# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email leila.boubkeur@univ-paris-diderot.fr loop_ _publ_author_name 'Koyel X. Bhattacharyya' 'Leila Boubekeur- Lecaque' 'Issa apsoba' 'Emmanuel Maisonhaute' 'Bernd Schollhorn' 'Christian Amatore' _publ_contact_author_name 'Leila Boubekeur-Lecaque' data_clb15p _database_code_depnum_ccdc_archive 'CCDC 894007' #TrackingRef 'web_deposit_cif_file_0_Boubekeur-Lecaque_1346659810.clb15F2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C43 H50 Fe N2 O10, C H2 Cl2' _chemical_formula_sum 'C44 H52 Cl2 Fe N2 O10' _chemical_formula_weight 895.63 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' Cl Cl 0.1484 0.1585 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.9797(10) _cell_length_b 13.0797(10) _cell_length_c 13.7456(11) _cell_angle_alpha 96.115(5) _cell_angle_beta 101.424(4) _cell_angle_gamma 93.178(4) _cell_volume 2267.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 9237 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 31.26 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.312 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 940 _exptl_absorpt_coefficient_mu 0.507 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8803 _exptl_absorpt_correction_T_max 0.9807 _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'curved graphite' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3333 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 140962 _diffrn_reflns_av_R_equivalents 0.0673 _diffrn_reflns_av_sigmaI/netI 0.0475 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 31.74 _reflns_number_total 15326 _reflns_number_gt 9669 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0663P)^2^+5.6956P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15326 _refine_ls_number_parameters 537 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0844 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.1246 _refine_ls_wR_factor_gt 0.0995 _refine_ls_goodness_of_fit_ref 1.147 _refine_ls_restrained_S_all 1.147 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.45183(4) 0.21382(3) 0.42462(4) 0.02650(13) Uani 1 1 d . . . N1 N 0.9161(2) -0.3016(2) 0.30060(19) 0.0235(5) Uani 1 1 d . . . N2 N 0.6829(2) -0.5075(2) -0.15051(19) 0.0241(5) Uani 1 1 d . . . O1 O 1.1536(2) -0.1637(3) 0.4531(2) 0.0580(9) Uani 1 1 d . . . O2 O 1.0820(2) -0.1636(2) 0.2912(2) 0.0387(6) Uani 1 1 d . . . O3 O 0.9146(2) -0.5178(2) 0.2801(2) 0.0385(6) Uani 1 1 d . . . O4 O 0.9226(2) -0.52105(19) 0.11837(18) 0.0329(5) Uani 1 1 d . . . O5 O 0.71532(16) -0.36507(17) 0.20160(18) 0.0266(5) Uani 1 1 d . . . O6 O 0.64147(19) -0.51689(17) 0.03315(17) 0.0273(5) Uani 1 1 d . . . O7 O 0.8299(2) -0.5589(3) -0.2770(2) 0.0464(7) Uani 1 1 d . . . O8 O 0.7334(2) -0.4791(2) -0.39550(19) 0.0364(6) Uani 1 1 d . . . O9 O 0.6177(2) -0.3126(2) -0.0967(2) 0.0376(6) Uani 1 1 d . . . O10 O 0.7809(2) -0.2597(2) -0.0112(2) 0.0421(6) Uani 1 1 d . . . C1 C 0.5587(4) 0.2313(3) 0.5559(4) 0.0585(14) Uani 1 1 d . . . H1 H 0.5712 0.1810 0.6010 0.070 Uiso 1 1 calc R . . C2 C 0.4856(4) 0.3061(3) 0.5570(3) 0.0500(11) Uani 1 1 d . . . H2 H 0.4405 0.3154 0.6033 0.060 Uiso 1 1 calc R . . C3 C 0.4906(3) 0.3648(3) 0.4780(4) 0.0482(11) Uani 1 1 d . . . H3 H 0.4494 0.4208 0.4614 0.058 Uiso 1 1 calc R . . C4 C 0.5675(4) 0.3259(4) 0.4279(4) 0.0560(12) Uani 1 1 d . . . H4 H 0.5875 0.3504 0.3712 0.067 Uiso 1 1 calc R . . C5 C 0.6095(3) 0.2432(4) 0.4779(5) 0.0621(16) Uani 1 1 d . . . H5 H 0.6634 0.2029 0.4607 0.075 Uiso 1 1 calc R . . C6 C 0.3738(3) 0.0730(2) 0.4151(3) 0.0288(7) Uani 1 1 d . . . H6 H 0.3828 0.0272 0.4649 0.035 Uiso 1 1 calc R . . C7 C 0.3006(3) 0.1499(3) 0.4056(3) 0.0341(8) Uani 1 1 d . . . H7 H 0.2522 0.1646 0.4477 0.041 Uiso 1 1 calc R . . C8 C 0.3126(3) 0.2007(3) 0.3226(3) 0.0354(8) Uani 1 1 d . . . H8 H 0.2732 0.2555 0.2995 0.043 Uiso 1 1 calc R . . C9 C 0.3930(3) 0.1569(3) 0.2790(3) 0.0326(7) Uani 1 1 d . . . H9 H 0.4168 0.1770 0.2223 0.039 Uiso 1 1 calc R . . C10 C 0.4316(2) 0.0761(2) 0.3369(2) 0.0257(6) Uani 1 1 d . . . C11 C 0.5159(3) 0.0143(2) 0.3222(3) 0.0292(7) Uani 1 1 d . . . C12 C 0.5860(3) -0.0392(3) 0.3144(3) 0.0316(7) Uani 1 1 d . . . C13 C 0.6711(3) -0.1044(2) 0.3099(3) 0.0273(6) Uani 1 1 d . . . C14 C 0.7724(3) -0.0739(3) 0.3644(3) 0.0328(7) Uani 1 1 d . . . H14 H 0.7866 -0.0089 0.4044 0.039 Uiso 1 1 calc R . . C15 C 0.8527(3) -0.1390(3) 0.3599(3) 0.0292(7) Uani 1 1 d . . . H15 H 0.9215 -0.1173 0.3974 0.035 Uiso 1 1 calc R . . C16 C 0.8359(2) -0.2352(2) 0.3023(2) 0.0223(6) Uani 1 1 d . . . C17 C 0.7315(2) -0.2667(2) 0.2507(2) 0.0216(6) Uani 1 1 d . . . C18 C 0.6514(2) -0.2013(2) 0.2531(2) 0.0264(6) Uani 1 1 d . . . H18 H 0.5824 -0.2225 0.2157 0.032 Uiso 1 1 calc R . . C19 C 1.0076(3) -0.2861(3) 0.3798(3) 0.0305(7) Uani 1 1 d . . . H19A H 1.0439 -0.3507 0.3796 0.037 Uiso 1 1 calc R . . H19B H 0.9833 -0.2757 0.4438 0.037 Uiso 1 1 calc R . . C20 C 1.0889(3) -0.1979(3) 0.3796(3) 0.0341(8) Uani 1 1 d . . . C21 C 1.1587(3) -0.0787(4) 0.2885(4) 0.0531(12) Uani 1 1 d . . . H21A H 1.2311 -0.1011 0.3052 0.064 Uiso 1 1 calc R . . H21B H 1.1522 -0.0200 0.3381 0.064 Uiso 1 1 calc R . . C22 C 1.1383(4) -0.0469(4) 0.1868(4) 0.0683(15) Uani 1 1 d . . . H22A H 1.1397 -0.1066 0.1377 0.102 Uiso 1 1 calc R . . H22B H 1.1928 0.0063 0.1822 0.102 Uiso 1 1 calc R . . H22C H 1.0690 -0.0191 0.1730 0.102 Uiso 1 1 calc R . . C23 C 0.9300(2) -0.3582(2) 0.2078(2) 0.0240(6) Uani 1 1 d . . . H23A H 1.0004 -0.3373 0.1957 0.029 Uiso 1 1 calc R . . H23B H 0.8765 -0.3396 0.1518 0.029 Uiso 1 1 calc R . . C24 C 0.9200(2) -0.4738(3) 0.2088(2) 0.0261(6) Uani 1 1 d . . . C25 C 0.9229(3) -0.6327(3) 0.1100(3) 0.0401(9) Uani 1 1 d . . . H25A H 0.8554 -0.6635 0.1212 0.048 Uiso 1 1 calc R . . H25B H 0.9811 -0.6532 0.1607 0.048 Uiso 1 1 calc R . . C26 C 0.9373(4) -0.6695(4) 0.0066(3) 0.0490(11) Uani 1 1 d . . . H26A H 0.8792 -0.6491 -0.0429 0.074 Uiso 1 1 calc R . . H26B H 0.9379 -0.7448 -0.0013 0.074 Uiso 1 1 calc R . . H26C H 1.0043 -0.6387 -0.0036 0.074 