# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Pablo Albores' _publ_contact_author_email ALBORES@QI.FCEN.UBA.AR _publ_section_title ; Rational design of covalently bridged [FeIII2MIIO] clusters ; loop_ _publ_author_name 'Pablo Albores' 'Eva Rentschler' # Attachment 'albores_et_al.cif' data_pa_429_0m _database_code_depnum_ccdc_archive 'CCDC 750190' #TrackingRef 'albores_et_al.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H67 Co Fe2 N3 O14' _chemical_formula_weight 1008.62 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.4643(4) _cell_length_b 12.0792(5) _cell_length_c 19.9530(7) _cell_angle_alpha 77.597(2) _cell_angle_beta 88.046(2) _cell_angle_gamma 72.215(2) _cell_volume 2568.15(17) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.304 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1062 _exptl_absorpt_coefficient_mu 0.937 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.7880 _exptl_absorpt_correction_T_max 0.8959 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 54053 _diffrn_reflns_av_R_equivalents 0.0694 _diffrn_reflns_av_sigmaI/netI 0.0659 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.05 _diffrn_reflns_theta_max 27.52 _reflns_number_total 11748 _reflns_number_gt 7838 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0570P)^2^+0.2334P] 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 11748 _refine_ls_number_parameters 565 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0854 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.1209 _refine_ls_wR_factor_gt 0.1016 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O14 O 0.74752(19) 0.35239(19) 0.33556(11) 0.0336(5) Uani 1 1 d . . . C42 C 0.8589(5) 0.3728(5) 0.4635(2) 0.0899(18) Uani 1 1 d . . . H42A H 0.9320 0.3625 0.4912 0.135 Uiso 1 1 calc R . . H42B H 0.8496 0.2948 0.4638 0.135 Uiso 1 1 calc R . . H42C H 0.7864 0.4212 0.4830 0.135 Uiso 1 1 calc R . . C41 C 0.9823(4) 0.3601(5) 0.3575(3) 0.108(2) Uani 1 1 d . . . H41A H 0.9900 0.4018 0.3104 0.162 Uiso 1 1 calc R . . H41B H 0.9706 0.2834 0.3567 0.162 Uiso 1 1 calc R . . H41C H 1.0569 0.3468 0.3845 0.162 Uiso 1 1 calc R . . Fe1 Fe 0.61253(4) 0.47095(3) 0.12065(2) 0.02202(11) Uani 1 1 d . . . Fe2 Fe 0.61563(4) 0.33588(4) 0.27809(2) 0.02287(11) Uani 1 1 d . . . Co1 Co 0.58271(4) 0.62878(4) 0.24013(2) 0.02829(11) Uani 1 1 d . . . O1 O 0.59046(17) 0.47630(16) 0.21396(9) 0.0228(4) Uani 1 1 d . . . O10 O 0.48086(17) 0.38335(17) 0.11918(10) 0.0249(4) Uani 1 1 d . . . O5 O 0.75219(18) 0.31319(17) 0.13692(10) 0.0292(5) Uani 1 1 d . . . O6 O 0.73586(18) 0.56286(18) 0.10291(10) 0.0285(5) Uani 1 1 d . . . O4 O 0.75113(19) 0.21247(18) 0.24466(11) 0.0328(5) Uani 1 1 d . . . O9 O 0.47384(18) 0.62470(17) 0.07704(10) 0.0289(5) Uani 1 1 d . . . O3 O 0.48387(19) 0.39688(18) 0.34530(11) 0.0315(5) Uani 1 1 d . . . O12 O 0.6378(2) 0.45655(18) 0.01532(11) 0.0281(5) Uani 1 1 d D . . O13 O 0.6776(2) 0.5477(2) 0.33263(11) 0.0360(5) Uani 1 1 d . . . O8 O 0.4969(2) 0.73631(18) 0.14834(10) 0.0327(5) Uani 1 1 d . . . O7 O 0.74719(19) 0.6315(2) 0.19754(11) 0.0336(5) Uani 1 1 d . . . O11 O 0.49371(19) 0.28664(19) 0.22918(10) 0.0326(5) Uani 1 1 d . . . O2 O 0.58550(19) 0.20790(18) 0.37000(10) 0.0290(5) Uani 1 1 d . . . N2 N 0.5599(2) 0.7889(2) 0.27562(13) 0.0310(6) Uani 1 1 d . . . C21 C 0.7979(3) 0.2284(3) 0.18615(15) 0.0256(6) Uani 1 1 d . . . C6 C 0.4435(3) 0.3224(2) 0.16998(15) 0.0242(6) Uani 1 1 d . . . N1 N 0.4008(2) 0.6706(2) 0.27803(12) 0.0265(5) Uani 1 1 d . . . C11 C 0.4486(3) 0.7234(2) 0.09729(15) 0.0264(6) Uani 1 1 d . . . C30 C 0.3653(3) 0.7654(3) 0.30819(15) 0.0292(7) Uani 1 1 d . . . C16 C 0.7812(3) 0.6141(3) 0.13910(15) 0.0254(6) Uani 1 1 d . . . C1 C 0.5058(3) 0.2950(3) 0.38539(15) 0.0270(7) Uani 1 1 d . . . C31 C 0.4564(3) 0.8290(3) 0.30853(15) 0.0297(7) Uani 1 1 d . . . C2 C 0.4335(3) 0.2853(3) 0.45129(17) 0.0381(8) Uani 1 1 d . . . C17 C 0.8852(3) 0.6631(3) 0.10839(15) 0.0282(7) Uani 1 1 d . . . C22 C 0.9195(3) 0.1353(3) 0.17620(16) 0.0308(7) Uani 1 1 d . . . C32 C 0.4373(3) 0.9260(3) 0.33924(17) 0.0398(8) Uani 1 1 d . . . H32 H 0.3646 0.9523 0.3634 0.048 Uiso 1 1 calc R . . C38 C 0.7557(3) 0.4481(3) 0.34923(15) 0.0319(7) Uani 1 1 d . . . C7 C 0.3266(3) 0.2890(3) 0.16211(16) 0.0301(7) Uani 1 1 d . . . C20 C 0.9585(3) 0.5871(3) 0.06051(18) 0.0429(9) Uani 1 1 d . . . H20A H 0.9040 0.5865 0.0239 0.064 Uiso 1 1 calc R . . H20B H 0.9959 0.5055 0.0865 0.064 Uiso 1 1 calc R . . H20C H 1.0230 0.6202 0.0403 0.064 Uiso 1 1 calc R . . C12 C 0.3525(3) 0.8305(3) 0.05542(17) 0.0364(8) Uani 1 1 d . . . C26 C 0.3207(3) 0.6134(3) 0.27132(17) 0.0339(7) Uani 1 1 d . . . H26 H 0.3458 0.5477 0.2495 0.041 Uiso 1 1 calc R . . C33 C 0.5253(4) 0.9834(3) 0.33411(18) 0.0470(9) Uani 1 1 d . . . H33 H 0.5136 1.0499 0.3546 0.056 Uiso 1 1 calc R . . C18 C 0.9676(3) 0.6667(4) 0.16556(18) 0.0456(9) Uani 1 1 d . . . H18A H 0.9188 0.7165 0.1956 0.068 Uiso 1 1 calc R . . H18B H 1.0320 0.7001 0.1455 0.068 Uiso 1 1 calc R . . H18C H 1.0052 0.5858 0.1924 0.068 Uiso 1 1 calc R . . C27 C 0.2025(3) 0.6454(3) 0.29481(18) 0.0423(8) Uani 1 1 d . . . H27 H 0.1471 0.6037 0.2883 0.051 Uiso 1 1 calc R . . C34 C 0.6290(4) 0.9444(3) 0.29960(18) 0.0453(9) Uani 1 1 d . . . H34 H 0.6897 0.9841 0.2949 0.054 Uiso 1 1 calc R . . C19 C 0.8221(4) 0.7897(3) 0.0684(2) 0.0524(10) Uani 1 1 d . . . H19A H 0.7693 0.7871 0.0315 0.079 Uiso 1 1 calc R . . H19B H 0.8842 0.8265 0.0486 0.079 Uiso 1 1 calc R . . H19C H 0.7723 0.8366 0.0995 0.079 Uiso 1 1 calc R . . C35 C 0.6441(3) 0.8452(3) 0.27136(18) 0.0426(9) Uani 1 1 d . . . H35 H 0.7173 0.8167 0.2482 0.051 Uiso 1 1 calc R . . C39 C 0.8723(3) 0.4354(4) 0.3897(2) 0.0490(10) Uani 1 1 d . . . C8 C 0.2367(4) 0.3409(6) 0.2119(3) 0.106(2) Uani 1 1 d . . . H8A H 0.2731 0.3108 0.2585 0.159 Uiso 1 1 calc R . . H8B H 0.1622 0.3180 0.2095 0.159 Uiso 1 1 calc R . . H8C H 0.2159 0.4279 0.2003 0.159 Uiso 1 1 calc R . . C29 C 0.2485(3) 0.8005(3) 0.33405(19) 0.0450(9) Uani 1 1 d . . . H29 H 0.2249 0.8663 0.3559 0.054 Uiso 1 1 calc R . . C10 C 0.2721(4) 0.3341(5) 0.0897(2) 0.0770(16) Uani 1 1 d . . . H10A H 0.3314 0.2984 0.0579 0.115 Uiso 1 1 calc R . . H10B H 0.2526 0.4209 0.0773 0.115 Uiso 1 1 calc R . . H10C H 0.1971 0.3121 0.0871 0.115 Uiso 1 1 calc R . . C28 C 0.1673(3) 0.7388(4) 0.3277(2) 0.0509(10) Uani 1 1 d . . . H28 H 0.0878 0.7608 0.3459 0.061 Uiso 1 1 calc R . . C13 C 0.3391(5) 0.9401(3) 0.0833(2) 0.0742(14) Uani 1 1 d . . . H13A H 0.2767 1.0080 0.0558 0.111 Uiso 1 1 calc R . . H13B H 0.4176 0.9570 0.0812 0.111 Uiso 1 1 calc R . . H13C H 0.3143 0.9266 0.1311 0.111 Uiso 1 1 calc R . . C40 C 0.8872(4) 0.5573(4) 0.3879(2) 0.0660(13) Uani 1 1 d . . . H40A H 0.8979 0.5951 0.3404 0.099 Uiso 1 1 calc R . . H40B H 0.9593 0.5478 0.4162 0.099 Uiso 1 1 calc R . . H40C H 0.8140 0.6073 0.4058 0.099 Uiso 1 1 calc R . . C14 C 0.3826(5) 0.8489(4) -0.0195(2) 0.0712(14) Uani 1 1 d . . . H14A H 0.3893 0.7764 -0.0359 0.107 Uiso 1 1 calc R . . H14B H 0.4607 0.8667 -0.0253 0.107 Uiso 1 1 calc R . . H14C H 0.3176 0.9155 -0.0459 0.107 Uiso 1 1 calc R . . C15 C 0.2278(4) 0.8022(4) 0.0644(3) 0.0732(14) Uani 1 1 d . . . H15A H 0.2334 0.7319 0.0460 0.110 Uiso 1 1 calc R . . H15B H 0.1623 0.8704 0.0395 0.110 Uiso 1 1 calc R . . H15C H 0.2097 0.7868 0.1132 0.110 Uiso 1 1 calc R . . C24 C 1.0069(4) 0.1150(5) 0.2359(2) 0.0817(16) Uani 1 1 d . . . H24A H 1.0245 0.1892 0.2366 0.123 Uiso 1 1 calc R . . H24B H 1.0834 0.0533 0.2309 0.123 Uiso 1 1 calc R . . H24C H 0.9695 0.0892 0.2790 0.123 Uiso 1 1 calc R . . C23 C 0.9767(4) 0.1786(4) 0.1103(2) 0.0797(16) Uani 1 1 d . . . H23A H 0.9944 0.2521 0.1125 0.120 Uiso 1 1 calc R . . H23B H 0.9197 0.1940 0.0714 0.120 Uiso 1 1 calc R . . H23C H 1.0530 0.1176 0.1042 0.120 Uiso 1 1 calc R . . C3 C 0.4924(5) 0.3320(4) 0.5017(2) 0.0692(13) Uani 1 1 d . . . H3A H 0.4860 0.4156 0.4827 0.104 Uiso 1 1 calc R . . H3B H 0.5790 0.2850 0.5095 0.104 Uiso 1 1 calc R . . H3C H 0.4503 0.3256 0.5452 0.104 Uiso 1 1 calc R . . C4 C 0.4406(5) 0.1571(4) 0.4804(2) 0.0703(14) Uani 1 1 d . . . H4A H 0.3942 0.1521 0.5226 0.105 Uiso 1 1 calc R . . H4B H 0.5264 0.1093 0.4909 0.105 Uiso 1 1 calc R . . H4C H 0.4057 0.1267 0.4468 0.105 Uiso 1 1 calc R . . C25 C 0.8940(4) 0.0206(4) 0.1750(4) 0.105(2) Uani 1 1 d . . . H25A H 0.9707 -0.0397 0.1687 0.157 Uiso 1 1 calc R . . H25B H 0.8360 0.0338 0.1370 0.157 Uiso 1 1 calc R . . H25C H 0.8589 -0.0068 0.2185 0.157 Uiso 1 1 calc R . . C9 C 0.3586(4) 0.1553(4) 0.1795(3) 0.0816(17) Uani 1 1 d . . . H9A H 0.3942 0.1247 0.2263 0.122 Uiso 1 1 calc R . . H9B H 0.4182 0.1218 0.1471 0.122 Uiso 1 1 calc R . . H9C H 0.2844 0.1324 0.1763 0.122 Uiso 1 1 calc R . . C5 C 0.3008(4) 0.3594(5) 0.4349(2) 0.0910(19) Uani 1 1 d . . . H5A H 0.2962 0.4428 0.4169 0.136 Uiso 1 1 calc R . . H5B H 0.2537 0.3532 0.4767 0.136 Uiso 1 1 calc R . . H5C H 0.2666 0.3300 0.4004 0.136 Uiso 1 1 calc R . . C36 C 0.8371(4) 0.0204(5) 0.4916(3) 0.0715(14) Uani 1 1 d . . . N3 N 0.8269(4) 0.0144(5) 0.5485(3) 0.0981(16) Uani 1 1 d . . . C37 C 0.8525(5) 0.0279(5) 0.4186(2) 0.0944(19) Uani 1 1 d . . . H37A H 0.8151 0.1103 0.3938 0.142 Uiso 1 1 calc R . . H37B H 0.8128 -0.0240 0.4033 0.142 Uiso 1 1 calc R . . H37C H 0.9401 0.0025 0.4093 0.142 Uiso 1 1 calc R . . H12B H 0.611(5) 0.418(5) -0.008(3) 0.142 Uiso 1 1 d D . . H12A H 0.616(6) 0.522(3) -0.010(3) 0.142 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O14 0.0316(12) 0.0369(13) 0.0350(13) -0.0086(10) -0.0068(9) -0.0128(10) C42 0.131(5) 0.088(4) 0.059(3) 0.003(3) -0.055(3) -0.051(4) C41 0.030(2) 0.138(5) 0.180(6) -0.101(5) -0.013(3) -0.012(3) Fe1 0.0220(2) 0.0188(2) 0.0272(2) -0.00697(17) -0.00192(17) -0.00730(17) Fe2 0.0231(2) 0.0228(2) 0.0246(2) -0.00727(17) 0.00119(17) -0.00834(17) Co1 0.0309(2) 0.0271(2) 0.0319(2) -0.01030(18) 0.00040(17) -0.01338(18) O1 0.0266(10) 0.0221(10) 0.0220(10) -0.0074(8) 0.0000(8) -0.0089(8) O10 0.0267(11) 0.0266(11) 0.0265(11) -0.0082(9) 0.0020(8) -0.0138(9) O5 0.0308(11) 0.0242(11) 0.0294(12) -0.0066(9) 0.0020(9) -0.0031(9) O6 0.0354(12) 0.0301(11) 0.0268(11) -0.0115(9) 0.0021(9) -0.0165(10) O4 0.0330(12) 0.0301(12) 0.0295(12) -0.0076(9) 0.0058(9) -0.0011(9) O9 0.0305(11) 0.0229(11) 0.0331(12) -0.0131(9) -0.0067(9) -0.0023(9) O3 0.0347(12) 0.0269(11) 0.0306(12) -0.0051(9) 0.0073(9) -0.0074(9) O12 0.0355(12) 0.0259(11) 0.0265(12) -0.0083(9) 0.0001(9) -0.0126(10) O13 0.0437(14) 0.0363(13) 0.0319(13) -0.0128(10) -0.0034(10) -0.0135(11) O8 0.0459(13) 0.0282(12) 0.0266(12) -0.0109(9) -0.0032(10) -0.0110(10) O7 0.0343(12) 0.0475(14) 0.0317(12) -0.0219(10) 0.0082(10) -0.0225(11) O11 0.0387(13) 0.0365(12) 0.0285(12) -0.0035(10) -0.0061(10) -0.0218(10) O2 0.0344(12) 0.0246(11) 0.0294(12) -0.0091(9) 0.0032(9) -0.0088(9) N2 0.0415(16) 0.0300(14) 0.0277(14) -0.0138(11) 0.0010(12) -0.0146(12) C21 0.0254(15) 0.0277(16) 0.0284(17) -0.0094(13) 0.0005(13) -0.0127(13) C6 0.0257(15) 0.0198(14) 0.0289(17) -0.0087(12) -0.0006(12) -0.0069(12) N1 0.0300(14) 0.0238(13) 0.0267(14) -0.0066(10) -0.0012(11) -0.0084(11) C11 0.0299(16) 0.0202(15) 0.0301(17) -0.0092(13) 0.0052(13) -0.0068(12) C30 0.0349(17) 0.0264(16) 0.0237(16) -0.0046(13) -0.0012(13) -0.0061(13) C16 0.0239(15) 0.0248(15) 0.0282(17) -0.0073(13) -0.0018(12) -0.0072(12) C1 0.0299(16) 0.0313(17) 0.0253(16) -0.0083(13) -0.0005(13) -0.0155(14) C31 0.0433(19) 0.0254(16) 0.0190(15) -0.0028(12) -0.0014(13) -0.0095(14) C2 0.046(2) 0.0380(19) 0.0294(18) -0.0065(15) 0.0085(15) -0.0131(16) C17 0.0293(16) 0.0302(16) 0.0294(17) -0.0089(13) 0.0033(13) -0.0138(13) C22 0.0242(16) 0.0271(16) 0.0385(19) -0.0087(14) 0.0028(13) -0.0034(13) C32 0.062(2) 0.0287(18) 0.0321(19) -0.0113(14) 0.0066(16) -0.0160(17) C38 0.0328(18) 0.047(2) 0.0226(16) -0.0121(15) 0.0035(13) -0.0193(16) C7 0.0269(16) 0.0344(17) 0.0330(18) -0.0030(14) -0.0019(13) -0.0178(14) C20 0.0325(19) 0.060(2) 0.042(2) -0.0212(18) 0.0102(16) -0.0162(17) C12 0.042(2) 0.0251(17) 0.0367(19) -0.0085(14) -0.0036(15) -0.0010(14) C26 0.0334(18) 0.0325(18) 0.0366(19) -0.0078(14) -0.0035(14) -0.0104(14) C33 0.083(3) 0.0326(19) 0.034(2) -0.0179(16) 0.0066(19) -0.024(2) C18 0.038(2) 0.066(3) 0.045(2) -0.0164(18) 0.0021(16) -0.0301(19) C27 0.0304(18) 0.048(2) 0.049(2) -0.0079(17) -0.0046(16) -0.0137(16) C34 0.068(3) 0.042(2) 0.041(2) -0.0152(17) 0.0028(18) -0.0335(19) C19 0.058(2) 0.037(2) 0.060(3) 0.0000(18) 0.006(2) -0.0185(18) C35 0.050(2) 0.045(2) 0.045(2) -0.0216(17) 0.0088(17) -0.0261(18) C39 0.041(2) 0.065(3) 0.051(2) -0.026(2) -0.0098(17) -0.0194(19) C8 0.048(3) 0.189(6) 0.138(5) -0.118(5) 0.053(3) -0.069(4) C29 0.042(2) 0.044(2) 0.047(2) -0.0185(17) 0.0057(17) -0.0053(17) C10 0.055(3) 0.119(4) 0.063(3) 0.019(3) -0.023(2) -0.060(3) C28 0.033(2) 0.065(3) 0.056(3) -0.023(2) 0.0093(17) -0.0100(19) C13 0.099(4) 0.032(2) 0.077(3) -0.019(2) -0.026(3) 0.009(2) C40 0.071(3) 0.083(3) 0.070(3) -0.030(2) -0.006(2) -0.051(3) C14 0.113(4) 0.039(2) 0.041(2) 0.0017(19) 0.005(2) -0.001(2) C15 0.040(2) 0.068(3) 0.103(4) -0.019(3) -0.008(2) -0.001(2) C24 0.037(2) 0.125(5) 0.065(3) -0.028(3) -0.009(2) 0.009(3) C23 0.048(3) 0.093(4) 0.062(3) 0.002(3) 0.029(2) 0.015(2) C3 0.113(4) 0.082(3) 0.035(2) -0.024(2) 0.011(2) -0.055(3) C4 0.116(4) 0.060(3) 0.049(3) -0.014(2) 0.036(3) -0.050(3) C25 0.060(3) 0.055(3) 0.223(7) -0.083(4) 0.047(4) -0.021(2) C9 0.074(3) 0.046(3) 0.133(5) 0.003(3) -0.036(3) -0.040(2) C5 0.046(3) 0.145(5) 0.048(3) 0.008(3) 0.020(2) -0.003(3) C36 0.046(3) 0.087(4) 0.080(4) -0.042(3) 0.004(2) -0.002(2) N3 0.095(3) 0.126(4) 0.081(3) -0.053(3) 0.025(3) -0.025(3) C37 0.066(3) 0.131(5) 0.066(4) -0.037(3) -0.013(3) 0.011(3) _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 O14 C38 1.274(4) . ? O14 Fe2 2.010(2) . ? C42 C39 1.530(6) . ? C41 C39 1.525(6) . ? Fe1 O1 1.8827(19) . ? Fe1 O6 2.0281(19) . ? Fe1 O5 2.051(2) . ? Fe1 O9 2.081(2) . ? Fe1 O10 2.0955(18) . ? Fe1 O12 2.148(2) . ? Fe2 O1 1.8416(19) . ? Fe2 O4 2.006(2) . ? Fe2 O11 2.027(2) . ? Fe2 O3 2.057(2) . ? Fe2 O2 2.222(2) . ? Fe2 C1 2.481(3) . ? Co1 O1 1.9958(19) . ? Co1 O7 2.048(2) . ? Co1 O13 2.064(2) . ? Co1 O8 2.081(2) . ? Co1 N2 2.139(2) . ? Co1 N1 2.142(2) . ? O10 C6 1.263(3) . ? O5 C21 1.251(3) . ? O6 C16 1.261(3) . ? O4 C21 1.269(3) . ? O9 C11 1.287(3) . ? O3 C1 1.273(3) . ? O13 C38 1.244(4) . ? O8 C11 1.236(3) . ? O7 C16 1.257(3) . ? O11 C6 1.260(3) . ? O2 C1 1.252(4) . ? N2 C35 1.332(4) . ? N2 C31 1.344(4) . ? C21 C22 1.538(4) . ? C6 C7 1.534(4) . ? N1 C26 1.333(4) . ? N1 C30 1.354(4) . ? C11 C12 1.522(4) . ? C30 C29 1.392(4) . ? C30 C31 1.474(4) . ? C16 C17 1.540(4) . ? C1 C2 1.533(4) . ? C31 C32 1.393(4) . ? C2 C4 1.511(5) . ? C2 C5 1.516(5) . ? C2 C3 1.520(5) . ? C17 C20 1.521(4) . ? C17 C18 1.522(4) . ? C17 C19 1.529(4) . ? C22 C25 1.506(5) . ? C22 C23 1.512(5) . ? C22 C24 1.513(5) . ? C32 C33 1.378(5) . ? C38 C39 1.536(5) . ? C7 C8 1.499(5) . ? C7 C9 1.507(5) . ? C7 C10 1.513(5) . ? C12 C14 1.507(5) . ? C12 C13 1.508(5) . ? C12 C15 1.564(5) . ? C26 C27 1.386(4) . ? C33 C34 1.360(5) . ? C27 C28 1.375(5) . ? C34 C35 1.393(5) . ? C39 C40 1.526(5) . ? C29 C28 1.383(5) . ? C36 N3 1.125(6) . ? C36 C37 1.448(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C38 O14 Fe2 126.9(2) . . ? O1 Fe1 O6 97.09(8) . . ? O1 Fe1 O5 96.00(8) . . ? O6 Fe1 O5 90.39(8) . . ? O1 Fe1 O9 99.34(8) . . ? O6 Fe1 O9 89.82(8) . . ? O5 Fe1 O9 164.52(8) . . ? O1 Fe1 O10 93.02(8) . . ? O6 Fe1 O10 169.40(8) . . ? O5 Fe1 O10 91.72(8) . . ? O9 Fe1 O10 85.39(8) . . ? O1 Fe1 O12 177.39(8) . . ? O6 Fe1 O12 84.86(8) . . ? O5 Fe1 O12 82.23(8) . . ? O9 Fe1 O12 82.37(8) . . ? O10 Fe1 O12 85.14(8) . . ? O1 Fe2 O4 107.02(9) . . ? O1 Fe2 O14 97.98(8) . . ? O4 Fe2 O14 85.40(9) . . ? O1 Fe2 O11 92.30(8) . . ? O4 Fe2 O11 88.61(9) . . ? O14 Fe2 O11 169.26(9) . . ? O1 Fe2 O3 98.18(8) . . ? O4 Fe2 O3 154.79(8) . . ? O14 Fe2 O3 91.42(9) . . ? O11 Fe2 O3 90.21(9) . . ? O1 Fe2 O2 159.06(8) . . ? O4 Fe2 O2 93.76(8) . . ? O14 Fe2 O2 85.95(8) . . ? O11 Fe2 O2 85.55(8) . . ? O3 Fe2 O2 61.05(8) . . ? O1 Fe2 C1 128.97(10) . . ? O4 Fe2 C1 123.99(9) . . ? O14 Fe2 C1 87.95(9) . . ? O11 Fe2 C1 88.02(9) . . ? O3 Fe2 C1 30.80(9) . . ? O2 Fe2 C1 30.25(8) . . ? O1 Co1 O7 92.98(8) . . ? O1 Co1 O13 94.67(8) . . ? O7 Co1 O13 87.60(9) . . ? O1 Co1 O8 94.75(8) . . ? O7 Co1 O8 88.09(9) . . ? O13 Co1 O8 169.83(8) . . ? O1 Co1 N2 173.94(9) . . ? O7 Co1 N2 92.81(9) . . ? O13 Co1 N2 83.81(9) . . ? O8 Co1 