# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 182 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Calvo, Sergio' 'Ferreira, Kerry' 'McIntosh, Ruaraidh' 'Dalgarno, Scott' 'Brechin, Euan' _publ_contact_author_name 'Dr Scott Dalgarno' _publ_contact_author_email S.J.Dalgarno@hw.ac.uk _publ_section_title ; Calixarene-supported FeIII2LnIII2 clusters ; # Attachment '- 1.CIF' data_S56 _database_code_depnum_ccdc_archive 'CCDC 827077' #TrackingRef '- 1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common S56 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C110 H157 Cl Fe2 Gd2 N8 O18' _chemical_formula_weight 2341.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 19.5796(18) _cell_length_b 38.647(4) _cell_length_c 15.6623(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11852(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7950. _cell_measurement_theta_min 2.30. _cell_measurement_theta_max 22.73. _exptl_crystal_description Block _exptl_crystal_colour Brown _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.312 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4856 _exptl_absorpt_coefficient_mu 1.430 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5986 _exptl_absorpt_correction_T_max 0.7630 _exptl_absorpt_process_details Bruker-SADABS _exptl_special_details ; Data were corrected for decay and absorption using the program SADABS based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995). ; _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 'Bruker Apex II CCD Diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 83285 _diffrn_reflns_av_R_equivalents 0.0978 _diffrn_reflns_av_sigmaI/netI 0.1000 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -49 _diffrn_reflns_limit_k_max 48 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 27.25 _reflns_number_total 13340 _reflns_number_gt 8261 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex II' _computing_cell_refinement 'SAINT (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed (Barbour, 2001)' _computing_publication_material 'local program' _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. Crystals were weakly diffracting. The routine SQUEEZE was applied to the data in order to remove diffuse electron density. It was not possible to model the disorder associated with this density. Unit cell contents do not match reported formulae due to hydrogen atoms on water, methanol and OH ligands. ; _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^)+(0.0581P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13340 _refine_ls_number_parameters 672 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0980 _refine_ls_R_factor_gt 0.0507 _refine_ls_wR_factor_ref 0.1194 _refine_ls_wR_factor_gt 0.1060 _refine_ls_goodness_of_fit_ref 0.951 _refine_ls_restrained_S_all 0.951 _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 Gd1 Gd 0.208341(16) 0.2500 0.34312(2) 0.01888(9) Uani 1 2 d S . . Fe1 Fe 0.20119(3) 0.203900(16) 0.52884(4) 0.01930(16) Uani 1 1 d . . . Cl1 Cl 0.45424(9) 0.2500 0.24049(12) 0.0418(5) Uani 1 2 d S . . O1 O 0.20461(15) 0.19873(7) 0.6510(2) 0.0226(7) Uani 1 1 d . . . N1 N 0.5112(2) 0.17060(11) 0.4402(3) 0.0340(11) Uani 1 1 d . . . C1 C 0.1332(2) 0.15881(12) 0.7261(3) 0.0208(11) Uani 1 1 d . . . Gd2 Gd 0.349460(16) 0.2500 0.52041(2) 0.02151(10) Uani 1 2 d S . . O2 O 0.30235(14) 0.19279(8) 0.52974(19) 0.0190(7) Uani 1 1 d . . . N2 N 0.3050(2) 0.17661(11) 0.1471(3) 0.0385(11) Uani 1 1 d . . . C2 C 0.1276(2) 0.12890(12) 0.7752(3) 0.0244(11) Uani 1 1 d . . . H2 H 0.0835 0.1217 0.7930 0.029 Uiso 1 1 calc R . . O3 O 0.19891(14) 0.19349(7) 0.40222(19) 0.0191(7) Uani 1 1 d . . . N3 N 0.4393(2) 0.08696(13) 0.2387(3) 0.0398(12) Uani 1 1 d . . . C3 C 0.1834(2) 0.10920(12) 0.7993(3) 0.0229(11) Uani 1 1 d . . . O4 O 0.10305(15) 0.19948(8) 0.52629(19) 0.0229(7) Uani 1 1 d . . . N4 N 0.1664(3) 0.03048(14) 0.5925(4) 0.0638(16) Uani 1 1 d . . . C4 C 0.2476(2) 0.12093(12) 0.7743(3) 0.0237(11) Uani 1 1 d . . . H4 H 0.2869 0.1082 0.7909 0.028 Uiso 1 1 calc R . . O5 O 0.2948(2) 0.2500 0.6640(3) 0.0263(11) Uani 1 2 d S . . C5 C 0.2559(2) 0.15111(11) 0.7253(3) 0.0191(10) Uani 1 1 d . . . O6 O 0.4308(3) 0.2500 0.6399(3) 0.0476(15) Uani 1 2 d S . . C6 C 0.1981(2) 0.16999(11) 0.7003(3) 0.0211(10) Uani 1 1 d . . . O7 O 0.43920(17) 0.21218(8) 0.4831(2) 0.0343(9) Uani 1 1 d . . . C7 C 0.3264(2) 0.16097(12) 0.6948(3) 0.0214(10) Uani 1 1 d . . . H7A H 0.3605 0.1540 0.7383 0.026 Uiso 1 1 calc R . . H7B H 0.3290 0.1864 0.6880 0.026 Uiso 1 1 calc R . . O8 O 0.3226(2) 0.2500 0.3779(3) 0.0227(10) Uani 1 2 d S . . C8 C 0.3435(2) 0.14357(11) 0.6099(3) 0.0195(10) Uani 1 1 d . . . O9 O 0.24104(17) 0.21228(8) 0.2301(2) 0.0269(8) Uani 1 1 d . . . C9 C 0.3687(2) 0.11002(11) 0.6102(3) 0.0207(10) Uani 1 1 d . . . H9 H 0.3771 0.0991 0.6636 0.025 Uiso 1 1 calc R . . O10 O 0.1139(2) 0.2500 0.2433(3) 0.0386(13) Uani 1 2 d S . . C10 C 0.3822(2) 0.09160(11) 0.5357(3) 0.0197(10) Uani 1 1 d . . . O11 O 0.0952(2) 0.2500 0.4127(3) 0.0225(10) Uani 1 2 d S . . C11 C 0.3692(2) 0.10886(11) 0.4593(3) 0.0185(10) Uani 1 1 d . . . H11 H 0.3788 0.0973 0.4073 0.022 Uiso 1 1 calc R . . O12 O 0.2221(2) 0.2500 0.5038(3) 0.0230(11) Uani 1 2 d S . . C12 C 0.3427(2) 0.14249(11) 0.4555(3) 0.0192(10) Uani 1 1 d . . . C13 C 0.3290(2) 0.16005(11) 0.5325(3) 0.0195(10) Uani 1 1 d . . . C14 C 0.3231(2) 0.15748(11) 0.3705(3) 0.0189(10) Uani 1 1 d . . . H14A H 0.3579 0.1513 0.3272 0.023 Uiso 1 1 calc R . . H14B H 0.3209 0.1830 0.3745 0.023 Uiso 1 1 calc R . . C15 C 0.2543(2) 0.14330(11) 0.3441(3) 0.0182(10) Uani 1 1 d . . . C16 C 0.2498(2) 0.11107(11) 0.3055(3) 0.0194(10) Uani 1 1 d . . . H16 H 0.2907 0.0991 0.2915 0.023 Uiso 1 1 calc R . . C17 C 0.1872(2) 0.09555(11) 0.2867(3) 0.0191(10) Uani 1 1 d . . . C18 C 0.1289(2) 0.11408(11) 0.3081(3) 0.0180(10) Uani 1 1 d . . . H18 H 0.0856 0.1041 0.2960 0.022 Uiso 1 1 calc R . . C19 C 0.1312(2) 0.14677(11) 0.3467(3) 0.0183(10) Uani 1 1 d . . . C20 C 0.1951(2) 0.16144(11) 0.3654(3) 0.0182(10) Uani 1 1 d . . . C21 C 0.0640(2) 0.16377(11) 0.3728(3) 0.0202(10) Uani 1 1 d . . . H21A H 0.0694 0.1892 0.3715 0.024 Uiso 1 1 calc R . . H21B H 0.0280 0.1574 0.3311 0.024 Uiso 1 1 calc R . . C22 C 0.0419(2) 0.15270(11) 0.4611(3) 0.0180(10) Uani 1 1 d . . . C23 C 0.0035(2) 0.12273(11) 0.4709(3) 0.0201(10) Uani 1 1 d . . . H23 H -0.0104 0.1106 0.4211 0.024 Uiso 1 1 calc R . . C24 C -0.0155(2) 0.10962(12) 0.5502(3) 0.0203(10) Uani 1 1 d . . . C25 C 0.0043(2) 0.12878(12) 0.6203(3) 0.0243(11) Uani 1 1 d . . . H25 H -0.0093 0.1210 0.6753 0.029 Uiso 1 1 calc R . . C26 C 0.0433(2) 0.15883(12) 0.6150(3) 0.0224(11) Uani 1 1 d . . . C27 C 0.0634(2) 0.17085(11) 0.5337(3) 0.0196(10) Uani 1 1 d . . . C28 C 0.0690(2) 0.17675(12) 0.6947(3) 0.0230(11) Uani 1 1 d . . . H28A H 0.0334 0.1760 0.7396 0.028 Uiso 1 1 calc R . . H28B H 0.0791 0.2013 0.6819 0.028 Uiso 1 1 calc R . . C29 C 0.1756(2) 0.07541(13) 0.8511(3) 0.0287(12) Uani 1 1 d . . . C30 C 0.1819(3) 0.08359(15) 0.9453(3) 0.0430(15) Uani 1 1 d . . . H30A H 0.2261 0.0946 0.9563 0.064 Uiso 1 1 calc R . . H30B H 0.1786 0.0621 0.9784 0.064 Uiso 1 1 calc R . . H30C H 0.1450 0.0993 0.9622 0.064 Uiso 1 1 calc R . . C31 C 0.2294(3) 0.04843(13) 0.8264(3) 0.0364(13) Uani 1 1 d . . . H31A H 0.2749 0.0569 0.8422 0.055 Uiso 1 1 calc R . . H31B H 0.2277 0.0444 0.7647 0.055 Uiso 1 1 calc R . . H31C H 0.2201 0.0267 0.8566 0.055 Uiso 1 1 calc R . . C32 C 0.1054(3) 0.05915(14) 0.8347(4) 0.0441(15) Uani 1 1 d . . . H32A H 0.1029 0.0366 0.8632 0.066 Uiso 1 1 calc R . . H32B H 0.0988 0.0560 0.7731 0.066 Uiso 1 1 calc R . . H32C H 0.0697 0.0744 0.8572 0.066 Uiso 1 1 calc R . . C33 C 0.4077(2) 0.05415(11) 0.5333(3) 0.0224(11) Uani 1 1 d . . . C34 C 0.4744(2) 0.05236(13) 0.4815(3) 0.0321(12) Uani 1 1 d . . . H34A H 0.4657 0.0600 0.4229 0.048 Uiso 1 1 calc R . . H34B H 0.4912 0.0285 0.4808 0.048 Uiso 1 1 calc R . . H34C H 0.5087 0.0674 0.5078 0.048 Uiso 1 1 calc R . . C35 C 0.3548(3) 0.03115(12) 0.4892(3) 0.0347(13) Uani 1 1 d . . . H35A H 0.3117 0.0322 0.5207 0.052 Uiso 1 1 calc R . . H35B H 0.3714 0.0072 0.4880 0.052 Uiso 1 1 calc R . . H35C H 0.3476 0.0393 0.4307 0.052 Uiso 1 1 calc R . . C36 C 0.4200(2) 0.03980(12) 0.6225(3) 0.0276(12) Uani 1 1 d . . . H36A H 0.4529 0.0545 0.6526 0.041 Uiso 1 1 calc R . . H36B H 0.4383 0.0163 0.6182 0.041 Uiso 1 1 calc R . . H36C H 0.3769 0.0394 0.6541 0.041 Uiso 1 1 calc R . . C37 C 0.1810(2) 0.05951(12) 0.2453(3) 0.0234(11) Uani 1 1 d . . . C38 C 0.1330(3) 0.06130(13) 0.1685(3) 0.0337(13) Uani 1 1 d . . . H38A H 0.0873 0.0682 0.1876 0.051 Uiso 1 1 calc R . . H38B H 0.1305 0.0385 0.1411 0.051 Uiso 1 1 calc R . . H38C H 0.1503 0.0783 0.1275 0.051 Uiso 1 1 calc R . . C39 C 0.1507(3) 0.03413(12) 0.3115(3) 0.0341(13) Uani 1 1 d . . . H39A H 0.1819 0.0321 0.3602 0.051 Uiso 1 1 calc R . . H39B H 0.1446 0.0114 0.2851 0.051 Uiso 1 1 calc R . . H39C H 0.1064 0.0428 0.3313 0.051 Uiso 1 1 calc R . . C40 C 0.2502(3) 0.04545(12) 0.2156(4) 0.0369(13) Uani 1 1 d . . . H40A H 0.2699 0.0613 0.1733 0.055 Uiso 1 1 calc R . . H40B H 0.2438 0.0226 0.1897 0.055 Uiso 1 1 calc R . . H40C H 0.2810 0.0435 0.2646 0.055 Uiso 1 1 calc R . . C41 C -0.0565(2) 0.07571(12) 0.5551(3) 0.0266(11) Uani 1 1 d . . . C42 C -0.1251(2) 0.08057(13) 0.5099(3) 0.0354(13) Uani 1 1 d . . . H42A H -0.1512 0.0590 0.5128 0.053 Uiso 1 1 calc R . . H42B H -0.1171 0.0867 0.4500 0.053 Uiso 1 1 calc R . . H42C H -0.1508 0.0991 0.5379 0.053 Uiso 1 1 calc R . . C43 C -0.0691(3) 0.06465(13) 0.6467(3) 0.0339(13) Uani 1 1 d . . . H43A H -0.0252 0.0616 0.6759 0.051 Uiso 1 1 calc R . . H43B H -0.0943 0.0428 0.6473 0.051 Uiso 1 1 calc R . . H43C H -0.0958 0.0825 0.6762 0.051 Uiso 1 1 calc R . . C44 C -0.0168(3) 0.04668(12) 0.5112(3) 0.0342(13) Uani 1 1 d . . . H44A H 0.0263 0.0428 0.5415 0.051 Uiso 1 1 calc R . . H44B H -0.0073 0.0532 0.4519 0.051 Uiso 1 1 calc R . . H44C H -0.0440 0.0254 0.5121 0.051 Uiso 1 1 calc R . . C45 C 0.2480(3) 0.15703(16) 0.1157(4) 0.0532(17) Uani 1 1 d . . . H45A H 0.2062 0.1645 0.1449 0.080 