# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_amcb16dyy _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H52 Dy2 Fe2 N8 O20, 6(C2 H3 N)' _chemical_formula_sum 'C72 H70 Dy2 Fe2 N14 O20' _chemical_formula_weight 1888.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9912(6) _cell_length_b 12.8733(7) _cell_length_c 14.5474(8) _cell_angle_alpha 70.567(4) _cell_angle_beta 79.101(4) _cell_angle_gamma 67.143(4) _cell_volume 1946.78(18) _cell_formula_units_Z 1 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 68334 _cell_measurement_theta_min 1.49 _cell_measurement_theta_max 29.56 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.611 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 944 _exptl_absorpt_coefficient_mu 2.341 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.453 _exptl_absorpt_correction_T_max 0.585 _exptl_absorpt_process_details ; XPREP in SHELXTL 6.14 (BrukerAXS Inc., 2003) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean 6.667 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 56533 _diffrn_reflns_av_R_equivalents 0.0465 _diffrn_reflns_av_sigmaI/netI 0.0275 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 29.21 _reflns_number_total 10469 _reflns_number_gt 9443 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'WinXpose 1.6.8 (Stoe & Cie GmbH, 2004)' _computing_cell_refinement 'X-Area 1.38 (Stoe & Cie GmbH, 2006)' _computing_data_reduction 'X-Area 1.38 (Stoe & Cie GmbH, 2006)' _computing_structure_solution 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_structure_refinement 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_molecular_graphics 'Diamond 2.1 (Crystal Impact, 1998)' _computing_publication_material 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0354P)^2^+0.5276P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10469 _refine_ls_number_parameters 505 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0318 _refine_ls_R_factor_gt 0.0261 _refine_ls_wR_factor_ref 0.0593 _refine_ls_wR_factor_gt 0.0579 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.278990(8) 0.425652(8) 0.535934(8) 0.02092(3) Uani 1 1 d . . . Fe1 Fe 0.45040(3) 0.59272(3) 0.39865(2) 0.02139(6) Uani 1 1 d . . . O1 O 0.39507(13) 0.53786(13) 0.54369(11) 0.0221(3) Uani 1 1 d D . . H1 H 0.358(3) 0.584(2) 0.573(2) 0.027 Uiso 1 1 d D . . N1 N 0.37831(17) 0.25864(16) 0.45071(15) 0.0268(4) Uani 1 1 d . . . C1 C 0.4482(2) 0.2970(2) 0.35765(19) 0.0317(5) Uani 1 1 d . . . H1B H 0.4428 0.2593 0.3102 0.038 Uiso 1 1 calc R . . H1C H 0.5347 0.2701 0.3703 0.038 Uiso 1 1 calc R . . C2 C 0.4017(2) 0.4297(2) 0.31336(17) 0.0287(4) Uani 1 1 d . . . H2A H 0.4624 0.4532 0.2630 0.034 Uiso 1 1 calc R . . H2B H 0.3257 0.4546 0.2816 0.034 Uiso 1 1 calc R . . O2 O 0.37988(14) 0.48512(13) 0.38688(11) 0.0242(3) Uani 1 1 d . . . C3 C 0.4600(2) 0.15899(19) 0.52164(19) 0.0302(5) Uani 1 1 d . . . H3A H 0.5103 0.0971 0.4898 0.036 Uiso 1 1 calc R . . H3B H 0.4109 0.1248 0.5773 0.036 Uiso 1 1 calc R . . C4 C 0.5421(2) 0.1989(2) 0.5591(2) 0.0301(5) Uani 1 1 d . . . H4A H 0.5810 0.1371 0.6173 0.036 Uiso 1 1 calc R . . H4B H 0.6068 0.2117 0.5081 0.036 Uiso 1 1 calc R . . O3 O 0.47379(13) 0.30433(13) 0.58388(12) 0.0239(3) Uani 1 1 d . . . C5 C 0.2827(2) 0.2226(2) 0.43439(19) 0.0310(5) Uani 1 1 d . . . H5A H 0.2494 0.1831 0.4981 0.037 Uiso 1 1 calc R . . H5B H 0.3180 0.1657 0.3955 0.037 Uiso 1 1 calc R . . C6 C 0.1817(2) 0.3277(2) 0.38122(19) 0.0323(5) Uani 1 1 d . . . H6A H 0.2097 0.3580 0.3125 0.039 Uiso 1 1 calc R . . H6B H 0.1114 0.3052 0.3816 0.039 Uiso 1 1 calc R . . O4 O 0.14775(15) 0.41576(15) 0.43095(13) 0.0303(3) Uani 1 1 d D . . H4 H 0.071(2) 0.459(3) 0.424(2) 0.036 Uiso 1 1 d D . . O5 O 0.29000(14) 0.72233(14) 0.38046(12) 0.0272(3) Uani 1 1 d . . . O6 O 0.15952(14) 0.63432(14) 0.47310(12) 0.0273(3) Uani 1 1 d . . . C7 C 0.18607(19) 0.72232(19) 0.42141(16) 0.0245(4) Uani 1 1 d . . . C8 C 0.08900(19) 0.84310(19) 0.40282(17) 0.0257(4) Uani 1 1 d . . . C9 C 0.1198(2) 0.9409(2) 0.3520(2) 0.0434(7) Uani 1 1 d . . . H9A H 0.2009 0.9313 0.3263 0.052 Uiso 1 1 calc R . . C10 C 0.0333(2) 1.0528(2) 0.3382(3) 0.0475(7) Uani 1 1 d . . . H10A H 0.0553 1.1199 0.3044 0.057 Uiso 1 1 calc R . . C11 C -0.0852(2) 1.0662(2) 0.37397(19) 0.0307(5) Uani 1 1 d . . . C12 C -0.1174(2) 0.9689(2) 0.4230(3) 0.0450(7) Uani 1 1 d . . . H12A H -0.1991 0.9782 0.4468 0.054 Uiso 1 1 calc R . . C13 C -0.0293(2) 0.8571(2) 0.4374(2) 0.0405(6) Uani 1 1 d . . . H13A H -0.0510 0.7899 0.4713 0.049 Uiso 1 1 calc R . . C14 C -0.1738(2) 1.1836(2) 0.3621(2) 0.0336(5) Uani 1 1 d . . . N2 N -0.2430(2) 1.2766(2) 0.3545(2) 0.0409(5) Uani 1 1 d . . . O7 O 0.52875(15) 0.61018(15) 0.26304(12) 0.0292(3) Uani 1 1 d . . . O8 O 0.71675(14) 0.58388(15) 0.29283(12) 0.0296(3) Uani 1 1 d . . . C15 C 0.6350(2) 0.6153(2) 0.23743(17) 0.0269(4) Uani 1 1 d . . . C16 C 0.6592(2) 0.6678(2) 0.13007(17) 0.0294(5) Uani 1 1 d . . . C17 C 0.5756(3) 0.6924(3) 0.0647(2) 0.0429(6) Uani 1 1 d . . . H17A H 0.5046 0.6728 0.0875 0.051 Uiso 1 1 calc R . . C18 C 0.5951(3) 0.7451(3) -0.0335(2) 0.0476(7) Uani 1 1 d . . . H18A H 0.5390 0.7600 -0.0786 0.057 Uiso 1 1 calc R . . C19 C 0.6975(3) 0.7761(2) -0.06553(19) 0.0372(5) Uani 1 1 d . . . C20 C 0.7817(2) 0.7531(2) -0.00086(19) 0.0369(5) Uani 1 1 d . . . H20A H 0.8514 0.7749 -0.0235 0.044 Uiso 1 1 calc R . . C21 C 0.7625(2) 0.6978(2) 0.09701(18) 0.0336(5) Uani 1 1 d . . . H21A H 0.8200 0.6802 0.1418 0.040 Uiso 1 1 calc R . . C22 C 0.7172(3) 0.8325(3) -0.1682(2) 0.0425(6) Uani 1 1 d . . . N3 N 0.7305(3) 0.8774(3) -0.24920(19) 0.0535(7) Uani 1 1 d . . . O9 O 0.21543(14) 0.26408(14) 0.64287(13) 0.0304(3) Uani 1 1 d . . . O10 O 0.07229(14) 0.43865(14) 0.62550(13) 0.0285(3) Uani 1 1 d . . . C23 C 0.11010(19) 0.3272(2) 0.66408(17) 0.0260(4) Uani 1 1 d . . . C24 C 0.0291(2) 0.2700(2) 0.73632(17) 0.0286(4) Uani 1 1 d . . . C25 C -0.0927(2) 0.3333(2) 0.7529(2) 0.0376(6) Uani 1 1 d . . . H25A H -0.1244 0.4153 0.7210 0.045 Uiso 1 1 calc R . . C26 C -0.1686(3) 0.2779(3) 0.8156(2) 0.0457(7) Uani 1 1 d . . . H26A H -0.2522 0.3213 0.8254 0.055 Uiso 1 1 calc R . . C27 C -0.1219(3) 0.1592(3) 0.8636(2) 0.0417(6) Uani 1 1 d . . . C28 C -0.0003(3) 0.0954(3) 0.8487(2) 0.0440(6) Uani 1 1 d . . . H28A H 0.0316 0.0139 0.8819 0.053 Uiso 1 1 calc R . . C29 C 0.0744(2) 0.1508(2) 0.7854(2) 0.0397(6) Uani 1 1 d . . . H29A H 0.1578 0.1069 0.7754 0.048 Uiso 1 1 calc R . . C30 C -0.2011(3) 0.1018(3) 0.9286(3) 0.0611(10) Uani 1 1 d . . . N4 N -0.2657(3) 0.0583(3) 0.9787(3) 0.0946(15) Uani 1 1 d . . . N31 N 0.6152(4) 0.0823(3) 0.2471(4) 0.0884(12) Uani 1 1 d . . . C31 C 0.5974(4) 0.0171(3) 0.2216(3) 0.0644(10) Uani 1 1 d . . . C32 C 0.5784(4) -0.0689(3) 0.1889(3) 0.0662(10) Uani 1 1 d . . . H32A H 0.6192 -0.0688 0.1238 0.099 Uiso 1 1 calc R . . H32B H 0.4913 -0.0491 0.1860 0.099 Uiso 1 1 calc R . . H32C H 0.6119 -0.1472 0.2347 0.099 Uiso 1 1 calc R . . N32 N 0.9320(5) 0.2076(5) 0.0971(4) 0.1126(17) Uani 1 1 d . . . C33 C 0.8286(6) 0.2634(5) 0.0946(4) 0.0876(14) Uani 1 1 d . . . C34 C 0.7019(5) 0.3332(6) 0.0936(6) 0.118(2) Uani 1 1 d . . . H34A H 0.6542 0.2813 0.1161 0.176 Uiso 1 1 calc R . . H34B H 0.6826 0.3830 0.0270 0.176 Uiso 1 1 calc R . . H34C H 0.6823 0.3828 0.1371 0.176 Uiso 1 1 calc R . . N33 N 1.1340(8) 0.5070(6) 0.0851(5) 0.156(3) Uani 1 1 d . . . C35 C 1.0629(6) 0.4681(4) 0.1267(4) 0.0844(14) Uani 1 1 d . . . C36 C 0.9760(4) 0.4178(4) 0.1802(4) 0.0804(13) Uani 1 1 d . . . H36A H 1.0145 0.3319 0.2016 0.121 Uiso 1 1 calc R . . H36B H 0.9102 0.4394 0.1388 0.121 Uiso 1 1 calc R . . H36C H 0.9429 0.4470 0.2375 0.121 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.01434(5) 0.01813(5) 0.02943(5) -0.00653(3) -0.00028(3) -0.00561(3) Fe1 0.01517(13) 0.01876(13) 0.02882(15) -0.00571(11) -0.00093(11) -0.00566(10) O1 0.0166(6) 0.0183(7) 0.0288(7) -0.0082(6) 0.0009(5) -0.0033(5) N1 0.0207(8) 0.0229(9) 0.0378(10) -0.0105(8) -0.0006(7) -0.0078(7) C1 0.0270(11) 0.0288(11) 0.0415(13) -0.0168(10) 0.0067(9) -0.0105(9) C2 0.0269(11) 0.0302(11) 0.0324(11) -0.0127(9) 0.0023(9) -0.0125(9) O2 0.0211(7) 0.0245(7) 0.0303(8) -0.0110(6) 0.0015(6) -0.0102(6) C3 0.0233(10) 0.0191(10) 0.0478(14) -0.0124(9) -0.0028(9) -0.0044(8) C4 0.0199(10) 0.0214(10) 0.0486(14) -0.0130(10) -0.0021(9) -0.0044(8) O3 0.0170(7) 0.0177(7) 0.0362(8) -0.0083(6) -0.0014(6) -0.0053(5) C5 0.0260(11) 0.0265(11) 0.0450(13) -0.0134(10) -0.0030(9) -0.0110(9) C6 0.0282(11) 0.0331(12) 0.0422(13) -0.0150(10) -0.0028(10) -0.0140(10) O4 0.0193(7) 0.0296(8) 0.0422(9) -0.0136(7) -0.0050(6) -0.0046(6) O5 0.0172(7) 0.0211(7) 0.0393(9) -0.0059(6) -0.0031(6) -0.0043(6) O6 0.0207(7) 0.0213(7) 0.0377(9) -0.0062(6) -0.0015(6) -0.0073(6) C7 0.0192(9) 0.0248(10) 0.0307(11) -0.0090(8) -0.0078(8) -0.0055(8) C8 0.0197(9) 0.0210(10) 0.0346(11) -0.0072(8) -0.0039(8) -0.0050(8) C9 0.0208(11) 0.0244(11) 0.0694(19) -0.0033(12) 0.0059(11) -0.0041(9) C10 0.0260(12) 0.0232(12) 0.077(2) -0.0025(12) 0.0075(12) -0.0064(10) C11 0.0228(10) 0.0237(10) 0.0403(13) -0.0090(9) -0.0004(9) -0.0034(8) C12 0.0209(11) 0.0286(12) 0.073(2) -0.0105(13) 0.0089(12) -0.0053(9) C13 0.0229(11) 0.0242(11) 0.0651(18) -0.0066(11) 0.0065(11) -0.0082(9) C14 0.0247(11) 0.0278(11) 0.0442(14) -0.0109(10) 0.0043(10) -0.0072(9) N2 0.0282(11) 0.0274(10) 0.0602(15) -0.0136(10) 0.0027(10) -0.0044(8) O7 0.0239(8) 0.0337(9) 0.0305(8) -0.0074(7) 0.0011(6) -0.0136(7) O8 0.0220(7) 0.0339(9) 0.0316(8) -0.0088(7) -0.0009(6) -0.0097(6) C15 0.0247(10) 0.0256(10) 0.0297(11) -0.0085(9) 0.0005(8) -0.0089(8) C16 0.0265(11) 0.0312(11) 0.0303(11) -0.0078(9) 0.0025(9) -0.0126(9) C17 0.0364(14) 