data_amer16at _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C54 H58 Dy2 Fe2 N2 O20), 3(C2 H3 N)' _chemical_formula_sum 'C60 H67 Dy2 Fe2 N5 O20' _chemical_formula_weight 1614.89 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 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.7113(9) _cell_length_b 15.8961(8) _cell_length_c 21.8206(11) _cell_angle_alpha 90.00 _cell_angle_beta 110.308(1) _cell_angle_gamma 90.00 _cell_volume 6086.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6792 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 28.11 _exptl_crystal_description block _exptl_crystal_colour 'yellow-brown' _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.762 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3224 _exptl_absorpt_coefficient_mu 2.974 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.692 _exptl_absorpt_correction_T_max 0.878 _exptl_absorpt_process_details 'TWINABS 1.05 (Bruker AXS Inc., 2006)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART Apex' _diffrn_measurement_method 'CCD area detector' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18655 _diffrn_reflns_av_R_equivalents 0.0557 _diffrn_reflns_av_sigmaI/netI 0.0636 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 26.37 _reflns_number_total 6215 _reflns_number_gt 4794 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT 5.6 (Bruker AXS Inc., 2005)' _computing_cell_refinement 'SMART-NT 5.6 (Bruker AXS Inc., 2005)' _computing_data_reduction 'SAINT+ 6.45 (Bruker AXS Inc., 2003)' _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^)+(0.0330P)^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 6215 _refine_ls_number_parameters 410 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0542 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.0808 _refine_ls_wR_factor_gt 0.0755 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _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 0.155145(12) 0.406406(13) 0.495660(10) 0.01942(7) Uani 1 1 d . . . Fe1 Fe 0.17308(4) 0.19807(4) 0.46234(3) 0.01954(15) Uani 1 1 d . . . O1 O 0.21939(17) 0.27832(19) 0.53976(14) 0.0182(6) Uani 1 1 d D . . H1 H 0.222(3) 0.272(3) 0.5782(16) 0.022 Uiso 1 1 d D . . N1 N 0.1551(2) 0.4628(2) 0.38251(18) 0.0242(9) Uani 1 1 d . . . C1 C 0.1361(3) 0.3945(3) 0.3330(2) 0.0279(11) Uani 1 1 d . . . H1A H 0.1837 0.3732 0.3284 0.033 Uiso 1 1 calc R . . H1B H 0.1040 0.4177 0.2903 0.033 Uiso 1 1 calc R . . C2 C 0.0945(3) 0.3220(3) 0.3508(2) 0.0256(10) Uani 1 1 d . . . H2A H 0.0408 0.3376 0.3426 0.031 Uiso 1 1 calc R . . H2B H 0.0952 0.2721 0.3238 0.031 Uiso 1 1 calc R . . O2 O 0.13170(18) 0.3035(2) 0.41759(14) 0.0229(7) Uani 1 1 d . . . C3 C 0.2333(3) 0.4941(3) 0.3963(2) 0.0292(11) Uani 1 1 d . . . H3A H 0.2411 0.5455 0.4234 0.035 Uiso 1 1 calc R . . H3B H 0.2403 0.5091 0.3547 0.035 Uiso 1 1 calc R . . C4 C 0.2916(3) 0.4289(3) 0.4316(2) 0.0244(10) Uani 1 1 d . . . H4A H 0.2887 0.3804 0.4024 0.029 Uiso 1 1 calc R . . H4B H 0.3434 0.4532 0.4443 0.029 Uiso 1 1 calc R . . O3 O 0.27736(17) 0.40170(19) 0.48805(14) 0.0221(7) Uani 1 1 d . . . C5 C 0.1000(3) 0.5336(3) 0.3629(2) 0.0306(12) Uani 1 1 d . . . H5A H 0.0953 0.5529 0.3185 0.037 Uiso 1 1 calc R . . H5B H 0.1191 0.5813 0.3934 0.037 Uiso 1 1 calc R . . C6 C 0.0232(3) 0.5073(3) 0.3633(2) 0.0314(12) Uani 1 1 d . . . H6A H -0.0093 0.5574 0.3603 0.038 Uiso 1 1 calc R . . H6B H -0.0021 0.4704 0.3254 0.038 Uiso 1 1 calc R . . O4 O 0.03397(19) 0.4629(2) 0.42317(16) 0.0270(8) Uani 1 1 d D . . H4 H -0.003(2) 0.477(3) 0.439(2) 0.032 Uiso 1 1 d D . . O5 O 0.08223(18) 0.1841(2) 0.48882(15) 0.0244(7) Uani 1 1 d . . . O6 O 0.06506(18) 0.3150(2) 0.52049(15) 0.0242(7) Uani 1 1 d . . . C7 C 0.0480(2) 0.2393(3) 0.5121(2) 0.0198(9) Uani 1 1 d . . . C8 C -0.0137(3) 0.2037(3) 0.5341(2) 0.0232(10) Uani 1 1 d . . . C9 C -0.0485(3) 0.2542(3) 0.5670(3) 0.0368(13) Uani 1 1 d . . . H9A H -0.0339 0.3116 0.5746 0.044 Uiso 1 1 calc R . . C10 C -0.1041(3) 0.2230(4) 0.5891(3) 0.0483(16) Uani 1 1 d . . . H10A H -0.1267 0.2579 0.6127 0.058 Uiso 1 1 calc R . . C11 C -0.1261(3) 0.1401(4) 0.5763(3) 0.0385(13) Uani 1 1 d . . . H11A H -0.1657 0.1184 0.5897 0.046 Uiso 1 1 calc R . . C12 C -0.0918(3) 0.0887(3) 0.5445(2) 0.0307(11) Uani 1 1 d . . . H12A H -0.1063 0.0312 0.5371 0.037 Uiso 1 1 calc R . . C13 C -0.0351(3) 0.1217(3) 0.5230(2) 0.0282(11) Uani 1 1 d . . . H13A H -0.0113 0.0864 0.5006 0.034 Uiso 1 1 calc R . . O7 O 0.14325(18) 0.1343(2) 0.37849(15) 0.0247(7) Uani 1 1 d . . . O8 O 0.25462(18) 0.0682(2) 0.39505(15) 0.0241(7) Uani 1 1 d . . . C14 C 0.1876(3) 0.0846(3) 0.3618(2) 0.0229(10) Uani 1 1 d . . . C15 C 0.1546(3) 0.0451(3) 0.2956(2) 0.0292(11) Uani 1 1 d . . . C16 C 0.0889(3) 0.0762(4) 0.2493(2) 0.0362(13) Uani 1 1 d . . . H16A H 0.0633 0.1225 0.2600 0.043 Uiso 1 1 calc R . . C17 C 0.0602(3) 0.0407(4) 0.1879(3) 0.0473(16) Uani 1 1 d . . . H17A H 0.0155 0.0633 0.1563 0.057 Uiso 1 1 calc R . . C18 C 0.0956(4) -0.0270(5) 0.1723(3) 0.0540(18) Uani 1 1 d . . . H18A H 0.0756 -0.0517 0.1301 0.065 Uiso 1 1 calc R . . C19 C 0.1614(4) -0.0596(4) 0.2187(3) 0.0487(16) Uani 1 1 d . . . H19A H 0.1864 -0.1065 0.2080 0.058 Uiso 1 1 calc R . . C20 C 0.1901(3) -0.0243(3) 0.2796(3) 0.0351(13) Uani 1 1 d . . . H20A H 0.2346 -0.0473 0.3111 0.042 Uiso 1 1 calc R . . O9 O 0.17601(19) 0.5545(2) 0.51118(16) 0.0279(8) Uani 1 1 d . . . O10 O 0.09943(17) 0.5057(2) 0.55990(15) 0.0247(7) Uani 1 1 d . . . C21 C 0.1400(3) 0.5643(3) 0.5504(2) 0.0237(10) Uani 1 1 d . . . C22 C 0.1500(3) 0.6451(3) 0.5862(2) 0.0294(11) Uani 1 1 d . . . C23 C 0.1918(3) 0.7090(3) 0.5713(3) 0.0418(14) Uani 1 1 d . . . H23A H 0.2134 0.7008 0.5382 0.050 Uiso 1 1 calc R . . C24 C 0.2021(4) 0.7857(4) 0.6051(3) 0.0548(17) Uani 1 1 d . . . H24A H 0.2312 0.8293 0.5953 0.066 Uiso 1 1 calc R . . C25 C 0.1710(4) 0.7976(4) 0.6512(3) 0.0496(16) Uani 1 1 d . . . H25A H 0.1766 0.8505 0.6726 0.060 Uiso 1 1 calc R . . C26 C 0.1308(4) 0.7337(4) 0.6681(3) 0.0558(18) Uani 1 1 d . . . H26A H 0.1100 0.7424 0.7016 0.067 Uiso 1 1 calc R . . C27 C 0.1210(4) 0.6580(4) 0.6362(3) 0.0465(15) Uani 1 1 d . . . H27A H 0.0943 0.6139 0.6483 0.056 Uiso 1 1 calc R . . N31 N 0.2157(3) 0.2525(3) 0.6732(2) 0.0493(13) Uani 1 1 d . . . C31 C 0.1901(3) 0.3094(4) 0.6889(2) 0.0364(13) Uani 1 1 d . . . C32 C 0.1584(4) 0.3850(4) 0.7070(3) 0.0506(16) Uani 1 1 d . . . H32A H 0.1427 0.4240 0.6699 0.076 Uiso 1 1 calc R . . H32B H 0.1971 0.4119 0.7443 0.076 Uiso 1 1 calc R . . H32C H 0.1141 0.3700 0.7189 0.076 Uiso 1 1 calc R . . N32 N 0.0000 0.3179(5) 0.7500 0.0536(19) Uani 1 2 d S . . C33 C 0.0000 0.2475(6) 0.7500 0.045(2) Uani 1 2 d S . . C34 C 0.0000 0.1556(7) 0.7500 0.092(4) Uani 1 2 d S . . 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 0.01974(12) 0.02013(11) 0.02179(11) 0.00075(10) 0.01153(8) 0.00089(10) Fe1 0.0178(3) 0.0217(3) 0.0215(3) -0.0023(3) 0.0098(3) -0.0005(3) O1 0.0215(17) 0.0197(16) 0.0168(15) -0.0009(13) 0.0109(13) -0.0006(13) N1 0.025(2) 0.024(2) 0.029(2) 0.0043(16) 0.0168(18) 0.0029(17) C1 0.032(3) 0.036(3) 0.019(2) 0.006(2) 0.0122(19) 0.004(2) C2 0.022(3) 0.028(3) 0.027(2) 0.003(2) 0.009(2) 0.005(2) O2 0.0236(18) 0.0266(18) 0.0196(16) 0.0005(13) 0.0088(13) 0.0039(14) C3 0.033(3) 0.028(3) 0.033(3) 0.006(2) 0.019(2) 0.001(2) C4 0.026(3) 0.028(3) 0.025(2) -0.0005(19) 0.015(2) -0.004(2) O3 0.0220(17) 0.0240(17) 0.0235(15) -0.0011(14) 0.0119(12) -0.0028(14) C5 0.030(3) 0.032(3) 0.035(3) 0.013(2) 0.019(2) 0.008(2) C6 0.030(3) 0.033(3) 0.034(3) 0.014(2) 0.014(2) 0.012(2) O4 0.0240(19) 0.034(2) 0.0288(18) 0.0055(14) 0.0161(15) 0.0067(15) O5 0.0219(18) 0.0237(17) 0.0323(18) -0.0039(14) 0.0156(14) -0.0009(14) O6 0.0237(18) 0.0235(18) 0.0297(18) 0.0012(14) 0.0147(14) 0.0029(14) C7 0.014(2) 0.026(3) 0.020(2) 0.0002(18) 0.0065(18) -0.0026(18) C8 0.017(2) 0.030(3) 0.023(2) 0.0013(19) 0.0070(18) -0.001(2) C9 0.042(3) 0.031(3) 0.050(3) -0.004(2) 0.031(3) -0.006(2) C10 0.040(4) 