N2 87.21(9) . . ? O1 Co1 N1 98.61(8) . . ? O7 Co1 N1 166.48(9) . . ? O13 Co1 N1 98.30(9) . . ? O8 Co1 N1 84.06(9) . . ? N2 Co1 N1 75.86(9) . . ? Fe2 O1 Fe1 119.05(10) . . ? Fe2 O1 Co1 122.15(10) . . ? Fe1 O1 Co1 116.95(9) . . ? C6 O10 Fe1 127.11(18) . . ? C21 O5 Fe1 137.5(2) . . ? C16 O6 Fe1 133.64(19) . . ? C21 O4 Fe2 124.57(19) . . ? C11 O9 Fe1 124.17(19) . . ? C1 O3 Fe2 93.35(18) . . ? C38 O13 Co1 129.1(2) . . ? C11 O8 Co1 136.98(19) . . ? C16 O7 Co1 126.92(18) . . ? C6 O11 Fe2 133.44(18) . . ? C1 O2 Fe2 86.39(17) . . ? C35 N2 C31 118.8(3) . . ? C35 N2 Co1 124.5(2) . . ? C31 N2 Co1 116.5(2) . . ? O5 C21 O4 124.8(3) . . ? O5 C21 C22 118.6(3) . . ? O4 C21 C22 116.6(3) . . ? O11 C6 O10 125.2(3) . . ? O11 C6 C7 115.2(2) . . ? O10 C6 C7 119.7(3) . . ? C26 N1 C30 118.9(3) . . ? C26 N1 Co1 124.6(2) . . ? C30 N1 Co1 116.40(19) . . ? O8 C11 O9 124.4(3) . . ? O8 C11 C12 118.3(3) . . ? O9 C11 C12 117.4(3) . . ? N1 C30 C29 120.9(3) . . ? N1 C30 C31 115.2(3) . . ? C29 C30 C31 123.9(3) . . ? O7 C16 O6 125.8(3) . . ? O7 C16 C17 116.8(2) . . ? O6 C16 C17 117.3(3) . . ? O2 C1 O3 119.2(3) . . ? O2 C1 C2 123.0(3) . . ? O3 C1 C2 117.9(3) . . ? O2 C1 Fe2 63.36(15) . . ? O3 C1 Fe2 55.85(14) . . ? C2 C1 Fe2 173.4(2) . . ? N2 C31 C32 121.3(3) . . ? N2 C31 C30 115.5(3) . . ? C32 C31 C30 123.1(3) . . ? C4 C2 C5 109.6(4) . . ? C4 C2 C3 110.1(3) . . ? C5 C2 C3 111.3(4) . . ? C4 C2 C1 110.3(3) . . ? C5 C2 C1 109.0(3) . . ? C3 C2 C1 106.6(3) . . ? C20 C17 C18 110.8(3) . . ? C20 C17 C19 110.4(3) . . ? C18 C17 C19 109.6(3) . . ? C20 C17 C16 110.1(2) . . ? C18 C17 C16 110.1(2) . . ? C19 C17 C16 105.7(2) . . ? C25 C22 C23 110.7(4) . . ? C25 C22 C24 109.2(4) . . ? C23 C22 C24 109.0(3) . . ? C25 C22 C21 108.4(3) . . ? C23 C22 C21 110.5(3) . . ? C24 C22 C21 109.1(3) . . ? C33 C32 C31 119.0(3) . . ? O13 C38 O14 125.2(3) . . ? O13 C38 C39 119.3(3) . . ? O14 C38 C39 115.5(3) . . ? C8 C7 C9 109.8(4) . . ? C8 C7 C10 110.4(4) . . ? C9 C7 C10 108.5(3) . . ? C8 C7 C6 107.6(3) . . ? C9 C7 C6 108.3(3) . . ? C10 C7 C6 112.1(2) . . ? C14 C12 C13 111.9(3) . . ? C14 C12 C11 110.6(3) . . ? C13 C12 C11 110.7(3) . . ? C14 C12 C15 109.3(3) . . ? C13 C12 C15 107.6(3) . . ? C11 C12 C15 106.6(3) . . ? N1 C26 C27 122.9(3) . . ? C34 C33 C32 119.8(3) . . ? C28 C27 C26 118.4(3) . . ? C33 C34 C35 118.5(3) . . ? N2 C35 C34 122.5(3) . . ? C41 C39 C40 109.6(4) . . ? C41 C39 C42 110.6(4) . . ? C40 C39 C42 110.6(3) . . ? C41 C39 C38 108.5(3) . . ? C40 C39 C38 110.6(3) . . ? C42 C39 C38 106.9(3) . . ? C28 C29 C30 119.4(3) . . ? C27 C28 C29 119.4(3) . . ? N3 C36 C37 179.0(6) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.591 _refine_diff_density_min -0.328 _refine_diff_density_rms 0.081 #END data_pa_453_0m _database_code_depnum_ccdc_archive 'CCDC 750191' #TrackingRef 'albores_et_al.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H67 Fe2 N3 Ni O14' _chemical_formula_weight 1008.40 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.4460(7) _cell_length_b 12.0370(7) _cell_length_c 19.9590(12) _cell_angle_alpha 77.711(2) _cell_angle_beta 88.033(2) _cell_angle_gamma 72.212(2) _cell_volume 2557.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.310 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1064 _exptl_absorpt_coefficient_mu 0.985 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.6877 _exptl_absorpt_correction_T_max 0.7839 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71069 _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 28596 _diffrn_reflns_av_R_equivalents 0.0316 _diffrn_reflns_av_sigmaI/netI 0.0426 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.04 _diffrn_reflns_theta_max 27.53 _reflns_number_total 11719 _reflns_number_gt 9083 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0554P)^2^+0.0196P] 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 11719 _refine_ls_number_parameters 587 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0534 _refine_ls_R_factor_gt 0.0354 _refine_ls_wR_factor_ref 0.1007 _refine_ls_wR_factor_gt 0.0889 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 C1 C 0.44434(18) 0.32302(18) 0.67015(11) 0.0227(4) Uani 1 1 d . . . C1S C 0.8535(4) 0.0286(4) 0.9187(2) 0.0984(16) Uani 1 1 d . . . H1S1 H 0.9392 0.0236 0.9088 0.148 Uiso 1 1 calc R . . H1S2 H 0.7994 0.1043 0.8926 0.148 Uiso 1 1 calc R . . H1S3 H 0.8345 -0.0380 0.9055 0.148 Uiso 1 1 calc R . . C2S C 0.8350(3) 0.0225(4) 0.9915(2) 0.0747(11) Uani 1 1 d . . . C3 C 0.9587(2) 0.5835(2) 0.56170(13) 0.0389(6) Uani 1 1 d . . . H3A H 1.0252 0.6149 0.5426 0.058 Uiso 1 1 calc R . . H3B H 0.9052 0.5840 0.5243 0.058 Uiso 1 1 calc R . . H3C H 0.9937 0.5016 0.5880 0.058 Uiso 1 1 calc R . . C4 C 0.9670(2) 0.6659(3) 0.66614(13) 0.0428(6) Uani 1 1 d . . . H4A H 0.9179 0.7161 0.6960 0.064 Uiso 1 1 calc R . . H4B H 1.0315 0.6994 0.6461 0.064 Uiso 1 1 calc R . . H4C H 1.0046 0.5849 0.6931 0.064 Uiso 1 1 calc R . . C5 C 0.3691(2) 0.76365(19) 0.80713(11) 0.0283(5) Uani 1 1 d . . . C6 C 0.3244(2) 0.6118(2) 0.76916(12) 0.0312(5) Uani 1 1 d . . . H6 H 0.3490 0.5470 0.7464 0.037 Uiso 1 1 calc R . . C7 C 0.6331(3) 0.9443(2) 0.79712(13) 0.0446(7) Uani 1 1 d . . . H7 H 0.6935 0.9846 0.7915 0.053 Uiso 1 1 calc R . . C8 C 0.2531(2) 0.7978(2) 0.83360(14) 0.0441(6) Uani 1 1 d . . . H8 H 0.2301 0.8627 0.8563 0.053 Uiso 1 1 calc R . . C9 C 0.4427(3) 0.9232(2) 0.83976(13) 0.0387(6) Uani 1 1 d . . . H9 H 0.3712 0.9481 0.8652 0.046 Uiso 1 1 calc R . . C10 C 0.4339(2) 0.2846(2) 0.95028(12) 0.0362(5) Uani 1 1 d D . . C11 C 0.3274(2) 0.2888(2) 0.66217(12) 0.0291(5) Uani 1 1 d . . . C12 C 0.5059(2) 0.2959(2) 0.88514(11) 0.0271(5) Uani 1 1 d . A . C13 C 0.8843(2) 0.6615(2) 0.60880(11) 0.0265(5) Uani 1 1 d . . . C14 C 0.3499(2) 0.8309(2) 0.55495(12) 0.0331(5) Uani 1 1 d . . . C15 C 0.9190(2) 0.1381(2) 0.67534(12) 0.0312(5) Uani 1 1 d D . . C16 C 0.79709(19) 0.23079(18) 0.68582(11) 0.0238(4) Uani 1 1 d . A . C17 C 0.77955(19) 0.61410(18) 0.63968(11) 0.0233(4) Uani 1 1 d . . . C18 C 0.44751(19) 0.72408(18) 0.59722(11) 0.0245(4) Uani 1 1 d . . . C19 C 0.4605(2) 0.82783(19) 0.80745(11) 0.0287(5) Uani 1 1 d . . . C20 C 0.2069(2) 0.6431(2) 0.79337(14) 0.0409(6) Uani 1 1 d . . . H20 H 0.1515 0.6010 0.7872 0.049 Uiso 1 1 calc R . . C21 C 0.3358(3) 0.9415(2) 0.58338(17) 0.0597(9) Uani 1 1 d . . . H21A H 0.2729 1.0094 0.5561 0.090 Uiso 1 1 calc R . . H21B H 0.4142 0.9589 0.5812 0.090 Uiso 1 1 calc R . . H21C H 0.3111 0.9275 0.6312 0.090 Uiso 1 1 calc R . . C22 C 0.7538(2) 0.4532(2) 0.84802(11) 0.0299(5) Uani 1 1 d . . . C23 C 0.6461(3) 0.8463(2) 0.76786(13) 0.0399(6) Uani 1 1 d . . . H23 H 0.7182 0.8188 0.7434 0.048 Uiso 1 1 calc R . . C24 C 0.8690(3) 0.4401(3) 0.89001(15) 0.0475(7) Uani 1 1 d . . . C25 C 0.8228(3) 0.7887(2) 0.56783(15) 0.0466(7) Uani 1 1 d . . . H25A H 0.7752 0.8378 0.5987 0.070 Uiso 1 1 calc R . . H25B H 0.7680 0.7862 0.5319 0.070 Uiso 1 1 calc R . . H25C H 0.8859 0.8233 0.5468 0.070 Uiso 1 1 calc R . . C26 C 0.8821(3) 0.5630(3) 0.88883(18) 0.0649(9) Uani 1 1 d . . . H26A H 0.9557 0.5538 0.9158 0.097 Uiso 1 1 calc R . . H26B H 0.8096 0.6112 0.9085 0.097 Uiso 1 1 calc R . . H26C H 0.8896 0.6028 0.8414 0.097 Uiso 1 1 calc R . . C28 C 0.1716(2) 0.7372(3) 0.82684(15) 0.0499(7) Uani 1 1 d . . . H28 H 0.0919 0.7595 0.8449 0.060 Uiso 1 1 calc R . . C31 C 0.5318(3) 0.9810(2) 0.83401(13) 0.0465(7) Uani 1 1 d . . . H31 H 0.5220 1.0461 0.8558 0.056 Uiso 1 1 calc R . . C32 C 0.2276(3) 0.8012(3) 0.56223(19) 0.0641(9) Uani 1 1 d . . . H32A H 0.2354 0.7302 0.5438 0.096 Uiso 1 1 calc R . . H32B H 0.1620 0.8688 0.5368 0.096 Uiso 1 1 calc R . . H32C H 0.2077 0.7857 0.6108 0.096 Uiso 1 1 calc R . . C35 C 0.9803(3) 0.3657(4) 0.8581(3) 0.1017(16) Uani 1 1 d . . . H35A H 1.0548 0.3563 0.8843 0.153 Uiso 1 1 calc R . . H35B H 0.9861 0.4060 0.8106 0.153 Uiso 1 1 calc R . . H35C H 0.9715 0.2869 0.8590 0.153 Uiso 1 1 calc R . . C36 C 0.3839(3) 0.8505(3) 0.48029(15) 0.0635(9) Uani 1 1 d . . . H36A H 0.3919 0.7781 0.4631 0.095 Uiso 1 1 calc R . . H36B H 0.4622 0.8683 0.4761 0.095 Uiso 1 1 calc R . . H36C H 0.3197 0.9175 0.4534 0.095 Uiso 1 1 calc R . . C40 C 0.8538(4) 0.3777(4) 0.96339(17) 0.0866(13) Uani 1 1 d . . . H40A H 0.9260 0.3681 0.9917 0.130 Uiso 1 1 calc R . . H40B H 0.8455 0.2991 0.9634 0.130 Uiso 1 1 calc R . . H40C H 0.7802 0.4260 0.9822 0.130 Uiso 1 1 calc R . . N1 N 0.56261(18) 0.78979(17) 0.77255(10) 0.0300(4) Uani 1 1 d . . . N1S N 0.8227(3) 0.0174(4) 1.0479(2) 0.1017(12) Uani 1 1 d . . . N2 N 0.40505(17) 0.66908(16) 0.77645(9) 0.0257(4) Uani 1 1 d . . . O1 O 0.58959(13) 0.47814(12) 0.71261(7) 0.0217(3) Uani 1 1 d . . . O2 O 0.48151(13) 0.38408(13) 0.61925(7) 0.0239(3) Uani 1 1 d . . . O3 O 0.73260(13) 0.56421(13) 0.60230(7) 0.0250(3) Uani 1 1 d . . . O4 O 0.74585(14) 0.63145(14) 0.69771(8) 0.0299(3) Uani 1 1 d . . . O5 O 0.74763(14) 0.35602(14) 0.83389(8) 0.0331(4) Uani 1 1 d . . . O6 O 0.49421(15) 0.28752(14) 0.72920(8) 0.0319(4) Uani 1 1 d . . . O7 O 0.47273(13) 0.62424(13) 0.57774(8) 0.0267(3) Uani 1 1 d . . . O8 O 0.58658(14) 0.20897(13) 0.86949(8) 0.0288(3) Uani 1 1 d . . . O9 O 0.75062(13) 0.31500(13) 0.63598(8) 0.0279(3) Uani 1 1 d . . . O10 O 0.63691(14) 0.45704(13) 0.51630(8) 0.0253(3) Uani 1 1 d D . . O11 O 0.75105(14) 0.21446(14) 0.74402(8) 0.0316(4) Uani 1 1 d . . . O12 O 0.48385(14) 0.39834(13) 0.84528(8) 0.0312(4) Uani 1 1 d . . . O13 O 0.67613(15) 0.55190(15) 0.83124(8) 0.0327(4) Uani 1 1 d . . . O14 O 0.49619(15) 0.73884(13) 0.64763(8) 0.0299(3) Uani 1 1 d . . . Fe1 Fe 0.61100(3) 0.47280(2) 0.621852(14) 0.01948(8) Uani 1 1 d . A . Fe2 Fe 0.61595(3) 0.33888(3) 0.778178(15) 0.02125(8) Uani 1 1 d . A . Ni1 Ni 0.58109(2) 0.63375(2) 0.738785(14) 0.02339(7) Uani 1 1 d . . . C2 C 0.2362(3) 0.3445(4) 0.7109(2) 0.0895(15) Uani 1 1 d . . . H2A H 0.2159 0.4316 0.6979 0.134 Uiso 1 1 calc R . . H2B H 0.2718 0.3165 0.7577 0.134 Uiso 1 1 calc R . . H2C H 0.1614 0.3217 0.7089 0.134 Uiso 1 1 calc R . . C30 C 0.2738(3) 0.3325(3) 0.58960(16) 0.0665(10) Uani 1 1 d . . . H30A H 0.2521 0.4198 0.5771 0.100 Uiso 1 1 calc R . . H30B H 0.2001 0.3083 0.5867 0.100 Uiso 1 1 calc R . . H30C H 0.3345 0.2977 0.5580 0.100 Uiso 1 1 calc R . . C37 C 0.3598(3) 0.1548(3) 0.6809(2) 0.0749(12) Uani 1 1 d . . . H37A H 0.4191 0.1201 0.6487 0.112 Uiso 1 1 calc R . . H37B H 0.2855 0.1313 0.6787 0.112 Uiso 1 1 calc R . . H37C H 0.3960 0.1258 0.7276 0.112 Uiso 1 1 calc R . . C29A C 0.9806(4) 0.1870(5) 0.6117(2) 0.0582(15) Uani 0.856(12) 1 d PD A 1 H29D H 0.9903 0.2635 0.6156 0.087 Uiso 0.856(12) 1 calc PR A 1 H29E H 0.9297 0.1986 0.5708 0.087 Uiso 0.856(12) 1 calc PR A 1 H29F H 1.0615 0.1302 0.6080 0.087 Uiso 0.856(12) 1 calc PR A 1 C33A C 0.979(3) 0.065(3) 0.7440(10) 0.0679(17) Uani 0.144(12) 1 d PD A 1 H33A H 1.0166 0.1131 0.7651 0.102 Uiso 0.144(12) 1 calc PR A 1 H33B H 1.0421 -0.0070 0.7371 0.102 Uiso 0.144(12) 1 calc PR A 1 H33C H 0.9166 0.0431 0.7742 0.102 Uiso 0.144(12) 1 calc PR A 1 C39A C 0.880(6) 0.047(4) 0.648(3) 0.090(3) Uani 0.144(12) 1 d PD A 1 H39A H 0.9529 -0.0177 0.6410 0.135 Uiso 0.144(12) 1 calc PR A 1 H39B H 0.8341 0.0847 0.6045 0.135 Uiso 0.144(12) 1 calc PR A 1 H39C H 0.8277 0.0137 0.6813 0.135 Uiso 0.144(12) 1 calc PR A 1 C29B C 0.944(3) 0.153(3) 0.5999(9) 0.0582(15) Uani 0.144(12) 1 d PD A 2 H29A H 0.9810 0.2177 0.5858 0.087 Uiso 0.144(12) 1 calc PR A 2 H29B H 0.8673 0.1726 0.5736 0.087 Uiso 0.144(12) 1 calc PR A 2 H29C H 1.0012 0.0786 0.5911 0.087 Uiso 0.144(12) 1 calc PR A 2 C33B C 1.0078(4) 0.1193(6) 0.7355(2) 0.0679(17) Uani 0.856(12) 1 d PD A 2 H33D H 1.0233 0.1948 0.7362 0.102 Uiso 0.856(12) 1 calc PR A 2 H33E H 1.0854 0.0590 0.7300 0.102 Uiso 0.856(12) 1 calc PR A 2 H33F H 0.9716 0.0922 0.7787 0.102 Uiso 0.856(12) 1 calc PR A 2 C39B C 0.8958(8) 0.0211(5) 0.6744(5) 0.090(3) Uani 0.856(12) 1 d PD A 2 H39D H 0.9732 -0.0384 0.6678 0.135 Uiso 0.856(12) 1 calc PR A 2 H39E H 0.8375 0.0331 0.6367 0.135 Uiso 0.856(12) 1 calc PR A 2 H39F H 0.8615 -0.0072 0.7181 0.135 Uiso 0.856(12) 1 calc PR A 2 C27A C 0.472(7) 0.362(5) 0.992(3) 0.0576(15) Uani 0.116(13) 1 d PD B 1 H27D H 0.4296 0.3591 1.0353 0.086 Uiso 0.116(13) 1 calc PR B 1 H27E H 0.4503 0.4443 0.9656 0.086 Uiso 0.116(13) 1 calc PR B 1 H27F H 0.5611 0.3311 1.0011 0.086 Uiso 0.116(13) 1 calc PR B 1 C34A C 0.2979(4) 0.3546(6) 0.9326(2) 0.0670(16) Uani 0.884(13) 1 d PD B 1 H34A H 0.2504 0.3482 0.9743 0.100 Uiso 0.884(13) 1 calc PR B 1 H34B H 0.2669 0.3214 0.8988 0.100 Uiso 0.884(13) 1 calc PR B 1 H34C H 0.2899 0.4387 0.9136 0.100 Uiso 0.884(13) 1 calc PR B 1 C38A C 0.4460(6) 0.1542(3) 0.9807(3) 0.0566(13) Uani 0.884(13) 1 d PD B 1 H38A H 0.3991 0.1488 1.0227 0.085 Uiso 0.884(13) 1 calc PR B 1 H38B H 0.5327 0.1094 0.9917 0.085 Uiso 0.884(13) 1 calc PR B 1 H38C H 0.4140 0.1206 0.9475 0.085 Uiso 0.884(13) 1 calc PR B 1 C27B C 0.4912(8) 0.3299(5) 1.0021(3) 0.0576(15) Uani 0.884(13) 1 d PD B 2 H27A H 0.4468 0.3239 1.0449 0.086 Uiso 0.884(13) 1 calc PR B 2 H27B H 0.4866 0.4135 0.9837 0.086 Uiso 0.884(13) 1 calc PR B 2 H27C H 0.5774 0.2816 1.0111 0.086 Uiso 0.884(13) 1 calc PR B 2 C34B C 0.326(3) 0.397(3) 0.9477(19) 0.0670(16) Uani 0.116(13) 1 d PD B 2 H34D H 0.2799 0.3879 0.9899 0.100 Uiso 0.116(13) 1 calc PR B 2 H34E H 0.2714 0.4081 0.9081 0.100 Uiso 0.116(13) 1 calc PR B 2 H34F H 0.3555 0.4657 0.9433 0.100 Uiso 0.116(13) 1 calc PR B 2 C38B C 0.394(4) 0.175(3) 0.963(2) 0.0566(13) Uani 0.116(13) 1 d PD B 2 H38D H 0.3479 0.1704 1.0053 0.085 Uiso 0.116(13) 1 calc PR B 2 H38E H 0.4659 0.1042 0.9674 0.085 Uiso 0.116(13) 1 calc PR B 2 H38F H 0.3409 0.1787 0.9244 0.085 Uiso 0.116(13) 1 calc PR B 2 H10B H 0.629(3) 0.517(2) 0.4857(13) 0.068 Uiso 1 1 d D . . H10A H 0.605(3) 0.421(3) 0.4955(15) 0.068 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0237(10) 0.0183(10) 0.0287(11) -0.0100(9) 0.0019(8) -0.0066(8) C1S 0.068(2) 0.144(4) 0.064(2) -0.042(3) -0.0171(19) 0.012(3) C2S 0.052(2) 0.090(3) 0.083(3) -0.045(2) 0.0043(18) -0.0055(19) C3 0.0308(12) 0.0512(16) 0.0406(15) -0.0184(12) 0.0080(10) -0.0161(12) C4 0.0375(13) 0.0651(18) 0.0395(15) -0.0170(13) 0.0038(11) -0.0318(13) C5 0.0350(12) 0.0257(11) 0.0224(11) -0.0056(9) 0.0003(9) -0.0062(9) C6 0.0317(12) 0.0298(12) 0.0327(13) -0.0079(10) -0.0025(9) -0.0092(10) C7 0.0663(18) 0.0432(15) 0.0378(15) -0.0136(12) 0.0057(13) -0.0335(14) C8 0.0404(14) 0.0469(16) 0.0464(16) -0.0235(13) 0.0092(12) -0.0069(12) C9 0.0591(16) 0.0297(12) 0.0313(13) -0.0141(10) 0.0090(11) -0.0150(12) C10 0.0438(14) 0.0404(14) 0.0255(12) -0.0072(10) 0.0060(10) -0.0147(11) C11 0.0271(11) 0.0325(12) 0.0325(12) -0.0069(10) 0.0017(9) -0.0164(10) C12 0.0316(11) 0.0311(12) 0.0241(11) -0.0093(9) -0.0001(9) -0.0153(10) C13 0.0287(11) 0.0296(11) 0.0256(11) -0.0076(9) 0.0032(9) -0.0142(9) C14 0.0384(13) 0.0225(11) 0.0332(13) -0.0081(10) -0.0030(10) 0.0003(10) C15 0.0247(11) 0.0291(12) 0.0363(13) -0.0090(10) 0.0040(9) -0.0020(9) C16 0.0234(10) 0.0227(10) 0.0293(12) -0.0100(9) 0.0010(8) -0.0099(9) C17 0.0253(10) 0.0209(10) 0.0259(11) -0.0073(8) -0.0005(8) -0.0088(8) C18 0.0261(10) 0.0213(10) 0.0276(11) -0.0086(9) 0.0058(8) -0.0077(9) C19 0.0411(13) 0.0252(11) 0.0200(11) -0.0070(9) 0.0000(9) -0.0089(10) C20 0.0305(12) 0.0471(15) 0.0459(15) -0.0108(12) -0.0023(11) -0.0121(11) C21 0.080(2) 0.0262(13) 0.063(2) -0.0162(13) -0.0159(17) 0.0056(14) C22 0.0312(12) 0.0438(14) 0.0215(11) -0.0129(10) 0.0030(9) -0.0176(11) C23 0.0491(15) 0.0438(15) 0.0390(14) -0.0177(12) 0.0062(11) -0.0263(13) C24 0.0416(15) 0.0618(18) 0.0480(16) -0.0229(14) -0.0099(12) -0.0197(14) C25 0.0565(17) 0.0315(13) 0.0513(17) 0.0006(12) 0.0067(13) -0.0195(13) C26 0.067(2) 0.081(2) 0.069(2) -0.0284(18) -0.0090(17) -0.0458(19) C28 0.0331(14) 0.0587(18) 0.0592(19) -0.0223(15) 0.0090(12) -0.0098(13) C31 0.083(2) 0.0314(13) 0.0334(14) -0.0147(11) 0.0044(13) -0.0235(14) C32 0.0350(15) 0.060(2) 0.090(3) -0.0182(18) -0.0098(15) 0.0002(14) C35 0.0318(17) 0.131(4) 0.163(4) -0.086(3) -0.014(2) -0.015(2) C36 0.094(3) 0.0394(16) 0.0387(17) 0.0009(13) 0.0014(16) 0.0000(16) C40 0.126(3) 0.087(3) 0.054(2) 0.0000(19) -0.050(2) -0.046(3) N1 0.0399(11) 0.0293(10) 0.0264(10) -0.0119(8) 0.0012(8) -0.0147(9) N1S 0.099(3) 0.128(3) 0.082(3) -0.055(3) 0.028(2) -0.020(2) N2 0.0312(10) 0.0243(9) 0.0241(9) -0.0088(7) 0.0017(7) -0.0100(8) O1 0.0262(7) 0.0207(7) 0.0210(7) -0.0084(6) 0.0025(6) -0.0091(6) O2 0.0271(7) 0.0262(8) 0.0239(8) -0.0084(6) 0.0019(6) -0.0140(6) O3 