# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_1 _database_code_depnum_ccdc_archive 'CCDC 858952' #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H62 Fe2 N6 O18 Y2' _chemical_formula_weight 1108.40 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' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 17.9932(8) _cell_length_b 11.5546(7) _cell_length_c 21.7382(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4519.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 36229 _cell_measurement_theta_min 1.47 _cell_measurement_theta_max 26.97 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.629 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2280 _exptl_absorpt_coefficient_mu 3.247 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3877 _exptl_absorpt_correction_T_max 0.5925 _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 '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate ( 34 cm diameter )' _diffrn_detector_type STOE _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29723 _diffrn_reflns_av_R_equivalents 0.0688 _diffrn_reflns_av_sigmaI/netI 0.0389 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 26.75 _reflns_number_total 4781 _reflns_number_gt 4108 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0701P)^2^+4.3313P] 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 4781 _refine_ls_number_parameters 274 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0686 _refine_ls_R_factor_gt 0.0539 _refine_ls_wR_factor_ref 0.1279 _refine_ls_wR_factor_gt 0.1193 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.00997(2) 0.59820(3) 0.427837(16) 0.02997(13) Uani 1 1 d . . . Fe1 Fe -0.05200(3) 0.32085(5) 0.42713(3) 0.03417(16) Uani 1 1 d . . . O1 O -0.06452(14) 0.4701(2) 0.48234(12) 0.0298(5) Uani 1 1 d D . . H1 H -0.1100(19) 0.486(4) 0.484(2) 0.045 Uiso 1 1 d D . . O2 O 0.03089(16) 0.4185(2) 0.38878(12) 0.0353(6) Uani 1 1 d . . . O3 O 0.03947(17) 0.6099(2) 0.32058(13) 0.0398(7) Uani 1 1 d . . . O4 O 0.00336(17) 0.7916(2) 0.38687(13) 0.0396(7) Uani 1 1 d . . . O5 O -0.01447(15) 0.7292(2) 0.50304(13) 0.0358(6) Uani 1 1 d . . . O6 O -0.14130(16) 0.2554(3) 0.47553(13) 0.0402(7) Uani 1 1 d . . . O7 O -0.13149(16) 0.3302(2) 0.57003(12) 0.0371(6) Uani 1 1 d . . . O8 O -0.12664(17) 0.4003(2) 0.36933(14) 0.0411(7) Uani 1 1 d . . . O9 O -0.10395(16) 0.5906(2) 0.37597(13) 0.0371(6) Uani 1 1 d . . . N1 N -0.0423(2) 0.1839(3) 0.3741(2) 0.0521(10) Uani 1 1 d . . . N2 N 0.0127(3) 0.1370(4) 0.3572(2) 0.0578(11) Uani 1 1 d . . . N3 N 0.0623(4) 0.0886(5) 0.3388(4) 0.110(3) Uani 1 1 d . . . C1 C 0.0480(3) 0.4077(4) 0.3254(2) 0.0430(10) Uani 1 1 d . . . H1A H 0.0017 0.3953 0.3016 0.052 Uiso 1 1 calc R . . H1B H 0.0807 0.3398 0.3189 0.052 Uiso 1 1 calc R . . C2 C 0.0863(3) 0.5153(4) 0.3031(2) 0.0462(10) Uani 1 1 d . . . H2A H 0.1360 0.5229 0.3223 0.055 Uiso 1 1 calc R . . H2B H 0.0926 0.5130 0.2578 0.055 Uiso 1 1 calc R . . C3 C 0.0586(3) 0.7224(4) 0.2968(2) 0.0462(11) Uani 1 1 d . . . H3A H 0.0577 0.7221 0.2513 0.055 Uiso 1 1 calc R . . H3B H 0.1088 0.7455 0.3107 0.055 Uiso 1 1 calc R . . C4 C 0.0008(3) 0.8045(4) 0.3217(2) 0.0467(11) Uani 1 1 d . . . H4A H 0.0125 0.8852 0.3098 0.056 Uiso 1 1 calc R . . H4B H -0.0491 0.7844 0.3058 0.056 Uiso 1 1 calc R . . C5 C -0.0475(3) 0.8594(4) 0.4222(2) 0.0455(10) Uani 1 1 d . . . H5A H -0.0989 0.8302 0.4171 0.055 Uiso 1 1 calc R . . H5B H -0.0460 0.9414 0.4091 0.055 Uiso 1 1 calc R . . C6 C -0.0231(3) 0.8480(4) 0.4878(2) 0.0420(10) Uani 1 1 d . . . H6A H 0.0246 0.8891 0.4937 0.050 Uiso 1 1 calc R . . H6B H -0.0606 0.8838 0.5152 0.050 Uiso 1 1 calc R . . C7 C -0.1633(2) 0.2683(3) 0.5307(2) 0.0364(9) Uani 1 1 d . . . C8 C -0.2336(2) 0.2023(4) 0.5488(2) 0.0426(10) Uani 1 1 d . . . C9 C -0.2939(3) 0.2269(5) 0.5016(3) 0.0632(14) Uani 1 1 d . . . H9A H -0.3392 0.1846 0.5127 0.095 Uiso 1 1 calc R . . H9B H -0.2770 0.2018 0.4609 0.095 Uiso 1 1 calc R . . H9C H -0.3044 0.3101 0.5008 0.095 Uiso 1 1 calc R . . C10 C -0.2145(4) 0.0725(4) 0.5487(4) 0.0754(18) Uani 1 1 d . . . H10A H -0.1766 0.0569 0.5799 0.113 Uiso 1 1 calc R . . H10B H -0.1955 0.0504 0.5081 0.113 Uiso 1 1 calc R . . H10C H -0.2593 0.0274 0.5579 0.113 Uiso 1 1 calc R . . C11 C -0.2619(3) 0.2391(5) 0.6116(2) 0.0629(15) Uani 1 1 d . . . H11A H -0.2235 0.2244 0.6426 0.094 Uiso 1 1 calc R . . H11B H -0.3067 0.1948 0.6218 0.094 Uiso 1 1 calc R . . H11C H -0.2738 0.3218 0.6109 0.094 Uiso 1 1 calc R . . C12 C -0.1403(2) 0.5051(3) 0.35635(18) 0.0354(9) Uani 1 1 d . . . C13 C -0.2081(2) 0.5255(4) 0.3152(2) 0.0411(10) Uani 1 1 d . . . C14 C -0.2021(3) 0.4467(4) 0.2593(2) 0.0490(11) Uani 1 1 d . . . H14A H -0.1585 0.4685 0.2350 0.074 Uiso 1 1 calc R . . H14B H -0.2469 0.4546 0.2340 0.074 Uiso 1 1 calc R . . H14C H -0.1971 0.3662 0.2729 0.074 Uiso 1 1 calc R . . C15 C -0.2766(3) 0.4911(6) 0.3533(3) 0.0654(15) Uani 1 1 d . . . H15A H -0.2808 0.5422 0.3891 