0.055(4) 0.066(4) -0.008(3) 0.038(3) -0.004(3) C11 0.032(3) 0.042(3) 0.050(3) 0.001(3) 0.026(3) -0.010(3) C12 0.029(3) 0.028(3) 0.033(3) 0.002(2) 0.008(2) -0.008(2) C13 0.024(3) 0.032(3) 0.029(3) 0.000(2) 0.010(2) 0.000(2) O7 0.0234(18) 0.0282(18) 0.0251(17) -0.0056(14) 0.0118(14) 0.0006(14) O8 0.0224(18) 0.0271(18) 0.0254(17) -0.0022(13) 0.0116(14) 0.0020(14) C14 0.025(3) 0.024(2) 0.024(2) -0.003(2) 0.0144(19) -0.008(2) C15 0.029(3) 0.036(3) 0.029(3) -0.007(2) 0.018(2) -0.006(2) C16 0.032(3) 0.048(4) 0.031(3) -0.009(2) 0.013(2) -0.004(2) C17 0.034(3) 0.076(5) 0.031(3) -0.015(3) 0.009(3) -0.004(3) C18 0.042(4) 0.088(5) 0.035(3) -0.033(3) 0.018(3) -0.017(3) C19 0.044(4) 0.062(4) 0.050(4) -0.023(3) 0.029(3) -0.006(3) C20 0.029(3) 0.045(3) 0.037(3) -0.015(2) 0.018(2) -0.003(2) O9 0.029(2) 0.0232(17) 0.038(2) 0.0009(14) 0.0201(16) -0.0016(14) O10 0.0219(17) 0.0211(17) 0.0351(18) 0.0029(14) 0.0150(14) -0.0009(14) C21 0.016(2) 0.024(2) 0.030(3) 0.0019(19) 0.007(2) 0.0038(19) C22 0.026(3) 0.024(3) 0.038(3) -0.004(2) 0.011(2) 0.002(2) C23 0.049(4) 0.030(3) 0.052(3) -0.003(3) 0.023(3) -0.005(3) C24 0.060(4) 0.034(3) 0.077(5) -0.013(3) 0.032(4) -0.016(3) C25 0.050(4) 0.035(3) 0.063(4) -0.014(3) 0.019(3) -0.008(3) C26 0.064(5) 0.048(4) 0.066(4) -0.025(3) 0.037(4) -0.012(3) C27 0.054(4) 0.039(3) 0.059(4) -0.013(3) 0.035(3) -0.011(3) N31 0.079(4) 0.044(3) 0.036(3) -0.005(2) 0.035(3) 0.000(3) C31 0.037(3) 0.048(4) 0.027(3) 0.001(2) 0.016(2) -0.005(3) C32 0.042(4) 0.064(4) 0.056(4) 0.010(3) 0.030(3) 0.014(3) N32 0.062(5) 0.049(5) 0.046(4) 0.000 0.014(4) 0.000 C33 0.049(6) 0.044(5) 0.044(5) 0.000 0.017(4) 0.000 C34 0.089(9) 0.034(6) 0.142(12) 0.000 0.026(8) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O2 2.291(3) . ? Dy1 O3 2.351(3) . ? Dy1 O1 2.390(3) . ? Dy1 O9 2.390(3) . ? Dy1 O6 2.425(3) . ? Dy1 O8 2.430(3) 7_556 ? Dy1 O4 2.441(3) . ? Dy1 O10 2.560(3) . ? Dy1 N1 2.627(4) . ? Dy1 Fe1 3.4320(7) . ? Dy1 Fe1 3.4472(7) 7_556 ? Fe1 O2 1.959(3) . ? Fe1 O3 1.962(3) 7_556 ? Fe1 O5 1.989(3) . ? Fe1 O7 1.994(3) . ? Fe1 O1 2.053(3) . ? Fe1 O1 2.063(3) 7_556 ? Fe1 Dy1 3.4472(7) 7_556 ? O1 Fe1 2.063(3) 7_556 ? O1 H1 0.83(3) . ? N1 C3 1.473(6) . ? N1 C1 1.485(6) . ? N1 C5 1.487(6) . ? C1 C2 1.514(7) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 O2 1.411(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.508(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O3 1.415(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? O3 Fe1 1.962(3) 7_556 ? C5 C6 1.498(7) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 O4 1.437(5) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? O4 H4 0.90(3) . ? O5 C7 1.289(5) . ? O6 C7 1.243(5) . ? C7 C8 1.507(6) . ? C8 C13 1.361(7) . ? C8 C9 1.381(7) . ? C9 C10 1.382(7) . ? C9 H9A 0.9500 . ? C10 C11 1.380(8) . ? C10 H10A 0.9500 . ? C11 C12 1.368(7) . ? C11 H11A 0.9500 . ? C12 C13 1.403(7) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? O7 C14 1.285(5) . ? O8 C14 1.240(5) . ? O8 Dy1 2.430(3) 7_556 ? C14 C15 1.498(6) . ? C15 C16 1.383(7) . ? C15 C20 1.394(7) . ? C16 C17 1.381(7) . ? C16 H16A 0.9500 . ? C17 C18 1.368(9) . ? C17 H17A 0.9500 . ? C18 C19 1.394(9) . ? C18 H18A 0.9500 . ? C19 C20 1.368(7) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? O9 C21 1.269(5) . ? O10 C21 1.264(5) . ? C21 C22 1.481(7) . ? C22 C23 1.388(7) . ? C22 C27 1.391(7) . ? C23 C24 1.405(8) . ? C23 H23A 0.9500 . ? C24 C25 1.337(9) . ? C24 H24A 0.9500 . ? C25 C26 1.389(9) . ? C25 H25A 0.9500 . ? C26 C27 1.371(8) . ? C26 H26A 0.9500 . ? C27 H27A 0.9500 . ? N31 C31 1.131(7) . ? C31 C32 1.453(8) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? N32 C33 1.118(11) . ? C33 C34 1.462(14) . ? 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 82.22(11) . . ? O2 Dy1 O1 68.35(10) . . ? O3 Dy1 O1 68.64(10) . . ? O2 Dy1 O9 141.98(11) . . ? O3 Dy1 O9 85.78(11) . . ? O1 Dy1 O9 138.33(11) . . ? O2 Dy1 O6 76.70(11) . . ? O3 Dy1 O6 139.95(11) . . ? O1 Dy1 O6 72.01(10) . . ? O9 Dy1 O6 130.56(11) . . ? O2 Dy1 O8 137.45(11) . 7_556 ? O3 Dy1 O8 73.33(10) . 7_556 ? O1 Dy1 O8 70.45(10) . 7_556 ? O9 Dy1 O8 70.96(11) . 7_556 ? O6 Dy1 O8 100.39(10) . 7_556 ? O2 Dy1 O4 83.43(11) . . ? O3 Dy1 O4 132.34(10) . . ? O1 Dy1 O4 142.97(11) . . ? O9 Dy1 O4 78.41(12) . . ? O6 Dy1 O4 78.68(11) . . ? O8 Dy1 O4 138.37(11) 7_556 . ? O2 Dy1 O10 146.89(11) . . ? O3 Dy1 O10 130.48(10) . . ? O1 Dy1 O10 123.22(10) . . ? O9 Dy1 O10 52.64(10) . . ? O6 Dy1 O10 78.47(10) . . ? O8 Dy1 O10 68.69(10) 7_556 . ? O4 Dy1 O10 70.43(10) . . ? O2 Dy1 N1 66.87(11) . . ? O3 Dy1 N1 68.11(11) . . ? O1 Dy1 N1 120.33(11) . . ? O9 Dy1 N1 75.17(12) . . ? O6 Dy1 N1 129.88(12) . . ? O8 Dy1 N1 129.73(11) 7_556 . ? O4 Dy1 N1 64.44(11) . . ? O10 Dy1 N1 115.93(11) . . ? O2 Fe1 O3 174.80(13) . 7_556 ? O2 Fe1 O5 90.61(13) . . ? O3 Fe1 O5 92.13(13) 7_556 . ? O2 Fe1 O7 92.36(13) . . ? O3 Fe1 O7 91.36(13) 7_556 . ? O5 Fe1 O7 102.39(13) . . ? O2 Fe1 O1 81.92(12) . . ? O3 Fe1 O1 93.70(12) 7_556 . ? O5 Fe1 O1 89.40(12) . . ? O7 Fe1 O1 167.00(13) . . ? O2 Fe1 O1 93.04(13) . 7_556 ? O3 Fe1 O1 83.19(12) 7_556 7_556 ? O5 Fe1 O1 164.90(12) . 7_556 ? O7 Fe1 O1 92.11(12) . 7_556 ? O1 Fe1 O1 76.64(12) . 7_556 ? Fe1 O1 Fe1 103.36(12) . 7_556 ? Fe1 O1 Dy1 100.85(12) . . ? Fe1 O1 Dy1 101.20(12) 7_556 . ? Fe1 O1 H1 128(3) . . ? Fe1 O1 H1 110(3) 7_556 . ? Dy1 O1 H1 111(3) . . ? C3 N1 C1 111.4(4) . . ? C3 N1 C5 110.1(4) . . ? C1 N1 C5 112.2(4) . . ? C3 N1 Dy1 104.3(3) . . ? C1 N1 Dy1 110.9(3) . . ? C5 N1 Dy1 107.6(3) . . ? N1 C1 C2 112.7(4) . . ? N1 C1 H1A 109.1 . . ? C2 C1 H1A 109.1 . . ? N1 C1 H1B 109.1 . . ? C2 C1 H1B 109.1 . . ? H1A C1 H1B 107.8 . . ? O2 C2 C1 108.0(4) . . ? O2 C2 H2A 110.1 . . ? C1 C2 H2A 110.1 . . ? O2 C2 H2B 110.1 . . ? C1 C2 H2B 110.1 . . ? H2A C2 H2B 108.4 . . ? C2 O2 Fe1 131.4(3) . . ? C2 O2 Dy1 121.2(3) . . ? Fe1 O2 Dy1 107.43(13) . . ? N1 C3 C4 111.3(4) . . ? 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 109.5(4) . . ? O3 C4 H4A 109.8 . . ? C3 C4 H4A 109.8 . . ? O3 C4 H4B 109.8 . . ? C3 C4 H4B 109.8 . . ? H4A C4 H4B 108.2 . . ? C4 O3 Fe1 122.1(3) . 7_556 ? C4 O3 Dy1 122.2(3) . . ? Fe1 O3 Dy1 105.77(12) 7_556 . ? 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 108.1(4) . . ? 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 125.1(3) . . ? C6 O4 H4 110(3) . . ? Dy1 O4 H4 120(3) . . ? C7 O5 Fe1 129.0(3) . . ? C7 O6 Dy1 135.2(3) . . ? O6 C7 O5 125.5(4) . . ? O6 C7 C8 120.1(4) . . ? O5 C7 C8 114.3(4) . . ? C13 C8 C9 119.1(4) . . ? C13 C8 C7 120.9(4) . . ? C9 C8 C7 120.0(4) . . ? C8 C9 C10 121.4(5) . . ? C8 C9 H9A 119.3 . . ? C10 C9 H9A 119.3 . . ? C11 C10 C9 118.6(5) . . ? C11 C10 H10A 120.7 . . ? C9 C10 H10A 120.7 . . ? C12 C11 C10 120.9(5) . . ? C12 C11 H11A 119.5 . . ? C10 C11 H11A 119.5 . . ? C11 C12 C13 119.3(5) . . ? C11 C12 H12A 120.4 . . ? C13 C12 H12A 120.4 . . ? C8 C13 C12 120.6(5) . . ? C8 C13 H13A 119.7 . . ? C12 C13 H13A 119.7 . . ? C14 O7 Fe1 124.7(3) . . ? C14 O8 Dy1 139.1(3) . 7_556 ? O8 C14 O7 125.8(4) . . ? O8 C14 C15 118.0(4) . . ? O7 C14 C15 116.1(4) . . ? C16 C15 C20 118.7(5) . . ? C16 C15 C14 121.2(5) . . ? C20 C15 C14 120.1(5) . . ? C17 C16 C15 120.8(5) . . ? C17 C16 H16A 119.6 . . ? C15 C16 H16A 119.6 . . ? C18 C17 C16 120.3(6) . . ? C18 C17 H17A 119.9 . . ? C16 C17 H17A 119.9 . . ? C17 C18 C19 119.6(5) . . ? C17 C18 H18A 120.2 . . ? C19 C18 H18A 120.2 . . ? C20 C19 C18 120.2(6) . . ? C20 C19 H19A 119.9 . . ? C18 C19 H19A 119.9 . . ? C19 C20 C15 120.5(5) . . ? C19 C20 H20A 119.7 . . ? C15 C20 H20A 119.7 . . ? C21 O9 Dy1 96.8(3) . . ? C21 O10 Dy1 89.0(3) . . ? O10 C21 O9 120.6(4) . . ? O10 C21 C22 121.8(4) . . ? O9 C21 C22 117.6(4) . . ? C23 C22 C27 118.8(5) . . ? C23 C22 C21 119.3(5) . . ? C27 C22 C21 121.9(5) . . ? C22 C23 C24 119.8(5) . . ? C22 C23 H23A 120.1 . . ? C24 C23 H23A 120.1 . . ? C25 C24 C23 120.1(6) . . ? C25 C24 H24A 119.9 . . ? C23 C24 H24A 119.9 . . ? C24 C25 C26 120.9(6) . . ? C24 C25 H25A 119.5 . . ? C26 C25 H25A 119.5 . . ? C27 C26 C25 119.7(6) . . ? C27 C26 H26A 120.1 . . ? C25 C26 H26A 120.1 . . ? C26 C27 C22 120.5(6) . . ? C26 C27 H27A 119.7 . . ? C22 C27 H27A 119.7 . . ? N31 C31 C32 177.3(6) . . ? 