0.0603(18) 0.0343(13) -0.0034(12) -0.0022(10) -0.0282(13) C18 0.0432(16) 0.070(2) 0.0326(13) -0.0027(13) -0.0054(11) -0.0319(15) C19 0.0383(13) 0.0403(14) 0.0317(12) -0.0075(10) 0.0025(10) -0.0169(11) C20 0.0352(13) 0.0415(14) 0.0352(13) -0.0097(11) 0.0063(10) -0.0198(11) C21 0.0289(11) 0.0410(13) 0.0321(12) -0.0093(10) 0.0020(9) -0.0164(10) C22 0.0419(15) 0.0509(16) 0.0370(14) -0.0088(12) 0.0007(11) -0.0232(13) N3 0.0611(17) 0.0708(19) 0.0371(13) -0.0082(12) 0.0024(11) -0.0407(15) O9 0.0209(7) 0.0248(8) 0.0428(9) -0.0081(7) 0.0014(6) -0.0080(6) O10 0.0194(7) 0.0241(7) 0.0396(9) -0.0065(7) -0.0021(6) -0.0073(6) C23 0.0194(9) 0.0260(10) 0.0336(11) -0.0070(9) -0.0012(8) -0.0106(8) C24 0.0253(11) 0.0293(11) 0.0326(11) -0.0077(9) 0.0006(9) -0.0133(9) C25 0.0287(12) 0.0321(12) 0.0436(14) -0.0066(11) 0.0060(10) -0.0093(10) C26 0.0315(13) 0.0457(16) 0.0491(16) -0.0084(13) 0.0115(12) -0.0132(12) C27 0.0383(14) 0.0437(15) 0.0422(14) -0.0066(12) 0.0074(11) -0.0226(12) C28 0.0378(14) 0.0329(13) 0.0516(16) 0.0012(12) 0.0002(12) -0.0149(11) C29 0.0271(12) 0.0337(13) 0.0497(15) -0.0028(11) 0.0009(11) -0.0110(10) C30 0.0454(18) 0.0520(19) 0.067(2) 0.0024(16) 0.0135(16) -0.0222(15) N4 0.064(2) 0.077(3) 0.108(3) 0.011(2) 0.027(2) -0.035(2) N31 0.079(3) 0.060(2) 0.118(3) -0.046(2) 0.004(2) -0.0027(19) C31 0.057(2) 0.0418(18) 0.069(2) -0.0166(17) 0.0070(17) 0.0045(15) C32 0.064(2) 0.0493(19) 0.073(2) -0.0164(18) 0.0045(19) -0.0115(17) N32 0.090(4) 0.096(4) 0.139(5) -0.021(3) -0.001(3) -0.032(3) C33 0.102(4) 0.072(3) 0.092(4) -0.017(3) -0.003(3) -0.041(3) C34 0.078(4) 0.110(5) 0.151(6) -0.028(4) 0.006(4) -0.034(4) N33 0.230(8) 0.128(5) 0.139(5) -0.078(4) 0.077(5) -0.103(6) C35 0.114(4) 0.059(3) 0.079(3) -0.037(2) 0.000(3) -0.018(3) C36 0.076(3) 0.062(3) 0.096(3) -0.030(2) -0.022(3) -0.003(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 O2 2.3183(15) . ? Dy1 O3 2.3322(15) . ? Dy1 O1 2.4014(15) . ? Dy1 O9 2.4407(16) . ? Dy1 O6 2.4445(16) . ? Dy1 O4 2.4534(17) . ? Dy1 O8 2.4622(17) 2_666 ? Dy1 O10 2.5438(16) . ? Dy1 N1 2.6084(19) . ? Dy1 Fe1 3.4442(4) . ? Dy1 Fe1 3.4516(3) 2_666 ? Fe1 O2 1.9455(15) . ? Fe1 O3 1.9735(15) 2_666 ? Fe1 O5 1.9897(15) . ? Fe1 O7 1.9982(16) . ? Fe1 O1 2.0477(15) 2_666 ? Fe1 O1 2.0576(16) . ? Fe1 Dy1 3.4516(3) 2_666 ? O1 Fe1 2.0477(15) 2_666 ? O1 H1 0.79(2) . ? N1 C5 1.475(3) . ? N1 C3 1.482(3) . ? N1 C1 1.492(3) . ? C1 C2 1.519(3) . ? C1 H1B 0.9900 . ? C1 H1C 0.9900 . ? C2 O2 1.407(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.521(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O3 1.411(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? O3 Fe1 1.9736(15) 2_666 ? C5 C6 1.510(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 O4 1.432(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? O4 H4 0.88(3) . ? O5 C7 1.276(3) . ? O6 C7 1.254(3) . ? C7 C8 1.510(3) . ? C8 C13 1.374(3) . ? C8 C9 1.380(3) . ? C9 C10 1.384(3) . ? C9 H9A 0.9500 . ? C10 C11 1.382(3) . ? C10 H10A 0.9500 . ? C11 C12 1.380(4) . ? C11 C14 1.446(3) . ? C12 C13 1.391(3) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? C14 N2 1.144(3) . ? O7 C15 1.279(3) . ? O8 C15 1.244(3) . ? O8 Dy1 2.4622(17) 2_666 ? C15 C16 1.503(3) . ? C16 C17 1.387(4) . ? C16 C21 1.392(3) . ? C17 C18 1.381(4) . ? C17 H17A 0.9500 . ? C18 C19 1.387(4) . ? C18 H18A 0.9500 . ? C19 C20 1.391(4) . ? C19 C22 1.447(4) . ? C20 C21 1.384(3) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? C22 N3 1.137(4) . ? O9 C23 1.254(3) . ? O10 C23 1.278(3) . ? C23 C24 1.498(3) . ? C24 C25 1.388(3) . ? C24 C29 1.389(4) . ? C25 C26 1.388(4) . ? C25 H25A 0.9500 . ? C26 C27 1.382(4) . ? C26 H26A 0.9500 . ? C27 C28 1.384(4) . ? C27 C30 1.443(4) . ? C28 C29 1.380(4) . ? C28 H28A 0.9500 . ? C29 H29A 0.9500 . ? C30 N4 1.139(4) . ? N31 C31 1.124(6) . ? C31 C32 1.447(6) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? N32 C33 1.167(7) . ? C33 C34 1.433(8) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? N33 C35 1.132(8) . ? C35 C36 1.412(8) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 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 O2 Dy1 O3 83.79(5) . . ? O2 Dy1 O1 68.06(5) . . ? O3 Dy1 O1 68.53(5) . . ? O2 Dy1 O9 143.13(5) . . ? O3 Dy1 O9 85.73(5) . . ? O1 Dy1 O9 138.35(6) . . ? O2 Dy1 O6 76.23(5) . . ? O3 Dy1 O6 140.00(5) . . ? O1 Dy1 O6 71.92(5) . . ? O9 Dy1 O6 129.83(5) . . ? O2 Dy1 O4 82.11(6) . . ? O3 Dy1 O4 131.90(5) . . ? O1 Dy1 O4 142.48(6) . . ? O9 Dy1 O4 78.97(6) . . ? O6 Dy1 O4 79.46(6) . . ? O2 Dy1 O8 137.43(5) . 2_666 ? O3 Dy1 O8 72.88(5) . 2_666 ? O1 Dy1 O8 70.37(5) . 2_666 ? O9 Dy1 O8 71.01(6) . 2_666 ? O6 Dy1 O8 99.35(6) . 2_666 ? O4 Dy1 O8 139.53(6) . 2_666 ? O2 Dy1 O10 144.97(5) . . ? O3 Dy1 O10 130.80(5) . . ? O1 Dy1 O10 124.26(5) . . ? O9 Dy1 O10 52.39(5) . . ? O6 Dy1 O10 77.75(5) . . ? O4 Dy1 O10 70.36(6) . . ? O8 Dy1 O10 69.92(5) 2_666 . ? O2 Dy1 N1 67.74(6) . . ? O3 Dy1 N1 67.21(6) . . ? O1 Dy1 N1 119.24(5) . . ? O9 Dy1 N1 75.59(6) . . ? O6 Dy1 N1 131.60(6) . . ? O4 Dy1 N1 64.87(6) . . ? O8 Dy1 N1 129.04(6) 2_666 . ? O10 Dy1 N1 115.98(5) . . ? O2 Fe1 O3 177.15(7) . 2_666 ? O2 Fe1 O5 90.32(7) . . ? O3 Fe1 O5 91.74(6) 2_666 . ? O2 Fe1 O7 92.45(7) . . ? O3 Fe1 O7 89.00(7) 2_666 . ? O5 Fe1 O7 103.28(7) . . ? O2 Fe1 O1 94.49(6) . 2_666 ? O3 Fe1 O1 83.02(6) 2_666 2_666 ? O5 Fe1 O1 164.09(7) . 2_666 ? O7 Fe1 O1 91.68(7) . 2_666 ? O2 Fe1 O1 82.55(6) . . ? O3 Fe1 O1 95.54(6) 2_666 . ? O5 Fe1 O1 88.09(6) . . ? O7 Fe1 O1 167.65(7) . . ? O1 Fe1 O1 77.53(6) 2_666 . ? Fe1 O1 Fe1 102.47(6) 2_666 . ? Fe1 O1 Dy1 101.46(6) 2_666 . ? Fe1 O1 Dy1 100.86(6) . . ? Fe1 O1 H1 117(2) 2_666 . ? Fe1 O1 H1 120(2) . . ? Dy1 O1 H1 112(2) . . ? C5 N1 C3 108.79(18) . . ? C5 N1 C1 111.68(19) . . ? C3 N1 C1 110.64(18) . . ? C5 N1 Dy1 108.88(13) . . ? C3 N1 Dy1 105.43(14) . . ? C1 N1 Dy1 111.20(13) . . ? N1 C1 C2 112.38(18) . . ? N1 C1 H1B 109.1 . . ? C2 C1 H1B 109.1 . . ? N1 C1 H1C 109.1 . . ? C2 C1 H1C 109.1 . . ? H1B C1 H1C 107.9 . . ? O2 C2 C1 109.74(19) . . ? O2 C2 H2A 109.7 . . ? C1 C2 H2A 109.7 . . ? O2 C2 H2B 109.7 . . ? C1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? C2 O2 Fe1 129.49(13) . . ? C2 O2 Dy1 121.87(13) . . ? Fe1 O2 Dy1 107.44(7) . . ? N1 C3 C4 111.04(18) . . ? N1 C3 H3A 109.4 . . ? C4 C3 H3A 109.4 . . ? N1 C3 H3B 109.4 . . ? C4 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? O3 C4 C3 109.99(18) . . ? O3 C4 H4A 109.7 . . ? C3 C4 H4A 109.7 . . ? O3 C4 H4B 109.7 . . ? C3 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? C4 O3 Fe1 122.56(13) . 2_666 ? C4 O3 Dy1 124.70(13) . . ? Fe1 O3 Dy1 106.27(6) 2_666 . ? N1 C5 C6 110.92(19) . . ? N1 C5 H5A 109.5 . . ? C6 C5 H5A 109.5 . . ? N1 C5 H5B 109.5 . . ? C6 C5 H5B 109.5 . . ? H5A C5 H5B 108.0 . . ? O4 C6 C5 107.41(19) . . ? O4 C6 H6A 110.2 . . ? C5 C6 H6A 110.2 . . ? O4 C6 H6B 110.2 . . ? C5 C6 H6B 110.2 . . ? H6A C6 H6B 108.5 . . ? C6 O4 Dy1 124.43(14) . . ? C6 O4 H4 109(2) . . ? Dy1 O4 H4 126(2) . . ? C7 O5 Fe1 129.31(15) . . ? C7 O6 Dy1 133.44(14) . . ? O6 C7 O5 126.7(2) . . ? O6 C7 C8 119.50(19) . . ? O5 C7 C8 113.82(19) . . ? C13 C8 C9 119.6(2) . . ? C13 C8 C7 120.8(2) . . ? C9 C8 C7 119.6(2) . . ? C8 C9 C10 120.6(2) . . ? C8 C9 H9A 119.7 . . ? C10 C9 H9A 119.7 . . ? C11 C10 C9 119.5(2) . . ? C11 C10 H10A 120.2 . . ? C9 C10 H10A 120.2 . . ? C12 C11 C10 120.3(2) . . ? C12 C11 C14 120.6(2) . . ? C10 C11 C14 119.0(2) . . ? C11 C12 C13 119.5(2) . . ? C11 C12 H12A 120.3 . . ? C13 C12 H12A 120.3 . . ? C8 C13 C12 120.5(2) . . ? C8 C13 H13A 119.7 . . ? C12 C13 H13A 119.7 . . ? N2 C14 C11 178.5(3) . . ? C15 O7 Fe1 125.10(15) . . ? C15 O8 Dy1 134.67(15) . 2_666 ? O8 C15 O7 126.2(2) . . ? O8 C15 C16 118.4(2) . . ? O7 C15 C16 115.3(2) . . ? C17 C16 C21 120.0(2) . . ? C17 C16 C15 120.1(2) . . ? C21 C16 C15 119.8(2) . . ? C18 C17 C16 120.3(2) . . ? C18 C17 H17A 119.9 . . ? C16 C17 H17A 119.9 . . ? C17 C18 C19 119.3(3) . . ? C17 C18 H18A 120.3 . . ? C19 C18 H18A 120.3 . . ? C18 C19 C20 121.2(2) . . ? C18 C19 C22 119.3(3) . . ? C20 C19 C22 119.6(2) . . ? C21 C20 C19 119.0(2) . . ? C21 C20 H20A 120.5 . . ? C19 C20 H20A 120.5 . . ? C20 C21 C16 120.3(2) . . ? C20 C21 H21A 119.9 . . ? C16 C21 H21A 119.9 . . ? N3 C22 C19 178.7(3) . . ? C23 O9 Dy1 96.07(13) . . ? C23 O10 Dy1 90.64(13) . . ? O9 C23 O10 120.8(2) . . ? O9 C23 C24 118.9(2) . . ? O10 C23 C24 120.3(2) . . ? C25 C24 C29 118.8(2) . . ? C25 C24 C23 121.1(2) . . ? C29 C24 C23 120.0(2) . . ? C24 C25 C26 120.6(2) . . ? C24 C25 H25A 119.7 . . ? C26 C25 H25A 119.7 . . ? C27 C26 C25 119.7(3) . . ? C27 C26 H26A 120.2 . . ? C25 C26 H26A 120.2 . . ? C26 C27 C28 120.3(2) . . ? C26 C27 C30 119.5(3) . . ? C28 C27 C30 120.2(3) . . ? C29 C28 C27 119.8(3) . . ? C29 C28 H28A 120.1 . . ? C27 C28 H28A 120.1 . . ? C28 C29 C24 120.8(2) . . ? C28 C29 H29A 119.6 . . ? C24 C29 H29A 119.6 . . ? N4 C30 C27 178.5(5) . . ? N31 C31 C32 178.3(4) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N32 C33 C34 178.4(7) . . ? 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 . . ? N33 C35 C36 178.7(8) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 N2 0.79(2) 2.24(2) 3.029(3) 175(3) 2_576 O4 H4 O10 0.88(3) 1.81(3) 2.665(2) 164(3) 2_566 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.853 _refine_diff_density_min -1.083 _refine_diff_density_rms 0.082 _database_code_depnum_ccdc_archive 'CCDC 866243' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_ampt16dyx _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H70 Dy2 Fe2 N2 O20, 2(C8 H8 O2), 2(C2 H3 N)' _chemical_formula_sum 'C80 H92 Dy2 Fe2 N4 O24' _chemical_formula_weight 1930.