Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 222 _publ_contact_author_name 'Prof Spyros P. Perlepes' _publ_contact_author_address ; Department of Chemistry University of Patras Patras 26504 GREECE ; _publ_contact_author_phone '(30) 2610997146' _publ_contact_author_fax '(30) 2610997118' _publ_contact_author_email perlepes@patreas.upatras.gr _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Use of the di-2-pyridyl ketone/3,5-di-tert-butylcatechol blend” in iron(III) chemistry: a cationic tetranuclear cluster and an anionic trinuclear complex ; loop_ _publ_author_name _publ_author_address 'Boudalis, Athanassios K.' ; Department of Chemistry University of Patras 26504 Patras Greece ; 'Dahan, Francoise' ; Laboratoire de Chimie de Coordination du CNRS 205 Route de Narbonne 31077 Toulouse Cedex 4 France ; 'Tuchagues, Jean-Pierre' ; Laboratoire de Chimie de Coordination du CNRS 205 Route de Narbonne 31077 Toulouse Cedex 4 France ; 'Perlepes, Spyros P.' ; Department of Chemistry University of Patras 26504 Patras Greece ; 'Azzedine Bousseksou' ; ? ; data_(1) _database_code_CSD 211396 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C104 H126 Cl2 Fe4 N8 O24' _chemical_formula_weight 2166.43 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2904(11) _cell_length_b 15.3440(17) _cell_length_c 17.2747(16) _cell_angle_alpha 99.013(12) _cell_angle_beta 101.928(11) _cell_angle_gamma 108.254(12) _cell_volume 2700.6(5) _cell_formula_units_Z 1 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Black _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.332 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1136 _exptl_absorpt_coefficient_mu 0.649 _exptl_absorpt_correction_type Numerical _exptl_absorpt_process_details 'X-SHAPE (Stoe & Cie, 1996)' _exptl_absorpt_correction_T_min 0.6806 _exptl_absorpt_correction_T_max 0.8319 _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type STOE-IPDS _diffrn_measurement_method 'Imaging Plate Detector System' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26615 _diffrn_reflns_av_R_equivalents 0.0381 _diffrn_reflns_av_sigmaI/netI 0.0411 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 26.06 _reflns_number_total 9838 _reflns_number_gt 7159 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE-IPDS software (Stoe, 2.93, 1997)' _computing_cell_refinement 'STOE-IPDS software (Stoe, 2.93, 1997)' _computing_data_reduction 'XRED (Stoe, 1.08, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ZORTEP (Zsolnai, 1996)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0496P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9838 _refine_ls_number_parameters 640 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0437 _refine_ls_R_factor_gt 0.0351 _refine_ls_wR_factor_ref 0.0691 _refine_ls_wR_factor_gt 0.0666 _refine_ls_goodness_of_fit_ref 0.878 _refine_ls_restrained_S_all 0.878 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.47552(2) 0.525567(18) 0.410168(17) 0.01581(7) Uani 1 d . . . Fe2 Fe 0.53358(3) 0.49534(2) 0.236289(18) 0.01996(8) Uani 1 d . . . O1 O 0.38217(12) 0.45852(9) 0.28816(8) 0.0202(3) Uani 1 d . . . O2 O 0.62444(12) 0.52957(9) 0.35975(8) 0.0192(3) Uani 1 d . . . O3 O 0.51632(12) 0.65639(9) 0.41357(8) 0.0206(3) Uani 1 d . . . O4 O 0.53070(12) 0.58126(8) 0.53531(8) 0.0181(3) Uani 1 d . . . O5 O 0.69353(13) 0.58404(10) 0.23595(9) 0.0258(3) Uani 1 d . . . O6 O 0.45507(14) 0.43086(10) 0.12184(9) 0.0283(3) Uani 1 d . . . O7 O 0.18576(14) 0.39818(11) 0.18741(9) 0.0324(4) Uani 1 d . . . O8 O 0.53830(16) 0.38131(11) 0.01689(10) 0.0371(4) Uani 1 d . . . N1 N 0.27731(15) 0.51692(11) 0.39504(11) 0.0224(4) Uani 1 d . . . N2 N 0.60091(16) 0.37820(12) 0.22460(11) 0.0252(4) Uani 1 d . . . N3 N 0.43283(16) 0.58948(12) 0.21061(11) 0.0245(4) Uani 1 d . . . N4 N 0.25997(19) 0.28258(15) 0.05339(13) 0.0432(5) Uani 1 d . . . H4A H 0.2644 0.3366 0.0823 0.048 Uiso 1 calc R . . C1 C 0.27229(19) 0.47524(15) 0.25266(13) 0.0256(5) Uani 1 d . . . C2 C 0.20505(18) 0.49589(14) 0.31858(13) 0.0241(4) Uani 1 d . . . C3 C 0.0800(2) 0.49736(17) 0.30111(16) 0.0334(5) Uani 1 d . . . H3 H 0.0274 0.4782 0.2465 0.037 Uiso 1 calc R . . C4 C 0.0334(2) 0.52685(17) 0.36386(17) 0.0369(6) Uani 1 d . . . H4 H -0.0507 0.5304 0.3529 0.041 Uiso 1 calc R . . C5 C 0.1099(2) 0.55113(16) 0.44259(16) 0.0330(5) Uani 1 d . . . H5 H 0.0798 0.5722 0.4868 0.036 Uiso 1 calc R . . C6 C 0.2314(2) 0.54436(15) 0.45632(14) 0.0277(5) Uani 1 d . . . H6 H 0.2837 0.5596 0.5107 0.030 Uiso 1 calc R . . C7 C 0.56206(17) 0.67703(13) 0.55497(13) 0.0196(4) Uani 1 d . . . C8 C 0.59723(18) 0.73200(13) 0.63322(13) 0.0217(4) Uani 1 d . . . H8 H 0.5989 0.7036 0.6783 0.024 Uiso 1 calc R . . C9 C 0.63038(19) 0.82979(14) 0.64555(13) 0.0249(4) Uani 1 d . . . C10 C 0.62752(19) 0.86803(14) 0.57700(14) 0.0254(4) Uani 1 d . . . H10 H 0.6520 0.9347 0.5856 0.028 Uiso 1 calc R . . C11 C 0.59133(18) 0.81529(13) 0.49727(13) 0.0223(4) Uani 1 d . . . C12 C 0.55578(17) 0.71651(13) 0.48649(12) 0.0202(4) Uani 1 d . . . C13 C 0.6762(2) 0.89534(14) 0.73059(14) 0.0311(5) Uani 1 d . . . C14 C 0.8246(2) 0.9385(2) 0.75604(18) 0.0526(7) Uani 1 d . . . H14A H 0.8546 0.9806 0.8106 0.058 Uiso 1 calc R . . H14B H 0.8540 0.9746 0.7172 0.058 Uiso 1 calc R . . H14C H 0.8602 0.8879 0.7566 0.058 Uiso 1 calc R . . C15 C 0.6340(3) 0.84416(17) 0.79470(16) 0.0472(7) Uani 1 d . . . H15A H 0.6658 0.8891 0.8479 0.052 Uiso 1 calc R . . H15B H 0.6699 0.7939 0.7973 0.052 Uiso 1 calc R . . H15C H 0.5391 0.8166 0.7801 0.052 Uiso 1 calc R . . C16 C 0.6225(3) 0.97507(19) 0.73175(17) 0.0512(7) Uani 1 d . . . H16A H 0.6532 1.0160 0.7868 0.056 Uiso 1 calc R . . H16B H 0.5276 0.9483 0.7156 0.056 Uiso 1 calc R . . H16C H 0.6523 1.0121 0.6936 0.056 Uiso 1 calc R . . C17 C 0.5852(2) 0.85966(14) 0.42384(14) 0.0262(5) Uani 1 d . . . C18 C 0.6679(2) 0.83171(16) 0.37159(15) 0.0329(5) Uani 1 d . . . H18A H 0.6383 0.7627 0.3544 0.036 Uiso 1 calc R . . H18B H 0.7589 0.8565 0.4036 0.036 Uiso 1 calc R . . H18C H 0.6594 0.8580 0.3235 0.036 Uiso 1 calc R . . C19 C 0.6365(2) 0.96774(15) 0.44963(15) 0.0355(5) Uani 1 d . . . H19A H 0.5858 0.9883 0.4834 0.039 Uiso 1 calc R . . H19B H 0.6288 0.9933 0.4011 0.039 Uiso 1 calc R . . H19C H 0.7277 0.9908 0.4809 0.039 Uiso 1 calc R . . C20 C 0.4436(2) 0.82515(16) 0.37301(15) 0.0333(5) Uani 1 d . . . H20A H 0.4094 0.7560 0.3563 0.037 Uiso 1 calc R . . H20B H 0.4387 0.8510 0.3245 0.037 Uiso 1 calc R . . H20C H 0.3921 0.8464 0.4057 0.037 Uiso 1 calc R . . C21 C 0.3097(2) 0.55897(16) 0.21307(14) 0.0285(5) Uani 1 d . . . C22 C 0.2251(3) 0.6008(2) 0.18033(19) 0.0536(8) Uani 1 d . . . H22 H 0.1368 0.5776 0.1808 0.059 Uiso 1 calc R . . C23 C 0.2705(3) 0.6766(2) 0.14701(19) 0.0551(8) Uani 1 d . . . H23 H 0.2137 0.7063 0.1248 0.061 Uiso 1 calc R . . C24 C 0.3972(3) 0.70845(18) 0.14612(16) 0.0412(6) Uani 1 d . . . H24 H 0.4306 0.7610 0.1241 0.045 Uiso 1 calc R . . C25 C 0.4755(2) 0.66241(15) 0.17796(14) 0.0316(5) Uani 1 d . . . H25 H 0.5635 0.6835 0.1766 0.035 Uiso 1 calc R . . C26 C 0.4904(2) 0.36172(15) 0.08504(14) 0.0301(5) Uani 1 d . . . C27 C 0.5880(2) 0.33924(15) 0.14714(14) 0.0298(5) Uani 1 d . . . C28 C 0.6602(3) 0.28613(19) 0.12537(17) 0.0448(6) Uani 1 d . . . H28 H 0.6523 0.2617 0.0697 0.049 Uiso 1 calc R . . C29 C 0.7444(3) 0.26965(19) 0.18707(18) 0.0491(7) Uani 1 d . . . H29 H 0.7946 0.2328 0.1742 0.054 Uiso 1 calc R . . C30 C 0.7548(2) 0.30670(19) 0.26633(18) 0.0449(6) Uani 1 d . . . H30 H 0.8110 0.2949 0.3091 0.049 Uiso 1 calc R . . C31 C 0.6826(2) 0.36158(16) 0.28388(15) 0.0325(5) Uani 1 d . . . H31 H 0.6911 0.3881 0.3392 0.036 Uiso 1 calc R . . C32 C 0.3699(2) 0.27292(17) 0.04412(14) 