# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_1 _database_code_depnum_ccdc_archive 'CCDC 895300' #TrackingRef 'compound_1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H22 Fe N2 O6, C9 H22 N,2(C H4 O)' _chemical_formula_sum 'C39 H52 Fe N3 O8' _chemical_formula_weight 746.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Pc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' _cell_length_a 12.7901(4) _cell_length_b 11.2349(3) _cell_length_c 17.2291(6) _cell_angle_alpha 90.00 _cell_angle_beta 130.203(2) _cell_angle_gamma 90.00 _cell_volume 1890.88(12) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 14482 _cell_measurement_theta_min 2.9698 _cell_measurement_theta_max 33.3585 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.311 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 794 _exptl_absorpt_coefficient_mu 0.454 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.98355 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.5 (release 18-04-2008 CrysAlis171 .NET) (compiled Apr 18 2008,18:17:43) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm ; _exptl_special_details ; face-indexed (CrysAlis RED; Oxford Diffraction, 2006) ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Goniometer KM4/Xcalibur detector: Sapphire2 (large Be window)' _diffrn_measurement_method ; Rotation method data acquisition using omega and phi scans ; _diffrn_detector_area_resol_mean 8.3611 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16025 _diffrn_reflns_av_R_equivalents 0.0205 _diffrn_reflns_av_sigmaI/netI 0.0269 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6213 _reflns_number_gt 5764 _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 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'MERCURY (Macrae et al., 2006)' _computing_publication_material ' enCIFer (Allen et al., 2004)' _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^)+(0.0647P)^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' _refine_ls_abs_structure_Flack 0.041(11) _refine_ls_number_reflns 6213 _refine_ls_number_parameters 465 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0374 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.0910 _refine_ls_wR_factor_gt 0.0899 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _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 C1 C 1.1265(3) 0.5624(2) 1.12809(19) 0.0260(6) Uani 1 1 d . . . C1S C 0.5523(4) 0.2305(4) 1.0653(3) 0.0754(13) Uani 1 1 d . . . H1C1 H 0.4894 0.2022 0.9949 0.113 Uiso 1 1 calc R . . H2C1 H 0.5487 0.3176 1.0662 0.113 Uiso 1 1 calc R . . H3C1 H 0.5255 0.1970 1.1027 0.113 Uiso 1 1 calc R . . C2 C 1.1510(3) 0.4846(2) 1.2037(2) 0.0328(7) Uani 1 1 d . . . C2S C 0.7464(5) 0.3727(4) 0.9819(4) 0.0876(16) Uani 1 1 d . . . H2C2 H 0.6792 0.3809 0.9078 0.131 Uiso 1 1 calc R . . H3C2 H 0.8273 0.4210 1.0088 0.131 Uiso 1 1 calc R . . H1C2 H 0.7059 0.4000 1.0114 0.131 Uiso 1 1 calc R . . C3 C 1.2757(4) 0.4790(3) 1.2981(2) 0.0448(8) Uani 1 1 d . . . H3 H 1.2886 0.4280 1.3476 0.054 Uiso 1 1 calc R . . C4 C 1.3848(4) 0.5470(4) 1.3233(3) 0.0579(10) Uani 1 1 d . . . H4 H 1.4719 0.5415 1.3893 0.070 Uiso 1 1 calc R . . C5 C 1.3660(3) 0.6217(3) 1.2527(2) 0.0501(9) Uani 1 1 d . . . H5 H 1.4407 0.6683 1.2705 0.060 Uiso 1 1 calc R . . C6 C 1.2382(3) 0.6311(3) 1.1541(2) 0.0331(7) Uani 1 1 d . . . C7 C 1.2254(3) 0.7112(2) 1.0850(2) 0.0274(6) Uani 1 1 d . . . H7 H 1.3068 0.7507 1.1083 0.033 Uiso 1 1 calc R . . C8 C 1.1156(3) 0.8250(2) 0.9344(2) 0.0198(6) Uani 1 1 d . . . C9 C 1.2294(3) 0.8834(2) 0.9600(2) 0.0292(6) Uani 1 1 d . . . H9 H 1.3179 0.8628 1.0209 0.035 Uiso 1 1 calc R . . C10 C 1.2154(3) 0.9718(3) 0.8975(2) 0.0334(7) Uani 1 1 d . . . H10 H 1.2935 1.0119 0.9151 0.040 Uiso 1 1 calc R . . C11 C 1.0856(3) 1.0003(2) 0.8091(2) 0.0321(7) Uani 1 1 d . . . H11 H 1.0753 1.0610 0.7661 0.039 Uiso 1 1 calc R . . C12 C 0.9711(3) 0.9426(2) 0.7819(2) 0.0265(6) Uani 1 1 d . . . H12 H 0.8829 0.9641 0.7211 0.032 Uiso 1 1 calc R . . C13 C 0.9848(3) 0.8520(2) 0.8443(2) 0.0219(6) Uani 1 1 d . . . C14 C 0.7752(3) 0.4921(2) 0.75958(18) 0.0219(6) Uani 1 1 d . . . C15 C 0.7916(3) 0.4125(2) 0.70363(19) 0.0237(6) Uani 1 1 d . . . C16 C 0.6803(3) 0.3563(2) 0.6174(2) 0.0284(6) Uani 1 1 d . . . H16 H 0.6927 0.3052 0.5800 0.034 Uiso 1 1 calc R . . C17 C 0.5495(3) 0.3745(3) 0.5849(2) 0.0339(7) Uani 1 1 d . . . H17 H 0.4733 0.3349 0.5258 0.041 Uiso 1 1 calc R . . C18 C 0.5308(3) 0.4484(3) 0.6371(2) 0.0327(6) Uani 1 1 d . . . H18 H 0.4413 0.4588 0.6149 0.039 Uiso 1 1 calc R . . C19 C 0.6421(3) 0.5104(2) 0.7244(2) 0.0252(6) Uani 1 1 d . . . C20 C 0.6132(3) 0.5919(2) 0.7723(2) 0.0259(6) Uani 1 1 d . . . H20 H 0.5209 0.5959 0.7451 0.031 Uiso 1 1 calc R . . C21 C 0.6598(3) 0.7436(2) 0.8864(2) 0.0236(6) Uani 1 1 d . . . C22 C 0.5273(3) 0.7571(3) 0.8534(2) 0.0333(7) Uani 1 1 d . . . H22 H 0.4552 0.7065 0.8022 0.040 Uiso 1 1 calc R . . C23 C 0.5029(3) 0.8446(3) 0.8960(2) 0.0371(7) Uani 1 1 d . . . H23 H 0.4137 0.8536 0.8744 0.045 Uiso 1 1 calc R . . C24 C 0.6067(3) 0.9193(3) 0.9698(2) 0.0343(7) Uani 1 1 d . . . H24 H 0.5880 0.9803 0.9975 0.041 Uiso 1 1 calc R . . C25 C 0.7384(3) 0.9059(2) 1.0039(2) 0.0304(7) Uani 1 1 d . . . H25 H 0.8092 0.9576 1.0549 0.037 Uiso 1 1 calc R . . C26 C 0.7672(3) 0.8169(2) 0.9636(2) 0.0239(6) Uani 1 1 d . . . C27 C 1.0526(4) 0.3505(3) 1.2476(3) 0.0489(9) Uani 1 1 d . . . H27A H 0.9656 0.3099 1.2161 0.073 Uiso 1 1 calc R . . H27B H 1.0754 0.4020 1.3026 0.073 Uiso 1 1 calc R . . H27C H 1.1251 0.2912 1.2753 0.073 Uiso 1 1 calc R . . C28 C 0.9474(3) 0.3180(2) 0.6932(3) 0.0352(7) Uani 1 1 d . . . H28A H 1.0459 0.3130 0.7301 0.053 Uiso 1 1 calc R . . H28B H 0.9004 0.3485 0.6245 0.053 Uiso 1 1 calc R . . H28C H 0.9121 0.2387 0.6890 0.053 Uiso 1 1 calc R . . C29 C 0.2064(4) 0.6195(4) 0.4889(3) 0.0703(12) Uani 1 1 d . . . H29A H 0.2717 0.6339 0.4781 0.105 Uiso 1 1 calc R . . H29B H 0.1403 0.5587 0.4411 0.105 Uiso 1 1 calc R . . H29C H 0.2556 0.5918 0.5587 0.105 Uiso 1 1 calc R . . C30 C 0.1322(4) 0.7326(3) 0.4720(3) 0.0527(9) Uani 1 1 d . . . H30A H 0.0834 0.7612 0.4018 0.063 Uiso 1 1 calc R . . H30B H 0.1990 0.7944 0.5196 0.063 Uiso 1 1 calc R . . C31 C 0.0313(4) 0.7127(3) 0.4882(2) 0.0401(8) Uani 1 1 d . A . H31A H 0.0827 0.6917 0.5604 0.048 Uiso 1 1 calc R . . H31B H -0.0268 0.6436 0.4467 0.048 Uiso 1 1 calc R . . C32 C -0.3931(4) 0.9273(4) 0.2107(3) 0.0662(11) Uani 1 1 d . . . H32A H -0.4573 0.9902 0.1950 0.099 Uiso 1 1 calc R . . H32B H -0.4387 0.8498 0.1925 0.099 Uiso 1 1 calc R . . H32C H -0.3627 0.9405 0.1717 0.099 Uiso 1 1 calc R . . C34 C -0.2697(4) 0.9292(3) 0.3239(3) 0.0486(9) Uani 1 1 d . . . H34A H -0.2246 1.0080 0.3424 0.058 Uiso 1 1 calc R . . H34B H -0.3007 0.9173 0.3632 0.058 Uiso 1 1 calc R . . C35 C -0.1684(4) 0.8336(3) 0.3513(3) 0.0433(9) Uani 1 1 d . A . H35A H -0.2177 0.7574 0.3205 0.052 Uiso 1 1 calc R . . H35B H -0.1244 0.8543 0.3224 0.052 Uiso 1 1 calc R . . C37A C 0.0276(4) 0.9318(3) 0.5161(3) 0.0492(9) Uani 0.728(5) 1 d P A 1 H37A H 0.0758 0.9497 0.4900 0.059 Uiso 0.728(5) 1 calc PR A 1 H37B H -0.0330 1.0001 0.4991 0.059 Uiso 0.728(5) 1 calc PR A 1 C37B C 0.0276(4) 0.9318(3) 0.5161(3) 0.0492(9) Uani 0.272(5) 1 d P A 2 H37C H 0.1215 0.9051 0.5484 0.059 Uiso 0.272(5) 1 calc PR A 2 H37D H 0.0000 0.9844 0.4594 0.059 Uiso 0.272(5) 1 calc PR A 2 C38A C 0.1320(4) 0.9183(3) 0.6304(3) 0.0273(8) Uani 0.728(5) 1 d P A 1 H38A H 0.0854 0.8998 0.6577 0.033 Uiso 0.728(5) 1 calc PR A 1 H38B H 0.1959 0.8526 0.6489 0.033 Uiso 0.728(5) 1 calc PR A 1 C38B C 0.0433(11) 1.0002(9) 0.5785(7) 0.0273(8) Uani 0.272(5) 1 d P A 2 H38C H 0.0034 0.9641 0.6067 0.033 Uiso 0.272(5) 1 calc PR A 2 H38D H -0.0065 1.0752 0.5440 0.033 Uiso 0.272(5) 1 calc PR A 2 C39A C 0.2071(4) 1.0309(3) 0.6731(3) 0.0465(8) Uani 0.728(5) 1 d P A 1 H39A H 0.2755 1.0244 0.7472 0.070 Uiso 0.728(5) 1 calc PR A 1 H39B H 0.1429 1.0953 0.6547 0.070 Uiso 0.728(5) 1 calc PR A 1 H39C H 0.2529 1.0484 0.6457 0.070 Uiso 0.728(5) 1 calc PR A 1 C39B C 0.2071(4) 1.0309(3) 0.6731(3) 0.0465(8) Uani 0.272(5) 1 d P A 2 H39D H 0.2147 1.0858 0.7207 0.070 Uiso 0.272(5) 1 calc PR A 2 H39E H 0.2467 1.0679 0.6457 0.070 Uiso 0.272(5) 1 calc PR A 2 H39F H 0.2564 0.9572 0.7086 0.070 Uiso 0.272(5) 1 calc PR A 2 