0.098 Uiso 1 1 calc R . . H15B H -0.2714 0.4108 0.3671 0.098 Uiso 1 1 calc R . . H15C H -0.3214 0.4985 0.3279 0.098 Uiso 1 1 calc R . . C16 C -0.2126(4) 0.6508(4) 0.2947(3) 0.0754(19) Uani 1 1 d . . . H16A H -0.1684 0.6702 0.2705 0.113 Uiso 1 1 calc R . . H16B H -0.2152 0.7012 0.3309 0.113 Uiso 1 1 calc R . . H16C H -0.2572 0.6620 0.2694 0.113 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 Y1 0.0327(2) 0.02943(19) 0.0277(2) 0.00148(15) -0.00122(15) -0.00222(14) Fe1 0.0377(3) 0.0355(3) 0.0293(3) 0.0047(2) -0.0051(2) -0.0072(2) O1 0.0304(13) 0.0301(13) 0.0289(13) 0.0004(10) -0.0019(11) -0.0014(11) O2 0.0424(15) 0.0344(14) 0.0292(14) -0.0011(11) 0.0001(12) 0.0033(12) O3 0.0460(16) 0.0396(15) 0.0339(15) 0.0051(12) 0.0029(13) -0.0034(13) O4 0.0466(17) 0.0351(15) 0.0371(15) 0.0057(12) -0.0006(13) 0.0013(13) O5 0.0419(16) 0.0283(13) 0.0372(15) -0.0011(12) 0.0022(12) -0.0006(12) O6 0.0396(16) 0.0433(16) 0.0375(15) -0.0038(13) -0.0004(13) -0.0081(13) O7 0.0375(15) 0.0388(15) 0.0348(14) 0.0019(12) -0.0008(12) -0.0054(12) O8 0.0458(17) 0.0343(14) 0.0434(16) 0.0024(13) -0.0116(13) -0.0032(12) O9 0.0388(15) 0.0342(14) 0.0383(15) 0.0013(12) -0.0050(12) -0.0025(12) N1 0.055(2) 0.044(2) 0.057(3) -0.0001(19) 0.001(2) 0.0013(19) N2 0.070(3) 0.039(2) 0.064(3) 0.002(2) 0.023(2) 0.007(2) N3 0.105(5) 0.063(3) 0.163(7) -0.006(4) 0.059(5) 0.012(3) C1 0.055(3) 0.042(2) 0.032(2) -0.0030(18) 0.0023(19) 0.007(2) C2 0.047(3) 0.056(3) 0.035(2) -0.008(2) 0.0093(19) 0.006(2) C3 0.060(3) 0.047(2) 0.032(2) 0.0058(18) 0.001(2) -0.009(2) C4 0.062(3) 0.039(2) 0.039(2) 0.0095(19) -0.004(2) 0.000(2) C5 0.046(2) 0.034(2) 0.057(3) 0.007(2) 0.004(2) 0.0036(19) C6 0.048(2) 0.030(2) 0.048(2) 0.0009(18) 0.005(2) 0.0030(18) C7 0.033(2) 0.034(2) 0.042(2) 0.0035(18) -0.0043(18) -0.0007(16) C8 0.037(2) 0.042(2) 0.048(2) 0.0069(19) 0.0015(19) -0.0058(18) C9 0.035(2) 0.085(4) 0.070(3) 0.006(3) -0.006(2) -0.010(3) C10 0.066(4) 0.039(3) 0.121(5) 0.017(3) 0.016(4) -0.009(3) C11 0.054(3) 0.081(4) 0.053(3) -0.003(3) 0.013(2) -0.022(3) C12 0.035(2) 0.038(2) 0.033(2) 0.0014(17) -0.0015(16) 0.0003(16) C13 0.040(2) 0.042(2) 0.042(2) -0.0003(19) -0.0120(18) 0.0054(19) C14 0.056(3) 0.053(3) 0.038(2) 0.002(2) -0.008(2) -0.001(2) C15 0.038(3) 0.101(5) 0.057(3) -0.009(3) -0.001(2) 0.004(3) C16 0.097(5) 0.044(3) 0.085(4) 0.001(3) -0.055(4) 0.011(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y1 O5 2.271(3) . ? Y1 O2 2.275(3) . ? Y1 O1 2.322(3) . ? Y1 O1 2.324(3) 5_566 ? Y1 O7 2.338(3) 5_566 ? Y1 O9 2.341(3) . ? Y1 O3 2.395(3) . ? Y1 O4 2.408(3) . ? Y1 Fe1 3.3745(7) 5_566 ? Y1 Fe1 3.3931(7) . ? Fe1 N1 1.965(4) . ? Fe1 O5 2.017(3) 5_566 ? Fe1 O2 2.047(3) . ? Fe1 O8 2.056(3) . ? Fe1 O6 2.064(3) . ? Fe1 O1 2.113(3) . ? Fe1 Y1 3.3744(7) 5_566 ? O1 Y1 2.324(3) 5_566 ? O1 H1 0.84(3) . ? O2 C1 1.418(5) . ? O3 C2 1.432(5) . ? O3 C3 1.440(5) . ? O4 C4 1.425(5) . ? O4 C5 1.430(5) . ? O5 C6 1.421(5) . ? O5 Fe1 2.017(3) 5_566 ? O6 C7 1.271(5) . ? O7 C7 1.253(5) . ? O7 Y1 2.338(3) 5_566 ? O8 C12 1.267(5) . ? O9 C12 1.259(5) . ? N1 N2 1.188(6) . ? N2 N3 1.126(7) . ? C1 C2 1.503(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.507(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.496(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.530(6) . ? C8 C11 1.517(7) . ? C8 C9 1.520(7) . ? C8 C10 1.539(7) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.532(6) . ? C13 C16 1.517(7) . ? C13 C14 1.523(6) . ? C13 C15 1.537(7) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 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 O5 Y1 O2 155.38(10) . . ? O5 Y1 O1 86.88(9) . . ? O2 Y1 O1 72.79(10) . . ? O5 Y1 O1 72.74(10) . 5_566 ? O2 Y1 O1 86.19(9) . 5_566 ? O1 Y1 O1 66.32(11) . 5_566 ? O5 Y1 O7 86.04(10) . 5_566 ? O2 Y1 O7 100.12(10) . 5_566 ? O1 Y1 O7 139.05(9) . 5_566 ? O1 Y1 O7 73.06(9) 5_566 5_566 ? O5 Y1 O9 101.66(10) . . ? O2 Y1 O9 86.04(10) . . ? O1 Y1 O9 73.52(9) . . ? O1 Y1 O9 139.62(9) 5_566 . ? O7 Y1 O9 147.31(10) 5_566 . ? O5 Y1 O3 134.91(10) . . ? O2 Y1 O3 69.62(10) . . ? O1 Y1 O3 131.36(10) . . ? O1 Y1 O3 138.05(10) 5_566 . ? O7 Y1 O3 78.00(10) 5_566 . ? O9 Y1 O3 74.18(10) . . ? O5 Y1 O4 68.80(10) . . ? O2 Y1 O4 135.82(10) . . ? O1 Y1 O4 138.72(10) . . ? O1 Y1 O4 130.31(10) 5_566 . ? O7 Y1 O4 74.05(10) 5_566 . ? O9 Y1 O4 79.25(10) . . ? O3 Y1 O4 66.32(10) . . ? O5 Y1 Fe1 35.51(7) . 5_566 ? O2 Y1 Fe1 124.38(7) . 5_566 ? O1 Y1 Fe1 80.17(6) . 5_566 ? O1 Y1 Fe1 38.22(6) 5_566 5_566 ? O7 Y1 Fe1 70.97(7) 5_566 5_566 ? O9 Y1 Fe1 131.04(7) . 5_566 ? O3 Y1 Fe1 147.59(7) . 5_566 ? O4 Y1 Fe1 95.71(7) . 5_566 ? O5 Y1 Fe1 124.69(7) . . ? O2 Y1 Fe1 35.95(7) . . ? O1 Y1 Fe1 37.87(7) . . ? O1 Y1 Fe1 79.73(6) 5_566 . ? O7 Y1 Fe1 129.91(7) 5_566 . ? O9 Y1 Fe1 71.01(7) . . ? O3 Y1 Fe1 97.00(7) . . ? O4 Y1 Fe1 149.13(7) . . ? Fe1 Y1 Fe1 109.857(15) 5_566 . ? N1 Fe1 O5 99.07(15) . 