Uiso 1 1 calc R . . H45B H 0.2556 0.1324 0.1267 0.080 Uiso 1 1 calc R . . H45C H 0.2431 0.1608 0.0541 0.080 Uiso 1 1 calc R . . C46 C 0.3724(3) 0.16661(19) 0.1212(4) 0.066(2) Uani 1 1 d . . . H46A H 0.4054 0.1837 0.1418 0.100 Uiso 1 1 calc R . . H46B H 0.3744 0.1654 0.0587 0.100 Uiso 1 1 calc R . . H46C H 0.3833 0.1439 0.1453 0.100 Uiso 1 1 calc R . . C47 C 0.2963(3) 0.20267(13) 0.2030(4) 0.0379(13) Uani 1 1 d . . . H47 H 0.3359 0.2144 0.2227 0.045 Uiso 1 1 calc R . . C48 C 0.5232(3) 0.15721(15) 0.5240(4) 0.0509(16) Uani 1 1 d . . . H48A H 0.4979 0.1710 0.5658 0.076 Uiso 1 1 calc R . . H48B H 0.5721 0.1583 0.5369 0.076 Uiso 1 1 calc R . . H48C H 0.5078 0.1331 0.5267 0.076 Uiso 1 1 calc R . . C49 C 0.5401(4) 0.1530(2) 0.3681(4) 0.077(2) Uani 1 1 d . . . H49A H 0.5188 0.1302 0.3621 0.115 Uiso 1 1 calc R . . H49B H 0.5894 0.1502 0.3766 0.115 Uiso 1 1 calc R . . H49C H 0.5319 0.1666 0.3163 0.115 Uiso 1 1 calc R . . C50 C 0.4688(3) 0.19698(15) 0.4288(4) 0.0410(14) Uani 1 1 d . . . H50 H 0.4614 0.2044 0.3717 0.049 Uiso 1 1 calc R . . C51 C 0.5056(6) 0.2500 0.6392(7) 0.091(4) Uani 1 2 d S . . H51A H 0.5223 0.2261 0.6362 0.136 Uiso 0.50 1 calc PR . . H51B H 0.5226 0.2610 0.6915 0.136 Uiso 0.50 1 calc PR . . H51C H 0.5220 0.2629 0.5894 0.136 Uiso 0.50 1 calc PR . . C52 C 0.1145(4) 0.2500 0.1539(6) 0.068(3) Uani 1 2 d S . . H52A H 0.1269 0.2731 0.1332 0.102 Uiso 0.50 1 calc PR . . H52B H 0.0690 0.2438 0.1326 0.102 Uiso 0.50 1 calc PR . . H52C H 0.1479 0.2331 0.1333 0.102 Uiso 0.50 1 calc PR . . C53 C 0.4385(3) 0.02073(15) 0.2179(4) 0.0538(17) Uani 1 1 d . . . H53A H 0.4849 0.0129 0.2044 0.081 Uiso 1 1 calc R . . H53B H 0.4077 0.0144 0.1712 0.081 Uiso 1 1 calc R . . H53C H 0.4231 0.0097 0.2708 0.081 Uiso 1 1 calc R . . C54 C 0.4384(3) 0.05796(16) 0.2286(3) 0.0338(13) Uani 1 1 d . . . C55 C 0.1829(3) 0.09446(13) 0.5441(3) 0.0334(13) Uani 1 1 d . . . H55A H 0.1556 0.1097 0.5807 0.050 Uiso 1 1 calc R . . H55B H 0.1684 0.0971 0.4846 0.050 Uiso 1 1 calc R . . H55C H 0.2313 0.1007 0.5493 0.050 Uiso 1 1 calc R . . C56 C 0.1736(3) 0.05895(15) 0.5705(3) 0.0321(13) 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 Gd1 0.01901(17) 0.01437(16) 0.02325(19) 0.000 0.00117(14) 0.000 Fe1 0.0215(4) 0.0130(3) 0.0234(4) -0.0004(3) 0.0010(3) 0.0000(3) Cl1 0.0324(10) 0.0514(13) 0.0415(12) 0.000 0.0013(9) 0.000 O1 0.0234(17) 0.0168(16) 0.0276(19) -0.0016(14) -0.0009(15) 0.0002(14) N1 0.026(2) 0.031(3) 0.045(3) -0.007(2) 0.003(2) 0.009(2) C1 0.028(3) 0.022(3) 0.013(3) -0.004(2) 0.004(2) -0.003(2) Gd2 0.02073(18) 0.01470(17) 0.0291(2) 0.000 -0.00227(15) 0.000 O2 0.0176(16) 0.0165(16) 0.0228(18) 0.0022(14) 0.0021(14) 0.0007(13) N2 0.039(3) 0.033(3) 0.044(3) -0.008(2) 0.002(2) 0.008(2) C2 0.027(3) 0.026(3) 0.021(3) -0.002(2) 0.000(2) -0.003(2) O3 0.0216(17) 0.0125(15) 0.0231(18) -0.0025(13) -0.0012(14) 0.0019(13) N3 0.042(3) 0.049(3) 0.028(3) -0.003(2) 0.006(2) -0.005(2) C3 0.031(3) 0.023(3) 0.015(3) 0.002(2) 0.002(2) -0.005(2) O4 0.0282(18) 0.0171(17) 0.0235(19) 0.0016(14) 0.0004(15) -0.0021(14) N4 0.062(4) 0.047(4) 0.082(4) 0.023(3) 0.005(3) 0.002(3) C4 0.028(3) 0.025(3) 0.018(3) 0.001(2) -0.003(2) 0.004(2) O5 0.030(3) 0.022(2) 0.026(3) 0.000 -0.006(2) 0.000 C5 0.023(2) 0.018(2) 0.017(3) -0.0059(19) 0.000(2) -0.003(2) O6 0.025(3) 0.070(4) 0.047(4) 0.000 -0.013(3) 0.000 C6 0.032(3) 0.015(2) 0.016(3) -0.002(2) 0.003(2) 0.000(2) O7 0.0263(19) 0.0223(19) 0.054(3) -0.0100(18) 0.0016(18) 0.0040(15) C7 0.026(3) 0.018(2) 0.020(3) -0.001(2) 0.002(2) 0.002(2) O8 0.020(2) 0.014(2) 0.034(3) 0.000 -0.001(2) 0.000 C8 0.023(3) 0.012(2) 0.023(3) -0.0011(19) 0.002(2) -0.0039(19) O9 0.0274(19) 0.0268(19) 0.027(2) 0.0005(15) 0.0075(16) 0.0089(16) C9 0.022(2) 0.020(2) 0.019(3) 0.005(2) 0.000(2) -0.001(2) O10 0.031(3) 0.062(4) 0.023(3) 0.000 -0.006(2) 0.000 C10 0.016(2) 0.014(2) 0.029(3) -0.001(2) -0.002(2) -0.0015(19) O11 0.014(2) 0.025(3) 0.029(3) 0.000 -0.003(2) 0.000 C11 0.016(2) 0.018(2) 0.021(3) -0.001(2) 0.0009(19) 0.0020(19) O12 0.021(2) 0.020(2) 0.028(3) 0.000 -0.002(2) 0.000 C12 0.015(2) 0.017(2) 0.025(3) 0.002(2) 0.004(2) -0.0035(19) C13 0.020(2) 0.010(2) 0.028(3) -0.002(2) -0.002(2) -0.0011(19) C14 0.021(2) 0.015(2) 0.021(3) 0.0018(19) 0.002(2) 0.0034(19) C15 0.018(2) 0.019(2) 0.017(2) 0.005(2) 0.003(2) 0.0009(19) C16 0.022(2) 0.014(2) 0.023(3) 0.002(2) 0.004(2) 0.0010(19) C17 0.025(3) 0.017(2) 0.015(3) 0.0043(19) 0.000(2) -0.0026(19) C18 0.019(2) 0.019(2) 0.016(2) 0.001(2) -0.0008(19) -0.0036(19) C19 0.023(2) 0.017(2) 0.015(2) 0.004(2) 0.005(2) 0.0023(19) C20 0.028(3) 0.014(2) 0.012(2) 0.0041(18) 0.0032(19) -0.004(2) C21 0.020(2) 0.018(2) 0.022(3) -0.002(2) 0.003(2) -0.003(2) C22 0.016(2) 0.019(2) 0.020(3) 0.001(2) 0.0034(19) 0.0036(19) C23 0.019(2) 0.018(2) 0.023(3) -0.002(2) -0.002(2) 0.0013(19) C24 0.018(2) 0.019(2) 0.024(3) 0.002(2) 0.002(2) 0.001(2) C25 0.027(3) 0.022(3) 0.023(3) 0.007(2) 0.006(2) 0.002(2) C26 0.020(2) 0.021(3) 0.026(3) -0.001(2) 0.005(2) 0.002(2) C27 0.015(2) 0.020(2) 0.024(3) -0.002(2) 0.003(2) 0.0048(19) C28 0.022(2) 0.024(3) 0.023(3) -0.002(2) 0.005(2) -0.001(2) C29 0.029(3) 0.033(3) 0.025(3) 0.008(2) 0.004(2) 0.000(2) C30 0.055(4) 0.043(4) 0.031(3) 0.008(3) -0.001(3) 0.004(3) C31 0.044(3) 0.023(3) 0.042(4) 0.009(2) 0.007(3) 0.003(2) C32 0.045(3) 0.034(3) 0.054(4) 0.021(3) 0.006(3) -0.011(3) C33 0.023(2) 0.018(2) 0.027(3) 0.003(2) 0.001(2) 0.003(2) C34 0.037(3) 0.023(3) 0.036(3) 0.005(2) 0.007(3) 0.013(2) C35 0.041(3) 0.019(3) 0.043(3) 0.000(2) -0.002(3) 0.002(2) C36 0.034(3) 0.015(2) 0.034(3) 0.002(2) 0.000(2) 0.007(2) C37 0.022(2) 0.018(2) 0.031(3) -0.004(2) 0.002(2) -0.003(2) C38 0.050(3) 0.030(3) 0.022(3) -0.010(2) -0.003(2) 0.002(3) C39 0.042(3) 0.019(3) 0.041(3) -0.003(2) 0.007(3) -0.005(2) C40 0.039(3) 0.022(3) 0.049(4) -0.008(3) 0.008(3) 0.000(2) C41 0.027(3) 0.025(3) 0.028(3) 0.002(2) -0.002(2) -0.004(2) C42 0.030(3) 0.027(3) 0.049(4) 0.005(3) 0.005(3) -0.008(2) C43 0.037(3) 0.029(3) 0.035(3) 0.003(2) 0.003(2) -0.009(2) C44 0.039(3) 0.020(3) 0.043(3) 0.002(2) 0.004(3) -0.005(2) C45 0.052(4) 0.057(4) 0.051(4) -0.001(3) 0.005(3) -0.004(3) C46 0.048(4) 0.084(5) 0.068(5) -0.016(4) 0.004(4) 0.011(4) C47 0.045(4) 0.028(3) 0.041(4) 0.002(3) -0.009(3) 0.000(3) C48 0.052(4) 0.040(4) 0.060(5) 0.014(3) -0.008(3) 0.003(3) C49 0.071(5) 0.097(6) 0.062(5) -0.032(4) 0.008(4) 0.002(4) C50 0.035(3) 0.041(4) 0.047(4) 0.004(3) -0.007(3) -0.011(3) C51 0.127(11) 0.060(7) 0.084(9) 0.000 -0.037(8) 0.000 C52 0.032(5) 0.092(8) 0.080(8) 0.000 -0.001(5) 0.000 C53 0.065(4) 0.041(4) 0.056(4) 0.000(3) 0.001(3) -0.007(3) C54 0.029(3) 0.045(4) 0.027(3) -0.003(3) 0.005(2) -0.005(3) C55 0.034(3) 0.027(3) 0.039(3) 0.003(2) 0.000(2) 0.001(2) C56 0.028(3) 0.039(3) 0.029(3) 0.004(3) 0.001(2) 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 Gd1 O8 2.303(4) . ? Gd1 O3 2.379(3) 8_565 ? Gd1 O3 2.379(3) . ? Gd1 O9 2.381(3) . ? Gd1 O9 2.381(3) 8_565 ? Gd1 O10 2.421(5) . ? Gd1 O11 2.469(4) . ? Gd1 O12 2.530(4) . ? Gd1 Fe1 3.4140(8) 8_565 ? Gd1 Fe1 3.4140(8) . ? Gd1 Gd2 3.9172(5) . ? Fe1 O12 1.8699(15) . ? Fe1 O1 1.925(3) . ? Fe1 O4 1.929(3) . ? Fe1 O3 2.024(3) . ? Fe1 O2 2.027(3) . ? Fe1 Gd2 3.4087(7) . ? O1 C6 1.359(5) . ? N1 C50 1.328(7) . ? N1 C48 1.430(7) . ? N1 C49 1.434(7) . ? C1 C2 1.393(6) . ? C1 C6 1.401(6) . ? C1 C28 1.517(6) . ? Gd2 O8 2.293(4) . ? Gd2 O7 2.359(3) 8_565 ? Gd2 O7 2.359(3) . ? Gd2 O2 2.400(3) . ? Gd2 O2 2.400(3) 8_565 ? Gd2 O6 2.457(5) . ? Gd2 O5 2.490(5) . ? Gd2 O12 2.507(4) . ? Gd2 Fe1 3.4087(7) 8_565 ? O2 C13 1.369(5) . ? N2 C47 1.345(7) . ? N2 C46 1.433(7) . ? N2 C45 1.435(7) . ? C2 C3 1.383(6) . ? O3 C20 1.368(5) . ? N3 C54 1.132(6) . ? C3 C4 1.392(6) . ? C3 C29 1.545(6) . ? O4 C27 1.357(5) . ? N4 C56 1.162(7) . ? C4 C5 1.406(6) . ? C5 C6 1.403(6) . ? C5 C7 1.510(6) . ? O6 C51 1.465(12) . ? O7 C50 1.185(6) . ? C7 C8 1.527(6) . ? C8 C9 1.387(6) . ? C8 C13 1.399(6) . ? O9 C47 1.220(6) . ? C9 C10 1.392(6) . ? O10 C52 1.400(10) . ? C10 C11 1.393(6) . ? C10 C33 1.532(6) . ? C11 C12 1.401(6) . ? O12 Fe1 1.8699(14) 8_565 ? C12 C13 1.409(6) . ? C12 C14 1.502(6) . ? C14 C15 1.512(6) . ? C15 C16 1.387(6) . ? C15 C20 1.395(6) . ? C16 C17 1.396(6) . ? C17 C18 1.388(6) . ? C17 C37 1.541(6) . ? C18 C19 1.401(6) . ? C19 C20 1.406(6) . ? C19 C21 1.526(6) . ? C21 C22 1.512(6) . ? C22 C23 1.389(6) . ? C22 C27 1.400(6) . ? C23 C24 1.392(6) . ? C24 C25 1.381(6) . ? C24 C41 1.539(6) . ? C25 C26 1.392(6) . ? C26 C27 1.412(6) . ? C26 C28 1.513(6) . ? C29 C30 1.514(7) . ? C29 C31 1.532(7) . ? C29 C32 1.533(7) . ? C33 C36 1.521(6) . ? C33 C35 1.530(6) . ? C33 C34 1.538(6) . ? C37 C38 1.529(7) . ? C37 C40 1.532(6) . ? C37 C39 1.545(7) . ? C41 C43 1.518(6) . ? C41 C44 1.528(7) . ? C41 C42 1.528(7) . ? C53 C54 1.449(8) . ? C55 C56 1.445(7) . ? 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 O8 Gd1 O3 89.05(8) . 8_565 ? O8 Gd1 O3 89.05(8) . . ? O3 Gd1 O3 133.26(14) 8_565 . ? O8 Gd1 O9 85.10(12) . . ? O3 Gd1 O9 150.71(10) 8_565 . ? O3 Gd1 O9 75.41(10) . . ? O8 Gd1 O9 85.10(12) . 8_565 ? O3 Gd1 O9 75.41(10) 8_565 8_565 ? O3 Gd1 O9 150.71(10) . 8_565 ? O9 Gd1 O9 75.50(15) . 8_565 ? O8 Gd1 O10 153.44(16) . . ? O3 Gd1 O10 101.07(8) 8_565 . ? O3 Gd1 O10 101.07(8) . . ? O9 Gd1 O10 74.04(12) . . ? O9 Gd1 O10 74.04(12) 8_565 . ? O8 Gd1 O11 140.14(15) . . ? O3 Gd1 O11 76.04(7) 8_565 . ? O3 Gd1 O11 76.04(7) . . ? O9 Gd1 O11 124.71(10) . . ? O9 Gd1 O11 124.71(10) 8_565 . ? O10 Gd1 O11 66.42(15) . . ? O8 Gd1 O12 70.20(15) . . ? O3 Gd1 O12 67.76(7) 8_565 . ? O3 Gd1 O12 67.76(7) . . ? O9 Gd1 O12 135.29(9) . . ? O9 Gd1 O12 135.29(9) 8_565 . ? O10 Gd1 O12 136.36(15) . . ? O11 Gd1 O12 69.94(14) . . ? O8 Gd1 Fe1 80.70(10) . 8_565 ? O3 Gd1 Fe1 35.54(7) 8_565 8_565 ? O3 Gd1 Fe1 98.30(7) . 8_565 ? O9 Gd1 Fe1 164.59(8) . 8_565 ? O9 Gd1 Fe1 108.97(8) 8_565 8_565 ? O10 Gd1 Fe1 121.27(9) . 8_565 ? O11 Gd1 Fe1 65.62(8) . 8_565 ? O12 Gd1 Fe1 32.56(3) . 