Fe1 Fe 0.91387(3) 0.67714(3) 0.92411(2) 0.01924(10) Uani 1 1 d . . . N1 N 1.1162(2) 0.73702(19) 0.99408(16) 0.0212(5) Uani 1 1 d . . . N2 N 0.7001(2) 0.66094(18) 0.84889(17) 0.0221(5) Uani 1 1 d . . . N3 N -0.0619(3) 0.81787(19) 0.4620(2) 0.0376(7) Uani 1 1 d . . . H3A H -0.1048 0.8020 0.4871 0.045 Uiso 1 1 d R A . O1 O 1.0047(2) 0.56689(16) 1.03866(14) 0.0267(5) Uani 1 1 d . . . O1S O 0.6873(3) 0.1940(3) 1.1118(2) 0.0717(9) Uani 1 1 d . . . H1O1 H 0.7216 0.1588 1.1666 0.108 Uiso 1 1 calc R . . O2 O 0.87729(19) 0.79338(17) 0.81990(13) 0.0246(4) Uani 1 1 d . . . O2S O 0.7851(3) 0.2521(3) 1.0076(2) 0.0760(9) Uani 1 1 d . . . H1O2 H 0.7631 0.2269 1.0412 0.114 Uiso 1 1 calc R . . O3 O 0.88395(18) 0.54301(16) 0.84078(13) 0.0250(4) Uani 1 1 d . . . O4 O 0.8918(2) 0.80150(15) 0.99466(15) 0.0260(5) Uani 1 1 d . . . O5 O 1.0404(2) 0.4210(2) 1.17284(16) 0.0404(6) Uani 1 1 d . . . O6 O 0.9241(2) 0.39598(17) 0.74545(14) 0.0296(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0352(16) 0.0225(14) 0.0207(14) 0.0007(11) 0.0183(13) 0.0069(12) C1S 0.052(3) 0.075(3) 0.052(2) -0.016(2) 0.012(2) 0.013(2) C2 0.0483(19) 0.0272(14) 0.0261(15) 0.0008(12) 0.0255(15) 0.0092(14) C2S 0.059(3) 0.065(3) 0.065(3) 0.017(2) 0.007(2) -0.008(2) C3 0.056(2) 0.0414(17) 0.0288(17) 0.0120(14) 0.0239(17) 0.0092(17) C4 0.047(2) 0.067(2) 0.0275(18) 0.0167(16) 0.0098(17) 0.0060(19) C5 0.0344(19) 0.055(2) 0.0366(19) 0.0092(16) 0.0121(16) 0.0019(16) C6 0.0338(17) 0.0350(16) 0.0233(15) 0.0009(12) 0.0151(13) 0.0030(13) C7 0.0214(14) 0.0304(14) 0.0272(15) -0.0005(12) 0.0143(13) 0.0005(12) C8 0.0251(15) 0.0181(13) 0.0252(14) -0.0020(10) 0.0203(13) 0.0021(11) C9 0.0322(16) 0.0278(14) 0.0319(15) -0.0052(12) 0.0226(14) -0.0035(13) C10 0.0392(18) 0.0295(15) 0.0455(19) -0.0046(13) 0.0337(16) -0.0097(13) C11 0.0456(18) 0.0233(14) 0.0437(18) 0.0032(12) 0.0362(16) 0.0002(13) C12 0.0383(17) 0.0240(14) 0.0262(15) 0.0043(11) 0.0249(14) 0.0049(12) C13 0.0313(16) 0.0187(13) 0.0258(14) -0.0046(11) 0.0230(13) -0.0020(12) C14 0.0281(15) 0.0193(13) 0.0186(13) 0.0019(10) 0.0153(12) -0.0005(11) C15 0.0311(16) 0.0212(13) 0.0188(14) 0.0011(11) 0.0161(12) 0.0006(12) C16 0.0397(18) 0.0248(14) 0.0237(14) -0.0028(11) 0.0218(14) 0.0009(13) C17 0.0361(18) 0.0305(15) 0.0225(14) -0.0082(12) 0.0132(13) -0.0079(13) C18 0.0256(15) 0.0372(16) 0.0281(15) -0.0039(12) 0.0140(13) -0.0012(12) C19 0.0254(15) 0.0236(14) 0.0231(14) -0.0009(11) 0.0140(12) -0.0011(11) C20 0.0237(15) 0.0299(14) 0.0250(14) 0.0000(12) 0.0161(12) 0.0008(12) C21 0.0293(15) 0.0212(13) 0.0231(13) 0.0048(10) 0.0181(12) 0.0072(11) C22 0.0358(17) 0.0349(16) 0.0314(16) 0.0019(12) 0.0227(14) 0.0059(13) C23 0.0393(18) 0.0403(17) 0.0419(18) 0.0129(14) 0.0308(16) 0.0197(14) C24 0.053(2) 0.0293(15) 0.0378(17) 0.0060(13) 0.0367(17) 0.0157(15) C25 0.0494(19) 0.0219(14) 0.0300(15) 0.0033(11) 0.0301(15) 0.0035(13) C26 0.0337(19) 0.0233(14) 0.0233(15) 0.0047(11) 0.0222(14) 0.0042(12) C27 0.075(3) 0.0400(18) 0.044(2) 0.0183(15) 0.044(2) 0.0107(18) C28 0.0446(19) 0.0325(16) 0.0430(18) -0.0124(13) 0.0348(16) -0.0041(14) C29 0.050(2) 0.100(3) 0.064(3) 0.012(2) 0.038(2) 0.018(2) C30 0.060(2) 0.047(2) 0.042(2) -0.0043(16) 0.0290(18) -0.0106(19) C31 0.056(2) 0.0301(15) 0.0367(18) 0.0000(14) 0.0309(18) -0.0019(15) C32 0.048(2) 0.084(3) 0.045(2) -0.015(2) 0.0202(19) 0.002(2) C34 0.062(2) 0.0332(18) 0.052(2) -0.0055(15) 0.037(2) -0.0021(17) C35 0.054(2) 0.0355(18) 0.0381(19) -0.0072(14) 0.0289(18) 0.0002(15) C37A 0.053(2) 0.0374(19) 0.048(2) 0.0052(15) 0.0287(19) 0.0040(16) C37B 0.053(2) 0.0374(19) 0.048(2) 0.0052(15) 0.0287(19) 0.0040(16) C38A 0.037(2) 0.0248(18) 0.0214(18) 0.0022(14) 0.0194(17) -0.0004(15) C38B 0.037(2) 0.0248(18) 0.0214(18) 0.0022(14) 0.0194(17) -0.0004(15) C39A 0.049(2) 0.051(2) 0.0417(19) 0.0129(15) 0.0301(17) 0.0046(16) C39B 0.049(2) 0.051(2) 0.0417(19) 0.0129(15) 0.0301(17) 0.0046(16) Fe1 0.0231(2) 0.01891(17) 0.01776(17) -0.00111(16) 0.01407(15) -0.00158(18) N1 0.0240(12) 0.0241(12) 0.0196(12) -0.0021(9) 0.0159(10) 0.0007(9) N2 0.0273(13) 0.0217(11) 0.0221(12) 0.0019(9) 0.0181(11) 0.0012(9) N3 0.065(2) 0.0216(12) 0.0384(16) 0.0018(10) 0.0388(17) 0.0066(11) O1 0.0322(12) 0.0232(10) 0.0216(10) 0.0019(8) 0.0160(9) -0.0013(8) O1S 0.0608(18) 0.090(2) 0.0357(14) -0.0101(13) 0.0184(13) 0.0303(15) O2 0.0248(11) 0.0271(9) 0.0225(10) 0.0021(8) 0.0155(9) -0.0018(8) O2S 0.092(2) 0.071(2) 0.087(2) -0.0119(16) 0.068(2) -0.0076(16) O3 0.0265(11) 0.0260(10) 0.0230(10) -0.0075(8) 0.0162(9) -0.0028(8) O4 0.0325(12) 0.0231(10) 0.0273(11) -0.0029(8) 0.0216(10) -0.0029(9) O5 0.0564(15) 0.0368(12) 0.0353(12) 0.0111(9) 0.0329(12) 0.0024(11) O6 0.0342(12) 0.0317(10) 0.0302(10) -0.0084(8) 0.0241(10) -0.0023(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.306(3) . ? C1 C6 1.419(4) . ? C1 C2 1.425(4) . ? C1S O1S 1.416(5) . ? C1S H1C1 0.9800 . ? C1S H2C1 0.9800 . ? C1S H3C1 0.9800 . ? C2 O5 1.351(4) . ? C2 C3 1.357(4) . ? C2S O2S 1.412(5) . ? C2S H2C2 0.9800 . ? C2S H3C2 0.9800 . ? C2S H1C2 0.9800 . ? C3 C4 1.392(5) . ? C3 H3 0.9500 . ? C4 C5 1.365(5) . ? C4 H4 0.9500 . ? C5 C6 1.409(4) . ? C5 H5 0.9500 . ? C6 C7 1.415(4) . ? C7 N1 1.290(3) . ? C7 H7 0.9500 . ? C8 C9 1.384(4) . ? C8 C13 1.396(4) . ? C8 N1 1.422(3) . ? C9 C10 1.390(4) . ? C9 H9 0.9500 . ? C10 C11 1.383(4) . ? C10 H10 0.9500 . ? C11 C12 1.378(4) . ? C11 H11 0.9500 . ? C12 C13 1.408(4) . ? C12 H12 0.9500 . ? C13 O2 1.324(3) . ? C14 O3 1.306(3) . ? C14 C19 1.406(4) . ? C14 C15 1.426(4) . ? C15 O6 1.359(3) . ? C15 C16 1.379(4) . ? C16 C17 1.394(4) . ? C16 H16 0.9500 . ? C17 C18 1.355(4) . ? C17 H17 0.9500 . ? C18 C19 1.418(4) . ? C18 H18 0.9500 . ? C19 C20 1.431(4) . ? C20 N2 1.298(3) . ? C20 H20 0.9500 . ? C21 C22 1.405(4) . ? C21 C26 1.406(4) . ? C21 N2 1.407(3) . ? C22 C23 1.377(4) . ? C22 H22 0.9500 . ? C23 C24 1.380(5) . ? C23 H23 0.9500 . ? C24 C25 1.387(5) . ? C24 H24 0.9500 . ? C25 C26 1.395(4) . ? C25 H25 0.9500 . ? C26 O4 1.325(4) . ? C27 O5 1.432(3) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 O6 1.419(3) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.498(6) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.504(5) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 N3 1.524(4) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C34 1.524(5) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C34 C35 1.506(5) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 N3 1.473(5) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C37A C38A 1.514(5) . ? C37A N3 1.562(4) . ? C37A H37A 0.9900 . ? C37A H37B 0.9900 . ? C38A C39A 1.467(5) . ? C38A H38A 0.9900 . ? C38A H38B 0.9900 . ? C38B H38C 0.9900 . ? C38B H38D 0.9900 . ? C39A H39A 0.9800 . ? C39A H39B 0.9800 . ? C39A H39C 0.9800 . ? Fe1 O3 1.9414(17) . ? Fe1 O1 1.9542(18) . ? Fe1 O4 1.9881(19) . ? Fe1 O2 2.0159(18) . ? Fe1 N1 2.139(2) . ? Fe1 N2 2.148(2) . ? N3 H3A 0.9109 . ? O1S H1O1 0.8400 . ? O2S H1O2 0.8400 . ? 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 C1 C6 122.9(2) . . ? O1 C1 C2 119.6(3) . . ? C6 C1 C2 117.5(3) . . ? O1S C1S H1C1 109.5 . . ? O1S C1S H2C1 109.5 . . ? H1C1 C1S H2C1 109.5 . . ? O1S C1S H3C1 109.5 . . ? H1C1 C1S H3C1 109.5 . . ? H2C1 C1S H3C1 109.5 . . ? O5 C2 C3 124.7(3) . . ? O5 C2 C1 114.1(3) . . ? C3 C2 C1 121.2(3) . . ? O2S C2S H2C2 109.5 . . ? O2S C2S H3C2 109.5 . . ? H2C2 C2S H3C2 109.5 . . ? O2S C2S H1C2 109.5 . . ? H2C2 C2S H1C2 109.5 . . ? H3C2 C2S H1C2 109.5 . . ? C2 C3 C4 120.9(3) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? C5 C4 C3 119.7(3) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C4 C5 C6 121.4(3) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C5 C6 C7 118.5(3) . . ? C5 C6 C1 119.2(3) . . ? C7 C6 C1 122.3(3) . . ? N1 C7 C6 127.7(3) . . ? N1 C7 H7 116.2 . . ? C6 C7 H7 116.2 . . ? C9 C8 C13 120.7(2) . . ? C9 C8 N1 125.8(3) . . ? C13 C8 N1 113.5(2) . . ? C8 C9 C10 120.6(3) . . ? C8 C9 H9 119.7 . . ? C10 C9 H9 119.7 . . ? C11 C10 C9 118.8(3) . . ? C11 C10 H10 120.6 . . ? C9 C10 H10 120.6 . . ? C12 C11 C10 121.4(2) . . ? C12 C11 H11 119.3 . . ? C10 C11 H11 119.3 . . ? C11 C12 C13 120.0(3) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? O2 C13 C8 119.9(2) . . ? O2 C13 C12 121.7(3) . . ? C8 C13 C12 118.4(2) . . ? O3 C14 C19 