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.5412(10) _cell_length_b 14.2757(13) _cell_length_c 14.4870(12) _cell_angle_alpha 61.979(6) _cell_angle_beta 87.646(7) _cell_angle_gamma 80.384(7) _cell_volume 2075.5(3) _cell_formula_units_Z 1 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 19893 _cell_measurement_theta_min 1.59 _cell_measurement_theta_max 28.41 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.544 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 976 _exptl_absorpt_coefficient_mu 2.198 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.516 _exptl_absorpt_correction_T_max 0.654 _exptl_absorpt_process_details ; XPREP in SHELXTL 6.14 (BrukerAXS Inc., 2003) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean 6.667 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24227 _diffrn_reflns_av_R_equivalents 0.0428 _diffrn_reflns_av_sigmaI/netI 0.0416 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 26.37 _reflns_number_total 8476 _reflns_number_gt 7303 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'WinXpose 1.6.8 (Stoe & Cie GmbH, 2004)' _computing_cell_refinement 'X-Area 1.38 (Stoe & Cie GmbH, 2006)' _computing_data_reduction 'X-Area 1.38 (Stoe & Cie GmbH, 2006)' _computing_structure_solution 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_structure_refinement 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_molecular_graphics 'Diamond 2.1 (Crystal Impact, 1998)' _computing_publication_material 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0708P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8476 _refine_ls_number_parameters 517 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0458 _refine_ls_R_factor_gt 0.0400 _refine_ls_wR_factor_ref 0.0972 _refine_ls_wR_factor_gt 0.0956 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.565146(15) 0.479869(14) 0.708675(14) 0.02411(7) Uani 1 1 d . . . Fe1 Fe 0.43405(4) 0.62281(4) 0.46244(4) 0.02479(12) Uani 1 1 d . . . O1 O 0.5896(2) 0.5198(2) 0.5305(2) 0.0238(5) Uani 1 1 d D . . H1 H 0.649(3) 0.550(4) 0.500(3) 0.029 Uiso 1 1 d D . . N1 N 0.3780(3) 0.4060(3) 0.8052(3) 0.0302(7) Uani 1 1 d . . . C1 C 0.2703(4) 0.4649(3) 0.7362(3) 0.0334(9) Uani 1 1 d . . . H1A H 0.2032 0.4692 0.7796 0.040 Uiso 1 1 calc R . . H1B H 0.2522 0.4243 0.7004 0.040 Uiso 1 1 calc R . . C2 C 0.2845(3) 0.5784(3) 0.6543(3) 0.0295(8) Uani 1 1 d . . . H2A H 0.2201 0.6085 0.6000 0.035 Uiso 1 1 calc R . . H2B H 0.2802 0.6255 0.6877 0.035 Uiso 1 1 calc R . . O2 O 0.3935(2) 0.5756(2) 0.6079(2) 0.0273(6) Uani 1 1 d . . . C3 C 0.3995(4) 0.2907(3) 0.8300(3) 0.0335(9) Uani 1 1 d . . . H3A H 0.3277 0.2591 0.8579 0.040 Uiso 1 1 calc R . . H3B H 0.4638 0.2506 0.8843 0.040 Uiso 1 1 calc R . . C4 C 0.4327(4) 0.2803(3) 0.7323(3) 0.0319(8) Uani 1 1 d . . . H4A H 0.4614 0.2038 0.7517 0.038 Uiso 1 1 calc R . . H4B H 0.3625 0.3057 0.6844 0.038 Uiso 1 1 calc R . . O3 O 0.5208(2) 0.3416(2) 0.6816(2) 0.0273(5) Uani 1 1 d . . . C5 C 0.3721(4) 0.4139(4) 0.9031(3) 0.0347(9) Uani 1 1 d . . . H5A H 0.4381 0.3631 0.9516 0.042 Uiso 1 1 calc R . . H5B H 0.2976 0.3932 0.9369 0.042 Uiso 1 1 calc R . . C6 C 0.3787(4) 0.5271(4) 0.8822(4) 0.0353(9) Uani 1 1 d . . . H6A H 0.3028 0.5751 0.8512 0.042 Uiso 1 1 calc R . . H6B H 0.3963 0.5277 0.9482 0.042 Uiso 1 1 calc R . . O4 O 0.4715(3) 0.5629(3) 0.8103(2) 0.0349(6) Uani 1 1 d D . . H4 H 0.507(4) 0.607(4) 0.829(4) 0.042 Uiso 1 1 d D . . O5 O 0.5074(2) 0.7420(2) 0.4588(2) 0.0303(6) Uani 1 1 d . . . O6 O 0.6084(2) 0.6577(2) 0.6147(2) 0.0307(6) Uani 1 1 d . . . C7 C 0.5749(3) 0.7391(3) 0.5287(3) 0.0302(8) Uani 1 1 d . . . C8 C 0.6154(3) 0.8424(3) 0.5030(3) 0.0284(8) Uani 1 1 d . . . C9 C 0.6966(4) 0.8450(4) 0.5704(4) 0.0373(9) Uani 1 1 d . . . H9A H 0.7293 0.7804 0.6302 0.045 Uiso 1 1 calc R . . C10 C 0.7294(4) 0.9409(4) 0.5502(4) 0.0421(10) Uani 1 1 d . . . H10A H 0.7841 0.9418 0.5969 0.051 Uiso 1 1 calc R . . C11 C 0.6838(4) 1.0367(4) 0.4628(4) 0.0387(10) Uani 1 1 d . . . C12 C 0.6043(4) 1.0338(3) 0.3951(4) 0.0386(10) Uani 1 1 d . . . H12A H 0.5727 1.0983 0.3348 0.046 Uiso 1 1 calc R . . C13 C 0.5710(4) 0.9377(4) 0.4148(4) 0.0348(9) Uani 1 1 d . . . H13A H 0.5170 0.9368 0.3676 0.042 Uiso 1 1 calc R . . C14 C 0.7168(5) 1.1424(4) 0.4440(5) 0.0558(14) Uani 1 1 d . . . H14A H 0.6822 1.1999 0.3763 0.084 Uiso 1 1 calc R . . H14B H 0.8026 1.1367 0.4436 0.084 Uiso 1 1 calc R . . H14C H 0.6869 1.1591 0.4998 0.084 Uiso 1 1 calc R . . O7 O 0.2669(2) 0.6898(2) 0.4109(2) 0.0314(6) Uani 1 1 d . . . O8 O 0.2478(2) 0.6154(2) 0.3065(2) 0.0315(6) Uani 1 1 d . . . C15 C 0.2108(3) 0.6775(3) 0.3436(3) 0.0300(8) Uani 1 1 d . . . C16 C 0.0904(3) 0.7435(3) 0.3087(3) 0.0321(8) Uani 1 1 d . . . C17 C 0.0373(4) 0.8038(4) 0.3556(4) 0.0418(10) Uani 1 1 d . . . H17A H 0.0772 0.8032 0.4120 0.050 Uiso 1 1 calc R . . C18 C -0.0741(4) 0.8652(4) 0.3209(4) 0.0474(12) Uani 1 1 d . . . H18A H -0.1099 0.9051 0.3546 0.057 Uiso 1 1 calc R . . C19 C -0.1332(4) 0.8689(4) 0.2381(4) 0.0418(10) Uani 1 1 d . . . C20 C -0.0788(4) 0.8099(4) 0.1901(4) 0.0461(11) Uani 1 1 d . . . H20A H -0.1174 0.8128 0.1319 0.055 Uiso 1 1 calc R . . C21 C 0.0312(4) 0.7467(4) 0.2256(4) 0.0435(11) Uani 1 1 d . . . H21A H 0.0661 0.7054 0.1929 0.052 Uiso 1 1 calc R . . C22 C -0.2534(4) 0.9370(5) 0.1991(5) 0.0574(14) Uani 1 1 d . . . H22A H -0.3078 0.9145 0.2564 0.086 Uiso 1 1 calc R . . H22B H -0.2825 0.9278 0.1418 0.086 Uiso 1 1 calc R . . H22C H -0.2478 1.0129 0.1739 0.086 Uiso 1 1 calc R . . O9 O 0.6402(2) 0.3482(2) 0.8843(2) 0.0320(6) Uani 1 1 d . . . O10 O 0.7198(2) 0.4949(2) 0.8205(2) 0.0321(6) Uani 1 1 d . . . C23 C 0.7120(3) 0.3995(3) 0.8938(3) 0.0289(8) Uani 1 1 d . . . C24 C 0.7876(3) 0.3505(3) 0.9912(3) 0.0322(8) Uani 1 1 d . . . C25 C 0.7685(4) 0.2552(4) 1.0752(4) 0.0423(10) Uani 1 1 d . . . H25A H 0.7101 0.2187 1.0688 0.051 Uiso 1 1 calc R . . C26 C 0.8334(5) 0.2118(4) 1.1692(4) 0.0487(12) Uani 1 1 d . . . H26A H 0.8193 0.1459 1.2260 0.058 Uiso 1 1 calc R . . C27 C 0.9190(4) 0.2642(4) 1.1807(4) 0.0418(10) Uani 1 1 d . . . C28 C 0.9381(4) 0.3583(5) 1.0961(4) 0.0488(12) Uani 1 1 d . . . H28A H 0.9971 0.3945 1.1022 0.059 Uiso 1 1 calc R . . C29 C 0.8742(4) 0.4021(4) 1.0023(4) 0.0422(10) Uani 1 1 d . . . H29A H 0.8895 0.4674 0.9453 0.051 Uiso 1 1 calc R . . C30 C 0.9853(5) 0.2200(5) 1.2847(4) 0.0567(14) Uani 1 1 d . . . H30A H 1.0625 0.2427 1.2727 0.085 Uiso 1 1 calc R . . H30B H 0.9957 0.1412 1.3202 0.085 Uiso 1 1 calc R . . H30C H 0.9406 0.2475 1.3284 0.085 Uiso 1 1 calc R . . O11 O 0.7423(3) 0.6663(3) 0.8407(3) 0.0411(7) Uani 1 1 d . . . H11 H 0.7248 0.6230 0.8218 0.062 Uiso 1 1 calc R . . O12 O 0.5463(3) 0.7158(3) 0.8332(3) 0.0452(8) Uani 1 1 d . . . C31 C 0.6450(4) 0.7304(4) 0.8423(3) 0.0356(9) Uani 1 1 d . . . C32 C 0.6665(4) 0.8214(4) 0.8587(3) 0.0342(9) Uani 1 1 d . . . C33 C 0.5696(4) 0.8891(4) 0.8675(4) 0.0390(10) Uani 1 1 d . . . H33A H 0.4924 0.8762 0.8629 0.047 Uiso 1 1 calc R . . C34 C 0.5850(4) 0.9746(4) 0.8828(4) 0.0440(11) Uani 1 1 d . . . H34A H 0.5182 1.0189 0.8904 0.053 Uiso 1 1 calc R . . C35 C 0.6968(5) 0.9969(4) 0.8875(4) 0.0459(11) Uani 1 1 d . . . C36 C 0.7924(5) 0.9286(5) 0.8807(5) 0.0572(14) Uani 1 1 d . . . H36A H 0.8694 0.9418 0.8851 0.069 Uiso 1 1 calc R . . C37 C 0.7782(4) 0.8406(4) 0.8676(5) 0.0480(12) Uani 1 1 d . . . H37A H 0.8454 0.7936 0.8647 0.058 Uiso 1 1 calc R . . C38 C 0.7117(6) 1.0948(5) 0.8980(5) 0.0592(14) Uani 1 1 d . . . H38A H 0.7927 1.0867 0.9218 0.089 Uiso 1 1 calc R . . H38B H 0.6573 1.1018 0.9489 0.089 Uiso 1 1 calc R . . H38C H 0.6947 1.1593 0.8299 0.089 Uiso 1 1 calc R . . N41 N 0.8317(4) 0.5780(5) 0.4612(4) 0.0672(14) Uani 1 1 d . . . C41 C 0.8760(4) 0.5764(5) 0.5294(5) 0.0520(13) Uani 1 1 d . . . C42 C 0.9313(6) 0.5718(7) 0.6201(6) 0.0726(19) Uani 1 1 d . . . H42A H 0.8784 0.5485 0.6786 0.109 Uiso 1 1 calc R . . H42B H 0.9475 0.6433 0.6030 0.109 Uiso 1 1 calc R . . H42C H 1.0052 0.5205 0.6399 0.109 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.02790(10) 0.02179(10) 0.02411(10) -0.01219(7) -0.00195(6) -0.00280(6) Fe1 0.0288(3) 0.0215(3) 0.0252(3) -0.0122(2) -0.0027(2) -0.0023(2) O1 0.0282(12) 0.0228(13) 0.0215(13) -0.0110(11) -0.0017(10) -0.0047(10) N1 0.0350(16) 0.0267(17) 0.0288(18) -0.0135(15) -0.0022(14) -0.0024(13) C1 0.0338(19) 0.033(2) 0.032(2) -0.0138(18) -0.0014(16) -0.0078(16) C2 0.0280(18) 0.030(2) 0.030(2) -0.0141(17) 0.0006(15) -0.0018(15) O2 0.0249(12) 0.0280(14) 0.0278(14) -0.0135(12) -0.0026(10) 0.0009(10) C3 0.041(2) 0.024(2) 0.033(2) -0.0103(17) 0.0031(17) -0.0091(16) C4 0.040(2) 0.026(2) 0.031(2) -0.0129(17) 0.0016(16) -0.0103(16) O3 0.0343(13) 0.0231(13) 0.0275(14) -0.0132(11) 0.0002(11) -0.0079(11) C5 0.039(2) 0.037(2) 0.029(2) -0.0158(18) 0.0018(17) -0.0060(17) C6 0.037(2) 0.041(2) 0.033(2) -0.0218(19) 0.0040(17) -0.0039(18) O4 0.0392(15) 0.0373(17) 0.0394(17) -0.0261(14) 0.0087(13) -0.0109(13) O5 0.0394(14) 0.0253(14) 0.0291(15) -0.0144(12) -0.0034(11) -0.0065(11) O6 0.0421(15) 0.0209(13) 0.0284(15) -0.0095(12) -0.0044(12) -0.0084(11) C7 0.0333(19) 0.030(2) 0.031(2) -0.0174(18) 0.0014(16) -0.0045(16) C8 0.0329(18) 0.0244(19) 0.031(2) -0.0145(17) 0.0017(15) -0.0076(15) C9 0.040(2) 0.030(2) 0.042(2) -0.0164(19) -0.0042(18) -0.0057(17) C10 0.045(2) 0.037(2) 0.053(3) -0.025(2) -0.004(2) -0.0142(19) C11 0.045(2) 0.029(2) 0.047(3) -0.021(2) 0.012(2) -0.0127(18) C12 0.050(2) 0.023(2) 0.038(2) -0.0103(18) 0.0049(19) -0.0068(18) C13 0.041(2) 0.031(2) 0.034(2) -0.0164(19) -0.0012(17) -0.0056(17) C14 0.062(3) 0.037(3) 0.078(4) -0.032(3) 0.016(3) -0.021(2) O7 0.0317(13) 0.0325(15) 0.0325(15) -0.0194(13) -0.0060(11) 0.0029(11) O8 0.0270(13) 0.0341(16) 0.0365(16) -0.0210(13) -0.0042(11) 