0.0360(5) Uani 1 d . . . C33 C 0.3636(3) 0.18854(18) -0.00001(16) 0.0490(7) Uani 1 d . . . H33 H 0.4403 0.1802 -0.0084 0.054 Uiso 1 calc R . . C34 C 0.2466(3) 0.1163(2) -0.03200(18) 0.0599(8) Uani 1 d . . . H34 H 0.2426 0.0572 -0.0614 0.066 Uiso 1 calc R . . C35 C 0.1352(3) 0.1283(2) -0.0221(2) 0.0657(9) Uani 1 d . . . H35 H 0.0539 0.0781 -0.0446 0.072 Uiso 1 calc R . . C36 C 0.1421(3) 0.2137(2) 0.02070(19) 0.0598(8) Uani 1 d . . . H36 H 0.0658 0.2243 0.0272 0.066 Uiso 1 calc R . . C37 C 0.73877(17) 0.60481(13) 0.37743(13) 0.0195(4) Uani 1 d . . . C38 C 0.77589(18) 0.63211(14) 0.30955(13) 0.0218(4) Uani 1 d . . . C39 C 0.89323(18) 0.70769(15) 0.32122(14) 0.0258(5) Uani 1 d . . . C40 C 0.96209(19) 0.75367(15) 0.40134(14) 0.0282(5) Uani 1 d . . . H40 H 1.0410 0.8050 0.4105 0.031 Uiso 1 calc R . . C41 C 0.92412(19) 0.73022(15) 0.46944(14) 0.0268(5) Uani 1 d . . . C42 C 0.81019(18) 0.65289(14) 0.45626(13) 0.0223(4) Uani 1 d . . . H42 H 0.7821 0.6336 0.5011 0.024 Uiso 1 calc R . . C43 C 0.9415(2) 0.74312(17) 0.25105(16) 0.0353(5) Uani 1 d . . . C44 C 0.8701(4) 0.8041(3) 0.2218(3) 0.0985(16) Uani 1 d . . . H44A H 0.8826 0.8560 0.2673 0.108 Uiso 1 calc R . . H44B H 0.7775 0.7663 0.2000 0.108 Uiso 1 calc R . . H44C H 0.9034 0.8300 0.1790 0.108 Uiso 1 calc R . . C45 C 0.9215(3) 0.6633(3) 0.1813(2) 0.0804(12) Uani 1 d . . . H45A H 0.9539 0.6889 0.1381 0.088 Uiso 1 calc R . . H45B H 0.8288 0.6254 0.1600 0.088 Uiso 1 calc R . . H45C H 0.9686 0.6234 0.2003 0.088 Uiso 1 calc R . . C46 C 1.0867(3) 0.7994(3) 0.2774(2) 0.0725(11) Uani 1 d . . . H46A H 1.1063 0.8530 0.3232 0.080 Uiso 1 calc R . . H46B H 1.1133 0.8228 0.2317 0.080 Uiso 1 calc R . . H46C H 1.1338 0.7587 0.2942 0.080 Uiso 1 calc R . . C47 C 1.00394(19) 0.79254(15) 0.55422(14) 0.0298(5) Uani 1 d . . . C48 C 0.9561(2) 0.75106(18) 0.62177(15) 0.0392(6) Uani 1 d . . . H48A H 1.0097 0.7926 0.6749 0.043 Uiso 1 calc R . . H48B H 0.9624 0.6884 0.6182 0.043 Uiso 1 calc R . . H48C H 0.8656 0.7456 0.6155 0.043 Uiso 1 calc R . . C49 C 0.9924(2) 0.89070(17) 0.56132(17) 0.0446(6) Uani 1 d . . . H49A H 1.0437 0.9311 0.6153 0.049 Uiso 1 calc R . . H49B H 0.9013 0.8842 0.5537 0.049 Uiso 1 calc R . . H49C H 1.0250 0.9193 0.5194 0.049 Uiso 1 calc R . . C50 C 1.1472(2) 0.80405(17) 0.56728(16) 0.0381(6) Uani 1 d . . . H50A H 1.1971 0.8440 0.6217 0.042 Uiso 1 calc R . . H50B H 1.1806 0.8337 0.5260 0.042 Uiso 1 calc R . . H50C H 1.1555 0.7419 0.5625 0.042 Uiso 1 calc R . . C51 C 0.1303(2) 0.31278(17) 0.21269(17) 0.0424(6) Uani 1 d . . . H51A H 0.0720 0.2629 0.1650 0.047 Uiso 1 calc R . . H51B H 0.0813 0.3245 0.2513 0.047 Uiso 1 calc R . . H51C H 0.1997 0.2929 0.2389 0.047 Uiso 1 calc R . . C52 C 0.6469(2) 0.46746(18) 0.03703(16) 0.0435(6) Uani 1 d . . . H52A H 0.6760 0.4769 -0.0117 0.048 Uiso 1 calc R . . H52B H 0.7175 0.4643 0.0790 0.048 Uiso 1 calc R . . H52C H 0.6217 0.5203 0.0576 0.048 Uiso 1 calc R . . Cl1 Cl 0.20753(8) 0.85981(6) 0.00922(5) 0.0645(2) Uani 1 d . . . O9 O 0.3389(3) 0.8721(2) 0.0310(2) 0.1069(11) Uani 1 d . . . O10 O 0.1410(3) 0.7605(2) -0.0148(2) 0.1013(9) Uani 1 d . . . O11 O 0.1574(4) 0.8805(2) -0.0668(2) 0.1196(11) Uani 1 d . . . O12 O 0.1730(3) 0.9095(3) 0.0655(2) 0.1433(15) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.01734(13) 0.01275(13) 0.01770(16) 0.00494(10) 0.00527(10) 0.00493(10) Fe2 0.02153(15) 0.01987(15) 0.01973(17) 0.00532(11) 0.00690(11) 0.00795(12) O1 0.0191(7) 0.0217(7) 0.0209(8) 0.0067(6) 0.0042(5) 0.0087(6) O2 0.0187(6) 0.0160(7) 0.0222(8) 0.0049(5) 0.0057(5) 0.0050(5) O3 0.0253(7) 0.0151(7) 0.0211(8) 0.0044(5) 0.0059(5) 0.0072(5) O4 0.0234(7) 0.0105(6) 0.0203(8) 0.0050(5) 0.0058(5) 0.0055(5) O5 0.0244(7) 0.0291(8) 0.0251(9) 0.0092(6) 0.0091(6) 0.0085(6) O6 0.0348(8) 0.0280(8) 0.0224(9) 0.0035(6) 0.0057(6) 0.0144(6) O7 0.0255(8) 0.0404(9) 0.0242(9) 0.0074(7) 0.0002(6) 0.0068(7) O8 0.0520(10) 0.0355(9) 0.0246(10) 0.0069(7) 0.0163(7) 0.0132(8) N1 0.0222(8) 0.0194(9) 0.0280(10) 0.0072(7) 0.0095(7) 0.0080(7) N2 0.0261(9) 0.0251(9) 0.0254(11) 0.0063(7) 0.0069(7) 0.0105(7) N3 0.0288(9) 0.0214(9) 0.0257(10) 0.0074(7) 0.0085(7) 0.0105(7) N4 0.0405(12) 0.0409(12) 0.0346(13) -0.0004(9) 0.0021(9) 0.0060(10) C1 0.0209(10) 0.0322(12) 0.0248(12) 0.0097(9) 0.0030(8) 0.0119(9) C2 0.0202(10) 0.0235(11) 0.0305(13) 0.0113(9) 0.0069(8) 0.0080(8) C3 0.0236(11) 0.0404(13) 0.0413(15) 0.0187(11) 0.0094(9) 0.0134(10) C4 0.0226(11) 0.0409(14) 0.0579(18) 0.0230(12) 0.0172(11) 0.0165(10) C5 0.0317(12) 0.0289(12) 0.0449(16) 0.0099(10) 0.0224(10) 0.0112(9) C6 0.0290(11) 0.0246(11) 0.0313(13) 0.0064(9) 0.0152(9) 0.0077(9) C7 0.0194(9) 0.0128(9) 0.0276(12) 0.0059(8) 0.0070(8) 0.0060(7) C8 0.0227(10) 0.0181(10) 0.0232(12) 0.0060(8) 0.0045(8) 0.0066(8) C9 0.0231(10) 0.0169(10) 0.0302(13) 0.0027(8) 0.0036(8) 0.0049(8) C10 0.0302(11) 0.0133(10) 0.0322(13) 0.0049(8) 0.0083(9) 0.0074(8) C11 0.0244(10) 0.0155(10) 0.0282(12) 0.0085(8) 0.0082(8) 0.0067(8) C12 0.0176(9) 0.0152(10) 0.0256(12) 0.0019(8) 0.0055(8) 0.0048(7) C13 0.0383(12) 0.0170(10) 0.0299(13) 0.0017(9) 0.0048(9) 0.0038(9) C14 0.0424(15) 0.0503(17) 0.0416(17) -0.0085(12) -0.0017(12) 0.0029(12) C15 0.0761(19) 0.0248(13) 0.0299(15) 0.0006(10) 0.0111(13) 0.0085(12) C16 0.085(2) 0.0395(15) 0.0329(16) -0.0011(11) 0.0106(14) 0.0361(15) C17 0.0321(11) 0.0200(10) 0.0297(13) 0.0105(9) 0.0094(9) 0.0106(9) C18 0.0407(13) 0.0285(12) 0.0386(15) 0.0183(10) 0.0180(10) 0.0151(10) C19 0.0495(14) 0.0202(11) 0.0407(15) 0.0151(10) 0.0158(11) 0.0116(10) C20 0.0359(12) 0.0316(12) 0.0353(14) 0.0134(10) 0.0051(10) 0.0166(10) C21 0.0323(11) 0.0357(12) 0.0265(13) 0.0149(9) 0.0120(9) 0.0182(10) C22 0.0458(15) 0.082(2) 0.068(2) 0.0539(18) 0.0307(14) 0.0417(15) C23 0.0717(19) 0.078(2) 0.061(2) 0.0525(17) 0.0391(15) 0.0570(17) C24 0.0651(17) 0.0397(14) 0.0402(16) 0.0236(11) 0.0286(13) 0.0313(13) C25 0.0421(13) 0.0278(12) 0.0320(14) 0.0134(10) 0.0154(10) 0.0157(10) C26 0.0414(13) 0.0297(12) 0.0237(13) 0.0048(9) 0.0131(9) 0.0168(10) C27 0.0387(12) 0.0266(12) 0.0277(13) 0.0063(9) 0.0135(9) 0.0136(10) C28 0.0580(16) 0.0476(16) 0.0408(17) 0.0068(12) 0.0212(12) 0.0321(13) C29 0.0551(16) 0.0485(16) 0.058(2) 0.0083(13) 0.0195(13) 0.0369(14) C30 0.0442(14) 0.0484(16) 0.0488(18) 0.0137(12) 0.0064(12) 0.0284(13) C31 0.0349(12) 0.0337(13) 0.0309(14) 0.0089(10) 0.0062(10) 0.0162(10) C32 0.0498(14) 0.0328(13) 0.0219(13) 0.0070(9) 0.0069(10) 0.0116(11) C33 0.0728(19) 0.0368(15) 0.0314(16) 0.0043(11) 0.0141(13) 0.0133(13) C34 0.091(2) 0.0365(16) 0.0326(17) 0.0005(12) 0.0090(15) 0.0053(15) C35 0.068(2) 0.0501(19) 0.043(2) -0.0008(14) -0.0008(15) -0.0112(15) C36 0.0493(16) 0.062(2) 0.0432(19) 0.0002(14) 0.0020(13) -0.0012(14) C37 0.0163(9) 0.0156(9) 0.0308(12) 0.0096(8) 0.0093(8) 0.0074(7) C38 0.0224(10) 0.0222(10) 0.0265(12) 0.0100(8) 0.0093(8) 0.0120(8) C39 0.0197(10) 0.0283(11) 0.0360(13) 0.0169(9) 0.0103(9) 0.0114(8) C40 0.0171(10) 0.0237(11) 0.0416(14) 0.0131(9) 0.0085(9) 0.0012(8) C41 0.0225(10) 0.0255(11) 0.0327(13) 0.0113(9) 0.0056(9) 0.0082(8) C42 0.0197(9) 0.0228(10) 0.0249(12) 0.0095(8) 0.0064(8) 0.0063(8) C43 0.0278(11) 0.0397(14) 0.0446(16) 0.0216(11) 0.0195(10) 0.0084(10) C44 0.105(3) 0.146(4) 0.121(4) 0.104(3) 0.076(3) 0.083(3) C45 0.077(2) 0.074(2) 0.073(3) -0.0004(19) 0.056(2) -0.0092(18) C46 0.0499(17) 0.088(3) 0.052(2) 0.0192(18) 0.0240(14) -0.0195(16) C47 0.0226(10) 0.0240(11) 0.0348(14) 0.0062(9) 0.0005(9) 0.0026(9) C48 0.0321(12) 0.0406(14) 0.0304(14) 0.0055(10) 0.0006(10) -0.0001(10) C49 0.0433(14) 0.0320(14) 0.0498(17) 0.0047(11) 0.0015(12) 0.0114(11) C50 0.0234(11) 0.0337(13) 0.0477(16) 0.0123(11) -0.0008(10) 0.0029(9) C51 0.0363(13) 0.0369(14) 0.0431(16) 0.0069(11) 