123.6(2) . . ? O3 C14 C15 118.6(2) . . ? C19 C14 C15 117.8(2) . . ? O6 C15 C16 125.1(2) . . ? O6 C15 C14 113.8(2) . . ? C16 C15 C14 121.0(3) . . ? C15 C16 C17 120.2(3) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C18 C17 C16 120.3(3) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C17 C18 C19 121.2(3) . . ? C17 C18 H18 119.4 . . ? C19 C18 H18 119.4 . . ? C14 C19 C18 119.5(2) . . ? C14 C19 C20 122.4(2) . . ? C18 C19 C20 118.0(3) . . ? N2 C20 C19 126.7(3) . . ? N2 C20 H20 116.6 . . ? C19 C20 H20 116.6 . . ? C22 C21 C26 120.4(2) . . ? C22 C21 N2 126.1(3) . . ? C26 C21 N2 113.4(2) . . ? C23 C22 C21 119.3(3) . . ? C23 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? C22 C23 C24 120.7(3) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? C23 C24 C25 120.5(3) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C24 C25 C26 120.3(3) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? O4 C26 C25 121.9(3) . . ? O4 C26 C21 119.4(2) . . ? C25 C26 C21 118.7(3) . . ? O5 C27 H27A 109.5 . . ? O5 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O5 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O6 C28 H28A 109.5 . . ? O6 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? O6 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 H29A 109.5 . . ? C30 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C30 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C29 C30 C31 110.5(3) . . ? C29 C30 H30A 109.6 . . ? C31 C30 H30A 109.6 . . ? C29 C30 H30B 109.6 . . ? C31 C30 H30B 109.6 . . ? H30A C30 H30B 108.1 . . ? C30 C31 N3 115.5(3) . . ? C30 C31 H31A 108.4 . . ? N3 C31 H31A 108.4 . . ? C30 C31 H31B 108.4 . . ? N3 C31 H31B 108.4 . . ? H31A C31 H31B 107.5 . . ? C34 C32 H32A 109.5 . . ? C34 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C34 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C35 C34 C32 111.2(3) . . ? C35 C34 H34A 109.4 . . ? C32 C34 H34A 109.4 . . ? C35 C34 H34B 109.4 . . ? C32 C34 H34B 109.4 . . ? H34A C34 H34B 108.0 . . ? N3 C35 C34 112.4(3) . . ? N3 C35 H35A 109.1 . . ? C34 C35 H35A 109.1 . . ? N3 C35 H35B 109.1 . . ? C34 C35 H35B 109.1 . . ? H35A C35 H35B 107.9 . . ? C38A C37A N3 112.7(3) . . ? C38A C37A H37A 109.1 . . ? N3 C37A H37A 109.1 . . ? C38A C37A H37B 109.1 . . ? N3 C37A H37B 109.1 . . ? H37A C37A H37B 107.8 . . ? C39A C38A C37A 107.9(3) . . ? C39A C38A H38A 110.1 . . ? C37A C38A H38A 110.1 . . ? C39A C38A H38B 110.1 . . ? C37A C38A H38B 110.1 . . ? H38A C38A H38B 108.4 . . ? H38C C38B H38D 107.9 . . ? C38A C39A H39A 109.5 . . ? C38A C39A H39B 109.5 . . ? H39A C39A H39B 109.5 . . ? C38A C39A H39C 109.5 . . ? H39A C39A H39C 109.5 . . ? H39B C39A H39C 109.5 . . ? O3 Fe1 O1 87.70(8) . . ? O3 Fe1 O4 163.66(8) . . ? O1 Fe1 O4 93.12(8) . . ? O3 Fe1 O2 91.29(8) . . ? O1 Fe1 O2 162.75(8) . . ? O4 Fe1 O2 92.66(7) . . ? O3 Fe1 N1 104.49(8) . . ? O1 Fe1 N1 85.18(8) . . ? O4 Fe1 N1 91.83(8) . . ? O2 Fe1 N1 78.40(8) . . ? O3 Fe1 N2 85.50(8) . . ? O1 Fe1 N2 104.54(8) . . ? O4 Fe1 N2 78.50(9) . . ? O2 Fe1 N2 92.53(8) . . ? N1 Fe1 N2 166.51(9) . . ? C7 N1 C8 122.0(2) . . ? C7 N1 Fe1 125.58(18) . . ? C8 N1 Fe1 111.77(17) . . ? C20 N2 C21 122.3(2) . . ? C20 N2 Fe1 125.81(18) . . ? C21 N2 Fe1 111.63(17) . . ? C35 N3 C31 111.7(2) . . ? C35 N3 C37A 112.6(2) . . ? C31 N3 C37A 109.1(3) . . ? C35 N3 H3A 107.5 . . ? C31 N3 H3A 107.7 . . ? C37A N3 H3A 108.1 . . ? C1 O1 Fe1 134.03(17) . . ? C1S O1S H1O1 109.5 . . ? C13 O2 Fe1 116.28(17) . . ? C2S O2S H1O2 109.5 . . ? C14 O3 Fe1 134.18(16) . . ? C26 O4 Fe1 116.99(17) . . ? C2 O5 C27 117.4(3) . . ? C15 O6 C28 116.7(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 O5 0.2(4) . . . . ? C6 C1 C2 O5 -179.1(2) . . . . ? O1 C1 C2 C3 -178.8(3) . . . . ? C6 C1 C2 C3 1.8(4) . . . . ? O5 C2 C3 C4 179.4(3) . . . . ? C1 C2 C3 C4 -1.7(5) . . . . ? C2 C3 C4 C5 0.9(6) . . . . ? C3 C4 C5 C6 -0.4(6) . . . . ? C4 C5 C6 C7 179.3(3) . . . . ? C4 C5 C6 C1 0.7(5) . . . . ? O1 C1 C6 C5 179.4(3) . . . . ? C2 C1 C6 C5 -1.3(4) . . . . ? O1 C1 C6 C7 0.8(4) . . . . ? C2 C1 C6 C7 -179.9(3) . . . . ? C5 C6 C7 N1 -175.9(3) . . . . ? C1 C6 C7 N1 2.7(5) . . . . ? C13 C8 C9 C10 1.4(4) . . . . ? N1 C8 C9 C10 -177.2(2) . . . . ? C8 C9 C10 C11 -0.1(4) . . . . ? C9 C10 C11 C12 -0.4(4) . . . . ? C10 C11 C12 C13 -0.5(4) . . . . ? C9 C8 C13 O2 178.5(2) . . . . ? N1 C8 C13 O2 -2.8(3) . . . . ? C9 C8 C13 C12 -2.2(4) . . . . ? N1 C8 C13 C12 176.5(2) . . . . ? C11 C12 C13 O2 -179.0(2) . . . . ? C11 C12 C13 C8 1.7(4) . . . . ? O3 C14 C15 O6 2.1(3) . . . . ? C19 C14 C15 O6 -177.2(2) . . . . ? O3 C14 C15 C16 180.0(2) . . . . ? C19 C14 C15 C16 0.6(4) . . . . ? O6 C15 C16 C17 175.9(2) . . . . ? C14 C15 C16 C17 -1.6(4) . . . . ? C15 C16 C17 C18 0.7(4) . . . . ? C16 C17 C18 C19 1.2(4) . . . . ? O3 C14 C19 C18 -178.1(2) . . . . ? C15 C14 C19 C18 1.2(4) . . . . ? O3 C14 C19 C20 3.3(4) . . . . ? C15 C14 C19 C20 -177.4(2) . . . . ? C17 C18 C19 C14 -2.2(4) . . . . ? C17 C18 C19 C20 176.6(3) . . . . ? C14 C19 C20 N2 2.7(4) . . . . ? C18 C19 C20 N2 -176.0(3) . . . . ? C26 C21 C22 C23 1.3(4) . . . . ? N2 C21 C22 C23 -178.4(3) . . . . ? C21 C22 C23 C24 0.6(4) . . . . ? C22 C23 C24 C25 -1.3(4) . . . . ? C23 C24 C25 C26 0.2(4) . . . . ? C24 C25 C26 O4 -179.8(2) . . . . ? C24 C25 C26 C21 1.6(4) . . . . ? C22 C21 C26 O4 179.0(2) . . . . ? N2 C21 C26 O4 -1.3(3) . . . . ? C22 C21 C26 C25 -2.4(4) . . . . ? N2 C21 C26 C25 177.3(2) . . . . ? C29 C30 C31 N3 -173.6(3) . . . . ? C32 C34 C35 N3 -168.9(3) . . . . ? N3 C37A C38A C39A -178.5(3) . . . . ? C6 C7 N1 C8 176.1(3) . . . . ? C6 C7 N1 Fe1 6.1(4) . . . . ? C9 C8 N1 C7 7.0(4) . . . . ? C13 C8 N1 C7 -171.6(2) . . . . ? C9 C8 N1 Fe1 178.3(2) . . . . ? C13 C8 N1 Fe1 -0.3(2) . . . . ? O3 Fe1 N1 C7 -98.8(2) . . . . ? O1 Fe1 N1 C7 -12.4(2) . . . . ? O4 Fe1 N1 C7 80.6(2) . . . . ? O2 Fe1 N1 C7 172.9(2) . . . . ? N2 Fe1 N1 C7 124.4(4) . . . . ? O3 Fe1 N1 C8 90.38(16) . . . . ? O1 Fe1 N1 C8 176.74(16) . . . . ? O4 Fe1 N1 C8 -90.29(15) . . . . ? O2 Fe1 N1 C8 2.05(15) . . . . ? N2 Fe1 N1 C8 -46.5(4) . . . . ? C19 C20 N2 C21 175.9(2) . . . . ? C19 C20 N2 Fe1 2.1(4) . . . . ? C22 C21 N2 C20 5.0(4) . . . . ? C26 C21 N2 C20 -174.7(2) . . . . ? C22 C21 N2 Fe1 179.6(2) . . . . ? C26 C21 N2 Fe1 -0.1(3) . . . . ? O3 Fe1 N2 C20 -8.1(2) . . . . ? O1 Fe1 N2 C20 -94.5(2) . . . . ? O4 Fe1 N2 C20 175.2(2) . . . . ? O2 Fe1 N2 C20 83.0(2) . . . . ? N1 Fe1 N2 C20 130.3(3) . . . . ? O3 Fe1 N2 C21 177.53(17) . . . . ? O1 Fe1 N2 C21 91.09(16) . . . . ? O4 Fe1 N2 C21 0.83(15) . . . . ? O2 Fe1 N2 C21 -91.37(16) . . . . ? N1 Fe1 N2 C21 -44.1(4) . . . . ? C34 C35 N3 C31 174.4(3) . . . . ? C34 C35 N3 C37A -62.5(4) . . . . ? C30 C31 N3 C35 74.1(4) . . . . ? C30 C31 N3 C37A -50.9(4) . . . . ? C38A C37A N3 C35 176.8(3) . . . . ? C38A C37A N3 C31 -58.7(4) . . . . ? C6 C1 O1 Fe1 -15.3(4) . . . . ? C2 C1 O1 Fe1 165.45(18) . . . . ? O3 Fe1 O1 C1 122.5(2) . . . . ? O4 Fe1 O1 C1 -73.9(2) . . . . ? O2 Fe1 O1 C1 35.5(4) . . . . ? N1 Fe1 O1 C1 17.7(2) . . . . ? N2 Fe1 O1 C1 -152.8(2) . . . . ? C8 C13 O2 Fe1 4.8(3) . . . . ? C12 C13 O2 Fe1 -174.56(18) . . . . ? O3 Fe1 O2 C13 -108.15(18) . . . . ? O1 Fe1 O2 C13 -21.7(4) . . . . ? O4 Fe1 O2 C13 87.71(19) . . . . ? N1 Fe1 O2 C13 -3.62(17) . . . . ? N2 Fe1 O2 C13 166.31(17) . . . . ? C19 C14 O3 Fe1 -15.7(4) . . . . ? C15 C14 O3 Fe1 164.99(17) . . . . ? O1 Fe1 O3 C14 120.2(2) . . . . ? O4 Fe1 O3 C14 27.0(4) . . . . ? O2 Fe1 O3 C14 -77.0(2) . . . . ? N1 Fe1 O3 C14 -155.4(2) . . . . ? N2 Fe1 O3 C14 15.4(2) . . . . ? C25 C26 O4 Fe1 -176.47(19) . . . . ? C21 C26 O4 Fe1 2.1(3) . . . . ? O3 Fe1 O4 C26 -13.3(4) . . . . ? O1 Fe1 O4 C26 -105.76(18) . . . . ? O2 Fe1 O4 C26 90.49(18) . . . . ? N1 Fe1 O4 C26 168.97(18) . . . . ? N2 Fe1 O4 C26 -1.55(17) . . . . ? C3 C2 O5 C27 5.6(4) . . . . ? C1 C2 O5 C27 -173.4(2) . . . . ? C16 C15 O6 C28 2.5(4) . . . . ? C14 C15 O6 C28 -179.8(2) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.557 _refine_diff_density_min -0.271 _refine_diff_density_rms 0.054 data_2b _database_code_depnum_ccdc_archive 'CCDC 895301' #TrackingRef 'compound_2b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H46 Fe2 n5 O16 Tb, 3(H2 O)' _chemical_formula_sum 'C56 H52 Fe2 N5 O19 Tb' _chemical_formula_weight 1369.