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 180.000(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 N31 0.83(3) 2.14(3) 2.965(5) 174(5) . O4 H4 O10 0.90(3) 1.83(4) 2.694(4) 158(5) 5_566 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.504 _refine_diff_density_min -0.674 _refine_diff_density_rms 0.128 ######################################################################## 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 ###################################################################### data_amtb16dys _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C78 H106 Dy2 Fe2 N2 O20, 2(C11 H14 O2), 3(C2 H3 N), (C H2 Cl2)' _chemical_formula_sum 'C107 H145 Cl2 Dy2 Fe2 N5 O24' _chemical_formula_weight 2392.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Dy' 'Dy' -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 18.1723(9) _cell_length_b 11.6948(6) _cell_length_c 26.4638(14) _cell_angle_alpha 90.00 _cell_angle_beta 96.466(1) _cell_angle_gamma 90.00 _cell_volume 5588.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 12858 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 27.78 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.422 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2464 _exptl_absorpt_coefficient_mu 1.694 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.724 _exptl_absorpt_correction_T_max 0.902 _exptl_absorpt_process_details 'SADABS 2.10 (Bruker AXS Inc., 2005)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART Apex' _diffrn_measurement_method 'CCD area detector' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27522 _diffrn_reflns_av_R_equivalents 0.0227 _diffrn_reflns_av_sigmaI/netI 0.0280 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 28.07 _reflns_number_total 12356 _reflns_number_gt 10940 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT 5.6 (Bruker AXS Inc., 2005)' _computing_cell_refinement 'SMART-NT 5.6 (Bruker AXS Inc., 2005)' _computing_data_reduction 'SAINT+ 6.45 (Bruker AXS Inc., 2003)' _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. ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.036 0.250 288 69 'CH2Cl2 + MeCN' 2 0.500 -0.013 0.750 288 69 'CH2Cl2 + MeCN' _platon_squeeze_details ; ; _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^)+(0.0392P)^2^+11.8117P] 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 12356 _refine_ls_number_parameters 635 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0499 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.1023 _refine_ls_wR_factor_gt 0.1001 _refine_ls_goodness_of_fit_ref 1.170 _refine_ls_restrained_S_all 1.170 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.568674(9) 0.309895(14) 0.442941(7) 0.02291(6) Uani 1 1 d . . . Fe1 Fe 0.50606(3) 0.58541(5) 0.45255(2) 0.02580(12) Uani 1 1 d . . . O1 O 0.56694(14) 0.4697(2) 0.49944(10) 0.0249(5) Uani 1 1 d . . . H1 H 0.603(2) 0.487(4) 0.5139(17) 0.030 Uiso 1 1 d . . . N1 N 0.44664(17) 0.2208(3) 0.39798(13) 0.0310(7) Uani 1 1 d . . . C1 C 0.4219(2) 0.3037(4) 0.35672(16) 0.0344(9) Uani 1 1 d . . . H1A H 0.3715 0.2832 0.3413 0.041 Uiso 1 1 calc R . . H1B H 0.4556 0.2993 0.3298 0.041 Uiso 1 1 calc R . . C2 C 0.4216(2) 0.4258(4) 0.37728(16) 0.0316(8) Uani 1 1 d . . . H2A H 0.4125 0.4801 0.3486 0.038 Uiso 1 1 calc R . . H2B H 0.3810 0.4343 0.3990 0.038 Uiso 1 1 calc R . . O2 O 0.49028(13) 0.4519(2) 0.40605(10) 0.0263(5) Uani 1 1 d . . . C3 C 0.3900(2) 0.2092(4) 0.43424(17) 0.0345(9) Uani 1 1 d . . . H3A H 0.3608 0.1387 0.4263 0.041 Uiso 1 1 calc R . . H3B H 0.3556 0.2750 0.4301 0.041 Uiso 1 1 calc R . . C4 C 0.4254(2) 0.2043(3) 0.48904(16) 0.0315(8) Uani 1 1 d . . . H4A H 0.3872 0.2144 0.5125 0.038 Uiso 1 1 calc R . . H4B H 0.4496 0.1292 0.4960 0.038 Uiso 1 1 calc R . . O3 O 0.47843(13) 0.2928(2) 0.49634(10) 0.0275(6) Uani 1 1 d . . . C5 C 0.4639(2) 0.1097(3) 0.37539(17) 0.0343(9) Uani 1 1 d . . . H5A H 0.4940 0.1227 0.3470 0.041 Uiso 1 1 calc R . . H5B H 0.4172 0.0719 0.3614 0.041 Uiso 1 1 calc R . . C6 C 0.5059(2) 0.0321(3) 0.41466(18) 0.0365(10) Uani 1 1 d . . . H6A H 0.4720 0.0013 0.4381 0.044 Uiso 1 1 calc R . . H6B H 0.5279 -0.0329 0.3977 0.044 Uiso 1 1 calc R . . O4 O 0.56357(15) 0.1001(2) 0.44251(12) 0.0347(7) Uani 1 1 d . . . H4 H 0.602(3) 0.060(4) 0.4436(18) 0.042 Uiso 1 1 d . . . O5 O 0.59660(14) 0.6302(2) 0.42091(11) 0.0309(6) Uani 1 1 d . . . O6 O 0.65256(14) 0.4591(2) 0.42018(10) 0.0293(6) Uani 1 1 d . . . C7 C 0.6510(2) 0.5648(3) 0.41476(14) 0.0274(8) Uani 1 1 d . . . C8 C 0.7199(2) 0.6236(3) 0.40100(15) 0.0272(8) Uani 1 1 d . . . C9 C 0.7213(2) 0.7403(4) 0.39211(18) 0.0381(10) Uani 1 1 d . . . H9A H 0.6772 0.7838 0.3925 0.046 Uiso 1 1 calc R . . C10 C 0.7863(2) 0.7943(3) 0.38259(17) 0.0345(9) Uani 1 1 d . . . H10A H 0.7856 0.8743 0.3761 0.041 Uiso 1 1 calc R . . C11 C 0.8522(2) 0.7346(3) 0.38226(14) 0.0271(8) Uani 1 1 d . . . C12 C 0.8496(2) 0.6167(3) 0.39037(16) 0.0320(9) Uani 1 1 d . . . H12A H 0.8936 0.5730 0.3900 0.038 Uiso 1 1 calc R . . C13 C 0.7847(2) 0.5617(3) 0.39897(15) 0.0318(9) Uani 1 1 d . . . H13A H 0.7844 0.4811 0.4035 0.038 Uiso 1 1 calc R . . C14 C 0.9257(2) 0.7915(3) 0.37355(15) 0.0290(8) Uani 1 1 d . . . C15 C 0.9174(2) 0.9223(3) 0.36956(16) 0.0327(9) Uani 1 1 d . . . H15A H 0.8801 0.9414 0.3411 0.049 Uiso 1 1 calc R . . H15B H 0.9650 0.9564 0.3638 0.049 Uiso 1 1 calc R . . H15C H 0.9017 0.9523 0.4012 0.049 Uiso 1 1 calc R . . C16 C 0.9851(3) 0.7647(4) 0.41792(19) 0.0467(11) Uani 1 1 d . . . H16A H 0.9915 0.6817 0.4211 0.070 Uiso 1 1 calc R . . H16B H 0.9696 0.7954 0.4495 0.070 Uiso 1 1 calc R . . H16C H 1.0321 0.7999 0.4115 0.070 Uiso 1 1 calc R . . C17 C 0.9513(3) 0.7468(4) 0.32396(19) 0.0438(11) Uani 1 1 d . . . H17A H 0.9136 0.7641 0.2955 0.066 Uiso 1 1 calc R . . H17B H 0.9587 0.6639 0.3264 0.066 Uiso 1 1 calc R . . H17C H 0.9980 0.7839 0.3182 0.066 Uiso 1 1 calc R . . O7 O 0.42676(15) 0.6795(2) 0.41379(11) 0.0310(6) Uani 1 1 d . . . O8 O 0.36556(14) 0.7465(2) 0.47755(10) 0.0267(5) Uani 1 1 d . . . C18 C 0.37918(19) 0.7442(3) 0.43187(15) 0.0261(8) Uani 1 1 d . . . C19 C 0.3352(2) 0.8215(3) 0.39431(15) 0.0272(8) Uani 1 1 d . . . C20 C 0.2779(2) 0.8870(3) 0.40926(14) 0.0312(8) Uani 1 1 d . . . H20A H 0.2683 0.8857 0.4438 0.037 Uiso 1 1 calc R . . C21 C 0.2345(2) 0.9543(4) 0.37459(16) 0.0367(9) Uani 1 1 d . . . H21A H 0.1960 0.9993 0.3858 0.044 Uiso 1 1 calc R . . C22 C 0.2465(2) 0.9569(3) 0.32334(15) 0.0299(8) Uani 1 1 d . A . C23 C 0.3055(2) 0.8928(4) 0.30950(16) 0.0378(10) Uani 1 1 d . . . H23A H 0.3160 0.8947 0.2751 0.045 Uiso 1 1 calc R . . C24 C 0.3491(2) 0.8266(4) 0.34385(16) 0.0342(9) Uani 1 1 d . . . H24A H 0.3889 0.7841 0.3330 0.041 Uiso 1 1 calc R . . C25 C 0.1973(2) 1.0274(4) 0.28407(16) 0.0400(10) Uani 1 1 d DU . . C26A C 0.2450(4) 1.1109(7) 0.2561(3) 0.0525(18) Uani 0.66 1 d PDU A 1 H26A H 0.2705 1.1644 0.2807 0.079 Uiso 0.66 1 calc PR A 1 H26B H 0.2131 1.1536 0.2304 0.079 Uiso 0.66 1 calc PR A 1 H26C H 0.2818 1.0675 0.2396 0.079 Uiso 0.66 1 calc PR A 1 C27A C 0.1377(5) 1.0964(8) 0.3060(3) 0.058(2) Uani 0.66 1 d PDU A 1 H27A H 0.1608 1.1482 0.3322 0.087 Uiso 0.66 1 calc PR A 1 H27B H 0.1038 1.0446 0.3209 0.087 Uiso 0.66 1 calc PR A 1 H27C H 0.1101 1.1412 0.2788 0.087 Uiso 0.66 1 calc PR A 1 C28A C 0.1587(5) 0.9468(6) 0.2426(3) 0.057(2) Uani 0.66 1 d PDU A 1 H28A H 0.1278 0.8916 0.2584 0.085 Uiso 0.66 1 calc PR A 1 H28B H 0.1964 0.9058 0.2260 0.085 Uiso 0.66 1 calc PR A 1 H28C H 0.1278 0.9920 0.2173 0.085 Uiso 0.66 1 calc PR A 1 C26B C 0.2022(10) 1.1498(15) 0.3035(7) 0.059(4) Uiso 0.34 1 d P A 2 H26D H 0.2374 1.1536 0.3343 0.089 Uiso 0.34 1 calc PR A 2 H26E H 0.1533 1.1750 0.3112 0.089 Uiso 0.34 1 calc PR A 2 H26F