Uiso 1 1 calc R . . C27 C 0.6083(2) -0.4062(3) 0.1676(2) 0.0260(6) Uani 1 1 d . . . H27A H 0.5718 -0.3668 0.1151 0.031 Uiso 1 1 calc R . . H27B H 0.5707 -0.4011 0.2237 0.031 Uiso 1 1 calc R . . C28 C 0.6089(3) -0.5170(3) 0.1262(2) 0.0259(6) Uani 1 1 d . . . H28A H 0.6585 -0.5530 0.1728 0.031 Uiso 1 1 calc R . . H28B H 0.5376 -0.5526 0.1162 0.031 Uiso 1 1 calc R . . C29 C 0.6428(2) -0.6098(2) -0.0227(2) 0.0218(6) Uani 1 1 d . . . C30 C 0.6189(3) -0.7047(2) 0.0079(3) 0.0281(6) Uani 1 1 d . . . H30 H 0.6045 -0.7071 0.0728 0.034 Uiso 1 1 calc R . . C31 C 0.6159(3) -0.7961(3) -0.0546(3) 0.0337(7) Uani 1 1 d . . . C32 C 0.6381(3) -0.7908(3) -0.1483(3) 0.0334(7) Uani 1 1 d . . . H32 H 0.6354 -0.8524 -0.1924 0.040 Uiso 1 1 calc R . . C33 C 0.6643(3) -0.6968(3) -0.1788(3) 0.0293(7) Uani 1 1 d . . . H33 H 0.6812 -0.6954 -0.2428 0.035 Uiso 1 1 calc R . . C34 C 0.6663(2) -0.6045(2) -0.1178(2) 0.0222(6) Uani 1 1 d . . . C35 C 0.7572(2) -0.4288(2) -0.0892(2) 0.0255(6) Uani 1 1 d . . . H35A H 0.8159 -0.4150 -0.1236 0.031 Uiso 1 1 calc R . . H35B H 0.7872 -0.4545 -0.0252 0.031 Uiso 1 1 calc R . . C36 C 0.7076(3) -0.3293(2) -0.0676(2) 0.0269(6) Uani 1 1 d . . . C37 C 0.7456(4) -0.1582(3) 0.0127(4) 0.0496(11) Uani 1 1 d . . . H37A H 0.6915 -0.1628 0.0540 0.060 Uiso 1 1 calc R . . H37B H 0.7144 -0.1296 -0.0494 0.060 Uiso 1 1 calc R . . C38 C 0.8396(5) -0.0905(4) 0.0689(5) 0.0769(18) Uani 1 1 d . . . H38A H 0.8723 -0.1216 0.1281 0.115 Uiso 1 1 calc R . . H38B H 0.8176 -0.0225 0.0897 0.115 Uiso 1 1 calc R . . H38C H 0.8906 -0.0829 0.0257 0.115 Uiso 1 1 calc R . . C39 C 0.6613(2) -0.4978(3) -0.2556(2) 0.0257(6) Uani 1 1 d . . . H39A H 0.6395 -0.4275 -0.2647 0.031 Uiso 1 1 calc R . . H39B H 0.6008 -0.5471 -0.2887 0.031 Uiso 1 1 calc R . . C40 C 0.7525(3) -0.5165(3) -0.3086(2) 0.0270(6) Uani 1 1 d . . . C41 C 0.8094(3) -0.4948(3) -0.4604(3) 0.0428(10) Uani 1 1 d . . . H41A H 0.8086 -0.5689 -0.4849 0.051 Uiso 1 1 calc R . . H41B H 0.8816 -0.4703 -0.4235 0.051 Uiso 1 1 calc R . . C42 C 0.7767(5) -0.4345(4) -0.5453(4) 0.0623(14) Uani 1 1 d . . . H42A H 0.7048 -0.4588 -0.5803 0.094 Uiso 1 1 calc R . . H42B H 0.8249 -0.4435 -0.5917 0.094 Uiso 1 1 calc R . . H42C H 0.7788 -0.3613 -0.5200 0.094 Uiso 1 1 calc R . . C43 C 0.5847(4) -0.8980(3) -0.0213(4) 0.0564(12) Uani 1 1 d . . . H43A H 0.5496 -0.9458 -0.0798 0.085 Uiso 1 1 calc R . . H43B H 0.5365 -0.8868 0.0247 0.085 Uiso 1 1 calc R . . H43C H 0.6480 -0.9273 0.0127 0.085 Uiso 1 1 calc R . . Cl1 Cl 0.7694(2) 0.18112(19) 0.24016(16) 0.1297(10) Uani 1 1 d . . . Cl2 Cl 0.9931(2) 0.1855(3) 0.3251(2) 0.1490(11) Uani 1 1 d . . . C44 C 0.8758(5) 0.2394(5) 0.3316(4) 0.0741(17) Uani 1 1 d . . . H44A H 0.8841 0.3137 0.3241 0.089 Uiso 1 1 calc R . . H44B H 0.8599 0.2336 0.3984 0.089 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0255(2) 0.0193(2) 0.0315(3) -0.00400(17) 0.00147(18) 0.00301(16) N1 0.0203(11) 0.0290(13) 0.0208(12) -0.0034(10) 0.0056(9) 0.0041(10) N2 0.0260(12) 0.0262(12) 0.0191(12) 0.0018(10) 0.0051(10) -0.0062(10) O1 0.0350(15) 0.084(2) 0.0434(17) -0.0073(16) -0.0081(13) -0.0106(15) O2 0.0287(12) 0.0427(15) 0.0401(15) -0.0044(12) 0.0045(11) -0.0097(11) O3 0.0555(17) 0.0315(13) 0.0337(14) 0.0031(11) 0.0210(12) 0.0067(12) O4 0.0407(14) 0.0311(12) 0.0273(12) -0.0036(10) 0.0110(10) 0.0050(10) O5 0.0176(10) 0.0252(11) 0.0342(12) -0.0077(9) 0.0045(9) 0.0020(8) O6 0.0398(13) 0.0217(10) 0.0220(11) -0.0012(8) 0.0136(9) -0.0016(9) O7 0.0337(14) 0.071(2) 0.0440(16) 0.0216(15) 0.0171(12) 0.0233(14) O8 0.0364(13) 0.0526(16) 0.0306(13) 0.0161(12) 0.0217(11) 0.0181(12) O9 0.0330(13) 0.0337(13) 0.0458(15) 0.0048(11) 0.0072(11) 0.0026(10) O10 0.0432(15) 0.0281(12) 0.0478(16) -0.0018(11) -0.0028(12) -0.0047(11) C1 0.070(3) 0.033(2) 0.051(3) -0.0034(18) -0.035(2) 0.002(2) C2 0.062(3) 0.042(2) 0.037(2) -0.0180(18) 0.0035(19) -0.0052(19) C3 0.046(2) 0.0180(15) 0.066(3) -0.0101(16) -0.016(2) 0.0007(14) C4 0.054(3) 0.048(2) 0.060(3) -0.001(2) 0.007(2) -0.028(2) C5 0.0245(18) 0.047(2) 0.097(4) -0.027(3) -0.011(2) 0.0040(17) C6 0.0286(15) 0.0213(14) 0.0338(17) -0.0008(12) 0.0044(13) -0.0047(12) C7 0.0224(15) 0.0314(17) 0.047(2) -0.0080(15) 0.0094(14) 0.0034(13) C8 0.0269(16) 0.0237(15) 0.048(2) -0.0035(14) -0.0090(14) 0.0077(12) C9 0.0353(17) 0.0291(16) 0.0302(17) 0.0015(13) -0.0001(14) 0.0046(13) C10 0.0259(14) 0.0211(13) 0.0263(15) -0.0054(11) -0.0003(12) 0.0052(11) C11 0.0302(16) 0.0224(14) 0.0321(17) -0.0056(12) 0.0038(13) 0.0025(12) C12 0.0334(17) 0.0268(15) 0.0343(18) -0.0016(13) 0.0088(14) 0.0037(13) C13 0.0279(15) 0.0253(15) 0.0306(16) -0.0013(12) 0.0117(13) 0.0068(12) C14 0.0318(17) 0.0262(15) 0.0392(19) -0.0077(14) 0.0103(14) 0.0042(13) C15 0.0229(14) 0.0283(15) 0.0337(17) -0.0061(13) 0.0056(12) -0.0014(12) C16 0.0218(13) 0.0249(14) 0.0214(14) -0.0003(11) 0.0088(11) 0.0024(11) C17 0.0205(13) 0.0232(13) 0.0217(14) -0.0017(11) 0.0076(11) 0.0017(10) C18 0.0218(14) 0.0279(15) 0.0284(16) -0.0031(12) 0.0050(12) 0.0046(11) C19 0.0259(15) 0.0379(18) 0.0256(16) -0.0011(13) 0.0018(12) 0.0076(13) C20 0.0209(14) 0.0431(19) 0.0341(18) -0.0075(15) 0.0020(13) 0.0036(13) C21 0.038(2) 0.053(3) 0.063(3) -0.006(2) 0.013(2) -0.0207(19) C22 0.059(3) 0.066(3) 0.076(4) 0.016(3) 0.009(3) -0.022(3) C23 0.0216(13) 0.0301(15) 0.0222(14) 0.0003(12) 0.0103(11) 0.0035(11) C24 0.0219(14) 0.0308(15) 0.0259(15) -0.0016(12) 0.0080(11) 0.0033(12) C25 0.047(2) 0.0296(17) 0.045(2) -0.0060(15) 0.0154(17) 0.0044(15) C26 0.046(2) 0.049(2) 0.046(2) -0.0188(19) 0.0075(18) 0.0089(19) C27 0.0188(13) 0.0322(16) 0.0268(15) -0.0060(12) 0.0101(11) -0.0013(11) C28 0.0279(15) 0.0316(16) 0.0192(14) -0.0022(12) 0.0115(11) -0.0047(12) C29 0.0213(13) 0.0213(13) 0.0215(14) -0.0008(11) 0.0042(11) -0.0009(10) C30 0.0319(16) 0.0273(15) 0.0250(15) 0.0036(12) 0.0066(12) -0.0012(12) C31 0.0345(17) 0.0245(15) 0.0398(19) 0.0047(14) 0.0029(14) -0.0009(13) C32 0.0337(17) 0.0246(15) 0.0370(19) -0.0090(13) 0.0034(14) -0.0014(13) C33 0.0269(15) 0.0329(17) 0.0266(16) -0.0043(13) 