5_566 ? N1 Fe1 O2 98.05(15) . . ? O5 Fe1 O2 91.85(11) 5_566 . ? N1 Fe1 O8 93.41(15) . . ? O5 Fe1 O8 167.26(12) 5_566 . ? O2 Fe1 O8 88.91(12) . . ? N1 Fe1 O6 94.18(15) . . ? O5 Fe1 O6 88.44(12) 5_566 . ? O2 Fe1 O6 167.56(12) . . ? O8 Fe1 O6 88.10(13) . . ? N1 Fe1 O1 178.41(15) . . ? O5 Fe1 O1 82.52(10) 5_566 . ? O2 Fe1 O1 81.91(11) . . ? O8 Fe1 O1 85.00(11) . . ? O6 Fe1 O1 85.80(11) . . ? N1 Fe1 Y1 138.68(13) . 5_566 ? O5 Fe1 Y1 40.84(8) 5_566 5_566 ? O2 Fe1 Y1 93.69(8) . 5_566 ? O8 Fe1 Y1 126.42(9) . 5_566 ? O6 Fe1 Y1 78.45(8) . 5_566 ? O1 Fe1 Y1 42.87(7) . 5_566 ? N1 Fe1 Y1 137.22(13) . . ? O5 Fe1 Y1 94.15(8) 5_566 . ? O2 Fe1 Y1 40.73(8) . . ? O8 Fe1 Y1 78.21(8) . . ? O6 Fe1 Y1 126.84(9) . . ? O1 Fe1 Y1 42.40(7) . . ? Y1 Fe1 Y1 70.142(15) 5_566 . ? Fe1 O1 Y1 99.72(11) . . ? Fe1 O1 Y1 98.91(10) . 5_566 ? Y1 O1 Y1 113.67(11) . 5_566 ? Fe1 O1 H1 108(3) . . ? Y1 O1 H1 117(3) . . ? Y1 O1 H1 116(3) 5_566 . ? C1 O2 Fe1 120.4(3) . . ? C1 O2 Y1 118.6(2) . . ? Fe1 O2 Y1 103.32(12) . . ? C2 O3 C3 116.9(3) . . ? C2 O3 Y1 110.2(2) . . ? C3 O3 Y1 116.9(2) . . ? C4 O4 C5 117.2(3) . . ? C4 O4 Y1 117.8(3) . . ? C5 O4 Y1 109.9(2) . . ? C6 O5 Fe1 121.2(3) . 5_566 ? C6 O5 Y1 119.8(3) . . ? Fe1 O5 Y1 103.65(12) 5_566 . ? C7 O6 Fe1 132.8(3) . . ? C7 O7 Y1 130.0(3) . 5_566 ? C12 O8 Fe1 133.6(3) . . ? C12 O9 Y1 130.3(3) . . ? N2 N1 Fe1 128.6(4) . . ? N3 N2 N1 175.8(7) . . ? O2 C1 C2 109.9(3) . . ? O2 C1 H1A 109.7 . . ? C2 C1 H1A 109.7 . . ? O2 C1 H1B 109.7 . . ? C2 C1 H1B 109.7 . . ? H1A C1 H1B 108.2 . . ? O3 C2 C1 106.0(3) . . ? O3 C2 H2A 110.5 . . ? C1 C2 H2A 110.5 . . ? O3 C2 H2B 110.5 . . ? C1 C2 H2B 110.5 . . ? H2A C2 H2B 108.7 . . ? O3 C3 C4 105.9(4) . . ? O3 C3 H3A 110.6 . . ? C4 C3 H3A 110.6 . . ? O3 C3 H3B 110.6 . . ? C4 C3 H3B 110.6 . . ? H3A C3 H3B 108.7 . . ? O4 C4 C3 105.6(4) . . ? O4 C4 H4A 110.6 . . ? C3 C4 H4A 110.6 . . ? O4 C4 H4B 110.6 . . ? C3 C4 H4B 110.6 . . ? H4A C4 H4B 108.8 . . ? O4 C5 C6 106.0(3) . . ? O4 C5 H5A 110.5 . . ? C6 C5 H5A 110.5 . . ? O4 C5 H5B 110.5 . . ? C6 C5 H5B 110.5 . . ? H5A C5 H5B 108.7 . . ? O5 C6 C5 109.8(4) . . ? O5 C6 H6A 109.7 . . ? C5 C6 H6A 109.7 . . ? O5 C6 H6B 109.7 . . ? C5 C6 H6B 109.7 . . ? H6A C6 H6B 108.2 . . ? O7 C7 O6 124.7(4) . . ? O7 C7 C8 119.1(4) . . ? O6 C7 C8 116.2(4) . . ? C11 C8 C9 108.4(4) . . ? C11 C8 C7 111.7(4) . . ? C9 C8 C7 108.9(4) . . ? C11 C8 C10 110.5(5) . . ? C9 C8 C10 109.9(5) . . ? C7 C8 C10 107.5(4) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O9 C12 O8 125.0(4) . . ? O9 C12 C13 119.4(4) . . ? O8 C12 C13 115.6(4) . . ? C16 C13 C14 109.9(4) . . ? C16 C13 C12 111.2(4) . . ? C14 C13 C12 108.5(4) . . ? C16 C13 C15 111.3(5) . . ? C14 C13 C15 109.4(4) . . ? C12 C13 C15 106.6(4) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.767 _refine_diff_density_min -0.683 _refine_diff_density_rms 0.072 data_2 _database_code_depnum_ccdc_archive 'CCDC 858953' #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H62 Dy2 Fe2 N6 O18' _chemical_formula_weight 1255.58 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 orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 17.968(4) _cell_length_b 11.556(2) _cell_length_c 21.806(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4527.8(16) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 7025 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 26.15 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.842 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2496 _exptl_absorpt_coefficient_mu 3.966 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5043 _exptl_absorpt_correction_T_max 0.5695 _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 '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate ( 34 cm diameter )' _diffrn_detector_type STOE _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13333 _diffrn_reflns_av_R_equivalents 0.0411 _diffrn_reflns_av_sigmaI/netI 0.0611 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 25.61 _reflns_number_total 4215 _reflns_number_gt 2772 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0005P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4215 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0531 _refine_ls_R_factor_gt 0.0241 _refine_ls_wR_factor_ref 0.0360 _refine_ls_wR_factor_gt 0.0341 _refine_ls_goodness_of_fit_ref 0.861 _refine_ls_restrained_S_all 0.861 _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 Fe1 Fe 1.05371(3) -0.17803(4) 0.57300(3) 0.02238(12) Uani 1 1 d . . . Dy1 Dy 0.990051(8) 0.098636(14) 0.572254(9) 0.02225(5) Uani 1 1 d . . . C1 C 0.9549(2) -0.0922(4) 0.67516(18) 0.0286(9) Uani 1 1 d . . . H1A H 1.0019 -0.1030 0.6980 0.034 Uiso 1 1 calc R . . H1B H 0.9231 -0.1607 0.6825 0.034 Uiso 1 1 calc R . . C2 C 0.9159(2) 0.0147(4) 0.6980(2) 0.0315(11) Uani 1 1 d . . . H2A H 0.8658 0.0214 0.6794 0.038 Uiso 1 1 calc R . . H2B H 0.9104 0.0120 0.7432 0.038 Uiso 1 1 calc R . . C3 C 0.9417(3) 0.2223(4) 0.7037(2) 0.0337(12) Uani 1 1 d . . . H3A