H 0.2192 1.1996 0.2774 0.089 Uiso 0.34 1 calc PR A 2 C27B C 0.1153(8) 0.9881(14) 0.2879(6) 0.050(3) Uiso 0.34 1 d P A 2 H27D H 0.0976 1.0223 0.3180 0.074 Uiso 0.34 1 calc PR A 2 H27E H 0.1137 0.9046 0.2905 0.074 Uiso 0.34 1 calc PR A 2 H27F H 0.0837 1.0128 0.2574 0.074 Uiso 0.34 1 calc PR A 2 C28B C 0.2137(11) 1.0114(17) 0.2327(7) 0.069(5) Uiso 0.34 1 d P A 2 H28D H 0.2542 1.0623 0.2260 0.103 Uiso 0.34 1 calc PR A 2 H28E H 0.1696 1.0290 0.2091 0.103 Uiso 0.34 1 calc PR A 2 H28F H 0.2283 0.9318 0.2280 0.103 Uiso 0.34 1 calc PR A 2 O9 O 0.68704(14) 0.2292(2) 0.41518(9) 0.0252(5) Uani 1 1 d . . . O10 O 0.59399(14) 0.2687(2) 0.35679(10) 0.0314(6) Uani 1 1 d . . . C29 C 0.6586(2) 0.2325(3) 0.36863(15) 0.0271(8) Uani 1 1 d . . . C30 C 0.7027(2) 0.1898(3) 0.32776(14) 0.0267(7) Uani 1 1 d . . . C31 C 0.7789(2) 0.1839(3) 0.33529(15) 0.0305(8) Uani 1 1 d . . . H31A H 0.8046 0.2076 0.3668 0.037 Uiso 1 1 calc R . . C32 C 0.8183(2) 0.1436(4) 0.29704(15) 0.0309(8) Uani 1 1 d . . . H32A H 0.8708 0.1415 0.3028 0.037 Uiso 1 1 calc R . . C33 C 0.7836(2) 0.1063(3) 0.25076(14) 0.0302(8) Uani 1 1 d . . . C34 C 0.7058(2) 0.1145(5) 0.24366(17) 0.0448(11) Uani 1 1 d . . . H34A H 0.6799 0.0902 0.2123 0.054 Uiso 1 1 calc R . . C35 C 0.6663(2) 0.1571(4) 0.28107(16) 0.0403(10) Uani 1 1 d . . . H35A H 0.6140 0.1641 0.2748 0.048 Uiso 1 1 calc R . . C36 C 0.8262(2) 0.0570(4) 0.20845(16) 0.0350(9) Uani 1 1 d . . . C37 C 0.8198(4) 0.1374(5) 0.16344(19) 0.0674(18) Uani 1 1 d . . . H37A H 0.7674 0.1485 0.1510 0.101 Uiso 1 1 calc R . . H37B H 0.8457 0.1047 0.1363 0.101 Uiso 1 1 calc R . . H37C H 0.8420 0.2113 0.1739 0.101 Uiso 1 1 calc R . . C38 C 0.7961(3) -0.0622(5) 0.1937(3) 0.0697(18) Uani 1 1 d . . . H38A H 0.7429 -0.0571 0.1826 0.105 Uiso 1 1 calc R . . H38B H 0.8043 -0.1132 0.2232 0.105 Uiso 1 1 calc R . . H38C H 0.8218 -0.0926 0.1660 0.105 Uiso 1 1 calc R . . C39 C 0.9099(3) 0.0459(5) 0.22566(19) 0.0523(13) Uani 1 1 d . . . H39A H 0.9303 0.1213 0.2354 0.078 Uiso 1 1 calc R . . H39B H 0.9349 0.0152 0.1977 0.078 Uiso 1 1 calc R . . H39C H 0.9176 -0.0060 0.2549 0.078 Uiso 1 1 calc R . . O11 O 0.69393(14) -0.0272(2) 0.46601(11) 0.0312(6) Uani 1 1 d . . . O12 O 0.78578(15) 0.0970(2) 0.45824(11) 0.0289(6) Uani 1 1 d . . . H12 H 0.757(3) 0.136(4) 0.4423(17) 0.035 Uiso 1 1 d . . . C41 C 0.7590(2) 0.0007(3) 0.47410(14) 0.0254(8) Uani 1 1 d . . . C42 C 0.81565(19) -0.0725(3) 0.50361(14) 0.0240(7) Uani 1 1 d . . . C43 C 0.8873(2) -0.0324(3) 0.51879(14) 0.0276(8) Uani 1 1 d . . . H43A H 0.9003 0.0437 0.5110 0.033 Uiso 1 1 calc R . . C44 C 0.9390(2) -0.1034(3) 0.54509(16) 0.0316(9) Uani 1 1 d . . . H44A H 0.9873 -0.0748 0.5551 0.038 Uiso 1 1 calc R . . C45 C 0.9223(2) -0.2157(3) 0.55743(15) 0.0276(8) Uani 1 1 d . . . C46 C 0.8503(2) -0.2532(3) 0.54290(17) 0.0330(9) Uani 1 1 d . . . H46A H 0.8368 -0.3288 0.5511 0.040 Uiso 1 1 calc R . . C47 C 0.7981(2) -0.1824(3) 0.51681(17) 0.0332(9) Uani 1 1 d . . . H47A H 0.7492 -0.2101 0.5078 0.040 Uiso 1 1 calc R . . C48 C 0.9811(2) -0.2942(4) 0.58538(18) 0.0372(10) Uani 1 1 d . . . C49 C 0.9575(3) -0.4186(4) 0.5828(3) 0.0711(19) Uani 1 1 d . . . H49A H 0.9501 -0.4432 0.5472 0.107 Uiso 1 1 calc R . . H49B H 0.9111 -0.4273 0.5981 0.107 Uiso 1 1 calc R . . H49C H 0.9961 -0.4656 0.6015 0.107 Uiso 1 1 calc R . . C50 C 1.0550(3) -0.2785(6) 0.5654(3) 0.0709(19) Uani 1 1 d . . . H50A H 1.0505 -0.2987 0.5292 0.106 Uiso 1 1 calc R . . H50B H 1.0919 -0.3280 0.5843 0.106 Uiso 1 1 calc R . . H50C H 1.0706 -0.1985 0.5696 0.106 Uiso 1 1 calc R . . C51 C 0.9922(3) -0.2614(6) 0.6427(2) 0.0628(15) Uani 1 1 d . . . H51A H 1.0063 -0.1807 0.6462 0.094 Uiso 1 1 calc R . . H51B H 1.0314 -0.3090 0.6604 0.094 Uiso 1 1 calc R . . H51C H 0.9460 -0.2740 0.6577 0.094 Uiso 1 1 calc R . . N61 N 0.7244(2) 0.5298(4) 0.54198(16) 0.0459(10) Uani 1 1 d . . . C61 C 0.7576(2) 0.4553(4) 0.52975(17) 0.0360(9) Uani 1 1 d . . . C62 C 0.8000(3) 0.3594(4) 0.5138(2) 0.0473(12) Uani 1 1 d . . . H62A H 0.8056 0.3019 0.5409 0.071 Uiso 1 1 calc R . . H62B H 0.8490 0.3859 0.5068 0.071 Uiso 1 1 calc R . . H62C H 0.7739 0.3255 0.4829 0.071 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 0.01674(8) 0.02089(9) 0.03136(10) 0.00297(7) 0.00388(6) 0.00150(6) Fe1 0.0196(2) 0.0227(3) 0.0359(3) 0.0048(2) 0.0062(2) 0.0025(2) O1 0.0179(12) 0.0240(13) 0.0327(14) 0.0045(11) 0.0023(10) -0.0020(10) N1 0.0230(16) 0.0281(17) 0.0406(19) 0.0010(14) -0.0018(14) 0.0020(13) C1 0.0248(19) 0.036(2) 0.040(2) 0.0006(18) -0.0036(16) 0.0036(17) C2 0.0216(18) 0.035(2) 0.037(2) 0.0052(18) -0.0010(15) 0.0038(16) O2 0.0193(12) 0.0264(13) 0.0326(14) 0.0048(11) 0.0004(10) 0.0025(10) C3 0.0198(18) 0.032(2) 0.050(3) 0.0028(18) -0.0011(17) -0.0057(15) C4 0.0229(18) 0.027(2) 0.044(2) 0.0046(17) 0.0051(16) -0.0037(15) O3 0.0190(12) 0.0235(13) 0.0402(15) 0.0025(11) 0.0042(11) -0.0026(10) C5 0.0264(19) 0.028(2) 0.046(2) -0.0039(18) -0.0045(17) -0.0002(16) C6 0.0271(19) 0.0215(19) 0.058(3) -0.0047(18) -0.0087(18) -0.0030(15) O4 0.0257(14) 0.0198(13) 0.0579(19) 0.0022(13) 0.0018(13) 0.0047(11) O5 0.0210(12) 0.0283(14) 0.0452(16) 0.0092(12) 0.0111(11) 0.0017(11) O6 0.0256(13) 0.0224(13) 0.0412(15) 0.0032(11) 0.0094(11) -0.0002(10) C7 0.0257(18) 0.029(2) 0.0285(19) 0.0008(16) 0.0096(15) 0.0014(15) C8 0.0232(18) 0.0256(19) 0.034(2) 0.0012(16) 0.0088(15) -0.0022(15) C9 0.030(2) 0.025(2) 0.063(3) -0.003(2) 0.019(2) 0.0020(16) C10 0.034(2) 0.0210(19) 0.051(2) -0.0026(17) 0.0161(19) -0.0023(16) C11 0.0258(18) 0.0290(19) 0.0275(19) -0.0047(15) 0.0076(15) -0.0053(15) C12 0.0220(18) 0.028(2) 0.047(2) 0.0032(18) 0.0091(17) 0.0035(15) C13 0.033(2) 0.0236(19) 0.041(2) 0.0056(17) 0.0123(17) -0.0002(16) C14 0.0216(17) 0.031(2) 0.035(2) -0.0032(16) 0.0042(15) -0.0056(15) C15 0.034(2) 0.026(2) 0.040(2) -0.0013(17) 0.0125(17) -0.0094(16) C16 0.037(2) 0.044(3) 0.056(3) 0.002(2) -0.007(2) -0.008(2) C17 0.036(2) 0.042(3) 0.056(3) -0.010(2) 0.020(2) -0.011(2) O7 0.0283(14) 0.0286(14) 0.0363(15) 0.0062(12) 0.0045(11) 0.0084(11) O8 0.0239(13) 0.0275(14) 0.0286(14) 0.0033(11) 0.0028(10) 0.0031(11) C18 0.0205(17) 0.0233(18) 0.034(2) 0.0033(15) -0.0010(15) 0.0014(14) C19 0.0270(18) 0.0209(18) 0.033(2) 0.0032(15) 0.0016(15) 0.0015(14) C20 0.038(2) 0.032(2) 0.0229(18) 0.0005(16) 0.0002(16) 0.0116(17) C21 0.041(2) 0.033(2) 0.036(2) -0.0020(18) 0.0028(18) 0.0154(18) C22 0.037(2) 0.0225(19) 0.0290(19) 0.0018(15) -0.0023(16) 0.0044(16) C23 0.045(2) 0.037(2) 0.034(2) 0.0068(18) 0.0102(18) 0.0094(19) C24 0.034(2) 0.033(2) 0.037(2) 0.0055(17) 0.0104(17) 0.0067(17) C25 0.047(2) 0.036(2) 0.034(2) 0.0034(18) -0.0065(19) 0.0154(19) C26A 0.062(5) 0.044(4) 0.048(4) 0.022(3) -0.007(3) 0.010(3) C27A 0.072(5) 0.066(5) 0.037(4) 0.013(3) 0.003(3) 0.039(4) C28A 0.077(5) 0.041(4) 0.045(4) 0.003(3) -0.028(4) 0.011(4) O9 0.0256(13) 0.0251(13) 0.0247(13) 0.0004(10) 0.0019(10) 0.0033(10) O10 0.0261(13) 0.0333(15) 0.0345(15) 0.0033(12) 0.0021(11) 0.0049(11) C29 0.0270(19) 0.0217(18) 0.033(2) 0.0035(15) 0.0055(16) 0.0011(15) C30 0.0265(18) 0.0264(19) 0.0274(18) 0.0035(15) 0.0037(14) 0.0002(15) C31 0.0288(19) 0.035(2) 0.0273(19) -0.0016(17) 0.0012(15) -0.0013(16) C32 0.0244(18) 0.034(2) 0.033(2) 0.0014(17) 0.0000(16) 0.0007(16) C33 0.035(2) 0.029(2) 0.0263(19) 0.0029(16) 0.0028(16) 0.0003(16) C34 0.038(2) 0.065(3) 0.029(2) -0.013(2) -0.0041(18) -0.002(2) C35 0.027(2) 0.058(3) 0.035(2) -0.001(2) -0.0009(17) 0.0025(19) C36 0.038(2) 0.035(2) 0.032(2) -0.0034(17) 0.0052(17) 0.0018(18) C37 0.091(4) 0.078(4) 0.038(3) 0.012(3) 0.025(3) 0.044(4) C38 0.060(3) 0.059(4) 0.095(5) -0.035(3) 0.030(3) -0.012(3) C39 0.045(3) 0.070(4) 0.044(3) -0.001(2) 0.016(2) 0.009(3) O11 0.0205(13) 0.0241(13) 0.0481(17) 0.0024(12) -0.0003(11) -0.0007(10) O12 0.0261(13) 0.0245(14) 0.0357(15) 0.0095(11) 0.0018(11) 0.0020(11) C41 0.0248(18) 0.0227(18) 0.0295(19) -0.0037(15) 0.0068(15) 0.0030(14) C42 0.0199(16) 0.0225(18) 0.0300(19) -0.0006(15) 0.0048(14) 0.0011(14) C43 