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.8762(4) _cell_length_b 16.7247(3) _cell_length_c 22.2668(5) _cell_angle_alpha 90.00 _cell_angle_beta 108.368(2) _cell_angle_gamma 90.00 _cell_volume 5611.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 14680 _cell_measurement_theta_min 2.9375 _cell_measurement_theta_max 33.3339 _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.621 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2768 _exptl_absorpt_coefficient_mu 1.837 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.91946 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.5 (release 18-04-2008 CrysAlis171 .NET) (compiled Apr 18 2008,18:17:43) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm ; _exptl_special_details ; face-indexed (CrysAlis RED; Oxford Diffraction, 2006) ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Goniometer KM4/Xcalibur detector: Sapphire2 (large Be window)' _diffrn_measurement_method ; Rotation method data acquisition using omega and phi scans ; _diffrn_detector_area_resol_mean 8.3611 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28976 _diffrn_reflns_av_R_equivalents 0.0417 _diffrn_reflns_av_sigmaI/netI 0.0554 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9862 _reflns_number_gt 6891 _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 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'MERCURY (Macrae et al., 2006)' _computing_publication_material ' enCIFer (Allen et al., 2004)' _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^)+(0.0352P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9862 _refine_ls_number_parameters 752 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0559 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.0654 _refine_ls_wR_factor_gt 0.0616 _refine_ls_goodness_of_fit_ref 0.901 _refine_ls_restrained_S_all 0.901 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.188172(11) 0.507639(9) 0.294116(8) 0.01681(5) Uani 1 1 d . . . Fe1 Fe 0.28054(3) 0.47154(3) 0.16872(3) 0.02132(13) Uani 1 1 d . . . Fe2 Fe -0.01194(3) 0.48735(3) 0.33563(2) 0.01570(11) Uani 1 1 d . . . O1 O 0.30575(16) 0.45104(13) 0.26578(11) 0.0222(6) Uani 1 1 d . . . O2 O 0.27978(18) 0.53165(15) 0.09408(12) 0.0308(6) Uani 1 1 d . . . O3 O 0.35103(18) 0.37902(15) 0.16084(13) 0.0340(7) Uani 1 1 d . . . O4 O 0.17100(14) 0.51176(13) 0.18562(10) 0.0177(5) Uani 1 1 d . . . O5 O 0.2796(2) 0.54977(19) -0.02916(14) 0.0465(8) Uani 1 1 d . . . O6 O 0.07707(16) 0.61440(13) 0.22086(11) 0.0186(6) Uani 1 1 d . . . O7 O 0.30952(17) 0.52918(14) 0.39214(12) 0.0268(6) Uani 1 1 d . . . O8 O 0.23813(18) 0.41841(14) 0.38667(12) 0.0281(6) Uani 1 1 d . . . O9 O 0.3443(2) 0.44857(17) 0.47275(13) 0.0424(8) Uani 1 1 d . . . O10 O 0.25165(17) 0.63331(13) 0.29019(12) 0.0266(6) Uani 1 1 d . . . H10A H 0.2969 0.6592 0.3116 0.040 Uiso 1 1 d R . . H10B H 0.2215 0.6643 0.2610 0.040 Uiso 1 1 d R . . O11 O 0.10287(15) 0.55495(13) 0.35756(11) 0.0185(5) Uani 1 1 d . . . O12 O -0.06639(17) 0.38361(13) 0.33176(11) 0.0217(6) Uani 1 1 d . . . O13 O -0.08447(16) 0.56598(13) 0.36018(11) 0.0221(6) Uani 1 1 d . . . O14 O 0.04568(15) 0.45636(13) 0.27120(11) 0.0168(5) Uani 1 1 d . . . O15 O 0.15573(17) 0.35739(13) 0.25464(12) 0.0244(6) Uani 1 1 d . . . O16 O -0.18763(17) 0.26349(13) 0.29063(12) 0.0239(6) Uani 1 1 d . . . N1 N 0.3924(2) 0.54490(19) 0.21443(15) 0.0265(7) Uani 1 1 d . . . N2 N 0.1830(2) 0.39798(16) 0.09986(14) 0.0206(7) Uani 1 1 d . . . N5 N 0.2985(2) 0.46425(19) 0.41915(15) 0.0276(8) Uani 1 1 d . . . N4 N -0.12347(18) 0.50402(16) 0.24698(12) 0.0171(6) Uani 1 1 d . . . N3 N 0.05346(19) 0.45784(16) 0.43218(13) 0.0185(7) Uani 1 1 d . . . C1 C 0.3924(2) 0.4592(2) 0.29863(18) 0.0247(9) Uani 1 1 d . . . C2 C 0.4351(3) 0.4172(2) 0.35344(19) 0.0301(10) Uani 1 1 d . . . H2 H 0.4043 0.3789 0.3685 0.036 Uiso 1 1 calc R . . C3 C 0.5232(3) 0.4322(3) 0.3855(2) 0.0430(12) Uani 1 1 d . . . H3 H 0.5512 0.4050 0.4229 0.052 Uiso 1 1 calc R . . C4 C 0.5703(3) 0.4873(3) 0.3628(2) 0.0545(13) Uani 1 1 d . . . H4 H 0.6295 0.4975 0.3851 0.065 Uiso 1 1 calc R . . C5 C 0.5288(3) 0.5276(3) 0.3063(2) 0.0476(12) Uani 1 1 d . . . H5 H 0.5605 0.5638 0.2901 0.057 Uiso 1 1 calc R . . C6 C 0.4403(2) 0.5134(2) 0.27466(18) 0.0297(9) Uani 1 1 d . . . C7 C 0.4176(3) 0.6101(2) 0.1935(2) 0.0323(10) Uani 1 1 d . . . H7 H 0.4572 0.6431 0.2227 0.039 Uiso 1 1 calc R . . C8 C 0.3889(3) 0.6350(2) 0.1286(2) 0.0306(10) Uani 1 1 d . . . C9 C 0.4330(3) 0.6995(2) 0.1112(2) 0.0388(11) Uani 1 1 d . . . H9 H 0.4699 0.7319 0.1425 0.047 Uiso 1 1 calc R . . C10 C 0.4227(3) 0.7154(3) 0.0494(2) 0.0433(12) Uani 1 1 d . . . H10 H 0.4496 0.7601 0.0384 0.052 Uiso 1 1 calc R . . C11 C 0.3718(3) 0.6648(3) 0.0031(2) 0.0464(12) Uani 1 1 d . . . H11 H 0.3679 0.6738 -0.0389 0.056 Uiso 1 1 calc R . . C12 C 0.3269(3) 0.6011(3) 0.0178(2) 0.0370(11) Uani 1 1 d . . . C13 C 0.3295(3) 0.5879(2) 0.0817(2) 0.0307(10) Uani 1 1 d . . . C14 C 0.3239(3) 0.4748(3) -0.0256(2) 0.0550(14) Uani 1 1 d . . . H14A H 0.3322 0.4511 0.0151 0.082 Uiso 1 1 calc R . . H14B H 0.3806 0.4831 -0.0315 0.082 Uiso 1 1 calc R . . H14C H 0.2887 0.4399 -0.0580 0.082 Uiso 1 1 calc R . . C15 C 0.3178(3) 0.3328(2) 0.1096(2) 0.0326(10) Uani 1 1 d . . . C16 C 0.3700(3) 0.2800(3) 0.0883(2) 0.0525(14) Uani 1 1 d . . . H16 H 0.4307 0.2765 0.1092 0.063 Uiso 1 1 calc R . . C17 C 0.3315(4) 0.2330(3) 0.0362(3) 0.0568(15) Uani 1 1 d . . . H17 H 0.3667 0.1971 0.0228 0.068 Uiso 1 1 calc R . . C18 C 0.2425(3) 0.2377(2) 0.0035(2) 0.0431(12) Uani 1 1 d . . . H18 H 0.2177 0.2053 -0.0316 0.052 Uiso 1 1 calc R . . C19 C 0.1905(3) 0.2904(2) 0.02294(19) 0.0310(10) Uani 1 1 d . . . H19 H 0.1304 0.2944 0.0006 0.037 Uiso 1 1 calc R . . C20 C 0.2272(3) 0.3380(2) 0.07600(18) 0.0258(9) Uani 1 1 d . . . C21 C 0.0994(3) 0.41149(19) 0.07448(17) 0.0205(8) Uani 1 1 d . . . H21 H 0.0683 0.3781 0.0416 0.025 Uiso 1 1 calc R . . C22 C 0.0501(2) 0.47434(19) 0.09298(16) 0.0187(8) Uani 1 1 d . . . C23 C -0.0381(2) 0.4873(2) 0.05756(16) 0.0207(8) Uani 1 1 d . . . H23 H -0.0640 0.4549 0.0227 0.025 Uiso 1 1 calc R . . C24 C -0.0878(3) 0.5460(2) 0.07231(17) 0.0234(9) Uani 1 1 d . . . H24 H -0.1458 0.5549 0.0466 0.028 Uiso 1 1 calc R . . C25 C -0.0510(2) 0.5928(2) 0.12628(17) 0.0207(8) Uani 1 1 d . . . H25 H -0.0842 0.6330 0.1369 0.025 Uiso 1 1 calc R . . C26 C 0.0348(2) 0.57851(18) 0.16350(16) 0.0163(8) Uani 1 1 d . . . C27 C 0.0876(2) 0.52148(18) 0.14649(16) 0.0156(7) Uani 1 1 d . . . C28 C 0.0285(3) 0.6748(2) 0.24219(18) 0.0246(9) Uani 1 1 d . . . H28A H -0.0241 0.6517 0.2473 0.037 Uiso 1 1 calc R . . H28B H 0.0123 0.7171 0.2115 0.037 Uiso 1 1 calc R . . H28C H 0.0649 0.6960 0.2819 0.037 Uiso 1 1 calc R . . C29 C 0.1376(2) 0.5699(2) 0.42038(16) 0.0196(8) Uani 1 1 d . . . C30 C 0.1970(2) 0.6320(2) 0.44389(18) 0.0228(9) Uani 1 1 d . . . H30 H 0.2119 0.6668 0.4162 0.027 Uiso 1 1 calc R . . C31 C 0.2340(3) 0.6419(2) 0.50848(19) 0.0267(9) Uani 1 1 d . . . H31 H 0.2740 0.6832 0.5242 0.032 Uiso 1 1 calc R . . C32 C 0.2122(3) 0.5910(2) 0.54974(18) 0.0272(9) Uani 1 1 d . . . H32 H 0.2375 0.5982 0.5931 0.033 Uiso 1 1 calc R . . C33 C 0.1529(2) 0.5294(2) 0.52729(17) 0.0237(9) Uani 1 1 d . . . H33 H 0.1380 0.4954 0.5554 0.028 Uiso 1 1 calc R . . C34 C 0.1157(2) 0.51819(19) 0.46253(15) 0.0166(7) Uani 1 1 d . . . C35 C 0.0401(2) 0.3968(2) 0.46334(17) 0.0200(8) Uani 1 1 d . . . H35 H 0.0737 0.3932 0.5058 0.024 Uiso 1 1 calc R . . C36 C -0.0222(2) 0.3340(2) 0.43779(17) 0.0192(8) Uani 1 1 d . . . C37 C -0.0344(3) 0.2754(2) 0.47971(18) 0.0225(8) Uani 1 1 d . . . H37 H -0.0002 0.2773 0.5221 0.027 Uiso 1 1 calc R . . C38 C -0.0958(3) 0.2156(2) 0.45914(19) 0.0271(9) Uani 1 1 d . . . H38 H -0.1033 0.1775 0.4874 0.033 Uiso 1 1 calc R . . C39 C -0.1467(3) 0.2123(2) 0.39569(18) 0.0241(9) Uani 1 1 d . . . H39 H -0.1881 0.1716 0.3816 0.029 Uiso 1 1 calc R . . C40 C -0.1365(2) 0.26853(19) 0.35377(17) 0.0189(8) Uani 1 1 d . . . C41 C -0.0736(2) 0.33125(19) 0.37351(17) 0.0178(8) Uani 1 1 d . . . C42 C -0.1630(3) 0.5850(2) 0.31995(17) 0.0222(9) Uani 1 1 d . . . C43 C -0.2237(3) 0.6331(2) 0.3374(2) 0.0271(9) Uani 1 1 d . . . H43 H -0.2101 0.6516 0.3787 0.032 Uiso 1 1 calc R . . C44 C -0.3036(3) 0.6532(2) 0.2934(2) 0.0328(10) Uani 1 1 d . . . H44 H -0.3434 0.6851 0.3055 