H 0.9431 0.2226 0.7491 0.040 Uiso 1 1 calc R . . H3B H 0.8911 0.2440 0.6901 0.040 Uiso 1 1 calc R . . C4 C 0.9987(3) 0.3052(3) 0.67800(17) 0.0365(10) Uani 1 1 d . . . H4A H 0.9870 0.3856 0.6902 0.044 Uiso 1 1 calc R . . H4B H 1.0491 0.2855 0.6931 0.044 Uiso 1 1 calc R . . C5 C 1.0467(2) 0.3613(3) 0.5773(2) 0.0332(11) Uani 1 1 d . . . H5A H 1.0981 0.3320 0.5823 0.040 Uiso 1 1 calc R . . H5B H 1.0452 0.4435 0.5901 0.040 Uiso 1 1 calc R . . C6 C 1.0208(3) 0.3482(3) 0.51093(19) 0.0295(10) Uani 1 1 d . . . H6A H 0.9726 0.3884 0.5054 0.035 Uiso 1 1 calc R . . H6B H 1.0576 0.3842 0.4830 0.035 Uiso 1 1 calc R . . C7 C 1.1421(2) 0.0067(4) 0.64315(19) 0.0291(10) Uani 1 1 d . . . C8 C 1.2094(2) 0.0264(4) 0.6848(2) 0.0336(12) Uani 1 1 d . . . C9 C 1.2785(2) -0.0087(5) 0.6466(3) 0.0533(15) Uani 1 1 d . . . H9A H 1.3236 0.0026 0.6712 0.080 Uiso 1 1 calc R . . H9B H 1.2812 0.0393 0.6096 0.080 Uiso 1 1 calc R . . H9C H 1.2744 -0.0903 0.6348 0.080 Uiso 1 1 calc R . . C10 C 1.2031(2) -0.0527(4) 0.7411(2) 0.0380(12) Uani 1 1 d . . . H10A H 1.2460 -0.0404 0.7679 0.057 Uiso 1 1 calc R . . H10B H 1.2019 -0.1337 0.7277 0.057 Uiso 1 1 calc R . . H10C H 1.1572 -0.0346 0.7634 0.057 Uiso 1 1 calc R . . C11 C 1.2152(3) 0.1520(4) 0.7041(3) 0.067(2) Uani 1 1 d . . . H11A H 1.2588 0.1621 0.7306 0.100 Uiso 1 1 calc R . . H11B H 1.1702 0.1741 0.7267 0.100 Uiso 1 1 calc R . . H11C H 1.2203 0.2009 0.6677 0.100 Uiso 1 1 calc R . . C12 C 0.8353(2) 0.2302(3) 0.5308(2) 0.0259(10) Uani 1 1 d . . . C13 C 0.7649(2) 0.2974(4) 0.5495(2) 0.0287(11) Uani 1 1 d . . . C14 C 0.7376(3) 0.2618(5) 0.6121(3) 0.0574(16) Uani 1 1 d . . . H14A H 0.6925 0.3055 0.6223 0.086 Uiso 1 1 calc R . . H14B H 0.7762 0.2778 0.6426 0.086 Uiso 1 1 calc R . . H14C H 0.7262 0.1788 0.6120 0.086 Uiso 1 1 calc R . . C15 C 0.7848(3) 0.4265(4) 0.5479(3) 0.0586(17) Uani 1 1 d . . . H15A H 0.8022 0.4473 0.5068 0.088 Uiso 1 1 calc R . . H15B H 0.8244 0.4421 0.5778 0.088 Uiso 1 1 calc R . . H15C H 0.7408 0.4725 0.5582 0.088 Uiso 1 1 calc R . . C16 C 0.7050(3) 0.2743(5) 0.5009(3) 0.0514(14) Uani 1 1 d . . . H16A H 0.7238 0.2966 0.4604 0.077 Uiso 1 1 calc R . . H16B H 0.6604 0.3197 0.5105 0.077 Uiso 1 1 calc R . . H16C H 0.6924 0.1917 0.5008 0.077 Uiso 1 1 calc R . . N1 N 1.0444(2) -0.3157(3) 0.62607(17) 0.0342(9) Uani 1 1 d . . . N2 N 0.9883(3) -0.3622(3) 0.64321(19) 0.0425(10) Uani 1 1 d . . . N3 N 0.9369(3) -0.4101(5) 0.6606(3) 0.0818(18) Uani 1 1 d . . . O1 O 1.06540(14) -0.0291(2) 0.51756(12) 0.0221(6) Uani 1 1 d . . . H1 H 1.1179 -0.0023 0.5123 0.033 Uiso 1 1 calc R . . O2 O 0.97035(13) -0.0827(2) 0.61180(11) 0.0251(7) Uani 1 1 d . . . O3 O 0.96172(13) 0.1102(3) 0.68025(11) 0.0293(6) Uani 1 1 d . . . O4 O 0.99473(17) 0.2927(2) 0.61302(11) 0.0289(6) Uani 1 1 d . . . O5 O 1.01270(16) 0.23006(19) 0.49623(12) 0.0256(6) Uani 1 1 d . . . O6 O 1.10484(13) 0.0912(2) 0.62405(12) 0.0265(6) Uani 1 1 d . . . O7 O 1.12843(13) -0.0994(3) 0.63023(12) 0.0314(6) Uani 1 1 d . . . O8 O 0.85659(16) 0.2427(2) 0.47547(14) 0.0290(7) Uani 1 1 d . . . O9 O 0.86728(13) 0.1692(2) 0.57024(16) 0.0291(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0244(3) 0.0229(3) 0.0199(3) -0.0029(3) -0.0030(4) 0.0049(2) Dy1 0.02404(8) 0.02159(7) 0.02112(8) -0.00055(11) -0.00110(10) 0.00237(9) C1 0.035(2) 0.029(2) 0.022(2) 0.003(2) 0.0039(18) -0.001(2) C2 0.032(3) 0.037(3) 0.026(3) 0.001(2) 0.005(2) 0.002(2) C3 0.043(3) 0.034(3) 0.024(3) -0.004(2) 0.004(2) 0.008(2) C4 0.052(3) 0.032(2) 0.026(2) -0.0065(17) -0.001(3) 0.002(3) C5 0.031(2) 0.0229(19) 0.046(3) -0.009(2) 0.005(3) -0.0105(16) C6 0.036(3) 0.023(2) 0.030(2) -0.0003(18) 0.003(2) -0.0050(19) C7 0.027(2) 0.033(2) 0.028(3) -0.006(2) 0.0009(19) -0.0035(19) C8 0.032(3) 0.033(2) 0.036(3) 0.004(2) -0.013(2) -0.003(2) C9 0.027(3) 0.082(4) 0.051(4) 0.012(3) -0.006(2) -0.010(3) C10 0.040(3) 0.042(3) 0.032(3) 0.000(2) -0.006(2) -0.002(2) C11 0.076(4) 0.039(3) 0.085(5) -0.004(3) -0.054(4) -0.008(3) C12 0.024(2) 0.022(2) 0.032(3) -0.008(2) 0.000(2) -0.0018(18) C13 0.024(2) 0.027(2) 0.035(3) -0.0040(19) 0.0001(19) 0.0026(18) C14 0.044(3) 0.077(4) 0.051(4) -0.001(3) 0.013(3) 0.025(3) C15 0.049(3) 0.032(3) 0.095(5) -0.015(3) 0.007(3) 0.007(2) C16 0.031(3) 0.067(4) 0.056(4) 0.007(3) -0.004(3) 0.012(3) N1 0.037(2) 0.031(2) 0.035(2) 0.0077(19) -0.0066(19) -0.0001(18) N2 0.056(3) 0.0263(19) 0.045(3) 0.0009(16) 0.004(3) 0.004(2) N3 0.073(3) 0.053(3) 0.119(5) 0.020(4) 0.035(3) -0.004(3) O1 0.0172(14) 0.0266(16) 0.0226(18) -0.0007(12) 0.0013(12) 0.0001(12) O2 0.0309(16) 0.0270(16) 0.0175(14) -0.0005(12) 0.0026(11) 0.0014(13) O3 0.0353(15) 0.0279(16) 0.0248(15) -0.0025(14) 0.0022(12) -0.0002(14) O4 0.0383(18) 0.0266(13) 0.0218(14) -0.0014(11) -0.0002(15) -0.0028(15) O5 0.0264(15) 0.0214(12) 0.0292(15) -0.0003(11) -0.0019(15) -0.0003(13) O6 0.0240(14) 0.0236(14) 0.0317(16) -0.0036(15) -0.0038(12) 0.0016(15) O7 0.0336(15) 0.0237(14) 