Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'C. McKenzie' 'Morten Ghiladi' 'Frank B. Larsen' 'Inger Sotofte' 'Jean-Pierre Tuchagues' _publ_contact_author_name 'Dr C McKenzie' _publ_contact_author_address ; Department of Chemistry Odense University Campusvej 55 Odense 5230 DENMARK ; _publ_contact_author_email CHK@CHEM.SDU.DK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; 2:2 Fe(III):ligand and adamantane core 4:2 Fe(III):ligand (hydr)oxo complexes of an acyclic ditopic ligand ; data_frank2m _database_code_depnum_ccdc_archive 'CCDC 257918' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C72 H80 Fe4 N12 O6, 4(Cl O4), 4(C H4 O) ; _chemical_formula_sum 'C76 H96 Cl4 Fe4 N12 O26' _chemical_formula_weight 1958.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.991(5) _cell_length_b 25.140(7) _cell_length_c 20.922(6) _cell_angle_alpha 90.00 _cell_angle_beta 93.457(6) _cell_angle_gamma 90.00 _cell_volume 8395(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 11279 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 23.07 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.550 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4064 _exptl_absorpt_coefficient_mu 0.890 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8323 _exptl_absorpt_correction_T_max 0.8973 _exptl_absorpt_process_details 'XPREP 1995' _exptl_special_details ; Data was truncated to 0.9 resolution. Disorder in tert-butyl groups of the ligand as well as one of the perchlorate anions accounts for the high R-value. Attempts of low temperature data aquccion caused the crystals to crack. Geometry of the disordered moities was restrained. Disorder for the tert-butyl groups was due to 2-fold axis. A disordered perchlorate anion was modeled in two close by positions each with 50/50 occupancy. The terminal carbons on each tert-Butyl group as well as oxygens on the disordered perchlorate was refined with common isotropic displacement parameters each group given one parameter. The structures contains 4 solvent-accessible voids per unit cell, with the symmetry-unique void located at (0,0,0). PLATON/SQUEEZE estimated the solvent-accessible region of each void to occupy 203 \%A^3^ and contain 79 electrons. The electron density was modelled as 4 methanol molecules which accounts for 72 electrons. This model is in good agreement with elemental analysis of the crystals. H3O was located from the difference Fourier map. Original position of H3O gave d(O3-H3O)= 1.06, which is slighty longer than excpected for O-H bonds. H3O was therefore refined with a restrained distance of 1.00 \%A. Final refinments cycles was done with coordinates of H3O riding on O3. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART CCD diffractometer' _diffrn_measurement_method ; \w rotation scans with narrow frames ; _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35889 _diffrn_reflns_av_R_equivalents 0.1422 _diffrn_reflns_av_sigmaI/netI 0.0749 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.51 _diffrn_reflns_theta_max 23.46 _reflns_number_total 6098 _reflns_number_gt 4598 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (L- J- Barbour)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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^)+(0.0908P)^2^+96.9920P] 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 6098 _refine_ls_number_parameters 501 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.1152 _refine_ls_R_factor_gt 0.0904 _refine_ls_wR_factor_ref 0.2360 _refine_ls_wR_factor_gt 0.2234 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.083 _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 O10 O 0.2800(5) 0.3184(5) 0.1292(4) 0.124(4) Uani 1 1 d . . . O11 O 0.3820(8) 0.3317(7) 0.0576(5) 0.183(6) Uani 1 1 d . . . O12 O 0.4182(10) 0.2940(7) 0.1476(9) 0.237(8) Uani 1 1 d . . . O13 O 0.3843(10) 0.3764(5) 0.1498(7) 0.213(8) Uani 1 1 d . . . Cl1 Cl 0.36411(18) 0.33090(13) 0.11978(14) 0.0822(8) Uani 1 1 d . . . O21 O 0.3164(14) 0.0582(7) 0.4868(10) 0.177(4) Uiso 0.50 1 d PD A 1 O22 O 0.1956(6) 0.1032(9) 0.4546(11) 0.177(4) Uiso 0.50 1 d PD A 1 O23 O 0.3050(14) 0.0995(10) 0.3891(6) 0.177(4) Uiso 0.50 1 d PD A 1 O24 O 0.3148(14) 0.1495(6) 0.4803(11) 0.177(4) Uiso 0.50 1 d PD A 1 Cl2 Cl 0.2821(4) 0.1017(3) 0.4528(3) 0.0806(16) Uiso 0.50 1 d PD A 1 O31 O 0.2778(13) 0.0864(9) 0.4071(9) 0.177(4) Uiso 0.50 1 d PD B 2 O32 O 0.3904(11) 0.0873(8) 0.4816(10) 0.177(4) Uiso 0.50 1 d PD B 2 O33 O 0.3550(13) 0.1619(6) 0.4255(11) 0.177(4) Uiso 0.50 1 d PD B 2 O34 O 0.2668(13) 0.1321(9) 0.4998(9) 0.177(4) Uiso 0.50 1 d PD B 2 Cl3 Cl 0.3239(4) 0.1164(2) 0.4551(3) 0.0721(15) Uiso 0.50 1 d PD B 2 C1 C 0.5187(6) 0.8232(3) 0.0338(4) 0.056(2) Uani 1 1 d . . . H1 H 0.4655 0.8112 0.0426 0.067 Uiso 1 1 calc R . . C2 C 0.5570(7) 0.8010(4) -0.0171(4) 0.066(3) Uani 1 1 d . . . H2 H 0.5302 0.7748 -0.0420 0.080 Uiso 1 1 calc R . . C3 C 0.6344(7) 0.8181(4) -0.0300(4) 0.070(3) Uani 1 1 d . . . H3 H 0.6624 0.8024 -0.0628 0.084 Uiso 1 1 calc R . . C4 C 0.6711(6) 0.8583(4) 0.0052(4) 0.056(2) Uani 1 1 d . . . H4 H 0.7232 0.8715 -0.0045 0.067 Uiso 1 1 calc R . . C5 C 0.6291(5) 0.8796(3) 0.0560(3) 0.0407(19) Uani 1 1 d . . . C6 C 0.6650(5) 0.9237(3) 0.0981(4) 0.046(2) Uani 1 1 d . . . H6A H 0.7075 0.9094 0.1284 0.055 Uiso 1 1 calc R . . H6B H 0.6910 0.9502 0.0721 0.055 Uiso 1 1 calc R . . C7 C 0.3448(6) 0.9386(4) 0.1347(4) 0.062(3) Uani 1 1 d . . . H7 H 0.3224 0.9073 0.1499 0.074 Uiso 1 1 calc R . . C8 C 0.2922(7) 0.9817(6) 0.1228(6) 0.096(4) Uani 1 1 d . . . H8 H 0.2354 0.9793 0.1298 0.115 Uiso 1 1 calc R . . C9 C 0.3240(8) 1.0269(5) 0.1011(6) 0.095(4) Uani 1 1 d . . . H9 H 0.2892 1.0559 0.0923 0.114 Uiso 1 1 calc R . . C10 C 0.4089(7) 1.0305(4) 0.0917(4) 0.064(3) Uani 1 1 d . . . H10 H 0.4320 1.0621 0.0777 0.077 Uiso 1 1 calc R . . C11 C 0.4576(6) 0.9865(3) 0.1033(3) 0.048(2) Uani 1 1 d . . . C12 C 0.5470(5) 0.9844(3) 0.0896(4) 0.047(2) Uani 1 1 d . . . H12A H 0.5703 1.0199 0.0931 0.056 Uiso 1 1 calc R . . H12B H 0.5516 0.9724 0.0459 0.056 Uiso 1 1 calc R . . C13 C 0.6327(5) 0.9770(3) 0.1909(3) 0.0417(19) Uani 1 1 d . . . H13A H 0.6749 1.0021 0.1785 0.050 Uiso 1 1 calc R . . H13B H 0.6593 0.9516 0.2205 0.050 Uiso 1 1 calc R . . C14 C 0.5643(5) 1.0062(3) 0.2231(3) 0.0384(18) Uani 1 1 d . . . C15 C 0.5000 0.9786(4) 0.2500 0.039(3) Uani 1 2 d S . . C16 C 0.5626(5) 1.0615(3) 0.2234(3) 0.0435(19) Uani 1 1 d . . . H16 H 0.6057 1.0797 0.2048 0.052 Uiso 1 1 calc R . . C17 C 0.5000 1.0911(4) 0.2500 0.041(3) Uani 1 2 d S . . C18 C 0.5000 1.1515(4) 0.2500 0.048(3) Uani 1 2 d SD . . C19 C 0.5861(11) 1.1684(11) 0.2804(13) 0.117(5) Uiso 0.50 1 d PD . . H19A H 0.6278 1.1643 0.2496 0.176 Uiso 0.50 1 calc PR . . H19B H 0.6003 1.1465 0.3170 0.176 Uiso 0.50 1 calc PR . . H19C H 0.5839 1.2050 0.2934 0.176 Uiso 0.50 1 calc PR . . C20 C 0.4349(14) 1.1785(11) 0.2891(12) 0.117(5) Uiso 0.50 1 d PD . . H20A H 0.4578 1.2109 0.3072 0.176 Uiso 0.50 1 calc PR . . H20B H 0.4199 1.1552 0.3228 0.176 Uiso 0.50 1 calc PR . . H20C H 0.3861 1.1865 0.2618 0.176 Uiso 0.50 1 calc PR . . C21 C 0.4953(18) 1.1725(11) 0.1816(8) 0.117(5) Uiso 0.50 1 d PD . . H21A H 0.4873 1.1434 0.1523 0.176 Uiso 0.50 1 calc PR . . H21B H 0.5465 1.1907 0.1737 0.176 Uiso 0.50 1 calc PR . . H21C H 0.4491 1.1968 0.1758 0.176 Uiso 0.50 1 calc PR . . C22 C 0.7938(6) 0.8432(5) 0.2860(5) 0.072(3) Uani 1 1 d . . . H22 H 0.7809 0.8582 0.2460 0.086 Uiso 1 1 calc R . . C23 C 0.8701(7) 0.8550(6) 0.3185(7) 0.101(4) Uani 1 1 d . . . H23 H 0.9082 0.8766 0.2989 0.121 Uiso 1 1 calc R . . C24 C 0.8899(9) 0.8361(9) 0.3772(7) 0.142(7) Uani 1 1 d . . . H24 H 0.9391 0.8461 0.4000 0.170 Uiso 1 1 calc R . . C25 C 0.8329(8) 0.8002(7) 0.4033(6) 0.113(5) Uani 1 1 d . . . H25 H 0.8454 0.7841 0.4428 0.136 Uiso 1 1 calc R . . C26 C 0.7598(6) 0.7898(5) 0.3695(5) 0.068(3) Uani 1 1 d . . . C27 C 0.6955(7) 0.7526(4) 0.3922(4) 0.068(3) Uani 1 1 d . . . H27A H 0.7224 0.7260 0.4200 0.082 Uiso 1 1 calc R . . H27B H 0.6559 0.7721 0.4166 0.082 Uiso 1 1 calc R . . C28 C 0.7085(6) 0.6898(4) 0.3054(5) 0.070(3) Uani 1 1 d . . . H28A H 0.7057 0.6549 0.3248 0.084 Uiso 1 1 calc R . . H28B H 0.7655 0.7027 0.3123 0.084 Uiso 1 1 calc R . . C29 C 0.6877(6) 0.6850(4) 0.2349(5) 0.062(3) Uani 1 1 d . . . C30 C 0.6951(7) 0.6388(4) 0.2008(6) 0.083(4) Uani 1 1 d . . . H30 H 0.7136 0.6078 0.2213 0.099 Uiso 1 1 calc R . . C31 C 0.6747(8) 0.6386(5) 0.1349(7) 0.093(4) Uani 1 1 d . . . H31 H 0.6768 0.6073 0.1115 0.112 Uiso 1 1 calc R . . C32 C 0.6516(7) 0.6849(5) 0.1056(5) 0.076(3) Uani 1 1 d . . . H32 H 0.6405 0.6860 0.0614 0.091 Uiso 1 1 calc R . . C33 C 0.6449(5) 0.7306(4) 0.1423(4) 0.054(2) Uani 1 1 d . . . H33 H 0.6281 0.7621 0.1220 0.065 Uiso 1 1 calc R . . C34 C 0.5748(6) 0.6965(4) 0.3575(5) 0.064(3) Uani 1 1 d . . . H34A H 0.5916 0.6716 0.3914 0.077 Uiso 1 1 calc R . . H34B H 0.5352 0.7213 0.3742 0.077 Uiso 1 1 calc R . . C35 C 0.5342(6) 0.6672(3) 0.3027(5) 0.056(2) Uani 1 1 d . . . C36 C 0.5000 0.6947(4) 0.2500 0.047(3) Uani 1 2 d S . . C37 C 0.5330(8) 0.6110(4) 0.3023(6) 0.084(4) Uani 1 1 d . . . H37 H 0.5549 0.5925 0.3380 0.101 Uiso 1 1 calc R . . C38 C 0.5000 0.5831(6) 0.2500 0.095(6) Uani 1 2 d S . . C39 C 0.5000 0.5208(7) 0.2500 0.141(9) Uani 1 2 d SD . . C40 C 0.544(2) 0.5039(14) 0.1904(11) 0.157(8) Uiso 0.50 1 d PD . . H40A H 0.6007 0.5167 0.1934 0.235 Uiso 0.50 