8_565 ? O8 Gd1 Fe1 80.70(10) . . ? O3 Gd1 Fe1 98.30(7) 8_565 . ? O3 Gd1 Fe1 35.54(7) . . ? O9 Gd1 Fe1 108.97(8) . . ? O9 Gd1 Fe1 164.59(8) 8_565 . ? O10 Gd1 Fe1 121.27(9) . . ? O11 Gd1 Fe1 65.62(8) . . ? O12 Gd1 Fe1 32.56(3) . . ? Fe1 Gd1 Fe1 62.91(2) 8_565 . ? O8 Gd1 Gd2 31.47(11) . . ? O3 Gd1 Gd2 77.23(7) 8_565 . ? O3 Gd1 Gd2 77.23(7) . . ? O9 Gd1 Gd2 109.72(8) . . ? O9 Gd1 Gd2 109.72(8) 8_565 . ? O10 Gd1 Gd2 175.09(12) . . ? O11 Gd1 Gd2 108.68(10) . . ? O12 Gd1 Gd2 38.74(9) . . ? Fe1 Gd1 Gd2 54.897(13) 8_565 . ? Fe1 Gd1 Gd2 54.897(13) . . ? O12 Fe1 O1 107.46(16) . . ? O12 Fe1 O4 107.36(15) . . ? O1 Fe1 O4 92.64(12) . . ? O12 Fe1 O3 89.33(16) . . ? O1 Fe1 O3 162.56(12) . . ? O4 Fe1 O3 86.56(12) . . ? O12 Fe1 O2 89.37(15) . . ? O1 Fe1 O2 86.40(12) . . ? O4 Fe1 O2 162.67(12) . . ? O3 Fe1 O2 89.21(12) . . ? O12 Fe1 Gd2 46.15(12) . . ? O1 Fe1 Gd2 93.62(9) . . ? O4 Fe1 Gd2 153.33(9) . . ? O3 Fe1 Gd2 94.86(8) . . ? O2 Fe1 Gd2 43.83(8) . . ? O12 Fe1 Gd1 46.74(13) . . ? O1 Fe1 Gd1 154.11(9) . . ? O4 Fe1 Gd1 93.98(9) . . ? O3 Fe1 Gd1 43.10(8) . . ? O2 Fe1 Gd1 94.38(8) . . ? Gd2 Fe1 Gd1 70.080(14) . . ? C6 O1 Fe1 130.2(3) . . ? C50 N1 C48 120.2(5) . . ? C50 N1 C49 120.3(5) . . ? C48 N1 C49 119.1(5) . . ? C2 C1 C6 119.0(4) . . ? C2 C1 C28 119.6(4) . . ? C6 C1 C28 121.1(4) . . ? O8 Gd2 O7 85.97(12) . 8_565 ? O8 Gd2 O7 85.97(12) . . ? O7 Gd2 O7 76.57(16) 8_565 . ? O8 Gd2 O2 88.35(8) . . ? O7 Gd2 O2 150.70(11) 8_565 . ? O7 Gd2 O2 74.37(10) . . ? O8 Gd2 O2 88.35(8) . 8_565 ? O7 Gd2 O2 74.37(10) 8_565 8_565 ? O7 Gd2 O2 150.70(11) . 8_565 ? O2 Gd2 O2 134.20(13) . 8_565 ? O8 Gd2 O6 152.86(16) . . ? O7 Gd2 O6 72.90(13) 8_565 . ? O7 Gd2 O6 72.90(13) . . ? O2 Gd2 O6 101.69(8) . . ? O2 Gd2 O6 101.69(8) 8_565 . ? O8 Gd2 O5 141.32(14) . . ? O7 Gd2 O5 122.92(11) 8_565 . ? O7 Gd2 O5 122.92(11) . . ? O2 Gd2 O5 77.29(8) . . ? O2 Gd2 O5 77.29(8) 8_565 . ? O6 Gd2 O5 65.82(16) . . ? O8 Gd2 O12 70.78(14) . . ? O7 Gd2 O12 135.65(9) 8_565 . ? O7 Gd2 O12 135.65(9) . . ? O2 Gd2 O12 67.92(7) . . ? O2 Gd2 O12 67.92(7) 8_565 . ? O6 Gd2 O12 136.36(16) . . ? O5 Gd2 O12 70.54(14) . . ? O8 Gd2 Fe1 80.94(9) . . ? O7 Gd2 Fe1 165.43(9) 8_565 . ? O7 Gd2 Fe1 108.67(8) . . ? O2 Gd2 Fe1 35.79(7) . . ? O2 Gd2 Fe1 98.73(7) 8_565 . ? O6 Gd2 Fe1 121.49(10) . . ? O5 Gd2 Fe1 66.37(8) . . ? O12 Gd2 Fe1 32.54(3) . . ? O8 Gd2 Fe1 80.94(9) . 8_565 ? O7 Gd2 Fe1 108.67(8) 8_565 8_565 ? O7 Gd2 Fe1 165.43(9) . 8_565 ? O2 Gd2 Fe1 98.73(7) . 8_565 ? O2 Gd2 Fe1 35.79(7) 8_565 8_565 ? O6 Gd2 Fe1 121.49(10) . 8_565 ? O5 Gd2 Fe1 66.37(8) . 8_565 ? O12 Gd2 Fe1 32.54(3) . 8_565 ? Fe1 Gd2 Fe1 63.02(2) . 8_565 ? O8 Gd2 Gd1 31.61(10) . . ? O7 Gd2 Gd1 110.49(9) 8_565 . ? O7 Gd2 Gd1 110.49(9) . . ? O2 Gd2 Gd1 76.83(7) . . ? O2 Gd2 Gd1 76.83(7) 8_565 . ? O6 Gd2 Gd1 175.53(12) . . ? O5 Gd2 Gd1 109.70(10) . . ? O12 Gd2 Gd1 39.17(10) . . ? Fe1 Gd2 Gd1 55.023(13) . . ? Fe1 Gd2 Gd1 55.023(13) 8_565 . ? C13 O2 Fe1 124.6(3) . . ? C13 O2 Gd2 135.0(2) . . ? Fe1 O2 Gd2 100.37(12) . . ? C47 N2 C46 120.2(5) . . ? C47 N2 C45 121.3(5) . . ? C46 N2 C45 118.5(5) . . ? C3 C2 C1 123.1(4) . . ? C20 O3 Fe1 126.5(3) . . ? C20 O3 Gd1 132.1(3) . . ? Fe1 O3 Gd1 101.36(12) . . ? C2 C3 C4 117.2(4) . . ? C2 C3 C29 122.1(4) . . ? C4 C3 C29 120.7(4) . . ? C27 O4 Fe1 129.9(3) . . ? C3 C4 C5 121.9(4) . . ? C6 C5 C4 119.4(4) . . ? C6 C5 C7 121.2(4) . . ? C4 C5 C7 119.2(4) . . ? C51 O6 Gd2 129.9(5) . . ? O1 C6 C1 120.1(4) . . ? O1 C6 C5 120.5(4) . . ? C1 C6 C5 119.4(4) . . ? C50 O7 Gd2 148.1(4) . . ? C5 C7 C8 111.4(4) . . ? Gd2 O8 Gd1 116.92(18) . . ? C9 C8 C13 120.0(4) . . ? C9 C8 C7 119.1(4) . . ? C13 C8 C7 120.7(4) . . ? C47 O9 Gd1 133.1(3) . . ? C8 C9 C10 122.9(4) . . ? C52 O10 Gd1 129.8(5) . . ? C11 C10 C9 116.1(4) . . ? C11 C10 C33 119.4(4) . . ? C9 C10 C33 124.4(4) . . ? C10 C11 C12 123.3(4) . . ? Fe1 O12 Fe1 144.6(3) . 8_565 ? Fe1 O12 Gd2 101.31(13) . . ? Fe1 O12 Gd2 101.31(13) 8_565 . ? Fe1 O12 Gd1 100.69(13) . . ? Fe1 O12 Gd1 100.69(13) 8_565 . ? Gd2 O12 Gd1 102.10(15) . . ? C11 C12 C13 118.8(4) . . ? C11 C12 C14 119.3(4) . . ? C13 C12 C14 121.6(4) . . ? O2 C13 C8 121.7(4) . . ? O2 C13 C12 119.4(4) . . ? C8 C13 C12 118.9(4) . . ? C12 C14 C15 109.2(4) . . ? C16 C15 C20 120.1(4) . . ? C16 C15 C14 120.1(4) . . ? C20 C15 C14 119.5(4) . . ? C15 C16 C17 122.3(4) . . ? C18 C17 C16 116.7(4) . . ? C18 C17 C37 120.2(4) . . ? C16 C17 C37 123.1(4) . . ? C17 C18 C19 122.9(4) . . ? C18 C19 C20 118.8(4) . . ? C18 C19 C21 118.5(4) . . ? C20 C19 C21 122.6(4) . . ? O3 C20 C15 120.7(4) . . ? O3 C20 C19 120.1(4) . . ? C15 C20 C19 119.2(4) . . ? C22 C21 C19 111.7(4) . . ? C23 C22 C27 119.4(4) . . ? C23 C22 C21 119.4(4) . . ? C27 C22 C21 121.0(4) . . ? C22 C23 C24 123.1(4) . . ? C25 C24 C23 116.1(4) . . ? C25 C24 C41 124.3(4) . . ? C23 C24 C41 119.6(4) . . ? C24 C25 C26 123.7(4) . . ? C25 C26 C27 118.7(4) . . ? C25 C26 C28 121.0(4) . . ? C27 C26 C28 120.1(4) . . ? O4 C27 C22 120.8(4) . . ? O4 C27 C26 120.3(4) . . ? C22 C27 C26 119.0(4) . . ? C26 C28 C1 109.5(4) . . ? C30 C29 C31 109.4(4) . . ? C30 C29 C32 108.8(4) . . ? C31 C29 C32 107.2(4) . . ? C30 C29 C3 109.1(4) . . ? C31 C29 C3 112.1(4) . . ? C32 C29 C3 110.3(4) . . ? C36 C33 C35 108.1(4) . . ? C36 C33 C10 112.0(4) . . ? C35 C33 C10 109.8(4) . . ? C36 C33 C34 109.5(4) . . ? C35 C33 C34 108.0(4) . . ? C10 C33 C34 109.4(4) . . ? C38 C37 C40 108.7(4) . . ? C38 C37 C17 109.8(4) . . ? C40 C37 C17 112.3(4) . . ? C38 C37 C39 108.7(4) . . ? C40 C37 C39 108.6(4) . . ? C17 C37 C39 108.8(4) . . ? C43 C41 C44 107.5(4) . . ? C43 C41 C42 109.3(4) . . ? C44 C41 C42 109.2(4) . . ? C43 C41 C24 111.8(4) . . ? C44 C41 C24 109.7(4) . . ? C42 C41 C24 109.3(4) . . ? O9 C47 N2 124.5(5) . . ? O7 C50 N1 126.2(6) . . ? N3 C54 C53 178.4(7) . . ? N4 C56 C55 179.2(7) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.25 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.829 _refine_diff_density_min -1.131 _refine_diff_density_rms 0.125 # Attachment '- 2.cif' data_S117 _database_code_depnum_ccdc_archive 'CCDC 827078' #TrackingRef '- 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common S117 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C110 H157 Cl Fe2 N8 O18 Tb2' _chemical_formula_weight 2344.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 19.5960(9) _cell_length_b 38.5567(17) _cell_length_c 15.7077(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11868.1(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9368 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 27.08 _exptl_crystal_description Block _exptl_crystal_colour Black _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.312 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4864 _exptl_absorpt_coefficient_mu 1.502 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6215 _exptl_absorpt_correction_T_max 0.7532 _exptl_absorpt_process_details Bruker-SADABS _exptl_special_details ; Data were corrected for decay and absorption using the program SADABS based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995). ; _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 'Bruker X8 Apex II CCD Diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 246749 _diffrn_reflns_av_R_equivalents 0.0446 _diffrn_reflns_av_sigmaI/netI 0.0213 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -49 _diffrn_reflns_limit_k_max 49 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.06 _diffrn_reflns_theta_max 27.18 _reflns_number_total 13352 _reflns_number_gt 11535 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex II' _computing_cell_refinement 'SAINT (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed (Barbour, 2001)' _computing_publication_material 'local program' _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. There was diffuse electron density associated with badly disordered solvent that could not be modelled appropriately. Given this the routine SQUEEZE was applied to the date to remove this density. This had the effect of markedly improving the agreement indices. ; _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^)+(0.0426P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13352 _refine_ls_number_parameters 672 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0497 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.1233 _refine_ls_wR_factor_gt 0.1192 _refine_ls_goodness_of_fit_ref 1.224 _refine_ls_restrained_S_all 1.224 _refine_ls_shift/su_max 0.008 _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 0.291191(12) 0.2500 0.343532(16) 0.01546(7) Uani 1 2 d S . . Fe1 Fe 0.29864(3) 0.203964(12) 0.52857(3) 0.01509(11) Uani 1 1 d . . . O1 O 0.27782(18) 0.2500 0.5035(2) 0.0200(8) Uani 1 2 d S . . O12 O 0.19736(12) 0.19326(6) 0.52953(16) 0.0169(5) Uani 1 1 d . . . N1 N 0.3338(3) 0.03079(13) 0.5924(4) 0.0600(14) Uani 1 1 d . . . C1 C 0.15687(18) 0.14244(9) 0.4558(2) 0.0171(7) Uani 1 1 d . . . Tb2 Tb 0.150751(12) 0.2500 0.519797(17) 0.01805(8) Uani 1 2 d S . . Cl2 Cl 0.54515(7) 0.2500 0.25968(10) 0.0333(3) Uani 1 2 d S . . O2 O 0.29531(13) 0.19880(6) 0.65108(16) 0.0192(5) Uani 1 1 d . . . N2 N 0.0607(2) 0.08697(11) 0.2388(3) 0.0397(9) Uani 1 1 d . . . C2 C 0.13053(18) 0.10907(9) 0.4588(2) 0.0172(7) Uani 1 1 d . . . H2 H 0.1207 0.0975 0.4068 0.021 Uiso 1 1 calc R . . O3 O 0.39680(13) 0.19930(6) 0.52644(16) 0.0203(5) Uani 1 1 d . . . N3 N 0.1958(2) 0.17704(10) 0.1477(2) 0.0341(9) Uani 1 1 d . . . C3 C 0.11789(18) 0.09178(9) 0.5358(2) 0.0188(7) Uani 1 1 d . . . O4 O 0.30079(12) 0.19366(6) 0.40207(16) 0.0164(5) Uani 1 1 d . . . N4 N -0.01045(17) 0.17064(9) 0.4397(3) 0.0307(8) Uani 1 1 d . . . C4 C 0.13111(18) 0.11000(9) 0.6104(2) 0.0176(7) Uani 1 1 d . . . H4 H 0.1224 0.0990 0.6635 0.021 Uiso 1 1 calc R . . O5 O 0.25783(14) 0.21251(7) 0.23138(17) 0.0236(6) Uani 1 1 d . . . C5 C 0.15669(18) 0.14380(9) 0.6104(2) 0.0173(7) Uani 1 1 d . . . O6 O 0.06171(14) 0.21232(7) 0.4825(2) 0.0324(7) Uani 1 1 d . . . C6 C 0.17077(18) 0.16040(9) 0.5319(2) 0.0163(7) Uani 1 1 d . . . O7 O 0.0694(2) 0.2500 0.6380(3) 0.0425(12) Uani 1 2 d S . . C7 C 0.17307(19) 0.16120(9) 0.6952(2) 0.0187(7) Uani 1 1 d . . . H7A H 0.1702 0.1867 0.6886 0.022 Uiso 1 1 calc R . . H7B H 0.1390 0.1541 0.7383 0.022 Uiso 1 1 calc R . . O8 O 0.3855(2) 0.2500 0.2439(3) 0.0357(10) Uani 1 2 d S . . C8 C 0.24391(19) 0.15134(9) 0.7255(2) 0.0181(7) Uani 1 1 d . . . O9 O 0.17827(18) 0.2500 0.3778(2) 0.0198(8) Uani 1 2 d S . . C9 C 0.25227(19) 0.12124(10) 0.7747(2) 0.0213(8) Uani 1 1 d . . . H9 H 0.2129 0.1087 0.7922 0.026 Uiso 1 1 calc R . . O10 O 0.40365(18) 0.2500 0.4118(2) 0.0191(7) Uani 1 2 d S . . C10 C 0.3166(2) 0.10907(10) 0.7988(2) 0.0218(8) Uani 1 1 d . . . O11 O 0.2044(2) 0.2500 0.6632(3) 0.0243(8) Uani 1 2 d S . . C11 C 0.3725(2) 0.12887(10) 0.7751(2) 0.0224(8) Uani 1 1 d . . . H11 H 0.4166 0.1217 0.7930 0.027 Uiso 1 1 calc R . . C12 C 0.36668(19) 0.15890(9) 0.7259(2) 0.0190(7) Uani 1 1 d . . . C13 C 0.30191(19) 0.17004(9) 0.7004(2) 0.0189(7) Uani 1 1 d . . . C14 C 0.43113(19) 0.17678(10) 0.6946(2) 0.0205(7) Uani 1 1 d . . . H14A H 0.4214 0.2015 0.6824 0.025 Uiso 1 1 calc R . . H14B H 0.4668 0.1757 0.7391 0.025 Uiso 1 1 calc R . . C15 C 0.45625(18) 0.15893(9) 0.6143(2) 0.0195(7) Uani 1 1 d . . . C16 C 0.49575(19) 0.12871(9) 0.6208(2) 0.0208(7) Uani 1 1 d . . . H16 H 0.5095 0.1210 0.6757 0.025 Uiso 1 1 calc R . . C17 C 0.51547(18) 0.10964(9) 0.5499(2) 0.0197(7) Uani 1 1 d . . . C18 C 0.49633(18) 0.12268(9) 0.4699(2) 0.0185(7) Uani 1 1 d . . . H18 H 0.5102 0.1105 0.4203 0.022 Uiso 1 1 calc R . . C19 C 0.45788(18) 0.15273(9) 0.4606(2) 0.0174(7) Uani 1 1 d . . . C20 C 0.43670(18) 0.17088(9) 0.5336(2) 0.0177(7) Uani 1 1 d . . . C21 C 0.43619(17) 0.16390(9) 0.3718(2) 0.0170(7) Uani 1 1 d . . . H21A H 0.4720 0.1574 0.3303 0.020 Uiso 1 1 calc R . . H21B H 0.4308 0.1894 0.3702 0.020 Uiso 1 1 calc R . . C22 C 0.36905(18) 0.14675(9) 0.3467(2) 0.0152(7) Uani 1 1 d . . . C23 C 0.37136(18) 0.11414(9) 0.3085(2) 0.0163(7) Uani 1 1 d . . . H23 H 0.4146 0.1041 0.2968 0.020 Uiso 1 1 calc R . . C24 C 0.31266(19) 0.09578(9) 0.2867(2) 0.0178(7) Uani 1 1 d . . . C25 C 0.25007(18) 0.11112(9) 0.3053(2) 0.0160(7) Uani 1 1 d . . . H25 H 0.2093 0.0992 0.2908 0.019 Uiso 1 1 calc R . . C26 C 0.24557(18) 0.14365(9) 0.3447(2) 0.0152(7) Uani 1 1 d . . . C27 C 0.30546(18) 0.16168(9) 0.3647(2) 0.0161(7) Uani 1 1 d . . . C28 C 0.17626(17) 0.15763(9) 0.3701(2) 0.0155(7) Uani 1 1 d . . . H28A H 0.1418 0.1511 0.3269 0.019 Uiso 1 1 calc R . . H28B H 0.1779 0.1832 0.3738 0.019 Uiso 1 1 calc R . . C29 C 0.0918(2) 0.05419(9) 0.5332(2) 0.0205(8) Uani 1 1 d . . . C30 C 0.1454(2) 0.03112(11) 0.4893(3) 0.0319(10) Uani 1 1 d . . . H30A H 0.1526 0.0392 0.4308 0.048 Uiso 1 1 calc R . . H30B H 0.1293 0.0071 0.4883 0.048 Uiso 1 1 calc R . . H30C H 0.1886 0.0324 0.5207 0.048 Uiso 1 1 calc R . . C31 C 0.0798(2) 0.03972(10) 0.6227(3) 0.0249(8) Uani 1 1 d . . . H31A H 0.1230 0.0394 0.6541 0.037 Uiso 1 1 calc R . . H31B H 0.0617 0.0161 0.6186 0.037 Uiso 1 1 calc R . . H31C H 0.0469 0.0544 0.6528 0.037 Uiso 1 1 calc R . . C32 C 0.0252(2) 0.05255(11) 0.4818(3) 0.0295(9) Uani 1 1 d . . . H32A H -0.0093 0.0673 0.5089 0.044 Uiso 1 1 calc R . . H32B H 0.0087 0.0286 0.4800 0.044 Uiso 1 1 calc R . . H32C H 0.0336 0.0608 0.4237 0.044 Uiso 1 1 calc R . . C33 C 0.3243(2) 0.07540(10) 0.8503(2) 0.0244(8) Uani 1 1 d . . . C34 C 0.3950(3) 0.05901(13) 0.8344(3) 0.0426(12) Uani 1 1 d . . . H34A H 0.4305 0.0740 0.8586 0.064 Uiso 1 1 calc R . . H34B H 0.4025 0.0565 0.7731 0.064 Uiso 1 1 calc R . . H34C H 0.3970 0.0361 0.8616 0.064 Uiso 1 1 calc R . . C35 C 0.3186(3) 0.08391(13) 0.9452(3) 0.0378(11) Uani 1 1 d . . . H35A H 0.2735 0.0938 0.9570 0.057 Uiso 1 1 calc R . . H35B H 0.3539 0.1007 0.9607 0.057 Uiso 1 1 calc R . . H35C H 0.3248 0.0627 0.9786 0.057 Uiso 1 1 calc R . . C36 C 0.2702(2) 0.04863(11) 0.8264(3) 0.0325(10) Uani 1 1 d . . . H36A H 0.2776 0.0274 0.8593 0.049 Uiso 1 1 calc R . . H36B H 0.2735 0.0434 0.7655 0.049 Uiso 1 1 calc R . . H36C H 0.2248 0.0579 0.8391 0.049 Uiso 1 1 calc R . . C37 C 0.55628(19) 0.07575(10) 0.5552(3) 0.0225(8) Uani 1 1 d . . . C38 C 0.5168(2) 0.04664(10) 0.5106(3) 0.0329(10) Uani 1 1 d . . . H38A H 0.4723 0.0437 0.5381 0.049 Uiso 1 1 calc R . . H38B H 0.5427 0.0250 0.5146 0.049 Uiso 1 1 calc R . . H38C H 0.5101 0.0527 0.4506 0.049 Uiso 1 1 calc R . . C39 C 0.6250(2) 0.08060(11) 0.5101(3) 0.0314(9) Uani 1 1 d . . . H39A H 0.6171 0.0870 0.4505 0.047 Uiso 1 1 calc R . . H39B H 0.6509 0.0589 0.5125 0.047 Uiso 1 1 calc R . . H39C H 0.6509 0.0990 0.5383 0.047 Uiso 1 1 calc R . . C40 C 0.5686(2) 0.06469(12) 0.6471(3) 0.0329(10) Uani 1 1 d . . . H40A H 0.5946 0.0828 0.6767 0.049 Uiso 1 1 calc R . . H40B H 0.5945 0.0429 0.6479 0.049 Uiso 1 1 calc R . . H40C H 0.5247 0.0613 0.6758 0.049 Uiso 1 1 calc R . . C41 C 0.31912(19) 0.05967(9) 0.2459(2) 0.0206(7) Uani 1 1 d . . . C42 C 0.3487(2) 0.03436(10) 0.3119(3) 0.0321(10) Uani 1 1 d . . . H42A H 0.3931 0.0429 0.3315 0.048 Uiso 1 1 calc R . . H42B H 0.3545 0.0115 0.2858 0.048 Uiso 1 1 calc R . . H42C H 0.3175 0.0326 0.3604 0.048 Uiso 1 1 calc R . . C43 C 0.2500(2) 0.04533(10) 0.2164(3) 0.0338(10) Uani 1 1 d . . . H43A H 0.2191 0.0437 0.2652 0.051 Uiso 1 1 calc R . . H43B H 0.2565 0.0222 0.1916 0.051 Uiso 1 1 calc R . . H43C H 0.2304 0.0609 0.1735 0.051 Uiso 1 1 calc R . . C44 C 0.3670(2) 0.06155(11) 0.1687(3) 0.0322(10) Uani 1 1 d . . . H44A H 0.3499 0.0789 0.1285 0.048 Uiso 1 1 calc R . . H44B H 0.3687 0.0389 0.1407 0.048 Uiso 1 1 calc R . . H44C H 0.4129 0.0681 0.1877 0.048 Uiso 1 1 calc R . . C45 C 0.3173(2) 0.09461(11) 0.5438(3) 0.0306(9) Uani 1 1 d . . . H45A H 0.3495 0.0998 0.4979 0.046 Uiso 1 1 calc R . . H45B H 0.3257 0.1102 0.5919 0.046 Uiso 1 1 calc R . . H45C H 0.2705 0.0979 0.5232 0.046 Uiso 1 1 calc R . . C46 C 0.3261(2) 0.05891(12) 0.5711(3) 0.0343(10) Uani 1 1 d . . . C47 C 0.0613(3) 0.02068(13) 0.2189(4) 0.0517(14) Uani 1 1 d . . . H47A H 0.0977 0.0140 0.1793 0.078 Uiso 1 1 calc R . . H47B H 0.0171 0.0132 0.1961 0.078 Uiso 1 1 calc R . . H47C H 0.0691 0.0095 0.2741 0.078 Uiso 1 1 calc R . . C48 C 0.0613(2) 0.05804(13) 0.2297(3) 0.0329(10) Uani 1 1 d . . . C49 C 0.2030(2) 0.20297(11) 0.2028(3) 0.0290(9) Uani 1 1 d . . . H49 H 0.1630 0.2148 0.2210 0.035 Uiso 1 1 calc R . . C50 C 0.2528(3) 0.15729(14) 0.1173(3) 0.0441(12) Uani 1 1 d . . . H50A H 0.2614 0.1631 0.0575 0.066 Uiso 1 1 calc R . . H50B H 0.2426 0.1325 0.1223 0.066 Uiso 1 1 calc R . . H50C H 0.2933 0.1628 0.1513 0.066 Uiso 1 1 calc R . . C51 C 0.1278(3) 0.16688(17) 0.1203(4) 0.0570(15) Uani 1 1 d . . . H51A H 0.1179 0.1434 0.1408 0.086 Uiso 1 1 calc R . . H51B H 0.1256 0.1672 0.0579 0.086 Uiso 1 1 calc R . . H51C H 0.0942 0.1831 0.1435 0.086 Uiso 1 1 calc R . . C52 C 0.0323(2) 0.19708(11) 0.4267(3) 0.0301(9) Uani 1 1 d . . . H52 H 0.0399 0.2043 0.3697 0.036 Uiso 1 1 calc R . . C53 C -0.0226(3) 0.15757(13) 0.5233(4) 0.0451(13) Uani 1 1 d . . . H53A H -0.0095 0.1331 0.5258 0.068 Uiso 1 1 calc R . . H53B H -0.0711 0.1599 0.5372 0.068 Uiso 1 1 calc R . . H53C H 0.0046 0.1708 0.5645 0.068 Uiso 1 1 calc R . . C54 C -0.0403(3) 0.15263(19) 0.3689(4) 0.0681(19) Uani 1 1 d . . . H54A H -0.0295 0.1650 0.3160 0.102 Uiso 1 1 calc R . . H54B H -0.0899 0.1516 0.3761 0.102 Uiso 1 1 calc R . . H54C H -0.0219 0.1290 0.3661 0.102 Uiso 1 1 calc R . . C55 C -0.0034(4) 0.2500 0.6382(6) 0.060(2) Uani 1 2 d S . . H55A H -0.0200 0.2337 0.6814 0.090 Uiso 0.50 1 calc PR . . H55B H -0.0201 0.2429 0.5820 0.090 Uiso 0.50 1 calc PR . . H55C H -0.0200 0.2734 0.6512 0.090 Uiso 0.50 1 calc PR . . C56 C 0.3850(4) 0.2500 0.1538(5) 0.0484(19) Uani 1 2 d S . . H56A H 0.3811 0.2261 0.1330 0.073 Uiso 0.50 1 calc PR . . H56B H 0.4275 0.2603 0.1326 0.073 Uiso 0.50 1 calc PR . . H56C H 0.3461 0.2636 0.1333 0.073 Uiso 0.50 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 Tb1 0.01527(12) 0.00890(11) 0.02220(13) 0.000 -0.00092(9) 0.000 Fe1 0.0181(2) 0.0069(2) 0.0202(3) -0.00006(18) -0.0008(2) 0.00044(18) O1 0.0162(17) 0.0182(18) 0.0256(19) 0.000 0.0030(15) 0.000 O12 0.0173(12) 0.0108(11) 0.0226(13) 0.0000(10) 0.0000(10) -0.0050(9) N1 0.055(3) 0.043(3) 0.082(4) 0.026(3) 0.004(3) 0.005(2) C1 0.0161(16) 0.0117(16) 0.0233(18) -0.0009(14) -0.0016(14) 0.0018(13) Tb2 0.01761(13) 0.00890(12) 0.02764(15) 0.000 0.00241(10) 0.000 Cl2 0.0232(7) 0.0403(8) 0.0362(8) 0.000 0.0010(6) 0.000 O2 0.0235(13) 0.0131(12) 0.0211(13) 0.0007(10) 0.0000(10) 0.0000(10) N2 0.041(2) 0.040(2) 0.038(2) -0.0026(18) -0.0066(18) 0.0042(18) C2 0.0159(16) 0.0137(16) 0.0221(18) -0.0016(14) -0.0010(14) -0.0006(13) O3 0.0221(13) 0.0156(12) 0.0230(13) -0.0005(10) -0.0014(11) 0.0009(10) N3 0.037(2) 0.0274(19) 0.038(2) -0.0076(16) -0.0055(17) -0.0046(16) C3 0.0177(17) 0.0102(16) 0.028(2) 0.0011(14) 0.0012(14) 0.0005(13) O4 0.0204(12) 0.0080(11) 0.0207(13) -0.0017(9) -0.0020(10) 0.0013(9) N4 0.0214(16) 0.0259(18) 0.045(2) -0.0059(16) -0.0045(16) -0.0026(14) C4 0.0153(16) 0.0142(16) 0.0234(18) 0.0028(14) 0.0026(14) -0.0015(13) O5 0.0258(14) 0.0170(12) 0.0278(15) -0.0007(11) -0.0025(12) -0.0048(11) C5 0.0166(17) 0.0116(15) 0.0237(18) -0.0004(14) -0.0006(14) -0.0001(13) O6 0.0200(14) 0.0181(14) 0.059(2) -0.0062(14) -0.0035(14) -0.0020(11) C6 0.0162(16) 0.0080(15) 0.0248(19) 0.0006(13) 0.0006(14) 0.0020(13) O7 0.027(2) 0.059(3) 0.041(3) 0.000 0.008(2) 0.000 C7 0.0229(18) 0.0148(16) 0.0185(18) -0.0013(14) 0.0022(15) -0.0030(14) O8 0.024(2) 0.051(3) 0.032(2) 0.000 0.0037(18) 0.000 C8 0.0235(18) 0.0139(16) 0.0169(17) -0.0029(13) -0.0014(14) 0.0008(14) O9 0.0207(18) 0.0074(15) 0.031(2) 0.000 0.0010(16) 0.000 C9 0.0224(18) 0.0194(18) 0.0219(18) 0.0004(15) -0.0003(15) -0.0035(14) O10 0.0142(16) 0.0171(17) 0.0259(19) 0.000 -0.0028(15) 0.000 C10 0.028(2) 0.0184(18) 0.0187(18) 0.0013(15) -0.0007(15) 0.0008(15) O11 0.029(2) 0.0136(18) 0.030(2) 0.000 0.0015(16) 0.000 C11 0.0226(18) 0.0242(19) 0.0205(18) -0.0007(15) -0.0057(15) 0.0025(15) C12 0.0236(18) 0.0187(17) 0.0146(17) -0.0049(14) -0.0017(14) -0.0017(14) C13 0.0295(19) 0.0109(16) 0.0162(17) -0.0031(13) -0.0019(15) 0.0005(14) C14 0.0219(18) 0.0183(17) 0.0211(18) -0.0033(15) -0.0059(15) -0.0011(14) C15 0.0171(17) 0.0173(17) 0.0240(19) -0.0005(15) -0.0024(15) -0.0024(14) C16 0.0219(18) 0.0179(17) 0.0226(19) 0.0028(15) -0.0032(15) -0.0015(14) C17 0.0163(17) 0.0157(17) 0.0269(19) 0.0010(15) -0.0040(15) -0.0004(14) C18 0.0168(17) 