0.0368(17) -0.0020(16) -0.0071(13) 0.0001(15) O8 0.0282(16) 0.0286(16) 0.0302(19) -0.0006(13) -0.0023(14) 0.0063(13) O9 0.0292(14) 0.0284(14) 0.0298(15) 0.0006(17) 0.0032(17) 0.0036(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1 1.974(4) . ? Fe1 O5 2.016(3) 5_756 ? Fe1 O2 2.043(3) . ? Fe1 O7 2.046(3) . ? Fe1 O8 2.067(3) 5_756 ? Fe1 O1 2.114(3) . ? Fe1 Dy1 3.3900(9) 5_756 ? Fe1 Dy1 3.3956(8) . ? Dy1 O5 2.285(3) . ? Dy1 O2 2.294(3) . ? Dy1 O1 2.331(3) . ? Dy1 O1 2.340(3) 5_756 ? Dy1 O9 2.352(2) . ? Dy1 O6 2.353(2) . ? Dy1 O3 2.413(3) . ? Dy1 O4 2.414(2) . ? Dy1 Fe1 3.3901(9) 5_756 ? C1 O2 1.414(4) . ? C1 C2 1.504(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 O3 1.431(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 O3 1.438(5) . ? C3 C4 1.509(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O4 1.426(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 O4 1.452(5) . ? C5 C6 1.528(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 O5 1.410(4) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 O6 1.254(5) . ? C7 O7 1.282(5) . ? C7 C8 1.530(6) . ? C8 C11 1.515(6) . ? C8 C10 1.534(6) . ? C8 C9 1.549(6) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 O9 1.251(5) . ? C12 O8 1.274(5) . ? C12 C13 1.540(6) . ? C13 C14 1.508(7) . ? C13 C16 1.534(6) . ? C13 C15 1.534(6) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? N1 N2 1.202(5) . ? N2 N3 1.142(6) . ? O1 Dy1 2.340(3) 5_756 ? O1 H1 1.0000 . ? O5 Fe1 2.016(3) 5_756 ? O8 Fe1 2.067(3) 5_756 ? 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 N1 Fe1 O5 98.55(13) . 5_756 ? N1 Fe1 O2 97.44(14) . . ? O5 Fe1 O2 92.12(11) 5_756 . ? N1 Fe1 O7 93.19(14) . . ? O5 Fe1 O7 167.86(11) 5_756 . ? O2 Fe1 O7 89.37(11) . . ? N1 Fe1 O8 94.27(14) . 5_756 ? O5 Fe1 O8 88.32(11) 5_756 5_756 ? O2 Fe1 O8 168.08(11) . 5_756 ? O7 Fe1 O8 87.75(11) . 5_756 ? N1 Fe1 O1 178.72(14) . . ? O5 Fe1 O1 82.73(10) 5_756 . ? O2 Fe1 O1 82.57(10) . . ? O7 Fe1 O1 85.53(11) . . ? O8 Fe1 O1 85.67(11) 5_756 . ? N1 Fe1 Dy1 138.26(11) . 5_756 ? O5 Fe1 Dy1 40.87(7) 5_756 5_756 ? O2 Fe1 Dy1 94.08(7) . 5_756 ? O7 Fe1 Dy1 127.01(8) . 5_756 ? O8 Fe1 Dy1 78.52(8) 5_756 5_756 ? O1 Fe1 Dy1 42.98(7) . 5_756 ? N1 Fe1 Dy1 137.13(12) . . ? O5 Fe1 Dy1 94.47(7) 5_756 . ? O2 Fe1 Dy1 41.18(7) . . ? O7 Fe1 Dy1 78.81(8) . . ? O8 Fe1 Dy1 126.91(8) 5_756 . ? O1 Fe1 Dy1 42.61(7) . . ? Dy1 Fe1 Dy1 70.281(14) 5_756 . ? O5 Dy1 O2 155.18(9) . . ? O5 Dy1 O1 86.91(9) . . ? O2 Dy1 O1 72.75(9) . . ? O5 Dy1 O1 72.35(9) . 5_756 ? O2 Dy1 O1 86.28(9) . 5_756 ? O1 Dy1 O1 66.52(10) . 5_756 ? O5 Dy1 O9 85.58(10) . . ? O2 Dy1 O9 100.32(9) . . ? O1 Dy1 O9 139.00(10) . . ? O1 Dy1 O9 72.80(10) 5_756 . ? O5 Dy1 O6 102.50(10) . . ? O2 Dy1 O6 85.49(9) . . ? O1 Dy1 O6 73.34(9) . . ? O1 Dy1 O6 139.68(9) 5_756 . ? O9 Dy1 O6 147.52(10) . . ? O5 Dy1 O3 135.15(9) . . ? O2 Dy1 O3 69.57(9) . . ? O1 Dy1 O3 131.06(9) . . ? O1 Dy1 O3 138.25(9) 5_756 . ? O9 Dy1 O3 78.53(10) . . ? O6 Dy1 O3 73.65(9) . . ? O5 Dy1 O4 69.11(9) . . ? O2 Dy1 O4 135.71(8) . . ? O1 Dy1 O4 139.15(9) . . ? O1 Dy1 O4 129.96(9) 5_756 . ? O9 Dy1 O4 73.58(10) . . ? O6 Dy1 O4 80.02(10) . . ? O3 Dy1 O4 66.21(9) . . ? O5 Dy1 Fe1 35.26(7) . 5_756 ? O2 Dy1 Fe1 124.25(6) . 5_756 ? O1 Dy1 Fe1 80.10(6) . 5_756 ? O1 Dy1 Fe1 38.01(6) 5_756 5_756 ? O9 Dy1 Fe1 70.80(8) . 5_756 ? O6 Dy1 Fe1 131.43(7) . 5_756 ? O3 Dy1 Fe1 147.99(6) . 5_756 ? O4 Dy1 Fe1 95.78(6) . 5_756 ? O5 Dy1 Fe1 124.70(6) . . ? O2 Dy1 Fe1 35.89(6) . . ? O1 Dy1 Fe1 37.88(6) . . ? O1 Dy1 Fe1 79.86(6) 5_756 . ? O9 Dy1 Fe1 129.98(6) . . ? O6 Dy1 Fe1 70.61(7) . . ? O3 Dy1 Fe1 96.80(7) . . ? O4 Dy1 Fe1 149.46(7) . . ? Fe1 Dy1 Fe1 109.719(14) 5_756 . ? O2 C1 C2 110.6(4) . . ? O2 C1 H1A 109.5 . . ? C2 C1 H1A 109.5 . . ? O2 C1 H1B 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 108.1 . . ? O3 C2 C1 106.0(3) . . ? O3 C2 H2A 110.5 . . ? C1 C2 H2A 110.5 . . ? O3 C2 H2B 110.5 . . ? C1 C2 H2B 110.5 . . ? H2A C2 H2B 108.7 . . ? O3 C3 C4 105.7(3) . . ? O3 C3 H3A 110.6 . . ? C4 C3 H3A 110.6 . . ? O3 C3 H3B 110.6 . . ? C4 C3 H3B 110.6 . . ? H3A C3 H3B 108.7 . . ? O4 C4 C3 105.7(4) . . ? O4 C4 H4A 110.6 . . ? C3 C4 H4A 110.6 . . ? O4 C4 H4B 110.6 . . ? C3 C4 H4B 110.6 . . ? H4A C4 H4B 108.7 . . ? O4 C5 C6 104.9(3) . . ? O4 C5 H5A 110.8 . . ? C6 C5 H5A 110.8 . . ? O4 C5 H5B 110.8 . . ? C6 C5 H5B 110.8 . . ? H5A C5 H5B 108.8 . . ? O5 C6 C5 110.1(3) . . ? O5 C6 H6A 109.7 . . ? C5 C6 H6A 109.7 . . ? O5 C6 H6B 109.7 . . ? C5 C6 H6B 109.7 . . ? H6A C6 H6B 108.2 . . ? O6 C7 O7 124.7(4) . . ? O6 C7 C8 120.2(4) . . ? O7 C7 C8 115.1(4) . . ? C11 C8 C7 111.2(4) . . ? C11 C8 C10 110.7(4) . . ? C7 C8 C10 109.1(4) . . ? C11 C8 C9 110.2(5) . . ? C7 C8 C9 106.0(4) . . ? C10 C8 C9 109.5(4) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O9 C12 O8 125.3(4) . . ? O9 C12 C13 118.6(4) . . ? O8 C12 C13 116.1(4) . . ? C14 C13 C16 110.4(4) . . ? C14 C13 C15 111.2(4) . . ? C16 C13 C15 108.6(4) . . ? C14 C13 C12 111.7(4) . . ? C16 C13 C12 107.8(4) . . ? C15 C13 C12 107.0(4) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N2 N1 Fe1 127.9(3) . . ? N3 N2 N1 177.0(5) . . ? Fe1 O1 Dy1 99.51(10) . . ? Fe1 O1 Dy1 99.01(10) . 