0.0275(18) 0.0219(18) 0.033(2) -0.0009(15) 0.0023(15) -0.0047(15) C44 0.0240(18) 0.029(2) 0.040(2) 0.0042(17) -0.0041(16) -0.0059(15) C45 0.0247(18) 0.0253(19) 0.033(2) -0.0007(16) 0.0024(15) 0.0002(14) C46 0.0234(18) 0.024(2) 0.051(2) 0.0087(18) 0.0024(17) -0.0041(15) C47 0.0195(17) 0.028(2) 0.052(3) 0.0050(18) 0.0031(16) -0.0041(15) C48 0.0258(19) 0.033(2) 0.051(3) 0.0129(19) -0.0040(18) -0.0011(17) C49 0.043(3) 0.036(3) 0.128(6) 0.017(3) -0.020(3) 0.007(2) C50 0.028(2) 0.094(5) 0.092(4) 0.051(4) 0.015(3) 0.024(3) C51 0.058(3) 0.070(4) 0.056(3) 0.011(3) -0.015(3) 0.011(3) N61 0.0276(18) 0.045(2) 0.066(3) -0.005(2) 0.0104(18) -0.0061(17) C61 0.0238(19) 0.043(3) 0.041(2) -0.0005(19) 0.0026(17) -0.0082(18) C62 0.037(2) 0.048(3) 0.057(3) -0.014(2) 0.007(2) -0.001(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 O3 2.291(3) . ? Dy1 O2 2.329(2) . ? Dy1 O8 2.392(3) 3_666 ? Dy1 O1 2.396(3) . ? Dy1 O10 2.424(3) . ? Dy1 O6 2.437(3) . ? Dy1 O4 2.455(3) . ? Dy1 O9 2.532(2) . ? Dy1 N1 2.612(3) . ? Dy1 Fe1 3.4361(6) . ? Dy1 Fe1 3.4405(6) 3_666 ? Fe1 O3 1.963(3) 3_666 ? Fe1 O2 1.989(3) . ? Fe1 O5 1.998(3) . ? Fe1 O7 2.002(3) . ? Fe1 O1 2.042(3) 3_666 ? Fe1 O1 2.070(3) . ? O1 Fe1 2.042(3) 3_666 ? O1 H1 0.74(4) . ? N1 C5 1.479(5) . ? N1 C3 1.491(5) . ? N1 C1 1.491(5) . ? C1 C2 1.528(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 O2 1.420(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.520(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O3 1.412(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? O3 Fe1 1.963(3) 3_666 ? C5 C6 1.519(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 O4 1.449(5) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? O4 H4 0.84(5) . ? O5 C7 1.274(4) . ? O6 C7 1.244(5) . ? C7 C8 1.510(5) . ? C8 C9 1.386(6) . ? C8 C13 1.387(5) . ? C9 C10 1.387(6) . ? C9 H9A 0.9500 . ? C10 C11 1.387(5) . ? C10 H10A 0.9500 . ? C11 C12 1.398(6) . ? C11 C14 1.534(5) . ? C12 C13 1.385(5) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? C14 C17 1.533(6) . ? C14 C16 1.535(6) . ? C14 C15 1.539(5) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? O7 C18 1.281(4) . ? O8 C18 1.261(5) . ? O8 Dy1 2.392(3) 3_666 ? C18 C19 1.505(5) . ? C19 C20 1.385(5) . ? C19 C24 1.388(6) . ? C20 C21 1.386(5) . ? C20 H20A 0.9500 . ? C21 C22 1.398(6) . ? C21 H21A 0.9500 . ? C22 C23 1.390(6) . ? C22 C25 1.533(5) . ? C23 C24 1.375(6) . ? C23 H23A 0.9500 . ? C24 H24A 0.9500 . ? C25 C28B 1.437(18) . ? C25 C26B 1.519(18) . ? C25 C27A 1.516(8) . ? C25 C26A 1.548(8) . ? C25 C28A 1.552(8) . ? C25 C27B 1.572(15) . ? C26A H26A 0.9800 . ? C26A H26B 0.9800 . ? C26A H26C 0.9800 . ? C27A H27A 0.9800 . ? C27A H27B 0.9800 . ? C27A H27C 0.9800 . ? C28A H28A 0.9800 . ? C28A H28B 0.9800 . ? C28A H28C 0.9800 . ? C26B H26D 0.9800 . ? C26B H26E 0.9800 . ? C26B H26F 0.9800 . ? C27B H27D 0.9800 . ? C27B H27E 0.9800 . ? C27B H27F 0.9800 . ? C28B H28D 0.9800 . ? C28B H28E 0.9800 . ? C28B H28F 0.9800 . ? O9 C29 1.282(5) . ? O10 C29 1.255(4) . ? C29 C30 1.501(5) . ? C30 C31 1.379(5) . ? C30 C35 1.388(6) . ? C31 C32 1.387(6) . ? C31 H31A 0.9500 . ? C32 C33 1.384(5) . ? C32 H32A 0.9500 . ? C33 C34 1.407(6) . ? C33 C36 1.543(6) . ? C34 C35 1.380(6) . ? C34 H34A 0.9500 . ? C35 H35A 0.9500 . ? C36 C37 1.512(7) . ? C36 C38 1.532(7) . ? C36 C39 1.543(6) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? O11 C41 1.223(4) . ? O12 C41 1.314(4) . ? O12 H12 0.78(5) . ? C41 C42 1.490(5) . ? C42 C47 1.379(5) . ? C42 C43 1.399(5) . ? C43 C44 1.381(5) . ? C43 H43A 0.9500 . ? C44 C45 1.395(5) . ? C44 H44A 0.9500 . ? C45 C46 1.393(5) . ? C45 C48 1.534(5) . ? C46 C47 1.384(5) . ? C46 H46A 0.9500 . ? C47 H47A 0.9500 . ? C48 C50 1.510(6) . ? C48 C49 1.515(7) . ? C48 C51 1.556(7) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? N61 C61 1.127(6) . ? C61 C62 1.450(6) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 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 82.77(9) . . ? O3 Dy1 O8 75.81(9) . 3_666 ? O2 Dy1 O8 141.84(9) . 3_666 ? O3 Dy1 O1 67.83(9) . . ? O2 Dy1 O1 69.82(9) . . ? O8 Dy1 O1 72.93(9) 3_666 . ? O3 Dy1 O10 141.96(9) . . ? O2 Dy1 O10 85.37(9) . . ? O8 Dy1 O10 130.05(9) 3_666 . ? O1 Dy1 O10 139.37(9) . . ? O3 Dy1 O6 136.57(9) . . ? O2 Dy1 O6 75.89(9) . . ? O8 Dy1 O6 98.64(9) 3_666 . ? O1 Dy1 O6 69.40(9) . . ? O10 Dy1 O6 73.71(9) . . ? O3 Dy1 O4 83.47(9) . . ? O2 Dy1 O4 133.57(9) . . ? O8 Dy1 O4 75.15(10) 3_666 . ? O1 Dy1 O4 141.20(10) . . ? O10 Dy1 O4 78.94(10) . . ? O6 Dy1 O4 137.63(9) . . ? O3 Dy1 O9 146.81(9) . . ? O2 Dy1 O9 130.05(8) . . ? O8 Dy1 O9 78.23(8) 3_666 . ? O1 Dy1 O9 122.90(8) . . ? O10 Dy1 O9 52.83(8) . . ? O6 Dy1 O9 67.65(8) . . ? O4 Dy1 O9 70.07(9) . . ? O3 Dy1 N1 67.43(10) . . ? O2 Dy1 N1 69.24(9) . . ? O8 Dy1 N1 127.24(10) 3_666 . ? O1 Dy1 N1 121.68(10) . . ? O10 Dy1 N1 74.56(10) . . ? O6 Dy1 N1 134.07(10) . . ? O4 Dy1 N1 64.51(10) . . ? O9 Dy1 N1 115.11(9) . . ? O3 Fe1 O2 174.70(11) 3_666 . ? O3 Fe1 O5 92.15(11) 3_666 . ? O2 Fe1 O5 90.84(11) . . ? O3 Fe1 O7 89.62(11) 3_666 . ? O2 Fe1 O7 93.98(11) . . ? O5 Fe1 O7 102.73(11) . . ? O3 Fe1 O1 81.57(11) 3_666 3_666 ? O2 Fe1 O1 94.50(11) . 3_666 ? O5 Fe1 O1 165.19(11) . 3_666 ? O7 Fe1 O1 90.68(11) . 3_666 ? O3 Fe1 O1 92.04(11) 3_666 . ? O2 Fe1 O1 83.55(11) . . ? O5 Fe1 O1 90.73(10) . . ? O7 Fe1 O1 166.37(11) . . ? O1 Fe1 O1 76.19(11) 3_666 . ? Fe1 O1 Fe1 103.81(11) 3_666 . ? Fe1 O1 Dy1 101.36(10) 3_666 . ? Fe1 O1 Dy1 100.34(11) . . ? Fe1 O1 H1 111(3) 3_666 . ? Fe1 O1 H1 121(4) . . ? Dy1 O1 H1 117(4) . . ? C5 N1 C3 111.9(3) . . ? C5 N1 C1 109.6(3) . . ? C3 N1 C1 111.0(3) . . ? C5 N1 Dy1 109.1(2) . . ? C3 N1 Dy1 110.8(2) . . ? C1 N1 Dy1 104.2(2) . . ? N1 C1 C2 111.1(3) . . ? 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 110.7(3) . . ? 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 123.9(2) . . ? C2 O2 Dy1 122.1(2) . . ? Fe1 O2 Dy1 105.17(11) . . ? N1 C3 C4 111.6(3) . . ? N1 C3 H3A 109.3 . . ? C4 C3 H3A 109.3 . . ? N1 C3 H3B 109.3 . . ? C4 C3 H3B 109.3 . . ? H3A C3 H3B 108.0 . . ? O3 C4 C3 108.2(3) . . ? 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 132.0(2) . 3_666 ? C4 O3 Dy1 120.3(2) . . ? Fe1 O3 Dy1 107.72(11) 3_666 . ? N1 C5 C6 111.2(3) . . ? 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 107.4(3) . . ? 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 125.2(2) . . ? C6 O4 H4 105(3) . . ? Dy1 O4 H4 122(3) . . ? C7 O5 Fe1 125.7(2) . . ? C7 O6 Dy1 137.1(2) . . ? O6 C7 O5 126.1(3) . . ? O6 C7 C8 118.1(3) . . ? O5 C7 C8 115.8(3) . . ? C9 C8 C13 118.4(3) . . ? C9 C8 C7 121.4(3) . . ? C13 C8 C7 120.2(3) . . ? C10 C9 C8 120.8(4) . . ? C10 C9 H9A 119.6 . . ? C8 C9 H9A 119.6 . . ? C9 C10 C11 121.6(4) . . ? C9 C10 H10A 119.2 . . ? C11 C10 H10A 119.2 . . ? C10 C11 C12 116.9(3) . . ? C10 C11 C14 123.4(4) . . ? C12 C11 C14 119.7(3) . . ? C13 C12 C11 121.9(4) . . ? C13 C12 H12A 119.1 . . ? C11 C12 H12A 119.1 . . ? C12 C13 C8 120.4(4) . . ? C12 C13 H13A 119.8 . . ? C8 C13 H13A 119.8 . . ? C17 C14 C11 109.6(3) . . ? C17 C14 C16 109.3(4) . . ? C11 C14 C16 110.3(3) . . ? C17 C14 C15 108.5(3) . . ? C11 C14 C15 111.1(3) . . ? C16 C14 C15 108.1(3) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C18 O7 Fe1 127.6(2) . . ? C18 O8 Dy1 134.8(2) . 