0.0021(11) C15 0.0300(18) 0.029(2) 0.029(2) -0.0125(17) -0.0011(15) -0.0026(15) C16 0.0291(18) 0.031(2) 0.036(2) -0.0173(18) -0.0028(16) -0.0012(16) C17 0.040(2) 0.046(3) 0.044(3) -0.029(2) -0.0069(19) 0.0033(19) C18 0.042(2) 0.047(3) 0.056(3) -0.031(3) -0.003(2) 0.008(2) C19 0.032(2) 0.040(3) 0.050(3) -0.020(2) -0.0044(19) -0.0002(18) C20 0.035(2) 0.056(3) 0.051(3) -0.030(3) -0.014(2) 0.004(2) C21 0.039(2) 0.054(3) 0.048(3) -0.035(3) -0.008(2) 0.003(2) C22 0.035(2) 0.053(3) 0.081(4) -0.033(3) -0.014(2) 0.009(2) O9 0.0391(14) 0.0268(14) 0.0287(15) -0.0119(12) -0.0056(12) -0.0039(12) O10 0.0387(14) 0.0278(15) 0.0300(15) -0.0144(12) -0.0021(12) -0.0026(11) C23 0.0320(18) 0.028(2) 0.029(2) -0.0164(17) -0.0006(15) 0.0014(15) C24 0.0335(19) 0.028(2) 0.034(2) -0.0159(18) -0.0002(16) 0.0018(16) C25 0.053(3) 0.036(2) 0.038(3) -0.015(2) -0.009(2) -0.013(2) C26 0.060(3) 0.042(3) 0.038(3) -0.013(2) -0.010(2) -0.010(2) C27 0.035(2) 0.049(3) 0.042(3) -0.023(2) -0.0070(19) -0.0010(19) C28 0.036(2) 0.055(3) 0.052(3) -0.020(3) -0.009(2) -0.013(2) C29 0.035(2) 0.040(3) 0.044(3) -0.012(2) -0.0038(19) -0.0099(18) C30 0.044(3) 0.077(4) 0.042(3) -0.022(3) -0.012(2) -0.010(3) O11 0.0467(17) 0.0361(17) 0.0479(19) -0.0267(16) -0.0037(14) -0.0026(13) O12 0.0447(17) 0.047(2) 0.059(2) -0.0359(18) 0.0026(15) -0.0118(15) C31 0.048(2) 0.031(2) 0.026(2) -0.0124(18) 0.0013(17) -0.0055(18) C32 0.042(2) 0.031(2) 0.030(2) -0.0144(18) 0.0006(17) -0.0066(17) C33 0.042(2) 0.033(2) 0.043(3) -0.020(2) -0.0031(19) -0.0032(18) C34 0.049(3) 0.029(2) 0.051(3) -0.018(2) -0.002(2) -0.0014(19) C35 0.061(3) 0.033(2) 0.044(3) -0.018(2) -0.001(2) -0.012(2) C36 0.046(3) 0.060(4) 0.086(4) -0.048(3) 0.005(3) -0.017(2) C37 0.041(2) 0.047(3) 0.068(4) -0.037(3) 0.004(2) -0.008(2) C38 0.076(4) 0.041(3) 0.069(4) -0.031(3) 0.006(3) -0.020(3) N41 0.058(3) 0.088(4) 0.058(3) -0.031(3) -0.002(2) -0.029(3) C41 0.041(2) 0.060(3) 0.057(3) -0.027(3) 0.003(2) -0.015(2) C42 0.064(4) 0.106(6) 0.075(4) -0.060(4) -0.001(3) -0.028(4) _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 O2 2.320(3) . ? Dy1 O3 2.322(3) . ? Dy1 O6 2.381(3) . ? Dy1 O1 2.384(3) . ? Dy1 O8 2.413(3) 2_666 ? Dy1 O4 2.413(3) . ? Dy1 O9 2.429(3) . ? Dy1 O10 2.559(3) . ? Dy1 N1 2.619(3) . ? Dy1 Fe1 3.4208(6) 2_666 ? Dy1 Fe1 3.4279(7) . ? Fe1 O2 1.950(3) . ? Fe1 O3 1.971(3) 2_666 ? Fe1 O5 2.002(3) . ? Fe1 O7 2.006(3) . ? Fe1 O1 2.054(3) 2_666 ? Fe1 O1 2.064(3) . ? Fe1 Dy1 3.4208(6) 2_666 ? O1 Fe1 2.054(3) 2_666 ? O1 H1 0.87(3) . ? N1 C5 1.471(5) . ? N1 C1 1.488(5) . ? N1 C3 1.489(5) . ? C1 C2 1.525(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 O2 1.405(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.518(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O3 1.405(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? O3 Fe1 1.971(3) 2_666 ? C5 C6 1.514(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 O4 1.444(5) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? O4 H4 0.95(3) . ? O5 C7 1.284(5) . ? O6 C7 1.257(5) . ? C7 C8 1.494(5) . ? C8 C13 1.391(6) . ? C8 C9 1.398(6) . ? C9 C10 1.375(6) . ? C9 H9A 0.9500 . ? C10 C11 1.393(7) . ? C10 H10A 0.9500 . ? C11 C12 1.389(7) . ? C11 C14 1.514(6) . ? C12 C13 1.382(6) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? O7 C15 1.284(5) . ? O8 C15 1.249(5) . ? O8 Dy1 2.413(3) 2_666 ? C15 C16 1.499(5) . ? C16 C17 1.385(6) . ? C16 C21 1.387(6) . ? C17 C18 1.391(6) . ? C17 H17A 0.9500 . ? C18 C19 1.379(7) . ? C18 H18A 0.9500 . ? C19 C20 1.388(7) . ? C19 C22 1.512(6) . ? C20 C21 1.387(6) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? O9 C23 1.245(5) . ? O10 C23 1.289(5) . ? C23 C24 1.487(6) . ? C24 C25 1.379(6) . ? C24 C29 1.392(6) . ? C25 C26 1.392(7) . ? C25 H25A 0.9500 . ? C26 C27 1.393(7) . ? C26 H26A 0.9500 . ? C27 C28 1.374(8) . ? C27 C30 1.514(7) . ? C28 C29 1.383(7) . ? C28 H28A 0.9500 . ? C29 H29A 0.9500 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? O11 C31 1.332(5) . ? O11 H11 0.8400 . ? O12 C31 1.216(5) . ? C31 C32 1.485(6) . ? C32 C37 1.385(6) . ? C32 C33 1.395(6) . ? C33 C34 1.379(7) . ? C33 H33A 0.9500 . ? C34 C35 1.391(7) . ? C34 H34A 0.9500 . ? C35 C36 1.378(8) . ? C35 C38 1.512(7) . ? C36 C37 1.392(7) . ? C36 H36A 0.9500 . ? C37 H37A 0.9500 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? N41 C41 1.120(7) . ? C41 C42 1.453(8) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 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 O2 Dy1 O3 83.72(10) . . ? O2 Dy1 O6 77.35(10) . . ? O3 Dy1 O6 141.01(10) . . ? O2 Dy1 O1 68.69(9) . . ? O3 Dy1 O1 69.47(9) . . ? O6 Dy1 O1 71.94(9) . . ? O2 Dy1 O8 138.49(10) . 2_666 ? O3 Dy1 O8 74.52(10) . 2_666 ? O6 Dy1 O8 97.92(10) . 2_666 ? O1 Dy1 O8 70.67(9) . 2_666 ? O2 Dy1 O4 79.20(10) . . ? O3 Dy1 O4 131.42(10) . . ? O6 Dy1 O4 78.01(10) . . ? O1 Dy1 O4 139.76(10) . . ? O8 Dy1 O4 140.93(10) 2_666 . ? O2 Dy1 O9 143.27(10) . . ? O3 Dy1 O9 89.35(10) . . ? O6 Dy1 O9 125.45(9) . . ? O1 Dy1 O9 141.04(9) . . ? O8 Dy1 O9 72.33(10) 2_666 . ? O4 Dy1 O9 78.70(10) . . ? O2 Dy1 O10 141.06(9) . . ? O3 Dy1 O10 134.74(9) . . ? O6 Dy1 O10 73.49(9) . . ? O1 Dy1 O10 123.57(9) . . ? O8 Dy1 O10 71.61(9) 2_666 . ? O4 Dy1 O10 70.01(10) . . ? O9 Dy1 O10 52.26(9) . . ? O2 Dy1 N1 67.88(10) . . ? O3 Dy1 N1 67.36(10) . . ? O6 Dy1 N1 131.97(10) . . ? O1 Dy1 N1 120.61(10) . . ? O8 Dy1 N1 130.08(10) 2_666 . ? O4 Dy1 N1 64.06(10) . . ? O9 Dy1 N1 76.14(10) . . ? O10 Dy1 N1 115.73(10) . . ? O2 Fe1 O3 175.45(11) . 2_666 ? O2 Fe1 O5 91.57(12) . . ? O3 Fe1 O5 91.74(12) 2_666 . ? O2 Fe1 O7 92.09(12) . . ? O3 Fe1 O7 90.10(12) 2_666 . ? O5 Fe1 O7 104.74(12) . . ? O2 Fe1 O1 92.40(11) . 2_666 ? O3 Fe1 O1 83.54(11) 2_666 2_666 ? O5 Fe1 O1 162.92(11) . 2_666 ? O7 Fe1 O1 91.71(11) . 2_666 ? O2 Fe1 O1 82.75(11) . . ? O3 Fe1 O1 94.22(11) 2_666 . ? O5 Fe1 O1 88.30(11) . . ? O7 Fe1 O1 166.15(12) . . ? O1 Fe1 O1 75.74(11) 2_666 . ? O2 Fe1 Dy1 135.33(8) . 2_666 ? O3 Fe1 Dy1 40.88(8) 2_666 2_666 ? O5 Fe1 Dy1 132.11(9) . 2_666 ? O7 Fe1 Dy1 85.79(8) . 2_666 ? O1 Fe1 Dy1 43.23(7) 2_666 2_666 ? O1 Fe1 Dy1 88.87(7) . 2_666 ? O2 Fe1 Dy1 40.48(7) . . ? O3 Fe1 Dy1 137.00(8) 2_666 . ? O5 Fe1 Dy1 83.44(8) . . ? O7 Fe1 Dy1 132.51(9) . . ? O1 Fe1 Dy1 88.84(7) 2_666 . ? O1 Fe1 Dy1 43.12(7) . . ? Dy1 Fe1 Dy1 123.336(17) 2_666 . ? Fe1 O1 Fe1 104.26(11) 2_666 . ? Fe1 O1 Dy1 100.61(11) 2_666 . ? Fe1 O1 Dy1 100.60(10) . . ? Fe1 O1 H1 121(3) 2_666 . ? Fe1 O1 H1 111(3) . . ? Dy1 O1 H1 117(3) . . ? C5 N1 C1 112.4(3) . . ? C5 N1 C3 109.5(3) . . ? C1 N1 C3 110.9(3) . . ? C5 N1 Dy1 108.5(2) . . ? C1 N1 Dy1 110.7(2) . . ? C3 N1 Dy1 104.5(2) . . ? N1 C1 C2 112.2(3) . . ? N1 C1 H1A 109.2 . . ? C2 C1 H1A 109.2 . . ? N1 C1 H1B 109.2 . . ? C2 C1 H1B 109.2 . . ? H1A C1 H1B 107.9 . . ? O2 C2 C1 109.7(3) . . ? O2 C2 H2A 109.7 . . ? C1 C2 H2A 109.7 . . ? O2 C2 H2B 109.7 . . ? C1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? C2 O2 Fe1 131.7(2) . . ? C2 O2 Dy1 121.2(2) . . ? Fe1 O2 Dy1 106.47(11) . . ? N1 C3 C4 110.2(3) . . ? N1 C3 H3A 109.6 . . ? C4 C3 H3A 109.6 . . ? N1 C3 H3B 109.6 . . ? C4 C3 H3B 109.6 . . ? H3A C3 H3B 108.1 . . ? O3 C4 C3 110.0(3) . . ? O3 C4 H4A 109.7 . . ? C3 C4 H4A 109.7 . . ? O3 C4 H4B 109.7 . . ? C3 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? C4 O3 Fe1 123.6(2) . 2_666 ? C4 O3 Dy1 124.5(2) . . ? Fe1 O3 Dy1 105.37(11) 2_666 . ? N1 C5 C6 111.0(4) . . ? N1 C5 H5A 109.4 . . ? C6 C5 H5A 109.4 . . ? N1 C5 H5B 109.4 . . ? C6 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? O4 C6 C5 106.9(3) . . ? O4 C6 H6A 110.3 . . ? C5 C6 H6A 110.3 . . ? O4 C6 H6B 110.3 . . ? C5 C6 H6B 110.3 . . ? H6A C6 H6B 108.6 . . ? C6 O4 Dy1 126.7(2) . . ? C6 O4 H4 106(3) . . ? Dy1 O4 H4 124(3) . . ? C7 O5 Fe1 128.3(3) . . ? C7 O6 Dy1 136.0(2) . . ? O6 C7 O5 125.5(4) . . ? O6 C7 C8 118.9(3) . . ? O5 C7 C8 115.6(4) . . ? C13 C8 C9 118.7(4) . . ? C13 C8 C7 121.4(4) . . ? C9 C8 C7 119.8(4) . . ? C10 C9 C8 120.1(4) . . ? C10 C9 H9A 120.0 . . ? C8 C9 H9A 120.0 . . ? C9 C10 C11 121.3(4) . . ? C9 C10 H10A 119.4 . . ? C11 C10 H10A 119.4 . . ? C12 C11 C10 118.6(4) . . ? C12 C11 C14 120.7(5) . . ? C10 C11 C14 120.7(5) . . ? C13 C12 C11 120.5(4) . . ? C13 C12 H12A 119.8 . . ? C11 C12 H12A 119.8 . . ? C12 C13 C8 120.8(4) . . ? C12 C13 H13A 119.6 . . ? C8 C13 H13A 119.6 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C15 O7 Fe1 125.1(3) . . ? C15 O8 Dy1 137.2(2) . 2_666 ? O8 C15 O7 125.6(4) . . ? O8 C15 C16 118.3(4) . . ? O7 C15 C16 116.1(4) . . ? C17 C16 C21 118.7(4) . . ? C17 C16 C15 121.7(4) . . ? C21 C16 C15 119.5(4) . . ? C16 C17 C18 120.5(4) . . ? C16 C17 H17A 119.8 . . ? C18 C17 H17A 119.8 . . ? C19 C18 C17 121.0(5) . . ? C19 C18 H18A 119.5 . . ? C17 C18 H18A 119.5 . . ? C18 C19 C20 118.3(4) . . ? C18 C19 C22 121.0(5) . . ? C20 C19 C22 120.7(5) . . ? C21 C20 C19 121.1(4) . . ? C21 C20 H20A 119.5 . . ? C19 C20 H20A 119.5 . . ? C16 C21 C20 120.3(4) . . ? C16 C21 H21A 119.8 . . ? C20 C21 H21A 119.8 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C23 O9 Dy1 97.2(2) . . ? C23 O10 Dy1 90.0(2) . . ? O9 C23 O10 120.4(4) . . ? O9 C23 C24 119.3(4) . . ? O10 C23 C24 120.2(4) . . ? C25 C24 C29 118.4(4) . . ? C25 C24 C23 120.3(4) . . ? C29 C24 C23 121.2(4) . . ? C24 C25 C26 121.0(4) . . ? C24 C25 H25A 119.5 . . ? C26 C25 H25A 119.5 . . ? C25 C26 C27 120.6(5) . . ? C25 C26 H26A 119.7 . . ? C27 C26 H26A 119.7 . . ? C28 C27 C26 117.8(4) . . ? C28 C27 C30 121.5(5) . . ? C26 C27 C30 120.6(5) . . ? C27 C28 C29 122.0(5) . . ? C27 C28 H28A 119.0 . . ? C29 C28 H28A 119.0 . . ? C28 C29 C24 120.1(5) . . ? C28 C29 H29A 119.9 . . ? C24 C29 H29A 119.9 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C31 O11 H11 109.5 . . ? O12 C31 O11 123.6(4) . . ? O12 C31 C32 122.0(4) . . ? O11 C31 C32 114.4(4) . . ? C37 C32 C33 118.8(4) . . ? C37 C32 C31 123.0(4) . . ? C33 C32 C31 118.3(4) . . ? C34 C33 C32 120.4(4) . . ? C34 C33 H33A 119.8 . . ? C32 C33 H33A 119.8 . . ? C33 C34 C35 121.1(5) . . ? C33 C34 H34A 119.5 . . ? C35 C34 H34A 119.5 . . ? C36 C35 C34 118.2(5) . . ? C36 C35 C38 121.4(5) . . ? C34 C35 C38 120.4(5) . . ? C35 C36 C37 121.3(5) . . ? C35 C36 H36A 119.4 . . ? C37 C36 H36A 119.4 . . ? C32 C37 C36 120.1(5) . . ? C32 C37 H37A 119.9 . . ? C36 C37 H37A 119.9 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N41 C41 C42 178.1(7) . . ? 