ? C21 C20 C19 107.1(3) . . ? C20 C21 N8 106.4(3) . . ? N9 C22 C23 123.4(2) . . ? N9 C22 N8 110.1(2) . . ? C23 C22 N8 126.5(2) . . ? C22 C23 C24 117.7(2) . . ? C23 C24 C25 119.6(2) . . ? C23 C24 C30 121.5(2) . . ? C25 C24 C30 118.8(2) . . ? C26 C25 C24 117.3(2) . . ? N9 C26 C25 123.7(2) . . ? N9 C26 N10 110.6(2) . . ? C25 C26 N10 125.7(2) . . ? C28 C27 N10 107.3(3) . . ? C27 C28 C29 106.1(3) . . ? N11 C29 C28 110.9(3) . . ? C35 C30 C31 119.7(3) . . ? C35 C30 C24 119.7(2) . . ? C31 C30 C24 120.6(3) . . ? C32 C31 C30 120.1(3) . . ? C31 C32 C33 119.6(3) . . ? C32 C33 C34 120.8(3) . . ? C32 C33 C36 120.1(3) . . ? C34 C33 C36 119.1(3) . . ? C35 C34 C33 119.2(3) . . ? C34 C35 C30 120.6(3) . . ? N12 C36 C33 179.7(4) . . ? F2 B1 F1 109.5(3) . . ? F2 B1 F4 110.3(3) . . ? F1 B1 F4 109.8(3) . . ? F2 B1 F3 109.7(3) . . ? F1 B1 F3 109.0(3) . . ? F4 B1 F3 108.5(3) . . ? F5 B2 F5 82.4(11) . 2_556 ? F5 B2 F6 115.9(8) . . ? F5 B2 F6 134.2(7) 2_556 . ? F5 B2 F6 134.2(7) . 2_556 ? F5 B2 F6 115.9(8) 2_556 2_556 ? F6 B2 F6 82.2(16) . 2_556 ? F5 B2 F8 121.8(8) . . ? F5 B2 F8 96.0(7) 2_556 . ? F6 B2 F8 106.2(9) . . ? F6 B2 F8 24.2(11) 2_556 . ? F5 B2 F8 96.0(7) . 2_556 ? F5 B2 F8 121.8(8) 2_556 2_556 ? F6 B2 F8 24.2(11) . 2_556 ? F6 B2 F8 106.2(9) 2_556 2_556 ? F8 B2 F8 130.3(12) . 2_556 ? F5 B2 F7 36.7(7) . 2_556 ? F5 B2 F7 110.4(7) 2_556 2_556 ? F6 B2 F7 107.1(6) . 2_556 ? F6 B2 F7 99.1(8) 2_556 2_556 ? F8 B2 F7 94.6(8) . 2_556 ? F8 B2 F7 99.9(7) 2_556 2_556 ? F5 B2 F7 110.4(7) . . ? F5 B2 F7 36.7(7) 2_556 . ? F6 B2 F7 99.1(8) . . ? F6 B2 F7 107.1(6) 2_556 . ? F8 B2 F7 99.9(7) . . ? F8 B2 F7 94.6(8) 2_556 . ? F7 B2 F7 145.0(11) 2_556 . ? F7 F5 B2 78.9(9) 2_556 . ? F7 F5 F5 116.0(12) 2_556 2_556 ? B2 F5 F5 48.8(6) . 2_556 ? F8 F6 B2 82(2) 2_556 . ? F8 F6 F6 130.0(19) 2_556 2_556 ? B2 F6 F6 48.9(8) . 2_556 ? F5 F7 B2 64.4(9) 2_556 . ? F6 F8 B2 74.3(17) 2_556 . ? F10 B3 F10 64.4(10) . 2_655 ? F10 B3 F12 114.4(8) . . ? F10 B3 F12 121.0(8) 2_655 . ? F10 B3 F12 121.0(8) . 2_655 ? F10 B3 F12 114.4(8) 2_655 2_655 ? F12 B3 F12 113.6(14) . 2_655 ? F10 B3 F11 111.6(7) . . ? F10 B3 F11 123.6(8) 2_655 . ? F12 B3 F11 111.5(5) . . ? F12 B3 F11 15.6(10) 2_655 . ? F10 B3 F11 123.6(8) . 2_655 ? F10 B3 F11 111.6(7) 2_655 2_655 ? F12 B3 F11 15.6(10) . 2_655 ? F12 B3 F11 111.5(5) 2_655 2_655 ? F11 B3 F11 114.0(14) . 2_655 ? F10 B3 F9 45.3(5) . 2_655 ? F10 B3 F9 109.5(9) 2_655 2_655 ? F12 B3 F9 88.2(8) . 2_655 ? F12 B3 F9 105.8(8) 2_655 2_655 ? F11 B3 F9 90.4(8) . 2_655 ? F11 B3 F9 103.4(7) 2_655 2_655 ? F10 B3 F9 109.5(9) . . ? F10 B3 F9 45.3(5) 2_655 . ? F12 B3 F9 105.8(8) . . ? F12 B3 F9 88.2(8) 2_655 . ? F11 B3 F9 103.4(7) . . ? F11 B3 F9 90.4(8) 2_655 . ? F9 B3 F9 154.8(11) 2_655 . ? F10 F9 B3 62.5(5) 2_655 . ? F9 F10 B3 72.2(6) 2_655 . ? F9 F10 F10 129.7(7) 2_655 2_655 ? B3 F10 F10 57.8(5) . 2_655 ? F12 F11 B3 79(3) 2_655 . ? F11 F12 B3 85(3) 2_655 . ? N13 C37 C38 178.6(5) . . ? N14 C39 C40 179.2(5) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.71 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.498 _refine_diff_density_min -0.476 _refine_diff_density_rms 0.070 data_II _database_code_depnum_ccdc_archive 'CCDC 634175' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H30 B2 F8 Fe N14' _chemical_formula_weight 936.25 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 Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 19.503(4) _cell_length_b 19.129(4) _cell_length_c 11.409(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4256.3(15) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description coffin _exptl_crystal_colour red _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.461 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 0.439 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8797 _exptl_absorpt_correction_T_max 0.9380 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 1 -1 0.0950 -1 1 0 0.1820 1 -1 0 0.1960 0 -1 -1 0.1250 0 -1 1 0.1180 0 1 1 0.1160 1 1 0 0.1970 -1 -1 0 0.2180 _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 29710 _diffrn_reflns_av_R_equivalents 0.0372 _diffrn_reflns_av_sigmaI/netI 0.0246 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 25.66 _reflns_number_total 7938 _reflns_number_gt 7295 _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^)+(0.1132P)^2^+0.3112P] 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 0.0219(16) _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 0.011(16) _refine_ls_number_reflns 7938 _refine_ls_number_parameters 550 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0545 _refine_ls_R_factor_gt 0.0514 _refine_ls_wR_factor_ref 0.1460 _refine_ls_wR_factor_gt 0.1429 