0.0314(8) 0.0284(8) 0.0233(8) -0.0107(6) 0.0037(6) -0.0175(7) O4 0.0317(8) 0.0403(9) 0.0277(8) -0.0163(7) 0.0067(6) -0.0197(7) O5 0.0320(8) 0.0344(9) 0.0365(9) -0.0095(7) -0.0082(7) -0.0128(7) O6 0.0402(9) 0.0345(9) 0.0274(8) -0.0020(7) -0.0067(7) -0.0226(8) O7 0.0295(8) 0.0202(7) 0.0296(8) -0.0091(6) -0.0046(6) -0.0034(6) O8 0.0351(8) 0.0252(8) 0.0274(8) -0.0077(6) 0.0022(6) -0.0097(7) O9 0.0274(8) 0.0245(8) 0.0292(8) -0.0069(7) 0.0028(6) -0.0034(6) O10 0.0340(8) 0.0244(8) 0.0216(8) -0.0079(6) 0.0022(6) -0.0129(7) O11 0.0339(8) 0.0281(8) 0.0280(9) -0.0064(7) 0.0067(7) -0.0029(7) O12 0.0359(9) 0.0269(8) 0.0295(9) -0.0047(7) 0.0083(7) -0.0092(7) O13 0.0402(9) 0.0362(9) 0.0260(8) -0.0128(7) -0.0007(7) -0.0137(8) O14 0.0402(9) 0.0241(8) 0.0272(8) -0.0100(6) -0.0004(7) -0.0091(7) Fe1 0.02147(15) 0.01882(14) 0.02048(15) -0.00766(11) 0.00010(11) -0.00712(11) Fe2 0.02256(15) 0.02202(15) 0.02112(16) -0.00687(12) 0.00085(11) -0.00810(12) Ni1 0.02837(15) 0.02393(14) 0.02349(15) -0.01193(11) 0.00335(11) -0.01170(11) C2 0.0415(18) 0.155(4) 0.114(3) -0.091(3) 0.036(2) -0.052(2) C30 0.0507(18) 0.108(3) 0.0504(19) 0.0087(18) -0.0159(14) -0.054(2) C37 0.068(2) 0.0416(17) 0.121(3) 0.0053(18) -0.034(2) -0.0363(17) C29A 0.032(2) 0.065(3) 0.059(2) -0.0010(19) 0.0211(18) 0.0013(18) C33A 0.0270(19) 0.105(4) 0.059(2) -0.022(3) -0.0055(16) 0.003(2) C39A 0.057(3) 0.041(3) 0.184(9) -0.057(4) 0.039(4) -0.013(3) C29B 0.032(2) 0.065(3) 0.059(2) -0.0010(19) 0.0211(18) 0.0013(18) C33B 0.0270(19) 0.105(4) 0.059(2) -0.022(3) -0.0055(16) 0.003(2) C39B 0.057(3) 0.041(3) 0.184(9) -0.057(4) 0.039(4) -0.013(3) C27A 0.090(4) 0.065(3) 0.031(3) -0.017(3) 0.0072(19) -0.039(3) C34A 0.0362(19) 0.117(4) 0.039(2) -0.010(2) 0.0110(15) -0.017(2) C38A 0.087(4) 0.054(2) 0.039(2) -0.0074(17) 0.020(2) -0.041(2) C27B 0.090(4) 0.065(3) 0.031(3) -0.017(3) 0.0072(19) -0.039(3) C34B 0.0362(19) 0.117(4) 0.039(2) -0.010(2) 0.0110(15) -0.017(2) C38B 0.087(4) 0.054(2) 0.039(2) -0.0074(17) 0.020(2) -0.041(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O6 1.257(3) . ? C1 O2 1.264(2) . ? C1 C11 1.538(3) . ? C1S C2S 1.450(5) . ? C2S N1S 1.122(5) . ? C3 C13 1.524(3) . ? C4 C13 1.529(3) . ? C5 N2 1.354(3) . ? C5 C8 1.386(3) . ? C5 C19 1.479(3) . ? C6 N2 1.338(3) . ? C6 C20 1.382(3) . ? C7 C31 1.359(4) . ? C7 C23 1.391(3) . ? C8 C28 1.374(4) . ? C9 C31 1.390(4) . ? C9 C19 1.392(3) . ? C10 C38B 1.495(17) . ? C10 C27B 1.517(4) . ? C10 C12 1.519(3) . ? C10 C34B 1.520(18) . ? C10 C38A 1.522(4) . ? C10 C27A 1.530(19) . ? C10 C34A 1.539(4) . ? C11 C37 1.506(4) . ? C11 C2 1.506(4) . ? C11 C30 1.514(4) . ? C12 O8 1.255(3) . ? C12 O12 1.274(3) . ? C12 Fe2 2.481(2) . ? C13 C25 1.535(3) . ? C13 C17 1.537(3) . ? C14 C36 1.515(4) . ? C14 C21 1.517(3) . ? C14 C18 1.530(3) . ? C14 C32 1.542(4) . ? C15 C29B 1.507(16) . ? C15 C39A 1.507(18) . ? C15 C39B 1.515(5) . ? C15 C33A 1.517(16) . ? C15 C29A 1.527(4) . ? C15 C33B 1.534(4) . ? C15 C16 1.537(3) . ? C16 O9 1.256(3) . ? C16 O11 1.261(3) . ? C17 O4 1.248(3) . ? C17 O3 1.273(2) . ? C18 O14 1.237(3) . ? C18 O7 1.288(2) . ? C19 N1 1.347(3) . ? C20 C28 1.384(4) . ? C22 O13 1.233(3) . ? C22 O5 1.282(3) . ? C22 C24 1.536(3) . ? C23 N1 1.322(3) . ? C24 C35 1.523(5) . ? C24 C40 1.527(5) . ? C24 C26 1.527(4) . ? N1 Ni1 2.0768(18) . ? N2 Ni1 2.0771(18) . ? O1 Fe1 1.8317(14) . ? O1 Fe2 1.8433(14) . ? O1 Ni1 2.0230(14) . ? O2 Fe1 2.0823(14) . ? O3 Fe1 2.0040(14) . ? O4 Ni1 2.0250(15) . ? O5 Fe2 1.9883(15) . ? O6 Fe2 2.0387(15) . ? O7 Fe1 2.0622(14) . ? O8 Fe2 2.2240(15) . ? O9 Fe1 2.0468(15) . ? O10 Fe1 2.1575(15) . ? O11 Fe2 2.0115(15) . ? O12 Fe2 2.0494(15) . ? O13 Ni1 2.0660(16) . ? O14 Ni1 2.0603(15) . ? 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 O6 C1 O2 125.48(19) . . ? O6 C1 C11 115.06(19) . . ? O2 C1 C11 119.45(19) . . ? N1S C2S C1S 178.8(4) . . ? N2 C5 C8 121.1(2) . . ? N2 C5 C19 114.94(19) . . ? C8 C5 C19 123.9(2) . . ? N2 C6 C20 122.7(2) . . ? C31 C7 C23 118.4(2) . . ? C28 C8 C5 119.6(2) . . ? C31 C9 C19 118.5(2) . . ? C38B C10 C27B 127.2(18) . . ? C38B C10 C12 111.7(15) . . ? C27B C10 C12 107.4(4) . . ? C38B C10 C34B 111(2) . . ? C27B C10 C34B 86(2) . . ? C12 C10 C34B 110.4(13) . . ? C38B C10 C38A 25.2(18) . . ? C27B C10 C38A 107.2(4) . . ? C12 C10 C38A 110.7(2) . . ? C34B C10 C38A 130.4(16) . . ? C38B C10 C27A 139(3) . . ? C27B C10 C27A 15(2) . . ? C12 C10 C27A 104(3) . . ? C34B C10 C27A 73(4) . . ? C38A C10 C27A 121(2) . . ? C38B C10 C34A 86.0(18) . . ? C27B C10 C34A 113.6(5) . . ? C12 C10 C34A 108.6(2) . . ? C34B C10 C34A 29.7(18) . . ? C38A C10 C34A 109.4(3) . . ? C27A C10 C34A 102(3) . . ? C37 C11 C2 110.6(3) . . ? C37 C11 C30 109.0(3) . . ? C2 C11 C30 109.9(3) . . ? C37 C11 C1 108.2(2) . . ? C2 C11 C1 107.0(2) . . ? C30 C11 C1 112.13(19) . . ? O8 C12 O12 118.9(2) . . ? O8 C12 C10 122.7(2) . . ? O12 C12 C10 118.3(2) . . ? O8 C12 Fe2 63.43(11) . . ? O12 C12 Fe2 55.52(11) . . ? C10 C12 Fe2 173.55(17) . . ? C3 C13 C4 110.4(2) . . ? C3 C13 C25 110.3(2) . . ? C4 C13 C25 109.4(2) . . ? C3 C13 C17 110.52(18) . . ? C4 C13 C17 109.98(18) . . ? C25 C13 C17 106.06(18) . . ? C36 C14 C21 111.1(2) . . ? C36 C14 C18 110.0(2) . . ? C21 C14 C18 110.0(2) . . ? C36 C14 C32 109.9(3) . . ? C21 C14 C32 108.7(2) . . ? C18 C14 C32 107.1(2) . . ? C29B C15 C39A 72(3) . . ? C29B C15 C39B 89.4(16) . . ? C39A C15 C39B 21(3) . . ? C29B C15 C33A 140.0(15) . . ? C39A C15 C33A 101(3) . . ? C39B C15 C33A 80.5(15) . . ? C29B C15 C29A 28.2(13) . . ? C39A C15 C29A 99(3) . . ? C39B C15 C29A 114.4(5) . . ? C33A C15 C29A 127.9(13) . . ? C29B C15 C33B 128.5(13) . . ? C39A C15 C33B 129(2) . . ? C39B C15 C33B 109.2(4) . . ? C33A C15 C33B 30.4(14) . . ? C29A C15 C33B 105.0(5) . . ? C29B C15 C16 109.5(10) . . ? C39A C15 C16 104(2) . . ? C39B C15 C16 109.1(4) . . ? C33A C15 C16 110.4(11) . . ? C29A C15 C16 110.3(2) . . ? C33B C15 C16 108.6(2) . . ? O9 C16 O11 125.37(19) . . ? O9 C16 C15 117.93(19) . . ? O11 C16 C15 116.69(19) . . ? O4 C17 O3 126.20(19) . . ? O4 C17 C13 117.27(18) . . ? O3 C17 C13 116.48(18) . . ? O14 C18 O7 124.5(2) . . ? O14 C18 C14 118.27(19) . . ? O7 C18 C14 117.21(19) . . ? N1 C19 C9 121.4(2) . . ? N1 C19 C5 115.38(19) . . ? C9 C19 C5 123.2(2) . . ? C6 C20 C28 118.6(2) . . ? O13 C22 O5 125.6(2) . . ? O13 C22 C24 119.6(2) . . ? O5 C22 C24 114.8(2) . . ? N1 C23 C7 122.9(3) . . ? C35 C24 C40 111.0(3) . . ? C35 C24 C26 109.7(3) . . ? C40 C24 C26 110.4(3) . . ? C35 C24 C22 108.3(2) . . ? C40 C24 C22 107.4(2) . . ? C26 C24 C22 110.0(2) . . ? C8 C28 C20 119.2(2) . . ? C7 C31 C9 119.8(2) . . ? C23 N1 C19 118.9(2) . . ? C23 N1 Ni1 125.64(17) . . ? C19 N1 Ni1 115.14(15) . . ? C6 N2 C5 118.76(19) . . ? C6 N2 Ni1 125.78(15) . . ? C5 N2 Ni1 115.33(14) . . ? Fe1 O1 Fe2 120.22(7) . . ? Fe1 O1 Ni1 116.74(7) . . ? Fe2 O1 Ni1 121.11(7) . . ? C1 O2 Fe1 126.37(13) . . ? C17 O3 Fe1 131.98(14) . . ? C17 O4 Ni1 126.88(14) . . ? C22 O5 Fe2 126.32(15) . . ? C1 O6 Fe2 133.09(14) . . ? C18 O7 Fe1 123.79(13) . . ? C12 O8 Fe2 86.26(13) . . ? C16 O9 Fe1 135.99(14) . . ? C16 O11 Fe2 124.37(14) . . ? C12 O12 Fe2 93.65(13) . . ? C22 O13 Ni1 129.64(14) . . ? C18 O14 Ni1 136.59(14) . . ? O1 Fe1 O3 98.20(6) . . ? O1 Fe1 O9 97.06(6) . . ? O3 Fe1 O9 90.43(6) . . ? O1 Fe1 O7 100.02(6) . . ? O3 Fe1 O7 89.84(6) . . ? O9 Fe1 O7 162.69(6) . . ? O1 Fe1 O2 93.80(6) . . ? O3 Fe1 O2 167.64(6) . . ? O9 Fe1 O2 91.03(6) . . ? O7 Fe1 O2 85.15(6) . . ? O1 Fe1 O10 177.10(6) . . ? O3 Fe1 O10 83.86(6) . . ? O9 Fe1 O10 80.84(6) . . ? O7 Fe1 O10 81.99(6) . . ? O2 Fe1 O10 84.26(6) . . ? O1 Fe2 O5 98.65(6) . . ? O1 Fe2 O11 106.35(6) . . ? O5 Fe2 O11 85.54(7) . . ? O1 Fe2 O6 91.48(6) . . ? O5 Fe2 O6 169.07(7) . . ? O11 Fe2 O6 87.69(7) . . ? O1 Fe2 O12 99.21(6) . . ? O5 Fe2 O12 92.36(7) . . ? O11 Fe2 O12 154.39(6) . . ? O6 Fe2 O12 90.03(7) . . ? O1 Fe2 O8 159.95(6) . . ? O5 Fe2 O8 86.79(6) . . ? O11 Fe2 O8 93.26(6) . . ? O6 Fe2 O8 85.03(6) . . ? O12 Fe2 O8 61.13(6) . . ? O1 Fe2 C12 129.98(7) . . ? O5 Fe2 C12 89.03(7) . . ? O11 Fe2 C12 123.56(7) . . ? O6 Fe2 C12 87.57(7) . . ? O12 Fe2 C12 30.83(7) . . ? O8 Fe2 C12 30.30(6) . . ? O1 Ni1 O4 91.72(6) . . ? O1 Ni1 O14 94.46(6) . . ? O4 Ni1 O14 89.17(6) . . ? O1 Ni1 O13 94.17(6) . . ? O4 Ni1 O13 86.72(6) . . ? O14 Ni1 O13 170.55(6) . . ? O1 Ni1 N1 175.01(7) . . ? O4 Ni1 N1 92.74(7) . . ? O14 Ni1 N1 87.84(7) . . ? O13 Ni1 N1 83.86(7) . . ? O1 Ni1 N2 97.22(6) . . ? O4 Ni1 N2 169.74(7) . . ? O14 Ni1 N2 85.15(7) . . ? O13 Ni1 N2 97.58(7) . . ? N1 Ni1 N2 78.54(7) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.436 _refine_diff_density_min -0.330 _refine_diff_density_rms 0.071 #END data_pa_487_0m _database_code_depnum_ccdc_archive 'CCDC 750192' #TrackingRef 'albores_et_al.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H67 Fe2 Mn N3 O14' _chemical_formula_weight 1028.65 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' Mn Mn 0.3368 0.7283 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.5312(7) _cell_length_b 12.2514(8) _cell_length_c 19.4796(13) _cell_angle_alpha 78.256(2) _cell_angle_beta 86.361(2) _cell_angle_gamma 74.106(2) _cell_volume 2591.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.318 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1082 _exptl_absorpt_coefficient_mu 0.854 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.8197 _exptl_absorpt_correction_T_max 0.9915 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71069 _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 56676 _diffrn_reflns_av_R_equivalents 0.1207 _diffrn_reflns_av_sigmaI/netI 0.0975 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.07 _diffrn_reflns_theta_max 27.57 _reflns_number_total 11916 _reflns_number_gt 7211 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0457P)^2^+0.7804P] 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 11916 _refine_ls_number_parameters 614 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1085 _refine_ls_R_factor_gt 0.0518 _refine_ls_wR_factor_ref 0.1217 _refine_ls_wR_factor_gt 0.0976 _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_restrained_S_all 0.991 _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 C1 C 0.5407(3) 0.1777(3) 0.19128(17) 0.0256(8) Uani 1 1 d . . . C2 C 0.5745(4) 0.0737(3) 0.16508(19) 0.0336(9) Uani 1 1 d . . . C3 C 0.4868(4) 0.0120(3) 0.1698(2) 0.0400(10) Uani 1 1 d . . . H3 H 0.5052 -0.0589 0.1535 0.048 Uiso 1 1 calc R . . C4 C 0.3765(4) 0.0527(4) 0.1973(2) 0.0431(11) Uani 1 1 d . . . H4 H 0.3170 0.0114 0.2002 0.052 Uiso 1 1 calc R . . C5 C 0.3516(4) 0.1570(3) 0.2214(2) 0.0399(10) Uani 1 1 d . . . H5 H 0.2738 0.1852 0.2405 0.048 Uiso 1 1 calc R . . C6 C 0.6706(3) 0.3991(3) 0.22126(19) 0.0305(8) Uani 1 1 d . . . H6 H 0.6466 0.4661 0.2417 0.037 Uiso 1 1 calc R . . C7 C 0.7891(4) 0.3659(3) 0.1964(2) 0.0383(10) Uani 1 1 d . . . H7 H 0.8438 0.4103 0.1996 0.046 Uiso 1 1 calc R . . C8 C 0.8256(4) 0.2692(4) 0.1675(2) 0.0399(10) Uani 1 1 d . . . H8 H 0.9055 0.2465 0.1498 0.048 Uiso 1 1 calc R . . C9 C 0.7438(3) 0.2036(3) 0.16416(19) 0.0328(9) Uani 1 1 d . . . C10 C 0.6268(3) 0.2432(3) 0.19047(18) 0.0267(8) Uani 1 1 d . . . C11 C 0.7737(4) 0.0990(3) 0.1367(2) 0.0430(10) Uani 1 1 d . . . H11 H 0.8518 0.0729 0.1174 0.052 Uiso 1 1 calc R . . C12 C 0.6934(4) 0.0374(3) 0.1378(2) 0.0429(10) Uani 1 1 d . . . H12 H 0.7164 -0.0322 0.1200 0.052 Uiso 1 1 calc R . . C13 C 0.5428(3) 0.2747(3) 0.39806(18) 0.0263(8) Uani 1 1 d . C . C14 C 0.6362(4) 0.1665(3) 0.4334(2) 0.0366(9) Uani 1 1 d D . . C18 C 0.2093(3) 0.3765(3) 0.36281(18) 0.0261(8) Uani 1 1 d . B . C19 C 0.1058(3) 0.3242(3) 0.39141(19) 0.0304(8) Uani 1 1 d . . . C20 C 0.0295(4) 0.3939(4) 0.4430(2) 0.0444(11) Uani 1 1 d . . . H20A H -0.0367 0.3599 0.4611 0.067 Uiso 1 1 calc R . . H20B H -0.0037 0.4741 0.4190 0.067 Uiso 1 1 calc R . . H20C H 0.0799 0.3924 0.4820 0.067 Uiso 1 1 calc R . . C21 C 0.1646(4) 0.2005(4) 0.4292(2) 0.0530(12) Uani 1 1 d . . . H21A H 0.1018 0.1627 0.4486 0.079 Uiso 1 1 calc R . . H21B H 0.2152 0.2025 0.4672 0.079 Uiso 1 1 calc R . . H21C H 0.2145 0.1571 0.3959 0.079 Uiso 1 1 calc R . . C22 C 0.0271(4) 0.3224(4) 0.3313(2) 0.0480(11) Uani 1 1 d . . . H22A H -0.0387 0.2886 0.3505 0.072 Uiso 1 1 calc R . . H22B H 0.0762 0.2758 0.2993 0.072 Uiso 1 1 calc R . . H22C H -0.0065 0.4016 0.3059 0.072 Uiso 1 1 calc R . . C23 C 0.2101(3) 0.7700(3) 0.3145(2) 0.0283(8) Uani 1 1 d . A . C24 C 0.0936(3) 0.8643(3) 0.32311(19) 0.0313(8) Uani 1 1 d D . . C28 C 0.5677(3) 0.6708(3) 0.32951(18) 0.0241(8) Uani 1 1 d . B . C29 C 0.6845(3) 0.7047(3) 0.33482(19) 0.0310(9) Uani 1 1 d D . . C33 C 0.5053(3) 0.7046(3) 0.10989(17) 0.0256(8) Uani 1 1 d . A . C34 C 0.5791(3) 0.7200(3) 0.04307(18) 0.0313(9) Uani 1 1 d . . . C35 C 0.7127(4) 0.6664(4) 0.0617(2) 0.0494(12) Uani 1 1 d . . . H35A H 0.7622 0.6753 0.0193 0.074 Uiso 1 1 calc R . . H35B H 0.7258 0.5840 0.0821 0.074 Uiso 1 1 calc R . . H35C H 0.7353 0.7058 0.0958 0.074 Uiso 1 1 calc R . . C36 C 0.5598(5) 0.8478(4) 0.0099(2) 0.0536(12) Uani 1 1 d . . . H36A H 0.6087 0.8549 -0.0330 0.080 Uiso 1 1 calc R . . H36B H 0.5839 0.8878 0.0429 0.080 Uiso 1 1 calc R . . H36C H 0.4744 0.8825 -0.0017 0.080 Uiso 1 1 calc R . . C37 C 0.5399(4) 0.6562(4) -0.0076(2) 0.0462(11) Uani 1 1 d . . . H37A H 0.5863 0.6644 -0.0514 0.069 Uiso 1 1 calc R . . H37B H 0.4538 0.6895 -0.0176 0.069 Uiso 1 1 calc R . . H37C H 0.5545 0.5741 0.0137 0.069 Uiso 1 1 calc R . . C38 C 0.1803(6) -0.0728(5) 0.0666(3) 0.097(2) Uani 1 1 d . . . H38A H 0.2623 -0.0795 0.0479 0.145 Uiso 1 1 calc R . . H38B H 0.1350 -0.1016 0.0367 0.145 Uiso 1 1 calc R . . H38C H 0.1836 -0.1184 0.1143 0.145 Uiso 1 1 calc R . . C39 C 0.1230(5) 0.0432(5) 0.0677(3) 0.0798(19) Uani 1 1 d . . . C40 C 0.2491(3) 0.5487(3) 0.14914(17) 0.0283(8) Uani 1 1 d . C . C41 C 0.1360(4) 0.5601(4) 0.1075(2) 0.0437(11) Uani 1 1 d . . . C42 C 0.1119(4) 0.4414(4) 0.1136(3) 0.0616(14) Uani 1 1 d . . . H42A H 0.0397 0.4499 0.0868 0.092 Uiso 1 1 calc R . . H42B H 0.0992 0.4094 0.1630 0.092 Uiso 1 1 calc R . . H42C H 0.1812 0.3890 0.0949 0.092 Uiso 1 1 calc R . . C43 C 0.1590(5) 0.6111(4) 0.0308(2) 0.0640(15) Uani 1 1 d . . . H43A H 0.0885 0.6193 0.0027 0.096 Uiso 1 1 calc R . . H43B H 0.2298 0.5595 0.0129 0.096 Uiso 1 1 calc R . . H43C H 0.1733 0.6872 0.0279 0.096 Uiso 1 1 calc R . . C44 C 0.0287(4) 0.6411(5) 0.1373(3) 0.086(2) Uani 1 1 d . . . H44A H -0.0441 0.6490 0.1113 0.130 Uiso 1 1 calc R . . H44B H 0.0437 0.7172 0.1329 0.130 Uiso 1 1 calc R . . H44C H 0.0175 0.6092 0.1869 0.130 Uiso 1 1 calc R . . N1 N 0.5907(3) 0.3410(2) 0.21739(15) 0.0277(7) Uani 1 1 d . . . N2 N 0.4301(3) 0.2182(2) 0.21915(15) 0.0272(7) Uani 1 1 d . . . N3 N 0.0771(6) 0.1355(6) 0.0701(4) 0.163(3) Uani 1 1 d . . . O1 O 0.4088(2) 0.51845(18) 0.28069(11) 0.0221(5) Uani 1 1 d . . . O2 O 0.5210(2) 0.3650(2) 0.42355(13) 0.0323(6) Uani 1 1 d . . . O3 O 0.4914(2) 0.26689(19) 0.34473(12) 0.0297(6) Uani 1 1 d . . . O4 O 0.3197(2) 0.4498(2) 0.16768(12) 0.0304(6) Uani 1 1 d . . . O5 O 0.2639(2) 0.6414(2) 0.16062(13) 0.0336(6) Uani 1 1 d . . . O6 O 0.5202(2) 0.6040(2) 0.14662(12) 0.0299(6) Uani 1 1 d . . . O7 O 0.4301(2) 0.7881(2) 0.12990(12) 0.0298(6) Uani 1 1 d . . . O8 O 0.5195(2) 0.7013(2) 0.26916(13) 0.0324(6) Uani 1 1 d . . . O9 O 0.5283(2) 0.6138(2) 0.38182(12) 0.0289(6) Uani 1 1 d . . . O10 O 0.2495(2) 0.4297(2) 0.39962(13) 0.0327(6) Uani 1 1 d . . . O11 O 0.2504(2) 0.3579(2) 0.30260(13) 0.0303(6) Uani 1 1 d . . . O12 O 0.3581(2) 0.5413(2) 0.49793(13) 0.0290(6) Uani 1 1 d D . . O13 O 0.2471(2) 0.6910(2) 0.36534(13) 0.0371(6) Uani 1 1 d . . . O14 O 0.2614(2) 0.7798(2) 0.25468(13) 0.0326(6) Uani 1 1 d . . . Fe2 Fe 0.40576(4) 0.37945(4) 0.26019(3) 0.02352(13) Uani 1 1 d . B . Fe1 Fe 0.39316(4) 0.65943(4) 0.22146(2) 0.02164(12) Uani 1 1 d . A . Mn1 Mn 0.38040(5) 0.52805(4) 0.38808(3) 0.02211(13) Uani 1 1 d . A . C25A C 0.069(3) 0.868(3) 0.3994(10) 0.085(3) Uani 0.200(14) 1 d PD A 1 H25A H 0.1254 0.8029 0.4281 0.128 Uiso 0.200(14) 1 calc PR A 1 H25B H -0.0140 0.8639 0.4110 0.128 Uiso 0.200(14) 1 calc PR A 1 H25C H 0.0787 0.9409 0.4087 0.128 Uiso 0.200(14) 1 calc PR A 1 C26A C 0.134(5) 0.944(4) 0.359(3) 0.118(5) Uani 0.200(14) 1 d PD A 1 H26A H 0.1640 0.9030 0.4054 0.176 Uiso 0.200(14) 1 calc PR A 1 H26B H 0.0653 1.0104 0.3632 0.176 Uiso 0.200(14) 1 calc PR A 1 H26C H 0.1978 0.9709 0.3310 0.176 Uiso 0.200(14) 1 calc PR A 1 C27A C 0.050(3) 0.938(4) 0.2517(12) 