5_756 ? Dy1 O1 Dy1 113.48(10) . 5_756 ? Fe1 O1 H1 114.3 . . ? Dy1 O1 H1 114.3 . . ? Dy1 O1 H1 114.3 5_756 . ? C1 O2 Fe1 120.5(2) . . ? C1 O2 Dy1 117.9(3) . . ? Fe1 O2 Dy1 102.93(10) . . ? C2 O3 C3 117.1(3) . . ? C2 O3 Dy1 110.1(2) . . ? C3 O3 Dy1 116.7(2) . . ? C4 O4 C5 116.5(3) . . ? C4 O4 Dy1 117.5(2) . . ? C5 O4 Dy1 109.4(2) . . ? C6 O5 Fe1 121.3(2) . 5_756 ? C6 O5 Dy1 119.8(2) . . ? Fe1 O5 Dy1 103.87(11) 5_756 . ? C7 O6 Dy1 130.9(3) . . ? C7 O7 Fe1 133.2(3) . . ? C12 O8 Fe1 132.6(3) . 5_756 ? C12 O9 Dy1 129.7(3) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.689 _refine_diff_density_min -0.593 _refine_diff_density_rms 0.083 data_5 _database_code_depnum_ccdc_archive 'CCDC 858954' #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H66 Dy2 Fe2 N2 O24' _chemical_formula_weight 1323.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' 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 P2/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 12.6964(3) _cell_length_b 8.7711(2) _cell_length_c 22.3611(6) _cell_angle_alpha 90.00 _cell_angle_beta 96.513(2) _cell_angle_gamma 90.00 _cell_volume 2474.09(10) _cell_formula_units_Z 2 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 22787 _cell_measurement_theta_min 1.76 _cell_measurement_theta_max 27.24 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.777 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 3.640 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7594 _exptl_absorpt_correction_T_max 0.9308 _exptl_absorpt_process_details 'XPREP in SHELXTL 6.14 (BrukerAXS Inc., 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(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 '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate ( 34 cm diameter )' _diffrn_detector_type STOE _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17615 _diffrn_reflns_av_R_equivalents 0.0340 _diffrn_reflns_av_sigmaI/netI 0.0382 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 26.74 _reflns_number_total 5230 _reflns_number_gt 4229 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0182P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5230 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0407 _refine_ls_R_factor_gt 0.0250 _refine_ls_wR_factor_ref 0.0436 _refine_ls_wR_factor_gt 0.0414 _refine_ls_goodness_of_fit_ref 0.989 _refine_ls_restrained_S_all 0.989 _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 0.289013(11) 0.439893(17) 0.544987(7) 0.01901(4) Uani 1 1 d . . . Fe1 Fe 0.44700(3) 0.47737(5) 0.43169(2) 0.02022(10) Uani 1 1 d . . . O1 O 0.41865(16) 0.6216(2) 0.57931(10) 0.0217(5) Uani 1 1 d . . . O2 O 0.22306(17) 0.6380(3) 0.61006(11) 0.0287(5) Uani 1 1 d . . . O3 O 0.13212(17) 0.5863(3) 0.49716(10) 0.0290(5) Uani 1 1 d . . . O4 O 0.32508(15) 0.5776(3) 0.45945(9) 0.0226(4) Uani 1 1 d . . . O5 O 0.54672(16) 0.6305(2) 0.48366(10) 0.0198(4) Uani 1 1 d . . . O6 O 0.35783(17) 0.3107(3) 0.39309(10) 0.0284(5) Uani 1 1 d . . . O7 O 0.23614(17) 0.2908(3) 0.45776(11) 0.0274(5) Uani 1 1 d . . . O8 O 0.45082(17) 0.6007(3) 0.35705(10) 0.0287(5) Uani 1 1 d . . . O9 O 0.62512(18) 0.6444(3) 0.36224(10) 0.0281(5) Uani 1 1 d . . . C1 C 0.4013(3) 0.7179(4) 0.62764(18) 0.0327(8) Uani 1 1 d . . . H1A H 0.4494 0.8055 0.6288 0.039 Uiso 1 1 calc R . . H1B H 0.4155 0.6624 0.6657 0.039 Uiso 1 1 calc R . . C2 C 0.2893(3) 0.7714(4) 0.6196(2) 0.0382(9) Uani 1 1 d . . . H2A H 0.2728 0.8266 0.6555 0.046 Uiso 1 1 calc R . . H2B H 0.2775 0.8399 0.5849 0.046 Uiso 1 1 calc R . . C3 C 0.1130(3) 0.6736(5) 0.59482(17) 0.0372(9) Uani 1 1 d . . . H3A H 0.0945 0.7621 0.6183 0.045 Uiso 1 1 calc R . . H3B H 0.0698 0.5872 0.6054 0.045 Uiso 1 1 calc R . . C4 C 0.0886(3) 0.7076(5) 0.52940(18) 0.0404(9) Uani 1 1 d . . . H4A H 0.0117 0.7138 0.5185 0.048 Uiso 1 1 calc R . . H4B H 0.1202 0.8052 0.5197 0.048 Uiso 1 1 calc R . . C5 C 0.1404(3) 0.6227(5) 0.43461(17) 0.0361(9) Uani 1 1 d . . . H5A H 0.0893 0.7025 0.4209 0.043 Uiso 1 1 calc R . . H5B H 0.1246 0.5321 0.4095 0.043 Uiso 1 1 calc R . . C6 C 0.2509(3) 0.6767(5) 0.42891(17) 0.0351(9) Uani 1 1 d . . . H6A H 0.2621 0.6813 0.3863 0.042 Uiso 1 1 calc R . . H6B H 0.2605 0.7796 0.4458 0.042 Uiso 1 1 calc R . . C7 C 0.5174(3) 0.7899(4) 0.48045(16) 0.0277(7) Uani 1 1 d . . . H7A H 0.5689 0.8489 0.5061 0.042 Uiso 1 1 calc R . . H7B H 0.4478 0.8025 0.4938 0.042 Uiso 1 1 calc R . . H7C H 0.5156 0.8252 0.4392 0.042 Uiso 1 1 calc R . . C8 C 0.2714(2) 0.2582(4) 0.40974(15) 0.0229(7) Uani 1 1 d . . . C9 C 0.2094(3) 0.1504(4) 0.36572(16) 0.0273(7) Uani 1 1 d . . . C10 C 0.2860(3) 0.0431(4) 0.33854(18) 0.0386(9) Uani 1 1 d . . . H10A H 0.3356 0.1024 0.3181 0.058 Uiso 1 1 calc R . . H10B