1 calc PR . . H40B H 0.5149 0.5187 0.1530 0.235 Uiso 0.50 1 calc PR . . H40C H 0.5440 0.4658 0.1873 0.235 Uiso 0.50 1 calc PR . . C41 C 0.531(2) 0.4916(14) 0.3098(11) 0.157(8) Uiso 0.50 1 d PD . . H41A H 0.5268 0.4539 0.3026 0.235 Uiso 0.50 1 calc PR . . H41B H 0.4979 0.5014 0.3446 0.235 Uiso 0.50 1 calc PR . . H41C H 0.5886 0.5008 0.3201 0.235 Uiso 0.50 1 calc PR . . C42 C 0.4065(10) 0.5071(14) 0.2362(17) 0.157(8) Uiso 0.50 1 d PD . . H42A H 0.3991 0.4895 0.1956 0.235 Uiso 0.50 1 calc PR . . H42B H 0.3740 0.5393 0.2352 0.235 Uiso 0.50 1 calc PR . . H42C H 0.3881 0.4842 0.2692 0.235 Uiso 0.50 1 calc PR . . N1 N 0.5537(4) 0.8605(3) 0.0705(3) 0.0474(17) Uani 1 1 d . . . N2 N 0.4260(4) 0.9405(3) 0.1250(3) 0.0447(17) Uani 1 1 d . . . N3 N 0.5967(4) 0.9486(2) 0.1331(3) 0.0392(15) Uani 1 1 d . . . N4 N 0.7396(5) 0.8110(3) 0.3111(3) 0.061(2) Uani 1 1 d . . . N5 N 0.6617(4) 0.7309(3) 0.2063(3) 0.0467(17) Uani 1 1 d . . . N6 N 0.6511(5) 0.7265(3) 0.3374(3) 0.057(2) Uani 1 1 d . . . O1 O 0.5000 0.9239(3) 0.2500 0.0359(17) Uani 1 2 d S . . O2 O 0.5000 0.7492(3) 0.2500 0.0418(18) Uani 1 2 d S . . O3 O 0.6142(3) 0.8438(2) 0.2029(2) 0.0417(13) Uani 1 1 d . . . O4 O 0.4371(3) 0.8311(2) 0.1703(2) 0.0414(13) Uani 1 1 d . . . Fe1 Fe 0.51373(7) 0.88315(4) 0.16446(4) 0.0339(3) Uani 1 1 d . . . Fe2 Fe 0.61186(7) 0.79089(4) 0.27117(5) 0.0388(3) Uani 1 1 d . . . H3O H 0.6644 0.8438 0.1766 0.06(3) Uiso 1 1 d 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 O10 0.063(5) 0.196(11) 0.112(7) 0.026(7) 0.003(5) -0.024(6) O11 0.163(11) 0.298(18) 0.091(7) -0.035(9) 0.041(7) -0.039(11) O12 0.184(14) 0.253(18) 0.275(19) 0.092(15) 0.030(13) 0.128(13) O13 0.269(17) 0.169(12) 0.215(14) -0.122(11) 0.123(12) -0.138(12) Cl1 0.0738(19) 0.092(2) 0.0819(19) -0.0161(16) 0.0136(15) 0.0109(16) C1 0.073(6) 0.052(5) 0.043(5) -0.008(4) 0.008(4) -0.006(5) C2 0.087(8) 0.068(7) 0.046(5) -0.020(5) 0.020(5) 0.000(6) C3 0.095(8) 0.077(7) 0.040(5) -0.009(5) 0.027(5) 0.020(6) C4 0.068(6) 0.061(6) 0.042(5) 0.004(4) 0.027(4) 0.010(5) C5 0.055(5) 0.035(4) 0.034(4) 0.003(3) 0.016(4) 0.007(4) C6 0.051(5) 0.045(5) 0.045(4) 0.001(4) 0.026(4) 0.003(4) C7 0.056(6) 0.078(7) 0.052(5) 0.009(5) 0.007(4) 0.020(5) C8 0.063(7) 0.135(12) 0.092(8) 0.028(8) 0.024(6) 0.042(8) C9 0.104(10) 0.092(9) 0.092(8) 0.032(7) 0.027(7) 0.061(8) C10 0.088(8) 0.053(6) 0.052(5) 0.010(4) 0.017(5) 0.037(5) C11 0.072(6) 0.052(5) 0.022(4) 0.002(4) 0.011(4) 0.013(5) C12 0.067(6) 0.037(5) 0.038(4) 0.013(4) 0.013(4) 0.007(4) C13 0.046(5) 0.044(5) 0.037(4) 0.001(4) 0.017(4) -0.002(4) C14 0.054(5) 0.026(4) 0.036(4) -0.003(3) 0.008(4) -0.003(4) C15 0.054(7) 0.031(6) 0.033(6) 0.000 0.003(5) 0.000 C16 0.051(5) 0.046(5) 0.035(4) 0.005(4) 0.010(4) -0.005(4) C17 0.060(7) 0.028(6) 0.036(6) 0.000 -0.002(5) 0.000 C18 0.065(8) 0.035(6) 0.047(7) 0.000 0.027(6) 0.000 C22 0.056(6) 0.096(8) 0.064(6) 0.018(6) 0.011(5) -0.003(6) C23 0.062(8) 0.148(13) 0.093(9) 0.009(9) 0.012(7) -0.024(8) C24 0.071(9) 0.26(2) 0.087(10) -0.004(12) -0.019(8) -0.023(12) C25 0.062(8) 0.204(17) 0.073(8) 0.025(9) -0.006(7) 0.008(9) C26 0.049(6) 0.104(8) 0.053(6) 0.004(6) 0.010(5) 0.018(6) C27 0.075(7) 0.085(7) 0.044(5) 0.024(5) 0.003(5) 0.025(6) C28 0.065(6) 0.076(7) 0.072(7) 0.017(5) 0.021(5) 0.039(5) C29 0.056(6) 0.066(6) 0.069(6) 0.018(5) 0.039(5) 0.026(5) C30 0.098(9) 0.047(6) 0.108(10) 0.006(6) 0.043(7) 0.034(6) C31 0.107(10) 0.075(8) 0.102(10) -0.016(7) 0.047(8) 0.031(7) C32 0.089(8) 0.081(8) 0.062(6) -0.020(6) 0.034(6) 0.020(6) C33 0.056(6) 0.057(6) 0.053(5) 0.008(4) 0.029(4) 0.011(5) C34 0.071(6) 0.060(6) 0.065(6) 0.031(5) 0.033(5) 0.022(5) C35 0.074(6) 0.032(5) 0.066(6) 0.006(4) 0.040(5) 0.008(4) C36 0.057(7) 0.027(6) 0.061(8) 0.000 0.034(6) 0.000 C37 0.115(10) 0.063(8) 0.080(7) 0.025(6) 0.053(7) 0.030(7) C38 0.140(16) 0.040(9) 0.112(14) 0.000 0.067(13) 0.000 C39 0.19(2) 0.082(14) 0.16(2) 0.000 0.091(19) 0.000 N1 0.061(5) 0.050(4) 0.034(3) 0.000(3) 0.019(3) 0.005(4) N2 0.052(4) 0.055(4) 0.027(3) 0.001(3) 0.007(3) 0.020(3) N3 0.056(4) 0.033(3) 0.031(3) 0.004(3) 0.020(3) 0.006(3) N4 0.051(5) 0.082(6) 0.051(4) 0.004(4) 0.016(4) 0.011(4) N5 0.049(4) 0.046(4) 0.048(4) 0.013(3) 0.025(3) 0.013(3) N6 0.060(5) 0.066(5) 0.047(4) 0.021(4) 0.016(4) 0.022(4) O1 0.052(4) 0.031(4) 0.026(3) 0.000 0.014(3) 0.000 O2 0.051(5) 0.032(4) 0.044(4) 0.000 0.018(4) 0.000 O3 0.046(3) 0.042(3) 0.039(3) 0.010(2) 0.017(2) 0.003(3) O4 0.044(3) 0.046(3) 0.036(3) -0.005(2) 0.011(2) 0.000(3) Fe1 0.0451(7) 0.0317(6) 0.0261(5) 0.0011(4) 0.0119(5) 0.0032(5) Fe2 0.0408(7) 0.0415(7) 0.0353(6) 0.0094(5) 0.0122(5) 0.0075(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O10 Cl1 1.406(8) . ? O11 Cl1 1.350(10) . ? O12 Cl1 1.373(13) . ? O13 Cl1 1.335(10) . ? O21 Cl2 1.396(8) . ? O22 Cl2 1.386(8) . ? O23 Cl2 1.405(8) . ? O24 Cl2 1.420(8) . ? O31 Cl3 1.425(8) . ? O32 Cl3 1.378(8) . ? O33 Cl3 1.406(8) . ? O34 Cl3 1.402(8) . ? C1 N1 1.316(10) . ? C1 C2 1.377(12) . ? C1 H1 0.9300 . ? C2 C3 1.352(14) . ? C2 H2 0.9300 . ? C3 C4 1.363(13) . ? C3 H3 0.9300 . ? C4 C5 1.398(11) . ? C4 H4 0.9300 . ? C5 N1 1.348(10) . ? C5 C6 1.507(11) . ? C6 N3 1.490(9) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 N2 1.327(11) . ? C7 C8 1.385(14) . ? C7 H7 0.9300 . ? C8 C9 1.335(17) . ? C8 H8 0.9300 . ? C9 C10 1.386(16) . ? C9 H9 0.9300 . ? C10 C11 1.367(12) . ? C10 H10 0.9300 . ? C11 N2 1.352(11) . ? C11 C12 1.475(12) . ? C12 N3 1.476(10) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 N3 1.490(10) . ? C13 C14 1.510(10) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.388(9) . ? C14 C16 1.390(11) . ? C15 O1 1.374(12) . ? C15 C14 1.388(9) 2_655 ? C16 C17 1.391(10) . ? C16 H16 0.9300 . ? C17 C16 1.391(10) 2_655 ? C17 C18 1.518(15) . ? C18 C20 1.521(14) 2_655 ? C18 C20 1.521(14) . ? C18 C21 1.522(14) 2_655 ? C18 C21 1.522(14) . ? C18 C19 1.541(15) . ? C18 C19 1.541(14) 2_655 ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 N4 1.318(12) . ? C22 C23 1.392(15) . ? C22 H22 0.9300 . ? C23 C24 1.339(18) . ? C23 H23 0.9300 . ? C24 C25 1.41(2) . ? C24 H24 0.9300 . ? C25 C26 1.355(15) . ? C25 H25 0.9300 . ? C26 N4 1.355(12) . ? C26 C27 1.488(14) . ? C27 N6 1.468(12) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 N6 1.489(11) . ? C28 C29 1.497(14) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 N5 1.353(11) . ? C29 C30 1.373(14) . ? C30 C31 1.397(16) . ? C30 H30 0.9300 . ? C31 C32 1.355(16) . ? C31 H31 0.9300 . ? C32 C33 1.391(13) . ? C32 H32 0.9300 . ? C33 N5 1.349(11) . ? C33 H33 0.9300 . ? C34 C35 1.479(14) . ? C34 N6 1.514(12) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.387(11) . ? C35 C37 1.413(13) . ? C36 O2 1.368(13) . ? C36 C35 1.387(11) 2_655 ? C37 C38 1.378(14) . ? C37 H37 0.9300 . ? C38 C37 1.378(14) 2_655 ? C38 C39 1.57(2) . ? C39 C41 1.509(15) 2_655 ? C39 C41 1.509(15) . ? C39 C40 1.529(15) 2_655 ? C39 C40 1.529(15) . ? C39 C42 1.545(15) . ? C39 C42 1.545(15) 2_655 ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? N1 Fe1 2.180(6) . ? N2 Fe1 2.142(6) . ? N3 Fe1 2.237(6) . ? N4 Fe2 2.218(8) . ? N5 Fe2 2.210(7) . ? N6 Fe2 2.198(7) . ? O1 Fe1 2.086(3) . ? O1 Fe1 2.086(3) 2_655 ? O2 Fe2 2.098(4) . ? O2 Fe2 2.098(4) 2_655 ? O3 Fe2 1.953(5) . ? O3 Fe1 2.013(5) . ? O3 H3O 0.9998 . ? O4 Fe1 1.802(5) . ? O4 Fe2 1.803(5) 2_655 ? Fe1 Fe2 3.3989(16) 2_655 ? Fe1 Fe2 3.5220(16) . ? Fe2 O4 1.803(5) 2_655 ? Fe2 Fe2 3.633(2) 2_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O13 Cl1 O11 112.4(9) . . ? O13 Cl1 O12 104.5(12) . . ? O11 Cl1 O12 104.7(10) . . ? O13 Cl1 O10 109.4(8) . . ? O11 Cl1 O10 113.5(7) . . ? O12 Cl1 O10 111.9(9) . . ? O22 Cl2 O21 111.8(11) . . ? O22 Cl2 O23 110.1(11) . . ? O21 Cl2 O23 109.6(11) . . ? O22 Cl2 O24 108.0(11) . . ? O21 Cl2 O24 109.4(10) . . ? O23 Cl2 O24 107.9(11) . . ? O32 Cl3 O34 113.4(11) . . ? O32 Cl3 O33 108.9(11) . . ? O34 Cl3 O33 109.1(11) . . ? O32 Cl3 O31 110.9(11) . . ? O34 Cl3 O31 106.8(11) . . ? O33 Cl3 O31 107.6(11) . . ? N1 C1 C2 123.0(9) . . ? N1 C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? C3 C2 C1 118.8(9) . . ? C3 C2 H2 120.6 . . ? C1 C2 H2 120.6 . . ? C2 C3 C4 119.8(8) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C3 C4 C5 118.9(9) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? N1 C5 C4 120.8(8) . . ? N1 C5 C6 116.4(6) . . ? C4 C5 C6 122.8(8) . . ? N3 C6 C5 109.4(6) . . ? N3 C6 H6A 109.8 . . ? C5 C6 H6A 109.8 . . ? N3 C6 H6B 109.8 . . ? C5 C6 H6B 109.8 . . ? H6A C6 H6B 108.2 . . ? N2 C7 C8 122.3(10) . . ? N2 C7 H7 118.8 . . ? C8 C7 H7 118.8 . . ? C9 C8 C7 119.1(11) . . ? C9 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? C8 C9 C10 120.1(10) . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? C11 C10 C9 118.3(10) . . ? C11 C10 H10 120.8 . . ? C9 C10 H10 120.8 . . ? N2 C11 C10 122.1(9) . . ? N2 C11 C12 114.9(7) . . ? C10 C11 C12 122.9(8) . . ? C11 C12 N3 113.2(6) . . ? C11 C12 H12A 108.9 . . ? N3 C12 H12A 108.9 . . ? C11 C12 H12B 108.9 . . ? N3 C12 H12B 108.9 . . ? H12A C12 H12B 107.8 . . ? N3 C13 C14 109.9(6) . . ? N3 C13 H13A 109.7 . . ? C14 C13 H13A 109.7 . . ? N3 C13 H13B 109.7 . . ? C14 C13 H13B 109.7 . . ? H13A C13 H13B 108.2 . . ? C15 C14 C16 119.0(7) . . ? C15 C14 C13 120.8(7) . . ? C16 C14 C13 120.2(7) . . ? O1 C15 C14 120.1(5) . . ? O1 C15 C14 120.1(5) . 2_655 ? C14 C15 C14 119.9(9) . 