data_jb34 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C110 H116 Fe3 N12 O8' _chemical_formula_weight 1901.70 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 C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 28.9533(7) _cell_length_b 13.0045(3) _cell_length_c 26.7340(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.526(2) _cell_angle_gamma 90.00 _cell_volume 10065.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9155 _cell_measurement_theta_min 2.84 _cell_measurement_theta_max 29.29 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.255 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4008 _exptl_absorpt_coefficient_mu 0.489 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'ABSPACK(CrysAlis, Oxford Diffraction)' _exptl_special_details ; The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cobra. The data collection nominally covered over a hemisphere of Reciprocal space, by a combination of four sets of exposures with different \f angles for the crystal; each 60 s exposure covered 1.0\% in \w. The crystal-to-detector distance was 5.5 cm. Crystal decay was found to be negligible by by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms; H-atoms were given isotropic displacement parameter equal to 1.2 (or 1.5 for methyl H-atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. The asymmetric unit contains a trimer unit with an infinite zig-zag repeat through the cell.There are three bis phenoxyimine copper complexes connected by pyrazine.The middle complex has a trans orientation of the phenoxyimines and of the pyrazines. The terminal complexes have an L shaped arrangement of the phenoxy imine ligands and of the connecting pyrazines. Also two diethyl ethers were located. There are 4 times all this in the unit cell. The crystals were weakly diffracting and restraints were used to give the two diethyl ethers chemically reasonable bond lengths and angles and thermal parameters. Restraints were also used on the large thermal parameters of the outer carbons of phenylimine ligands. The cif checker has an A alert to highlight the large voids in the structure. Squeeze (Run via Platon) calculates that there are 748.4 Angstroms cubed of solvent accessible void. There were no major peaks left in the difference map. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 10.2833 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 24234 _diffrn_reflns_av_R_equivalents 0.0369 _diffrn_reflns_av_sigmaI/netI 0.0956 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 29.35 _reflns_number_total 16354 _reflns_number_gt 11575 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0887P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881, 4291 Friedel pairs' _refine_ls_abs_structure_Flack 0.018(16) _chemical_absolute_configuration rmad _refine_ls_number_reflns 16354 _refine_ls_number_parameters 1208 _refine_ls_number_restraints 1192 _refine_ls_R_factor_all 0.0790 _refine_ls_R_factor_gt 0.0582 _refine_ls_wR_factor_ref 0.1542 _refine_ls_wR_factor_gt 0.1476 _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_restrained_S_all 1.010 _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 N1 N 0.30418(14) 0.4663(3) 0.18962(17) 0.0180(7) Uani 1 1 d U . . C1 C 0.27354(17) 0.4060(4) 0.2130(2) 0.0181(7) Uani 1 1 d U . . H1A H 0.2630 0.3459 0.1963 0.022 Uiso 1 1 calc R . . C2 C 0.25660(17) 0.4266(4) 0.2598(2) 0.0173(7) Uani 1 1 d U . . H2A H 0.2353 0.3801 0.2744 0.021 Uiso 1 1 calc R . . N2 N 0.26943(14) 0.5112(3) 0.28553(17) 0.0170(6) Uani 1 1 d U . . C3 C 0.30023(17) 0.5712(4) 0.2625(2) 0.0185(7) Uani 1 1 d U . . H3A H 0.3104 0.6321 0.2788 0.022 Uiso 1 1 calc R . . C4 C 0.31790(17) 0.5483(4) 0.2159(2) 0.0183(7) Uani 1 1 d U . . H4A H 0.3406 0.5924 0.2021 0.022 Uiso 1 1 calc R . . Fe1 Fe 0.24478(2) 0.55093(5) 0.36360(3) 0.01365(17) Uani 1 1 d U . . O1 O 0.26593(11) 0.6962(3) 0.35614(14) 0.0173(6) Uani 1 1 d U . . C5 C 0.30326(17) 0.7451(5) 0.3690(2) 0.0202(6) Uani 1 1 d U . . C6 C 0.30479(19) 0.8532(5) 0.3631(2) 0.0242(7) Uani 1 1 d U . . H6A H 0.2785 0.8884 0.3502 0.029 Uiso 1 1 calc R . . C7 C 0.34449(18) 0.9091(5) 0.3759(2) 0.0274(8) Uani 1 1 d U . . H7A H 0.3446 0.9816 0.3718 0.033 Uiso 1 1 calc R . . C8 C 0.3839(2) 0.8601(5) 0.3947(2) 0.0272(8) Uani 1 1 d U . . H8A H 0.4109 0.8980 0.4032 0.033 Uiso 1 1 calc R . . C9 C 0.38237(18) 0.7572(5) 0.4002(2) 0.0252(7) Uani 1 1 d U . . H9A H 0.4092 0.7233 0.4126 0.030 Uiso 1 1 calc R . . C10 C 0.34346(18) 0.6971(5) 0.3887(2) 0.0219(6) Uani 1 1 d U . . C11 C 0.34612(18) 0.5862(4) 0.3979(2) 0.0213(7) Uani 1 1 d U . . H11A H 0.3747 0.5604 0.4103 0.026 Uiso 1 1 calc R . . N3 N 0.31349(14) 0.5205(4) 0.39093(17) 0.0197(6) Uani 1 1 d U . . C12 C 0.32286(18) 0.4101(4) 0.4036(2) 0.0224(7) Uani 1 1 d U . . H12A H 0.2942 0.3821 0.4192 0.027 Uiso 1 1 calc R . . C13 C 0.36306(18) 0.3896(5) 0.4408(2) 0.0299(11) Uani 1 1 d U . . H13A H 0.3617 0.3180 0.4522 0.045 Uiso 1 1 calc R . . H13B H 0.3604 0.4358 0.4695 0.045 Uiso 1 1 calc R . . H13C H 0.3925 0.4018 0.4241 0.045 Uiso 1 1 calc R . . C14 C 0.33038(18) 0.3503(5) 0.3553(2) 0.0220(7) Uani 1 1 d U . . C15 C 0.30708(18) 0.2582(5) 0.3466(2) 0.0237(7) Uani 1 1 d U . . H15A H 0.2856 0.2338 0.3705 0.028 Uiso 1 1 calc R . . C16 C 0.31469(19) 0.2016(5) 0.3036(2) 0.0264(8) Uani 1 1 d U . . H16A H 0.2990 0.1382 0.2986 0.032 Uiso 1 1 calc R . . C17 C 0.34541(18) 0.2373(5) 0.2674(2) 0.0267(8) Uani 1 1 d U . . H17A H 0.3497 0.2000 0.2373 0.032 Uiso 1 1 calc R . . C18 C 0.36944(18) 0.3277(4) 0.2762(2) 0.0250(8) Uani 1 1 d U . . H18A H 0.3909 0.3516 0.2521 0.030 Uiso 1 1 calc R . . C19 C 0.36254(18) 0.3842(5) 0.3201(2) 0.0231(8) Uani 1 1 d U . . H19A H 0.3796 0.4454 0.3260 0.028 Uiso 1 1 calc R . . O2 O 0.21696(11) 0.4115(3) 0.36157(14) 0.0168(6) Uani 1 1 d U . . C20 C 0.19496(17) 0.3544(4) 0.3934(2) 0.0174(6) Uani 1 1 d U . . C21 C 0.17728(17) 0.2582(4) 0.3782(2) 0.0197(7) Uani 1 1 d U . . H21A H 0.1812 0.2365 0.3446 0.024 Uiso 1 1 calc R . . C22 C 0.15434(18) 0.1945(4) 0.4113(2) 0.0219(8) Uani 1 1 d U . . H22A H 0.1424 0.1306 0.3999 0.026 Uiso 1 1 calc R . . C23 C 0.14856(18) 0.2225(4) 0.4607(2) 0.0232(8) Uani 1 1 d U . . H23A H 0.1336 0.1772 0.4832 0.028 Uiso 1 1 calc R . . C24 C 0.16476(18) 0.3176(4) 0.4772(2) 0.0226(7) Uani 1 1 d U . . H24A H 0.1607 0.3372 0.5111 0.027 Uiso 1 1 calc R . . C25 C 0.18720(17) 0.3850(4) 0.4439(2) 0.0186(6) Uani 1 1 d U . . C26 C 0.20080(16) 0.4842(4) 0.4644(2) 0.0170(7) Uani 1 1 d U . . H26A H 0.1957 0.4943 0.4991 0.020 Uiso 1 1 calc R . . N4 N 0.21883(13) 0.5586(4) 0.44083(16) 0.0166(6) Uani 1 1 d U . . C27 C 0.22857(18) 0.6558(4) 0.4683(2) 0.0183(6) Uani 1 1 d U . . H27A H 0.2599 0.6790 0.4578 0.022 Uiso 1 1 calc R . . C28 C 0.22979(19) 0.6487(4) 0.5249(2) 0.0240(10) Uani 1 1 d U . . H28A H 0.2501 0.5920 0.5352 0.036 Uiso 1 1 calc R . . H28B H 0.1985 0.6362 0.5373 0.036 Uiso 1 1 calc R . . H28C H 0.2416 0.7134 0.5389 0.036 Uiso 1 1 calc R . . C29 C 0.19480(17) 0.7376(4) 0.4509(2) 0.0195(6) Uani 1 1 d U . . C30 C 0.21013(19) 0.8370(4) 0.4401(2) 0.0219(7) Uani 1 1 d U . . H30A H 0.2420 0.8527 0.4437 0.026 Uiso 1 1 calc R . . C31 C 0.18013(19) 0.9124(5) 0.4244(2) 0.0244(8) Uani 1 1 d U . . H31A H 0.1914 0.9791 0.4167 0.029 Uiso 1 1 calc R . . C32 C 0.13307(19) 0.8911(4) 0.4197(2) 0.0253(8) Uani 1 1 d U . . H32A H 0.1122 0.9427 0.4084 0.030 Uiso 1 1 calc R . . C33 C 0.11713(19) 0.7944(4) 0.4319(2) 0.0236(8) Uani 1 1 d U . . H33A H 0.0850 0.7800 0.4301 0.028 Uiso 1 1 calc R . . C34 C 0.14750(18) 0.7184(4) 0.4466(2) 0.0209(7) Uani 1 1 d U . . H34A H 0.1360 0.6517 0.4540 0.025 Uiso 1 1 calc R . . N5 N 0.17897(14) 0.6098(3) 0.32619(17) 0.0168(6) Uani 1 1 d U . . C35 C 0.15091(16) 0.5466(5) 0.3007(2) 0.0187(7) Uani 1 1 d U . . H35A H 0.1567 0.4747 0.3013 0.022 Uiso 1 1 calc R . . C36 C 0.11365(17) 0.5836(4) 0.2735(2) 0.0194(7) Uani 1 1 d U . . H36A H 0.0952 0.5362 0.2551 0.023 Uiso 1 1 calc R . . N6 N 0.10251(14) 0.6834(4) 0.27186(18) 0.0187(6) Uani 1 1 d U . . C37 C 0.13018(16) 0.7468(5) 0.2983(2) 0.0178(7) Uani 1 1 d U . . H37A H 0.1234 0.8182 0.2990 0.021 Uiso 1 1 calc R . . C38 C 0.16816(17) 0.7104(4) 0.3245(2) 0.0174(7) Uani 1 1 d U . . H38A H 0.1873 0.7580 0.3418 0.021 Uiso 1 1 calc R . . Fe2 Fe 0.03920(3) 0.74277(7) 0.23211(3) 0.01689(17) Uani 1 1 d U . . O3 O 0.02039(13) 0.6025(3) 0.21388(16) 0.0260(6) Uani 1 1 d U . . C39 C 0.0279(2) 0.5410(5) 0.1760(3) 0.0350(7) Uani 1 1 d U . . C40 C 0.0078(2) 0.4440(5) 0.1746(3) 0.0423(9) Uani 1 1 d U . . H40A H -0.0119 0.4241 0.2011 0.051 Uiso 1 1 calc R . . C41 C 0.0153(3) 0.3763(6) 0.1367(3) 0.0516(10) Uani 1 1 d U . . H41A H 0.0002 0.3115 0.1364 0.062 Uiso 1 1 calc R . . C42 C 0.0455(3) 0.4031(6) 0.0980(3) 0.0565(10) Uani 1 1 d U . . H42A H 0.0517 0.3546 0.0723 0.068 Uiso 1 1 calc R . . C43 C 0.0662(3) 0.4972(6) 0.0965(3) 0.0520(9) Uani 1 1 d U . . H43A H 0.0860 0.5144 0.0697 0.062 Uiso 1 1 calc R . . C44 C 0.0579(2) 0.5709(6) 0.1358(3) 0.0421(8) Uani 1 1 d U . . C45 C 0.0791(2) 0.6693(5) 0.1303(3) 0.0379(8) Uani 1 1 d U . . H45A H 0.0974 0.6780 0.1013 0.045 Uiso 1 1 calc R . . N7 N 0.07675(16) 0.7476(4) 0.15949(19) 0.0322(6) Uani 1 1 d U . . C46 C 0.1027(2) 0.8411(5) 0.1424(3) 0.0357(7) Uani 1 1 d U . . H46A H 0.1190 0.8211 0.1110 0.043 Uiso 1 1 calc R . . C47 C 0.1398(2) 0.8725(6) 0.1798(3) 0.0468(13) Uani 1 1 d U . . H47A H 0.1607 0.8145 0.1858 0.070 Uiso 1 1 calc R . . H47B H 0.1253 0.8926 0.2113 0.070 Uiso 1 1 calc R . . H47C H 0.1573 0.9307 0.1665 0.070 Uiso 1 1 calc R . . C48 C 0.06927(19) 0.9285(5) 0.1282(2) 0.0317(7) Uani 1 1 d U . . C49 C 0.03608(18) 0.9122(5) 0.0916(2) 0.0299(8) Uani 1 1 d U . . H49A H 0.0331 0.8461 0.0768 0.036 Uiso 1 1 calc R . . C50 C 0.0068(2) 0.9919(5) 0.0760(2) 0.0292(8) Uani 1 1 d U . . H50A H -0.0159 0.9800 0.0509 0.035 Uiso 1 1 calc R . . C51 C 0.0114(2) 1.0881(5) 0.0976(2) 0.0306(9) Uani 1 1 d U . . H51A H -0.0087 1.1427 0.0881 0.037 Uiso 1 1 calc R . . C52 C 0.0456(2) 1.1034(5) 0.1332(3) 0.0335(9) Uani 1 1 d U . . H52A H 0.0496 1.1700 0.1472 0.040 Uiso 1 1 calc R . . C53 C 0.0740(2) 1.0253(5) 0.1489(3) 0.0337(8) Uani 1 1 d U . . H53A H 0.0969 1.0376 0.1739 0.040 Uiso 1 1 calc R . . O4 O 0.05629(13) 0.8838(3) 0.25267(16) 0.0263(6) Uani 1 1 d U . . C54 C 0.0456(2) 0.9416(5) 0.2901(3) 0.0315(7) Uani 1 1 d U . . C55 C 0.0683(2) 1.0385(5) 0.2957(3) 0.0385(8) Uani 1 1 d U . . H55A H 0.0916 1.0585 0.2729 0.046 Uiso 1 1 calc R . . C56 C 0.0560(3) 1.1048(6) 0.3355(3) 0.0457(9) Uani 1 1 d U . . H56A H 0.0716 1.1687 0.3391 0.055 Uiso 1 1 calc R . . C57 C 0.0253(3) 1.0821(5) 0.3661(3) 0.0491(10) Uani 1 1 d U . . H57A H 0.0177 1.1295 0.3918 0.059 Uiso 1 1 calc R . . C58 C 0.0013(3) 0.9866(5) 0.3633(3) 0.0451(9) Uani 1 1 d U . . H58A H -0.0226 0.9712 0.3863 0.054 Uiso 1 1 calc R . . C59 C 0.0131(2) 0.9164(5) 0.3265(3) 0.0357(7) Uani 1 1 d U . . C60 C -0.0088(2) 0.8145(5) 0.3299(2) 0.0295(7) Uani 1 1 d U . . H60A H -0.0308 0.8058 0.3556 0.035 Uiso 1 1 calc R . . N8 N -0.00148(15) 0.7366(4) 0.30203(18) 0.0243(6) Uani 1 1 d U . . C61 C -0.02665(19) 0.6402(5) 0.3140(2) 0.0267(7) Uani 1 1 d U . . H61A H -0.0402 0.6143 0.2818 0.032 Uiso 1 1 calc R . . C62 C -0.06602(19) 0.6468(5) 0.3510(3) 0.0340(12) Uani 1 1 d U . . H62A H -0.0890 0.6965 0.3390 0.051 Uiso 1 1 calc R . . H62B H -0.0539 0.6690 0.3837 0.051 Uiso 1 1 calc R . . H62C H -0.0805 0.5791 0.3544 0.051 Uiso 1 1 calc R . . C63 C 0.00679(19) 0.5583(5) 0.3325(2) 0.0269(7) Uani 1 1 d U . . C64 C -0.0013(2) 0.4569(5) 0.3204(3) 0.0326(8) Uani 1 1 d U . . H64A H -0.0257 0.4408 0.2977 0.039 Uiso 1 1 calc R . . C65 C 0.0251(2) 0.3779(5) 0.3402(3) 0.0350(9) Uani 1 1 d U . . H65A H 0.0188 0.3087 0.3309 0.042 Uiso 1 1 calc R . . C66 C 0.0611(2) 0.4000(5) 0.3737(3) 0.0325(9) Uani 1 1 d U . . H66A H 0.0792 0.3465 0.3879 0.039 Uiso 1 1 calc R . . C67 C 0.0695(2) 0.5021(5) 0.3857(2) 0.0297(8) Uani 1 1 d U . . H67A H 0.0940 0.5188 0.4083 0.036 Uiso 1 1 calc R . . C68 C 0.04284(19) 0.5797(5) 0.3653(2) 0.0268(8) Uani 1 1 d U . . H68A H 0.0493 0.6491 0.3739 0.032 Uiso 1 1 calc R . . N9 N -0.02512(14) 0.8027(4) 0.19362(18) 0.0181(6) Uani 1 1 d U . . C69 C -0.03388(17) 0.9034(4) 0.1889(2) 0.0178(7) Uani 1 1 d U . . H69A H -0.0125 0.9520 0.2021 0.021 Uiso 1 1 calc R . . C70 C -0.07357(16) 0.9373(5) 0.1651(2) 0.0175(7) Uani 1 1 d U . . H70A H -0.0790 1.0093 0.1633 0.021 Uiso 1 1 calc R . . N10 N -0.10470(14) 0.8739(3) 0.14454(17) 0.0166(6) Uani 1 1 d U . . C71 C -0.09535(17) 0.7740(4) 0.1488(2) 0.0175(7) Uani 1 1 d U . . H71A H -0.1164 0.7258 0.1348 0.021 Uiso 1 1 calc R . . C72 C -0.05618(16) 0.7379(5) 0.1729(2) 0.0179(7) Uani 1 1 d U . . H72A H -0.0510 0.6658 0.1748 0.021 Uiso 1 1 calc R . . Fe3 Fe -0.17166(2) 0.93339(6) 0.10881(3) 0.01603(18) Uani 1 1 d U . . O5 O -0.14665(12) 1.0736(3) 0.11670(14) 0.0197(6) Uani 1 1 d U . . C73 C -0.12171(18) 1.1373(4) 0.0896(2) 0.0208(6) Uani 1 1 d U . . C74 C -0.11060(18) 1.2340(4) 0.1102(2) 0.0247(7) Uani 1 1 d U . . H74A H -0.1203 1.2508 0.1430 0.030 Uiso 1 1 calc R . . C75 C -0.08571(19) 1.3047(5) 0.0827(2) 0.0288(8) Uani 1 1 d U . . H75A H -0.0789 1.3700 0.0970 0.035 Uiso 1 1 calc R . . C76 C -0.0702(2) 1.2822(5) 0.0340(2) 0.0295(8) Uani 1 1 d U . . H76A H -0.0529 1.3311 0.0155 0.035 Uiso 1 1 calc R . . C77 C -0.08087(19) 1.1871(4) 0.0141(2) 0.0258(8) Uani 1 1 d U . . H77A H -0.0709 1.1708 -0.0188 0.031 Uiso 1 1 calc R . . C78 C -0.10623(18) 1.1132(4) 0.0413(2) 0.0217(7) Uani 1 1 d U . . C79 C -0.11397(17) 1.0148(4) 0.0173(2) 0.0203(7) Uani 1 1 d U . . H79A H -0.1008 1.0062 -0.0148 0.024 Uiso 1 1 calc R . . N11 N -0.13658(14) 0.9379(4) 0.03451(17) 0.0200(6) Uani 1 1 d U . . C80 C -0.13824(18) 0.8490(4) -0.0012(2) 0.0234(7) Uani 1 1 d U . . H80A H -0.1208 0.8701 -0.0317 0.028 Uiso 1 1 calc R . . C81 C -0.18871(18) 0.8315(5) -0.0178(2) 0.0273(11) Uani 1 1 d U . . H81A H -0.2009 0.8946 -0.0330 0.041 Uiso 1 1 calc R . . H81B H -0.2073 0.8134 0.0114 0.041 Uiso 1 1 calc R . . H81C H -0.1901 0.7755 -0.0423 0.041 Uiso 1 1 calc R . . C82 C -0.11428(18) 0.7538(5) 0.0199(2) 0.0244(7) Uani 1 1 d U . . C83 C -0.1365(2) 0.6614(5) 0.0289(2) 0.0273(8) Uani 1 1 d U . . H83A H -0.1689 0.6560 0.0230 0.033 Uiso 1 1 calc R . . C84 C -0.1122(2) 0.5768(5) 0.0462(2) 0.0300(8) Uani 1 1 d U . . H84A H -0.1280 0.5141 0.0522 0.036 Uiso 1 1 calc R . . C85 C -0.0651(2) 0.5822(5) 0.0549(2) 0.0292(8) Uani 1 1 d U . . H85A H -0.0486 0.5239 0.0669 0.035 Uiso 1 1 calc R . . C86 C -0.0423(2) 0.6745(5) 0.0459(2) 0.0273(8) Uani 1 1 d U . . H86A H -0.0100 0.6796 0.0519 0.033 Uiso 1 1 calc R . . C87 C -0.06702(19) 0.7599(5) 0.0280(2) 0.0252(8) Uani 1 1 d U . . H87A H -0.0512 0.8224 0.0213 0.030 Uiso 1 1 calc R . . O6 O -0.19163(11) 0.7874(3) 0.11448(15) 0.0204(6) Uani 1 1 d U . . N12 N -0.24451(15) 0.9619(4) 0.08418(18) 0.0237(6) Uani 1 1 d U . . C88 C -0.22976(17) 0.7359(5) 0.1077(2) 0.0220(6) Uani 1 1 d U . . C89 C -0.23035(19) 0.6285(5) 0.1167(2) 0.0245(7) Uani 1 1 d U . . H89A H -0.2026 0.5956 0.1273 0.029 Uiso 1 1 calc R . . C90 C -0.26960(18) 0.5704(5) 0.1106(2) 0.0271(8) Uani 1 1 d U . . H90A H -0.2689 0.4988 0.1177 0.033 Uiso 1 1 calc R . . C91 C -0.3111(2) 0.6173(5) 0.0939(2) 0.0285(8) Uani 1 1 d U . . H91A H -0.3384 0.5777 0.0890 0.034 Uiso 1 1 calc R . . C92 C -0.31115(18) 0.7212(5) 0.0848(2) 0.0269(8) Uani 1 1 d U . . H92A H -0.3389 0.7527 0.0735 0.032 Uiso 1 1 calc R . . C93 C -0.27176(18) 0.7828(5) 0.0917(2) 0.0241(6) Uani 1 1 d U . . C94 C -0.27559(18) 0.8906(5) 0.0811(2) 0.0240(7) Uani 1 1 d U . . H94A H -0.3053 0.9130 0.0703 0.029 Uiso 1 1 calc R . . C95 C -0.25965(18) 1.0676(5) 0.0705(2) 0.0267(7) Uani 1 1 d U . . H95A H -0.2929 1.0629 0.0603 0.032 Uiso 1 1 calc R . . C96 C -0.23355(19) 1.1019(5) 0.0253(2) 0.0311(11) Uani 1 1 d U . . H96A H -0.2383 1.0523 -0.0019 0.047 Uiso 1 1 calc R . . H96B H -0.2006 1.1063 0.0335 0.047 Uiso 1 1 calc R . . H96C H -0.2448 1.1696 0.0146 0.047 Uiso 1 1 calc R . . C97 C -0.25734(19) 1.1368(5) 0.1159(2) 0.0283(7) Uani 1 1 d U . . C98 C -0.2836(2) 1.1131(5) 0.1578(2) 0.0311(8) Uani 1 1 d U . . H98A H -0.3035 1.0550 0.1573 0.037 Uiso 1 1 calc R . . C99 C -0.2807(2) 1.1737(5) 0.1999(3) 0.0345(9) Uani 1 1 d U . . H99A H -0.2982 1.1556 0.2284 0.041 Uiso 1 1 calc R . . C100 C -0.2533(2) 1.2596(5) 0.2019(3) 0.0357(9) Uani 1 1 d U . . H10A H -0.2515 1.3002 0.2314 0.043 Uiso 1 1 calc R . . C101 C -0.2283(2) 1.2857(5) 0.1599(3) 0.0341(8) Uani 1 1 d U . . H10B H -0.2100 1.3463 0.1601 0.041 Uiso 1 1 calc R . . C102 C -0.22966(19) 1.2250(5) 0.1177(3) 0.0307(8) Uani 1 1 d U . . H10C H -0.2116 1.2431 0.0895 0.037 Uiso 1 1 calc R . . C201 C 0.1071(3) 1.2984(6) 0.2334(3) 0.0581(16) Uani 1 1 d U . . H20A H 0.1012 1.3568 0.2111 0.087 Uiso 1 1 calc R . . H20B H 0.1106 1.3231 0.2679 0.087 Uiso 1 1 calc R . . H20C H 0.0810 1.2503 0.2315 0.087 Uiso 1 1 calc R . . C202 C 0.1510(2) 1.2440(6) 0.2177(3) 0.0491(11) Uani 1 1 d U . . H20D H 0.1463 1.2111 0.1846 0.059 Uiso 1 1 calc R . . H20E H 0.1765 1.2942 0.2150 0.059 Uiso 1 1 calc R . . O203 O 0.16220(16) 1.1680(4) 0.25425(19) 0.0452(9) Uani 1 1 d U . . C204 C 0.1999(3) 1.1101(6) 0.2456(3) 0.0484(11) Uani 1 1 d U . . H20F H 0.2274 1.1553 0.2443 0.058 Uiso 1 1 calc R . . H20G H 0.1965 1.0764 0.2126 0.058 Uiso 1 1 calc R . . C205 C 0.2076(2) 1.0303(6) 0.2842(3) 0.0490(14) Uani 1 1 d U . . H20H H 0.2350 0.9897 0.2758 0.073 Uiso 1 1 calc R . . H20I H 0.1806 0.9851 0.2857 0.073 Uiso 1 1 calc R . . H20J H 0.2124 1.0633 0.3168 0.073 Uiso 1 1 calc R . . C301 C -0.1305(3) 0.4685(7) 0.2101(3) 0.0618(16) Uani 1 1 d U . . H30B H -0.1600 0.5025 0.2167 0.093 Uiso 1 1 calc R . . H30C H -0.1297 0.4461 0.1751 0.093 Uiso 1 1 calc R . . H30D H -0.1051 0.5168 0.2165 0.093 Uiso 1 1 calc R . . C302 C -0.1253(3) 0.3769(7) 0.2438(3) 0.0572(12) Uani 1 1 d U . . H30E H -0.1237 0.3997 0.2791 0.069 Uiso 1 1 calc R . . H30F H -0.1523 0.3310 0.2397 0.069 Uiso 1 1 calc R . . O303 O -0.08413(17) 0.3226(4) 0.2314(2) 0.0539(10) Uani 1 1 d U . . C304 C -0.0777(3) 0.2336(7) 0.2609(3) 0.0565(12) Uani 1 1 d U . . H30G H -0.1048 0.1875 0.2576 0.068 Uiso 1 1 calc R . . H30H H -0.0738 0.2524 0.2966 0.068 Uiso 1 1 calc R . . C305 C -0.0352(3) 0.1813(6) 0.2420(3) 0.0593(16) Uani 1 1 d U . . H30I H -0.0283 0.1212 0.2629 0.089 Uiso 1 1 calc R . . H30J H -0.0091 0.2293 0.2435 0.089 Uiso 1 1 calc R . . H30K H -0.0403 0.1593 0.2074 0.089 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0181(14) 0.0198(15) 0.0161(15) 0.0004(12) -0.0005(12) 0.0023(13) C1 0.0186(15) 0.0193(15) 0.0164(15) -0.0009(12) -0.0001(13) 0.0014(13) C2 0.0187(15) 0.0183(15) 0.0150(14) 0.0009(12) -0.0004(12) 0.0022(13) N2 0.0180(13) 0.0185(14) 0.0146(11) 0.0004(10) 0.0005(10) 0.0027(12) C3 0.0200(15) 0.0186(15) 0.0171(14) -0.0002(13) 0.0011(12) 0.0019(13) C4 0.0190(15) 0.0190(15) 0.0169(15) 0.0012(14) 0.0011(12) 0.0018(13) Fe1 0.0137(3) 0.0154(4) 0.0119(4) -0.0001(3) -0.0002(3) -0.0001(3) O1 0.0168(12) 0.0193(11) 0.0158(15) -0.0005(11) 0.0030(12) -0.0025(10) C5 0.0204(12) 0.0250(12) 0.0153(14) -0.0028(13) 0.0028(12) -0.0059(10) C6 0.0266(14) 0.0268(14) 0.0193(17) -0.0022(15) 0.0027(14) -0.0084(13) C7 0.0300(15) 0.0304(15) 0.0218(18) -0.0044(16) 0.0049(15) -0.0113(13) C8 0.0267(14) 0.0347(16) 0.0204(18) -0.0053(16) 0.0039(15) -0.0126(14) C9 0.0222(13) 0.0349(15) 0.0186(17) -0.0049(16) 0.0030(14) -0.0080(13) C10 0.0193(12) 0.0302(12) 0.0164(15) -0.0039(13) 0.0028(12) -0.0054(11) C11 0.0177(12) 0.0304(13) 0.0158(16) -0.0015(14) 0.0011(13) -0.0007(12) N3 0.0173(11) 0.0268(12) 0.0151(14) 0.0004(12) -0.0002(10) 0.0025(10) C12 0.0203(14) 0.0278(13) 0.0191(15) 0.0049(13) -0.0013(12) 0.0046(12) C13 0.027(2) 0.037(3) 0.026(2) 0.005(2) -0.0086(18) 0.007(2) C14 0.0203(14) 0.0250(14) 0.0207(14) 0.0052(12) 0.0000(12) 0.0054(13) C15 0.0221(16) 0.0264(16) 0.0226(16) 0.0053(14) 0.0015(14) 0.0029(14) C16 0.0265(16) 0.0275(17) 0.0252(18) 0.0028(14) 0.0024(15) 0.0014(15) C17 0.0270(17) 0.0286(17) 0.0246(17) 0.0023(15) 0.0036(14) 0.0030(15) C18 0.0240(16) 0.0269(17) 0.0241(17) 0.0048(15) 0.0043(14) 0.0040(14) C19 0.0209(15) 0.0256(16) 0.0227(16) 0.0053(14) 0.0013(13) 0.0038(14) O2 0.0176(13) 0.0158(11) 0.0169(14) -0.0017(11) 0.0012(11) 0.0010(10) C20 0.0174(14) 0.0156(12) 0.0193(13) 0.0005(11) -0.0008(12) 0.0018(11) C21 0.0208(16) 0.0172(14) 0.0213(15) 0.0006(13) -0.0017(14) 0.0004(13) C22 0.0237(16) 0.0180(15) 0.0242(17) 0.0032(14) -0.0007(15) 0.0007(14) C23 0.0249(16) 0.0205(15) 0.0240(16) 0.0047(15) 0.0014(15) -0.0007(14) C24 0.0247(16) 0.0212(15) 0.0218(15) 0.0037(13) 0.0025(14) 0.0005(14) C25 0.0191(14) 0.0179(12) 0.0188(13) 0.0022(11) 0.0014(12) 0.0022(12) C26 0.0179(15) 0.0191(13) 0.0140(14) 0.0010(12) 0.0019(13) 0.0024(13) N4 0.0177(13) 0.0190(12) 0.0130(11) -0.0004(10) 0.0005(10) 0.0001(12) C27 0.0206(13) 0.0211(13) 0.0131(13) -0.0028(12) 0.0002(13) -0.0002(12) C28 0.032(2) 0.027(3) 0.0132(17) -0.0029(17) -0.0023(19) -0.001(2) C29 0.0231(13) 0.0205(13) 0.0149(14) -0.0029(13) -0.0001(12) 0.0003(12) C30 0.0262(15) 0.0204(14) 0.0188(17) -0.0031(15) -0.0012(15) -0.0006(13) C31 0.0306(16) 0.0204(15) 0.0222(18) -0.0023(15) -0.0013(15) 0.0014(14) C32 0.0303(15) 0.0219(15) 0.0236(19) -0.0019(15) -0.0033(15) 0.0039(15) C33 0.0262(15) 0.0230(16) 0.0214(18) -0.0032(16) -0.0049(15) 0.0013(13) C34 0.0239(14) 0.0207(15) 0.0181(17) -0.0022(15) -0.0022(14) 0.0002(13) N5 0.0161(11) 0.0184(13) 0.0159(14) -0.0004(13) -0.0005(10) 0.0005(10) C35 0.0165(13) 0.0196(14) 0.0199(17) -0.0015(14) -0.0024(12) 0.0013(12) C36 0.0170(14) 0.0196(14) 0.0218(17) -0.0005(14) -0.0027(12) 0.0015(12) N6 0.0164(12) 0.0191(13) 0.0205(15) 0.0006(13) -0.0023(10) -0.0002(11) C37 0.0160(13) 0.0193(14) 0.0180(16) 0.0009(14) -0.0018(12) -0.0001(12) C38 0.0160(13) 0.0191(14) 0.0170(16) 0.0001(14) -0.0005(12) 0.0003(12) Fe2 0.0144(3) 0.0172(3) 0.0190(4) 0.0008(3) -0.0036(3) 0.0001(3) O3 0.0293(16) 0.0213(12) 0.0273(16) -0.0036(11) -0.0127(12) 0.0033(11) C39 0.0464(16) 0.0283(13) 0.0300(16) -0.0055(12) -0.0151(13) 0.0124(14) C40 0.060(2) 0.0298(16) 0.0367(19) -0.0095(15) -0.0217(16) 0.0115(16) C41 0.075(2) 0.0378(17) 0.042(2) -0.0134(16) -0.0222(18) 0.0146(18) C42 0.081(2) 0.0464(18) 0.041(2) -0.0126(17) -0.0168(18) 0.0212(19) C43 0.073(2) 0.0466(17) 0.0359(18) -0.0069(16) -0.0102(17) 0.0245(18) C44 0.0559(17) 0.0400(14) 0.0301(15) -0.0023(13) -0.0080(14) 0.0217(14) C45 0.0442(17) 0.0427(15) 0.0268(16) 0.0039(14) 0.0023(15) 0.0224(15) N7 0.0316(14) 0.0391(14) 0.0261(13) 0.0105(12) 0.0056(12) 0.0167(13) C46 0.0304(15) 0.0459(15) 0.0308(16) 0.0156(14) 0.0080(12) 0.0107(13) C47 0.030(2) 0.061(3) 0.050(3) 0.025(2) -0.0005(19) 0.003(2) C48 0.0265(14) 0.0400(15) 0.0288(17) 0.0140(14) 0.0053(12) 0.0047(14) C49 0.0266(16) 0.0354(17) 0.0280(18) 0.0108(16) 0.0064(13) 0.0034(15) C50 0.0262(16) 0.0347(18) 0.0266(19) 0.0097(16) 0.0034(14) 0.0022(15) C51 0.0285(16) 0.0344(17) 0.029(2) 0.0097(17) 0.0023(15) 0.0023(16) C52 0.0319(17) 0.0371(17) 0.032(2) 0.0087(17) 0.0001(15) 0.0001(16) C53 0.0289(16) 0.0409(16) 0.0314(19) 0.0124(16) 0.0011(15) 0.0007(15) O4 0.0266(15) 0.0181(12) 0.0339(17) 0.0015(11) -0.0129(12) -0.0015(11) C54 0.0384(16) 0.0204(13) 0.0353(16) -0.0005(11) -0.0151(13) 0.0016(13) C55 0.0510(19) 0.0220(16) 0.0420(19) -0.0021(14) -0.0188(16) 0.0000(15) C56 0.063(2) 0.0274(17) 0.046(2) -0.0067(15) -0.0180(18) 0.0009(17) C57 0.070(2) 0.0322(17) 0.045(2) -0.0087(17) -0.0126(17) 0.0046(18) C58 0.063(2) 0.0325(16) 0.0397(19) -0.0063(15) -0.0075(16) 0.0061(16) C59 0.0461(16) 0.0272(13) 0.0336(16) -0.0018(13) -0.0094(13) 0.0054(13) C60 0.0347(16) 0.0280(14) 0.0257(16) 0.0001(13) -0.0023(14) 0.0076(14) N8 0.0246(13) 0.0257(13) 0.0226(13) 0.0029(11) -0.0003(11) 0.0045(12) C61 0.0259(14) 0.0279(13) 0.0262(16) 0.0056(14) 0.0006(12) 0.0012(12) C62 0.027(2) 0.037(3) 0.037(3) 0.014(2) 0.0044(19) 0.0054(19) C63 0.0272(14) 0.0257(13) 0.0279(16) 0.0041(14) -0.0015(13) 0.0005(13) C64 0.0350(17) 0.0274(15) 0.0351(19) 0.0024(16) -0.0085(15) -0.0015(15) C65 0.0400(18) 0.0262(16) 0.039(2) 0.0009(17) -0.0089(16) 0.0002(16) C66 0.0360(18) 0.0259(16) 0.035(2) 0.0020(17) -0.0073(15) 0.0040(16) C67 0.0309(17) 0.0266(17) 0.031(2) 0.0009(16) -0.0053(15) 0.0026(15) C68 0.0281(16) 0.0245(16) 0.0277(19) 0.0022(15) -0.0017(14) 0.0010(14) N9 0.0153(11) 0.0197(13) 0.0194(14) 0.0008(13) -0.0014(10) -0.0006(11) C69 0.0152(13) 0.0197(13) 0.0184(16) 0.0014(14) -0.0004(12) -0.0005(12) C70 0.0160(13) 0.0196(14) 0.0168(16) 0.0012(15) 0.0004(12) -0.0003(12) N10 0.0148(11) 0.0192(13) 0.0160(14) 0.0001(13) 0.0002(11) 0.0007(11) C71 0.0159(13) 0.0193(14) 0.0171(16) -0.0004(14) -0.0015(12) 0.0005(12) C72 0.0154(13) 0.0192(14) 0.0191(16) 0.0001(15) -0.0016(12) 0.0009(12) Fe3 0.0145(3) 0.0199(4) 0.0136(4) 0.0007(3) -0.0006(3) 0.0001(3) O5 0.0202(14) 0.0199(11) 0.0190(15) 0.0022(11) 0.0025(12) 0.0022(10) C73 0.0225(14) 0.0202(12) 0.0196(14) 0.0038(11) 0.0023(12) 0.0023(11) C74 0.0300(17) 0.0208(14) 0.0233(16) 0.0026(13) 0.0041(14) 0.0000(14) C75 0.0369(18) 0.0226(15) 0.0269(18) 0.0022(14) 0.0072(15) -0.0016(15) C76 0.0386(18) 0.0243(15) 0.0258(18) 0.0037(15) 0.0085(15) -0.0023(15) C77 0.0307(17) 0.0244(15) 0.0223(17) 0.0040(14) 0.0059(14) -0.0001(14) C78 0.0234(14) 0.0227(13) 0.0190(14) 0.0038(12) 0.0022(12) 0.0019(12) C79 0.0203(15) 0.0247(14) 0.0158(15) 0.0039(12) 0.0007(13) 0.0011(13) N11 0.0200(13) 0.0245(13) 0.0156(12) 0.0006(11) 0.0004(11) 0.0001(12) C80 0.0248(14) 0.0273(13) 0.0181(14) -0.0025(12) 0.0019(13) -0.0010(13) C81 0.0272(19) 0.033(3) 0.021(3) -0.001(2) -0.0030(19) -0.0060(19) C82 0.0269(14) 0.0253(13) 0.0212(15) -0.0030(13) 0.0043(13) -0.0019(12) C83 0.0298(16) 0.0263(15) 0.0259(18) -0.0038(15) 0.0054(16) -0.0040(13) C84 0.0349(17) 0.0255(16) 0.0297(19) -0.0031(16) 0.0077(16) -0.0031(15) C85 0.0335(16) 0.0252(16) 0.029(2) -0.0017(16) 0.0095(16) 0.0006(15) C86 0.0291(16) 0.0262(17) 0.0267(19) -0.0017(16) 0.0076(16) 0.0008(13) C87 0.0268(14) 0.0252(16) 0.0235(18) -0.0022(15) 0.0062(15) -0.0008(13) O6 0.0179(12) 0.0240(12) 0.0193(16) -0.0005(13) -0.0012(12) -0.0028(10) N12 0.0183(11) 0.0328(13) 0.0200(16) 0.0002(13) -0.0011(11) 0.0043(10) C88 0.0188(11) 0.0288(12) 0.0184(15) -0.0023(13) 0.0020(12) -0.0036(10) C89 0.0238(14) 0.0300(14) 0.0197(17) -0.0020(15) 