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 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 N41 0.87(3) 2.21(3) 3.043(6) 162(4) . O4 H4 O12 0.95(3) 1.71(4) 2.637(4) 163(5) . O11 H11 O10 0.84 1.85 2.652(4) 159.9 . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.498 _refine_diff_density_min -2.104 _refine_diff_density_rms 0.146 _database_code_depnum_ccdc_archive 'CCDC 866240' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_am3cbdy _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H52 Dy2 Fe2 N8 O20, 2(C2 H3 N)' _chemical_formula_sum 'C64 H58 Dy2 Fe2 N10 O20' _chemical_formula_weight 1723.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.700(2) _cell_length_b 12.915(3) _cell_length_c 14.427(3) _cell_angle_alpha 87.159(17) _cell_angle_beta 74.068(18) _cell_angle_gamma 73.135(17) _cell_volume 1662.2(6) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5918 _cell_measurement_theta_min 1.47 _cell_measurement_theta_max 25.65 _exptl_crystal_description plate _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.722 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 856 _exptl_absorpt_coefficient_mu 2.731 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.701 _exptl_absorpt_correction_T_max 0.801 _exptl_absorpt_process_details ; XPREP in SHELXTL 6.14 (BrukerAXS Inc., 2003) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean 6.667 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15190 _diffrn_reflns_av_R_equivalents 0.0975 _diffrn_reflns_av_unetI/netI 0.1302 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 25.35 _reflns_number_total 6039 _reflns_number_gt 3726 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'WinXpose 1.6.8 (Stoe & Cie GmbH, 2004)' _computing_cell_refinement 'X-Area 1.38 (Stoe & Cie GmbH, 2006)' _computing_data_reduction 'X-Area 1.38 (Stoe & Cie GmbH, 2006)' _computing_structure_solution 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_structure_refinement 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_molecular_graphics 'Diamond 2.1 (Crystal Impact, 1998)' _computing_publication_material 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _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. O-H distances were restrained: DFIX 0.92 0.04 O1 H1 O4 H4 DFIX 2.00 0.04 H4 N31 ; _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^)+(0.0648P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6039 _refine_ls_number_parameters 449 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1076 _refine_ls_R_factor_gt 0.0616 _refine_ls_wR_factor_ref 0.1467 _refine_ls_wR_factor_gt 0.1311 _refine_ls_goodness_of_fit_ref 0.984 _refine_ls_restrained_S_all 0.984 _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 Dy1 Dy 0.70891(7) 0.32132(4) 0.35603(4) 0.03422(16) Uani 1 1 d . . . Fe1 Fe 0.55476(17) 0.43057(11) 0.58639(10) 0.0350(4) Uani 1 1 d . . . O1 O 0.4804(8) 0.4165(5) 0.4679(5) 0.0367(16) Uani 1 1 d D . . H1 H 0.394(7) 0.401(9) 0.489(7) 0.044 Uiso 1 1 d D . . N1 N 0.9395(10) 0.3928(6) 0.3129(5) 0.036(2) Uani 1 1 d . . . C1 C 1.0001(11) 0.3677(8) 0.4003(7) 0.038(2) Uani 1 1 d . . . H1A H 1.0412 0.2884 0.4039 0.045 Uiso 1 1 calc R . . H1B H 1.0824 0.4007 0.3939 0.045 Uiso 1 1 calc R . . C2 C 0.8785(12) 0.4111(9) 0.4912(7) 0.041(3) Uani 1 1 d . . . H2A H 0.9171 0.3874 0.5479 0.049 Uiso 1 1 calc R . . H2B H 0.8478 0.4912 0.4919 0.049 Uiso 1 1 calc R . . O2 O 0.7522(8) 0.3734(5) 0.4973(5) 0.0361(16) Uani 1 1 d . . . C3 C 0.8986(14) 0.5119(8) 0.2975(8) 0.046(3) Uani 1 1 d . . . H3A H 0.9787 0.5285 0.2450 0.055 Uiso 1 1 calc R . . H3B H 0.8915 0.5506 0.3570 0.055 Uiso 1 1 calc R . . C4 C 0.7511(13) 0.5527(9) 0.2717(8) 0.045(3) Uani 1 1 d . . . H4A H 0.7142 0.6326 0.2787 0.054 Uiso 1 1 calc R . . H4B H 0.7647 0.5317 0.2040 0.054 Uiso 1 1 calc R . . O3 O 0.6464(8) 0.5061(5) 0.3348(5) 0.0381(17) Uani 1 1 d . . . C5 C 1.0498(13) 0.3312(9) 0.2276(7) 0.045(3) Uani 1 1 d . . . H5A H 1.0843 0.2541 0.2433 0.054 Uiso 1 1 calc R . . H5B H 1.1378 0.3595 0.2090 0.054 Uiso 1 1 calc R . . C6 C 0.9797(14) 0.3406(10) 0.1433(8) 0.055(3) Uani 1 1 d . . . H6A H 0.9662 0.4142 0.1173 0.066 Uiso 1 1 calc R . . H6B H 1.0454 0.2875 0.0910 0.066 Uiso 1 1 calc R . . O4 O 0.8360(9) 0.3193(6) 0.1798(5) 0.0464(19) Uani 1 1 d D . . H4 H 0.836(13) 0.260(6) 0.144(6) 0.056 Uiso 1 1 d D . . O5 O 0.6312(9) 0.2001(5) 0.4765(5) 0.0427(18) Uani 1 1 d . . . O6 O 0.5500(9) 0.2806(5) 0.6268(5) 0.0417(18) Uani 1 1 d . . . C7 C 0.5900(13) 0.1999(8) 0.5683(8) 0.041(3) Uani 1 1 d . . . C8 C 0.5886(12) 0.0918(8) 0.6120(8) 0.039(2) Uani 1 1 d . . . C9 C 0.6417(13) -0.0009(8) 0.5518(8) 0.041(3) Uani 1 1 d . . . H9A H 0.6796 0.0043 0.4842 0.049 Uiso 1 1 calc R . . C10 C 0.6387(14) -0.1008(8) 0.5916(8) 0.046(3) Uani 1 1 d . . . C11 C 0.5893(17) -0.1104(9) 0.6900(9) 0.064(4) Uani 1 1 d . . . H11A H 0.5896 -0.1793 0.7164 0.076 Uiso 1 1 calc R . . C12 C 0.5397(19) -0.0196(10) 0.7499(9) 0.073(5) Uani 1 1 d . . . H12A H 0.5039 -0.0255 0.8176 0.088 Uiso 1 1 calc R . . C13 C 0.5420(15) 0.0801(8) 0.7113(8) 0.052(3) Uani 1 1 d . . . H13A H 0.5112 0.1419 0.7532 0.063 Uiso 1 1 calc R . . C14 C 0.6918(14) -0.1963(8) 0.5285(8) 0.046(3) Uani 1 1 d . . . N2 N 0.7341(13) -0.2746(8) 0.4820(8) 0.061(3) Uani 1 1 d . . . O7 O 0.5164(9) 0.3559(5) 0.2758(5) 0.0429(18) Uani 1 1 d . . . O8 O 0.3685(8) 0.5285(5) 0.3063(5) 0.0394(17) Uani 1 1 d . . . C15 C 0.4308(13) 0.4405(9) 0.2554(8) 0.040(3) Uani 1 1 d . . . C16 C 0.3922(12) 0.4385(8) 0.1612(7) 0.035(2) Uani 1 1 d . . . C17 C 0.4345(12) 0.3384(9) 0.1105(7) 0.041(2) Uani 1 1 d . . . H17A H 0.4918 0.2748 0.1334 0.049 Uiso 1 1 calc R . . C18 C 0.3922(16) 0.3334(10) 0.0273(8) 0.055(3) Uani 1 1 d . . . C19 C 0.3150(16) 0.4261(11) -0.0096(9) 0.062(4) Uani 1 1 d . . . H19A H 0.2854 0.4216 -0.0664 0.075 Uiso 1 1 calc R . . C20 C 0.2811(16) 0.5248(11) 0.0364(9) 0.064(4) Uani 1 1 d . . . H20A H 0.2324 0.5888 0.0093 0.077 Uiso 1 1 calc R . . C21 C 0.3174(13) 0.5317(9) 0.1223(8) 0.048(3) Uani 1 1 d . . . H21A H 0.2913 0.6000 0.1544 0.057 Uiso 1 1 calc R . . C22 C 0.4242(17) 0.2293(11) -0.0191(10) 0.067(4) Uani 1 1 d . . . N3 N 0.4516(18) 0.1444(11) -0.0508(10) 0.097(5) Uani 1 1 d . . . O9 O 0.7453(9) 0.1473(5) 0.2787(5) 0.0407(17) Uani 1 1 d . . . O10 O 0.9170(9) 0.1612(5) 0.3491(6) 0.0469(19) Uani 1 1 d . . . C23 C 0.8579(14) 0.1054(9) 0.3100(8) 0.044(3) Uani 1 1 d . . . C24 C 0.9284(13) -0.0145(8) 0.3009(8) 0.041(3) Uani 1 1 d . . . C25 C 0.8867(13) -0.0751(8) 0.2406(8) 0.044(3) Uani 1 1 d . . . H25A H 0.8158 -0.0403 0.2065 0.053 Uiso 1 1 calc R . . C26 C 0.9508(14) -0.1872(8) 0.2315(8) 0.046(3) Uani 1 1 d . . . C27 C 1.0480(15) -0.2388(9) 0.2865(9) 0.055(3) Uani 1 1 d . . . H27A H 1.0900 -0.3152 0.2810 0.066 Uiso 1 1 calc R . . C28 C 1.0832(15) -0.1790(9) 0.3489(10) 0.059(3) Uani 1 1 d . . . H28A H 1.1486 -0.2139 0.3867 0.071 Uiso 1 1 calc R . . C29 C 1.0211(14) -0.0662(9) 0.3557(9) 0.055(3) Uani 1 1 d . . . H29A H 1.0439 -0.0250 0.3991 0.066 Uiso 1 1 calc R . . C30 C 0.9186(16) -0.2471(9) 0.1637(9) 0.057(3) Uani 1 1 d . . . N4 N 0.8951(15) -0.2963(9) 0.1074(8) 0.074(3) Uani 1 1 d . . . N31 N 0.8242(17) 0.1681(12) 0.0381(9) 0.090(4) Uani 1 1 d D . . C31 C 0.8148(19) 0.0974(15) -0.0036(12) 0.082(5) Uani 1 1 d . . . C32 C 0.806(2) 0.0070(15) -0.0568(14) 0.102(6) Uani 1 1 d . . . H32A H 0.7905 0.0312 -0.1196 0.153 Uiso 1 1 calc R . . H32B H 0.7220 -0.0190 -0.0200 0.153 Uiso 1 1 calc R . . H32C H 0.8994 -0.0519 -0.0665 0.153 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.0437(3) 0.0250(2) 0.0390(3) -0.00189(17) -0.0197(2) -0.0090(2) Fe1 0.0453(10) 0.0247(7) 0.0400(8) -0.0008(6) -0.0210(7) -0.0088(7) O1 0.045(4) 0.030(4) 0.044(4) 0.002(3) -0.025(4) -0.012(3) N1 0.050(6) 0.031(4) 0.032(4) -0.005(3) -0.017(4) -0.011(4) C1 0.032(6) 0.040(6) 0.050(6) -0.004(5) -0.021(5) -0.012(5) C2 0.044(7) 0.046(6) 0.043(6) 0.005(5) -0.024(5) -0.021(5) O2 0.043(4) 0.034(4) 0.039(4) -0.004(3) -0.023(3) -0.011(3) C3 0.057(8) 0.034(6) 0.053(7) 0.013(5) -0.020(6) -0.022(5) C4 0.062(8) 0.035(6) 0.046(6) 0.015(5) -0.024(6) -0.020(6) O3 0.047(4) 0.024(3) 0.045(4) 0.005(3) -0.017(4) -0.010(3) C5 0.040(7) 0.048(6) 0.040(6) -0.012(5) -0.005(5) -0.006(5) C6 0.062(8) 0.061(8) 0.039(6) -0.018(6) -0.007(6) -0.018(7) O4 0.046(5) 0.053(5) 0.042(4) -0.007(4) -0.014(4) -0.015(4) O5 0.057(5) 0.027(4) 0.046(4) 0.002(3) -0.018(4) -0.011(3) O6 0.054(5) 0.031(4) 0.046(4) -0.004(3) -0.022(4) -0.011(3) C7 0.049(7) 0.029(5) 0.052(7) 0.004(5) -0.022(6) -0.014(5) C8 0.048(7) 0.024(5) 0.049(6) 0.004(4) -0.021(5) -0.012(5) C9 0.052(7) 0.030(5) 0.051(6) 0.002(5) -0.027(5) -0.017(5) C10 0.070(8) 0.025(5) 0.055(7) -0.002(5) -0.029(6) -0.019(5) C11 0.109(12) 0.034(6) 0.051(7) 0.010(5) -0.023(7) -0.026(7) C12 0.126(14) 0.047(7) 0.046(7) 0.002(6) -0.015(8) -0.033(8) C13 0.084(9) 0.027(5) 0.047(7) 0.000(5) -0.021(6) -0.014(6) C14 0.062(8) 0.032(6) 0.054(7) -0.008(5) -0.032(6) -0.013(5) N2 0.067(7) 