0.039 Uiso 1 1 calc R . . C45 C -0.3258(3) 0.6269(2) 0.2313(2) 0.0313(10) Uani 1 1 d . . . H45 H -0.3792 0.6423 0.2019 0.038 Uiso 1 1 calc R . . C46 C -0.2681(3) 0.5775(2) 0.21352(19) 0.0271(9) Uani 1 1 d . . . H46 H -0.2830 0.5588 0.1721 0.032 Uiso 1 1 calc R . . C47 C -0.1875(2) 0.5556(2) 0.25756(18) 0.0216(8) Uani 1 1 d . . . C48 C -0.1403(2) 0.4572(2) 0.19885(17) 0.0214(8) Uani 1 1 d . . . H48 H -0.1964 0.4596 0.1690 0.026 Uiso 1 1 calc R . . C49 C -0.0773(2) 0.40126(19) 0.18844(16) 0.0176(8) Uani 1 1 d . . . C50 C -0.1051(3) 0.3438(2) 0.14008(17) 0.0220(8) Uani 1 1 d . . . H50 H -0.1640 0.3430 0.1143 0.026 Uiso 1 1 calc R . . C51 C -0.0464(3) 0.2889(2) 0.13062(17) 0.0251(9) Uani 1 1 d . . . H51 H -0.0661 0.2509 0.0988 0.030 Uiso 1 1 calc R . . C52 C 0.0428(3) 0.2895(2) 0.16832(17) 0.0219(8) Uani 1 1 d . . . H52 H 0.0825 0.2521 0.1620 0.026 Uiso 1 1 calc R . . C53 C 0.0707(2) 0.34639(19) 0.21479(17) 0.0196(8) Uani 1 1 d . . . C54 C 0.0116(2) 0.40254(19) 0.22536(16) 0.0165(8) Uani 1 1 d . . . C55 C 0.2174(3) 0.2944(2) 0.2580(2) 0.0412(12) Uani 1 1 d . . . H55A H 0.2318 0.2924 0.2192 0.062 Uiso 1 1 calc R . . H55B H 0.1916 0.2444 0.2642 0.062 Uiso 1 1 calc R . . H55C H 0.2704 0.3038 0.2927 0.062 Uiso 1 1 calc R . . C56 C -0.2557(3) 0.3233(2) 0.2723(2) 0.0343(10) Uani 1 1 d . . . H56A H -0.2295 0.3754 0.2820 0.051 Uiso 1 1 calc R . . H56B H -0.2975 0.3151 0.2949 0.051 Uiso 1 1 calc R . . H56C H -0.2858 0.3195 0.2276 0.051 Uiso 1 1 calc R . . O1S O 0.5297(2) 0.11970(17) 0.04771(16) 0.0560(9) Uani 1 1 d . . . H1S1 H 0.5722 0.0864 0.0534 0.084 Uiso 1 1 d R . . H2S1 H 0.4825 0.0917 0.0380 0.084 Uiso 1 1 d R . . O2S O 0.5034(3) 0.3056(2) 0.23494(18) 0.0860(13) Uani 1 1 d . . . H1S2 H 0.4639 0.3426 0.2231 0.129 Uiso 1 1 d R . . H2S2 H 0.5337 0.3091 0.2090 0.129 Uiso 1 1 d R . . O3S O 0.5961(2) 0.2097(2) 0.1575(2) 0.0896(15) Uani 1 1 d . . . H1S3 H 0.5776 0.2029 0.1177 0.134 Uiso 1 1 d R . . H2S3 H 0.5625 0.1827 0.1726 0.134 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.01452(9) 0.01770(9) 0.01744(9) 0.00180(8) 0.00391(6) -0.00065(7) Fe1 0.0173(3) 0.0223(3) 0.0251(3) 0.0031(2) 0.0078(2) 0.0036(2) Fe2 0.0154(3) 0.0185(3) 0.0128(2) 0.0001(2) 0.0040(2) -0.0012(2) O1 0.0156(14) 0.0220(13) 0.0264(15) 0.0032(11) 0.0029(12) 0.0035(10) O2 0.0272(16) 0.0356(15) 0.0304(16) 0.0098(12) 0.0101(13) -0.0020(12) O3 0.0247(17) 0.0371(16) 0.0378(18) 0.0006(13) 0.0065(14) 0.0139(12) O4 0.0145(13) 0.0199(12) 0.0183(12) 0.0002(10) 0.0046(10) 0.0030(10) O5 0.039(2) 0.063(2) 0.0337(19) 0.0162(16) 0.0047(16) -0.0068(16) O6 0.0176(15) 0.0180(12) 0.0203(14) -0.0048(10) 0.0063(12) 0.0038(10) O7 0.0247(16) 0.0250(14) 0.0277(15) 0.0050(12) 0.0039(12) 0.0000(11) O8 0.0313(17) 0.0232(14) 0.0251(15) 0.0040(11) 0.0024(13) -0.0017(12) O9 0.0403(19) 0.0527(18) 0.0235(17) 0.0125(14) -0.0053(15) 0.0080(15) O10 0.0245(16) 0.0199(13) 0.0272(15) 0.0070(11) -0.0037(13) -0.0050(11) O11 0.0215(14) 0.0186(12) 0.0143(13) -0.0015(10) 0.0038(11) -0.0032(10) O12 0.0282(16) 0.0197(13) 0.0163(14) 0.0023(10) 0.0058(12) -0.0053(10) O13 0.0211(15) 0.0246(13) 0.0189(14) -0.0029(10) 0.0041(12) 0.0037(10) O14 0.0192(14) 0.0164(12) 0.0161(13) -0.0032(10) 0.0070(11) -0.0038(10) O15 0.0200(15) 0.0205(13) 0.0308(16) -0.0015(11) 0.0055(13) 0.0029(10) O16 0.0250(16) 0.0199(13) 0.0241(15) -0.0061(11) 0.0040(13) -0.0038(11) N1 0.0165(18) 0.0341(18) 0.0279(19) 0.0089(15) 0.0055(15) 0.0015(14) N2 0.026(2) 0.0157(15) 0.0224(18) 0.0032(12) 0.0114(15) 0.0032(13) N5 0.025(2) 0.0333(19) 0.0220(19) 0.0050(15) 0.0032(16) 0.0073(15) N4 0.0164(15) 0.0211(15) 0.0132(14) 0.0019(13) 0.0039(12) -0.0006(13) N3 0.0194(17) 0.0194(15) 0.0164(16) -0.0010(13) 0.0053(13) -0.0001(12) C1 0.016(2) 0.032(2) 0.026(2) -0.0007(17) 0.0058(18) 0.0047(16) C2 0.025(2) 0.033(2) 0.029(2) 0.0063(18) 0.0053(19) 0.0077(17) C3 0.031(3) 0.053(3) 0.038(3) 0.012(2) 0.001(2) 0.011(2) C4 0.021(2) 0.075(3) 0.056(3) 0.013(3) -0.005(2) 0.000(2) C5 0.021(2) 0.063(3) 0.053(3) 0.018(2) 0.004(2) -0.005(2) C6 0.020(2) 0.034(2) 0.034(2) 0.0070(18) 0.0063(18) 0.0038(17) C7 0.022(2) 0.035(2) 0.039(3) 0.0006(19) 0.008(2) -0.0016(17) C8 0.025(2) 0.027(2) 0.042(3) 0.0123(18) 0.013(2) 0.0066(17) C9 0.029(3) 0.028(2) 0.058(3) 0.012(2) 0.014(2) 0.0036(18) C10 0.038(3) 0.034(2) 0.061(3) 0.022(2) 0.020(3) 0.004(2) C11 0.038(3) 0.054(3) 0.048(3) 0.028(2) 0.014(2) 0.002(2) C12 0.026(3) 0.045(3) 0.039(3) 0.015(2) 0.008(2) 0.0031(19) C13 0.022(2) 0.032(2) 0.040(3) 0.0158(19) 0.013(2) 0.0088(18) C14 0.053(3) 0.072(4) 0.043(3) -0.005(3) 0.020(3) -0.004(3) C15 0.040(3) 0.025(2) 0.034(3) -0.0009(18) 0.013(2) 0.0064(18) C16 0.034(3) 0.052(3) 0.071(4) -0.007(3) 0.015(3) 0.019(2) C17 0.063(4) 0.038(3) 0.073(4) -0.019(3) 0.028(3) 0.019(2) C18 0.053(3) 0.032(2) 0.051(3) -0.009(2) 0.026(3) 0.003(2) C19 0.035(3) 0.025(2) 0.037(3) -0.0017(18) 0.018(2) 0.0013(17) C20 0.035(3) 0.0188(19) 0.029(2) 0.0025(16) 0.019(2) 0.0055(16) C21 0.026(2) 0.0181(18) 0.018(2) 0.0024(15) 0.0082(18) -0.0007(15) C22 0.022(2) 0.0169(18) 0.0188(19) 0.0041(14) 0.0091(16) 0.0025(14) C23 0.024(2) 0.0219(19) 0.0159(17) 0.0002(15) 0.0063(15) -0.0037(16) C24 0.020(2) 0.027(2) 0.021(2) 0.0083(16) 0.0032(17) 0.0017(16) C25 0.023(2) 0.0196(19) 0.021(2) 0.0047(15) 0.0092(18) 0.0047(15) C26 0.024(2) 0.0124(17) 0.0130(18) 0.0030(14) 0.0060(16) -0.0021(14) C27 0.0161(19) 0.0137(17) 0.0181(18) 0.0050(14) 0.0070(15) -0.0003(13) C28 0.025(2) 0.023(2) 0.028(2) -0.0039(16) 0.0114(19) 0.0024(16) C29 0.021(2) 0.0201(19) 0.017(2) -0.0026(15) 0.0063(17) 0.0075(15) C30 0.019(2) 0.0205(19) 0.028(2) -0.0035(16) 0.0056(18) -0.0031(15) C31 0.018(2) 0.024(2) 0.035(2) -0.0126(17) 0.0039(19) -0.0037(15) C32 0.022(2) 0.038(2) 0.018(2) -0.0100(17) -0.0002(18) 0.0050(17) C33 0.022(2) 0.028(2) 0.021(2) -0.0029(16) 0.0071(17) 0.0035(16) C34 0.0134(18) 0.0187(18) 0.0153(17) -0.0039(14) 0.0012(14) 0.0008(14) C35 0.017(2) 0.027(2) 0.0149(19) 0.0036(16) 0.0031(16) 0.0033(15) C36 0.015(2) 0.0221(19) 0.021(2) 0.0002(15) 0.0064(17) 0.0031(15) C37 0.022(2) 0.024(2) 0.023(2) 0.0070(16) 0.0105(17) 0.0035(16) C38 0.032(2) 0.021(2) 0.031(2) 0.0113(16) 0.013(2) 0.0031(17) C39 0.025(2) 0.0164(19) 0.035(2) -0.0029(16) 0.015(2) -0.0035(15) C40 0.018(2) 0.0186(18) 0.020(2) -0.0015(15) 0.0068(17) 0.0036(14) C41 0.018(2) 0.0152(18) 0.021(2) 0.0011(15) 0.0083(17) 0.0027(14) C42 0.027(2) 0.0159(18) 0.026(2) 0.0025(15) 0.0116(19) -0.0033(15) C43 0.028(2) 0.023(2) 0.035(2) -0.0035(17) 0.016(2) -0.0007(16) C44 0.028(2) 0.023(2) 0.054(3) -0.006(2) 0.021(2) -0.0001(18) C45 0.016(2) 0.030(2) 0.045(3) 0.0064(19) 0.006(2) 0.0008(17) C46 0.024(2) 0.027(2) 0.027(2) 0.0025(17) 0.0040(19) 0.0003(17) C47 0.019(2) 0.0192(19) 0.029(2) 0.0046(16) 0.0118(18) -0.0013(15) C48 0.020(2) 0.0253(19) 0.017(2) 0.0075(16) 0.0032(17) -0.0031(16) C49 0.021(2) 0.0172(18) 0.0159(19) 0.0031(14) 0.0070(17) -0.0043(14) C50 0.025(2) 0.0230(19) 0.017(2) -0.0004(15) 0.0039(17) -0.0049(16) C51 0.037(3) 0.022(2) 0.017(2) -0.0043(15) 0.0102(19) -0.0083(17) C52 0.031(2) 0.0166(18) 0.022(2) 0.0019(15) 0.0151(19) -0.0018(15) C53 0.022(2) 0.0171(18) 0.022(2) 0.0030(15) 0.0103(18) -0.0029(15) C54 0.021(2) 0.0159(18) 0.0137(19) 0.0019(14) 0.0071(16) -0.0033(14) C55 0.032(3) 0.020(2) 0.065(3) -0.005(2) 0.006(2) 0.0052(18) C56 0.033(3) 0.027(2) 0.034(3) -0.0017(18) -0.001(2) 0.0005(18) O1S 0.035(2) 0.0458(19) 0.069(2) -0.0004(16) -0.0088(18) 0.0063(15) O2S 0.064(3) 0.116(3) 0.068(3) 0.000(2) 0.006(2) 0.050(2) O3S 0.045(2) 0.073(3) 0.110(4) -0.033(2) -0.033(2) 0.0271(19) _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 Tb1 O14 2.321(2) . ? Tb1 O10 2.344(2) . ? Tb1 O4 2.345(2) . ? Tb1 O1 2.350(2) . ? Tb1 O11 2.379(2) . ? Tb1 O7 2.440(3) . ? Tb1 O8 2.464(2) . ? Tb1 O15 2.658(2) . ? Tb1 O6 2.673(2) . ? Tb1 N5 2.876(3) . ? Fe1 O2 1.939(3) . ? Fe1 O3 1.950(3) . ? Fe1 O4 2.008(2) . ? Fe1 O1 2.099(2) . ? Fe1 N1 2.135(3) . ? Fe1 N2 2.184(3) . ? Fe2 O12 1.928(2) . ? Fe2 O13 1.937(2) . ? Fe2 O14 1.998(2) . ? Fe2 O11 2.068(2) . ? Fe2 N3 2.130(3) . ? Fe2 N4 2.215(3) . ? O1 C1 1.347(4) . ? O2 C13 1.311(4) . ? O3 C15 1.341(5) . ? O4 C27 1.346(4) . ? O5 C12 1.378(5) . ? O5 C14 1.427(5) . ? O6 C26 1.379(4) . ? O6 C28 1.440(4) . ? O7 N5 1.280(4) . ? O8 N5 1.262(4) . ? O9 N5 