0.0031(14) -0.0053(12) C90 0.0267(15) 0.0335(16) 0.0211(18) -0.0029(16) 0.0033(15) -0.0077(13) C91 0.0253(14) 0.0382(16) 0.0219(18) -0.0040(17) 0.0031(15) -0.0080(14) C92 0.0210(13) 0.0385(15) 0.0212(17) -0.0048(16) 0.0016(14) -0.0042(13) C93 0.0182(11) 0.0345(13) 0.0196(15) -0.0040(14) 0.0013(12) -0.0020(11) C94 0.0171(12) 0.0349(13) 0.0198(17) -0.0035(15) -0.0010(14) 0.0021(12) C95 0.0204(14) 0.0350(14) 0.0247(15) 0.0039(13) -0.0001(13) 0.0074(12) C96 0.027(2) 0.040(3) 0.026(2) 0.0080(19) 0.000(2) 0.007(2) C97 0.0232(14) 0.0332(14) 0.0286(15) 0.0026(13) 0.0006(13) 0.0118(13) C98 0.0281(16) 0.0352(18) 0.0300(17) 0.0020(15) 0.0042(15) 0.0137(15) C99 0.0330(18) 0.0378(19) 0.0328(18) 0.0002(16) 0.0050(16) 0.0147(15) C100 0.0337(18) 0.0374(19) 0.0359(19) -0.0020(16) 0.0008(16) 0.0148(16) C101 0.0299(17) 0.0348(18) 0.0377(19) -0.0014(15) -0.0009(16) 0.0123(15) C102 0.0253(16) 0.0332(17) 0.0336(18) 0.0010(15) -0.0005(15) 0.0115(14) C201 0.076(3) 0.049(3) 0.049(4) -0.002(3) -0.018(3) 0.006(3) C202 0.058(2) 0.051(2) 0.038(2) 0.005(2) -0.009(2) -0.010(2) O203 0.0536(19) 0.047(2) 0.035(2) 0.0016(17) -0.0016(17) -0.0032(16) C204 0.052(2) 0.054(2) 0.039(2) -0.002(2) 0.000(2) -0.0022(18) C205 0.051(3) 0.049(3) 0.047(3) -0.003(2) -0.002(3) 0.000(2) C301 0.058(3) 0.062(3) 0.066(4) -0.017(3) 0.003(3) -0.002(3) C302 0.058(2) 0.067(3) 0.047(3) -0.016(2) 0.004(2) -0.005(2) O303 0.060(2) 0.059(2) 0.043(2) -0.0132(19) 0.0011(19) -0.0059(18) C304 0.065(2) 0.060(3) 0.044(3) -0.010(2) -0.005(2) -0.012(2) C305 0.075(3) 0.052(3) 0.050(4) -0.014(3) -0.009(3) -0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C4 1.336(7) . ? N1 C1 1.342(7) . ? N1 Fe3 2.317(5) 3_545 ? C1 C2 1.374(7) . ? C1 H1A 0.9500 . ? C2 N2 1.348(7) . ? C2 H2A 0.9500 . ? N2 C3 1.339(7) . ? N2 Fe1 2.271(5) . ? C3 C4 1.382(7) . ? C3 H3A 0.9500 . ? C4 H4A 0.9500 . ? Fe1 O2 1.985(4) . ? Fe1 O1 1.996(4) . ? Fe1 N3 2.150(4) . ? Fe1 N4 2.206(4) . ? Fe1 N5 2.276(4) . ? O1 C5 1.298(6) . ? C5 C6 1.415(8) . ? C5 C10 1.418(8) . ? C6 C7 1.400(8) . ? C6 H6A 0.9500 . ? C7 C8 1.396(8) . ? C7 H7A 0.9500 . ? C8 C9 1.347(9) . ? C8 H8A 0.9500 . ? C9 C10 1.403(8) . ? C9 H9A 0.9500 . ? C10 C11 1.464(8) . ? C11 N3 1.287(7) . ? C11 H11A 0.9500 . ? N3 C12 1.500(7) . ? C12 C14 1.525(8) . ? C12 C13 1.546(7) . ? C12 H12A 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.393(8) . ? C14 C19 1.402(8) . ? C15 C16 1.384(8) . ? C15 H15A 0.9500 . ? C16 C17 1.399(8) . ? C16 H16A 0.9500 . ? C17 C18 1.385(8) . ? C17 H17A 0.9500 . ? C18 C19 1.400(8) . ? C18 H18A 0.9500 . ? C19 H19A 0.9500 . ? O2 C20 1.300(6) . ? C20 C21 1.411(7) . ? C20 C25 1.428(8) . ? C21 C22 1.385(8) . ? C21 H21A 0.9500 . ? C22 C23 1.381(8) . ? C22 H22A 0.9500 . ? C23 C24 1.393(8) . ? C23 H23A 0.9500 . ? C24 C25 1.412(8) . ? C24 H24A 0.9500 . ? C25 C26 1.454(7) . ? C26 N4 1.271(7) . ? C26 H26A 0.9500 . ? N4 C27 1.488(7) . ? C27 C29 1.516(7) . ? C27 C28 1.516(8) . ? C27 H27A 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C34 1.396(7) . ? C29 C30 1.398(8) . ? C30 C31 1.374(8) . ? C30 H30A 0.9500 . ? C31 C32 1.395(8) . ? C31 H31A 0.9500 . ? C32 C33 1.380(8) . ? C32 H32A 0.9500 . ? C33 C34 1.377(8) . ? C33 H33A 0.9500 . ? C34 H34A 0.9500 . ? N5 C35 1.338(7) . ? N5 C38 1.345(7) . ? C35 C36 1.382(7) . ? C35 H35A 0.9500 . ? C36 N6 1.338(7) . ? C36 H36A 0.9500 . ? N6 C37 1.345(7) . ? N6 Fe2 2.247(4) . ? C37 C38 1.382(7) . ? C37 H37A 0.9500 . ? C38 H38A 0.9500 . ? Fe2 O3 1.964(4) . ? Fe2 O4 1.977(4) . ? Fe2 N8 2.220(5) . ? Fe2 N7 2.235(5) . ? Fe2 N9 2.258(4) . ? O3 C39 1.310(7) . ? C39 C40 1.389(9) . ? C39 C44 1.441(10) . ? C40 C41 1.361(10) . ? C40 H40A 0.9500 . ? C41 C42 1.406(12) . ? C41 H41A 0.9500 . ? C42 C43 1.364(11) . ? C42 H42A 0.9500 . ? C43 C44 1.444(10) . ? C43 H43A 0.9500 . ? C44 C45 1.428(10) . ? C45 N7 1.284(9) . ? C45 H45A 0.9500 . ? N7 C46 1.502(8) . ? C46 C47 1.518(9) . ? C46 C48 1.538(9) . ? C46 H46A 1.0000 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 C53 1.381(10) . ? C48 C49 1.382(9) . ? C49 C50 1.399(8) . ? C49 H49A 0.9500 . ? C50 C51 1.384(9) . ? C50 H50A 0.9500 . ? C51 C52 1.383(9) . ? C51 H51A 0.9500 . ? C52 C53 1.370(9) . ? C52 H52A 0.9500 . ? C53 H53A 0.9500 . ? O4 C54 1.291(8) . ? C54 C59 1.399(9) . ? C54 C55 1.429(9) . ? C55 C56 1.418(10) . ? C55 H55A 0.9500 . ? C56 C57 1.250(11) . ? C56 H56A 0.9500 . ? C57 C58 1.425(10) . ? C57 H57A 0.9500 . ? C58 C59 1.387(9) . ? C58 H58A 0.9500 . ? C59 C60 1.471(9) . ? C60 N8 1.276(8) . ? C60 H60A 0.9500 . ? N8 C61 1.487(7) . ? C61 C63 1.520(8) . ? C61 C62 1.520(8) . ? C61 H61A 1.0000 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 C64 1.377(9) . ? C63 C68 1.385(8) . ? C64 C65 1.383(8) . ? C64 H64A 0.9500 . ? C65 C66 1.397(9) . ? C65 H65A 0.9500 . ? C66 C67 1.387(9) . ? C66 H66A 0.9500 . ? C67 C68 1.380(8) . ? C67 H67A 0.9500 . ? C68 H68A 0.9500 . ? N9 C69 1.340(7) . ? N9 C72 1.348(7) . ? C69 C70 1.381(7) . ? C69 H69A 0.9500 . ? C70 N10 1.336(7) . ? C70 H70A 0.9500 . ? N10 C71 1.332(7) . ? N10 Fe3 2.288(4) . ? C71 C72 1.380(7) . ? C71 H71A 0.9500 . ? C72 H72A 0.9500 . ? Fe3 O5 1.972(4) . ? Fe3 O6 1.991(4) . ? Fe3 N12 2.235(4) . ? Fe3 N11 2.240(4) . ? Fe3 N1 2.317(5) 3_455 ? O5 C73 1.319(6) . ? C73 C78 1.406(8) . ? C73 C74 1.409(8) . ? C74 C75 1.383(8) . ? C74 H74A 0.9500 . ? C75 C76 1.413(9) . ? C75 H75A 0.9500 . ? C76 C77 1.382(8) . ? C76 H76A 0.9500 . ? C77 C78 1.415(8) . ? C77 H77A 0.9500 . ? C78 C79 1.448(8) . ? C79 N11 1.283(7) . ? C79 H79A 0.9500 . ? N11 C80 1.500(7) . ? C80 C82 1.526(8) . ? C80 C81 1.540(7) . ? C80 H80A 1.0000 . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? C82 C83 1.385(8) . ? C82 C87 1.385(8) . ? C83 C84 1.385(8) . ? C83 H83A 0.9500 . ? C84 C85 1.381(8) . ? C84 H84A 0.9500 . ? C85 C86 1.393(8) . ? C85 H85A 0.9500 . ? C86 C87 1.404(8) . ? C86 H86A 0.9500 . ? C87 H87A 0.9500 . ? O6 C88 1.302(6) . ? N12 C94 1.293(7) . ? N12 C95 1.488(8) . ? C88 C89 1.418(9) . ? C88 C93 1.423(8) . ? C89 C90 1.373(8) . ? C89 H89A 0.9500 . ? C90 C91 1.418(8) . ? C90 H90A 0.9500 . ? C91 C92 1.372(9) . ? C91 H91A 0.9500 . ? C92 C93 1.405(8) . ? C92 H92A 0.9500 . ? C93 C94 1.434(9) . ? C94 H94A 0.9500 . ? C95 C96 1.499(8) . ? C95 C97 1.513(9) . ? C95 H95A 1.0000 . ? C96 H96A 0.9800 . ? C96 H96B 0.9800 . ? C96 H96C 0.9800 . ? C97 C98 1.395(9) . ? C97 C102 1.400(9) . ? C98 C99 1.376(9) . ? C98 H98A 0.9500 . ? C99 C100 1.371(9) . ? C99 H99A 0.9500 . ? C100 C101 1.384(9) . ? C100 H10A 0.9500 . ? C101 C102 1.377(9) . ? C101 H10B 0.9500 . ? C102 H10C 0.9500 . ? C201 C202 1.518(11) . ? C201 H20A 0.9800 . ? C201 H20B 0.9800 . ? C201 H20C 0.9800 . ? C202 O203 1.425(9) . ? C202 H20D 0.9900 . ? C202 H20E 0.9900 . ? O203 C204 1.348(8) . ? C204 C205 1.479(10) . ? C204 H20F 0.9900 . ? C204 H20G 0.9900 . ? C205 H20H 0.9800 . ? C205 H20I 0.9800 . ? C205 H20J 0.9800 . ? C301 C302 1.499(12) . ? C301 H30B 0.9800 . ? C301 H30C 0.9800 . ? C301 H30D 0.9800 . ? C302 O303 1.426(9) . ? C302 H30E 0.9900 . ? C302 H30F 0.9900 . ? O303 C304 1.411(10) . ? C304 C305 1.499(11) . ? C304 H30G 0.9900 . ? C304 H30H 0.9900 . ? C305 H30I 0.9800 . ? C305 H30J 0.9800 . ? C305 H30K 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 C4 N1 C1 114.5(5) . . ? C4 N1 Fe3 123.2(3) . 3_545 ? C1 N1 Fe3 122.2(4) . 3_545 ? N1 C1 C2 123.6(5) . . ? N1 C1 H1A 118.2 . . ? C2 C1 H1A 118.2 . . ? N2 C2 C1 121.7(5) . . ? N2 C2 H2A 119.2 . . ? C1 C2 H2A 119.2 . . ? C3 N2 C2 115.0(5) . . ? C3 N2 Fe1 120.4(4) . . ? C2 N2 Fe1 124.5(3) . . ? N2 C3 C4 122.8(5) . . ? N2 C3 H3A 118.6 . . ? C4 C3 H3A 118.6 . . ? N1 C4 C3 122.4(5) . . ? N1 C4 H4A 118.8 . . ? C3 C4 H4A 118.8 . . ? O2 Fe1 O1 170.61(15) . . ? O2 Fe1 N3 102.43(16) . . ? O1 Fe1 N3 85.66(16) . . ? O2 Fe1 N4 85.71(16) . . ? O1 Fe1 N4 99.09(16) . . ? N3 Fe1 N4 90.70(16) . . ? O2 Fe1 N2 84.16(15) . . ? O1 Fe1 N2 91.38(15) . . ? N3 Fe1 N2 88.44(16) . . ? N4 Fe1 N2 169.40(17) . . ? O2 Fe1 N5 87.56(15) . . ? O1 Fe1 N5 83.93(15) . . ? N3 Fe1 N5 168.37(17) . . ? N4 Fe1 N5 96.03(16) . . ? N2 Fe1 N5 86.65(16) . . ? C5 O1 Fe1 133.9(4) . . ? O1 C5 C6 119.0(5) . . ? O1 C5 C10 124.1(5) . . ? C6 C5 C10 116.9(5) . . ? C7 C6 C5 120.9(6) . . ? C7 C6 H6A 119.5 . . ? C5 C6 H6A 119.5 . . ? C8 C7 C6 121.2(6) . . ? C8 C7 H7A 119.4 . . ? C6 C7 H7A 119.4 . . ? C9 C8 C7 117.7(6) . . ? C9 C8 H8A 121.2 . . ? C7 C8 H8A 121.2 . . ? C8 C9 C10 123.8(6) . . ? C8 C9 H9A 118.1 . . ? C10 C9 H9A 118.1 . . ? C9 C10 C5 119.4(6) . . ? C9 C10 C11 118.1(5) . . ? C5 C10 C11 122.6(5) . . ? N3 C11 C10 126.3(5) . . ? N3 C11 H11A 116.8 . . ? C10 C11 H11A 116.8 . . ? C11 N3 C12 118.2(4) . . ? C11 N3 Fe1 127.1(4) . . ? C12 N3 Fe1 114.7(3) . . ? N3 C12 C14 108.9(4) . . ? N3 C12 C13 116.4(5) . . ? C14 C12 C13 110.1(4) . . ? N3 C12 H12A 107.0 . . ? C14 C12 H12A 107.0 . . ? C13 C12 H12A 107.0 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C19 118.8(5) . . ? C15 C14 C12 120.5(5) . . ? C19 C14 C12 120.7(5) . . ? C16 C15 C14 121.1(5) . . ? C16 C15 H15A 119.5 . . ? C14 C15 H15A 119.5 . . ? C15 C16 C17 120.3(6) . . ? C15 C16 H16A 119.9 . . ? C17 C16 H16A 119.9 . . ? C18 C17 C16 119.1(6) . . ? C18 C17 H17A 120.4 . . ? C16 C17 H17A 120.4 . . ? C17 C18 C19 120.8(5) . . ? C17 C18 H18A 119.6 . . ? C19 C18 H18A 119.6 . . ? C18 C19 C14 119.9(5) . . ? C18 C19 H19A 120.0 . . ? C14 C19 H19A 120.0 . . ? C20 O2 Fe1 134.8(3) . . ? O2 C20 C21 119.8(5) . . ? O2 C20 C25 122.9(5) . . ? C21 C20 C25 117.3(5) . . ? C22 C21 C20 121.4(6) . . ? C22 C21 H21A 119.3 . . ? C20 C21 H21A 119.3 . . ? C23 C22 C21 121.0(5) . . ? C23 C22 H22A 119.5 . . ? C21 C22 H22A 119.5 . . ? C22 C23 C24 119.6(5) . . ? C22 C23 H23A 120.2 . . ? C24 C23 H23A 120.2 . . ? C23 C24 C25 120.4(6) . . ? C23 C24 H24A 119.8 . . ? C25 C24 H24A 119.8 . . ? C24 C25 C20 120.1(5) . . ? C24 C25 C26 115.9(5) . . ? C20 C25 C26 124.0(5) . . ? N4 C26 C25 126.8(5) . . ? N4 C26 H26A 116.6 . . ? C25 C26 H26A 116.6 . . ? C26 N4 C27 118.6(5) . . ? C26 N4 Fe1 125.1(4) . . ? C27 N4 Fe1 115.9(3) . . ? N4 C27 C29 109.0(4) . . ? N4 C27 C28 116.4(4) . . ? C29 C27 C28 111.0(4) . . ? N4 C27 H27A 106.6 . . ? C29 C27 H27A 106.6 . . ? C28 C27 H27A 106.6 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C34 C29 C30 117.5(5) . . ? C34 C29 C27 122.0(5) . . ? C30 C29 C27 120.5(4) . . ? C31 C30 C29 121.5(5) . . ? C31 C30 H30A 119.2 . . ? C29 C30 H30A 119.2 . . ? C30 C31 C32 120.0(5) . . ? C30 C31 H31A 120.0 . . ? C32 C31 H31A 120.0 . . ? C33 C32 C31 119.2(5) . . ? C33 C32 H32A 120.4 . . ? C31 C32 H32A 120.4 . . ? C34 C33 C32 120.5(5) . . ? C34 C33 H33A 119.8 . . ? C32 C33 H33A 119.8 . . ? C33 C34 C29 121.2(5) . . ? C33 C34 H34A 119.4 . . ? C29 C34 H34A 119.4 . . ? C35 N5 C38 116.1(5) . . ? C35 N5 Fe1 121.3(4) . . ? C38 N5 Fe1 122.4(4) . . ? N5 C35 C36 121.5(5) . . ? N5 C35 H35A 119.3 . . ? C36 C35 H35A 119.3 . . ? N6 C36 C35 122.8(5) . . ? N6 C36 H36A 118.6 . . ? C35 C36 H36A 118.6 . . ? C36 N6 C37 115.8(5) . . ? C36 N6 Fe2 123.0(4) . . ? C37 N6 Fe2 121.1(4) . . ? N6 C37 C38 121.6(5) . . ? N6 C37 H37A 119.2 . . ? C38 C37 H37A 119.2 . . ? N5 C38 C37 122.3(5) . . ? N5 C38 H38A 118.8 . . ? C37 C38 H38A 118.8 . . ? O3 Fe2 O4 177.7(2) . . ? O3 Fe2 N8 91.57(19) . . ? O4 Fe2 N8 86.14(18) . . ? O3 Fe2 N7 86.9(2) . . ? O4 Fe2 N7 95.3(2) . . ? N8 Fe2 N7 177.0(2) . . ? O3 Fe2 N6 91.21(16) . . ? O4 Fe2 N6 89.21(16) . . ? N8 Fe2 N6 91.50(17) . . ? N7 Fe2 N6 91.11(17) . . ? O3 Fe2 N9 88.96(16) . . ? O4 Fe2 N9 90.58(16) . . ? N8 Fe2 N9 87.39(16) . . ? N7 Fe2 N9 90.01(17) . . ? N6 Fe2 N9 178.88(18) . . ? C39 O3 Fe2 135.3(4) . . ? O3 C39 C40 120.2(7) . . ? O3 C39 C44 121.1(6) . . ? C40 C39 C44 118.7(6) . . ? C41 C40 C39 122.5(8) . . ? C41 C40 H40A 118.7 . . ? C39 C40 H40A 118.7 . . ? C40 C41 C42 119.5(8) . . ? C40 C41 H41A 120.2 . . ? C42 C41 H41A 120.2 . . ? C43 C42 C41 121.3(7) . . ? C43 C42 H42A 119.4 . . ? C41 C42 H42A 119.4 . . ? C42 C43 C44 119.9(8) . . ? C42 C43 H43A 120.0 . . ? C44 C43 H43A 120.0 . . ? C45 C44 C39 125.6(6) . . ? C45 C44 C43 116.4(7) . . ? C39 C44 C43 118.0(7) . . ? N7 C45 C44 128.5(7) . . ? N7 C45 H45A 115.7 . . ? C44 C45 H45A 115.7 . . ? C45 N7 C46 115.3(5) . . ? C45 N7 Fe2 122.2(5) . . ? C46 N7 Fe2 122.4(4) . . ? N7 C46 C47 111.7(5) . . ? N7 C46 C48 110.9(5) . . ? C47 C46 C48 113.8(6) . . ? N7 C46 H46A 106.6 . . ? C47 C46 H46A 106.6 . . ? C48 C46 H46A 106.6 . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C53 C48 C49 119.3(6) . . ? C53 C48 C46 121.0(6) . . ? C49 C48 C46 119.6(6) . . ? C48 C49 C50 120.9(6) . . ? C48 C49 H49A 119.6 . . ? C50 C49 H49A 119.6 . . ? C51 C50 C49 119.4(6) . . ? C51 C50 H50A 120.3 . . ? C49 C50 H50A 120.3 . . ? C52 C51 C50 118.8(6) . . ? C52 C51 H51A 120.6 . . ? C50 C51 H51A 120.6 . . ? C53 C52 C51 121.9(7) . . ? C53 C52 H52A 119.0 . . ? C51 C52 H52A 119.0 . . ? C52 C53 C48 119.7(6) . . ? C52 C53 H53A 120.1 . . ? C48 C53 H53A 120.1 . . ? C54 O4 Fe2 134.0(4) . . ? O4 C54 C59 124.8(6) . . ? O4 C54 C55 118.7(6) . . ? C59 C54 C55 116.5(6) . . ? C56 C55 C54 119.7(7) . . ? C56 C55 H55A 120.1 . . ? C54 C55 H55A 120.1 . . ? C57 C56 C55 122.3(7) . . ? C57 C56 H56A 118.9 . . ? C55 C56 H56A 118.9 . . ? C56 C57 C58 121.4(7) . . ? C56 C57 H57A 119.3 . . ? C58 C57 H57A 119.3 . . ? C59 C58 C57 119.2(7) . . ? C59 C58 H58A 120.4 . . ? C57 C58 H58A 120.4 . . ? C58 C59 C54 120.7(6) . . ? C58 C59 C60 116.1(6) . . ? C54 C59 C60 123.1(6) . . ? N8 C60 C59 127.3(6) . . ? N8 C60 H60A 116.4 . . ? C59 C60 H60A 116.4 . . ? C60 N8 C61 117.4(5) . . ? C60 N8 Fe2 123.7(4) . . ? C61 N8 Fe2 118.4(4) . . ? N8 C61 C63 110.5(4) . . ? N8 C61 C62 117.7(5) . . ? C63 C61 C62 107.8(5) . . ? N8 C61 H61A 106.8 . . ? C63 C61 H61A 106.8 . . ? C62 C61 H61A 106.8 . . ? 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 . . ? C64 C63 C68 117.8(6) . . ? C64 C63 C61 119.2(5) . . ? C68 C63 C61 122.7(6) . . ? C63 C64 C65 121.9(6) . . ? C63 C64 H64A 119.0 . . ? C65 C64 H64A 119.0 . . ? C64 C65 C66 119.9(6) . . ? C64 C65 H65A 120.1 . . ? C66 C65 H65A 120.1 . . ? C67 C66 C65 118.4(6) . . ? C67 C66 H66A 120.8 . . ? C65 C66 H66A 120.8 . . ? C68 C67 C66 120.7(6) . . ? C68 C67 H67A 119.7 . . ? C66 C67 H67A 119.7 . . ? C67 C68 C63 121.3(6) . . ? C67 C68 H68A 119.4 . . ? C63 C68 H68A 119.4 . . ? C69 N9 C72 116.6(5) . . ? C69 N9 Fe2 122.3(4) . . ? C72 N9 Fe2 121.1(4) . . ? N9 C69 C70 120.8(5) . . ? N9 C69 H69A 119.6 . . ? C70 C69 H69A 119.6 . . ? N10 C70 C69 123.2(5) . . ? N10 C70 H70A 118.4 . . ? C69 C70 H70A 118.4 . . ? C71 N10 C70 115.5(5) . . ? C71 N10 Fe3 122.5(4) . . ? C70 N10 Fe3 121.9(4) . . ? N10 C71 C72 122.5(5) . . ? N10 C71 H71A 118.7 . . ? C72 C71 H71A 118.7 . . ? N9 C72 C71 121.4(5) . . ? N9 C72 H72A 119.3 . . ? C71 C72 H72A 119.3 . . ? O5 Fe3 O6 168.52(17) . . ? O5 Fe3 N12 102.88(16) . . ? O6 Fe3 N12 84.64(16) . . ? O5 Fe3 N11 84.36(16) . . ? O6 Fe3 N11 103.10(17) . . ? N12 Fe3 N11 99.73(17) . . ? O5 Fe3 N10 87.65(15) . . ? O6 Fe3 N10 83.76(15) . . ? N12 Fe3 N10 166.61(17) . . ? N11 Fe3 N10 89.40(16) . . ? O5 Fe3 N1 80.99(16) . 3_455 ? O6 Fe3 N1 90.83(16) . 3_455 ? N12 Fe3 N1 87.25(16) . 3_455 ? N11 Fe3 N1 164.88(16) . 3_455 ? N10 Fe3 N1 86.27(16) . 3_455 ? C73 O5 Fe3 136.4(4) . . ? O5 C73 C78 123.0(5) . . ? O5 C73 C74 118.1(5) . . ? C78 C73 C74 118.9(5) . . ? C75 C74 C73 120.4(6) . . ? C75 C74 H74A 119.8 . . ? C73 C74 H74A 119.8 . . ? C74 C75 C76 121.6(6) . . ? C74 C75 H75A 119.2 . . ? C76 C75 H75A 119.2 . . ? C77 C76 C75 118.0(5) . . ? C77 C76 H76A 121.0 . . ? C75 C76 H76A 121.0 . . ? C76 C77 C78 121.7(6) . . ? C76 C77 H77A 119.2 . . ? C78 C77 H77A 119.2 . . ? C73 C78 C77 119.5(5) . . ? C73 C78 C79 123.7(5) . . ? C77 C78 C79 116.8(5) . . ? N11 C79 C78 127.4(5) . . ? N11 C79 H79A 116.3 . . ? C78 C79 H79A 116.3 . . ? C79 N11 C80 112.7(5) . . ? C79 N11 Fe3 125.1(4) . . ? C80 N11 Fe3 122.2(3) . . ? N11 C80 C82 112.1(5) . . ? N11 C80 C81 108.7(4) . . ? C82 C80 C81 114.4(5) . . ? N11 C80 H80A 107.0 . . ? C82 C80 H80A 107.0 . . ? C81 C80 H80A 107.0 . . ? C80 C81 H81A 109.5 . . ? C80 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C80 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C83 C82 C87 118.9(6) . . ? C83 C82 C80 123.9(5) . . ? C87 C82 C80 117.1(5) . . ? C84 C83 C82 120.7(5) . . ? C84 C83 H83A 119.6 . . ? C82 C83 H83A 119.6 . . ? C85 C84 C83 121.0(6) . . ? C85 C84 H84A 119.5 . . ? C83 C84 H84A 119.5 . . ? C84 C85 C86 118.9(6) . . ? C84 C85 H85A 120.5 . . ? C86 C85 H85A 120.5 . . ? C85 C86 C87 120.0(5) . . ? C85 C86 H86A 120.0 . . ? C87 C86 H86A 120.0 . . ? C82 C87 C86 120.5(5) . . ? C82 C87 H87A 119.8 . . ? C86 C87 H87A 119.8 . . ? C88 O6 Fe3 136.6(4) . . ? C94 N12 C95 116.3(4) . . ? C94 N12 Fe3 123.6(4) . . ? C95 N12 Fe3 120.0(3) . . ? O6 C88 C89 119.6(5) . . ? O6 C88 C93 122.9(6) . . ? C89 C88 C93 117.5(5) . . ? C90 C89 C88 122.3(6) . . ? C90 C89 H89A 118.9 . . ? C88 C89 H89A 118.9 . . ? C89 C90 C91 119.9(6) . . ? C89 C90 H90A 120.0 . . ? C91 C90 H90A 120.0 . . ? C92 C91 C90 118.6(6) . . ? C92 C91 H91A 120.7 . . ? C90 C91 H91A 120.7 . . ? C91 C92 C93 122.7(6) . . ? C91 C92 H92A 118.7 . . ? C93 C92 H92A 118.7 . . ? C92 C93 C88 119.0(6) . . ? C92 C93 C94 118.1(5) . . ? C88 C93 C94 122.8(5) . . ? N12 C94 C93 129.4(5) . . ? N12 C94 H94A 115.3 . . ? C93 C94 H94A 115.3 . . ? N12 C95 C96 108.9(5) . . ? N12 C95 C97 109.9(5) . . ? C96 C95 C97 116.9(5) . . ? N12 C95 H95A 106.9 . . ? C96 C95 H95A 106.9 . . ? C97 C95 H95A 106.9 . . ? C95 C96 H96A 109.5 . . ? C95 C96 H96B 109.5 . . ? H96A C96 H96B 109.5 . . ? C95 C96 H96C 109.5 . . ? H96A C96 H96C 109.5 . . ? H96B C96 H96C 109.5 . . ? C98 C97 C102 118.1(6) . . ? C98 C97 C95 119.6(6) . . ? C102 C97 C95 122.4(6) . . ? C99 C98 C97 120.0(6) . . ? C99 C98 H98A 120.0 . . ? C97 C98 H98A 120.0 . . ? C100 C99 C98 122.0(7) . . ? C100 C99 H99A 119.0 . . ? C98 C99 H99A 119.0 . . ? C99 C100 C101 118.3(7) . . ? C99 C100 H10A 120.8 . . ? C101 C100 H10A 120.8 . . ? C102 C101 C100 120.9(6) . . ? C102 C101 H10B 119.6 . . ? C100 C101 H10B 119.6 . . ? C101 C102 C97 120.6(6) . . ? C101 C102 H10C 119.7 . . ? C97 C102 H10C 119.7 . . ? C202 C201 H20A 109.5 . . ? C202 C201 H20B 109.5 . . ? H20A C201 H20B 109.5 . . ? C202 C201 H20C 109.5 . . ? H20A C201 H20C 109.5 . . ? H20B C201 H20C 109.5 . . ? O203 C202 C201 108.7(6) . . ? O203 C202 H20D 110.0 . . ? C201 C202 H20D 110.0 . . ? O203 C202 H20E 110.0 . . ? C201 C202 H20E 110.0 . . ? H20D C202 H20E 108.3 . . ? C204 O203 C202 116.7(6) . . ? O203 C204 C205 112.9(6) . . ? O203 C204 H20F 109.0 . . ? C205 C204 H20F 109.0 . . ? O203 C204 H20G 109.0 . . ? C205 C204 H20G 109.0 . . ? H20F C204 H20G 107.8 . . ? C204 C205 H20H 109.5 . . ? C204 C205 H20I 109.5 . . ? H20H C205 H20I 109.5 . . ? C204 C205 H20J 109.5 . . ? H20H C205 H20J 109.5 . . ? H20I C205 H20J 109.5 . . ? C302 C301 H30B 109.5 . . ? C302 C301 H30C 109.5 . . ? H30B C301 H30C 109.5 . . ? C302 C301 H30D 109.5 . . ? H30B C301 H30D 109.5 . . ? H30C C301 H30D 109.5 . . ? O303 C302 C301 109.5(7) . . ? O303 C302 H30E 109.8 . . ? C301 C302 H30E 109.8 . . ? O303 C302 H30F 109.8 . . ? C301 C302 H30F 109.8 . . ? H30E C302 H30F 108.2 . . ? C304 O303 C302 112.5(6) . . ? O303 C304 C305 106.8(7) . . ? O303 C304 H30G 110.4 . . ? C305 C304 H30G 110.4 . . ? O303 C304 H30H 110.4 . . ? C305 C304 H30H 110.4 . . ? H30G C304 H30H 108.6 . . ? C304 C305 H30I 109.5 . . ? C304 C305 H30J 109.5 . . ? H30I C305 H30J 109.5 . . ? C304 C305 H30K 109.5 . . ? H30I C305 H30K 109.5 . . ? H30J C305 H30K 109.5 . . ? _diffrn_measured_fraction_theta_max 0.839 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.398 _refine_diff_density_min -0.768 _refine_diff_density_rms 0.096 #===END data_ll22 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H42 Fe N6 O2' _chemical_formula_weight 742.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' -1.1336 3.1974 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 26.8700(6) _cell_length_b 11.5749(2) _cell_length_c 14.8955(3) _cell_angle_alpha 90.00 _cell_angle_beta 121.146(3) _cell_angle_gamma 90.00 _cell_volume 3964.96(16) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4373 _cell_measurement_theta_min 3.47 _cell_measurement_theta_max 61.95 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.244 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1560 _exptl_absorpt_coefficient_mu 3.393 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.51 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'ABSPACK(CrysAlis, Oxford Diffraction)' _exptl_special_details ; The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cobra. The data collection nominally covered over a hemisphere of Reciprocal space, by a combination of 12 sets of exposures with different \f angles for the crystal; low angle data was collected at 25 s exposure and high angle at 100s and covered 1.0\% in \w. The crystal-to-detector distance was 5.5 cm. Crystal decay was found to be negligible by by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms; H-atoms were given isotropic displacement parameter equal to 1.2 (or 1.5 for methyl H-atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. Poor quality very weakly diffracting crystals of a coordination polymer with no meaningful diffraction above 62 degrees. Many crystals investigated but this was the only one to give any measurable diffraction. Both crystallographiclly independant but chemically identical complexes lie on a 2 fold axis through the bipy and iron. Two acetonitrile molecules of crystalisation were also located in the asymmetric unit. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 10.2833 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 6483 _diffrn_reflns_av_R_equivalents 0.0169 _diffrn_reflns_av_sigmaI/netI 0.0349 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.47 _diffrn_reflns_theta_max 62.04 _reflns_number_total 4934 _reflns_number_gt 4417 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0690P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881, 1704 Friedel pairs' _refine_ls_abs_structure_Flack 0.005(4) _chemical_absolute_configuration rmad _refine_ls_number_reflns 4934 _refine_ls_number_parameters 485 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0411 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.0951 _refine_ls_wR_factor_gt 0.0932 _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_restrained_S_all 0.985 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 1.0000 0.96099(6) 1.5000 0.01736(18) Uani 1 2 d S . . O1 O 0.91885(8) 0.9617(2) 1.37629(15) 0.0203(5) Uani 1 1 d . . . C1 C 0.89731(13) 0.9688(3) 1.2765(2) 0.0214(7) Uani 1 1 d . . . N1 N 1.02832(11) 0.9569(3) 1.38785(19) 0.0225(6) Uani 1 1 d . . . C2 C 0.83680(15) 0.9805(3) 1.2085(3) 0.0306(8) Uani 1 1 d . . . H2A H 0.8128 0.9843 1.2379 0.037 Uiso 1 1 calc R . . N2 N 1.0000 0.7686(4) 1.5000 0.0176(9) Uani 1 2 d S . . C3 C 0.81089(16) 0.9869(3) 1.1008(3) 0.0368(10) Uani 1 1 d . . . H3A H 0.7699 0.9943 1.0581 0.044 Uiso 1 1 calc R . . N3 N 1.0000 0.1544(4) 1.5000 0.0218(9) Uani 1 2 d S . . C4 C 0.84452(16) 0.9824(4) 1.0545(3) 0.0392(10) Uani 1 1 d . . . H4A H 0.8269 0.9872 0.9805 0.047 Uiso 1 1 calc R . . C5 C 0.90395(15) 0.9707(4) 1.1186(2) 0.0348(9) Uani 1 1 d . . . H5A H 0.9270 0.9665 1.0873 0.042 Uiso 1 1 calc R . . C6 C 0.93168(13) 0.9650(3) 1.2283(2) 0.0240(7) Uani 1 1 d . . . C7 C 0.99419(14) 0.9565(3) 1.2869(2) 0.0259(7) Uani 1 1 d . . . H7A H 1.0124 0.9498 1.2469 0.031 Uiso 1 1 calc R . . C8 C 1.09140(14) 0.9551(3) 1.4277(2) 0.0280(8) Uani 1 1 d . . . H8A H 1.1112 0.9482 1.5057 0.034 Uiso 1 1 calc R . . C9 C 1.10989(18) 1.0720(4) 1.4063(3) 0.0438(10) Uani 1 1 d . . . H9A H 1.0937 1.1342 1.4282 0.066 Uiso 1 1 calc R . . H9B H 1.0954 1.0792 1.3312 0.066 Uiso 1 1 calc R . . H9C H 1.1524 1.0773 1.4459 0.066 Uiso 1 1 calc R . . C10 C 1.11099(14) 0.8505(4) 1.3910(2) 0.0265(8) Uani 1 1 d . . . C11 C 1.08654(16) 0.7424(3) 1.3832(3) 0.0336(9) Uani 1 1 d . . . H11A H 1.0551 0.7350 1.3948 0.040 Uiso 1 1 calc R . . C12 C 1.10734(17) 0.6450(3) 1.3587(3) 0.0361(9) Uani 1 1 d . . . H12A H 1.0901 0.5719 1.3539 0.043 Uiso 1 1 calc R . . C13 C 1.15302(16) 0.6537(4) 1.3412(3) 0.0398(10) Uani 1 1 d . . . H13A H 1.1676 0.5871 1.3252 0.048 Uiso 1 1 calc R . . C14 C 1.17689(15) 0.7612(4) 1.3476(3) 0.0414(11) Uani 1 1 d . . . H14A H 1.2083 0.7688 1.3358 0.050 Uiso 1 1 calc R . . C15 C 1.15545(14) 0.8576(4) 1.3710(3) 0.0353(9) Uani 1 1 d . . . H15A H 1.1719 0.9310 1.3733 0.042 Uiso 1 1 calc R . . C16 C 0.95862(15) 0.7073(3) 1.4186(3) 0.0236(8) Uani 1 1 d . . . H16A H 0.9288 0.7486 1.3606 0.028 Uiso 1 1 calc R . . C17 C 0.95689(15) 0.5877(3) 1.4143(3) 0.0233(8) Uani 1 1 d . . . H17A H 0.9270 0.5489 1.3543 0.028 Uiso 1 1 calc R . . C18 C 1.0000 0.5246(4) 1.5000 0.0212(12) Uani 1 2 d S . . C19 C 1.0000 0.3971(4) 1.5000 0.0191(11) Uani 1 2 d S . . C20 C 0.94888(15) 0.3337(3) 1.4446(3) 0.0234(8) Uani 1 1 d . . . H20A H 0.9127 0.3726 1.4054 0.028 Uiso 1 1 calc R . . C21 C 0.95057(15) 0.2152(3) 1.4462(3) 0.0223(8) Uani 1 1 d . . . H21A H 0.9150 0.1741 1.4074 0.027 Uiso 1 1 calc R . . Fe2 Fe 1.0000 0.36442(6) 1.0000 0.01866(19) Uani 1 2 d S . . O2 O 0.94196(9) 0.3614(2) 0.84570(16) 0.0277(5) Uani 1 1 d . . . N4 N 0.92631(11) 0.3765(2) 1.0210(2) 0.0265(6) Uani 1 1 d . . . N5 N 1.0000 0.5580(4) 1.0000 0.0195(9) Uani 1 2 d S . . N6 N 1.0000 1.1712(4) 1.0000 0.0195(9) Uani 1 2 d S . . C22 C 0.88556(13) 0.3565(3) 0.7903(3) 0.0276(8) Uani 1 1 d . . . C23 C 0.85665(16) 0.3404(3) 0.6803(3) 0.0340(9) Uani 1 1 d . . . H23A H 0.8792 0.3305 0.6484 0.041 Uiso 1 1 calc R . . C24 C 0.79696(17) 0.3386(4) 0.6182(3) 0.0419(11) Uani 1 1 d . . . H24A H 0.7790 0.3287 0.5445 0.050 Uiso 1 1 calc R . . C25 C 0.76321(16) 0.3511(4) 0.6624(3) 0.0439(10) Uani 1 1 d . . . H25A H 0.7220 0.3522 0.6194 0.053 Uiso 1 1 calc R . . C26 C 0.78978(15) 0.3620(4) 0.7692(3) 0.0402(9) Uani 1 1 d . . . H26A H 0.7662 0.3678 0.7994 0.048 Uiso 1 1 calc R . . C27 C 0.85024(14) 0.3650(3) 0.8354(2) 0.0292(7) Uani 1 1 d . . . C28 C 0.87278(14) 0.3777(3) 0.9465(3) 0.0304(8) Uani 1 1 d . . . H28A H 0.8448 0.3881 0.9667 0.036 Uiso 1 1 calc R . . C29 C 0.94033(15) 0.3894(3) 1.1322(3) 0.0303(9) Uani 1 1 d . . . H29A H 0.9791 0.4283 1.1718 0.036 Uiso 1 1 calc R . . C30 C 0.94812(18) 0.2702(4) 1.1790(3) 0.0432(10) Uani 1 1 d . . . H30A H 0.9586 0.2769 1.2524 0.065 Uiso 1 1 calc