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 0.84767(2) 0.27680(2) -0.01590(5) 0.04766(15) Uani 1 1 d . . . N1 N 0.80404(14) 0.19856(16) 0.0666(2) 0.0520(6) Uani 1 1 d . . . N2 N 0.74367(14) 0.17697(15) 0.0144(2) 0.0520(6) Uani 1 1 d . . . N3 N 0.77072(14) 0.26220(14) -0.1137(2) 0.0488(6) Uani 1 1 d . . . N4 N 0.81475(14) 0.35101(15) -0.2193(3) 0.0511(6) Uani 1 1 d . . . N5 N 0.86318(14) 0.35047(15) -0.1314(3) 0.0531(6) Uani 1 1 d . . . N6 N 0.3614(2) 0.2292(3) -0.5771(5) 0.1061(18) Uani 1 1 d . . . N7 N 0.80814(14) 0.34439(17) 0.0937(3) 0.0579(7) Uani 1 1 d . . . N8 N 0.85343(15) 0.36725(17) 0.1764(3) 0.0583(7) Uani 1 1 d . . . N9 N 0.92388(13) 0.29257(13) 0.0819(2) 0.0473(6) Uani 1 1 d . . . N10 N 0.97707(14) 0.21435(13) -0.0327(3) 0.0473(6) Uani 1 1 d . . . N11 N 0.91469(14) 0.21471(15) -0.0904(3) 0.0507(6) Uani 1 1 d . . . N12 N 1.2964(2) 0.3600(3) 0.6207(4) 0.0925(13) Uani 1 1 d . . . C1 C 0.81170(19) 0.15587(19) 0.1592(3) 0.0563(8) Uani 1 1 d . . . H1A H 0.8489 0.1579 0.2128 0.068 Uiso 1 1 calc R . . C2 C 0.75739(19) 0.1078(2) 0.1660(3) 0.0592(8) Uani 1 1 d . . . H2A H 0.7513 0.0724 0.2234 0.071 Uiso 1 1 calc R . . C3 C 0.71492(18) 0.12241(19) 0.0731(3) 0.0560(7) Uani 1 1 d . . . H3A H 0.6735 0.0990 0.0536 0.067 Uiso 1 1 calc R . . C4 C 0.72405(17) 0.21343(17) -0.0877(3) 0.0492(7) Uani 1 1 d . . . C5 C 0.66527(17) 0.20302(19) -0.1520(3) 0.0522(7) Uani 1 1 d . . . H5A H 0.6324 0.1687 -0.1303 0.063 Uiso 1 1 calc R . . C6 C 0.65598(16) 0.24587(18) -0.2525(3) 0.0504(7) Uani 1 1 d . . . C7 C 0.70599(17) 0.29496(18) -0.2808(3) 0.0508(7) Uani 1 1 d . . . H7A H 0.7016 0.3231 -0.3491 0.061 Uiso 1 1 calc R . . C8 C 0.76210(17) 0.30205(17) -0.2077(3) 0.0503(7) Uani 1 1 d . . . C9 C 0.8262(2) 0.4045(2) -0.2957(4) 0.0604(8) Uani 1 1 d . . . H9A H 0.8000 0.4153 -0.3635 0.072 Uiso 1 1 calc R . . C10 C 0.8826(2) 0.4397(2) -0.2558(4) 0.0659(9) Uani 1 1 d . . . H10A H 0.9032 0.4797 -0.2901 0.079 Uiso 1 1 calc R . . C11 C 0.9039(2) 0.4048(2) -0.1539(4) 0.0632(9) Uani 1 1 d . . . H11A H 0.9421 0.4180 -0.1074 0.076 Uiso 1 1 calc R . . C12 C 0.59333(16) 0.23978(18) -0.3252(3) 0.0518(7) Uani 1 1 d . . . C13 C 0.5729(2) 0.2950(2) -0.3963(4) 0.0673(10) Uani 1 1 d . . . H13A H 0.6010 0.3355 -0.4010 0.081 Uiso 1 1 calc R . . C14 C 0.5127(2) 0.2925(3) -0.4606(4) 0.0719(10) Uani 1 1 d . . . H14A H 0.4990 0.3314 -0.5067 0.086 Uiso 1 1 calc R . . C15 C 0.47329(18) 0.2336(2) -0.4573(3) 0.0621(9) Uani 1 1 d . . . C16 C 0.4940(2) 0.1763(3) -0.3913(4) 0.0737(11) Uani 1 1 d . . . H16A H 0.4676 0.1345 -0.3920 0.088 Uiso 1 1 calc R . . C17 C 0.5534(2) 0.1801(2) -0.3243(4) 0.0656(9) Uani 1 1 d . . . H17A H 0.5667 0.1413 -0.2775 0.079 Uiso 1 1 calc R . . C18 C 0.4102(2) 0.2308(3) -0.5229(5) 0.0808(12) Uani 1 1 d . . . C19 C 0.7503(2) 0.3782(2) 0.1170(4) 0.0719(11) Uani 1 1 d . . . H19A H 0.7092 0.3736 0.0728 0.086 Uiso 1 1 calc R . . C20 C 0.7575(3) 0.4215(3) 0.2147(5) 0.0945(16) Uani 1 1 d . . . H20A H 0.7235 0.4511 0.2479 0.113 Uiso 1 1 calc R . . C21 C 0.8239(2) 0.4128(3) 0.2533(4) 0.0789(13) Uani 1 1 d . . . H21A H 0.8447 0.4341 0.3196 0.095 Uiso 1 1 calc R . . C22 C 0.91973(17) 0.33825(17) 0.1729(3) 0.0518(7) Uani 1 1 d . . . C23 C 0.97348(17) 0.35129(17) 0.2457(3) 0.0524(7) Uani 1 1 d . . . H23A H 0.9696 0.3847 0.3069 0.063 Uiso 1 1 calc R . . C24 C 1.03492(16) 0.31436(15) 0.2283(3) 0.0457(6) Uani 1 1 d . . . C25 C 1.03949(16) 0.26759(15) 0.1336(3) 0.0467(6) Uani 1 1 d . . . H25A H 1.0807 0.2428 0.1183 0.056 Uiso 1 1 calc R . . C26 C 0.98263(16) 0.25873(16) 0.0639(3) 0.0453(6) Uani 1 1 d . . . C27 C 1.02119(18) 0.16706(18) -0.0827(3) 0.0544(7) Uani 1 1 d . . . H27A H 1.0670 0.1573 -0.0593 0.065 Uiso 1 1 calc R . . C28 C 0.9861(2) 0.1371(2) -0.1721(3) 0.0612(8) Uani 1 1 d . . . H28A H 1.0027 0.1018 -0.2233 0.073 Uiso 1 1 calc R . . C29 C 0.92146(19) 0.16739(19) -0.1755(3) 0.0566(8) Uani 1 1 d . . . H29A H 0.8868 0.1560 -0.2308 0.068 Uiso 1 1 calc R . . C30 C 1.09382(16) 0.32415(17) 0.3084(3) 0.0508(7) Uani 1 1 d . . . C31 C 1.14056(19) 0.27022(18) 0.3282(4) 0.0573(8) Uani 1 1 d . . . H31A H 1.1353 0.2268 0.2888 0.069 Uiso 1 1 calc R . . C32 C 1.19499(19) 0.2798(2) 0.4057(4) 0.0619(9) Uani 1 1 d . . . H32A H 1.2273 0.2434 0.4179 0.074 Uiso 1 1 calc R . . C33 C 1.20178(18) 0.3429(2) 0.4651(3) 0.0624(9) Uani 1 1 d . . . C34 C 1.15630(19) 0.3977(2) 0.4455(4) 0.0635(9) Uani 1 1 d . . . H34A H 1.1619 0.4411 0.4848 0.076 Uiso 1 1 calc R . . C35 C 1.10223(18) 0.38752(19) 0.3669(3) 0.0582(8) Uani 1 1 d . . . H35A H 1.0707 0.4245 0.3532 0.070 Uiso 1 1 calc R . . C36 C 1.2559(2) 0.3517(2) 0.5515(4) 0.0738(11) Uani 1 1 d . . . B1 B 1.0370(3) 0.0849(2) 0.2148(4) 0.0649(10) Uiso 1 1 d . . . F1 F 