0.047(6) 0.077(7) -0.008(5) -0.034(6) -0.015(5) O7 0.060(5) 0.024(4) 0.048(4) -0.004(3) -0.033(4) 0.000(3) O8 0.051(5) 0.027(4) 0.043(4) -0.006(3) -0.022(4) -0.005(3) C15 0.048(7) 0.040(6) 0.046(6) -0.002(5) -0.025(5) -0.021(6) C16 0.037(6) 0.036(5) 0.039(5) -0.003(4) -0.017(5) -0.012(5) C17 0.039(6) 0.048(6) 0.040(6) 0.001(5) -0.019(5) -0.014(5) C18 0.081(9) 0.057(7) 0.037(6) -0.012(5) -0.023(6) -0.026(7) C19 0.085(10) 0.062(8) 0.045(7) -0.007(6) -0.036(7) -0.009(7) C20 0.075(10) 0.061(8) 0.061(8) 0.011(7) -0.043(7) -0.004(7) C21 0.052(7) 0.037(6) 0.057(7) 0.000(5) -0.030(6) -0.004(5) C22 0.083(10) 0.061(8) 0.064(8) -0.017(7) -0.034(8) -0.018(8) N3 0.129(13) 0.079(9) 0.092(10) -0.026(8) -0.042(9) -0.027(9) O9 0.050(5) 0.024(3) 0.052(4) -0.007(3) -0.025(4) -0.004(3) O10 0.050(5) 0.030(4) 0.066(5) -0.004(3) -0.028(4) -0.006(3) C23 0.051(7) 0.036(6) 0.044(6) -0.004(5) -0.013(6) -0.013(6) C24 0.043(7) 0.026(5) 0.053(6) 0.001(5) -0.017(5) -0.005(5) C25 0.051(7) 0.027(5) 0.059(7) -0.003(5) -0.024(6) -0.010(5) C26 0.059(8) 0.030(5) 0.052(7) 0.003(5) -0.016(6) -0.013(5) C27 0.063(8) 0.035(6) 0.067(8) -0.007(6) -0.015(7) -0.015(6) C28 0.065(9) 0.032(6) 0.087(9) 0.001(6) -0.041(8) -0.005(6) C29 0.053(8) 0.044(7) 0.073(8) -0.003(6) -0.031(7) -0.010(6) C30 0.077(9) 0.038(6) 0.061(8) -0.007(6) -0.015(7) -0.026(6) N4 0.105(10) 0.050(6) 0.070(7) -0.001(6) -0.020(7) -0.033(7) N31 0.113(12) 0.103(11) 0.065(8) -0.010(7) -0.015(8) -0.054(10) C31 0.082(12) 0.102(13) 0.073(10) -0.007(9) -0.015(9) -0.048(10) C32 0.091(13) 0.101(13) 0.133(15) -0.024(12) -0.029(12) -0.053(11) _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 O3 2.312(6) . ? Dy1 O2 2.356(6) . ? Dy1 O7 2.383(7) . ? Dy1 O1 2.383(7) . ? Dy1 O5 2.395(7) . ? Dy1 O10 2.418(7) . ? Dy1 O9 2.447(6) . ? Dy1 O4 2.501(7) . ? Dy1 N1 2.573(8) . ? Fe1 O3 1.928(7) 2_666 ? Fe1 O2 1.946(7) . ? Fe1 O6 2.004(7) . ? Fe1 O8 2.043(7) 2_666 ? Fe1 O1 2.058(7) 2_666 ? Fe1 O1 2.064(7) . ? O1 Fe1 2.058(7) 2_666 ? O1 H1 0.89(4) . ? N1 C5 1.474(12) . ? N1 C3 1.495(13) . ? N1 C1 1.515(13) . ? C1 C2 1.505(14) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 O2 1.424(12) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.516(16) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O3 1.420(12) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? O3 Fe1 1.928(7) 2_666 ? C5 C6 1.532(16) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 O4 1.450(14) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? O4 H4 0.93(3) . ? O5 C7 1.275(12) . ? O6 C7 1.273(12) . ? C7 C8 1.506(13) . ? C8 C13 1.393(15) . ? C8 C9 1.398(14) . ? C9 C10 1.390(14) . ? C9 H9A 0.9500 . ? C10 C11 1.381(16) . ? C10 C14 1.449(14) . ? C11 C12 1.378(16) . ? C11 H11A 0.9500 . ? C12 C13 1.381(15) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? C14 N2 1.148(13) . ? O7 C15 1.243(13) . ? O8 C15 1.278(12) . ? O8 Fe1 2.043(7) 2_666 ? C15 C16 1.509(14) . ? C16 C21 1.393(15) . ? C16 C17 1.413(14) . ? C17 C18 1.380(15) . ? C17 H17A 0.9500 . ? C18 C19 1.382(18) . ? C18 C22 1.445(16) . ? C19 C20 1.376(17) . ? C19 H19A 0.9500 . ? C20 C21 1.392(16) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? C22 N3 1.139(16) . ? O9 C23 1.262(14) . ? O10 C23 1.274(13) . ? C23 C24 1.497(14) . ? C24 C29 1.367(17) . ? C24 C25 1.406(14) . ? C25 C26 1.397(14) . ? C25 H25A 0.9500 . ? C26 C27 1.399(17) . ? C26 C30 1.426(16) . ? C27 C28 1.384(17) . ? C27 H27A 0.9500 . ? C28 C29 1.402(16) . ? C28 H28A 0.9500 . ? C29 H29A 0.9500 . ? C30 N4 1.162(16) . ? N31 C31 1.155(18) . ? C31 C32 1.46(2) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 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 O3 Dy1 O2 82.0(2) . . ? O3 Dy1 O7 75.4(2) . . ? O2 Dy1 O7 140.4(2) . . ? O3 Dy1 O1 67.4(2) . . ? O2 Dy1 O1 68.8(2) . . ? O7 Dy1 O1 72.5(2) . . ? O3 Dy1 O5 137.1(2) . . ? O2 Dy1 O5 74.5(2) . . ? O7 Dy1 O5 100.8(3) . . ? O1 Dy1 O5 70.8(2) . . ? O3 Dy1 O10 143.6(3) . . ? O2 Dy1 O10 87.0(2) . . ? O7 Dy1 O10 129.5(2) . . ? O1 Dy1 O10 138.9(2) . . ? O5 Dy1 O10 71.0(3) . . ? O3 Dy1 O9 143.3(2) . . ? O2 Dy1 O9 134.4(2) . . ? O7 Dy1 O9 75.5(2) . . ? O1 Dy1 O9 123.1(2) . . ? O5 Dy1 O9 70.7(2) . . ? O10 Dy1 O9 54.4(2) . . ? O3 Dy1 O4 81.6(2) . . ? O2 Dy1 O4 134.6(2) . . ? O7 Dy1 O4 73.8(3) . . ? O1 Dy1 O4 138.7(2) . . ? O5 Dy1 O4 139.5(2) . . ? O10 Dy1 O4 81.8(3) . . ? O9 Dy1 O4 69.1(2) . . ? O3 Dy1 N1 67.8(3) . . ? O2 Dy1 N1 69.8(2) . . ? O7 Dy1 N1 127.3(3) . . ? O1 Dy1 N1 121.7(2) . . ? O5 Dy1 N1 131.8(3) . . ? O10 Dy1 N1 75.9(3) . . ? O9 Dy1 N1 115.2(2) . . ? O4 Dy1 N1 64.8(2) . . ? O3 Fe1 O2 174.9(3) 2_666 . ? O3 Fe1 O6 92.4(3) 2_666 . ? O2 Fe1 O6 90.7(3) . . ? O3 Fe1 O8 88.3(3) 2_666 2_666 ? O2 Fe1 O8 95.2(3) . 2_666 ? O6 Fe1 O8 98.6(3) . 2_666 ? O3 Fe1 O1 81.5(3) 2_666 2_666 ? O2 Fe1 O1 94.6(3) . 2_666 ? O6 Fe1 O1 166.7(3) . 2_666 ? O8 Fe1 O1 93.0(3) 2_666 2_666 ? O3 Fe1 O1 92.0(3) 2_666 . ? O2 Fe1 O1 83.8(3) . . ? O6 Fe1 O1 91.9(3) . . ? O8 Fe1 O1 169.4(3) 2_666 . ? O1 Fe1 O1 76.6(3) 2_666 . ? Fe1 O1 Fe1 103.4(3) 2_666 . ? Fe1 O1 Dy1 101.3(3) 2_666 . ? Fe1 O1 Dy1 100.8(3) . . ? Fe1 O1 H1 110(7) 2_666 . ? Fe1 O1 H1 108(7) . . ? Dy1 O1 H1 130(7) . . ? C5 N1 C3 111.9(8) . . ? C5 N1 C1 109.8(8) . . ? C3 N1 C1 110.3(8) . . ? C5 N1 Dy1 108.8(6) . . ? C3 N1 Dy1 112.0(6) . . ? C1 N1 Dy1 103.6(5) . . ? C2 C1 N1 110.6(8) . . ? C2 C1 H1A 109.5 . . ? N1 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 108.1 . . ? O2 C2 C1 110.7(8) . . ? O2 C2 H2A 109.5 . . ? C1 C2 H2A 109.5 . . ? O2 C2 H2B 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? C2 O2 Fe1 125.3(6) . . ? C2 O2 Dy1 120.1(6) . . ? Fe1 O2 Dy1 105.5(3) . . ? N1 C3 C4 112.1(8) . . ? N1 C3 H3A 109.2 . . ? C4 C3 H3A 109.2 . . ? N1 C3 H3B 109.2 . . ? C4 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? O3 C4 C3 108.2(8) . . ? O3 C4 H4A 110.1 . . ? C3 C4 H4A 110.1 . . ? O3 C4 H4B 110.1 . . ? C3 C4 H4B 110.1 . . ? H4A C4 H4B 108.4 . . ? C4 O3 Fe1 131.7(6) . 2_666 ? C4 O3 Dy1 120.1(6) . . ? Fe1 O3 Dy1 108.2(3) 2_666 . ? N1 C5 C6 110.2(9) . . ? N1 C5 H5A 109.6 . . ? C6 C5 H5A 109.6 . . ? N1 C5 H5B 109.6 . . ? C6 C5 H5B 109.6 . . ? H5A C5 H5B 108.1 . . ? O4 C6 C5 107.5(9) . . ? O4 C6 H6A 110.2 . . ? C5 C6 H6A 110.2 . . ? O4 C6 H6B 110.2 . . ? C5 C6 H6B 110.2 . . ? H6A C6 H6B 108.5 . . ? C6 O4 Dy1 122.5(6) . . ? C6 O4 H4 108(7) . . ? Dy1 O4 H4 114(6) . . ? C7 O5 Dy1 136.7(6) . . ? C7 O6 Fe1 124.0(7) . . ? O6 C7 O5 127.3(9) . . ? O6 C7 C8 116.7(9) . . ? O5 C7 C8 115.9(9) . . ? C13 C8 C9 118.6(9) . . ? C13 C8 C7 122.1(9) . . ? C9 C8 C7 119.2(9) . . ? C10 C9 C8 119.5(10) . . ? C10 C9 H9A 120.2 . . ? C8 C9 H9A 120.2 . . ? C11 C10 C9 121.0(10) . . ? C11 C10 C14 119.8(10) . . ? C9 C10 C14 119.2(10) . . ? C12 C11 C10 119.7(10) . . ? C12 C11 H11A 120.2 . . ? C10 C11 H11A 120.2 . . ? C11 C12 C13 119.9(11) . . ? C11 C12 H12A 120.1 . . ? C13 C12 H12A 120.1 . . ? C12 C13 C8 121.3(10) . . ? C12 C13 H13A 119.4 . . ? C8 C13 H13A 119.4 . . ? N2 C14 C10 177.1(12) . . ? C15 O7 Dy1 133.1(6) . . ? C15 O8 Fe1 123.4(7) . 2_666 ? O7 C15 O8 127.5(9) . . ? O7 C15 C16 116.4(9) . . ? O8 C15 C16 116.0(10) . . ? C21 C16 C17 119.0(9) . . ? C21 C16 C15 122.3(9) . . ? C17 C16 C15 118.7(9) . . ? C18 C17 C16 119.7(11) . . ? C18 C17 H17A 120.2 . . ? C16 C17 H17A 120.2 . . ? C17 C18 C19 120.8(11) . . ? C17 C18 C22 119.2(12) . . ? C19 C18 C22 119.9(11) . . ? C20 C19 C18 119.8(11) . . ? C20 C19 H19A 120.1 . . ? C18 C19 H19A 120.1 . . ? C19 C20 C21 120.6(12) . . ? C19 C20 H20A 119.7 . . ? C21 C20 H20A 119.7 . . ? C20 C21 C16 119.9(10) . . ? C20 C21 H21A 120.0 . . ? C16 C21 H21A 120.0 . . ? N3 C22 C18 175.8(16) . . ? C23 O9 Dy1 90.4(6) . . ? C23 O10 Dy1 91.4(7) . . ? O9 C23 O10 122.7(10) . . ? O9 C23 C24 119.9(9) . . ? O10 C23 C24 117.3(11) . . ? C29 C24 C25 119.9(10) . . ? C29 C24 C23 121.5(10) . . ? C25 C24 C23 118.4(10) . . ? C26 C25 C24 119.2(11) . . ? C26 C25 H25A 120.4 . . ? C24 C25 H25A 120.4 . . ? C25 C26 C27 120.1(11) . . ? C25 C26 C30 119.0(12) . . ? C27 C26 C30 120.9(10) . . ? C28 C27 C26 120.2(11) . . ? C28 C27 H27A 119.9 . . ? C26 C27 H27A 119.9 . . ? C27 C28 C29 119.2(12) . . ? C27 C28 H28A 120.4 . . ? C29 C28 H28A 120.4 . . ? C24 C29 C28 121.2(12) . . ? C24 C29 H29A 119.4 . . ? C28 C29 H29A 119.4 . . ? N4 C30 C26 178.7(15) . . ? N31 C31 C32 179(2) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 N2 0.89(4) 2.28(7) 3.076(12) 149(9) 2_656 O4 H4 N31 0.93(3) 2.04(3) 2.942(15) 162(9) . _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.911 _refine_diff_density_min -2.908 _refine_diff_density_rms 0.191 _database_code_depnum_ccdc_archive 'CCDC 926560' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_ammt16dyx _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C60 H70 Dy2 Fe2 N2 O20), 2(C2 H3 N), 2(C H4 O)' _chemical_formula_sum 'C66 H84 Dy2 Fe2 N4 O22' _chemical_formula_weight 1722.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.4404(8) _cell_length_b 21.4830(15) _cell_length_c 13.7050(9) _cell_angle_alpha 90.00 _cell_angle_beta 100.532(5) _cell_angle_gamma 90.00 _cell_volume 3601.