1.214(4) . ? O10 H10A 0.8458 . ? O10 H10B 0.8510 . ? O11 C29 1.355(4) . ? O12 C41 1.308(4) . ? O13 C42 1.324(4) . ? O14 C54 1.341(4) . ? O15 C53 1.375(4) . ? O15 C55 1.425(4) . ? O16 C40 1.387(4) . ? O16 C56 1.435(4) . ? N1 C7 1.298(5) . ? N1 C6 1.418(5) . ? N2 C21 1.287(5) . ? N2 C20 1.420(5) . ? N4 C48 1.285(4) . ? N4 C47 1.408(4) . ? N3 C35 1.289(4) . ? N3 C34 1.425(4) . ? C1 C2 1.386(5) . ? C1 C6 1.393(5) . ? C2 C3 1.379(6) . ? C2 H2 0.9300 . ? C3 C4 1.379(6) . ? C3 H3 0.9300 . ? C4 C5 1.398(6) . ? C4 H4 0.9300 . ? C5 C6 1.379(6) . ? C5 H5 0.9300 . ? C7 C8 1.432(6) . ? C7 H7 0.9300 . ? C8 C9 1.406(5) . ? C8 C13 1.407(6) . ? C9 C10 1.360(6) . ? C9 H9 0.9300 . ? C10 C11 1.382(7) . ? C10 H10 0.9300 . ? C11 C12 1.378(6) . ? C11 H11 0.9300 . ? C12 C13 1.428(6) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.394(6) . ? C15 C20 1.399(6) . ? C16 C17 1.374(7) . ? C16 H16 0.9300 . ? C17 C18 1.374(7) . ? C17 H17 0.9300 . ? C18 C19 1.368(6) . ? C18 H18 0.9300 . ? C19 C20 1.391(5) . ? C19 H19 0.9300 . ? C21 C22 1.446(5) . ? C21 H21 0.9300 . ? C22 C23 1.391(5) . ? C22 C27 1.396(5) . ? C23 C24 1.363(5) . ? C23 H23 0.9300 . ? C24 C25 1.398(5) . ? C24 H24 0.9300 . ? C25 C26 1.374(5) . ? C25 H25 0.9300 . ? C26 C27 1.399(5) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C30 1.390(5) . ? C29 C34 1.398(5) . ? C30 C31 1.381(5) . ? C30 H30 0.9300 . ? C31 C32 1.374(5) . ? C31 H31 0.9300 . ? C32 C33 1.379(5) . ? C32 H32 0.9300 . ? C33 C34 1.388(5) . ? C33 H33 0.9300 . ? C35 C36 1.433(5) . ? C35 H35 0.9300 . ? C36 C41 1.407(5) . ? C36 C37 1.408(5) . ? C37 C38 1.370(5) . ? C37 H37 0.9300 . ? C38 C39 1.390(5) . ? C38 H38 0.9300 . ? C39 C40 1.370(5) . ? C39 H39 0.9300 . ? C40 C41 1.419(5) . ? C42 C43 1.403(5) . ? C42 C47 1.408(5) . ? C43 C44 1.378(6) . ? C43 H43 0.9300 . ? C44 C45 1.386(6) . ? C44 H44 0.9300 . ? C45 C46 1.382(5) . ? C45 H45 0.9300 . ? C46 C47 1.393(5) . ? C46 H46 0.9300 . ? C48 C49 1.441(5) . ? C48 H48 0.9300 . ? C49 C54 1.391(5) . ? C49 C50 1.407(5) . ? C50 C51 1.370(5) . ? C50 H50 0.9300 . ? C51 C52 1.401(5) . ? C51 H51 0.9300 . ? C52 C53 1.372(5) . ? C52 H52 0.9300 . ? C53 C54 1.399(5) . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? O1S H1S1 0.8531 . ? O1S H2S1 0.8513 . ? O2S H1S2 0.8615 . ? O2S H2S2 0.8618 . ? O3S H1S3 0.8500 . ? O3S H2S3 0.8458 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O14 Tb1 O10 136.37(8) . . ? O14 Tb1 O4 89.74(8) . . ? O10 Tb1 O4 81.20(8) . . ? O14 Tb1 O1 126.44(8) . . ? O10 Tb1 O1 87.93(8) . . ? O4 Tb1 O1 65.14(8) . . ? O14 Tb1 O11 63.62(8) . . ? O10 Tb1 O11 93.19(8) . . ? O4 Tb1 O11 134.32(8) . . ? O1 Tb1 O11 160.45(8) . . ? O14 Tb1 O7 133.73(8) . . ? O10 Tb1 O7 70.94(8) . . ? O4 Tb1 O7 136.03(8) . . ? O1 Tb1 O7 80.19(8) . . ? O11 Tb1 O7 81.75(8) . . ? O14 Tb1 O8 89.70(8) . . ? O10 Tb1 O8 123.04(9) . . ? O4 Tb1 O8 141.40(8) . . ? O1 Tb1 O8 84.66(8) . . ? O11 Tb1 O8 78.36(8) . . ? O7 Tb1 O8 52.13(8) . . ? O14 Tb1 O15 60.27(8) . . ? O10 Tb1 O15 151.15(9) . . ? O4 Tb1 O15 74.91(8) . . ? O1 Tb1 O15 67.54(8) . . ? O11 Tb1 O15 115.05(8) . . ? O7 Tb1 O15 116.83(8) . . ? O8 Tb1 O15 71.45(8) . . ? O14 Tb1 O6 72.70(7) . . ? O10 Tb1 O6 65.62(8) . . ? O4 Tb1 O6 60.77(7) . . ? O1 Tb1 O6 122.17(8) . . ? O11 Tb1 O6 75.56(7) . . ? O7 Tb1 O6 129.07(7) . . ? O8 Tb1 O6 153.04(8) . . ? O15 Tb1 O6 114.06(7) . . ? O14 Tb1 N5 111.94(9) . . ? O10 Tb1 N5 97.15(9) . . ? O4 Tb1 N5 147.38(8) . . ? O1 Tb1 N5 82.26(9) . . ? O11 Tb1 N5 78.23(8) . . ? O7 Tb1 N5 26.26(8) . . ? O8 Tb1 N5 25.89(8) . . ? O15 Tb1 N5 94.42(8) . . ? O6 Tb1 N5 147.41(8) . . ? O2 Fe1 O3 100.55(12) . . ? O2 Fe1 O4 102.42(10) . . ? O3 Fe1 O4 146.97(11) . . ? O2 Fe1 O1 156.21(10) . . ? O3 Fe1 O1 91.97(11) . . ? O4 Fe1 O1 75.94(9) . . ? O2 Fe1 N1 83.70(11) . . ? O3 Fe1 N1 94.82(12) . . ? O4 Fe1 N1 110.97(10) . . ? O1 Fe1 N1 75.10(11) . . ? O2 Fe1 N2 83.04(11) . . ? O3 Fe1 N2 77.88(11) . . ? O4 Fe1 N2 81.69(10) . . ? O1 Fe1 N2 119.60(10) . . ? N1 Fe1 N2 163.40(12) . . ? O12 Fe2 O13 108.99(11) . . ? O12 Fe2 O14 92.00(10) . . ? O13 Fe2 O14 145.74(10) . . ? O12 Fe2 O11 148.40(10) . . ? O13 Fe2 O11 96.91(10) . . ? O14 Fe2 O11 75.08(9) . . ? O12 Fe2 N3 84.58(10) . . ? O13 Fe2 N3 90.94(10) . . ? O14 Fe2 N3 118.48(10) . . ? O11 Fe2 N3 77.02(10) . . ? O12 Fe2 N4 81.50(10) . . ? O13 Fe2 N4 77.69(10) . . ? O14 Fe2 N4 79.11(10) . . ? O11 Fe2 N4 122.63(9) . . ? N3 Fe2 N4 157.99(11) . . ? C1 O1 Fe1 111.9(2) . . ? C1 O1 Tb1 125.2(2) . . ? Fe1 O1 Tb1 107.51(10) . . ? C13 O2 Fe1 135.2(3) . . ? C15 O3 Fe1 116.8(2) . . ? C27 O4 Fe1 130.7(2) . . ? C27 O4 Tb1 116.20(19) . . ? Fe1 O4 Tb1 110.90(10) . . ? C12 O5 C14 111.3(3) . . ? C26 O6 C28 117.1(3) . . ? C26 O6 Tb1 108.02(18) . . ? C28 O6 Tb1 125.9(2) . . ? N5 O7 Tb1 96.23(19) . . ? N5 O8 Tb1 95.6(2) . . ? Tb1 O10 H10A 137.5 . . ? Tb1 O10 H10B 115.4 . . ? H10A O10 H10B 107.0 . . ? C29 O11 Fe2 112.7(2) . . ? C29 O11 Tb1 123.5(2) . . ? Fe2 O11 Tb1 107.58(9) . . ? C41 O12 Fe2 135.2(2) . . ? C42 O13 Fe2 119.2(2) . . ? C54 O14 Fe2 123.7(2) . . ? C54 O14 Tb1 123.2(2) . . ? Fe2 O14 Tb1 112.42(10) . . ? C53 O15 C55 117.0(3) . . ? C53 O15 Tb1 112.86(18) . . ? C55 O15 Tb1 128.6(2) . . ? C40 O16 C56 113.2(3) . . ? C7 N1 C6 121.2(3) . . ? C7 N1 Fe1 128.0(3) . . ? C6 N1 Fe1 110.8(2) . . ? C21 N2 C20 121.5(3) . . ? C21 N2 Fe1 127.9(2) . . ? C20 N2 Fe1 109.6(2) . . ? O9 N5 O8 122.9(3) . . ? O9 N5 O7 121.1(3) . . ? O8 N5 O7 116.0(3) . . ? O9 N5 Tb1 177.6(3) . . ? O8 N5 Tb1 58.51(17) . . ? O7 N5 Tb1 57.51(16) . . ? C48 N4 C47 122.7(3) . . ? C48 N4 Fe2 124.3(2) . . ? C47 N4 Fe2 110.2(2) . . ? C35 N3 C34 120.8(3) . . ? C35 N3 Fe2 128.1(2) . . ? C34 N3 Fe2 111.0(2) . . ? O1 C1 C2 124.0(4) . . ? O1 C1 C6 116.5(3) . . ? C2 C1 C6 119.6(4) . . ? C3 C2 C1 119.9(4) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C4 C3 C2 120.7(4) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C3 C4 C5 119.8(4) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C6 C5 C4 119.5(4) . . ? C6 C5 H5 120.3 . . ? C4 C5 H5 120.3 . . ? C5 C6 C1 120.5(4) . . ? C5 C6 N1 125.1(4) . . ? C1 C6 N1 114.2(3) . . ? N1 C7 C8 124.8(4) . . ? N1 C7 H7 117.6 . . ? C8 C7 H7 117.6 . . ? C9 C8 C13 120.0(4) . . ? C9 C8 C7 118.2(4) . . ? C13 C8 C7 120.8(4) . . ? C10 C9 C8 121.2(4) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C9 C10 C11 119.4(4) . . ? C9 C10 H10 120.3 . . ? C11 C10 H10 120.3 . . ? C12 C11 C10 121.4(4) . . ? C12 C11 H11 119.3 . . ? C10 C11 H11 119.3 . . ? C11 C12 O5 120.0(4) . . ? C11 C12 C13 120.1(4) . . ? O5 C12 C13 119.8(4) . . ? O2 C13 C8 123.5(4) . . ? O2 C13 C12 119.3(4) . . ? C8 C13 C12 117.1(4) . . ? O5 C14 H14A 109.5 . . ? O5 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O5 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O3 C15 C16 122.6(4) . . ? O3 C15 C20 118.8(3) . . ? C16 C15 C20 118.6(4) . . ? C17 C16 C15 119.7(5) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C18 C17 C16 121.6(4) . . ? C18 C17 H17 119.2 . . ? C16 C17 H17 119.2 . . ? C19 C18 C17 119.5(4) . . ? C19 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? C18 C19 C20 120.3(4) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? C19 C20 C15 120.2(4) . . ? C19 C20 N2 126.7(4) . . ? C15 C20 N2 113.0(3) . . ? N2 C21 C22 125.3(3) . . ? N2 C21 H21 117.3 . . ? C22 C21 H21 117.3 . . ? C23 C22 C27 118.6(3) . . ? C23 C22 C21 119.4(3) . . ? C27 C22 C21 122.0(3) . . ? C24 C23 C22 122.1(3) . . ? C24 C23 H23 118.9 . . ? C22 C23 H23 118.9 . . ? C23 C24 C25 119.5(3) . . ? C23 C24 H24 120.2 . . ? C25 C24 H24 120.2 . . ? C26 C25 C24 119.2(3) . . ? C26 C25 H25 120.4 . . ? C24 C25 H25 120.4 . . ? C25 C26 O6 125.7(3) . . ? C25 C26 C27 121.3(3) . . ? O6 C26 C27 112.9(3) . . ? O4 C27 C22 123.5(3) . . ? O4 C27 C26 117.3(3) . . ? C22 C27 C26 119.0(3) . . ? O6 C28 H28A 109.5 . . ? O6 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? O6 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O11 C29 C30 122.2(3) . . ? O11 C29 C34 118.2(3) . . ? C30 C29 C34 119.5(3) . . ? C31 C30 C29 119.8(3) . . ? C31 C30 H30 120.1 . . ? C29 C30 H30 120.1 . . ? C32 C31 C30 120.6(3) . . ? C32 C31 H31 119.7 . . ? C30 C31 H31 119.7 . . ? C31 C32 C33 120.5(4) . . ? C31 C32 H32 119.8 . . ? C33 C32 H32 119.8 . . ? C32 C33 C34 119.7(3) . . ? C32 C33 H33 120.1 . . ? C34 C33 H33 