Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Hung, Chen-Hsiung' 'Chen, Wan-Chin' 'Lee, Gene-Hsiung' 'Peng, Shie-ming' _publ_contact_author_name 'Prof Chen-Hsiung Hung' _publ_contact_author_address ; Department of Chemistry National Changhua University of Education Department of chemistry National Changhua University of Edu Changhua Taiwan 50058 TAIWAN ; _publ_contact_author_email 'CHHUNG@CC.NCUE.EDU.TW' _publ_section_title ; Dimeric Iron N-Confused Porphyrin Complexes ; data_h200m _database_code_CSD 184398 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H72 Fe2 N8 O2' _chemical_formula_weight 1481.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 15.867(5) _cell_length_b 20.697(6) _cell_length_c 22.397(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7355(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour 'Dark Green' _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.338 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3088 _exptl_absorpt_coefficient_mu 0.454 _exptl_absorpt_correction_type 'Empirical Used SADABS' _exptl_absorpt_correction_T_min 0.7211 _exptl_absorpt_correction_T_max 0.9486 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45278 _diffrn_reflns_av_R_equivalents 0.1119 _diffrn_reflns_av_sigmaI/netI 0.2515 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 27.67 _reflns_number_total 8528 _reflns_number_gt 1890 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.0400P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8528 _refine_ls_number_parameters 462 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2719 _refine_ls_R_factor_gt 0.0756 _refine_ls_wR_factor_ref 0.1788 _refine_ls_wR_factor_gt 0.1546 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.983 _refine_ls_shift/su_max 0.004 _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 0.95188(6) 0.02364(4) 0.60422(4) 0.0731(3) Uani 1 1 d . . . N1 N 0.9811(3) -0.0551(2) 0.6603(2) 0.0606(14) Uani 1 1 d . . . N2 N 0.9283(3) 0.0766(2) 0.6780(2) 0.0604(14) Uani 1 1 d . . . N3 N 0.8538(3) 0.0742(2) 0.5620(2) 0.0625(14) Uani 1 1 d . . . N4 N 0.9504(3) -0.0665(2) 0.4465(2) 0.0533(12) Uani 1 1 d . . . C1 C 0.9958(4) -0.1200(3) 0.6473(3) 0.0639(18) Uani 1 1 d . . . C2 C 1.0255(4) -0.1526(3) 0.6996(3) 0.080(2) Uani 1 1 d . . . H2A H 1.0379 -0.1964 0.7028 0.096 Uiso 1 1 calc R . . C3 C 1.0322(4) -0.1086(3) 0.7429(3) 0.077(2) Uani 1 1 d . . . H3A H 1.0516 -0.1159 0.7815 0.092 Uiso 1 1 calc R . . C4 C 1.0038(4) -0.0477(3) 0.7189(3) 0.0637(18) Uani 1 1 d . . . C5 C 1.0010(4) 0.0105(3) 0.7527(3) 0.0664(18) Uani 1 1 d . . . C6 C 0.9646(4) 0.0681(3) 0.7330(3) 0.0667(18) Uani 1 1 d . . . C7 C 0.9521(4) 0.1243(3) 0.7687(3) 0.0746(19) Uani 1 1 d . . . H7A H 0.9724 0.1306 0.8072 0.089 Uiso 1 1 calc R . . C8 C 0.9066(4) 0.1661(3) 0.7375(3) 0.076(2) Uani 1 1 d . . . H8A H 0.8889 0.2068 0.7499 0.091 Uiso 1 1 calc R . . C9 C 0.8899(4) 0.1361(3) 0.6805(3) 0.0649(18) Uani 1 1 d . . . C10 C 0.8395(4) 0.1617(3) 0.6359(3) 0.0652(18) Uani 1 1 d . . . C11 C 0.8196(4) 0.1317(3) 0.5820(3) 0.0659(19) Uani 1 1 d . . . C12 C 0.7616(4) 0.1563(3) 0.5394(3) 0.079(2) Uani 1 1 d . . . H12A H 0.7298 0.1938 0.5428 0.095 Uiso 1 1 calc R . . C13 C 0.7614(4) 0.1147(3) 0.4931(3) 0.0721(19) Uani 1 1 d . . . H13A H 0.7290 0.1188 0.4587 0.086 Uiso 1 1 calc R . . C14 C 0.8180(4) 0.0642(3) 0.5052(3) 0.0601(17) Uani 1 1 d . . . C15 C 0.8420(4) 0.0147(3) 0.4663(3) 0.0582(17) Uani 1 1 d . . . C16 C 0.8947(4) -0.0363(3) 0.4863(3) 0.0612(17) Uani 1 1 d . . . C17 C 0.8991(4) -0.0598(3) 0.5445(3) 0.0609(17) Uani 1 1 d . . . H17A H 0.8712 -0.0432 0.5776 0.073 Uiso 1 1 calc R . . C18 C 0.9527(4) -0.1129(3) 0.5439(3) 0.0552(16) Uani 1 1 d . . . C19 C 0.9790(4) -0.1163(3) 0.4839(3) 0.080(2) Uani 1 1 d . . . H19A H 1.0132 -0.1496 0.4699 0.096 Uiso 1 1 calc R . . C20 C 0.9858(4) -0.1488(3) 0.5923(3) 0.0627(18) Uani 1 1 d . . . C21 C 0.8012(5) 0.2275(4) 0.6456(4) 0.081(2) Uani 1 1 d . . . C22 C 0.7379(7) 0.2363(5) 0.6829(4) 0.142(4) Uani 1 1 d . . . H22A H 0.7168 0.2014 0.7043 0.170 Uiso 1 1 calc R . . C23 C 0.7026(9) 0.2967(7) 