0.0026(11) 0.0047(11) C52 0.0515(15) 0.0464(15) 0.0322(15) 0.0099(11) 0.0184(11) 0.0122(12) Cl1 0.0627(5) 0.0655(5) 0.0606(5) -0.0045(4) 0.0064(4) 0.0329(4) O9 0.0685(17) 0.096(2) 0.119(3) -0.0296(18) 0.0065(16) 0.0179(15) O10 0.117(2) 0.0783(19) 0.118(3) 0.0293(17) 0.0364(19) 0.0405(17) O11 0.155(3) 0.076(2) 0.114(3) 0.0329(18) 0.014(2) 0.033(2) O12 0.115(3) 0.176(4) 0.095(3) -0.057(2) 0.0007(19) 0.053(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O3 1.9020(13) . ? Fe1 O4 2.0045(13) 2_666 ? Fe1 O2 2.0363(13) . ? Fe1 O4 2.0791(14) . ? Fe1 O1 2.0820(14) . ? Fe1 N1 2.1576(16) . ? Fe2 O5 1.8923(14) . ? Fe2 O6 1.9460(15) . ? Fe2 O1 2.0570(14) . ? Fe2 O2 2.0698(14) . ? Fe2 N3 2.1444(17) . ? Fe2 N2 2.1576(17) . ? O1 C1 1.384(2) . ? O2 C37 1.373(2) . ? O3 C12 1.335(2) . ? O4 C7 1.367(2) . ? O4 Fe1 2.0045(13) 2_666 ? O5 C38 1.346(2) . ? O6 C26 1.359(3) . ? O7 C1 1.424(3) . ? O7 C51 1.442(3) . ? O8 C52 1.427(3) . ? O8 C26 1.429(3) . ? N1 C2 1.331(3) . ? N1 C6 1.338(3) . ? N2 C27 1.335(3) . ? N2 C31 1.343(3) . ? N3 C25 1.332(3) . ? N3 C21 1.333(3) . ? N4 C32 1.334(3) . ? N4 C36 1.352(3) . ? N4 H4A 0.8800 . ? C1 C21 1.533(3) . ? C1 C2 1.539(3) . ? C2 C3 1.389(3) . ? C3 C4 1.374(3) . ? C3 H3 0.9500 . ? C4 C5 1.374(4) . ? C4 H4 0.9500 . ? C5 C6 1.382(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.381(3) . ? C7 C12 1.410(3) . ? C8 C9 1.397(3) . ? C8 H8 0.9500 . ? C9 C10 1.400(3) . ? C9 C13 1.528(3) . ? C10 C11 1.389(3) . ? C10 H10 0.9500 . ? C11 C12 1.412(3) . ? C11 C17 1.530(3) . ? C13 C16 1.525(3) . ? C13 C15 1.525(3) . ? C13 C14 1.533(3) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C19 1.531(3) . ? C17 C18 1.533(3) . ? C17 C20 1.534(3) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.385(3) . ? C22 C23 1.379(4) . ? C22 H22 0.9500 . ? C23 C24 1.364(4) . ? C23 H23 0.9500 . ? C24 C25 1.377(3) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C32 1.531(3) . ? C26 C27 1.533(3) . ? C27 C28 1.385(3) . ? C28 C29 1.386(4) . ? C28 H28 0.9500 . ? C29 C30 1.364(4) . ? C29 H29 0.9500 . ? C30 C31 1.384(3) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C33 1.369(4) . ? C33 C34 1.367(4) . ? C33 H33 0.9500 . ? C34 C35 1.368(5) . ? C34 H34 0.9500 . ? C35 C36 1.371(5) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C42 1.381(3) . ? C37 C38 1.405(3) . ? C38 C39 1.412(3) . ? C39 C40 1.387(3) . ? C39 C43 1.535(3) . ? C40 C41 1.393(3) . ? C40 H40 0.9500 . ? C41 C42 1.397(3) . ? C41 C47 1.532(3) . ? C42 H42 0.9500 . ? C43 C44 1.494(4) . ? C43 C45 1.502(4) . ? C43 C46 1.523(3) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C48 1.529(3) . ? C47 C50 1.535(3) . ? C47 C49 1.540(3) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? Cl1 O12 1.337(3) . ? Cl1 O9 1.396(3) . ? Cl1 O10 1.419(3) . ? Cl1 O11 1.442(3) . ? 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 O4 151.69(6) . 2_666 ? O3 Fe1 O2 88.28(6) . . ? O4 Fe1 O2 100.55(5) 2_666 . ? O3 Fe1 O4 79.61(5) . . ? O4 Fe1 O4 72.27(6) 2_666 . ? O2 Fe1 O4 114.98(5) . . ? O3 Fe1 O1 104.29(6) . . ? O4 Fe1 O1 103.91(5) 2_666 . ? O2 Fe1 O1 76.57(5) . . ? O4 Fe1 O1 168.15(5) . . ? O3 Fe1 N1 86.52(6) . . ? O4 Fe1 N1 98.50(6) 2_666 . ? O2 Fe1 N1 148.79(6) . . ? O4 Fe1 N1 94.27(6) . . ? O1 Fe1 N1 74.99(6) . . ? O5 Fe2 O6 103.20(7) . . ? O5 Fe2 O1 149.13(6) . . ? O6 Fe2 O1 103.79(6) . . ? O5 Fe2 O2 81.61(6) . . ? O6 Fe2 O2 164.37(6) . . ? O1 Fe2 O2 76.39(5) . . ? O5 Fe2 N3 92.23(6) . . ? O6 Fe2 N3 85.36(6) . . ? O1 Fe2 N3 75.36(6) . . ? O2 Fe2 N3 109.50(6) . . ? O5 Fe2 N2 93.68(6) . . ? O6 Fe2 N2 77.26(6) . . ? O1 Fe2 N2 106.63(6) . . ? O2 Fe2 N2 87.66(6) . . ? N3 Fe2 N2 162.51(7) . . ? C1 O1 Fe2 116.43(12) . . ? C1 O1 Fe1 117.55(12) . . ? Fe2 O1 Fe1 101.24(6) . . ? C37 O2 Fe1 125.49(11) . . ? C37 O2 Fe2 109.61(11) . . ? Fe1 O2 Fe2 102.36(6) . . ? C12 O3 Fe1 117.89(12) . . ? C7 O4 Fe1 139.82(12) . 2_666 ? C7 O4 Fe1 112.43(11) . . ? Fe1 O4 Fe1 107.73(6) 2_666 . ? C38 O5 Fe2 116.03(12) . . ? C26 O6 Fe2 122.00(13) . . ? C1 O7 C51 113.78(18) . . ? C52 O8 C26 113.06(17) . . ? C2 N1 C6 119.55(18) . . ? C2 N1 Fe1 115.99(13) . . ? C6 N1 Fe1 123.71(14) . . ? C27 N2 C31 118.76(19) . . ? C27 N2 Fe2 112.50(13) . . ? C31 N2 Fe2 125.70(15) . . ? C25 N3 C21 119.52(18) . . ? C25 N3 Fe2 124.43(15) . . ? C21 N3 Fe2 114.59(13) . . ? C32 N4 C36 123.5(3) . . ? C32 N4 H4A 118.2 . . ? C36 N4 H4A 118.2 . . ? O1 C1 O7 111.99(16) . . ? O1 C1 C21 109.83(16) . . ? O7 C1 C21 104.61(17) . . ? O1 C1 C2 108.89(16) . . ? O7 C1 C2 110.88(16) . . ? C21 C1 C2 110.60(17) . . ? N1 C2 C3 121.3(2) . . ? N1 C2 C1 115.29(16) . . ? C3 C2 C1 123.38(19) . . ? C4 C3 C2 119.2(2) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C3 C4 C5 119.2(2) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? C4 C5 C6 118.9(2) . . ? C4 C5 H5 120.6 . . ? C6 C5 H5 120.6 . . ? N1 C6 C5 121.8(2) . . ? N1 C6 H6 119.1 . . ? C5 C6 H6 119.1 . . ? O4 C7 C8 124.90(17) . . ? O4 C7 C12 113.23(17) . . ? C8 C7 C12 121.87(17) . . ? C7 C8 C9 119.45(18) . . ? C7 C8 H8 120.3 . . ? C9 C8 H8 120.3 . . ? C8 C9 C10 117.86(19) . . ? C8 C9 C13 122.26(19) . . ? C10 C9 C13 119.79(18) . . ? C11 C10 C9 124.56(18) . . ? C11 C10 H10 117.7 . . ? C9 C10 H10 117.7 . . ? C10 C11 C12 116.35(18) . . ? C10 C11 C17 122.87(17) . . ? C12 C11 C17 120.75(18) . . ? O3 C12 C7 116.78(16) . . ? O3 C12 C11 123.36(18) . . ? C7 C12 C11 119.86(18) . . ? C16 C13 C15 107.1(2) . . ? C16 C13 C9 111.04(19) . . ? C15 C13 C9 112.73(18) . . ? C16 C13 C14 108.8(2) . . ? C15 C13 C14 108.0(2) . . ? C9 C13 C14 109.08(19) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C11 C17 C19 111.97(18) . . ? C11 C17 C18 110.54(17) . . ? C19 C17 C18 107.19(18) . . ? C11 C17 C20 108.65(17) . . ? C19 C17 C20 108.66(17) . . ? C18 C17 C20 109.80(19) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N3 C21 C22 120.7(2) . . ? N3 C21 C1 114.71(17) . . ? C22 C21 C1 124.6(2) . . ? C23 C22 C21 119.3(2) . . ? C23 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? C24 C23 C22 119.6(2) . . ? C24 C23 H23 120.2 . . ? C22 C23 H23 120.2 . . ? C23 C24 C25 118.2(2) . . ? C23 C24 H24 120.9 . . ? C25 C24 H24 120.9 . . ? N3 C25 C24 122.6(2) . . ? N3 C25 H25 118.7 . . ? C24 C25 H25 118.7 . . ? O6 C26 O8 114.00(18) . . ? O6 C26 C32 109.60(18) . . ? O8 C26 C32 101.17(18) . . ? O6 C26 C27 110.60(18) . . ? O8 C26 C27 110.89(18) . . ? C32 C26 C27 110.19(18) . . ? N2 C27 C28 122.6(2) . . ? N2 C27 C26 114.04(18) . . ? C28 C27 C26 123.4(2) . . ? C27 C28 C29 118.1(3) . . ? C27 C28 H28 121.0 . . ? C29 C28 H28 121.0 . . ? C30 C29 C28 119.5(2) . . ? C30 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? C29 C30 C31 119.5(2) . . ? C29 C30 H30 120.3 . . ? C31 C30 H30 120.3 . . ? N2 C31 C30 121.5(2) . . ? N2 C31 H31 119.2 . . ? C30 C31 H31 119.2 . . ? N4 C32 C33 118.4(2) . . ? N4 C32 C26 113.7(2) . . ? C33 C32 C26 127.9(2) . . ? C34 C33 C32 119.8(3) . . ? C34 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? C33 C34 C35 120.6(3) . . ? C33 C34 H34 119.7 . . ? C35 C34 H34 119.7 . . ? C34 C35 C36 119.2(3) . . ? C34 C35 H35 120.4 . . ? C36 C35 H35 120.4 . . ? N4 C36 C35 118.4(3) . . ? N4 C36 H36 120.8 . . ? C35 C36 H36 120.8 . . ? O2 C37 C42 122.63(17) . . ? O2 C37 C38 115.29(17) . . ? C42 C37 C38 122.03(18) . . ? O5 C38 C37 116.49(17) . . ? O5 C38 C39 123.83(18) . . ? C37 C38 C39 119.67(19) . . ? C40 C39 C38 116.27(19) . . ? C40 C39 C43 120.11(19) . . ? C38 C39 C43 123.5(2) . . ? C39 C40 C41 124.87(19) . . ? C39 C40 H40 117.6 . . ? C41 C40 H40 117.6 . . ? C40 C41 C42 117.7(2) . . ? C40 C41 C47 119.14(18) . . ? C42 C41 C47 123.10(19) . . ? C37 C42 C41 119.36(19) . . ? C37 C42 H42 120.3 . . ? C41 C42 H42 120.3 . . ? C44 C43 C45 109.3(3) . . ? C44 C43 C46 109.4(3) . . ? C45 C43 C46 105.4(2) . . ? C44 C43 C39 108.7(2) . . ? C45 C43 C39 112.1(2) . . ? C46 C43 C39 111.8(2) . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C43 C46 H46A 109.5 . . ? C43 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C43 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C48 C47 C41 111.88(17) . . ? C48 C47 C50 108.51(19) . . ? C41 C47 C50 110.32(19) . . ? C48 C47 C49 108.2(2) . . ? C41 C47 C49 109.03(18) . . ? C50 C47 C49 108.86(18) . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C47 C49 H49A 109.5 . . ? C47 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C47 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C47 C50 H50A 109.5 . . ? C47 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C47 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? O7 C51 H51A 109.5 . . ? O7 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? O7 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? O8 C52 H52A 109.5 . . ? O8 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? O8 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? O12 Cl1 O9 113.38(19) . . ? O12 Cl1 O10 117.7(2) . . ? O9 Cl1 O10 105.13(18) . . ? O12 Cl1 O11 105.7(2) . . ? O9 Cl1 O11 117.2(2) . . ? O10 Cl1 O11 97.12(18) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N4 H4A O6 0.88 2.08 2.523(3) 110.3 . N4 H4A O7 0.88 2.37 3.107(3) 141.1 . _diffrn_measured_fraction_theta_max 0.921 _diffrn_reflns_theta_full 26.06 _diffrn_measured_fraction_theta_full 0.921 _refine_diff_density_max 0.595 _refine_diff_density_min -0.290 _refine_diff_density_rms 0.052 #===END data_(2) _database_code_CSD 211397 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C86 H117 Fe3 N6 O12' _chemical_formula_weight 1594.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y+1/2, z+1/2' '-x, -y, -z' '-x, y-1/2, -z-1/2' _cell_length_a 21.495(2) _cell_length_b 18.6521(13) _cell_length_c 23.326(3) _cell_angle_alpha 90.00 _cell_angle_beta 112.586(14) _cell_angle_gamma 90.00 _cell_volume 8634.8(16) _cell_formula_units_Z 4 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Parallelepiped _exptl_crystal_colour Dark-Red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.226 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3396 _exptl_absorpt_coefficient_mu 0.558 _exptl_absorpt_correction_type None _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(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 STOE-IPDS _diffrn_measurement_method 'Imaging Plate Detector System' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 67360 _diffrn_reflns_av_R_equivalents 0.0535 _diffrn_reflns_av_sigmaI/netI 0.0528 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 26.36 _reflns_number_total 17043 _reflns_number_gt 10336 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE-IPDS software (Stoe, 2.93, 1997)' _computing_cell_refinement 'STOE-IPDS software (Stoe, 2.93, 1997)' _computing_data_reduction 'XRED (Stoe, 1.08, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ZORTEP (Zsolnai, 1996)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0615P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17043 _refine_ls_number_parameters 964 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0849 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.0932 _refine_ls_wR_factor_gt 0.0877 _refine_ls_goodness_of_fit_ref 0.854 _refine_ls_restrained_S_all 0.854 _refine_ls_shift/su_max 0.003 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.702251(12) 0.187532(14) 0.032669(11) 0.03320(6) Uani 1 d . . . Fe2 Fe 0.800852(12) 0.069557(13) 0.005636(11) 0.03294(6) Uani 1 d . . . Fe3 Fe 0.863295(12) 0.237473(13) 0.057904(11) 0.03286(6) Uani 1 d . . . O1 O 0.71301(6) 0.11938(7) -0.03178(6) 0.0412(3) Uani 1 d . . . O2 O 0.79405(7) 0.13292(8) 0.07475(6) 0.0466(3) Uani 1 d . . . O3 O 0.62011(7) 0.20929(8) -0.03696(6) 0.0448(3) Uani 1 d . . . O4 O 0.76405(7) 0.26213(7) 0.02346(6) 0.0425(3) Uani 1 d . . . O5 O 0.69113(7) 0.23239(7) 0.10175(6) 0.0431(3) Uani 1 d . . . O6 O 0.71735(7) 0.18318(7) 0.20045(6) 0.0450(3) Uani 1 d . . . H6 H 0.7277 0.2213 0.2211 0.050 Uiso 1 calc R . . O7 O 0.86172(6) 0.15770(7) -0.00002(6) 0.0383(3) Uani 1 d . . . O8 O 0.77113(7) -0.02576(7) 0.01415(6) 0.0431(3) Uani 1 d . . . O9 O 0.80968(7) 0.03133(8) -0.06890(6) 0.0455(3) Uani 1 d . . . O10 O 0.91845(7) 0.10655(8) -0.05674(7) 0.0530(4) Uani 1 d . . . H10 H 0.8846 0.0796 -0.0707 0.058 Uiso 1 calc R . . O11 O 0.89471(7) 0.22202(8) 0.14314(7) 0.0482(3) Uani 1 d . . . O12 O 0.87009(7) 0.33877(7) 0.04973(6) 0.0439(3) Uani 1 d . . . N1 N 0.65087(8) 0.10291(9) 0.06352(8) 0.0420(4) Uani 1 d . . . N2 N 0.90170(8) 0.04082(9) 0.06380(7) 0.0414(3) Uani 1 d . . . N3 N 0.96306(8) 0.24596(10) 0.05286(8) 0.0463(4) Uani 1 d . . . C1 C 0.65249(10) 0.11039(11) -0.08098(9) 0.0456(4) Uani 1 d . . . C2 C 0.63979(10) 0.05421(11) -0.12341(9) 0.0443(4) Uani 1 d . . . H2 H 0.6743 0.0207 -0.1201 0.049 Uiso 1 calc R . . C3 C 0.57555(10) 0.04726(11) -0.17125(9) 0.0425(4) Uani 1 d . . . C4 C 0.52643(10) 0.09744(11) -0.17360(9) 0.0457(4) Uani 1 d . . . H4 H 0.4830 0.0926 -0.2057 0.050 Uiso 1 calc R . . C5 C 0.53680(10) 0.15397(11) -0.13208(9) 0.0444(4) Uani 1 d . . . C6 C 0.60089(10) 0.16037(11) -0.08267(9) 0.0463(5) Uani 1 d . . . C7 C 0.56205(11) -0.01464(13) -0.21781(10) 0.0542(5) Uani 1 d . . . C8 C 0.48805(11) -0.02011(14) -0.26278(11) 0.0587(6) Uani 1 d . . . H8A H 0.4826 -0.0611 -0.2906 0.065 Uiso 1 calc R . . H8B H 0.4749 0.0240 -0.2873 0.065 Uiso 1 calc R . . H8C H 0.4594 -0.0268 -0.2391 0.065 Uiso 1 calc R . . C9 C 0.58118(12) -0.08577(13) -0.18107(12) 0.0618(6) Uani 1 d . . . H9A H 0.5731 -0.1259 -0.2101 0.068 Uiso 1 calc R . . H9B H 0.5536 -0.0918 -0.1563 0.068 Uiso 1 calc R . . H9C H 0.6289 -0.0846 -0.1535 0.068 Uiso 1 calc R . . C10 C 0.60613(11) -0.00595(14) -0.25560(11) 0.0572(5) Uani 1 d . . . H10A H 0.5982 -0.0462 -0.2846 0.063 Uiso 1 calc R . . H10B H 0.6537 -0.0052 -0.2275 0.063 Uiso 1 calc R . . H10C H 0.5948 0.0391 -0.2789 0.063 Uiso 1 calc R . . C11 C 0.48193(10) 0.20888(12) -0.13705(11) 0.0497(5) Uani 1 d . . . C12 C 0.41503(12) 0.19081(14) -0.19100(12) 0.0640(6) Uani 1 d . . . H12A H 0.3808 0.2263 -0.1925 0.070 Uiso 1 calc R . . H12B H 0.4000 0.1429 -0.1846 0.070 Uiso 1 calc R . . H12C H 0.4217 0.1917 -0.2303 0.070 Uiso 1 calc R . . C13 C 0.46769(12) 0.20784(14) -0.07792(11) 0.0572(5) Uani 1 d . . . H13A H 0.4328 0.2433 -0.0813 0.063 Uiso 1 calc R . . H13B H 0.5090 0.2196 -0.0423 0.063 Uiso 1 calc R . . H13C H 0.4521 0.1600 -0.0722 0.063 Uiso 1 calc R . . C14 C 0.50329(12) 0.28323(12) -0.14753(11) 0.0572(6) Uani 1 d . . . H14A H 0.4681 0.3177 -0.1496 0.063 Uiso 1 calc R . . H14B H 0.5103 0.2842 -0.1866 0.063 Uiso 1 calc R . . H14C H 0.5454 0.2960 -0.1132 0.063 Uiso 1 calc R . . C15 C 0.63485(10) 0.12569(11) 0.10987(9) 0.0450(4) Uani 1 d . . . C16 C 0.59480(10) 0.08499(11) 0.13275(10) 0.0475(4) Uani 1 d . . . H16 H 0.5854 0.1010 0.1673 0.052 Uiso 1 calc R . . C17 C 0.56931(10) 0.02081(11) 0.10359(9) 0.0449(4) Uani 1 d . . . H17 H 0.5397 -0.0065 0.1165 0.049 Uiso 1 calc R . . C18 C 0.58632(10) -0.00378(11) 0.05612(9) 0.0424(4) Uani 1 d . . . H18 H 0.5708 -0.0488 0.0369 0.047 Uiso 1 calc R . . C19 C 0.62667(9) 0.03960(10) 0.03769(9) 0.0425(4) Uani 1 d . . . H19 H 0.6382 0.0236 0.0044 0.047 Uiso 1 calc R . . C20 C 0.66330(10) 0.19840(11) 0.13778(9) 0.0432(4) Uani 1 d . . . C21 C 0.60979(10) 0.24294(11) 0.14703(9) 0.0456(4) Uani 1 d . . . C22 C 0.55803(10) 0.26967(11) 0.09374(9) 0.0474(5) Uani 1 d . . . H22 H 0.5596 0.2638 0.0539 0.052 Uiso 1 calc R . . C23 C 0.50404(10) 0.30512(12) 0.10073(10) 0.0483(5) Uani 1 d . . . H23 H 