0.097(4) Uani 0.200(14) 1 d PD A 1 H27A H -0.0239 0.9973 0.2577 0.145 Uiso 0.200(14) 1 calc PR A 1 H27B H 0.0344 0.8882 0.2217 0.145 Uiso 0.200(14) 1 calc PR A 1 H27C H 0.1126 0.9744 0.2298 0.145 Uiso 0.200(14) 1 calc PR A 1 C25B C 0.0218(8) 0.8218(8) 0.3859(4) 0.085(3) Uani 0.800(14) 1 d PD A 2 H25D H 0.0114 0.7464 0.3824 0.128 Uiso 0.800(14) 1 calc PR A 2 H25E H -0.0574 0.8774 0.3868 0.128 Uiso 0.800(14) 1 calc PR A 2 H25F H 0.0651 0.8143 0.4290 0.128 Uiso 0.800(14) 1 calc PR A 2 C26B C 0.1235(10) 0.9780(7) 0.3172(8) 0.118(5) Uani 0.800(14) 1 d PD A 2 H26D H 0.1781 0.9723 0.3550 0.176 Uiso 0.800(14) 1 calc PR A 2 H26E H 0.0492 1.0390 0.3208 0.176 Uiso 0.800(14) 1 calc PR A 2 H26F H 0.1626 0.9966 0.2718 0.176 Uiso 0.800(14) 1 calc PR A 2 C27B C 0.0080(7) 0.8779(11) 0.2634(5) 0.097(4) Uani 0.800(14) 1 d PD A 2 H27D H -0.0133 0.8051 0.2657 0.145 Uiso 0.800(14) 1 calc PR A 2 H27E H 0.0477 0.8977 0.2184 0.145 Uiso 0.800(14) 1 calc PR A 2 H27F H -0.0652 0.9397 0.2678 0.145 Uiso 0.800(14) 1 calc PR A 2 C30A C 0.688(6) 0.728(6) 0.4069(17) 0.089(5) Uani 0.214(16) 1 d PD B 1 H30A H 0.7019 0.6555 0.4411 0.134 Uiso 0.214(16) 1 calc PR B 1 H30B H 0.6101 0.7803 0.4173 0.134 Uiso 0.214(16) 1 calc PR B 1 H30C H 0.7524 0.7649 0.4095 0.134 Uiso 0.214(16) 1 calc PR B 1 C31A C 0.752(3) 0.690(4) 0.2673(15) 0.101(5) Uani 0.214(16) 1 d PD B 1 H31A H 0.7988 0.6087 0.2710 0.151 Uiso 0.214(16) 1 calc PR B 1 H31B H 0.8069 0.7397 0.2582 0.151 Uiso 0.214(16) 1 calc PR B 1 H31C H 0.6947 0.7105 0.2287 0.151 Uiso 0.214(16) 1 calc PR B 1 C32A C 0.686(6) 0.803(4) 0.276(2) 0.102(5) Uani 0.214(16) 1 d PD B 1 H32A H 0.6331 0.8746 0.2872 0.153 Uiso 0.214(16) 1 calc PR B 1 H32B H 0.6566 0.7884 0.2331 0.153 Uiso 0.214(16) 1 calc PR B 1 H32C H 0.7681 0.8106 0.2678 0.153 Uiso 0.214(16) 1 calc PR B 1 C30B C 0.7259(13) 0.6887(15) 0.4092(5) 0.089(5) Uani 0.786(16) 1 d PD B 2 H30D H 0.7358 0.6081 0.4329 0.134 Uiso 0.786(16) 1 calc PR B 2 H30E H 0.6657 0.7398 0.4345 0.134 Uiso 0.786(16) 1 calc PR B 2 H30F H 0.8032 0.7079 0.4085 0.134 Uiso 0.786(16) 1 calc PR B 2 C31B C 0.7845(6) 0.6164(11) 0.3065(8) 0.101(5) Uani 0.786(16) 1 d PD B 2 H31D H 0.7865 0.5388 0.3330 0.151 Uiso 0.786(16) 1 calc PR B 2 H31E H 0.8619 0.6326 0.3113 0.151 Uiso 0.786(16) 1 calc PR B 2 H31F H 0.7701 0.6204 0.2569 0.151 Uiso 0.786(16) 1 calc PR B 2 C32B C 0.6672(15) 0.8313(8) 0.3019(7) 0.102(5) Uani 0.786(16) 1 d PD B 2 H32D H 0.6009 0.8788 0.3257 0.153 Uiso 0.786(16) 1 calc PR B 2 H32E H 0.6481 0.8437 0.2521 0.153 Uiso 0.786(16) 1 calc PR B 2 H32F H 0.7415 0.8533 0.3065 0.153 Uiso 0.786(16) 1 calc PR B 2 C15A C 0.6099(7) 0.1429(5) 0.5121(3) 0.0646(19) Uani 0.813(5) 1 d PD C 1 H15A H 0.6101 0.2107 0.5314 0.097 Uiso 0.813(5) 1 calc PR C 1 H15B H 0.6721 0.0757 0.5352 0.097 Uiso 0.813(5) 1 calc PR C 1 H15C H 0.5308 0.1272 0.5201 0.097 Uiso 0.813(5) 1 calc PR C 1 C16A C 0.6377(6) 0.0622(4) 0.4025(4) 0.066(2) Uani 0.813(5) 1 d PD C 1 H16A H 0.6988 -0.0053 0.4263 0.098 Uiso 0.813(5) 1 calc PR C 1 H16B H 0.6571 0.0776 0.3524 0.098 Uiso 0.813(5) 1 calc PR C 1 H16C H 0.5583 0.0468 0.4089 0.098 Uiso 0.813(5) 1 calc PR C 1 C17A C 0.7592(5) 0.1932(5) 0.4217(4) 0.0669(19) Uani 0.813(5) 1 d PD C 1 H17A H 0.7577 0.2607 0.4418 0.100 Uiso 0.813(5) 1 calc PR C 1 H17B H 0.7764 0.2097 0.3713 0.100 Uiso 0.813(5) 1 calc PR C 1 H17C H 0.8219 0.1264 0.4445 0.100 Uiso 0.813(5) 1 calc PR C 1 C15B C 0.691(3) 0.181(2) 0.4972(12) 0.0646(19) Uani 0.187(5) 1 d PD C 2 H15D H 0.7498 0.1087 0.5169 0.097 Uiso 0.187(5) 1 calc PR C 2 H15E H 0.6274 0.2006 0.5320 0.097 Uiso 0.187(5) 1 calc PR C 2 H15F H 0.7310 0.2433 0.4846 0.097 Uiso 0.187(5) 1 calc PR C 2 C16B C 0.560(2) 0.0766(17) 0.4505(15) 0.066(2) Uani 0.187(5) 1 d PD C 2 H16D H 0.6114 0.0015 0.4731 0.098 Uiso 0.187(5) 1 calc PR C 2 H16E H 0.5275 0.0689 0.4070 0.098 Uiso 0.187(5) 1 calc PR C 2 H16F H 0.4935 0.1030 0.4822 0.098 Uiso 0.187(5) 1 calc PR C 2 C17B C 0.729(2) 0.125(2) 0.3759(12) 0.0669(19) Uani 0.187(5) 1 d PD C 2 H17D H 0.7903 0.0552 0.3971 0.100 Uiso 0.187(5) 1 calc PR C 2 H17E H 0.7679 0.1859 0.3555 0.100 Uiso 0.187(5) 1 calc PR C 2 H17F H 0.6871 0.1071 0.3390 0.100 Uiso 0.187(5) 1 calc PR C 2 H12B H 0.375(5) 0.593(3) 0.513(3) 0.080 Uiso 1 1 d D . . H12A H 0.376(4) 0.479(3) 0.527(2) 0.080 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.033(2) 0.0248(17) 0.0181(17) 0.0005(14) -0.0033(15) -0.0098(16) C2 0.048(3) 0.0283(19) 0.026(2) -0.0068(16) -0.0015(18) -0.0116(18) C3 0.059(3) 0.033(2) 0.034(2) -0.0147(18) 0.001(2) -0.018(2) C4 0.063(3) 0.044(2) 0.036(2) -0.014(2) 0.002(2) -0.033(2) C5 0.045(3) 0.047(2) 0.038(2) -0.014(2) 0.0073(19) -0.028(2) C6 0.034(2) 0.0278(19) 0.032(2) -0.0059(16) -0.0037(17) -0.0111(17) C7 0.032(2) 0.039(2) 0.046(3) -0.0067(19) 0.0000(19) -0.0141(18) C8 0.026(2) 0.049(2) 0.041(2) -0.008(2) 0.0007(18) -0.0053(19) C9 0.031(2) 0.036(2) 0.029(2) -0.0040(17) -0.0019(17) -0.0053(17) C10 0.032(2) 0.0260(18) 0.0211(18) -0.0013(15) -0.0038(15) -0.0081(16) C11 0.039(2) 0.042(2) 0.047(3) -0.016(2) 0.005(2) -0.005(2) C12 0.051(3) 0.035(2) 0.044(3) -0.0179(19) 0.004(2) -0.005(2) C13 0.032(2) 0.0209(17) 0.0272(19) -0.0020(15) 0.0010(16) -0.0104(15) C14 0.043(2) 0.0262(19) 0.037(2) -0.0042(17) -0.0106(19) -0.0016(18) C18 0.028(2) 0.0254(18) 0.0262(19) -0.0047(15) -0.0019(16) -0.0089(15) C19 0.032(2) 0.039(2) 0.027(2) -0.0110(17) 0.0068(16) -0.0195(17) C20 0.038(2) 0.065(3) 0.037(2) -0.017(2) 0.0115(19) -0.021(2) C21 0.071(3) 0.039(2) 0.053(3) -0.001(2) 0.006(2) -0.028(2) C22 0.038(3) 0.077(3) 0.044(3) -0.020(2) 0.005(2) -0.035(2) C23 0.027(2) 0.0280(19) 0.034(2) -0.0100(17) -0.0002(17) -0.0113(16) C24 0.025(2) 0.034(2) 0.030(2) -0.0059(17) 0.0010(16) -0.0016(16) C28 0.028(2) 0.0209(17) 0.0247(19) -0.0067(15) -0.0029(15) -0.0064(15) C29 0.029(2) 0.037(2) 0.032(2) -0.0038(17) -0.0020(17) -0.0184(17) C33 0.026(2) 0.035(2) 0.0187(18) -0.0061(16) -0.0041(15) -0.0112(16) C34 0.038(2) 0.036(2) 0.0220(19) -0.0043(16) -0.0010(16) -0.0140(18) C35 0.043(3) 0.075(3) 0.032(2) -0.008(2) 0.007(2) -0.023(2) C36 0.082(4) 0.049(3) 0.030(2) 0.000(2) 0.012(2) -0.028(3) C37 0.054(3) 0.064(3) 0.031(2) -0.019(2) 0.005(2) -0.026(2) C38 0.101(5) 0.085(4) 0.075(4) -0.012(4) -0.012(4) 0.024(4) C39 0.040(3) 0.074(4) 0.093(5) 0.016(3) 0.016(3) 0.010(3) C40 0.030(2) 0.042(2) 0.0150(17) -0.0073(16) 0.0034(15) -0.0132(18) C41 0.032(2) 0.063(3) 0.043(3) -0.027(2) -0.0074(19) -0.010(2) C42 0.052(3) 0.084(4) 0.069(3) -0.030(3) -0.012(3) -0.036(3) C43 0.086(4) 0.065(3) 0.040(3) -0.010(2) -0.030(3) -0.012(3) C44 0.027(3) 0.116(5) 0.134(6) -0.079(4) -0.012(3) -0.007(3) N1 0.0308(17) 0.0259(15) 0.0284(17) -0.0040(13) -0.0034(13) -0.0111(13) N2 0.0296(17) 0.0287(15) 0.0254(16) -0.0074(13) 0.0010(13) -0.0102(13) N3 0.126(6) 0.093(5) 0.214(8) 0.013(5) 0.062(6) 0.021(4) O1 0.0264(13) 0.0237(12) 0.0181(12) -0.0037(10) -0.0021(10) -0.0097(10) O2 0.0378(15) 0.0255(13) 0.0345(15) -0.0093(11) -0.0100(12) -0.0056(11) O3 0.0420(16) 0.0258(13) 0.0238(13) -0.0051(11) -0.0054(12) -0.0116(11) O4 0.0365(15) 0.0326(14) 0.0238(13) -0.0092(11) -0.0032(11) -0.0086(12) O5 0.0338(15) 0.0343(14) 0.0339(15) -0.0040(12) -0.0122(12) -0.0102(12) O6 0.0351(15) 0.0271(13) 0.0254(13) -0.0013(11) 0.0032(11) -0.0085(11) O7 0.0365(15) 0.0282(13) 0.0251(13) -0.0070(11) -0.0018(11) -0.0077(12) O8 0.0407(16) 0.0374(14) 0.0242(14) -0.0002(11) -0.0062(12) -0.0218(12) O9 0.0331(15) 0.0338(14) 0.0243(13) -0.0019(11) -0.0053(11) -0.0178(12) O10 0.0395(16) 0.0410(15) 0.0266(14) -0.0123(12) 0.0032(12) -0.0223(13) O11 0.0283(14) 0.0438(15) 0.0274(14) -0.0135(12) 0.0053(11) -0.0199(12) O12 0.0366(15) 0.0287(14) 0.0239(14) -0.0051(11) -0.0022(11) -0.0120(12) O13 0.0409(16) 0.0333(14) 0.0289(15) -0.0018(12) -0.0002(12) 0.0008(12) O14 0.0330(15) 0.0310(13) 0.0285(14) -0.0037(11) 0.0051(12) -0.0027(11) Fe2 0.0258(3) 0.0253(3) 0.0229(3) -0.0078(2) -0.0004(2) -0.0101(2) Fe1 0.0230(3) 0.0226(2) 0.0193(3) -0.0033(2) -0.0017(2) -0.0063(2) Mn1 0.0259(3) 0.0220(3) 0.0202(3) -0.0043(2) -0.0034(2) -0.0084(2) C25A 0.044(5) 0.081(6) 0.093(5) 0.023(4) 0.035(4) 0.010(4) C26A 0.065(5) 0.042(6) 0.255(16) -0.066(8) 0.061(9) -0.016(5) C27A 0.032(5) 0.153(10) 0.090(5) -0.054(6) -0.028(4) 0.027(5) C25B 0.044(5) 0.081(6) 0.093(5) 0.023(4) 0.035(4) 0.010(4) C26B 0.065(5) 0.042(6) 0.255(16) -0.066(8) 0.061(9) -0.016(5) C27B 0.032(5) 0.153(10) 0.090(5) -0.054(6) -0.028(4) 0.027(5) C30A 0.081(11) 0.166(14) 0.051(4) 0.004(5) -0.022(4) -0.096(10) C31A 0.023(4) 0.114(9) 0.192(12) -0.101(9) 0.010(5) -0.014(5) C32A 0.103(7) 0.061(6) 0.154(10) 0.037(6) -0.075(9) -0.067(7) C30B 0.081(11) 0.166(14) 0.051(4) 0.004(5) -0.022(4) -0.096(10) C31B 0.023(4) 0.114(9) 0.192(12) -0.101(9) 0.010(5) -0.014(5) C32B 0.103(7) 0.061(6) 0.154(10) 0.037(6) -0.075(9) -0.067(7) C15A 0.095(6) 0.040(3) 0.045(3) 0.005(3) -0.007(3) -0.002(3) C16A 0.085(5) 0.020(2) 0.084(5) -0.013(3) -0.033(4) 0.008(3) C17A 0.032(3) 0.053(4) 0.107(6) -0.013(4) -0.010(3) 0.004(3) C15B 0.095(6) 0.040(3) 0.045(3) 0.005(3) -0.007(3) -0.002(3) C16B 0.085(5) 0.020(2) 0.084(5) -0.013(3) -0.033(4) 0.008(3) C17B 0.032(3) 0.053(4) 0.107(6) -0.013(4) -0.010(3) 0.004(3) _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 C1 N2 1.357(4) . ? C1 C2 1.415(5) . ? C1 C10 1.436(5) . ? C2 C3 1.408(5) . ? C2 C12 1.424(5) . ? C3 C4 1.353(6) . ? C4 C5 1.401(5) . ? C5 N2 1.318(5) . ? C6 N1 1.324(4) . ? C6 C7 1.400(5) . ? C7 C8 1.366(5) . ? C8 C9 1.409(5) . ? C9 C10 1.405(5) . ? C9 C11 1.435(5) . ? C10 N1 1.356(4) . ? C11 C12 1.342(6) . ? C13 O2 1.260(4) . ? C13 O3 1.261(4) . ? C13 C14 1.527(5) . ? C14 C15B 1.492(17) . ? C14 C16A 1.514(6) . ? C14 C15A 1.528(7) . ? C14 C17A 1.534(7) . ? C14 C16B 1.561(17) . ? C14 C17B 1.563(17) . ? C18 O10 1.246(4) . ? C18 O11 1.277(4) . ? C18 C19 1.527(5) . ? C19 C20 1.530(5) . ? C19 C21 1.532(5) . ? C19 C22 1.533(5) . ? C23 O13 1.239(4) . ? C23 O14 1.272(4) . ? C23 C24 1.538(5) . ? C24 C26A 1.486(19) . ? C24 C25A 1.503(18) . ? C24 C26B 1.505(7) . ? C24 C25B 1.516(7) . ? C24 C27A 1.525(18) . ? C24 C27B 1.527(7) . ? C28 O9 1.247(4) . ? C28 O8 1.273(4) . ? C28 C29 1.530(5) . ? C29 C32A 1.490(18) . ? C29 C30A 1.495(18) . ? C29 C31A 1.504(18) . ? C29 C31B 1.511(7) . ? C29 C30B 1.513(8) . ? C29 C32B 1.517(7) . ? C33 O7 1.259(4) . ? C33 O6 1.266(4) . ? C33 C34 1.517(5) . ? C33 Fe1 2.500(3) . ? C34 C36 1.528(5) . ? C34 C37 1.534(5) . ? C34 C35 1.535(5) . ? C38 C39 1.398(8) . ? C39 N3 1.118(8) . ? C40 O4 1.257(4) . ? C40 O5 1.259(4) . ? C40 C41 1.539(5) . ? C41 C44 1.525(6) . ? C41 C43 1.533(6) . ? C41 C42 1.534(6) . ? N1 Fe2 2.202(3) . ? N2 Fe2 2.220(3) . ? O1 Fe2 1.836(2) . ? O1 Fe1 1.842(2) . ? O1 Mn1 2.119(2) . ? O2 Mn1 2.214(2) . ? O3 Fe2 2.031(2) . ? O4 Fe2 2.025(2) . ? O5 Fe1 2.046(2) . ? O6 Fe1 2.078(2) . ? O7 Fe1 2.231(2) . ? O8 Fe1 2.006(2) . ? O9 Mn1 2.221(2) . ? O10 Mn1 2.151(2) . ? O11 Fe2 1.986(2) . ? O12 Mn1 2.172(3) . ? O13 Mn1 2.143(2) . ? O14 Fe1 1.984(2) . ? 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 C1 C2 123.1(3) . . ? N2 C1 C10 117.5(3) . . ? C2 C1 C10 119.5(3) . . ? C3 C2 C1 116.3(4) . . ? C3 C2 C12 124.8(4) . . ? C1 C2 C12 118.8(3) . . ? C4 C3 C2 120.6(4) . . ? C3 C4 C5 118.7(4) . . ? N2 C5 C4 123.7(4) . . ? N1 C6 C7 122.6(3) . . ? C8 C7 C6 119.5(4) . . ? C7 C8 C9 119.4(4) . . ? C10 C9 C8 117.2(3) . . ? C10 C9 C11 118.8(4) . . ? C8 C9 C11 124.0(4) . . ? N1 C10 C9 122.8(3) . . ? N1 C10 C1 117.2(3) . . ? C9 C10 C1 120.0(3) . . ? C12 C11 C9 121.2(4) . . ? C11 C12 C2 121.7(4) . . ? O2 C13 O3 124.2(3) . . ? O2 C13 C14 119.1(3) . . ? O3 C13 C14 116.8(3) . . ? C15B C14 C16A 133.4(10) . . ? C15B C14 C13 113.9(10) . . ? C16A C14 C13 111.8(3) . . ? C15B C14 C15A 44.7(12) . . ? C16A C14 C15A 110.3(4) . . ? C13 C14 C15A 109.3(4) . . ? C15B C14 C17A 64.9(13) . . ? C16A C14 C17A 109.8(4) . . ? C13 C14 C17A 106.6(3) . . ? C15A C14 C17A 108.8(5) . . ? C15B C14 C16B 112.5(16) . . ? C16A C14 C16B 48.2(10) . . ? C13 C14 C16B 101.6(9) . . ? C15A C14 C16B 70.4(11) . . ? C17A C14 C16B 149.9(10) . . ? C15B C14 C17B 114.7(16) . . ? C16A C14 C17B 57.3(11) . . ? C13 C14 C17B 107.6(10) . . ? C15A C14 C17B 142.9(10) . . ? C17A C14 C17B 56.1(10) . . ? C16B C14 C17B 105.5(15) . . ? O10 C18 O11 125.1(3) . . ? O10 C18 C19 119.0(3) . . ? O11 C18 C19 115.8(3) . . ? C18 C19 C20 110.0(3) . . ? C18 C19 C21 106.1(3) . . ? C20 C19 C21 110.2(3) . . ? C18 C19 C22 110.5(3) . . ? C20 C19 C22 110.0(3) . . ? C21 C19 C22 110.1(3) . . ? O13 C23 O14 124.9(3) . . ? O13 C23 C24 118.6(3) . . ? O14 C23 C24 116.5(3) . . ? C26A C24 C25A 57(3) . . ? C26A C24 C26B 32(2) . . ? C25A C24 C26B 86(2) . . ? C26A C24 C25B 94(2) . . ? C25A C24 C25B 37.4(14) . . ? C26B C24 C25B 119.5(9) . . ? C26A C24 C27A 104(2) . . ? C25A C24 C27A 139(2) . . ? C26B C24 C27A 72.4(17) . . ? C25B C24 C27A 129.8(16) . . ? C26A C24 C27B 136(2) . . ? C25A C24 C27B 130.7(15) . . ? C26B C24 C27B 107.4(6) . . ? C25B C24 C27B 100.9(9) . . ? C27A C24 C27B 37.0(16) . . ? C26A C24 C23 104(2) . . ? C25A C24 C23 110.3(12) . . ? C26B C24 C23 109.1(5) . . ? C25B C24 C23 110.1(4) . . ? C27A C24 C23 110.0(14) . . ? C27B C24 C23 109.2(4) . . ? O9 C28 O8 124.8(3) . . ? O9 C28 C29 119.8(3) . . ? O8 C28 C29 115.4(3) . . ? C32A C29 C30A 116(3) . . ? C32A C29 C31A 57(3) . . ? C30A C29 C31A 147(3) . . ? C32A C29 C31B 96(3) . . ? C30A C29 C31B 122(3) . . ? C31A C29 C31B 40.7(14) . . ? C32A C29 C30B 128(2) . . ? C30A C29 C30B 21(3) . . ? C31A C29 C30B 132.4(16) . . ? C31B C29 C30B 101.3(9) . . ? C32A C29 C32B 26(3) . . ? C30A C29 C32B 92(3) . . ? C31A C29 C32B 81(2) . . ? C31B C29 C32B 118.1(10) . . ? C30B C29 C32B 107.0(8) . . ? C32A C29 C28 107(2) . . ? C30A C29 C28 107(3) . . ? C31A C29 C28 106.0(12) . . ? C31B C29 C28 106.9(4) . . ? C30B C29 C28 114.0(7) . . ? C32B C29 C28 109.7(6) . . ? O7 C33 O6 119.1(3) . . ? O7 C33 C34 122.4(3) . . ? O6 C33 C34 118.5(3) . . ? O7 C33 Fe1 63.00(18) . . ? O6 C33 Fe1 56.08(17) . . ? C34 C33 Fe1 174.6(3) . . ? C33 C34 C36 111.4(3) . . ? C33 C34 C37 107.6(3) . . ? C36 C34 C37 110.2(3) . . ? C33 C34 C35 108.0(3) . . ? C36 C34 C35 109.2(3) . . ? C37 C34 C35 110.5(3) . . ? N3 C39 C38 178.6(8) . . ? O4 C40 O5 125.4(3) . . ? O4 C40 C41 118.5(3) . . ? O5 C40 C41 116.1(3) . . ? C44 C41 C43 110.4(4) . . ? C44 C41 C42 109.5(4) . . ? C43 C41 C42 110.6(4) . . ? C44 C41 C40 108.6(3) . . ? C43 C41 C40 107.4(4) . . ? C42 C41 C40 110.3(4) . . ? C6 N1 C10 118.4(3) . . ? C6 N1 Fe2 125.6(2) . . ? C10 N1 Fe2 115.8(2) . . ? C5 N2 C1 117.7(3) . . ? C5 N2 Fe2 127.3(3) . . ? C1 N2 Fe2 115.0(2) . . ? Fe2 O1 Fe1 129.26(12) . . ? Fe2 O1 Mn1 114.35(11) . . ? Fe1 O1 Mn1 114.28(11) . . ? C13 O2 Mn1 126.3(2) . . ? C13 O3 Fe2 135.7(2) . . ? C40 O4 Fe2 128.6(2) . . ? C40 O5 Fe1 127.3(2) . . ? C33 O6 Fe1 93.6(2) . . ? C33 O7 Fe1 86.8(2) . . ? C28 O8 Fe1 135.8(2) . . ? C28 O9 Mn1 128.9(2) . . ? C18 O10 Mn1 136.8(2) . . ? C18 O11 Fe2 126.2(2) . . ? C23 O13 Mn1 139.0(2) . . ? C23 O14 Fe1 126.0(2) . . ? O1 Fe2 O11 102.64(10) . . ? O1 Fe2 O4 95.02(10) . . ? O11 Fe2 O4 88.49(10) . . ? O1 Fe2 O3 101.15(9) . . ? O11 Fe2 O3 88.53(10) . . ? O4 Fe2 O3 163.82(9) . . ? O1 Fe2 N1 94.93(10) . . ? O11 Fe2 N1 161.03(10) . . ? O4 Fe2 N1 97.13(10) . . ? O3 Fe2 N1 81.02(10) . . ? O1 Fe2 N2 168.37(10) . . ? O11 Fe2 N2 88.41(10) . . ? O4 Fe2 N2 81.49(10) . . ? O3 Fe2 N2 82.53(10) . . ? N1 Fe2 N2 74.62(11) . . ? O1 Fe1 O14 110.29(10) . . ? O1 Fe1 O8 94.74(10) . . ? O14 Fe1 O8 92.36(11) . . ? O1 Fe1 O5 94.85(10) . . ? O14 Fe1 O5 85.32(10) . . ? O8 Fe1 O5 170.35(10) . . ? O1 Fe1 O6 97.92(10) . . ? O14 Fe1 O6 151.45(10) . . ? O8 Fe1 O6 89.51(10) . . ? O5 Fe1 O6 88.11(10) . . ? O1 Fe1 O7 158.43(10) . . ? O14 Fe1 O7 91.27(10) . . ? O8 Fe1 O7 84.43(9) . . ? O5 Fe1 O7 86.25(9) . . ? O6 Fe1 O7 60.55(9) . . ? O1 Fe1 C33 128.29(11) . . ? O14 Fe1 C33 121.33(11) . . ? O8 Fe1 C33 86.51(11) . . ? O5 Fe1 C33 86.70(11) . . ? O6 Fe1 C33 30.37(10) . . ? O7 Fe1 C33 30.18(10) . . ? O1 Mn1 O13 92.87(9) . . ? O1 Mn1 O10 92.12(9) . . ? O13 Mn1 O10 93.52(10) . . ? O1 Mn1 O12 177.43(10) . . ? O13 Mn1 O12 87.35(10) . . ? O10 Mn1 O12 90.42(9) . . ? O1 Mn1 O2 93.40(9) . . ? O13 Mn1 O2 173.24(10) . . ? O10 Mn1 O2 88.78(10) . . ? O12 Mn1 O2 86.28(9) . . ? O1 Mn1 O9 89.33(9) . . ? O13 Mn1 O9 91.92(10) . . ? O10 Mn1 O9 174.29(10) . . ? O12 Mn1 O9 88.10(9) . . ? O2 Mn1 O9 85.62(9) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.57 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.446 _refine_diff_density_min -0.452 _refine_diff_density_rms 0.082 #END data_pa_396_0m _database_code_depnum_ccdc_archive 'CCDC 750193' #TrackingRef 'albores_et_al.