H 0.2464 -0.0245 0.3099 0.058 Uiso 1 1 calc R . . H10C H 0.3246 -0.0167 0.3703 0.058 Uiso 1 1 calc R . . C11 C 0.1495(3) 0.2488(5) 0.31638(18) 0.0474(11) Uani 1 1 d . . . H11A H 0.1999 0.3065 0.2959 0.071 Uiso 1 1 calc R . . H11B H 0.1028 0.3185 0.3344 0.071 Uiso 1 1 calc R . . H11C H 0.1079 0.1837 0.2877 0.071 Uiso 1 1 calc R . . C12 C 0.1298(3) 0.0589(5) 0.39764(18) 0.0403(8) Uani 1 1 d . . . H12A H 0.1676 -0.0040 0.4287 0.061 Uiso 1 1 calc R . . H12B H 0.0882 -0.0055 0.3687 0.061 Uiso 1 1 calc R . . H12C H 0.0832 0.1284 0.4158 0.061 Uiso 1 1 calc R . . C13 C 0.5339(3) 0.6459(4) 0.33492(14) 0.0239(7) Uani 1 1 d . . . C14 C 0.5206(3) 0.7057(4) 0.27017(15) 0.0307(8) Uani 1 1 d . . . C15 C 0.5659(5) 0.8661(6) 0.2704(2) 0.0696(16) Uani 1 1 d . . . H15A H 0.5263 0.9319 0.2947 0.104 Uiso 1 1 calc R . . H15B H 0.5605 0.9046 0.2295 0.104 Uiso 1 1 calc R . . H15C H 0.6398 0.8640 0.2873 0.104 Uiso 1 1 calc R . . C16 C 0.5815(4) 0.6001(6) 0.23272(19) 0.0583(13) Uani 1 1 d . . . H16A H 0.6556 0.5983 0.2491 0.087 Uiso 1 1 calc R . . H16B H 0.5755 0.6364 0.1915 0.087 Uiso 1 1 calc R . . H16C H 0.5524 0.4979 0.2336 0.087 Uiso 1 1 calc R . . C17 C 0.4045(3) 0.7082(6) 0.24372(18) 0.0468(10) Uani 1 1 d . . . H17A H 0.3651 0.7762 0.2672 0.070 Uiso 1 1 calc R . . H17B H 0.3753 0.6061 0.2447 0.070 Uiso 1 1 calc R . . H17C H 0.3992 0.7439 0.2024 0.070 Uiso 1 1 calc R . . N1 N 0.1652(2) 0.1800(3) 0.58153(14) 0.0317(7) Uani 1 1 d . . . O10 O 0.25535(19) 0.1514(3) 0.56733(12) 0.0349(6) Uani 1 1 d . . . O11 O 0.13667(19) 0.3202(3) 0.57946(12) 0.0316(6) Uani 1 1 d . . . O12 O 0.1054(3) 0.0824(4) 0.59673(18) 0.0679(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.01500(6) 0.02231(7) 0.01998(7) 0.00127(8) 0.00308(4) -0.00058(7) Fe1 0.0161(2) 0.0240(2) 0.0206(2) 0.00093(17) 0.00274(16) -0.00173(16) O1 0.0196(11) 0.0231(11) 0.0229(11) -0.0016(9) 0.0041(9) -0.0021(8) O2 0.0195(11) 0.0298(12) 0.0368(14) -0.0044(11) 0.0032(10) 0.0041(9) O3 0.0232(11) 0.0348(14) 0.0297(12) 0.0049(10) 0.0056(9) 0.0084(10) O4 0.0171(10) 0.0263(12) 0.0240(11) 0.0057(10) 0.0010(8) 0.0022(9) O5 0.0167(10) 0.0185(10) 0.0245(11) 0.0020(9) 0.0045(9) 0.0008(8) O6 0.0216(11) 0.0347(13) 0.0298(13) -0.0063(10) 0.0061(10) -0.0073(10) O7 0.0258(13) 0.0340(13) 0.0234(12) -0.0051(11) 0.0065(10) -0.0063(9) O8 0.0219(11) 0.0398(14) 0.0245(12) 0.0059(10) 0.0032(9) -0.0007(9) O9 0.0214(12) 0.0373(13) 0.0248(12) 0.0080(11) -0.0005(9) -0.0044(10) C1 0.0273(18) 0.0313(19) 0.040(2) -0.0162(16) 0.0068(15) -0.0010(14) C2 0.0318(19) 0.0305(19) 0.054(2) -0.0131(18) 0.0102(17) 0.0001(15) C3 0.0253(18) 0.049(2) 0.039(2) -0.0049(18) 0.0062(16) 0.0104(16) C4 0.032(2) 0.046(2) 0.043(2) -0.0026(18) 0.0034(17) 0.0154(17) C5 0.0216(17) 0.053(2) 0.033(2) 0.0104(17) 0.0015(15) 0.0083(16) C6 0.0242(17) 0.045(2) 0.036(2) 0.0180(18) 0.0048(15) 0.0114(16) C7 0.0275(17) 0.0221(16) 0.0335(19) 0.0019(14) 0.0039(14) 0.0007(13) C8 0.0209(15) 0.0218(16) 0.0259(17) 0.0014(13) 0.0020(13) -0.0016(12) C9 0.0239(16) 0.0274(18) 0.0314(18) -0.0087(15) 0.0060(14) -0.0043(13) C10 0.0371(19) 0.035(2) 0.046(2) -0.0137(18) 0.0139(16) -0.0061(17) C11 0.044(2) 0.060(3) 0.036(2) -0.012(2) -0.0073(18) 0.005(2) C12 0.0305(17) 0.0358(19) 0.057(2) -0.015(2) 0.0144(16) -0.0105(18) C13 0.0263(17) 0.0229(17) 0.0228(16) 0.0001(13) 0.0043(13) -0.0008(13) C14 0.0273(17) 0.042(2) 0.0223(17) 0.0072(15) 0.0021(14) 0.0009(15) C15 0.094(4) 0.060(3) 0.050(3) 0.029(2) -0.010(3) -0.029(3) C16 0.054(3) 0.091(4) 0.031(2) 0.000(2) 0.0129(19) 0.019(2) C17 0.038(2) 0.071(3) 0.030(2) 0.008(2) -0.0006(17) 0.006(2) N1 0.0272(15) 0.0316(16) 0.0368(17) 0.0055(13) 0.0054(13) -0.0050(12) O10 0.0291(13) 0.0373(14) 0.0384(15) 0.0020(12) 0.0043(11) 0.0018(11) O11 0.0260(12) 0.0302(14) 0.0404(15) 0.0042(11) 0.0111(11) -0.0026(10) O12 0.0525(18) 0.0410(18) 0.116(3) 0.0192(19) 0.0332(18) -0.0177(15) _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 O5 2.333(2) 3_666 ? Dy1 O9 2.351(2) 3_666 ? Dy1 O4 2.351(2) . ? Dy1 O1 2.356(2) . ? Dy1 O7 2.381(2) . ? Dy1 O11 2.403(2) . ? Dy1 O2 2.473(2) . ? Dy1 O3 2.505(2) . ? Dy1 O10 2.624(3) . ? Dy1 N1 2.937(3) . ? Dy1 Fe1 3.4111(4) 3_666 ? Dy1 Fe1 3.4210(5) . ? Fe1 O4 1.942(2) . ? Fe1 O1 1.954(2) 3_666 ? Fe1 O6 1.986(2) . ? Fe1 O8 1.994(2) . ? Fe1 O5 2.103(2) . ? Fe1 O5 2.110(2) 3_666 ? Fe1 Dy1 3.4111(4) 3_666 ? O1 C1 1.408(4) . ? O1 Fe1 1.954(2) 3_666 ? O2 C3 1.434(4) . ? O2 C2 1.442(4) . ? O3 C4 1.431(4) . ? O3 C5 1.450(4) . ? O4 C6 1.401(4) . ? O5 C7 1.447(4) . ? O5 Fe1 2.110(2) 3_666 ? O5 Dy1 2.333(2) 3_666 ? O6 C8 1.284(4) . ? O7 C8 1.242(4) . ? O8 C13 1.278(4) . ? O9 C13 1.246(4) . ? O9 Dy1 2.351(2) 3_666 ? C1 C2 1.490(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C3 C4 1.491(5) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C5 C6 1.499(5) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 H7C 0.9700 . ? C8 C9 1.519(4) . ? C9 C10 1.527(5) . ? C9 C12 1.529(5) . ? C9 C11 1.533(5) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 H10C 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 H11C 0.9700 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 H12C 0.9700 . ? C13 C14 1.531(5) . ? C14 C16 1.518(6) . ? C14 C15 1.519(6) . ? C14 C17 1.525(5) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? N1 O12 1.219(4) . ? N1 O10 1.247(4) . ? N1 O11 1.281(4) . ? 