0.6905(5) 0.184(6) Uani 1 1 d . . . H23A H 0.6569 0.3013 0.7162 0.221 Uiso 1 1 calc R . . C24 C 0.7309(9) 0.3466(6) 0.6633(5) 0.154(6) Uani 1 1 d . . . H24A H 0.7079 0.3870 0.6715 0.184 Uiso 1 1 calc R . . C25 C 0.7946(7) 0.3416(5) 0.6224(5) 0.155(4) Uani 1 1 d . . . H25A H 0.8130 0.3770 0.6005 0.185 Uiso 1 1 calc R . . C26 C 0.8304(5) 0.2806(5) 0.6153(4) 0.138(3) Uani 1 1 d . . . H26A H 0.8756 0.2758 0.5892 0.166 Uiso 1 1 calc R . . C27 C 0.8079(4) 0.0131(3) 0.4043(3) 0.0656(18) Uani 1 1 d . . . C28 C 0.8056(4) 0.0654(3) 0.3673(3) 0.078(2) Uani 1 1 d . . . H28A H 0.8279 0.1048 0.3794 0.093 Uiso 1 1 calc R . . C29 C 0.7694(5) 0.0588(4) 0.3110(3) 0.101(3) Uani 1 1 d . . . H29A H 0.7678 0.0942 0.2855 0.121 Uiso 1 1 calc R . . C30 C 0.7371(5) 0.0029(5) 0.2928(4) 0.111(3) Uani 1 1 d . . . H30A H 0.7125 -0.0002 0.2552 0.134 Uiso 1 1 calc R . . C31 C 0.7400(5) -0.0498(4) 0.3291(4) 0.130(3) Uani 1 1 d . . . H31A H 0.7177 -0.0890 0.3164 0.156 Uiso 1 1 calc R . . C32 C 0.7760(5) -0.0445(4) 0.3842(3) 0.101(2) Uani 1 1 d . . . H32A H 0.7789 -0.0807 0.4086 0.121 Uiso 1 1 calc R . . C33 C 1.0111(5) -0.2167(3) 0.5810(3) 0.0683(19) Uani 1 1 d . . . C34 C 0.9574(6) -0.2605(4) 0.5625(4) 0.147(4) Uani 1 1 d . . . H34A H 0.9018 -0.2480 0.5565 0.176 Uiso 1 1 calc R . . C35 C 0.9790(6) -0.3245(4) 0.5515(5) 0.158(4) Uani 1 1 d . . . H35A H 0.9374 -0.3534 0.5394 0.190 Uiso 1 1 calc R . . C36 C 1.0559(7) -0.3449(4) 0.5576(4) 0.107(3) Uani 1 1 d . . . H36A H 1.0698 -0.3880 0.5512 0.129 Uiso 1 1 calc R . . C37 C 1.1131(6) -0.3024(4) 0.5732(4) 0.154(4) Uani 1 1 d . . . H37A H 1.1694 -0.3145 0.5758 0.185 Uiso 1 1 calc R . . C38 C 1.0894(6) -0.2385(4) 0.5858(4) 0.139(4) Uani 1 1 d . . . H38A H 1.1310 -0.2099 0.5983 0.167 Uiso 1 1 calc R . . C39 C 1.0333(5) 0.0073(3) 0.8146(3) 0.072(2) Uani 1 1 d . . . C40 C 1.1126(5) 0.0310(3) 0.8263(3) 0.094(2) Uani 1 1 d . . . H40A H 1.1440 0.0502 0.7961 0.113 Uiso 1 1 calc R . . C41 C 1.1452(6) 0.0258(4) 0.8836(4) 0.117(3) Uani 1 1 d . . . H41A H 1.1992 0.0408 0.8918 0.140 Uiso 1 1 calc R . . C42 C 1.0988(8) -0.0008(4) 0.9274(4) 0.125(4) Uani 1 1 d . . . H42A H 1.1210 -0.0034 0.9658 0.150 Uiso 1 1 calc R . . C43 C 1.0207(6) -0.0237(4) 0.9167(4) 0.117(3) Uani 1 1 d . . . H43A H 0.9888 -0.0419 0.9472 0.141 Uiso 1 1 calc R . . C44 C 0.9892(5) -0.0197(3) 0.8594(3) 0.094(2) Uani 1 1 d . . . H44A H 0.9358 -0.0361 0.8516 0.113 Uiso 1 1 calc R . . O1 O 0.1146(10) 0.2025(6) 0.6651(5) 0.376(6) Uiso 1 1 d . . . C45 C 0.0564(9) 0.2575(7) 0.6489(6) 0.290(7) Uiso 1 1 d . . . H45A H 0.0147 0.2435 0.6199 0.348 Uiso 1 1 calc R . . H45B H 0.0274 0.2735 0.6840 0.348 Uiso 1 1 calc R . . C46 C 0.1095(10) 0.3063(7) 0.6241(7) 0.290(7) Uiso 1 1 d . . . H46A H 0.0807 0.3321 0.5942 0.348 Uiso 1 1 calc R . . H46B H 0.1336 0.3341 0.6544 0.348 Uiso 1 1 calc R . . C47 C 0.1669(12) 0.2659(9) 0.5999(7) 0.344(9) Uiso 1 1 d . . . H47A H 0.1418 0.2397 0.5687 0.413 Uiso 1 1 calc R . . H47B H 0.2139 0.2899 0.5832 0.413 Uiso 1 1 calc R . . C48 C 0.1907(12) 0.2313(8) 0.6431(8) 0.355(10) Uiso 1 1 d . . . H48A H 0.2174 0.2573 0.6737 0.426 Uiso 1 1 calc R . . H48B H 0.2300 0.1984 0.6299 0.426 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 0.0927(7) 0.0685(6) 0.0581(6) -0.0005(5) -0.0045(6) 0.0158(6) N1 0.076(4) 0.053(3) 0.053(3) -0.002(3) -0.002(3) -0.006(3) N2 0.067(4) 0.056(3) 0.058(4) 0.004(3) -0.002(3) 0.001(3) N3 0.058(4) 0.064(4) 0.066(4) 0.001(3) 0.004(3) -0.002(3) N4 0.048(3) 0.041(3) 0.070(3) -0.005(3) 0.004(3) 0.009(3) C1 0.082(5) 0.051(4) 0.059(4) 0.001(4) -0.009(4) -0.002(4) C2 0.101(6) 0.058(4) 0.081(5) 0.011(4) -0.016(5) 0.007(4) C3 0.100(6) 0.063(5) 0.068(5) 0.007(4) -0.011(4) -0.001(4) C4 0.061(5) 0.071(5) 0.059(4) 0.015(4) -0.003(4) 0.002(4) C5 0.077(5) 0.067(5) 0.056(4) -0.003(4) 0.003(4) 0.004(4) C6 0.079(5) 0.063(5) 0.058(4) -0.004(4) 0.000(4) -0.003(4) C7 0.093(6) 0.069(5) 0.061(4) -0.008(4) 0.000(4) -0.004(4) C8 0.096(6) 0.063(5) 0.070(5) -0.012(4) -0.007(4) 0.009(4) C9 0.073(5) 0.065(5) 0.057(5) 0.001(4) 0.002(4) -0.002(4) C10 0.068(5) 0.061(5) 0.067(5) -0.005(4) 0.006(4) 