0.4664 0.3208 0.0656 0.053 Uiso 1 calc R . . C24 C 0.50712(10) 0.31657(11) 0.16027(9) 0.0448(4) Uani 1 d . . . H24 H 0.4720 0.3417 0.1669 0.049 Uiso 1 calc R . . C25 C 0.56123(10) 0.29127(11) 0.20946(10) 0.0504(5) Uani 1 d . . . H25 H 0.5616 0.2999 0.2497 0.055 Uiso 1 calc R . . N4 N 0.61476(8) 0.25470(9) 0.20616(7) 0.0419(3) Uani 1 d . . . C26 C 0.77429(10) -0.07095(11) -0.03038(9) 0.0426(4) Uani 1 d . . . C27 C 0.75693(10) -0.14501(11) -0.03472(9) 0.0442(4) Uani 1 d . . . C28 C 0.75931(10) -0.18147(12) -0.08574(10) 0.0495(5) Uani 1 d . . . H28 H 0.7478 -0.2309 -0.0892 0.054 Uiso 1 calc R . . C29 C 0.77713(11) -0.15208(12) -0.13251(10) 0.0509(5) Uani 1 d . . . C30 C 0.79437(9) -0.07799(11) -0.12755(9) 0.0441(4) Uani 1 d . . . H30 H 0.8060 -0.0552 -0.1584 0.049 Uiso 1 calc R . . C31 C 0.79381(10) -0.03959(11) -0.07644(9) 0.0448(4) Uani 1 d . . . C32 C 0.73620(11) -0.18254(13) 0.01299(10) 0.0523(5) Uani 1 d . . . C33 C 0.67313(13) -0.14627(14) 0.01449(13) 0.0643(6) Uani 1 d . . . H33A H 0.6604 -0.1691 0.0462 0.071 Uiso 1 calc R . . H33B H 0.6362 -0.1511 -0.0262 0.071 Uiso 1 calc R . . H33C H 0.6824 -0.0953 0.0244 0.071 Uiso 1 calc R . . C34 C 0.71861(13) -0.26167(13) -0.00108(12) 0.0619(6) Uani 1 d . . . H34A H 0.7070 -0.2826 0.0320 0.068 Uiso 1 calc R . . H34B H 0.7575 -0.2871 -0.0035 0.068 Uiso 1 calc R . . H34C H 0.6801 -0.2661 -0.0408 0.068 Uiso 1 calc R . . C35 C 0.79340(13) -0.17746(14) 0.07720(11) 0.0645(6) Uani 1 d . . . H35A H 0.7797 -0.2012 0.1079 0.071 Uiso 1 calc R . . H35B H 0.8034 -0.1269 0.0885 0.071 Uiso 1 calc R . . H35C H 0.8337 -0.2010 0.0762 0.071 Uiso 1 calc R . . C36 C 0.77536(11) -0.19283(13) -0.19093(11) 0.0540(5) Uani 1 d . . . C37 C 0.72414(13) -0.15936(14) -0.24976(12) 0.0648(6) Uani 1 d . . . H37A H 0.7238 -0.1861 -0.2861 0.071 Uiso 1 calc R . . H37B H 0.7365 -0.1093 -0.2528 0.071 Uiso 1 calc R . . H37C H 0.6793 -0.1612 -0.2482 0.071 Uiso 1 calc R . . C38 C 0.75743(13) -0.27210(13) -0.18753(12) 0.0648(6) Uani 1 d . . . H38A H 0.7899 -0.2935 -0.1495 0.071 Uiso 1 calc R . . H38B H 0.7589 -0.2977 -0.2237 0.071 Uiso 1 calc R . . H38C H 0.7120 -0.2756 -0.1873 0.071 Uiso 1 calc R . . C39 C 0.84586(12) -0.19053(15) -0.19310(12) 0.0645(6) Uani 1 d . . . H39A H 0.8785 -0.2127 -0.1554 0.071 Uiso 1 calc R . . H39B H 0.8587 -0.1406 -0.1956 0.071 Uiso 1 calc R . . H39C H 0.8454 -0.2169 -0.2296 0.071 Uiso 1 calc R . . C40 C 0.92483(10) 0.13335(10) 0.00223(9) 0.0434(4) Uani 1 d . . . C41 C 0.95096(11) 0.07584(11) 0.05148(10) 0.0481(5) Uani 1 d . . . C42 C 1.01949(11) 0.06021(12) 0.08418(10) 0.0503(5) Uani 1 d . . . H42 H 1.0529 0.0848 0.0745 0.055 Uiso 1 calc R . . C43 C 1.03802(10) 0.00938(12) 0.13011(10) 0.0483(5) Uani 1 d . . . H43 H 1.0841 -0.0021 0.1523 0.053 Uiso 1 calc R . . C44 C 0.98820(11) -0.02475(13) 0.14347(10) 0.0546(5) Uani 1 d . . . H44 H 0.9997 -0.0582 0.1766 0.060 Uiso 1 calc R . . C45 C 0.92132(11) -0.00968(13) 0.10801(10) 0.0515(5) Uani 1 d . . . H45 H 0.8876 -0.0365 0.1154 0.057 Uiso 1 calc R . . C46 C 0.97379(10) 0.19543(11) 0.01725(9) 0.0439(4) Uani 1 d . . . C47 C 1.02663(10) 0.19963(11) -0.00399(9) 0.0448(4) Uani 1 d . . . H47 H 1.0324 0.1636 -0.0303 0.049 Uiso 1 calc R . . C48 C 1.07022(10) 0.25792(11) 0.01448(9) 0.0452(4) Uani 1 d . . . H48 H 1.1063 0.2624 0.0008 0.050 Uiso 1 calc R . . C49 C 1.06040(10) 0.30951(11) 0.05313(9) 0.0464(4) Uani 1 d . . . H49 H 1.0906 0.3487 0.0674 0.051 Uiso 1 calc R . . C50 C 1.00640(10) 0.30304(11) 0.07040(9) 0.0449(4) Uani 1 d . . . H50 H 0.9988 0.3395 0.0954 0.049 Uiso 1 calc R . . C51 C 0.82623(11) 0.12138(11) 0.13782(9) 0.0478(5) Uani 1 d . . . C52 C 0.80907(10) 0.06155(11) 0.16722(9) 0.0464(4) Uani 1 d . . . H52 H 0.7739 0.0300 0.1436 0.051 Uiso 1 calc R . . C53 C 0.84384(10) 0.04951(11) 0.23044(9) 0.0469(5) Uani 1 d . . . C54 C 0.89508(10) 0.09818(11) 0.26352(9) 0.0463(4) Uani 1 d . . . H54 H 0.9186 0.0904 0.3068 0.051 Uiso 1 calc R . . C55 C 0.91379(10) 0.15791(11) 0.23654(9) 0.0460(4) Uani 1 d . . . C56 C 0.87867(10) 0.16896(11) 0.17279(9) 0.0455(4) Uani 1 d . . . C57 C 0.82861(11) -0.01877(13) 0.25905(10) 0.0494(5) Uani 1 d . . . C58 C 0.75481(13) -0.03484(15) 0.23408(13) 0.0698(7) Uani 1 d . . . H58A H 0.7469 -0.0785 0.2536 0.077 Uiso 1 calc R . . H58B H 0.7385 -0.0419 0.1890 0.077 Uiso 1 calc R . . H58C H 0.7307 0.0053 0.2432 0.077 Uiso 1 calc R . . C59 C 0.86770(13) -0.08175(13) 0.24849(12) 0.0638(6) Uani 1 d . . . H59A H 0.9160 -0.0708 0.2662 0.070 Uiso 1 calc R . . H59B H 0.8533 -0.0905 0.2038 0.070 Uiso 1 calc R . . H59C H 0.8590 -0.1246 0.2686 0.070 Uiso 1 calc R . . C60 C 0.85178(14) -0.01288(15) 0.32927(12) 0.0681(7) Uani 1 d . . . H60A H 0.9004 -0.0036 0.3475 0.075 Uiso 1 calc R . . H60B H 0.8420 -0.0578 0.3459 0.075 Uiso 1 calc R . . H60C H 0.8278 0.0266 0.3396 0.075 Uiso 1 calc R . . C61 C 0.97220(10) 0.20666(12) 0.27385(9) 0.0494(5) Uani 1 d . . . C62 C 1.02878(13) 0.20034(15) 0.24946(13) 0.0694(7) Uani 1 d . . . H62A H 1.0662 0.2318 0.2736 0.076 Uiso 1 calc R . . H62B H 1.0117 0.2146 0.2057 0.076 Uiso 1 calc R . . H62C H 1.0446 0.1506 0.2535 0.076 Uiso 1 calc R . . C63 C 1.00159(13) 0.18678(16) 0.34288(12) 0.0751(8) Uani 1 d . . . H63A H 0.9662 0.1899 0.3596 0.083 Uiso 1 calc R . . H63B H 1.0382 0.2200 0.3654 0.083 Uiso 1 calc R . . H63C H 1.0192 0.1377 0.3478 0.083 Uiso 1 calc R . . C64 C 0.94727(13) 0.28485(13) 0.26890(12) 0.0659(6) Uani 1 d . . . H64A H 0.9108 0.2880 0.2842 0.073 Uiso 1 calc R . . H64B H 0.9306 0.3003 0.2254 0.073 Uiso 1 calc R . . H64C H 0.9846 0.3159 0.2939 0.073 Uiso 1 calc R . . C65 C 0.81301(10) 0.37681(11) 0.03635(9) 0.0453(4) Uani 1 d . . . C66 C 0.80975(11) 0.45235(11) 0.03459(9) 0.0489(5) Uani 1 d . . . C67 C 0.74671(10) 0.48181(12) 0.02065(9) 0.0488(5) Uani 1 d . . . H67 H 0.7432 0.5326 0.0191 0.054 Uiso 1 calc R . . C68 C 0.68729(10) 0.44212(11) 0.00858(9) 0.0451(4) Uani 1 d . . . C69 C 0.69122(10) 0.36680(10) 0.00773(9) 0.0422(4) Uani 1 d . . . H69 H 0.6522 0.3378 -0.0016 0.046 Uiso 1 calc R . . C70 C 0.75331(9) 0.33688(10) 0.02088(8) 0.0380(4) Uani 1 d . . . C71 C 0.87353(11) 0.49827(12) 0.05089(10) 0.0492(5) Uani 1 d . . . C72 C 0.85706(13) 0.57788(14) 0.04337(13) 0.0681(7) Uani 1 d . . . H72A H 0.8339 0.5916 0.0706 0.075 Uiso 1 calc R . . H72B H 0.8278 0.5879 0.0001 0.075 Uiso 1 calc R . . H72C H 0.8989 0.6055 0.0545 0.075 Uiso 1 calc R . . C73 C 0.92104(13) 0.48473(13) 0.11793(12) 0.0646(6) Uani 1 d . . . H73A H 0.8985 0.4976 0.1458 0.071 Uiso 1 calc R . . H73B H 0.9617 0.5140 0.1277 0.071 Uiso 1 calc R . . H73C H 0.9335 0.4339 0.1233 0.071 Uiso 1 calc R . . C74 C 0.90920(13) 0.47937(14) 0.00772(12) 0.0634(6) Uani 1 d . . . H74A H 0.8790 0.4886 -0.0354 0.070 Uiso 1 calc R . . H74B H 0.9217 0.4286 0.0126 0.070 Uiso 1 calc R . . H74C H 0.9498 0.5088 0.0182 0.070 Uiso 1 calc R . . C75 C 0.62154(10) 0.48063(11) 0.00023(10) 0.0487(5) Uani 1 d . . . C76 C 0.62677(14) 0.53564(16) 0.04727(13) 0.0732(7) Uani 1 d . . . H76A H 0.6538 0.5170 0.0887 0.081 Uiso 1 calc R . . H76B H 0.5816 0.5479 0.0451 0.081 Uiso 1 calc R . . H76C H 0.6484 0.5786 0.0393 0.081 Uiso 1 calc R . . C77 C 0.56390(14) 0.43166(15) -0.01548(13) 0.0717(7) Uani 1 d . . . H77A H 0.5660 0.4063 0.0220 0.079 Uiso 1 calc R . . H77B H 0.5653 0.3969 -0.0464 0.079 Uiso 1 calc R . . H77C H 0.5219 0.4592 -0.0325 0.079 Uiso 1 calc R . . C78 C 0.60131(14) 0.52533(18) -0.05926(13) 0.0800(8) Uani 1 d . . . H78A H 0.5946 0.4936 -0.0947 0.088 Uiso 1 calc R . . H78B H 0.6371 0.5599 -0.0553 0.088 Uiso 1 calc R . . H78C H 0.5594 0.5511 -0.0659 0.088 Uiso 1 calc R . . N5 N 0.73267(10) 0.23515(11) 0.32488(10) 0.0599(5) Uani 1 d . . . H5 H 0.7064 0.2327 0.2826 0.066 Uiso 1 calc R . . C79 C 0.74095(14) 0.31360(15) 0.34028(13) 0.0692(7) Uani 1 d . . . H79A H 0.6964 0.3340 0.3344 0.076 Uiso 1 calc R . . H79B H 0.7705 0.3191 0.3846 0.076 Uiso 1 calc R . . C80 C 0.77024(14) 0.35582(16) 0.30195(14) 0.0750(8) Uani 1 d . . . H80A H 0.7759 0.4059 0.3157 0.082 Uiso 1 calc R . . H80B H 0.7398 0.3535 0.2581 0.082 Uiso 1 calc R . . H80C H 0.8141 0.3357 0.3069 0.082 Uiso 1 calc R . . C81 C 0.79590(13) 0.19890(16) 0.33306(13) 0.0688(7) Uani 1 d . . . H81A H 0.8182 0.2251 0.3093 0.076 Uiso 1 calc R . . H81B H 0.7856 0.1499 0.3156 0.076 Uiso 1 calc R . . C82 C 0.84464(14) 0.19375(16) 0.40074(13) 0.0764(8) Uani 1 d . . . H82A H 0.8862 0.1701 0.4030 0.084 Uiso 1 calc R . . H82B H 0.8239 0.1658 0.4243 0.084 Uiso 1 calc R . . H82C H 0.8551 0.2420 0.4184 0.084 Uiso 1 calc R . . C83 C 0.69075(13) 0.20399(15) 0.35659(13) 0.0668(6) Uani 1 d . . . H83A H 0.6472 0.2299 0.3430 0.073 Uiso 1 calc R . . H83B H 0.7140 0.2107 0.4020 0.073 Uiso 1 calc R . . C84 C 0.67719(14) 0.12346(15) 0.34247(13) 0.0693(7) Uani 1 d . . . H84A H 0.6501 0.1049 0.3647 0.076 Uiso 1 calc R . . H84B H 0.7201 0.0976 0.3560 0.076 Uiso 1 calc R . . H84C H 0.6527 0.1167 0.2977 0.076 Uiso 1 calc R . . N6 N 0.17728(11) 0.99044(12) 0.25873(10) 0.0681(6) Uani 1 d . . . C85 C 0.19270(15) 0.93949(16) 0.28920(13) 0.0761(8) Uani 1 d . . . C86 C 0.21690(15) 0.87619(18) 0.33467(13) 0.0808(8) Uani 1 d . . . H86A H 0.2305 0.8938 0.3773 0.089 Uiso 1 calc R . . H86B H 0.2554 0.8530 0.3296 0.089 Uiso 1 calc R . . H86C H 0.1802 0.8414 0.3260 0.089 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 0.03202(12) 0.03016(13) 0.03302(12) 0.00001(10) 0.00761(10) 0.00087(10) Fe2 0.03227(12) 0.02901(12) 0.03346(12) -0.00069(9) 0.00811(10) 0.00071(10) Fe3 0.03217(12) 0.02764(12) 0.03388(12) 0.00061(9) 0.00724(10) 0.00044(10) O1 0.0396(7) 0.0392(7) 0.0429(7) -0.0063(6) 0.0136(6) 0.0000(6) O2 0.0458(7) 0.0463(8) 0.0466(7) -0.0051(6) 0.0164(6) 0.0046(6) O3 0.0407(7) 0.0428(8) 0.0441(7) 0.0008(6) 0.0085(6) -0.0018(6) O4 0.0436(7) 0.0378(7) 0.0459(7) 0.0027(6) 0.0169(6) 0.0044(6) O5 0.0454(7) 0.0345(7) 0.0466(7) -0.0064(6) 0.0144(6) 0.0023(6) O6 0.0465(7) 0.0373(7) 0.0459(7) -0.0026(6) 0.0116(6) 0.0031(6) O7 0.0371(6) 0.0338(7) 0.0397(6) -0.0014(5) 0.0101(5) 0.0094(5) O8 0.0421(7) 0.0377(7) 0.0454(7) 0.0009(6) 0.0122(6) 0.0022(6) O9 0.0450(7) 0.0434(8) 0.0479(7) -0.0096(6) 0.0177(6) -0.0081(6) O10 0.0480(8) 0.0528(9) 0.0557(8) -0.0088(7) 0.0174(7) -0.0128(7) O11 0.0427(7) 0.0422(8) 0.0500(7) 0.0093(6) 0.0071(6) -0.0078(6) O12 0.0457(7) 0.0313(7) 0.0496(7) 0.0026(6) 0.0126(6) 0.0003(5) N1 0.0411(8) 0.0366(9) 0.0454(8) -0.0015(7) 0.0133(7) 0.0050(7) N2 0.0407(8) 0.0369(8) 0.0437(8) 0.0021(7) 0.0129(7) 0.0007(7) N3 0.0426(8) 0.0432(9) 0.0455(8) -0.0066(7) 0.0087(7) 0.0045(7) C1 0.0397(10) 0.0476(11) 0.0472(10) 0.0062(9) 0.0141(8) -0.0089(8) C2 0.0348(9) 0.0434(11) 0.0452(9) -0.0014(8) 0.0048(8) 0.0020(8) C3 0.0429(10) 0.0398(10) 0.0431(9) -0.0026(8) 0.0147(8) -0.0039(8) C4 0.0391(10) 0.0431(11) 0.0459(10) -0.0007(8) 0.0065(8) 0.0006(8) C5 0.0370(10) 0.0445(11) 0.0465(10) 0.0033(8) 0.0102(8) 0.0070(8) C6 0.0426(10) 0.0441(11) 0.0464(10) 0.0128(9) 0.0107(9) 0.0044(8) C7 0.0481(11) 0.0526(13) 0.0538(11) -0.0116(10) 0.0106(10) -0.0041(10) C8 0.0446(12) 0.0566(14) 0.0645(13) -0.0079(11) 0.0095(11) -0.0072(10) C9 0.0580(13) 0.0523(13) 0.0627(13) -0.0084(11) 0.0097(11) -0.0031(11) C10 0.0523(12) 0.0569(14) 0.0608(13) -0.0058(11) 0.0199(11) -0.0003(10) C11 0.0342(9) 0.0430(11) 0.0622(12) -0.0045(10) 0.0077(9) 0.0040(8) C12 0.0526(13) 0.0583(14) 0.0643(13) -0.0094(12) 0.0038(11) 0.0146(11) C13 0.0502(12) 0.0599(14) 0.0620(13) 0.0046(11) 0.0221(11) 0.0067(11) C14 0.0548(13) 0.0454(12) 0.0620(13) 0.0104(10) 0.0120(11) 0.0043(10) C15 0.0471(10) 0.0380(10) 0.0477(10) 0.0033(8) 0.0157(9) 0.0039(8) C16 0.0465(11) 0.0382(10) 0.0526(11) 0.0025(9) 0.0131(9) -0.0009(9) C17 0.0427(10) 0.0404(10) 0.0484(10) 0.0017(8) 0.0140(8) -0.0008(8) C18 0.0394(9) 0.0388(10) 0.0442(9) 0.0034(8) 0.0108(8) -0.0022(8) C19 0.0399(10) 0.0383(10) 0.0431(9) -0.0043(8) 0.0092(8) 0.0040(8) C20 0.0437(10) 0.0391(10) 0.0428(9) 0.0012(8) 0.0120(8) 0.0036(8) C21 0.0450(10) 0.0412(11) 0.0464(10) -0.0044(8) 0.0130(9) -0.0023(9) C22 0.0455(11) 0.0469(11) 0.0395(9) -0.0007(8) 0.0047(8) 0.0056(9) C23 0.0400(10) 0.0478(12) 0.0466(10) 0.0013(9) 0.0051(8) 0.0086(9) C24 0.0399(10) 0.0399(10) 0.0470(10) -0.0011(8) 0.0082(8) 0.0037(8) C25 0.0447(11) 0.0402(11) 0.0513(11) 0.0038(9) 0.0018(9) 0.0052(9) N4 0.0394(8) 0.0401(9) 0.0412(8) -0.0009(7) 0.0099(7) 0.0033(7) C26 0.0385(9) 0.0420(11) 0.0452(9) -0.0033(8) 0.0138(8) 0.0061(8) C27 0.0417(10) 0.0397(10) 0.0449(9) -0.0024(8) 0.0095(8) 0.0048(8) C28 0.0405(10) 0.0473(12) 0.0484(10) -0.0013(9) 0.0034(9) -0.0027(9) C29 0.0464(11) 0.0485(12) 0.0482(10) -0.0105(9) 0.0075(9) 0.0026(9) C30 0.0349(9) 0.0458(11) 0.0465(10) -0.0038(9) 0.0099(8) -0.0035(8) C31 0.0478(11) 0.0384(10) 0.0431(9) -0.0109(8) 0.0119(9) -0.0056(8) C32 0.0491(11) 0.0498(12) 0.0530(11) 0.0017(10) 0.0140(10) -0.0035(10) C33 0.0614(14) 0.0573(14) 0.0709(15) 0.0060(12) 0.0215(12) 0.0017(12) C34 0.0596(13) 0.0481(13) 0.0696(14) 0.0002(11) 0.0155(12) -0.0096(11) C35 0.0646(15) 0.0595(15) 0.0624(14) -0.0016(12) 0.0167(12) -0.0114(12) C36 0.0447(11) 0.0509(12) 0.0593(12) -0.0125(10) 0.0121(10) -0.0006(10) C37 0.0572(14) 0.0622(16) 0.0642(14) -0.0166(12) 0.0113(12) -0.0025(11) C38 0.0645(15) 0.0529(14) 0.0670(14) -0.0176(12) 0.0143(12) 0.0023(11) C39 0.0585(14) 0.0606(15) 0.0672(14) -0.0160(12) 0.0162(12) -0.0025(12) C40 0.0403(10) 0.0344(10) 0.0509(10) -0.0016(8) 0.0125(8) -0.0056(8) C41 0.0494(11) 0.0372(10) 0.0480(10) -0.0010(8) 0.0080(9) 0.0034(9) C42 0.0480(11) 0.0442(11) 0.0501(11) -0.0036(9) 0.0094(9) 0.0069(9) C43 0.0418(10) 0.0468(12) 0.0466(10) 0.0027(9) 0.0060(9) 0.0061(9) C44 0.0518(12) 0.0528(13) 0.0482(11) 0.0101(10) 0.0069(10) 0.0160(10) C45 0.0501(11) 0.0527(13) 0.0465(10) -0.0009(9) 0.0128(9) 0.0012(10) C46 0.0372(9) 0.0459(11) 0.0416(9) 0.0007(8) 0.0071(8) -0.0039(8) C47 0.0441(10) 0.0408(10) 0.0460(10) -0.0053(8) 0.0133(8) -0.0116(8) C48 0.0430(10) 0.0385(10) 0.0483(10) -0.0024(8) 0.0110(8) -0.0037(8) C49 0.0414(10) 0.0444(11) 0.0469(10) 0.0012(9) 0.0096(8) -0.0109(9) C50 0.0434(10) 0.0350(10) 0.0477(10) -0.0029(8) 0.0080(8) -0.0103(8) C51 0.0530(11) 0.0406(11) 0.0470(10) -0.0039(9) 0.0161(9) 0.0012(9) C52 0.0440(10) 0.0393(10) 0.0481(10) -0.0066(8) 0.0090(9) -0.0044(8) C53 0.0446(11) 0.0404(11) 0.0458(10) 0.0107(8) 0.0064(9) 0.0040(8) C54 0.0393(10) 0.0426(11) 0.0452(10) 0.0007(8) 0.0031(8) 0.0064(8) C55 0.0435(11) 0.0445(11) 0.0443(10) 0.0040(8) 0.0105(9) -0.0018(8) C56 0.0413(10) 0.0436(11) 0.0459(10) -0.0003(8) 0.0103(8) 0.0057(8) C57 0.0445(11) 0.0523(12) 0.0476(10) 0.0023(9) 0.0134(9) 0.0022(9) C58 0.0591(14) 0.0628(16) 0.0698(15) 0.0190(13) 0.0050(12) -0.0053(12) C59 0.0641(14) 0.0475(13) 0.0714(15) 0.0100(11) 0.0166(12) 0.0080(11) C60 0.0755(17) 0.0618(16) 0.0629(14) 0.0068(12) 0.0220(13) -0.0043(13) C61 0.0416(10) 0.0481(12) 0.0444(10) -0.0027(9) 0.0008(8) -0.0090(9) C62 0.0600(14) 0.0666(16) 0.0741(16) -0.0096(14) 0.0173(13) -0.0078(13) C63 0.0593(14) 0.0695(17) 0.0676(15) 0.0039(13) -0.0077(12) -0.0178(13) C64 0.0630(14) 0.0548(14) 0.0662(14) -0.0130(12) 0.0094(12) -0.0044(11) C65 0.0435(10) 0.0401(10) 0.0453(10) 0.0047(8) 0.0094(8) 0.0094(8) C66 0.0493(11) 0.0410(11) 0.0448(10) -0.0002(8) 0.0053(9) -0.0006(9) C67 0.0449(11) 0.0473(12) 0.0439(10) 0.0003(9) 0.0058(9) 0.0012(9) C68 0.0367(10) 0.0428(11) 0.0452(10) -0.0015(8) 0.0040(8) 0.0125(8) C69 0.0381(9) 0.0359(10) 0.0430(9) -0.0068(8) 0.0051(8) 0.0089(8) C70 0.0339(9) 0.0342(9) 