R . . H30B H 0.9791 0.2295 1.1757 0.065 Uiso 1 1 calc R . . H30C H 0.9117 0.2268 1.1394 0.065 Uiso 1 1 calc R . . C31 C 0.89789(14) 0.4665(4) 1.1414(2) 0.0293(8) Uani 1 1 d . . . C32 C 0.90190(17) 0.5878(3) 1.1331(3) 0.0352(9) Uani 1 1 d . . . H32A H 0.9314 0.6188 1.1229 0.042 Uiso 1 1 calc R . . C33 C 0.86350(16) 0.6613(3) 1.1397(3) 0.0352(9) Uani 1 1 d . . . H33A H 0.8664 0.7423 1.1332 0.042 Uiso 1 1 calc R . . C34 C 0.82052(18) 0.6169(4) 1.1557(3) 0.0429(11) Uani 1 1 d . . . H34A H 0.7942 0.6677 1.1606 0.052 Uiso 1 1 calc R . . C35 C 0.81624(15) 0.5009(4) 1.1641(3) 0.0369(10) Uani 1 1 d . . . H35A H 0.7868 0.4708 1.1749 0.044 Uiso 1 1 calc R . . C36 C 0.85475(15) 0.4255(3) 1.1571(3) 0.0334(9) Uani 1 1 d . . . H36A H 0.8512 0.3447 1.1633 0.040 Uiso 1 1 calc R . . C37 C 1.03720(16) 0.6179(3) 1.0845(3) 0.0303(9) Uani 1 1 d . . . H37A H 1.0644 0.5769 1.1458 0.036 Uiso 1 1 calc R . . C38 C 1.03803(16) 0.7372(3) 1.0874(3) 0.0324(9) Uani 1 1 d . . . H38A H 1.0651 0.7759 1.1503 0.039 Uiso 1 1 calc R . . C39 C 1.0000 0.8007(4) 1.0000 0.0187(11) Uani 1 2 d S . . C40 C 1.0000 0.9285(4) 1.0000 0.0180(11) Uani 1 2 d S . . C41 C 1.04915(14) 0.9912(3) 1.0703(2) 0.0216(8) Uani 1 1 d . . . H41A H 1.0837 0.9523 1.1203 0.026 Uiso 1 1 calc R . . C42 C 1.04735(15) 1.1107(3) 1.0668(3) 0.0227(8) Uani 1 1 d . . . H42A H 1.0816 1.1520 1.1144 0.027 Uiso 1 1 calc R . . N7 N 0.69600(15) 0.7652(4) 0.6906(3) 0.0591(11) Uani 1 1 d . . . C43 C 0.73532(19) 0.7354(4) 0.7664(4) 0.0448(11) Uani 1 1 d . . . C44 C 0.7877(2) 0.6998(5) 0.8634(3) 0.0709(15) Uani 1 1 d . . . H44A H 0.7933 0.6164 0.8616 0.106 Uiso 1 1 calc R . . H44B H 0.7836 0.7184 0.9234 0.106 Uiso 1 1 calc R . . H44C H 0.8215 0.7408 0.8703 0.106 Uiso 1 1 calc R . . N8 N 0.69515(15) 0.5233(3) 1.2164(3) 0.0527(10) Uani 1 1 d . . . C45 C 0.73773(18) 0.5393(4) 1.2916(3) 0.0427(11) Uani 1 1 d . . . C46 C 0.79275(19) 0.5558(5) 1.3897(3) 0.0634(14) Uani 1 1 d . . . H46A H 0.7875 0.5394 1.4488 0.095 Uiso 1 1 calc R . . H46B H 0.8057 0.6359 1.3942 0.095 Uiso 1 1 calc R . . H46C H 0.8220 0.5033 1.3920 0.095 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0205(4) 0.0140(4) 0.0161(4) 0.000 0.0084(3) 0.000 O1 0.0254(11) 0.0179(11) 0.0171(11) -0.0001(11) 0.0107(9) -0.0006(11) C1 0.0241(17) 0.0136(17) 0.0208(17) 0.0009(16) 0.0076(14) 0.0018(16) N1 0.0258(14) 0.0199(14) 0.0228(14) -0.0002(14) 0.0131(12) -0.0013(13) C2 0.0321(19) 0.033(2) 0.0278(18) 0.0006(17) 0.0160(16) 0.0022(17) N2 0.023(2) 0.016(2) 0.015(2) 0.000 0.0111(19) 0.000 C3 0.029(2) 0.044(3) 0.0236(19) 0.0001(18) 0.0036(17) 0.0014(18) N3 0.026(2) 0.016(2) 0.022(2) 0.000 0.012(2) 0.000 C4 0.044(2) 0.045(3) 0.0201(18) 0.0029(18) 0.0110(17) 0.003(2) C5 0.041(2) 0.042(2) 0.0232(18) 0.0042(19) 0.0178(17) 0.006(2) C6 0.0284(17) 0.0213(17) 0.0203(16) 0.0014(16) 0.0112(14) 0.0008(16) C7 0.0334(18) 0.0249(18) 0.0260(18) 0.0004(18) 0.0201(16) -0.0010(17) C8 0.0269(18) 0.035(2) 0.0259(17) -0.0055(19) 0.0162(16) -0.0071(18) C9 0.044(2) 0.039(2) 0.059(3) -0.012(2) 0.035(2) -0.014(2) C10 0.0239(17) 0.036(2) 0.0155(16) 0.0020(17) 0.0077(14) 0.0031(17) C11 0.041(2) 0.036(2) 0.033(2) 0.0025(18) 0.0257(19) 0.0057(19) C12 0.047(2) 0.033(2) 0.027(2) 0.0023(17) 0.0181(19) 0.0064(19) C13 0.038(2) 0.052(3) 0.0207(19) -0.0006(19) 0.0093(18) 0.018(2) C14 0.0230(19) 0.064(3) 0.034(2) -0.018(2) 0.0128(18) -0.003(2) C15 0.0256(17) 0.049(2) 0.0303(19) -0.015(2) 0.0135(16) -0.006(2) C16 0.0262(19) 0.024(2) 0.0176(16) 0.0046(16) 0.0093(15) 0.0028(16) C17 0.0248(19) 0.019(2) 0.0202(18) -0.0037(16) 0.0077(16) -0.0042(16) C18 0.027(3) 0.020(3) 0.022(3) 0.000 0.016(2) 0.000 C19 0.020(3) 0.016(3) 0.018(3) 0.000 0.008(2) 0.000 C20 0.0237(19) 0.017(2) 0.0256(19) 0.0020(14) 0.0096(17) 0.0044(14) C21 0.0202(18) 0.019(2) 0.0231(19) -0.0013(15) 0.0078(16) -0.0011(14) Fe2 0.0206(4) 0.0156(4) 0.0158(4) 0.000 0.0066(3) 0.000 O2 0.0288(12) 0.0248(12) 0.0263(12) -0.0020(12) 0.0118(11) -0.0022(12) N4 0.0273(15) 0.0237(16) 0.0235(14) 0.0026(14) 0.0095(13) 0.0017(14) N5 0.023(2) 0.014(2) 0.019(2) 0.000 0.009(2) 0.000 N6 0.019(2) 0.023(2) 0.016(2) 0.000 0.0086(18) 0.000 C22 0.0237(17) 0.0145(18) 0.0286(19) 0.0029(17) 0.0023(16) 0.0007(16) C23 0.043(2) 0.025(2) 0.036(2) -0.0021(17) 0.0215(19) 0.0008(17) C24 0.042(2) 0.042(3) 0.0219(19) -0.0044(18) 0.0022(18) -0.0004(19) C25 0.0265(19) 0.049(3) 0.039(2) -0.001(2) 0.0048(18) 0.004(2) C26 0.035(2) 0.041(2) 0.041(2) -0.005(2) 0.0174(18) 0.006(2) C27 0.0331(18) 0.0221(17) 0.0244(17) -0.0008(17) 0.0093(15) 0.0039(18) C28 0.0301(19) 0.029(2) 0.0330(19) -0.0010(17) 0.0173(17) 0.0032(17) C29 0.0276(19) 0.035(2) 0.0286(19) -0.0030(17) 0.0149(17) -0.0031(16) C30 0.051(3) 0.046(3) 0.040(2) 0.013(2) 0.029(2) 0.018(2) C31 0.038(2) 0.0288(19) 0.0163(16) -0.0041(18) 0.0102(15) -0.0012(19) C32 0.042(2) 0.039(2) 0.025(2) 0.0030(18) 0.0171(19) 0.0046(19) C33 0.045(2) 0.030(2) 0.0249(19) 0.0015(17) 0.0138(18) 0.0125(19) C34 0.041(2) 0.051(3) 0.027(2) -0.002(2) 0.0103(19) 0.014(2) C35 0.027(2) 0.053(3) 0.0247(19) -0.0089(19) 0.0090(17) -0.0016(18) C36 0.030(2) 0.039(2) 0.030(2) -0.0068(17) 0.0148(18) -0.0008(16) C37 0.035(2) 0.017(2) 0.0205(18) 0.0020(16) 0.0009(17) 0.0020(16) C38 0.034(2) 0.025(2) 0.0232(19) -0.0030(17) 0.0038(17) -0.0019(17) C39 0.017(3) 0.018(3) 0.021(3) 0.000 0.009(2) 0.000 C40 0.025(3) 0.014(3) 0.019(2) 0.000 0.014(2) 0.000 C41 0.0220(18) 0.020(2) 0.0196(17) 0.0039(14) 0.0087(15) 0.0036(14) C42 0.0226(18) 0.021(2) 0.0215(19) -0.0027(15) 0.0097(16) -0.0043(15) N7 0.035(2) 0.060(3) 0.076(3) 0.009(2) 0.025(2) -0.003(2) C43 0.037(2) 0.044(3) 0.057(3) 0.002(2) 0.027(2) -0.004(2) C44 0.071(3) 0.076(4) 0.045(3) 0.011(3) 0.016(3) -0.012(3) N8 0.034(2) 0.083(3) 0.039(2) -0.008(2) 0.0175(19) -0.0059(19) C45 0.037(2) 0.059(3) 0.035(2) -0.009(2) 0.021(2) 0.001(2) C46 0.046(3) 0.081(4) 0.039(3) -0.012(3) 0.005(2) -0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O1 1.999(2) 2_758 ? Fe1 O1 1.999(2) . ? Fe1 N1 2.165(2) 2_758 ? Fe1 N1 2.165(2) . ? Fe1 N2 2.227(4) . ? Fe1 N3 2.239(4) 1_565 ? O1 C1 1.289(3) . ? C1 C2 1.409(4) . ? C1 C6 1.433(4) . ? N1 C7 1.294(4) . ? N1 C8 1.478(4) . ? C2 C3 1.380(5) . ? C2 H2A 0.9500 . ? N2 C16 1.348(4) . ? N2 C16 1.348(4) 2_758 ? C3 C4 1.393(5) . ? C3 H3A 0.9500 . ? N3 C21 1.342(4) 2_758 ? N3 C21 1.342(4) . ? N3 Fe1 2.239(4) 1_545 ? C4 C5 1.379(5) . ? C4 H4A 0.9500 . ? C5 C6 1.404(4) . ? C5 H5A 0.9500 . ? C6 C7 1.441(4) . ? C7 H7A 0.9500 . ? C8 C10 1.530(5) . ? C8 C9 1.531(5) . ? C8 H8A 1.0000 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C15 1.375(5) . ? C10 C11 1.391(5) . ? C11 C12 1.387(5) . ? C11 H11A 0.9500 . ? C12 C13 1.384(5) . ? C12 H12A 0.9500 . ? C13 C14 1.380(6) . ? C13 H13A 0.9500 . ? C14 C15 1.381(6) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C16 C17 1.385(5) . ? C16 H16A 0.9500 . ? C17 C18 1.405(4) . ? C17 H17A 0.9500 . ? C18 C17 1.405(4) 2_758 ? C18 C19 1.477(6) . ? C19 C20 1.390(4) . ? C19 C20 1.390(4) 2_758 ? C20 C21 1.373(5) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? Fe2 O2 2.002(2) 2_757 ? Fe2 O2 2.002(2) . ? Fe2 N4 2.163(3) 2_757 ? Fe2 N4 2.163(3) . ? Fe2 N6 2.237(4) 1_545 ? Fe2 N5 2.240(4) . ? O2 C22 1.299(4) . ? N4 C28 1.284(4) . ? N4 C29 1.504(4) . ? N5 C37 1.328(4) . ? N5 C37 1.328(4) 2_757 ? N6 C42 1.338(4) . ? N6 C42 1.338(4) 2_757 ? N6 Fe2 2.237(4) 1_565 ? C22 C23 1.416(5) . ? C22 C27 1.422(5) . ? C23 C24 1.376(5) . ? C23 H23A 0.9500 . ? C24 C25 1.376(6) . ? C24 H24A 0.9500 . ? C25 C26 1.373(5) . ? C25 H25A 0.9500 . ? C26 C27 1.398(5) . ? C26 H26A 0.9500 . ? C27 C28 1.447(5) . ? C28 H28A 0.9500 . ? C29 C31 1.509(5) . ? C29 C30 1.511(5) . ? C29 H29A 1.0000 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C36 1.380(5) . ? C31 C32 1.419(6) . ? C32 C33 1.379(5) . ? C32 H32A 0.9500 . ? C33 C34 1.393(6) . ? C33 H33A 0.9500 . ? C34 C35 1.360(6) . ? C34 H34A 0.9500 . ? C35 C36 1.398(5) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C37 C38 1.381(5) . ? C37 H37A 0.9500 . ? C38 C39 1.379(4) . ? C38 H38A 0.9500 . ? C39 C38 1.379(4) 2_757 ? C39 C40 1.479(6) . ? C40 C41 1.392(4) . ? C40 C41 1.392(4) 2_757 ? C41 C42 1.384(5) . ? C41 H41A 0.9500 . ? C42 H42A 0.9500 . ? N7 C43 1.129(5) . ? C43 C44 1.462(6) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? N8 C45 1.128(5) . ? C45 C46 1.457(5) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 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 O1 Fe1 O1 179.52(14) 2_758 . ? O1 Fe1 N1 86.55(8) 2_758 2_758 ? O1 Fe1 N1 93.46(8) . 2_758 ? O1 Fe1 N1 93.46(8) 2_758 . ? O1 Fe1 N1 86.55(8) . . ? N1 Fe1 N1 177.50(16) 2_758 . ? O1 Fe1 N2 90.24(7) 2_758 . ? O1 Fe1 N2 90.24(7) . . ? N1 Fe1 N2 88.75(8) 2_758 . ? N1 Fe1 N2 88.75(8) . . ? O1 Fe1 N3 89.76(7) 2_758 1_565 ? O1 Fe1 N3 89.76(7) . 1_565 ? N1 Fe1 N3 91.25(8) 2_758 1_565 ? N1 Fe1 N3 91.25(8) . 1_565 ? N2 Fe1 N3 180.000(3) . 1_565 ? C1 O1 Fe1 133.51(19) . . ? O1 C1 C2 119.9(3) . . ? O1 C1 C6 123.6(3) . . ? C2 C1 C6 116.5(3) . . ? C7 N1 C8 116.3(2) . . ? C7 N1 Fe1 125.2(2) . . ? C8 N1 Fe1 118.54(18) . . ? C3 C2 C1 122.8(3) . . ? C3 C2 H2A 118.6 . . ? C1 C2 H2A 118.6 . . ? C16 N2 C16 116.4(4) . 2_758 ? C16 N2 Fe1 121.8(2) . . ? C16 N2 Fe1 121.8(2) 2_758 . ? C2 C3 C4 120.4(3) . . ? C2 C3 H3A 119.8 . . ? C4 C3 H3A 119.8 . . ? C21 N3 C21 116.8(4) 2_758 . ? C21 N3 Fe1 121.6(2) 2_758 1_545 ? C21 N3 Fe1 121.6(2) . 1_545 ? C5 C4 C3 118.4(3) . . ? C5 C4 H4A 120.8 . . ? C3 C4 H4A 120.8 . . ? C4 C5 C6 122.6(3) . . ? C4 C5 H5A 118.7 . . ? C6 C5 H5A 118.7 . . ? C5 C6 C1 119.3(3) . . ? C5 C6 C7 117.3(3) . . ? C1 C6 C7 123.4(3) . . ? N1 C7 C6 127.4(3) . . ? N1 C7 H7A 116.3 . . ? C6 C7 H7A 116.3 . . ? N1 C8 C10 113.7(3) . . ? N1 C8 C9 109.4(3) . . ? C10 C8 C9 114.6(3) . . ? N1 C8 H8A 106.1 . . ? C10 C8 H8A 106.1 . . ? C9 C8 H8A 106.1 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C15 C10 C11 117.5(4) . . ? C15 C10 C8 121.9(4) . . ? C11 C10 C8 120.5(3) . . ? C12 C11 C10 121.1(3) . . ? C12 C11 H11A 119.5 . . ? C10 C11 H11A 119.5 . . ? C13 C12 C11 120.5(4) . . ? C13 C12 H12A 119.8 . . ? C11 C12 H12A 119.8 . . ? C14 C13 C12 118.6(4) . . ? C14 C13 H13A 120.7 . . ? C12 C13 H13A 120.7 . . ? C13 C14 C15 120.4(4) . . ? C13 C14 H14A 119.8 . . ? C15 C14 H14A 119.8 . . ? C10 C15 C14 121.9(4) . . ? C10 C15 H15A 119.0 . . ? C14 C15 H15A 119.0 . . ? N2 C16 C17 124.1(4) . . ? N2 C16 H16A 118.0 . . ? C17 C16 H16A 118.0 . . ? C16 C17 C18 119.0(4) . . ? C16 C17 H17A 120.5 . . ? C18 C17 H17A 120.5 . . ? C17 C18 C17 117.4(5) 2_758 . ? C17 C18 C19 121.3(2) 2_758 . ? C17 C18 C19 121.3(2) . . ? C20 C19 C20 116.4(4) . 2_758 ? C20 C19 C18 121.8(2) . . ? C20 C19 C18 121.8(2) 2_758 . ? C21 C20 C19 120.2(3) . . ? C21 C20 H20A 119.9 . . ? C19 C20 H20A 119.9 . . ? N3 C21 C20 123.2(3) . . ? N3 C21 H21A 118.4 . . ? C20 C21 H21A 118.4 . . ? O2 Fe2 O2 177.98(15) 2_757 . ? O2 Fe2 N4 86.54(9) 2_757 2_757 ? O2 Fe2 N4 93.59(9) . 2_757 ? O2 Fe2 N4 93.59(9) 2_757 . ? O2 Fe2 N4 86.54(9) . . ? N4 Fe2 N4 172.61(16) 2_757 . ? O2 Fe2 N6 88.99(8) 2_757 1_545 ? O2 Fe2 N6 88.99(8) . 1_545 ? N4 Fe2 N6 93.69(8) 2_757 1_545 ? N4 Fe2 N6 93.69(8) . 1_545 ? O2 Fe2 N5 91.01(7) 2_757 . ? O2 Fe2 N5 91.01(8) . . ? N4 Fe2 N5 86.31(8) 2_757 . ? N4 Fe2 N5 86.31(8) . . ? N6 Fe2 N5 180.000(2) 1_545 . ? C22 O2 Fe2 133.7(2) . . ? C28 N4 C29 118.7(3) . . ? C28 N4 Fe2 125.1(2) . . ? C29 N4 Fe2 116.1(2) . . ? C37 N5 C37 117.0(5) . 2_757 ? C37 N5 Fe2 121.5(2) . . ? C37 N5 Fe2 121.5(2) 2_757 . ? C42 N6 C42 116.9(4) . 2_757 ? C42 N6 Fe2 121.5(2) . 1_565 ? C42 N6 Fe2 121.5(2) 2_757 1_565 ? O2 C22 C23 120.2(3) . . ? O2 C22 C27 122.8(3) . . ? C23 C22 C27 117.1(3) . . ? C24 C23 C22 122.1(3) . . ? C24 C23 H23A 119.0 . . ? C22 C23 H23A 119.0 . . ? C25 C24 C23 120.3(4) . . ? C25 C24 H24A 119.9 . . ? C23 C24 H24A 119.9 . . ? C26 C25 C24 119.2(3) . . ? C26 C25 H25A 120.4 . . ? C24 C25 H25A 120.4 . . ? C25 C26 C27 122.5(4) . . ? C25 C26 H26A 118.8 . . ? C27 C26 H26A 118.8 . . ? C26 C27 C22 118.8(3) . . ? C26 C27 C28 117.0(3) . . ? C22 C27 C28 124.2(3) . . ? N4 C28 C27 127.3(3) . . ? N4 C28 H28A 116.3 . . ? C27 C28 H28A 116.3 . . ? N4 C29 C31 112.8(3) . . ? N4 C29 C30 108.3(3) . . ? C31 C29 C30 115.4(3) . . ? N4 C29 H29A 106.6 . . ? C31 C29 H29A 106.6 . . ? C30 C29 H29A 106.6 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C36 C31 C32 117.6(3) . . ? C36 C31 C29 123.6(4) . . ? C32 C31 C29 118.8(3) . . ? C33 C32 C31 120.7(4) . . ? C33 C32 H32A 119.6 . . ? C31 C32 H32A 119.6 . . ? C32 C33 C34 120.1(4) . . ? C32 C33 H33A 119.9 . . ? C34 C33 H33A 119.9 . . ? C35 C34 C33 119.8(4) . . ? C35 C34 H34A 120.1 . . ? C33 C34 H34A 120.1 . . ? C34 C35 C36 120.6(4) . . ? C34 C35 H35A 119.7 . . ? C36 C35 H35A 119.7 . . ? C31 C36 C35 121.2(4) . . ? C31 C36 H36A 119.4 . . ? C35 C36 H36A 119.4 . . ? N5 C37 C38 122.9(4) . . ? N5 C37 H37A 118.5 . . ? C38 C37 H37A 118.5 . . ? C39 C38 C37 120.7(4) . . ? C39 C38 H38A 119.6 . . ? C37 C38 H38A 119.6 . . ? C38 C39 C38 115.6(5) 2_757 . ? C38 C39 C40 122.2(2) 2_757 . ? C38 C39 C40 122.2(2) . . ? C41 C40 C41 117.1(4) . 2_757 ? C41 C40 C39 121.4(2) . . ? C41 C40 C39 121.4(2) 2_757 . ? C42 C41 C40 119.5(3) . . ? C42 C41 H41A 120.3 . . ? C40 C41 H41A 120.3 . . ? N6 C42 C41 123.5(3) . . ? N6 C42 H42A 118.2 . . ? C41 C42 H42A 118.2 . . ? N7 C43 C44 177.6(5) . . ? 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 . . ? N8 C45 C46 178.0(5) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 35.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.391 _refine_diff_density_min -0.208 _refine_diff_density_rms 0.045 #===END data_ll5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C130.50 H150.75 Fe3 N14.25 O6' _chemical_formula_weight 2182.45 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 C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 25.4871(8) _cell_length_b 21.9537(8) _cell_length_c 24.8107(11) _cell_angle_alpha 90.00 _cell_angle_beta 116.882(5) _cell_angle_gamma 90.00 _cell_volume 12382.3(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 19364 _cell_measurement_theta_min 2.92 _cell_measurement_theta_max 32.78 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.171 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4638 _exptl_absorpt_coefficient_mu 0.405 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.92 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'ABSPACK(CrysAlis, Oxford Diffraction)' _exptl_special_details ; The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cobra. The data collection nominally covered over a hemisphere of Reciprocal space, by a combination of four sets of exposures with different \f angles for the crystal; each 75 s exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.5 cm. Crystal decay was found to be negligible by by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms; H-atoms were given isotropic displacement parameter equal to 1.2 (or 1.5 for methyl H-atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. The poor quality crystals were weakly diffracting. There is a pseudo centre of inversion that relates nearly 80% of the atoms of the two polymeric chains with only variation around the chiral centre. This leads to some high elements in the correlation matrix. Many restraints were needed to make the thermal parameters of many of the atoms chemically sensible. There are three solvent acetonitriles which were refined at 75% occupancy. All the iron atoms and the nitrogens of the bridging pyrazine lie on two fold axes. The atoms of the tertiary butyl groups also exhibited large thermal motion which are responsible for the A and B alerts in the cif checker. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 10.2833 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 74329 _diffrn_reflns_av_R_equivalents 0.1277 _diffrn_reflns_av_sigmaI/netI 0.5876 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 32.87 _reflns_number_total 40956 _reflns_number_gt 8360 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0369P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881, 19364 Friedel pairs' _refine_ls_abs_structure_Flack 0.02(2) _chemical_absolute_configuration rmad _refine_ls_number_reflns 40956 _refine_ls_number_parameters 1430 _refine_ls_number_restraints 1818 _refine_ls_R_factor_all 0.3046 _refine_ls_R_factor_gt 0.0740 _refine_ls_wR_factor_ref 0.1691 _refine_ls_wR_factor_gt 0.1272 _refine_ls_goodness_of_fit_ref 0.693 _refine_ls_restrained_S_all 0.695 _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 N1 N 1.5000 0.9398(4) 0.5000 0.0271(18) Uani 1 2 d SU . . C1 C 1.5495(3) 0.9715(4) 0.5260(4) 0.0279(15) Uani 1 1 d U . . H1A H 1.5860 0.9504 0.5442 0.034 Uiso 1 1 calc R . . C2 C 1.5497(3) 1.0339(4) 0.5272(4) 0.0302(14) Uani 1 1 d U . . H2A H 1.5860 1.0549 0.5479 0.036 Uiso 1 1 calc R . . N2 N 1.5000 1.0658(4) 0.5000 0.0263(15) Uani 1 2 d SU . . Fe1 Fe 1.5000 1.16958(7) 0.5000 0.0249(5) Uani 1 2 d SU . . O1 O 1.58427(19) 1.1697(2) 0.5619(3) 0.0232(11) Uani 1 1 d U . . C3 C 1.6112(3) 1.1642(4) 0.6181(4) 0.0230(11) Uani 1 1 d U . . C4 C 1.6750(3) 1.1613(3) 0.6489(4) 0.0264(14) Uani 1 1 d U . . H4A H 1.6962 1.1642 0.6259 0.032 Uiso 1 1 calc R . . C5 C 1.7053(3) 1.1546(3) 0.7101(4) 0.0300(13) Uani 1 1 d U . . H5A H 1.7470 1.1518 0.7276 0.036 Uiso 1 1 calc R . . C6 C 1.6785(3) 1.1515(4) 0.7487(4) 0.0391(14) Uani 1 1 d U . . C7 C 1.6178(3) 1.1516(3) 0.7229(4) 0.0313(14) Uani 1 1 d U . . H7A H 1.5978 1.1478 0.7471 0.038 Uiso 1 1 calc R . . C8 C 1.5835(3) 1.1582(4) 0.6540(4) 0.0252(12) Uani 1 1 d U . . C9 C 1.5215(3) 1.1584(3) 0.6345(4) 0.0265(14) Uani 1 1 d U . . H9A H 1.5101 1.1528 0.6657 0.032 Uiso 1 1 calc R . . N3 N 1.4811(2) 1.1647(3) 0.5839(3) 0.0241(11) Uani 1 1 d U . . C10 C 1.4210(3) 1.1669(4) 0.5809(4) 0.0250(12) Uani 1 1 d U . . H10A H 1.4256 1.1598 0.6227 0.030 Uiso 1 1 calc R . . C11 C 1.3800(3) 1.1167(3) 0.5396(3) 0.0313(16) Uani 1 1 d U . . H11A H 1.3989 1.0768 0.5526 0.047 Uiso 1 1 calc R . . H11B H 1.3724 1.1242 0.4977 0.047 Uiso 1 1 calc R . . H11C H 1.3427 1.1171 0.5421 0.047 Uiso 1 1 calc R . . C12 C 1.3957(3) 1.2300(4) 0.5617(4) 0.0222(14) Uani 1 1 d U . . C13 C 1.3388(3) 1.2452(4) 0.5210(4) 0.0242(16) Uani 1 1 d U . . H13A H 1.3134 1.2138 0.4968 0.029 Uiso 1 1 calc R . . C14 C 1.3174(3) 1.3034(4) 0.5140(4) 0.0263(16) Uani 1 1 d U . . H14A H 1.2775 1.3116 0.4867 0.032 Uiso 1 1 calc R . . C15 C 1.3555(3) 1.3514(4) 0.5482(4) 0.0305(17) Uani 1 1 d U . . H15A H 1.3409 1.3920 0.5421 0.037 Uiso 1 1 calc R . . C16 C 1.4129(3) 1.3407(4) 0.5898(4) 0.0335(18) Uani 1 1 d U . . H16A H 1.4387 1.3728 0.6118 0.040 Uiso 1 1 calc R . . C17 C 1.4316(3) 1.2778(4) 0.5980(4) 0.0323(18) Uani 1 1 d U . . H17A H 1.4696 1.2681 0.6291 0.039 Uiso 1 1 calc R . . C18 C 1.7105(3) 1.1470(5) 0.8188(4) 0.0507(12) Uani 1 1 d U . . C19 C 1.6951(3) 1.2054(4) 0.8461(5) 0.0518(13) Uani 1 1 d U . . H19A H 1.7104 1.2005 0.8899 0.078 Uiso 1 1 calc R . . H19B H 1.6523 1.2105 0.8277 0.078 Uiso 1 1 calc R . . H19C H 1.7129 1.2414 0.8377 0.078 Uiso 1 1 calc R . . C20 C 1.6892(3) 1.0974(4) 0.8410(4) 0.0502(13) Uani 1 1 d U . . H20A H 1.7069 1.0994 0.8852 0.075 Uiso 1 1 calc R . . H20B H 1.6999 1.0588 0.8288 0.075 Uiso 1 1 calc R . . H20C H 1.6463 1.1001 0.8241 0.075 Uiso 1 1 calc R . . C21 C 1.7755(3) 1.1450(4) 0.8434(4) 0.0502(13) Uani 1 1 d U . . H21A H 1.7937 1.1488 0.8875 0.075 Uiso 1 1 calc R . . H21B H 1.7886 1.1788 0.8265 0.075 Uiso 1 1 calc R . . H21C H 1.7872 1.1063 0.8324 0.075 Uiso 1 1 calc R . . N4 N 1.5000 1.2741(4) 0.5000 0.0166(14) Uani 1 2 d SU . . C22 C 1.5478(3) 1.3058(3) 0.5251(4) 0.0167(13) Uani 1 1 d U . . H22A H 1.5841 1.2847 0.5457 0.020 Uiso 1 1 calc R . . C23 C 1.5490(3) 1.3659(4) 0.5238(4) 0.0162(13) Uani 1 1 d U . . H23A H 1.5858 1.3863 0.5404 0.019 Uiso 1 1 calc R . . N5 N 1.5000 1.3983(4) 0.5000 0.0181(14) Uani 1 2 d SU . . Fe2 Fe 1.5000 1.50410(7) 0.5000 0.0143(4) Uani 1 2 d SU . . O2 O 1.41358(16) 1.5026(2) 0.4734(2) 0.0149(9) Uani 1 1 d U . . C24 C 1.3831(2) 1.5036(3) 0.5042(3) 0.0131(10) Uani 1 1 d U . . C25 C 1.3204(2) 1.5008(3) 0.4719(3) 0.0173(12) Uani 1 1 d U . . H25A H 1.3019 1.4999 0.4290 0.021 Uiso 1 1 calc R . . C26 C 1.2857(2) 1.4993(3) 0.5027(3) 0.0179(11) Uani 1 1 d U . . H26A H 1.2441 1.4981 0.4798 0.021 Uiso 1 1 calc R . . C27 C 1.3097(2) 1.4994(3) 0.5644(3) 0.0200(11) Uani 1 1 d U . . C28 C 1.3694(2) 1.5052(3) 0.5951(3) 0.0142(11) Uani 1 1 d U . . H28A H 1.3870 1.5078 0.6379 0.017 Uiso 1 1 calc R . . C29 C 1.4057(3) 1.5075(3) 0.5669(3) 0.0150(11) Uani 1 1 d U . . C30 C 1.4704(2) 1.5137(3) 0.6079(3) 0.0171(12) Uani 1 1 d U . . H30A H 1.4819 1.5201 0.6497 0.021 Uiso 1 1 calc R . . N6 N 1.5109(2) 1.5112(3) 0.5918(3) 0.0164(10) Uani 1 1 d U . . C31 C 1.5726(2) 1.5181(3) 0.6404(3) 0.0173(12) Uani 1 1 d U . . H31A H 1.5958 1.5339 0.6200 0.021 Uiso 1 1 calc R . . C32 C 1.5974(2) 1.4555(3) 0.6641(3) 0.0210(14) Uani 1 1 d U . . H32A H 1.5944 1.4298 0.6306 0.032 Uiso 1 1 calc R . . H32B H 1.5750 1.4369 0.6832 0.032 Uiso 1 1 calc R . . H32C H 1.6387 1.4592 0.6940 0.032 Uiso 1 1 calc R . . C33 C 1.5788(3) 1.5654(3) 0.6877(4) 0.0186(12) Uani 1 1 d U . . C34 C 1.5915(2) 1.5478(3) 0.7460(3) 0.0244(13) Uani 1 1 d U . . H34A H 1.5940 1.5057 0.7557 0.029 Uiso 1 1 calc R . . C35 C 1.6006(2) 1.5919(3) 0.7917(3) 0.0251(13) Uani 1 1 d U . . H35A H 1.6093 1.5798 0.8316 0.030 Uiso 1 1 calc R . . C36 C 1.5965(2) 1.6539(3) 0.7757(3) 0.0299(13) Uani 1 1 d U . . H36A H 1.6029 1.6846 0.8050 0.036 Uiso 1 1 calc R . . C37 C 1.5833(3) 1.6693(3) 0.7180(3) 0.0273(13) Uani 1 1 d U . . H37A H 1.5799 1.7110 0.7070 0.033 Uiso 1 1 calc R . . C38 C 1.5744(2) 1.6245(3) 0.6742(3) 0.0242(13) Uani 1 1 d U . . H38A H 1.5651 1.6367 0.6341 0.029 Uiso 1 1 calc R . . C39 C 1.2721(3) 1.4965(4) 0.5987(3) 0.0338(9) Uani 1 1 d U . . C40 C 1.2091(2) 1.4827(3) 0.5584(3) 0.0363(11) Uani 1 1 d U . . H40A H 1.2062 1.4445 0.5367 0.054 Uiso 1 1 calc R . . H40B H 1.1918 1.5159 0.5292 0.054 Uiso 1 1 calc R . . H40C H 1.1879 1.4786 0.5827 0.054 Uiso 1 1 calc R . . C41 C 1.2776(3) 1.5610(4) 0.6299(4) 0.0365(11) Uani 1 1 d U . . H41A H 1.3183 1.5755 0.6462 0.055 Uiso 1 1 calc R . . H41B H 1.2666 1.5570 0.6629 0.055 Uiso 1 1 calc R . . H41C H 1.2513 1.5902 0.6001 0.055 Uiso 1 1 calc R . . C42 C 1.2976(3) 1.4475(3) 0.6486(4) 0.0348(11) Uani 1 1 d U . . H42A H 1.3052 1.4101 0.6317 0.052 Uiso 1 1 calc R . . H42B H 1.2693 1.4390 0.6643 0.052 Uiso 1 1 calc R . . H42C H 1.3344 1.4623 0.6815 0.052 Uiso 1 1 calc R . . N7 N 1.5000 1.6070(4) 0.5000 0.0130(14) Uani 1 2 d SU . . C43 C 1.5486(3) 1.6403(3) 0.5172(3) 0.0123(12) Uani 1 1 d U . . H43A H 1.5850 1.6193 0.5307 0.015 Uiso 1 1 calc R . . C44 C 1.5500(3) 1.7047(3) 0.5167(3) 0.0135(12) Uani 1 1 d U . . H44A H 1.5862 1.7254 0.5282 0.016 Uiso 1 1 calc R . . N8 N 1.5000 1.7367(4) 0.5000 0.0126(14) Uani 1 2 d SU . . Fe3 Fe 1.5000 1.83667(7) 0.5000 0.0196(4) Uani 1 2 d SU . . O3 O 1.5861(2) 1.8369(3) 0.5570(3) 0.0245(11) Uani 1 1 d U . . C45 C 1.6151(3) 1.8380(4) 0.6162(4) 0.0252(12) Uani 1 1 d U . . C46 C 1.6774(3) 1.8403(4) 0.6417(4) 0.0273(15) Uani 1 1 d U . . H46A H 1.6964 1.8414 0.6164 0.033 Uiso 1 1 calc R . . C47 C 1.7101(3) 1.8411(4) 0.7039(4) 0.0296(15) Uani 1 1 d U . . H47A H 1.7517 1.8422 0.7201 0.036 Uiso 1 1 calc R . . C48 C 1.6854(3) 1.8402(4) 0.7448(4) 0.0324(14) Uani 1 1 d U . . C49 C 1.6223(3) 1.8418(3) 0.7126(4) 0.0291(14) Uani 1 1 d U . . H49A H 1.6028 1.8441 0.7374 0.035 Uiso 1 1 calc R . . C50 C 1.5880(3) 1.8407(4) 0.6553(4) 0.0267(13) Uani 1 1 d U . . C51 C 1.5249(3) 1.8448(3) 0.6358(4) 0.0274(14) Uani 1 1 d U . . H51A H 1.5120 1.8509 0.6658 0.033 Uiso 1 1 calc R . . N9 N 1.4847(2) 1.8405(3) 0.5788(3) 0.0275(12) Uani 1 1 d U . . C52 C 1.4223(3) 1.8465(4) 0.5682(4) 0.0277(13) Uani 1 1 d U . . H52A H 1.4006 1.8689 0.5292 0.033 Uiso 1 1 calc R . . C53 C 1.4117(3) 1.8808(3) 0.6158(4) 0.0318(16) Uani 1 1 d U . . H53A H 1.4219 1.9238 0.6158 0.048 Uiso 1 1 calc R . . H53B H 1.4361 1.8632 0.6557 0.048 Uiso 1 1 calc R . . H53C H 1.3701 1.8774 0.6066 0.048 Uiso 1 1 calc R . . C54 C 1.3956(3) 1.7816(3) 0.5590(4) 0.0239(14) Uani 1 1 d U . . C55 C 1.4227(3) 1.7350(3) 0.5962(4) 0.0246(15) Uani 1 1 d U . . H55A H 1.4598 1.7413 0.6302 0.029 Uiso 1 1 calc R . . C56 C 1.3967(3) 1.6768(4) 0.5855(4) 0.0317(17) Uani 1 1 d U . . H56A H 1.4177 1.6432 0.6097 0.038 Uiso 1 1 calc R . . C57 C 1.3413(3) 1.6693(4) 0.5402(4) 0.0292(16) Uani 1 1 d U . . H57A H 1.3225 1.6309 0.5350 0.035 Uiso 1 1 calc R . . C58 C 1.3126(3) 1.7159(4) 0.5023(4) 0.0305(17) Uani 1 1 d U . . H58A H 1.2753 1.7095 0.4687 0.037 Uiso 1 1 calc R . . C59 C 1.3389(3) 1.7738(4) 0.5137(4) 0.0271(16) Uani 1 1 d U . . H59A H 1.3177 1.8077 0.4901 0.033 Uiso 1 1 calc R . . C60 C 1.7199(3) 1.8384(4) 0.8140(4) 0.0442(12) Uani 1 1 d U . . C61 C 1.7091(3) 1.8973(4) 0.8382(4) 0.0450(13) Uani 1 1 d U . . H61A H 1.7252 1.8946 0.8822 0.067 Uiso 1 1 calc R . . H61B H 1.6667 1.9051 0.8203 0.067 Uiso 1 1 calc R . . H61C H 1.7284 1.9307 0.8277 0.067 Uiso 1 1 calc R . . C62 C 1.6984(3) 1.7838(3) 0.8355(4) 0.0440(13) Uani 1 1 d U . . H62A H 1.7206 1.7805 0.8795 0.066 Uiso 1 1 calc R . . H62B H 1.7041 1.7468 0.8167 0.066 Uiso 1 1 calc R . . H62C H 1.6565 1.7888 0.8242 0.066 Uiso 1 1 calc R . . C63 C 1.7844(3) 1.8314(4) 0.8320(4) 0.0450(13) Uani 1 1 d U . . H63A H 1.8066 1.8321 0.8762 0.068 Uiso 1 1 calc R . . H63B H 1.7975 1.8649 0.8149 0.068 Uiso 1 1 calc R . . H63C H 1.7911 1.7925 0.8167 0.068 Uiso 1 1 calc R . . N10 N 1.5000 -0.0760(4) 1.0000 0.0262(18) Uani 1 2 d SU . . C64 C 1.4549(3) -0.0420(4) 0.9623(4) 0.0296(14) Uani 1 1 d U . . H64A H 1.4202 -0.0624 0.9348 0.036 Uiso 1 1 calc R . . C65 C 1.4553(3) 0.0203(3) 0.9606(4) 0.0273(13) Uani 1 1 d U . . H65A H 1.4228 0.0415 0.9306 0.033 Uiso 1 1 calc R . . N11 N 1.5000 0.0504(4) 1.0000 0.0229(15) Uani 1 2 d SU . . Fe4 Fe 1.5000 0.15564(7) 1.0000 0.0190(4) Uani 1 2 d SU . . O4 O 1.41408(18) 0.1566(2) 0.9466(2) 0.0176(11) Uani 1 1 d U . . C66 C 1.3803(3) 0.1526(3) 0.8883(4) 0.0149(11) Uani 1 1 d U . . C67 C 1.3197(3) 0.1542(3) 0.8664(3) 0.0182(13) Uani 1 1 d U . . H67A H 1.3034 0.1594 0.8938 0.022 Uiso 1 1 calc R . . C68 C 1.2827(3) 0.1483(3) 0.8055(3) 0.0207(13) Uani 1 1 d U . . H68A H 1.2415 0.1518 0.7921 0.025 Uiso 1 1 calc R . . C69 C 