0.005(4) C11 0.064(5) 0.058(5) 0.076(5) 0.004(4) -0.008(4) 0.008(4) C12 0.084(6) 0.072(5) 0.082(5) -0.002(4) -0.004(5) 0.018(4) C13 0.077(5) 0.076(5) 0.063(5) 0.002(4) -0.007(4) 0.010(4) C14 0.058(5) 0.066(5) 0.056(5) 0.012(4) -0.006(4) 0.002(4) C15 0.060(4) 0.060(4) 0.055(4) 0.004(4) -0.005(4) -0.002(4) C16 0.058(5) 0.062(5) 0.063(5) 0.005(4) -0.007(4) -0.002(4) C17 0.078(5) 0.053(4) 0.053(4) -0.004(3) -0.004(4) 0.017(4) C18 0.066(5) 0.048(4) 0.051(4) 0.002(3) 0.000(4) -0.009(4) C19 0.092(6) 0.072(5) 0.077(5) -0.010(4) 0.012(4) 0.007(4) C20 0.070(5) 0.040(4) 0.077(5) 0.019(4) 0.004(4) -0.011(3) C21 0.080(6) 0.077(6) 0.085(6) -0.004(5) -0.013(5) 0.014(5) C22 0.172(10) 0.128(8) 0.125(8) 0.012(6) 0.039(7) 0.078(7) C23 0.254(15) 0.182(12) 0.117(9) 0.006(9) 0.024(9) 0.126(13) C24 0.217(16) 0.116(10) 0.128(12) -0.060(8) -0.092(11) 0.079(11) C25 0.182(12) 0.076(8) 0.206(13) 0.001(8) -0.031(9) 0.018(8) C26 0.144(8) 0.073(6) 0.197(10) 0.005(7) 0.005(7) 0.026(6) C27 0.069(5) 0.056(4) 0.072(5) -0.006(4) -0.012(4) 0.006(4) C28 0.084(5) 0.084(5) 0.065(5) 0.010(4) -0.009(4) 0.000(4) C29 0.103(7) 0.129(8) 0.071(6) 0.017(5) -0.008(5) 0.014(6) C30 0.113(8) 0.144(9) 0.077(6) -0.013(6) -0.030(6) 0.022(7) C31 0.149(8) 0.117(8) 0.125(8) -0.025(6) -0.071(7) -0.017(6) C32 0.116(7) 0.092(6) 0.094(6) 0.006(5) -0.032(5) -0.016(5) C33 0.079(6) 0.058(5) 0.068(4) -0.002(4) -0.011(4) 0.005(5) C34 0.125(8) 0.063(6) 0.251(10) -0.049(6) -0.058(7) 0.007(6) C35 0.126(9) 0.062(7) 0.286(13) -0.032(7) -0.037(9) -0.004(6) C36 0.139(9) 0.057(6) 0.126(6) -0.013(5) -0.028(7) 0.013(7) C37 0.109(8) 0.072(6) 0.281(13) -0.032(7) 0.007(8) 0.023(6) C38 0.088(7) 0.071(6) 0.257(12) -0.032(6) 0.007(7) -0.007(5) C39 0.087(6) 0.076(5) 0.054(5) -0.002(4) -0.016(5) 0.003(4) C40 0.103(7) 0.110(6) 0.070(6) -0.014(5) -0.022(5) -0.005(5) C41 0.115(8) 0.106(7) 0.130(9) -0.025(7) -0.040(8) 0.011(6) C42 0.200(13) 0.089(8) 0.086(7) -0.017(5) -0.065(8) 0.023(8) C43 0.172(10) 0.117(7) 0.063(6) 0.001(5) -0.014(6) 0.008(7) C44 0.123(7) 0.109(6) 0.050(5) 0.011(4) -0.013(5) -0.008(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 N2 2.017(5) . ? Fe1 N3 2.101(5) . ? Fe1 N1 2.110(4) . ? Fe1 N4 2.117(5) 5_756 ? Fe1 C17 2.341(5) . ? N1 C4 1.370(6) . ? N1 C1 1.394(6) . ? N2 C6 1.372(6) . ? N2 C9 1.376(6) . ? N3 C11 1.380(6) . ? N3 C14 1.410(6) . ? N4 C19 1.404(7) . ? N4 C16 1.403(6) . ? N4 Fe1 2.117(5) 5_756 ? C1 C20 1.377(7) . ? C1 C2 1.432(7) . ? C2 C3 1.335(7) . ? C3 C4 1.442(7) . ? C4 C5 1.424(7) . ? C5 C6 1.396(7) . ? C5 C39 1.482(8) . ? C6 C7 1.424(7) . ? C7 C8 1.326(7) . ? C8 C9 1.443(7) . ? C9 C10 1.386(7) . ? C10 C11 1.394(7) . ? C10 C21 1.506(8) . ? C11 C12 1.420(7) . ? C12 C13 1.347(7) . ? C13 C14 1.405(7) . ? C14 C15 1.397(7) . ? C15 C16 1.420(7) . ? C15 C27 1.490(7) . ? C16 C17 1.393(7) . ? C17 C18 1.390(7) . ? C18 C19 1.409(7) . ? C18 C20 1.415(7) . ? C20 C33 1.483(8) . ? C21 C22 1.319(9) . ? C21 C26 1.372(9) . ? C22 C23 1.381(11) . ? C23 C24 1.282(13) . ? C24 C25 1.367(13) . ? C25 C26 1.393(10) . ? C27 C28 1.365(7) . ? C27 C32 1.371(7) . ? C28 C29 1.393(8) . ? C29 C30 1.329(8) . ? C30 C31 1.360(9) . ? C31 C32 1.365(8) . ? C33 C34 1.310(8) . ? C33 C38 1.327(8) . ? C34 C35 1.391(9) . ? C35 C36 1.298(9) . ? C36 C37 1.313(9) . ? C37 C38 1.402(9) . ? C39 C44 1.345(8) . ? C39 C40 1.375(8) . ? C40 C41 1.388(9) . ? C41 C42 1.343(10) . ? C42 C43 1.349(10) . ? C43 C44 1.379(8) . ? O1 C48 1.433(17) . ? O1 C45 1.510(14) . ? C45 C46 1.428(15) . ? C46 C47 1.350(17) . ? C47 C48 1.263(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 N2 Fe1 N3 87.7(2) . . ? N2 Fe1 N1 88.5(2) . . ? N3 Fe1 N1 144.69(18) . . ? N2 Fe1 N4 110.32(17) . 5_756 ? N3 Fe1 N4 95.30(18) . 5_756 ? N1 Fe1 N4 118.83(18) . 5_756 ? N2 Fe1 C17 143.4(2) . . ? N3 Fe1 C17 81.1(2) . . ? N1 Fe1 C17 81.3(2) . . ? N4 Fe1 C17 105.38(18) 5_756 . ? C4 N1 C1 105.3(5) . . ? C4 N1 Fe1 122.8(4) . . ? C1 N1 Fe1 131.1(4) . . ? C6 N2 C9 105.2(5) . . ? C6 N2 Fe1 126.1(4) . . ? C9 N2 Fe1 127.1(4) . . ? C11 N3 C14 105.1(5) . . ? C11 N3 Fe1 125.1(4) . . ? C14 N3 Fe1 129.1(4) . . ? C19 N4 C16 98.7(5) . . ? C19 N4 Fe1 113.0(4) . 