3_666 ? O8 C18 O7 125.7(3) . . ? O8 C18 C19 118.3(3) . . ? O7 C18 C19 116.0(3) . . ? C20 C19 C24 118.4(3) . . ? C20 C19 C18 120.2(3) . . ? C24 C19 C18 121.4(3) . . ? C19 C20 C21 121.0(4) . . ? C19 C20 H20A 119.5 . . ? C21 C20 H20A 119.5 . . ? C20 C21 C22 121.0(4) . . ? C20 C21 H21A 119.5 . . ? C22 C21 H21A 119.5 . . ? C23 C22 C21 117.0(4) . . ? C23 C22 C25 121.3(4) . . ? C21 C22 C25 121.7(4) . . ? C24 C23 C22 122.2(4) . . ? C24 C23 H23A 118.9 . . ? C22 C23 H23A 118.9 . . ? C23 C24 C19 120.4(4) . . ? C23 C24 H24A 119.8 . . ? C19 C24 H24A 119.8 . . ? C28B C25 C26B 115.6(11) . . ? C28B C25 C22 113.8(8) . . ? C26B C25 C22 105.6(7) . . ? C27A C25 C22 114.5(4) . . ? C27A C25 C26A 108.0(5) . . ? C22 C25 C26A 110.3(4) . . ? C27A C25 C28A 108.0(6) . . ? C22 C25 C28A 109.5(4) . . ? C26A C25 C28A 106.1(5) . . ? C28B C25 C27B 108.7(10) . . ? C26B C25 C27B 105.9(9) . . ? C22 C25 C27B 106.5(6) . . ? C25 C26A H26A 109.5 . . ? C25 C26A H26B 109.5 . . ? H26A C26A H26B 109.5 . . ? C25 C26A H26C 109.5 . . ? H26A C26A H26C 109.5 . . ? H26B C26A H26C 109.5 . . ? C25 C27A H27A 109.5 . . ? C25 C27A H27B 109.5 . . ? H27A C27A H27B 109.5 . . ? C25 C27A H27C 109.5 . . ? H27A C27A H27C 109.5 . . ? H27B C27A H27C 109.5 . . ? C25 C28A H28A 109.5 . . ? C25 C28A H28B 109.5 . . ? H28A C28A H28B 109.5 . . ? C25 C28A H28C 109.5 . . ? H28A C28A H28C 109.5 . . ? H28B C28A H28C 109.5 . . ? C25 C26B H26D 109.5 . . ? C25 C26B H26E 109.5 . . ? H26D C26B H26E 109.5 . . ? C25 C26B H26F 109.5 . . ? H26D C26B H26F 109.5 . . ? H26E C26B H26F 109.5 . . ? C25 C27B H27D 109.5 . . ? C25 C27B H27E 109.5 . . ? H27D C27B H27E 109.5 . . ? C25 C27B H27F 109.5 . . ? H27D C27B H27F 109.5 . . ? H27E C27B H27F 109.5 . . ? C25 C28B H28D 109.5 . . ? C25 C28B H28E 109.5 . . ? H28D C28B H28E 109.5 . . ? C25 C28B H28F 109.5 . . ? H28D C28B H28F 109.5 . . ? H28E C28B H28F 109.5 . . ? C29 O9 Dy1 90.3(2) . . ? C29 O10 Dy1 96.0(2) . . ? O10 C29 O9 121.0(3) . . ? O10 C29 C30 119.5(3) . . ? O9 C29 C30 119.5(3) . . ? C31 C30 C35 119.0(4) . . ? C31 C30 C29 121.4(3) . . ? C35 C30 C29 119.6(3) . . ? C30 C31 C32 120.3(4) . . ? C30 C31 H31A 119.9 . . ? C32 C31 H31A 119.9 . . ? C33 C32 C31 122.1(4) . . ? C33 C32 H32A 118.9 . . ? C31 C32 H32A 118.9 . . ? C32 C33 C34 116.6(4) . . ? C32 C33 C36 122.9(4) . . ? C34 C33 C36 120.5(4) . . ? C35 C34 C33 121.7(4) . . ? C35 C34 H34A 119.2 . . ? C33 C34 H34A 119.2 . . ? C34 C35 C30 120.3(4) . . ? C34 C35 H35A 119.9 . . ? C30 C35 H35A 119.9 . . ? C37 C36 C38 111.8(5) . . ? C37 C36 C39 105.7(4) . . ? C38 C36 C39 108.1(4) . . ? C37 C36 C33 109.8(4) . . ? C38 C36 C33 109.3(4) . . ? C39 C36 C33 112.1(3) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C41 O12 H12 115(4) . . ? O11 C41 O12 123.9(3) . . ? O11 C41 C42 122.4(3) . . ? O12 C41 C42 113.7(3) . . ? C47 C42 C43 118.4(3) . . ? C47 C42 C41 120.1(3) . . ? C43 C42 C41 121.5(3) . . ? C44 C43 C42 120.0(3) . . ? C44 C43 H43A 120.0 . . ? C42 C43 H43A 120.0 . . ? C43 C44 C45 122.1(4) . . ? C43 C44 H44A 119.0 . . ? C45 C44 H44A 119.0 . . ? C46 C45 C44 117.0(4) . . ? C46 C45 C48 121.7(3) . . ? C44 C45 C48 121.3(3) . . ? C47 C46 C45 121.4(4) . . ? C47 C46 H46A 119.3 . . ? C45 C46 H46A 119.3 . . ? C42 C47 C46 121.2(4) . . ? C42 C47 H47A 119.4 . . ? C46 C47 H47A 119.4 . . ? C50 C48 C49 111.1(5) . . ? C50 C48 C45 110.9(4) . . ? C49 C48 C45 112.0(4) . . ? C50 C48 C51 106.8(4) . . ? C49 C48 C51 106.6(5) . . ? C45 C48 C51 109.3(4) . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C48 C50 H50A 109.5 . . ? C48 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C48 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C48 C51 H51A 109.5 . . ? C48 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C48 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? N61 C61 C62 179.6(6) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? 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 N61 0.74(4) 2.31(5) 3.037(4) 167(5) . O4 H4 O11 0.84(5) 1.99(5) 2.808(4) 165(5) . _diffrn_measured_fraction_theta_max 0.908 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.653 _refine_diff_density_min -0.949 _refine_diff_density_rms 0.098 ####################################################################### data_amnb16dy _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H52 Dy2 Fe2 N8 O32, 2(C H4 O), 7.7(C2 H3 N), 0.3(H2 O)' _chemical_formula_sum 'C71.4 H83.7 Dy2 Fe2 N15.7 O34.3' _chemical_formula_weight 2147.34 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 11.0959(10) _cell_length_b 14.0354(12) _cell_length_c 14.3715(11) _cell_angle_alpha 85.882(7) _cell_angle_beta 89.474(7) _cell_angle_gamma 75.941(7) _cell_volume 2165.4(3) _cell_formula_units_Z 1 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 19649 _cell_measurement_theta_min 1.42 _cell_measurement_theta_max 27.10 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.647 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1080 _exptl_absorpt_coefficient_mu 2.128 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.512 _exptl_absorpt_correction_T_max 0.597 _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 15906 _diffrn_reflns_av_R_equivalents 0.0482 _diffrn_reflns_av_sigmaI/netI 0.0799 _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 16 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 26.82 _reflns_number_total 9149 _reflns_number_gt 6930 _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^)+(0.0167P)^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 9149 _refine_ls_number_parameters 590 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0589 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.0643 _refine_ls_wR_factor_gt 0.0612 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.984 _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 0.59449(2) 0.564644(15) 0.677379(15) 0.02603(6) Uani 1 1 d . . . Fe1 Fe 0.50656(5) 0.39360(4) 0.55103(4) 0.02735(13) Uani 1 1 d . . . O1 O 0.4430(2) 0.54008(19) 0.56985(18) 0.0267(6) Uani 1 1 d D . . H1 H 0.369(3) 0.557(3) 0.584(3) 0.032 Uiso 1 1 d D . . N1 N 0.8295(3) 0.5115(2) 0.6406(2) 0.0294(7) Uani 1 1 d . . . C1 C 0.8622(4) 0.4122(3) 0.6026(3) 0.0382(10) Uani 1 1 d . . . H1A H 0.9465 0.3767 0.6246 0.046 Uiso 1 1 calc R . . H1B H 0.8637 0.4203 0.5336 0.046 Uiso 1 1 calc R . . C2 C 0.7709(4) 0.3512(3) 0.6322(3) 0.0332(9) Uani 1 1 d . . . H2A H 0.7830 0.2936 0.5942 0.040 Uiso 1 1 calc R . . H2B H 0.7850 0.3271 0.6985 0.040 Uiso 1 1 calc R . . O2 O 0.6479(2) 0.41093(18) 0.61928(18) 0.0293(6) Uani 1 1 d . . . C3 C 0.8508(4) 0.5890(3) 0.5711(3) 0.0351(9) Uani 1 1 d . . . H3A H 0.9362 0.5690 0.5466 0.042 Uiso 1 1 calc R . . H3B H 0.8427 0.6512 0.6017 0.042 Uiso 1 1 calc R . . C4 C 0.7585(4) 0.6058(3) 0.4910(3) 0.0335(9) Uani 1 1 d . . . H4B H 0.7640 0.6656 0.4520 0.040 Uiso 1 1 calc R . . H4C H 0.7790 0.5492 0.4515 0.040 Uiso 1 1 calc R . . O3 O 0.6369(2) 0.61700(18) 0.52468(17) 0.0290(6) Uani 1 1 d . . . C5 C 0.9012(4) 0.5127(3) 0.7270(3) 0.0352(10) Uani 1 1 d . . . H5A H 0.8875 0.5812 0.7451 0.042 Uiso 1 1 calc R . . H5B H 0.9910 0.4877 0.7151 0.042 Uiso 1 1 calc R . . C6 C 0.8622(4) 0.4499(3) 0.8054(3) 0.0402(11) Uani 1 1 d . . . H6A H 0.8919 0.3793 0.7943 0.048 Uiso 1 1 calc R . . H6B H 0.8973 0.4615 0.8655 0.048 Uiso 1 1 calc R . . O4 O 0.7294(3) 0.4778(2) 0.8072(2) 0.0382(7) Uani 1 1 d D . . H4 H 0.699(4) 0.446(3) 0.847(3) 0.046 Uiso 1 1 d D . . O5 O 0.4209(3) 0.36281(19) 0.66943(18) 0.0338(6) Uani 1 1 d . . . O6 O 0.4660(3) 0.4748(2) 0.76041(19) 0.0340(7) Uani 1 1 d . . . C7 C 0.4114(4) 0.4091(3) 0.7438(3) 0.0320(9) Uani 1 1 d . . . C8 C 0.3254(4) 0.3831(3) 0.8158(3) 0.0301(9) Uani 1 1 d . . . C9 C 0.3140(4) 0.4257(3) 0.9011(3) 0.0378(10) Uani 1 1 d . . . H9A H 0.3643 0.4692 0.9142 0.045 Uiso 1 1 calc R . . C10 C 0.2308(4) 0.4055(3) 0.9667(3) 0.0410(11) Uani 1 1 d . . . H10A H 0.2232 0.4346 1.0248 0.049 Uiso 1 1 calc R . . C11 C 0.1589(4) 0.3423(3) 0.9465(3) 0.0339(9) Uani 1 1 d . . . C12 C 0.1684(4) 0.2979(3) 0.8627(3) 0.0363(10) Uani 1 1 d . . . H12A H 0.1186 0.2538 0.8503 0.044 Uiso 1 1 calc R . . C13 C 0.2520(4) 0.3193(3) 0.7980(3) 0.0358(10) Uani 1 1 d . . . H13A H 0.2596 0.2898 0.7401 0.043 Uiso 1 1 calc R . . N2 N 0.0713(4) 0.3184(3) 1.0161(3) 0.0452(9) Uani 1 1 d . . . O7 O 0.0199(3) 0.2534(3) 1.0030(2) 0.0632(10) Uani 1 1 d . . . O8 O 0.0554(4) 0.3635(3) 1.0863(2) 0.0684(11) Uani 1 1 d . . . O9 O 0.6031(3) 0.26147(18) 0.51321(18) 0.0313(6) Uani 1 1 d . . . O10 O 0.5611(3) 0.28150(19) 0.35880(18) 0.0331(7) Uani 1 1 d . . . C14 C 0.6139(4) 0.2346(3) 0.4299(3) 0.0300(9) Uani 1 1 d . . . C15 C 0.6999(4) 0.1347(3) 0.4192(3) 