2_655 ? C14 C16 C17 123.4(8) . . ? C14 C16 H16 118.3 . . ? C17 C16 H16 118.3 . . ? C16 C17 C16 115.3(10) 2_655 . ? C16 C17 C18 122.3(5) 2_655 . ? C16 C17 C18 122.3(5) . . ? C17 C18 C20 116.5(11) . 2_655 ? C17 C18 C20 116.5(11) . . ? C20 C18 C20 127(2) 2_655 . ? C17 C18 C21 110.3(11) . 2_655 ? C20 C18 C21 110.7(11) 2_655 2_655 ? C20 C18 C21 48.5(11) . 2_655 ? C17 C18 C21 110.3(11) . . ? C20 C18 C21 48.5(11) 2_655 . ? C20 C18 C21 110.7(11) . . ? C21 C18 C21 139(2) 2_655 . ? C17 C18 C19 106.0(11) . . ? C20 C18 C19 58.3(11) 2_655 . ? C20 C18 C19 106.2(11) . . ? C21 C18 C19 61.6(11) 2_655 . ? C21 C18 C19 106.5(11) . . ? C17 C18 C19 106.0(11) . 2_655 ? C20 C18 C19 106.2(11) 2_655 2_655 ? C20 C18 C19 58.3(11) . 2_655 ? C21 C18 C19 106.5(11) 2_655 2_655 ? C21 C18 C19 61.6(11) . 2_655 ? C19 C18 C19 148(2) . 2_655 ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N4 C22 C23 121.0(10) . . ? N4 C22 H22 119.5 . . ? C23 C22 H22 119.5 . . ? C24 C23 C22 121.6(12) . . ? C24 C23 H23 119.2 . . ? C22 C23 H23 119.2 . . ? C23 C24 C25 117.3(12) . . ? C23 C24 H24 121.3 . . ? C25 C24 H24 121.3 . . ? C26 C25 C24 118.5(12) . . ? C26 C25 H25 120.8 . . ? C24 C25 H25 120.8 . . ? N4 C26 C25 123.2(11) . . ? N4 C26 C27 113.8(9) . . ? C25 C26 C27 123.1(10) . . ? N6 C27 C26 110.1(7) . . ? N6 C27 H27A 109.6 . . ? C26 C27 H27A 109.6 . . ? N6 C27 H27B 109.6 . . ? C26 C27 H27B 109.6 . . ? H27A C27 H27B 108.2 . . ? N6 C28 C29 112.7(7) . . ? N6 C28 H28A 109.0 . . ? C29 C28 H28A 109.0 . . ? N6 C28 H28B 109.0 . . ? C29 C28 H28B 109.0 . . ? H28A C28 H28B 107.8 . . ? N5 C29 C30 121.7(10) . . ? N5 C29 C28 114.3(8) . . ? C30 C29 C28 124.0(9) . . ? C29 C30 C31 119.5(10) . . ? C29 C30 H30 120.3 . . ? C31 C30 H30 120.3 . . ? C32 C31 C30 119.1(11) . . ? C32 C31 H31 120.5 . . ? C30 C31 H31 120.5 . . ? C31 C32 C33 119.1(10) . . ? C31 C32 H32 120.4 . . ? C33 C32 H32 120.4 . . ? N5 C33 C32 122.4(9) . . ? N5 C33 H33 118.8 . . ? C32 C33 H33 118.8 . . ? C35 C34 N6 110.8(7) . . ? C35 C34 H34A 109.5 . . ? N6 C34 H34A 109.5 . . ? C35 C34 H34B 109.5 . . ? N6 C34 H34B 109.5 . . ? H34A C34 H34B 108.1 . . ? C36 C35 C37 119.3(10) . . ? C36 C35 C34 120.2(8) . . ? C37 C35 C34 120.5(9) . . ? O2 C36 C35 119.9(5) . 2_655 ? O2 C36 C35 119.9(5) . . ? C35 C36 C35 120.2(11) 2_655 . ? C38 C37 C35 121.3(11) . . ? C38 C37 H37 119.4 . . ? C35 C37 H37 119.4 . . ? C37 C38 C37 118.7(14) 2_655 . ? C37 C38 C39 120.6(7) 2_655 . ? C37 C38 C39 120.6(7) . . ? C41 C39 C41 122(3) 2_655 . ? C41 C39 C40 113.3(13) 2_655 2_655 ? C41 C39 C40 48.2(14) . 2_655 ? C41 C39 C40 48.2(14) 2_655 . ? C41 C39 C40 113.3(13) . . ? C40 C39 C40 148(3) 2_655 . ? C41 C39 C42 57.9(14) 2_655 . ? C41 C39 C42 108.3(12) . . ? C40 C39 C42 66.6(12) 2_655 . ? C40 C39 C42 105.9(12) . . ? C41 C39 C42 108.3(12) 2_655 2_655 ? C41 C39 C42 57.9(14) . 2_655 ? C40 C39 C42 105.9(12) 2_655 2_655 ? C40 C39 C42 66.6(12) . 2_655 ? C42 C39 C42 154(3) . 2_655 ? C41 C39 C38 119.1(14) 2_655 . ? C41 C39 C38 119.1(14) . . ? C40 C39 C38 106.1(14) 2_655 . ? C40 C39 C38 106.1(14) . . ? C42 C39 C38 102.8(14) . . ? C42 C39 C38 102.8(14) 2_655 . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C39 C42 H42A 109.5 . . ? C39 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C39 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C1 N1 C5 118.6(7) . . ? C1 N1 Fe1 125.1(6) . . ? C5 N1 Fe1 115.1(5) . . ? C7 N2 C11 118.1(7) . . ? C7 N2 Fe1 122.8(6) . . ? C11 N2 Fe1 117.1(6) . . ? C12 N3 C13 112.1(6) . . ? C12 N3 C6 109.7(6) . . ? C13 N3 C6 110.0(6) . . ? C12 N3 Fe1 108.8(5) . . ? C13 N3 Fe1 108.8(4) . . ? C6 N3 Fe1 107.4(4) . . ? C22 N4 C26 118.3(9) . . ? C22 N4 Fe2 127.1(7) . . ? C26 N4 Fe2 114.5(6) . . ? C33 N5 C29 118.1(8) . . ? C33 N5 Fe2 123.7(5) . . ? C29 N5 Fe2 115.0(5) . . ? C27 N6 C28 110.2(8) . . ? C27 N6 C34 111.4(7) . . ? C28 N6 C34 110.3(8) . . ? C27 N6 Fe2 105.6(6) . . ? C28 N6 Fe2 109.4(5) . . ? C34 N6 Fe2 109.8(5) . . ? C15 O1 Fe1 119.45(16) . . ? C15 O1 Fe1 119.45(16) . 2_655 ? Fe1 O1 Fe1 121.1(3) . 2_655 ? C36 O2 Fe2 120.01(17) . . ? C36 O2 Fe2 120.01(17) . 2_655 ? Fe2 O2 Fe2 120.0(3) . 2_655 ? Fe2 O3 Fe1 125.2(3) . . ? Fe2 O3 H3O 117.0 . . ? Fe1 O3 H3O 115.3 . . ? Fe1 O4 Fe2 141.1(3) . 2_655 ? O4 Fe1 O3 98.4(2) . . ? O4 Fe1 O1 101.06(19) . . ? O3 Fe1 O1 91.26(17) . . ? O4 Fe1 N2 94.7(3) . . ? O3 Fe1 N2 166.7(3) . . ? O1 Fe1 N2 84.2(2) . . ? O4 Fe1 N1 96.3(2) . . ? O3 Fe1 N1 87.8(2) . . ? O1 Fe1 N1 162.6(2) . . ? N2 Fe1 N1 92.8(2) . . ? O4 Fe1 N3 166.4(2) . . ? O3 Fe1 N3 90.3(2) . . ? O1 Fe1 N3 89.1(2) . . ? N2 Fe1 N3 77.2(3) . . ? N1 Fe1 N3 73.5(2) . . ? O4 Fe1 Fe2 19.47(15) . 2_655 ? O3 Fe1 Fe2 89.00(14) . 2_655 ? O1 Fe1 Fe2 84.28(14) . 2_655 ? N2 Fe1 Fe2 102.9(2) . 2_655 ? N1 Fe1 Fe2 113.06(19) . 2_655 ? N3 Fe1 Fe2 173.36(15) . 2_655 ? O4 Fe1 Fe2 75.99(17) . . ? O3 Fe1 Fe2 26.94(13) . . ? O1 Fe1 Fe2 81.13(14) . . ? N2 Fe1 Fe2 160.70(17) . . ? N1 Fe1 Fe2 104.84(18) . . ? N3 Fe1 Fe2 114.91(17) . . ? Fe2 Fe1 Fe2 63.31(4) 2_655 . ? O4 Fe2 O3 98.3(2) 2_655 . ? O4 Fe2 O2 91.4(2) 2_655 . ? O3 Fe2 O2 103.9(2) . . ? O4 Fe2 N6 96.0(2) 2_655 . ? O3 Fe2 N6 160.9(2) . . ? O2 Fe2 N6 88.4(3) . . ? O4 Fe2 N5 170.9(2) 2_655 . ? O3 Fe2 N5 89.5(2) . . ? O2 Fe2 N5 82.2(2) . . ? N6 Fe2 N5 77.6(3) . . ? O4 Fe2 N4 92.5(3) 2_655 . ? O3 Fe2 N4 93.6(3) . . ? O2 Fe2 N4 161.4(3) . . ? N6 Fe2 N4 73.1(3) . . ? N5 Fe2 N4 91.7(3) . . ? O4 Fe2 Fe1 82.33(16) 2_655 . ? O3 Fe2 Fe1 27.84(15) . . ? O2 Fe2 Fe1 81.60(14) . . ? N6 Fe2 Fe1 169.8(2) . . ? N5 Fe2 Fe1 102.90(17) . . ? N4 Fe2 Fe1 117.0(2) . . ? O4 Fe2 Fe2 72.81(17) 2_655 2_655 ? O3 Fe2 Fe2 83.32(16) . 2_655 ? O2 Fe2 Fe2 30.01(17) . 2_655 ? N6 Fe2 Fe2 113.1(2) . 2_655 ? N5 Fe2 Fe2 103.69(19) . 2_655 ? N4 Fe2 Fe2 164.3(2) . 2_655 ? Fe1 Fe2 Fe2 56.69(3) . 2_655 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 0.2(15) . . . . ? C1 C2 C3 C4 -3.1(15) . . . . ? C2 C3 C4 C5 2.8(14) . . . . ? C3 C4 C5 N1 0.4(13) . . . . ? C3 C4 C5 C6 179.3(8) . . . . ? N1 C5 C6 N3 -18.8(9) . . . . ? C4 C5 C6 N3 162.3(7) . . . . ? N2 C7 C8 C9 -0.2(18) . . . . ? C7 C8 C9 C10 -1(2) . . . . ? C8 C9 C10 C11 1.9(17) . . . . ? C9 C10 C11 N2 -1.6(13) . . . . ? C9 C10 C11 C12 174.5(9) . . . . ? N2 C11 C12 N3 -33.5(10) . . . . ? C10 C11 C12 N3 150.1(8) . . . . ? N3 C13 C14 C15 64.7(8) . . . . ? N3 C13 C14 C16 -112.0(8) . . . . ? C16 C14 C15 O1 179.6(5) . . . . ? C13 C14 C15 O1 2.9(8) . . . . ? C16 C14 C15 C14 -0.4(5) . . . 2_655 ? C13 C14 C15 C14 -177.1(8) . . . 2_655 ? C15 C14 C16 C17 0.8(11) . . . . ? C13 C14 C16 C17 177.5(6) . . . . ? C14 C16 C17 C16 -0.4(5) . . . 2_655 ? C14 C16 C17 C18 179.6(5) . . . . ? C16 C17 C18 C20 -171.4(13) 2_655 . . 2_655 ? C16 C17 C18 C20 8.6(13) . . . 2_655 ? C16 C17 C18 C20 8.6(13) 2_655 . . . ? C16 C17 C18 C20 -171.4(13) . . . . ? C16 C17 C18 C21 61.3(12) 2_655 . . 2_655 ? C16 C17 C18 C21 -118.7(12) . . . 2_655 ? C16 C17 C18 C21 -118.7(12) 2_655 . . . ? C16 C17 C18 C21 61.3(12) . . . . ? C16 C17 C18 C19 126.4(12) 2_655 . . . ? C16 C17 C18 C19 -53.6(12) . . . . ? C16 C17 C18 C19 -53.6(11) 2_655 . . 2_655 ? C16 C17 C18 C19 126.4(11) . . . 2_655 ? N4 C22 C23 C24 -3(2) . . . . ? C22 C23 C24 C25 5(3) . . . . ? C23 C24 C25 C26 -4(2) . . . . ? C24 C25 C26 N4 2(2) . . . . ? C24 C25 C26 C27 179.7(13) . . . . ? N4 C26 C27 N6 29.9(12) . . . . ? C25 C26 C27 N6 -148.2(11) . . . . ? N6 C28 C29 N5 37.3(12) . . . . ? N6 C28 C29 C30 -143.7(10) . . . . ? N5 C29 C30 C31 -0.6(16) . . . . ? C28 C29 C30 C31 -179.5(10) . . . . ? C29 C30 C31 C32 3.0(18) . . . . ? C30 C31 C32 C33 -3.2(17) . . . . ? C31 C32 C33 N5 1.1(15) . . . . ? N6 C34 C35 C36 -63.3(10) . . . . ? N6 C34 C35 C37 114.0(9) . . . . ? C37 C35 C36 O2 179.3(6) . . . . ? C34 C35 C36 O2 -3.3(9) . . . . ? C37 C35 C36 C35 -0.7(6) . . . 2_655 ? C34 C35 C36 C35 176.7(9) . . . 2_655 ? C36 C35 C37 C38 1.3(13) . . . . ? C34 C35 C37 C38 -176.0(7) . . . . ? C35 C37 C38 C37 -0.7(7) . . . 2_655 ? C35 C37 C38 C39 179.3(7) . . . . ? C37 C38 C39 C41 4.2(17) 2_655 . . 2_655 ? C37 C38 C39 C41 -175.8(17) . . . 2_655 ? C37 C38 C39 C41 -175.8(17) 2_655 . . . ? C37 C38 C39 C41 4.2(17) . . . . ? C37 C38 C39 C40 -125.0(15) 2_655 . . 2_655 ? C37 C38 C39 C40 55.0(15) . . . 2_655 ? C37 C38 C39 C40 55.0(15) 2_655 . . . ? C37 C38 C39 C40 -125.0(15) . . . . ? C37 C38 C39 C42 -56.1(15) 2_655 . . . ? C37 C38 C39 C42 123.9(15) . . . . ? C37 C38 C39 C42 123.9(15) 2_655 . . 2_655 ? C37 C38 C39 C42 -56.1(15) . . . 2_655 ? C2 C1 N1 C5 2.9(13) . . . . ? C2 C1 N1 Fe1 -163.5(7) . . . . ? C4 C5 N1 C1 -3.2(12) . . . . ? C6 C5 N1 C1 177.8(7) . . . . ? C4 C5 N1 Fe1 164.5(6) . . . . ? C6 C5 N1 Fe1 -14.4(9) . . . . ? C8 C7 N2 C11 0.5(13) . . . . ? C8 C7 N2 Fe1 164.0(8) . . . . ? C10 C11 N2 C7 0.4(11) . . . . ? C12 C11 N2 C7 -176.0(7) . . . . ? C10 C11 N2 Fe1 -164.0(6) . . . . ? C12 C11 N2 Fe1 19.6(8) . . . . ? C11 C12 N3 C13 -90.6(8) . . . . ? C11 C12 N3 C6 147.0(7) . . . . ? C11 C12 N3 Fe1 29.8(8) . . . . ? C14 C13 N3 C12 52.9(8) . . . . ? C14 C13 N3 C6 175.1(6) . . . . ? C14 C13 N3 Fe1 -67.5(6) . . . . ? C5 C6 N3 C12 -77.3(8) . . . . ? C5 C6 N3 C13 159.1(6) . . . . ? C5 C6 N3 Fe1 40.8(7) . . . . ? C23 C22 N4 C26 0.2(16) . . . . ? C23 C22 N4 Fe2 175.7(9) . . . . ? C25 C26 N4 C22 0.2(16) . . . . ? C27 C26 N4 C22 -177.9(9) . . . . ? C25 C26 N4 Fe2 -175.9(10) . . . . ? C27 C26 N4 Fe2 6.1(11) . . . . ? C32 C33 N5 C29 1.4(13) . . . . ? C32 C33 N5 Fe2 -157.6(7) . . . . ? C30 C29 N5 C33 -1.6(13) . . . . ? C28 C29 N5 C33 177.4(8) . . . . ? C30 C29 N5 Fe2 159.2(8) . . . . ? C28 C29 N5 Fe2 -21.8(10) . . . . ? C26 C27 N6 C28 68.0(9) . . . . ? C26 C27 N6 C34 -169.3(7) . . . . ? C26 C27 N6 Fe2 -50.1(8) . . . . ? C29 C28 N6 C27 -148.8(9) . . . . ? C29 C28 N6 C34 87.7(10) . . . . ? C29 C28 N6 Fe2 -33.2(10) . . . . ? C35 C34 N6 C27 -176.0(7) . . . . ? C35 C34 N6 C28 -53.2(9) . . . . ? C35 C34 N6 Fe2 67.4(8) . . . . ? C14 C15 O1 Fe1 -51.7(4) . . . . ? C14 C15 O1 Fe1 128.3(4) 2_655 . . . ? C14 C15 O1 Fe1 128.3(4) . . . 