1.3034(3) 0.1370(3) 0.7614(3) 0.0222(12) Uani 1 1 d U . . C70 C 1.3620(2) 0.1382(3) 0.7824(3) 0.0186(12) Uani 1 1 d U . . H70A H 1.3781 0.1349 0.7547 0.022 Uiso 1 1 calc R . . C71 C 1.4024(3) 0.1447(3) 0.8481(3) 0.0173(11) Uani 1 1 d U . . C72 C 1.4642(3) 0.1427(3) 0.8616(4) 0.0196(12) Uani 1 1 d U . . H72A H 1.4726 0.1358 0.8285 0.024 Uiso 1 1 calc R . . N12 N 1.5079(2) 0.1493(3) 0.9130(3) 0.0206(11) Uani 1 1 d U . . C73 C 1.5673(2) 0.1478(3) 0.9107(4) 0.0231(13) Uani 1 1 d U . . H73A H 1.5586 0.1420 0.8675 0.028 Uiso 1 1 calc R . . C74 C 1.6026(3) 0.0901(3) 0.9468(4) 0.0300(19) Uani 1 1 d U . . H74A H 1.5768 0.0543 0.9340 0.045 Uiso 1 1 calc R . . H74B H 1.6165 0.0968 0.9902 0.045 Uiso 1 1 calc R . . H74C H 1.6363 0.0833 0.9386 0.045 Uiso 1 1 calc R . . C75 C 1.5984(3) 0.2070(4) 0.9309(4) 0.0248(15) Uani 1 1 d U . . C76 C 1.5672(3) 0.2612(4) 0.9025(4) 0.0304(14) Uani 1 1 d U . . H76A H 1.5268 0.2589 0.8744 0.036 Uiso 1 1 calc R . . C77 C 1.5948(3) 0.3165(4) 0.9151(4) 0.0322(15) Uani 1 1 d U . . H77A H 1.5744 0.3511 0.8922 0.039 Uiso 1 1 calc R . . C78 C 1.6529(3) 0.3236(4) 0.9613(4) 0.0306(17) Uani 1 1 d U . . H78A H 1.6710 0.3624 0.9728 0.037 Uiso 1 1 calc R . . C79 C 1.6817(3) 0.2707(4) 0.9887(4) 0.0300(17) Uani 1 1 d U . . H79A H 1.7218 0.2732 1.0178 0.036 Uiso 1 1 calc R . . C80 C 1.6552(3) 0.2144(4) 0.9761(4) 0.0280(16) Uani 1 1 d U . . H80A H 1.6763 0.1800 0.9988 0.034 Uiso 1 1 calc R . . C81 C 1.2614(3) 0.1260(3) 0.6940(3) 0.0246(13) Uani 1 1 d U . . C82 C 1.2226(3) 0.0702(3) 0.6892(3) 0.0306(15) Uani 1 1 d U . . H82A H 1.2473 0.0338 0.7037 0.046 Uiso 1 1 calc R . . H82B H 1.1937 0.0643 0.6469 0.046 Uiso 1 1 calc R . . H82C H 1.2020 0.0771 0.7138 0.046 Uiso 1 1 calc R . . C83 C 1.2192(3) 0.1843(3) 0.6690(4) 0.0364(17) Uani 1 1 d U . . H83A H 1.1914 0.1779 0.6265 0.055 Uiso 1 1 calc R . . H83B H 1.2430 0.2206 0.6727 0.055 Uiso 1 1 calc R . . H83C H 1.1974 0.1901 0.6926 0.055 Uiso 1 1 calc R . . C84 C 1.2913(3) 0.1180(4) 0.6554(4) 0.0351(18) Uani 1 1 d U . . H84A H 1.3174 0.0825 0.6692 0.053 Uiso 1 1 calc R . . H84B H 1.3145 0.1545 0.6579 0.053 Uiso 1 1 calc R . . H84C H 1.2619 0.1117 0.6134 0.053 Uiso 1 1 calc R . . N13 N 1.5000 0.2596(4) 1.0000 0.0211(18) Uani 1 2 d SU . . C85 C 1.4503(3) 0.2934(3) 0.9729(4) 0.0193(14) Uani 1 1 d U . . H85A H 1.4138 0.2728 0.9521 0.023 Uiso 1 1 calc R . . C86 C 1.4499(3) 0.3549(3) 0.9741(4) 0.0155(13) Uani 1 1 d U . . H86A H 1.4135 0.3760 0.9561 0.019 Uiso 1 1 calc R . . N14 N 1.5000 0.3865(4) 1.0000 0.0187(14) Uani 1 2 d SU . . Fe5 Fe 1.5000 0.49132(7) 1.0000 0.0143(4) Uani 1 2 d SU . . O5 O 1.58742(16) 0.4921(2) 1.0311(2) 0.0152(10) Uani 1 1 d U . . C87 C 1.6214(2) 0.4886(3) 1.0050(3) 0.0162(10) Uani 1 1 d U . . C88 C 1.6829(2) 0.4928(3) 1.0388(3) 0.0171(12) Uani 1 1 d U . . H88A H 1.6992 0.5006 1.0810 0.021 Uiso 1 1 calc R . . C89 C 1.7195(3) 0.4861(3) 1.0134(3) 0.0205(12) Uani 1 1 d U . . H89A H 1.7606 0.4889 1.0389 0.025 Uiso 1 1 calc R . . C90 C 1.7000(2) 0.4749(3) 0.9492(3) 0.0203(11) Uani 1 1 d U . . C91 C 1.6397(2) 0.4743(3) 0.9160(3) 0.0201(12) Uani 1 1 d U . . H91A H 1.6241 0.4681 0.8736 0.024 Uiso 1 1 calc R . . C92 C 1.5984(3) 0.4824(3) 0.9405(3) 0.0168(11) Uani 1 1 d U . . C93 C 1.5367(3) 0.4831(3) 0.8973(3) 0.0182(12) Uani 1 1 d U . . H93A H 1.5279 0.4781 0.8560 0.022 Uiso 1 1 calc R . . N15 N 1.4921(2) 0.4898(3) 0.9088(3) 0.0214(11) Uani 1 1 d U . . C94 C 1.4345(2) 0.4935(3) 0.8551(3) 0.0203(12) Uani 1 1 d U . . H94A H 1.4051 0.5006 0.8708 0.024 Uiso 1 1 calc R . . C95 C 1.4183(3) 0.4331(3) 0.8226(4) 0.031(2) Uani 1 1 d U . . H95A H 1.4219 0.4008 0.8514 0.046 Uiso 1 1 calc R . . H95B H 1.4447 0.4245 0.8047 0.046 Uiso 1 1 calc R . . H95C H 1.3776 0.4347 0.7907 0.046 Uiso 1 1 calc R . . C96 C 1.4295(2) 0.5472(3) 0.8157(3) 0.0207(12) Uani 1 1 d U . . C97 C 1.4059(2) 0.6016(3) 0.8260(3) 0.0244(13) Uani 1 1 d U . . H97A H 1.3917 0.6025 0.8554 0.029 Uiso 1 1 calc R . . C98 C 1.4035(2) 0.6536(3) 0.7936(3) 0.0282(13) Uani 1 1 d U . . H98A H 1.3866 0.6894 0.8005 0.034 Uiso 1 1 calc R . . C99 C 1.4251(2) 0.6552(3) 0.7508(3) 0.0241(12) Uani 1 1 d U . . H99A H 1.4240 0.6916 0.7295 0.029 Uiso 1 1 calc R . . C100 C 1.4486(2) 0.6007(3) 0.7405(3) 0.0244(13) Uani 1 1 d U . . H10B H 1.4632 0.5999 0.7115 0.029 Uiso 1 1 calc R . . C101 C 1.4504(2) 0.5471(3) 0.7734(3) 0.0235(12) Uani 1 1 d U . . H10C H 1.4663 0.5107 0.7661 0.028 Uiso 1 1 calc R . . C102 C 1.7406(3) 0.4674(3) 0.9223(3) 0.0274(13) Uani 1 1 d U . . C103 C 1.7137(3) 0.4384(4) 0.8630(4) 0.0355(18) Uani 1 1 d U . . H10D H 1.6793 0.4621 0.8356 0.053 Uiso 1 1 calc R . . H10E H 1.7013 0.3970 0.8668 0.053 Uiso 1 1 calc R . . H10F H 1.7423 0.4366 0.8468 0.053 Uiso 1 1 calc R . . C104 C 1.7951(3) 0.4318(3) 0.9650(3) 0.0346(18) Uani 1 1 d U . . H10G H 1.7832 0.3926 0.9749 0.052 Uiso 1 1 calc R . . H10H H 1.8168 0.4553 1.0022 0.052 Uiso 1 1 calc R . . H10I H 1.8204 0.4247 0.9454 0.052 Uiso 1 1 calc R . . C105 C 1.7621(3) 0.5305(3) 0.9127(4) 0.0372(16) Uani 1 1 d U . . H10J H 1.7281 0.5559 0.8878 0.056 Uiso 1 1 calc R . . H10K H 1.7869 0.5253 0.8922 0.056 Uiso 1 1 calc R . . H10L H 1.7849 0.5501 0.9519 0.056 Uiso 1 1 calc R . . N16 N 1.5000 0.5932(4) 1.0000 0.0152(14) Uani 1 2 d SU . . C106 C 1.4496(3) 0.6247(4) 0.9757(3) 0.0161(13) Uani 1 1 d U . . H10M H 1.4133 0.6031 0.9578 0.019 Uiso 1 1 calc R . . C107 C 1.4487(3) 0.6905(3) 0.9761(4) 0.0171(13) Uani 1 1 d U . . H10N H 1.4120 0.7112 0.9595 0.021 Uiso 1 1 calc R . . N17 N 1.5000 0.7239(4) 1.0000 0.0170(15) Uani 1 2 d SU . . Fe6 Fe 1.5000 0.82259(6) 1.0000 0.0174(4) Uani 1 2 d SU . . O6 O 1.4141(2) 0.8223(2) 0.9448(3) 0.0222(12) Uani 1 1 d U . . C108 C 1.3842(3) 0.8232(4) 0.8850(4) 0.0217(12) Uani 1 1 d U . . C109 C 1.3224(3) 0.8181(3) 0.8571(4) 0.0276(15) Uani 1 1 d U . . H10O H 1.3026 0.8122 0.8812 0.033 Uiso 1 1 calc R . . C110 C 1.2887(3) 0.8217(3) 0.7921(4) 0.0292(14) Uani 1 1 d U . . H11D H 1.2470 0.8193 0.7749 0.035 Uiso 1 1 calc R . . C111 C 1.3134(3) 0.8283(4) 0.7552(4) 0.0291(13) Uani 1 1 d U . . C112 C 1.3749(3) 0.8319(3) 0.7808(4) 0.0248(13) Uani 1 1 d U . . H11E H 1.3931 0.8365 0.7550 0.030 Uiso 1 1 calc R . . C113 C 1.4098(3) 0.8288(4) 0.8431(4) 0.0238(12) Uani 1 1 d U . . C114 C 1.4727(3) 0.8311(3) 0.8658(4) 0.0231(13) Uani 1 1 d U . . H11F H 1.4861 0.8359 0.8360 0.028 Uiso 1 1 calc R . . N18 N 1.5149(2) 0.8273(3) 0.9226(3) 0.0209(11) Uani 1 1 d U . . C115 C 1.5760(3) 0.8270(3) 0.9324(4) 0.0200(12) Uani 1 1 d U . . H11G H 1.6006 0.8451 0.9731 0.024 Uiso 1 1 calc R . . C116 C 1.5891(3) 0.8626(3) 0.8866(4) 0.0341(18) Uani 1 1 d U . . H11H H 1.5760 0.9048 0.8847 0.051 Uiso 1 1 calc R . . H11I H 1.5683 0.8437 0.8466 0.051 Uiso 1 1 calc R . . H11J H 1.6315 0.8619 0.8993 0.051 Uiso 1 1 calc R . . C117 C 1.5962(3) 0.7611(3) 0.9341(4) 0.0186(14) Uani 1 1 d U . . C118 C 1.5604(3) 0.7133(3) 0.9012(4) 0.0215(15) Uani 1 1 d U . . H11K H 1.5205 0.7212 0.8737 0.026 Uiso 1 1 calc R . . C119 C 1.5814(3) 0.6552(4) 0.9075(4) 0.0206(14) Uani 1 1 d U . . H11L H 1.5554 0.6237 0.8842 0.025 Uiso 1 1 calc R . . C120 C 1.6388(3) 0.6405(4) 0.9463(4) 0.0245(14) Uani 1 1 d U . . H12A H 1.6530 0.6000 0.9494 0.029 Uiso 1 1 calc R . . C121 C 1.6744(3) 0.6866(4) 0.9801(4) 0.0260(16) Uani 1 1 d U . . H12B H 1.7139 0.6774 1.0081 0.031 Uiso 1 1 calc R . . C122 C 1.6547(3) 0.7479(4) 0.9751(4) 0.0230(16) Uani 1 1 d U . . H12C H 1.6804 0.7791 0.9990 0.028 Uiso 1 1 calc R . . C123 C 1.2780(3) 0.8310(3) 0.6880(4) 0.0339(15) Uani 1 1 d U . . C124 C 1.2125(3) 0.8238(3) 0.6653(4) 0.0344(16) Uani 1 1 d U . . H12D H 1.1983 0.8544 0.6843 0.052 Uiso 1 1 calc R . . H12E H 1.2041 0.7830 0.6754 0.052 Uiso 1 1 calc R . . H12F H 1.1925 0.8293 0.6213 0.052 Uiso 1 1 calc R . . C125 C 1.2889(3) 0.8925(4) 0.6626(4) 0.0390(17) Uani 1 1 d U . . H12G H 1.2781 0.9266 0.6811 0.059 Uiso 1 1 calc R . . H12H H 1.2648 0.8936 0.6187 0.059 Uiso 1 1 calc R . . H12I H 1.3305 0.8957 0.6722 0.059 Uiso 1 1 calc R . . C126 C 1.2965(3) 0.7764(4) 0.6569(4) 0.0374(17) Uani 1 1 d U . . H12J H 1.3380 0.7807 0.6663 0.056 Uiso 1 1 calc R . . H12K H 1.2722 0.7779 0.6130 0.056 Uiso 1 1 calc R . . H12L H 1.2906 0.7373 0.6724 0.056 Uiso 1 1 calc R . . N300 N 1.4698(3) 0.2195(3) 0.7426(3) 0.0232(16) Uani 0.75 1 d PU . . C301 C 1.4318(3) 0.2476(4) 0.7306(4) 0.0214(18) Uani 0.75 1 d PU . . C302 C 1.37878(18) 0.2862(2) 0.7144(2) 0.034(2) Uani 0.75 1 d PU . . H30B H 1.3842 0.3253 0.6985 0.051 Uiso 0.75 1 calc PR . . H30C H 1.3731 0.2932 0.7504 0.051 Uiso 0.75 1 calc PR . . H30D H 1.3442 0.2655 0.6835 0.051 Uiso 0.75 1 calc PR . . N400 N 1.51266(18) 0.3967(2) 0.7505(2) 0.0305(18) Uani 0.75 1 d PRU . . C401 C 1.54592(18) 0.3617(2) 0.7560(2) 0.0263(19) Uani 0.75 1 d PRU . . C402 C 1.58580(18) 0.3106(2) 0.7593(2) 0.040(2) Uani 0.75 1 d PRU . . H40D H 1.6062 0.3207 0.7351 0.060 Uiso 0.75 1 calc PR . . H40E H 1.5626 0.2734 0.7434 0.060 Uiso 0.75 1 calc PR . . H40F H 1.6148 0.3042 0.8014 0.060 Uiso 0.75 1 calc PR . . N500 N 1.5185(3) 1.0050(4) 0.6485(4) 0.056(2) Uani 0.75 1 d PU . . C501 C 1.5683(4) 1.0021(6) 0.6684(5) 0.058(2) Uani 0.75 1 d PU . . C502 C 1.6360(3) 0.9998(5) 0.6861(5) 0.050(2) Uani 0.75 1 d PU . . H50A H 1.6586 0.9937 0.7298 0.075 Uiso 0.75 1 calc PR . . H50B H 1.6479 1.0382 0.6747 0.075 Uiso 0.75 1 calc PR . . H50C H 1.6437 0.9660 0.6648 0.075 Uiso 0.75 1 calc PR . . 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 N1 0.0273(19) 0.0255(19) 0.028(2) 0.000 0.0119(11) 0.000 C1 0.0276(16) 0.0257(16) 0.0290(17) 0.0002(9) 0.0115(10) 0.0008(9) C2 0.0298(16) 0.0274(16) 0.0309(17) -0.0002(10) 0.0116(10) 0.0000(9) N2 0.0264(17) 0.0240(16) 0.0272(18) 0.000 0.0110(10) 0.000 Fe1 0.0237(7) 0.0138(7) 0.0301(8) 0.000 0.0060(6) 0.000 O1 0.0224(12) 0.0220(14) 0.0238(13) 0.0005(9) 0.0094(9) 0.0007(9) C3 0.0231(13) 0.0204(14) 0.0239(13) 0.0004(9) 0.0093(9) -0.0002(9) C4 0.026(2) 0.019(3) 0.029(2) 0.000(3) 0.009(2) 0.003(2) C5 0.0294(15) 0.0278(16) 0.0299(15) 0.0003(10) 0.0108(10) 0.0008(9) C6 0.039(2) 0.037(3) 0.031(2) 0.010(2) 0.0070(19) -0.002(2) C7 0.035(2) 0.027(3) 0.029(2) 0.009(3) 0.011(2) 0.000(3) C8 0.0258(13) 0.0229(15) 0.0256(14) 0.0009(9) 0.0104(9) 0.0003(9) C9 0.026(2) 0.018(3) 0.033(3) 0.007(3) 0.011(2) 0.003(3) N3 0.0244(19) 0.013(2) 0.029(2) 0.000(2) 0.0069(18) -0.0010(19) C10 0.0248(14) 0.0245(15) 0.0254(15) -0.0007(9) 0.0111(9) 0.0010(9) C11 0.0314(17) 0.0301(17) 0.0317(18) 0.0001(10) 0.0137(11) -0.0001(10) C12 0.022(2) 0.019(2) 0.027(3) 0.005(2) 0.012(2) -0.0028(19) C13 0.021(2) 0.023(3) 0.026(3) 0.001(3) 0.008(2) -0.005(2) C14 0.021(3) 0.029(3) 0.028(3) 0.006(3) 0.010(3) 0.007(2) C15 0.035(3) 0.025(3) 0.028(4) 0.006(3) 0.011(3) 0.005(2) C16 0.036(3) 0.028(3) 0.029(4) -0.003(3) 0.007(3) -0.002(3) C17 0.027(3) 0.029(3) 0.029(3) 0.001(3) 0.003(3) 0.000(2) C18 0.047(2) 0.067(3) 0.034(2) 0.011(2) 0.0148(18) 0.002(2) C19 0.048(2) 0.068(3) 0.034(2) 0.010(2) 0.0146(19) 0.002(2) C20 0.047(2) 0.067(3) 0.033(2) 0.012(2) 0.0153(19) 0.002(2) C21 0.047(2) 0.068(3) 0.033(2) 0.010(2) 0.0156(19) 0.002(2) N4 0.0169(16) 0.0146(15) 0.0168(17) 0.000 0.0064(10) 0.000 C22 0.0169(15) 0.0149(15) 0.0180(16) -0.0003(9) 0.0076(10) 0.0018(9) C23 0.0165(15) 0.0147(15) 0.0166(16) 0.0001(9) 0.0069(9) -0.0011(9) N5 0.0188(16) 0.0161(15) 0.0185(17) 0.000 0.0076(10) 0.000 Fe2 0.0157(6) 0.0074(7) 0.0192(7) 0.000 0.0074(5) 0.000 O2 0.0152(11) 0.0140(13) 0.0150(12) 0.0008(9) 0.0064(8) -0.0007(9) C24 0.0135(12) 0.0111(13) 0.0137(13) -0.0001(9) 0.0052(9) -0.0005(9) C25 0.0176(19) 0.015(3) 0.015(2) 0.003(2) 0.0037(17) 0.000(2) C26 0.0165(13) 0.0170(14) 0.0192(14) 0.0004(9) 0.0073(9) 0.0002(9) C27 0.0192(18) 0.015(2) 0.025(2) -0.002(2) 0.0098(17) 0.004(2) C28 0.0147(12) 0.0126(14) 0.0148(13) -0.0006(9) 0.0062(9) 0.0001(9) C29 0.0178(18) 0.011(2) 0.015(2) -0.002(2) 0.0062(16) 0.000(2) C30 0.0174(13) 0.0156(15) 0.0164(14) 0.0001(9) 0.0060(9) -0.0002(9) N6 0.0212(19) 0.010(2) 0.015(2) 0.0038(18) 0.0057(17) -0.0027(19) C31 0.016(2) 0.017(2) 0.018(2) 0.001(2) 0.007(2) -0.001(2) C32 0.0207(16) 0.0207(16) 0.0208(17) -0.0011(10) 0.0087(10) 0.0005(9) C33 0.020(2) 0.020(2) 0.018(2) -0.003(2) 0.011(2) 0.000(2) C34 0.031(3) 0.019(2) 0.025(3) -0.002(2) 0.014(2) 0.002(2) C35 0.029(2) 0.026(2) 0.023(3) -0.003(2) 0.014(2) 0.001(2) C36 0.0308(15) 0.0293(15) 0.0294(15) -0.0018(9) 0.0134(10) 0.0003(9) C37 0.032(2) 0.022(2) 0.029(3) -0.003(2) 0.014(2) -0.002(2) C38 0.031(3) 0.021(2) 0.023(3) 0.000(2) 0.015(2) -0.001(2) C39 0.0334(13) 0.0378(15) 0.0368(15) 0.0020(13) 0.0217(12) 0.0002(12) C40 0.0353(12) 0.0386(13) 0.0375(13) 0.0018(9) 0.0186(9) -0.0004(9) C41 0.0365(17) 0.0400(18) 0.0386(18) 0.0003(16) 0.0219(16) 0.0023(16) C42 0.0337(16) 0.0391(18) 0.0371(18) 0.0026(16) 0.0209(15) -0.0008(16) N7 0.0140(15) 0.0114(15) 0.0129(16) 0.000 0.0054(10) 0.000 C43 0.0131(14) 0.0115(14) 0.0125(15) -0.0008(9) 0.0059(9) 0.0009(9) C44 0.0142(14) 0.0129(14) 0.0136(15) 0.0006(9) 0.0065(9) -0.0012(9) N8 0.0130(16) 0.0116(16) 0.0129(17) 0.000 0.0055(10) 0.000 Fe3 0.0166(6) 0.0098(7) 0.0277(8) 0.000 0.0060(6) 0.000 O3 0.0238(13) 0.0233(14) 0.0258(14) -0.0006(9) 0.0108(9) 0.0007(9) C45 0.0256(14) 0.0224(15) 0.0258(14) -0.0011(9) 0.0100(9) 0.0007(9) C46 0.030(2) 0.021(3) 0.029(3) -0.004(3) 0.012(2) 0.000(3) C47 0.027(3) 0.023(3) 0.033(3) -0.004(3) 0.009(2) -0.003(3) C48 0.036(2) 0.027(3) 0.030(2) -0.006(2) 0.011(2) -0.003(2) C49 0.036(2) 0.023(3) 0.032(3) 0.000(3) 0.018(2) -0.004(3) C50 0.030(2) 0.016(2) 0.030(2) -0.002(3) 0.0112(18) -0.002(2) C51 0.031(2) 0.017(3) 0.037(3) -0.008(3) 0.018(2) -0.005(3) N9 0.025(2) 0.017(3) 0.041(3) -0.006(2) 0.015(2) 0.000(2) C52 0.026(2) 0.022(3) 0.042(3) -0.004(3) 0.022(2) -0.002(2) C53 0.0318(18) 0.0312(18) 0.0332(18) -0.0020(10) 0.0153(11) -0.0004(10) C54 0.026(2) 0.014(2) 0.037(3) -0.005(2) 0.019(2) -0.001(2) C55 0.029(3) 0.023(3) 0.026(3) -0.005(2) 0.016(2) -0.004(2) C56 0.037(3) 0.023(3) 0.035(3) 0.005(3) 0.017(3) -0.004(2) C57 0.034(3) 0.024(3) 0.038(4) -0.004(3) 0.023(3) -0.010(2) C58 0.023(3) 0.030(3) 0.041(4) -0.007(3) 0.017(3) -0.005(2) C59 0.024(3) 0.020(3) 0.039(4) 0.001(3) 0.016(2) 0.002(2) C60 0.048(2) 0.043(2) 0.029(2) -0.005(2) 0.0071(18) -0.010(2) C61 0.049(2) 0.044(3) 0.029(2) -0.006(2) 0.007(2) -0.012(2) C62 0.049(2) 0.044(3) 0.029(2) -0.004(2) 0.008(2) -0.009(2) C63 0.049(2) 0.045(3) 0.028(2) -0.004(2) 0.006(2) -0.010(2) N10 0.0262(19) 0.0246(19) 0.027(2) 0.000 0.0111(11) 0.000 C64 0.0290(16) 0.0269(16) 0.0299(17) -0.0013(9) 0.0107(10) -0.0005(9) C65 0.0271(15) 0.0239(15) 0.0275(16) 0.0000(9) 0.0094(9) 0.0003(9) N11 0.0232(17) 0.0204(16) 0.0239(17) 0.000 0.0094(10) 0.000 Fe4 0.0182(6) 0.0103(7) 0.0246(8) 0.000 0.0062(6) 0.000 O4 0.0208(18) 0.012(2) 0.017(2) -0.005(2) 0.0057(17) 0.0007(16) C66 0.0158(13) 0.0122(14) 0.0155(13) -0.0006(9) 0.0060(9) 0.0001(9) C67 0.019(2) 0.014(3) 0.023(3) 0.001(3) 0.0115(19) 0.000(2) C68 0.018(2) 0.019(3) 0.025(3) 0.003(3) 0.0093(19) 0.003(2) C69 0.023(2) 0.018(2) 0.022(2) 0.002(2) 0.0072(18) 0.002(2) C70 0.0192(13) 0.0179(15) 0.0185(14) -0.0007(9) 0.0085(9) 0.0003(9) C71 0.0178(13) 0.0160(14) 0.0172(13) 0.0007(9) 0.0072(9) -0.0011(9) C72 0.0200(13) 0.0188(15) 0.0201(14) -0.0001(9) 0.0092(9) 0.0003(9) N12 0.0172(18) 0.019(3) 0.026(2) -0.003(2) 0.0100(18) 0.003(2) C73 0.019(2) 0.023(2) 0.028(3) -0.003(2) 0.011(2) -0.001(2) C74 0.024(3) 0.024(3) 0.042(5) -0.001(3) 0.015(3) 0.006(3) C75 0.025(2) 0.021(2) 0.028(3) -0.002(2) 0.012(2) -0.005(2) C76 0.0303(16) 0.0295(16) 0.0299(17) -0.0002(10) 0.0123(10) -0.0010(9) C77 0.0324(17) 0.0309(17) 0.0322(17) 0.0011(10) 0.0137(10) -0.0007(9) C78 0.032(3) 0.030(3) 0.031(3) -0.003(3) 0.016(2) -0.010(2) C79 0.020(3) 0.037(3) 0.031(4) -0.003(3) 0.010(2) -0.007(2) C80 0.028(3) 0.027(3) 0.032(3) 0.003(3) 0.016(2) -0.003(2) C81 0.024(2) 0.024(3) 0.024(3) -0.002(3) 0.009(2) -0.003(2) C82 0.0301(16) 0.0304(17) 0.0304(18) -0.0015(10) 0.0128(10) -0.0011(9) C83 0.0368(18) 0.0354(18) 0.0352(19) 0.0016(10) 0.0148(11) 0.0003(10) C84 0.031(3) 0.050(5) 0.020(4) -0.002(4) 0.007(3) -0.006(3) N13 0.028(3) 0.008(2) 0.025(4) 0.000 0.010(3) 0.000 C85 0.0195(16) 0.0172(15) 0.0201(16) 0.0002(9) 0.0082(10) -0.0004(9) C86 0.0160(15) 0.0140(15) 0.0163(16) -0.0003(9) 0.0070(9) 0.0005(9) N14 0.0195(16) 0.0161(15) 0.0187(17) 0.000 0.0069(10) 0.000 Fe5 0.0143(6) 0.0071(7) 0.0185(7) 0.000 0.0049(5) 0.000 O5 0.0171(16) 0.010(2) 0.020(2) -0.003(2) 0.0097(15) -0.0014(16) C87 0.0168(12) 0.0139(13) 0.0170(13) -0.0003(9) 0.0068(9) -0.0001(9) C88 0.0166(19) 0.013(3) 0.019(2) 0.001(2) 0.0059(17) 0.000(2) C89 0.0195(14) 0.0202(15) 0.0211(14) 0.0007(9) 0.0085(9) -0.0010(9) C90 0.0190(19) 0.017(2) 0.026(2) -0.001(2) 0.0106(18) 0.0005(19) C91 0.026(2) 0.016(3) 0.020(3) 0.003(2) 0.0113(19) 0.002(2) C92 0.0204(18) 0.012(2) 0.019(2) 0.003(2) 0.0101(17) 0.000(2) C93 0.021(2) 0.010(3) 0.019(2) -0.004(2) 0.0047(18) -0.001(2) N15 0.0209(19) 0.015(2) 0.022(2) -0.0011(19) 0.0040(17) 0.002(2) C94 0.012(2) 0.025(2) 0.021(2) -0.002(2) 0.0053(19) 0.001(2) C95 0.025(4) 0.031(3) 0.025(5) 0.005(3) 0.001(3) -0.009(3) C96 0.011(2) 0.024(2) 0.021(3) 0.000(2) 0.0012(19) 0.0020(19) C97 0.018(2) 0.027(2) 0.023(3) 0.002(2) 0.005(2) 0.007(2) C98 0.025(2) 0.022(2) 0.028(3) -0.003(2) 0.003(2) 0.004(2) C99 0.0237(14) 0.0219(14) 0.0243(15) 0.0001(9) 0.0086(9) -0.0002(9) C100 0.023(2) 0.022(3) 0.024(3) 0.002(2) 0.007(2) 0.002(2) C101 0.017(2) 0.025(2) 0.023(3) 0.001(2) 0.004(2) 0.007(2) C102 0.021(2) 0.029(3) 0.033(3) 0.003(2) 0.013(2) 0.000(2) C103 0.032(4) 0.046(4) 0.034(4) 0.004(3) 0.020(3) 0.015(3) C104 0.033(3) 0.035(4) 0.037(4) 0.000(3) 0.017(3) 0.013(3) C105 0.0371(18) 0.0382(18) 0.0380(19) 0.0020(10) 0.0184(11) -0.0003(10) N16 0.0159(16) 0.0131(15) 0.0154(17) 0.000 0.0061(10) 0.000 C106 0.0168(15) 0.0141(14) 0.0165(16) 0.0004(9) 0.0068(9) -0.0009(9) C107 0.0173(15) 0.0159(15) 0.0181(16) -0.0004(9) 0.0080(10) 0.0016(9) N17 0.0179(16) 0.0146(16) 0.0174(17) 0.000 0.0069(10) 0.000 Fe6 0.0166(6) 0.0073(7) 0.0236(8) 0.000 0.0051(6) 0.000 O6 0.0235(19) 0.012(2) 0.026(2) -0.001(2) 0.0071(18) -0.0018(18) C108 0.0221(13) 0.0190(15) 0.0224(14) 0.0001(9) 0.0087(9) -0.0006(9) C109 0.024(2) 0.024(3) 0.030(3) -0.006(3) 0.007(2) 0.001(2) C110 0.015(2) 0.031(3) 0.034(3) -0.005(3) 0.004(2) 0.004(3) C111 0.025(2) 0.025(3) 0.030(2) -0.001(2) 0.0050(18) 0.000(2) C112 0.0254(14) 0.0245(16) 0.0250(15) 0.0014(10) 0.0118(9) 0.0008(9) C113 0.0268(19) 0.016(2) 0.025(2) -0.005(2) 0.0089(17) 0.006(2) C114 0.026(2) 0.018(3) 0.027(2) -0.002(3) 0.0129(19) 0.004(2) N18 0.0210(13) 0.0191(14) 0.0215(14) 0.0000(9) 0.0088(9) 0.0002(9) C115 0.020(2) 0.017(2) 0.021(3) 0.000(2) 0.0072(19) 0.003(2) C116 0.030(3) 0.025(3) 0.051(5) 0.015(3) 0.021(3) 0.005(3) C117 0.015(2) 0.016(2) 0.022(3) -0.001(2) 0.007(2) 0.0013(19) C118 0.019(2) 0.023(3) 0.021(3) -0.003(3) 0.008(2) 0.002(2) C119 0.027(2) 0.021(3) 0.018(3) -0.003(3) 0.014(2) 0.000(2) C120 0.0246(15) 0.0246(16) 0.0251(16) 0.0001(10) 0.0119(10) -0.0001(9) C121 0.015(2) 0.025(3) 0.035(3) 0.004(3) 0.009(2) 0.006(2) C122 0.016(2) 0.022(3) 0.029(3) -0.004(3) 0.009(2) 0.003(2) C123 0.030(2) 0.030(3) 0.033(3) -0.003(3) 0.007(2) 0.007(3) C124 0.0343(17) 0.0342(18) 0.0332(18) -0.0008(10) 0.0141(11) 0.0006(9) C125 0.0395(19) 0.0382(19) 0.038(2) 0.0008(10) 0.0167(11) 0.0014(10) C126 0.0376(19) 0.0377(19) 0.037(2) -0.0008(10) 0.0170(12) 0.0010(10) N300 0.0238(17) 0.0239(18) 0.0223(19) 0.0010(10) 0.0106(11) -0.0026(9) C301 0.0224(19) 0.0210(19) 0.021(2) 0.0011(10) 0.0100(11) -0.0032(9) C302 0.034(2) 0.033(2) 0.034(2) -0.0005(10) 0.0153(12) 0.0004(10) N400 0.0307(19) 0.032(2) 0.030(2) -0.0003(10) 0.0147(12) -0.0012(9) C401 0.026(2) 0.026(2) 0.026(2) 0.0007(10) 0.0122(12) -0.0027(10) C402 0.040(2) 0.040(2) 0.040(2) -0.0006(10) 0.0178(13) -0.0006(10) N500 0.057(2) 0.054(2) 0.058(2) 0.0006(10) 0.0262(12) -0.0011(10) C501 0.059(2) 0.056(2) 0.058(2) -0.0002(10) 0.0259(13) -0.0001(10) C502 0.053(2) 0.048(2) 0.049(2) 0.0000(10) 0.0220(13) 0.0006(10) _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 N1 C1 1.326(8) . ? N1 C1 1.326(8) 2_856 ? N1 Fe3 2.264(10) 1_545 ? C1 C2 1.369(10) . ? C1 H1A 0.9500 . ? C2 N2 1.333(8) . ? C2 H2A 0.9500 . ? N2 C2 1.333(8) 2_856 ? N2 Fe1 2.279(10) . ? Fe1 O1 1.997(5) 2_856 ? Fe1 O1 1.997(5) . ? Fe1 N4 2.295(9) . ? Fe1 N3 2.343(7) 2_856 ? Fe1 N3 2.343(7) . ? O1 C3 1.252(9) . ? C3 C8 1.369(11) . ? C3 C4 1.451(9) . ? C4 C5 1.364(10) . ? C4 H4A 0.9500 . ? C5 C6 1.408(11) . ? C5 H5A 0.9500 . ? C6 C7 1.381(9) . ? C6 C18 1.554(12) . ? C7 C8 1.535(11) . ? C7 H7A 0.9500 . ? C8 C9 1.427(9) . ? C9 N3 1.219(9) . ? C9 H9A 0.9500 . ? N3 C10 1.500(8) . ? C10 C12 1.512(10) . ? C10 C11 1.546(9) . ? C10 H10A 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.382(9) . ? C12 C17 1.415(10) . ? C13 C14 1.369(10) . ? C13 H13A 0.9500 . ? C14 C15 1.425(10) . ? C14 H14A 0.9500 . ? C15 C16 1.377(10) . ? C15 H15A 0.9500 . ? C16 C17 1.446(11) . ? C16 H16A 0.9500 . ? C17 H17A 0.9500 . ? C18 C20 1.434(11) . ? C18 C21 1.484(9) . ? C18 C19 1.581(13) . ? 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 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? N4 C22 1.293(8) . ? N4 C22 1.293(8) 2_856 ? C22 C23 1.321(10) . ? C22 H22A 0.9500 . ? C23 N5 1.322(8) . ? C23 H23A 0.9500 . ? N5 C23 1.322(8) 2_856 ? N5 Fe2 2.323(9) . ? Fe2 O2 1.994(4) 2_856 ? Fe2 O2 1.994(4) . ? Fe2 N6 2.172(6) 2_856 ? Fe2 N6 2.172(6) . ? Fe2 N7 2.259(9) . ? O2 C24 1.315(8) . ? C24 C29 1.394(9) . ? C24 C25 1.428(8) . ? C25 C26 1.406(9) . ? C25 H25A 0.9500 . ? C26 C27 1.369(9) . ? C26 H26A 0.9500 . ? C27 C28 1.364(7) . ? C27 C39 1.543(9) . ? C28 C29 1.390(9) . ? C28 H28A 0.9500 . ? C29 C30 1.503(8) . ? C30 N6 1.267(8) . ? C30 H30A 0.9500 . ? N6 C31 1.493(7) . ? C31 C32 1.517(8) . ? C31 C33 1.519(10) . ? C31 H31A 1.0000 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C38 1.331(9) . ? C33 C34 1.388(10) . ? C34 C35 1.427(9) . ? C34 H34A 0.9500 . ? C35 C36 1.409(9) . ? C35 H35A 0.9500 . ? C36 C37 1.357(10) . ? C36 H36A 0.9500 . ? C37 C38 1.407(9) . ? C37 H37A 0.9500 . ? C38 H38A 0.9500 . ? C39 C40 1.489(8) . ? C39 C42 1.546(10) . ? C39 C41 1.589(11) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? N7 C43 1.332(7) . ? N7 C43 1.332(7) 2_856 ? C43 C44 1.415(9) . ? C43 H43A 0.9500 . ? C44 N8 1.345(7) . ? C44 H44A 0.9500 . ? N8 C44 1.345(7) 2_856 ? N8 Fe3 2.195(9) . ? Fe3 O3 2.003(5) 2_856 ? Fe3 O3 2.003(5) . ? Fe3 N9 2.161(8) 2_856 ? Fe3 N9 2.161(8) . ? Fe3 N1 2.264(10) 1_565 ? O3 C45 1.313(10) . ? C45 C46 1.421(9) . ? C45 C50 1.423(12) . ? C46 C47 1.382(12) . ? C46 H46A 0.9500 . ? C47 C48 1.417(12) . ? C47 H47A 0.9500 . ? C48 C49 1.436(10) . ? C48 C60 1.535(12) . ? C49 C50 1.290(11) . ? C49 H49A 0.9500 . ? C50 C51 1.457(9) . ? C51 N9 1.323(10) . ? C51 H51A 0.9500 . ? N9 C52 1.495(8) . ? C52 C53 1.525(11) . ? C52 C54 1.550(10) . ? C52 H52A 1.0000 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 C55 1.343(11) . ? C54 C59 1.383(10) . ? C55 C56 1.406(10) . ? C55 H55A 0.9500 . ? C56 C57 1.360(10) . ? C56 H56A 0.9500 . ? C57 C58 1.358(11) . ? C57 H57A 0.9500 . ? C58 C59 1.404(10) . ? C58 H58A 0.9500 . ? C59 H59A 0.9500 . ? C60 C61 1.502(11) . ? C60 C63 1.503(10) . ? C60 C62 1.513(11) . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? N10 C64 1.335(9) 2_857 ? N10 C64 1.335(9) . ? N10 Fe6 2.227(10) 1_545 ? C64 C65 1.369(9) . ? C64 H64A 0.9500 . ? C65 N11 1.297(8) . ? C65 H65A 0.9500 . ? N11 C65 1.297(8) 2_857 ? N11 Fe4 2.310(9) . ? Fe4 O4 1.982(4) 2_857 ? Fe4 O4 1.982(4) . ? Fe4 N12 2.262(7) . ? Fe4 N12 2.262(7) 2_857 ? Fe4 N13 2.282(9) . ? O4 C66 1.310(8) . ? C66 C71 1.360(10) . ? C66 C67 1.388(8) . ? C67 C68 1.379(9) . ? C67 H67A 0.9500 . ? C68 C69 1.435(10) . ? C68 H68A 0.9500 . ? C69 C70 1.341(8) . ? C69 C81 1.543(9) . ? C70 C71 1.489(9) . ? C70 H70A 0.9500 . ? C71 C72 1.456(8) . ? C72 N12 1.266(8) . ? C72 H72A 0.9500 . ? N12 C73 1.539(8) . ? C73 C75 1.485(10) . ? C73 C74 1.578(9) . ? C73 H73A 1.0000 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 C80 1.383(9) . ? C75 C76 1.429(10) . ? C76 C77 1.365(10) . ? C76 H76A 0.9500 . ? C77 C78 1.412(10) . ? C77 H77A 0.9500 . ? C78 C79 1.377(11) . ? C78 H78A 0.9500 . ? C79 C80 1.374(10) . ? C79 H79A 0.9500 . ? C80 H80A 0.9500 . ? C81 C84 1.481(10) . ? C81 C82 1.545(8) . ? C81 C83 1.606(9) . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? C83 H83A 0.9800 . ? C83 H83B 0.9800 . ? C83 H83C 0.9800 . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 0.9800 . ? N13 C85 1.356(8) 2_857 ? N13 C85 1.356(8) . ? C85 C86 1.350(10) . ? C85 H85A 0.9500 . ? C86 N14 1.335(8) . ? C86 H86A 0.9500 . ? N14 C86 1.335(8) 2_857 ? N14 Fe5 2.301(9) . ? Fe5 O5 2.001(4) . ? Fe5 O5 2.001(4) 2_857 ? Fe5 N15 2.179(7) . ? Fe5 N15 2.179(7) 2_857 ? Fe5 N16 2.236(9) . ? O5 C87 1.298(8) . ? C87 C88 1.406(8) . ? C87 C92 1.440(10) . ? C88 C89 1.351(9) . ? C88 H88A 0.9500 . ? C89 C90 1.458(9) . ? C89 H89A 0.9500 . ? C90 C91 1.376(8) . ? C90 C102 1.473(10) . ? C91 C92 1.447(10) . ? C91 H91A 0.9500 . ? C92 C93 1.449(8) . ? C93 N15 1.299(8) . ? C93 H93A 0.9500 . ? N15 C94 1.472(7) . ? C94 C96 1.500(9) . ? C94 C95 1.510(9) . ? C94 H94A 1.0000 . ? C95 H95A 0.9800 . ? C95 H95B 0.9800 . ? C95 H95C 0.9800 . ? C96 C101 1.377(10) . ? C96 C97 1.410(9) . ? C97 C98 1.382(9) . ? C97 H97A 0.9500 . ? C98 C99 1.399(9) . ? C98 H98A 0.9500 . ? C99 C100 1.411(9) . ? C99 H99A 0.9500 . ? C100 C101 1.420(9) . ? C100 H10B 0.9500 . ? C101 H10C 0.9500 . ? C102 C103 1.458(11) . ? C102 C104 1.528(8) . ? C102 C105 1.547(9) . ? C103 H10D 0.9800 . ? C103 H10E 0.9800 . ? C103 H10F 0.9800 . ? C104 H10G 0.9800 . ? C104 H10H 0.9800 . ? C104 H10I 0.9800 . ? C105 H10J 0.9800 . ? C105 H10K 0.9800 . ? C105 H10L 0.9800 . ? N16 C106 1.339(8) 2_857 ? N16 C106 1.339(8) . ? C106 C107 1.445(10) . ? C106 H10M 0.9500 . ? C107 N17 1.378(8) . ? C107 H10N 0.9500 . ? N17 C107 1.378(8) 2_857 ? N17 Fe6 2.167(9) . ? Fe6 O6 1.990(5) 2_857 ? Fe6 O6 1.990(5) . ? Fe6 N18 2.122(7) . ? Fe6 N18 2.122(7) 2_857 ? Fe6 N10 2.227(10) 1_565 ? O6 C108 1.327(10) . ? C108 C109 1.410(9) . ? C108 C113 1.462(12) . ? C109 C110 1.446(12) . ? C109 H10O 0.9500 . ? C110 C111 1.333(12) . ? C110 H11D 0.9500 . ? C111 C112 1.402(9) . ? C111 C123 1.495(12) . ? C112 C113 1.394(11) . ? C112 H11E 0.9500 . ? C113 C114 1.439(9) . ? C114 N18 1.334(9) . ? C114 H11F 0.9500 . ? N18 C115 1.463(8) . ? C115 C117 1.530(10) . ? C115 C116 1.535(10) . ? C115 H11G 1.0000 . ? C116 H11H 0.9800 . ? C116 H11I 0.9800 . ? C116 H11J 0.9800 . ? C117 C118 1.387(10) . ? C117 C122 1.404(9) . ? C118 C119 1.366(10) . ? C118 H11K 0.9500 . ? C119 C120 1.378(9) . ? C119 H11L 0.9500 . ? C120 C121 1.366(10) . ? C120 H12A 0.9500 . ? C121 C122 1.421(10) . ? C121 H12B 0.9500 . ? C122 H12C 0.9500 . ? C123 C124 1.512(9) . ? C123 C125 1.565(11) . ? C123 C126 1.608(11) . ? C124 H12D 0.9800 . ? C124 H12E 0.9800 . ? C124 H12F 0.9800 . ? C125 H12G 0.9800 . ? C125 H12H 0.9800 . ? C125 H12I 0.9800 . ? C126 H12J 0.9800 . ? C126 H12K 0.9800 . ? C126 H12L 0.9800 . ? N300 C301 1.072(9) . ? C301 C302 1.487(9) . ? C302 H30B 0.9800 . ? C302 H30C 0.9800 . ? C302 H30D 0.9800 . ? N400 C401 1.1061 . ? C401 C402 1.4911 . ? C402 H40D 0.9800 . ? C402 H40E 0.9800 . ? C402 H40F 0.9800 . ? N500 C501 1.136(10) . ? C501 C502 1.578(12) . ? C502 H50A 0.9800 . ? C502 H50B 0.9800 . ? C502 H50C 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 C1 N1 C1 116.6(10) . 