1.0316(2) 0.01421(13) 0.2093(3) 0.1079(11) Uani 1 1 d . . . F2 F 1.0528(2) 0.1046(2) 0.3247(3) 0.1148(11) Uani 1 1 d . . . F3 F 1.08860(13) 0.10781(13) 0.1395(2) 0.0775(6) Uani 1 1 d . . . F4 F 0.97636(16) 0.11554(17) 0.1828(4) 0.1139(12) Uani 1 1 d . . . B2 B 1.0578(2) 0.4769(2) -0.0445(4) 0.0643(10) Uiso 1 1 d . . . F5 F 1.05907(13) 0.40613(13) -0.0264(3) 0.0863(8) Uani 1 1 d . . . F6 F 1.11958(14) 0.50640(15) -0.0147(3) 0.0903(7) Uani 1 1 d . . . F7 F 1.0049(2) 0.5037(2) 0.0224(4) 0.1380(16) Uani 1 1 d . . . F8 F 1.04130(19) 0.48828(19) -0.1603(3) 0.1124(12) Uani 1 1 d . . . N13 N 0.7978(2) -0.0811(2) 0.0071(4) 0.0942(12) Uiso 1 1 d . . . C37 C 0.8366(3) -0.0367(3) -0.0023(5) 0.0846(12) Uiso 1 1 d . . . C38 C 0.8848(5) 0.0190(5) -0.0197(11) 0.155(3) Uiso 1 1 d . . . H38A H 0.9160 0.0068 -0.0837 0.232 Uiso 1 1 calc R . . H38B H 0.9111 0.0263 0.0524 0.232 Uiso 1 1 calc R . . H38C H 0.8601 0.0620 -0.0396 0.232 Uiso 1 1 calc R . . N14 N 0.6769(4) 0.4463(4) -0.1489(8) 0.139(2) Uiso 1 1 d . . . C39 C 0.6409(3) 0.4864(3) -0.1072(5) 0.0836(12) Uiso 1 1 d . . . C40 C 0.5946(3) 0.5338(3) -0.0567(5) 0.0920(14) Uiso 1 1 d . . . H40A H 0.5553 0.5402 -0.1091 0.138 Uiso 1 1 calc R . . H40B H 0.6175 0.5789 -0.0445 0.138 Uiso 1 1 calc R . . H40C H 0.5788 0.5155 0.0188 0.138 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0392(2) 0.0557(2) 0.0481(2) -0.0008(2) -0.0066(2) -0.00167(15) N1 0.0444(14) 0.0650(15) 0.0466(14) -0.0009(12) -0.0112(11) -0.0005(12) N2 0.0428(13) 0.0644(14) 0.0488(15) 0.0044(11) -0.0098(11) -0.0056(11) N3 0.0425(13) 0.0553(13) 0.0487(15) 0.0016(11) -0.0016(11) 0.0011(11) N4 0.0433(14) 0.0551(14) 0.0548(15) 0.0025(11) -0.0078(12) -0.0030(11) N5 0.0397(13) 0.0619(15) 0.0577(16) -0.0032(12) -0.0108(12) -0.0035(11) N6 0.056(2) 0.156(5) 0.106(4) -0.039(3) -0.032(3) 0.017(2) N7 0.0397(14) 0.0716(17) 0.0625(17) -0.0016(14) -0.0119(12) 0.0036(12) N8 0.0438(15) 0.0673(16) 0.0638(18) -0.0116(14) -0.0087(13) 0.0074(12) N9 0.0421(13) 0.0511(12) 0.0486(14) -0.0044(11) -0.0014(11) 0.0003(10) N10 0.0432(13) 0.0519(12) 0.0467(16) -0.0019(11) -0.0075(11) -0.0001(9) N11 0.0448(14) 0.0610(15) 0.0464(14) -0.0006(11) -0.0077(12) -0.0067(11) N12 0.081(3) 0.117(3) 0.079(3) 0.017(2) -0.039(2) -0.024(2) C1 0.0535(18) 0.0662(19) 0.0493(17) 0.0041(14) -0.0046(14) -0.0013(15) C2 0.0556(19) 0.073(2) 0.0487(17) 0.0071(15) -0.0002(15) -0.0021(16) C3 0.0478(17) 0.0667(18) 0.0533(17) 0.0092(15) -0.0013(14) -0.0067(14) C4 0.0446(17) 0.0558(15) 0.0472(17) 0.0009(13) -0.0068(13) 0.0004(12) C5 0.0445(16) 0.0601(17) 0.0520(18) 0.0011(14) -0.0065(14) -0.0027(13) C6 0.0462(18) 0.0573(16) 0.0477(16) -0.0005(14) -0.0061(13) 0.0014(13) C7 0.0398(16) 0.0610(16) 0.0515(17) 0.0044(14) -0.0081(13) 0.0002(13) C8 0.0432(16) 0.0518(15) 0.0560(18) 0.0022(13) -0.0023(14) -0.0006(12) C9 0.059(2) 0.0581(18) 0.064(2) 0.0066(16) -0.0044(17) -0.0007(15) C10 0.064(2) 0.066(2) 0.068(2) 0.0063(18) -0.0029(17) -0.0118(17) C11 0.0547(19) 0.069(2) 0.065(2) 0.0035(16) -0.0029(16) -0.0144(17) C12 0.0427(17) 0.0639(17) 0.0487(17) 0.0011(13) -0.0027(13) 0.0007(14) C13 0.0497(19) 0.082(2) 0.070(2) 0.0127(19) -0.0143(17) -0.0006(17) C14 0.053(2) 0.090(3) 0.072(2) 0.007(2) -0.0173(19) 0.0062(19) C15 0.0404(17) 0.094(3) 0.0521(18) -0.0103(17) -0.0084(15) 0.0111(16) C16 0.057(2) 0.093(3) 0.071(2) 0.004(2) -0.0164(19) -0.015(2) C17 0.054(2) 0.075(2) 0.067(2) 0.0064(17) -0.0160(18) -0.0104(17) C18 0.052(2) 0.116(3) 0.074(3) -0.020(3) -0.013(2) 0.012(2) C19 0.0444(19) 0.099(3) 0.072(2) -0.020(2) -0.0078(17) 0.0195(18) C20 0.061(3) 0.130(4) 0.092(3) -0.043(3) -0.017(2) 0.036(3) C21 0.058(2) 0.099(3) 0.080(3) -0.039(3) -0.012(2) 0.019(2) C22 0.0399(15) 0.0594(16) 0.0560(17) -0.0070(14) -0.0050(13) 0.0050(13) C23 0.0481(17) 0.0565(16) 0.0526(17) -0.0074(14) -0.0078(14) 0.0009(13) C24 0.0378(14) 0.0518(15) 0.0476(16) 0.0000(12) -0.0051(12) -0.0030(11) C25 0.0402(15) 0.0495(14) 0.0504(17) -0.0001(12) -0.0030(13) 0.0026(11) C26 0.0409(15) 0.0499(14) 0.0450(15) 0.0026(12) -0.0008(12) 0.0005(12) C27 0.0476(17) 0.0590(17) 0.0567(18) -0.0026(14) -0.0011(14) 0.0037(13) C28 0.061(2) 0.0683(19) 0.0543(19) -0.0082(16) 0.0008(15) 0.0049(16) C29 0.0570(19) 0.0638(18) 0.0491(18) -0.0081(15) -0.0058(14) -0.0049(15) C30 0.0397(15) 0.0617(17) 0.0510(16) 0.0031(14) -0.0069(13) -0.0039(13) C31 0.0487(18) 0.0607(19) 0.063(2) 0.0037(15) -0.0100(16) -0.0024(14) C32 0.0486(19) 0.071(2) 0.067(2) 0.0125(16) -0.0166(17) -0.0043(15) C33 0.0468(17) 0.086(2) 0.054(2) 0.0070(17) -0.0095(15) -0.0139(15) C34 0.055(2) 0.079(2) 0.0571(19) -0.0072(17) -0.0101(15) -0.0135(16) C35 0.0497(18) 0.0657(18) 0.0593(19) -0.0062(15) -0.0100(15) -0.0043(15) C36 