0.0070(12) -0.0013(13) C34 0.0188(13) 0.0267(14) 0.0197(14) -0.0012(11) 0.0036(10) -0.0009(11) C35 0.0235(14) 0.0291(15) 0.0238(15) 0.0044(12) 0.0053(11) -0.0028(12) C36 0.0331(16) 0.0270(15) 0.0217(15) 0.0053(12) 0.0088(12) -0.0044(12) C37 0.066(3) 0.0281(18) 0.049(2) -0.0016(17) 0.002(2) 0.0001(18) C38 0.103(5) 0.038(2) 0.071(4) -0.004(2) -0.018(3) -0.011(3) C39 0.0240(14) 0.0340(16) 0.0206(14) 0.0027(12) 0.0086(11) 0.0030(12) C40 0.0261(15) 0.0336(16) 0.0250(15) 0.0057(13) 0.0116(12) 0.0057(12) C41 0.044(2) 0.057(2) 0.041(2) 0.0131(18) 0.0339(18) 0.0186(18) C42 0.083(4) 0.071(3) 0.056(3) 0.030(3) 0.050(3) 0.027(3) C43 0.078(3) 0.0252(18) 0.063(3) 0.0052(19) 0.011(3) -0.006(2) Cl1 0.160(2) 0.1151(16) 0.0886(13) 0.0342(12) -0.0277(13) -0.0561(15) Cl2 0.155(2) 0.176(3) 0.142(2) 0.058(2) 0.0522(19) 0.087(2) C44 0.099(5) 0.070(4) 0.052(3) 0.020(3) 0.007(3) -0.002(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 Fe1 C1 2.029(4) . ? Fe1 C2 2.029(4) . ? Fe1 C4 2.030(4) . ? Fe1 C10 2.031(3) . ? Fe1 C6 2.031(3) . ? Fe1 C3 2.032(3) . ? Fe1 C5 2.033(4) . ? Fe1 C9 2.039(4) . ? Fe1 C8 2.042(3) . ? Fe1 C7 2.046(3) . ? N1 C16 1.395(4) . ? N1 C19 1.432(4) . ? N1 C23 1.453(4) . ? N2 C34 1.410(4) . ? N2 C39 1.437(4) . ? N2 C35 1.444(4) . ? O1 C20 1.205(4) . ? O2 C20 1.329(5) . ? O2 C21 1.459(5) . ? O3 C24 1.200(4) . ? O4 C24 1.336(4) . ? O4 C25 1.453(4) . ? O5 C17 1.373(4) . ? O5 C27 1.430(4) . ? O6 C29 1.369(4) . ? O6 C28 1.425(4) . ? O7 C40 1.202(4) . ? O8 C40 1.322(4) . ? O8 C41 1.464(4) . ? O9 C36 1.197(4) . ? O10 C36 1.340(4) . ? O10 C37 1.454(5) . ? C1 C5 1.384(8) . ? C1 C2 1.400(7) . ? C1 H1 0.9500 . ? C2 C3 1.405(7) . ? C2 H2 0.9500 . ? C3 C4 1.410(7) . ? C3 H3 0.9500 . ? C4 C5 1.419(7) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.420(5) . ? C6 C10 1.431(5) . ? C6 H6 0.9500 . ? C7 C8 1.410(6) . ? C7 H7 0.9500 . ? C8 C9 1.420(5) . ? C8 H8 0.9500 . ? C9 C10 1.443(5) . ? C9 H9 0.9500 . ? C10 C11 1.429(4) . ? C11 C12 1.193(5) . ? C12 C13 1.438(4) . ? C13 C14 1.392(5) . ? C13 C18 1.399(4) . ? C14 C15 1.388(5) . ? C14 H14 0.9500 . ? C15 C16 1.395(4) . ? C15 H15 0.9500 . ? C16 C17 1.415(4) . ? C17 C18 1.386(4) . ? C18 H18 0.9500 . ? C19 C20 1.520(5) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C21 C22 1.479(7) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.511(5) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C25 C26 1.504(6) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.500(4) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.390(4) . ? C29 C34 1.408(4) . ? C30 C31 1.390(5) . ? C30 H30 0.9500 . ? C31 C32 1.382(5) . ? C31 C43 1.514(5) . ? C32 C33 1.386(5) . ? C32 H32 0.9500 . ? C33 C34 1.390(4) . ? C33 H33 0.9500 . ? C35 C36 1.511(5) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C37 C38 1.493(7) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.526(4) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C41 C42 1.484(6) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? Cl1 C44 1.749(6) . ? Cl2 C44 1.729(7) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? 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 C1 Fe1 C2 40.4(2) . . ? C1 Fe1 C4 68.1(2) . . ? C2 Fe1 C4 68.1(2) . . ? C1 Fe1 C10 119.16(15) . . ? C2 Fe1 C10 154.41(17) . . ? C4 Fe1 C10 124.89(18) . . ? C1 Fe1 C6 106.21(17) . . ? C2 Fe1 C6 119.69(18) . . ? C4 Fe1 C6 161.67(19) . . ? C10 Fe1 C6 41.24(14) . . ? C1 Fe1 C3 68.13(17) . . ? C2 Fe1 C3 40.48(19) . . ? C4 Fe1 C3 40.6(2) . . ? C10 Fe1 C3 162.82(18) . . ? C6 Fe1 C3 155.31(18) . . ? C1 Fe1 C5 39.8(2) . . ? C2 Fe1 C5 67.5(2) . . ? C4 Fe1 C5 40.9(2) . . ? C10 Fe1 C5 106.68(16) . . ? C6 Fe1 C5 123.80(18) . . ? C3 Fe1 C5 68.16(17) . . ? C1 Fe1 C9 155.33(19) . . ? C2 Fe1 C9 162.96(17) . . ? C4 Fe1 C9 108.08(18) . . ? C10 Fe1 C9 41.53(13) . . ? C6 Fe1 C9 69.34(15) . . ? C3 Fe1 C9 125.90(17) . . ? C5 Fe1 C9 121.3(2) . . ? C1 Fe1 C8 162.0(2) . . ? C2 Fe1 C8 126.09(18) . . ? C4 Fe1 C8 122.27(19) . . ? C10 Fe1 C8 68.86(13) . . ? C6 Fe1 C8 68.37(14) . . ? C3 Fe1 C8 109.19(15) . . ? C5 Fe1 C8 157.3(2) . . ? C9 Fe1 C8 40.70(15) . . ? C1 Fe1 C7 124.6(2) . . ? C2 Fe1 C7 107.79(18) . . ? C4 Fe1 C7 156.69(19) . . ? C10 Fe1 C7 69.03(13) . . ? C6 Fe1 C7 40.77(14) . . ? C3 Fe1 C7 121.29(16) . . ? C5 Fe1 C7 160.7(2) . . ? C9 Fe1 C7 68.76(16) . . ? C8 Fe1 C7 40.34(16) . . ? C16 N1 C19 118.8(3) . . ? C16 N1 C23 121.4(3) . . ? C19 N1 C23 115.8(2) . . ? C34 N2 C39 119.8(3) . . ? C34 N2 C35 120.7(3) . . ? C39 N2 C35 115.1(3) . . ? C20 O2 C21 115.0(3) . . ? C24 O4 C25 115.9(3) . . ? C17 O5 C27 116.9(2) . . ? C29 O6 C28 118.1(2) . . ? C40 O8 C41 117.7(3) . . ? C36 O10 C37 115.8(3) . . ? C5 C1 C2 108.3(4) . . ? C5 C1 Fe1 70.2(3) . . ? C2 C1 Fe1 69.8(2) . . ? C5 C1 H1 125.8 . . ? C2 C1 H1 125.8 . . ? Fe1 C1 H1 125.7 . . ? C1 C2 C3 108.4(5) . . ? C1 C2 Fe1 69.8(2) . . ? C3 C2 Fe1 69.9(2) . . ? C1 C2 H2 125.8 . . ? C3 C2 H2 125.8 . . ? Fe1 C2 H2 126.1 . . ? C2 C3 C4 107.7(4) . . ? C2 C3 Fe1 69.7(2) . . ? C4 C3 Fe1 69.6(2) . . ? C2 C3 H3 126.2 . . ? C4 C3 H3 126.2 . . ? Fe1 C3 H3 126.1 . . ? C3 C4 C5 107.3(5) . . ? C3 C4 Fe1 69.8(2) . . ? C5 C4 Fe1 69.7(2) . . ? C3 C4 H4 126.4 . . ? C5 C4 H4 126.4 . . ? Fe1 C4 H4 125.8 . . ? C1 C5 C4 108.4(4) . . ? C1 C5 Fe1 69.9(2) . . ? C4 C5 Fe1 69.4(2) . . ? C1 C5 H5 125.8 . . ? C4 C5 H5 125.8 . . ? Fe1 C5 H5 126.4 . . ? C7 C6 C10 108.3(3) . . ? C7 C6 Fe1 70.17(19) . . ? C10 C6 Fe1 69.37(18) . . ? C7 C6 H6 125.9 . . ? C10 C6 H6 125.9 . . ? Fe1 C6 H6 126.2 . . ? C8 C7 C6 108.0(3) . . ? C8 C7 Fe1 69.7(2) . . ? C6 C7 Fe1 69.06(18) . . ? C8 C7 H7 126.0 . . ? C6 C7 H7 126.0 . . ? Fe1 C7 H7 126.8 . . ? C7 C8 C9 109.3(3) . . ? C7 C8 Fe1 70.0(2) . . ? C9 C8 Fe1 69.54(19) . . ? C7 C8 H8 125.4 . . ? C9 C8 H8 125.4 . . ? Fe1 C8 H8 126.7 . . ? C8 C9 C10 107.1(3) . . ? C8 C9 Fe1 69.8(2) . . ? C10 C9 Fe1 68.92(18) . . ? C8 C9 H9 126.4 . . ? C10 C9 H9 126.4 . . ? Fe1 C9 H9 126.4 . . ? C11 C10 C6 126.2(3) . . ? C11 C10 C9 126.4(3) . . ? C6 C10 C9 107.4(3) . . ? C11 C10 Fe1 123.9(2) . . ? C6 C10 