2_856 ? C1 N1 Fe3 121.7(5) . 1_545 ? C1 N1 Fe3 121.7(5) 2_856 1_545 ? N1 C1 C2 121.9(8) . . ? N1 C1 H1A 119.0 . . ? C2 C1 H1A 119.0 . . ? N2 C2 C1 121.4(8) . . ? N2 C2 H2A 119.3 . . ? C1 C2 H2A 119.3 . . ? C2 N2 C2 116.7(10) 2_856 . ? C2 N2 Fe1 121.7(5) 2_856 . ? C2 N2 Fe1 121.7(5) . . ? O1 Fe1 O1 179.9(3) 2_856 . ? O1 Fe1 N2 90.05(16) 2_856 . ? O1 Fe1 N2 90.05(16) . . ? O1 Fe1 N4 89.95(16) 2_856 . ? O1 Fe1 N4 89.95(16) . . ? N2 Fe1 N4 180.000(3) . . ? O1 Fe1 N3 84.2(2) 2_856 2_856 ? O1 Fe1 N3 95.8(2) . 2_856 ? N2 Fe1 N3 87.38(16) . 2_856 ? N4 Fe1 N3 92.62(16) . 2_856 ? O1 Fe1 N3 95.8(2) 2_856 . ? O1 Fe1 N3 84.2(2) . . ? N2 Fe1 N3 87.38(16) . . ? N4 Fe1 N3 92.62(16) . . ? N3 Fe1 N3 174.8(3) 2_856 . ? C3 O1 Fe1 135.6(5) . . ? O1 C3 C8 123.3(7) . . ? O1 C3 C4 120.7(8) . . ? C8 C3 C4 115.9(8) . . ? C5 C4 C3 121.8(8) . . ? C5 C4 H4A 119.1 . . ? C3 C4 H4A 119.1 . . ? C4 C5 C6 123.8(7) . . ? C4 C5 H5A 118.1 . . ? C6 C5 H5A 118.1 . . ? C7 C6 C5 118.1(8) . . ? C7 C6 C18 115.5(8) . . ? C5 C6 C18 126.3(7) . . ? C6 C7 C8 118.1(8) . . ? C6 C7 H7A 121.0 . . ? C8 C7 H7A 121.0 . . ? C3 C8 C9 126.6(8) . . ? C3 C8 C7 122.1(7) . . ? C9 C8 C7 111.3(8) . . ? N3 C9 C8 129.8(9) . . ? N3 C9 H9A 115.1 . . ? C8 C9 H9A 115.1 . . ? C9 N3 C10 115.1(7) . . ? C9 N3 Fe1 120.1(6) . . ? C10 N3 Fe1 124.8(5) . . ? N3 C10 C12 108.9(6) . . ? N3 C10 C11 112.2(6) . . ? C12 C10 C11 112.4(6) . . ? N3 C10 H10A 107.7 . . ? C12 C10 H10A 107.7 . . ? C11 C10 H10A 107.7 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C17 116.7(7) . . ? C13 C12 C10 127.4(7) . . ? C17 C12 C10 114.7(7) . . ? C14 C13 C12 123.0(8) . . ? C14 C13 H13A 118.5 . . ? C12 C13 H13A 118.5 . . ? C13 C14 C15 119.3(7) . . ? C13 C14 H14A 120.4 . . ? C15 C14 H14A 120.4 . . ? C16 C15 C14 121.8(8) . . ? C16 C15 H15A 119.1 . . ? C14 C15 H15A 119.1 . . ? C15 C16 C17 116.1(8) . . ? C15 C16 H16A 122.0 . . ? C17 C16 H16A 122.0 . . ? C12 C17 C16 122.7(7) . . ? C12 C17 H17A 118.6 . . ? C16 C17 H17A 118.6 . . ? C20 C18 C21 111.4(8) . . ? C20 C18 C6 112.2(8) . . ? C21 C18 C6 112.8(8) . . ? C20 C18 C19 103.9(8) . . ? C21 C18 C19 107.2(8) . . ? C6 C18 C19 108.8(7) . . ? 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 . . ? C22 N4 C22 114.9(9) . 2_856 ? C22 N4 Fe1 122.5(5) . . ? C22 N4 Fe1 122.6(5) 2_856 . ? N4 C22 C23 123.5(7) . . ? N4 C22 H22A 118.2 . . ? C23 C22 H22A 118.2 . . ? C22 C23 N5 121.4(7) . . ? C22 C23 H23A 119.3 . . ? N5 C23 H23A 119.3 . . ? C23 N5 C23 114.9(9) 2_856 . ? C23 N5 Fe2 122.5(5) 2_856 . ? C23 N5 Fe2 122.5(5) . . ? O2 Fe2 O2 178.1(3) 2_856 . ? O2 Fe2 N6 87.0(2) 2_856 2_856 ? O2 Fe2 N6 93.2(2) . 2_856 ? O2 Fe2 N6 93.2(2) 2_856 . ? O2 Fe2 N6 87.0(2) . . ? N6 Fe2 N6 171.8(3) 2_856 . ? O2 Fe2 N7 90.94(15) 2_856 . ? O2 Fe2 N7 90.94(15) . . ? N6 Fe2 N7 85.88(16) 2_856 . ? N6 Fe2 N7 85.88(16) . . ? O2 Fe2 N5 89.06(15) 2_856 . ? O2 Fe2 N5 89.06(15) . . ? N6 Fe2 N5 94.12(16) 2_856 . ? N6 Fe2 N5 94.12(16) . . ? N7 Fe2 N5 180.000(4) . . ? C24 O2 Fe2 131.5(4) . . ? O2 C24 C29 126.5(5) . . ? O2 C24 C25 118.5(6) . . ? C29 C24 C25 115.0(6) . . ? C26 C25 C24 120.9(7) . . ? C26 C25 H25A 119.5 . . ? C24 C25 H25A 119.5 . . ? C27 C26 C25 122.3(5) . . ? C27 C26 H26A 118.8 . . ? C25 C26 H26A 118.8 . . ? C28 C27 C26 116.5(6) . . ? C28 C27 C39 120.7(6) . . ? C26 C27 C39 122.8(5) . . ? C27 C28 C29 123.4(7) . . ? C27 C28 H28A 118.3 . . ? C29 C28 H28A 118.3 . . ? C28 C29 C24 121.7(6) . . ? C28 C29 C30 116.0(7) . . ? C24 C29 C30 122.4(7) . . ? N6 C30 C29 125.7(7) . . ? N6 C30 H30A 117.1 . . ? C29 C30 H30A 117.1 . . ? C30 N6 C31 116.8(7) . . ? C30 N6 Fe2 126.7(5) . . ? C31 N6 Fe2 116.3(4) . . ? N6 C31 C32 108.8(5) . . ? N6 C31 C33 113.4(5) . . ? C32 C31 C33 116.2(6) . . ? N6 C31 H31A 105.9 . . ? C32 C31 H31A 105.9 . . ? C33 C31 H31A 105.9 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C38 C33 C34 119.2(7) . . ? C38 C33 C31 120.3(8) . . ? C34 C33 C31 120.5(7) . . ? C33 C34 C35 121.1(6) . . ? C33 C34 H34A 119.5 . . ? C35 C34 H34A 119.5 . . ? C36 C35 C34 117.9(7) . . ? C36 C35 H35A 121.0 . . ? C34 C35 H35A 121.0 . . ? C37 C36 C35 119.2(7) . . ? C37 C36 H36A 120.4 . . ? C35 C36 H36A 120.4 . . ? C36 C37 C38 121.3(7) . . ? C36 C37 H37A 119.3 . . ? C38 C37 H37A 119.3 . . ? C33 C38 C37 121.3(7) . . ? C33 C38 H38A 119.3 . . ? C37 C38 H38A 119.3 . . ? C40 C39 C27 112.9(6) . . ? C40 C39 C42 109.3(6) . . ? C27 C39 C42 109.2(6) . . ? C40 C39 C41 109.9(6) . . ? C27 C39 C41 107.0(6) . . ? C42 C39 C41 108.4(6) . . ? 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 . . ? C43 N7 C43 113.5(8) . 2_856 ? C43 N7 Fe2 123.3(4) . . ? C43 N7 Fe2 123.3(4) 2_856 . ? N7 C43 C44 124.6(6) . . ? N7 C43 H43A 117.7 . . ? C44 C43 H43A 117.7 . . ? N8 C44 C43 120.1(6) . . ? N8 C44 H44A 120.0 . . ? C43 C44 H44A 120.0 . . ? C44 N8 C44 117.1(8) 2_856 . ? C44 N8 Fe3 121.5(4) 2_856 . ? C44 N8 Fe3 121.5(4) . . ? O3 Fe3 O3 179.7(3) 2_856 . ? O3 Fe3 N9 87.1(2) 2_856 2_856 ? O3 Fe3 N9 92.9(2) . 2_856 ? O3 Fe3 N9 92.9(2) 2_856 . ? O3 Fe3 N9 87.1(2) . . ? N9 Fe3 N9 175.5(4) 2_856 . ? O3 Fe3 N8 90.15(17) 2_856 . ? O3 Fe3 N8 90.15(17) . . ? N9 Fe3 N8 92.26(18) 2_856 . ? N9 Fe3 N8 92.26(18) . . ? O3 Fe3 N1 89.85(17) 2_856 1_565 ? O3 Fe3 N1 89.85(17) . 1_565 ? N9 Fe3 N1 87.74(18) 2_856 1_565 ? N9 Fe3 N1 87.74(18) . 1_565 ? N8 Fe3 N1 180.000(6) . 1_565 ? C45 O3 Fe3 132.2(5) . . ? O3 C45 C46 116.6(8) . . ? O3 C45 C50 124.3(7) . . ? C46 C45 C50 119.0(9) . . ? C47 C46 C45 119.0(9) . . ? C47 C46 H46A 120.5 . . ? C45 C46 H46A 120.5 . . ? C46 C47 C48 124.2(8) . . ? C46 C47 H47A 117.9 . . ? C48 C47 H47A 117.9 . . ? C47 C48 C49 110.4(8) . . ? C47 C48 C60 125.9(7) . . ? C49 C48 C60 123.7(9) . . ? C50 C49 C48 130.1(9) . . ? C50 C49 H49A 115.0 . . ? C48 C49 H49A 115.0 . . ? C49 C50 C45 117.1(8) . . ? C49 C50 C51 117.4(9) . . ? C45 C50 C51 125.4(9) . . ? N9 C51 C50 123.8(9) . . ? N9 C51 H51A 118.1 . . ? C50 C51 H51A 118.1 . . ? C51 N9 C52 115.5(7) . . ? C51 N9 Fe3 126.9(5) . . ? C52 N9 Fe3 117.2(5) . . ? N9 C52 C53 117.1(6) . . ? N9 C52 C54 107.8(6) . . ? C53 C52 C54 110.3(6) . . ? N9 C52 H52A 107.1 . . ? C53 C52 H52A 107.1 . . ? C54 C52 H52A 107.1 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C55 C54 C59 119.2(7) . . ? C55 C54 C52 123.0(7) . . ? C59 C54 C52 117.5(7) . . ? C54 C55 C56 120.7(8) . . ? C54 C55 H55A 119.6 . . ? C56 C55 H55A 119.6 . . ? C57 C56 C55 119.4(8) . . ? C57 C56 H56A 120.3 . . ? C55 C56 H56A 120.3 . . ? C58 C57 C56 120.9(8) . . ? C58 C57 H57A 119.5 . . ? C56 C57 H57A 119.5 . . ? C57 C58 C59 118.9(8) . . ? C57 C58 H58A 120.5 . . ? C59 C58 H58A 120.5 . . ? C54 C59 C58 120.3(8) . . ? C54 C59 H59A 119.8 . . ? C58 C59 H59A 119.8 . . ? C61 C60 C63 110.1(7) . . ? C61 C60 C62 112.3(9) . . ? C63 C60 C62 109.6(7) . . ? C61 C60 C48 108.0(7) . . ? C63 C60 C48 109.4(8) . . ? C62 C60 C48 107.3(6) . . ? C60 C61 H61A 109.5 . . ? C60 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C60 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C60 C62 H62A 109.5 . . ? C60 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C60 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C60 C63 H63A 109.5 . . ? C60 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C60 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C64 N10 C64 112.1(10) 2_857 . ? C64 N10 Fe6 124.0(5) 2_857 1_545 ? C64 N10 Fe6 124.0(5) . 1_545 ? N10 C64 C65 124.2(8) . . ? N10 C64 H64A 117.9 . . ? C65 C64 H64A 117.9 . . ? N11 C65 C64 120.3(8) . . ? N11 C65 H65A 119.9 . . ? C64 C65 H65A 119.9 . . ? C65 N11 C65 118.6(10) . 2_857 ? C65 N11 Fe4 120.7(5) . . ? C65 N11 Fe4 120.7(5) 2_857 . ? O4 Fe4 O4 178.8(3) 2_857 . ? O4 Fe4 N12 95.1(2) 2_857 . ? O4 Fe4 N12 84.9(2) . . ? O4 Fe4 N12 84.9(2) 2_857 2_857 ? O4 Fe4 N12 95.1(2) . 2_857 ? N12 Fe4 N12 173.0(3) . 2_857 ? O4 Fe4 N13 89.38(16) 2_857 . ? O4 Fe4 N13 89.38(16) . . ? N12 Fe4 N13 93.52(17) . . ? N12 Fe4 N13 93.52(17) 2_857 . ? O4 Fe4 N11 90.62(16) 2_857 . ? O4 Fe4 N11 90.62(16) . . ? N12 Fe4 N11 86.48(17) . . ? N12 Fe4 N11 86.48(17) 2_857 . ? N13 Fe4 N11 180.000(3) . . ? C66 O4 Fe4 135.4(5) . . ? O4 C66 C71 122.5(6) . . ? O4 C66 C67 119.3(7) . . ? C71 C66 C67 118.2(7) . . ? C68 C67 C66 121.0(7) . . ? C68 C67 H67A 119.5 . . ? C66 C67 H67A 119.5 . . ? C67 C68 C69 123.2(6) . . ? C67 C68 H68A 118.4 . . ? C69 C68 H68A 118.4 . . ? C70 C69 C68 115.4(7) . . ? C70 C69 C81 121.9(7) . . ? C68 C69 C81 122.6(6) . . ? C69 C70 C71 121.7(7) . . ? C69 C70 H70A 119.2 . . ? C71 C70 H70A 119.2 . . ? C66 C71 C72 126.7(7) . . ? C66 C71 C70 120.3(6) . . ? C72 C71 C70 113.0(7) . . ? N12 C72 C71 126.6(7) . . ? N12 C72 H72A 116.7 . . ? C71 C72 H72A 116.7 . . ? C72 N12 C73 113.1(7) . . ? C72 N12 Fe4 123.4(5) . . ? C73 N12 Fe4 123.3(4) . . ? C75 C73 N12 110.6(6) . . ? C75 C73 C74 115.5(5) . . ? N12 C73 C74 108.3(6) . . ? C75 C73 H73A 107.4 . . ? N12 C73 H73A 107.4 . . ? C74 C73 H73A 107.4 . . ? C73 C74 H74A 109.5 . . ? C73 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C73 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C80 C75 C76 116.5(7) . . ? C80 C75 C73 125.5(7) . . ? C76 C75 C73 118.0(6) . . ? C77 C76 C75 120.9(7) . . ? C77 C76 H76A 119.5 . . ? C75 C76 H76A 119.5 . . ? C76 C77 C78 121.8(8) . . ? C76 C77 H77A 119.1 . . ? C78 C77 H77A 119.1 . . ? C79 C78 C77 115.9(8) . . ? C79 C78 H78A 122.1 . . ? C77 C78 H78A 122.1 . . ? C80 C79 C78 123.3(7) . . ? C80 C79 H79A 118.4 . . ? C78 C79 H79A 118.4 . . ? C79 C80 C75 121.1(8) . . ? C79 C80 H80A 119.4 . . ? C75 C80 H80A 119.4 . . ? C84 C81 C69 114.3(5) . . ? C84 C81 C82 110.8(6) . . ? C69 C81 C82 108.3(6) . . ? C84 C81 C83 107.2(6) . . ? C69 C81 C83 108.0(6) . . ? C82 C81 C83 107.9(5) . . ? 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 . . ? C81 C83 H83A 109.5 . . ? C81 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C81 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? C81 C84 H84A 109.5 . . ? C81 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C81 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? C85 N13 C85 113.7(9) 2_857 . ? C85 N13 Fe4 123.2(4) 2_857 . ? C85 N13 Fe4 123.2(4) . . ? C86 C85 N13 123.3(7) . . ? C86 C85 H85A 118.3 . . ? N13 C85 H85A 118.3 . . ? N14 C86 C85 121.1(7) . . ? N14 C86 H86A 119.4 . . ? C85 C86 H86A 119.4 . . ? C86 N14 C86 117.2(9) . 2_857 ? C86 N14 Fe5 121.4(5) . . ? C86 N14 Fe5 121.4(5) 2_857 . ? O5 Fe5 O5 179.0(3) . 2_857 ? O5 Fe5 N15 88.0(2) . . ? O5 Fe5 N15 92.0(2) 2_857 . ? O5 Fe5 N15 92.0(2) . 2_857 ? O5 Fe5 N15 88.0(2) 2_857 2_857 ? N15 Fe5 N15 178.3(3) . 2_857 ? O5 Fe5 N16 89.49(15) . . ? O5 Fe5 N16 89.49(15) 2_857 . ? N15 Fe5 N16 90.85(17) . . ? N15 Fe5 N16 90.85(17) 2_857 . ? O5 Fe5 N14 90.51(15) . . ? O5 Fe5 N14 90.51(15) 2_857 . ? N15 Fe5 N14 89.15(17) . . ? N15 Fe5 N14 89.15(17) 2_857 . ? N16 Fe5 N14 180.000(3) . . ? C87 O5 Fe5 133.2(5) . . ? O5 C87 C88 120.9(7) . . ? O5 C87 C92 122.1(5) . . ? C88 C87 C92 117.0(7) . . ? C89 C88 C87 122.2(7) . . ? C89 C88 H88A 118.9 . . ? C87 C88 H88A 118.9 . . ? C88 C89 C90 124.2(6) . . ? C88 C89 H89A 117.9 . . ? C90 C89 H89A 117.9 . . ? C91 C90 C89 113.2(6) . . ? C91 C90 C102 123.3(7) . . ? C89 C90 C102 123.4(6) . . ? C90 C91 C92 125.0(7) . . ? C90 C91 H91A 117.5 . . ? C92 C91 H91A 117.5 . . ? C87 C92 C91 118.1(6) . . ? C87 C92 C93 125.6(7) . . ? C91 C92 C93 116.3(7) . . ? N15 C93 C92 127.1(7) . . ? N15 C93 H93A 116.4 . . ? C92 C93 H93A 116.4 . . ? C93 N15 C94 114.9(6) . . ? C93 N15 Fe5 123.4(5) . . ? C94 N15 Fe5 121.6(4) . . ? N15 C94 C96 112.9(5) . . ? N15 C94 C95 110.8(6) . . ? C96 C94 C95 114.9(6) . . ? N15 C94 H94A 105.8 . . ? C96 C94 H94A 105.8 . . ? C95 C94 H94A 105.8 . . ? C94 C95 H95A 109.5 . . ? C94 C95 H95B 109.5 . . ? H95A C95 H95B 109.5 . . ? C94 C95 H95C 109.5 . . ? H95A C95 H95C 109.5 . . ? H95B C95 H95C 109.5 . . ? C101 C96 C97 118.9(7) . . ? C101 C96 C94 123.2(6) . . ? C97 C96 C94 117.7(7) . . ? C98 C97 C96 120.2(7) . . ? C98 C97 H97A 119.9 . . ? C96 C97 H97A 119.9 . . ? C97 C98 C99 122.3(7) . . ? C97 C98 H98A 118.9 . . ? C99 C98 H98A 118.9 . . ? C98 C99 C100 117.3(7) . . ? C98 C99 H99A 121.3 . . ? C100 C99 H99A 121.3 . . ? C99 C100 C101 120.4(7) . . ? C99 C100 H10B 119.8 . . ? C101 C100 H10B 119.8 . . ? C96 C101 C100 120.9(6) . . ? C96 C101 H10C 119.6 . . ? C100 C101 H10C 119.6 . . ? C103 C102 C90 113.6(6) . . ? C103 C102 C104 110.0(6) . . ? C90 C102 C104 110.4(6) . . ? C103 C102 C105 105.8(7) . . ? C90 C102 C105 109.9(6) . . ? C104 C102 C105 106.9(5) . . ? C102 C103 H10D 109.5 . . ? C102 C103 H10E 109.5 . . ? H10D C103 H10E 109.5 . . ? C102 C103 H10F 109.5 . . ? H10D C103 H10F 109.5 . . ? H10E C103 H10F 109.5 . . ? C102 C104 H10G 109.5 . . ? C102 C104 H10H 109.5 . . ? H10G C104 H10H 109.5 . . ? C102 C104 H10I 109.5 . . ? H10G C104 H10I 109.5 . . ? H10H C104 H10I 109.5 . . ? C102 C105 H10J 109.5 . . ? C102 C105 H10K 109.5 . . ? H10J C105 H10K 109.5 . . ? C102 C105 H10L 109.5 . . ? H10J C105 H10L 109.5 . . ? H10K C105 H10L 109.5 . . ? C106 N16 C106 117.8(9) 2_857 . ? C106 N16 Fe5 121.1(5) 2_857 . ? C106 N16 Fe5 121.1(5) . . ? N16 C106 C107 121.9(7) . . ? N16 C106 H10M 119.1 . . ? C107 C106 H10M 119.1 . . ? N17 C107 C106 121.3(7) . . ? N17 C107 H10N 119.3 . . ? C106 C107 H10N 119.3 . . ? C107 N17 C107 115.8(9) . 2_857 ? C107 N17 Fe6 122.1(4) . . ? C107 N17 Fe6 122.1(4) 2_857 . ? O6 Fe6 O6 179.7(3) 2_857 . ? O6 Fe6 N18 91.8(2) 2_857 . ? O6 Fe6 N18 88.2(2) . . ? O6 Fe6 N18 88.2(2) 2_857 2_857 ? O6 Fe6 N18 91.8(2) . 2_857 ? N18 Fe6 N18 174.4(4) . 2_857 ? O6 Fe6 N17 89.84(15) 2_857 . ? O6 Fe6 N17 89.84(15) . . ? N18 Fe6 N17 92.80(18) . . ? N18 Fe6 N17 92.80(18) 2_857 . ? O6 Fe6 N10 90.16(15) 2_857 1_565 ? O6 Fe6 N10 90.16(15) . 1_565 ? N18 Fe6 N10 87.20(18) . 1_565 ? N18 Fe6 N10 87.20(18) 2_857 1_565 ? N17 Fe6 N10 180.000(4) . 1_565 ? C108 O6 Fe6 131.8(5) . . ? O6 C108 C109 119.8(8) . . ? O6 C108 C113 125.5(7) . . ? C109 C108 C113 114.7(8) . . ? C108 C109 C110 120.8(9) . . ? C108 C109 H10O 119.6 . . ? C110 C109 H10O 119.6 . . ? C111 C110 C109 123.0(7) . . ? C111 C110 H11D 118.5 . . ? C109 C110 H11D 118.5 . . ? C110 C111 C112 118.3(8) . . ? C110 C111 C123 122.4(7) . . ? C112 C111 C123 119.3(8) . . ? C113 C112 C111 121.5(8) . . ? C113 C112 H11E 119.3 . . ? C111 C112 H11E 119.3 . . ? C112 C113 C114 118.2(8) . . ? C112 C113 C108 121.7(7) . . ? C114 C113 C108 120.1(8) . . ? N18 C114 C113 129.4(8) . . ? N18 C114 H11F 115.3 . . ? C113 C114 H11F 115.3 . . ? C114 N18 C115 117.7(7) . . ? C114 N18 Fe6 124.8(5) . . ? C115 N18 Fe6 117.6(5) . . ? N18 C115 C117 109.2(6) . . ? N18 C115 C116 116.6(6) . . ? C117 C115 C116 108.6(6) . . ? N18 C115 H11G 107.4 . . ? C117 C115 H11G 107.4 . . ? C116 C115 H11G 107.4 . . ? C115 C116 H11H 109.5 . . ? C115 C116 H11I 109.5 . . ? H11H C116 H11I 109.5 . . ? C115 C116 H11J 109.5 . . ? H11H C116 H11J 109.5 . . ? H11I C116 H11J 109.5 . . ? C118 C117 C122 118.0(7) . . ? C118 C117 C115 125.1(6) . . ? C122 C117 C115 116.7(7) . . ? C119 C118 C117 121.4(7) . . ? C119 C118 H11K 119.3 . . ? C117 C118 H11K 119.3 . . ? C118 C119 C120 122.4(8) . . ? C118 C119 H11L 118.8 . . ? C120 C119 H11L 118.8 . . ? C121 C120 C119 117.2(7) . . ? C121 C120 H12A 121.4 . . ? C119 C120 H12A 121.4 . . ? C120 C121 C122 122.5(7) . . ? C120 C121 H12B 118.8 . . ? C122 C121 H12B 118.8 . . ? C117 C122 C121 118.5(7) . . ? C117 C122 H12C 120.8 . . ? C121 C122 H12C 120.8 . . ? C111 C123 C124 114.8(7) . . ? C111 C123 C125 110.9(6) . . ? C124 C123 C125 107.9(6) . . ? C111 C123 C126 110.2(6) . . ? C124 C123 C126 104.9(6) . . ? C125 C123 C126 107.8(7) . . ? C123 C124 H12D 109.5 . . ? C123 C124 H12E 109.5 . . ? H12D C124 H12E 109.5 . . ? C123 C124 H12F 109.5 . . ? H12D C124 H12F 109.5 . . ? H12E C124 H12F 109.5 . . ? C123 C125 H12G 109.5 . . ? C123 C125 H12H 109.5 . . ? H12G C125 H12H 109.5 . . ? C123 C125 H12I 109.5 . . ? H12G C125 H12I 109.5 . . ? H12H C125 H12I 109.5 . . ? C123 C126 H12J 109.5 . . ? C123 C126 H12K 109.5 . . ? H12J C126 H12K 109.5 . . ? C123 C126 H12L 109.5 . . ? H12J C126 H12L 109.5 . . ? H12K C126 H12L 109.5 . . ? N300 C301 C302 179.3(10) . . ? C301 C302 H30B 109.5 . . ? C301 C302 H30C 109.5 . . ? H30B C302 H30C 109.5 . . ? C301 C302 H30D 109.5 . . ? H30B C302 H30D 109.5 . . ? H30C C302 H30D 109.5 . . ? N400 C401 C402 174.3 . . ? C401 C402 H40D 109.5 . . ? C401 C402 H40E 109.5 . . ? H40D C402 H40E 109.5 . . ? C401 C402 H40F 109.5 . . ? H40D C402 H40F 109.5 . . ? H40E C402 H40F 109.5 . . ? N500 C501 C502 171.5(12) . . ? C501 C502 H50A 109.5 . . ? C501 C502 H50B 109.5 . . ? H50A C502 H50B 109.5 . . ? C501 C502 H50C 109.5 . . ? H50A C502 H50C 109.5 . . ? H50B C502 H50C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.914 _diffrn_reflns_theta_full 28.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.139 _refine_diff_density_min -0.613 _refine_diff_density_rms 0.085 #===END data_jb30 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35.50 H32.25 Fe N6.75 O6' _chemical_formula_weight 705.28 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 P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 7.3694(6) _cell_length_b 19.797(3) _cell_length_c 12.1347(18) _cell_angle_alpha 90.00 _cell_angle_beta 102.388(12) _cell_angle_gamma 90.00 _cell_volume 1729.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3514 _cell_measurement_theta_min 2.67 _cell_measurement_theta_max 29.37 _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.355 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 733 _exptl_absorpt_coefficient_mu 0.491 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; The tiny crystal (smallest dimension less than 0.01mm) was mounted on a fibre of glass wool with Araldite. The data collection nominally covered over a hemisphere of Reciprocal space, by a combination of eighteen sets of exposures at different \w and \f angles for the crystal; each 80s exposure covered 1.0\% in \w. There was virtually no data beyond 50 degrees 2 theta. The crystal-to-detector distance was 5.5 cm. Crystal decay was found to be negligible by by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms; H-atoms were given isotropic displacement parameter equal to 1.2 (or 1.5 for methyl H-atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. The solvent acetonitrile was modelled at 75% occupancy. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 10.2833 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 34948 _diffrn_reflns_av_R_equivalents 0.1937 _diffrn_reflns_av_sigmaI/netI 0.2814 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.68 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6087 _reflns_number_gt 2148 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0312P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881, 3973 Friedel Pairs' _refine_ls_abs_structure_Flack 0.05(3) _chemical_absolute_configuration rmad _refine_ls_number_reflns 6087 _refine_ls_number_parameters 453 _refine_ls_number_restraints 37 _refine_ls_R_factor_all 0.1659 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.0990 _refine_ls_wR_factor_gt 0.0833 _refine_ls_goodness_of_fit_ref 0.689 _refine_ls_restrained_S_all 0.708 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.70039(14) 0.85307(8) 0.11531(10) 0.0425(3) Uani 1 1 d . . . O1 O 0.6565(7) 0.9126(3) -0.0214(5) 0.0418(16) Uani 1 1 d . . . C1 C 0.6025(11) 0.9008(5) -0.1277(8) 0.048(3) Uani 1 1 d . . . C2 C 0.5648(10) 0.9574(5) -0.2021(7) 0.059(2) Uani 1 1 d . . . H2A H 0.5841 1.0009 -0.1730 0.071 Uiso 1 1 calc R . . C3 C 0.4994(10) 0.9483(5) -0.3179(7) 0.061(3) Uani 1 1 d . . . H3A H 0.4746 0.9857 -0.3652 0.073 Uiso 1 1 calc R . . C4 C 0.4711(12) 0.8830(5) -0.3632(7) 0.054(3) Uani 1 1 d . . . N3 N 0.3954(13) 0.8734(5) -0.4847(7) 0.073(3) Uani 1 1 d . . . O3A O 0.3530(11) 0.9252(4) -0.5409(7) 0.118(3) Uani 1 1 d U . . O3B O 0.3746(11) 0.8156(4) -0.5212(6) 0.100(3) Uani 1 1 d U . . C5 C 0.5066(10) 0.8304(5) -0.2950(7) 0.056(3) Uani 1 1 d . . . H5A H 0.4880 0.7874 -0.3263 0.067 Uiso 1 1 calc R . . C6 C 0.5706(10) 0.8359(5) -0.1782(7) 0.041(2) Uani 1 1 d . . . C7 C 0.5968(11) 0.7748(5) -0.1133(9) 0.048(3) Uani 1 1 d . . . H7A H 0.5795 0.7349 -0.1547 0.058 Uiso 1 1 calc R . . N1 N 0.6414(8) 0.7677(4) -0.0047(6) 0.039(2) Uani 1 1 d . . . C8 C 0.6431(10) 0.6970(4) 0.0434(7) 0.052(2) Uani 1 1 d . . . H8A H 0.7506 0.6935 0.1067 0.063 Uiso 1 1 calc R . . C9 C 0.6566(10) 0.6395(4) -0.0386(7) 0.071(3) Uani 1 1 d . . . H9A H 0.7578 0.6480 -0.0750 0.106 Uiso 1 1 calc R . . H9B H 0.5428 0.6367 -0.0945 0.106 Uiso 1 1 calc R . . H9C H 0.6777 0.5976 0.0020 0.106 Uiso 1 1 calc R . . C10 C 0.4700(10) 0.6882(4) 0.0899(7) 0.050(2) Uani 1 1 d . . . C11 C 0.4859(12) 0.6631(4) 0.2009(7) 0.066(3) Uani 1 1 d . . . H11A H 0.6019 0.6518 0.2442 0.079 Uiso 1 1 calc R . . C12 C 0.3272(15) 0.6554(5) 0.2451(8) 0.083(3) Uani 1 1 d . . . H12A H 0.3360 0.6387 0.3177 0.099 Uiso 1 1 calc R . . C13 C 0.1555(12) 0.6732(5) 0.1785(10) 0.082(3) Uani 1 1 d . . . H13A H 0.0495 0.6698 0.2082 0.099 Uiso 1 1 calc R . . C14 C 0.1399(12) 0.6955(5) 0.0710(9) 0.077(3) Uani 1 1 d . . . H14A H 0.0239 0.7065 0.0273 0.093 Uiso 1 1 calc R . . C15 C 0.2963(11) 0.7019(4) 0.0269(7) 0.060(2) Uani 1 1 d . . . H15A H 0.2838 0.7158 -0.0476 0.072 Uiso 1 1 calc R . . O2 O 0.7573(7) 0.7903(3) 0.2465(5) 0.0427(18) Uani 1 1 d . . . C16 C 0.8103(10) 0.7982(5) 0.3561(8) 0.038(3) Uani 1 1 d . . . C17 C 0.8546(10) 0.7395(4) 0.4278(7) 0.056(2) Uani 1 1 d . . . H17A H 0.8438 0.6967 0.3952 0.067 Uiso 1 1 calc R . . C18 C 0.9105(10) 0.7450(5) 0.5398(8) 0.057(3) Uani 1 1 d . . . H18A H 0.9326 0.7062 0.5838 0.068 Uiso 1 1 calc R . . C19 C 0.9356(11) 0.8067(6) 0.5900(7) 0.055(2) Uani 1 1 d . . . N4 N 1.0018(13) 0.8136(5) 0.7113(8) 0.087(3) Uani 1 1 d . . . O4A O 1.0266(10) 0.7612(4) 0.7645(6) 0.107(3) Uani 1 1 d U . . O4B O 1.0337(10) 0.8704(4) 0.7522(5) 0.096(3) Uani 1 1 d U . . C20 C 0.8977(9) 0.8673(5) 0.5262(6) 0.053(3) Uani 1 1 d U . . H20A H 0.9145 0.9092 0.5617 0.064 Uiso 1 1 calc R . . C21 C 0.8345(8) 0.8628(6) 0.4087(6) 0.039(2) Uani 1 1 d . . . C22 C 0.7943(12) 0.9267(5) 0.3470(9) 0.046(3) Uani 1 1 d . . . H22A H 0.8074 0.9663 0.3893 0.056 Uiso 1 1 calc R . . N2 N 0.7434(9) 0.9324(4) 0.2410(6) 0.039(2) Uani 1 1 d . . . C23 C 0.7090(10) 1.0060(4) 0.1968(7) 0.048(2) Uani 1 1 d . . . H23A H 0.6104 1.0032 0.1285 0.057 Uiso 1 1 calc R . . C24 C 0.8816(11) 1.0290(4) 0.1584(7) 0.083(3) Uani 1 1 d . . . H24A H 0.9064 0.9986 0.1017 0.125 Uiso 1 1 calc R . . H24B H 0.9854 1.0293 0.2215 0.125 Uiso 1 1 calc R . . H24C H 0.8622 1.0737 0.1274 0.125 Uiso 1 1 calc R . . C25 C 0.6365(12) 1.0514(4) 0.2759(6) 0.051(2) Uani 1 1 d . . . C26 C 0.7316(11) 1.1070(5) 0.3264(8) 0.083(3) Uani 1 1 d . . . H26A H 0.8463 1.1174 0.3104 0.099 Uiso 1 1 calc R . . C27 C 0.6622(14) 1.1482(5) 0.4005(8) 0.089(3) Uani 1 1 d . . . H27A H 0.7349 1.1833 0.4373 0.106 Uiso 1 1 calc R . . C28 C 0.4894(15) 1.1379(5) 0.4196(8) 0.087(3) Uani 1 1 d . . . H28A H 0.4386 1.1674 0.4645 0.105 Uiso 1 1 calc R . . C29 C 0.3912(13) 1.0822(6) 0.3701(9) 0.086(3) Uani 1 1 d . . . H29A H 0.2766 1.0726 0.3868 0.103 Uiso 1 1 calc R . . C30 C 0.4579(13) 1.0403(5) 0.2966(8) 0.080(3) Uani 1 1 d . . . H30A H 0.3851 1.0049 0.2610 0.096 Uiso 1 1 calc R . . N5 N 1.0134(6) 0.8550(4) 0.1175(4) 0.0421(13) Uani 1 1 d . . . C31 C 1.1455(8) 0.8468(6) 0.2092(5) 0.053(2) Uani 1 1 d . . . H31A H 1.1110 0.8402 0.2777 0.063 Uiso 1 1 calc R . . C32 C 1.3292(7) 0.8474(5) 0.2079(5) 0.0407(18) Uani 1 1 d . . . H32A H 1.4145 0.8410 0.2756 0.049 Uiso 1 1 calc R . . N6 N 1.3932(6) 0.8567(4) 0.1143(4) 0.0434(13) Uani 1 1 d . . . C33 C 1.2612(8) 0.8687(4) 0.0213(5) 0.043(2) Uani 1 1 d . . . H33A H 1.2976 0.8782 -0.0458 0.051 Uiso 1 1 calc R . . C34 C 1.0742(9) 0.8674(5) 0.0210(6) 0.047(3) Uani 1 1 d . . . H34A H 0.9883 0.8751 -0.0460 0.057 Uiso 1 1 calc R . . N7 N 1.067(2) 1.0569(9) 0.6023(13) 0.136(6) Uani 0.75 1 d P . . C35 C 1.074(2) 1.0403(9) 0.6899(15) 0.099(6) Uani 0.75 1 d P . . C36 C 1.0659(17) 1.0187(7) 0.7994(11) 0.106(5) Uani 0.75 1 d PU . . H36A H 1.1879 1.0204 0.8471 0.159 Uiso 0.75 1 calc PR . . H36B H 1.0198 0.9733 0.7963 0.159 Uiso 0.75 1 calc PR . . H36C H 0.9842 1.0479 0.8295 0.159 Uiso 0.75 1 calc PR . . 