0.065(2) 0.092(3) 0.065(2) 0.011(2) -0.016(2) -0.020(2) F1 0.145(3) 0.0623(13) 0.117(3) 0.0089(15) 0.018(2) -0.0103(15) F2 0.143(3) 0.125(3) 0.0765(18) -0.0136(17) -0.0018(19) -0.022(2) F3 0.0639(14) 0.0828(14) 0.0857(16) 0.0163(12) 0.0038(12) -0.0010(11) F4 0.0652(16) 0.114(2) 0.163(3) 0.054(2) 0.0016(19) 0.0022(15) F5 0.0687(14) 0.0728(12) 0.118(2) 0.0267(15) -0.0058(15) 0.0008(10) F6 0.0811(16) 0.1011(16) 0.0888(17) 0.0016(16) -0.0177(16) -0.0253(13) F7 0.096(2) 0.141(3) 0.177(4) -0.076(3) -0.010(2) 0.035(2) F8 0.119(3) 0.116(2) 0.103(2) 0.0392(18) -0.041(2) -0.0436(19) _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 1.883(3) . ? Fe1 N3 1.891(3) . ? Fe1 N5 1.953(3) . ? Fe1 N7 1.957(3) . ? Fe1 N11 1.960(3) . ? Fe1 N1 1.962(3) . ? N1 C1 1.343(5) . ? N1 N2 1.383(4) . ? N2 C3 1.361(5) . ? N2 C4 1.410(4) . ? N3 C8 1.327(4) . ? N3 C4 1.337(4) . ? N4 C9 1.363(5) . ? N4 N5 1.378(4) . ? N4 C8 1.396(4) . ? N5 C11 1.332(5) . ? N6 C18 1.137(6) . ? N7 C19 1.328(5) . ? N7 N8 1.364(4) . ? N8 C21 1.365(5) . ? N8 C22 1.408(4) . ? N9 C26 1.332(4) . ? N9 C22 1.359(4) . ? N10 C27 1.372(4) . ? N10 N11 1.383(4) . ? N10 C26 1.396(4) . ? N11 C29 1.334(5) . ? N12 C36 1.129(6) . ? C1 C2 1.405(5) . ? C2 C3 1.374(5) . ? C4 C5 1.376(5) . ? C5 C6 1.420(5) . ? C6 C7 1.392(5) . ? C6 C12 1.482(4) . ? C7 C8 1.382(5) . ? C9 C10 1.367(6) . ? C10 C11 1.403(6) . ? C12 C17 1.382(5) . ? C12 C13 1.390(5) . ? C13 C14 1.386(5) . ? C14 C15 1.364(6) . ? C15 C16 1.391(6) . ? C15 C18 1.440(5) . ? C16 C17 1.390(5) . ? C19 C20 1.396(6) . ? C20 C21 1.377(6) . ? C22 C23 1.360(5) . ? C23 C24 1.405(4) . ? C24 C25 1.405(4) . ? C24 C30 1.480(4) . ? C25 C26 1.375(4) . ? C27 C28 1.356(5) . ? C28 C29 1.388(5) . ? C30 C35 1.394(5) . ? C30 C31 1.395(5) . ? C31 C32 1.393(5) . ? C32 C33 1.391(6) . ? C33 C34 1.390(6) . ? C33 C36 1.454(5) . ? C34 C35 1.398(5) . ? B1 F2 1.345(6) . ? B1 F1 1.358(5) . ? B1 F4 1.370(6) . ? B1 F3 1.394(5) . ? B2 F5 1.369(5) . ? B2 F6 1.373(5) . ? B2 F8 1.377(6) . ? B2 F7 1.383(6) . ? N13 C37 1.142(6) . ? C37 C38 1.435(10) . ? N14 C39 1.143(9) . ? C39 C40 1.404(8) . ? 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 179.23(12) . . ? N9 Fe1 N5 99.33(11) . . ? N3 Fe1 N5 80.29(12) . . ? N9 Fe1 N7 80.01(11) . . ? N3 Fe1 N7 99.32(12) . . ? N5 Fe1 N7 90.86(13) . . ? N9 Fe1 N11 80.08(11) . . ? N3 Fe1 N11 100.60(12) . . ? N5 Fe1 N11 92.40(12) . . ? N7 Fe1 N11 160.08(11) . . ? N9 Fe1 N1 100.37(12) . . ? N3 Fe1 N1 80.00(11) . . ? N5 Fe1 N1 160.27(11) . . ? N7 Fe1 N1 91.53(13) . . ? N11 Fe1 N1 92.00(12) . . ? C1 N1 N2 104.6(3) . . ? C1 N1 Fe1 142.4(2) . . ? N2 N1 Fe1 113.0(2) . . ? C3 N2 N1 111.6(3) . . ? C3 N2 C4 132.4(3) . . ? N1 N2 C4 116.0(3) . . ? C8 N3 C4 119.6(3) . . ? C8 N3 Fe1 119.5(2) . . ? C4 N3 Fe1 120.8(2) . . ? C9 N4 N5 111.0(3) . . ? C9 N4 C8 133.2(3) . . ? N5 N4 C8 115.5(3) . . ? C11 N5 N4 105.2(3) . . ? C11 N5 Fe1 141.7(3) . . ? N4 N5 Fe1 113.0(2) . . ? C19 N7 N8 104.8(3) . . ? C19 N7 Fe1 141.7(3) . . ? N8 N7 Fe1 113.5(2) . . ? N7 N8 C21 112.1(3) . . ? N7 N8 C22 116.7(3) . . ? C21 N8 C22 131.1(3) . . ? C26 N9 C22 118.8(3) . . ? C26 N9 Fe1 120.6(2) . . ? C22 N9 Fe1 120.6(2) . . ? C27 N10 N11 111.0(3) . . ? C27 N10 C26 132.9(3) . . ? N11 N10 C26 116.2(2) . . ? C29 N11 N10 104.8(3) . . ? C29 N11 Fe1 142.4(2) . . ? N10 N11 Fe1 112.6(2) . . ? N1 C1 C2 111.0(3) . . ? C3 C2 C1 106.2(3) . . ? N2 C3 C2 106.7(3) . . ? N3 C4 C5 123.3(3) . . ? N3 C4 N2 110.1(3) . . ? C5 C4 N2 126.5(3) . . ? C4 C5 C6 117.0(3) . . ? C7 C6 C5 119.2(3) . . ? C7 C6 C12 120.0(3) . . ? C5 C6 C12 120.8(3) . . ? C8 C7 C6 118.7(3) . . ? N3 C8 C7 122.1(3) . . ? N3 C8 N4 111.6(3) . . ? C7 C8 N4 126.2(3) . . ? N4 C9 C10 106.8(3) . . ? C9 C10 C11 106.2(3) . . ? N5 C11 C10 110.8(3) . . ? C17 C12 C13 118.1(3) . . ? C17 C12 C6 121.7(3) . . ? C13 C12 C6 120.2(3) . . ? C14 C13 C12 121.7(4) . . ? C15 C14 C13 119.5(4) . . ? C14 C15 C16 120.2(3) . . ? C14 C15 C18 119.8(4) . . ? C16 C15 C18 120.0(4) . . ? C17 C16 C15 119.9(4) . . ? C12 C17 C16 120.6(4) . . ? N6 C18 C15 178.2(7) . . ? N7 C19 C20 111.2(4) . . ? C21 C20 C19 106.2(4) . . ? N8 C21 C20 105.6(4) . . ? N9 C22 C23 122.6(3) . . ? N9 C22 N8 109.2(3) . . ? C23 C22 N8 128.2(3) . . ? C22 C23 C24 118.6(3) . . ? C25 C24 C23 118.9(3) . . ? C25 C24 C30 120.4(3) . . ? C23 C24 C30 120.7(3) . . ? C26 C25 C24 118.1(3) . . ? N9 C26 C25 123.0(3) . . ? N9 C26 N10 110.5(3) . . ? C25 C26 N10 126.5(3) . . ? C28 C27 N10 105.9(3) . . ? C27 C28 C29 107.6(3) . . ? N11 C29 C28 110.7(3) . . ? C35 C30 C31 119.3(3) . . ? C35 C30 C24 119.8(3) . . ? C31 C30 C24 120.9(3) . . ? C32 C31 C30 120.2(3) . . ? C33 C32 C31 119.7(3) . . ? C34 C33 C32 121.0(3) . . ? C34 C33 C36 119.0(4) . . ? C32 C33 C36 