2_655 ? C14 C15 O1 Fe1 -51.7(4) 2_655 . . 2_655 ? C35 C36 O2 Fe2 -127.7(4) 2_655 . . . ? C35 C36 O2 Fe2 52.3(4) . . . . ? C35 C36 O2 Fe2 52.3(4) 2_655 . . 2_655 ? C35 C36 O2 Fe2 -127.7(4) . . . 2_655 ? Fe2 O4 Fe1 O3 62.0(5) 2_655 . . . ? Fe2 O4 Fe1 O1 -30.9(5) 2_655 . . . ? Fe2 O4 Fe1 N2 -115.9(5) 2_655 . . . ? Fe2 O4 Fe1 N1 150.7(5) 2_655 . . . ? Fe2 O4 Fe1 N3 -168.7(7) 2_655 . . . ? Fe2 O4 Fe1 Fe2 46.9(4) 2_655 . . . ? Fe2 O3 Fe1 O4 -33.9(3) . . . . ? Fe2 O3 Fe1 O1 67.4(3) . . . . ? Fe2 O3 Fe1 N2 137.1(8) . . . . ? Fe2 O3 Fe1 N1 -129.9(4) . . . . ? Fe2 O3 Fe1 N3 156.6(3) . . . . ? Fe2 O3 Fe1 Fe2 -16.8(3) . . . 2_655 ? C15 O1 Fe1 O4 -137.67(17) . . . . ? Fe1 O1 Fe1 O4 42.33(17) 2_655 . . . ? C15 O1 Fe1 O3 123.54(14) . . . . ? Fe1 O1 Fe1 O3 -56.46(14) 2_655 . . . ? C15 O1 Fe1 N2 -44.0(2) . . . . ? Fe1 O1 Fe1 N2 136.0(2) 2_655 . . . ? C15 O1 Fe1 N1 37.0(7) . . . . ? Fe1 O1 Fe1 N1 -143.0(7) 2_655 . . . ? C15 O1 Fe1 N3 33.22(17) . . . . ? Fe1 O1 Fe1 N3 -146.78(17) 2_655 . . . ? C15 O1 Fe1 Fe2 -147.58(3) . . . 2_655 ? Fe1 O1 Fe1 Fe2 32.42(2) 2_655 . . 2_655 ? C15 O1 Fe1 Fe2 148.60(3) . . . . ? Fe1 O1 Fe1 Fe2 -31.40(3) 2_655 . . . ? C7 N2 Fe1 O4 25.4(7) . . . . ? C11 N2 Fe1 O4 -171.0(5) . . . . ? C7 N2 Fe1 O3 -145.7(9) . . . . ? C11 N2 Fe1 O3 17.9(12) . . . . ? C7 N2 Fe1 O1 -75.3(7) . . . . ? C11 N2 Fe1 O1 88.4(5) . . . . ? C7 N2 Fe1 N1 121.9(7) . . . . ? C11 N2 Fe1 N1 -74.4(5) . . . . ? C7 N2 Fe1 N3 -165.7(7) . . . . ? C11 N2 Fe1 N3 -2.1(5) . . . . ? C7 N2 Fe1 Fe2 7.5(7) . . . 2_655 ? C11 N2 Fe1 Fe2 171.1(5) . . . 2_655 ? C7 N2 Fe1 Fe2 -34.6(11) . . . . ? C11 N2 Fe1 Fe2 129.0(6) . . . . ? C1 N1 Fe1 O4 6.4(7) . . . . ? C5 N1 Fe1 O4 -160.4(5) . . . . ? C1 N1 Fe1 O3 104.6(7) . . . . ? C5 N1 Fe1 O3 -62.2(6) . . . . ? C1 N1 Fe1 O1 -168.3(6) . . . . ? C5 N1 Fe1 O1 24.9(11) . . . . ? C1 N1 Fe1 N2 -88.7(7) . . . . ? C5 N1 Fe1 N2 104.5(6) . . . . ? C1 N1 Fe1 N3 -164.4(7) . . . . ? C5 N1 Fe1 N3 28.8(5) . . . . ? C1 N1 Fe1 Fe2 16.6(7) . . . 2_655 ? C5 N1 Fe1 Fe2 -150.2(5) . . . 2_655 ? C1 N1 Fe1 Fe2 83.5(7) . . . . ? C5 N1 Fe1 Fe2 -83.3(5) . . . . ? C12 N3 Fe1 O4 39.4(12) . . . . ? C13 N3 Fe1 O4 161.7(9) . . . . ? C6 N3 Fe1 O4 -79.3(11) . . . . ? C12 N3 Fe1 O3 169.4(5) . . . . ? C13 N3 Fe1 O3 -68.3(5) . . . . ? C6 N3 Fe1 O3 50.8(5) . . . . ? C12 N3 Fe1 O1 -99.4(4) . . . . ? C13 N3 Fe1 O1 23.0(4) . . . . ? C6 N3 Fe1 O1 142.0(5) . . . . ? C12 N3 Fe1 N2 -15.1(4) . . . . ? C13 N3 Fe1 N2 107.2(5) . . . . ? C6 N3 Fe1 N2 -133.7(5) . . . . ? C12 N3 Fe1 N1 81.8(5) . . . . ? C13 N3 Fe1 N1 -155.9(5) . . . . ? C6 N3 Fe1 N1 -36.8(5) . . . . ? C12 N3 Fe1 Fe2 -106.3(14) . . . 2_655 ? C13 N3 Fe1 Fe2 16.1(18) . . . 2_655 ? C6 N3 Fe1 Fe2 135.1(13) . . . 2_655 ? C12 N3 Fe1 Fe2 -179.2(4) . . . . ? C13 N3 Fe1 Fe2 -56.8(5) . . . . ? C6 N3 Fe1 Fe2 62.2(5) . . . . ? Fe1 O3 Fe2 O4 -55.7(3) . . . 2_655 ? Fe1 O3 Fe2 O2 37.8(3) . . . . ? Fe1 O3 Fe2 N6 166.5(7) . . . . ? Fe1 O3 Fe2 N5 119.6(3) . . . . ? Fe1 O3 Fe2 N4 -148.7(3) . . . . ? Fe1 O3 Fe2 Fe2 15.8(3) . . . 2_655 ? C36 O2 Fe2 O4 -129.31(16) . . . 2_655 ? Fe2 O2 Fe2 O4 50.69(16) 2_655 . . 2_655 ? C36 O2 Fe2 O3 131.82(15) . . . . ? Fe2 O2 Fe2 O3 -48.18(15) 2_655 . . . ? C36 O2 Fe2 N6 -33.38(19) . . . . ? Fe2 O2 Fe2 N6 146.62(19) 2_655 . . . ? C36 O2 Fe2 N5 44.29(17) . . . . ? Fe2 O2 Fe2 N5 -135.71(17) 2_655 . . . ? C36 O2 Fe2 N4 -27.2(6) . . . . ? Fe2 O2 Fe2 N4 152.8(6) 2_655 . . . ? C36 O2 Fe2 Fe1 148.65(2) . . . . ? Fe2 O2 Fe2 Fe1 -31.35(2) 2_655 . . . ? C36 O2 Fe2 Fe2 180.0 . . . 2_655 ? C27 N6 Fe2 O4 -51.2(6) . . . 2_655 ? C28 N6 Fe2 O4 -169.8(6) . . . 2_655 ? C34 N6 Fe2 O4 69.0(6) . . . 2_655 ? C27 N6 Fe2 O3 86.9(9) . . . . ? C28 N6 Fe2 O3 -31.7(12) . . . . ? C34 N6 Fe2 O3 -152.8(7) . . . . ? C27 N6 Fe2 O2 -142.5(5) . . . . ? C28 N6 Fe2 O2 99.0(6) . . . . ? C34 N6 Fe2 O2 -22.2(6) . . . . ? C27 N6 Fe2 N5 135.2(6) . . . . ? C28 N6 Fe2 N5 16.6(6) . . . . ? C34 N6 Fe2 N5 -104.5(6) . . . . ? C27 N6 Fe2 N4 39.6(5) . . . . ? C28 N6 Fe2 N4 -79.0(7) . . . . ? C34 N6 Fe2 N4 159.9(6) . . . . ? C27 N6 Fe2 Fe1 -131.1(10) . . . . ? C28 N6 Fe2 Fe1 110.4(11) . . . . ? C34 N6 Fe2 Fe1 -10.8(15) . . . . ? C27 N6 Fe2 Fe2 -125.0(5) . . . 2_655 ? C28 N6 Fe2 Fe2 116.4(6) . . . 2_655 ? C34 N6 Fe2 Fe2 -4.8(6) . . . 2_655 ? C33 N5 Fe2 O4 117.1(15) . . . 2_655 ? C29 N5 Fe2 O4 -42.4(19) . . . 2_655 ? C33 N5 Fe2 O3 -32.0(7) . . . . ? C29 N5 Fe2 O3 168.5(7) . . . . ? C33 N5 Fe2 O2 72.1(7) . . . . ? C29 N5 Fe2 O2 -87.4(6) . . . . ? C33 N5 Fe2 N6 162.1(7) . . . . ? C29 N5 Fe2 N6 2.6(6) . . . . ? C33 N5 Fe2 N4 -125.5(7) . . . . ? C29 N5 Fe2 N4 74.9(7) . . . . ? C33 N5 Fe2 Fe1 -7.4(7) . . . . ? C29 N5 Fe2 Fe1 -166.9(6) . . . . ? C33 N5 Fe2 Fe2 51.0(7) . . . 2_655 ? C29 N5 Fe2 Fe2 -108.5(6) . . . 2_655 ? C22 N4 Fe2 O4 -106.3(8) . . . 2_655 ? C26 N4 Fe2 O4 69.3(7) . . . 2_655 ? C22 N4 Fe2 O3 -7.8(8) . . . . ? C26 N4 Fe2 O3 167.8(7) . . . . ? C22 N4 Fe2 O2 151.8(7) . . . . ? C26 N4 Fe2 O2 -32.6(11) . . . . ? C22 N4 Fe2 N6 158.3(9) . . . . ? C26 N4 Fe2 N6 -26.1(7) . . . . ? C22 N4 Fe2 N5 81.8(8) . . . . ? C26 N4 Fe2 N5 -102.6(7) . . . . ? C22 N4 Fe2 Fe1 -23.6(9) . . . . ? C26 N4 Fe2 Fe1 152.0(6) . . . . ? C22 N4 Fe2 Fe2 -85.8(11) . . . 2_655 ? C26 N4 Fe2 Fe2 89.8(10) . . . 2_655 ? O4 Fe1 Fe2 O4 -90.24(16) . . . 2_655 ? O3 Fe1 Fe2 O4 124.4(4) . . . 2_655 ? O1 Fe1 Fe2 O4 13.59(19) . . . 2_655 ? N2 Fe1 Fe2 O4 -27.4(6) . . . 2_655 ? N1 Fe1 Fe2 O4 176.9(3) . . . 2_655 ? N3 Fe1 Fe2 O4 98.5(2) . . . 2_655 ? Fe2 Fe1 Fe2 O4 -74.43(17) 2_655 . . 2_655 ? O4 Fe1 Fe2 O3 145.3(4) . . . . ? O1 Fe1 Fe2 O3 -110.9(3) . . . . ? N2 Fe1 Fe2 O3 -151.8(7) . . . . ? N1 Fe1 Fe2 O3 52.4(4) . . . . ? N3 Fe1 Fe2 O3 -26.0(4) . . . . ? Fe2 Fe1 Fe2 O3 161.1(3) 2_655 . . . ? O4 Fe1 Fe2 O2 2.34(18) . . . . ? O3 Fe1 Fe2 O2 -143.0(3) . . . . ? O1 Fe1 Fe2 O2 106.16(12) . . . . ? N2 Fe1 Fe2 O2 65.2(6) . . . . ? N1 Fe1 Fe2 O2 -90.5(2) . . . . ? N3 Fe1 Fe2 O2 -168.97(19) . . . . ? Fe2 Fe1 Fe2 O2 18.14(9) 2_655 . . . ? O4 Fe1 Fe2 N6 -9.2(11) . . . . ? O3 Fe1 Fe2 N6 -154.5(12) . . . . ? O1 Fe1 Fe2 N6 94.6(11) . . . . ? N2 Fe1 Fe2 N6 53.7(13) . . . . ? N1 Fe1 Fe2 N6 -102.1(11) . . . . ? N3 Fe1 Fe2 N6 179.5(11) . . . . ? Fe2 Fe1 Fe2 N6 6.6(11) 2_655 . . . ? O4 Fe1 Fe2 N5 82.2(2) . . . . ? O3 Fe1 Fe2 N5 -63.1(4) . . . . ? O1 Fe1 Fe2 N5 -173.9(2) . . . . ? N2 Fe1 Fe2 N5 145.1(6) . . . . ? N1 Fe1 Fe2 N5 -10.6(3) . . . . ? N3 Fe1 Fe2 N5 -89.1(2) . . . . ? Fe2 Fe1 Fe2 N5 98.05(19) 2_655 . . . ? O4 Fe1 Fe2 N4 -179.1(3) . . . . ? O3 Fe1 Fe2 N4 35.5(4) . . . . ? O1 Fe1 Fe2 N4 -75.3(2) . . . . ? N2 Fe1 Fe2 N4 -116.3(6) . . . . ? N1 Fe1 Fe2 N4 88.0(3) . . . . ? N3 Fe1 Fe2 N4 9.5(3) . . . . ? Fe2 Fe1 Fe2 N4 -163.3(2) 2_655 . . . ? O4 Fe1 Fe2 Fe2 -15.80(16) . . . 2_655 ? O3 Fe1 Fe2 Fe2 -161.1(3) . . . 2_655 ? O1 Fe1 Fe2 Fe2 88.02(9) . . . 2_655 ? N2 Fe1 Fe2 Fe2 47.1(6) . . . 2_655 ? N1 Fe1 Fe2 Fe2 -108.7(2) . . . 2_655 ? N3 Fe1 Fe2 Fe2 172.89(17) . . . 2_655 ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 23.46 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.854 _refine_diff_density_min -0.733 _refine_diff_density_rms 0.104 data_fe76 _database_code_depnum_ccdc_archive 'CCDC 257919' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ; C72 H82 Fe4 N12 O4, 4(Cl O4), 2(C3 H6 O) ; _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C78 H94 Cl4 Fe2 N12 O22' _chemical_formula_weight 1805.15 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 15.180(3) _cell_length_b 10.722(2) _cell_length_c 25.921(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.24(3) _cell_angle_gamma 90.00 _cell_volume 4201.1(14) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used no _cell_measurement_theta_min 0.79 _cell_measurement_theta_max 27.00 _exptl_crystal_description Block _exptl_crystal_colour purple _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.427 _exptl_crystal_density_method ? _exptl_crystal_F_000 1884 _exptl_absorpt_coefficient_mu 0.552 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8229 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens SMART CCD Platform' _diffrn_measurement_method 'omega scans' _diffrn_standards_number no _diffrn_standards_interval_count no _diffrn_standards_interval_time no _diffrn_standards_decay_% 'no decay' _diffrn_reflns_number 26554 _diffrn_reflns_av_R_equivalents 0.0530 _diffrn_reflns_av_sigmaI/netI 0.1249 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 0.79 _diffrn_reflns_theta_max 27.00 _reflns_number_total 17248 _reflns_number_observed 11651 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXTL/PC (Sheldrick, 1994)' _computing_structure_refinement 'SHELXTL/PC (Sheldrick, 1994)' _computing_molecular_graphics 'X-Seed (L- J- Barbour)' _computing_publication_material 'WinGX (Farrugia, 1999)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 62 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+2.7429P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.15(2) _refine_ls_number_reflns 17186 _refine_ls_number_parameters 1079 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1210 _refine_ls_R_factor_obs 0.0700 _refine_ls_wR_factor_all 0.1555 _refine_ls_wR_factor_obs 0.1283 _refine_ls_goodness_of_fit_all 1.050 _refine_ls_goodness_of_fit_obs 1.074 _refine_ls_restrained_S_all 1.057 _refine_ls_restrained_S_obs 1.073 _refine_ls_shift/esd_max 0.143 _refine_ls_shift/esd_mean 0.011 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe1 Fe 0.40841(5) 0.19697(7) 0.22030(3) 0.0154(2) Uani 1 d . . Fe2 Fe 0.56698(5) 0.35685(7) 0.26700(3) 0.0156(2) Uani 1 d . . O1 O 0.5368(2) 0.1861(4) 0.24864(14) 0.0155(9) Uani 1 d . . H1 H 0.5735(2) 0.1143(4) 0.25211(14) 0.019 Uiso 1 calc R . O2 O 0.4388(2) 0.3684(4) 0.23938(14) 0.0166(9) Uani 1 d . . H2 H 0.4020(2) 0.4402(4) 0.23638(14) 0.020 Uiso 1 calc R . O3 O 0.2924(2) 0.2277(4) 0.1914(2) 0.0176(9) Uani 1 d . . C1 C 0.2512(4) 0.1645(5) 0.1512(2) 0.0155(13) Uani 1 d . . C2 C 0.2550(4) 0.0330(6) 0.1504(2) 0.0168(13) Uani 1 d . . C3 C 0.2970(4) -0.0371(6) 0.1964(2) 0.0190(13) Uani 1 d . . H31 H 0.2918(4) -0.1276(6) 0.1891(2) 0.023 Uiso 1 calc R . H32 H 0.2636(4) -0.0192(6) 0.2266(2) 0.023 Uiso 1 calc R . N1 N 0.3933(3) -0.0065(5) 0.2106(2) 0.0164(11) Uani 1 d . . C4 C 0.2047(4) 0.2282(5) 0.1106(2) 0.0144(13) Uani 1 d . . C5 C 0.1631(4) 0.1616(6) 0.0693(2) 0.0184(13) Uani 1 d . . H5 H 0.1319(4) 0.2059(6) 0.0416(2) 0.022 Uiso 1 calc R . C6 C 0.1658(4) 0.0315(6) 0.0673(2) 0.0172(13) Uani 1 d . . C7 C 0.2130(4) -0.0301(6) 0.1081(2) 0.0175(13) Uani 1 d . . H7 H 0.2169(4) -0.1184(6) 0.1071(2) 0.021 Uiso 1 calc R . C8 C 0.1227(4) -0.0399(6) 0.0198(2) 0.0186(13) Uani 1 d . . C9 C 0.1950(4) -0.0674(7) -0.0158(2) 0.033(2) Uani 1 d . . H91 H 0.2452(4) -0.1076(7) 0.0041(2) 0.039 Uiso 1 calc R . H92 H 0.2146(4) 0.0108(7) -0.0306(2) 0.039 Uiso 1 calc R . H93 H 0.1716(4) -0.1230(7) -0.0438(2) 0.039 Uiso 1 calc R . C10 C 0.0823(5) -0.1625(7) 0.0361(3) 0.033(2) Uani 1 d . . H101 H 0.0494(5) -0.2012(7) 0.0060(3) 0.039 Uiso 1 calc R . H102 H 0.0421(5) -0.1461(7) 0.0628(3) 0.039 Uiso 1 calc R . H103 H 0.1295(5) -0.2188(7) 0.0499(3) 0.039 Uiso 1 calc R . C11 C 0.0492(4) 0.0367(6) -0.0102(3) 0.032(2) Uani 1 d . . H111 H 0.0757(4) 0.1053(6) -0.0283(3) 0.039 Uiso 1 calc R . H112 H 0.0095(4) 0.0706(6) 0.0141(3) 0.039 Uiso 1 calc R . H113 H 0.0155(4) -0.0171(6) -0.0354(3) 0.039 Uiso 1 calc R . C12 C 0.2004(4) 0.3682(6) 0.1105(2) 0.0190(13) Uani 1 d . . H121 H 0.1934(4) 0.3981(6) 0.0742(2) 0.023 Uiso 1 calc R . H122 H 0.2568(4) 0.4017(6) 0.1270(2) 0.023 Uiso 1 calc R . N13 N 0.1241(3) 0.4188(4) 0.1391(2) 0.0180(11) Uani 1 d . . H13 H 0.0727(3) 0.3803(4) 0.1248(2) 0.022 Uiso 1 calc R . C14 C 0.1129(4) 0.5552(5) 0.1304(2) 0.0220(14) Uani 1 d . . H141 H 0.1195(4) 0.5751(5) 0.0937(2) 0.026 Uiso 1 calc R . H142 H 0.1591(4) 0.6011(5) 0.1521(2) 0.026 Uiso 1 calc R . C15 C 0.0223(4) 0.5956(6) 0.1440(2) 0.0216(14) Uani 1 d . . N16 N -0.0394(3) 0.5049(5) 0.1411(2) 0.0241(12) Uani 1 d . . C17 C -0.1218(4) 0.5363(7) 0.1506(3) 0.029(2) Uani 1 d . . H17 H -0.1656(4) 0.4728(7) 0.1493(3) 0.034 Uiso 1 calc R . C18 C -0.1461(4) 0.6564(7) 0.1620(2) 0.033(2) Uani 1 d . . H18 H -0.2055(4) 0.6756(7) 0.1679(2) 0.039 Uiso 1 calc R . C19 C -0.0821(5) 0.7475(7) 0.1648(3) 0.037(2) Uani 1 d . . H19 H -0.0970(5) 0.8311(7) 0.1724(3) 0.044 Uiso 1 calc R . C20 C 0.0044(4) 0.7173(6) 0.1564(2) 0.028(2) Uani 1 d . . H20 H 0.0498(4) 0.7786(6) 0.1592(2) 0.034 Uiso 1 calc R . C21 C 0.1333(4) 0.3888(6) 0.1953(2) 0.0178(14) Uani 1 d . . H211 H 0.1030(4) 0.4536(6) 0.2144(2) 0.021 Uiso 1 calc R . H212 H 0.1967(4) 0.3893(6) 0.2083(2) 0.021 Uiso 1 calc R . C22 C 0.0944(4) 0.2634(6) 0.2057(2) 0.0207(14) Uani 1 d . . N23 N 0.0354(3) 0.2178(5) 0.1692(2) 0.0238(12) Uani 1 d . . C24 C 0.0007(5) 0.1057(7) 0.1776(3) 0.038(2) Uani 1 d . . H24 H -0.0412(5) 0.0722(7) 0.1519(3) 0.045 Uiso 1 calc R . C25 C 0.0225(5) 0.0362(7) 0.2217(3) 0.040(2) Uani 1 d . . H25 H -0.0029(5) -0.0437(7) 0.2259(3) 0.048 Uiso 1 calc R . C26 C 0.0822(5) 0.0861(7) 0.2594(3) 0.038(2) Uani 1 d . . H26 H 0.0972(5) 0.0414(7) 0.2906(3) 0.046 Uiso 1 calc R . C27 C 0.1203(4) 0.2012(6) 0.2518(2) 0.0234(14) Uani 1 d . . H27 H 0.1626(4) 0.2363(6) 0.2769(2) 0.028 Uiso 1 calc R . C28 C 0.4208(4) -0.0627(6) 0.2624(2) 0.0191(14) Uani 1 d . . H281 H 0.4862(4) -0.0645(6) 0.2682(2) 0.023 Uiso 1 calc R . H282 H 0.3989(4) -0.1495(6) 0.2635(2) 0.023 Uiso 1 calc R . C29 C 0.3839(4) 0.0127(5) 0.3039(2) 0.0176(13) Uani 1 d . . C30 C 0.3666(4) -0.0380(7) 0.3516(2) 0.0267(15) Uani 1 d . . H30 H 0.3769(4) -0.1239(7) 0.3588(2) 0.032 Uiso 1 calc R . C31 C 0.3346(5) 0.0392(7) 0.3876(3) 0.036(2) Uani 1 d . . H311 H 0.3240(5) 0.0072(7) 0.4207(3) 0.043 Uiso 1 calc R . C32 C 0.3178(4) 0.1626(6) 0.3763(3) 0.029(2) Uani 1 d . . H321 H 0.2930(4) 0.2150(6) 0.4007(3) 0.035 Uiso 1 calc R . C33 C 0.3376(4) 0.2101(7) 0.3287(2) 0.0237(14) Uani 1 d . . H33 H 0.3282(4) 0.2959(7) 0.3210(2) 0.028 Uiso 1 calc R . N2 N 0.3701(3) 0.1341(5) 0.2933(2) 0.0182(11) Uani 1 d . . C34 C 0.4486(4) -0.0500(6) 0.1706(2) 0.0200(13) Uani 1 d . . H341 H 0.4231(4) -0.1277(6) 0.1549(2) 0.024 Uiso 1 calc R . H342 H 0.5086(4) -0.0694(6) 0.1868(2) 0.024 Uiso 1 calc R . C35 C 0.4550(4) 0.0460(6) 0.1290(2) 0.0206(14) Uani 1 d . . C36 C 0.4736(4) 0.0170(7) 0.0789(3) 0.028(2) Uani 1 d . . H36 H 0.4817(4) -0.0673(7) 0.0691(3) 0.034 Uiso 1 calc R . C37 C 0.4802(4) 0.1125(7) 0.0433(2) 0.028(2) Uani 1 d . . H37 H 0.4936(4) 0.0944(7) 0.0090(2) 0.033 Uiso 1 calc R . C38 C 0.4673(4) 0.2334(6) 0.0583(2) 0.026(2) Uani 1 d . . H38 H 0.4710(4) 0.2997(6) 0.0343(2) 0.031 Uiso 1 calc R . C39 C 0.4487(4) 0.2582(6) 0.1086(2) 0.0213(14) Uani 1 d . . H39 H 0.4388(4) 0.3419(6) 0.1186(2) 0.026 Uiso 1 calc R . N3 N 0.4446(3) 0.1659(4) 0.1437(2) 0.0149(11) Uani 1 d . . O4 O 0.6846(3) 0.3217(4) 0.2942(2) 0.0183(10) Uani 1 d . . C40 C 0.7243(4) 0.3831(6) 0.3351(2) 0.0191(14) Uani 1 d . . C41 C 0.7263(4) 0.5128(6) 0.3368(2) 0.0185(14) Uani 1 d . . C42 C 0.6830(4) 0.5869(6) 0.2918(2) 0.0203(14) Uani 1 d . . H421 H 0.6896(4) 0.6769(6) 0.2998(2) 0.024 Uiso 1 calc R . H422 H 0.7144(4) 0.5698(6) 0.2607(2) 0.024 Uiso 1 calc R . N4 N 0.5863(3) 0.5582(5) 0.2795(2) 0.0170(11) Uani 1 d . . C43 C 0.7644(4) 0.3140(6) 0.3779(2) 0.0198(14) Uani 1 d . . C44 C 0.8089(4) 0.3773(6) 0.4188(2) 0.0221(14) Uani 1 d . . H44 H 0.8351(4) 0.3305(6) 0.4473(2) 0.027 Uiso 1 calc R . C45 C 0.8169(4) 0.5071(6) 0.4199(2) 0.0203(14) Uani 1 d . . C46 C 0.7719(4) 0.5730(6) 0.3787(2) 0.0209(14) Uani 1 d . . H46 H 0.7725(4) 0.6616(6) 0.3794(2) 0.025 Uiso 1 calc R . C47 C 0.8666(4) 0.5741(6) 0.4662(2) 0.0208(14) Uani 1 d . . C48 C 0.8053(5) 0.5802(8) 0.5101(3) 0.042(2) Uani 1 d . . H481 H 0.7503(5) 0.6228(8) 0.4977(3) 0.050 Uiso 1 calc R . H482 H 0.8347(5) 0.6262(8) 0.5395(3) 0.050 Uiso 1 calc R . H483 H 0.7918(5) 0.4954(8) 0.5211(3) 0.050 Uiso 1 calc R . C49 C 0.8935(6) 0.7067(8) 0.4526(3) 0.054(2) Uani 1 d . . H491 H 0.8403(6) 0.7565(8) 0.4432(3) 0.065 Uiso 1 calc R . H492 H 0.9299(6) 0.7041(8) 0.4233(3) 0.065 Uiso 1 calc R . H493 H 0.9274(6) 0.7444(8) 0.4826(3) 0.065 Uiso 1 calc R . C50 C 0.9508(4) 0.5039(8) 0.4841(3) 0.038(2) Uani 1 d . . H501 H 0.9360(4) 0.4179(8) 0.4929(3) 0.046 Uiso 1 calc R . H502 H 0.9802(4) 0.5450(8) 0.5148(3) 0.046 Uiso 1 calc R . H503 H 0.9904(4) 0.5033(8) 0.4563(3) 0.046 Uiso 1 calc R . C51 C 0.7575(4) 0.1744(6) 0.3784(2) 0.025(2) Uani 1 d . . H511 H 0.7029(4) 0.1491(6) 0.3571(2) 0.030 Uiso 1 calc R . H512 H 0.7521(4) 0.1463(6) 0.4143(2) 0.030 Uiso 1 calc R . N52 N 0.8362(3) 0.1093(5) 0.3579(2) 0.0190(11) Uani 1 d . . H52 H 0.8856(3) 0.1273(5) 0.3806(2) 0.023 Uiso 1 calc R . C53 C 0.8237(4) -0.0307(6) 0.3582(3) 0.0246(14) Uani 1 d . . H531 H 0.7791(4) -0.0558(6) 0.3298(3) 0.030 Uiso 1 calc R . H532 H 0.8028(4) -0.0577(6) 0.3915(3) 0.030 Uiso 1 calc R . C54 C 0.9121(4) -0.0906(6) 0.3508(2) 0.0243(14) Uani 1 d . . C55 C 0.9241(5) -0.1756(6) 0.3126(2) 0.031(2) Uani 1 d . . H55 H 0.8761(5) -0.2027(6) 0.2892(2) 0.038 Uiso 1 calc R . C56 C 1.0104(5) -0.2212(7) 0.3094(3) 0.035(2) Uani 1 d . . H56 H 1.0222(5) -0.2776(7) 0.2827(3) 0.042 Uiso 1 calc R . C57 C 1.0765(5) -0.1840(6) 0.3449(3) 0.032(2) Uani 1 d . . H57 H 1.1348(5) -0.2154(6) 0.3438(3) 0.039 Uiso 1 calc R . C58 C 1.0572(4) -0.0996(7) 0.3825(3) 0.033(2) Uani 1 d . . H58 H 1.1036(4) -0.0745(7) 0.4074(3) 0.039 Uiso 1 calc R . N59 N 0.9770(3) -0.0516(5) 0.3856(2) 0.0264(12) Uani 1 d . . C60 C 0.8542(4) 0.1569(6) 0.3055(2) 0.0194(14) Uani 1 d . . H601 H 0.7981(4) 0.1830(6) 0.2860(2) 0.023 Uiso 1 calc R . H602 H 0.8807(4) 0.0897(6) 0.2857(2) 0.023 Uiso 1 calc R . C61 C 0.9173(4) 0.2671(6) 0.3116(3) 0.0224(15) Uani 1 d . . N62 N 0.9755(3) 0.2615(5) 0.3532(2) 0.0270(13) Uani 1 d . . C63 C 1.0336(4) 0.3560(7) 0.3594(3) 0.034(2) Uani 1 d . . H63 H 1.0764(4) 0.3540(7) 0.3886(3) 0.041 Uiso 1 calc R . C64 C 1.0345(4) 0.4568(7) 0.3256(3) 0.036(2) Uani 1 d . . H64 H 1.0764(4) 0.5223(7) 0.3312(3) 0.043 Uiso 1 calc R . C65 C 0.9723(5) 0.4574(7) 0.2837(3) 0.037(2) Uani 1 d . . H65 H 0.9704(5) 0.5248(7) 0.2598(3) 0.045 Uiso 1 calc R . C66 C 0.9127(4) 0.3611(7) 0.2761(3) 0.029(2) Uani 1 d . . H66 H 0.8697(4) 0.3603(7) 0.2471(3) 0.035 Uiso 1 calc R . C67 C 0.5334(4) 0.6006(6) 0.3218(2) 0.0216(14) Uani 1 d . . H671 H 0.4722(4) 0.6197(6) 0.3075(2) 0.026 Uiso 1 calc R . H672 H 0.5597(4) 0.6775(6) 0.3377(2) 0.026 Uiso 1 calc R . C68 C 0.5320(4) 