5_756 ? C16 N4 Fe1 127.9(4) . 5_756 ? C20 C1 N1 125.8(6) . . ? C20 C1 C2 124.5(6) . . ? N1 C1 C2 109.7(5) . . ? C3 C2 C1 107.5(6) . . ? C2 C3 C4 107.4(6) . . ? N1 C4 C5 126.5(6) . . ? N1 C4 C3 110.0(6) . . ? C5 C4 C3 123.5(6) . . ? C6 C5 C4 124.7(6) . . ? C6 C5 C39 118.5(6) . . ? C4 C5 C39 116.6(6) . . ? N2 C6 C5 124.5(6) . . ? N2 C6 C7 110.0(6) . . ? C5 C6 C7 125.3(7) . . ? C8 C7 C6 108.2(6) . . ? C7 C8 C9 106.5(6) . . ? N2 C9 C10 124.6(6) . . ? N2 C9 C8 110.0(6) . . ? C10 C9 C8 125.4(7) . . ? C9 C10 C11 125.8(6) . . ? C9 C10 C21 118.3(6) . . ? C11 C10 C21 115.9(6) . . ? N3 C11 C10 125.1(6) . . ? N3 C11 C12 110.2(6) . . ? C10 C11 C12 124.6(7) . . ? C13 C12 C11 106.8(6) . . ? C12 C13 C14 109.0(6) . . ? C15 C14 C13 126.9(6) . . ? C15 C14 N3 124.1(6) . . ? C13 C14 N3 108.8(6) . . ? C14 C15 C16 120.6(6) . . ? C14 C15 C27 119.9(6) . . ? C16 C15 C27 119.4(6) . . ? C17 C16 N4 114.0(5) . . ? C17 C16 C15 125.8(6) . . ? N4 C16 C15 120.1(6) . . ? C18 C17 C16 107.3(5) . . ? C18 C17 Fe1 111.7(4) . . ? C16 C17 Fe1 107.1(4) . . ? C17 C18 C19 103.3(5) . . ? C17 C18 C20 129.4(6) . . ? C19 C18 C20 126.5(6) . . ? N4 C19 C18 115.9(6) . . ? C1 C20 C18 120.0(6) . . ? C1 C20 C33 122.1(6) . . ? C18 C20 C33 117.8(6) . . ? C22 C21 C26 117.3(8) . . ? C22 C21 C10 121.6(9) . . ? C26 C21 C10 121.2(8) . . ? C21 C22 C23 120.9(10) . . ? C24 C23 C22 121.9(14) . . ? C23 C24 C25 121.1(15) . . ? C24 C25 C26 116.6(12) . . ? C21 C26 C25 122.2(9) . . ? C28 C27 C32 118.7(6) . . ? C28 C27 C15 123.9(6) . . ? C32 C27 C15 117.4(7) . . ? C27 C28 C29 118.9(7) . . ? C30 C29 C28 121.5(8) . . ? C29 C30 C31 120.1(9) . . ? C30 C31 C32 119.3(8) . . ? C31 C32 C27 121.4(7) . . ? C34 C33 C38 113.5(7) . . ? C34 C33 C20 122.2(8) . . ? C38 C33 C20 124.2(7) . . ? C33 C34 C35 123.7(8) . . ? C36 C35 C34 121.5(9) . . ? C35 C36 C37 117.4(9) . . ? C36 C37 C38 120.0(9) . . ? C33 C38 C37 123.7(8) . . ? C44 C39 C40 118.8(7) . . ? C44 C39 C5 122.5(7) . . ? C40 C39 C5 118.6(7) . . ? C39 C40 C41 119.3(8) . . ? C42 C41 C40 120.1(10) . . ? C41 C42 C43 121.2(11) . . ? C42 C43 C44 118.5(9) . . ? C39 C44 C43 122.0(8) . . ? C48 O1 C45 96.9(13) . . ? C46 C45 O1 105.4(12) . . ? C47 C46 C45 96.7(13) . . ? C48 C47 C46 104.2(16) . . ? C47 C48 O1 104.4(17) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.67 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.782 _refine_diff_density_min -0.651 _refine_diff_density_rms 0.070 data_h313m _database_code_CSD 184399 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C108 H95 Fe2 N8 Na O8' _chemical_formula_weight 1767.61 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Fe' 'Fe' 0.3463 0.8444 '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' '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' 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 28.473(3) _cell_length_b 18.7702(18) _cell_length_c 16.8963(16) _cell_angle_alpha 90.00 _cell_angle_beta 104.922(2) _cell_angle_gamma 90.00 _cell_volume 8725.6(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Brown _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.346 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3704 _exptl_absorpt_coefficient_mu 0.404 _exptl_absorpt_correction_type 'Empirical Used SADABS' _exptl_absorpt_correction_T_min 0.6301 _exptl_absorpt_correction_T_max 0.9486 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24722 _diffrn_reflns_av_R_equivalents 0.0936 _diffrn_reflns_av_sigmaI/netI 0.1360 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 25.02 _reflns_number_total 7695 _reflns_number_gt 3643 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.1194P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7695 _refine_ls_number_parameters 578 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1538 _refine_ls_R_factor_gt 0.0702 _refine_ls_wR_factor_ref 0.2238 _refine_ls_wR_factor_gt 0.1815 _refine_ls_goodness_of_fit_ref 0.924 _refine_ls_restrained_S_all 0.924 _refine_ls_shift/su_max 0.005 _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 0.98931(3) 0.68950(4) 0.35312(5) 