120.0(4) . . ? C33 C34 C35 118.7(4) . . ? C30 C35 C34 121.1(3) . . ? N12 C36 C33 177.6(6) . . ? F2 B1 F1 109.9(4) . . ? F2 B1 F4 109.1(5) . . ? F1 B1 F4 110.3(4) . . ? F2 B1 F3 108.7(4) . . ? F1 B1 F3 109.9(4) . . ? F4 B1 F3 108.9(4) . . ? F5 B2 F6 110.7(4) . . ? F5 B2 F8 107.8(4) . . ? F6 B2 F8 112.2(4) . . ? F5 B2 F7 107.3(4) . . ? F6 B2 F7 111.4(4) . . ? F8 B2 F7 107.2(4) . . ? N13 C37 C38 177.4(8) . . ? N14 C39 C40 177.8(7) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.66 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.471 _refine_diff_density_min -0.443 _refine_diff_density_rms 0.080 data_III _database_code_depnum_ccdc_archive 'CCDC 634176' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H30 Cl2 Fe N14 O8' _chemical_formula_weight 961.53 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 P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 10.808(2) _cell_length_b 13.925(3) _cell_length_c 28.685(6) _cell_angle_alpha 90.00 _cell_angle_beta 97.77(3) _cell_angle_gamma 90.00 _cell_volume 4277.5(15) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.493 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1968 _exptl_absorpt_coefficient_mu 0.548 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.7702 _exptl_absorpt_correction_T_max 0.9199 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 -1 0 0.0990 0 1 0 0.0470 -1 0 0 0.2560 1 0 1 0.1930 0 0 -1 0.1370 0 0 1 0.1340 _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'planar graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm, multiple pinhole' _diffrn_measurement_method 'rotation method' _diffrn_measurement_details '300 frames, detector distance = 130 mm' _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate ( 34 cm diameter )' _diffrn_detector_type STOE'_diffrn_measurement_device_type _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28842 _diffrn_reflns_av_R_equivalents 0.0411 _diffrn_reflns_av_sigmaI/netI 0.0315 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 25.71 _reflns_number_total 8036 _reflns_number_gt 6477 _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^)+(0.0496P)^2^+1.1282P] 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 0.00140(19) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8036 _refine_ls_number_parameters 626 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0508 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.0940 _refine_ls_wR_factor_gt 0.0892 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _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 0.37864(3) 0.73280(2) 0.624713(10) 0.03139(9) Uani 1 1 d . . . N1 N 0.34490(16) 0.66146(12) 0.68103(6) 0.0362(4) Uani 1 1 d . . . N2 N 0.38770(16) 0.56755(12) 0.68206(6) 0.0344(4) Uani 1 1 d . . . N3 N 0.45877(15) 0.61258(12) 0.61506(6) 0.0342(4) Uani 1 1 d . . . N4 N 0.51411(17) 0.68322(13) 0.55039(6) 0.0385(4) Uani 1 1 d . . . N5 N 0.45060(17) 0.76079(13) 0.56579(7) 0.0397(4) Uani 1 1 d . . . N6 N 0.8259(2) -0.00317(17) 0.56505(9) 0.0644(6) Uani 1 1 d . . . N7 N 0.51290(16) 0.81002(13) 0.66103(7) 0.0384(4) Uani 1 1 d . . . N8 N 0.47101(16) 0.89849(13) 0.67488(6) 0.0375(4) Uani 1 1 d . . . N9 N 0.28779(15) 0.84662(12) 0.63728(6) 0.0329(4) Uani 1 1 d . . . N10 N 0.12283(16) 0.77169(12) 0.59664(6) 0.0368(4) Uani 1 1 d . . . N11 N 0.21098(17) 0.70341(12) 0.59003(6) 0.0368(4) Uani 1 1 d . . . N12 N -0.2059(2) 1.38775(17) 0.70885(9) 0.0673(7) Uani 1 1 d . . . C1 C 0.2892(2) 0.67077(16) 0.71927(8) 0.0416(5) Uani 1 1 d . . . H1A H 0.2512 0.7281 0.7283 0.050 Uiso 1 1 calc R . . C2 C 0.2942(2) 0.58404(17) 0.74474(8) 0.0445(5) Uani 1 1 d . . . H2A H 0.2613 0.5725 0.7733 0.053 Uiso 1 1 calc R . . C3 C 0.3557(2) 0.51978(16) 0.72004(8) 0.0397(5) Uani 1 1 d . . . H3A H 0.3728 0.4544 0.7279 0.048 Uiso 1 1 calc R . . C4 C 0.45431(18) 0.54009(15) 0.64540(7) 0.0340(4) Uani 1 1 d . . . C5 C 0.50921(19) 0.45250(15) 0.64048(8) 0.0370(5) Uani 1 1 d . . . H5A H 0.5071 0.4035 0.6634 0.044 Uiso 1 1 calc R . . C6 C 0.56870(19) 0.43771(15) 0.60043(8) 0.0377(5) Uani 1 1 d . . . C7 C 0.57147(19) 0.51262(16) 0.56786(8) 0.0387(5) Uani 1 1 d . . . H7A H 0.6098 0.5042 0.5402 0.046 Uiso 1 1 calc R . . C8 C 0.51695(19) 0.59872(15) 0.57716(7) 0.0357(5) Uani 1 1 d . . . C9 C 0.5732(2) 0.70858(18) 0.51300(8) 0.0472(6) Uani 1 1 d . . . H9A H 0.6228 0.6682 0.4963 0.057 Uiso 1 1 calc R . . C10 C 0.5467(2) 0.80341(19) 0.50430(9) 0.0515(6) Uani 1 1 d . . . H10A H 0.5745 0.8418 0.4804 0.062 Uiso 1 1 calc R . . C11 C 0.4706(2) 0.83305(17) 0.53755(8) 0.0457(5) Uani 1 1 d . . . H11A H 0.4380 0.8960 0.5396 0.055 Uiso 1 1 calc R . . C12 C 0.6268(2) 0.34309(16) 0.59319(8) 0.0404(5) Uani 1 1 d . . . C13 C 