0.0141(16) 0.0247(19) -0.0005(14) -0.0029(14) -0.0016(13) C19 0.0141(16) 0.0137(16) 0.0244(19) 0.0019(14) -0.0012(14) -0.0039(13) C20 0.0164(16) 0.0134(16) 0.0234(19) -0.0009(14) -0.0017(14) -0.0021(13) C21 0.0141(16) 0.0162(16) 0.0208(18) 0.0001(14) -0.0004(14) 0.0020(13) C22 0.0174(16) 0.0112(15) 0.0170(17) 0.0033(13) -0.0022(13) -0.0014(13) C23 0.0181(16) 0.0129(16) 0.0180(17) 0.0005(13) -0.0006(14) 0.0034(13) C24 0.0234(18) 0.0106(15) 0.0192(17) 0.0000(13) -0.0005(14) 0.0016(13) C25 0.0164(16) 0.0133(16) 0.0182(17) 0.0016(13) -0.0021(13) -0.0015(13) C26 0.0166(17) 0.0100(15) 0.0190(17) 0.0032(13) -0.0021(13) 0.0028(12) C27 0.0220(18) 0.0088(15) 0.0175(17) 0.0016(13) -0.0005(14) 0.0021(13) C28 0.0158(16) 0.0114(15) 0.0193(17) 0.0017(13) -0.0031(14) 0.0005(13) C29 0.0240(19) 0.0135(16) 0.0242(19) 0.0011(14) -0.0010(15) -0.0033(14) C30 0.040(2) 0.0144(18) 0.041(3) -0.0043(17) 0.008(2) -0.0022(17) C31 0.030(2) 0.0151(17) 0.030(2) 0.0040(15) -0.0007(17) -0.0036(15) C32 0.032(2) 0.023(2) 0.033(2) 0.0048(17) -0.0074(18) -0.0132(17) C33 0.027(2) 0.0216(19) 0.025(2) 0.0075(16) -0.0026(16) 0.0012(16) C34 0.038(3) 0.037(3) 0.053(3) 0.023(2) 0.006(2) 0.013(2) C35 0.049(3) 0.037(3) 0.028(2) 0.009(2) -0.004(2) -0.004(2) C36 0.040(2) 0.021(2) 0.037(2) 0.0089(18) -0.005(2) -0.0027(18) C37 0.0219(18) 0.0186(18) 0.027(2) 0.0027(15) -0.0023(15) 0.0037(14) C38 0.035(2) 0.0157(19) 0.048(3) -0.0010(18) -0.005(2) 0.0026(17) C39 0.024(2) 0.028(2) 0.042(3) 0.0048(19) 0.0016(18) 0.0096(17) C40 0.036(2) 0.029(2) 0.033(2) 0.0077(18) -0.0033(19) 0.0132(19) C41 0.0235(18) 0.0142(16) 0.0239(19) -0.0049(15) -0.0037(15) 0.0016(14) C42 0.044(3) 0.0172(19) 0.035(2) -0.0019(17) -0.005(2) 0.0053(17) C43 0.032(2) 0.0177(19) 0.052(3) -0.0131(19) -0.009(2) 0.0019(16) C44 0.044(3) 0.023(2) 0.029(2) -0.0101(17) 0.0065(19) 0.0005(18) C45 0.031(2) 0.027(2) 0.034(2) -0.0013(18) 0.0021(18) 0.0009(17) C46 0.032(2) 0.035(2) 0.036(2) 0.006(2) 0.0007(19) -0.0005(19) C47 0.056(3) 0.035(3) 0.064(4) -0.002(3) -0.002(3) 0.007(2) C48 0.029(2) 0.040(3) 0.029(2) 0.0018(19) -0.0042(18) 0.0056(19) C49 0.030(2) 0.024(2) 0.033(2) -0.0005(17) -0.0023(18) 0.0029(16) C50 0.048(3) 0.043(3) 0.042(3) -0.007(2) -0.001(2) 0.002(2) C51 0.044(3) 0.066(4) 0.062(4) -0.019(3) -0.007(3) -0.011(3) C52 0.025(2) 0.028(2) 0.037(2) 0.0034(19) 0.0056(18) 0.0051(17) C53 0.039(3) 0.030(2) 0.066(4) 0.009(2) 0.008(2) -0.007(2) C54 0.058(4) 0.080(5) 0.066(4) -0.034(4) -0.017(3) -0.001(3) C55 0.059(5) 0.056(5) 0.065(5) 0.000 0.022(4) 0.000 C56 0.028(4) 0.064(5) 0.053(5) 0.000 0.003(3) 0.000 _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 O9 2.277(4) . ? Tb1 O4 2.366(2) . ? Tb1 O4 2.366(2) 8_565 ? Tb1 O5 2.371(3) . ? Tb1 O5 2.371(3) 8_565 ? Tb1 O8 2.422(4) . ? Tb1 O10 2.451(3) . ? Tb1 O1 2.526(4) . ? Tb1 Fe1 3.4088(6) . ? Tb1 Fe1 3.4088(6) 8_565 ? Tb1 Tb2 3.9038(4) . ? Fe1 O1 1.8635(13) . ? Fe1 O3 1.932(3) . ? Fe1 O2 1.936(3) . ? Fe1 O4 2.027(3) . ? Fe1 O12 2.027(2) . ? Fe1 Tb2 3.4013(5) . ? O1 Fe1 1.8636(13) 8_565 ? O1 Tb2 2.503(4) . ? O12 C6 1.370(4) . ? O12 Tb2 2.376(2) . ? N1 C46 1.145(6) . ? C1 C2 1.387(5) . ? C1 C6 1.408(5) . ? C1 C28 1.516(5) . ? Tb2 O9 2.295(4) . ? Tb2 O6 2.345(3) . ? Tb2 O6 2.345(3) 8_565 ? Tb2 O12 2.376(2) 8_565 ? Tb2 O7 2.447(5) . ? Tb2 O11 2.485(4) . ? Tb2 Fe1 3.4013(5) 8_565 ? O2 C13 1.359(4) . ? N2 C48 1.124(6) . ? C2 C3 1.404(5) . ? C2 H2 0.9500 . ? O3 C20 1.351(4) . ? N3 C49 1.329(6) . ? N3 C50 1.434(6) . ? N3 C51 1.453(6) . ? C3 C4 1.390(5) . ? C3 C29 1.538(5) . ? O4 C27 1.368(4) . ? N4 C52 1.335(5) . ? N4 C53 1.427(6) . ? N4 C54 1.436(7) . ? C4 C5 1.396(5) . ? C4 H4 0.9500 . ? O5 C49 1.222(5) . ? C5 C6 1.416(5) . ? C5 C7 1.526(5) . ? O6 C52 1.203(5) . ? O7 C55 1.425(10) . ? C7 C8 1.516(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? O8 C56 1.416(9) . ? C8 C13 1.403(5) . ? C8 C9 1.404(5) . ? C9 C10 1.397(5) . ? C9 H9 0.9500 . ? C10 C11 1.387(5) . ? C10 C33 1.538(5) . ? C11 C12 1.396(5) . ? C11 H11 0.9500 . ? C12 C13 1.399(5) . ? C12 C14 1.521(5) . ? C14 C15 1.518(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.403(5) . ? C15 C20 1.403(5) . ? C16 C17 1.390(5) . ? C16 H16 0.9500 . ? C17 C18 1.404(5) . ? C17 C37 1.534(5) . ? C18 C19 1.390(5) . ? C18 H18 0.9500 . ? C19 C20 1.406(5) . ? C19 C21 1.521(5) . ? C21 C22 1.524(5) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.394(5) . ? C22 C27 1.402(5) . ? C23 C24 1.393(5) . ? C23 H23 0.9500 . ? C24 C25 1.393(5) . ? C24 C41 1.538(5) . ? C25 C26 1.402(5) . ? C25 H25 0.9500 . ? C26 C27 1.400(5) . ? C26 C28 1.515(5) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C31 1.531(5) . ? C29 C32 1.537(5) . ? C29 C30 1.540(6) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C36 1.527(6) . ? C33 C35 1.529(6) . ? C33 C34 1.543(6) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C40 1.524(6) . ? C37 C38 1.533(6) . ? C37 C39 1.534(6) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C44 1.534(6) . ? C41 C43 1.534(5) . ? C41 C42 1.537(6) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C46 1.452(6) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C47 C48 1.450(7) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C49 H49 0.9500 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52 0.9500 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 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 O9 Tb1 O4 89.17(7) . . ? O9 Tb1 O4 89.17(7) . 8_565 ? O4 Tb1 O4 133.27(12) . 8_565 ? O9 Tb1 O5 84.69(10) . . ? O4 Tb1 O5 75.57(9) . . ? O4 Tb1 O5 150.50(9) 8_565 . ? O9 Tb1 O5 84.69(10) . 8_565 ? O4 Tb1 O5 150.51(9) . 8_565 ? O4 Tb1 O5 75.57(9) 8_565 8_565 ? O5 Tb1 O5 75.15(13) . 8_565 ? O9 Tb1 O8 153.41(14) . . ? O4 Tb1 O8 100.98(7) . . ? O4 Tb1 O8 100.98(7) 8_565 . ? O5 Tb1 O8 74.36(10) . . ? O5 Tb1 O8 74.36(10) 8_565 . ? O9 Tb1 O10 140.40(13) . . ? O4 Tb1 O10 76.03(6) . . ? O4 Tb1 O10 76.03(6) 8_565 . ? O5 Tb1 O10 124.96(9) . . ? O5 Tb1 O10 124.97(9) 8_565 . ? O8 Tb1 O10 66.20(14) . . ? O9 Tb1 O1 70.39(13) . . ? O4 Tb1 O1 67.78(6) . . ? O4 Tb1 O1 67.78(6) 8_565 . ? O5 Tb1 O1 135.27(8) . . ? O5 Tb1 O1 135.27(8) 8_565 . ? O8 Tb1 O1 136.20(13) . . ? O10 Tb1 O1 70.01(12) . . ? O9 Tb1 Fe1 80.81(8) . . ? O4 Tb1 Fe1 35.64(6) . . ? O4 Tb1 Fe1 98.24(6) 8_565 . ? O5 Tb1 Fe1 109.14(6) . . ? O5 Tb1 Fe1 164.35(7) 8_565 . ? O8 Tb1 Fe1 121.21(8) . . ? O10 Tb1 Fe1 65.69(7) . . ? O1 Tb1 Fe1 32.48(2) . . ? O9 Tb1 Fe1 80.81(8) . 8_565 ? O4 Tb1 Fe1 98.24(6) . 8_565 ? O4 Tb1 Fe1 35.64(6) 8_565 8_565 ? O5 Tb1 Fe1 164.35(7) . 8_565 ? O5 Tb1 Fe1 109.14(6) 8_565 8_565 ? O8 Tb1 Fe1 121.21(8) . 8_565 ? O10 Tb1 Fe1 65.70(7) . 8_565 ? O1 Tb1 Fe1 32.48(2) . 8_565 ? Fe1 Tb1 Fe1 62.763(17) . 8_565 ? O9 Tb1 Tb2 31.52(10) . . ? O4 Tb1 Tb2 77.32(6) . . ? O4 Tb1 Tb2 77.32(6) 8_565 . ? O5 Tb1 Tb2 109.43(7) . . ? O5 Tb1 Tb2 109.43(7) 8_565 . ? O8 Tb1 Tb2 175.08(11) . . ? O10 Tb1 Tb2 108.88(9) . . ? O1 Tb1 Tb2 38.87(8) . . ? Fe1 Tb1 Tb2 54.933(10) . . ? Fe1 Tb1 Tb2 54.933(10) 8_565 . ? O1 Fe1 O3 107.64(13) . . ? O1 Fe1 O2 107.50(14) . . ? O3 Fe1 O2 92.36(11) . . ? O1 Fe1 O4 89.08(14) . . ? O3 Fe1 O4 86.80(10) . . ? O2 Fe1 O4 162.78(10) . . ? O1 Fe1 O12 88.92(13) . . ? O3 Fe1 O12 162.90(11) . . ? O2 Fe1 O12 86.48(11) . . ? O4 Fe1 O12 89.29(10) . . ? O1 Fe1 Tb2 46.19(11) . . ? O3 Fe1 Tb2 153.66(8) . . ? O2 Fe1 Tb2 93.74(8) . . ? O4 Fe1 Tb2 94.60(7) . . ? O12 Fe1 Tb2 43.31(7) . . ? O1 Fe1 Tb1 46.71(12) . . ? O3 Fe1 Tb1 94.38(8) . . ? O2 Fe1 Tb1 154.12(8) . . ? O4 Fe1 Tb1 42.86(7) . . ? O12 Fe1 Tb1 94.04(7) . . ? Tb2 Fe1 Tb1 69.953(11) . . ? Fe1 O1 Fe1 144.6(2) . 8_565 ? Fe1 O1 Tb2 101.31(11) . . ? Fe1 O1 Tb2 101.31(11) 8_565 . ? Fe1 O1 Tb1 100.81(12) . . ? Fe1 O1 Tb1 100.82(12) 8_565 . ? Tb2 O1 Tb1 101.83(13) . . ? C6 O12 Fe1 124.1(2) . . ? C6 O12 Tb2 135.0(2) . . ? Fe1 O12 Tb2 100.86(10) . . ? C2 C1 C6 120.0(3) . . ? C2 C1 C28 118.8(3) . . ? C6 C1 C28 121.0(3) . . ? O9 Tb2 O6 86.11(11) . . ? O9 Tb2 O6 86.11(11) . 8_565 ? O6 Tb2 O6 76.58(14) . 8_565 ? O9 Tb2 O12 88.41(7) . . ? O6 Tb2 O12 74.43(9) . . ? O6 Tb2 O12 150.78(9) 8_565 . ? O9 Tb2 O12 88.41(7) . 8_565 ? O6 Tb2 O12 150.78(9) . 8_565 ? O6 Tb2 O12 74.43(9) 8_565 8_565 ? O12 Tb2 O12 134.11(12) . 8_565 ? O9 Tb2 O7 152.92(15) . . ? O6 Tb2 O7 72.81(12) . . ? O6 Tb2 O7 72.81(12) 8_565 . ? O12 Tb2 O7 101.64(7) . . ? O12 Tb2 O7 101.64(7) 8_565 . ? O9 Tb2 O11 141.40(13) . . ? O6 Tb2 O11 122.74(10) . . ? O6 Tb2 O11 122.74(10) 8_565 . ? O12 Tb2 O11 77.24(7) . . ? O12 Tb2 O11 77.24(7) 8_565 . ? O7 Tb2 O11 65.68(15) . . ? O9 Tb2 O1 70.54(13) . . ? O6 Tb2 O1 135.62(8) . . ? O6 Tb2 O1 135.62(8) 8_565 . ? O12 Tb2 O1 67.92(6) . . ? O12 Tb2 O1 67.92(6) 8_565 . ? O7 Tb2 O1 136.54(15) . . ? O11 Tb2 O1 70.86(13) . . ? O9 Tb2 Fe1 80.75(8) . . ? O6 Tb2 Fe1 108.71(7) . . ? O6 Tb2 Fe1 165.36(8) 8_565 . ? O12 Tb2 Fe1 35.83(6) . . ? O12 Tb2 Fe1 98.65(6) 8_565 . ? O7 Tb2 Fe1 121.64(9) . . ? O11 Tb2 Fe1 66.61(7) . . ? O1 Tb2 Fe1 32.49(2) . . ? O9 Tb2 Fe1 80.75(8) . 8_565 ? O6 Tb2 Fe1 165.36(8) . 8_565 ? O6 Tb2 Fe1 108.71(7) 8_565 8_565 ? O12 Tb2 Fe1 98.65(6) . 8_565 ? O12 Tb2 Fe1 35.82(6) 8_565 8_565 ? O7 Tb2 Fe1 121.64(9) . 8_565 ? O11 Tb2 Fe1 66.61(7) . 8_565 ? O1 Tb2 Fe1 32.50(2) . 8_565 ? Fe1 Tb2 Fe1 62.917(17) . 