Fe1 69.40(17) . . ? C9 C10 Fe1 69.55(18) . . ? C12 C11 C10 176.7(4) . . ? C11 C12 C13 177.3(4) . . ? C14 C13 C18 119.3(3) . . ? C14 C13 C12 120.9(3) . . ? C18 C13 C12 119.8(3) . . ? C15 C14 C13 119.7(3) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C14 C15 C16 122.3(3) . . ? C14 C15 H15 118.9 . . ? C16 C15 H15 118.9 . . ? N1 C16 C15 122.0(3) . . ? N1 C16 C17 120.6(3) . . ? C15 C16 C17 117.2(3) . . ? O5 C17 C18 123.1(3) . . ? O5 C17 C16 116.1(3) . . ? C18 C17 C16 120.7(3) . . ? C17 C18 C13 120.7(3) . . ? C17 C18 H18 119.7 . . ? C13 C18 H18 119.7 . . ? N1 C19 C20 118.4(3) . . ? N1 C19 H19A 107.7 . . ? C20 C19 H19A 107.7 . . ? N1 C19 H19B 107.7 . . ? C20 C19 H19B 107.7 . . ? H19A C19 H19B 107.1 . . ? O1 C20 O2 123.9(4) . . ? O1 C20 C19 122.5(4) . . ? O2 C20 C19 113.6(3) . . ? O2 C21 C22 108.5(4) . . ? O2 C21 H21A 110.0 . . ? C22 C21 H21A 110.0 . . ? O2 C21 H21B 110.0 . . ? C22 C21 H21B 110.0 . . ? H21A C21 H21B 108.4 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N1 C23 C24 112.8(3) . . ? N1 C23 H23A 109.0 . . ? C24 C23 H23A 109.0 . . ? N1 C23 H23B 109.0 . . ? C24 C23 H23B 109.0 . . ? H23A C23 H23B 107.8 . . ? O3 C24 O4 124.2(3) . . ? O3 C24 C23 126.0(3) . . ? O4 C24 C23 109.7(3) . . ? O4 C25 C26 107.6(3) . . ? O4 C25 H25A 110.2 . . ? C26 C25 H25A 110.2 . . ? O4 C25 H25B 110.2 . . ? C26 C25 H25B 110.2 . . ? H25A C25 H25B 108.5 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O5 C27 C28 108.0(2) . . ? O5 C27 H27A 110.1 . . ? C28 C27 H27A 110.1 . . ? O5 C27 H27B 110.1 . . ? C28 C27 H27B 110.1 . . ? H27A C27 H27B 108.4 . . ? O6 C28 C27 106.7(3) . . ? O6 C28 H28A 110.4 . . ? C27 C28 H28A 110.4 . . ? O6 C28 H28B 110.4 . . ? C27 C28 H28B 110.4 . . ? H28A C28 H28B 108.6 . . ? O6 C29 C30 124.0(3) . . ? O6 C29 C34 115.5(3) . . ? C30 C29 C34 120.4(3) . . ? C31 C30 C29 121.2(3) . . ? C31 C30 H30 119.4 . . ? C29 C30 H30 119.4 . . ? C32 C31 C30 118.4(3) . . ? C32 C31 C43 121.4(3) . . ? C30 C31 C43 120.1(4) . . ? C31 C32 C33 120.9(3) . . ? C31 C32 H32 119.5 . . ? C33 C32 H32 119.5 . . ? C32 C33 C34 121.5(3) . . ? C32 C33 H33 119.3 . . ? C34 C33 H33 119.3 . . ? C33 C34 C29 117.6(3) . . ? C33 C34 N2 122.5(3) . . ? C29 C34 N2 119.7(3) . . ? N2 C35 C36 112.6(3) . . ? N2 C35 H35A 109.1 . . ? C36 C35 H35A 109.1 . . ? N2 C35 H35B 109.1 . . ? C36 C35 H35B 109.1 . . ? H35A C35 H35B 107.8 . . ? O9 C36 O10 124.1(3) . . ? O9 C36 C35 126.5(3) . . ? O10 C36 C35 109.4(3) . . ? O10 C37 C38 107.5(4) . . ? O10 C37 H37A 110.2 . . ? C38 C37 H37A 110.2 . . ? O10 C37 H37B 110.2 . . ? C38 C37 H37B 110.2 . . ? H37A C37 H37B 108.5 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N2 C39 C40 115.6(3) . . ? N2 C39 H39A 108.4 . . ? C40 C39 H39A 108.4 . . ? N2 C39 H39B 108.4 . . ? C40 C39 H39B 108.4 . . ? H39A C39 H39B 107.4 . . ? O7 C40 O8 124.8(3) . . ? O7 C40 C39 125.7(3) . . ? O8 C40 C39 109.5(3) . . ? O8 C41 C42 106.4(3) . . ? O8 C41 H41A 110.4 . . ? C42 C41 H41A 110.4 . . ? O8 C41 H41B 110.4 . . ? C42 C41 H41B 110.4 . . ? H41A C41 H41B 108.6 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C31 C43 H43A 109.5 . . ? C31 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C31 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? Cl2 C44 Cl1 113.2(4) . . ? Cl2 C44 H44A 108.9 . . ? Cl1 C44 H44A 108.9 . . ? Cl2 C44 H44B 108.9 . . ? Cl1 C44 H44B 108.9 . . ? H44A C44 H44B 107.8 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 31.74 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.841 _refine_diff_density_min -0.922 _refine_diff_density_rms 0.100 # Attachment 'web_deposit_cif_file_1_Boubekeur-Lecaque_1346659810.kxb25F2.cif' data_kxb25 _database_code_depnum_ccdc_archive 'CCDC 894008' #TrackingRef 'web_deposit_cif_file_1_Boubekeur-Lecaque_1346659810.kxb25F2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H56 Fe2 N2 O10' _chemical_formula_sum 'C54 H56 Fe2 N2 O10' _chemical_formula_weight 1004.71 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' 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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.9200(15) _cell_length_b 13.1070(14) _cell_length_c 18.3190(15) _cell_angle_alpha 69.343(8) _cell_angle_beta 77.511(7) _cell_angle_gamma 62.753(7) _cell_volume 2575.1(5) _cell_formula_units_Z 2 _cell_measurement_temperature 250(2) _cell_measurement_reflns_used 115 _cell_measurement_theta_min 3.62 _cell_measurement_theta_max 19.33 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.296 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1052 _exptl_absorpt_coefficient_mu 0.621 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8902 _exptl_absorpt_correction_T_max 0.9027 _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 250(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 KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 49165 _diffrn_reflns_av_R_equivalents 0.0446 _diffrn_reflns_av_sigmaI/netI 0.0633 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 30.00 _reflns_number_total 14955 _reflns_number_gt 6751 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^ > 2\s(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. A void with a volume of 263 A^3^ (10% of the cell volume) and which centre of gravity located at 0.5 0.0 0.0 was identified. In this void, the highest peaks observed in the last difference-Fourier maps indicate the presence of a solvent molecule but several attempts to modelize the disorder were unsuccessful. The size of the void and the results of the chemical analysis are in accordance and suggest the presence of one molecule of ethyl acetate per formula unit of the compound. ; _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^)+(0.0710P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14955 _refine_ls_number_parameters 617 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1139 _refine_ls_R_factor_gt 0.0501 _refine_ls_wR_factor_ref 0.1084 _refine_ls_wR_factor_gt 0.0851 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 1.11847(4) 0.24861(4) 