120.1 . . ? C33 C34 C29 120.0(3) . . ? C33 C34 N3 126.3(3) . . ? C29 C34 N3 113.7(3) . . ? N3 C35 C36 125.3(3) . . ? N3 C35 H35 117.4 . . ? C36 C35 H35 117.4 . . ? C41 C36 C37 119.7(3) . . ? C41 C36 C35 122.3(3) . . ? C37 C36 C35 118.0(3) . . ? C38 C37 C36 121.2(4) . . ? C38 C37 H37 119.4 . . ? C36 C37 H37 119.4 . . ? C37 C38 C39 119.6(3) . . ? C37 C38 H38 120.2 . . ? C39 C38 H38 120.2 . . ? C40 C39 C38 120.6(3) . . ? C40 C39 H39 119.7 . . ? C38 C39 H39 119.7 . . ? C39 C40 O16 119.4(3) . . ? C39 C40 C41 121.3(3) . . ? O16 C40 C41 119.3(3) . . ? O12 C41 C36 123.3(3) . . ? O12 C41 C40 119.0(3) . . ? C36 C41 C40 117.7(3) . . ? O13 C42 C43 122.2(3) . . ? O13 C42 C47 119.5(3) . . ? C43 C42 C47 118.2(4) . . ? C44 C43 C42 120.2(4) . . ? C44 C43 H43 119.9 . . ? C42 C43 H43 119.9 . . ? C43 C44 C45 121.3(4) . . ? C43 C44 H44 119.4 . . ? C45 C44 H44 119.4 . . ? C46 C45 C44 119.5(4) . . ? C46 C45 H45 120.2 . . ? C44 C45 H45 120.2 . . ? C45 C46 C47 120.0(4) . . ? C45 C46 H46 120.0 . . ? C47 C46 H46 120.0 . . ? C46 C47 C42 120.7(4) . . ? C46 C47 N4 126.5(3) . . ? C42 C47 N4 112.9(3) . . ? N4 C48 C49 123.9(3) . . ? N4 C48 H48 118.1 . . ? C49 C48 H48 118.1 . . ? C54 C49 C50 118.6(3) . . ? C54 C49 C48 121.4(3) . . ? C50 C49 C48 120.0(3) . . ? C51 C50 C49 120.7(4) . . ? C51 C50 H50 119.7 . . ? C49 C50 H50 119.7 . . ? C50 C51 C52 120.8(3) . . ? C50 C51 H51 119.6 . . ? C52 C51 H51 119.6 . . ? C53 C52 C51 118.8(3) . . ? C53 C52 H52 120.6 . . ? C51 C52 H52 120.6 . . ? C52 C53 O15 126.7(3) . . ? C52 C53 C54 121.2(3) . . ? O15 C53 C54 112.1(3) . . ? O14 C54 C49 123.5(3) . . ? O14 C54 C53 116.6(3) . . ? C49 C54 C53 120.0(3) . . ? O15 C55 H55A 109.5 . . ? O15 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? O15 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? O16 C56 H56A 109.5 . . ? O16 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? O16 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? H1S1 O1S H2S1 105.7 . . ? H1S2 O2S H2S2 104.6 . . ? H1S3 O3S H2S3 106.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Fe1 O1 C1 -57.8(4) . . . . ? O3 Fe1 O1 C1 64.4(2) . . . . ? O4 Fe1 O1 C1 -146.7(2) . . . . ? N1 Fe1 O1 C1 -30.1(2) . . . . ? N2 Fe1 O1 C1 141.6(2) . . . . ? O2 Fe1 O1 Tb1 83.3(3) . . . . ? O3 Fe1 O1 Tb1 -154.55(11) . . . . ? O4 Fe1 O1 Tb1 -5.66(9) . . . . ? N1 Fe1 O1 Tb1 110.98(12) . . . . ? N2 Fe1 O1 Tb1 -77.38(13) . . . . ? O14 Tb1 O1 C1 -150.7(2) . . . . ? O10 Tb1 O1 C1 58.4(3) . . . . ? O4 Tb1 O1 C1 139.7(3) . . . . ? O11 Tb1 O1 C1 -35.3(4) . . . . ? O7 Tb1 O1 C1 -12.6(3) . . . . ? O8 Tb1 O1 C1 -65.0(3) . . . . ? O15 Tb1 O1 C1 -137.1(3) . . . . ? O6 Tb1 O1 C1 117.7(3) . . . . ? N5 Tb1 O1 C1 -39.1(3) . . . . ? O14 Tb1 O1 Fe1 74.80(12) . . . . ? O10 Tb1 O1 Fe1 -76.08(10) . . . . ? O4 Tb1 O1 Fe1 5.18(8) . . . . ? O11 Tb1 O1 Fe1 -169.81(17) . . . . ? O7 Tb1 O1 Fe1 -147.10(11) . . . . ? O8 Tb1 O1 Fe1 160.46(11) . . . . ? O15 Tb1 O1 Fe1 88.35(11) . . . . ? O6 Tb1 O1 Fe1 -16.79(13) . . . . ? N5 Tb1 O1 Fe1 -173.59(11) . . . . ? O3 Fe1 O2 C13 -91.6(4) . . . . ? O4 Fe1 O2 C13 112.3(3) . . . . ? O1 Fe1 O2 C13 29.0(5) . . . . ? N1 Fe1 O2 C13 2.1(3) . . . . ? N2 Fe1 O2 C13 -167.9(4) . . . . ? O2 Fe1 O3 C15 -62.4(3) . . . . ? O4 Fe1 O3 C15 71.1(3) . . . . ? O1 Fe1 O3 C15 137.9(3) . . . . ? N1 Fe1 O3 C15 -146.9(3) . . . . ? N2 Fe1 O3 C15 18.1(3) . . . . ? O2 Fe1 O4 C27 47.8(3) . . . . ? O3 Fe1 O4 C27 -85.2(3) . . . . ? O1 Fe1 O4 C27 -156.6(3) . . . . ? N1 Fe1 O4 C27 135.8(2) . . . . ? N2 Fe1 O4 C27 -33.1(2) . . . . ? O2 Fe1 O4 Tb1 -149.82(11) . . . . ? O3 Fe1 O4 Tb1 77.1(2) . . . . ? O1 Fe1 O4 Tb1 5.79(9) . . . . ? N1 Fe1 O4 Tb1 -61.88(13) . . . . ? N2 Fe1 O4 Tb1 129.24(11) . . . . ? O14 Tb1 O4 C27 28.6(2) . . . . ? O10 Tb1 O4 C27 -108.5(2) . . . . ? O1 Tb1 O4 C27 159.7(2) . . . . ? O11 Tb1 O4 C27 -22.7(2) . . . . ? O7 Tb1 O4 C27 -159.03(18) . . . . ? O8 Tb1 O4 C27 117.8(2) . . . . ? O15 Tb1 O4 C27 87.8(2) . . . . ? O6 Tb1 O4 C27 -41.63(19) . . . . ? N5 Tb1 O4 C27 161.9(2) . . . . ? O14 Tb1 O4 Fe1 -136.58(10) . . . . ? O10 Tb1 O4 Fe1 86.28(11) . . . . ? O1 Tb1 O4 Fe1 -5.53(9) . . . . ? O11 Tb1 O4 Fe1 172.13(8) . . . . ? O7 Tb1 O4 Fe1 35.79(16) . . . . ? O8 Tb1 O4 Fe1 -47.39(17) . . . . ? O15 Tb1 O4 Fe1 -77.40(10) . . . . ? O6 Tb1 O4 Fe1 153.19(13) . . . . ? N5 Tb1 O4 Fe1 -3.3(2) . . . . ? O14 Tb1 O6 C26 -61.8(2) . . . . ? O10 Tb1 O6 C26 131.4(2) . . . . ? O4 Tb1 O6 C26 37.90(19) . . . . ? O1 Tb1 O6 C26 60.8(2) . . . . ? O11 Tb1 O6 C26 -128.2(2) . . . . ? O7 Tb1 O6 C26 165.35(19) . . . . ? O8 Tb1 O6 C26 -113.2(2) . . . . ? O15 Tb1 O6 C26 -16.9(2) . . . . ? N5 Tb1 O6 C26 -165.7(2) . . . . ? O14 Tb1 O6 C28 84.1(2) . . . . ? O10 Tb1 O6 C28 -82.7(2) . . . . ? O4 Tb1 O6 C28 -176.2(3) . . . . ? O1 Tb1 O6 C28 -153.3(2) . . . . ? O11 Tb1 O6 C28 17.7(2) . . . . ? O7 Tb1 O6 C28 -48.8(3) . . . . ? O8 Tb1 O6 C28 32.7(3) . . . . ? O15 Tb1 O6 C28 129.0(2) . . . . ? N5 Tb1 O6 C28 -19.8(3) . . . . ? O14 Tb1 O7 N5 39.6(2) . . . . ? O10 Tb1 O7 N5 176.4(2) . . . . ? O4 Tb1 O7 N5 -129.84(18) . . . . ? O1 Tb1 O7 N5 -92.40(19) . . . . ? O11 Tb1 O7 N5 80.10(19) . . . . ? O8 Tb1 O7 N5 -1.54(18) . . . . ? O15 Tb1 O7 N5 -33.9(2) . . . . ? O6 Tb1 O7 N5 143.85(17) . . . . ? O14 Tb1 O8 N5 -150.1(2) . . . . ? O10 Tb1 O8 N5 -0.8(2) . . . . ? O4 Tb1 O8 N5 120.7(2) . . . . ? O1 Tb1 O8 N5 83.3(2) . . . . ? O11 Tb1 O8 N5 -87.0(2) . . . . ? O7 Tb1 O8 N5 1.56(18) . . . . ? O15 Tb1 O8 N5 151.3(2) . . . . ? O6 Tb1 O8 N5 -101.9(2) . . . . ? O12 Fe2 O11 C29 -79.8(3) . . . . ? O13 Fe2 O11 C29 65.6(2) . . . . ? O14 Fe2 O11 C29 -148.4(2) . . . . ? N3 Fe2 O11 C29 -23.8(2) . . . . ? N4 Fe2 O11 C29 145.3(2) . . . . ? O12 Fe2 O11 Tb1 59.7(2) . . . . ? O13 Fe2 O11 Tb1 -154.95(10) . . . . ? O14 Fe2 O11 Tb1 -8.93(9) . . . . ? N3 Fe2 O11 Tb1 115.68(11) . . . . ? N4 Fe2 O11 Tb1 -75.17(13) . . . . ? O14 Tb1 O11 C29 142.3(2) . . . . ? O10 Tb1 O11 C29 -76.3(2) . . . . ? O4 Tb1 O11 C29 -157.1(2) . . . . ? O1 Tb1 O11 C29 16.6(4) . . . . ? O7 Tb1 O11 C29 -6.0(2) . . . . ? O8 Tb1 O11 C29 46.8(2) . . . . ? O15 Tb1 O11 C29 109.8(2) . . . . ? O6 Tb1 O11 C29 -140.1(2) . . . . ? N5 Tb1 O11 C29 20.4(2) . . . . ? O14 Tb1 O11 Fe2 8.28(8) . . . . ? O10 Tb1 O11 Fe2 149.68(10) . . . . ? O4 Tb1 O11 Fe2 68.86(13) . . . . ? O1 Tb1 O11 Fe2 -117.5(2) . . . . ? O7 Tb1 O11 Fe2 -140.11(11) . . . . ? O8 Tb1 O11 Fe2 -87.23(10) . . . . ? O15 Tb1 O11 Fe2 -24.28(12) . . . . ? O6 Tb1 O11 Fe2 85.86(10) . . . . ? N5 Tb1 O11 Fe2 -113.67(11) . . . . ? O13 Fe2 O12 C41 -75.2(3) . . . . ? O14 Fe2 O12 C41 132.3(3) . . . . ? O11 Fe2 O12 C41 68.1(4) . . . . ? N3 Fe2 O12 C41 13.9(3) . . . . ? N4 Fe2 O12 C41 -149.0(3) . . . . ? O12 Fe2 O13 C42 -69.7(3) . . . . ? O14 Fe2 O13 C42 55.1(3) . . . . ? O11 Fe2 O13 C42 128.7(2) . . . . ? N3 Fe2 O13 C42 -154.3(2) . . . . ? N4 Fe2 O13 C42 6.7(2) . . . . ? O12 Fe2 O14 C54 29.3(2) . . . . ? O13 Fe2 O14 C54 -99.7(3) . . . . ? O11 Fe2 O14 C54 -179.9(3) . . . . ? N3 Fe2 O14 C54 114.2(2) . . . . ? N4 Fe2 O14 C54 -51.7(2) . . . . ? O12 Fe2 O14 Tb1 -141.33(11) . . . . ? O13 Fe2 O14 Tb1 89.65(19) . . . . ? O11 Fe2 O14 Tb1 9.44(9) . . . . ? N3 Fe2 O14 Tb1 -56.41(14) . . . . ? N4 Fe2 O14 Tb1 137.72(12) . . . . ? O10 Tb1 O14 C54 115.9(2) . . . . ? O4 Tb1 O14 C54 39.0(2) . . . . ? O1 Tb1 O14 C54 -19.2(3) . . . . ? O11 Tb1 O14 C54 -179.5(3) . . . . ? O7 Tb1 O14 C54 -133.6(2) . . . . ? O8 Tb1 O14 C54 -102.4(2) . . . . ? O15 Tb1 O14 C54 -33.7(2) . . . . ? O6 Tb1 O14 C54 98.4(2) . . . . ? N5 Tb1 O14 C54 -116.0(2) . . . . ? O10 Tb1 O14 Fe2 -73.38(15) . . . . ? O4 Tb1 O14 Fe2 -150.30(11) . . . . ? O1 Tb1 O14 Fe2 151.43(9) . . . . ? O11 Tb1 O14 Fe2 -8.85(9) . . . . ? O7 Tb1 O14 Fe2 37.03(16) . . . . ? O8 Tb1 O14 Fe2 68.30(11) . . . . ? O15 Tb1 O14 Fe2 136.99(13) . . . . ? O6 Tb1 O14 Fe2 -90.97(11) . . . . ? N5 Tb1 O14 Fe2 54.72(12) . . . . ? O14 Tb1 O15 C53 30.4(2) . . . . ? O10 Tb1 O15 C53 -103.3(3) . . . . ? O4 Tb1 O15 C53 -68.1(2) . . . . ? O1 Tb1 O15 C53 -137.0(2) . . . . ? O11 Tb1 O15 C53 64.2(2) . . . . ? O7 Tb1 O15 C53 157.5(2) . . . . ? O8 Tb1 O15 C53 131.1(2) . . . . ? O6 Tb1 O15 C53 -20.5(2) . . . . ? N5 Tb1 O15 C53 143.2(2) . . . . ? O14 Tb1 O15 C55 -164.4(3) . . . . ? O10 Tb1 O15 C55 61.9(4) . . . . ? O4 Tb1 O15 C55 97.0(3) . . . . ? O1 Tb1 O15 C55 28.1(3) . . . . ? O11 