8_565 ? O9 Tb2 Tb1 31.24(9) . . ? O6 Tb2 Tb1 110.34(8) . . ? O6 Tb2 Tb1 110.34(8) 8_565 . ? O12 Tb2 Tb1 76.97(6) . . ? O12 Tb2 Tb1 76.97(6) 8_565 . ? O7 Tb2 Tb1 175.84(12) . . ? O11 Tb2 Tb1 110.16(9) . . ? O1 Tb2 Tb1 39.29(9) . . ? Fe1 Tb2 Tb1 55.113(10) . . ? Fe1 Tb2 Tb1 55.115(10) 8_565 . ? C13 O2 Fe1 130.3(2) . . ? C1 C2 C3 122.3(3) . . ? C1 C2 H2 118.8 . . ? C3 C2 H2 118.8 . . ? C20 O3 Fe1 130.6(2) . . ? C49 N3 C50 122.2(4) . . ? C49 N3 C51 119.5(4) . . ? C50 N3 C51 118.2(4) . . ? C4 C3 C2 117.0(3) . . ? C4 C3 C29 124.1(3) . . ? C2 C3 C29 118.9(3) . . ? C27 O4 Fe1 126.7(2) . . ? C27 O4 Tb1 131.8(2) . . ? Fe1 O4 Tb1 101.50(10) . . ? C52 N4 C53 121.0(4) . . ? C52 N4 C54 120.4(5) . . ? C53 N4 C54 118.3(5) . . ? C3 C4 C5 122.6(3) . . ? C3 C4 H4 118.7 . . ? C5 C4 H4 118.7 . . ? C49 O5 Tb1 134.4(3) . . ? C4 C5 C6 119.5(3) . . ? C4 C5 C7 119.1(3) . . ? C6 C5 C7 121.4(3) . . ? C52 O6 Tb2 147.3(3) . . ? O12 C6 C1 120.4(3) . . ? O12 C6 C5 121.0(3) . . ? C1 C6 C5 118.6(3) . . ? C55 O7 Tb2 130.8(5) . . ? C8 C7 C5 110.9(3) . . ? C8 C7 H7A 109.5 . . ? C5 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 108.0 . . ? C56 O8 Tb1 129.8(4) . . ? C13 C8 C9 119.1(3) . . ? C13 C8 C7 121.6(3) . . ? C9 C8 C7 119.1(3) . . ? Tb1 O9 Tb2 117.24(16) . . ? C10 C9 C8 122.1(3) . . ? C10 C9 H9 118.9 . . ? C8 C9 H9 118.9 . . ? C11 C10 C9 117.1(3) . . ? C11 C10 C33 121.9(3) . . ? C9 C10 C33 121.0(3) . . ? C10 C11 C12 122.7(4) . . ? C10 C11 H11 118.7 . . ? C12 C11 H11 118.7 . . ? C11 C12 C13 119.2(3) . . ? C11 C12 C14 119.1(3) . . ? C13 C12 C14 121.4(3) . . ? O2 C13 C12 120.0(3) . . ? O2 C13 C8 120.2(3) . . ? C12 C13 C8 119.8(3) . . ? C15 C14 C12 109.4(3) . . ? C15 C14 H14A 109.8 . . ? C12 C14 H14A 109.8 . . ? C15 C14 H14B 109.8 . . ? C12 C14 H14B 109.8 . . ? H14A C14 H14B 108.2 . . ? C16 C15 C20 119.3(3) . . ? C16 C15 C14 119.7(3) . . ? C20 C15 C14 120.9(3) . . ? C17 C16 C15 122.3(4) . . ? C17 C16 H16 118.8 . . ? C15 C16 H16 118.8 . . ? C16 C17 C18 117.0(3) . . ? C16 C17 C37 123.5(3) . . ? C18 C17 C37 119.5(3) . . ? C19 C18 C17 122.5(3) . . ? C19 C18 H18 118.7 . . ? C17 C18 H18 118.7 . . ? C18 C19 C20 119.3(3) . . ? C18 C19 C21 118.9(3) . . ? C20 C19 C21 121.6(3) . . ? O3 C20 C15 120.0(3) . . ? O3 C20 C19 120.5(3) . . ? C15 C20 C19 119.5(3) . . ? C19 C21 C22 110.8(3) . . ? C19 C21 H21A 109.5 . . ? C22 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 108.1 . . ? C23 C22 C27 119.1(3) . . ? C23 C22 C21 118.3(3) . . ? C27 C22 C21 122.5(3) . . ? C24 C23 C22 122.5(3) . . ? C24 C23 H23 118.8 . . ? C22 C23 H23 118.8 . . ? C25 C24 C23 117.4(3) . . ? C25 C24 C41 123.0(3) . . ? C23 C24 C41 119.6(3) . . ? C24 C25 C26 121.9(3) . . ? C24 C25 H25 119.1 . . ? C26 C25 H25 119.1 . . ? C27 C26 C25 119.4(3) . . ? C27 C26 C28 121.1(3) . . ? C25 C26 C28 119.4(3) . . ? O4 C27 C26 119.2(3) . . ? O4 C27 C22 121.1(3) . . ? C26 C27 C22 119.7(3) . . ? C26 C28 C1 108.7(3) . . ? C26 C28 H28A 109.9 . . ? C1 C28 H28A 109.9 . . ? C26 C28 H28B 109.9 . . ? C1 C28 H28B 109.9 . . ? H28A C28 H28B 108.3 . . ? C31 C29 C32 109.7(3) . . ? C31 C29 C3 111.7(3) . . ? C32 C29 C3 109.6(3) . . ? C31 C29 C30 107.9(3) . . ? C32 C29 C30 108.7(3) . . ? C3 C29 C30 109.2(3) . . ? 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 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C36 C33 C35 109.5(4) . . ? C36 C33 C10 111.9(3) . . ? C35 C33 C10 109.0(3) . . ? C36 C33 C34 107.9(4) . . ? C35 C33 C34 108.1(4) . . ? C10 C33 C34 110.4(3) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C40 C37 C38 108.0(3) . . ? C40 C37 C39 109.4(3) . . ? C38 C37 C39 108.7(4) . . ? C40 C37 C17 111.9(3) . . ? C38 C37 C17 109.6(3) . . ? C39 C37 C17 109.2(3) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C44 C41 C43 108.5(3) . . ? C44 C41 C42 109.4(3) . . ? C43 C41 C42 107.9(3) . . ? C44 C41 C24 109.7(3) . . ? C43 C41 C24 112.3(3) . . ? C42 C41 C24 109.0(3) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C46 C45 H45A 109.5 . . ? C46 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C46 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N1 C46 C45 179.3(6) . . ? C48 C47 H47A 109.5 . . ? C48 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C48 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? N2 C48 C47 179.2(6) . . ? O5 C49 N3 124.0(4) . . ? O5 C49 H49 118.0 . . ? N3 C49 H49 118.0 . . ? N3 C50 H50A 109.5 . . ? N3 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? N3 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? N3 C51 H51A 109.5 . . ? N3 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? N3 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? O6 C52 N4 124.2(4) . . ? O6 C52 H52 117.9 . . ? N4 C52 H52 117.9 . . ? N4 C53 H53A 109.5 . . ? N4 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? N4 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N4 C54 H54A 109.5 . . ? N4 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? N4 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? O7 C55 H55A 109.5 . . ? O7 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? O7 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? O8 C56 H56A 109.5 . . ? O8 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? O8 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.18 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.526 _refine_diff_density_min -1.234 _refine_diff_density_rms 0.226 # Attachment '- 3.CIF' data_S124 _database_code_depnum_ccdc_archive 'CCDC 827079' #TrackingRef '- 3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common S124 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C110 H157 Cl Dy2 Fe2 N8 O18' _chemical_formula_weight 2351.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 19.5864(13) _cell_length_b 38.560(2) _cell_length_c 15.7383(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11886.3(13) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9779. _cell_measurement_theta_min 2.45. _cell_measurement_theta_max 26.06. _exptl_crystal_description Block _exptl_crystal_colour Brown _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.314 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4872 _exptl_absorpt_coefficient_mu 1.567 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6100 _exptl_absorpt_correction_T_max 0.6954 _exptl_absorpt_process_details Bruker-SADABS _exptl_special_details ; Data were corrected for decay and absorption using the program SADABS based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995). ; _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 'Bruker Apex II CCD Diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 186494 _diffrn_reflns_av_R_equivalents 0.0656 _diffrn_reflns_av_sigmaI/netI 0.0321 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -48 _diffrn_reflns_limit_k_max 48 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 26.48 _reflns_number_total 12378 _reflns_number_gt 10370 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex II' _computing_cell_refinement 'SAINT (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed (Barbour, 2001)' _computing_publication_material 'local program' _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. Crystals were weakly diffracting. The routine SQUEEZE was applied to the data in order to remove diffuse electron density. It was not possible to model the disorder associated with this density. Unit cell contents do not match reported formulae due to hydrogen atoms on water, methanol and OH ligands. ; _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^)+(0.0471P)^2^+57.7003P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12378 _refine_ls_number_parameters 672 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0635 _refine_ls_R_factor_gt 0.0507 _refine_ls_wR_factor_ref 0.1218 _refine_ls_wR_factor_gt 0.1168 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.112 _refine_ls_shift/su_max 0.007 _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 Dy1 Dy 0.291261(15) 0.2500 0.343966(19) 0.01641(8) Uani 1 2 d S . . Cl1 Cl 0.54496(9) 0.2500 0.25941(12) 0.0336(4) Uani 1 2 d S . . O1 O 0.30085(16) 0.19363(8) 0.4019(2) 0.0173(6) Uani 1 1 d . . . N1 N 0.1958(2) 0.17728(12) 0.1483(3) 0.0328(10) Uani 1 1 d . . . C1 C 0.3690(2) 0.14678(11) 0.3463(3) 0.0156(9) Uani 1 1 d . . . Dy2 Dy 0.151350(16) 0.2500 0.51939(2) 0.01801(9) Uani 1 2 d S . . O2 O 0.19711(15) 0.19357(8) 0.52903(19) 0.0161(6) Uani 1 1 d . . . N2 N -0.0102(2) 0.17120(12) 0.4395(3) 0.0314(10) Uani 1 1 d . . . C2 C 0.3714(2) 0.11434(11) 0.3085(3) 0.0180(9) Uani 1 1 d . . . H2 H 0.4147 0.1043 0.2969 0.022 Uiso 1 1 calc R . . Fe3 Fe 0.29890(3) 0.204038(15) 0.52808(4) 0.01482(14) Uani 1 1 d . . . O3 O 0.29554(16) 0.19886(8) 0.6503(2) 0.0195(7) Uani 1 1 d . . . N3 N 0.0608(3) 0.08702(14) 0.2389(3) 0.0405(12) Uani 1 1 d . . . C3 C 0.3128(2) 0.09573(11) 0.2870(3) 0.0175(9) Uani 1 1 d . . . O4 O 0.39752(18) 0.19933(8) 0.5261(2) 0.0243(7) Uani 1 1 d . . . N4 N 0.3340(3) 0.03107(16) 0.5928(4) 0.0610(17) Uani 1 1 d . . . C4 C 0.2504(2) 0.11128(11) 0.3054(3) 0.0164(9) Uani 1 1 d . . . H4 H 0.2095 0.0994 0.2913 0.020 Uiso 1 1 calc R . . O5 O 0.25813(18) 0.21276(8) 0.2324(2) 0.0247(7) Uani 1 1 d . . . C5 C 0.2460(2) 0.14381(11) 0.3440(3) 0.0149(9) Uani 1 1 d . . . O6 O 0.06285(18) 0.21259(9) 0.4826(3) 0.0346(9) Uani 1 1 d . . . C6 C 0.3053(2) 0.16188(11) 0.3648(3) 0.0165(9) Uani 1 1 d . . . O7 O 0.3850(3) 0.2500 0.2444(3) 0.0363(13) Uani 1 2 d S . . C7 C 0.1768(2) 0.15783(11) 0.3703(3) 0.0171(9) Uani 1 1 d . . . H7A H 0.1787 0.1834 0.3744 0.021 Uiso 1 1 calc R . . H7B H 0.1421 0.1516 0.3272 0.021 Uiso 1 1 calc R . . O8 O 0.0708(3) 0.2500 0.6365(4) 0.0451(15) Uani 1 2 d S . . C8 C 0.1573(2) 0.14254(11) 0.4558(3) 0.0160(9) Uani 1 1 d . . . O9 O 0.1787(2) 0.2500 0.3765(3) 0.0207(10) Uani 1 2 d S . . C9 C 0.1308(2) 0.10907(11) 0.4590(3) 0.0172(9) Uani 1 1 d . . . H9 H 0.1207 0.0975 0.4072 0.021 Uiso 1 1 calc R . . O10 O 0.2794(2) 0.2500 0.5019(3) 0.0257(11) Uani 1 2 d S . . C10 C 0.1183(2) 0.09177(11) 0.5356(3) 0.0188(9) Uani 1 1 d . . . O11 O 0.4037(2) 0.2500 0.4111(3) 0.0180(9) Uani 1 2 d S . . C11 C 0.1316(2) 0.11003(12) 0.6096(3) 0.0185(9) Uani 1 1 d . . . H11 H 0.1231 0.0990 0.6626 0.022 Uiso 1 1 calc R . . O12 O 0.2040(3) 0.2500 0.6615(3) 0.0274(11) Uani 1 2 d S . . C12 C 0.1570(2) 0.14395(11) 0.6098(3) 0.0165(9) Uani 1 1 d . . . C13 C 0.1705(2) 0.16047(11) 0.5320(3) 0.0167(9) Uani 1 1 d . . . C14 C 0.1737(2) 0.16129(11) 0.6946(3) 0.0182(9) Uani 1 1 d . . . H14A H 0.1711 0.1868 0.6881 0.022 Uiso 1 1 calc R . . H14B H 0.1394 0.1542 0.7376 0.022 Uiso 1 1 calc R . . C15 C 0.2443(2) 0.15133(11) 0.7251(3) 0.0166(9) Uani 1 1 d . . . C16 C 0.2529(3) 0.12129(12) 0.7742(3) 0.0225(10) Uani 1 1 d . . . H16 H 0.2136 0.1087 0.7915 0.027 Uiso 1 1 calc R . . C17 C 0.3171(2) 0.10926(12) 0.7985(3) 0.0206(10) Uani 1 1 d . . . C18 C 0.3730(3) 0.12923(13) 0.7748(3) 0.0232(10) Uani 1 1 d . . . H18 H 0.4172 0.1222 0.7930 0.028 Uiso 