0.62575(2) 0.03821(14) Uani 1 1 d . . . Fe2 Fe 0.70294(3) 1.11496(4) -0.40839(2) 0.03530(13) Uani 1 1 d . . . O1 O 0.3161(2) 0.5354(2) 0.39056(14) 0.0676(7) Uani 1 1 d . . . O2 O 0.42483(19) 0.41703(19) 0.31661(12) 0.0466(5) Uani 1 1 d . . . O3 O 0.5159(2) 0.7409(2) 0.10413(14) 0.0645(7) Uani 1 1 d . . . O4 O 0.55134(19) 0.6109(2) 0.03840(12) 0.0597(7) Uani 1 1 d . . . O5 O 0.76189(15) 0.53256(19) 0.17489(10) 0.0410(5) Uani 1 1 d . . . O6 O 0.85319(17) 0.50781(17) 0.02218(10) 0.0364(5) Uani 1 1 d . . . O7 O 0.7316(2) 0.2773(2) -0.10291(17) 0.0754(8) Uani 1 1 d . . . O8 O 0.8708(2) 0.0925(2) -0.08402(16) 0.0715(8) Uani 1 1 d . . . O9 O 0.9893(2) 0.2211(2) 0.10097(13) 0.0587(7) Uani 1 1 d . . . O10 O 0.82478(19) 0.2396(2) 0.17652(12) 0.0534(6) Uani 1 1 d . . . N1 N 0.54461(19) 0.5598(2) 0.24553(13) 0.0332(6) Uani 1 1 d . . . N2 N 0.8670(2) 0.3335(2) -0.03348(13) 0.0401(6) Uani 1 1 d . . . C1 C 1.0185(3) 0.3719(4) 0.6829(2) 0.0604(10) Uani 1 1 d . . . H1 H 0.9995 0.4579 0.6630 0.072 Uiso 1 1 calc R . . C2 C 1.1169(4) 0.2814(4) 0.7258(2) 0.0661(11) Uani 1 1 d . . . H2 H 1.1775 0.2944 0.7405 0.079 Uiso 1 1 calc R . . C3 C 1.1122(4) 0.1708(4) 0.7427(2) 0.0722(12) Uani 1 1 d . . . H3 H 1.1687 0.0926 0.7714 0.087 Uiso 1 1 calc R . . C4 C 1.0107(4) 0.1928(4) 0.7112(2) 0.0700(12) Uani 1 1 d . . . H4 H 0.9846 0.1321 0.7138 0.084 Uiso 1 1 calc R . . C5 C 0.9541(3) 0.3171(4) 0.6749(2) 0.0568(10) Uani 1 1 d . . . H5 H 0.8820 0.3575 0.6476 0.068 Uiso 1 1 calc R . . C6 C 1.1630(3) 0.3416(4) 0.51930(18) 0.0538(9) Uani 1 1 d . . . H6 H 1.1365 0.4289 0.4995 0.065 Uiso 1 1 calc R . . C7 C 1.2625(3) 0.2597(5) 0.5616(2) 0.0758(13) Uani 1 1 d . . . H7 H 1.3172 0.2806 0.5764 0.091 Uiso 1 1 calc R . . C8 C 1.2697(3) 0.1454(4) 0.5794(2) 0.0766(14) Uani 1 1 d . . . H8 H 1.3303 0.0719 0.6091 0.092 Uiso 1 1 calc R . . C9 C 1.1743(3) 0.1512(3) 0.5491(2) 0.0608(10) Uani 1 1 d . . . H9 H 1.1576 0.0834 0.5534 0.073 Uiso 1 1 calc R . . C10 C 1.1082(3) 0.2745(3) 0.51050(16) 0.0415(8) Uani 1 1 d . . . C11 C 1.0088(3) 0.3224(3) 0.46692(16) 0.0363(7) Uani 1 1 d . . . C12 C 0.9305(3) 0.3630(3) 0.42762(16) 0.0349(7) Uani 1 1 d . . . C13 C 0.8321(2) 0.4125(2) 0.38123(15) 0.0325(7) Uani 1 1 d . . . C14 C 0.7217(3) 0.4334(3) 0.41567(17) 0.0386(7) Uani 1 1 d . . . H14 H 0.7095 0.4161 0.4698 0.046 Uiso 1 1 calc R . . C15 C 0.6283(2) 0.4799(3) 0.37052(15) 0.0352(7) Uani 1 1 d . . . H15 H 0.5546 0.4920 0.3954 0.042 Uiso 1 1 calc R . . C16 C 0.6401(2) 0.5091(2) 0.28960(15) 0.0292(6) Uani 1 1 d . . . C17 C 0.7529(2) 0.4936(2) 0.25469(14) 0.0295(6) Uani 1 1 d . . . C18 C 0.8470(2) 0.4426(2) 0.30041(16) 0.0331(7) Uani 1 1 d . . . H18 H 0.9214 0.4284 0.2763 0.040 Uiso 1 1 calc R . . C19 C 0.4297(2) 0.6057(3) 0.28207(17) 0.0379(7) Uani 1 1 d . . . H19A H 0.3759 0.6581 0.2412 0.046 Uiso 1 1 calc R . . H19B H 0.4281 0.6549 0.3117 0.046 Uiso 1 1 calc R . . C20 C 0.3842(2) 0.5161(3) 0.33568(17) 0.0388(7) Uani 1 1 d . . . C21 C 0.3792(3) 0.3294(3) 0.3654(2) 0.0588(10) Uani 1 1 d . . . H21A H 0.2950 0.3642 0.3640 0.071 Uiso 1 1 calc R . . H21B H 0.3982 0.3043 0.4191 0.071 Uiso 1 1 calc R . . C22 C 0.4328(5) 0.2276(4) 0.3342(3) 0.1016(17) Uani 1 1 d . . . H22A H 0.4077 0.2520 0.2827 0.152 Uiso 1 1 calc R . . H22B H 0.4099 0.1651 0.3676 0.152 Uiso 1 1 calc R . . H22C H 0.5161 0.1982 0.3317 0.152 Uiso 1 1 calc R . . C23 C 0.5516(3) 0.5355(3) 0.17333(15) 0.0362(7) Uani 1 1 d . . . H23A H 0.4909 0.5102 0.1756 0.043 Uiso 1 1 calc R . . H23B H 0.6263 0.4700 0.1676 0.043 Uiso 1 1 calc R . . C24 C 0.5382(3) 0.6429(4) 0.10319(18) 0.0463(9) Uani 1 1 d . . . C25 C 0.5222(4) 0.7088(4) -0.0333(2) 0.0816(14) Uani 1 1 d . . . H25A H 0.5786 0.7433 -0.0476 0.098 Uiso 1 1 calc R . . H25B H 0.4455 0.7712 -0.0266 0.098 Uiso 1 1 calc R . . C26 C 0.5236(4) 0.6590(5) -0.0950(2) 0.108(2) Uani 1 1 d . . . H26A H 0.6018 0.6038 -0.1051 0.163 Uiso 1 1 calc R . . H26B H 0.4966 0.7232 -0.1421 0.163 Uiso 1 1 calc R . . H26C H 0.4735 0.6178 -0.0778 0.163 Uiso 1 1 calc R . . C27 C 0.8676(2) 0.5395(3) 0.13738(15) 0.0349(7) Uani 1 1 d . . . H27A H 0.9310 0.4599 0.1470 0.042 Uiso 1 1 calc R . . H27B H 0.8863 0.5880 0.1575 0.042 Uiso 1 1 calc R . . C28 C 0.8518(3) 0.5949(3) 0.05213(15) 0.0351(7) Uani 1 1 d . . . H28A H 0.7781 0.6653 0.0431 0.042 Uiso 1 1 calc R . . H28B H 0.9143 0.6192 0.0262 0.042 Uiso 1 1 calc R . . C29 C 0.8418(2) 0.5378(3) -0.05610(15) 0.0317(7) Uani 1 1 d . . . C30 C 0.8298(2) 0.6493(3) -0.10661(16) 0.0360(7) Uani 1 1 d . . . H30 H 0.8233 0.7085 -0.0870 0.043 Uiso 1 1 calc R . . C31 C 0.8273(2) 0.6733(3) -0.18712(17) 0.0393(7) Uani 1 1 d . . . C32 C 0.8355(3) 0.5848(3) -0.21447(17) 0.0437(8) Uani 1 1 d . . . H32 H 0.8348 0.5994 -0.2679 0.052 Uiso 1 1 calc R . . C33 C 0.8450(2) 0.4738(3) -0.16357(16) 0.0403(7) Uani 1 1 d . . . H33 H 0.8488 0.4159 -0.1835 0.048 Uiso 1 1 calc R . . C34 C 0.8490(2) 0.4476(3) -0.08373(15) 0.0329(7) Uani 1 1 d . . . C35 C 0.8047(2) 0.3176(3) 0.04233(16) 0.0384(7) Uani 1 1 d . . . H35A H 0.7622 0.2711 0.0461 0.046 Uiso 1 1 calc R . . H35B H 0.7484 0.3955 0.0477 0.046 Uiso 1 1 calc R . . C36 C 0.8859(3) 0.2546(3) 0.10843(18) 0.0424(8) Uani 1 1 d . . . C37 C 0.8931(3) 0.1751(3) 0.24527(19) 0.0653(11) Uani 1 1 d . . . H37A H 0.9329 0.2200 0.2494 0.078 Uiso 1 1 calc R . . H37B H 0.9513 0.0973 0.2410 0.078 Uiso 1 1 calc R . . C38 C 0.8132(4) 0.1601(4) 0.3150(2) 0.0920(15) Uani 1 1 d . . . H38A H 0.7598 0.2374 0.3211 0.138 Uiso 1 1 calc R . . H38B H 0.8574 0.1127 0.3604 0.138 Uiso 1 1 calc R . . H38C H 0.7703 0.1205 0.3088 0.138 Uiso 1 1 calc R . . C39 C 0.9153(3) 0.2312(3) -0.06222(18) 0.0451(8) Uani 1 1 d . . . H39A H 0.9603 0.1612 -0.0220 0.054 Uiso 1 1 calc R . . H39B H 0.9688 0.2433 -0.1071 0.054 Uiso 1 1 calc R . . C40 C 0.8273(3) 0.2051(3) -0.08587(18) 0.0473(8) Uani 1 1 d . . . C41 C 0.7952(4) 0.0523(4) -0.1039(3) 0.0946(16) Uani 1 1 d . . . H41A H 0.7298 0.1213 -0.1307 0.114 Uiso 1 1 calc R . . H41B H 0.8383 0.0033 -0.1389 0.114 Uiso 1 1 calc R . . C42 C 0.7512(5) -0.0191(5) -0.0316(4) 