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 0.0374(5) 0.0556(7) 0.0335(5) 0.0038(8) 0.0056(4) 0.0010(8) O1 0.031(3) 0.068(5) 0.027(4) 0.003(3) 0.006(3) 0.001(3) C1 0.036(5) 0.077(9) 0.034(7) 0.028(6) 0.012(5) 0.007(5) C2 0.072(6) 0.066(7) 0.041(6) 0.003(5) 0.013(5) -0.003(5) C3 0.066(6) 0.075(8) 0.045(6) 0.015(6) 0.017(4) 0.003(5) C4 0.075(6) 0.066(8) 0.019(5) 0.000(5) 0.009(5) -0.008(4) N3 0.092(6) 0.073(8) 0.054(6) 0.010(5) 0.017(5) -0.001(5) O3A 0.144(4) 0.112(4) 0.092(4) 0.010(3) 0.012(3) 0.001(3) O3B 0.131(5) 0.107(5) 0.052(4) 0.004(4) -0.003(4) -0.016(5) C5 0.053(5) 0.087(10) 0.028(5) 0.008(5) 0.009(4) -0.006(5) C6 0.038(4) 0.045(7) 0.040(6) -0.009(5) 0.005(4) -0.001(4) C7 0.025(5) 0.061(7) 0.057(7) -0.013(6) 0.008(5) 0.002(4) N1 0.032(4) 0.055(6) 0.027(4) -0.014(4) 0.000(3) -0.003(4) C8 0.043(5) 0.033(6) 0.073(6) -0.008(5) -0.005(4) 0.010(4) C9 0.082(6) 0.050(6) 0.076(6) -0.002(5) 0.008(5) -0.009(5) C10 0.044(5) 0.042(6) 0.059(6) 0.005(4) 0.003(4) 0.006(4) C11 0.063(6) 0.060(7) 0.068(6) 0.015(5) -0.001(5) -0.001(5) C12 0.093(7) 0.089(8) 0.073(7) 0.012(6) 0.031(7) -0.008(6) C13 0.041(6) 0.082(8) 0.122(9) -0.002(7) 0.015(6) -0.010(5) C14 0.060(6) 0.083(8) 0.084(8) 0.000(6) 0.003(5) -0.009(5) C15 0.055(5) 0.064(6) 0.062(5) 0.003(4) 0.011(5) 0.000(5) O2 0.039(3) 0.062(5) 0.026(4) 0.002(3) 0.004(3) 0.002(3) C16 0.017(4) 0.066(7) 0.034(6) 0.006(5) 0.009(4) 0.000(5) C17 0.063(6) 0.045(6) 0.053(6) 0.012(5) -0.002(5) 0.000(5) C18 0.050(5) 0.072(8) 0.047(6) 0.022(6) 0.007(4) 0.006(5) C19 0.059(6) 0.078(8) 0.024(5) 0.002(6) -0.003(4) 0.004(5) N4 0.112(7) 0.072(7) 0.076(7) 0.016(6) 0.020(5) 0.012(6) O4A 0.137(4) 0.098(4) 0.080(4) 0.007(3) 0.008(3) 0.010(3) O4B 0.133(5) 0.092(6) 0.053(4) -0.010(4) 0.001(3) -0.002(4) C20 0.052(4) 0.067(6) 0.041(5) 0.000(5) 0.009(3) 0.006(4) C21 0.043(4) 0.049(7) 0.026(5) -0.005(6) 0.009(3) -0.004(6) C22 0.048(6) 0.040(6) 0.048(7) 0.005(5) 0.004(5) -0.002(5) N2 0.041(5) 0.044(5) 0.030(5) 0.002(4) 0.005(4) 0.007(4) C23 0.049(5) 0.046(6) 0.045(5) 0.012(5) 0.003(4) 0.000(4) C24 0.114(8) 0.061(7) 0.091(7) 0.003(5) 0.058(6) 0.000(6) C25 0.075(6) 0.039(6) 0.035(4) -0.007(4) 0.006(4) 0.009(5) C26 0.061(6) 0.078(8) 0.104(8) -0.025(6) 0.008(5) 0.005(6) C27 0.082(7) 0.067(8) 0.115(9) -0.034(6) 0.018(6) 0.002(6) C28 0.090(8) 0.082(8) 0.087(7) -0.032(6) 0.014(6) 0.012(6) C29 0.070(6) 0.103(9) 0.089(7) -0.003(6) 0.028(6) 0.025(6) C30 0.064(6) 0.100(8) 0.075(7) -0.011(6) 0.012(5) -0.005(6) N5 0.035(3) 0.056(4) 0.036(3) -0.002(5) 0.009(3) 0.001(5) C31 0.038(4) 0.098(7) 0.023(4) -0.006(6) 0.011(3) -0.020(7) C32 0.038(4) 0.061(6) 0.023(4) -0.008(5) 0.007(3) -0.004(6) N6 0.040(3) 0.058(4) 0.035(3) -0.004(5) 0.014(3) 0.004(5) C33 0.027(3) 0.064(7) 0.040(4) 0.015(4) 0.012(3) 0.003(4) C34 0.040(4) 0.075(8) 0.027(4) 0.006(5) 0.006(4) 0.008(5) N7 0.105(10) 0.120(13) 0.175(17) 0.006(13) 0.010(13) 0.031(9) C35 0.080(10) 0.073(13) 0.135(17) -0.018(14) 0.005(13) 0.014(9) C36 0.097(6) 0.093(7) 0.124(7) -0.016(5) 0.016(5) -0.003(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 O2 1.993(6) . ? Fe1 O1 2.005(6) . ? Fe1 N2 2.165(7) . ? Fe1 N1 2.212(7) . ? Fe1 N6 2.262(5) 1_455 ? Fe1 N5 2.301(4) . ? O1 C1 1.286(10) . ? C1 C6 1.421(12) . ? C1 C2 1.429(11) . ? C2 C3 1.396(10) . ? C2 H2A 0.9300 . ? C3 C4 1.403(11) . ? C3 H3A 0.9300 . ? C4 C5 1.322(10) . ? C4 N3 1.473(11) . ? N3 O3B 1.226(9) . ? N3 O3A 1.233(10) . ? C5 C6 1.398(10) . ? C5 H5A 0.9300 . ? C6 C7 1.435(12) . ? C7 N1 1.296(10) . ? C7 H7A 0.9300 . ? N1 C8 1.516(9) . ? C8 C10 1.511(9) . ? C8 C9 1.530(9) . ? C8 H8A 0.9800 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C15 1.370(9) . ? C10 C11 1.416(10) . ? C11 C12 1.396(10) . ? C11 H11A 0.9300 . ? C12 C13 1.393(11) . ? C12 H12A 0.9300 . ? C13 C14 1.359(11) . ? C13 H13A 0.9300 . ? C14 C15 1.377(10) . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? O2 C16 1.312(10) . ? C16 C21 1.424(13) . ? C16 C17 1.447(11) . ? C17 C18 1.337(10) . ? C17 H17A 0.9300 . ? C18 C19 1.361(11) . ? C18 H18A 0.9300 . ? C19 C20 1.422(12) . ? C19 N4 1.455(12) . ? N4 O4A 1.214(10) . ? N4 O4B 1.232(10) . ? C20 C21 1.404(9) . ? C20 H20A 0.9300 . ? C21 C22 1.468(13) . ? C22 N2 1.265(10) . ? C22 H22A 0.9300 . ? N2 C23 1.553(9) . ? C23 C25 1.495(10) . ? C23 C24 1.516(10) . ? C23 H23A 0.9800 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.377(10) . ? C25 C30 1.409(10) . ? C26 C27 1.390(11) . ? C26 H26A 0.9300 . ? C27 C28 1.358(11) . ? C27 H27A 0.9300 . ? C28 C29 1.384(11) . ? C28 H28A 0.9300 . ? C29 C30 1.383(11) . ? C29 H29A 0.9300 . ? C30 H30A 0.9300 . ? N5 C31 1.322(6) . ? N5 C34 1.363(7) . ? C31 C32 1.357(7) . ? C31 H31A 0.9300 . ? C32 N6 1.333(6) . ? C32 H32A 0.9300 . ? N6 C33 1.344(6) . ? N6 Fe1 2.262(4) 1_655 ? C33 C34 1.377(7) . ? C33 H33A 0.9300 . ? C34 H34A 0.9300 . ? N7 C35 1.104(19) . ? C35 C36 1.409(18) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? 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 O2 Fe1 O1 175.9(3) . . ? O2 Fe1 N2 85.2(2) . . ? O1 Fe1 N2 97.4(3) . . ? O2 Fe1 N1 91.6(3) . . ? O1 Fe1 N1 86.0(2) . . ? N2 Fe1 N1 175.2(3) . . ? O2 Fe1 N6 93.6(2) . 1_455 ? O1 Fe1 N6 89.6(2) . 1_455 ? N2 Fe1 N6 88.6(3) . 1_455 ? N1 Fe1 N6 88.0(2) . 1_455 ? O2 Fe1 N5 87.9(2) . . ? O1 Fe1 N5 89.0(2) . . ? N2 Fe1 N5 89.1(2) . . ? N1 Fe1 N5 94.3(3) . . ? N6 Fe1 N5 177.2(4) 1_455 . ? C1 O1 Fe1 133.0(6) . . ? O1 C1 C6 125.8(9) . . ? O1 C1 C2 117.8(10) . . ? C6 C1 C2 116.3(8) . . ? C3 C2 C1 120.9(9) . . ? C3 C2 H2A 119.5 . . ? C1 C2 H2A 119.5 . . ? C2 C3 C4 120.2(9) . . ? C2 C3 H3A 119.9 . . ? C4 C3 H3A 119.9 . . ? C5 C4 C3 119.3(8) . . ? C5 C4 N3 120.4(8) . . ? C3 C4 N3 120.2(8) . . ? O3B N3 O3A 125.4(10) . . ? O3B N3 C4 118.3(8) . . ? O3A N3 C4 116.3(9) . . ? C4 C5 C6 123.4(9) . . ? C4 C5 H5A 118.3 . . ? C6 C5 H5A 118.3 . . ? C5 C6 C1 119.9(8) . . ? C5 C6 C7 117.8(9) . . ? C1 C6 C7 122.4(7) . . ? N1 C7 C6 128.6(10) . . ? N1 C7 H7A 115.7 . . ? C6 C7 H7A 115.7 . . ? C7 N1 C8 118.1(7) . . ? C7 N1 Fe1 124.0(7) . . ? C8 N1 Fe1 117.9(5) . . ? C10 C8 N1 108.2(6) . . ? C10 C8 C9 109.6(6) . . ? N1 C8 C9 115.6(7) . . ? C10 C8 H8A 107.7 . . ? N1 C8 H8A 107.7 . . ? C9 C8 H8A 107.7 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C15 C10 C11 118.5(8) . . ? C15 C10 C8 122.1(7) . . ? C11 C10 C8 119.4(7) . . ? C12 C11 C10 119.9(8) . . ? C12 C11 H11A 120.0 . . ? C10 C11 H11A 120.0 . . ? C13 C12 C11 118.8(9) . . ? C13 C12 H12A 120.6 . . ? C11 C12 H12A 120.6 . . ? C14 C13 C12 121.2(9) . . ? C14 C13 H13A 119.4 . . ? C12 C13 H13A 119.4 . . ? C13 C14 C15 119.9(9) . . ? C13 C14 H14A 120.1 . . ? C15 C14 H14A 120.1 . . ? C10 C15 C14 121.6(8) . . ? C10 C15 H15A 119.2 . . ? C14 C15 H15A 119.2 . . ? C16 O2 Fe1 134.5(6) . . ? O2 C16 C21 122.9(9) . . ? O2 C16 C17 119.6(9) . . ? C21 C16 C17 117.5(8) . . ? C18 C17 C16 121.7(9) . . ? C18 C17 H17A 119.1 . . ? C16 C17 H17A 119.1 . . ? C17 C18 C19 120.8(9) . . ? C17 C18 H18A 119.6 . . ? C19 C18 H18A 119.6 . . ? C18 C19 C20 121.5(7) . . ? C18 C19 N4 121.4(9) . . ? C20 C19 N4 117.2(10) . . ? O4A N4 O4B 124.9(10) . . ? O4A N4 C19 116.0(10) . . ? O4B N4 C19 119.1(9) . . ? C21 C20 C19 118.8(9) . . ? C21 C20 H20A 120.6 . . ? C19 C20 H20A 120.6 . . ? C20 C21 C16 119.7(9) . . ? C20 C21 C22 116.7(10) . . ? C16 C21 C22 123.6(6) . . ? N2 C22 C21 125.4(10) . . ? N2 C22 H22A 117.3 . . ? C21 C22 H22A 117.3 . . ? C22 N2 C23 115.2(8) . . ? C22 N2 Fe1 128.1(8) . . ? C23 N2 Fe1 116.7(5) . . ? C25 C23 C24 117.2(7) . . ? C25 C23 N2 113.3(6) . . ? C24 C23 N2 107.6(6) . . ? C25 C23 H23A 106.0 . . ? C24 C23 H23A 106.0 . . ? N2 C23 H23A 106.0 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C30 116.8(8) . . ? C26 C25 C23 123.3(8) . . ? C30 C25 C23 119.8(8) . . ? C25 C26 C27 122.3(8) . . ? C25 C26 H26A 118.8 . . ? C27 C26 H26A 118.8 . . ? C28 C27 C26 120.7(9) . . ? C28 C27 H27A 119.7 . . ? C26 C27 H27A 119.7 . . ? C27 C28 C29 117.9(9) . . ? C27 C28 H28A 121.0 . . ? C29 C28 H28A 121.0 . . ? C30 C29 C28 122.2(9) . . ? C30 C29 H29A 118.9 . . ? C28 C29 H29A 118.9 . . ? C29 C30 C25 119.7(9) . . ? C29 C30 H30A 120.1 . . ? C25 C30 H30A 120.1 . . ? C31 N5 C34 115.3(5) . . ? C31 N5 Fe1 124.3(4) . . ? C34 N5 Fe1 120.4(4) . . ? N5 C31 C32 123.1(6) . . ? N5 C31 H31A 118.5 . . ? C32 C31 H31A 118.5 . . ? N6 C32 C31 123.2(5) . . ? N6 C32 H32A 118.4 . . ? C31 C32 H32A 118.4 . . ? C32 N6 C33 114.5(5) . . ? C32 N6 Fe1 121.9(4) . 1_655 ? C33 N6 Fe1 123.6(4) . 1_655 ? N6 C33 C34 122.9(6) . . ? N6 C33 H33A 118.6 . . ? C34 C33 H33A 118.6 . . ? N5 C34 C33 120.9(6) . . ? N5 C34 H34A 119.5 . . ? C33 C34 H34A 119.5 . . ? N7 C35 C36 175(2) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 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 C31 H31A O3A 0.93 3.03 3.458(11) 109.9 1_656 C32 H32A O3B 0.93 2.59 3.293(10) 132.3 1_656 C31 H31A O3A 0.93 3.03 3.458(11) 109.9 1_656 C32 H32A O3B 0.93 2.59 3.293(10) 132.3 1_656 C18 H18A O4A 0.93 2.41 2.697(12) 97.5 . C34 H34A O4B 0.93 2.54 3.212(9) 129.1 1_554 C36 H36B O4B 0.96 2.11 2.991(16) 151.4 . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.303 _refine_diff_density_min -0.264 _refine_diff_density_rms 0.049 #===END data_jb35 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H54 Fe N6 O8.50' _chemical_formula_weight 930.84 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 P2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' _cell_length_a 13.3100(3) _cell_length_b 11.6027(2) _cell_length_c 15.9378(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.807(2) _cell_angle_gamma 90.00 _cell_volume 2390.19(9) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9637 _cell_measurement_theta_min 2.87 _cell_measurement_theta_max 29.06 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.293 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 980 _exptl_absorpt_coefficient_mu 0.376 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.86 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'ABSPACK(CrysAlis, Oxford Diffraction)' _exptl_special_details ; The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cobra. The data collection nominally covered over a hemisphere of Reciprocal space, by a combination of four sets of exposures with different \f angles for the crystal; each 40 s exposure covered 1.0\% in \w. The crystal-to-detector distance was 5.5 cm. Crystal decay was found to be negligible by by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms; H-atoms were given isotropic displacement parameter equal to 1.2 (or 1.5 for methyl H-atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. The unit cell contains two polymeric units composed of an iron with two phenoxy imine ligands and a 4,4'-bipyridyl. One chain lies on the two fold axis through the centre of the cell and the other at the corners. In the first polymer, Fe1 and the nitrogens and two of the carbons of the 4,4'-bipyridyl (N3, N4 C18 and C19) lie on the two fold axis. In the second polymer Fe2 and the nitrogens and two of the carbons of the coordinated 4,4'-bipyridyl (N7, N8, C39 and C40) lie on the other two fold axis. The polymers run infinitely along the "b" axis of the cell. There are five molecules of THF in the unit cell, two and a half in the asymmetric unit. THF (O100-C104) was refined as fully occupied. One fully occupied THF was modeled as disordered over two positions (O200-C204 and C20A-C24A) in a 50:50 ratio. The position of the oxygen in component C20A-C24A could not be determined. THF (O300-C304) was modeled as half occupied and lies on a two fold axis (but has no atoms on the axis). The molecule had two puckered forms related by the two fold axis. The atom in the pucker was modeled as the oxygen (O300). THF (C400-C402) was modeled as half occupied with the two fold axis running through the THF and C400 lying on the two fold axis. The oxygen position could not be determined. The formula for the cell contents has been modified to reflect the actual contents of the cell so as to calculate the correct density as no hydrogens were added to the minor component THF molecules and the assignment of their oxygen atoms could not be determined. These partially occupied and disordered THFs were refined isotropically. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 10.2833 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 23230 _diffrn_reflns_av_R_equivalents 0.0381 _diffrn_reflns_av_sigmaI/netI 0.0864 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.24 _diffrn_reflns_theta_max 29.14 _reflns_number_total 11055 _reflns_number_gt 7838 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0810P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881, 4944 friedel pairs' _refine_ls_abs_structure_Flack 0.016(15) _chemical_absolute_configuration rmad _refine_ls_number_reflns 11055 _refine_ls_number_parameters 590 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0805 _refine_ls_R_factor_gt 0.0561 _refine_ls_wR_factor_ref 0.1413 _refine_ls_wR_factor_gt 0.1342 _refine_ls_goodness_of_fit_ref 0.975 _refine_ls_restrained_S_all 0.987 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.5000 0.42372(5) 0.5000 0.01539(16) Uani 1 2 d S . . O1 O 0.54966(15) 0.4238(2) 0.38959(15) 0.0187(5) Uani 1 1 d . . . N1 N 0.66108(19) 0.4228(2) 0.56657(17) 0.0165(5) Uani 1 1 d . . . C1 C 0.6408(2) 0.4338(3) 0.3735(2) 0.0167(7) Uani 1 1 d . . . C2 C 0.6488(3) 0.4431(3) 0.2866(2) 0.0222(8) Uani 1 1 d . . . H2A H 0.5874 0.4429 0.2416 0.027 Uiso 1 1 calc R . . O2B O 0.9359(2) 0.4471(2) 0.23454(18) 0.0326(7) Uani 1 1 d . . . N2 N 0.9322(2) 0.4594(3) 0.3092(2) 0.0256(7) Uani 1 1 d . . . O2A O 1.0096(2) 0.4785(3) 0.3686(2) 0.0394(8) Uani 1 1 d . . . N3 N 0.5000 0.6184(4) 0.5000 0.0165(9) Uani 1 2 d S . . C3 C 0.7431(3) 0.4525(3) 0.2656(2) 0.0232(8) Uani 1 1 d . . . H3A H 0.7470 0.4582 0.2070 0.028 Uiso 1 1 calc R . . N4 N 0.5000 1.2298(4) 0.5000 0.0196(10) Uani 1 2 d S . . C4 C 0.8323(2) 0.4534(3) 0.3319(2) 0.0209(8) Uani 1 1 d . . . C5 C 0.8287(3) 0.4456(3) 0.4170(2) 0.0205(8) Uani 1 1 d . . . H5A H 0.8912 0.4479 0.4608 0.025 Uiso 1 1 calc R . . C6 C 0.7344(2) 0.4343(3) 0.4399(2) 0.0192(7) Uani 1 1 d . . . C7 C 0.7381(2) 0.4279(3) 0.5315(2) 0.0200(7) Uani 1 1 d . . . H7A H 0.8049 0.4273 0.5697 0.024 Uiso 1 1 calc R . . C8 C 0.6866(2) 0.4155(3) 0.6628(2) 0.0208(7) Uani 1 1 d . . . H8A H 0.6202 0.4259 0.6808 0.025 Uiso 1 1 calc R . . C9 C 0.7585(3) 0.5113(3) 0.7052(3) 0.0264(9) Uani 1 1 d . . . H9A H 0.7285 0.5860 0.6839 0.040 Uiso 1 1 calc R . . H9B H 0.8258 0.5023 0.6912 0.040 Uiso 1 1 calc R . . H9C H 0.7674 0.5076 0.7680 0.040 Uiso 1 1 calc R . . C10 C 0.7264(3) 0.2949(3) 0.6919(3) 0.0274(9) Uani 1 1 d . . . C11 C 0.6597(3) 0.2103(4) 0.7046(3) 0.0374(10) Uani 1 1 d . . . H11A H 0.5883 0.2278 0.6961 0.045 Uiso 1 1 calc R . . C12 C 0.6940(4) 0.0997(4) 0.7298(3) 0.0431(12) Uani 1 1 d . . . H12A H 0.6462 0.0431 0.7390 0.052 Uiso 1 1 calc R . . C13 C 0.7967(4) 0.0720(4) 0.7413(3) 0.0476(13) Uani 1 1 d . . . H13A H 0.8206 -0.0036 0.7584 0.057 Uiso 1 1 calc R . . C14 C 0.8642(4) 0.1552(4) 0.7277(3) 0.0416(11) Uani 1 1 d . . . H14A H 0.9352 0.1365 0.7348 0.050 Uiso 1 1 calc R . . C15 C 0.8311(3) 0.2657(3) 0.7039(3) 0.0353(10) Uani 1 1 d . . . H15A H 0.8794 0.3223 0.6956 0.042 Uiso 1 1 calc R . . C16 C 0.4586(3) 0.6797(3) 0.5544(2) 0.0231(8) Uani 1 1 d . . . H16A H 0.4285 0.6390 0.5940 0.028 Uiso 1 1 calc R . . C17 C 0.4572(3) 0.7987(3) 0.5565(2) 0.0233(8) Uani 1 1 d . . . H17A H 0.4267 0.8373 0.5968 0.028 Uiso 1 1 calc R . . C18 C 0.5000 0.8622(4) 0.5000 0.0168(12) Uani 1 2 d S . . C19 C 0.5000 0.9902(4) 0.5000 0.0178(12) Uani 1 2 d S . . C20 C 0.4254(3) 1.0530(3) 0.5280(2) 0.0216(8) Uani 1 1 d . . . H20A H 0.3730 1.0143 0.5483 0.026 Uiso 1 1 calc R . . C21 C 0.4276(3) 1.1711(3) 0.5261(2) 0.0213(8) Uani 1 1 d . . . H21A H 0.3750 1.2126 0.5442 0.026 Uiso 1 1 calc R . . Fe2 Fe 1.0000 -0.17388(5) 1.0000 0.01541(17) Uani 1 2 d S . . O3 O 0.88504(16) -0.1773(2) 0.89075(14) 0.0168(5) Uani 1 1 d . . . O4B O 0.41832(19) -0.2635(3) 0.87972(19) 0.0376(7) Uani 1 1 d . . . O4A O 0.41491(19) -0.2646(3) 0.74357(19) 0.0329(7) Uani 1 1 d . . . N5 N 0.8772(2) -0.1667(2) 1.06952(18) 0.0178(6) Uani 1 1 d . . . N6 N 0.4610(2) -0.2551(3) 0.8193(2) 0.0281(7) Uani 1 1 d . . . N7 N 1.0000 -0.3703(3) 1.0000 0.0173(10) Uani 1 2 d S . . N8 N 1.0000 -0.9831(4) 1.0000 0.0149(9) Uani 1 2 d S . . C22 C 0.7865(2) -0.1946(2) 0.8777(2) 0.0159(7) Uani 1 1 d . . . C23 C 0.7279(3) -0.2128(3) 0.7924(2) 0.0206(8) Uani 1 1 d . . . H23A H 0.7626 -0.2125 0.7468 0.025 Uiso 1 1 calc R . . C24 C 0.6233(3) -0.2306(3) 0.7726(2) 0.0224(8) Uani 1 1 d . . . H24A H 0.5863 -0.2426 0.7145 0.027 Uiso 1 1 calc R . . C25 C 0.5718(3) -0.2310(3) 0.8395(3) 0.0222(8) Uani 1 1 d . . . C26 C 0.6243(3) -0.2130(3) 0.9232(3) 0.0243(8) Uani 1 1 d . . . H26A H 0.5875 -0.2125 0.9675 0.029 Uiso 1 1 calc R . . C27 C 0.7318(3) -0.1951(3) 0.9449(2) 0.0195(8) Uani 1 1 d . . . C28 C 0.7809(3) -0.1762(3) 1.0354(2) 0.0230(8) Uani 1 1 d . . . H28A H 0.7360 -0.1703 1.0735 0.028 Uiso 1 1 calc R . . C29 C 0.9053(3) -0.1518(3) 1.1653(3) 0.0242(9) Uani 1 1 d . . . H29A H 0.9801 -0.1300 1.1819 0.029 Uiso 1 1 calc R . . C30 C 0.8954(3) -0.2679(4) 1.2084(3) 0.0328(9) Uani 1 1 d . . . H30A H 0.9361 -0.3262 1.1866 0.049 Uiso 1 1 calc R . . H30B H 0.8226 -0.2914 1.1950 0.049 Uiso 1 1 calc R . . H30C H 0.9212 -0.2605 1.2711 0.049 Uiso 1 1 calc R . . C31 C 0.8458(3) -0.0549(3) 1.1949(2) 0.0236(8) Uani 1 1 d . . . C32 C 0.8668(3) 0.0605(3) 1.1748(3) 0.0297(9) Uani 1 1 d . . . H32A H 0.9178 0.0755 1.1434 0.036 Uiso 1 1 calc R . . C33 C 0.8140(4) 0.1510(4) 1.2004(3) 0.0402(11) Uani 1 1 d . . . H33A H 0.8305 0.2278 1.1879 0.048 Uiso 1 1 calc R . . C34 C 0.7380(4) 0.1315(4) 1.2437(4) 0.0464(12) Uani 1 1 d . . . H34A H 0.7004 0.1941 1.2596 0.056 Uiso 1 1 calc R . . C35 C 0.7170(4) 0.0213(4) 1.2638(3) 0.0430(11) Uani 1 1 d . . . H35A H 0.6651 0.0077 1.2945 0.052 Uiso 1 1 calc R . . C36 C 0.7699(3) -0.0716(4) 1.2401(3) 0.0321(9) Uani 1 1 d . . . H36A H 0.7540 -0.1476 1.2550 0.038 Uiso 1 1 calc R . . C37 C 0.9561(3) -0.4309(3) 0.9294(2) 0.0193(7) Uani 1 1 d . . . H37A H 0.9247 -0.3896 0.8784 0.023 Uiso 1 1 calc R . . C38 C 0.9537(3) -0.5503(3) 0.9262(2) 0.0195(7) Uani 1 1 d . . . H38A H 0.9209 -0.5893 0.8745 0.023 Uiso 1 1 calc R . . C39 C 1.0000 -0.6119(4) 1.0000 0.0179(12) Uani 1 2 d S . . C40 C 1.0000 -0.7398(4) 1.0000 0.0138(11) Uani 1 2 d S . . C41 C 0.9139(3) -0.8021(3) 0.9559(2) 0.0216(8) Uani 1 1 d . . . H41A H 0.8537 -0.7631 0.9248 0.026 Uiso 1 1 calc R . . C42 C 0.9171(3) -0.9211(3) 0.9580(2) 0.0196(8) Uani 1 1 d . . . H42A H 0.8573 -0.9619 0.9281 0.024 Uiso 1 1 calc R . . O100 O 0.7740(3) -0.1228(3) 0.4732(2) 0.0467(8) Uani 1 1 d . . . C101 C 0.7948(4) -0.1129(6) 0.5635(4) 0.0671(19) Uani 1 1 d . . . H10A H 0.7331 -0.1352 0.5843 0.081 Uiso 1 1 calc R . . H10B H 0.8129 -0.0323 0.5813 0.081 Uiso 1 1 calc R . . C102 C 0.8836(4) -0.1914(6) 0.6010(3) 0.0620(16) Uani 1 1 d . . . H10C H 0.9510 -0.1549 0.6018 0.074 Uiso 1 1 calc R . . H10D H 0.8825 -0.2169 0.6601 0.074 Uiso 1 1 calc R . . C103 C 0.8606(5) -0.2877(6) 0.5380(4) 0.0742(18) Uani 1 1 d . . . H10E H 0.8074 -0.3398 0.5511 0.089 Uiso 1 1 calc R . . H10F H 0.9237 -0.3329 0.5380 0.089 Uiso 1 1 calc R . . C104 C 0.8209(4) -0.2269(4) 0.4525(3) 0.0474(12) Uani 1 1 d . . . H10G H 0.8785 -0.2093 0.4251 0.057 Uiso 1 1 calc R . . H10H H 0.7695 -0.2753 0.4126 0.057 Uiso 1 1 calc R . . O200 O 0.7255(4) -0.5963(5) 0.9293(4) 0.0396(14) Uiso 0.50 1 d PU A 1 C201 C 0.7397(8) -0.5357(9) 1.0121(7) 0.043(2) Uiso 0.50 1 d PU A 1 C202 C 0.6351(7) -0.5350(8) 1.0360(6) 0.041(2) Uiso 0.50 1 d PU A 1 C203 C 0.5586(7) -0.5412(8) 0.9438(6) 0.044(2) Uiso 0.50 1 d PU A 1 C204 C 0.6275(8) -0.5545(10) 0.8791(7) 0.045(2) Uiso 0.50 1 d PU A 1 C20A C 0.6970(10) -0.6750(12) 0.9419(8) 0.071(2) Uiso 0.50 1 d PU B 2 C22A C 0.7065(11) -0.4923(12) 1.0104(9) 0.069(3) Uiso 0.50 1 d PU B 2 C21A C 0.7296(11) -0.6200(12) 1.0338(10) 0.078(3) Uiso 0.50 1 d PU B 2 C23A C 0.6131(12) -0.6211(14) 0.8920(10) 0.081(3) Uiso 0.50 1 d PU B 2 C24A C 0.6381(10) -0.4943(12) 0.9206(9) 0.072(3) Uiso 0.50 1 d PU B 2 O300 O 0.9518(14) 0.2311(18) 0.5245(13) 0.089(5) Uiso 0.25 1 d P . . C301 C 0.9439(11) 0.1722(13) 0.4357(9) 0.080(4) Uiso 0.50 1 d P . . C302 C 0.9727(9) 0.0684(11) 0.4485(5) 0.067(3) Uiso 0.50 1 d PD . . C400 C 0.5000 -0.0007(16) 1.0000 0.074(5) Uiso 0.50 2 d SPD . . C401 C 0.5589(11) 0.0557(13) 1.0572(9) 0.085(4) Uiso 0.50 1 d PD . . C402 C 0.5510(8) 0.1801(12) 1.0415(7) 0.077(4) Uiso 0.50 1 d PD . . 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 0.0132(3) 0.0107(3) 0.0242(4) 0.000 0.0083(3) 0.000 O1 0.0136(10) 0.0192(11) 0.0244(13) -0.0009(11) 0.0067(9) -0.0013(11) N1 0.0169(13) 0.0122(12) 0.0210(15) 0.0032(13) 0.0056(11) 0.0048(13) C1 0.0181(15) 0.0069(15) 0.029(2) -0.0028(14) 0.0125(14) 0.0004(14) C2 0.0184(16) 0.0220(19) 0.025(2) -0.0024(15) 0.0039(14) 0.0023(15) O2B 0.0324(14) 0.0388(17) 0.0339(17) 0.0008(13) 0.0225(12) 0.0019(13) N2 0.0233(16) 0.0254(17) 0.032(2) 0.0023(14) 0.0137(15) 0.0035(14) O2A 0.0181(13) 0.063(2) 0.0394(19) -0.0064(15) 0.0117(13) -0.0064(14) N3 0.018(2) 0.013(2) 0.021(3) 0.000 0.0079(19) 0.000 C3 0.0262(19) 0.0229(19) 0.023(2) -0.0013(14) 0.0106(15) 0.0012(15) N4 0.018(2) 0.010(2) 0.032(3) 0.000 0.007(2) 0.000 C4 0.0137(16) 0.0170(17) 0.034(2) 0.0016(14) 0.0106(15) 0.0026(14) C5 0.0181(16) 0.0177(18) 0.027(2) 0.0006(14) 0.0082(14) 0.0022(14) C6 0.0157(16) 0.0151(16) 0.028(2) 0.0023(16) 0.0072(14) 0.0022(16) C7 0.0133(15) 0.0200(16) 0.026(2) 0.0035(17) 0.0042(14) -0.0001(17) C8 0.0160(15) 0.0244(17) 0.024(2) 0.0038(17) 0.0078(14) 0.0010(17) C9 0.029(2) 0.026(2) 0.027(2) -0.0017(17) 0.0123(17) -0.0017(18) C10 0.029(2) 0.028(2) 0.023(2) 0.0012(15) 0.0035(16) -0.0015(17) C11 0.040(2) 0.035(2) 0.033(3) 0.0050(18) 0.0017(19) -0.009(2) C12 0.065(3) 0.024(2) 0.035(3) -0.0003(18) 0.001(2) -0.021(2) C13 0.072(4) 0.031(2) 0.034(3) 0.0082(19) 0.002(2) 0.009(2) C14 0.051(3) 0.035(2) 0.040(3) 0.011(2) 0.013(2) 0.015(2) C15 0.032(2) 0.032(2) 0.044(3) 0.0058(18) 0.015(2) 0.0031(18) C16 0.031(2) 0.0137(16) 0.031(2) 0.0019(15) 0.0189(18) -0.0014(15) C17 0.029(2) 0.0155(17) 0.030(2) -0.0046(14) 0.0161(17) -0.0025(15) C18 0.016(3) 0.012(2) 0.022(3) 0.000 0.003(2) 0.000 C19 0.017(3) 0.015(3) 0.019(3) 0.000 0.000(2) 0.000 C20 0.0191(18) 0.0165(17) 0.032(2) -0.0002(15) 0.0113(16) -0.0027(15) C21 0.0192(18) 0.0123(16) 0.034(2) -0.0010(15) 0.0105(16) 0.0011(14) Fe2 0.0148(3) 0.0084(3) 0.0244(4) 0.000 0.0074(3) 0.000 O3 0.0159(11) 0.0143(10) 0.0222(13) -0.0002(11) 0.0084(9) 0.0011(11) O4B 0.0191(13) 0.0616(19) 0.0357(18) -0.0087(15) 0.0139(12) -0.0041(14) O4A 0.0192(13) 0.0481(17) 0.0316(18) -0.0088(14) 0.0065(12) -0.0075(13) N5 0.0187(14) 0.0147(13) 0.0218(16) 0.0000(13) 0.0083(12) 0.0010(13) N6 0.0162(15) 0.0374(19) 0.031(2) -0.0052(15) 0.0069(15) -0.0028(15) N7 0.017(2) 0.010(2) 0.026(3) 0.000 0.0062(19) 0.000 N8 0.016(2) 0.013(2) 0.018(3) 0.000 0.0079(18) 0.000 C22 0.0188(17) 0.0053(15) 0.025(2) 0.0019(13) 0.0090(15) 0.0018(13) C23 0.0231(18) 0.0178(17) 0.024(2) -0.0008(14) 0.0114(15) -0.0037(15) C24 0.0225(18) 0.0251(19) 0.019(2) -0.0041(14) 0.0047(15) 0.0019(15) C25 0.0147(16) 0.0245(18) 0.030(2) -0.0038(15) 0.0097(15) -0.0002(14) C26 0.0193(17) 0.031(2) 0.024(2) -0.0028(16) 0.0095(15) 0.0023(16) C27 0.0176(17) 0.0154(18) 0.027(2) -0.0039(14) 0.0073(15) -0.0025(15) C28 0.0191(17) 0.0255(18) 0.027(2) 0.0017(18) 0.0110(15) 0.0005(18) C29 0.0203(18) 0.028(2) 0.027(2) -0.0047(15) 0.0096(16) 0.0002(16) C30 0.039(2) 0.032(2) 0.031(2) 0.0064(18) 0.0171(19) 0.012(2) C31 0.0231(17) 0.025(2) 0.024(2) -0.0056(15) 0.0071(15) 0.0003(16) C32 0.036(2) 0.031(2) 0.023(2) -0.0030(16) 0.0105(18) -0.0056(18) C33 0.054(3) 0.026(2) 0.041(3) -0.0030(19) 0.013(2) 0.000(2) C34 0.062(3) 0.031(2) 0.052(3) -0.0110(19) 0.024(2) 0.011(2) C35 0.048(3) 0.043(3) 0.049(3) -0.004(2) 0.033(2) 0.007(2) C36 0.034(2) 0.032(2) 0.034(2) -0.002(2) 0.0146(17) -0.004(2) C37 0.0197(18) 0.0141(16) 0.026(2) 0.0038(14) 0.0088(15) 0.0029(14) C38 0.0211(17) 0.0156(17) 0.022(2) -0.0027(13) 0.0048(14) -0.0006(14) C39 0.020(3) 0.012(2) 0.026(3) 0.000 0.014(2) 0.000 C40 0.015(2) 0.009(2) 0.020(3) 0.000 0.009(2) 0.000 C41 0.0218(18) 0.0134(16) 0.032(2) 0.0033(14) 0.0109(16) 0.0024(14) C42 0.0177(18) 0.0111(15) 0.031(2) -0.0003(14) 0.0072(16) 0.0000(14) O100 0.0459(18) 0.0504(19) 0.044(2) -0.0051(15) 0.0117(15) 0.0162(15) C101 0.041(3) 0.112(5) 0.045(3) -0.019(3) 0.004(2) 0.026(3) C102 0.038(3) 0.115(5) 0.035(3) 0.008(3) 0.011(2) 0.013(3) C103 0.074(4) 0.072(4) 0.071(5) 0.027(3) 0.006(3) 0.005(3) C104 0.048(3) 0.041(3) 0.056(4) 0.009(2) 0.019(2) 0.007(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 O1 2.022(2) 2_656 ? Fe1 O1 2.022(2) . ? Fe1 N1 2.153(3) 2_656 ? Fe1 N1 2.153(3) . ? Fe1 N4 2.250(4) 1_545 ? Fe1 N3 2.259(4) . ? O1 C1 1.303(4) . ? N1 C7 1.280(4) . ? N1 C8 1.492(4) . ? C1 C2 1.418(5) . ? C1 C6 1.430(5) . ? C2 C3 1.379(5) . ? C2 H2A 0.9500 . ? O2B N2 1.211(4) . ? N2 O2A 1.241(4) . ? N2 C4 1.461(4) . ? N3 C16 1.338(4) . ? N3 C16 1.338(4) 2_656 ? C3 C4 1.388(5) . ? C3 H3A 0.9500 . ? N4 C21 1.325(4) . ? N4 C21 1.325(4) 2_656 ? N4 Fe1 2.250(4) 1_565 ? C4 C5 1.371(5) . ? C5 C6 1.394(5) . ? C5 H5A 0.9500 . ? C6 C7 1.452(5) . ? C7 H7A 0.9500 . ? C8 C9 1.517(5) . ? C8 C10 1.528(5) . ? C8 H8A 1.0000 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.370(6) . ? C10 C15 1.402(6) . ? C11 C12 1.389(6) . ? C11 H11A 0.9500 . ? C12 C13 1.374(7) . ? C12 H12A 0.9500 . ? C13 C14 1.372(7) . ? C13 H13A 0.9500 . ? C14 C15 1.379(6) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C16 C17 1.381(5) . ? C16 H16A 0.9500 . ? C17 C18 1.386(4) . ? C17 H17A 0.9500 . ? C18 C17 1.386(4) 2_656 ? C18 C19 1.486(6) . ? C19 C20 1.388(4) . ? C19 C20 1.388(4) 2_656 ? C20 C21 1.371(5) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? Fe2 O3 2.026(2) . ? Fe2 O3 2.026(2) 2_757 ? Fe2 N5 2.184(3) . ? Fe2 N5 2.184(3) 2_757 ? Fe2 N8 2.213(4) 1_565 ? Fe2 N7 2.279(4) . ? O3 C22 1.294(4) . ? O4B N6 1.232(4) . ? O4A N6 1.222(4) . ? N5 C28 1.272(4) . ? N5 C29 1.492(5) . ? N6 C25 1.459(5) . ? N7 C37 1.337(4) . ? N7 C37 1.337(4) 2_757 ? N8 C42 1.354(4) 2_757 ? N8 C42 1.354(4) . ? N8 Fe2 2.213(4) 1_545 ? C22 C23 1.413(5) . ? C22 C27 1.431(5) . ? C23 C24 1.368(5) . ? C23 H23A 0.9500 . ? C24 C25 1.398(5) . ? C24 H24A 0.9500 . ? C25 C26 1.367(5) . ? C26 C27 1.404(5) . ? C26 H26A 0.9500 . ? C27 C28 1.451(5) . ? C28 H28A 0.9500 . ? C29 C31 1.515(5) . ? C29 C30 1.532(5) . ? C29 H29A 1.0000 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C36 1.387(5) . ? C31 C32 1.420(5) . ? C32 C33 1.377(6) . ? C32 H32A 0.9500 . ? C33 C34 1.374(7) . ? C33 H33A 0.9500 . ? C34 C35 1.363(7) . ? C34 H34A 0.9500 . ? C35 C36 1.389(6) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C37 C38 1.387(4) . ? C37 H37A 0.9500 . ? C38 C39 1.389(4) . ? C38 H38A 0.9500 . ? C39 C38 1.389(4) 2_757 ? C39 C40 1.484(6) . ? C40 C41 1.395(4) . ? C40 C41 1.395(4) 2_757 ? C41 C42 1.382(5) . ? C41 H41A 0.9500 . ? C42 H42A 0.9500 . ? O100 C101 1.404(6) . ? O100 C104 1.434(5) . ? C101 C102 1.499(8) . ? C101 H10A 0.9900 . ? C101 H10B 0.9900 . ? C102 C103 1.484(9) . ? C102 H10C 0.9900 . ? C102 H10D 0.9900 . ? C103 C104 1.514(7) . ? C103 H10E 0.9900 . ? C103 H10F 0.9900 . ? C104 H10G 0.9900 . ? C104 H10H 0.9900 . ? O200 C204 1.440(11) . ? O200 C201 1.468(12) . ? C201 C202 1.529(15) . ? C202 C203 1.577(13) . ? C203 C204 1.543(15) . ? C20A C23A 1.359(18) . ? C20A C21A 1.561(19) . ? C22A C24A 1.502(19) . ? C22A C21A 1.541(19) . ? C23A C24A 1.55(2) . ? O300 C301 1.54(2) 2_756 ? O300 C301 1.55(2) . ? O300 O300 1.65(4) 2_756 ? C301 C302 1.264(18) . ? C301 O300 1.54(2) 2_756 ? C302 C302 1.630(16) 2_756 ? C400 C401 1.238(13) . ? C400 C401 1.238(13) 2_657 ? C401 C402 1.465(19) . ? C402 C402 1.655(16) 2_657 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Fe1 O1 179.92(15) 2_656 . ? O1 Fe1 N1 86.27(9) 2_656 2_656 ? O1 Fe1 N1 93.73(9) . 