0.0337(3) Uani 1 1 d . . . O1 O 1.0000 0.6565(3) 0.2500 0.0437(14) Uani 1 2 d S . . H1A H 1.0000 0.6070 0.2500 0.052 Uiso 1 2 calc SR . . O2 O 0.99221(15) 0.6348(2) 0.4529(2) 0.0438(10) Uani 1 1 d . . . N1 N 1.06113(17) 0.7182(2) 0.4113(3) 0.0354(11) Uani 1 1 d . . . N2 N 0.96972(16) 0.7929(2) 0.3505(3) 0.0326(11) Uani 1 1 d . . . N3 N 0.91616(17) 0.6590(2) 0.3208(3) 0.0354(11) Uani 1 1 d . . . N4 N 1.00349(18) 0.4704(3) 0.3493(3) 0.0403(12) Uani 1 1 d . . . C1 C 1.0998(2) 0.6733(3) 0.4469(3) 0.0365(14) Uani 1 1 d . . . C2 C 1.1399(2) 0.7144(3) 0.4911(3) 0.0398(15) Uani 1 1 d . . . H2 H 1.1697 0.6968 0.5211 0.048 Uiso 1 1 calc R . . C3 C 1.1269(2) 0.7833(3) 0.4817(3) 0.0377(14) Uani 1 1 d . . . H3 H 1.1461 0.8222 0.5036 0.045 Uiso 1 1 calc R . . C4 C 1.0780(2) 0.7859(3) 0.4314(3) 0.0353(14) Uani 1 1 d . . . C5 C 1.0505(2) 0.8485(3) 0.4065(3) 0.0319(13) Uani 1 1 d . . . C6 C 1.0015(2) 0.8511(3) 0.3661(3) 0.0320(13) Uani 1 1 d . . . C7 C 0.9745(2) 0.9140(3) 0.3359(3) 0.0324(13) Uani 1 1 d . . . H7 H 0.9869 0.9600 0.3384 0.039 Uiso 1 1 calc R . . C8 C 0.9278(2) 0.8950(3) 0.3033(3) 0.0342(13) Uani 1 1 d . . . H8 H 0.9025 0.9255 0.2790 0.041 Uiso 1 1 calc R . . C9 C 0.92424(19) 0.8190(3) 0.3127(3) 0.0321(13) Uani 1 1 d . . . C10 C 0.8809(2) 0.7799(3) 0.2912(3) 0.0334(13) Uani 1 1 d . . . C11 C 0.8770(2) 0.7045(3) 0.2997(3) 0.0357(14) Uani 1 1 d . . . C12 C 0.8324(2) 0.6658(3) 0.2881(3) 0.0395(14) Uani 1 1 d . . . H12 H 0.8011 0.6845 0.2737 0.047 Uiso 1 1 calc R . . C13 C 0.8450(2) 0.5964(3) 0.3024(3) 0.0414(15) Uani 1 1 d . . . H13 H 0.8235 0.5586 0.3000 0.050 Uiso 1 1 calc R . . C14 C 0.8967(2) 0.5912(3) 0.3217(3) 0.0361(14) Uani 1 1 d . . . C15 C 0.9244(2) 0.5270(3) 0.3351(3) 0.0360(14) Uani 1 1 d . . . C16 C 0.9745(2) 0.5271(3) 0.3671(3) 0.0368(14) Uani 1 1 d . . . C17 C 1.0058(2) 0.5797(3) 0.4139(3) 0.0371(14) Uani 1 1 d . . . C18 C 1.0544(2) 0.5593(3) 0.4169(3) 0.0354(14) Uani 1 1 d . . . C19 C 1.0489(2) 0.4906(3) 0.3783(3) 0.0390(14) Uani 1 1 d . . . H19A H 1.0752 0.4627 0.3741 0.047 Uiso 1 1 calc R . . C20 C 1.0982(2) 0.5975(3) 0.4426(3) 0.0365(14) Uani 1 1 d . . . C21 C 1.0767(2) 0.9177(3) 0.4270(3) 0.0349(14) Uani 1 1 d . . . C22 C 1.1181(2) 0.9330(3) 0.4009(3) 0.0365(14) Uani 1 1 d . . . H22 H 1.1291 0.8998 0.3689 0.044 Uiso 1 1 calc R . . C23 C 1.1435(2) 0.9962(3) 0.4212(3) 0.0428(15) Uani 1 1 d . . . H23 H 1.1709 1.0050 0.4026 0.051 Uiso 1 1 calc R . . C24 C 1.1279(2) 1.0463(3) 0.4692(4) 0.0472(16) Uani 1 1 d . . . H24 H 1.1448 1.0889 0.4831 0.057 Uiso 1 1 calc R . . C25 C 1.0870(2) 1.0319(3) 0.4959(3) 0.0457(16) Uani 1 1 d . . . H25 H 1.0762 1.0651 0.5281 0.055 Uiso 1 1 calc R . . C26 C 1.0619(2) 0.9690(3) 0.4756(3) 0.0405(15) Uani 1 1 d . . . H26 H 1.0345 0.9605 0.4945 0.049 Uiso 1 1 calc R . . C27 C 0.8346(2) 0.8191(3) 0.2547(3) 0.0338(13) Uani 1 1 d . . . C28 C 0.8090(2) 0.8053(3) 0.1745(3) 0.0402(14) Uani 1 1 d . . . H28 H 0.8200 0.7702 0.1448 0.048 Uiso 1 1 calc R . . C29 C 0.7672(2) 0.8430(4) 0.1381(4) 0.0505(17) Uani 1 1 d . . . H29 H 0.7511 0.8339 0.0838 0.061 Uiso 1 1 calc R . . C30 C 0.7496(2) 0.8931(4) 0.1808(5) 0.060(2) Uani 1 1 d . . . H30 H 0.7211 0.9175 0.1562 0.072 Uiso 1 1 calc R . . C31 C 0.7740(2) 0.9075(4) 0.2602(5) 0.0573(18) Uani 1 1 d . . . H31 H 0.7623 0.9423 0.2893 0.069 Uiso 1 1 calc R . . C32 C 0.8166(2) 0.8702(3) 0.2982(4) 0.0463(16) Uani 1 1 d . . . H32 H 0.8327 0.8799 0.3523 0.056 Uiso 1 1 calc R . . C33 C 0.8995(2) 0.4585(3) 0.3089(3) 0.0346(14) Uani 1 1 d . . . C34 C 0.8646(2) 0.4512(3) 0.2332(3) 0.0434(15) Uani 1 1 d . . . H34 H 0.8560 0.4906 0.1992 0.052 Uiso 1 1 calc R . . C35 C 0.8429(2) 0.3858(3) 0.2088(4) 0.0497(17) Uani 1 1 d . . . H35 H 0.8201 0.3820 0.1586 0.060 Uiso 1 1 calc R . . C36 C 0.8546(2) 0.3270(3) 0.2577(4) 0.0499(17) Uani 1 1 d . . . H36 H 0.8395 0.2835 0.2413 0.060 Uiso 1 1 calc R . . C37 C 0.8894(3) 0.3332(3) 0.3322(4) 0.0512(17) Uani 1 1 d . . . H37 H 0.8980 0.2931 0.3651 0.061 Uiso 1 1 calc R . . C38 C 0.9114(2) 0.3973(3) 0.3582(3) 0.0400(15) Uani 1 1 d . . . H38 H 0.9342 0.4002 0.4086 0.048 Uiso 1 1 calc R . . C39 C 