0.4992(6) 0.3626(2) 0.0186(13) Uani 1 d . . N5 N 0.5342(3) 0.3810(4) 0.3446(2) 0.0173(11) Uani 1 d . . C69 C 0.5254(4) 0.5255(7) 0.4143(3) 0.028(2) Uani 1 d . . H69 H 0.5239(4) 0.6093(7) 0.4261(3) 0.034 Uiso 1 calc R . C70 C 0.5209(5) 0.4272(7) 0.4484(3) 0.034(2) Uani 1 d . . H70 H 0.5157(5) 0.4426(7) 0.4841(3) 0.041 Uiso 1 calc R . C71 C 0.5240(4) 0.3082(7) 0.4305(3) 0.027(2) Uani 1 d . . H71 H 0.5212(4) 0.2399(7) 0.4537(3) 0.032 Uiso 1 calc R . C72 C 0.5311(4) 0.2870(6) 0.3788(2) 0.0214(14) Uani 1 d . . H72 H 0.5339(4) 0.2035(6) 0.3669(2) 0.026 Uiso 1 calc R . C73 C 0.5556(4) 0.6192(6) 0.2290(2) 0.0199(14) Uani 1 d . . H731 H 0.4902(4) 0.6212(6) 0.2246(2) 0.024 Uiso 1 calc R . H732 H 0.5775(4) 0.7062(6) 0.2288(2) 0.024 Uiso 1 calc R . C74 C 0.5899(4) 0.5476(6) 0.1855(2) 0.0217(14) Uani 1 d . . C75 C 0.6033(4) 0.5996(7) 0.1382(2) 0.0263(15) Uani 1 d . . H75 H 0.5920(4) 0.6857(7) 0.1322(2) 0.032 Uiso 1 calc R . C76 C 0.6330(4) 0.5270(7) 0.1000(3) 0.030(2) Uani 1 d . . H76 H 0.6420(4) 0.5623(7) 0.0673(3) 0.036 Uiso 1 calc R . C77 C 0.6500(4) 0.4013(7) 0.1094(2) 0.027(2) Uani 1 d . . H77 H 0.6711(4) 0.3495(7) 0.0834(2) 0.032 Uiso 1 calc R . C78 C 0.6356(4) 0.3537(6) 0.1572(2) 0.0198(13) Uani 1 d . . H78 H 0.6483(4) 0.2683(6) 0.1643(2) 0.024 Uiso 1 calc R . N6 N 0.6039(3) 0.4245(5) 0.1944(2) 0.0187(12) Uani 1 d . . Cl1 Cl 0.26349(10) 0.60407(15) 0.28066(6) 0.0234(3) Uani 1 d . . O5 O 0.1817(3) 0.6528(4) 0.2568(2) 0.0330(11) Uani 1 d . . O6 O 0.2481(3) 0.4869(4) 0.3057(2) 0.0378(12) Uani 1 d . . O7 O 0.3030(3) 0.6914(6) 0.3175(2) 0.053(2) Uani 1 d . . O8 O 0.3232(3) 0.5827(5) 0.2415(2) 0.0432(14) Uani 1 d . . Cl2 Cl 0.59178(11) 0.9070(2) 0.41509(6) 0.0276(4) Uani 1 d . . O9 O 0.5961(4) 1.0216(5) 0.4431(2) 0.051(2) Uani 1 d . . O10 O 0.5169(3) 0.8361(5) 0.4288(2) 0.0394(13) Uani 1 d . . O11 O 0.5832(4) 0.9345(6) 0.3604(2) 0.062(2) Uani 1 d . . O12 O 0.6704(4) 0.8359(6) 0.4282(3) 0.072(2) Uani 1 d . . Cl3 Cl 0.37060(10) 0.6283(2) 0.08081(6) 0.0271(4) Uani 1 d . . O13 O 0.3888(4) 0.5159(5) 0.0556(2) 0.053(2) Uani 1 d . . O14 O 0.3916(17) 0.5921(35) 0.1373(9) 0.063(6) Uani 0.62(5) d P . O14' O 0.3856(29) 0.6481(47) 0.1313(15) 0.063(6) Uani 0.38(5) d P . O15 O 0.2796(3) 0.6590(6) 0.0704(2) 0.059(2) Uani 1 d . . O16 O 0.4257(4) 0.7233(5) 0.0629(3) 0.067(2) Uani 1 d . . Cl4 Cl 0.70749(10) 0.9621(2) 0.20603(6) 0.0243(4) Uani 1 d . . O17 O 0.6646(4) 0.9899(6) 0.2519(2) 0.060(2) Uani 1 d . . O18' O 0.6789(7) 0.8541(10) 0.1827(5) 0.110(5) Uani 0.795(12) d P . O18 O 0.7401(26) 0.8378(35) 0.2235(19) 0.110(5) Uani 0.205(12) d P . O19 O 0.7971(4) 0.9718(10) 0.2112(3) 0.135(4) Uani 1 d . . O20 O 0.6754(8) 1.0528(11) 0.1699(4) 0.131(6) Uani 0.779(13) d P . O20' O 0.6525(32) 0.9398(45) 0.1635(17) 0.131(6) Uani 0.221(13) d P . OA O 0.8223(5) 0.1205(13) 0.5026(5) 0.082(4) Uani 0.78(2) d P . OA' O 0.8269(21) 0.1965(51) 0.5316(16) 0.082(4) Uani 0.22(2) d P . C1A C 0.7647(6) 0.1047(11) 0.5323(3) 0.061(3) Uani 1 d . . C2A C 0.6958(7) 0.1945(10) 0.5451(4) 0.074(3) Uani 1 d . . H21 H 0.6975(7) 0.2036(10) 0.5828(4) 0.088 Uiso 1 calc R . H22 H 0.6375(7) 0.1637(10) 0.5315(4) 0.088 Uiso 1 calc R . H23 H 0.7068(7) 0.2756(10) 0.5295(4) 0.088 Uiso 1 calc R . C3A C 0.7547(6) -0.0249(10) 0.5516(4) 0.071(3) Uiso 1 d . . H3A1 H 0.6964(6) -0.0574(10) 0.5387(4) 0.086 Uiso 1 calc R . H3A2 H 0.7601(6) -0.0247(10) 0.5896(4) 0.086 Uiso 1 calc R . H3A3 H 0.8009(6) -0.0780(10) 0.5392(4) 0.086 Uiso 1 calc R . OB O 0.8545(5) 0.9120(9) 0.0213(4) 0.083(3) Uani 0.803(10) d P . OB' O 0.8694(21) 0.9300(36) 0.0677(16) 0.083(3) Uani 0.197(10) d P . C1B C 0.7893(6) 0.9469(9) 0.0433(4) 0.054(2) Uani 1 d . . C2B C 0.7730(7) 1.0764(8) 0.0599(3) 0.065(3) Uani 1 d . . H41 H 0.7501(7) 1.0753(8) 0.0941(3) 0.078 Uiso 1 calc R . H42 H 0.7296(7) 1.1160(8) 0.0348(3) 0.078 Uiso 1 calc R . H43 H 0.8285(7) 1.1236(8) 0.0619(3) 0.078 Uiso 1 calc R . C3B C 0.7181(5) 0.8564(9) 0.0453(3) 0.054(2) Uani 1 d . . H3B1 H 0.6659(5) 0.8854(9) 0.0236(3) 0.065 Uiso 1 calc R . H3B2 H 0.7035(5) 0.8473(9) 0.0812(3) 0.065 Uiso 1 calc R . H3B3 H 0.7372(5) 0.7757(9) 0.0325(3) 0.065 Uiso 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 0.0149(4) 0.0144(4) 0.0172(4) 0.0001(4) 0.0039(3) 0.0015(4) Fe2 0.0155(4) 0.0156(5) 0.0161(4) -0.0001(4) 0.0034(3) 0.0014(4) O1 0.013(2) 0.016(2) 0.018(2) -0.002(2) 0.003(2) 0.006(2) O2 0.015(2) 0.016(2) 0.019(2) 0.000(2) 0.002(2) 0.002(2) O3 0.015(2) 0.018(2) 0.020(2) -0.005(2) 0.002(2) 0.002(2) C1 0.012(3) 0.018(3) 0.017(3) -0.003(3) 0.004(2) -0.001(2) C2 0.012(3) 0.012(3) 0.028(4) 0.003(3) 0.008(3) 0.003(2) C3 0.021(3) 0.019(3) 0.018(3) -0.001(3) 0.009(3) 0.003(3) N1 0.017(3) 0.016(3) 0.017(3) 0.002(2) 0.008(2) 0.008(2) C4 0.013(3) 0.010(3) 0.022(3) -0.004(2) 0.007(2) 0.001(2) C5 0.017(3) 0.025(4) 0.015(3) 0.003(3) 0.006(2) 0.004(2) C6 0.017(3) 0.018(3) 0.017(3) 0.000(3) 0.005(3) -0.004(2) C7 0.018(3) 0.016(3) 0.020(3) -0.001(3) 0.008(3) 0.000(3) C8 0.018(3) 0.020(3) 0.018(3) -0.004(3) 0.002(2) -0.001(3) C9 0.042(4) 0.039(5) 0.018(4) -0.009(3) 0.003(3) -0.001(3) C10 0.039(4) 0.029(4) 0.028(4) 0.003(3) -0.007(3) -0.011(3) C11 0.035(4) 0.027(4) 0.032(4) -0.005(3) -0.011(3) 0.005(3) C12 0.015(3) 0.019(3) 0.024(3) 0.003(3) 0.009(2) 0.006(3) N13 0.020(3) 0.015(3) 0.020(3) 0.002(2) 0.005(2) 0.005(2) C14 0.033(4) 0.013(3) 0.022(3) 0.001(3) 0.012(3) -0.001(3) C15 0.020(3) 0.031(4) 0.013(3) 0.006(3) 0.001(2) 0.008(3) N16 0.020(3) 0.029(3) 0.023(3) -0.003(2) 0.003(2) 0.002(2) C17 0.014(3) 0.039(4) 0.032(4) 0.002(3) -0.001(3) 0.001(3) C18 0.022(4) 0.049(5) 0.028(4) -0.001(3) 0.004(3) 0.010(3) C19 0.035(4) 0.036(5) 0.039(4) -0.012(4) 0.005(3) 0.019(4) C20 0.032(4) 0.025(4) 0.029(4) -0.001(3) 0.012(3) 0.007(3) C21 0.021(3) 0.020(4) 0.013(3) 0.002(2) 0.004(2) -0.001(3) C22 0.016(3) 0.024(4) 0.024(4) -0.002(3) 0.008(3) 0.002(3) N23 0.028(3) 0.014(3) 0.030(3) -0.003(2) 0.007(2) -0.004(2) C24 0.044(5) 0.027(4) 0.043(5) -0.004(4) 0.017(4) -0.017(4) C25 0.045(5) 0.035(5) 0.043(5) 0.002(4) 0.019(4) -0.009(4) C26 0.043(4) 0.040(5) 0.036(4) 0.009(4) 0.026(3) 0.002(4) C27 0.023(3) 0.026(4) 0.023(3) 0.001(3) 0.009(3) -0.002(3) C28 0.021(3) 0.017(3) 0.020(3) 0.004(3) 0.002(3) 0.001(3) C29 0.018(3) 0.014(3) 0.020(3) 0.002(3) -0.001(3) 0.000(2) C30 0.034(4) 0.025(4) 0.022(4) 0.009(3) 0.008(3) -0.001(3) C31 0.055(5) 0.038(5) 0.018(4) -0.001(3) 0.019(3) -0.007(4) C32 0.031(4) 0.024(4) 0.034(4) -0.003(3) 0.017(3) -0.004(3) C33 0.023(3) 0.026(4) 0.023(3) -0.003(3) 0.006(3) -0.006(3) N2 0.016(3) 0.018(3) 0.021(3) -0.004(2) 0.007(2) -0.001(2) C34 0.030(3) 0.017(3) 0.014(3) -0.006(3) 0.006(3) 0.007(3) C35 0.014(3) 0.020(3) 0.027(4) -0.001(3) -0.003(3) 0.006(2) C36 0.028(4) 0.033(4) 0.024(4) -0.003(3) 0.008(3) 0.006(3) C37 0.030(4) 0.034(4) 0.021(3) -0.007(3) 0.006(3) -0.002(3) C38 0.022(3) 0.034(4) 0.020(3) 0.006(3) -0.002(3) -0.005(3) C39 0.019(3) 0.019(3) 0.027(4) 0.001(3) 0.003(3) -0.005(3) N3 0.011(2) 0.016(3) 0.018(3) -0.001(2) 0.004(2) 0.000(2) O4 0.011(2) 0.021(3) 0.023(2) -0.003(2) 0.002(2) 0.003(2) C40 0.016(3) 0.020(4) 0.022(3) 0.001(3) 0.010(3) 0.004(3) C41 0.013(3) 0.025(4) 0.018(3) 0.000(3) 0.004(3) 0.004(3) C42 0.018(3) 0.015(3) 0.027(4) 0.007(3) 0.000(3) -0.004(3) N4 0.014(3) 0.020(3) 0.017(3) 0.000(2) 0.002(2) 0.001(2) C43 0.014(3) 0.026(4) 0.020(3) 0.005(3) 0.007(3) 0.005(3) C44 0.019(3) 0.030(4) 0.017(3) 0.004(3) 0.004(3) 0.003(3) C45 0.015(3) 0.025(4) 0.020(3) 0.002(3) 0.002(3) 0.001(3) C46 0.019(3) 0.022(4) 0.022(4) 0.004(3) 0.002(3) 0.005(3) C47 0.028(4) 0.022(4) 0.012(3) 0.002(3) 0.000(3) -0.002(3) C48 0.043(5) 0.057(6) 0.025(4) -0.006(4) 0.005(3) -0.003(4) C49 0.075(6) 0.053(6) 0.029(4) 0.006(4) -0.014(4) -0.034(5) C50 0.029(4) 0.063(6) 0.022(4) -0.002(4) -0.006(3) 0.008(4) C51 0.023(3) 0.032(4) 0.022(3) 0.002(3) 0.010(3) 0.004(3) N52 0.018(3) 0.024(3) 0.014(3) 0.002(2) 0.001(2) -0.002(2) C53 0.034(4) 0.011(3) 0.029(4) 0.003(3) 0.002(3) -0.002(3) C54 0.031(4) 0.021(3) 0.021(3) 0.007(3) 0.005(3) 0.005(3) C55 0.055(5) 0.022(4) 0.017(3) 0.004(3) 0.003(3) 0.002(3) C56 0.050(5) 0.026(4) 0.030(4) -0.002(3) 0.014(4) 0.011(3) C57 0.040(4) 0.029(4) 0.029(4) 0.005(3) 0.006(3) 0.015(3) C58 0.035(4) 0.038(4) 0.024(4) -0.002(3) -0.003(3) 0.008(3) N59 0.028(3) 0.027(3) 0.025(3) -0.002(2) 0.007(2) 0.006(2) C60 0.023(3) 0.021(3) 0.016(3) 0.003(3) 0.005(3) 0.008(3) C61 0.013(3) 0.029(4) 0.027(4) -0.004(3) 0.010(3) 0.006(3) N62 0.021(3) 0.025(3) 0.035(3) 0.002(3) 0.008(2) -0.001(2) C63 0.027(4) 0.038(4) 0.037(4) -0.009(4) 0.005(3) -0.002(3) C64 0.030(4) 0.026(4) 0.053(5) -0.006(4) 0.018(4) -0.010(3) C65 0.040(4) 0.025(4) 0.051(5) -0.001(4) 0.026(4) -0.001(3) C66 0.034(4) 0.025(4) 0.032(4) 0.003(3) 0.014(3) 0.005(3) C67 0.027(3) 0.021(3) 0.018(3) 0.005(3) 0.007(3) 0.003(3) C68 0.014(3) 0.020(3) 0.022(3) 0.000(3) 0.007(3) 0.002(2) N5 0.021(3) 0.015(3) 0.017(3) -0.001(2) 0.005(2) 0.004(2) C69 0.040(4) 0.022(4) 0.025(4) -0.006(3) 0.013(3) 0.004(3) C70 0.046(5) 0.038(5) 0.021(4) 0.002(3) 0.012(3) -0.005(3) C71 0.025(4) 0.030(4) 0.025(4) 0.008(3) 0.005(3) 0.004(3) C72 0.015(3) 0.025(4) 0.024(4) -0.001(3) 0.002(3) 0.003(3) C73 0.025(3) 0.019(3) 0.015(3) 0.004(3) -0.004(3) 0.008(3) C74 0.018(3) 0.026(4) 0.021(3) 0.001(3) 0.001(3) -0.003(3) C75 0.029(4) 0.027(4) 0.024(4) 0.005(3) 0.005(3) -0.004(3) C76 0.022(4) 0.039(5) 0.028(4) 0.016(3) 0.002(3) -0.001(3) C77 0.021(3) 0.040(4) 0.021(3) -0.005(3) 