0.123(2) Uani 1 1 d . . . H42A H 0.8157 -0.0902 -0.0070 0.185 Uiso 1 1 calc R . . H42B H 0.6983 -0.0412 -0.0453 0.185 Uiso 1 1 calc R . . H42C H 0.7113 0.0284 0.0038 0.185 Uiso 1 1 calc R . . C43 C 0.8223(3) 0.7850(3) -0.23947(17) 0.0446(8) Uani 1 1 d . . . C44 C 0.8226(3) 0.8755(3) -0.28286(18) 0.0442(8) Uani 1 1 d . . . C45 C 0.8298(3) 0.9815(3) -0.33810(17) 0.0422(8) Uani 1 1 d . . . C46 C 0.7976(3) 1.0940(3) -0.32520(19) 0.0468(8) Uani 1 1 d . . . H46 H 0.7662 1.1130 -0.2756 0.056 Uiso 1 1 calc R . . C47 C 0.8184(3) 1.1727(3) -0.39592(19) 0.0478(8) Uani 1 1 d . . . H47 H 0.8036 1.2563 -0.4044 0.057 Uiso 1 1 calc R . . C48 C 0.8632(3) 1.1110(3) -0.45228(19) 0.0467(8) Uani 1 1 d . . . H48 H 0.8842 1.1448 -0.5072 0.056 Uiso 1 1 calc R . . C49 C 0.8708(2) 0.9932(3) -0.41782(18) 0.0419(8) Uani 1 1 d . . . H49 H 0.8990 0.9309 -0.4441 0.050 Uiso 1 1 calc R . . C50 C 0.5612(3) 1.0764(3) -0.3780(2) 0.0531(9) Uani 1 1 d . . . H50 H 0.5549 1.0085 -0.3351 0.064 Uiso 1 1 calc R . . C51 C 0.5311(3) 1.1906(3) -0.3726(2) 0.0488(8) Uani 1 1 d . . . H51 H 0.5001 1.2167 -0.3253 0.059 Uiso 1 1 calc R . . C52 C 0.5545(3) 1.2603(3) -0.4463(2) 0.0508(9) Uani 1 1 d . . . H52 H 0.5422 1.3442 -0.4596 0.061 Uiso 1 1 calc R . . C53 C 0.5975(3) 1.1908(4) -0.4977(2) 0.0560(10) Uani 1 1 d . . . H53 H 0.6205 1.2173 -0.5533 0.067 Uiso 1 1 calc R . . C54 C 0.6025(3) 1.0754(3) -0.4557(2) 0.0570(10) Uani 1 1 d . . . H54 H 0.6290 1.0076 -0.4767 0.068 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0356(3) 0.0499(3) 0.0333(3) -0.0144(2) -0.00623(18) -0.0179(2) Fe2 0.0308(2) 0.0388(3) 0.0361(3) -0.00749(19) -0.00631(18) -0.0151(2) O1 0.0496(15) 0.0832(18) 0.0656(17) -0.0355(14) 0.0251(13) -0.0263(14) O2 0.0552(14) 0.0525(14) 0.0413(13) -0.0167(11) 0.0063(10) -0.0321(12) O3 0.0732(19) 0.0580(16) 0.0592(17) -0.0022(13) -0.0162(13) -0.0308(15) O4 0.0487(15) 0.0835(17) 0.0310(13) -0.0159(12) -0.0048(10) -0.0141(13) O5 0.0269(11) 0.0734(15) 0.0230(11) -0.0075(10) -0.0004(8) -0.0266(11) O6 0.0470(13) 0.0397(11) 0.0224(11) -0.0065(9) -0.0017(8) -0.0202(10) O7 0.0499(17) 0.0537(16) 0.124(2) -0.0305(16) -0.0305(16) -0.0090(14) O8 0.0718(18) 0.0432(15) 0.101(2) -0.0278(14) -0.0338(15) -0.0080(13) O9 0.0424(15) 0.0700(16) 0.0540(15) -0.0120(13) -0.0070(11) -0.0183(13) O10 0.0528(14) 0.0617(15) 0.0330(13) -0.0023(11) 0.0015(10) -0.0238(12) N1 0.0270(13) 0.0468(15) 0.0268(13) -0.0115(11) -0.0018(10) -0.0156(12) N2 0.0435(15) 0.0407(15) 0.0332(14) -0.0108(12) 0.0022(11) -0.0173(13) C1 0.067(3) 0.069(2) 0.059(2) -0.037(2) 0.0133(19) -0.033(2) C2 0.081(3) 0.107(3) 0.041(2) -0.035(2) 0.0067(19) -0.060(3) C3 0.087(3) 0.092(3) 0.032(2) -0.003(2) -0.0100(19) -0.040(3) C4 0.088(3) 0.090(3) 0.054(2) -0.015(2) 0.010(2) -0.066(3) C5 0.047(2) 0.086(3) 0.050(2) -0.032(2) 0.0119(16) -0.035(2) C6 0.043(2) 0.083(3) 0.041(2) -0.0109(18) 0.0016(15) -0.038(2) C7 0.038(2) 0.146(4) 0.054(2) -0.037(3) 0.0025(17) -0.043(3) C8 0.041(2) 0.101(3) 0.061(3) -0.043(3) -0.0204(18) 0.013(2) C9 0.057(2) 0.061(2) 0.054(2) -0.0328(19) -0.0213(18) 0.0024(19) C10 0.0336(17) 0.060(2) 0.0288(16) -0.0160(15) -0.0030(13) -0.0154(16) C11 0.0361(17) 0.0475(18) 0.0265(16) -0.0101(14) -0.0014(13) -0.0192(15) C12 0.0393(17) 0.0437(17) 0.0246(15) -0.0043(13) -0.0029(13) -0.0235(15) C13 0.0351(17) 0.0378(16) 0.0266(16) -0.0045(13) -0.0061(12) -0.0187(14) C14 0.0401(18) 0.0492(18) 0.0260(16) -0.0082(14) -0.0018(13) -0.0204(16) C15 0.0329(16) 0.0464(18) 0.0265(16) -0.0111(13) 0.0036(12) -0.0188(14) C16 0.0295(15) 0.0279(15) 0.0311(16) -0.0096(12) -0.0030(12) -0.0116(13) C17 0.0328(16) 0.0368(16) 0.0214(15) -0.0058(12) -0.0008(11) -0.0190(13) C18 0.0311(16) 0.0412(17) 0.0320(16) -0.0115(13) -0.0015(12) -0.0189(14) C19 0.0304(16) 0.0428(18) 0.0393(18) -0.0165(14) -0.0055(13) -0.0095(14) C20 0.0235(16) 0.053(2) 0.0382(18) -0.0151(16) -0.0032(13) -0.0125(15) C21 0.070(3) 0.071(3) 0.048(2) -0.0014(19) -0.0116(18) -0.047(2) C22 0.153(5) 0.077(3) 0.099(4) -0.022(3) -0.016(3) -0.068(3) C23 0.0329(16) 0.0502(18) 0.0306(16) -0.0150(14) -0.0031(12) -0.0188(15) C24 0.0307(17) 0.070(3) 0.0347(19) -0.0082(18) -0.0076(13) -0.0208(18) C25 0.065(3) 0.117(4) 0.034(2) 0.000(2) -0.0079(18) -0.028(3) C26 0.067(3) 0.191(6) 0.043(3) -0.037(3) -0.012(2) -0.029(3) C27 0.0288(16) 0.0542(19) 0.0282(16) -0.0113(14) 0.0010(12) -0.0245(15) C28 0.0355(17) 0.0416(17) 0.0286(16) -0.0072(13) 0.0021(12) -0.0205(14) C29 0.0245(15) 0.0402(17) 0.0256(16) -0.0081(13) 0.0014(11) -0.0119(13) C30 0.0331(16) 0.0406(17) 0.0304(17) -0.0103(13) 0.0018(12) -0.0140(14) C31 0.0294(16) 0.0499(19) 0.0316(17) -0.0045(15) -0.0011(12) -0.0167(15) C32 0.0382(18) 0.058(2) 0.0286(17) -0.0044(16) -0.0077(13) -0.0185(16) C33 0.0350(17) 0.053(2) 0.0359(18) -0.0155(15) -0.0007(13) -0.0193(15) C34 0.0254(15) 0.0431(17) 0.0277(16) -0.0075(13) 0.0005(11) -0.0153(14) C35 0.0341(17) 0.0404(17) 0.0390(18) -0.0062(14) -0.0004(13) -0.0189(14) C36 0.049(2) 0.0392(18) 0.0379(19) -0.0052(14) -0.0028(15) -0.0219(17) C37 0.083(3) 0.057(2) 0.042(2) -0.0017(18) -0.0160(19) -0.022(2) C38 0.127(4) 0.088(3) 0.046(3) 0.001(2) -0.002(2) -0.049(3) C39 0.0418(19) 0.0437(19) 0.0444(19) -0.0137(15) -0.0032(14) -0.0126(16) C40 0.048(2) 0.047(2) 0.043(2) -0.0157(16) -0.0043(15) -0.0141(18) C41 0.093(4) 0.066(3) 0.138(5) -0.051(3) -0.052(3) -0.009(3) C42 0.087(4) 0.115(4) 0.176(6) -0.048(4) -0.007(4) -0.045(4) C43 0.0378(18) 0.054(2) 0.0278(17) -0.0014(16) -0.0044(13) -0.0144(16) C44 0.0389(19) 0.048(2) 0.0367(19) -0.0017(16) -0.0096(14) -0.0157(16) C45 0.0355(17) 0.049(2) 0.0358(18) -0.0021(15) -0.0115(13) -0.0164(16) C46 0.0421(19) 0.060(2) 0.0411(19) -0.0149(17) -0.0119(14) -0.0198(17) C47 0.050(2) 0.050(2) 0.051(2) -0.0070(17) -0.0148(16) -0.0283(17) C48 0.0354(18) 0.054(2) 0.046(2) -0.0027(17) -0.0040(14) -0.0233(16) C49 0.0311(17) 0.0460(19) 0.0426(19) -0.0090(15) -0.0066(13) -0.0124(15) C50 0.042(2) 0.054(2) 0.073(3) -0.0180(19) -0.0029(17) -0.0283(18) C51 0.0339(18) 0.062(2) 0.054(2) -0.0251(18) 