1 1 calc R . . C19 C 0.3669(2) 0.15901(12) 0.7256(3) 0.0177(9) Uani 1 1 d . . . C20 C 0.3022(2) 0.17013(11) 0.7001(3) 0.0185(9) Uani 1 1 d . . . C21 C 0.4313(2) 0.17673(12) 0.6937(3) 0.0216(10) Uani 1 1 d . . . H21A H 0.4215 0.2014 0.6815 0.026 Uiso 1 1 calc R . . H21B H 0.4671 0.1757 0.7381 0.026 Uiso 1 1 calc R . . C22 C 0.4567(2) 0.15903(12) 0.6139(3) 0.0196(10) Uani 1 1 d . . . C23 C 0.4956(2) 0.12880(12) 0.6202(3) 0.0220(10) Uani 1 1 d . . . H23 H 0.5089 0.1209 0.6749 0.026 Uiso 1 1 calc R . . C24 C 0.5157(2) 0.10978(12) 0.5495(3) 0.0192(9) Uani 1 1 d . . . C25 C 0.4966(2) 0.12270(12) 0.4704(3) 0.0205(10) Uani 1 1 d . . . H25 H 0.5105 0.1105 0.4209 0.025 Uiso 1 1 calc R . . C26 C 0.4582(2) 0.15275(12) 0.4608(3) 0.0175(9) Uani 1 1 d . . . C27 C 0.4369(2) 0.17087(11) 0.5332(3) 0.0174(9) Uani 1 1 d . . . C28 C 0.4363(2) 0.16382(11) 0.3715(3) 0.0185(9) Uani 1 1 d . . . H28A H 0.4310 0.1894 0.3698 0.022 Uiso 1 1 calc R . . H28B H 0.4721 0.1573 0.3302 0.022 Uiso 1 1 calc R . . C29 C 0.3190(2) 0.05969(12) 0.2458(3) 0.0209(10) Uani 1 1 d . . . C30 C 0.3489(3) 0.03438(13) 0.3113(4) 0.0331(12) Uani 1 1 d . . . H30A H 0.3938 0.0427 0.3298 0.050 Uiso 1 1 calc R . . H30B H 0.3537 0.0114 0.2854 0.050 Uiso 1 1 calc R . . H30C H 0.3183 0.0329 0.3604 0.050 Uiso 1 1 calc R . . C31 C 0.2505(3) 0.04548(13) 0.2161(4) 0.0346(13) Uani 1 1 d . . . H31A H 0.2572 0.0226 0.1904 0.052 Uiso 1 1 calc R . . H31B H 0.2307 0.0613 0.1740 0.052 Uiso 1 1 calc R . . H31C H 0.2196 0.0434 0.2648 0.052 Uiso 1 1 calc R . . C32 C 0.3670(3) 0.06155(14) 0.1687(3) 0.0343(13) Uani 1 1 d . . . H32A H 0.4132 0.0675 0.1877 0.051 Uiso 1 1 calc R . . H32B H 0.3506 0.0794 0.1292 0.051 Uiso 1 1 calc R . . H32C H 0.3678 0.0390 0.1399 0.051 Uiso 1 1 calc R . . C33 C 0.0920(2) 0.05412(12) 0.5334(3) 0.0204(10) Uani 1 1 d . . . C34 C 0.0798(3) 0.03982(12) 0.6222(3) 0.0253(11) Uani 1 1 d . . . H34A H 0.1230 0.0394 0.6536 0.038 Uiso 1 1 calc R . . H34B H 0.0616 0.0162 0.6181 0.038 Uiso 1 1 calc R . . H34C H 0.0470 0.0546 0.6521 0.038 Uiso 1 1 calc R . . C35 C 0.0254(3) 0.05273(14) 0.4822(3) 0.0300(12) Uani 1 1 d . . . H35A H 0.0090 0.0288 0.4797 0.045 Uiso 1 1 calc R . . H35B H 0.0338 0.0612 0.4244 0.045 Uiso 1 1 calc R . . H35C H -0.0091 0.0673 0.5097 0.045 Uiso 1 1 calc R . . C36 C 0.1454(3) 0.03121(13) 0.4891(4) 0.0332(12) Uani 1 1 d . . . H36A H 0.1888 0.0327 0.5199 0.050 Uiso 1 1 calc R . . H36B H 0.1519 0.0392 0.4306 0.050 Uiso 1 1 calc R . . H36C H 0.1295 0.0071 0.4887 0.050 Uiso 1 1 calc R . . C37 C 0.3245(3) 0.07569(13) 0.8506(3) 0.0256(11) Uani 1 1 d . . . C38 C 0.3949(3) 0.05940(16) 0.8347(4) 0.0426(15) Uani 1 1 d . . . H38A H 0.4305 0.0749 0.8563 0.064 Uiso 1 1 calc R . . H38B H 0.4014 0.0559 0.7736 0.064 Uiso 1 1 calc R . . H38C H 0.3977 0.0370 0.8640 0.064 Uiso 1 1 calc R . . C39 C 0.3190(3) 0.08434(15) 0.9447(3) 0.0371(13) Uani 1 1 d . . . H39A H 0.2744 0.0949 0.9562 0.056 Uiso 1 1 calc R . . H39B H 0.3552 0.1007 0.9604 0.056 Uiso 1 1 calc R . . H39C H 0.3237 0.0631 0.9782 0.056 Uiso 1 1 calc R . . C40 C 0.2708(3) 0.04894(14) 0.8272(4) 0.0335(13) Uani 1 1 d . . . H40A H 0.2797 0.0274 0.8582 0.050 Uiso 1 1 calc R . . H40B H 0.2726 0.0445 0.7660 0.050 Uiso 1 1 calc R . . H40C H 0.2255 0.0577 0.8424 0.050 Uiso 1 1 calc R . . C41 C 0.5565(2) 0.07565(13) 0.5549(3) 0.0236(10) Uani 1 1 d . . . C42 C 0.5170(3) 0.04656(13) 0.5104(4) 0.0342(13) Uani 1 1 d . . . H42A H 0.5437 0.0251 0.5126 0.051 Uiso 1 1 calc R . . H42B H 0.5089 0.0530 0.4510 0.051 Uiso 1 1 calc R . . H42C H 0.4732 0.0430 0.5392 0.051 Uiso 1 1 calc R . . C43 C 0.6251(3) 0.08070(14) 0.5101(4) 0.0314(12) Uani 1 1 d . . . H43A H 0.6510 0.0990 0.5388 0.047 Uiso 1 1 calc R . . H43B H 0.6173 0.0873 0.4507 0.047 Uiso 1 1 calc R . . H43C H 0.6511 0.0590 0.5120 0.047 Uiso 1 1 calc R . . C44 C 0.5688(3) 0.06475(15) 0.6464(3) 0.0350(13) Uani 1 1 d . . . H44A H 0.5949 0.0828 0.6757 0.052 Uiso 1 1 calc R . . H44B H 0.5946 0.0430 0.6473 0.052 Uiso 1 1 calc R . . H44C H 0.5249 0.0614 0.6751 0.052 Uiso 1 1 calc R . . C45 C 0.2032(3) 0.20328(13) 0.2036(4) 0.0304(12) Uani 1 1 d . . . H45 H 0.1633 0.2152 0.2217 0.036 Uiso 1 1 calc R . . C46 C 0.1278(4) 0.1668(2) 0.1217(5) 0.062(2) Uani 1 1 d . . . H46A H 0.0941 0.1829 0.1454 0.093 Uiso 1 1 calc R . . H46B H 0.1184 0.1433 0.1422 0.093 Uiso 1 1 calc R . . H46C H 0.1251 0.1672 0.0595 0.093 Uiso 1 1 calc R . . C47 C 0.2534(3) 0.15774(17) 0.1175(4) 0.0468(16) Uani 1 1 d . . . H47A H 0.2609 0.1631 0.0574 0.070 Uiso 1 1 calc R . . H47B H 0.2442 0.1329 0.1240 0.070 Uiso 1 1 calc R . . H47C H 0.2942 0.1640 0.1502 0.070 Uiso 1 1 calc R . . C48 C 0.0323(3) 0.19726(14) 0.4265(4) 0.0327(12) Uani 1 1 d . . . H48 H 0.0395 0.2046 0.3696 0.039 Uiso 1 1 calc R . . C49 C -0.0221(3) 0.15759(16) 0.5237(4) 0.0461(16) Uani 1 1 d . . . H49A H 0.0027 0.1717 0.5654 0.069 Uiso 1 1 calc R . . H49B H -0.0060 0.1336 0.5265 0.069 Uiso 1 1 calc R . . H49C H -0.0711 0.1583 0.5363 0.069 Uiso 1 1 calc R . . C50 C -0.0397(4) 0.1534(2) 0.3685(5) 0.070(2) Uani 1 1 d . . . H50A H -0.0311 0.1666 0.3164 0.105 Uiso 1 1 calc R . . H50B H -0.0890 0.1510 0.3772 0.105 Uiso 1 1 calc R . . H50C H -0.0191 0.1303 0.3634 0.105 Uiso 1 1 calc R . . C51 C 0.3848(5) 0.2500 0.1536(6) 0.049(2) Uani 1 2 d S . . H51A H 0.3817 0.2261 0.1328 0.074 Uiso 0.50 1 calc PR . . H51B H 0.4271 0.2606 0.1327 0.074 Uiso 0.50 1 calc PR . . H51C H 0.3455 0.2633 0.1329 0.074 Uiso 0.50 1 calc PR . . C52 C -0.0026(6) 0.2500 0.6361(8) 0.070(3) Uani 1 2 d S . . H52A H -0.0191 0.2606 0.5834 0.105 Uiso 0.50 1 calc PR . . H52B H -0.0195 0.2633 0.6848 0.105 Uiso 0.50 1 calc PR . . H52C H -0.0193 0.2261 0.6399 0.105 Uiso 0.50 1 calc PR . . C53 C 0.0614(4) 0.02054(16) 0.2188(5) 0.0536(18) Uani 1 1 d . . . H53A H 0.0731 0.0095 0.2729 0.080 Uiso 1 1 calc R . . H53B H 0.0951 0.0140 0.1756 0.080 Uiso 1 1 calc R . . H53C H 0.0160 0.0129 0.2007 0.080 Uiso 1 1 calc R . . C54 C 0.0616(3) 0.05826(16) 0.2294(3) 0.0346(13) Uani 1 1 d . . . C55 C 0.3182(3) 0.09474(14) 0.5440(4) 0.0306(12) Uani 1 1 d . . . H55A H 0.3543 0.1091 0.5688 0.046 Uiso 1 1 calc R . . H55B H 0.2736 0.1034 0.5628 0.046 Uiso 1 1 calc R . . H55C H 0.3208 0.0959 0.4819 0.046 Uiso 1 1 calc R . . C56 C 0.3266(3) 0.05927(15) 0.5714(4) 0.0341(13) 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 Dy1 0.01593(15) 0.01136(14) 0.02193(16) 0.000 -0.00137(12) 0.000 Cl1 0.0236(9) 0.0416(10) 0.0356(10) 0.000 0.0026(8) 0.000 O1 0.0198(17) 0.0100(14) 0.0220(16) -0.0018(12) -0.0012(13) 0.0001(12) N1 0.029(2) 0.030(2) 0.039(3) -0.009(2) -0.003(2) -0.0074(19) C1 0.015(2) 0.013(2) 0.018(2) 0.0044(17) -0.0032(17) -0.0023(17) Dy2 0.01666(16) 0.01069(14) 0.02669(17) 0.000 0.00154(12) 0.000 O2 0.0129(15) 0.0147(15) 0.0207(16) -0.0014(12) 0.0006(12) -0.0094(12) N2 0.021(2) 0.028(2) 0.045(3) -0.005(2) -0.003(2) -0.0029(19) C2 0.020(2) 0.016(2) 0.018(2) 0.0024(17) -0.0006(18) 0.0073(18) Fe3 0.0172(3) 0.0076(3) 0.0197(3) 0.0002(2) -0.0009(3) 0.0004(2) O3 0.0213(17) 0.0138(15) 0.0233(17) -0.0005(13) -0.0026(14) -0.0011(13) N3 0.046(3) 0.040(3) 0.036(3) -0.004(2) -0.005(2) 0.005(2) C3 0.021(2) 0.013(2) 0.018(2) -0.0009(17) -0.0005(18) -0.0005(18) O4 0.0324(19) 0.0186(17) 0.0217(17) 0.0015(13) -0.0012(15) -0.0004(14) N4 0.056(4) 0.045(3) 0.081(5) 0.023(3) -0.001(3) 0.003(3) C4 0.017(2) 0.013(2) 0.019(2) 0.0032(17) -0.0024(18) 0.0000(17) O5 0.0246(19) 0.0205(16) 0.0289(19) -0.0009(14) -0.0046(15) -0.0063(15) C5 0.015(2) 0.0101(19) 0.020(2) 0.0009(17) -0.0009(17) 0.0031(16) O6 0.0211(19) 0.0224(18) 0.060(3) -0.0094(18) -0.0015(18) -0.0026(15) C6 0.021(2) 0.011(2) 0.018(2) 0.0021(16) 0.0019(18) 0.0014(17) O7 0.032(3) 0.050(3) 0.027(3) 0.000 0.002(2) 0.000 C7 0.018(2) 0.013(2) 0.020(2) 0.0001(17) -0.0063(18) -0.0017(18) O8 0.020(3) 0.067(4) 0.048(4) 0.000 0.008(3) 0.000 C8 0.014(2) 0.013(2) 0.021(2) 0.0002(17) -0.0001(17) 0.0051(17) O9 0.018(2) 0.0032(19) 0.041(3) 0.000 0.000(2) 0.000 C9 0.014(2) 0.015(2) 0.023(2) -0.0011(17) -0.0023(18) -0.0003(17) O10 0.021(3) 0.024(3) 0.032(3) 0.000 0.019(2) 0.000 C10 0.014(2) 0.014(2) 0.028(3) 0.0022(18) 0.0022(18) 0.0025(17) O11 0.012(2) 0.018(2) 0.024(2) 0.000 -0.0029(18) 0.000 C11 0.014(2) 0.019(2) 0.022(2) 0.0045(18) 0.0030(18) 0.0030(18) O12 0.037(3) 0.015(2) 0.030(3) 0.000 0.000(2) 0.000 C12 0.013(2) 0.015(2) 0.022(2) -0.0019(17) -0.0013(17) 0.0023(17) C13 0.015(2) 0.0088(19) 0.026(2) 0.0007(17) 0.0028(18) 0.0024(17) C14 0.022(2) 0.015(2) 0.017(2) 0.0004(17) 0.0010(18) -0.0005(18) C15 0.020(2) 0.016(2) 0.014(2) -0.0049(16) -0.0021(17) 0.0030(18) C16 0.027(3) 0.020(2) 0.021(2) -0.0013(18) -0.002(2) -0.005(2) C17 0.027(3) 0.020(2) 0.014(2) 0.0019(18) -0.0042(19) 0.0035(19) C18 0.023(2) 0.026(3) 0.020(2) -0.0009(19) -0.0054(19) 0.002(2) C19 0.019(2) 0.018(2) 0.016(2) -0.0020(17) -0.0026(17) -0.0027(18) C20 0.030(3) 0.012(2) 0.014(2) -0.0039(17) -0.0010(19) 0.0013(18) C21 0.021(2) 0.020(2) 0.023(2) -0.0001(19) -0.003(2) -0.0041(19) C22 0.018(2) 0.020(2) 0.021(2) -0.0004(18) -0.0026(19) -0.0046(19) C23 0.021(2) 0.023(2) 0.022(2) 0.0048(19) -0.0028(19) -0.0018(19) C24 0.012(2) 0.018(2) 0.027(2) 0.0030(18) -0.0063(18) -0.0028(18) C25 0.021(2) 0.019(2) 0.022(2) -0.0011(18) -0.0034(19) -0.0030(19) C26 0.014(2) 0.017(2) 0.022(2) 0.0019(17) -0.0021(18) -0.0053(18) C27 0.014(2) 0.013(2) 0.025(2) -0.0001(17) -0.0022(18) -0.0020(17) C28 0.018(2) 0.015(2) 0.023(2) 0.0003(18) -0.0003(19) 0.0017(18) C29 0.021(2) 0.016(2) 0.025(2) -0.0058(19) -0.0003(19) 0.0021(19) C30 0.044(3) 0.017(2) 0.039(3) -0.001(2) -0.006(3) 0.005(2) C31 0.034(3) 0.022(3) 0.048(3) -0.014(2) -0.010(3) 0.004(2) C32 0.049(4) 0.025(3) 0.028(3) -0.011(2) 0.006(3) 0.003(3) C33 0.023(2) 0.017(2) 0.022(2) 0.0025(18) -0.0009(19) -0.0034(19) C34 0.029(3) 0.017(2) 0.030(3) 0.005(2) 0.000(2) -0.007(2) C35 0.032(3) 0.025(3) 0.033(3) 0.004(2) -0.007(2) -0.011(2) C36 0.040(3) 0.016(2) 0.044(3) -0.002(2) 0.010(3) -0.002(2) C37 0.027(3) 0.025(3) 0.024(3) 0.010(2) -0.002(2) 0.004(2) C38 0.033(3) 0.039(3) 0.056(4) 0.023(3) 0.001(3) 0.010(3) C39 0.049(4) 0.036(3) 0.027(3) 0.010(2) -0.003(3) -0.006(3) C40 