1.1450(2) 0.5572(3) 0.4614(3) 0.0389(14) Uani 1 1 d . . . C40 C 1.1490(2) 0.4937(3) 0.5055(3) 0.0437(15) Uani 1 1 d . . . H40 H 1.1235 0.4784 0.5263 0.052 Uiso 1 1 calc R . . C41 C 1.1913(3) 0.4533(3) 0.5180(4) 0.0539(18) Uani 1 1 d . . . H41 H 1.1942 0.4108 0.5472 0.065 Uiso 1 1 calc R . . C42 C 1.2291(3) 0.4765(4) 0.4871(4) 0.0583(19) Uani 1 1 d . . . H42 H 1.2572 0.4492 0.4950 0.070 Uiso 1 1 calc R . . C43 C 1.2255(2) 0.5388(4) 0.4452(4) 0.0512(17) Uani 1 1 d . . . H43 H 1.2514 0.5545 0.4258 0.061 Uiso 1 1 calc R . . C44 C 1.1833(2) 0.5790(3) 0.4313(4) 0.0447(15) Uani 1 1 d . . . H44 H 1.1809 0.6211 0.4015 0.054 Uiso 1 1 calc R . . Na1 Na 1.0000 0.3767(2) 0.2500 0.0834(14) Uani 1 2 d S . . O4 O 1.0377(2) 0.2921(3) 0.3449(3) 0.099(2) Uani 1 1 d . . . C45 C 1.0763(4) 0.3037(5) 0.4170(6) 0.110(3) Uani 1 1 d . . . H45A H 1.0703 0.3466 0.4449 0.132 Uiso 1 1 calc R . . H45B H 1.1070 0.3089 0.4028 0.132 Uiso 1 1 calc R . . C46 C 1.0775(4) 0.2409(5) 0.4698(5) 0.090(3) Uani 1 1 d . . . H46A H 1.0834 0.2545 0.5269 0.108 Uiso 1 1 calc R . . H46B H 1.1021 0.2071 0.4638 0.108 Uiso 1 1 calc R . . C47 C 1.0263(5) 0.2106(6) 0.4370(6) 0.119(4) Uani 1 1 d . . . H47A H 1.0278 0.1593 0.4314 0.143 Uiso 1 1 calc R . . H47B H 1.0066 0.2213 0.4744 0.143 Uiso 1 1 calc R . . C48 C 1.0071(5) 0.2403(9) 0.3643(9) 0.242(11) Uani 1 1 d . . . H48A H 0.9763 0.2621 0.3647 0.291 Uiso 1 1 calc R . . H48B H 1.0009 0.2037 0.3225 0.291 Uiso 1 1 calc R . . O5 O 0.1707(5) 0.1438(5) 0.2830(7) 0.225(6) Uani 1 1 d . . . C49 C 0.1165(5) 0.1288(8) 0.2551(7) 0.170(6) Uani 1 1 d . . . H49A H 0.1089 0.0899 0.2876 0.204 Uiso 1 1 calc R . . H49B H 0.0990 0.1706 0.2660 0.204 Uiso 1 1 calc R . . C50 C 0.0997(7) 0.1114(6) 0.1731(7) 0.252(12) Uani 1 1 d . . . H50A H 0.0883 0.1525 0.1387 0.302 Uiso 1 1 calc R . . H50B H 0.0750 0.0746 0.1632 0.302 Uiso 1 1 calc R . . C51 C 0.1543(5) 0.0813(7) 0.1645(8) 0.152(5) Uani 1 1 d . . . H51A H 0.1579 0.0317 0.1810 0.182 Uiso 1 1 calc R . . H51B H 0.1552 0.0839 0.1076 0.182 Uiso 1 1 calc R . . C52 C 0.1955(5) 0.1226(8) 0.2153(11) 0.234(10) Uani 1 1 d . . . H52A H 0.2036 0.1637 0.1865 0.281 Uiso 1 1 calc R . . H52B H 0.2242 0.0935 0.2360 0.281 Uiso 1 1 calc R . . C54 C 0.7393(4) 0.2581(5) 0.0629(7) 0.102(3) Uani 1 1 d . . . O3 O 0.7176(5) 0.3112(7) 0.0163(8) 0.103(4) Uani 0.50 1 d P . . C53 C 0.7823(4) 0.2254(8) 0.0507(7) 0.140(5) 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 0.0295(5) 0.0337(5) 0.0369(4) 0.0023(4) 0.0064(3) 0.0022(4) O1 0.044(4) 0.046(3) 0.040(3) 0.000 0.008(3) 0.000 O2 0.044(3) 0.044(2) 0.042(2) 0.000(2) 0.0092(19) -0.001(2) N1 0.034(3) 0.036(3) 0.036(3) 0.002(2) 0.007(2) 0.002(2) N2 0.023(3) 0.035(3) 0.038(3) 0.004(2) 0.004(2) -0.001(2) N3 0.036(3) 0.035(3) 0.034(3) 0.005(2) 0.008(2) 0.002(2) N4 0.042(4) 0.041(3) 0.038(3) 0.007(2) 0.010(2) 0.007(3) C1 0.030(3) 0.044(4) 0.034(3) 0.002(3) 0.006(3) 0.005(3) C2 0.029(4) 0.044(4) 0.043(3) -0.001(3) 0.003(3) 0.007(3) C3 0.034(4) 0.040(4) 0.037(3) 0.000(3) 0.004(3) -0.002(3) C4 0.029(3) 0.040(4) 0.036(3) 0.001(3) 0.006(3) 0.000(3) C5 0.028(4) 0.039(3) 0.029(3) 0.002(3) 0.009(2) 0.001(3) C6 0.030(4) 0.036(3) 0.030(3) -0.004(3) 0.009(3) 0.004(3) C7 0.030(4) 0.035(3) 0.034(3) 0.000(3) 0.011(3) 0.002(3) C8 0.032(4) 0.036(3) 0.034(3) 0.004(3) 0.008(3) 0.003(3) C9 0.024(3) 0.036(3) 0.037(3) -0.001(3) 0.008(2) 0.005(3) C10 0.028(3) 0.035(3) 0.036(3) 0.004(3) 0.006(2) 0.003(3) C11 0.028(3) 0.041(4) 0.036(3) 0.004(3) 0.004(2) 0.001(3) C12 0.033(4) 0.046(4) 0.039(3) 0.005(3) 0.008(3) 0.001(3) C13 0.034(4) 0.044(4) 0.046(3) 0.003(3) 0.011(3) -0.003(3) C14 0.036(4) 0.035(4) 0.037(3) 0.002(3) 0.009(3) -0.003(3) C15 0.035(4) 0.036(3) 0.039(3) 0.005(3) 0.013(3) -0.004(3) C16 0.040(4) 0.035(3) 0.037(3) 0.006(3) 0.013(3) 0.002(3) C17 0.040(4) 0.033(3) 0.037(3) 0.003(3) 0.007(3) 0.001(3) C18 0.032(4) 0.037(3) 0.038(3) 0.004(3) 0.009(3) 0.001(3) C19 0.039(4) 0.042(4) 0.037(3) 0.002(3) 0.012(3) 0.007(3) C20 0.036(4) 0.041(4) 0.031(3) 0.005(3) 0.006(3) 0.005(3) C21 0.031(3) 0.040(3) 0.032(3) 0.002(3) 0.002(2) 0.007(3) C22 0.034(4) 0.041(3) 