0.0057(15) -0.0213(17) C52 0.0381(19) 0.046(2) 0.060(2) -0.0095(18) -0.0104(16) -0.0118(16) C53 0.040(2) 0.080(3) 0.044(2) -0.013(2) -0.0159(16) -0.0197(19) C54 0.041(2) 0.066(3) 0.082(3) -0.041(2) -0.0123(18) -0.0193(19) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C8 2.010(4) . ? Fe1 C7 2.012(4) . ? Fe1 C3 2.024(3) . ? Fe1 C2 2.020(3) . ? Fe1 C4 2.025(4) . ? Fe1 C1 2.018(4) . ? Fe1 C9 2.026(3) . ? Fe1 C6 2.025(3) . ? Fe1 C5 2.031(3) . ? Fe1 C10 2.041(3) . ? Fe2 C46 2.024(3) . ? Fe2 C45 2.026(3) . ? Fe2 C52 2.021(3) . ? Fe2 C54 2.031(3) . ? Fe2 C49 2.036(3) . ? Fe2 C53 2.024(3) . ? Fe2 C51 2.039(3) . ? Fe2 C50 2.031(3) . ? Fe2 C48 2.037(3) . ? Fe2 C47 2.039(3) . ? O1 C20 1.201(3) . ? O2 C20 1.303(4) . ? O2 C21 1.461(4) . ? O3 C24 1.186(4) . ? O4 C24 1.346(4) . ? O4 C25 1.448(4) . ? O5 C17 1.366(3) . ? O5 C27 1.418(3) . ? O6 C29 1.369(3) . ? O6 C28 1.423(3) . ? O7 C40 1.187(4) . ? O8 C40 1.307(4) . ? O8 C41 1.458(5) . ? O9 C36 1.192(4) . ? O10 C36 1.327(4) . ? O10 C37 1.458(4) . ? N1 C16 1.385(3) . ? N1 C19 1.432(3) . ? N1 C23 1.442(3) . ? N2 C34 1.393(4) . ? N2 C39 1.433(4) . ? N2 C35 1.444(3) . ? C1 C5 1.379(5) . ? C1 C2 1.427(5) . ? C1 H1 0.9800 . ? C2 C3 1.398(5) . ? C2 H2 0.9800 . ? C3 C4 1.415(5) . ? C3 H3 0.9800 . ? C4 C5 1.409(5) . ? C4 H4 0.9800 . ? C5 H5 0.9800 . ? C6 C7 1.409(5) . ? C6 C10 1.422(5) . ? C6 H6 0.9800 . ? C7 C8 1.379(6) . ? C7 H7 0.9800 . ? C8 C9 1.419(5) . ? C8 H8 0.9800 . ? C9 C10 1.426(4) . ? C9 H9 0.9800 . ? C10 C11 1.425(4) . ? C11 C12 1.173(4) . ? C12 C13 1.443(4) . ? C13 C14 1.372(4) . ? C13 C18 1.385(4) . ? C14 C15 1.384(4) . ? C14 H14 0.9300 . ? C15 C16 1.386(4) . ? C15 H15 0.9300 . ? C16 C17 1.411(4) . ? C17 C18 1.388(4) . ? C18 H18 0.9300 . ? C19 C20 1.503(4) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C21 C22 1.452(5) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C24 1.504(4) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C25 C26 1.485(6) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C28 1.486(4) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.384(4) . ? C29 C34 1.402(4) . ? C30 C31 1.400(4) . ? C30 H30 0.9300 . ? C31 C32 1.371(4) . ? C31 C43 1.421(4) . ? C32 C33 1.390(4) . ? C32 H32 0.9300 . ? C33 C34 1.386(4) . ? C33 H33 0.9300 . ? C35 C36 1.516(4) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C37 C38 1.475(5) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 C40 1.507(4) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C41 C42 1.496(6) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 C44 1.174(4) . ? C44 C45 1.432(4) . ? C45 C49 1.421(4) . ? C45 C46 1.429(4) . ? C46 C47 1.406(4) . ? C46 H46 0.9800 . ? C47 C48 1.399(5) . ? C47 H47 0.9800 . ? C48 C49 1.412(4) . ? C48 H48 0.9800 . ? C49 H49 0.9800 . ? C50 C51 1.399(5) . ? C50 C54 1.410(5) . ? C50 H50 0.9800 . ? C51 C52 1.398(4) . ? C51 H51 0.9800 . ? C52 C53 1.394(5) . ? C52 H52 0.9800 . ? C53 C54 1.413(5) . ? C53 H53 0.9800 . ? C54 H54 0.9800 . ? 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 C8 Fe1 C7 40.12(17) . . ? C8 Fe1 C3 107.99(17) . . ? C7 Fe1 C3 123.95(17) . . ? C8 Fe1 C2 119.62(16) . . ? C7 Fe1 C2 105.78(17) . . ? C3 Fe1 C2 40.45(15) . . ? C8 Fe1 C4 127.2(2) . . ? C7 Fe1 C4 162.40(18) . . ? C3 Fe1 C4 40.90(15) . . ? C2 Fe1 C4 68.17(16) . . ? C8 Fe1 C1 154.37(18) . . ? C7 Fe1 C1 119.11(19) . . ? C3 Fe1 C1 68.87(17) . . ? C2 Fe1 C1 41.38(15) . . ? C4 Fe1 C1 68.05(16) . . ? C8 Fe1 C9 41.15(15) . . ? C7 Fe1 C9 68.80(19) . . ? C3 Fe1 C9 121.71(17) . . ? C2 Fe1 C9 155.73(16) . . ? C4 Fe1 C9 109.50(17) . . ? C1 Fe1 C9 162.15(15) . . ? C8 Fe1 C6 68.37(18) . . ? C7 Fe1 C6 40.87(14) . . ? C3 Fe1 C6 160.26(16) . . ? C2 Fe1 C6 123.07(16) . . ? C4 Fe1 C6 156.31(15) . . ? C1 Fe1 C6 105.57(16) . . ? C9 Fe1 C6 69.20(16) . . ? C8 Fe1 C5 164.7(2) . . ? C7 Fe1 C5 154.3(2) . . ? C3 Fe1 C5 68.60(16) . . ? C2 Fe1 C5 68.16(15) . . ? C4 Fe1 C5 40.64(15) . . ? C1 Fe1 C5 39.82(14) . . ? C9 Fe1 C5 126.88(15) . . ? C6 Fe1 C5 120.00(15) . . ? C8 Fe1 C10 68.60(13) . . ? C7 Fe1 C10 68.62(14) . . ? C3 Fe1 C10 157.60(16) . . ? C2 Fe1 C10 160.94(16) . . ? C4 Fe1 C10 122.41(15) . . ? C1 Fe1 C10 124.07(14) . . ? C9 Fe1 C10 41.06(13) . . ? C6 Fe1 C10 40.95(13) . . ? C5 Fe1 C10 108.51(13) . . ? C46 Fe2 C45 41.33(13) . . ? C46 Fe2 C52 124.92(14) . . ? C45 Fe2 C52 161.82(14) . . ? C46 Fe2 C54 155.64(15) . . ? C45 Fe2 C54 119.99(15) . . ? C52 Fe2 C54 68.22(14) . . ? C46 Fe2 C49 68.80(13) . . ? C45 Fe2 C49 40.95(12) . . ? C52 Fe2 C49 156.24(13) . . ? C54 Fe2 C49 107.49(14) . . ? C46 Fe2 C53 161.85(15) . . ? C45 Fe2 C53 155.81(15) . . ? C52 Fe2 C53 40.32(13) . . ? C54 Fe2 C53 40.78(14) . . ? C49 Fe2 C53 121.15(14) . . ? C46 Fe2 C51 107.54(14) . . ? C45 Fe2 C51 124.64(13) . . ? C52 Fe2 C51 40.29(13) . . ? C54 Fe2 C51 68.07(14) . . ? C49 Fe2 C51 161.84(13) . . ? C53 Fe2 C51 67.83(14) . . ? C46 Fe2 C50 120.54(14) . . ? C45 Fe2 C50 106.97(13) . . ? C52 Fe2 C50 67.83(14) . . ? C54 Fe2 C50 40.60(14) . . ? C49 Fe2 C50 125.09(14) . . ? C53 Fe2 C50 68.09(14) . . ? C51 Fe2 C50 40.21(13) . . ? C46 Fe2 C48 67.87(14) . . ? C45 Fe2 C48 68.41(12) . . ? C52 Fe2 C48 121.72(13) . . ? C54 Fe2 C48 125.88(15) . . ? C49 Fe2 C48 40.56(12) . . ? C53 Fe2 C48 108.81(14) . . ? C51 Fe2 C48 156.14(14) . . ? C50 Fe2 C48 162.58(15) . . ? C46 Fe2 C47 40.48(12) . . ? C45 Fe2 C47 68.85(13) . . ? C52 Fe2 C47 108.25(14) . . ? C54 Fe2 C47 162.50(15) . . ? C49 Fe2 C47 68.41(14) . . ? C53 Fe2 C47 125.53(14) . . ? C51 Fe2 C47 121.13(15) . . ? C50 Fe2 C47 155.61(15) . . ? C48 Fe2 C47 40.15(13) . . ? C20 O2 C21 115.6(3) . . ? C24 O4 C25 115.4(3) . . ? C17 O5 C27 118.2(2) . . ? C29 O6 C28 118.5(2) . . ? C40 O8 C41 117.2(3) . . ? C36 O10 C37 115.4(3) . . ? C16 N1 C19 119.2(2) . . ? C16 N1 C23 122.4(2) . . ? C19 N1 C23 115.4(2) . . ? C34 N2 C39 121.3(2) . . ? C34 N2 C35 121.1(2) . . ? C39 N2 C35 114.5(2) . . ? C5 C1 C2 108.0(3) . . ? C5 C1 Fe1 70.6(2) . . ? C2 C1 Fe1 69.4(2) . . ? C5 C1 H1 126.0 . . ? C2 C1 H1 126.0 . . ? Fe1 C1 H1 126.0 . . ? C3 C2 C1 