0.008(3) -0.007(3) C78 0.019(3) 0.018(3) 0.022(3) 0.001(3) 0.002(3) 0.002(3) N6 0.016(3) 0.024(3) 0.016(3) -0.003(2) 0.003(2) -0.002(2) Cl1 0.0220(8) 0.0222(8) 0.0271(9) -0.0042(7) 0.0089(7) -0.0011(7) O5 0.025(2) 0.033(3) 0.041(3) -0.003(2) 0.002(2) 0.010(2) O6 0.040(3) 0.029(3) 0.046(3) 0.015(2) 0.019(2) -0.006(2) O7 0.050(3) 0.051(4) 0.057(4) -0.033(3) -0.004(3) -0.013(3) O8 0.039(3) 0.051(4) 0.044(3) 0.009(3) 0.032(2) 0.019(3) Cl2 0.0311(9) 0.0269(9) 0.0260(9) -0.0019(7) 0.0084(7) -0.0012(7) O9 0.083(4) 0.025(3) 0.050(3) -0.013(3) 0.023(3) -0.015(3) O10 0.041(3) 0.040(3) 0.039(3) -0.001(2) 0.016(2) -0.018(2) O11 0.069(4) 0.102(6) 0.016(3) 0.007(3) 0.008(3) -0.031(4) O12 0.041(3) 0.074(5) 0.104(5) 0.033(4) 0.026(3) 0.024(3) Cl3 0.0263(9) 0.0308(10) 0.0251(9) -0.0050(7) 0.0079(7) -0.0018(7) O13 0.080(4) 0.023(3) 0.062(4) -0.001(3) 0.031(3) 0.008(3) O14 0.051(5) 0.125(22) 0.014(6) 0.020(10) 0.002(4) 0.006(12) O14' 0.051(5) 0.125(22) 0.014(6) 0.020(10) 0.002(4) 0.006(12) O15 0.033(3) 0.066(4) 0.077(4) 0.017(3) 0.005(3) 0.019(3) O16 0.078(4) 0.036(4) 0.096(5) -0.022(3) 0.051(4) -0.033(3) Cl4 0.0205(8) 0.0280(9) 0.0246(9) -0.0055(7) 0.0039(7) 0.0041(7) O17 0.068(4) 0.088(5) 0.026(3) -0.005(3) 0.017(3) 0.045(4) O18' 0.075(7) 0.087(7) 0.182(12) -0.115(8) 0.079(7) -0.057(6) O18 0.075(7) 0.087(7) 0.182(12) -0.115(8) 0.079(7) -0.057(6) O19 0.033(4) 0.250(11) 0.120(7) -0.136(7) -0.002(4) 0.006(5) O20 0.180(11) 0.108(9) 0.125(8) 0.092(8) 0.115(8) 0.120(9) O20' 0.180(11) 0.108(9) 0.125(8) 0.092(8) 0.115(8) 0.120(9) OA 0.048(4) 0.134(11) 0.064(8) 0.045(7) 0.013(5) 0.013(6) OA' 0.048(4) 0.134(11) 0.064(8) 0.045(7) 0.013(5) 0.013(6) C1A 0.045(5) 0.090(8) 0.047(6) 0.034(6) 0.000(4) -0.005(5) C2A 0.110(8) 0.051(6) 0.058(6) -0.006(5) 0.000(6) 0.011(6) OB 0.049(5) 0.102(7) 0.103(8) -0.056(6) 0.030(5) -0.017(4) OB' 0.049(5) 0.102(7) 0.103(8) -0.056(6) 0.030(5) -0.017(4) C1B 0.042(5) 0.055(6) 0.065(6) 0.005(5) 0.006(5) -0.007(4) C2B 0.101(8) 0.048(6) 0.045(5) -0.007(4) -0.002(5) -0.029(5) C3B 0.057(5) 0.060(6) 0.045(5) -0.007(5) 0.002(4) -0.016(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O3 1.879(4) . ? Fe1 O2 1.948(4) . ? Fe1 O1 2.022(4) . ? Fe1 N3 2.134(5) . ? Fe1 N2 2.139(5) . ? Fe1 N1 2.205(5) . ? Fe2 O4 1.897(4) . ? Fe2 O1 1.936(4) . ? Fe2 O2 2.015(4) . ? Fe2 N5 2.130(5) . ? Fe2 N6 2.139(5) . ? Fe2 N4 2.199(5) . ? O1 H1 0.95 . ? O2 H2 0.95 . ? O3 C1 1.348(7) . ? C1 C4 1.392(8) . ? C1 C2 1.411(8) . ? C2 C7 1.393(8) . ? C2 C3 1.501(8) . ? C3 N1 1.511(7) . ? C3 H31 0.99 . ? C3 H32 0.99 . ? N1 C34 1.469(7) . ? N1 C28 1.495(7) . ? C4 C5 1.390(8) . ? C4 C12 1.502(8) . ? C5 C6 1.397(8) . ? C5 H5 0.95 . ? C6 C7 1.388(8) . ? C6 C8 1.545(8) . ? C7 H7 0.95 . ? C8 C10 1.525(9) . ? C8 C9 1.526(8) . ? C8 C11 1.538(8) . ? C9 H91 0.98 . ? C9 H92 0.98 . ? C9 H93 0.98 . ? C10 H101 0.98 . ? C10 H102 0.98 . ? C10 H103 0.98 . ? C11 H111 0.98 . ? C11 H112 0.98 . ? C11 H113 0.98 . ? C12 N13 1.529(7) . ? C12 H121 0.99 . ? C12 H122 0.99 . ? N13 C21 1.487(7) . ? N13 C14 1.488(7) . ? N13 H13 0.93 . ? C14 C15 1.514(8) . ? C14 H141 0.99 . ? C14 H142 0.99 . ? C15 N16 1.347(8) . ? C15 C20 1.377(9) . ? N16 C17 1.340(8) . ? C17 C18 1.379(9) . ? C17 H17 0.95 . ? C18 C19 1.376(10) . ? C18 H18 0.95 . ? C19 C20 1.388(9) . ? C19 H19 0.95 . ? C20 H20 0.95 . ? C21 C22 1.502(8) . ? C21 H211 0.99 . ? C21 H212 0.99 . ? C22 N23 1.334(8) . ? C22 C27 1.392(9) . ? N23 C24 1.338(8) . ? C24 C25 1.377(10) . ? C24 H24 0.95 . ? C25 C26 1.379(10) . ? C25 H25 0.95 . ? C26 C27 1.385(10) . ? C26 H26 0.95 . ? C27 H27 0.95 . ? C28 C29 1.495(8) . ? C28 H281 0.99 . ? C28 H282 0.99 . ? C29 N2 1.343(8) . ? C29 C30 1.397(8) . ? C30 C31 1.370(9) . ? C30 H30 0.95 . ? C31 C32 1.373(10) . ? C31 H311 0.95 . ? C32 C33 1.395(9) . ? C32 H321 0.95 . ? C33 N2 1.353(8) . ? C33 H33 0.95 . ? C34 C35 1.501(9) . ? C34 H341 0.99 . ? C34 H342 0.99 . ? C35 N3 1.354(7) . ? C35 C36 1.388(9) . ? C36 C37 1.388(9) . ? C36 H36 0.95 . ? C37 C38 1.373(9) . ? C37 H37 0.95 . ? C38 C39 1.384(9) . ? C38 H38 0.95 . ? C39 N3 1.350(7) . ? C39 H39 0.95 . ? O4 C40 1.343(7) . ? C40 C41 1.391(9) . ? C40 C43 1.421(8) . ? C41 C46 1.392(9) . ? C41 C42 1.512(8) . ? C42 N4 1.505(7) . ? C42 H421 0.99 . ? C42 H422 0.99 . ? N4 C67 1.489(7) . ? N4 C73 1.498(7) . ? C43 C44 1.383(9) . ? C43 C51 1.501(9) . ? C44 C45 1.397(9) . ? C44 H44 0.95 . ? C45 C46 1.407(8) . ? C45 C47 1.535(8) . ? C46 H46 0.95 . ? C47 C50 1.519(9) . ? C47 C49 1.528(10) . ? C47 C48 1.536(9) . ? C48 H481 0.98 . ? C48 H482 0.98 . ? C48 H483 0.98 . ? C49 H491 0.98 . ? C49 H492 0.98 . ? C49 H493 0.98 . ? C50 H501 0.98 . ? C50 H502 0.98 . ? C50 H503 0.98 . ? C51 N52 1.520(7) . ? C51 H511 0.99 . ? C51 H512 0.99 . ? N52 C60 1.500(7) . ? N52 C53 1.512(8) . ? N52 H52 0.93 . ? C53 C54 1.516(9) . ? C53 H531 0.99 . ? C53 H532 0.99 . ? C54 N59 1.340(8) . ? C54 C55 1.369(9) . ? C55 C56 1.407(10) . ? C55 H55 0.95 . ? C56 C57 1.357(9) . ? C56 H56 0.95 . ? C57 C58 1.381(9) . ? C57 H57 0.95 . ? C58 N59 1.332(8) . ? C58 H58 0.95 . ? C60 C61 1.520(9) . ? C60 H601 0.99 . ? C60 H602 0.99 . ? C61 N62 1.332(8) . ? C61 C66 1.362(9) . ? N62 C63 1.343(8) . ? C63 C64 1.393(10) . ? C63 H63 0.95 . ? C64 C65 1.371(10) . ? C64 H64 0.95 . ? C65 C66 1.375(10) . ? C65 H65 0.95 . ? C66 H66 0.95 . ? C67 C68 1.518(8) . ? C67 H671 0.99 . ? C67 H672 0.99 . ? C68 N5 1.352(8) . ? C68 C69 1.382(9) . ? N5 C72 1.348(8) . ? C69 C70 1.382(9) . ? C69 H69 0.95 . ? C70 C71 1.360(10) . ? C70 H70 0.95 . ? C71 C72 1.372(9) . ? C71 H71 0.95 . ? C72 H72 0.95 . ? C73 C74 1.495(8) . ? C73 H731 0.99 . ? C73 H732 0.99 . ? C74 N6 1.353(8) . ? C74 C75 1.379(8) . ? C75 C76 1.368(9) . ? C75 H75 0.95 . ? C76 C77 1.389(9) . ? C76 H76 0.95 . ? C77 C78 1.377(8) . ? C77 H77 0.95 . ? C78 N6 1.350(8) . ? C78 H78 0.95 . ? Cl1 O7 1.429(5) . ? Cl1 O5 1.433(4) . ? Cl1 O8 1.440(5) . ? Cl1 O6 1.444(5) . ? Cl2 O9 1.426(5) . ? Cl2 O12 1.430(5) . ? Cl2 O10 1.439(5) . ? Cl2 O11 1.443(5) . ? Cl3 O14' 1.32(4) . ? Cl3 O13 1.411(5) . ? Cl3 O15 1.421(5) . ? Cl3 O16 1.422(5) . ? Cl3 O14 1.52(2) . ? O14 O14' 0.63(4) . ? Cl4 O20' 1.34(6) . ? Cl4 O18' 1.358(8) . ? Cl4 O19 1.359(6) . ? Cl4 O20 1.406(9) . ? Cl4 O17 1.438(5) . ? Cl4 O18 1.48(5) . ? O18' O20' 1.10(3) . ? O18' O18 1.35(5) . ? O18 O19 1.72(4) . ? O20 O20' 1.27(6) . ? OA OA' 1.11(5) . ? OA C1A 1.230(12) . ? OA' C1A 1.37(5) . ? C1A C2A 1.481(13) . ? C1A C3A 1.489(14) . ? C2A H21 0.98 . ? C2A H22 0.98 . ? C2A H23 0.98 . ? C3A H3A1 0.98 . ? C3A H3A2 0.98 . ? C3A H3A3 0.98 . ? OB OB' 1.22(4) . ? OB C1B 1.245(11) . ? OB' C1B 1.33(4) . ? C1B C3B 1.455(12) . ? C1B C2B 1.481(13) . ? C2B H41 0.98 . ? C2B H42 0.98 . ? C2B H43 0.98 . ? C3B H3B1 0.98 . ? C3B H3B2 0.98 . ? C3B H3B3 0.98 . ? 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 O3 Fe1 O2 97.3(2) . . ? O3 Fe1 O1 172.8(2) . . ? O2 Fe1 O1 76.4(2) . . ? O3 Fe1 N3 88.2(2) . . ? O2 Fe1 N3 108.0(2) . . ? O1 Fe1 N3 90.4(2) . . ? O3 Fe1 N2 95.0(2) . . ? O2 Fe1 N2 98.6(2) . . ? O1 Fe1 N2 89.5(2) . . ? N3 Fe1 N2 152.6(2) . . ? O3 Fe1 N1 92.5(2) . . ? O2 Fe1 N1 169.1(2) . . ? O1 Fe1 N1 94.1(2) . . ? N3 Fe1 N1 76.9(2) . . ? N2 Fe1 N1 75.8(2) . . ? O4 Fe2 O1 95.6(2) . . ? O4 Fe2 O2 171.9(2) . . ? O1 Fe2 O2 76.8(2) . . ? O4 Fe2 N5 88.1(2) . . ? O1 Fe2 N5 106.1(2) . . ? O2 Fe2 N5 91.5(2) . . ? O4 Fe2 N6 94.7(2) . . ? O1 Fe2 N6 100.3(2) . . ? O2 Fe2 N6 89.3(2) . . ? N5 Fe2 N6 153.1(2) . . ? O4 Fe2 N4 91.8(2) . . ? O1 Fe2 N4 171.9(2) . . ? O2 Fe2 N4 95.9(2) . . ? N5 Fe2 N4 77.4(2) . . ? N6 Fe2 N4 75.8(2) . . ? Fe2 O1 Fe1 103.5(2) . . ? Fe2 O1 H1 128.25(11) . . ? Fe1 O1 H1 128.25(11) . . ? Fe1 O2 Fe2 103.3(2) . . ? Fe1 O2 H2 128.34(11) . . ? Fe2 O2 H2 128.35(12) . . ? C1 O3 Fe1 124.9(4) . . ? O3 C1 C4 120.4(5) . . ? O3 C1 C2 119.8(5) . . ? C4 C1 C2 119.9(6) . . ? C7 C2 C1 118.7(6) . . ? C7 C2 C3 120.8(6) . . ? C1 C2 C3 120.3(6) . . ? C2 C3 N1 114.6(5) . . ? C2 C3 H31 108.6(3) . . ? N1 C3 H31 108.6(3) . . ? C2 C3 H32 108.6(3) . . ? N1 C3 H32 108.6(3) . . ? H31 C3 H32 107.6 . . ? C34 N1 C28 112.0(4) . . ? C34 N1 C3 111.1(5) . . ? C28 N1 C3 108.4(5) . . ? C34 N1 Fe1 109.5(4) . . ? C28 N1 Fe1 106.2(4) . . ? C3 N1 Fe1 109.3(3) . . ? C5 C4 C1 119.6(5) . . ? C5 C4 C12 119.7(5) . . ? C1 C4 C12 120.7(5) . . ? C4 C5 C6 121.8(6) . . ? C4 C5 H5 119.1(4) . . ? C6 C5 H5 119.1(4) . . ? C7 C6 C5 117.6(6) . . ? C7 C6 C8 121.5(6) . . ? C5 C6 C8 120.8(5) . . ? C6 C7 C2 122.4(6) . . ? C6 C7 H7 118.8(4) . . ? C2 C7 H7 118.8(4) . . ? C10 C8 C9 109.3(6) . . ? C10 C8 C11 108.0(5) . . ? C9 C8 C11 109.0(5) . . ? C10 C8 C6 111.0(5) . . ? C9 C8 C6 107.6(5) . . ? C11 C8 C6 111.9(5) . . ? C8 C9 H91 109.5(3) . . ? C8 C9 H92 109.5(4) . . ? H91 C9 H92 109.5 . . ? C8 C9 H93 109.5(3) . . ? H91 C9 H93 109.5 . . ? H92 C9 H93 109.5 . . ? C8 C10 H101 109.5(3) . . ? C8 C10 H102 109.5(4) . . ? H101 C10 H102 109.5 . . ? C8 C10 H103 109.5(3) . . ? H101 C10 H103 109.5 . . ? H102 C10 H103 109.5 . . ? C8 C11 H111 109.5(4) . . ? C8 C11 H112 109.5(4) . . ? H111 C11 H112 109.5 . . ? C8 C11 H113 109.5(3) . . ? H111 C11 H113 109.5 . . ? H112 C11 H113 109.5 . . ? C4 C12 N13 112.9(5) . . ? C4 C12 H121 109.0(3) . . ? N13 C12 H121 109.0(3) . . ? C4 C12 H122 109.0(3) . . ? N13 C12 H122 109.0(3) . . ? H121 C12 H122 107.8 . . ? C21 N13 C14 111.1(5) . . ? C21 N13 C12 113.1(4) . . ? C14 N13 C12 110.9(5) . . ? C21 N13 H13 107.1(3) . . ? C14 N13 H13 107.1(3) . . ? C12 N13 H13 107.1(3) . . ? N13 