0.5773(2) 0.25939(16) 0.60993(8) 0.0443(5) Uani 1 1 d . . . H13A H 0.5070 0.2635 0.6264 0.053 Uiso 1 1 calc R . . C14 C 0.6286(2) 0.17072(18) 0.60299(9) 0.0471(6) Uani 1 1 d . . . H14A H 0.5937 0.1143 0.6145 0.057 Uiso 1 1 calc R . . C15 C 0.7321(2) 0.16440(17) 0.57889(9) 0.0460(6) Uani 1 1 d . . . C16 C 0.7842(2) 0.24718(18) 0.56251(10) 0.0516(6) Uani 1 1 d . . . H16A H 0.8555 0.2428 0.5466 0.062 Uiso 1 1 calc R . . C17 C 0.7318(2) 0.33578(18) 0.56951(9) 0.0479(6) Uani 1 1 d . . . H17A H 0.7672 0.3922 0.5582 0.057 Uiso 1 1 calc R . . C18 C 0.7845(2) 0.0708(2) 0.57127(9) 0.0523(6) Uani 1 1 d . . . C19 C 0.6349(2) 0.81033(19) 0.67514(9) 0.0475(6) Uani 1 1 d . . . H19A H 0.6897 0.7588 0.6706 0.057 Uiso 1 1 calc R . . C20 C 0.6718(2) 0.8971(2) 0.69762(10) 0.0564(7) Uani 1 1 d . . . H20A H 0.7541 0.9146 0.7108 0.068 Uiso 1 1 calc R . . C21 C 0.5662(2) 0.95155(18) 0.69680(9) 0.0478(6) Uani 1 1 d . . . H21A H 0.5608 1.0144 0.7092 0.057 Uiso 1 1 calc R . . C22 C 0.34359(19) 0.91809(15) 0.66322(7) 0.0344(4) Uani 1 1 d . . . C23 C 0.2810(2) 0.99805(15) 0.67623(7) 0.0368(5) Uani 1 1 d . . . H23A H 0.3235 1.0476 0.6947 0.044 Uiso 1 1 calc R . . C24 C 0.1532(2) 1.00338(15) 0.66120(7) 0.0355(5) Uani 1 1 d . . . C25 C 0.09338(19) 0.92910(15) 0.63413(8) 0.0361(5) Uani 1 1 d . . . H25A H 0.0063 0.9314 0.6235 0.043 Uiso 1 1 calc R . . C26 C 0.16503(19) 0.85248(14) 0.62344(7) 0.0338(4) Uani 1 1 d . . . C27 C 0.0103(2) 0.74941(17) 0.57201(9) 0.0472(6) Uani 1 1 d . . . H27A H -0.0647 0.7854 0.5710 0.057 Uiso 1 1 calc R . . C28 C 0.0256(2) 0.66569(18) 0.54906(9) 0.0517(6) Uani 1 1 d . . . H28A H -0.0364 0.6318 0.5289 0.062 Uiso 1 1 calc R . . C29 C 0.1504(2) 0.63938(16) 0.56105(8) 0.0439(5) Uani 1 1 d . . . H29A H 0.1871 0.5833 0.5500 0.053 Uiso 1 1 calc R . . C30 C 0.0782(2) 1.08711(15) 0.67327(8) 0.0383(5) Uani 1 1 d . . . C31 C 0.1240(2) 1.18053(16) 0.67095(8) 0.0434(5) Uani 1 1 d . . . H31A H 0.2056 1.1909 0.6631 0.052 Uiso 1 1 calc R . . C32 C 0.0504(2) 1.25822(16) 0.68005(9) 0.0475(6) Uani 1 1 d . . . H32A H 0.0806 1.3219 0.6778 0.057 Uiso 1 1 calc R . . C33 C -0.0679(2) 1.24215(17) 0.69245(8) 0.0445(5) Uani 1 1 d . . . C34 C -0.1135(2) 1.14962(17) 0.69600(8) 0.0459(5) Uani 1 1 d . . . H34A H -0.1938 1.1393 0.7051 0.055 Uiso 1 1 calc R . . C35 C -0.0405(2) 1.07265(17) 0.68619(8) 0.0423(5) Uani 1 1 d . . . H35A H -0.0714 1.0091 0.6883 0.051 Uiso 1 1 calc R . . C36 C -0.1448(3) 1.32374(18) 0.70180(9) 0.0525(6) Uani 1 1 d . . . Cl1 Cl 0.19825(5) 0.37313(4) 0.57545(2) 0.04565(15) Uani 1 1 d . . . O1 O 0.06920(16) 0.34844(15) 0.56504(7) 0.0666(5) Uani 1 1 d . . . O2 O 0.21571(17) 0.43029(14) 0.61731(7) 0.0620(5) Uani 1 1 d . . . O3 O 0.2353(2) 0.42725(13) 0.53656(7) 0.0702(6) Uani 1 1 d . . . O4 O 0.27236(17) 0.28716(13) 0.58163(7) 0.0612(5) Uani 1 1 d . . . Cl2 Cl 0.0000 0.79500(6) 0.7500 0.0618(3) Uani 1 2 d S . . O5 O -0.0296(11) 0.7083(4) 0.7369(3) 0.156(6) Uani 0.50 1 d P . . O6 O -0.0874(13) 0.8469(9) 0.7667(5) 0.142(5) Uani 0.50 1 d P . . O7 O 0.0695(4) 0.7830(5) 0.8035(2) 0.103(2) Uani 0.50 1 d P . . O8 O 0.0937(7) 0.8494(4) 0.7322(3) 0.055(2) Uani 0.50 1 d P . . Cl3 Cl 0.5000 0.77706(5) 0.2500 0.04240(18) Uani 1 2 d S . . O9 O 0.5653(8) 0.7427(9) 0.2923(3) 0.159(5) Uani 0.50 1 d P . . O10 O 0.4647(8) 0.7015(5) 0.2236(3) 0.163(6) Uani 0.50 1 d P . . O11 O 0.5892(12) 0.8330(9) 0.2294(4) 0.081(3) Uani 0.50 1 d P . . O12 O 0.4015(10) 0.8318(9) 0.2606(5) 0.098(4) Uani 0.50 1 d P . . N13 N 0.3234(3) 1.03028(18) 0.56619(10) 0.0743(8) Uani 1 1 d . . . C37 C 0.2282(3) 1.06375(19) 0.55390(10) 0.0568(7) Uani 1 1 d . . . C38 C 0.1089(3) 1.1069(2) 0.53827(11) 0.0657(8) Uani 1 1 d . . . H38A H 0.0944 1.1599 0.5594 0.099 Uiso 1 1 calc R . . H38B H 0.0429 1.0587 0.5386 0.099 Uiso 1 1 calc R . . H38C H 0.1080 1.1316 0.5062 0.099 Uiso 1 1 calc R . . N14 N -0.2174(2) 0.6240(2) 0.63049(11) 0.0822(8) Uani 1 1 d . . . C39 C -0.1235(3) 0.5919(2) 0.64408(11) 0.0575(7) Uani 1 1 d . . . C40 C -0.0038(3) 0.5516(2) 0.66186(12) 0.0664(8) Uani 1 1 d . . . H40A H 0.0599 0.6021 0.6641 0.100 Uiso 1 1 calc R . . H40B H 0.0175 0.5012 0.6405 0.100 Uiso 1 1 calc R . . H40C H -0.0072 0.5241 0.6931 0.100 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.03584(16) 0.02945(15) 0.03041(16) 0.00016(12) 0.00998(12) 0.00244(12) N1 0.0414(9) 0.0329(9) 0.0363(10) -0.0030(8) 0.0126(8) -0.0001(7) N2 0.0360(9) 0.0375(9) 0.0308(9) 0.0000(7) 0.0085(7) 0.0001(7) N3 0.0353(9) 0.0379(9) 0.0306(9) 0.0011(7) 0.0095(7) 0.0004(7) N4 0.0430(10) 0.0407(10) 0.0337(10) 0.0030(8) 0.0124(8) 0.0002(8) N5 0.0481(10) 0.0354(9) 0.0369(10) 0.0020(8) 0.0106(8) 0.0006(8) N6 0.0655(14) 0.0602(14) 0.0654(16) -0.0109(12) 0.0011(12) 