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H124 Co2 Fe4 N6 O28' _chemical_formula_weight 1863.03 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.8218(10) _cell_length_b 13.6367(12) _cell_length_c 18.0729(16) _cell_angle_alpha 109.112(2) _cell_angle_beta 105.071(3) _cell_angle_gamma 107.185(3) _cell_volume 2415.9(6) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.281 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 980 _exptl_absorpt_coefficient_mu 0.990 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.8491 _exptl_absorpt_correction_T_max 0.9805 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71069 _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 25041 _diffrn_reflns_av_R_equivalents 0.1106 _diffrn_reflns_av_sigmaI/netI 0.1642 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 26.73 _reflns_number_total 9958 _reflns_number_gt 4954 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0541P)^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 9958 _refine_ls_number_parameters 542 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1514 _refine_ls_R_factor_gt 0.0629 _refine_ls_wR_factor_ref 0.1555 _refine_ls_wR_factor_gt 0.1206 _refine_ls_goodness_of_fit_ref 0.943 _refine_ls_restrained_S_all 0.943 _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 Fe2 Fe 0.38595(7) 0.31755(6) 0.33600(5) 0.0239(2) Uani 1 1 d . . . Co1 Co 0.23836(7) 0.10285(6) 0.14717(5) 0.0263(2) Uani 1 1 d . . . Fe1 Fe 0.25317(7) 0.06687(7) 0.32301(5) 0.0253(2) Uani 1 1 d . . . O1 O 0.5228(3) 0.3013(3) 0.4220(2) 0.0272(9) Uani 1 1 d . . . O2 O 0.1611(3) 0.1537(3) 0.3831(2) 0.0320(10) Uani 1 1 d . . . O3 O 0.5030(3) 0.3325(3) 0.2735(2) 0.0304(9) Uani 1 1 d . . . O4 O 0.4246(3) 0.1684(3) 0.1557(2) 0.0330(10) Uani 1 1 d . . . O5 O 0.3323(4) -0.0312(3) 0.2671(2) 0.0327(10) Uani 1 1 d . . . O6 O 0.0696(4) -0.0597(3) 0.2389(2) 0.0354(10) Uani 1 1 d . . . O7 O 0.1625(4) -0.0650(3) 0.3580(2) 0.0331(10) Uani 1 1 d . . . O8 O 0.2205(4) 0.2460(3) 0.1368(2) 0.0349(10) Uani 1 1 d . . . O9 O 0.2801(3) 0.3760(3) 0.2698(2) 0.0305(9) Uani 1 1 d . . . O10 O 0.4092(3) 0.1435(3) 0.4293(2) 0.0290(9) Uani 1 1 d . . . O11 O 0.2546(4) -0.0468(3) 0.1352(2) 0.0346(10) Uani 1 1 d . . . N2 N 0.0302(4) 0.0456(4) 0.1110(3) 0.0240(10) Uani 1 1 d . . . O12 O 0.4992(4) 0.4948(3) 0.4166(2) 0.0318(10) Uani 1 1 d D . . O13 O 0.2881(3) 0.3339(3) 0.4155(2) 0.0270(9) Uani 1 1 d . . . O14 O 0.2821(3) 0.1637(3) 0.2725(2) 0.0250(9) Uani 1 1 d . . . N1 N 0.1630(4) 0.0272(4) 0.0115(3) 0.0251(11) Uani 1 1 d . . . C1 C 0.6259(6) 0.3144(5) 0.1884(4) 0.0419(16) Uani 1 1 d D . . C2 C -0.0363(5) 0.0058(4) 0.0280(3) 0.0218(12) Uani 1 1 d . . . C3 C 0.2281(6) 0.0147(5) -0.0397(4) 0.0341(15) Uani 1 1 d . . . H3 H 0.3184 0.0371 -0.0149 0.041 Uiso 1 1 calc R . . C4 C 0.0693(6) -0.1086(5) 0.2879(4) 0.0325(14) Uani 1 1 d . B . C5 C 0.1680(5) -0.0292(5) -0.1260(3) 0.0320(14) Uani 1 1 d . . . H5 H 0.2145 -0.0395 -0.1614 0.038 Uiso 1 1 calc R . . C6 C 0.2289(5) 0.3368(5) 0.1900(4) 0.0305(14) Uani 1 1 d . C . C7 C 0.5133(5) 0.2263(5) 0.4479(3) 0.0271(13) Uani 1 1 d . . . C8 C 0.6369(5) 0.2294(5) 0.5050(4) 0.0339(14) Uani 1 1 d . . . C9 C 0.5081(5) 0.2671(5) 0.2078(4) 0.0289(13) Uani 1 1 d . A . C10 C 0.3824(6) -0.1483(5) 0.1604(4) 0.0388(16) Uani 1 1 d . . . C11 C -0.0468(6) -0.2195(6) 0.2589(4) 0.0474(18) Uani 1 1 d D . . C12 C 0.1701(7) 0.4053(6) 0.1537(4) 0.0472(18) Uani 1 1 d D . . C13 C 0.1880(5) 0.2591(5) 0.4092(3) 0.0282(13) Uani 1 1 d . . . C1S C 0.6650(7) 0.7688(6) 0.4005(4) 0.0468(18) Uani 1 1 d . . . C14 C 0.0870(6) 0.2984(5) 0.4319(4) 0.0442(17) Uani 1 1 d . . . C15 C -0.0368(6) 0.0585(5) 0.1604(4) 0.0313(14) Uani 1 1 d . . . H15 H 0.0067 0.0884 0.2204 0.038 Uiso 1 1 calc R . . C16A C 0.7375(10) 0.4152(11) 0.2653(8) 0.074(4) Uani 0.606(8) 1 d PD A 1 H16A H 0.7073 0.4721 0.2912 0.111 Uiso 0.606(8) 1 calc PR A 1 H16B H 0.8046 0.4494 0.2476 0.111 Uiso 0.606(8) 1 calc PR A 1 H16C H 0.7729 0.3894 0.3069 0.111 Uiso 0.606(8) 1 calc PR A 1 C29A C 0.5795(16) 0.3569(16) 0.1198(11) 0.109(6) Uani 0.606(8) 1 d PD A 1 H29A H 0.5555 0.4191 0.1444 0.164 Uiso 0.606(8) 1 calc PR A 1 H29B H 0.5046 0.2936 0.0702 0.164 Uiso 0.606(8) 1 calc PR A 1 H29C H 0.6494 0.3843 0.1020 0.164 Uiso 0.606(8) 1 calc PR A 1 C32A C 0.6683(18) 0.2218(13) 0.1480(12) 0.086(7) Uani 0.606(8) 1 d PD A 1 H32A H 0.5945 0.1575 0.0983 0.129 Uiso 0.606(8) 1 calc PR A 1 H32B H 0.7011 0.1953 0.1898 0.129 Uiso 0.606(8) 1 calc PR A 1 H32C H 0.7365 0.2532 0.1301 0.129 Uiso 0.606(8) 1 calc PR A 1 C16B C 0.7372(15) 0.3263(19) 0.2628(11) 0.074(4) Uani 0.394(8) 1 d PD A 2 H16D H 0.7431 0.3800 0.3169 0.111 Uiso 0.394(8) 1 calc PR A 2 H16E H 0.8184 0.3549 0.2560 0.111 Uiso 0.394(8) 1 calc PR A 2 H16F H 0.7209 0.2516 0.2630 0.111 Uiso 0.394(8) 1 calc PR A 2 C29B C 0.642(3) 0.4332(17) 0.1943(19) 0.109(6) Uani 0.394(8) 1 d PD A 2 H29D H 0.6552 0.4833 0.2520 0.164 Uiso 0.394(8) 1 calc PR A 2 H29E H 0.5637 0.4262 0.1530 0.164 Uiso 0.394(8) 1 calc PR A 2 H29F H 0.7160 0.4657 0.1818 0.164 Uiso 0.394(8) 1 calc PR A 2 C32B C 0.614(3) 0.235(2) 0.1027(13) 0.086(7) Uani 0.394(8) 1 d PD A 2 H32D H 0.6905 0.2683 0.0926 0.129 Uiso 0.394(8) 1 calc PR A 2 H32E H 0.5371 0.2240 0.0578 0.129 Uiso 0.394(8) 1 calc PR A 2 H32F H 0.6058 0.1611 0.1022 0.129 Uiso 0.394(8) 1 calc PR A 2 C26A C -0.006(5) -0.292(5) 0.301(4) 0.072(4) Uani 0.148(15) 1 d PD B 1 H26D H 0.0030 -0.2611 0.3603 0.109 Uiso 0.148(15) 1 calc PR B 1 H26E H 0.0759 -0.2913 0.2987 0.109 Uiso 0.148(15) 1 calc PR B 1 H26F H -0.0725 -0.3712 0.2699 0.109 Uiso 0.148(15) 1 calc PR B 1 C28A C -0.0469(14) -0.3095(10) 0.1833(9) 0.116(7) Uani 0.852(15) 1 d PD B 1 H28A H 0.0336 -0.3188 0.1999 0.174 Uiso 0.852(15) 1 calc PR B 1 H28B H -0.0543 -0.2860 0.1372 0.174 Uiso 0.852(15) 1 calc PR B 1 H28C H -0.1201 -0.3821 0.1638 0.174 Uiso 0.852(15) 1 calc PR B 1 C31A C -0.141(5) -0.181(5) 0.290(5) 0.096(5) Uani 0.148(15) 1 d PD B 1 H31D H -0.0973 -0.1280 0.3511 0.144 Uiso 0.148(15) 1 calc PR B 1 H31E H -0.2139 -0.2472 0.2813 0.144 Uiso 0.148(15) 1 calc PR B 1 H31F H -0.1729 -0.1417 0.2583 0.144 Uiso 0.148(15) 1 calc PR B 1 C26B C -0.0459(10) -0.2465(10) 0.3346(6) 0.072(4) Uani 0.852(15) 1 d PD B 2 H26A H -0.0563 -0.1869 0.3769 0.109 Uiso 0.852(15) 1 calc PR B 2 H26B H 0.0362 -0.2493 0.3605 0.109 Uiso 0.852(15) 1 calc PR B 2 H26C H -0.1170 -0.3205 0.3150 0.109 Uiso 0.852(15) 1 calc PR B 2 C28B C 0.005(8) -0.304(7) 0.221(6) 0.116(7) Uani 0.148(15) 1 d PD B 2 H28D H 0.0869 -0.2879 0.2631 0.174 Uiso 0.148(15) 1 calc PR B 2 H28E H 0.0179 -0.2966 0.1709 0.174 Uiso 0.148(15) 1 calc PR B 2 H28F H -0.0573 -0.3816 0.2029 0.174 Uiso 0.148(15) 1 calc PR B 2 C31B C -0.1731(8) -0.2076(10) 0.2251(10) 0.096(5) Uani 0.852(15) 1 d PD B 2 H31A H -0.1736 -0.1425 0.2690 0.144 Uiso 0.852(15) 1 calc PR B 2 H31B H -0.2464 -0.2775 0.2107 0.144 Uiso 0.852(15) 1 calc PR B 2 H31C H -0.1798 -0.1950 0.1741 0.144 Uiso 0.852(15) 1 calc PR B 2 C30A C 0.239(3) 0.5322(12) 0.2097(16) 0.125(14) Uani 0.594(10) 1 d PD C 1 H30A H 0.1977 0.5718 0.1833 0.187 Uiso 0.594(10) 1 calc PR C 1 H30B H 0.3294 0.5589 0.2166 0.187 Uiso 0.594(10) 1 calc PR C 1 H30C H 0.2347 0.5485 0.2657 0.187 Uiso 0.594(10) 1 calc PR C 1 C33A C 0.0341(15) 0.3740(19) 0.1570(16) 0.130(8) Uani 0.594(10) 1 d PD C 1 H33A H -0.0185 0.2919 0.1220 0.194 Uiso 0.594(10) 1 calc PR C 1 H33B H -0.0076 0.4167 0.1350 0.194 Uiso 0.594(10) 1 calc PR C 1 H33C H 0.0431 0.3937 0.2161 0.194 Uiso 0.594(10) 1 calc PR C 1 C35A C 0.160(3) 0.3797(19) 0.0632(10) 0.139(10) Uani 0.594(10) 1 d PD C 1 H35A H 0.1178 0.2969 0.0279 0.208 Uiso 0.594(10) 1 calc PR C 1 H35B H 0.2469 0.4097 0.0638 0.208 Uiso 0.594(10) 1 calc PR C 1 H35C H 0.1098 0.4159 0.0397 0.208 Uiso 0.594(10) 1 calc PR C 1 C30B C 0.175(6) 0.505(2) 0.223(2) 0.125(14) Uani 0.406(10) 1 d PD C 2 H30D H 0.1368 0.5474 0.1983 0.187 Uiso 0.406(10) 1 calc PR C 2 H30E H 0.2643 0.5546 0.2626 0.187 Uiso 0.406(10) 1 calc PR C 2 H30F H 0.1255 0.4773 0.2538 0.187 Uiso 0.406(10) 1 calc PR C 2 C33B C 0.039(2) 0.326(2) 0.0796(18) 0.130(8) Uani 0.406(10) 1 d PD C 2 H33D H 0.0481 0.2638 0.0384 0.194 Uiso 0.406(10) 1 calc PR C 2 H33E H 0.0084 0.3688 0.0517 0.194 Uiso 0.406(10) 1 calc PR C 2 H33F H -0.0229 0.2934 0.1015 0.194 Uiso 0.406(10) 1 calc PR C 2 C35B C 0.268(2) 0.460(2) 0.1211(17) 0.139(10) Uani 0.406(10) 1 d PD C 2 H35D H 0.2704 0.4005 0.0742 0.208 Uiso 0.406(10) 1 calc PR C 2 H35E H 0.3536 0.5038 0.1676 0.208 Uiso 0.406(10) 1 calc PR C 2 H35F H 0.2417 0.5118 0.1007 0.208 Uiso 0.406(10) 1 calc PR C 2 C17 C 0.4395(8) -0.1806(7) 0.2290(5) 0.072(2) Uani 1 1 d . . . H17A H 0.3707 -0.2232 0.2418 0.108 Uiso 1 1 calc R . . H17B H 0.5018 -0.1113 0.2806 0.108 Uiso 1 1 calc R . . H17C H 0.4832 -0.2283 0.2090 0.108 Uiso 1 1 calc R . . C18 C 0.3165(5) -0.0694(5) 0.1895(4) 0.0307(14) Uani 1 1 d . . . C19 C 0.6161(6) 0.1988(6) 0.5758(4) 0.0528(19) Uani 1 1 d . . . H19A H 0.5433 0.1242 0.5508 0.079 Uiso 1 1 calc R . . H19B H 0.5976 0.2569 0.6133 0.079 Uiso 1 1 calc R . . H19C H 0.6941 0.1959 0.6090 0.079 Uiso 1 1 calc R . . C20 C 0.1514(6) 0.4011(6) 0.5207(4) 0.0522(19) Uani 1 1 d . . . H20A H 0.0861 0.4247 0.5347 0.078 Uiso 1 1 calc R . . H20B H 0.2169 0.4646 0.5203 0.078 Uiso 1 1 calc R . . H20C H 0.1922 0.3792 0.5634 0.078 Uiso 1 1 calc R . . C21 C 0.7496(6) 0.3441(5) 0.5403(4) 0.0509(19) Uani 1 1 d . . . H21A H 0.8270 0.3439 0.5768 0.076 Uiso 1 1 calc R . . H21B H 0.7300 0.4046 0.5739 0.076 Uiso 1 1 calc R . . H21C H 0.7647 0.3581 0.4931 0.076 Uiso 1 1 calc R . . N1S N 0.6088(6) 0.6740(5) 0.3705(4) 0.0633(18) Uani 1 1 d . . . C22 C 0.6625(6) 0.1353(5) 0.4459(4) 0.055(2) Uani 1 1 d . . . H22A H 0.5899 0.0612 0.4236 0.082 Uiso 1 1 calc R . . H22B H 0.7417 0.1333 0.4781 0.082 Uiso 1 1 calc R . . H22C H 0.6720 0.1517 0.3984 0.082 Uiso 1 1 calc R . . C2S C 0.7365(7) 0.8924(5) 0.4406(4) 0.0542(19) Uani 1 1 d . . . H2S1 H 0.6998 0.9277 0.4789 0.081 Uiso 1 1 calc R . . H2S2 H 0.7308 0.9199 0.3966 0.081 Uiso 1 1 calc R . . H2S3 H 0.8271 0.9128 0.4733 0.081 Uiso 1 1 calc R . . C23 C -0.0212(7) 0.2015(6) 0.4286(6) 0.086(3) Uani 1 1 d . . . H23A H -0.0839 0.2287 0.4436 0.129 Uiso 1 1 calc R . . H23B H 0.0142 0.1744 0.4693 0.129 Uiso 1 1 calc R . . H23C H -0.0638 0.1387 0.3710 0.129 Uiso 1 1 calc R . . C24 C 0.2824(7) -0.2560(6) 0.0810(5) 0.071(2) Uani 1 1 d . . . H24A H 0.2146 -0.2972 0.0953 0.106 Uiso 1 1 calc R . . H24B H 0.3239 -0.3051 0.0597 0.106 Uiso 1 1 calc R . . H24C H 0.2443 -0.2349 0.0369 0.106 Uiso 1 1 calc R . . C25 C 0.4884(8) -0.0839(7) 0.1397(6) 0.087(3) Uani 1 1 d . . . H25A H 0.5318 -0.1321 0.1203 0.131 Uiso 1 1 calc R . . H25B H 0.5508 -0.0141 0.1909 0.131 Uiso 1 1 calc R . . H25C H 0.4511 -0.0640 0.0947 0.131 Uiso 1 1 calc R . . C27 C 0.0341(7) 0.3380(6) 0.3649(5) 0.063(2) Uani 1 1 d . . . H27A H -0.0316 0.3635 0.3762 0.095 Uiso 1 1 calc R . . H27B H -0.0044 0.2744 0.3078 0.095 Uiso 1 1 calc R . . H27C H 0.1046 0.4013 0.3681 0.095 Uiso 1 1 calc R . . H12A H 0.562(4) 0.527(5) 0.464(2) 0.076 Uiso 1 1 d D . . H12B H 0.524(7) 0.533(5) 0.391(4) 0.076 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe2 0.0236(4) 0.0248(5) 0.0200(4) 0.0079(4) 0.0086(4) 0.0080(4) Co1 0.0269(4) 0.0279(4) 0.0190(4) 0.0076(3) 0.0075(3) 0.0092(4) Fe1 0.0242(5) 0.0260(5) 0.0216(4) 0.0093(4) 0.0087(4) 0.0071(4) O1 0.027(2) 0.031(2) 0.024(2) 0.0131(18) 0.0097(17) 0.0117(18) O2 0.029(2) 0.024(2) 0.040(2) 0.0109(19) 0.0174(19) 0.0067(18) O3 0.032(2) 0.029(2) 0.025(2) 0.0064(18) 0.0161(19) 0.0082(19) O4 0.026(2) 0.026(2) 0.031(2) 0.0018(19) 0.0089(19) 0.0046(19) O5 0.037(2) 0.036(2) 0.026(2) 0.0140(19) 0.0132(19) 0.016(2) O6 0.033(2) 0.033(2) 0.030(2) 0.012(2) 0.0082(19) 0.0059(19) O7 0.032(2) 0.033(2) 0.028(2) 0.0126(19) 0.011(2) 0.0081(19) O8 0.045(3) 0.031(2) 0.022(2) 0.0112(19) 0.0070(19) 0.014(2) O9 0.033(2) 0.032(2) 0.023(2) 0.0106(18) 0.0069(19) 0.0144(19) O10 0.026(2) 0.034(2) 0.024(2) 0.0129(18) 0.0089(18) 0.0082(19) O11 0.045(3) 0.035(2) 0.027(2) 0.017(2) 0.013(2) 0.019(2) N2 0.028(3) 0.026(3) 0.016(2) 0.008(2) 0.011(2) 0.009(2) O12 0.032(2) 0.028(2) 0.022(2) 0.0026(19) 0.0082(18) 0.006(2) O13 0.026(2) 0.027(2) 0.028(2) 0.0092(18) 0.0144(18) 0.0113(18) O14 0.029(2) 0.025(2) 0.021(2) 0.0095(17) 0.0102(17) 0.0113(17) N1 0.025(3) 0.027(3) 0.023(3) 0.012(2) 0.008(2) 0.010(2) C1 0.037(4) 0.045(4) 0.038(4) 0.015(3) 0.021(3) 0.009(3) C2 0.028(3) 0.019(3) 0.016(3) 0.006(2) 0.008(2) 0.008(2) C3 0.030(3) 0.037(4) 0.038(4) 0.019(3) 0.018(3) 0.011(3) C4 0.037(4) 0.024(3) 0.032(4) 0.009(3) 0.013(3) 0.009(3) C5 0.029(3) 0.043(4) 0.021(3) 0.010(3) 0.011(3) 0.016(3) C6 0.026(3) 0.030(4) 0.030(4) 0.013(3) 0.007(3) 0.007(3) C7 0.024(3) 0.033(3) 0.019(3) 0.008(3) 0.008(2) 0.009(3) C8 0.030(3) 0.035(4) 0.037(4) 0.018(3) 0.012(3) 0.013(3) C9 0.030(3) 0.033(4) 0.028(3) 0.015(3) 0.014(3) 0.015(3) C10 0.054(4) 0.036(4) 0.039(4) 0.019(3) 0.023(3) 0.026(3) C11 0.036(4) 0.040(4) 0.056(5) 0.025(4) 0.015(3) 0.002(3) C12 0.067(5) 0.042(4) 0.036(4) 0.023(3) 0.011(4) 0.027(4) C13 0.025(3) 0.037(4) 0.025(3) 0.013(3) 0.013(3) 0.014(3) C1S 0.051(5) 0.053(5) 0.053(5) 0.032(4) 0.031(4) 0.022(4) C14 0.029(4) 0.043(4) 0.062(5) 0.017(4) 0.025(3) 0.019(3) C15 0.044(4) 0.031(3) 0.022(3) 0.012(3) 0.014(3) 0.018(3) C16A 0.034(6) 0.065(8) 0.082(8) 0.002(8) 0.029(6) -0.004(7) C29A 0.119(15) 0.122(15) 0.120(14) 0.083(12) 0.087(14) 0.027(12) C32A 0.083(16) 0.048(7) 0.131(17) 0.017(10) 0.086(14) 0.021(8) C16B 0.034(6) 0.065(8) 0.082(8) 0.002(8) 0.029(6) -0.004(7) C29B 0.119(15) 0.122(15) 0.120(14) 0.083(12) 0.087(14) 0.027(12) C32B 0.083(16) 0.048(7) 0.131(17) 0.017(10) 0.086(14) 0.021(8) C26A 0.060(7) 0.072(8) 0.069(7) 0.047(6) 0.020(5) -0.007(5) C28A 0.134(14) 0.032(5) 0.096(13) -0.027(7) 0.065(10) -0.030(7) C31A 0.033(6) 0.111(9) 0.129(12) 0.079(10) 0.013(7) -0.002(6) C26B 0.060(7) 0.072(8) 0.069(7) 0.047(6) 0.020(5) -0.007(5) C28B 0.134(14) 0.032(5) 0.096(13) -0.027(7) 0.065(10) -0.030(7) C31B 0.033(6) 0.111(9) 0.129(12) 0.079(10) 0.013(7) -0.002(6) C30A 0.19(4) 0.055(10) 0.087(12) 0.039(9) -0.012(13) 0.045(16) C33A 0.100(10) 0.166(19) 0.21(2) 0.14(2) 0.064(15) 0.098(12) C35A 0.30(3) 0.18(2) 0.061(10) 0.089(13) 0.094(15) 0.21(2) C30B 0.19(4) 0.055(10) 0.087(12) 0.039(9) -0.012(13) 0.045(16) C33B 0.100(10) 0.166(19) 0.21(2) 0.14(2) 0.064(15) 0.098(12) C35B 0.30(3) 0.18(2) 0.061(10) 0.089(13) 0.094(15) 0.21(2) C17 0.118(7) 0.084(6) 0.052(5) 0.035(5) 0.041(5) 0.078(6) C18 0.036(4) 0.020(3) 0.028(3) 0.006(3) 0.014(3) 0.004(3) C19 0.037(4) 0.080(5) 0.048(4) 0.042(4) 0.007(3) 0.026(4) C20 0.055(5) 0.059(5) 0.056(5) 0.022(4) 0.035(4) 0.032(4) C21 0.034(4) 0.038(4) 0.054(5) 0.021(3) -0.007(3) 0.001(3) N1S 0.069(5) 0.051(4) 0.073(5) 0.033(4) 0.033(4) 0.018(4) C22 0.032(4) 0.052(5) 0.075(6) 0.021(4) 0.020(4) 0.020(4) C2S 0.069(5) 0.041(4) 0.052(5) 0.022(4) 0.026(4) 0.019(4) C23 0.052(5) 0.060(5) 0.149(9) 0.028(6) 0.071(6) 0.018(4) C24 0.091(6) 0.056(5) 0.056(5) 0.010(4) 0.026(5) 0.037(5) C25 0.088(7) 0.081(6) 0.142(9) 0.058(6) 0.081(7) 0.057(6) C27 0.051(5) 0.074(6) 0.058(5) 0.015(4) 0.016(4) 0.038(4) _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 Fe2 O14 1.843(3) . ? Fe2 O3 2.007(4) . ? Fe2 O9 2.018(4) . ? Fe2 O1 2.052(4) . ? Fe2 O13 2.063(3) . ? Fe2 O12 2.127(4) . ? Co1 O14 1.999(3) . ? Co1 O11 2.053(4) . ? Co1 O4 2.060(4) . ? Co1 O8 2.086(4) . ? Co1 N1 2.130(4) . ? Co1 N2 2.188(4) . ? Fe1 O14 1.837(3) . ? Fe1 O10 1.972(4) . ? Fe1 O5 2.008(4) . ? Fe1 O2 2.074(4) . ? Fe1 O6 2.086(4) . ? Fe1 O7 2.177(4) . ? Fe1 C4 2.464(6) . ? O1 C7 1.245(6) . ? O2 C13 1.264(6) . ? O3 C9 1.259(6) . ? O4 C9 1.254(6) . ? O5 C18 1.265(6) . ? O6 C4 1.272(6) . ? O7 C4 1.250(6) . ? O8 C6 1.251(6) . ? O9 C6 1.257(6) . ? O10 C7 1.273(6) . ? O11 C18 1.246(7) . ? N2 C2 1.328(6) . ? N2 C15 1.343(6) . ? O13 C13 1.263(6) . ? N1 C2 1.338(6) 2 ? N1 C3 1.350(7) . ? C1 C16A 1.512(11) . ? C1 C32B 1.512(16) . ? C1 C32A 1.529(12) . ? C1 C9 1.533(8) . ? C1 C29B 1.539(17) . ? C1 C16B 1.542(16) . ? C1 C29A 1.574(14) . ? C2 N1 1.338(6) 2 ? C2 C2 1.488(10) 2 ? C3 C5 1.362(7) . ? C4 C11 1.525(8) . ? C5 C15 1.386(7) 2 ? C6 C12 1.529(8) . ? C7 C8 1.533(8) . ? C8 C21 1.518(8) . ? C8 C19 1.525(8) . ? C8 C22 1.542(8) . ? C10 C25 1.512(9) . ? C10 C17 1.512(9) . ? C10 C24 1.525(9) . ? C10 C18 1.542(8) . ? C11 C28A 1.507(10) . ? C11 C28B 1.51(2) . ? C11 C31A 1.53(2) . ? C11 C26B 1.527(10) . ? C11 C31B 1.537(10) . ? C11 C26A 1.54(2) . ? C12 C30B 1.490(19) . ? C12 C30A 1.508(15) . ? C12 C35A 1.520(13) . ? C12 C33B 1.531(18) . ? C12 C35B 1.542(18) . ? C12 C33A 1.559(14) . ? C13 C14 1.540(7) . ? C1S N1S 1.119(8) . ? C1S C2S 1.456(9) . ? C14 C23 1.515(9) . ? C14 C20 1.542(9) . ? C14 C27 1.544(9) . ? C15 C5 1.386(7) 2 ? 