0.0292(9) Uani 1 1 d . . . C16 C 0.7762(4) 0.0862(3) 0.4918(3) 0.0350(10) Uani 1 1 d . . . H16A H 0.7776 0.1172 0.5483 0.042 Uiso 1 1 calc R . . C17 C 0.8508(4) -0.0075(3) 0.4833(3) 0.0328(9) Uani 1 1 d . . . H17A H 0.9030 -0.0414 0.5332 0.039 Uiso 1 1 calc R . . C18 C 0.8469(4) -0.0497(3) 0.4006(3) 0.0351(10) Uani 1 1 d . . . C19 C 0.7733(4) -0.0025(3) 0.3254(3) 0.0388(10) Uani 1 1 d . . . H19A H 0.7732 -0.0333 0.2686 0.047 Uiso 1 1 calc R . . C20 C 0.7000(4) 0.0907(3) 0.3361(3) 0.0361(10) Uani 1 1 d . . . H20A H 0.6491 0.1251 0.2857 0.043 Uiso 1 1 calc R . . N3 N 0.9196(4) -0.1508(3) 0.3913(3) 0.0441(9) Uani 1 1 d . . . O11 O 0.9129(4) -0.1889(2) 0.3188(2) 0.0620(10) Uani 1 1 d . . . O12 O 0.9872(4) -0.1917(2) 0.4571(3) 0.0615(10) Uani 1 1 d . . . O13 O 0.6782(3) 0.69848(19) 0.72876(18) 0.0330(6) Uani 1 1 d . . . O14 O 0.5376(3) 0.6536(2) 0.82076(18) 0.0337(6) Uani 1 1 d . . . C21 C 0.6100(4) 0.7076(3) 0.8013(3) 0.0336(10) Uani 1 1 d . . . C22 C 0.6211(4) 0.7837(3) 0.8671(3) 0.0325(9) Uani 1 1 d . . . C23 C 0.5565(4) 0.7899(3) 0.9502(3) 0.0372(10) Uani 1 1 d . . . H23A H 0.5005 0.7492 0.9630 0.045 Uiso 1 1 calc R . . C24 C 0.5720(4) 0.8539(3) 1.0147(3) 0.0399(11) Uani 1 1 d . . . H24A H 0.5274 0.8581 1.0716 0.048 Uiso 1 1 calc R . . C25 C 0.6545(4) 0.9120(3) 0.9943(3) 0.0395(11) Uani 1 1 d . . . C26 C 0.7198(5) 0.9099(3) 0.9117(3) 0.0476(12) Uani 1 1 d . . . H26A H 0.7754 0.9511 0.8993 0.057 Uiso 1 1 calc R . . C27 C 0.7012(4) 0.8457(3) 0.8477(3) 0.0412(11) Uani 1 1 d . . . H27A H 0.7433 0.8436 0.7898 0.049 Uiso 1 1 calc R . . N4 N 0.6788(4) 0.9763(3) 1.0645(3) 0.0527(11) Uani 1 1 d . . . O15 O 0.6164(4) 0.9801(3) 1.1363(3) 0.0679(11) Uani 1 1 d . . . O16 O 0.7571(4) 1.0223(3) 1.0499(3) 0.0811(13) Uani 1 1 d . . . N31 N 0.1878(4) 0.6305(3) 0.6335(3) 0.0545(11) Uani 1 1 d . . . C31 C 0.1092(4) 0.6916(4) 0.6560(3) 0.0441(11) Uani 1 1 d . . . C32 C 0.0106(5) 0.7709(4) 0.6870(4) 0.0560(13) Uani 1 1 d . . . H32A H -0.0140 0.7532 0.7504 0.084 Uiso 1 1 calc R . . H32B H -0.0611 0.7819 0.6448 0.084 Uiso 1 1 calc R . . H32C H 0.0403 0.8312 0.6869 0.084 Uiso 1 1 calc R . . N32A N 0.6943(6) 0.3653(4) 0.9689(4) 0.0745(17) Uani 0.85 1 d P A 1 C33A C 0.7158(6) 0.3251(5) 1.0434(5) 0.0602(18) Uani 0.85 1 d P A 1 C34A C 0.7509(6) 0.2742(6) 1.1298(4) 0.073(2) Uani 0.85 1 d P A 1 H34A H 0.7263 0.2116 1.1328 0.109 Uiso 0.85 1 calc PR A 1 H34B H 0.7098 0.3140 1.1797 0.109 Uiso 0.85 1 calc PR A 1 H34C H 0.8412 0.2614 1.1376 0.109 Uiso 0.85 1 calc PR A 1 O32B O 0.699(2) 0.3191(15) 0.9015(15) 0.046(5) Uiso 0.15 1 d P B 2 N33 N 0.0938(5) 0.9874(4) 0.2747(4) 0.0849(16) Uani 1 1 d . . . C35 C 0.0836(6) 0.9434(5) 0.2134(5) 0.0709(16) Uani 1 1 d . . . C36 C 0.0715(8) 0.8880(6) 0.1338(5) 0.098(2) Uani 1 1 d . . . H36A H -0.0155 0.9044 0.1130 0.147 Uiso 1 1 calc R . . H36B H 0.0981 0.8173 0.1518 0.147 Uiso 1 1 calc R . . H36C H 0.1236 0.9048 0.0828 0.147 Uiso 1 1 calc R . . N34 N 0.3701(7) 0.8179(5) 0.1886(6) 0.109(2) Uani 1 1 d . . . C37 C 0.4054(8) 0.8579(7) 0.2451(7) 0.092(2) Uani 1 1 d . . . C38 C 0.4506(9) 0.9050(7) 0.3127(5) 0.114(3) Uani 1 1 d . . . H38A H 0.5015 0.9469 0.2836 0.170 Uiso 1 1 calc R . . H38B H 0.5015 0.8560 0.3575 0.170 Uiso 1 1 calc R . . H38C H 0.3810 0.9458 0.3453 0.170 Uiso 1 1 calc R . . O41 O 0.7111(5) 0.8492(4) 0.5997(4) 0.1010(16) Uani 1 1 d D . . H41 H 0.685(8) 0.793(5) 0.638(5) 0.151 Uiso 1 1 d D . . C41A C 0.6171(7) 0.8750(7) 0.5342(6) 0.085(3) Uani 0.85 1 d PD C 1 H41A H 0.6147 0.8177 0.4998 0.128 Uiso 0.85 1 calc PR C 1 H41B H 0.6322 0.9278 0.4906 0.128 Uiso 0.85 1 calc PR C 1 H41C H 0.5376 0.8980 0.5654 0.128 Uiso 0.85 1 calc PR C 1 C41B C 0.684(4) 0.810(3) 0.5173(19) 0.062(10) Uiso 0.15 1 d PD C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.02501(10) 0.02508(9) 0.02632(10) -0.00507(7) 0.00321(7) -0.00203(7) Fe1 0.0277(3) 0.0250(3) 0.0274(3) -0.0045(2) 0.0033(2) -0.0020(2) O1 0.0232(14) 0.0264(14) 0.0281(14) -0.0056(11) 0.0049(12) -0.0008(11) N1 0.0260(18) 0.0280(17) 0.0336(19) -0.0061(14) -0.0004(14) -0.0042(14) C1 0.032(2) 0.035(2) 0.044(3) -0.0104(19) 0.005(2) 0.0017(19) C2 0.026(2) 0.029(2) 0.039(2) -0.0048(17) -0.0008(18) 0.0026(17) O2 0.0248(15) 0.0263(14) 0.0344(15) -0.0067(11) 0.0017(12) -0.0004(11) C3 0.030(2) 0.037(2) 0.039(2) -0.0079(18) 0.0061(18) -0.0064(18) C4 0.028(2) 0.040(2) 0.033(2) -0.0052(18) 0.0015(18) -0.0081(18) O3 0.0264(15) 0.0295(14) 0.0292(15) -0.0042(11) 0.0074(11) -0.0030(11) C5 0.030(2) 0.042(2) 0.034(2) -0.0110(18) 0.0013(18) -0.0073(19) C6 0.034(2) 0.041(2) 0.040(3) -0.006(2) -0.006(2) 0.003(2) O4 0.0341(17) 0.0433(18) 0.0344(17) 0.0029(13) 0.0036(13) -0.0060(14) O5 0.0370(17) 0.0326(15) 0.0315(15) -0.0054(12) 0.0057(13) -0.0074(13) O6 0.0383(17) 0.0330(15) 0.0316(16) -0.0050(12) 0.0073(13) -0.0097(13) C7 0.034(2) 0.030(2) 0.029(2) -0.0019(17) 0.0018(18) -0.0017(18) C8 0.032(2) 0.034(2) 0.024(2) -0.0011(16) 0.0050(17) -0.0081(18) C9 0.044(3) 0.037(2) 0.034(2) -0.0104(19) 0.007(2) -0.012(2) C10 0.050(3) 0.045(3) 0.028(2) -0.0085(19) 0.011(2) -0.012(2) C11 0.026(2) 0.037(2) 0.036(2) 0.0007(18) 0.0059(18) -0.0029(18) C12 0.031(2) 0.037(2) 0.040(3) -0.0022(19) 0.0051(19) -0.0073(19) C13 0.038(3) 0.041(2) 0.028(2) -0.0056(18) 0.0011(18) -0.007(2) N2 0.041(2) 0.059(3) 0.036(2) -0.0031(19) 0.0110(18) -0.013(2) O7 0.056(2) 0.089(3) 0.059(2) -0.013(2) 0.0184(18) -0.044(2) O8 0.080(3) 0.087(3) 0.049(2) -0.024(2) 0.037(2) -0.036(2) O9 0.0340(16) 0.0259(14) 0.0308(15) -0.0060(11) 0.0015(12) 0.0000(12) O10 0.0337(16) 0.0284(14) 0.0313(16) -0.0028(12) 0.0004(13) 0.0040(12) C14 0.028(2) 0.028(2) 0.035(2) -0.0057(17) 0.0041(18) -0.0070(17) C15 0.026(2) 0.027(2) 0.034(2) -0.0059(16) 0.0027(17) -0.0047(16) C16 0.041(3) 0.029(2) 0.033(2) -0.0089(17) 0.0001(19) -0.0014(19) C17 0.029(2) 0.031(2) 0.034(2) -0.0029(17) -0.0042(18) -0.0007(17) C18 0.035(2) 0.027(2) 0.040(2) -0.0079(18) 0.0019(19) -0.0001(18) C19 0.043(3) 0.040(2) 0.032(2) -0.0128(19) 0.003(2) -0.006(2) C20 0.038(3) 0.035(2) 0.031(2) -0.0060(18) 0.0008(19) -0.0006(19) N3 0.041(2) 0.035(2) 0.051(2) -0.0103(18) -0.0015(19) 0.0034(17) O11 0.071(3) 0.045(2) 0.059(2) -0.0249(17) -0.0075(19) 0.0117(17) O12 0.067(3) 0.0403(19) 0.062(2) -0.0136(16) -0.008(2) 0.0196(17) O13 0.0304(16) 0.0377(16) 0.0301(15) -0.0114(12) 0.0092(12) -0.0043(12) O14 0.0317(16) 0.0347(15) 0.0331(16) -0.0069(12) 0.0047(12) -0.0037(13) C21 0.033(2) 0.029(2) 0.035(2) -0.0044(17) -0.0043(19) -0.0011(19) C22 0.029(2) 0.032(2) 0.033(2) -0.0068(17) 0.0008(18) 0.0003(17) C23 0.033(2) 0.043(2) 0.036(2) -0.0102(19) 0.0038(19) -0.009(2) C24 0.041(3) 0.045(3) 0.031(2) -0.015(2) 0.003(2) -0.002(2) C25 0.041(3) 0.035(2) 0.038(3) -0.0135(19) -0.009(2) 0.003(2) C26 0.051(3) 0.044(3) 0.052(3) -0.013(2) -0.001(2) -0.016(2) C27 0.043(3) 0.040(2) 0.041(3) -0.012(2) 0.007(2) -0.008(2) N4 0.055(3) 0.051(3) 0.050(3) -0.020(2) -0.008(2) -0.003(2) O15 0.086(3) 0.068(3) 0.047(2) -0.0229(19) -0.009(2) -0.007(2) O16 0.086(3) 0.092(3) 0.085(3) -0.046(2) 0.008(2) -0.049(3) N31 0.039(3) 0.061(3) 0.063(3) -0.025(2) 0.004(2) -0.008(2) C31 0.034(3) 0.055(3) 0.047(3) -0.013(2) 0.004(2) -0.015(2) C32 0.046(3) 0.059(3) 0.056(3) -0.013(2) 0.005(2) 0.001(2) N32A 0.083(5) 0.072(4) 0.068(4) 0.002(3) 0.010(3) -0.022(3) C33A 0.064(4) 0.055(4) 0.065(4) 0.010(3) -0.027(3) -0.023(3) C34A 0.048(4) 0.127(6) 0.035(3) 0.011(4) 0.010(3) -0.012(4) N33 0.082(4) 0.089(4) 0.084(4) -0.031(3) 0.015(3) -0.016(3) C35 0.065(4) 0.073(4) 0.080(4) -0.017(3) 0.021(3) -0.023(3) C36 0.109(6) 0.114(6) 0.094(5) -0.040(4) 0.004(4) -0.065(5) N34 0.094(5) 0.104(5) 0.120(6) -0.014(4) 0.027(5) -0.010(4) C37 0.087(6) 0.093(6) 0.086(6) 0.008(5) 0.032(5) -0.008(5) C38 0.135(8) 0.138(8) 0.074(5) 0.003(5) 0.021(5) -0.048(6) O41 0.117(4) 0.091(4) 0.100(4) 0.017(3) 0.001(3) -0.042(3) C41A 0.052(5) 0.107(7) 0.101(6) 0.031(5) -0.015(4) -0.038(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O2 2.309(2) . ? Dy1 O3 