0.034(3) -0.002(3) 0.008(3) 0.001(3) C23 0.032(4) 0.050(4) 0.047(3) -0.002(3) 0.011(3) -0.003(3) C24 0.044(4) 0.042(4) 0.055(4) -0.009(3) 0.010(3) -0.009(3) C25 0.053(4) 0.041(4) 0.043(3) -0.010(3) 0.012(3) 0.001(3) C26 0.038(4) 0.043(4) 0.043(3) -0.007(3) 0.016(3) 0.001(3) C27 0.026(3) 0.035(3) 0.041(3) 0.007(3) 0.009(3) -0.004(3) C28 0.028(3) 0.051(4) 0.043(3) 0.006(3) 0.011(3) -0.001(3) C29 0.028(4) 0.067(5) 0.050(4) 0.014(4) 0.000(3) -0.005(3) C30 0.027(4) 0.056(5) 0.090(6) 0.025(4) 0.000(4) 0.001(3) C31 0.039(4) 0.054(4) 0.081(5) 0.002(4) 0.021(4) 0.009(4) C32 0.035(4) 0.048(4) 0.055(4) 0.000(3) 0.009(3) 0.001(3) C33 0.031(4) 0.035(3) 0.040(3) 0.000(3) 0.012(3) -0.001(3) C34 0.043(4) 0.047(4) 0.043(3) 0.003(3) 0.016(3) -0.004(3) C35 0.047(4) 0.054(4) 0.047(4) -0.004(3) 0.009(3) -0.016(3) C36 0.051(4) 0.044(4) 0.057(4) -0.007(3) 0.016(3) -0.018(3) C37 0.069(5) 0.033(4) 0.058(4) 0.004(3) 0.028(4) -0.003(3) C38 0.047(4) 0.039(4) 0.035(3) 0.002(3) 0.013(3) -0.003(3) C39 0.038(4) 0.037(3) 0.039(3) -0.006(3) 0.006(3) 0.006(3) C40 0.043(4) 0.040(4) 0.042(3) 0.000(3) 0.001(3) 0.011(3) C41 0.057(5) 0.041(4) 0.053(4) -0.009(3) -0.007(3) 0.013(4) C42 0.039(5) 0.056(5) 0.071(5) -0.018(4) -0.002(4) 0.008(4) C43 0.031(4) 0.059(5) 0.062(4) -0.023(4) 0.008(3) -0.001(3) C44 0.040(4) 0.045(4) 0.048(3) -0.011(3) 0.007(3) -0.003(3) Na1 0.115(4) 0.061(3) 0.061(2) 0.000 0.001(2) 0.000 O4 0.119(6) 0.087(4) 0.077(4) 0.019(3) 0.002(4) 0.003(4) C45 0.109(9) 0.108(8) 0.102(8) 0.035(6) 0.009(6) 0.001(7) C46 0.114(8) 0.095(7) 0.069(5) 0.028(5) 0.038(5) 0.025(6) C47 0.156(11) 0.124(9) 0.083(7) 0.021(6) 0.043(7) -0.029(8) C48 0.120(12) 0.34(2) 0.246(18) 0.236(18) 0.007(11) -0.037(13) O5 0.256(13) 0.126(7) 0.215(11) -0.085(7) -0.077(9) 0.041(8) C49 0.170(14) 0.191(14) 0.099(9) 0.020(9) -0.055(8) -0.064(11) C50 0.46(3) 0.084(8) 0.114(10) -0.044(7) -0.103(14) 0.117(13) C51 0.132(12) 0.135(11) 0.156(12) 0.013(9) -0.021(9) 0.026(9) C52 0.103(11) 0.203(15) 0.37(2) -0.223(17) 0.006(13) 0.015(10) C54 0.124(9) 0.079(7) 0.115(8) -0.007(6) 0.052(7) -0.003(6) O3 0.110(11) 0.098(10) 0.092(9) -0.005(8) 0.009(8) 0.017(8) C53 0.116(10) 0.207(14) 0.093(8) -0.052(8) 0.019(7) 0.024(9) _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 O1 1.945(2) . ? Fe1 O2 1.957(4) . ? Fe1 N2 2.017(4) . ? Fe1 N3 2.093(5) . ? Fe1 N1 2.098(5) . ? Fe1 C17 2.296(5) . ? O1 Fe1 1.945(2) 2_755 ? O2 C17 1.336(6) . ? N1 C4 1.369(7) . ? N1 C1 1.394(7) . ? N2 C9 1.378(7) . ? N2 C6 1.398(7) . ? N3 C11 1.376(7) . ? N3 C14 1.389(7) . ? N4 C19 1.315(7) . ? N4 C16 1.427(7) . ? N4 Na1 2.414(6) . ? C1 C2 1.421(8) . ? C1 C20 1.424(8) . ? C2 C3 1.344(8) . ? C3 C4 1.434(8) . ? C4 C5 1.414(8) . ? C5 C6 1.389(7) . ? C5 C21 1.493(8) . ? C6 C7 1.430(7) . ? C7 C8 1.348(7) . ? C8 C9 1.441(7) . ? C9 C10 1.400(7) . ? C10 C11 1.431(8) . ? C10 C27 1.497(8) . ? C11 C12 1.433(8) . ? C12 C13 1.357(8) . ? C13 C14 1.427(8) . ? C14 C15 1.426(8) . ? C15 C16 1.389(8) . ? C15 C33 1.479(8) . ? C16 C17 1.425(8) . ? C17 C18 1.425(8) . ? C18 C20 1.406(8) . ? C18 C19 1.437(8) . ? C19 Na1 3.106(6) . ? C20 C39 1.495(8) . ? C21 C22 1.392(8) . ? C21 C26 1.399(7) . ? C22 C23 1.385(8) . ? C23 C24 1.388(8) . ? C24 C25 1.382(8) . ? C25 C26 1.375(8) . ? C27 C32 1.385(8) . ? C27 C28 1.388(8) . ? C28 C29 1.384(8) . ? C29 C30 1.358(9) . ? C30 C31 1.371(9) . ? C31 C32 1.405(9) . ? C33 C38 1.409(8) . ? C33 C34 1.410(8) . ? C34 C35 1.388(8) . ? C35 C36 1.367(8) . ? C36 C37 1.393(9) . ? C37 C38 1.376(8) . ? C39 C44 1.378(8) . ? C39 C40 1.395(8) . ? C40 C41 1.393(8) . ? C41 C42 1.381(9) . ? C42 C43 1.357(9) . ? C43 C44 1.387(8) . ? Na1 O4 2.315(6) 2_755 ? Na1 O4 2.315(6) . ? Na1 N4 2.414(6) 2_755 ? Na1 C19 3.106(6) 2_755 ? O4 C48 1.400(12) . ? O4 C45 1.430(10) . ? C45 C46 1.472(11) . ? C46 C47 1.528(13) . ? C47 C48 1.331(13) . ? O5 C49 1.522(16) . ? O5 C52 1.544(18) . ? C49 C50 1.384(14) . ? C50 C51 1.69(2) . ? C51 C52 1.483(15) . ? C54 O3 1.319(14) . ? C54 C53 1.431(14) . ? C54 C53 1.883(15) 7_655 ? O3 C53 1.325(15) 7_655 ? C53 O3 1.325(15) 7_655 ? C53 C54 1.883(15) 