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 29823 _cell_measurement_theta_min 1.67 _cell_measurement_theta_max 28.23 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.588 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1736 _exptl_absorpt_coefficient_mu 2.521 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.433 _exptl_absorpt_correction_T_max 0.589 _exptl_absorpt_process_details ; XPREP in SHELXTL 6.14 (BrukerAXS Inc., 2003) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS II' _diffrn_measurement_method 'area detector' _diffrn_detector_area_resol_mean 6.667 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38489 _diffrn_reflns_av_R_equivalents 0.0803 _diffrn_reflns_av_unetI/netI 0.0475 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 26.73 _reflns_number_total 7652 _reflns_number_gt 6012 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'WinXpose 1.6.8 (Stoe & Cie GmbH, 2004)' _computing_cell_refinement 'X-Area 1.38 (Stoe & Cie GmbH, 2006)' _computing_data_reduction 'X-Area 1.38 (Stoe & Cie GmbH, 2006)' _computing_structure_solution 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_structure_refinement 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _computing_molecular_graphics 'Diamond 2.1 (Crystal Impact, 1998)' _computing_publication_material 'SHELXTL 6.14 (BrukerAXS Inc., 2003)' _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. The disordered m-tolyl group of one of the carboxylate ligands was refined using two sets of isotropic half-occupancy atoms, with the aromatic rings constrained to rigid hexagons. O-H distances were restrained: DFIX 0.92 0.04 O1 H1 O4 H4 The m-toluyl ring of one of the carboxylate ligands was disordered, and was refined using 50% occupancy isotropic C-atoms; these aromatic rings were refined as rigid hexagons (AFIX 66). ; _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^)+(0.0879P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7652 _refine_ls_number_parameters 415 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0660 _refine_ls_R_factor_gt 0.0528 _refine_ls_wR_factor_ref 0.1262 _refine_ls_wR_factor_gt 0.1207 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.405200(18) 0.626140(10) 0.536579(16) 0.03849(9) Uani 1 1 d . . . Fe1 Fe 0.45109(5) 0.50649(3) 0.38239(5) 0.03637(15) Uani 1 1 d . . . O1 O 0.4079(3) 0.51514(16) 0.5203(2) 0.0354(7) Uani 1 1 d D . . H1 H 0.336(3) 0.497(2) 0.507(4) 0.042 Uiso 1 1 d D . . N1 N 0.5769(4) 0.6927(2) 0.5145(3) 0.0452(9) Uani 1 1 d . . . C1 C 0.5781(5) 0.6919(2) 0.4062(4) 0.0464(11) Uani 1 1 d . . . H1A H 0.6482 0.7093 0.3941 0.056 Uiso 1 1 calc R . . H1B H 0.5182 0.7185 0.3712 0.056 Uiso 1 1 calc R . . C2 C 0.5644(4) 0.6263(2) 0.3653(4) 0.0455(11) Uani 1 1 d . . . H2A H 0.5535 0.6275 0.2919 0.055 Uiso 1 1 calc R . . H2B H 0.6313 0.6019 0.3900 0.055 Uiso 1 1 calc R . . O2 O 0.4735(3) 0.59751(16) 0.3950(2) 0.0384(7) Uani 1 1 d . . . C3 C 0.6569(5) 0.6223(2) 0.6535(4) 0.0492(12) Uani 1 1 d . . . H3A H 0.7223 0.5965 0.6778 0.059 Uiso 1 1 calc R . . H3B H 0.6413 0.6477 0.7096 0.059 Uiso 1 1 calc R . . C4 C 0.6787(5) 0.6646(3) 0.5707(4) 0.0521(13) Uani 1 1 d . . . H4A H 0.7291 0.6982 0.5994 0.063 Uiso 1 1 calc R . . H4B H 0.7150 0.6404 0.5246 0.063 Uiso 1 1 calc R . . O3 O 0.5672(3) 0.58370(15) 0.6180(2) 0.0398(7) Uani 1 1 d . . . C5 C 0.5593(5) 0.7567(3) 0.5479(4) 0.0527(13) Uani 1 1 d . . . H5A H 0.4963 0.7756 0.5031 0.063 Uiso 1 1 calc R . . H5B H 0.6248 0.7823 0.5448 0.063 Uiso 1 1 calc R . . C6 C 0.5379(6) 0.7565(3) 0.6521(5) 0.0589(14) Uani 1 1 d . . . H6A H 0.6062 0.7472 0.6994 0.071 Uiso 1 1 calc R . . H6B H 0.5108 0.7977 0.6688 0.071 Uiso 1 1 calc R . . O4 O 0.4572(4) 0.70937(18) 0.6586(3) 0.0542(9) Uani 1 1 d D . . H4 H 0.413(5) 0.725(3) 0.697(4) 0.065 Uiso 1 1 d D . . O5 O 0.2962(3) 0.51819(16) 0.3139(3) 0.0429(8) Uani 1 1 d . . . O6 O 0.2477(3) 0.59043(17) 0.4163(3) 0.0443(8) Uani 1 1 d . . . C7 C 0.2272(4) 0.5550(2) 0.3432(4) 0.0418(10) Uani 1 1 d . . . C8 C 0.1143(4) 0.5545(3) 0.2835(4) 0.0436(11) Uani 1 1 d . . . C10 C 0.0374(4) 0.5967(3) 0.3053(5) 0.0512(12) Uani 1 1 d . . . H10A H 0.0569 0.6249 0.3590 0.061 Uiso 1 1 calc R . . C11 C -0.0673(5) 0.5983(4) 0.2497(5) 0.0651(17) Uani 1 1 d . . . C12 C -0.0937(5) 0.5557(4) 0.1724(5) 0.0723(19) Uani 1 1 d . . . H12A H -0.1658 0.5554 0.1348 0.087 Uiso 1 1 calc R . . C13 C -0.0181(5) 0.5139(4) 0.1489(5) 0.073(2) Uani 1 1 d . . . H13A H -0.0378 0.4862 0.0946 0.088 Uiso 1 1 calc R . . C14 C 0.0863(5) 0.5126(3) 0.2049(4) 0.0556(14) Uani 1 1 d . . . H14A H 0.1386 0.4835 0.1900 0.067 Uiso 1 1 calc R . . C15 C -0.1500(6) 0.6445(4) 0.2734(7) 0.086(2) Uani 1 1 d . . . H15A H -0.1865 0.6274 0.3251 0.129 Uiso 1 1 calc R . . H15B H -0.2045 0.6527 0.2135 0.129 Uiso 1 1 calc R . . H15C H -0.1130 0.6834 0.2969 0.129 Uiso 1 1 calc R . . O7 O 0.5321(3) 0.50168(17) 0.2688(3) 0.0452(8) Uani 1 1 d . . . O8 O 0.6376(3) 0.41774(17) 0.3156(3) 0.0461(8) Uani 1 1 d . . . C16 C 0.6015(4) 0.4605(2) 0.2554(4) 0.0435(11) Uani 1 1 d . . . C17 C 0.6421(4) 0.4633(3) 0.1587(4) 0.0437(11) Uani 1 1 d . . . C18 C 0.6174(4) 0.5141(3) 0.0956(4) 0.0478(12) Uani 1 1 d . . . H18A H 0.5753 0.5473 0.1146 0.057 Uiso 1 1 calc R . . C19 C 0.6531(5) 0.5172(3) 0.0050(4) 0.0524(13) Uani 1 1 d . . . C20 C 0.7121(5) 0.4668(3) -0.0222(5) 0.0637(16) Uani 1 1 d . . . H20A H 0.7345 0.4670 -0.0848 0.076 Uiso 1 1 calc R . . C21 C 0.7383(6) 0.4166(4) 0.0414(5) 0.0669(17) Uani 1 1 d . . . H21A H 0.7804 0.3833 0.0228 0.080 Uiso 1 1 calc R . . C22 C 0.7034(5) 0.4149(3) 0.1314(5) 0.0601(15) Uani 1 1 d . . . H22A H 0.7216 0.3804 0.1745 0.072 Uiso 1 1 calc R . . C23 C 0.6302(6) 0.5742(3) -0.0608(5) 0.0655(17) Uani 1 1 d . . . H23A H 0.6947 0.6012 -0.0505 0.098 Uiso 1 1 calc R . . H23B H 0.5678 0.5969 -0.0440 0.098 Uiso 1 1 calc R . . H23C H 0.6134 0.5612 -0.1305 0.098 Uiso 1 1 calc R . . O9 O 0.2406(4) 0.6804(2) 0.5627(3) 0.0589(10) Uani 1 1 d . A . O10 O 0.3172(3) 0.71573(18) 0.4418(3) 0.0534(9) Uani 1 1 d . A . C24 C 0.2362(5) 0.7141(3) 0.4866(5) 0.0599(15) Uani 1 1 d . . . C25A C 0.1396(6) 0.7521(4) 0.4317(7) 0.052(3) Uiso 0.50 1 d PG A 1 C26A C 0.1286(7) 0.7781(5) 0.3375(6) 0.062(3) Uiso 0.50 1 d PG A 1 H26A H 0.1850 0.7729 0.2999 0.075 Uiso 0.50 1 calc PR A 1 C27A C 0.0352(8) 0.8117(5) 0.2984(6) 0.075(4) Uiso 0.50 1 d PG A 1 H27A H 0.0277 0.8295 0.2341 0.091 Uiso 0.50 1 calc PR A 1 C28A C -0.0472(7) 0.8194(5) 0.3535(8) 0.087(5) Uiso 0.50 1 d PG A 1 H28A H -0.1111 0.8423 0.3268 0.104 Uiso 0.50 1 calc PR A 1 C29A C -0.0363(6) 0.7933(5) 0.4476(7) 0.068(3) Uiso 0.50 1 d PG A 1 C30A C 0.0571(7) 0.7597(4) 0.4867(6) 0.066(3) Uiso 0.50 1 d PG A 1 H30A H 0.0646 0.7419 0.5511 0.079 Uiso 0.50 1 calc PR A 1 C31A C -0.1250(16) 0.8028(10) 0.5089(15) 0.097(5) Uiso 0.50 1 d P A 1 H31A H -0.1563 0.8445 0.4964 0.146 Uiso 0.50 1 calc PR A 1 H31B H -0.0935 0.7985 0.5795 0.146 Uiso 0.50 1 calc PR A 1 H31C H -0.1825 0.7716 0.4902 0.146 Uiso 0.50 1 calc PR A 1 C25B C 0.1313(6) 0.7499(4) 0.4662(7) 0.057(3) Uiso 0.50 1 d PG A 2 C26B C 0.1037(7) 0.7748(4) 0.3713(6) 0.056(3) Uiso 0.50 1 d PG A 2 H26B H 0.1497 0.7678 0.3241 0.067 Uiso 0.50 1 calc PR A 2 C27B C 0.0089(8) 0.8099(4) 0.3454(6) 0.062(3) Uiso 0.50 1 d PG A 2 C28B C -0.0583(7) 0.8201(5) 0.4144(8) 0.084(4) Uiso 0.50 1 d PG A 2 H28B H -0.1231 0.8441 0.3967 0.100 Uiso 0.50 1 calc PR A 2 C29B C -0.0307(8) 0.7952(5) 0.5093(8) 0.091(5) Uiso 0.50 1 d PG A 2 H29A H -0.0767 0.8022 0.5565 0.110 Uiso 0.50 1 calc PR A 2 C30B C 0.0641(9) 0.7601(5) 0.5352(6) 0.077(4) Uiso 0.50 1 d PG A 2 H30B H 0.0829 0.7431 0.6001 0.092 Uiso 0.50 1 calc PR A 2 C31B C -0.0251(16) 0.8353(9) 0.2410(14) 0.088(5) Uiso 0.50 1 d P A 2 H31D H 0.0279 0.8222 0.2003 0.132 Uiso 0.50 1 calc PR A 2 H31E H -0.0276 0.8808 0.2433 0.132 Uiso 0.50 1 calc PR A 2 H31F H -0.0976 0.8192 0.2120 0.132 Uiso 0.50 1 calc PR A 2 N41 N 0.1827(5) 0.4630(3) 0.5354(6) 0.0823(19) Uani 1 1 d . . . C41 C 0.1435(6) 0.5033(4) 0.5671(6) 0.0722(19) Uani 1 1 d . . . C42 C 0.0934(6) 0.5571(4) 0.6106(7) 0.082(2) Uani 1 1 d . . . H42A H 0.1292 0.5957 0.5956 0.122 Uiso 1 1 calc R . . H42B H 0.1028 0.5519 0.6827 0.122 Uiso 1 1 calc R . . H42C H 0.0153 0.5592 0.5822 0.122 Uiso 1 1 calc R . . O41 O 0.3274(5) 0.7741(3) 0.7478(4) 0.0881(18) Uani 1 1 d . . . H41 H 0.3278 0.7798 0.8085 0.132 Uiso 1 1 calc R . . C43 C 0.2889(9) 0.8283(5) 0.6945(7) 0.116(4) Uani 1 1 d . . . H43A H 0.3287 0.8647 0.7259 0.174 Uiso 1 1 calc R . . H43B H 0.2107 0.8334 0.6946 0.174 Uiso 1 1 calc R . . H43C H 0.3007 0.8247 0.6260 0.174 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.04124(14) 0.03803(13) 0.03676(13) -0.00183(9) 0.00865(9) 0.00309(9) Fe1 0.0372(3) 0.0395(3) 0.0324(3) -0.0016(3) 0.0064(2) 0.0014(3) O1 0.0357(16) 0.0391(17) 0.0318(15) -0.0006(12) 0.0069(13) 0.0019(13) N1 0.050(2) 0.043(2) 0.042(2) -0.0024(18) 0.0052(18) -0.0004(19) C1 0.052(3) 0.044(3) 0.044(3) 0.003(2) 0.011(2) -0.004(2) C2 0.047(3) 0.044(3) 0.049(3) 0.002(2) 0.016(2) -0.002(2) O2 0.0401(17) 0.0429(18) 0.0336(16) -0.0011(13) 0.0104(13) -0.0003(14) C3 0.052(3) 0.044(3) 0.047(3) -0.002(2) -0.003(2) -0.010(2) C4 0.051(3) 0.050(3) 0.054(3) 0.001(2) 0.004(2) -0.007(2) O3 0.0367(16) 0.0423(18) 0.0384(17) -0.0034(14) 0.0018(13) 0.0001(14) C5 0.064(3) 0.040(3) 0.054(3) -0.004(2) 0.009(3) -0.006(2) C6 0.080(4) 0.045(3) 0.054(3) -0.011(2) 0.018(3) -0.007(3) O4 0.065(2) 0.047(2) 0.054(2) -0.0110(17) 0.0187(19) 0.0001(18) O5 0.0406(18) 0.0464(19) 0.0396(17) -0.0017(14) 0.0017(14) 0.0030(15) O6 0.0416(18) 0.0474(19) 0.0426(19) -0.0033(15) 0.0044(15) 0.0036(15) C7 0.036(2) 0.045(3) 0.044(3) 0.007(2) 0.0063(19) 0.001(2) C8 0.033(2) 0.052(3) 0.045(3) 0.004(2) 0.0032(19) -0.004(2) C10 0.038(3) 0.055(3) 0.059(3) 0.009(3) 0.007(2) -0.003(2) C11 0.038(3) 0.081(4) 0.076(4) 0.018(4) 0.010(3) 0.006(3) C12 0.040(3) 0.104(6) 0.067(4) 0.007(4) -0.005(3) -0.006(3) C13 0.049(3) 0.109(6) 0.055(4) -0.009(4) -0.006(3) -0.010(4) C14 0.043(3) 0.074(4) 0.050(3) -0.002(3) 0.009(2) -0.004(3) C15 0.040(3) 0.104(6) 0.114(7) 0.017(5) 0.010(4) 0.017(4) O7 0.050(2) 0.049(2) 0.0371(17) 0.0002(15) 0.0098(15) 0.0026(17) O8 0.053(2) 0.0481(19) 0.0397(18) 0.0030(15) 0.0149(16) 0.0061(16) C16 0.042(3) 0.052(3) 