108.0(4) . . ? C3 C2 Fe1 69.9(2) . . ? C1 C2 Fe1 69.3(2) . . ? C3 C2 H2 126.0 . . ? C1 C2 H2 126.0 . . ? Fe1 C2 H2 126.0 . . ? C2 C3 C4 107.4(4) . . ? C2 C3 Fe1 69.6(2) . . ? C4 C3 Fe1 69.6(2) . . ? C2 C3 H3 126.3 . . ? C4 C3 H3 126.3 . . ? Fe1 C3 H3 126.3 . . ? C5 C4 C3 108.1(4) . . ? C5 C4 Fe1 69.9(2) . . ? C3 C4 Fe1 69.5(2) . . ? C5 C4 H4 126.0 . . ? C3 C4 H4 126.0 . . ? Fe1 C4 H4 126.0 . . ? C1 C5 C4 108.5(4) . . ? C1 C5 Fe1 69.6(2) . . ? C4 C5 Fe1 69.5(2) . . ? C1 C5 H5 125.7 . . ? C4 C5 H5 125.7 . . ? Fe1 C5 H5 125.7 . . ? C7 C6 C10 107.6(4) . . ? C7 C6 Fe1 69.1(2) . . ? C10 C6 Fe1 70.12(17) . . ? C7 C6 H6 126.2 . . ? C10 C6 H6 126.2 . . ? Fe1 C6 H6 126.2 . . ? C8 C7 C6 108.8(4) . . ? C8 C7 Fe1 69.9(2) . . ? C6 C7 Fe1 70.07(19) . . ? C8 C7 H7 125.6 . . ? C6 C7 H7 125.6 . . ? Fe1 C7 H7 125.6 . . ? C7 C8 C9 109.2(3) . . ? C7 C8 Fe1 70.0(2) . . ? C9 C8 Fe1 70.0(2) . . ? C7 C8 H8 125.4 . . ? C9 C8 H8 125.4 . . ? Fe1 C8 H8 125.4 . . ? C8 C9 C10 106.7(4) . . ? C8 C9 Fe1 68.8(2) . . ? C10 C9 Fe1 70.03(18) . . ? C8 C9 H9 126.6 . . ? C10 C9 H9 126.6 . . ? Fe1 C9 H9 126.6 . . ? C11 C10 C9 126.6(3) . . ? C11 C10 C6 125.6(3) . . ? C9 C10 C6 107.7(3) . . ? C11 C10 Fe1 130.2(2) . . ? C9 C10 Fe1 68.91(17) . . ? C6 C10 Fe1 68.92(17) . . ? C12 C11 C10 176.6(3) . . ? C11 C12 C13 178.4(3) . . ? C14 C13 C18 118.5(2) . . ? C14 C13 C12 121.1(3) . . ? C18 C13 C12 120.4(3) . . ? C13 C14 C15 120.5(3) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? C14 C15 C16 122.6(3) . . ? C14 C15 H15 118.7 . . ? C16 C15 H15 118.7 . . ? C15 C16 N1 121.5(2) . . ? C15 C16 C17 116.3(2) . . ? N1 C16 C17 122.0(2) . . ? O5 C17 C18 123.4(2) . . ? O5 C17 C16 116.0(2) . . ? C18 C17 C16 120.7(2) . . ? C17 C18 C13 121.3(3) . . ? C17 C18 H18 119.4 . . ? C13 C18 H18 119.4 . . ? N1 C19 C20 117.4(2) . . ? N1 C19 H19A 107.9 . . ? C20 C19 H19A 107.9 . . ? N1 C19 H19B 107.9 . . ? C20 C19 H19B 107.9 . . ? H19A C19 H19B 107.2 . . ? O1 C20 O2 123.8(3) . . ? O1 C20 C19 122.4(3) . . ? O2 C20 C19 113.8(3) . . ? O2 C21 C22 107.2(3) . . ? O2 C21 H21A 110.3 . . ? C22 C21 H21A 110.3 . . ? O2 C21 H21B 110.3 . . ? C22 C21 H21B 110.3 . . ? H21A C21 H21B 108.5 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N1 C23 C24 112.5(3) . . ? N1 C23 H23A 109.1 . . ? C24 C23 H23A 109.1 . . ? N1 C23 H23B 109.1 . . ? C24 C23 H23B 109.1 . . ? H23A C23 H23B 107.8 . . ? O3 C24 O4 125.1(3) . . ? O3 C24 C23 126.3(3) . . ? O4 C24 C23 108.6(3) . . ? O4 C25 C26 107.3(4) . . ? O4 C25 H25A 110.2 . . ? C26 C25 H25A 110.2 . . ? O4 C25 H25B 110.2 . . ? C26 C25 H25B 110.2 . . ? H25A C25 H25B 108.5 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O5 C27 C28 107.9(2) . . ? O5 C27 H27A 110.1 . . ? C28 C27 H27A 110.1 . . ? O5 C27 H27B 110.1 . . ? C28 C27 H27B 110.1 . . ? H27A C27 H27B 108.4 . . ? O6 C28 C27 107.7(2) . . ? O6 C28 H28A 110.2 . . ? C27 C28 H28A 110.2 . . ? O6 C28 H28B 110.2 . . ? C27 C28 H28B 110.2 . . ? H28A C28 H28B 108.5 . . ? O6 C29 C30 122.2(3) . . ? O6 C29 C34 116.6(2) . . ? C30 C29 C34 121.2(3) . . ? C29 C30 C31 120.3(3) . . ? C29 C30 H30 119.8 . . ? C31 C30 H30 119.8 . . ? C32 C31 C30 118.7(3) . . ? C32 C31 C43 120.9(3) . . ? C30 C31 C43 120.3(3) . . ? C31 C32 C33 121.0(3) . . ? C31 C32 H32 119.5 . . ? C33 C32 H32 119.5 . . ? C32 C33 C34 121.3(3) . . ? C32 C33 H33 119.3 . . ? C34 C33 H33 119.3 . . ? C33 C34 N2 121.2(3) . . ? C33 C34 C29 117.5(3) . . ? N2 C34 C29 121.2(2) . . ? N2 C35 C36 112.1(2) . . ? N2 C35 H35A 109.2 . . ? C36 C35 H35A 109.2 . . ? N2 C35 H35B 109.2 . . ? C36 C35 H35B 109.2 . . ? H35A C35 H35B 107.9 . . ? O9 C36 O10 124.7(3) . . ? O9 C36 C35 125.6(3) . . ? O10 C36 C35 109.7(3) . . ? O10 C37 C38 108.3(3) . . ? O10 C37 H37A 110.0 . . ? C38 C37 H37A 110.0 . . ? O10 C37 H37B 110.0 . . ? C38 C37 H37B 110.0 . . ? H37A C37 H37B 108.4 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N2 C39 C40 115.1(3) . . ? N2 C39 H39A 108.5 . . ? C40 C39 H39A 108.5 . . ? N2 C39 H39B 108.5 . . ? C40 C39 H39B 108.5 . . ? H39A C39 H39B 107.5 . . ? O7 C40 O8 125.3(3) . . ? O7 C40 C39 124.2(3) . . ? O8 C40 C39 110.5(3) . . ? C42 C41 O8 110.4(4) . . ? C42 C41 H41A 109.6 . . ? O8 C41 H41A 109.6 . . ? C42 C41 H41B 109.6 . . ? O8 C41 H41B 109.6 . . ? H41A C41 H41B 108.1 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 C31 177.5(3) . . ? C43 C44 C45 176.4(4) . . ? C49 C45 C46 107.2(3) . . ? C49 C45 C44 125.0(3) . . ? C46 C45 C44 127.8(3) . . ? C49 C45 Fe2 69.92(16) . . ? C46 C45 Fe2 69.29(16) . . ? C44 C45 Fe2 125.6(2) . . ? C47 C46 C45 108.3(3) . . ? C47 C46 Fe2 70.32(17) . . ? C45 C46 Fe2 69.38(17) . . ? C47 C46 H46 125.8 . . ? C45 C46 H46 125.8 . . ? Fe2 C46 H46 125.8 . . ? C48 C47 C46 107.9(3) . . ? C48 C47 Fe2 69.85(18) . . ? C46 C47 Fe2 69.20(18) . . ? C48 C47 H47 126.1 . . ? C46 C47 H47 126.1 . . ? Fe2 C47 H47 126.1 . . ? C47 C48 C49 109.2(3) . . ? C47 C48 Fe2 70.00(18) . . ? C49 C48 Fe2 69.68(17) . . ? C47 C48 H48 125.4 . . ? C49 C48 H48 125.4 . . ? Fe2 C48 H48 125.4 . . ? C48 C49 C45 107.5(3) . . ? C48 C49 Fe2 69.76(17) . . ? C45 C49 Fe2 69.13(17) . . ? C48 C49 H49 126.3 . . ? C45 C49 H49 126.3 . . ? Fe2 C49 H49 126.3 . . ? C51 C50 C54 108.4(3) . . ? C51 C50 Fe2 70.18(19) . . ? C54 C50 Fe2 69.70(19) . . ? C51 C50 H50 125.8 . . ? C54 C50 H50 125.8 . . ? Fe2 C50 H50 125.8 . . ? C50 C51 C52 107.8(3) . . ? C50 C51 Fe2 69.60(19) . . ? C52 C51 Fe2 69.18(18) . . ? C50 C51 H51 126.1 . . ? C52 C51 H51 126.1 . . ? Fe2 C51 H51 126.1 . . ? C53 C52 C51 108.5(3) . . ? C53 C52 Fe2 69.94(19) . . ? C51 C52 Fe2 70.53(18) . . ? C53 C52 H52 125.7 . . ? C51 C52 H52 125.7 . . ? Fe2 C52 H52 125.7 . . ? C52 C53 C54 108.1(3) . . ? C52 C53 Fe2 69.74(19) . . ? C54 C53 Fe2 69.89(18) . . ? C52 C53 H53 125.9 . . ? C54 C53 H53 125.9 . . ? Fe2 C53 H53 125.9 . . ? C50 C54 C53 107.1(3) . . ? C50 C54 Fe2 69.70(19) . . ? C53 C54 Fe2 69.33(19) . . ? C50 C54 H54 126.4 . . ? C53 C54 H54 126.4 . . ? Fe2 C54 H54 126.4 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.435 _refine_diff_density_min -0.309 _refine_diff_density_rms 0.090