Tb1 O15 C55 -130.7(3) . . . . ? O7 Tb1 O15 C55 -37.3(3) . . . . ? O8 Tb1 O15 C55 -63.7(3) . . . . ? O6 Tb1 O15 C55 144.6(3) . . . . ? N5 Tb1 O15 C55 -51.6(3) . . . . ? O2 Fe1 N1 C7 14.9(3) . . . . ? O3 Fe1 N1 C7 115.0(3) . . . . ? O4 Fe1 N1 C7 -86.0(3) . . . . ? O1 Fe1 N1 C7 -154.2(4) . . . . ? N2 Fe1 N1 C7 52.1(6) . . . . ? O2 Fe1 N1 C6 -165.3(3) . . . . ? O3 Fe1 N1 C6 -65.2(3) . . . . ? O4 Fe1 N1 C6 93.8(2) . . . . ? O1 Fe1 N1 C6 25.6(2) . . . . ? N2 Fe1 N1 C6 -128.1(4) . . . . ? O2 Fe1 N2 C21 -81.2(3) . . . . ? O3 Fe1 N2 C21 176.4(3) . . . . ? O4 Fe1 N2 C21 22.5(3) . . . . ? O1 Fe1 N2 C21 91.1(3) . . . . ? N1 Fe1 N2 C21 -118.4(4) . . . . ? O2 Fe1 N2 C20 87.3(2) . . . . ? O3 Fe1 N2 C20 -15.1(2) . . . . ? O4 Fe1 N2 C20 -169.0(2) . . . . ? O1 Fe1 N2 C20 -100.4(2) . . . . ? N1 Fe1 N2 C20 50.1(5) . . . . ? Tb1 O8 N5 O9 177.7(3) . . . . ? Tb1 O8 N5 O7 -2.6(3) . . . . ? Tb1 O7 N5 O9 -177.7(3) . . . . ? Tb1 O7 N5 O8 2.6(3) . . . . ? O14 Tb1 N5 O9 -95(7) . . . . ? O10 Tb1 N5 O9 52(7) . . . . ? O4 Tb1 N5 O9 137(7) . . . . ? O1 Tb1 N5 O9 139(7) . . . . ? O11 Tb1 N5 O9 -40(7) . . . . ? O7 Tb1 N5 O9 55(7) . . . . ? O8 Tb1 N5 O9 -128(7) . . . . ? O15 Tb1 N5 O9 -155(7) . . . . ? O6 Tb1 N5 O9 -3(7) . . . . ? O14 Tb1 N5 O8 32.5(2) . . . . ? O10 Tb1 N5 O8 179.4(2) . . . . ? O4 Tb1 N5 O8 -95.8(2) . . . . ? O1 Tb1 N5 O8 -93.7(2) . . . . ? O11 Tb1 N5 O8 87.6(2) . . . . ? O7 Tb1 N5 O8 -177.2(3) . . . . ? O15 Tb1 N5 O8 -27.1(2) . . . . ? O6 Tb1 N5 O8 124.5(2) . . . . ? O14 Tb1 N5 O7 -150.25(18) . . . . ? O10 Tb1 N5 O7 -3.4(2) . . . . ? O4 Tb1 N5 O7 81.4(2) . . . . ? O1 Tb1 N5 O7 83.49(19) . . . . ? O11 Tb1 N5 O7 -95.22(19) . . . . ? O8 Tb1 N5 O7 177.2(3) . . . . ? O15 Tb1 N5 O7 150.09(19) . . . . ? O6 Tb1 N5 O7 -58.3(3) . . . . ? O12 Fe2 N4 C48 -54.5(3) . . . . ? O13 Fe2 N4 C48 -166.2(3) . . . . ? O14 Fe2 N4 C48 39.2(3) . . . . ? O11 Fe2 N4 C48 103.4(3) . . . . ? N3 Fe2 N4 C48 -105.9(4) . . . . ? O12 Fe2 N4 C47 107.0(2) . . . . ? O13 Fe2 N4 C47 -4.7(2) . . . . ? O14 Fe2 N4 C47 -159.3(2) . . . . ? O11 Fe2 N4 C47 -95.0(2) . . . . ? N3 Fe2 N4 C47 55.7(4) . . . . ? O12 Fe2 N3 C35 -7.1(3) . . . . ? O13 Fe2 N3 C35 101.9(3) . . . . ? O14 Fe2 N3 C35 -96.4(3) . . . . ? O11 Fe2 N3 C35 -161.2(3) . . . . ? N4 Fe2 N3 C35 43.8(5) . . . . ? O12 Fe2 N3 C34 175.6(2) . . . . ? O13 Fe2 N3 C34 -75.4(2) . . . . ? O14 Fe2 N3 C34 86.3(2) . . . . ? O11 Fe2 N3 C34 21.5(2) . . . . ? N4 Fe2 N3 C34 -133.5(3) . . . . ? Fe1 O1 C1 C2 -149.5(3) . . . . ? Tb1 O1 C1 C2 77.6(4) . . . . ? Fe1 O1 C1 C6 30.3(4) . . . . ? Tb1 O1 C1 C6 -102.6(3) . . . . ? O1 C1 C2 C3 -177.0(4) . . . . ? C6 C1 C2 C3 3.3(6) . . . . ? C1 C2 C3 C4 -1.7(7) . . . . ? C2 C3 C4 C5 -0.8(7) . . . . ? C3 C4 C5 C6 1.7(7) . . . . ? C4 C5 C6 C1 -0.2(7) . . . . ? C4 C5 C6 N1 -174.2(4) . . . . ? O1 C1 C6 C5 177.9(4) . . . . ? C2 C1 C6 C5 -2.3(6) . . . . ? O1 C1 C6 N1 -7.4(5) . . . . ? C2 C1 C6 N1 172.3(3) . . . . ? C7 N1 C6 C5 -24.2(6) . . . . ? Fe1 N1 C6 C5 156.0(4) . . . . ? C7 N1 C6 C1 161.4(4) . . . . ? Fe1 N1 C6 C1 -18.4(4) . . . . ? C6 N1 C7 C8 162.9(4) . . . . ? Fe1 N1 C7 C8 -17.4(6) . . . . ? N1 C7 C8 C9 -169.2(4) . . . . ? N1 C7 C8 C13 -0.4(6) . . . . ? C13 C8 C9 C10 -3.1(6) . . . . ? C7 C8 C9 C10 165.8(4) . . . . ? C8 C9 C10 C11 -3.6(7) . . . . ? C9 C10 C11 C12 4.0(7) . . . . ? C10 C11 C12 O5 -177.5(4) . . . . ? C10 C11 C12 C13 2.3(7) . . . . ? C14 O5 C12 C11 106.3(5) . . . . ? C14 O5 C12 C13 -73.4(5) . . . . ? Fe1 O2 C13 C8 -17.5(6) . . . . ? Fe1 O2 C13 C12 160.1(3) . . . . ? C9 C8 C13 O2 -173.4(4) . . . . ? C7 C8 C13 O2 18.0(6) . . . . ? C9 C8 C13 C12 9.0(6) . . . . ? C7 C8 C13 C12 -159.6(4) . . . . ? C11 C12 C13 O2 173.6(4) . . . . ? O5 C12 C13 O2 -6.6(6) . . . . ? C11 C12 C13 C8 -8.6(6) . . . . ? O5 C12 C13 C8 171.1(4) . . . . ? Fe1 O3 C15 C16 161.0(3) . . . . ? Fe1 O3 C15 C20 -18.6(5) . . . . ? O3 C15 C16 C17 178.7(4) . . . . ? C20 C15 C16 C17 -1.8(7) . . . . ? C15 C16 C17 C18 1.3(8) . . . . ? C16 C17 C18 C19 0.1(8) . . . . ? C17 C18 C19 C20 -1.0(7) . . . . ? C18 C19 C20 C15 0.5(6) . . . . ? C18 C19 C20 N2 176.6(4) . . . . ? O3 C15 C20 C19 -179.5(4) . . . . ? C16 C15 C20 C19 0.9(6) . . . . ? O3 C15 C20 N2 3.9(5) . . . . ? C16 C15 C20 N2 -175.7(4) . . . . ? C21 N2 C20 C19 3.3(6) . . . . ? Fe1 N2 C20 C19 -166.0(3) . . . . ? C21 N2 C20 C15 179.6(3) . . . . ? Fe1 N2 C20 C15 10.3(4) . . . . ? C20 N2 C21 C22 -175.9(3) . . . . ? Fe1 N2 C21 C22 -8.7(5) . . . . ? N2 C21 C22 C23 173.7(3) . . . . ? N2 C21 C22 C27 -7.9(5) . . . . ? C27 C22 C23 C24 2.1(5) . . . . ? C21 C22 C23 C24 -179.5(3) . . . . ? C22 C23 C24 C25 -2.9(5) . . . . ? C23 C24 C25 C26 0.0(5) . . . . ? C24 C25 C26 O6 -173.6(3) . . . . ? C24 C25 C26 C27 3.8(5) . . . . ? C28 O6 C26 C25 -3.1(5) . . . . ? Tb1 O6 C26 C25 146.2(3) . . . . ? C28 O6 C26 C27 179.2(3) . . . . ? Tb1 O6 C26 C27 -31.4(3) . . . . ? Fe1 O4 C27 C22 29.8(4) . . . . ? Tb1 O4 C27 C22 -131.8(3) . . . . ? Fe1 O4 C27 C26 -154.7(2) . . . . ? Tb1 O4 C27 C26 43.7(3) . . . . ? C23 C22 C27 O4 177.1(3) . . . . ? C21 C22 C27 O4 -1.3(5) . . . . ? C23 C22 C27 C26 1.6(5) . . . . ? C21 C22 C27 C26 -176.8(3) . . . . ? C25 C26 C27 O4 179.7(3) . . . . ? O6 C26 C27 O4 -2.6(4) . . . . ? C25 C26 C27 C22 -4.6(5) . . . . ? O6 C26 C27 C22 173.2(3) . . . . ? Fe2 O11 C29 C30 -160.3(3) . . . . ? Tb1 O11 C29 C30 67.6(4) . . . . ? Fe2 O11 C29 C34 23.0(4) . . . . ? Tb1 O11 C29 C34 -109.1(3) . . . . ? O11 C29 C30 C31 -176.5(3) . . . . ? C34 C29 C30 C31 0.2(5) . . . . ? C29 C30 C31 C32 -0.4(6) . . . . ? C30 C31 C32 C33 0.0(6) . . . . ? C31 C32 C33 C34 0.6(6) . . . . ? C32 C33 C34 C29 -0.7(5) . . . . ? C32 C33 C34 N3 -179.6(3) . . . . ? O11 C29 C34 C33 177.2(3) . . . . ? C30 C29 C34 C33 0.4(5) . . . . ? O11 C29 C34 N3 -3.8(4) . . . . ? C30 C29 C34 N3 179.4(3) . . . . ? C35 N3 C34 C33 -15.0(5) . . . . ? Fe2 N3 C34 C33 162.6(3) . . . . ? C35 N3 C34 C29 166.1(3) . . . . ? Fe2 N3 C34 C29 -16.4(4) . . . . ? C34 N3 C35 C36 178.4(3) . . . . ? Fe2 N3 C35 C36 1.3(5) . . . . ? N3 C35 C36 C41 2.9(6) . . . . ? N3 C35 C36 C37 -174.2(3) . . . . ? C41 C36 C37 C38 -0.2(5) . . . . ? C35 C36 C37 C38 177.1(3) . . . . ? C36 C37 C38 C39 0.3(6) . . . . ? C37 C38 C39 C40 -0.5(6) . . . . ? C38 C39 C40 O16 179.5(3) . . . . ? C38 C39 C40 C41 0.4(6) . . . . ? C56 O16 C40 C39 107.4(4) . . . . ? C56 O16 C40 C41 -73.6(4) . . . . ? Fe2 O12 C41 C36 -14.2(5) . . . . ? Fe2 O12 C41 C40 165.4(2) . . . . ? C37 C36 C41 O12 179.7(3) . . . . ? C35 C36 C41 O12 2.6(5) . . . . ? C37 C36 C41 C40 0.1(5) . . . . ? C35 C36 C41 C40 -177.0(3) . . . . ? C39 C40 C41 O12 -179.9(3) . . . . ? O16 C40 C41 O12 1.0(5) . . . . ? C39 C40 C41 C36 -0.2(5) . . . . ? O16 C40 C41 C36 -179.3(3) . . . . ? Fe2 O13 C42 C43 171.4(3) . . . . ? Fe2 O13 C42 C47 -8.0(4) . . . . ? O13 C42 C43 C44 178.1(3) . . . . ? C47 C42 C43 C44 -2.5(5) . . . . ? C42 C43 C44 C45 -0.2(6) . . . . ? C43 C44 C45 C46 2.0(6) . . . . ? C44 C45 C46 C47 -1.0(6) . . . . ? C45 C46 C47 C42 -1.7(5) . . . . ? C45 C46 C47 N4 178.0(3) . . . . ? O13 C42 C47 C46 -177.2(3) . . . . ? C43 C42 C47 C46 3.5(5) . . . . ? O13 C42 C47 N4 3.1(4) . . . . ? C43 C42 C47 N4 -176.3(3) . . . . ? C48 N4 C47 C46 -15.6(5) . . . . ? Fe2 N4 C47 C46 -177.5(3) . . . . ? C48 N4 C47 C42 164.1(3) . . . . ? Fe2 N4 C47 C42 2.2(3) . . . . ? C47 N4 C48 C49 -177.0(3) . . . . ? Fe2 N4 C48 C49 -17.7(5) . . . . ? N4 C48 C49 C54 -10.0(5) . . . . ? N4 C48 C49 C50 170.0(3) . . . . ? C54 C49 C50 C51 1.6(5) . . . . ? C48 C49 C50 C51 -178.4(3) . . . . ? C49 C50 C51 C52 -0.8(5) . . . . ? C50 C51 C52 C53 -0.3(5) . . . . ? C51 C52 C53 O15 -177.9(3) . . . . ? C51 C52 C53 C54 0.7(5) . . . . ? C55 O15 C53 C52 -14.6(5) . . . . ? Tb1 O15 C53 C52 152.5(3) . . . . ? C55 O15 C53 C54 166.8(3) . . . . ? Tb1 O15 C53 C54 -26.2(3) . . . . ? Fe2 O14 C54 C49 45.6(4) . . . . ? Tb1 O14 C54 C49 -144.8(3) . . . . ? Fe2 O14 C54 C53 -135.4(3) . . . . ? Tb1 O14 C54 C53 34.2(4) . . . . ? C50 C49 C54 O14 177.7(3) . . . . ? C48 C49 C54 O14 -2.2(5) . . . . ? C50 C49 C54 C53 -1.2(5) . . . . ? C48 C49 C54 C53 178.8(3) . . . . ? C52 C53 C54 O14 -178.9(3) . . . . ? O15 C53 C54 O14 -0.2(4) . . . . ? C52 C53 C54 C49 0.1(5) . . . . ? O15 C53 C54 C49 178.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.843 _refine_diff_density_min -0.592 _refine_diff_density_rms 0.086