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 O14 Fe2 O3 98.49(15) . . ? O14 Fe2 O9 98.18(15) . . ? O3 Fe2 O9 90.43(15) . . ? O14 Fe2 O1 96.34(15) . . ? O3 Fe2 O1 87.75(15) . . ? O9 Fe2 O1 165.47(15) . . ? O14 Fe2 O13 92.22(15) . . ? O3 Fe2 O13 169.26(15) . . ? O9 Fe2 O13 88.88(15) . . ? O1 Fe2 O13 90.24(14) . . ? O14 Fe2 O12 175.39(16) . . ? O3 Fe2 O12 86.01(15) . . ? O9 Fe2 O12 82.68(16) . . ? O1 Fe2 O12 82.82(15) . . ? O13 Fe2 O12 83.26(15) . . ? O14 Co1 O11 94.64(14) . . ? O14 Co1 O4 96.56(14) . . ? O11 Co1 O4 88.29(15) . . ? O14 Co1 O8 95.60(14) . . ? O11 Co1 O8 169.57(15) . . ? O4 Co1 O8 88.57(15) . . ? O14 Co1 N1 171.54(16) . . ? O11 Co1 N1 85.44(16) . . ? O4 Co1 N1 91.90(16) . . ? O8 Co1 N1 84.73(15) . . ? O14 Co1 N2 95.06(15) . . ? O11 Co1 N2 99.96(16) . . ? O4 Co1 N2 165.16(16) . . ? O8 Co1 N2 81.12(15) . . ? N1 Co1 N2 76.61(16) . . ? O14 Fe1 O10 103.07(15) . . ? O14 Fe1 O5 96.29(15) . . ? O10 Fe1 O5 89.55(15) . . ? O14 Fe1 O2 89.50(15) . . ? O10 Fe1 O2 91.20(15) . . ? O5 Fe1 O2 173.83(15) . . ? O14 Fe1 O6 102.82(16) . . ? O10 Fe1 O6 153.99(16) . . ? O5 Fe1 O6 90.07(16) . . ? O2 Fe1 O6 86.57(15) . . ? O14 Fe1 O7 163.62(15) . . ? O10 Fe1 O7 92.45(15) . . ? O5 Fe1 O7 88.92(15) . . ? O2 Fe1 O7 84.93(15) . . ? O6 Fe1 O7 61.53(15) . . ? O14 Fe1 C4 133.84(18) . . ? O10 Fe1 C4 122.90(18) . . ? O5 Fe1 C4 88.57(17) . . ? O2 Fe1 C4 85.87(17) . . ? O6 Fe1 C4 31.09(16) . . ? O7 Fe1 C4 30.46(16) . . ? C7 O1 Fe2 130.4(4) . . ? C13 O2 Fe1 126.7(3) . . ? C9 O3 Fe2 135.4(4) . . ? C9 O4 Co1 124.5(4) . . ? C18 O5 Fe1 126.6(4) . . ? C4 O6 Fe1 91.1(3) . . ? C4 O7 Fe1 87.5(3) . . ? C6 O8 Co1 132.3(4) . . ? C6 O9 Fe2 126.5(4) . . ? C7 O10 Fe1 126.7(3) . . ? C18 O11 Co1 129.9(4) . . ? C2 N2 C15 115.9(5) . . ? C2 N2 Co1 113.8(3) . . ? C15 N2 Co1 129.7(4) . . ? C13 O13 Fe2 128.0(3) . . ? Fe1 O14 Fe2 121.59(19) . . ? Fe1 O14 Co1 120.98(18) . . ? Fe2 O14 Co1 115.86(17) . . ? C2 N1 C3 115.7(5) 2 . ? C2 N1 Co1 116.0(3) 2 . ? C3 N1 Co1 128.2(4) . . ? C16A C1 C32B 133.6(13) . . ? C16A C1 C32A 111.0(10) . . ? C32B C1 C32A 38.6(12) . . ? C16A C1 C9 112.9(6) . . ? C32B C1 C9 112.0(13) . . ? C32A C1 C9 112.1(8) . . ? C16A C1 C29B 63.9(12) . . ? C32B C1 C29B 112.3(15) . . ? C32A C1 C29B 138.0(12) . . ? C9 C1 C29B 107.4(10) . . ? C16A C1 C16B 46.2(8) . . ? C32B C1 C16B 112.2(14) . . ? C32A C1 C16B 75.0(10) . . ? C9 C1 C16B 102.6(8) . . ? C29B C1 C16B 109.9(14) . . ? C16A C1 C29A 108.0(9) . . ? C32B C1 C29A 70.2(12) . . ? C32A C1 C29A 107.2(10) . . ? C9 C1 C29A 105.3(7) . . ? C29B C1 C29A 47.2(11) . . ? C16B C1 C29A 148.4(10) . . ? N2 C2 N1 127.0(5) . 2 ? N2 C2 C2 117.1(6) . 2 ? N1 C2 C2 115.9(6) 2 2 ? N1 C3 C5 121.9(5) . . ? O7 C4 O6 119.8(5) . . ? O7 C4 C11 122.0(5) . . ? O6 C4 C11 118.2(5) . . ? O7 C4 Fe1 62.0(3) . . ? O6 C4 Fe1 57.9(3) . . ? C11 C4 Fe1 175.5(4) . . ? C3 C5 C15 117.9(5) . 2 ? O8 C6 O9 126.3(5) . . ? O8 C6 C12 116.3(5) . . ? O9 C6 C12 117.5(5) . . ? O1 C7 O10 125.8(5) . . ? O1 C7 C8 118.5(5) . . ? O10 C7 C8 115.7(5) . . ? C21 C8 C19 111.7(5) . . ? C21 C8 C7 111.2(5) . . ? C19 C8 C7 110.8(5) . . ? C21 C8 C22 109.6(5) . . ? C19 C8 C22 108.3(5) . . ? C7 C8 C22 104.9(5) . . ? O4 C9 O3 126.3(5) . . ? O4 C9 C1 117.1(5) . . ? O3 C9 C1 116.6(5) . . ? C25 C10 C17 109.5(6) . . ? C25 C10 C24 110.3(6) . . ? C17 C10 C24 109.5(6) . . ? C25 C10 C18 107.3(5) . . ? C17 C10 C18 111.8(5) . . ? C24 C10 C18 108.5(5) . . ? C28A C11 C28B 29(4) . . ? C28A C11 C4 107.8(7) . . ? C28B C11 C4 99(4) . . ? C28A C11 C31A 140(3) . . ? C28B C11 C31A 156(5) . . ? C4 C11 C31A 104(2) . . ? C28A C11 C26B 116.5(11) . . ? C28B C11 C26B 96(5) . . ? C4 C11 C26B 109.6(6) . . ? C31A C11 C26B 73(3) . . ? C28A C11 C31B 105.2(11) . . ? C28B C11 C31B 133(4) . . ? C4 C11 C31B 110.6(6) . . ? C31A C11 C31B 39(3) . . ? C26B C11 C31B 107.0(7) . . ? C28A C11 C26A 80(3) . . ? C28B C11 C26A 57(5) . . ? C4 C11 C26A 110(2) . . ? C31A C11 C26A 111(3) . . ? C26B C11 C26A 39(3) . . ? C31B C11 C26A 135(2) . . ? C30B C12 C30A 34(2) . . ? C30B C12 C35A 133.1(18) . . ? C30A C12 C35A 110.2(13) . . ? C30B C12 C6 111(2) . . ? C30A C12 C6 113.0(14) . . ? C35A C12 C6 112.7(7) . . ? C30B C12 C33B 117(3) . . ? C30A C12 C33B 135.0(18) . . ? C35A C12 C33B 61.3(13) . . ? C6 C12 C33B 110.3(11) . . ? C30B C12 C35B 103.9(18) . . ? C30A C12 C35B 70.5(13) . . ? C35A C12 C35B 49.6(11) . . ? C6 C12 C35B 103.6(10) . . ? C33B C12 C35B 110.3(15) . . ? C30B C12 C33A 72(2) . . ? C30A C12 C33A 103.4(15) . . ? C35A C12 C33A 110.9(12) . . ? C6 C12 C33A 106.1(8) . . ? C33B C12 C33A 52.3(12) . . ? C35B C12 C33A 149.6(11) . . ? O13 C13 O2 125.8(5) . . ? O13 C13 C14 117.4(5) . . ? O2 C13 C14 116.8(5) . . ? N1S C1S C2S 178.7(8) . . ? C23 C14 C13 111.0(5) . . ? C23 C14 C20 110.7(6) . . ? C13 C14 C20 110.2(5) . . ? C23 C14 C27 110.2(6) . . ? C13 C14 C27 106.1(5) . . ? C20 C14 C27 108.4(5) . . ? N2 C15 C5 121.6(5) . 2 ? O11 C18 O5 125.6(5) . . ? O11 C18 C10 117.3(5) . . ? O5 C18 C10 117.1(5) . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 26.73 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.696 _refine_diff_density_min -0.420 _refine_diff_density_rms 0.101 #END data_pa_419_0m _database_code_depnum_ccdc_archive 'CCDC 750194' #TrackingRef 'albores_et_al.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H124 Fe4 N6 Ni2 O28' _chemical_formula_weight 1862.59 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7753(4) _cell_length_b 13.5794(4) _cell_length_c 17.9814(6) _cell_angle_alpha 108.7492(12) _cell_angle_beta 105.7623(12) _cell_angle_gamma 106.8220(12) _cell_volume 2385.93(20) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.59 _exptl_crystal_size_mid 0.47 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.296 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 982 _exptl_absorpt_coefficient_mu 1.049 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.5217 _exptl_absorpt_correction_T_max 0.6961 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71069 _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 35739 _diffrn_reflns_av_R_equivalents 0.0271 _diffrn_reflns_av_sigmaI/netI 0.0310 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 27.59 _reflns_number_total 10801 _reflns_number_gt 8606 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0402P)^2^+3.2510P] 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 10801 _refine_ls_number_parameters 533 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0531 _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_ref 0.1036 _refine_ls_wR_factor_gt 0.0933 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe2 Fe 0.11587(3) 0.18130(3) 0.16482(2) 0.01990(9) Uani 1 1 d . . . Ni1 Ni 0.26379(3) 0.39336(3) 0.354250(18) 0.02160(8) Uani 1 1 d . . . Fe1 Fe 0.24865(3) 0.43193(3) 0.17848(2) 0.02105(9) Uani 1 1 d . . . O1 O -0.02295(16) 0.19776(15) 0.07810(11) 0.0240(4) Uani 1 1 d . . . O2 O 0.34157(17) 0.34446(15) 0.11862(11) 0.0261(4) Uani 1 1 d . . . O3 O -0.00065(17) 0.16617(15) 0.22783(10) 0.0254(4) Uani 1 1 d . . . O4 O 0.33742(18) 0.56308(16) 0.14202(11) 0.0287(4) Uani 1 1 d . . . O5 O 0.24900(18) 0.54391(15) 0.36659(11) 0.0279(4) Uani 1 1 d . . . O6 O 0.21211(16) 0.16466(15) 0.08390(10) 0.0246(4) Uani 1 1 d . . . O7 O 0.07978(17) 0.33154(15) 0.34544(11) 0.0269(4) Uani 1 1 d . . . O8 O 0.16785(18) 0.52883(16) 0.23331(11) 0.0284(4) Uani 1 1 d . . . O9 O 0.28244(18) 0.25264(15) 0.36535(11) 0.0293(4) Uani 1 1 d . . . O10 O 0.43272(17) 0.55999(15) 0.26301(11) 0.0284(4) Uani 1 1 d . . . O11 O 0.09244(16) 0.35506(15) 0.07062(10) 0.0246(4) Uani 1 1 d . . . N1 N 0.4683(2) 0.45080(18) 0.38807(12) 0.0232(4) Uani 1 1 d . . . O12 O 0.00177(19) 0.00383(16) 0.08446(13) 0.0266(4) Uani 1 1 d . . . O13 O 0.22383(18) 0.12299(16) 0.23205(11) 0.0286(4) Uani 1 1 d . . . C1 C 0.6675(3) 0.4719(2) 0.37362(16) 0.0285(6) Uani 1 1 d . . . H1 H 0.7139 0.4619 0.3381 0.034 Uiso 1 1 calc R . . O14 O 0.22035(16) 0.33458(14) 0.22927(10) 0.0219(3) Uani 1 1 d . . . C2 C 0.3361(3) 0.0938(3) 0.35001(19) 0.0429(7) Uani 1 1 d D . . N2 N 0.3355(2) 0.46713(17) 0.48818(12) 0.0230(4) Uani 1 1 d . . . C3 C 0.4145(3) 0.1985(2) 0.06959(19) 0.0348(6) Uani 1 1 d . . . C4 C 0.4338(3) 0.6074(2) 0.21262(16) 0.0271(5) Uani 1 1 d . . . C5 C -0.0129(2) 0.2729(2) 0.05072(14) 0.0228(5) Uani 1 1 d . . . C6 C 0.5349(3) 0.4382(2) 0.33862(16) 0.0262(5) Uani 1 1 d . . . H6 H 0.4899 0.4052 0.2781 0.031 Uiso 1 1 calc R . . C7 C 0.1201(3) 0.6468(2) 0.34159(17) 0.0333(6) Uani 1 1 d . . . C8 C -0.1369(3) 0.2714(2) -0.00668(17) 0.0281(5) Uani 1 1 d . . . C9 C 0.5369(2) 0.49574(19) 0.47242(14) 0.0198(5) Uani 1 1 d . . . C10 C 0.2752(3) 0.1618(2) 0.31321(16) 0.0279(5) Uani 1 1 d . B . N3 N 0.1092(3) 0.1728(3) 0.8673(2) 0.0546(7) Uani 1 1 d . . . C11 C -0.2498(3) 0.1562(3) -0.0431(2) 0.0424(7) Uani 1 1 d . . . H11A H -0.3281 0.1570 -0.0796 0.064 Uiso 1 1 calc R . . H11B H -0.2643 0.1410 0.0040 0.064 Uiso 1 1 calc R . . H11C H -0.2300 0.0963 -0.0773 0.064 Uiso 1 1 calc R . . C12 C 0.5492(3) 0.7174(3) 0.23988(19) 0.0376(7) Uani 1 1 d . . . C13 C -0.0046(2) 0.2329(2) 0.29404(15) 0.0233(5) Uani 1 1 d . A . C14 C -0.1215(3) 0.1860(3) 0.3147(2) 0.0423(7) Uani 1 1 d D . . C15 C -0.1613(3) 0.3659(3) 0.0519(2) 0.0431(7) Uani 1 1 d . . . H15A H -0.0875 0.4394 0.0748 0.065 Uiso 1 1 calc R . . H15B H -0.1716 0.3494 0.0995 0.065 Uiso 1 1 calc R . . H15C H -0.2402 0.3694 0.0191 0.065 Uiso 1 1 calc R . . C16 C 0.2697(3) 0.4796(2) 0.53815(16) 0.0288(6) Uani 1 1 d . . . H16 H 0.1784 0.4546 0.5125 0.035 Uiso 1 1 calc R . . C17 C 0.1670(3) 0.2689(3) 0.8992(2) 0.0399(7) Uani 1 1 d . . . C18 C 0.2392(3) 0.3917(3) 0.9409(2) 0.0443(7) Uani 1 1 d . . . H18A H 0.2130 0.4251 0.9868 0.066 Uiso 1 1 calc R . . H18B H 0.2213 0.4225 0.8988 0.066 Uiso 1 1 calc R . . H18C H 0.3321 0.4105 0.9654 0.066 Uiso 1 1 calc R . . C19 C 0.3142(2) 0.2393(2) 0.09154(15) 0.0247(5) Uani 1 1 d . . . C20 C 0.3489(3) 0.0976(3) -0.0197(2) 0.0438(8) Uani 1 1 d . . . H20A H 0.2780 0.0363 -0.0213 0.066 Uiso 1 1 calc R . . H20B H 0.4125 0.0694 -0.0322 0.066 Uiso 1 1 calc R . . H20C H 0.3143 0.1227 -0.0628 0.066 Uiso 1 1 calc R . . C21 C 0.1851(3) 0.5667(2) 0.31191(16) 0.0268(5) Uani 1 1 d . . . C22 C -0.1156(3) 0.3009(3) -0.0785(2) 0.0443(8) Uani 1 1 d . . . H22A H -0.0425 0.3755 -0.0535 0.066 Uiso 1 1 calc R . . H22B H -0.1939 0.3037 -0.1129 0.066 Uiso 1 1 calc R . . H22C H -0.0967 0.2424 -0.1152 0.066 Uiso 1 1 calc R . . C24 C 0.2225(4) 0.7546(3) 0.4212(2) 0.0587(10) Uani 1 1 d . . . H24A H 0.2614 0.7334 0.4657 0.088 Uiso 1 1 calc R . . H24B H 0.1817 0.8046 0.4425 0.088 Uiso 1 1 calc R . . H24C H 0.2899 0.7948 0.4062 0.088 Uiso 1 1 calc R . . C25 C 0.5250(4) 0.2949(3) 0.0732(3) 0.0626(11) Uani 1 1 d . . . H25A H 0.5875 0.2666 0.0588 0.094 Uiso 1 1 calc R . . H25B H 0.5683 0.3577 0.1311 0.094 Uiso 1 1 calc R . . H25C H 0.4903 0.3225 0.0319 0.094 Uiso 1 1 calc R . . C26 C 0.0593(4) 0.6783(3) 0.2720(2) 0.0599(11) Uani 1 1 d . . . H26A H 0.1265 0.7185 0.2569 0.090 Uiso 1 1 calc R . . H26B H 0.0180 0.7281 0.2929 0.090 Uiso 1 1 calc R . . H26C H -0.0059 0.6088 0.2213 0.090 Uiso 1 1 calc R . . C27 C 0.4669(3) 0.1578(3) 0.1369(2) 0.0512(9) Uani 1 1 d . . . H27A H 0.3953 0.0960 0.1342 0.077 Uiso 1 1 calc R . . H27B H 0.5078 0.2216 0.1943 0.077 Uiso 1 1 calc R . . H27C H 0.5310 0.1299 0.1251 0.077 Uiso 1 1 calc R . . C29 C 0.5468(4) 0.7436(4) 0.1637(3) 0.0692(12) Uani 1 1 d . . . H29A H 0.6219 0.8144 0.1822 0.104 Uiso 1 1 calc R . . H29B H 0.4670 0.7526 0.1403 0.104 Uiso 1 1 calc R . . H29C H 0.5498 0.6806 0.1195 0.104 Uiso 1 1 calc R . . C31 C 0.0160(5) 0.5836(4) 0.3654(3) 0.0727(13) Uani 1 1 d . . . H31A H 0.0560 0.5636 0.4105 0.109 Uiso 1 1 calc R . . H31B H -0.0490 0.5138 0.3147 0.109 Uiso 1 1 calc R . . H31C H -0.0258 0.6328 0.3863 0.109 Uiso 1 1 calc R . . C32 C 0.6733(4) 0.7026(5) 0.2749(4) 0.0952(19) Uani 1 1 d . . . H32A H 0.7485 0.7730 0.2927 0.143 Uiso 1 1 calc R . . H32B H 0.6750 0.6393 0.2302 0.143 Uiso 1 1 calc R . . H32C H 0.6762 0.6861 0.3244 0.143 Uiso 1 1 calc R . . C33 C 0.5408(6) 0.8099(3) 0.3091(4) 0.107(2) Uani 1 1 d . . . H33A H 0.6139 0.8827 0.3288 0.161 Uiso 1 1 calc R . . H33B H 0.5436 0.7905 0.3573 0.161 Uiso 1 1 calc R . . H33C H 0.4593 0.8167 0.2861 0.161 Uiso 1 1 calc R . . C23A C -0.0715(7) 0.1485(6) 0.3863(4) 0.0835(19) Uani 0.753(4) 1 d PD A 1 H23A H 0.0010 0.2143 0.4362 0.125 Uiso 0.753(4) 1 calc PR A 1 H23B H -0.0425 0.0886 0.3644 0.125 Uiso 0.753(4) 1 calc PR A 1 H23C H -0.1418 0.1190 0.4032 0.125 Uiso 0.753(4) 1 calc PR A 1 C28A C -0.2319(4) 0.0822(4) 0.2405(3) 0.0610(15) Uani 0.753(4) 1 d PD A 1 H28A H -0.2004 0.0246 0.2179 0.091 Uiso 0.753(4) 1 calc PR A 1 H28B H -0.2691 0.1032 0.1953 0.091 Uiso 0.753(4) 1 calc PR A 1 H28C H -0.2985 0.0510 0.2596 0.091 Uiso 0.753(4) 1 calc PR A 1 C30A C -0.1653(6) 0.2785(5) 0.3527(5) 0.071(2) Uani 0.753(4) 1 d PD A 1 H30A H -0.0908 0.3447 0.4010 0.106 Uiso 0.753(4) 1 calc PR A 1 H30B H -0.2313 0.2487 0.3726 0.106 Uiso 0.753(4) 1 calc PR A 1 H30C H -0.2018 0.3016 0.3087 0.106 Uiso 0.753(4) 1 calc PR A 1 C23B C -0.136(2) 0.0666(14) 0.3093(13) 0.0835(19) Uani 0.247(4) 1 d PD A 2 H23D H -0.1432 0.0183 0.2528 0.125 Uiso 0.247(4) 1 calc PR A 2 H23E H -0.2136 0.0315 0.3177 0.125 Uiso 0.247(4) 1 calc PR A 2 H23F H -0.0594 0.0746 0.3539 0.125 Uiso 0.247(4) 1 calc PR A 2 C28B C -0.2323(12) 0.1743(14) 0.2399(9) 0.0610(15) Uani 0.247(4) 1 d PD A 2 H28D H -0.2409 0.1178 0.1861 0.091 Uiso 0.247(4) 1 calc PR A 2 H28E H -0.2141 0.2483 0.2378 0.091 Uiso 0.247(4) 1 calc PR A 2 H28F H -0.3133 0.1494 0.2478 0.091 Uiso 0.247(4) 1 calc PR A 2 C30B C -0.1060(19) 0.2706(14) 0.3976(12) 0.071(2) Uani 0.247(4) 1 d PD A 2 H30D H -0.0965 0.3431 0.3945 0.106 Uiso 0.247(4) 1 calc PR A 2 H30E H -0.0287 0.2826 0.4438 0.106 Uiso 0.247(4) 1 calc PR A 2 H30F H -0.1826 0.2419 0.4093 0.106 Uiso 0.247(4) 1 calc PR A 2 C34A C 0.2705(9) -0.0305(4) 0.2911(4) 0.108(3) Uani 0.800(6) 1 d PD B 1 H34A H 0.2674 -0.0417 0.2338 0.162 Uiso 0.800(6) 1 calc PR B 1 H34B H 0.1821 -0.0614 0.2877 0.162 Uiso 0.800(6) 1 calc PR B 1 H34C H 0.3188 -0.0702 0.3130 0.162 Uiso 0.800(6) 1 calc PR B 1 C35A C 0.4742(7) 0.1288(8) 0.3485(7) 0.123(3) Uani 0.800(6) 1 d PD B 1 H35A H 0.4659 0.1109 0.2894 0.185 Uiso 0.800(6) 1 calc PR B 1 H35B H 0.5177 0.0864 0.3706 0.185 Uiso 0.800(6) 1 calc PR B 1 H35C H 0.5252 0.2109 0.3844 0.185 Uiso 0.800(6) 1 calc PR B 1 C36A C 0.3564(11) 0.1260(7) 0.4408(4) 0.130(4) Uani 0.800(6) 1 d PD B 1 H36A H 0.3952 0.2094 0.4724 0.195 Uiso 0.800(6) 1 calc PR B 1 H36B H 0.4146 0.0955 0.4659 0.195 Uiso 0.800(6) 1 calc PR B 1 H36C H 0.2730 0.0944 0.4443 0.195 Uiso 0.800(6) 1 calc PR B 1 C34B C 0.235(2) 0.0426(18) 0.3824(16) 0.108(3) Uani 0.200(6) 1 d PD B 2 H34D H 0.1558 -0.0171 0.3333 0.162 Uiso 0.200(6) 1 calc PR B 2 H34E H 0.2143 0.1030 0.4153 0.162 Uiso 0.200(6) 1 calc PR B 2 H34F H 0.2703 0.0096 0.4192 0.162 Uiso 0.200(6) 1 calc PR B 2 C35B C 0.366(4) 0.014(3) 0.2850(17) 0.123(3) Uani 0.200(6) 1 d PD B 2 H35D H 0.2898 -0.0300 0.2306 0.185 Uiso 0.200(6) 1 calc PR B 2 H35E H 0.3904 -0.0378 0.3065 0.185 Uiso 0.200(6) 1 calc PR B 2 H35F H 0.4385 0.0592 0.2759 0.185 Uiso 0.200(6) 1 calc PR B 2 C36B C 0.457(2) 0.170(2) 0.4251(13) 0.130(4) Uani 0.200(6) 1 d PD B 2 H36D H 0.4943 0.1244 0.4477 0.195 Uiso 0.200(6) 1 calc PR B 2 H36E H 0.4392 0.2201 0.4693 0.195 Uiso 0.200(6) 1 calc PR B 2 H36F H 0.5177 0.2160 0.4091 0.195 Uiso 0.200(6) 1 calc PR B 2 H12A H -0.018(4) -0.037(3) 0.104(2) 0.046(11) Uiso 1 1 d . . . H12B H -0.064(4) -0.022(3) 0.039(3) 0.049(10) Uiso 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 Fe2 0.02108(18) 0.02180(18) 0.01535(16) 0.00722(13) 0.00781(13) 0.00744(14) Ni1 0.02238(16) 0.02394(16) 0.01467(14) 0.00674(12) 0.00670(12) 0.00717(13) Fe1 0.02186(18) 0.02272(18) 0.01677(16) 0.00850(14) 0.00796(14) 0.00675(14) O1 0.0224(9) 0.0263(9) 0.0231(8) 