0.040(3) 0.024(3) 0.036(3) 0.011(2) -0.006(2) -0.001(2) C41 0.020(2) 0.022(2) 0.029(3) 0.004(2) 0.000(2) 0.001(2) C42 0.035(3) 0.021(3) 0.047(3) 0.000(2) -0.005(3) 0.003(2) C43 0.024(3) 0.030(3) 0.040(3) 0.007(2) 0.002(2) 0.010(2) C44 0.035(3) 0.036(3) 0.034(3) 0.010(2) -0.005(2) 0.014(3) C45 0.032(3) 0.023(2) 0.037(3) 0.000(2) 0.004(2) 0.000(2) C46 0.046(4) 0.073(5) 0.067(5) -0.019(4) -0.007(4) -0.016(4) C47 0.048(4) 0.044(4) 0.049(4) -0.011(3) 0.001(3) 0.004(3) C48 0.030(3) 0.029(3) 0.040(3) 0.003(2) 0.004(2) 0.006(2) C49 0.043(4) 0.029(3) 0.066(4) 0.009(3) 0.006(3) -0.007(3) C50 0.053(5) 0.082(6) 0.075(5) -0.039(5) -0.018(4) -0.004(4) C51 0.042(5) 0.068(7) 0.038(5) 0.000 0.011(4) 0.000 C52 0.084(9) 0.058(7) 0.067(7) 0.000 0.026(6) 0.000 C53 0.060(4) 0.036(3) 0.065(5) -0.001(3) -0.002(4) 0.007(3) C54 0.032(3) 0.043(4) 0.029(3) 0.001(2) -0.006(2) 0.007(3) C55 0.028(3) 0.030(3) 0.035(3) -0.002(2) -0.002(2) 0.003(2) C56 0.034(3) 0.037(3) 0.032(3) 0.007(2) 0.000(2) -0.002(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 Dy1 O9 2.264(5) . ? Dy1 O5 2.359(3) 8_565 ? Dy1 O5 2.359(3) . ? Dy1 O1 2.364(3) . ? Dy1 O1 2.364(3) 8_565 ? Dy1 O7 2.414(5) . ? Dy1 O11 2.442(4) . ? Dy1 O10 2.496(5) . ? Dy1 Fe3 3.3999(7) 8_565 ? Dy1 Fe3 3.3999(7) . ? Dy1 Dy2 3.8900(5) . ? O1 C6 1.359(5) . ? O1 Fe3 2.026(3) . ? N1 C45 1.335(7) . ? N1 C47 1.440(8) . ? N1 C46 1.453(8) . ? C1 C2 1.386(6) . ? C1 C6 1.407(6) . ? C1 C28 1.525(6) . ? Dy2 O9 2.312(5) . ? Dy2 O6 2.328(4) . ? Dy2 O6 2.328(4) 8_565 ? Dy2 O2 2.358(3) 8_565 ? Dy2 O2 2.358(3) . ? Dy2 O8 2.426(6) . ? Dy2 O12 2.463(5) . ? Dy2 O10 2.524(5) . ? Dy2 Fe3 3.3928(7) 8_565 ? Dy2 Fe3 3.3928(7) . ? O2 C13 1.379(5) . ? O2 Fe3 2.034(3) . ? N2 C48 1.320(7) . ? N2 C50 1.434(8) . ? N2 C49 1.444(8) . ? C2 C3 1.396(6) . ? Fe3 O10 1.8590(17) . ? Fe3 O3 1.935(3) . ? Fe3 O4 1.940(4) . ? O3 C20 1.363(5) . ? N3 C54 1.119(7) . ? C3 C4 1.391(6) . ? C3 C29 1.538(6) . ? O4 C27 1.346(5) . ? N4 C56 1.147(8) . ? C4 C5 1.396(6) . ? O5 C45 1.223(6) . ? C5 C6 1.394(6) . ? C5 C7 1.517(6) . ? O6 C48 1.220(7) . ? O7 C51 1.429(10) . ? C7 C8 1.517(6) . ? O8 C52 1.438(13) . ? C8 C9 1.392(6) . ? C8 C13 1.409(6) . ? C9 C10 1.399(6) . ? O10 Fe3 1.8590(17) 8_565 ? C10 C11 1.385(7) . ? C10 C33 1.541(6) . ? C11 C12 1.399(6) . ? C12 C13 1.405(6) . ? C12 C14 1.528(6) . ? C14 C15 1.514(6) . ? C15 C16 1.402(6) . ? C15 C20 1.403(6) . ? C16 C17 1.393(7) . ? C17 C18 1.390(7) . ? C17 C37 1.539(6) . ? C18 C19 1.390(6) . ? C19 C20 1.396(6) . ? C19 C21 1.521(6) . ? C21 C22 1.514(7) . ? C22 C23 1.396(7) . ? C22 C27 1.403(6) . ? C23 C24 1.390(7) . ? C24 C25 1.391(6) . ? C24 C41 1.541(6) . ? C25 C26 1.390(6) . ? C26 C27 1.401(6) . ? C26 C28 1.529(6) . ? C29 C31 1.522(7) . ? C29 C30 1.535(7) . ? C29 C32 1.537(7) . ? C33 C34 1.522(6) . ? C33 C35 1.534(7) . ? C33 C36 1.536(7) . ? C37 C40 1.518(7) . ? C37 C39 1.522(7) . ? C37 C38 1.537(7) . ? C41 C44 1.520(7) . ? C41 C42 1.531(7) . ? C41 C43 1.532(7) . ? C53 C54 1.464(9) . ? C55 C56 1.443(8) . ? 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 O9 Dy1 O5 84.29(13) . 8_565 ? O9 Dy1 O5 84.29(13) . . ? O5 Dy1 O5 74.99(16) 8_565 . ? O9 Dy1 O1 89.43(9) . . ? O5 Dy1 O1 150.27(11) 8_565 . ? O5 Dy1 O1 75.48(11) . . ? O9 Dy1 O1 89.43(9) . 8_565 ? O5 Dy1 O1 75.48(11) 8_565 8_565 ? O5 Dy1 O1 150.27(11) . 8_565 ? O1 Dy1 O1 133.63(15) . 8_565 ? O9 Dy1 O7 152.59(18) . . ? O5 Dy1 O7 74.10(13) 8_565 . ? O5 Dy1 O7 74.10(13) . . ? O1 Dy1 O7 100.95(9) . . ? O1 Dy1 O7 100.95(9) 8_565 . ? O9 Dy1 O11 141.28(17) . . ? O5 Dy1 O11 124.75(11) 8_565 . ? O5 Dy1 O11 124.75(11) . . ? O1 Dy1 O11 76.21(8) . . ? O1 Dy1 O11 76.21(8) 8_565 . ? O7 Dy1 O11 66.13(17) . . ? O9 Dy1 O10 71.60(17) . . ? O5 Dy1 O10 135.68(10) 8_565 . ? O5 Dy1 O10 135.68(10) . . ? O1 Dy1 O10 67.88(8) . . ? O1 Dy1 O10 67.88(8) 8_565 . ? O7 Dy1 O10 135.81(17) . . ? O11 Dy1 O10 69.68(16) . . ? O9 Dy1 Fe3 81.37(11) . 8_565 ? O5 Dy1 Fe3 109.21(8) 8_565 8_565 ? O5 Dy1 Fe3 164.50(9) . 8_565 ? O1 Dy1 Fe3 98.46(8) . 8_565 ? O1 Dy1 Fe3 35.78(7) 8_565 8_565 ? O7 Dy1 Fe3 121.33(10) . 8_565 ? O11 Dy1 Fe3 65.89(9) . 8_565 ? O10 Dy1 Fe3 32.38(3) . 8_565 ? O9 Dy1 Fe3 81.37(11) . . ? O5 Dy1 Fe3 164.50(9) 8_565 . ? O5 Dy1 Fe3 109.21(8) . . ? O1 Dy1 Fe3 35.78(7) . . ? O1 Dy1 Fe3 98.46(8) 8_565 . ? O7 Dy1 Fe3 121.33(10) . . ? O11 Dy1 Fe3 65.89(9) . . ? O10 Dy1 Fe3 32.38(3) . . ? Fe3 Dy1 Fe3 62.83(2) 8_565 . ? O9 Dy1 Dy2 32.14(13) . . ? O5 Dy1 Dy2 109.54(8) 8_565 . ? O5 Dy1 Dy2 109.54(8) . . ? O1 Dy1 Dy2 77.42(8) . . ? O1 Dy1 Dy2 77.42(8) 8_565 . ? O7 Dy1 Dy2 175.28(13) . . ? O11 Dy1 Dy2 109.14(11) . . ? O10 Dy1 Dy2 39.46(11) . . ? Fe3 Dy1 Dy2 54.977(12) 8_565 . ? Fe3 Dy1 Dy2 54.978(12) . . ? C6 O1 Fe3 126.9(3) . . ? C6 O1 Dy1 131.9(3) . . ? Fe3 O1 Dy1 101.21(12) . . ? C45 N1 C47 121.8(5) . . ? C45 N1 C46 119.7(5) . . ? C47 N1 C46 118.4(5) . . ? C2 C1 C6 119.5(4) . . ? C2 C1 C28 118.1(4) . . ? C6 C1 C28 122.3(4) . . ? O9 Dy2 O6 86.02(14) . . ? O9 Dy2 O6 86.02(14) . 8_565 ? O6 Dy2 O6 76.57(18) . 8_565 ? O9 Dy2 O2 88.54(9) . 8_565 ? O6 Dy2 O2 150.53(12) . 8_565 ? O6 Dy2 O2 74.17(11) 8_565 8_565 ? O9 Dy2 O2 88.54(8) . . ? O6 Dy2 O2 74.17(11) . . ? O6 Dy2 O2 150.53(12) 8_565 . ? O2 Dy2 O2 134.66(14) 8_565 . ? O9 Dy2 O8 152.82(18) . . ? O6 Dy2 O8 72.82(15) . . ? O6 Dy2 O8 72.82(15) 8_565 . ? O2 Dy2 O8 101.44(9) 8_565 . ? O2 Dy2 O8 101.44(9) . . ? O9 Dy2 O12 141.86(17) . . ? O6 Dy2 O12 122.51(13) . . ? O6 Dy2 O12 122.51(13) 8_565 . ? O2 Dy2 O12 77.44(8) 8_565 . ? O2 Dy2 O12 77.44(8) . . ? O8 Dy2 O12 65.32(19) . . ? O9 Dy2 O10 70.35(16) . . ? O6 Dy2 O10 135.48(11) . . ? O6 Dy2 O10 135.48(11) 8_565 . ? O2 Dy2 O10 68.24(7) 8_565 . ? O2 Dy2 O10 68.24(7) . . ? O8 Dy2 O10 136.83(18) . . ? O12 Dy2 O10 71.51(17) . . ? O9 Dy2 Fe3 80.91(10) . 8_565 ? O6 Dy2 Fe3 165.43(10) . 8_565 ? O6 Dy2 Fe3 108.70(9) 8_565 8_565 ? O2 Dy2 Fe3 36.07(7) 8_565 8_565 ? O2 Dy2 Fe3 98.96(7) . 8_565 ? O8 Dy2 Fe3 121.56(11) . 8_565 ? O12 Dy2 Fe3 66.85(10) . 8_565 ? O10 Dy2 Fe3 32.62(3) . 8_565 ? O9 Dy2 Fe3 80.91(10) . . ? O6 Dy2 Fe3 108.70(9) . . ? O6 Dy2 Fe3 165.43(10) 8_565 . ? O2 Dy2 Fe3 98.96(7) 8_565 . ? O2 Dy2 Fe3 36.07(7) . . ? O8 Dy2 Fe3 121.56(11) . . ? O12 Dy2 Fe3 66.85(10) . . ? O10 Dy2 Fe3 32.62(3) . . ? Fe3 Dy2 Fe3 62.98(2) 8_565 . ? O9 Dy2 Dy1 31.39(11) . . ? O6 Dy2 Dy1 110.37(10) . . ? O6 Dy2 Dy1 110.37(10) 8_565 . ? O2 Dy2 Dy1 77.17(7) 8_565 . ? O2 Dy2 Dy1 77.17(7) . . ? O8 Dy2 Dy1 175.78(14) . . ? O12 Dy2 Dy1 110.46(12) . . ? O10 Dy2 Dy1 38.95(12) . . ? Fe3 Dy2 Dy1 55.149(12) 8_565 . ? Fe3 Dy2 Dy1 55.149(12) . . ? C13 O2 Fe3 123.7(3) . . ? C13 O2 Dy2 135.4(3) . . ? Fe3 O2 Dy2 100.88(12) . . ? C48 N2 C50 119.9(6) . . ? C48 N2 C49 121.3(5) . . ? C50 N2 C49 118.4(6) . . ? C1 C2 C3 122.7(4) . . ? O10 Fe3 O3 108.16(17) . . ? O10 Fe3 O4 106.84(17) . . ? O3 Fe3 O4 92.30(14) . . ? O10 Fe3 O1 88.59(17) . . ? O3 Fe3 O1 162.64(13) . . ? O4 Fe3 O1 86.97(13) . . ? O10 Fe3 O2 89.42(17) . . ? O3 Fe3 O2 86.50(13) . . ? O4 Fe3 O2 163.18(13) . . ? O1 Fe3 O2 89.22(13) . . ? O10 Fe3 Dy2 47.03(14) . . ? O3 Fe3 Dy2 93.73(10) . . ? O4 Fe3 Dy2 153.65(10) . . ? O1 Fe3 Dy2 94.59(9) . . ? O2 Fe3 Dy2 43.05(9) . . ? O10 Fe3 Dy1 45.99(15) . . ? O3 Fe3 Dy1 154.09(9) . . ? O4 Fe3 Dy1 94.53(10) . . ? O1 Fe3 Dy1 43.01(8) . . ? O2 Fe3 Dy1 93.82(9) . . ? Dy2 Fe3 Dy1 69.873(14) . . ? C20 O3 Fe3 130.7(3) . . ? C4 C3 C2 116.7(4) . . ? C4 C3 C29 123.2(4) . . ? C2 C3 C29 120.1(4) . . ? C27 O4 Fe3 130.2(3) . . ? C3 C4 C5 122.2(4) . . ? C45 O5 Dy1 134.4(3) . . ? C6 C5 C4 120.0(4) . . ? C6 C5 C7 120.2(4) . . ? C4 C5 C7 119.6(4) . . ? C48 O6 Dy2 147.8(4) . . ? O1 C6 C5 119.8(4) . . ? O1 C6 C1 121.3(4) . . ? C5 C6 C1 118.9(4) . . ? C51 O7 Dy1 130.3(5) . . ? C8 C7 C5 109.1(4) . . ? C52 O8 Dy2 130.3(6) . . ? C9 C8 C13 119.5(4) . . ? C9 C8 C7 119.1(4) . . ? C13 C8 C7 121.2(4) . . ? Dy1 O9 Dy2 116.5(2) . . ? C8 C9 C10 122.6(4) . . ? Fe3 O10 Fe3 144.9(3) 8_565 . ? Fe3 O10 Dy1 101.63(14) 8_565 . ? Fe3 O10 Dy1 101.63(14) . . ? Fe3 O10 Dy2 100.35(14) 8_565 . ? Fe3 O10 Dy2 100.35(14) . . ? Dy1 O10 Dy2 101.58(19) . . ? C11 C10 C9 116.7(4) . . ? C11 C10 C33 124.1(4) . . ? C9 C10 C33 119.2(4) . . ? C10 C11 C12 123.0(4) . . ? C11 C12 C13 119.2(4) . . ? C11 C12 C14 119.2(4) . . ? C13 C12 C14 121.5(4) . . ? O2 C13 C12 121.4(4) . . ? O2 C13 C8 119.6(4) . . ? C12 C13 C8 119.0(4) . . ? C15 C14 C12 111.1(4) . . ? C16 C15 C20 119.0(4) . . ? C16 C15 C14 119.6(4) . . ? C20 C15 C14 121.2(4) . . ? C17 C16 C15 122.3(4) . . ? C18 C17 C16 117.0(4) . . ? C18 C17 C37 122.3(4) . . ? C16 C17 C37 120.7(4) . . ? C17 C18 C19 122.6(4) . . ? C18 C19 C20 119.5(4) . . ? C18 C19 C21 118.9(4) . . ? C20 C19 C21 121.3(4) . . ? O3 C20 C19 120.1(4) . . ? O3 C20 C15 120.3(4) . . ? C19 C20 C15 119.6(4) . . ? C22 C21 C19 110.1(4) . . ? C23 C22 C27 119.1(4) . . ? C23 C22 C21 119.8(4) . . ? C27 C22 C21 120.9(4) . . ? C24 C23 C22 122.6(4) . . ? C25 C24 C23 116.8(4) . . ? C25 C24 C41 119.6(4) . . ? C23 C24 C41 123.6(4) . . ? C26 C25 C24 122.8(4) . . ? C25 C26 C27 119.2(4) . . ? C25 C26 C28 119.0(4) . . ? C27 C26 C28 121.6(4) . . ? O4 C27 C26 120.6(4) . . ? O4 C27 C22 119.9(4) . . ? C26 C27 C22 119.5(4) . . ? C1 C28 C26 111.2(4) . . ? C31 C29 C30 108.3(4) . . ? C31 C29 C3 112.6(4) . . ? C30 C29 C3 108.8(4) . . ? C31 C29 C32 108.2(4) . . ? C30 C29 C32 109.1(4) . . ? C3 C29 C32 109.8(4) . . ? C34 C33 C35 109.7(4) . . ? C34 C33 C36 108.3(4) . . ? C35 C33 C36 108.7(4) . . ? C34 C33 C10 111.9(4) . . ? C35 C33 C10 109.2(4) . . ? C36 C33 C10 108.9(4) . . ? C40 C37 C39 109.6(4) . . ? C40 C37 C38 107.7(5) . . ? C39 C37 C38 108.2(5) . . ? C40 C37 C17 112.2(4) . . ? C39 C37 C17 109.1(4) . . ? C38 C37 C17 110.0(4) . . ? C44 C41 C42 108.1(4) . . ? C44 C41 C43 109.4(4) . . ? C42 C41 C43 109.0(4) . . ? C44 C41 C24 111.8(4) . . ? C42 C41 C24 109.8(4) . . ? C43 C41 C24 108.7(4) . . ? O5 C45 N1 124.2(5) . . ? O6 C48 N2 124.5(5) . . ? N3 C54 C53 178.5(7) . . ? N4 C56 C55 179.3(7) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.48 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 4.067 _refine_diff_density_min -2.108 _refine_diff_density_rms 0.128