2_656 ? O1 Fe1 N1 93.73(9) 2_656 . ? O1 Fe1 N1 86.27(9) . . ? N1 Fe1 N1 179.44(16) 2_656 . ? O1 Fe1 N4 90.04(7) 2_656 1_545 ? O1 Fe1 N4 90.04(7) . 1_545 ? N1 Fe1 N4 89.72(8) 2_656 1_545 ? N1 Fe1 N4 89.72(8) . 1_545 ? O1 Fe1 N3 89.96(7) 2_656 . ? O1 Fe1 N3 89.96(7) . . ? N1 Fe1 N3 90.28(8) 2_656 . ? N1 Fe1 N3 90.28(8) . . ? N4 Fe1 N3 180.000(1) 1_545 . ? C1 O1 Fe1 133.2(2) . . ? C7 N1 C8 116.2(3) . . ? C7 N1 Fe1 126.3(2) . . ? C8 N1 Fe1 117.56(19) . . ? O1 C1 C2 119.3(3) . . ? O1 C1 C6 122.8(3) . . ? C2 C1 C6 117.8(3) . . ? C3 C2 C1 121.9(3) . . ? C3 C2 H2A 119.0 . . ? C1 C2 H2A 119.0 . . ? O2B N2 O2A 123.3(3) . . ? O2B N2 C4 119.4(3) . . ? O2A N2 C4 117.3(3) . . ? C16 N3 C16 115.8(4) . 2_656 ? C16 N3 Fe1 122.1(2) . . ? C16 N3 Fe1 122.1(2) 2_656 . ? C2 C3 C4 118.6(3) . . ? C2 C3 H3A 120.7 . . ? C4 C3 H3A 120.7 . . ? C21 N4 C21 118.1(5) . 2_656 ? C21 N4 Fe1 120.9(2) . 1_565 ? C21 N4 Fe1 120.9(2) 2_656 1_565 ? C5 C4 C3 121.8(3) . . ? C5 C4 N2 119.8(3) . . ? C3 C4 N2 118.4(3) . . ? C4 C5 C6 120.7(3) . . ? C4 C5 H5A 119.6 . . ? C6 C5 H5A 119.6 . . ? C5 C6 C1 119.1(3) . . ? C5 C6 C7 116.9(3) . . ? C1 C6 C7 123.9(3) . . ? N1 C7 C6 127.1(3) . . ? N1 C7 H7A 116.4 . . ? C6 C7 H7A 116.4 . . ? N1 C8 C9 112.4(3) . . ? N1 C8 C10 110.0(3) . . ? C9 C8 C10 113.6(3) . . ? N1 C8 H8A 106.8 . . ? C9 C8 H8A 106.8 . . ? C10 C8 H8A 106.8 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C15 117.7(4) . . ? C11 C10 C8 120.8(4) . . ? C15 C10 C8 121.6(3) . . ? C10 C11 C12 121.7(4) . . ? C10 C11 H11A 119.2 . . ? C12 C11 H11A 119.2 . . ? C13 C12 C11 120.2(4) . . ? C13 C12 H12A 119.9 . . ? C11 C12 H12A 119.9 . . ? C14 C13 C12 118.9(4) . . ? C14 C13 H13A 120.6 . . ? C12 C13 H13A 120.6 . . ? C13 C14 C15 121.3(4) . . ? C13 C14 H14A 119.4 . . ? C15 C14 H14A 119.4 . . ? C14 C15 C10 120.3(4) . . ? C14 C15 H15A 119.8 . . ? C10 C15 H15A 119.8 . . ? N3 C16 C17 123.8(3) . . ? N3 C16 H16A 118.1 . . ? C17 C16 H16A 118.1 . . ? C16 C17 C18 120.4(4) . . ? C16 C17 H17A 119.8 . . ? C18 C17 H17A 119.8 . . ? C17 C18 C17 115.8(4) . 2_656 ? C17 C18 C19 122.1(2) . . ? C17 C18 C19 122.1(2) 2_656 . ? C20 C19 C20 116.7(4) . 2_656 ? C20 C19 C18 121.7(2) . . ? C20 C19 C18 121.7(2) 2_656 . ? C21 C20 C19 119.8(3) . . ? C21 C20 H20A 120.1 . . ? C19 C20 H20A 120.1 . . ? N4 C21 C20 122.8(3) . . ? N4 C21 H21A 118.6 . . ? C20 C21 H21A 118.6 . . ? O3 Fe2 O3 177.75(14) . 2_757 ? O3 Fe2 N5 86.19(10) . . ? O3 Fe2 N5 93.90(10) 2_757 . ? O3 Fe2 N5 93.90(10) . 2_757 ? O3 Fe2 N5 86.19(10) 2_757 2_757 ? N5 Fe2 N5 175.61(15) . 2_757 ? O3 Fe2 N8 91.12(7) . 1_565 ? O3 Fe2 N8 91.12(7) 2_757 1_565 ? N5 Fe2 N8 87.80(8) . 1_565 ? N5 Fe2 N8 87.80(8) 2_757 1_565 ? O3 Fe2 N7 88.88(7) . . ? O3 Fe2 N7 88.88(7) 2_757 . ? N5 Fe2 N7 92.20(8) . . ? N5 Fe2 N7 92.20(8) 2_757 . ? N8 Fe2 N7 180.000(1) 1_565 . ? C22 O3 Fe2 132.1(2) . . ? C28 N5 C29 115.4(3) . . ? C28 N5 Fe2 125.4(2) . . ? C29 N5 Fe2 119.2(2) . . ? O4A N6 O4B 123.3(3) . . ? O4A N6 C25 118.5(3) . . ? O4B N6 C25 118.2(3) . . ? C37 N7 C37 116.6(4) . 2_757 ? C37 N7 Fe2 121.7(2) . . ? C37 N7 Fe2 121.7(2) 2_757 . ? C42 N8 C42 115.7(4) 2_757 . ? C42 N8 Fe2 122.1(2) 2_757 1_545 ? C42 N8 Fe2 122.1(2) . 1_545 ? O3 C22 C23 118.9(3) . . ? O3 C22 C27 123.9(3) . . ? C23 C22 C27 117.2(3) . . ? C24 C23 C22 122.9(3) . . ? C24 C23 H23A 118.6 . . ? C22 C23 H23A 118.6 . . ? C23 C24 C25 118.8(3) . . ? C23 C24 H24A 120.6 . . ? C25 C24 H24A 120.6 . . ? C26 C25 C24 120.9(3) . . ? C26 C25 N6 119.9(3) . . ? C24 C25 N6 119.1(3) . . ? C25 C26 C27 121.1(3) . . ? C25 C26 H26A 119.5 . . ? C27 C26 H26A 119.5 . . ? C26 C27 C22 119.1(3) . . ? C26 C27 C28 117.2(3) . . ? C22 C27 C28 123.7(3) . . ? N5 C28 C27 127.3(3) . . ? N5 C28 H28A 116.3 . . ? C27 C28 H28A 116.3 . . ? N5 C29 C31 112.5(3) . . ? N5 C29 C30 109.3(3) . . ? C31 C29 C30 113.9(3) . . ? N5 C29 H29A 106.9 . . ? C31 C29 H29A 106.9 . . ? C30 C29 H29A 106.9 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C36 C31 C32 117.1(4) . . ? C36 C31 C29 123.9(3) . . ? C32 C31 C29 119.0(3) . . ? C33 C32 C31 120.7(4) . . ? C33 C32 H32A 119.7 . . ? C31 C32 H32A 119.7 . . ? C34 C33 C32 120.8(4) . . ? C34 C33 H33A 119.6 . . ? C32 C33 H33A 119.6 . . ? C35 C34 C33 119.3(4) . . ? C35 C34 H34A 120.4 . . ? C33 C34 H34A 120.4 . . ? C34 C35 C36 121.2(4) . . ? C34 C35 H35A 119.4 . . ? C36 C35 H35A 119.4 . . ? C31 C36 C35 120.8(4) . . ? C31 C36 H36A 119.6 . . ? C35 C36 H36A 119.6 . . ? N7 C37 C38 123.9(3) . . ? N7 C37 H37A 118.1 . . ? C38 C37 H37A 118.1 . . ? C37 C38 C39 118.7(3) . . ? C37 C38 H38A 120.6 . . ? C39 C38 H38A 120.6 . . ? C38 C39 C38 118.1(4) 2_757 . ? C38 C39 C40 120.9(2) 2_757 . ? C38 C39 C40 120.9(2) . . ? C41 C40 C41 117.6(4) . 2_757 ? C41 C40 C39 121.2(2) . . ? C41 C40 C39 121.2(2) 2_757 . ? C42 C41 C40 119.2(3) . . ? C42 C41 H41A 120.4 . . ? C40 C41 H41A 120.4 . . ? N8 C42 C41 124.1(3) . . ? N8 C42 H42A 118.0 . . ? C41 C42 H42A 118.0 . . ? C101 O100 C104 108.4(4) . . ? O100 C101 C102 107.6(4) . . ? O100 C101 H10A 110.2 . . ? C102 C101 H10A 110.2 . . ? O100 C101 H10B 110.2 . . ? C102 C101 H10B 110.2 . . ? H10A C101 H10B 108.5 . . ? C103 C102 C101 99.9(4) . . ? C103 C102 H10C 111.8 . . ? C101 C102 H10C 111.8 . . ? C103 C102 H10D 111.8 . . ? C101 C102 H10D 111.8 . . ? H10C C102 H10D 109.5 . . ? C102 C103 C104 103.3(5) . . ? C102 C103 H10E 111.1 . . ? C104 C103 H10E 111.1 . . ? C102 C103 H10F 111.1 . . ? C104 C103 H10F 111.1 . . ? H10E C103 H10F 109.1 . . ? O100 C104 C103 105.2(4) . . ? O100 C104 H10G 110.7 . . ? C103 C104 H10G 110.7 . . ? O100 C104 H10H 110.7 . . ? C103 C104 H10H 110.7 . . ? H10G C104 H10H 108.8 . . ? C204 O200 C201 104.1(7) . . ? O200 C201 C202 107.2(8) . . ? C201 C202 C203 101.1(8) . . ? C204 C203 C202 105.8(8) . . ? O200 C204 C203 105.5(8) . . ? C23A C20A C21A 111.5(12) . . ? C24A C22A C21A 104.8(11) . . ? C22A C21A C20A 99.9(11) . . ? C20A C23A C24A 100.1(12) . . ? C22A C24A C23A 109.5(11) . . ? C301 O300 C301 92.2(14) 2_756 . ? C301 O300 O300 58.1(11) 2_756 2_756 ? C301 O300 O300 57.4(12) . 2_756 ? C302 C301 O300 98.5(13) . 2_756 ? C302 C301 O300 108.7(13) . . ? O300 C301 O300 64.6(14) 2_756 . ? C301 C302 C302 102.0(8) . 2_756 ? C401 C400 C401 116(2) . 2_657 ? C400 C401 C402 112.9(14) . . ? C401 C402 C402 98.5(6) . 2_657 ? _diffrn_measured_fraction_theta_max 0.908 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.039 _refine_diff_density_min -0.350 _refine_diff_density_rms 0.087 #===END data_ll21 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H35 Cl3 Fe N6 O2' _chemical_formula_weight 829.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' _cell_length_a 21.05493(13) _cell_length_b 16.11390(10) _cell_length_c 11.55863(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3921.58(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 16423 _cell_measurement_theta_min 3.45 _cell_measurement_theta_max 61.81 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.406 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1712 _exptl_absorpt_coefficient_mu 5.330 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.51 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'ABSPACK(CrysAlis, Oxford Diffraction)' _exptl_special_details ; The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cobra. The data collection nominally covered over a hemisphere of Reciprocal space, by a combination of seventeen sets of exposures with different \f angles for the crystal; low angle data was collected at 35 s exposure and high angle at 110s and covered 1.0\% in \w The crystal-to-detector distance was 5.5 cm. Crystal decay was found to be negligible by by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms; H-atoms were given isotropic displacement parameters equal to 1.2 (or 1.5 for methyl H-atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. There are B alerts for weak data. The crystals of the coordination polymer were very weakly diffracting and there is just no diffraction beyond 62 degrees. There is a molecule of chloroform trapped in a cavity between the polymer chains. This was modeled as disordered over two positions and refined to a ratio of 75:25 major minor. The minor component was refined isotropically. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 10.2833 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 23665 _diffrn_reflns_av_R_equivalents 0.0276 _diffrn_reflns_av_sigmaI/netI 0.0237 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.45 _diffrn_reflns_theta_max 61.94 _reflns_number_total 6066 _reflns_number_gt 5590 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0547P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881, 2419 Friedel pairs' _refine_ls_abs_structure_Flack 0.006(3) _chemical_absolute_configuration rmad _refine_ls_number_reflns 6066 _refine_ls_number_parameters 520 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0319 _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.0784 _refine_ls_wR_factor_gt 0.0775 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe2 Fe 1.0000 0.5000 0.36103(4) 0.01438(12) Uani 1 2 d S . . O2 O 0.90724(8) 0.46768(9) 0.36811(14) 0.0195(4) Uani 1 1 d . . . N5 N 0.96746(9) 0.62880(11) 0.37455(16) 0.0171(4) Uani 1 1 d . . . N6 N 0.67008(13) 0.65049(17) 0.6604(3) 0.0531(8) Uani 1 1 d . . . N7 N 1.0000 0.5000 0.5593(2) 0.0178(6) Uani 1 2 d S . . N8 N 1.0000 0.5000 1.1730(2) 0.0173(6) Uani 1 2 d S . . C23 C 0.86203(11) 0.50455(15) 0.42392(18) 0.0179(5) Uani 1 1 d . . . C24 C 0.80738(12) 0.45881(14) 0.4572(2) 0.0220(5) Uani 1 1 d . . . H24A H 0.8044 0.4020 0.4358 0.026 Uiso 1 1 calc R . . C25 C 0.75871(11) 0.49403(16) 0.5193(2) 0.0241(5) Uani 1 1 d . . . H25A H 0.7230 0.4615 0.5408 0.029 Uiso 1 1 calc R . . C26 C 0.76165(12) 0.57765(15) 0.5510(2) 0.0229(6) Uani 1 1 d . . . C27 C 0.81382(12) 0.62480(15) 0.5184(2) 0.0211(5) Uani 1 1 d . . . H27A H 0.8155 0.6817 0.5396 0.025 Uiso 1 1 calc R . . C28 C 0.86409(11) 0.59059(14) 0.4548(2) 0.0184(5) Uani 1 1 d . . . C29 C 0.91452(12) 0.64758(14) 0.4223(2) 0.0199(5) Uani 1 1 d . . . H29A H 0.9075 0.7047 0.4382 0.024 Uiso 1 1 calc R . . C30 C 1.01208(12) 0.69698(13) 0.3419(2) 0.0196(5) Uani 1 1 d . . . H30A H 1.0555 0.6789 0.3660 0.023 Uiso 1 1 calc R . . C31 C 1.00012(14) 0.78080(14) 0.3987(2) 0.0257(5) Uani 1 1 d . . . H31A H 0.9974 0.7737 0.4828 0.039 Uiso 1 1 calc R . . H31B H 0.9602 0.8040 0.3697 0.039 Uiso 1 1 calc R . . H31C H 1.0351 0.8186 0.3803 0.039 Uiso 1 1 calc R . . C32 C 1.01337(12) 0.70680(13) 0.2112(2) 0.0207(6) Uani 1 1 d . . . C33 C 1.07013(13) 0.72875(15) 0.1568(2) 0.0248(6) Uani 1 1 d . . . H33A H 1.1078 0.7347 0.2012 0.030 Uiso 1 1 calc R . . C34 C 1.07174(15) 0.74210(14) 0.0371(2) 0.0288(6) Uani 1 1 d . . . H34A H 1.1105 0.7572 0.0007 0.035 Uiso 1 1 calc R . . C35 C 1.01747(14) 0.73341(15) -0.0281(2) 0.0297(7) Uani 1 1 d . . . H35A H 1.0187 0.7422 -0.1093 0.036 Uiso 1 1 calc R . . C36 C 0.96114(14) 0.71188(16) 0.0253(2) 0.0301(6) Uani 1 1 d . . . H36A H 0.9236 0.7058 -0.0195 0.036 Uiso 1 1 calc R . . C37 C 0.95905(13) 0.69910(15) 0.1443(2) 0.0252(6) Uani 1 1 d . . . H37A H 0.9199 0.6849 0.1802 0.030 Uiso 1 1 calc R . . C38 C 0.71059(13) 0.61788(18) 0.6120(3) 0.0334(7) Uani 1 1 d . . . C39 C 0.96623(12) 0.44540(14) 0.6200(2) 0.0202(5) Uani 1 1 d . . . H39A H 0.9422 0.4052 0.5787 0.024 Uiso 1 1 calc R . . C40 C 0.96399(12) 0.44361(14) 0.7392(2) 0.0220(6) Uani 1 1 d . . . H40A H 0.9380 0.4042 0.7779 0.026 Uiso 1 1 calc R . . C41 C 1.0000 0.5000 0.8023(3) 0.0188(7) Uani 1 2 d S . . C42 C 1.0000 0.5000 0.9300(3) 0.0201(7) Uani 1 2 d S . . C43 C 0.94570(12) 0.47917(14) 0.9929(2) 0.0201(5) Uani 1 1 d . . . H43A H 0.9076 0.4645 0.9541 0.024 Uiso 1 1 calc R . . C44 C 0.94809(12) 0.48019(14) 1.1123(2) 0.0204(5) Uani 1 1 d . . . H44A H 0.9107 0.4660 1.1538 0.024 Uiso 1 1 calc R . . Fe1 Fe 1.0000 1.0000 -0.26460(4) 0.01519(13) Uani 1 2 d S . . O1 O 0.97035(7) 1.11910(9) -0.27221(14) 0.0191(4) Uani 1 1 d . . . N1 N 0.89998(10) 0.96850(11) -0.24903(16) 0.0175(4) Uani 1 1 d . . . C1 C 0.91579(11) 1.15205(14) -0.2917(2) 0.0167(5) Uani 1 1 d . . . C2 C 0.91152(12) 1.23736(14) -0.3202(2) 0.0200(5) Uani 1 1 d . . . H2A H 0.9496 1.2687 -0.3267 0.024 Uiso 1 1 calc R . . N2 N 0.69171(11) 1.30944(13) -0.3676(2) 0.0316(5) Uani 1 1 d . . . C3 C 0.85498(12) 1.27634(14) -0.3385(2) 0.0222(5) Uani 1 1 d . . . H3A H 0.8544 1.3337 -0.3576 0.027 Uiso 1 1 calc R . . N3 N 1.0000 1.0000 -0.0719(2) 0.0169(6) Uani 1 2 d S . . C4 C 0.79733(12) 1.23219(15) -0.3295(2) 0.0211(5) Uani 1 1 d . . . N4 N 1.0000 1.0000 0.5405(2) 0.0191(6) Uani 1 2 d S . . C5 C 0.79937(12) 1.14890(14) -0.3018(2) 0.0200(5) Uani 1 1 d . . . H5A H 0.7607 1.1190 -0.2952 0.024 Uiso 1 1 calc R . . C6 C 0.85689(11) 1.10708(14) -0.28324(19) 0.0188(5) Uani 1 1 d . . . C7 C 0.85316(12) 1.01951(14) -0.25444(19) 0.0191(5) Uani 1 1 d . . . H7A H 0.8122 0.9978 -0.2380 0.023 Uiso 1 1 calc R . . C8 C 0.88545(12) 0.87971(14) -0.2185(2) 0.0220(5) Uani 1 1 d . . . H8A H 0.9252 0.8562 -0.1845 0.026 Uiso 1 1 calc R . . C9 C 0.87353(16) 0.83233(16) -0.3291(3) 0.0392(7) Uani 1 1 d . . . H9A H 0.9092 0.8408 -0.3823 0.059 Uiso 1 1 calc R . . H9B H 0.8343 0.8524 -0.3651 0.059 Uiso 1 1 calc R . . H9C H 0.8694 0.7731 -0.3116 0.059 Uiso 1 1 calc R . . C10 C 0.83491(12) 0.87115(15) -0.1271(2) 0.0258(6) Uani 1 1 d . . . C11 C 0.77052(13) 0.86199(18) -0.1521(3) 0.0357(7) Uani 1 1 d . . . H11A H 0.7571 0.8578 -0.2304 0.043 Uiso 1 1 calc R . . C12 C 0.72570(16) 0.8588(2) -0.0637(3) 0.0569(10) Uani 1 1 d . . . H12A H 0.6818 0.8558 -0.0819 0.068 Uiso 1 1 calc R . . C13 C 0.74494(19) 0.8601(3) 0.0501(4) 0.0699(13) Uani 1 1 d . . . H13A H 0.7146 0.8551 0.1104 0.084 Uiso 1 1 calc R . . C14 C 0.80887(18) 0.8686(3) 0.0762(3) 0.0622(11) Uani 1 1 d . . . H14A H 0.8223 0.8704 0.1547 0.075 Uiso 1 1 calc R . . C15 C 0.85259(14) 0.87463(19) -0.0109(2) 0.0373(7) Uani 1 1 d . . . H15A H 0.8962 0.8813 0.0083 0.045 Uiso 1 1 calc R . . C16 C 0.73809(13) 1.27461(15) -0.3500(2) 0.0237(6) Uani 1 1 d . . . C17 C 0.96116(12) 1.04996(14) -0.0117(2) 0.0186(5) Uani 1 1 d . . . H17A H 0.9336 1.0858 -0.0532 0.022 Uiso 1 1 calc R . . C18 C 0.95933(11) 1.05177(14) 0.1081(2) 0.0190(5) Uani 1 1 d . . . H18A H 0.9308 1.0877 0.1474 0.023 Uiso 1 1 calc R . . C19 C 1.0000 1.0000 0.1699(3) 0.0172(7) Uani 1 2 d S . . C20 C 1.0000 1.0000 0.2986(3) 0.0166(7) Uani 1 2 d S . . C21 C 0.94363(11) 1.00377(16) 0.36057(19) 0.0213(5) Uani 1 1 d . . . H21A H 0.9040 1.0065 0.3215 0.026 Uiso 1 1 calc R . . C22 C 0.94600(11) 1.00348(16) 0.48029(19) 0.0206(5) Uani 1 1 d . . . H22A H 0.9071 1.0059 0.5218 0.025 Uiso 1 1 calc R . . C45 C 0.7768(3) 0.6353(3) -0.0447(5) 0.0423(13) Uani 0.747(3) 1 d PD A 1 H45A H 0.7754 0.6973 -0.0406 0.051 Uiso 0.747(3) 1 calc PR A 1 Cl1 Cl 0.81318(5) 0.59766(9) 0.08333(9) 0.0561(4) Uani 0.747(3) 1 d PD A 1 Cl2 Cl 0.69983(6) 0.59904(13) -0.05158(12) 0.0693(5) Uani 0.747(3) 1 d PD A 1 Cl3 Cl 0.82361(6) 0.60646(9) -0.16623(9) 0.0384(3) Uani 0.747(3) 1 d PD A 1 C45A C 0.7625(9) 0.6312(12) -0.0792(15) 0.068(8) Uiso 0.253(3) 1 d PD A 2 H45B H 0.7370 0.6716 -0.1255 0.081 Uiso 0.253(3) 1 calc PR A 2 Cl1A Cl 0.7864(2) 0.6797(3) 0.0465(5) 0.0894(18) Uiso 0.253(3) 1 d PD A 2 Cl2A Cl 0.7184(4) 0.5474(5) -0.0569(6) 0.116(2) Uiso 0.253(3) 1 d PD A 2 Cl3A Cl 0.8262(7) 0.6012(10) -0.1603(12) 0.213(6) Uiso 0.253(3) 1 d PD A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe2 0.0199(3) 0.0134(2) 0.0098(2) 0.000 0.000 0.0004(2) O2 0.0238(9) 0.0170(8) 0.0177(9) -0.0017(6) 0.0012(7) -0.0005(7) N5 0.0219(11) 0.0154(9) 0.0141(10) 0.0010(8) -0.0037(9) -0.0027(8) N6 0.0345(15) 0.0538(16) 0.071(2) -0.0220(15) 0.0186(15) 0.0010(13) N7 0.0226(15) 0.0159(12) 0.0151(14) 0.000 0.000 0.0008(13) N8 0.0263(15) 0.0111(12) 0.0145(13) 0.000 0.000 -0.0009(13) C23 0.0228(12) 0.0194(11) 0.0114(11) 0.0002(10) -0.0050(9) 0.0034(11) C24 0.0250(14) 0.0213(12) 0.0198(13) 0.0021(10) -0.0031(11) -0.0021(10) C25 0.0213(13) 0.0278(13) 0.0232(12) 0.0028(12) -0.0009(10) -0.0006(11) C26 0.0195(14) 0.0285(14) 0.0207(13) -0.0051(11) -0.0004(11) 0.0019(10) C27 0.0240(14) 0.0214(12) 0.0180(13) -0.0022(10) -0.0035(11) 0.0038(10) C28 0.0190(13) 0.0210(11) 0.0152(11) 0.0020(10) -0.0020(10) 0.0016(10) C29 0.0251(14) 0.0152(11) 0.0195(13) 0.0002(10) -0.0042(11) 0.0003(10) C30 0.0245(14) 0.0163(11) 0.0180(12) 0.0024(10) -0.0003(10) -0.0032(10) C31 0.0324(14) 0.0213(12) 0.0233(13) -0.0024(10) -0.0012(13) -0.0037(12) C32 0.0316(16) 0.0120(10) 0.0186(12) 0.0030(9) 0.0017(11) 0.0008(10) C33 0.0303(15) 0.0187(12) 0.0254(15) 0.0008(11) 0.0004(12) -0.0004(11) C34 0.0396(17) 0.0187(12) 0.0282(15) 0.0031(11) 0.0108(13) -0.0012(11) C35 0.049(2) 0.0204(12) 0.0197(13) 0.0044(11) 0.0053(13) 0.0032(12) C36 0.0386(17) 0.0298(14) 0.0217(15) 0.0041(11) -0.0055(13) 0.0027(12) C37 0.0286(15) 0.0266(13) 0.0204(14) 0.0047(11) 0.0013(11) -0.0009(11) C38 0.0258(15) 0.0344(15) 0.0400(18) -0.0070(13) 0.0046(13) -0.0027(12) C39 0.0311(15) 0.0156(11) 0.0140(12) 0.0007(10) -0.0022(11) -0.0034(10) C40 0.0326(15) 0.0164(11) 0.0169(13) 0.0015(10) 0.0028(11) -0.0072(11) C41 0.0260(18) 0.0176(15) 0.0128(16) 0.000 0.000 0.0023(16) C42 0.034(2) 0.0117(14) 0.0143(16) 0.000 0.000 -0.0008(16) C43 0.0273(14) 0.0184(12) 0.0145(12) 0.0006(9) -0.0031(10) -0.0050(10) C44 0.0276(14) 0.0179(13) 0.0156(12) 0.0018(9) 0.0025(11) -0.0032(10) Fe1 0.0202(3) 0.0156(2) 0.0098(2) 0.000 0.000 0.0004(2) O1 0.0201(9) 0.0208(8) 0.0163(9) 0.0004(7) -0.0031(7) -0.0022(7) N1 0.0248(11) 0.0166(9) 0.0111(10) 0.0025(8) 0.0020(8) -0.0009(8) C1 0.0220(13) 0.0183(11) 0.0097(12) -0.0018(9) 0.0005(10) -0.0013(10) C2 0.0238(14) 0.0202(12) 0.0161(13) 0.0009(10) -0.0007(11) -0.0022(10) N2 0.0278(13) 0.0268(11) 0.0401(14) -0.0028(10) -0.0032(11) 0.0046(10) C3 0.0303(15) 0.0169(11) 0.0194(13) 0.0005(10) -0.0016(11) 0.0022(11) N3 0.0201(14) 0.0161(12) 0.0144(14) 0.000 0.000 -0.0014(13) C4 0.0218(14) 0.0220(12) 0.0196(13) -0.0023(11) -0.0017(11) 0.0025(10) N4 0.0259(15) 0.0162(13) 0.0153(13) 0.000 0.000 -0.0003(13) C5 0.0229(13) 0.0215(12) 0.0156(13) -0.0029(10) 0.0023(10) -0.0048(10) C6 0.0245(13) 0.0208(12) 0.0110(11) -0.0012(10) -0.0001(10) 0.0017(11) C7 0.0218(13) 0.0219(13) 0.0135(12) 0.0021(9) 0.0001(10) -0.0061(10) C8 0.0247(13) 0.0171(12) 0.0241(14) 0.0037(10) 0.0000(11) -0.0029(10) C9 0.060(2) 0.0225(14) 0.0352(17) -0.0060(12) 0.0045(15) -0.0135(13) C10 0.0255(14) 0.0244(13) 0.0276(14) 0.0106(11) 0.0033(12) -0.0032(11) C11 0.0277(15) 0.0416(16) 0.0377(17) 0.0185(14) -0.0043(13) -0.0079(13) C12 0.0277(17) 0.067(2) 0.076(3) 0.033(2) 0.0054(17) -0.0018(16) C13 0.055(3) 0.098(3) 0.057(3) 0.032(2) 0.026(2) -0.003(2) C14 0.060(2) 0.095(3) 0.0312(19) 0.0186(19) 0.0122(18) -0.009(2) C15 0.0326(16) 0.0534(18) 0.0260(15) 0.0112(13) -0.0008(13) -0.0064(14) C16 0.0275(15) 0.0190(12) 0.0246(14) -0.0029(11) 0.0008(12) -0.0035(11) C17 0.0240(14) 0.0176(12) 0.0141(13) 0.0015(10) -0.0021(10) 0.0036(10) C18 0.0226(14) 0.0195(12) 0.0149(13) -0.0013(10) 0.0029(10) 0.0040(10) C19 0.0207(17) 0.0182(15) 0.0127(16) 0.000 0.000 -0.0022(16) C20 0.0276(18) 0.0078(13) 0.0144(16) 0.000 0.000 0.0026(15) C21 0.0228(13) 0.0240(12) 0.0170(12) 0.0003(12) -0.0022(10) 0.0025(11) C22 0.0226(12) 0.0242(12) 0.0152(11) -0.0019(11) 0.0014(10) -0.0003(11) C45 0.045(3) 0.034(3) 0.048(3) -0.008(2) -0.009(3) -0.002(2) Cl1 0.0349(6) 0.1002(10) 0.0333(6) -0.0024(6) 0.0018(5) 0.0072(6) Cl2 0.0279(6) 0.1177(13) 0.0623(8) -0.0046(8) -0.0038(5) -0.0015(7) Cl3 0.0347(6) 0.0614(7) 0.0191(5) 0.0003(4) -0.0031(4) 0.0073(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 Fe2 O2 2.0229(16) 2_765 ? Fe2 O2 2.0229(16) . ? Fe2 N8 2.173(3) 1_554 ? Fe2 N5 2.1912(18) . ? Fe2 N5 2.1912(18) 2_765 ? Fe2 N7 2.292(3) . ? O2 C23 1.294(3) . ? N5 C29 1.280(3) . ? N5 C30 1.494(3) . ? N6 C38 1.147(4) . ? N7 C39 1.331(3) 2_765 ? N7 C39 1.331(3) . ? N8 C44 1.337(3) . ? N8 C44 1.337(3) 2_765 ? N8 Fe2 2.173(3) 1_556 ? C23 C24 1.420(3) . ? C23 C28 1.432(3) . ? C24 C25 1.374(3) . ? C24 H24A 0.9500 . ? C25 C26 1.398(4) . ? C25 H25A 0.9500 . ? C26 C27 1.388(4) . ? C26 C38 1.440(4) . ? C27 C28 1.401(3) . ? C27 H27A 0.9500 . ? C28 C29 1.453(3) . ? C29 H29A 0.9500 . ? C30 C32 1.520(3) . ? C30 C31 1.523(3) . ? C30 H30A 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C37 1.386(4) . ? C32 C33 1.396(4) . ? C33 C34 1.401(4) . ? C33 H33A 0.9500 . ? C34 C35 1.376(4) . ? C34 H34A 0.9500 . ? C35 C36 1.381(4) . ? C35 H35A 0.9500 . ? C36 C37 1.392(4) . ? C36 H36A 0.9500 . ? C37 H37A 0.9500 . ? C39 C40 1.378(3) . ? C39 H39A 0.9500 . ? C40 C41 1.390(3) . ? C40 H40A 0.9500 . ? C41 C40 1.390(3) 2_765 ? C41 C42 1.475(4) . ? C42 C43 1.396(3) 2_765 ? C42 C43 1.396(3) . ? C43 C44 1.381(3) . ? C43 H43A 0.9500 . ? C44 H44A 0.9500 . ? Fe1 O1 2.0200(15) 2_775 ? Fe1 O1 2.0200(15) . ? Fe1 N1 2.174(2) 2_775 ? Fe1 N1 2.174(2) . ? Fe1 N3 2.228(3) . ? Fe1 N4 2.253(3) 1_554 ? O1 C1 1.285(3) . ? N1 C7 1.285(3) . ? N1 C8 1.505(3) . ? C1 C2 1.416(3) . ? C1 C6 1.440(3) . ? C2 C3 1.363(3) . ? C2 H2A 0.9500 . ? N2 C16 1.145(3) . ? C3 C4 1.411(3) . ? C3 H3A 0.9500 . ? N3 C17 1.342(3) 2_775 ? N3 C17 1.342(3) . ? C4 C5 1.380(3) . ? C4 C16 1.442(4) . ? N4 C22 1.334(3) . ? N4 C22 1.334(3) 2_775 ? N4 Fe1 2.253(3) 1_556 ? C5 C6 1.402(3) . ? C5 H5A 0.9500 . ? C6 C7 1.452(3) . ? C7 H7A 0.9500 . ? C8 C10 1.506(3) . ? C8 C9 1.509(4) . ? C8 H8A 1.0000 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.394(4) . ? C10 C15 1.395(4) . ? C11 C12 1.392(5) . ? C11 H11A 0.9500 . ? C12 C13 1.376(6) . ? C12 H12A 0.9500 . ? C13 C14 1.386(5) . ? C13 H13A 0.9500 . ? C14 C15 1.367(4) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C17 C18 1.385(3) . ? C17 H17A 0.9500 . ? C18 C19 1.393(3) . ? C18 H18A 0.9500 . ? C19 C18 1.393(3) 2_775 ? C19 C20 1.487(4) . ? C20 C21 1.388(3) 2_775 ? C20 C21 1.388(3) . ? C21 C22 1.385(3) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C45 Cl2 1.724(5) . ? C45 Cl1 1.774(6) . ? C45 Cl3 1.779(5) . ? C45 H45A 1.0000 . ? C45A Cl2A 1.659(16) . ? C45A Cl3A 1.706(16) . ? C45A Cl1A 1.725(15) . ? C45A H45B 1.0000 . ? 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 O2 Fe2 O2 175.36(9) 2_765 . ? O2 Fe2 N8 92.32(5) 2_765 1_554 ? O2 Fe2 N8 92.32(5) . 1_554 ? O2 Fe2 N5 93.16(7) 2_765 . ? O2 Fe2 N5 86.51(7) . . ? N8 Fe2 N5 94.09(5) 1_554 . ? O2 Fe2 N5 86.51(7) 2_765 2_765 ? O2 Fe2 N5 93.16(7) . 2_765 ? N8 Fe2 N5 94.09(5) 1_554 2_765 ? N5 Fe2 N5 171.82(10) . 2_765 ? O2 Fe2 N7 87.68(5) 2_765 . ? O2 Fe2 N7 87.68(5) . . ? N8 Fe2 N7 180.0 1_554 . ? N5 Fe2 N7 85.91(5) . . ? N5 Fe2 N7 85.91(5) 2_765 . ? C23 O2 Fe2 127.74(15) . . ? C29 N5 C30 118.85(19) . . ? C29 N5 Fe2 121.80(15) . . ? C30 N5 Fe2 118.81(14) . . ? C39 N7 C39 116.3(3) 2_765 . ? C39 N7 Fe2 121.83(14) 2_765 . ? C39 N7 Fe2 121.83(14) . . ? C44 N8 C44 116.8(3) . 2_765 ? C44 N8 Fe2 121.62(14) . 1_556 ? C44 N8 Fe2 121.62(14) 2_765 1_556 ? O2 C23 C24 119.5(2) . . ? O2 C23 C28 123.1(2) . . ? C24 C23 C28 117.3(2) . . ? C25 C24 C23 122.1(2) . . ? C25 C24 H24A 118.9 . . ? C23 C24 H24A 118.9 . . ? C24 C25 C26 120.1(2) . . ? C24 C25 H25A 119.9 . . ? C26 C25 H25A 119.9 . . ? C27 C26 C25 119.5(2) . . ? C27 C26 C38 118.5(2) . . ? C25 C26 C38 121.9(2) . . ? C26 C27 C28 121.7(2) . . ? C26 C27 H27A 119.2 . . ? C28 C27 H27A 119.2 . . ? C27 C28 C23 119.3(2) . . ? C27 C28 C29 116.0(2) . . ? C23 C28 C29 124.7(2) . . ? N5 C29 C28 126.7(2) . . ? N5 C29 H29A 116.6 . . ? C28 C29 H29A 116.6 . . ? N5 C30 C32 109.80(18) . . ? N5 C30 C31 116.1(2) . . ? C32 C30 C31 109.84(18) . . ? N5 C30 H30A 106.9 . . ? C32 C30 H30A 106.9 . . ? C31 C30 H30A 106.9 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C37 C32 C33 118.6(2) . . ? C37 C32 C30 122.0(2) . . ? C33 C32 C30 119.3(2) . . ? C32 C33 C34 120.3(3) . . ? C32 C33 H33A 119.9 . . ? C34 C33 H33A 119.9 . . ? C35 C34 C33 120.3(3) . . ? C35 C34 H34A 119.8 . . ? C33 C34 H34A 119.8 . . ? C34 C35 C36 119.6(3) . . ? C34 C35 H35A 120.2 . . ? C36 C35 H35A 120.2 . . ? C35 C36 C37 120.4(3) . . ? C35 C36 H36A 119.8 . . ? C37 C36 H36A 119.8 . . ? C32 C37 C36 120.8(2) . . ? C32 C37 H37A 119.6 . . ? C36 C37 H37A 119.6 . . ? N6 C38 C26 179.5(3) . . ? N7 C39 C40 124.0(2) . . ? N7 C39 H39A 118.0 . . ? C40 C39 H39A 118.0 . . ? C39 C40 C41 119.5(2) . . ? C39 C40 H40A 120.3 . . ? C41 C40 H40A 120.3 . . ? C40 C41 C40 116.7(3) . 2_765 ? C40 C41 C42 121.65(14) . . ? C40 C41 C42 121.65(14) 2_765 . ? C43 C42 C43 117.2(3) 2_765 . ? C43 C42 C41 121.42(15) 2_765 . ? C43 C42 C41 121.42(15) . . ? C44 C43 C42 119.2(2) . . ? C44 C43 H43A 120.4 . . ? C42 C43 H43A 120.4 . . ? N8 C44 C43 123.8(2) . . ? N8 C44 H44A 118.1 . . ? C43 C44 H44A 118.1 . . ? O1 Fe1 O1 175.00(9) 2_775 . ? O1 Fe1 N1 85.76(7) 2_775 2_775 ? O1 Fe1 N1 94.65(7) . 2_775 ? O1 Fe1 N1 94.65(7) 2_775 . ? O1 Fe1 N1 85.76(7) . . ? N1 Fe1 N1 170.50(10) 2_775 . ? O1 Fe1 N3 92.50(5) 2_775 . ? O1 Fe1 N3 92.50(5) . . ? N1 Fe1 N3 85.25(5) 2_775 . ? N1 Fe1 N3 85.25(5) . . ? O1 Fe1 N4 87.50(5) 2_775 1_554 ? O1 Fe1 N4 87.50(5) . 1_554 ? N1 Fe1 N4 94.75(5) 2_775 1_554 ? N1 Fe1 N4 94.75(5) . 1_554 ? N3 Fe1 N4 180.000(1) . 1_554 ? C1 O1 Fe1 132.56(14) . . ? C7 N1 C8 117.6(2) . . ? C7 N1 Fe1 126.13(15) . . ? C8 N1 Fe1 116.00(15) . . ? O1 C1 C2 119.9(2) . . ? O1 C1 C6 123.4(2) . . ? C2 C1 C6 116.7(2) . . ? C3 C2 C1 122.6(2) . . ? C3 C2 H2A 118.7 . . ? C1 C2 H2A 118.7 . . ? C2 C3 C4 120.5(2) . . ? C2 C3 H3A 119.7 . . ? C4 C3 H3A 119.7 . . ? C17 N3 C17 117.5(3) 2_775 . ? C17 N3 Fe1 121.23(14) 2_775 . ? C17 N3 Fe1 121.23(14) . . ? C5 C4 C3 118.7(2) . . ? C5 C4 C16 121.7(2) . . ? C3 C4 C16 119.5(2) . . ? C22 N4 C22 117.1(3) . 