0.0402(9) 0.0000(7) 0.0079(7) -0.0021(7) C71 0.0469(11) 0.0421(11) 0.0484(10) -0.0034(9) 0.0072(9) 0.0005(9) C72 0.0626(15) 0.0555(15) 0.0708(15) 0.0066(12) 0.0086(13) -0.0087(12) C73 0.0609(14) 0.0463(13) 0.0661(14) 0.0014(11) 0.0016(12) -0.0019(11) C74 0.0628(14) 0.0537(14) 0.0679(14) 0.0037(12) 0.0185(12) -0.0058(12) C75 0.0469(11) 0.0389(10) 0.0486(10) -0.0035(9) 0.0053(9) 0.0224(9) C76 0.0612(15) 0.0724(18) 0.0711(15) -0.0111(14) 0.0089(13) 0.0049(13) C77 0.0677(16) 0.0610(16) 0.0716(16) -0.0041(13) 0.0103(13) 0.0069(13) C78 0.0608(15) 0.090(2) 0.0676(16) -0.0011(15) 0.0012(13) 0.0166(15) N5 0.0577(11) 0.0594(12) 0.0592(11) -0.0064(9) 0.0186(9) 0.0008(9) C79 0.0654(15) 0.0624(16) 0.0698(15) -0.0152(13) 0.0148(13) 0.0012(13) C80 0.0686(16) 0.0620(16) 0.0781(17) 0.0032(14) 0.0101(14) 0.0074(13) C81 0.0684(16) 0.0628(16) 0.0685(15) -0.0049(13) 0.0189(13) 0.0047(13) C82 0.0699(16) 0.0660(17) 0.0675(15) -0.0068(13) -0.0023(13) 0.0095(14) C83 0.0617(14) 0.0683(17) 0.0668(14) -0.0045(13) 0.0208(12) -0.0030(13) C84 0.0619(15) 0.0700(17) 0.0672(15) -0.0062(13) 0.0151(12) -0.0139(13) N6 0.0683(13) 0.0566(13) 0.0617(12) 0.0073(10) 0.0052(11) 0.0017(10) C85 0.0776(18) 0.0693(18) 0.0641(15) 0.0141(14) 0.0079(14) 0.0017(15) C86 0.0707(17) 0.087(2) 0.0663(15) 0.0110(15) 0.0056(14) 0.0025(15) _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 O5 1.9104(14) . ? Fe1 O3 1.9280(14) . ? Fe1 O4 1.9915(14) . ? Fe1 O1 2.0486(13) . ? Fe1 O2 2.0992(14) . ? Fe1 N1 2.1999(17) . ? Fe2 O8 1.9250(14) . ? Fe2 O9 1.9547(14) . ? Fe2 O1 1.9811(13) . ? Fe2 O2 2.0490(14) . ? Fe2 O7 2.1364(14) . ? Fe2 N2 2.1373(16) . ? Fe3 O11 1.8603(14) . ? Fe3 O12 1.9103(13) . ? Fe3 O7 2.0015(12) . ? Fe3 O4 2.0226(14) . ? Fe3 N3 2.1980(18) . ? O1 C1 1.375(2) . ? O2 C51 1.381(2) . ? O3 C6 1.342(3) . ? O4 C70 1.411(2) . ? O5 C20 1.361(2) . ? O6 C20 1.504(2) . ? O6 H6 0.8400 . ? O7 C40 1.412(2) . ? O8 C26 1.359(2) . ? O9 C31 1.361(2) . ? O10 C40 1.420(3) . ? O10 H10 0.8400 . ? O11 C56 1.327(2) . ? O12 C65 1.346(2) . ? N1 C15 1.324(3) . ? N1 C19 1.337(2) . ? N2 C45 1.340(3) . ? N2 C41 1.365(3) . ? N3 C46 1.334(3) . ? N3 C50 1.370(2) . ? C1 C2 1.394(3) . ? C1 C6 1.438(3) . ? C2 C3 1.409(3) . ? C2 H2 0.9500 . ? C3 C4 1.396(3) . ? C3 C7 1.535(3) . ? C4 C5 1.391(3) . ? C4 H4 0.9500 . ? C5 C6 1.422(3) . ? C5 C11 1.533(3) . ? C7 C10 1.530(3) . ? C7 C8 1.536(3) . ? C7 C9 1.547(3) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C14 1.510(3) . ? C11 C13 1.523(3) . ? C11 C12 1.541(3) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.398(3) . ? C15 C20 1.527(3) . ? C16 C17 1.382(3) . ? C16 H16 0.9500 . ? C17 C18 1.372(3) . ? C17 H17 0.9500 . ? C18 C19 1.370(3) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C21 1.500(3) . ? C21 N4 1.360(3) . ? C21 C22 1.403(3) . ? C22 C23 1.398(3) . ? C22 H22 0.9500 . ? C23 C24 1.381(3) . ? C23 H23 0.9500 . ? C24 C25 1.366(3) . ? C24 H24 0.9500 . ? C25 N4 1.365(3) . ? C25 H25 0.9500 . ? C26 C31 1.421(3) . ? C26 C27 1.424(3) . ? C27 C28 1.389(3) . ? C27 C32 1.519(3) . ? C28 C29 1.400(3) . ? C28 H28 0.9500 . ? C29 C30 1.424(3) . ? C29 C36 1.548(3) . ? C30 C31 1.395(3) . ? C30 H30 0.9500 . ? C32 C34 1.528(3) . ? C32 C33 1.528(3) . ? C32 C35 1.533(3) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C37 1.525(3) . ? C36 C39 1.536(3) . ? C36 C38 1.538(3) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C46 1.513(3) . ? C40 C41 1.513(3) . ? C41 C42 1.405(3) . ? C42 C43 1.370(3) . ? C42 H42 0.9500 . ? C43 C44 1.380(3) . ? C43 H43 0.9500 . ? C44 C45 1.384(3) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C47 1.405(3) . ? C47 C48 1.391(3) . ? C47 H47 0.9500 . ? C48 C49 1.389(3) . ? C48 H48 0.9500 . ? C49 C50 1.372(3) . ? C49 H49 0.9500 . ? C50 H50 0.9500 . ? C51 C56 1.420(3) . ? C51 C52 1.430(3) . ? C52 C53 1.392(3) . ? C52 H52 0.9500 . ? C53 C54 1.407(3) . ? C53 C57 1.530(3) . ? C54 C55 1.412(3) . ? C54 H54 0.9500 . ? C55 C56 1.400(3) . ? C55 C61 1.524(3) . ? C57 C58 1.495(3) . ? C57 C59 1.518(3) . ? C57 C60 1.522(3) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 C63 1.532(3) . ? C61 C62 1.532(3) . ? C61 C64 1.543(3) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 C70 1.406(3) . ? C65 C66 1.410(3) . ? C66 C67 1.380(3) . ? C66 C71 1.535(3) . ? C67 C68 1.408(3) . ? C67 H67 0.9500 . ? C68 C69 1.408(3) . ? C68 C75 1.530(3) . ? C69 C70 1.368(3) . ? C69 H69 0.9500 . ? C71 C72 1.521(3) . ? C71 C74 1.523(3) . ? C71 C73 1.525(3) . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 C77 1.468(4) . ? C75 C76 1.474(3) . ? C75 C78 1.532(4) . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? N5 C81 1.463(3) . ? N5 C83 1.486(3) . ? N5 C79 1.501(3) . ? N5 H5 0.9300 . ? C79 C80 1.499(4) . ? C79 H79A 0.9900 . ? C79 H79B 0.9900 . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C81 C82 1.526(3) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? C83 C84 1.541(4) . ? C83 H83A 0.9900 . ? C83 H83B 0.9900 . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 0.9800 . ? N6 C85 1.156(3) . ? C85 C86 1.538(4) . ? C86 H86A 0.9800 . ? C86 H86B 0.9800 . ? C86 H86C 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 O5 Fe1 O3 104.34(6) . . ? O5 Fe1 O4 95.15(6) . . ? O3 Fe1 O4 101.25(6) . . ? O5 Fe1 O1 167.62(6) . . ? O3 Fe1 O1 80.64(6) . . ? O4 Fe1 O1 94.96(6) . . ? O5 Fe1 O2 102.58(6) . . ? O3 Fe1 O2 152.65(6) . . ? O4 Fe1 O2 80.99(6) . . ? O1 Fe1 O2 72.02(5) . . ? O5 Fe1 N1 78.29(6) . . ? O3 Fe1 N1 90.82(6) . . ? O4 Fe1 N1 167.44(6) . . ? O1 Fe1 N1 90.42(6) . . ? O2 Fe1 N1 89.93(6) . . ? O8 Fe2 O9 84.51(6) . . ? O8 Fe2 O1 100.41(6) . . ? O9 Fe2 O1 100.42(6) . . ? O8 Fe2 O2 108.95(6) . . ? O9 Fe2 O2 166.14(6) . . ? O1 Fe2 O2 74.46(5) . . ? O8 Fe2 O7 162.25(5) . . ? O9 Fe2 O7 87.41(5) . . ? O1 Fe2 O7 96.57(5) . . ? O2 Fe2 O7 80.52(5) . . ? O8 Fe2 N2 89.93(6) . . ? O9 Fe2 N2 92.98(6) . . ? O1 Fe2 N2 163.74(6) . . ? O2 Fe2 N2 90.38(6) . . ? O7 Fe2 N2 74.71(5) . . ? O11 Fe3 O12 104.45(6) . . ? O11 Fe3 O7 120.76(6) . . ? O12 Fe3 O7 130.55(6) . . ? O11 Fe3 O4 110.75(6) . . ? O12 Fe3 O4 81.07(6) . . ? O7 Fe3 O4 99.15(5) . . ? O11 Fe3 N3 96.16(6) . . ? O12 Fe3 N3 79.04(6) . . ? O7 Fe3 N3 77.37(6) . . ? O4 Fe3 N3 149.79(6) . . ? C1 O1 Fe2 138.29(13) . . ? C1 O1 Fe1 110.55(12) . . ? Fe2 O1 Fe1 108.96(6) . . ? C51 O2 Fe2 126.18(12) . . ? C51 O2 Fe1 124.75(12) . . ? Fe2 O2 Fe1 104.50(6) . . ? C6 O3 Fe1 115.40(12) . . ? C70 O4 Fe1 126.16(11) . . ? C70 O4 Fe3 111.85(11) . . ? Fe1 O4 Fe3 116.34(6) . . ? C20 O5 Fe1 122.95(12) . . ? C20 O6 H6 109.5 . . ? C40 O7 Fe3 116.55(11) . . ? C40 O7 Fe2 110.64(10) . . ? Fe3 O7 Fe2 112.48(6) . . ? C26 O8 Fe2 112.20(12) . . ? C31 O9 Fe2 111.37(12) . . ? C40 O10 H10 109.5 . . ? C56 O11 Fe3 127.77(13) . . ? C65 O12 Fe3 116.54(13) . . ? C15 N1 C19 118.24(18) . . ? C15 N1 Fe1 110.95(13) . . ? C19 N1 Fe1 130.06(14) . . ? C45 N2 C41 117.27(18) . . ? C45 N2 Fe2 127.42(14) . . ? C41 N2 Fe2 115.20(13) . . ? C46 N3 C50 118.35(18) . . ? C46 N3 Fe3 112.84(13) . . ? C50 N3 Fe3 127.27(14) . . ? O1 C1 C2 123.28(19) . . ? O1 C1 C6 114.60(18) . . ? C2 C1 C6 121.94(18) . . ? C1 C2 C3 119.77(19) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C4 C3 C2 117.76(18) . . ? C4 C3 C7 122.82(18) . . ? C2 C3 C7 119.41(18) . . ? C5 C4 C3 124.37(18) . . ? C5 C4 H4 117.8 . . ? C3 C4 H4 117.8 . . ? C4 C5 C6 118.32(18) . . ? C4 C5 C11 122.77(18) . . ? C6 C5 C11 118.90(18) . . ? O3 C6 C5 127.43(19) . . ? O3 C6 C1 114.85(17) . . ? C5 C6 C1 117.71(19) . . ? C10 C7 C3 109.72(18) . . ? C10 C7 C8 108.76(19) . . ? C3 C7 C8 113.45(19) . . ? C10 C7 C9 108.6(2) . . ? C3 C7 C9 108.38(18) . . ? C8 C7 C9 107.9(2) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C14 C11 C13 