0.0120(7) 0.0079(7) 0.0096(7) O2 0.0260(9) 0.0270(9) 0.0268(9) 0.0112(8) 0.0145(8) 0.0099(8) O3 0.0263(9) 0.0262(9) 0.0199(8) 0.0069(7) 0.0118(7) 0.0070(7) O4 0.0293(10) 0.0303(10) 0.0239(9) 0.0130(8) 0.0096(8) 0.0086(8) O5 0.0345(10) 0.0258(9) 0.0224(9) 0.0098(7) 0.0106(8) 0.0126(8) O6 0.0244(9) 0.0274(9) 0.0217(8) 0.0097(7) 0.0116(7) 0.0090(7) O7 0.0255(9) 0.0284(10) 0.0233(9) 0.0080(8) 0.0114(7) 0.0087(8) O8 0.0332(10) 0.0308(10) 0.0236(9) 0.0110(8) 0.0140(8) 0.0149(8) O9 0.0352(10) 0.0273(10) 0.0211(8) 0.0098(8) 0.0084(8) 0.0107(8) O10 0.0273(10) 0.0273(9) 0.0246(9) 0.0124(8) 0.0072(8) 0.0053(8) O11 0.0229(9) 0.0291(9) 0.0184(8) 0.0104(7) 0.0069(7) 0.0074(8) N1 0.0268(11) 0.0244(11) 0.0164(9) 0.0077(8) 0.0080(8) 0.0101(9) O12 0.0269(10) 0.0264(10) 0.0209(9) 0.0087(8) 0.0086(8) 0.0064(8) O13 0.0347(10) 0.0293(10) 0.0191(8) 0.0097(7) 0.0073(8) 0.0140(8) C1 0.0300(14) 0.0359(15) 0.0215(12) 0.0115(11) 0.0134(11) 0.0140(12) O14 0.0229(9) 0.0241(9) 0.0154(7) 0.0074(7) 0.0078(7) 0.0067(7) C2 0.061(2) 0.0372(17) 0.0297(14) 0.0176(13) 0.0070(14) 0.0256(16) N2 0.0232(11) 0.0246(11) 0.0194(10) 0.0087(8) 0.0083(8) 0.0087(9) C3 0.0302(15) 0.0357(15) 0.0435(16) 0.0150(13) 0.0214(13) 0.0163(13) C4 0.0272(13) 0.0288(13) 0.0260(12) 0.0125(11) 0.0128(11) 0.0098(11) C5 0.0219(12) 0.0279(13) 0.0162(11) 0.0059(10) 0.0082(9) 0.0111(10) C6 0.0329(14) 0.0282(13) 0.0185(11) 0.0103(10) 0.0104(10) 0.0136(11) C7 0.0463(17) 0.0329(15) 0.0277(13) 0.0127(12) 0.0195(13) 0.0220(13) C8 0.0235(13) 0.0286(14) 0.0286(13) 0.0132(11) 0.0058(11) 0.0094(11) C9 0.0247(12) 0.0155(11) 0.0190(11) 0.0083(9) 0.0082(10) 0.0076(9) C10 0.0284(13) 0.0272(13) 0.0250(12) 0.0134(11) 0.0078(11) 0.0081(11) N3 0.0595(19) 0.0459(18) 0.0634(19) 0.0290(16) 0.0262(16) 0.0210(15) C11 0.0282(15) 0.0361(16) 0.0485(18) 0.0200(14) 0.0005(13) 0.0068(13) C12 0.0295(15) 0.0336(15) 0.0394(16) 0.0180(13) 0.0094(12) 0.0013(12) C13 0.0229(12) 0.0284(13) 0.0181(11) 0.0103(10) 0.0076(10) 0.0102(11) C14 0.0327(16) 0.0437(18) 0.0372(16) 0.0053(14) 0.0204(13) 0.0062(14) C15 0.0293(15) 0.0416(17) 0.059(2) 0.0177(15) 0.0177(15) 0.0200(14) C16 0.0246(13) 0.0344(14) 0.0244(12) 0.0107(11) 0.0101(11) 0.0106(11) C17 0.0472(18) 0.0460(19) 0.0432(17) 0.0285(15) 0.0246(15) 0.0246(16) C18 0.057(2) 0.0393(17) 0.0380(16) 0.0168(14) 0.0214(15) 0.0189(16) C19 0.0247(13) 0.0298(14) 0.0193(11) 0.0098(10) 0.0100(10) 0.0110(11) C20 0.0503(19) 0.0498(19) 0.0420(17) 0.0152(15) 0.0284(15) 0.0308(16) C21 0.0326(14) 0.0218(12) 0.0245(12) 0.0087(10) 0.0139(11) 0.0084(11) C22 0.0341(16) 0.068(2) 0.0379(16) 0.0351(17) 0.0101(13) 0.0216(16) C24 0.080(3) 0.0399(19) 0.0430(19) 0.0040(15) 0.0163(19) 0.0314(19) C25 0.044(2) 0.055(2) 0.102(3) 0.030(2) 0.052(2) 0.0208(18) C26 0.094(3) 0.067(2) 0.0422(18) 0.0240(18) 0.030(2) 0.062(2) C27 0.0453(19) 0.054(2) 0.054(2) 0.0177(17) 0.0130(16) 0.0321(17) C29 0.054(2) 0.070(3) 0.073(3) 0.049(2) 0.018(2) -0.001(2) C31 0.086(3) 0.071(3) 0.115(4) 0.054(3) 0.077(3) 0.052(3) C32 0.032(2) 0.110(4) 0.144(5) 0.091(4) 0.016(3) 0.006(2) C33 0.133(5) 0.032(2) 0.108(4) -0.007(2) 0.075(4) -0.013(3) C23A 0.091(5) 0.103(5) 0.076(4) 0.061(4) 0.051(4) 0.026(4) C28A 0.035(2) 0.052(3) 0.067(3) 0.003(2) 0.029(2) -0.005(2) C30A 0.064(4) 0.049(3) 0.114(6) 0.021(3) 0.072(4) 0.024(3) C23B 0.091(5) 0.103(5) 0.076(4) 0.061(4) 0.051(4) 0.026(4) C28B 0.035(2) 0.052(3) 0.067(3) 0.003(2) 0.029(2) -0.005(2) C30B 0.064(4) 0.049(3) 0.114(6) 0.021(3) 0.072(4) 0.024(3) C34A 0.151(7) 0.036(3) 0.078(4) 0.022(3) -0.030(4) 0.034(3) C35A 0.089(5) 0.163(8) 0.197(10) 0.139(8) 0.056(6) 0.090(5) C36A 0.278(12) 0.160(7) 0.051(3) 0.076(4) 0.077(5) 0.178(9) C34B 0.151(7) 0.036(3) 0.078(4) 0.022(3) -0.030(4) 0.034(3) C35B 0.089(5) 0.163(8) 0.197(10) 0.139(8) 0.056(6) 0.090(5) C36B 0.278(12) 0.160(7) 0.051(3) 0.076(4) 0.077(5) 0.178(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 Fe2 O14 1.8389(17) . ? Fe2 O3 2.0098(17) . ? Fe2 O13 2.0168(18) . ? Fe2 O1 2.0504(17) . ? Fe2 O6 2.0701(16) . ? Fe2 O12 2.1292(19) . ? Ni1 O14 1.9838(15) . ? Ni1 O7 2.0249(18) . ? Ni1 O5 2.0480(18) . ? Ni1 O9 2.0504(19) . ? Ni1 N2 2.091(2) . ? Ni1 N1 2.142(2) . ? Fe1 O14 1.8382(17) . ? Fe1 O11 1.9707(17) . ? Fe1 O8 2.0024(18) . ? Fe1 O2 2.0824(17) . ? Fe1 O10 2.0884(18) . ? Fe1 O4 2.1770(18) . ? Fe1 C4 2.477(3) . ? O1 C5 1.258(3) . ? O2 C19 1.258(3) . ? O3 C13 1.266(3) . ? O4 C4 1.262(3) . ? O5 C21 1.247(3) . ? O6 C19 1.268(3) . ? O7 C13 1.253(3) . ? O8 C21 1.273(3) . ? O9 C10 1.249(3) . ? O10 C4 1.270(3) . ? O11 C5 1.270(3) . ? N1 C9 1.334(3) . ? N1 C6 1.339(3) . ? O13 C10 1.271(3) . ? C1 C16 1.381(3) 2_666 ? C1 C6 1.382(4) . ? C2 C36B 1.455(18) . ? C2 C36A 1.477(6) . ? C2 C34A 1.490(6) . ? C2 C35B 1.515(19) . ? C2 C10 1.524(4) . ? C2 C34B 1.551(18) . ? C2 C35A 1.566(8) . ? N2 C9 1.329(3) 2_666 ? N2 C16 1.340(3) . ? C3 C25 1.525(4) . ? C3 C19 1.533(4) . ? C3 C20 1.533(4) . ? C3 C27 1.540(5) . ? C4 C12 1.520(4) . ? C5 C8 1.533(3) . ? C7 C26 1.515(4) . ? C7 C31 1.529(5) . ? C7 C24 1.529(4) . ? C7 C21 1.545(4) . ? C8 C11 1.520(4) . ? C8 C22 1.531(4) . ? C8 C15 1.532(4) . ? C9 N2 1.329(3) 2_666 ? C9 C9 1.485(4) 2_666 ? N3 C17 1.134(4) . ? C12 C33 1.507(5) . ? C12 C29 1.516(5) . ? C12 C32 1.524(5) . ? C13 C14 1.536(4) . ? C14 C30B 1.486(14) . ? C14 C28A 1.498(5) . ? C14 C30A 1.525(5) . ? C14 C28B 1.525(14) . ? C14 C23B 1.548(15) . ? C14 C23A 1.565(7) . ? C16 C1 1.381(3) 2_666 ? C17 C18 1.447(5) . ? 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 O14 Fe2 O3 98.27(7) . . ? O14 Fe2 O13 97.51(7) . . ? O3 Fe2 O13 90.33(7) . . ? O14 Fe2 O1 96.89(7) . . ? O3 Fe2 O1 87.79(7) . . ? O13 Fe2 O1 165.60(7) . . ? O14 Fe2 O6 92.67(7) . . ? O3 Fe2 O6 169.01(7) . . ? O13 Fe2 O6 89.29(7) . . ? O1 Fe2 O6 89.85(7) . . ? O14 Fe2 O12 176.03(7) . . ? O3 Fe2 O12 85.69(7) . . ? O13 Fe2 O12 82.76(8) . . ? O1 Fe2 O12 82.86(8) . . ? O6 Fe2 O12 83.37(7) . . ? O14 Ni1 O7 96.90(7) . . ? O14 Ni1 O5 94.53(7) . . ? O7 Ni1 O5 87.89(7) . . ? O14 Ni1 O9 96.14(7) . . ? O7 Ni1 O9 89.51(8) . . ? O5 Ni1 O9 169.24(7) . . ? O14 Ni1 N2 172.15(8) . . ? O7 Ni1 N2 90.88(7) . . ? O5 Ni1 N2 84.71(8) . . ? O9 Ni1 N2 84.90(8) . . ? O14 Ni1 N1 93.71(7) . . ? O7 Ni1 N1 167.16(7) . . ? O5 Ni1 N1 98.48(8) . . ? O9 Ni1 N1 82.17(8) . . ? N2 Ni1 N1 78.70(8) . . ? O14 Fe1 O11 103.08(7) . . ? O14 Fe1 O8 96.26(7) . . ? O11 Fe1 O8 89.71(7) . . ? O14 Fe1 O2 89.26(7) . . ? O11 Fe1 O2 90.70(7) . . ? O8 Fe1 O2 174.22(7) . . ? O14 Fe1 O10 103.57(7) . . ? O11 Fe1 O10 153.21(7) . . ? O8 Fe1 O10 90.05(8) . . ? O2 Fe1 O10 86.99(7) . . ? O14 Fe1 O4 164.14(7) . . ? O11 Fe1 O4 91.78(7) . . ? O8 Fe1 O4 89.23(7) . . ? O2 Fe1 O4 84.99(7) . . ? O10 Fe1 O4 61.44(7) . . ? O14 Fe1 C4 134.24(8) . . ? O11 Fe1 C4 122.39(8) . . ? O8 Fe1 C4 89.39(8) . . ? O2 Fe1 C4 85.52(8) . . ? O10 Fe1 C4 30.83(8) . . ? O4 Fe1 C4 30.61(7) . . ? C5 O1 Fe2 129.95(16) . . ? C19 O2 Fe1 127.10(16) . . ? C13 O3 Fe2 134.74(16) . . ? C4 O4 Fe1 87.94(15) . . ? C21 O5 Ni1 129.58(16) . . ? C19 O6 Fe2 127.48(15) . . ? C13 O7 Ni1 124.54(16) . . ? C21 O8 Fe1 125.79(17) . . ? C10 O9 Ni1 132.99(17) . . ? C4 O10 Fe1 91.73(15) . . ? C5 O11 Fe1 127.52(15) . . ? C9 N1 C6 116.2(2) . . ? C9 N1 Ni1 112.87(15) . . ? C6 N1 Ni1 130.55(17) . . ? C10 O13 Fe2 126.49(17) . . ? C16 C1 C6 117.9(2) 2_666 . ? Fe1 O14 Fe2 121.19(8) . . ? Fe1 O14 Ni1 121.34(9) . . ? Fe2 O14 Ni1 115.84(8) . . ? C36B C2 C36A 52.9(11) . . ? C36B C2 C34A 136.3(10) . . ? C36A C2 C34A 116.7(5) . . ? C36B C2 C35B 107.8(17) . . ? C36A C2 C35B 136.2(11) . . ? C34A C2 C35B 45.8(14) . . ? C36B C2 C10 110.8(10) . . ? C36A C2 C10 112.2(3) . . ? C34A C2 C10 111.6(3) . . ? C35B C2 C10 111.5(10) . . ? C36B C2 C34B 107.0(14) . . ? C36A C2 C34B 54.3(9) . . ? C34A C2 C34B 75.0(10) . . ? C35B C2 C34B 119.3(17) . . ? C10 C2 C34B 100.2(8) . . ? C36B C2 C35A 55.4(12) . . ? C36A C2 C35A 106.4(6) . . ? C34A C2 C35A 102.9(6) . . ? C35B C2 C35A 58.4(15) . . ? C10 C2 C35A 105.8(3) . . ? C34B C2 C35A 152.6(9) . . ? C9 N2 C16 116.9(2) 2_666 . ? C9 N2 Ni1 114.63(15) 2_666 . ? C16 N2 Ni1 128.47(17) . . ? C25 C3 C19 111.1(2) . . ? C25 C3 C20 110.2(3) . . ? C19 C3 C20 109.8(2) . . ? C25 C3 C27 110.0(3) . . ? C19 C3 C27 106.4(2) . . ? C20 C3 C27 109.1(3) . . ? O4 C4 O10 118.9(2) . . ? O4 C4 C12 121.9(2) . . ? O10 C4 C12 119.2(2) . . ? O4 C4 Fe1 61.45(13) . . ? O10 C4 Fe1 57.44(13) . . ? C12 C4 Fe1 176.17(19) . . ? O1 C5 O11 125.0(2) . . ? O1 C5 C8 118.5(2) . . ? O11 C5 C8 116.3(2) . . ? N1 C6 C1 121.5(2) . . ? C26 C7 C31 109.9(3) . . ? C26 C7 C24 110.0(3) . . ? C31 C7 C24 109.3(3) . . ? C26 C7 C21 111.9(2) . . ? C31 C7 C21 107.1(2) . . ? C24 C7 C21 108.5(3) . . ? C11 C8 C22 111.0(2) . . ? C11 C8 C15 110.7(2) . . ? C22 C8 C15 108.8(3) . . ? C11 C8 C5 110.7(2) . . ? C22 C8 C5 110.2(2) . . ? C15 C8 C5 105.2(2) . . ? N2 C9 N1 126.5(2) 2_666 . ? N2 C9 C9 116.9(3) 2_666 2_666 ? N1 C9 C9 116.7(3) . 2_666 ? O9 C10 O13 125.3(2) . . ? O9 C10 C2 117.3(2) . . ? O13 C10 C2 117.4(2) . . ? C33 C12 C29 111.9(4) . . ? C33 C12 C4 106.7(3) . . ? C29 C12 C4 110.4(3) . . ? C33 C12 C32 110.4(4) . . ? C29 C12 C32 108.7(3) . . ? C4 C12 C32 108.7(3) . . ? O7 C13 O3 126.0(2) . . ? O7 C13 C14 117.4(2) . . ? O3 C13 C14 116.5(2) . . ? C30B C14 C28A 135.2(7) . . ? C30B C14 C30A 37.6(8) . . ? C28A C14 C30A 111.7(4) . . ? C30B C14 C28B 111.1(11) . . ? C28A C14 C28B 49.0(6) . . ? C30A C14 C28B 74.1(7) . . ? C30B C14 C13 109.7(7) . . ? C28A C14 C13 113.5(3) . . ? C30A C14 C13 111.7(3) . . ? C28B C14 C13 101.5(6) . . ? C30B C14 C23B 116.0(11) . . ? C28A C14 C23B 61.2(9) . . ? C30A C14 C23B 139.1(7) . . ? C28B C14 C23B 110.2(10) . . ? C13 C14 C23B 107.3(7) . . ? C30B C14 C23A 71.4(9) . . ? C28A C14 C23A 107.0(4) . . ? C30A C14 C23A 106.8(4) . . ? C28B C14 C23A 150.0(6) . . ? C13 C14 C23A 105.6(3) . . ? C23B C14 C23A 49.2(8) . . ? N2 C16 C1 121.0(2) . 2_666 ? N3 C17 C18 178.8(4) . . ? O2 C19 O6 125.1(2) . . ? O2 C19 C3 117.6(2) . . ? O6 C19 C3 117.2(2) . . ? O5 C21 O8 125.6(2) . . ? O5 C21 C7 117.5(2) . . ? O8 C21 C7 116.9(2) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 27.59 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.657 _refine_diff_density_min -0.421 _refine_diff_density_rms 0.078 #END data_pa_476_0m _database_code_depnum_ccdc_archive 'CCDC 750195' #TrackingRef 'albores_et_al.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 H130 Fe4 Mn2 N8 O28' _chemical_formula_weight 1937.16 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' Mn Mn 0.3368 0.7283 '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 P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.6170(16) _cell_length_b 16.8069(18) _cell_length_c 20.971(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.166(4) _cell_angle_gamma 90.00 _cell_volume 5144.0(10) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.251 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2040 _exptl_absorpt_coefficient_mu 0.856 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.7394 _exptl_absorpt_correction_T_max 0.9584 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71069 _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 56537 _diffrn_reflns_av_R_equivalents 0.2779 _diffrn_reflns_av_sigmaI/netI 0.2544 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 27.50 _reflns_number_total 11787 _reflns_number_gt 4146 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^)+(0.0486P)^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 11787 _refine_ls_number_parameters 568 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.2469 _refine_ls_R_factor_gt 0.0584 _refine_ls_wR_factor_ref 0.1740 _refine_ls_wR_factor_gt 0.1104 _refine_ls_goodness_of_fit_ref 0.958 _refine_ls_restrained_S_all 0.959 _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 C1 C 0.0206(5) 0.1690(4) 0.9318(4) 0.062(2) Uani 1 1 d . . . C1S C 0.4541(6) 0.0813(5) 0.1653(4) 0.068(2) Uani 1 1 d . . . C2 C 0.4498(5) 0.1597(4) 0.9042(3) 0.0502(19) Uani 1 1 d D . . C2S C 0.4804(6) 0.1236(4) 0.1088(4) 0.080(3) Uani 1 1 d . . . H2S1 H 0.5447 0.1122 0.1014 0.120 Uiso 1 1 calc R . . H2S2 H 0.4727 0.1810 0.1151 0.120 Uiso 1 1 calc R . . H2S3 H 0.4417 0.1063 0.0718 0.120 Uiso 1 1 calc R . . C3 C 0.4091(4) 0.2176(4) 0.9517(3) 0.0375(16) Uani 1 1 d . A . C3S C 0.2618(6) 0.9442(5) 0.9827(4) 0.075(3) Uani 1 1 d . . . C4 C 0.2527(4) 0.3917(4) 0.8364(3) 0.0382(16) Uani 1 1 d . B . C4S C 0.2533(5) 1.0030(5) 1.0325(4) 0.086(3) Uani 1 1 d . . . H4S1 H 0.2280 1.0522 1.0139 0.130 Uiso 1 1 calc R . . H4S2 H 0.3138 1.0137 1.0532 0.130 Uiso 1 1 calc R . . H4S3 H 0.2124 0.9827 1.0643 0.130 Uiso 1 1 calc R . . C5 C 0.2499(4) 0.3926(4) 0.7632(3) 0.0482(18) Uani 1 1 d . . . C6 C 0.2582(5) 0.6454(4) 0.9566(4) 0.059(2) Uani 1 1 d D . . C7 C 0.4370(4) 0.3774(4) 1.1789(3) 0.0434(18) Uani 1 1 d . . . C8 C -0.0223(4) 0.4649(4) 0.8639(3) 0.0445(18) Uani 1 1 d . . . H8 H 0.0029 0.4353 0.8305 0.053 Uiso 1 1 calc R . . N2 N 0.0175(3) 0.4606(3) 0.9223(2) 0.0353(13) Uani 1 1 d . . . C10 C 0.0206(4) 0.4972(3) 1.0327(3) 0.0303(15) Uani 1 1 d . . . C11 C 0.2643(4) 0.5549(4) 0.9582(3) 0.0394(16) Uani 1 1 d . B . C12 C 0.4079(4) 0.3586(4) 1.1090(3) 0.0350(16) Uani 1 1 d . A . C13 C 0.1337(4) 0.4480(4) 1.1006(3) 0.0445(18) Uani 1 1 d . . . H13 H 0.1872 0.4167 1.1089 0.053 Uiso 1 1 calc R . . C15 C -0.0143(6) 0.1218(5) 0.9884(5) 0.121(4) Uani 1 1 d . . . H15A H -0.0574 0.0808 0.9724 0.181 Uiso 1 1 calc R . . H15B H -0.0452 0.1580 1.0168 0.181 Uiso 1 1 calc R . . H15C H 0.0377 0.0965 1.0120 0.181 Uiso 1 1 calc R . . C16 C 0.0888(4) 0.2314(4) 0.9586(3) 0.0420(17) Uani 1 1 d . A . C18 C 0.1918(5) 0.2056(5) 1.1328(4) 0.055(2) Uani 1 1 d . A . C19 C 0.5048(5) 0.4449(4) 1.1862(3) 0.065(2) Uani 1 1 d . . . H19A H 0.4777 0.4932 1.1670 0.098 Uiso 1 1 calc R . . H19B H 0.5605 0.4312 1.1647 0.098 Uiso 1 1 calc R . . H19C H 0.5201 0.4543 1.2317 0.098 Uiso 1 1 calc R . . C20 C 0.4772(5) 0.3020(4) 1.2105(3) 0.067(2) Uani 1 1 d . . . H20A H 0.4319 0.2590 1.2066 0.101 Uiso 1 1 calc R . . H20B H 0.4928 0.3125 1.2558 0.101 Uiso 1 1 calc R . . H20C H 0.5325 0.2863 1.1893 0.101 Uiso 1 1 calc R . . C21 C 0.1840(5) 0.3285(5) 0.7371(4) 0.083(3) Uani 1 1 d . . . H21A H 0.1226 0.3388 0.7516 0.125 Uiso 1 1 calc R . . H21B H 0.2051 0.2762 0.7526 0.125 Uiso 1 1 calc R . . H21C H 0.1821 0.3292 0.6903 0.125 Uiso 1 1 calc R . . C24 C 0.1454(6) 0.1764(5) 1.1919(4) 0.067(2) Uani 1 1 d D . . C25 C -0.0601(5) 0.2108(5) 0.8945(4) 0.090(3) Uani 1 1 d . . . H25A H -0.1032 0.1707 0.8770 0.135 Uiso 1 1 calc R . . H25B H -0.0366 0.2421 0.8595 0.135 Uiso 1 1 calc R . . H25C H -0.0915 0.2461 0.9234 0.135 Uiso 1 1 calc R . . C27 C 0.3432(5) 0.3774(5) 0.7394(3) 0.070(2) Uani 1 1 d . . . H27A H 0.3398 0.3785 0.6926 0.105 Uiso 1 1 calc R . . H27B H 0.3650 0.3251 0.7542 0.105 Uiso 1 1 calc R . . H27C H 0.3857 0.4186 0.7558 0.105 Uiso 1 1 calc R . . C28 C 0.3493(5) 0.4006(5) 1.2109(3) 0.073(2) Uani 1 1 d . . . H28A H 0.3054 0.3565 1.2072 0.110 Uiso 1 1 calc R . . H28B H 0.3225 0.4478 1.1899 0.110 Uiso 1 1 calc R . . H28C H 0.3638 0.4122 1.2561 0.110 Uiso 1 1 calc R . . C29 C 0.0708(5) 0.1157(4) 0.8861(4) 0.089(3) Uani 1 1 d . . . H29A H 0.0287 0.0751 0.8683 0.134 Uiso 1 1 calc R . . H29B H 0.1228 0.0899 0.9093 0.134 Uiso 1 1 calc R . . H29C H 0.0933 0.1481 0.8513 0.134 Uiso 1 1 calc R . . C32 C 0.2149(6) 0.4744(5) 0.7429(4) 0.097(3) Uani 1 1 d . . . H32A H 0.1539 0.4828 0.7589 0.145 Uiso 1 1 calc R . . H32B H 0.2114 0.4779 0.6962 0.145 Uiso 1 1 calc R . . H32C H 0.2569 0.5152 0.7606 0.145 Uiso 1 1 calc R . . N1 N 0.0946(3) 0.4505(3) 1.0413(2) 0.0369(13) Uani 1 1 d . . . N1S N 0.4337(6) 0.0469(5) 0.2071(4) 0.114(3) Uani 1 1 d . . . N2S N 0.2692(6) 0.9004(4) 0.9433(4) 0.104(3) Uani 1 1 d . . . C35 C -0.0978(4) 0.5102(4) 0.8504(3) 0.0509(19) Uani 1 1 d . . . H35 H -0.1250 0.5128 0.8083 0.061 Uiso 1 1 calc R . . O1 O 0.2544(2) 0.3548(2) 0.99572(18) 0.0330(10) Uani 1 1 d . . . O2 O 0.3465(3) 0.1908(2) 0.9866(2) 0.0404(11) Uani 1 1 d . . . O3 O 0.1934(3) 0.5161(2) 0.9452(2) 0.0418(12) Uani 1 1 d . . . O4 O 0.1760(3) 0.3827(2) 0.86091(19) 0.0428(11) Uani 1 1 d . . . O5 O 0.5121(3) 0.4403(3) 0.9424(2) 0.0427(11) Uani 1 1 d D . . O6 O 0.4258(2) 0.4079(2) 1.06601(19) 0.0359(10) Uani 1 1 d . . . O7 O 0.3268(2) 0.4025(2) 0.86714(19) 0.0419(11) Uani 1 1 d . . . O8 O 0.3419(3) 0.5242(2) 0.9724(2) 0.0449(12) Uani 1 1 d . . . O9 O 0.3648(3) 0.2944(2) 1.09941(19) 