C14 C15 109.8(5) . . ? N13 C14 H141 109.7(3) . . ? C15 C14 H141 109.7(3) . . ? N13 C14 H142 109.7(3) . . ? C15 C14 H142 109.7(3) . . ? H141 C14 H142 108.2 . . ? N16 C15 C20 123.1(6) . . ? N16 C15 C14 115.0(6) . . ? C20 C15 C14 121.9(6) . . ? C17 N16 C15 117.7(6) . . ? N16 C17 C18 123.1(6) . . ? N16 C17 H17 118.4(4) . . ? C18 C17 H17 118.4(4) . . ? C19 C18 C17 118.2(6) . . ? C19 C18 H18 120.9(4) . . ? C17 C18 H18 120.9(4) . . ? C18 C19 C20 120.0(7) . . ? C18 C19 H19 120.0(4) . . ? C20 C19 H19 120.0(4) . . ? C15 C20 C19 117.8(6) . . ? C15 C20 H20 121.1(4) . . ? C19 C20 H20 121.1(4) . . ? N13 C21 C22 111.5(5) . . ? N13 C21 H211 109.3(3) . . ? C22 C21 H211 109.3(3) . . ? N13 C21 H212 109.3(3) . . ? C22 C21 H212 109.3(3) . . ? H211 C21 H212 108.0 . . ? N23 C22 C27 123.4(6) . . ? N23 C22 C21 116.7(5) . . ? C27 C22 C21 119.8(6) . . ? C22 N23 C24 117.5(6) . . ? N23 C24 C25 123.5(7) . . ? N23 C24 H24 118.2(4) . . ? C25 C24 H24 118.2(4) . . ? C24 C25 C26 118.1(7) . . ? C24 C25 H25 121.0(4) . . ? C26 C25 H25 121.0(4) . . ? C25 C26 C27 120.0(7) . . ? C25 C26 H26 120.0(4) . . ? C27 C26 H26 120.0(4) . . ? C26 C27 C22 117.4(6) . . ? C26 C27 H27 121.3(4) . . ? C22 C27 H27 121.3(4) . . ? N1 C28 C29 109.6(5) . . ? N1 C28 H281 109.7(3) . . ? C29 C28 H281 109.7(3) . . ? N1 C28 H282 109.7(3) . . ? C29 C28 H282 109.7(3) . . ? H281 C28 H282 108.2 . . ? N2 C29 C30 121.3(6) . . ? N2 C29 C28 116.0(5) . . ? C30 C29 C28 122.7(6) . . ? C31 C30 C29 118.4(7) . . ? C31 C30 H30 120.8(4) . . ? C29 C30 H30 120.8(4) . . ? C30 C31 C32 120.5(7) . . ? C30 C31 H311 119.8(4) . . ? C32 C31 H311 119.8(4) . . ? C31 C32 C33 119.3(7) . . ? C31 C32 H321 120.3(4) . . ? C33 C32 H321 120.4(4) . . ? N2 C33 C32 120.1(6) . . ? N2 C33 H33 119.9(4) . . ? C32 C33 H33 119.9(4) . . ? C29 N2 C33 120.3(5) . . ? C29 N2 Fe1 115.9(4) . . ? C33 N2 Fe1 123.7(4) . . ? N1 C34 C35 111.6(5) . . ? N1 C34 H341 109.3(3) . . ? C35 C34 H341 109.3(3) . . ? N1 C34 H342 109.3(3) . . ? C35 C34 H342 109.3(3) . . ? H341 C34 H342 108.0 . . ? N3 C35 C36 121.0(6) . . ? N3 C35 C34 115.6(5) . . ? C36 C35 C34 123.4(6) . . ? C35 C36 C37 119.3(7) . . ? C35 C36 H36 120.4(4) . . ? C37 C36 H36 120.4(4) . . ? C38 C37 C36 119.2(6) . . ? C38 C37 H37 120.4(4) . . ? C36 C37 H37 120.4(4) . . ? C37 C38 C39 119.6(6) . . ? C37 C38 H38 120.2(4) . . ? C39 C38 H38 120.2(4) . . ? N3 C39 C38 121.4(6) . . ? N3 C39 H39 119.3(3) . . ? C38 C39 H39 119.3(4) . . ? C39 N3 C35 119.4(5) . . ? C39 N3 Fe1 123.0(4) . . ? C35 N3 Fe1 117.2(4) . . ? C40 O4 Fe2 122.4(4) . . ? O4 C40 C41 121.4(5) . . ? O4 C40 C43 119.2(6) . . ? C41 C40 C43 119.4(6) . . ? C40 C41 C46 119.7(6) . . ? C40 C41 C42 119.7(6) . . ? C46 C41 C42 120.5(6) . . ? N4 C42 C41 113.7(5) . . ? N4 C42 H421 108.8(3) . . ? C41 C42 H421 108.8(3) . . ? N4 C42 H422 108.8(3) . . ? C41 C42 H422 108.8(3) . . ? H421 C42 H422 107.7 . . ? C67 N4 C73 111.4(5) . . ? C67 N4 C42 111.3(5) . . ? C73 N4 C42 108.4(5) . . ? C67 N4 Fe2 109.5(4) . . ? C73 N4 Fe2 105.9(4) . . ? C42 N4 Fe2 110.3(4) . . ? C44 C43 C40 119.1(6) . . ? C44 C43 C51 120.8(6) . . ? C40 C43 C51 120.1(6) . . ? C43 C44 C45 122.7(6) . . ? C43 C44 H44 118.7(4) . . ? C45 C44 H44 118.7(4) . . ? C44 C45 C46 116.7(6) . . ? C44 C45 C47 121.2(5) . . ? C46 C45 C47 121.9(6) . . ? C41 C46 C45 122.2(6) . . ? C41 C46 H46 118.9(4) . . ? C45 C46 H46 118.9(4) . . ? C50 C47 C49 107.3(6) . . ? C50 C47 C45 110.3(5) . . ? C49 C47 C45 112.3(5) . . ? C50 C47 C48 110.1(5) . . ? C49 C47 C48 108.8(6) . . ? C45 C47 C48 108.1(5) . . ? C47 C48 H481 109.5(4) . . ? C47 C48 H482 109.5(4) . . ? H481 C48 H482 109.5 . . ? C47 C48 H483 109.5(4) . . ? H481 C48 H483 109.5 . . ? H482 C48 H483 109.5 . . ? C47 C49 H491 109.5(4) . . ? C47 C49 H492 109.5(4) . . ? H491 C49 H492 109.5 . . ? C47 C49 H493 109.5(4) . . ? H491 C49 H493 109.5 . . ? H492 C49 H493 109.5 . . ? C47 C50 H501 109.5(4) . . ? C47 C50 H502 109.5(4) . . ? H501 C50 H502 109.5 . . ? C47 C50 H503 109.5(3) . . ? H501 C50 H503 109.5 . . ? H502 C50 H503 109.5 . . ? C43 C51 N52 113.4(5) . . ? C43 C51 H511 108.9(3) . . ? N52 C51 H511 108.9(3) . . ? C43 C51 H512 108.9(3) . . ? N52 C51 H512 108.9(3) . . ? H511 C51 H512 107.7 . . ? C60 N52 C53 112.0(5) . . ? C60 N52 C51 112.0(5) . . ? C53 N52 C51 110.6(5) . . ? C60 N52 H52 107.3(3) . . ? C53 N52 H52 107.3(3) . . ? C51 N52 H52 107.3(3) . . ? N52 C53 C54 107.9(5) . . ? N52 C53 H531 110.1(3) . . ? C54 C53 H531 110.1(4) . . ? N52 C53 H532 110.1(3) . . ? C54 C53 H532 110.1(3) . . ? H531 C53 H532 108.4 . . ? N59 C54 C55 123.8(6) . . ? N59 C54 C53 112.8(6) . . ? C55 C54 C53 123.4(6) . . ? C54 C55 C56 117.3(6) . . ? C54 C55 H55 121.3(4) . . ? C56 C55 H55 121.3(4) . . ? C57 C56 C55 119.5(7) . . ? C57 C56 H56 120.2(4) . . ? C55 C56 H56 120.2(4) . . ? C56 C57 C58 118.7(7) . . ? C56 C57 H57 120.7(4) . . ? C58 C57 H57 120.7(4) . . ? N59 C58 C57 123.3(6) . . ? N59 C58 H58 118.4(4) . . ? C57 C58 H58 118.3(4) . . ? C58 N59 C54 117.3(6) . . ? N52 C60 C61 109.7(5) . . ? N52 C60 H601 109.7(3) . . ? C61 C60 H601 109.7(3) . . ? N52 C60 H602 109.7(3) . . ? C61 C60 H602 109.7(3) . . ? H601 C60 H602 108.2 . . ? N62 C61 C66 124.7(6) . . ? N62 C61 C60 114.4(6) . . ? C66 C61 C60 120.9(6) . . ? C61 N62 C63 116.3(6) . . ? N62 C63 C64 123.6(6) . . ? N62 C63 H63 118.2(4) . . ? C64 C63 H63 118.2(4) . . ? C65 C64 C63 117.2(7) . . ? C65 C64 H64 121.4(4) . . ? C63 C64 H64 121.4(4) . . ? C64 C65 C66 120.4(7) . . ? C64 C65 H65 119.8(4) . . ? C66 C65 H65 119.8(4) . . ? C61 C66 C65 117.8(7) . . ? C61 C66 H66 121.1(4) . . ? C65 C66 H66 121.1(4) . . ? N4 C67 C68 109.8(5) . . ? N4 C67 H671 109.7(3) . . ? C68 C67 H671 109.7(3) . . ? N4 C67 H672 109.7(3) . . ? C68 C67 H672 109.7(3) . . ? H671 C67 H672 108.2 . . ? N5 C68 C69 122.2(6) . . ? N5 C68 C67 115.3(5) . . ? C69 C68 C67 122.4(6) . . ? C72 N5 C68 118.0(5) . . ? C72 N5 Fe2 123.8(4) . . ? C68 N5 Fe2 117.1(4) . . ? C68 C69 C70 118.6(6) . . ? C68 C69 H69 120.7(4) . . ? C70 C69 H69 120.7(4) . . ? C71 C70 C69 119.4(6) . . ? C71 C70 H70 120.3(4) . . ? C69 C70 H70 120.3(4) . . ? C70 C71 C72 119.8(6) . . ? C70 C71 H71 120.1(4) . . ? C72 C71 H71 120.1(4) . . ? N5 C72 C71 122.1(6) . . ? N5 C72 H72 119.0(3) . . ? C71 C72 H72 119.0(4) . . ? C74 C73 N4 109.4(5) . . ? C74 C73 H731 109.8(3) . . ? N4 C73 H731 109.8(3) . . ? C74 C73 H732 109.8(3) . . ? N4 C73 H732 109.8(3) . . ? H731 C73 H732 108.2 . . ? N6 C74 C75 120.8(6) . . ? N6 C74 C73 115.7(5) . . ? C75 C74 C73 123.5(6) . . ? C76 C75 C74 119.9(7) . . ? C76 C75 H75 120.0(4) . . ? C74 C75 H75 120.0(4) . . ? C75 C76 C77 119.6(6) . . ? C75 C76 H76 120.2(4) . . ? C77 C76 H76 120.2(4) . . ? C78 C77 C76 118.3(6) . . ? C78 C77 H77 120.9(4) . . ? C76 C77 H77 120.8(4) . . ? N6 C78 C77 122.1(6) . . ? N6 C78 H78 119.0(4) . . ? C77 C78 H78 119.0(4) . . ? C78 N6 C74 119.2(5) . . ? C78 N6 Fe2 125.2(4) . . ? C74 N6 Fe2 115.5(4) . . ? O7 Cl1 O5 110.1(3) . . ? O7 Cl1 O8 108.8(3) . . ? O5 Cl1 O8 109.3(3) . . ? O7 Cl1 O6 110.2(3) . . ? O5 Cl1 O6 110.0(3) . . ? O8 Cl1 O6 108.5(3) . . ? O9 Cl2 O12 109.9(4) . . ? O9 Cl2 O10 109.2(3) . . ? O12 Cl2 O10 108.7(4) . . ? O9 Cl2 O11 108.6(4) . . ? O12 Cl2 O11 109.9(4) . . ? O10 Cl2 O11 110.4(3) . . ? O14' Cl3 O13 124.9(20) . . ? O14' Cl3 O15 103.1(19) . . ? O13 Cl3 O15 109.8(4) . . ? O14' Cl3 O16 98.8(21) . . ? O13 Cl3 O16 108.4(3) . . ? O15 Cl3 O16 111.2(4) . . ? O14' Cl3 O14 24.1(22) . . ? O13 Cl3 O14 101.3(14) . . ? O15 Cl3 O14 110.9(10) . . ? O16 Cl3 O14 114.8(12) . . ? O14' O14 Cl3 60.0(56) . . ? O14 O14' Cl3 95.8(74) . . ? O20' Cl4 O18' 48.2(17) . . ? O20' Cl4 O19 129.5(15) . . ? O18' Cl4 O19 112.7(6) . . ? O20' Cl4 O20 54.9(18) . . ? O18' Cl4 O20 102.5(9) . . ? O19 Cl4 O20 107.2(7) . . ? O20' Cl4 O17 115.0(14) . . ? O18' Cl4 O17 113.2(5) . . ? O19 Cl4 O17 115.3(4) . . ? O20 Cl4 O17 104.5(4) . . ? O20' Cl4 O18 104.9(24) . . ? O18' Cl4 O18 56.8(16) . . ? O19 Cl4 O18 74.6(14) . . ? O20 Cl4 O18 156.0(17) . . ? O17 Cl4 O18 95.7(14) . . ? O20' O18' O18 130.9(39) . . ? O20' O18' Cl4 65.1(33) . . ? O18 O18' Cl4 66.0(15) . . ? O18' O18 Cl4 57.2(23) . . ? O18' O18 O19 94.0(31) . . ? Cl4 O18 O19 49.5(13) . . ? Cl4 O19 O18 55.8(16) . . ? O20' O20 Cl4 60.0(21) . . ? O18' O20' O20 130.8(54) . . ? O18' O20' Cl4 66.7(25) . . ? O20 O20' Cl4 65.1(32) . . ? OA' OA C1A 71.2(21) . . ? OA OA' C1A 58.6(27) . . ? OA C1A OA' 50.2(18) . . ? OA C1A C2A 127.5(11) . . ? OA' C1A C2A 92.2(22) . . ? OA C1A C3A 116.1(12) . . ? OA' C1A C3A 140.3(16) . . ? C2A C1A C3A 115.8(8) . . ? C1A C2A H21 109.5(5) . . ? C1A C2A H22 109.5(6) . . ? H21 C2A H22 109.5 . . ? C1A C2A H23 109.5(6) . . ? H21 C2A H23 109.5 . . ? H22 C2A H23 109.5 . . ? C1A C3A H3A1 109.5(5) . . ? C1A C3A H3A2 109.5(6) . . ? H3A1 C3A H3A2 109.5 . . ? C1A C3A H3A3 109.5(6) . . ? H3A1 C3A H3A3 109.5 . . ? H3A2 C3A H3A3 109.5 . . ? OB' OB C1B 65.4(16) . . ? OB OB' C1B 58.3(19) . . ? OB C1B OB' 56.3(15) . . ? OB C1B C3B 116.1(9) . . ? OB' C1B C3B 122.8(19) . . ? OB C1B C2B 125.1(9) . . ? OB' C1B C2B 99.2(17) . . ? C3B C1B C2B 118.1(8) . . ? C1B C2B H41 109.5(5) . . ? C1B C2B H42 109.5(5) . . ? H41 C2B H42 109.5 . . ? C1B C2B H43 109.5(5) . . ? H41 C2B H43 109.5 . . ? H42 C2B H43 109.5 . . ? C1B C3B H3B1 109.5(5) . . ? C1B C3B H3B2 109.5(5) . . ? H3B1 C3B H3B2 109.5 . . ? C1B C3B H3B3 109.5(5) . . ? H3B1 C3B H3B3 109.5 . . ? H3B2 C3B H3B3 109.5 . . ? _refine_diff_density_max 0.676 _refine_diff_density_min -0.619 _refine_diff_density_rms 0.088