2_775 ? C22 N4 Fe1 121.44(14) . 1_556 ? C22 N4 Fe1 121.44(14) 2_775 1_556 ? C4 C5 C6 122.0(2) . . ? C4 C5 H5A 119.0 . . ? C6 C5 H5A 119.0 . . ? C5 C6 C1 119.4(2) . . ? C5 C6 C7 117.1(2) . . ? C1 C6 C7 123.5(2) . . ? N1 C7 C6 126.3(2) . . ? N1 C7 H7A 116.9 . . ? C6 C7 H7A 116.9 . . ? N1 C8 C10 113.3(2) . . ? N1 C8 C9 108.4(2) . . ? C10 C8 C9 115.5(2) . . ? N1 C8 H8A 106.3 . . ? C10 C8 H8A 106.3 . . ? C9 C8 H8A 106.3 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C15 117.6(3) . . ? C11 C10 C8 123.5(2) . . ? C15 C10 C8 118.9(2) . . ? C12 C11 C10 120.7(3) . . ? C12 C11 H11A 119.6 . . ? C10 C11 H11A 119.6 . . ? C13 C12 C11 120.1(3) . . ? C13 C12 H12A 120.0 . . ? C11 C12 H12A 120.0 . . ? C12 C13 C14 119.7(3) . . ? C12 C13 H13A 120.1 . . ? C14 C13 H13A 120.1 . . ? C15 C14 C13 120.0(3) . . ? C15 C14 H14A 120.0 . . ? C13 C14 H14A 120.0 . . ? C14 C15 C10 121.8(3) . . ? C14 C15 H15A 119.1 . . ? C10 C15 H15A 119.1 . . ? N2 C16 C4 178.6(3) . . ? N3 C17 C18 123.2(2) . . ? N3 C17 H17A 118.4 . . ? C18 C17 H17A 118.4 . . ? C17 C18 C19 118.9(2) . . ? C17 C18 H18A 120.5 . . ? C19 C18 H18A 120.5 . . ? C18 C19 C18 118.2(3) 2_775 . ? C18 C19 C20 120.89(14) 2_775 . ? C18 C19 C20 120.89(14) . . ? C21 C20 C21 117.8(3) 2_775 . ? C21 C20 C19 121.09(14) 2_775 . ? C21 C20 C19 121.09(14) . . ? C22 C21 C20 119.0(2) . . ? C22 C21 H21A 120.5 . . ? C20 C21 H21A 120.5 . . ? N4 C22 C21 123.5(2) . . ? N4 C22 H22A 118.2 . . ? C21 C22 H22A 118.2 . . ? Cl2 C45 Cl1 109.2(3) . . ? Cl2 C45 Cl3 113.3(3) . . ? Cl1 C45 Cl3 109.2(3) . . ? Cl2 C45 H45A 108.3 . . ? Cl1 C45 H45A 108.3 . . ? Cl3 C45 H45A 108.3 . . ? Cl2A C45A Cl3A 107.2(12) . . ? Cl2A C45A Cl1A 113.7(11) . . ? Cl3A C45A Cl1A 111.2(11) . . ? Cl2A C45A H45B 108.2 . . ? Cl3A C45A H45B 108.2 . . ? Cl1A C45A H45B 108.2 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 61.94 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.223 _refine_diff_density_min -0.414 _refine_diff_density_rms 0.044 #===END data_ll9 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H52 Fe N4 O6' _chemical_formula_weight 836.79 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 triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 8.7967(2) _cell_length_b 8.9245(2) _cell_length_c 14.7428(4) _cell_angle_alpha 102.135(2) _cell_angle_beta 106.334(2) _cell_angle_gamma 97.4319(19) _cell_volume 1063.73(4) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 16258 _cell_measurement_theta_min 3.06 _cell_measurement_theta_max 32.65 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.306 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 442 _exptl_absorpt_coefficient_mu 0.409 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.94 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'ABSPACK(CrysAlis, Oxford Diffraction)' _exptl_special_details ; The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cobra. The data collection nominally covered over a hemisphere of Reciprocal space, by a combination of ten sets of exposures with different \f angles for the crystal; each 55 s exposure covered 1.0\% in \w. The crystal-to-detector distance was 5.5 cm. Crystal decay was found to be negligible by by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms; H-atoms were given isotropic displacement parameter equal to 1.2 (or 1.5 for methyl H-atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. There are two molecules of THF in the cell. One is alright (O101-C105), the other was modelled as disordered over two positions and refined to a ratio of 54: 46. These two THFs share the same oxygen (O201) Several restraints were required to give all the THFs reasonably sensible bond lengths and thermal parameters. The hydrogens were placed at calculated positions on the Os O2 and O4 and form an H bonded network with the phenols of symmetry related chains and the THFs. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 10.2833 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 25187 _diffrn_reflns_av_R_equivalents 0.0239 _diffrn_reflns_av_sigmaI/netI 0.0480 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 32.72 _reflns_number_total 13945 _reflns_number_gt 12531 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0695P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881, 6677 Friedel pairs' _refine_ls_abs_structure_Flack 0.014(8) _chemical_absolute_configuration rmad _refine_ls_number_reflns 13945 _refine_ls_number_parameters 571 _refine_ls_number_restraints 57 _refine_ls_R_factor_all 0.0476 _refine_ls_R_factor_gt 0.0425 _refine_ls_wR_factor_ref 0.1078 _refine_ls_wR_factor_gt 0.1061 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.045 _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 Fe1 Fe 0.33322(2) 0.51344(2) 0.564854(18) 0.01159(6) Uani 1 1 d . . . N1 N 0.3777(2) 0.6485(2) 0.71261(13) 0.0143(3) Uani 1 1 d . . . C1 C 0.5661(2) 0.3893(2) 0.71216(13) 0.0123(3) Uani 1 1 d . . . O1 O 0.49651(17) 0.39507(16) 0.62150(10) 0.0135(3) Uani 1 1 d . . . C2 C 0.6576(2) 0.2733(2) 0.72909(14) 0.0158(3) Uani 1 1 d . . . H2A H 0.6642 0.1990 0.6745 0.019 Uiso 1 1 calc R . . O2 O 0.8153(2) 0.3582(2) 0.99456(13) 0.0400(4) Uani 1 1 d U . . H2B H 0.7839 0.4117 1.0373 0.060 Uiso 1 1 calc R . . N2 N 0.3046(2) 0.39158(19) 0.41680(13) 0.0141(3) Uani 1 1 d . . . C3 C 0.7379(2) 0.2641(2) 0.82240(15) 0.0204(4) Uani 1 1 d . . . H3A H 0.7989 0.1847 0.8308 0.024 Uiso 1 1 calc R . . N3 N 0.1350(2) 0.3207(2) 0.57054(13) 0.0144(3) Uani 1 1 d . . . O3 O 0.15724(17) 0.62199(16) 0.50890(11) 0.0143(3) Uani 1 1 d . . . C4 C 0.7301(3) 0.3703(3) 0.90401(15) 0.0253(4) Uani 1 1 d . . . N4 N -0.4762(2) -0.2993(2) 0.55643(13) 0.0143(3) Uani 1 1 d . . . O4 O -0.2766(2) 0.5297(3) 0.13905(12) 0.0383(4) Uani 1 1 d . . . H4A H -0.3720 0.4985 0.1371 0.057 Uiso 1 1 calc R . . C5 C 0.6392(3) 0.4837(3) 0.89054(14) 0.0212(4) Uani 1 1 d . . . H5A H 0.6329 0.5559 0.9461 0.025 Uiso 1 1 calc R . . C6 C 0.5556(2) 0.4950(2) 0.79631(14) 0.0145(3) Uani 1 1 d . . . C7 C 0.4674(3) 0.6224(2) 0.79121(15) 0.0155(4) Uani 1 1 d . . . H7A H 0.4769 0.6928 0.8515 0.019 Uiso 1 1 calc R . . C8 C 0.3119(2) 0.7943(2) 0.72607(14) 0.0175(3) Uani 1 1 d . . . H8A H 0.2489 0.7993 0.6592 0.021 Uiso 1 1 calc R . . C9 C 0.4507(3) 0.9383(2) 0.76666(19) 0.0276(5) Uani 1 1 d . . . H9A H 0.5247 0.9289 0.7279 0.041 Uiso 1 1 calc R . . H9B H 0.5094 0.9450 0.8350 0.041 Uiso 1 1 calc R . . H9C H 0.4064 1.0330 0.7629 0.041 Uiso 1 1 calc R . . C10 C 0.1937(2) 0.7919(2) 0.78375(14) 0.0164(3) Uani 1 1 d . . . C11 C 0.0897(3) 0.6520(2) 0.77305(16) 0.0197(4) Uani 1 1 d . . . H11A H 0.1007 0.5572 0.7341 0.024 Uiso 1 1 calc R . . C12 C -0.0285(2) 0.6488(3) 0.81777(16) 0.0235(4) Uani 1 1 d . . . H12A H -0.0961 0.5521 0.8106 0.028 Uiso 1 1 calc R . . C13 C -0.0492(3) 0.7864(3) 0.87319(16) 0.0258(4) Uani 1 1 d . . . H13A H -0.1319 0.7847 0.9030 0.031 Uiso 1 1 calc R . . C14 C 0.0517(3) 0.9257(3) 0.88442(16) 0.0264(4) Uani 1 1 d . . . H14A H 0.0383 1.0201 0.9225 0.032 Uiso 1 1 calc R . . C15 C 0.1731(2) 0.9295(2) 0.84055(15) 0.0219(4) Uani 1 1 d . . . H15A H 0.2420 1.0262 0.8494 0.026 Uiso 1 1 calc R . . C16 C 0.0544(2) 0.5939(2) 0.42125(13) 0.0132(3) Uani 1 1 d . . . C17 C -0.0835(2) 0.6629(2) 0.40615(14) 0.0182(3) Uani 1 1 d . . . H17A H -0.1008 0.7268 0.4612 0.022 Uiso 1 1 calc R . . C18 C -0.1942(2) 0.6411(3) 0.31467(16) 0.0237(4) Uani 1 1 d . . . H18A H -0.2855 0.6894 0.3078 0.028 Uiso 1 1 calc R . . C19 C -0.1724(2) 0.5491(3) 0.23304(15) 0.0246(4) Uani 1 1 d . . . C20 C -0.0412(3) 0.4766(3) 0.24434(15) 0.0234(4) Uani 1 1 d . . . H20A H -0.0268 0.4128 0.1883 0.028 Uiso 1 1 calc R . . C21 C 0.0719(2) 0.4952(2) 0.33727(14) 0.0154(4) Uani 1 1 d . . . C22 C 0.1974(3) 0.4049(2) 0.33978(15) 0.0170(4) Uani 1 1 d . . . H22A H 0.2017 0.3493 0.2784 0.020 Uiso 1 1 calc R . . C23 C 0.4179(2) 0.2867(2) 0.39761(14) 0.0184(4) Uani 1 1 d . . . H23A H 0.4688 0.2602 0.4604 0.022 Uiso 1 1 calc R . . C24 C 0.5539(3) 0.3782(3) 0.37320(19) 0.0266(5) Uani 1 1 d . . . H24A H 0.6078 0.4723 0.4267 0.040 Uiso 1 1 calc R . . H24B H 0.5085 0.4086 0.3126 0.040 Uiso 1 1 calc R . . H24C H 0.6324 0.3125 0.3646 0.040 Uiso 1 1 calc R . . C25 C 0.3285(3) 0.1335(2) 0.32276(15) 0.0206(4) Uani 1 1 d . . . C26 C 0.2445(3) 0.0211(3) 0.35190(17) 0.0270(4) Uani 1 1 d . . . H26A H 0.2485 0.0395 0.4185 0.032 Uiso 1 1 calc R . . C27 C 0.1538(4) -0.1192(3) 0.2854(2) 0.0398(6) Uani 1 1 d . . . H27A H 0.0984 -0.1961 0.3070 0.048 Uiso 1 1 calc R . . C28 C 0.1450(4) -0.1457(3) 0.1884(2) 0.0482(8) Uani 1 1 d . . . H28A H 0.0806 -0.2395 0.1425 0.058 Uiso 1 1 calc R . . C29 C 0.2304(4) -0.0351(3) 0.1582(2) 0.0424(6) Uani 1 1 d . . . H29A H 0.2268 -0.0547 0.0917 0.051 Uiso 1 1 calc R . . C30 C 0.3216(3) 0.1048(3) 0.22456(17) 0.0304(5) Uani 1 1 d . . . H30A H 0.3790 0.1805 0.2031 0.036 Uiso 1 1 calc R . . C31 C -0.0223(2) 0.3315(2) 0.54625(15) 0.0172(4) Uani 1 1 d . . . H31A H -0.0501 0.4249 0.5312 0.021 Uiso 1 1 calc R . . C32 C -0.1459(2) 0.2132(2) 0.54202(15) 0.0172(4) Uani 1 1 d . . . H32A H -0.2549 0.2263 0.5240 0.021 Uiso 1 1 calc R . . C33 C -0.1087(2) 0.0752(2) 0.56440(14) 0.0137(4) Uani 1 1 d . . . C34 C -0.2362(2) -0.0537(2) 0.56119(14) 0.0123(4) Uani 1 1 d . . . C35 C -0.3934(2) -0.0844(2) 0.49529(15) 0.0168(3) Uani 1 1 d . . . H35A H -0.4216 -0.0222 0.4506 0.020 Uiso 1 1 calc R . . C36 C -0.5072(2) -0.2066(2) 0.49609(15) 0.0169(3) Uani 1 1 d . . . H36A H -0.6133 -0.2253 0.4512 0.020 Uiso 1 1 calc R . . C37 C -0.3259(2) -0.2708(2) 0.61927(14) 0.0155(3) Uani 1 1 d . . . H37A H -0.3017 -0.3358 0.6627 0.019 Uiso 1 1 calc R . . C38 C -0.2037(2) -0.1510(2) 0.62414(14) 0.0148(3) Uani 1 1 d . . . H38A H -0.0989 -0.1354 0.6699 0.018 Uiso 1 1 calc R . . C39 C 0.0542(2) 0.0645(2) 0.59027(15) 0.0170(3) Uani 1 1 d . . . H39A H 0.0860 -0.0268 0.6065 0.020 Uiso 1 1 calc R . . C40 C 0.1696(2) 0.1882(2) 0.59210(15) 0.0165(3) Uani 1 1 d . . . H40A H 0.2795 0.1780 0.6097 0.020 Uiso 1 1 calc R . . O101 O 0.4125(3) 0.4283(3) 1.11339(15) 0.0457(5) Uani 1 1 d U . . C102 C 0.3175(4) 0.5465(5) 1.1188(2) 0.0542(6) Uani 1 1 d U . . H10A H 0.3870 0.6499 1.1563 0.065 Uiso 1 1 calc R . . H10B H 0.2359 0.5214 1.1507 0.065 Uiso 1 1 calc R . . C103 C 0.2364(6) 0.5461(6) 1.0132(3) 0.0713(8) Uani 1 1 d U . . H10C H 0.1247 0.5635 1.0037 0.086 Uiso 1 1 calc R . . H10D H 0.2975 0.6298 0.9951 0.086 Uiso 1 1 calc R . . C104 C 0.2348(5) 0.3951(5) 0.9544(3) 0.0638(7) Uani 1 1 d U . . H10E H 0.2710 0.4068 0.8980 0.077 Uiso 1 1 calc R . . H10F H 0.1240 0.3308 0.9291 0.077 Uiso 1 1 calc R . . C105 C 0.3485(4) 0.3165(4) 1.0183(2) 0.0539(7) Uani 1 1 d U . . H10G H 0.2894 0.2176 1.0229 0.065 Uiso 1 1 calc R . . H10H H 0.4367 0.2934 0.9915 0.065 Uiso 1 1 calc R . . O201 O -0.3419(5) -0.1143(4) 0.0191(2) 0.0895(11) Uani 1 1 d . . . C202 C -0.2207(13) 0.0429(8) 0.0639(7) 0.081(3) Uani 0.548(7) 1 d P A 1 H20B H -0.1099 0.0302 0.0655 0.097 Uiso 0.548(7) 1 calc PR A 1 H20C H -0.2525 0.1211 0.0273 0.097 Uiso 0.548(7) 1 calc PR A 1 C203 C -0.2330(14) 0.0887(8) 0.1668(8) 0.088(3) Uani 0.548(7) 1 d P A 1 H20D H -0.1243 0.1252 0.2163 0.106 Uiso 0.548(7) 1 calc PR A 1 H20E H -0.2957 0.1727 0.1732 0.106 Uiso 0.548(7) 1 calc PR A 1 C204 C -0.3194(10) -0.0599(10) 0.1789(5) 0.068(2) Uani 0.548(7) 1 d P A 1 H20F H -0.2427 -0.1221 0.2077 0.081 Uiso 0.548(7) 1 calc PR A 1 H20G H -0.3913 -0.0385 0.2189 0.081 Uiso 0.548(7) 1 calc PR A 1 C205 C -0.4129(10) -0.1378(9) 0.0739(6) 0.070(2) Uani 0.548(7) 1 d P A 1 H20H H -0.4404 -0.2520 0.0658 0.084 Uiso 0.548(7) 1 calc PR A 1 H20I H -0.5156 -0.0999 0.0565 0.084 Uiso 0.548(7) 1 calc PR A 1 C302 C -0.2074(10) -0.0988(11) 0.0821(7) 0.069(2) Uani 0.452(7) 1 d PU A 2 H30B H -0.1221 -0.0644 0.0549 0.083 Uiso 0.452(7) 1 calc PR A 2 H30C H -0.1948 -0.2029 0.0931 0.083 Uiso 0.452(7) 1 calc PR A 2 C303 C -0.1787(10) 0.0114(12) 0.1776(7) 0.0691(19) Uani 0.452(7) 1 d PU A 2 H30D H -0.0829 0.0957 0.1939 0.083 Uiso 0.452(7) 1 calc PR A 2 H30E H -0.1647 -0.0427 0.2307 0.083 Uiso 0.452(7) 1 calc PR A 2 C304 C -0.3364(11) 0.0754(11) 0.1594(7) 0.0660(18) Uani 0.452(7) 1 d PU A 2 H30F H -0.3990 0.0442 0.2011 0.079 Uiso 0.452(7) 1 calc PR A 2 H30G H -0.3123 0.1910 0.1739 0.079 Uiso 0.452(7) 1 calc PR A 2 C305 C -0.4258(10) 0.0073(10) 0.0571(7) 0.0625(19) Uani 0.452(7) 1 d PU A 2 H30H H -0.4288 0.0887 0.0205 0.075 Uiso 0.452(7) 1 calc PR A 2 H30I H -0.5383 -0.0404 0.0492 0.075 Uiso 0.452(7) 1 calc PR A 2 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 0.00917(10) 0.01243(10) 0.01237(11) 0.00579(8) 0.00135(7) -0.00019(7) N1 0.0133(7) 0.0147(7) 0.0169(8) 0.0057(6) 0.0060(6) 0.0038(6) C1 0.0103(8) 0.0132(7) 0.0138(8) 0.0075(6) 0.0029(6) -0.0004(6) O1 0.0122(6) 0.0158(6) 0.0123(7) 0.0059(5) 0.0025(5) 0.0022(5) C2 0.0136(8) 0.0168(8) 0.0176(8) 0.0062(7) 0.0044(6) 0.0035(6) O2 0.0438(9) 0.0633(11) 0.0205(7) 0.0190(7) 0.0057(6) 0.0339(9) N2 0.0121(7) 0.0135(7) 0.0180(8) 0.0067(6) 0.0042(6) 0.0035(6) C3 0.0175(8) 0.0223(9) 0.0237(10) 0.0124(8) 0.0039(7) 0.0079(7) N3 0.0123(8) 0.0143(8) 0.0165(8) 0.0063(6) 0.0041(6) -0.0008(6) O3 0.0125(7) 0.0147(6) 0.0135(7) 0.0046(5) 0.0008(5) 0.0009(5) C4 0.0229(10) 0.0411(12) 0.0166(9) 0.0150(8) 0.0042(7) 0.0150(9) N4 0.0108(8) 0.0159(8) 0.0143(8) 0.0045(6) 0.0023(6) -0.0008(6) O4 0.0241(8) 0.0737(13) 0.0183(8) 0.0137(8) 0.0007(6) 0.0243(9) C5 0.0202(9) 0.0317(10) 0.0128(9) 0.0072(8) 0.0037(7) 0.0096(8) C6 0.0133(8) 0.0177(8) 0.0144(8) 0.0086(7) 0.0043(6) 0.0029(7) C7 0.0153(9) 0.0167(9) 0.0138(9) 0.0026(7) 0.0041(7) 0.0039(8) C8 0.0214(9) 0.0154(8) 0.0172(9) 0.0051(7) 0.0070(7) 0.0054(7) C9 0.0335(12) 0.0162(9) 0.0380(13) 0.0075(9) 0.0199(10) 0.0027(8) C10 0.0139(8) 0.0184(8) 0.0145(8) 0.0041(6) 0.0011(6) 0.0034(6) C11 0.0192(9) 0.0165(8) 0.0208(10) 0.0030(7) 0.0040(7) 0.0029(7) C12 0.0181(9) 0.0278(10) 0.0224(10) 0.0073(8) 0.0036(7) 0.0026(8) C13 0.0178(9) 0.0389(12) 0.0214(10) 0.0074(9) 0.0074(7) 0.0059(8) C14 0.0262(10) 0.0281(10) 0.0230(10) -0.0005(8) 0.0091(8) 0.0074(8) C15 0.0221(9) 0.0191(9) 0.0208(9) 0.0007(7) 0.0050(7) 0.0027(7) C16 0.0122(8) 0.0125(7) 0.0164(8) 0.0093(6) 0.0035(6) 0.0015(6) C17 0.0163(8) 0.0239(9) 0.0164(8) 0.0069(7) 0.0057(6) 0.0073(7) C18 0.0146(8) 0.0362(11) 0.0233(10) 0.0127(9) 0.0038(7) 0.0129(8) C19 0.0161(8) 0.0415(12) 0.0164(9) 0.0108(8) 0.0004(7) 0.0115(8) C20 0.0211(9) 0.0343(11) 0.0134(9) 0.0048(8) 0.0014(7) 0.0126(8) C21 0.0141(8) 0.0170(8) 0.0146(8) 0.0060(7) 0.0021(6) 0.0039(7) C22 0.0187(10) 0.0207(10) 0.0113(9) 0.0047(8) 0.0029(7) 0.0069(8) C23 0.0150(8) 0.0255(9) 0.0176(9) 0.0083(7) 0.0051(7) 0.0103(7) C24 0.0165(9) 0.0345(12) 0.0269(11) 0.0019(9) 0.0079(8) 0.0067(9) C25 0.0269(10) 0.0199(8) 0.0177(9) 0.0059(7) 0.0077(7) 0.0116(8) C26 0.0312(11) 0.0295(11) 0.0232(10) 0.0119(9) 0.0071(8) 0.0105(9) C27 0.0549(17) 0.0263(11) 0.0366(14) 0.0126(10) 0.0125(12) 0.0001(11) C28 0.074(2) 0.0241(11) 0.0340(15) -0.0009(10) 0.0095(14) -0.0038(13) C29 0.0654(19) 0.0332(13) 0.0234(12) -0.0007(10) 0.0144(12) 0.0041(13) C30 0.0465(14) 0.0252(10) 0.0218(11) 0.0069(8) 0.0139(10) 0.0071(10) C31 0.0144(8) 0.0154(8) 0.0245(10) 0.0107(7) 0.0063(7) 0.0025(6) C32 0.0118(8) 0.0179(8) 0.0230(9) 0.0098(7) 0.0041(7) 0.0025(7) C33 0.0097(8) 0.0148(9) 0.0155(9) 0.0044(7) 0.0035(7) -0.0008(7) C34 0.0126(8) 0.0111(8) 0.0146(9) 0.0048(7) 0.0060(7) 0.0011(7) C35 0.0127(8) 0.0174(8) 0.0198(9) 0.0107(7) 0.0017(6) -0.0005(6) C36 0.0115(8) 0.0181(8) 0.0179(9) 0.0075(7) 0.0000(6) -0.0027(6) C37 0.0134(8) 0.0158(8) 0.0179(9) 0.0089(7) 0.0038(7) 0.0000(6) C38 0.0108(7) 0.0170(8) 0.0160(9) 0.0072(7) 0.0017(6) 0.0015(6) C39 0.0123(8) 0.0153(8) 0.0245(10) 0.0093(7) 0.0053(7) 0.0008(6) C40 0.0099(7) 0.0171(8) 0.0231(9) 0.0085(7) 0.0045(7) 0.0015(6) O101 0.0418(9) 0.0567(11) 0.0347(9) 0.0207(8) 0.0004(7) 0.0079(8) C102 0.0441(12) 0.0847(15) 0.0354(11) 0.0206(11) 0.0071(10) 0.0235(12) C103 0.0667(14) 0.0908(17) 0.0445(13) 0.0171(13) -0.0058(12) 0.0281(14) C104 0.0588(14) 0.0780(15) 0.0419(13) 0.0205(12) -0.0079(11) 0.0147(13) C105 0.0481(12) 0.0608(13) 0.0404(11) 0.0183(11) -0.0058(10) 0.0036(11) O201 0.110(3) 0.077(2) 0.0549(17) -0.0075(15) -0.0024(18) 0.027(2) C202 0.129(8) 0.045(4) 0.072(5) 0.015(4) 0.044(6) 0.000(4) C203 0.099(7) 0.023(3) 0.147(9) 0.008(4) 0.065(7) -0.002(4) C204 0.074(5) 0.100(6) 0.050(4) 0.029(4) 0.032(3) 0.051(4) C205 0.081(5) 0.055(4) 0.072(5) 0.005(4) 0.040(4) -0.010(3) C302 0.046(3) 0.066(3) 0.070(3) -0.022(3) 0.004(2) 0.023(2) C303 0.046(3) 0.065(3) 0.071(3) -0.022(2) 0.003(2) 0.021(2) C304 0.044(3) 0.061(3) 0.070(3) -0.020(2) 0.004(2) 0.022(2) C305 0.044(3) 0.057(3) 0.067(3) -0.013(3) 0.005(2) 0.021(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 O1 1.9914(15) . ? Fe1 O3 2.0053(15) . ? Fe1 N2 2.1523(18) . ? Fe1 N1 2.1555(18) . ? Fe1 N4 2.2580(17) 1_665 ? Fe1 N3 2.3180(17) . ? N1 C7 1.291(3) . ? N1 C8 1.489(3) . ? C1 O1 1.319(2) . ? C1 C2 1.412(3) . ? C1 C6 1.426(3) . ? C2 C3 1.384(3) . ? C2 H2A 0.9500 . ? O2 C4 1.369(2) . ? O2 H2B 0.8400 . ? N2 C22 1.294(3) . ? N2 C23 1.496(2) . ? C3 C4 1.391(3) . ? C3 H3A 0.9500 . ? N3 C40 1.338(3) . ? N3 C31 1.350(3) . ? O3 C16 1.303(2) . ? C4 C5 1.381(3) . ? N4 C36 1.335(3) . ? N4 C37 1.340(2) . ? N4 Fe1 2.2580(16) 1_445 ? O4 C19 1.391(2) . ? O4 H4A 0.8400 . ? C5 C6 1.408(3) . ? C5 H5A 0.9500 . ? C6 C7 1.460(3) . ? C7 H7A 0.9500 . ? C8 C10 1.518(3) . ? C8 C9 1.536(3) . ? C8 H8A 1.0000 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C15 1.397(3) . ? C10 C11 1.401(3) . ? C11 C12 1.379(3) . ? C11 H11A 0.9500 . ? C12 C13 1.388(3) . ? C12 H12A 0.9500 . ? C13 C14 1.381(3) . ? C13 H13A 0.9500 . ? C14 C15 1.396(3) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C16 C17 1.414(3) . ? C16 C21 1.420(3) . ? C17 C18 1.381(3) . ? C17 H17A 0.9500 . ? C18 C19 1.384(3) . ? C18 H18A 0.9500 . ? C19 C20 1.382(3) . ? C20 C21 1.410(3) . ? C20 H20A 0.9500 . ? C21 C22 1.446(3) . ? C22 H22A 0.9500 . ? C23 C25 1.518(3) . ? C23 C24 1.530(3) . ? C23 H23A 1.0000 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.380(3) . ? C25 C30 1.399(3) . ? C26 C27 1.397(3) . ? C26 H26A 0.9500 . ? C27 C28 1.376(4) . ? C27 H27A 0.9500 . ? C28 C29 1.386(4) . ? C28 H28A 0.9500 . ? C29 C30 1.395(4) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C31 C32 1.392(3) . ? C31 H31A 0.9500 . ? C32 C33 1.395(3) . ? C32 H32A 0.9500 . ? C33 C39 1.397(3) . ? C33 C34 1.483(2) . ? C34 C38 1.397(3) . ? C34 C35 1.402(3) . ? C35 C36 1.386(3) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C37 C38 1.389(3) . ? C37 H37A 0.9500 . ? C38 H38A 0.9500 . ? C39 C40 1.390(3) . ? C39 H39A 0.9500 . ? C40 H40A 0.9500 . ? O101 C102 1.430(4) . ? O101 C105 1.449(4) . ? C102 C103 1.519(5) . ? C102 H10A 0.9900 . ? C102 H10B 0.9900 . ? C103 C104 1.437(6) . ? C103 H10C 0.9900 . ? C103 H10D 0.9900 . ? C104 C105 1.519(5) . ? C104 H10E 0.9900 . ? C104 H10F 0.9900 . ? C105 H10G 0.9900 . ? C105 H10H 0.9900 . ? O201 C205 1.186(7) . ? O201 C302 1.252(9) . ? O201 C305 1.489(8) . ? O201 C202 1.539(9) . ? C202 C203 1.525(13) . ? C202 H20B 0.9900 . ? C202 H20C 0.9900 . ? C203 C204 1.510(11) . ? C203 H20D 0.9900 . ? C203 H20E 0.9900 . ? C204 C205 1.496(11) . ? C204 H20F 0.9900 . ? C204 H20G 0.9900 . ? C205 H20H 0.9900 . ? C205 H20I 0.9900 . ? C302 C303 1.472(11) . ? C302 H30B 0.9900 . ? C302 H30C 0.9900 . ? C303 C304 1.544(11) . ? C303 H30D 0.9900 . ? C303 H30E 0.9900 . ? C304 C305 1.445(12) . ? C304 H30F 0.9900 . ? C304 H30G 0.9900 . ? C305 H30H 0.9900 . ? C305 H30I 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Fe1 O3 176.10(7) . . ? O1 Fe1 N2 92.96(6) . . ? O3 Fe1 N2 87.37(6) . . ? O1 Fe1 N1 86.82(6) . . ? O3 Fe1 N1 93.16(6) . . ? N2 Fe1 N1 175.41(7) . . ? O1 Fe1 N4 92.62(6) . 1_665 ? O3 Fe1 N4 91.27(6) . 1_665 ? N2 Fe1 N4 89.05(6) . 1_665 ? N1 Fe1 N4 86.39(7) . 1_665 ? O1 Fe1 N3 88.01(6) . . ? O3 Fe1 N3 88.10(6) . . ? N2 Fe1 N3 90.10(6) . . ? N1 Fe1 N3 94.47(6) . . ? N4 Fe1 N3 178.97(8) 1_665 . ? C7 N1 C8 116.00(18) . . ? C7 N1 Fe1 126.20(14) . . ? C8 N1 Fe1 117.55(13) . . ? O1 C1 C2 119.42(16) . . ? O1 C1 C6 123.84(17) . . ? C2 C1 C6 116.74(17) . . ? C1 O1 Fe1 132.21(12) . . ? C3 C2 C1 122.27(18) . . ? C3 C2 H2A 118.9 . . ? C1 C2 H2A 118.9 . . ? C4 O2 H2B 109.5 . . ? C22 N2 C23 115.44(17) . . ? C22 N2 Fe1 124.90(14) . . ? C23 N2 Fe1 119.62(12) . . ? C2 C3 C4 120.44(18) . . ? C2 C3 H3A 119.8 . . ? C4 C3 H3A 119.8 . . ? C40 N3 C31 116.49(16) . . ? C40 N3 Fe1 121.42(13) . . ? C31 N3 Fe1 121.95(13) . . ? C16 O3 Fe1 131.57(12) . . ? O2 C4 C5 123.0(2) . . ? O2 C4 C3 117.95(19) . . ? C5 C4 C3 119.06(18) . . ? C36 N4 C37 117.23(16) . . ? C36 N4 Fe1 123.39(13) . 1_445 ? C37 N4 Fe1 119.22(13) . 1_445 ? C19 O4 H4A 109.5 . . ? C4 C5 C6 121.57(19) . . ? C4 C5 H5A 119.2 . . ? C6 C5 H5A 119.2 . . ? C5 C6 C1 119.88(18) . . ? C5 C6 C7 116.65(18) . . ? C1 C6 C7 123.41(18) . . ? N1 C7 C6 126.26(19) . . ? N1 C7 H7A 116.9 . . ? C6 C7 H7A 116.9 . . ? N1 C8 C10 112.94(16) . . ? N1 C8 C9 110.13(17) . . ? C10 C8 C9 114.19(16) . . ? N1 C8 H8A 106.3 . . ? C10 C8 H8A 106.3 . . ? C9 C8 H8A 106.3 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C15 C10 C11 117.89(18) . . ? C15 C10 C8 121.62(17) . . ? C11 C10 C8 120.17(17) . . ? C12 C11 C10 121.41(19) . . ? C12 C11 H11A 119.3 . . ? C10 C11 H11A 119.3 . . ? C11 C12 C13 120.3(2) . . ? C11 C12 H12A 119.9 . . ? C13 C12 H12A 119.9 . . ? C14 C13 C12 119.2(2) . . ? C14 C13 H13A 120.4 . . ? C12 C13 H13A 120.4 . . ? C13 C14 C15 120.8(2) . . ? C13 C14 H14A 119.6 . . ? C15 C14 H14A 119.6 . . ? C14 C15 C10 120.35(19) . . ? C14 C15 H15A 119.8 . . ? C10 C15 H15A 119.8 . . ? O3 C16 C17 120.00(17) . . ? O3 C16 C21 123.42(17) . . ? C17 C16 C21 116.57(17) . . ? C18 C17 C16 122.63(18) . . ? C18 C17 H17A 118.7 . . ? C16 C17 H17A 118.7 . . ? C17 C18 C19 120.12(18) . . ? C17 C18 H18A 119.9 . . ? C19 C18 H18A 119.9 . . ? C20 C19 C18 119.38(18) . . ? C20 C19 O4 118.51(19) . . ? C18 C19 O4 122.10(18) . . ? C19 C20 C21 121.44(19) . . ? C19 C20 H20A 119.3 . . ? C21 C20 H20A 119.3 . . ? C20 C21 C16 119.79(18) . . ? C20 C21 C22 115.89(18) . . ? C16 C21 C22 124.28(18) . . ? N2 C22 C21 126.94(19) . . ? N2 C22 H22A 116.5 . . ? C21 C22 H22A 116.5 . . ? N2 C23 C25 111.64(16) . . ? N2 C23 C24 108.90(17) . . ? C25 C23 C24 115.18(17) . . ? N2 C23 H23A 106.9 . . ? C25 C23 H23A 106.9 . . ? C24 C23 H23A 106.9 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C30 118.8(2) . . ? C26 C25 C23 118.56(19) . . ? C30 C25 C23 122.6(2) . . ? C25 C26 C27 121.2(2) . . ? C25 C26 H26A 119.4 . . ? C27 C26 H26A 119.4 . . ? C28 C27 C26 119.8(2) . . ? C28 C27 H27A 120.1 . . ? C26 C27 H27A 120.1 . . ? C27 C28 C29 119.7(2) . . ? C27 C28 H28A 120.2 . . ? C29 C28 H28A 120.2 . . ? C28 C29 C30 120.6(2) . . ? C28 C29 H29A 119.7 . . ? C30 C29 H29A 119.7 . . ? C29 C30 C25 119.9(2) . . ? C29 C30 H30A 120.1 . . ? C25 C30 H30A 120.1 . . ? N3 C31 C32 123.50(18) . . ? N3 C31 H31A 118.3 . . ? C32 C31 H31A 118.3 . . ? C31 C32 C33 119.59(18) . . ? C31 C32 H32A 120.2 . . ? C33 C32 H32A 120.2 . . ? C32 C33 C39 116.92(17) . . ? C32 C33 C34 121.48(15) . . ? C39 C33 C34 121.60(15) . . ? C38 C34 C35 117.00(16) . . ? C38 C34 C33 120.91(15) . . ? C35 C34 C33 122.09(15) . . ? C36 C35 C34 119.29(17) . . ? C36 C35 H35A 120.4 . . ? C34 C35 H35A 120.4 . . ? N4 C36 C35 123.68(17) . . ? N4 C36 H36A 118.2 . . ? C35 C36 H36A 118.2 . . ? N4 C37 C38 123.33(17) . . ? N4 C37 H37A 118.3 . . ? C38 C37 H37A 118.3 . . ? C37 C38 C34 119.47(17) . . ? C37 C38 H38A 120.3 . . ? C34 C38 H38A 120.3 . . ? C40 C39 C33 119.61(18) . . ? C40 C39 H39A 120.2 . . ? C33 C39 H39A 120.2 . . ? N3 C40 C39 123.89(17) . . ? N3 C40 H40A 118.1 . . ? C39 C40 H40A 118.1 . . ? C102 O101 C105 110.2(2) . . ? O101 C102 C103 105.0(3) . . ? O101 C102 H10A 110.8 . . ? C103 C102 H10A 110.8 . . ? O101 C102 H10B 110.8 . . ? C103 C102 H10B 110.8 . . ? H10A C102 H10B 108.8 . . ? C104 C103 C102 106.4(4) . . ? C104 C103 H10C 110.4 . . ? C102 C103 H10C 110.4 . . ? C104 C103 H10D 110.4 . . ? C102 C103 H10D 110.4 . . ? H10C C103 H10D 108.6 . . ? C103 C104 C105 108.0(3) . . ? C103 C104 H10E 110.1 . . ? C105 C104 H10E 110.1 . . ? C103 C104 H10F 110.1 . . ? C105 C104 H10F 110.1 . . ? H10E C104 H10F 108.4 . . ? O101 C105 C104 105.0(3) . . ? O101 C105 H10G 110.7 . . ? C104 C105 H10G 110.7 . . ? O101 C105 H10H 110.7 . . ? C104 C105 H10H 110.7 . . ? H10G C105 H10H 108.8 . . ? C205 O201 C302 92.4(7) . . ? C205 O201 C305 60.9(6) . . ? C302 O201 C305 108.1(5) . . ? C205 O201 C202 109.9(5) . . ? C302 O201 C202 57.2(6) . . ? C305 O201 C202 71.1(5) . . ? C203 C202 O201 101.9(6) . . ? C203 C202 H20B 111.4 . . ? O201 C202 H20B 111.4 . . ? C203 C202 H20C 111.4 . . ? O201 C202 H20C 111.4 . . ? H20B C202 H20C 109.3 . . ? C204 C203 C202 104.3(6) . . ? C204 C203 H20D 110.9 . . ? C202 C203 H20D 110.9 . . ? C204 C203 H20E 110.9 . . ? C202 C203 H20E 110.9 . . ? H20D C203 H20E 108.9 . . ? C205 C204 C203 99.4(7) . . ? C205 C204 H20F 111.9 . . ? C203 C204 H20F 111.9 . . ? C205 C204 H20G 111.9 . . ? C203 C204 H20G 111.9 . . ? H20F C204 H20G 109.6 . . ? O201 C205 C204 113.3(7) . . ? O201 C205 H20H 108.9 . . ? C204 C205 H20H 108.9 . . ? O201 C205 H20I 108.9 . . ? C204 C205 H20I 108.9 . . ? H20H C205 H20I 107.7 . . ? O201 C302 C303 116.4(6) . . ? O201 C302 H30B 108.2 . . ? C303 C302 H30B 108.2 . . ? O201 C302 H30C 108.2 . . ? C303 C302 H30C 108.2 . . ? H30B C302 H30C 107.3 . . ? C302 C303 C304 101.3(7) . . ? C302 C303 H30D 111.5 . . ? C304 C303 H30D 111.5 . . ? C302 C303 H30E 111.5 . . ? C304 C303 H30E 111.5 . . ? H30D C303 H30E 109.3 . . ? C305 C304 C303 105.5(7) . . ? C305 C304 H30F 110.6 . . ? C303 C304 H30F 110.6 . . ? C305 C304 H30G 110.6 . . ? C303 C304 H30G 110.6 . . ? H30F C304 H30G 108.8 . . ? C304 C305 O201 107.4(6) . . ? C304 C305 H30H 110.2 . . ? O201 C305 H30H 110.2 . . ? C304 C305 H30I 110.2 . . ? O201 C305 H30I 110.2 . . ? H30H C305 H30I 108.5 . . ? 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 O2 H2B O4 0.84 1.89 2.729(3) 176.6 1_656 O4 H4A O101 0.84 1.83 2.660(3) 171.5 1_454 _diffrn_measured_fraction_theta_max 0.925 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.215 _refine_diff_density_min -0.628 _refine_diff_density_rms 0.069