0.0390(11) Uani 1 1 d . . . O10 O 0.2493(3) 0.1625(2) 1.1050(2) 0.0469(12) Uani 1 1 d . . . O11 O 0.0689(3) 0.3035(3) 0.9541(2) 0.0474(12) Uani 1 1 d . . . O12 O 0.4364(3) 0.2873(2) 0.9523(2) 0.0451(12) Uani 1 1 d . . . O13 O 0.1616(3) 0.2031(2) 0.9849(2) 0.0493(13) Uani 1 1 d . . . O14 O 0.1741(3) 0.2742(3) 1.1093(2) 0.0492(12) Uani 1 1 d . . . Fe1 Fe 0.15221(6) 0.39962(5) 0.95277(4) 0.0373(3) Uani 1 1 d . B . Mn1 Mn 0.37714(6) 0.40020(5) 0.96482(4) 0.0324(2) Uani 1 1 d . A . Fe2 Fe 0.26499(6) 0.25707(5) 1.03672(4) 0.0350(2) Uani 1 1 d . A . C14A C 0.4203(15) 0.0728(6) 0.9173(8) 0.104(7) Uani 0.684(14) 1 d PD A 1 H14A H 0.3534 0.0699 0.9174 0.156 Uiso 0.684(14) 1 calc PR A 1 H14B H 0.4472 0.0556 0.9589 0.156 Uiso 0.684(14) 1 calc PR A 1 H14C H 0.4419 0.0379 0.8838 0.156 Uiso 0.684(14) 1 calc PR A 1 C26A C 0.5516(7) 0.1730(12) 0.9018(10) 0.110(7) Uani 0.684(14) 1 d PD A 1 H26A H 0.5818 0.1597 0.9433 0.165 Uiso 0.684(14) 1 calc PR A 1 H26B H 0.5633 0.2289 0.8918 0.165 Uiso 0.684(14) 1 calc PR A 1 H26C H 0.5758 0.1390 0.8687 0.165 Uiso 0.684(14) 1 calc PR A 1 C34A C 0.4057(12) 0.1798(10) 0.8384(6) 0.090(5) Uani 0.684(14) 1 d PD A 1 H34A H 0.3397 0.1695 0.8380 0.135 Uiso 0.684(14) 1 calc PR A 1 H34B H 0.4331 0.1468 0.8059 0.135 Uiso 0.684(14) 1 calc PR A 1 H34C H 0.4161 0.2361 0.8289 0.135 Uiso 0.684(14) 1 calc PR A 1 C14B C 0.492(3) 0.0881(16) 0.9425(14) 0.104(7) Uani 0.316(14) 1 d PD A 2 H14D H 0.5436 0.1068 0.9706 0.156 Uiso 0.316(14) 1 calc PR A 2 H14E H 0.5143 0.0484 0.9127 0.156 Uiso 0.316(14) 1 calc PR A 2 H14F H 0.4456 0.0640 0.9682 0.156 Uiso 0.316(14) 1 calc PR A 2 C26B C 0.5252(19) 0.200(3) 0.8710(19) 0.110(7) Uani 0.316(14) 1 d PD A 2 H26D H 0.5772 0.2099 0.9016 0.165 Uiso 0.316(14) 1 calc PR A 2 H26E H 0.5029 0.2512 0.8534 0.165 Uiso 0.316(14) 1 calc PR A 2 H26F H 0.5449 0.1664 0.8363 0.165 Uiso 0.316(14) 1 calc PR A 2 C34B C 0.371(2) 0.140(2) 0.8574(14) 0.090(5) Uani 0.316(14) 1 d PD A 2 H34D H 0.3217 0.1155 0.8801 0.135 Uiso 0.316(14) 1 calc PR A 2 H34E H 0.3925 0.1022 0.8255 0.135 Uiso 0.316(14) 1 calc PR A 2 H34F H 0.3493 0.1884 0.8360 0.135 Uiso 0.316(14) 1 calc PR A 2 C17A C 0.1667(7) 0.6741(6) 0.9281(7) 0.100(5) Uani 0.762(9) 1 d PD B 1 H17A H 0.1173 0.6442 0.9468 0.151 Uiso 0.762(9) 1 calc PR B 1 H17B H 0.1639 0.6657 0.8817 0.151 Uiso 0.762(9) 1 calc PR B 1 H17C H 0.1597 0.7309 0.9371 0.151 Uiso 0.762(9) 1 calc PR B 1 C30A C 0.2602(8) 0.6690(6) 1.0314(5) 0.091(4) Uani 0.762(9) 1 d PD B 1 H30A H 0.2051 0.6484 1.0502 0.136 Uiso 0.762(9) 1 calc PR B 1 H30B H 0.2621 0.7271 1.0357 0.136 Uiso 0.762(9) 1 calc PR B 1 H30C H 0.3147 0.6459 1.0535 0.136 Uiso 0.762(9) 1 calc PR B 1 C31A C 0.3395(18) 0.684(2) 0.9321(14) 0.089(9) Uani 0.762(9) 1 d PD B 1 H31A H 0.3314 0.7415 0.9321 0.134 Uiso 0.762(9) 1 calc PR B 1 H31B H 0.3477 0.6654 0.8884 0.134 Uiso 0.762(9) 1 calc PR B 1 H31C H 0.3937 0.6695 0.9593 0.134 Uiso 0.762(9) 1 calc PR B 1 C17B C 0.225(3) 0.659(2) 0.8841(11) 0.100(5) Uani 0.238(9) 1 d PD B 2 H17D H 0.1680 0.6303 0.8746 0.151 Uiso 0.238(9) 1 calc PR B 2 H17E H 0.2724 0.6398 0.8565 0.151 Uiso 0.238(9) 1 calc PR B 2 H17F H 0.2154 0.7162 0.8766 0.151 Uiso 0.238(9) 1 calc PR B 2 C30B C 0.177(2) 0.6782(19) 0.991(2) 0.091(4) Uani 0.238(9) 1 d PD B 2 H30D H 0.1363 0.6342 1.0023 0.136 Uiso 0.238(9) 1 calc PR B 2 H30E H 0.1425 0.7160 0.9636 0.136 Uiso 0.238(9) 1 calc PR B 2 H30F H 0.1991 0.7053 1.0306 0.136 Uiso 0.238(9) 1 calc PR B 2 C31B C 0.344(6) 0.690(8) 0.956(6) 0.089(9) Uani 0.238(9) 1 d PD B 2 H31D H 0.3306 0.7474 0.9601 0.134 Uiso 0.238(9) 1 calc PR B 2 H31E H 0.3737 0.6803 0.9166 0.134 Uiso 0.238(9) 1 calc PR B 2 H31F H 0.3844 0.6738 0.9928 0.134 Uiso 0.238(9) 1 calc PR B 2 C22B C 0.0994(9) 0.0969(6) 1.1751(5) 0.107(5) Uani 0.891(13) 1 d PD C 1 H22D H 0.0496 0.0874 1.2035 0.160 Uiso 0.891(13) 1 calc PR C 1 H22E H 0.1446 0.0539 1.1802 0.160 Uiso 0.891(13) 1 calc PR C 1 H22F H 0.0746 0.0982 1.1307 0.160 Uiso 0.891(13) 1 calc PR C 1 C23B C 0.0737(9) 0.2327(8) 1.2097(7) 0.136(6) Uani 0.891(13) 1 d PD C 1 H23A H 0.0185 0.2031 1.2196 0.204 Uiso 0.891(13) 1 calc PR C 1 H23B H 0.0592 0.2691 1.1740 0.204 Uiso 0.891(13) 1 calc PR C 1 H23C H 0.0957 0.2633 1.2472 0.204 Uiso 0.891(13) 1 calc PR C 1 C33B C 0.2193(8) 0.1650(11) 1.2454(5) 0.144(7) Uani 0.891(13) 1 d PD C 1 H33D H 0.1957 0.1306 1.2785 0.217 Uiso 0.891(13) 1 calc PR C 1 H33E H 0.2363 0.2168 1.2639 0.217 Uiso 0.891(13) 1 calc PR C 1 H33F H 0.2733 0.1402 1.2281 0.217 Uiso 0.891(13) 1 calc PR C 1 C22A C 0.185(6) 0.095(3) 1.209(5) 0.107(5) Uani 0.109(13) 1 d PD C 2 H22A H 0.1629 0.0770 1.2493 0.160 Uiso 0.109(13) 1 calc PR C 2 H22B H 0.2525 0.0984 1.2122 0.160 Uiso 0.109(13) 1 calc PR C 2 H22C H 0.1667 0.0568 1.1749 0.160 Uiso 0.109(13) 1 calc PR C 2 C23A C 0.052(4) 0.206(8) 1.176(6) 0.136(6) Uani 0.109(13) 1 d PD C 2 H23D H 0.0167 0.2050 1.2145 0.204 Uiso 0.109(13) 1 calc PR C 2 H23E H 0.0221 0.1727 1.1431 0.204 Uiso 0.109(13) 1 calc PR C 2 H23F H 0.0554 0.2611 1.1606 0.204 Uiso 0.109(13) 1 calc PR C 2 C33A C 0.179(8) 0.221(7) 1.252(3) 0.144(7) Uani 0.109(13) 1 d PD C 2 H33A H 0.1323 0.2181 1.2837 0.217 Uiso 0.109(13) 1 calc PR C 2 H33B H 0.1907 0.2765 1.2415 0.217 Uiso 0.109(13) 1 calc PR C 2 H33C H 0.2358 0.1962 1.2696 0.217 Uiso 0.109(13) 1 calc PR C 2 H5A H 0.526(7) 0.488(2) 0.935(5) 0.173 Uiso 1 1 d D . . H5B H 0.549(6) 0.435(6) 0.975(3) 0.173 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.044(4) 0.065(5) 0.078(6) -0.027(5) 0.000(4) -0.015(4) C1S 0.074(6) 0.066(6) 0.063(7) -0.009(5) 0.002(5) 0.017(5) C2 0.065(5) 0.039(4) 0.049(5) -0.002(4) 0.023(4) 0.008(4) C2S 0.102(7) 0.053(5) 0.083(7) 0.007(5) -0.001(6) 0.021(5) C3 0.032(4) 0.034(4) 0.046(5) -0.002(3) -0.006(3) 0.003(3) C3S 0.091(7) 0.043(5) 0.092(8) -0.012(5) 0.010(6) -0.005(5) C4 0.036(4) 0.036(4) 0.044(4) -0.005(3) 0.004(3) 0.002(3) C4S 0.079(6) 0.072(6) 0.110(8) -0.031(6) 0.019(6) -0.009(5) C5 0.034(4) 0.073(5) 0.038(4) -0.001(4) 0.007(3) -0.001(4) C6 0.038(4) 0.029(4) 0.110(7) -0.006(5) 0.001(4) 0.002(4) C7 0.042(4) 0.042(4) 0.045(4) -0.006(3) -0.007(3) -0.001(3) C8 0.041(4) 0.049(4) 0.042(4) -0.012(3) -0.009(3) 0.006(3) N2 0.032(3) 0.040(3) 0.034(3) -0.003(3) 0.000(3) 0.001(2) C10 0.019(3) 0.027(3) 0.044(4) -0.003(3) 0.005(3) -0.002(3) C11 0.032(4) 0.042(4) 0.045(4) -0.008(4) 0.010(3) 0.007(4) C12 0.030(3) 0.032(4) 0.042(4) -0.006(3) -0.004(3) 0.010(3) C13 0.032(4) 0.049(4) 0.050(5) -0.009(4) -0.016(3) 0.010(3) C15 0.099(7) 0.129(9) 0.134(10) 0.014(7) 0.000(7) -0.082(7) C16 0.033(4) 0.049(5) 0.044(4) -0.010(4) 0.008(3) -0.008(4) C18 0.049(5) 0.056(5) 0.062(6) -0.001(4) 0.021(4) -0.013(4) C19 0.079(6) 0.066(5) 0.048(5) -0.009(4) -0.021(4) -0.017(4) C20 0.094(6) 0.059(5) 0.046(5) 0.013(4) -0.021(4) 0.005(5) C21 0.075(6) 0.118(8) 0.057(6) -0.036(5) -0.004(5) -0.023(5) C24 0.082(6) 0.056(5) 0.068(6) 0.004(4) 0.051(5) -0.010(5) C25 0.045(5) 0.112(7) 0.111(8) -0.058(6) -0.022(5) 0.002(5) C27 0.055(5) 0.103(7) 0.053(5) -0.016(5) 0.007(4) -0.006(4) C28 0.072(5) 0.090(6) 0.057(5) -0.019(5) 0.004(4) 0.004(5) C29 0.079(6) 0.080(6) 0.105(7) -0.053(6) -0.030(5) 0.014(5) C32 0.135(9) 0.089(7) 0.068(6) 0.039(5) 0.021(6) 0.038(6) N1 0.031(3) 0.033(3) 0.045(3) -0.005(3) -0.007(3) 0.003(2) N1S 0.138(8) 0.136(8) 0.072(6) 0.024(6) 0.026(6) 0.027(6) N2S 0.144(8) 0.065(5) 0.105(7) -0.022(5) 0.017(6) -0.001(5) C35 0.050(4) 0.060(5) 0.041(5) -0.006(4) -0.012(4) 0.012(4) O1 0.027(2) 0.030(2) 0.042(3) -0.0012(19) 0.0020(19) -0.0022(18) O2 0.046(3) 0.031(2) 0.045(3) -0.003(2) 0.009(2) 0.004(2) O3 0.027(2) 0.033(3) 0.064(3) 0.001(2) -0.006(2) -0.002(2) O4 0.032(2) 0.052(3) 0.044(3) -0.010(2) 0.002(2) 0.001(2) O5 0.039(3) 0.035(3) 0.054(3) 0.002(2) 0.001(2) -0.004(2) O6 0.035(2) 0.031(2) 0.041(3) 0.006(2) -0.003(2) -0.003(2) O7 0.028(2) 0.056(3) 0.042(3) -0.001(2) -0.003(2) -0.007(2) O8 0.038(3) 0.032(3) 0.064(3) -0.005(2) -0.006(2) 0.006(2) O9 0.043(3) 0.032(2) 0.042(3) 0.000(2) -0.002(2) -0.006(2) O10 0.049(3) 0.040(3) 0.053(3) 0.003(2) 0.011(2) -0.005(2) O11 0.032(2) 0.050(3) 0.061(3) -0.011(3) 0.004(2) -0.001(2) O12 0.037(3) 0.030(3) 0.069(3) -0.002(2) 0.013(2) -0.001(2) O13 0.039(3) 0.038(3) 0.070(4) -0.004(2) -0.007(3) -0.007(2) O14 0.047(3) 0.047(3) 0.056(3) 0.001(2) 0.021(2) 0.000(2) Fe1 0.0298(5) 0.0370(5) 0.0447(6) -0.0033(5) -0.0009(4) 0.0054(4) Mn1 0.0300(5) 0.0272(5) 0.0395(6) -0.0025(5) -0.0025(4) 0.0009(4) Fe2 0.0301(5) 0.0317(5) 0.0431(6) -0.0017(5) 0.0018(4) -0.0016(4) C14A 0.19(2) 0.027(6) 0.103(13) -0.011(7) 0.083(14) 0.010(9) C26A 0.048(8) 0.142(17) 0.139(19) -0.079(13) 0.006(9) 0.028(9) C34A 0.134(14) 0.094(14) 0.043(9) -0.023(8) 0.015(9) 0.000(9) C14B 0.19(2) 0.027(6) 0.103(13) -0.011(7) 0.083(14) 0.010(9) C26B 0.048(8) 0.142(17) 0.139(19) -0.079(13) 0.006(9) 0.028(9) C34B 0.134(14) 0.094(14) 0.043(9) -0.023(8) 0.015(9) 0.000(9) C17A 0.078(9) 0.036(6) 0.183(17) 0.007(8) -0.030(9) 0.018(6) C30A 0.101(9) 0.044(6) 0.128(12) -0.028(7) 0.019(8) 0.019(7) C31A 0.065(7) 0.041(9) 0.17(3) 0.013(15) 0.043(14) 0.009(5) C17B 0.078(9) 0.036(6) 0.183(17) 0.007(8) -0.030(9) 0.018(6) C30B 0.101(9) 0.044(6) 0.128(12) -0.028(7) 0.019(8) 0.019(7) C31B 0.065(7) 0.041(9) 0.17(3) 0.013(15) 0.043(14) 0.009(5) C22B 0.145(12) 0.089(8) 0.091(9) 0.006(7) 0.061(8) -0.057(8) C23B 0.166(12) 0.116(13) 0.138(15) 0.021(10) 0.122(11) 0.010(10) C33B 0.099(11) 0.29(2) 0.049(7) 0.052(10) 0.014(7) -0.033(11) C22A 0.145(12) 0.089(8) 0.091(9) 0.006(7) 0.061(8) -0.057(8) C23A 0.166(12) 0.116(13) 0.138(15) 0.021(10) 0.122(11) 0.010(10) C33A 0.099(11) 0.29(2) 0.049(7) 0.052(10) 0.014(7) -0.033(11) _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 C1 C29 1.529(9) . ? C1 C16 1.534(8) . ? C1 C15 1.537(10) . ? C1 C25 1.547(9) . ? C1S N1S 1.105(10) . ? C1S C2S 1.452(10) . ? C2 C26B 1.501(19) . ? C2 C34B 1.504(18) . ? C2 C26A 1.508(11) . ? C2 C34A 1.529(11) . ? C2 C3 1.536(9) . ? C2 C14A 1.552(11) . ? C2 C14B 1.556(18) . ? C3 O12 1.238(7) . ? C3 O2 1.284(7) . ? C3S N2S 1.117(9) . ? C3S C4S 1.448(10) . ? C4 O7 1.243(6) . ? C4 O4 1.268(7) . ? C4 C5 1.532(8) . ? C5 C27 1.500(8) . ? C5 C32 1.519(9) . ? C5 C21 1.527(9) . ? C6 C31B 1.46(2) . ? C6 C31A 1.469(13) . ? C6 C17A 1.514(10) . ? C6 C11 1.524(8) . ? C6 C30B 1.535(19) . ? C6 C17B 1.585(19) . ? C6 C30A 1.617(11) . ? C7 C19 1.509(8) . ? C7 C28 1.529(9) . ? C7 C20 1.532(8) . ? C7 C12 1.536(8) . ? C8 N2 1.328(7) . ? C8 C35 1.357(8) . ? N2 C10 1.328(7) 3_567 ? N2 Fe1 2.280(5) . ? C10 N2 1.328(7) 3_567 ? C10 N1 1.340(7) . ? C10 C10 1.470(11) 3_567 ? C11 O3 1.242(7) . ? C11 O8 1.265(7) . ? C12 O9 1.260(6) . ? C12 O6 1.262(7) . ? C13 N1 1.341(7) . ? C13 C35 1.373(8) 3_567 ? C16 O11 1.248(7) . ? C16 O13 1.265(7) . ? C18 O10 1.275(8) . ? C18 O14 1.275(8) . ? C18 C24 1.526(10) . ? C18 Fe2 2.488(8) . ? C24 C23A 1.47(2) . ? C24 C23B 1.476(11) . ? C24 C22A 1.52(2) . ? C24 C33A 1.52(2) . ? C24 C33B 1.527(12) . ? C24 C22B 1.529(11) . ? N1 Fe1 2.249(5) . ? C35 C13 1.373(8) 3_567 ? O1 Fe2 1.856(4) . ? O1 Fe1 1.861(4) . ? O1 Mn1 2.086(4) . ? O2 Fe2 1.976(4) . ? O3 Fe1 2.057(4) . ? O4 Fe1 1.997(4) . ? O5 Mn1 2.161(4) . ? O6 Mn1 2.204(4) . ? O7 Mn1 2.138(4) . ? O8 Mn1 2.155(4) . ? O9 Fe2 2.010(4) . ? O10 Fe2 2.160(4) . ? O11 Fe1 2.024(4) . ? O12 Mn1 2.108(4) . ? O13 Fe2 2.026(4) . ? O14 Fe2 2.095(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 C29 C1 C16 107.8(6) . . ? C29 C1 C15 111.9(7) . . ? C16 C1 C15 107.8(6) . . ? C29 C1 C25 109.2(6) . . ? C16 C1 C25 109.7(6) . . ? C15 C1 C25 110.4(7) . . ? N1S C1S C2S 177.7(10) . . ? C26B C2 C34B 110.5(19) . . ? C26B C2 C26A 33.4(14) . . ? C34B C2 C26A 136.7(16) . . ? C26B C2 C34A 76.4(15) . . ? C34B C2 C34A 36.1(12) . . ? C26A C2 C34A 107.7(10) . . ? C26B C2 C3 109.5(19) . . ? C34B C2 C3 104.9(15) . . ? C26A C2 C3 110.3(9) . . ? C34A C2 C3 106.6(7) . . ? C26B C2 C14A 136.7(19) . . ? C34B C2 C14A 72.3(13) . . ? C26A C2 C14A 115.4(10) . . ? C34A C2 C14A 105.1(9) . . ? C3 C2 C14A 111.1(7) . . ? C26B C2 C14B 108.0(19) . . ? C34B C2 C14B 115.6(18) . . ? C26A C2 C14B 76.4(15) . . ? C34A C2 C14B 140.6(14) . . ? C3 C2 C14B 108.3(13) . . ? C14A C2 C14B 44.6(13) . . ? O12 C3 O2 124.4(6) . . ? O12 C3 C2 118.1(6) . . ? O2 C3 C2 117.5(6) . . ? N2S C3S C4S 178.2(10) . . ? O7 C4 O4 124.8(6) . . ? O7 C4 C5 119.5(6) . . ? O4 C4 C5 115.6(5) . . ? C27 C5 C32 111.1(6) . . ? C27 C5 C21 109.1(6) . . ? C32 C5 C21 110.0(6) . . ? C27 C5 C4 110.9(5) . . ? C32 C5 C4 106.2(6) . . ? C21 C5 C4 109.5(6) . . ? C31B C6 C31A 21(5) . . ? C31B C6 C17A 125(7) . . ? C31A C6 C17A 115.9(19) . . ? C31B C6 C11 118(6) . . ? C31A C6 C11 113.4(17) . . ? C17A C6 C11 112.1(6) . . ? C31B C6 C30B 120(5) . . ? C31A C6 C30B 132(2) . . ? C17A C6 C30B 51.8(16) . . ? C11 C6 C30B 113.2(14) . . ? C31B C6 C17B 98(5) . . ? C31A C6 C17B 79(2) . . ? C17A C6 C17B 50.2(14) . . ? C11 C6 C17B 100.5(13) . . ? C30B C6 C17B 102(2) . . ? C31B C6 C30A 85(4) . . ? C31A C6 C30A 105.1(12) . . ? C17A C6 C30A 105.9(8) . . ? C11 C6 C30A 103.0(6) . . ? C30B C6 C30A 54.8(17) . . ? C17B C6 C30A 151.9(14) . . ? C19 C7 C28 109.0(6) . . ? C19 C7 C20 110.1(5) . . ? C28 C7 C20 109.4(6) . . ? C19 C7 C12 113.4(6) . . ? C28 C7 C12 106.0(5) . . ? C20 C7 C12 108.8(5) . . ? N2 C8 C35 122.1(6) . . ? C10 N2 C8 116.6(5) 3_567 . ? C10 N2 Fe1 115.5(4) 3_567 . ? C8 N2 Fe1 127.6(4) . . ? N2 C10 N1 125.8(5) 3_567 . ? N2 C10 C10 117.6(6) 3_567 3_567 ? N1 C10 C10 116.6(7) . 3_567 ? O3 C11 O8 124.4(6) . . ? O3 C11 C6 118.1(6) . . ? O8 C11 C6 117.5(6) . . ? O9 C12 O6 124.7(6) . . ? O9 C12 C7 115.9(6) . . ? O6 C12 C7 119.3(5) . . ? N1 C13 C35 121.1(6) . 3_567 ? O11 C16 O13 125.8(6) . . ? O11 C16 C1 119.5(6) . . ? O13 C16 C1 114.6(6) . . ? O10 C18 O14 117.5(7) . . ? O10 C18 C24 121.5(7) . . ? O14 C18 C24 121.0(7) . . ? O10 C18 Fe2 60.2(4) . . ? O14 C18 Fe2 57.3(4) . . ? C24 C18 Fe2 178.3(6) . . ? C23A C24 C23B 34(5) . . ? C23A C24 C22A 134(7) . . ? C23B C24 C22A 142(3) . . ? C23A C24 C33A 106(6) . . ? C23B C24 C33A 71(5) . . ? C22A C24 C33A 98(6) . . ? C23A C24 C18 99(5) . . ? C23B C24 C18 110.7(8) . . ? C22A C24 C18 107(3) . . ? C33A C24 C18 112(5) . . ? C23A C24 C33B 145(5) . . ? C23B C24 C33B 112.2(9) . . ? C22A C24 C33B 58(4) . . ? C33A C24 C33B 43(5) . . ? C18 C24 C33B 108.1(8) . . ? C23A C24 C22B 82(6) . . ? C23B C24 C22B 108.0(9) . . ? C22A C24 C22B 55(4) . . ? C33A C24 C22B 137(5) . . ? C18 C24 C22B 107.7(7) . . ? C33B C24 C22B 110.1(9) . . ? C10 N1 C13 116.3(5) . . ? C10 N1 Fe1 116.6(4) . . ? C13 N1 Fe1 126.4(4) . . ? C8 C35 C13 118.2(6) . 3_567 ? Fe2 O1 Fe1 128.8(2) . . ? Fe2 O1 Mn1 114.64(18) . . ? Fe1 O1 Mn1 112.49(19) . . ? C3 O2 Fe2 125.1(4) . . ? C11 O3 Fe1 136.6(4) . . ? C4 O4 Fe1 125.4(4) . . ? C12 O6 Mn1 125.5(4) . . ? C4 O7 Mn1 137.6(4) . . ? C11 O8 Mn1 126.3(4) . . ? C12 O9 Fe2 135.2(4) . . ? C18 O10 Fe2 89.0(4) . . ? C16 O11 Fe1 129.6(4) . . ? C3 O12 Mn1 136.0(4) . . ? C16 O13 Fe2 130.5(4) . . ? C18 O14 Fe2 91.9(4) . . ? O1 Fe1 O4 103.39(17) . . ? O1 Fe1 O11 97.88(17) . . ? O4 Fe1 O11 92.14(17) . . ? O1 Fe1 O3 101.10(16) . . ? O4 Fe1 O3 89.59(17) . . ? O11 Fe1 O3 159.99(16) . . ? O1 Fe1 N1 94.70(17) . . ? O4 Fe1 N1 160.61(17) . . ? O11 Fe1 N1 92.23(17) . . ? O3 Fe1 N1 80.01(17) . . ? O1 Fe1 N2 167.37(18) . . ? O4 Fe1 N2 89.25(17) . . ? O11 Fe1 N2 81.47(17) . . ? O3 Fe1 N2 78.62(16) . . ? N1 Fe1 N2 72.75(17) . . ? O1 Mn1 O12 94.32(15) . . ? O1 Mn1 O7 92.75(15) . . ? O12 Mn1 O7 91.12(17) . . ? O1 Mn1 O8 96.79(15) . . ? O12 Mn1 O8 168.88(16) . . ? O7 Mn1 O8 88.93(16) . . ? O1 Mn1 O5 173.24(16) . . ? O12 Mn1 O5 82.39(16) . . ? O7 Mn1 O5 93.22(16) . . ? O8 Mn1 O5 86.51(17) . . ? O1 Mn1 O6 87.70(15) . . ? O12 Mn1 O6 93.42(16) . . ? O7 Mn1 O6 175.39(16) . . ? O8 Mn1 O6 86.46(15) . . ? O5 Mn1 O6 86.60(16) . . ? O1 Fe2 O2 106.82(18) . . ? O1 Fe2 O9 93.78(16) . . ? O2 Fe2 O9 94.99(17) . . ? O1 Fe2 O13 96.15(17) . . ? O2 Fe2 O13 85.14(17) . . ? O9 Fe2 O13 169.59(17) . . ? O1 Fe2 O14 100.08(18) . . ? O2 Fe2 O14 152.80(18) . . ? O9 Fe2 O14 87.07(17) . . ? O13 Fe2 O14 88.12(18) . . ? O1 Fe2 O10 161.62(17) . . ? O2 Fe2 O10 91.55(18) . . ? O9 Fe2 O10 84.05(16) . . ? O13 Fe2 O10 85.54(17) . . ? O14 Fe2 O10 61.63(17) . . ? O1 Fe2 C18 130.9(2) . . ? O2 Fe2 C18 122.3(2) . . ? O9 Fe2 C18 84.7(2) . . ? O13 Fe2 C18 86.4(2) . . ? O14 Fe2 C18 30.81(19) . . ? O10 Fe2 C18 30.82(19) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.478 _refine_diff_density_min -0.498 _refine_diff_density_rms 0.086 #END