2.344(2) . ? Dy1 O6 2.381(3) . ? Dy1 O1 2.396(3) . ? Dy1 O10 2.441(3) 2_666 ? Dy1 O13 2.448(3) . ? Dy1 O4 2.459(3) . ? Dy1 O14 2.483(3) . ? Dy1 N1 2.592(3) . ? Fe1 O2 1.931(3) . ? Fe1 O3 1.977(3) 2_666 ? Fe1 O5 2.012(3) . ? Fe1 O9 2.013(3) . ? Fe1 O1 2.042(3) . ? Fe1 O1 2.050(3) 2_666 ? O1 Fe1 2.050(3) 2_666 ? O1 H1 0.82(3) . ? N1 C3 1.483(5) . ? N1 C5 1.485(5) . ? N1 C1 1.494(5) . ? C1 C2 1.516(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 O2 1.424(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.515(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O3 1.405(5) . ? C4 H4B 0.9900 . ? C4 H4C 0.9900 . ? O3 Fe1 1.977(3) 2_666 ? C5 C6 1.506(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 O4 1.430(5) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? O4 H4 0.82(3) . ? O5 C7 1.280(5) . ? O6 C7 1.257(5) . ? C7 C8 1.488(6) . ? C8 C13 1.387(6) . ? C8 C9 1.393(5) . ? C9 C10 1.376(6) . ? C9 H9A 0.9500 . ? C10 C11 1.376(6) . ? C10 H10A 0.9500 . ? C11 C12 1.387(6) . ? C11 N2 1.467(5) . ? C12 C13 1.376(6) . ? C12 H12A 0.9500 . ? C13 H13A 0.9500 . ? N2 O7 1.213(5) . ? N2 O8 1.218(5) . ? O9 C14 1.278(4) . ? O10 C14 1.244(4) . ? O10 Dy1 2.441(3) 2_666 ? C14 C15 1.509(5) . ? C15 C16 1.380(5) . ? C15 C20 1.383(5) . ? C16 C17 1.385(5) . ? C16 H16A 0.9500 . ? C17 C18 1.372(6) . ? C17 H17A 0.9500 . ? C18 C19 1.387(6) . ? C18 N3 1.466(5) . ? C19 C20 1.381(6) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? N3 O11 1.215(5) . ? N3 O12 1.230(5) . ? O13 C21 1.278(5) . ? O14 C21 1.248(5) . ? C21 C22 1.504(6) . ? C22 C23 1.384(6) . ? C22 C27 1.400(6) . ? C23 C24 1.376(6) . ? C23 H23A 0.9500 . ? C24 C25 1.382(6) . ? C24 H24A 0.9500 . ? C25 C26 1.383(6) . ? C25 N4 1.470(6) . ? C26 C27 1.383(6) . ? C26 H26A 0.9500 . ? C27 H27A 0.9500 . ? N4 O16 1.210(6) . ? N4 O15 1.235(5) . ? N31 C31 1.127(6) . ? C31 C32 1.451(7) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? N32A C33A 1.172(7) . ? C33A C34A 1.397(8) . ? C34A H34A 0.9800 . ? C34A H34B 0.9800 . ? C34A H34C 0.9800 . ? N33 C35 1.133(7) . ? C35 C36 1.454(9) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? N34 C37 1.143(10) . ? C37 C38 1.377(12) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? O41 C41A 1.375(8) . ? O41 C41B 1.405(19) . ? O41 H41 1.03(4) . ? C41A H41A 0.9800 . ? C41A H41B 0.9800 . ? C41A H41C 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 82.94(9) . . ? O2 Dy1 O6 75.75(9) . . ? O3 Dy1 O6 140.68(9) . . ? O2 Dy1 O1 67.30(9) . . ? O3 Dy1 O1 69.05(9) . . ? O6 Dy1 O1 72.31(9) . . ? O2 Dy1 O10 136.24(9) . 2_666 ? O3 Dy1 O10 74.59(9) . 2_666 ? O6 Dy1 O10 98.73(10) . 2_666 ? O1 Dy1 O10 69.69(9) . 2_666 ? O2 Dy1 O13 143.86(9) . . ? O3 Dy1 O13 86.96(9) . . ? O6 Dy1 O13 128.77(9) . . ? O1 Dy1 O13 139.29(9) . . ? O10 Dy1 O13 72.50(9) 2_666 . ? O2 Dy1 O4 82.10(10) . . ? O3 Dy1 O4 132.44(10) . . ? O6 Dy1 O4 77.06(10) . . ? O1 Dy1 O4 140.86(9) . . ? O10 Dy1 O4 139.91(9) 2_666 . ? O13 Dy1 O4 79.47(9) . . ? O2 Dy1 O14 144.29(9) . . ? O3 Dy1 O14 132.57(9) . . ? O6 Dy1 O14 76.00(9) . . ? O1 Dy1 O14 122.81(9) . . ? O10 Dy1 O14 69.70(9) 2_666 . ? O13 Dy1 O14 53.31(9) . . ? O4 Dy1 O14 70.64(9) . . ? O2 Dy1 N1 68.18(10) . . ? O3 Dy1 N1 68.23(9) . . ? O6 Dy1 N1 129.52(10) . . ? O1 Dy1 N1 120.54(9) . . ? O10 Dy1 N1 131.75(10) 2_666 . ? O13 Dy1 N1 75.83(9) . . ? O4 Dy1 N1 64.28(10) . . ? O14 Dy1 N1 116.44(10) . . ? O2 Fe1 O3 176.25(11) . 2_666 ? O2 Fe1 O5 91.94(11) . . ? O3 Fe1 O5 91.05(11) 2_666 . ? O2 Fe1 O9 91.26(11) . . ? O3 Fe1 O9 90.16(11) 2_666 . ? O5 Fe1 O9 104.51(11) . . ? O2 Fe1 O1 82.02(11) . . ? O3 Fe1 O1 95.79(11) 2_666 . ? O5 Fe1 O1 89.00(11) . . ? O9 Fe1 O1 165.16(11) . . ? O2 Fe1 O1 92.84(11) . 2_666 ? O3 Fe1 O1 83.69(10) 2_666 2_666 ? O5 Fe1 O1 164.39(11) . 2_666 ? O9 Fe1 O1 90.24(11) . 2_666 ? O1 Fe1 O1 76.98(11) . 2_666 ? Fe1 O1 Fe1 103.02(11) . 2_666 ? Fe1 O1 Dy1 101.20(11) . . ? Fe1 O1 Dy1 101.19(11) 2_666 . ? Fe1 O1 H1 115(3) . . ? Fe1 O1 H1 116(3) 2_666 . ? Dy1 O1 H1 118(3) . . ? C3 N1 C5 109.4(3) . . ? C3 N1 C1 111.6(3) . . ? C5 N1 C1 111.3(3) . . ? C3 N1 Dy1 104.6(2) . . ? C5 N1 Dy1 108.7(2) . . ? C1 N1 Dy1 111.1(2) . . ? N1 C1 C2 112.3(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 108.9(3) . . ? O2 C2 H2A 109.9 . . ? C1 C2 H2A 109.9 . . ? O2 C2 H2B 109.9 . . ? C1 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? C2 O2 Fe1 132.0(2) . . ? C2 O2 Dy1 119.9(2) . . ? Fe1 O2 Dy1 107.97(11) . . ? N1 C3 C4 111.0(3) . . ? 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 110.7(3) . . ? O3 C4 H4B 109.5 . . ? C3 C4 H4B 109.5 . . ? O3 C4 H4C 109.5 . . ? C3 C4 H4C 109.5 . . ? H4B C4 H4C 108.1 . . ? C4 O3 Fe1 124.5(2) . 2_666 ? C4 O3 Dy1 122.6(2) . . ? Fe1 O3 Dy1 105.30(11) 2_666 . ? N1 C5 C6 110.8(3) . . ? 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 106.5(3) . . ? O4 C6 H6A 110.4 . . ? C5 C6 H6A 110.4 . . ? O4 C6 H6B 110.4 . . ? C5 C6 H6B 110.4 . . ? H6A C6 H6B 108.6 . . ? C6 O4 Dy1 125.3(2) . . ? C6 O4 H4 114(3) . . ? Dy1 O4 H4 117(3) . . ? C7 O5 Fe1 126.5(3) . . ? C7 O6 Dy1 136.9(3) . . ? O6 C7 O5 126.2(4) . . ? O6 C7 C8 117.7(3) . . ? O5 C7 C8 116.1(4) . . ? C13 C8 C9 119.0(4) . . ? C13 C8 C7 120.7(4) . . ? C9 C8 C7 120.3(4) . . ? C10 C9 C8 120.8(4) . . ? C10 C9 H9A 119.6 . . ? C8 C9 H9A 119.6 . . ? C9 C10 C11 118.7(4) . . ? C9 C10 H10A 120.6 . . ? C11 C10 H10A 120.6 . . ? C10 C11 C12 122.1(4) . . ? C10 C11 N2 119.6(4) . . ? C12 C11 N2 118.3(4) . . ? C13 C12 C11 118.2(4) . . ? C13 C12 H12A 120.9 . . ? C11 C12 H12A 120.9 . . ? C12 C13 C8 121.2(4) . . ? C12 C13 H13A 119.4 . . ? C8 C13 H13A 119.4 . . ? O7 N2 O8 122.6(4) . . ? O7 N2 C11 119.2(4) . . ? O8 N2 C11 118.1(4) . . ? C14 O9 Fe1 125.4(2) . . ? C14 O10 Dy1 136.9(3) . 2_666 ? O10 C14 O9 126.9(4) . . ? O10 C14 C15 118.2(3) . . ? O9 C14 C15 114.9(3) . . ? C16 C15 C20 119.8(4) . . ? C16 C15 C14 120.8(3) . . ? C20 C15 C14 119.3(3) . . ? C15 C16 C17 120.7(4) . . ? C15 C16 H16A 119.7 . . ? C17 C16 H16A 119.7 . . ? C18 C17 C16 118.0(4) . . ? C18 C17 H17A 121.0 . . ? C16 C17 H17A 121.0 . . ? C17 C18 C19 123.0(4) . . ? C17 C18 N3 119.2(4) . . ? C19 C18 N3 117.7(4) . . ? C20 C19 C18 117.6(4) . . ? C20 C19 H19A 121.2 . . ? C18 C19 H19A 121.2 . . ? C19 C20 C15 120.9(4) . . ? C19 C20 H20A 119.5 . . ? C15 C20 H20A 119.5 . . ? O11 N3 O12 123.4(4) . . ? O11 N3 C18 118.9(4) . . ? O12 N3 C18 117.7(4) . . ? C21 O13 Dy1 92.6(2) . . ? C21 O14 Dy1 91.8(2) . . ? O14 C21 O13 122.3(4) . . ? O14 C21 C22 119.1(4) . . ? O13 C21 C22 118.6(4) . . ? C23 C22 C27 119.1(4) . . ? C23 C22 C21 120.1(4) . . ? C27 C22 C21 120.8(4) . . ? C24 C23 C22 121.2(4) . . ? C24 C23 H23A 119.4 . . ? C22 C23 H23A 119.4 . . ? C23 C24 C25 118.0(4) . . ? C23 C24 H24A 121.0 . . ? C25 C24 H24A 121.0 . . ? C24 C25 C26 123.1(4) . . ? C24 C25 N4 119.1(4) . . ? C26 C25 N4 117.8(4) . . ? C27 C26 C25 117.6(4) . . ? C27 C26 H26A 121.2 . . ? C25 C26 H26A 121.2 . . ? C26 C27 C22 121.0(4) . . ? C26 C27 H27A 119.5 . . ? C22 C27 H27A 119.5 . . ? O16 N4 O15 123.5(4) . . ? O16 N4 C25 119.6(5) . . ? O15 N4 C25 116.9(5) . . ? N31 C31 C32 178.3(5) . . ? 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 . . ? N32A C33A C34A 175.6(8) . . ? N33 C35 C36 179.1(7) . . ? 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 . . ? N34 C37 C38 178.7(10) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C41A O41 C41B 45.2(17) . . ? C41A O41 H41 101(5) . . ? C41B O41 H41 89(5) . . ? O41 C41A H41A 109.5 . . ? O41 C41A H41B 109.5 . . ? O41 C41A H41C 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 N31 0.82(3) 2.16(3) 2.972(5) 166(4) . O4 H4 N32A 0.82(3) 2.03(3) 2.793(6) 155(5) . O4 H4 O32B 0.82(3) 1.90(4) 2.62(2) 146(5) . O41 H41 O13 1.03(4) 1.81(4) 2.801(5) 162(7) . _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.710 _refine_diff_density_min -0.942 _refine_diff_density_rms 0.093 ####################################################################### 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