0.0224(12) N7 0.0381(9) 0.0402(10) 0.0388(10) 0.0017(8) 0.0124(8) 0.0039(8) N8 0.0360(9) 0.0393(10) 0.0380(10) -0.0016(8) 0.0074(8) -0.0028(7) N9 0.0345(9) 0.0322(9) 0.0326(9) 0.0020(7) 0.0067(7) -0.0014(7) N10 0.0384(9) 0.0336(9) 0.0378(10) -0.0015(8) 0.0036(8) -0.0008(7) N11 0.0466(10) 0.0315(9) 0.0335(10) -0.0019(7) 0.0097(8) 0.0014(8) N12 0.0819(17) 0.0524(13) 0.0694(17) -0.0058(12) 0.0171(13) 0.0209(12) C1 0.0501(12) 0.0409(12) 0.0375(12) -0.0051(10) 0.0197(10) -0.0044(10) C2 0.0502(13) 0.0506(13) 0.0357(12) -0.0008(10) 0.0165(10) -0.0046(11) C3 0.0424(11) 0.0444(12) 0.0334(12) 0.0065(10) 0.0094(9) -0.0030(10) C4 0.0335(10) 0.0387(11) 0.0306(11) 0.0011(9) 0.0075(8) 0.0007(8) C5 0.0384(11) 0.0382(11) 0.0355(12) 0.0018(9) 0.0091(9) 0.0027(9) C6 0.0344(10) 0.0407(12) 0.0381(12) -0.0031(10) 0.0048(9) 0.0008(9) C7 0.0392(11) 0.0447(12) 0.0341(12) -0.0017(10) 0.0127(9) 0.0001(9) C8 0.0370(11) 0.0398(11) 0.0314(11) 0.0006(9) 0.0085(9) -0.0007(9) C9 0.0518(13) 0.0573(15) 0.0355(13) -0.0004(11) 0.0166(10) -0.0062(11) C10 0.0615(15) 0.0532(14) 0.0428(14) 0.0091(11) 0.0173(12) -0.0072(12) C11 0.0571(14) 0.0402(12) 0.0410(13) 0.0075(10) 0.0104(11) -0.0034(10) C12 0.0397(11) 0.0447(12) 0.0375(12) -0.0029(10) 0.0071(9) 0.0052(9) C13 0.0458(12) 0.0457(13) 0.0433(13) 0.0009(10) 0.0124(10) 0.0067(10) C14 0.0540(14) 0.0444(13) 0.0437(14) 0.0030(11) 0.0097(11) 0.0093(11) C15 0.0460(12) 0.0464(13) 0.0442(14) -0.0050(11) 0.0012(10) 0.0134(10) C16 0.0440(13) 0.0577(15) 0.0553(15) -0.0050(12) 0.0152(11) 0.0087(11) C17 0.0450(12) 0.0483(13) 0.0534(15) -0.0027(11) 0.0176(11) 0.0026(10) C18 0.0519(14) 0.0577(16) 0.0466(15) -0.0051(12) 0.0039(11) 0.0153(12) C19 0.0351(11) 0.0572(14) 0.0508(15) 0.0022(12) 0.0084(10) 0.0018(10) C20 0.0353(12) 0.0702(17) 0.0630(17) 0.0002(14) 0.0044(11) -0.0071(12) C21 0.0465(13) 0.0496(14) 0.0469(14) -0.0039(11) 0.0052(11) -0.0111(11) C22 0.0374(11) 0.0346(11) 0.0318(11) 0.0019(9) 0.0068(9) -0.0022(9) C23 0.0450(12) 0.0341(11) 0.0321(11) -0.0016(9) 0.0086(9) -0.0028(9) C24 0.0429(11) 0.0328(10) 0.0327(11) 0.0055(9) 0.0121(9) 0.0003(9) C25 0.0365(11) 0.0356(11) 0.0368(12) 0.0041(9) 0.0069(9) 0.0026(9) C26 0.0371(10) 0.0323(10) 0.0318(11) 0.0017(8) 0.0043(8) -0.0015(8) C27 0.0433(12) 0.0475(14) 0.0480(14) 0.0003(11) -0.0036(10) -0.0030(10) C28 0.0597(15) 0.0459(13) 0.0467(15) -0.0060(11) -0.0032(12) -0.0113(11) C29 0.0580(14) 0.0366(12) 0.0368(13) -0.0040(10) 0.0050(10) -0.0062(10) C30 0.0465(12) 0.0378(11) 0.0316(11) 0.0007(9) 0.0085(9) 0.0054(9) C31 0.0512(13) 0.0376(12) 0.0438(14) 0.0000(10) 0.0153(11) 0.0023(10) C32 0.0641(15) 0.0339(12) 0.0455(14) -0.0004(10) 0.0115(11) 0.0031(10) C33 0.0559(14) 0.0441(13) 0.0340(12) -0.0024(10) 0.0084(10) 0.0127(10) C34 0.0478(13) 0.0497(14) 0.0416(13) -0.0021(11) 0.0116(10) 0.0069(11) C35 0.0471(12) 0.0404(12) 0.0410(13) 0.0000(10) 0.0122(10) 0.0034(10) C36 0.0645(15) 0.0483(14) 0.0465(15) -0.0039(11) 0.0139(12) 0.0109(12) Cl1 0.0487(3) 0.0433(3) 0.0466(3) -0.0061(2) 0.0126(2) 0.0017(2) O1 0.0483(10) 0.0832(14) 0.0657(13) -0.0124(11) -0.0016(9) -0.0041(9) O2 0.0559(10) 0.0732(12) 0.0580(12) -0.0282(10) 0.0117(9) -0.0078(9) O3 0.1024(16) 0.0468(10) 0.0713(13) 0.0060(9) 0.0470(12) 0.0140(10) O4 0.0656(11) 0.0494(10) 0.0710(13) 0.0034(9) 0.0182(10) 0.0140(9) Cl2 0.0387(4) 0.0424(5) 0.1074(8) 0.000 0.0219(5) 0.000 O5 0.257(13) 0.079(3) 0.171(11) -0.081(5) 0.167(10) -0.109(6) O6 0.129(9) 0.169(9) 0.132(10) -0.046(7) 0.033(8) 0.076(7) O7 0.052(2) 0.153(5) 0.099(4) 0.077(4) -0.011(2) -0.008(3) O8 0.066(4) 0.039(3) 0.070(5) 0.003(3) 0.046(4) 0.005(3) Cl3 0.0542(4) 0.0320(4) 0.0434(4) 0.000 0.0152(3) 0.000 O9 0.074(4) 0.335(14) 0.065(4) 0.096(7) -0.004(3) 0.014(6) O10 0.189(10) 0.094(4) 0.241(12) -0.136(6) 0.161(10) -0.115(6) O11 0.111(7) 0.052(5) 0.092(5) 0.036(4) 0.059(4) 0.005(4) O12 0.053(4) 0.062(6) 0.181(11) 0.014(6) 0.028(5) 0.031(4) N13 0.0915(19) 0.0621(15) 0.0789(19) 0.0250(13) 0.0460(16) 0.0156(14) C37 0.0781(19) 0.0437(14) 0.0552(17) 0.0085(12) 0.0331(15) 0.0009(14) C38 0.0746(19) 0.0628(17) 0.0606(18) -0.0058(14) 0.0123(15) 0.0022(15) N14 0.0536(15) 0.098(2) 0.094(2) -0.0254(17) 0.0073(14) 0.0018(14) C39 0.0491(15) 0.0603(16) 0.0656(18) -0.0154(14) 0.0174(13) -0.0067(13) C40 0.0590(16) 0.0654(18) 0.078(2) 0.0027(15) 0.0214(15) 0.0083(14) _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 1.9219(17) . ? Fe1 N9 1.9240(17) . ? Fe1 N1 1.9719(18) . ? Fe1 N7 1.985(2) . ? Fe1 N11 1.988(2) . ? Fe1 N5 1.9923(19) . ? N1 C1 1.327(3) . ? N1 N2 1.386(2) . ? N2 C3 1.360(3) . ? N2 C4 1.405(3) . ? N3 C4 1.338(3) . ? N3 C8 1.342(3) . ? N4 C9 1.366(3) . ? N4 N5 1.384(2) . ? N4 C8 1.403(3) . ? N5 C11 1.328(3) . ? N6 