0.038(2) -0.008(2) 0.011(2) -0.002(2) C17 0.043(3) 0.053(3) 0.036(2) -0.003(2) 0.009(2) -0.003(2) C18 0.043(3) 0.059(3) 0.042(3) -0.005(2) 0.009(2) -0.008(2) C19 0.054(3) 0.069(4) 0.035(2) -0.002(2) 0.009(2) -0.014(3) C20 0.062(4) 0.090(5) 0.043(3) -0.011(3) 0.020(3) -0.003(3) C21 0.071(4) 0.083(5) 0.052(3) -0.006(3) 0.024(3) 0.013(4) C22 0.061(4) 0.073(4) 0.048(3) -0.003(3) 0.015(3) 0.014(3) C23 0.072(4) 0.078(4) 0.045(3) 0.009(3) 0.006(3) -0.021(3) O9 0.058(2) 0.055(2) 0.067(3) -0.008(2) 0.021(2) 0.0101(19) O10 0.057(2) 0.047(2) 0.055(2) 0.0048(17) 0.0057(18) 0.0058(18) C24 0.055(3) 0.044(3) 0.077(4) -0.009(3) 0.003(3) 0.007(3) N41 0.061(4) 0.086(5) 0.103(5) 0.018(4) 0.026(3) 0.013(3) C41 0.051(4) 0.084(5) 0.083(5) 0.026(4) 0.014(3) -0.004(4) C42 0.056(4) 0.094(6) 0.096(6) 0.007(5) 0.019(4) 0.004(4) O41 0.091(4) 0.105(4) 0.062(3) -0.034(3) -0.003(3) 0.039(3) C43 0.136(8) 0.118(7) 0.078(6) -0.039(5) -0.024(5) 0.067(7) _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 O3 2.306(3) . ? Dy1 O2 2.339(3) . ? Dy1 O8 2.381(4) 3_666 ? Dy1 O1 2.396(3) . ? Dy1 O9 2.439(4) . ? Dy1 O6 2.442(3) . ? Dy1 O4 2.453(4) . ? Dy1 O10 2.464(4) . ? Dy1 N1 2.633(5) . ? Fe1 O3 1.951(3) 3_666 ? Fe1 O2 1.978(4) . ? Fe1 O5 1.998(3) . ? Fe1 O7 2.006(4) . ? Fe1 O1 2.053(3) 3_666 ? Fe1 O1 2.066(3) . ? O1 Fe1 2.053(3) 3_666 ? O1 H1 0.96(3) . ? N1 C5 1.479(7) . ? N1 C4 1.484(7) . ? N1 C1 1.488(7) . ? C1 C2 1.515(7) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 O2 1.412(6) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 O3 1.404(6) . ? C3 C4 1.516(8) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? O3 Fe1 1.951(3) 3_666 ? C5 C6 1.500(8) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 O4 1.439(7) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? O4 H4 0.89(4) . ? O5 C7 1.284(6) . ? O6 C7 1.246(6) . ? C7 C8 1.491(7) . ? C8 C10 1.390(8) . ? C8 C14 1.399(8) . ? C10 C11 1.383(8) . ? C10 H10A 0.9500 . ? C11 C12 1.393(11) . ? C11 C15 1.507(10) . ? C12 C13 1.380(11) . ? C12 H12A 0.9500 . ? C13 C14 1.383(8) . ? C13 H13A 0.9500 . ? C14 H14A 0.9500 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? O7 C16 1.273(6) . ? O8 C16 1.261(6) . ? O8 Dy1 2.381(4) 3_666 ? C16 C17 1.504(7) . ? C17 C22 1.380(8) . ? C17 C18 1.391(8) . ? C18 C19 1.395(7) . ? C18 H18A 0.9500 . ? C19 C20 1.395(9) . ? C19 C23 1.517(9) . ? C20 C21 1.387(10) . ? C20 H20A 0.9500 . ? C21 C22 1.381(9) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? O9 C24 1.263(8) . ? O10 C24 1.273(8) . ? C24 C25B 1.497(9) . ? C24 C25A 1.532(9) . ? C25A C26A 1.3900 . ? C25A C30A 1.3900 . ? C26A C27A 1.3900 . ? C26A H26A 0.9500 . ? C27A C28A 1.3900 . ? C27A H27A 0.9500 . ? C28A C29A 1.3900 . ? C28A H28A 0.9500 . ? C29A C30A 1.3900 . ? C29A C31A 1.52(2) . ? C30A H30A 0.9500 . ? C31A H31A 0.9800 . ? C31A H31B 0.9800 . ? C31A H31C 0.9800 . ? C25B C26B 1.3900 . ? C25B C30B 1.3900 . ? C26B C27B 1.3900 . ? C26B H26B 0.9500 . ? C27B C28B 1.3900 . ? C27B C31B 1.517(19) . ? C28B C29B 1.3900 . ? C28B H28B 0.9500 . ? C29B C30B 1.3900 . ? C29B H29A 0.9500 . ? C30B H30B 0.9500 . ? C31B H31D 0.9800 . ? C31B H31E 0.9800 . ? C31B H31F 0.9800 . ? N41 C41 1.119(10) . ? C41 C42 1.489(12) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? O41 C43 1.412(11) . ? O41 H41 0.8400 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 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 O3 Dy1 O2 83.06(12) . . ? O3 Dy1 O8 75.14(13) . 3_666 ? O2 Dy1 O8 140.67(12) . 3_666 ? O3 Dy1 O1 68.02(11) . . ? O2 Dy1 O1 69.37(11) . . ? O8 Dy1 O1 72.19(11) 3_666 . ? O3 Dy1 O9 143.24(14) . . ? O2 Dy1 O9 133.62(14) . . ? O8 Dy1 O9 74.93(14) 3_666 . ? O1 Dy1 O9 121.05(13) . . ? O3 Dy1 O6 136.46(12) . . ? O2 Dy1 O6 74.08(12) . . ? O8 Dy1 O6 99.99(13) 3_666 . ? O1 Dy1 O6 69.37(11) . . ? O9 Dy1 O6 69.99(14) . . ? O3 Dy1 O4 81.95(13) . . ? O2 Dy1 O4 131.81(13) . . ? O8 Dy1 O4 77.34(13) 3_666 . ? O1 Dy1 O4 141.49(12) . . ? O9 Dy1 O4 71.07(15) . . ? O6 Dy1 O4 140.21(13) . . ? O3 Dy1 O10 145.98(13) . . ? O2 Dy1 O10 87.81(13) . . ? O8 Dy1 O10 127.65(14) 3_666 . ? O1 Dy1 O10 137.81(12) . . ? O9 Dy1 O10 53.13(15) . . ? O6 Dy1 O10 70.44(13) . . ? O4 Dy1 O10 80.00(14) . . ? O3 Dy1 N1 67.31(13) . . ? O2 Dy1 N1 67.79(13) . . ? O8 Dy1 N1 128.66(13) 3_666 . ? O1 Dy1 N1 120.28(12) . . ? O9 Dy1 N1 118.55(15) . . ? O6 Dy1 N1 131.35(13) . . ? O4 Dy1 N1 64.14(14) . . ? O10 Dy1 N1 78.87(14) . . ? O3 Fe1 O2 175.20(14) 3_666 . ? O3 Fe1 O5 91.23(14) 3_666 . ? O2 Fe1 O5 91.45(14) . . ? O3 Fe1 O7 91.25(15) 3_666 . ? O2 Fe1 O7 92.04(14) . . ? O5 Fe1 O7 102.71(15) . . ? O3 Fe1 O1 82.10(14) 3_666 3_666 ? O2 Fe1 O1 94.40(14) . 3_666 ? O5 Fe1 O1 165.74(14) . 3_666 ? O7 Fe1 O1 90.09(14) . 3_666 ? O3 Fe1 O1 92.41(14) 3_666 . ? O2 Fe1 O1 83.54(13) . . ? O5 Fe1 O1 91.64(14) . . ? O7 Fe1 O1 165.11(14) . . ? O1 Fe1 O1 76.14(14) 3_666 . ? Fe1 O1 Fe1 103.86(14) 3_666 . ? Fe1 O1 Dy1 100.93(13) 3_666 . ? Fe1 O1 Dy1 100.67(13) . . ? Fe1 O1 H1 133(3) 3_666 . ? Fe1 O1 H1 100(3) . . ? Dy1 O1 H1 113(3) . . ? C5 N1 C4 112.2(4) . . ? C5 N1 C1 110.3(4) . . ? C4 N1 C1 110.5(5) . . ? C5 N1 Dy1 107.5(3) . . ? C4 N1 Dy1 110.7(3) . . ? C1 N1 Dy1 105.4(3) . . ? N1 C1 C2 111.0(4) . . ? N1 C1 H1A 109.4 . . ? C2 C1 H1A 109.4 . . ? N1 C1 H1B 109.4 . . ? C2 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? O2 C2 C1 110.1(4) . . ? O2 C2 H2A 109.6 . . ? C1 C2 H2A 109.6 . . ? O2 C2 H2B 109.6 . . ? C1 C2 H2B 109.6 . . ? H2A C2 H2B 108.2 . . ? C2 O2 Fe1 121.1(3) . . ? C2 O2 Dy1 123.7(3) . . ? Fe1 O2 Dy1 105.38(14) . . ? O3 C3 C4 109.5(4) . . ? O3 C3 H3A 109.8 . . ? C4 C3 H3A 109.8 . . ? O3 C3 H3B 109.8 . . ? C4 C3 H3B 109.8 . . ? H3A C3 H3B 108.2 . . ? N1 C4 C3 112.3(5) . . ? N1 C4 H4A 109.1 . . ? C3 C4 H4A 109.1 . . ? N1 C4 H4B 109.1 . . ? C3 C4 H4B 109.1 . . ? H4A C4 H4B 107.9 . . ? C3 O3 Fe1 132.3(3) . 3_666 ? C3 O3 Dy1 120.2(3) . . ? Fe1 O3 Dy1 107.46(14) 3_666 . ? N1 C5 C6 110.7(5) . . ? N1 C5 H5A 109.5 . . ? C6 C5 H5A 109.5 . . ? N1 C5 H5B 109.5 . . ? C6 C5 H5B 109.5 . . ? H5A C5 H5B 108.1 . . ? O4 C6 C5 108.0(5) . . ? O4 C6 H6A 110.1 . . ? C5 C6 H6A 110.1 . . ? O4 C6 H6B 110.1 . . ? C5 C6 H6B 110.1 . . ? H6A C6 H6B 108.4 . . ? C6 O4 Dy1 124.8(3) . . ? C6 O4 H4 107(4) . . ? Dy1 O4 H4 124(5) . . ? C7 O5 Fe1 124.9(3) . . ? C7 O6 Dy1 139.0(3) . . ? O6 C7 O5 125.3(5) . . ? O6 C7 C8 118.6(5) . . ? O5 C7 C8 116.2(5) . . ? C10 C8 C14 120.1(5) . . ? C10 C8 C7 119.7(5) . . ? C14 C8 C7 120.3(5) . . ? C11 C10 C8 120.9(6) . . ? C11 C10 H10A 119.5 . . ? C8 C10 H10A 119.5 . . ? C10 C11 C12 118.0(6) . . ? C10 C11 C15 120.6(7) . . ? C12 C11 C15 121.3(6) . . ? C13 C12 C11 121.9(6) . . ? C13 C12 H12A 119.0 . . ? C11 C12 H12A 119.0 . . ? C12 C13 C14 119.6(7) . . ? C12 C13 H13A 120.2 . . ? C14 C13 H13A 120.2 . . ? C13 C14 C8 119.4(6) . . ? C13 C14 H14A 120.3 . . ? C8 C14 H14A 120.3 . . ? C11 C15 H15A 109.5 . . ? C11 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C11 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C16 O7 Fe1 126.7(3) . . ? C16 O8 Dy1 137.4(3) . 3_666 ? O8 C16 O7 125.6(5) . . ? O8 C16 C17 118.0(5) . . ? O7 C16 C17 116.4(5) . . ? C22 C17 C18 119.5(5) . . ? C22 C17 C16 120.0(5) . . ? C18 C17 C16 120.5(5) . . ? C17 C18 C19 121.3(6) . . ? C17 C18 H18A 119.3 . . ? C19 C18 H18A 119.3 . . ? C20 C19 C18 118.0(6) . . ? C20 C19 C23 121.2(6) . . ? C18 C19 C23 120.8(6) . . ? C21 C20 C19 120.6(6) . . ? C21 C20 H20A 119.7 . . ? C19 C20 H20A 119.7 . . ? C22 C21 C20 120.4(6) . . ? C22 C21 H21A 119.8 . . ? C20 C21 H21A 119.8 . . ? C17 C22 C21 120.1(6) . . ? C17 C22 H22A 120.0 . . ? C21 C22 H22A 120.0 . . ? C19 C23 H23A 109.5 . . ? C19 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C19 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C24 O9 Dy1 93.6(4) . . ? C24 O10 Dy1 92.2(4) . . ? O9 C24 O10 119.7(5) . . ? O9 C24 C25B 110.7(7) . . ? O10 C24 C25B 129.5(7) . . ? O9 C24 C25A 128.5(7) . . ? O10 C24 C25A 111.6(6) . . ? C26A C25A C30A 120.0 . . ? C26A C25A C24 127.3(6) . . ? C30A C25A C24 112.7(6) . . ? C25A C26A C27A 120.0 . . ? C25A C26A H26A 120.0 . . ? C27A C26A H26A 120.0 . . ? C28A C27A C26A 120.0 . . ? C28A C27A H27A 120.0 . . ? C26A C27A H27A 120.0 . . ? C27A C28A C29A 120.0 . . ? C27A C28A H28A 120.0 . . ? C29A C28A H28A 120.0 . . ? C30A C29A C28A 120.0 . . ? C30A C29A C31A 119.9(10) . . ? C28A C29A C31A 120.1(10) . . ? C29A C30A C25A 120.0 . . ? C29A C30A H30A 120.0 . . ? C25A C30A H30A 120.0 . . ? C26B C25B C30B 120.0 . . ? C26B C25B C24 115.5(7) . . ? C30B C25B C24 124.5(7) . . ? C25B C26B C27B 120.0 . . ? C25B C26B H26B 120.0 . . ? C27B C26B H26B 120.0 . . ? C28B C27B C26B 120.0 . . ? C28B C27B C31B 119.1(10) . . ? C26B C27B C31B 120.9(10) . . ? C27B C28B C29B 120.0 . . ? C27B C28B H28B 120.0 . . ? C29B C28B H28B 120.0 . . ? C30B C29B C28B 120.0 . . ? C30B C29B H29A 120.0 . . ? C28B C29B H29A 120.0 . . ? C29B C30B C25B 120.0 . . ? C29B C30B H30B 120.0 . . ? C25B C30B H30B 120.0 . . ? C27B C31B H31D 109.5 . . ? C27B C31B H31E 109.5 . . ? H31D C31B H31E 109.5 . . ? C27B C31B H31F 109.5 . . ? H31D C31B H31F 109.5 . . ? H31E C31B H31F 109.5 . . ? N41 C41 C42 178.9(9) . . ? 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 . . ? C43 O41 H41 109.5 . . ? O41 C43 H43A 109.5 . . ? O41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? O41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 N41 0.96(3) 2.14(4) 3.058(7) 158(5) . O4 H4 O41 0.89(4) 1.74(4) 2.600(6) 162(7) . O41 H41 O10 0.84 1.86 2.694(7) 173.2 4_576 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.676 _refine_diff_density_min -2.641 _refine_diff_density_rms 0.159 _database_code_depnum_ccdc_archive 'CCDC 926561'