109.7(2) . . ? C14 C11 C5 110.67(18) . . ? C13 C11 C5 109.83(18) . . ? C14 C11 C12 108.37(19) . . ? C13 C11 C12 106.72(19) . . ? C5 C11 C12 111.42(18) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N1 C15 C16 121.9(2) . . ? N1 C15 C20 116.48(18) . . ? C16 C15 C20 121.60(19) . . ? C17 C16 C15 117.9(2) . . ? C17 C16 H16 121.0 . . ? C15 C16 H16 121.0 . . ? C18 C17 C16 120.6(2) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C19 C18 C17 116.94(19) . . ? C19 C18 H18 121.5 . . ? C17 C18 H18 121.5 . . ? N1 C19 C18 124.30(19) . . ? N1 C19 H19 117.8 . . ? C18 C19 H19 117.8 . . ? O5 C20 C21 111.96(17) . . ? O5 C20 O6 109.24(15) . . ? C21 C20 O6 108.27(15) . . ? O5 C20 C15 110.46(16) . . ? C21 C20 C15 110.45(17) . . ? O6 C20 C15 106.26(15) . . ? N4 C21 C22 124.61(19) . . ? N4 C21 C20 117.99(17) . . ? C22 C21 C20 117.40(18) . . ? C23 C22 C21 118.41(19) . . ? C23 C22 H22 120.8 . . ? C21 C22 H22 120.8 . . ? C24 C23 C22 117.97(18) . . ? C24 C23 H23 121.0 . . ? C22 C23 H23 121.0 . . ? C25 C24 C23 119.2(2) . . ? C25 C24 H24 120.4 . . ? C23 C24 H24 120.4 . . ? N4 C25 C24 126.1(2) . . ? N4 C25 H25 116.9 . . ? C24 C25 H25 116.9 . . ? C21 N4 C25 113.47(17) . . ? O8 C26 C31 116.01(18) . . ? O8 C26 C27 124.55(18) . . ? C31 C26 C27 119.39(18) . . ? C28 C27 C26 116.2(2) . . ? C28 C27 C32 121.3(2) . . ? C26 C27 C32 122.49(19) . . ? C27 C28 C29 126.0(2) . . ? C27 C28 H28 117.0 . . ? C29 C28 H28 117.0 . . ? C28 C29 C30 117.2(2) . . ? C28 C29 C36 124.9(2) . . ? C30 C29 C36 117.8(2) . . ? C31 C30 C29 118.7(2) . . ? C31 C30 H30 120.6 . . ? C29 C30 H30 120.6 . . ? O9 C31 C30 121.71(19) . . ? O9 C31 C26 115.77(17) . . ? C30 C31 C26 122.48(18) . . ? C27 C32 C34 113.9(2) . . ? C27 C32 C33 108.98(19) . . ? C34 C32 C33 106.5(2) . . ? C27 C32 C35 109.66(18) . . ? C34 C32 C35 108.01(19) . . ? C33 C32 C35 109.6(2) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C32 C35 H35A 109.5 . . ? C32 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C32 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C37 C36 C39 109.8(2) . . ? C37 C36 C38 109.35(19) . . ? C39 C36 C38 107.4(2) . . ? C37 C36 C29 110.89(19) . . ? C39 C36 C29 108.92(18) . . ? C38 C36 C29 110.4(2) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? O7 C40 O10 110.07(15) . . ? O7 C40 C46 109.60(16) . . ? O10 C40 C46 107.07(16) . . ? O7 C40 C41 109.11(16) . . ? O10 C40 C41 110.83(16) . . ? C46 C40 C41 110.15(16) . . ? N2 C41 C42 121.51(19) . . ? N2 C41 C40 114.03(17) . . ? C42 C41 C40 124.4(2) . . ? C43 C42 C41 119.8(2) . . ? C43 C42 H42 120.1 . . ? C41 C42 H42 120.1 . . ? C42 C43 C44 118.5(2) . . ? C42 C43 H43 120.7 . . ? C44 C43 H43 120.7 . . ? C43 C44 C45 119.3(2) . . ? C43 C44 H44 120.4 . . ? C45 C44 H44 120.4 . . ? N2 C45 C44 123.4(2) . . ? N2 C45 H45 118.3 . . ? C44 C45 H45 118.3 . . ? N3 C46 C47 122.47(19) . . ? N3 C46 C40 114.44(18) . . ? C47 C46 C40 123.08(19) . . ? C48 C47 C46 118.3(2) . . ? C48 C47 H47 120.9 . . ? C46 C47 H47 120.9 . . ? C49 C48 C47 119.3(2) . . ? C49 C48 H48 120.3 . . ? C47 C48 H48 120.3 . . ? C50 C49 C48 119.09(19) . . ? C50 C49 H49 120.5 . . ? C48 C49 H49 120.5 . . ? N3 C50 C49 122.4(2) . . ? N3 C50 H50 118.8 . . ? C49 C50 H50 118.8 . . ? O2 C51 C56 118.47(19) . . ? O2 C51 C52 121.10(18) . . ? C56 C51 C52 120.40(19) . . ? C53 C52 C51 120.10(19) . . ? C53 C52 H52 120.0 . . ? C51 C52 H52 120.0 . . ? C52 C53 C54 117.76(19) . . ? C52 C53 C57 118.59(19) . . ? C54 C53 C57 123.45(18) . . ? C53 C54 C55 124.17(19) . . ? C53 C54 H54 117.9 . . ? C55 C54 H54 117.9 . . ? C56 C55 C54 117.36(19) . . ? C56 C55 C61 120.58(19) . . ? C54 C55 C61 121.99(18) . . ? O11 C56 C55 121.42(19) . . ? O11 C56 C51 118.33(18) . . ? C55 C56 C51 120.2(2) . . ? C58 C57 C59 110.6(2) . . ? C58 C57 C60 107.1(2) . . ? C59 C57 C60 104.9(2) . . ? C58 C57 C53 111.69(18) . . ? C59 C57 C53 110.40(19) . . ? C60 C57 C53 111.9(2) . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C57 C59 H59A 109.5 . . ? C57 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C57 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C57 C60 H60A 109.5 . . ? C57 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C57 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C55 C61 C63 111.87(19) . . ? C55 C61 C62 109.84(19) . . ? C63 C61 C62 107.8(2) . . ? C55 C61 C64 109.58(17) . . ? C63 C61 C64 107.4(2) . . ? C62 C61 C64 110.3(2) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C61 C64 H64A 109.5 . . ? C61 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C61 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? O12 C65 C70 116.17(18) . . ? O12 C65 C66 124.3(2) . . ? C70 C65 C66 119.44(19) . . ? C67 C66 C65 116.0(2) . . ? C67 C66 C71 122.59(19) . . ? C65 C66 C71 121.36(19) . . ? C66 C67 C68 124.8(2) . . ? C66 C67 H67 117.6 . . ? C68 C67 H67 117.6 . . ? C69 C68 C67 118.21(18) . . ? C69 C68 C75 121.62(19) . . ? C67 C68 C75 120.09(19) . . ? C70 C69 C68 117.55(19) . . ? C70 C69 H69 121.2 . . ? C68 C69 H69 121.2 . . ? C69 C70 C65 123.85(18) . . ? C69 C70 O4 122.84(17) . . ? C65 C70 O4 113.22(16) . . ? C72 C71 C74 107.7(2) . . ? C72 C71 C73 108.33(19) . . ? C74 C71 C73 109.3(2) . . ? C72 C71 C66 111.72(19) . . ? C74 C71 C66 109.61(18) . . ? C73 C71 C66 110.13(19) . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C71 C73 H73A 109.5 . . ? C71 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C71 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C71 C74 H74A 109.5 . . ? C71 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C71 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C77 C75 C76 115.8(2) . . ? C77 C75 C68 112.92(19) . . ? C76 C75 C68 115.42(19) . . ? C77 C75 C78 101.2(2) . . ? C76 C75 C78 102.1(2) . . ? C68 C75 C78 107.3(2) . . ? C75 C76 H76A 109.5 . . ? C75 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C75 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C75 C77 H77A 109.5 . . ? C75 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C75 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C75 C78 H78A 109.5 . . ? C75 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C75 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C81 N5 C83 117.7(2) . . ? C81 N5 C79 113.6(2) . . ? C83 N5 C79 107.5(2) . . ? C81 N5 H5 105.7 . . ? C83 N5 H5 105.7 . . ? C79 N5 H5 105.7 . . ? C80 C79 N5 114.1(2) . . ? C80 C79 H79A 108.7 . . ? N5 C79 H79A 108.7 . . ? C80 C79 H79B 108.7 . . ? N5 C79 H79B 108.7 . . ? H79A C79 H79B 107.6 . . ? C79 C80 H80A 109.5 . . ? C79 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C79 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? N5 C81 C82 113.5(2) . . ? N5 C81 H81A 108.9 . . ? C82 C81 H81A 108.9 . . ? N5 C81 H81B 108.9 . . ? C82 C81 H81B 108.9 . . ? H81A C81 H81B 107.7 . . ? C81 C82 H82A 109.5 . . ? C81 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C81 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? N5 C83 C84 112.1(2) . . ? N5 C83 H83A 109.2 . . ? C84 C83 H83A 109.2 . . ? N5 C83 H83B 109.2 . . ? C84 C83 H83B 109.2 . . ? H83A C83 H83B 107.9 . . ? C83 C84 H84A 109.5 . . ? C83 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C83 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? N6 C85 C86 174.8(3) . . ? C85 C86 H86A 109.5 . . ? C85 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? C85 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O6 H6 N5 0.84 2.39 2.956(2) 124.9 . O10 H10 O9 0.84 1.86 2.647(2) 155.4 . N5 H5 N4 0.93 2.13 2.972(3) 150.2 . N5 H5 O6 0.93 2.22 2.956(2) 135.5 . _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 26.36 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 0.685 _refine_diff_density_min -0.513 _refine_diff_density_rms 0.077 #===END