C18 1.147(3) . ? N7 C19 1.325(3) . ? N7 N8 1.389(2) . ? N8 C21 1.351(3) . ? N8 C22 1.399(3) . ? N9 C26 1.335(3) . ? N9 C22 1.337(3) . ? N10 C27 1.357(3) . ? N10 N11 1.377(2) . ? N10 C26 1.403(3) . ? N11 C29 1.330(3) . ? N12 C36 1.143(3) . ? C1 C2 1.409(3) . ? C2 C3 1.368(3) . ? C4 C5 1.372(3) . ? C5 C6 1.406(3) . ? C6 C7 1.403(3) . ? C6 C12 1.486(3) . ? C7 C8 1.378(3) . ? C9 C10 1.367(4) . ? C10 C11 1.403(3) . ? C12 C13 1.395(3) . ? C12 C17 1.402(3) . ? C13 C14 1.379(3) . ? C14 C15 1.395(3) . ? C15 C16 1.392(4) . ? C15 C18 1.450(3) . ? C16 C17 1.384(3) . ? C19 C20 1.402(4) . ? C20 C21 1.369(4) . ? C22 C23 1.380(3) . ? C23 C24 1.393(3) . ? C24 C25 1.398(3) . ? C24 C30 1.487(3) . ? C25 C26 1.377(3) . ? C27 C28 1.360(3) . ? C28 C29 1.395(4) . ? C30 C31 1.397(3) . ? C30 C35 1.397(3) . ? C31 C32 1.388(3) . ? C32 C33 1.391(3) . ? C33 C34 1.388(3) . ? C33 C36 1.454(3) . ? C34 C35 1.382(3) . ? Cl1 O1 1.4284(19) . ? Cl1 O2 1.4315(18) . ? Cl1 O4 1.4380(18) . ? Cl1 O3 1.4470(19) . ? Cl2 O5 1.292(5) . ? Cl2 O6 1.329(11) . ? Cl2 O8 1.414(7) . ? Cl2 O7 1.624(5) . ? Cl3 O10 1.322(5) . ? Cl3 O12 1.376(9) . ? Cl3 O9 1.402(7) . ? Cl3 O11 1.429(9) . ? N13 C37 1.140(4) . ? C37 C38 1.439(4) . ? N14 C39 1.129(4) . ? C39 C40 1.438(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Fe1 N9 174.75(7) . . ? N3 Fe1 N1 79.40(7) . . ? N9 Fe1 N1 96.08(7) . . ? N3 Fe1 N7 103.64(7) . . ? N9 Fe1 N7 79.09(7) . . ? N1 Fe1 N7 92.64(8) . . ? N3 Fe1 N11 98.43(7) . . ? N9 Fe1 N11 79.03(7) . . ? N1 Fe1 N11 92.82(8) . . ? N7 Fe1 N11 157.89(7) . . ? N3 Fe1 N5 79.22(7) . . ? N9 Fe1 N5 105.40(7) . . ? N1 Fe1 N5 158.46(7) . . ? N7 Fe1 N5 89.87(8) . . ? N11 Fe1 N5 92.84(8) . . ? C1 N1 N2 105.18(17) . . ? C1 N1 Fe1 141.52(16) . . ? N2 N1 Fe1 113.24(12) . . ? C3 N2 N1 110.99(16) . . ? C3 N2 C4 132.64(18) . . ? N1 N2 C4 116.36(16) . . ? C4 N3 C8 118.73(18) . . ? C4 N3 Fe1 120.46(13) . . ? C8 N3 Fe1 120.78(14) . . ? C9 N4 N5 110.68(18) . . ? C9 N4 C8 131.93(19) . . ? N5 N4 C8 117.07(16) . . ? C11 N5 N4 105.56(18) . . ? C11 N5 Fe1 141.29(16) . . ? N4 N5 Fe1 112.67(13) . . ? C19 N7 N8 105.01(19) . . ? C19 N7 Fe1 142.04(17) . . ? N8 N7 Fe1 112.78(13) . . ? C21 N8 N7 111.17(18) . . ? C21 N8 C22 131.86(19) . . ? N7 N8 C22 116.94(17) . . ? C26 N9 C22 118.39(18) . . ? C26 N9 Fe1 120.43(14) . . ? C22 N9 Fe1 120.96(14) . . ? C27 N10 N11 110.99(18) . . ? C27 N10 C26 132.10(19) . . ? N11 N10 C26 116.69(17) . . ? C29 N11 N10 104.92(18) . . ? C29 N11 Fe1 142.14(16) . . ? N10 N11 Fe1 112.93(13) . . ? N1 C1 C2 110.8(2) . . ? C3 C2 C1 106.21(19) . . ? N2 C3 C2 106.8(2) . . ? N3 C4 C5 123.35(18) . . ? N3 C4 N2 110.40(17) . . ? C5 C4 N2 126.25(19) . . ? C4 C5 C6 117.8(2) . . ? C7 C6 C5 119.2(2) . . ? C7 C6 C12 121.24(19) . . ? C5 C6 C12 119.5(2) . . ? C8 C7 C6 118.03(19) . . ? N3 C8 C7 122.79(19) . . ? N3 C8 N4 110.17(18) . . ? C7 C8 N4 127.03(18) . . ? N4 C9 C10 106.5(2) . . ? C9 C10 C11 106.7(2) . . ? N5 C11 C10 110.5(2) . . ? C13 C12 C17 118.6(2) . . ? C13 C12 C6 120.24(19) . . ? C17 C12 C6 121.1(2) . . ? C14 C13 C12 121.2(2) . . ? C13 C14 C15 119.5(2) . . ? C16 C15 C14 120.2(2) . . ? C16 C15 C18 120.6(2) . . ? C14 C15 C18 119.2(2) . . ? C17 C16 C15 119.8(2) . . ? C16 C17 C12 120.6(2) . . ? N6 C18 C15 179.7(3) . . ? N7 C19 C20 110.7(2) . . ? C21 C20 C19 106.5(2) . . ? N8 C21 C20 106.6(2) . . ? N9 C22 C23 123.40(19) . . ? N9 C22 N8 110.07(17) . . ? C23 C22 N8 126.5(2) . . ? C22 C23 C24 117.5(2) . . ? C23 C24 C25 119.82(19) . . ? C23 C24 C30 121.2(2) . . ? C25 C24 C30 118.95(19) . . ? C26 C25 C24 117.7(2) . . ? N9 C26 C25 123.2(2) . . ? N9 C26 N10 110.50(18) . . ? C25 C26 N10 126.31(19) . . ? N10 C27 C28 106.8(2) . . ? C27 C28 C29 106.4(2) . . ? N11 C29 C28 110.9(2) . . ? C31 C30 C35 119.4(2) . . ? C31 C30 C24 120.76(19) . . ? C35 C30 C24 119.8(2) . . ? C32 C31 C30 120.1(2) . . ? C31 C32 C33 119.5(2) . . ? C34 C33 C32 121.0(2) . . ? C34 C33 C36 119.6(2) . . ? C32 C33 C36 119.3(2) . . ? C35 C34 C33 119.1(2) . . ? C34 C35 C30 120.8(2) . . ? N12 C36 C33 179.5(3) . . ? O1 Cl1 O2 108.88(12) . . ? O1 Cl1 O4 109.71(12) . . ? O2 Cl1 O4 110.57(13) . . ? O1 Cl1 O3 109.18(14) . . ? O2 Cl1 O3 109.77(12) . . ? O4 Cl1 O3 108.72(11) . . ? O5 Cl2 O6 117.0(8) . . ? O5 Cl2 O8 123.8(5) . . ? O6 Cl2 O8 114.7(4) . . ? O5 Cl2 O7 104.1(6) . . ? O6 Cl2 O7 88.6(7) . . ? O8 Cl2 O7 97.7(4) . . ? O10 Cl3 O9 107.2(7) . . ? O12 Cl3 O9 108.1(8) . . ? O10 Cl3 O11 110.9(7) . . ? O12 Cl3 O11 112.0(3) . . ? O9 Cl3 O11 104.8(7) . . ? N13 C37 C38 179.4(3) . . ? N14 C39 C40 179.3(3) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.71 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.477 _refine_diff_density_min -0.327 _refine_diff_density_rms 0.045