7_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Fe1 O2 128.6(2) . . ? O1 Fe1 N2 113.1(2) . . ? O2 Fe1 N2 118.27(17) . . ? O1 Fe1 N3 93.10(13) . . ? O2 Fe1 N3 84.23(17) . . ? N2 Fe1 N3 90.40(18) . . ? O1 Fe1 N1 98.20(13) . . ? O2 Fe1 N1 84.92(17) . . ? N2 Fe1 N1 89.64(18) . . ? N3 Fe1 N1 167.69(17) . . ? O1 Fe1 C17 93.1(2) . . ? O2 Fe1 C17 35.49(17) . . ? N2 Fe1 C17 153.76(19) . . ? N3 Fe1 C17 86.89(19) . . ? N1 Fe1 C17 87.64(19) . . ? Fe1 O1 Fe1 142.9(3) 2_755 . ? C17 O2 Fe1 86.2(3) . . ? C4 N1 C1 105.5(5) . . ? C4 N1 Fe1 126.2(4) . . ? C1 N1 Fe1 127.8(4) . . ? C9 N2 C6 107.1(4) . . ? C9 N2 Fe1 125.0(4) . . ? C6 N2 Fe1 125.8(4) . . ? C11 N3 C14 105.8(5) . . ? C11 N3 Fe1 125.6(4) . . ? C14 N3 Fe1 128.4(4) . . ? C19 N4 C16 105.9(5) . . ? C19 N4 Na1 109.2(4) . . ? C16 N4 Na1 140.1(4) . . ? N1 C1 C2 109.7(5) . . ? N1 C1 C20 124.8(5) . . ? C2 C1 C20 125.5(5) . . ? C3 C2 C1 107.5(5) . . ? C2 C3 C4 107.3(5) . . ? N1 C4 C5 124.5(5) . . ? N1 C4 C3 109.9(5) . . ? C5 C4 C3 125.6(5) . . ? C6 C5 C4 125.7(5) . . ? C6 C5 C21 117.5(5) . . ? C4 C5 C21 116.7(5) . . ? C5 C6 N2 125.8(5) . . ? C5 C6 C7 125.8(5) . . ? N2 C6 C7 108.4(5) . . ? C8 C7 C6 108.1(5) . . ? C7 C8 C9 107.9(5) . . ? N2 C9 C10 126.5(5) . . ? N2 C9 C8 108.6(5) . . ? C10 C9 C8 124.9(5) . . ? C9 C10 C11 125.3(5) . . ? C9 C10 C27 118.3(5) . . ? C11 C10 C27 116.4(5) . . ? N3 C11 C10 124.2(5) . . ? N3 C11 C12 110.6(5) . . ? C10 C11 C12 125.2(5) . . ? C13 C12 C11 106.1(5) . . ? C12 C13 C14 108.4(5) . . ? N3 C14 C15 124.7(5) . . ? N3 C14 C13 109.1(5) . . ? C15 C14 C13 126.2(5) . . ? C16 C15 C14 122.1(5) . . ? C16 C15 C33 118.8(5) . . ? C14 C15 C33 119.0(5) . . ? C15 C16 C17 130.6(5) . . ? C15 C16 N4 120.6(5) . . ? C17 C16 N4 108.7(5) . . ? O2 C17 C16 126.2(5) . . ? O2 C17 C18 126.3(5) . . ? C16 C17 C18 107.3(5) . . ? O2 C17 Fe1 58.3(3) . . ? C16 C17 Fe1 110.3(4) . . ? C18 C17 Fe1 110.0(4) . . ? C20 C18 C17 130.5(5) . . ? C20 C18 C19 125.7(5) . . ? C17 C18 C19 103.5(5) . . ? N4 C19 C18 114.2(5) . . ? N4 C19 Na1 47.2(3) . . ? C18 C19 Na1 155.8(4) . . ? C18 C20 C1 122.6(5) . . ? C18 C20 C39 118.6(5) . . ? C1 C20 C39 118.7(5) . . ? C22 C21 C26 116.8(5) . . ? C22 C21 C5 121.2(5) . . ? C26 C21 C5 122.0(5) . . ? C23 C22 C21 122.0(5) . . ? C22 C23 C24 120.1(6) . . ? C25 C24 C23 118.8(6) . . ? C26 C25 C24 120.9(6) . . ? C25 C26 C21 121.6(6) . . ? C32 C27 C28 118.3(6) . . ? C32 C27 C10 121.9(5) . . ? C28 C27 C10 119.8(5) . . ? C29 C28 C27 120.9(6) . . ? C30 C29 C28 120.8(6) . . ? C29 C30 C31 119.5(6) . . ? C30 C31 C32 120.7(7) . . ? C27 C32 C31 119.8(6) . . ? C38 C33 C34 117.6(5) . . ? C38 C33 C15 120.6(5) . . ? C34 C33 C15 121.9(5) . . ? C35 C34 C33 120.8(6) . . ? C36 C35 C34 120.9(6) . . ? C35 C36 C37 119.0(6) . . ? C38 C37 C36 121.4(6) . . ? C37 C38 C33 120.3(6) . . ? C44 C39 C40 119.2(6) . . ? C44 C39 C20 121.2(5) . . ? C40 C39 C20 119.4(5) . . ? C41 C40 C39 119.6(6) . . ? C42 C41 C40 119.9(6) . . ? C43 C42 C41 120.5(6) . . ? C42 C43 C44 120.3(7) . . ? C39 C44 C43 120.5(6) . . ? O4 Na1 O4 93.4(3) 2_755 . ? O4 Na1 N4 155.4(2) 2_755 . ? O4 Na1 N4 95.13(18) . . ? O4 Na1 N4 95.13(18) 2_755 2_755 ? O4 Na1 N4 155.4(2) . 2_755 ? N4 Na1 N4 86.6(2) . 2_755 ? O4 Na1 C19 179.0(2) 2_755 . ? O4 Na1 C19 86.79(18) . . ? N4 Na1 C19 23.56(15) . . ? N4 Na1 C19 85.14(18) 2_755 . ? O4 Na1 C19 86.79(18) 2_755 2_755 ? O4 Na1 C19 179.0(2) . 2_755 ? N4 Na1 C19 85.14(18) . 2_755 ? N4 Na1 C19 23.56(15) 2_755 2_755 ? C19 Na1 C19 93.1(2) . 2_755 ? C48 O4 C45 107.0(8) . . ? C48 O4 Na1 115.7(7) . . ? C45 O4 Na1 127.1(5) . . ? O4 C45 C46 106.7(8) . . ? C45 C46 C47 102.0(8) . . ? C48 C47 C46 107.8(9) . . ? C47 C48 O4 112.0(11) . . ? C49 O5 C52 110.1(9) . . ? C50 C49 O5 114.5(15) . . ? C49 C50 C51 94.4(12) . . ? C52 C51 C50 112.5(11) . . ? C51 C52 O5 96.8(11) . . ? O3 C54 C53 121.5(11) . . ? O3 C54 C53 44.7(7) . 7_655 ? C53 C54 C53 89.4(8) . 7_655 ? C54 O3 C53 90.8(11) . 7_655 ? O3 C53 C54 122.4(11) 7_655 . ? O3 C53 C54 44.4(7) 7_655 7_655 ? C54 C53 C54 90.6(8) . 7_655 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.392 _refine_diff_density_min -0.822 _refine_diff_density_rms 0.140