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 O5 Dy1 O9 79.60(8) 3_666 3_666 ? O5 Dy1 O4 69.50(7) 3_666 . ? O9 Dy1 O4 140.00(7) 3_666 . ? O5 Dy1 O1 69.84(7) 3_666 . ? O9 Dy1 O1 71.85(8) 3_666 . ? O4 Dy1 O1 73.98(7) . . ? O5 Dy1 O7 78.90(7) 3_666 . ? O9 Dy1 O7 127.57(8) 3_666 . ? O4 Dy1 O7 71.24(8) . . ? O1 Dy1 O7 139.46(7) . . ? O5 Dy1 O11 138.53(8) 3_666 . ? O9 Dy1 O11 83.63(8) 3_666 . ? O4 Dy1 O11 136.35(8) . . ? O1 Dy1 O11 138.50(8) . . ? O7 Dy1 O11 81.98(8) . . ? O5 Dy1 O2 136.09(7) 3_666 . ? O9 Dy1 O2 81.71(8) 3_666 . ? O4 Dy1 O2 103.18(8) . . ? O1 Dy1 O2 66.65(7) . . ? O7 Dy1 O2 141.74(7) . . ? O11 Dy1 O2 77.28(8) . . ? O5 Dy1 O3 135.28(7) 3_666 . ? O9 Dy1 O3 143.58(8) 3_666 . ? O4 Dy1 O3 66.94(7) . . ? O1 Dy1 O3 106.54(8) . . ? O7 Dy1 O3 78.17(8) . . ? O11 Dy1 O3 74.39(8) . . ? O2 Dy1 O3 65.49(7) . . ? O5 Dy1 O10 88.11(7) 3_666 . ? O9 Dy1 O10 66.28(8) 3_666 . ? O4 Dy1 O10 134.55(8) . . ? O1 Dy1 O10 135.50(7) . . ? O7 Dy1 O10 65.76(8) . . ? O11 Dy1 O10 50.44(8) . . ? O2 Dy1 O10 119.49(8) . . ? O3 Dy1 O10 115.89(8) . . ? O5 Dy1 N1 113.21(8) 3_666 . ? O9 Dy1 N1 73.71(8) 3_666 . ? O4 Dy1 N1 141.72(8) . . ? O1 Dy1 N1 144.14(8) . . ? O7 Dy1 N1 72.04(8) . . ? O11 Dy1 N1 25.32(8) . . ? O2 Dy1 N1 98.86(8) . . ? O3 Dy1 N1 95.27(8) . . ? O10 Dy1 N1 25.12(8) . . ? O5 Dy1 Fe1 37.34(5) 3_666 3_666 ? O9 Dy1 Fe1 65.34(6) 3_666 3_666 ? O4 Dy1 Fe1 74.71(5) . 3_666 ? O1 Dy1 Fe1 33.73(5) . 3_666 ? O7 Dy1 Fe1 115.02(5) . 3_666 ? O11 Dy1 Fe1 148.92(6) . 3_666 ? O2 Dy1 Fe1 98.80(5) . 3_666 ? O3 Dy1 Fe1 132.54(6) . 3_666 ? O10 Dy1 Fe1 110.76(5) . 3_666 ? N1 Dy1 Fe1 132.07(6) . 3_666 ? O5 Dy1 Fe1 37.31(5) 3_666 . ? O9 Dy1 Fe1 115.57(6) 3_666 . ? O4 Dy1 Fe1 33.21(5) . . ? O1 Dy1 Fe1 74.31(5) . . ? O7 Dy1 Fe1 65.20(5) . . ? O11 Dy1 Fe1 147.17(6) . . ? O2 Dy1 Fe1 129.38(6) . . ? O3 Dy1 Fe1 98.00(5) . . ? O10 Dy1 Fe1 110.83(6) . . ? N1 Dy1 Fe1 131.14(6) . . ? Fe1 Dy1 Fe1 56.241(13) 3_666 . ? O4 Fe1 O1 168.51(9) . 3_666 ? O4 Fe1 O6 92.09(9) . . ? O1 Fe1 O6 94.65(9) 3_666 . ? O4 Fe1 O8 96.77(9) . . ? O1 Fe1 O8 91.79(9) 3_666 . ? O6 Fe1 O8 95.89(10) . . ? O4 Fe1 O5 89.19(9) . . ? O1 Fe1 O5 82.75(9) 3_666 . ? O6 Fe1 O5 171.18(9) . . ? O8 Fe1 O5 92.62(9) . . ? O4 Fe1 O5 82.34(8) . 3_666 ? O1 Fe1 O5 88.22(9) 3_666 3_666 ? O6 Fe1 O5 91.22(9) . 3_666 ? O8 Fe1 O5 172.87(9) . 3_666 ? O5 Fe1 O5 80.30(9) . 3_666 ? O4 Fe1 Dy1 131.28(7) . 3_666 ? O1 Fe1 Dy1 42.03(6) 3_666 3_666 ? O6 Fe1 Dy1 136.47(7) . 3_666 ? O8 Fe1 Dy1 84.02(6) . 3_666 ? O5 Fe1 Dy1 42.29(6) . 3_666 ? O5 Fe1 Dy1 91.25(6) 3_666 3_666 ? O4 Fe1 Dy1 41.52(6) . . ? O1 Fe1 Dy1 130.09(7) 3_666 . ? O6 Fe1 Dy1 84.13(7) . . ? O8 Fe1 Dy1 138.07(7) . . ? O5 Fe1 Dy1 91.08(6) . . ? O5 Fe1 Dy1 42.10(6) 3_666 . ? Dy1 Fe1 Dy1 123.757(13) 3_666 . ? C1 O1 Fe1 125.26(19) . 3_666 ? C1 O1 Dy1 119.44(19) . . ? Fe1 O1 Dy1 104.25(9) 3_666 . ? C3 O2 C2 113.2(3) . . ? C3 O2 Dy1 113.5(2) . . ? C2 O2 Dy1 115.24(19) . . ? C4 O3 C5 113.4(3) . . ? C4 O3 Dy1 120.0(2) . . ? C5 O3 Dy1 112.54(18) . . ? C6 O4 Fe1 129.9(2) . . ? C6 O4 Dy1 122.21(19) . . ? Fe1 O4 Dy1 105.27(9) . . ? C7 O5 Fe1 117.01(18) . . ? C7 O5 Fe1 117.48(19) . 3_666 ? Fe1 O5 Fe1 99.70(9) . 3_666 ? C7 O5 Dy1 118.39(18) . 3_666 ? Fe1 O5 Dy1 100.37(9) . 3_666 ? Fe1 O5 Dy1 100.58(8) 3_666 3_666 ? C8 O6 Fe1 127.0(2) . . ? C8 O7 Dy1 137.6(2) . . ? C13 O8 Fe1 126.3(2) . . ? C13 O9 Dy1 138.4(2) . 3_666 ? O1 C1 C2 109.0(3) . . ? O1 C1 H1A 109.9 . . ? C2 C1 H1A 109.9 . . ? O1 C1 H1B 109.9 . . ? C2 C1 H1B 109.9 . . ? H1A C1 H1B 108.3 . . ? O2 C2 C1 107.2(3) . . ? O2 C2 H2A 110.3 . . ? C1 C2 H2A 110.3 . . ? O2 C2 H2B 110.3 . . ? C1 C2 H2B 110.3 . . ? H2A C2 H2B 108.5 . . ? O2 C3 C4 111.5(3) . . ? O2 C3 H3A 109.3 . . ? C4 C3 H3A 109.3 . . ? O2 C3 H3B 109.3 . . ? C4 C3 H3B 109.3 . . ? H3A C3 H3B 108.0 . . ? O3 C4 C3 107.2(3) . . ? O3 C4 H4A 110.3 . . ? C3 C4 H4A 110.3 . . ? O3 C4 H4B 110.3 . . ? C3 C4 H4B 110.3 . . ? H4A C4 H4B 108.5 . . ? O3 C5 C6 108.8(3) . . ? O3 C5 H5A 109.9 . . ? C6 C5 H5A 109.9 . . ? O3 C5 H5B 109.9 . . ? C6 C5 H5B 109.9 . . ? H5A C5 H5B 108.3 . . ? O4 C6 C5 110.2(3) . . ? O4 C6 H6A 109.6 . . ? C5 C6 H6A 109.6 . . ? O4 C6 H6B 109.6 . . ? C5 C6 H6B 109.6 . . ? H6A C6 H6B 108.1 . . ? O5 C7 H7A 109.5 . . ? O5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O7 C8 O6 124.8(3) . . ? O7 C8 C9 119.5(3) . . ? O6 C8 C9 115.6(3) . . ? C8 C9 C10 109.6(3) . . ? C8 C9 C12 110.2(3) . . ? C10 C9 C12 110.3(3) . . ? C8 C9 C11 107.1(3) . . ? C10 C9 C11 110.3(3) . . ? C12 C9 C11 109.3(3) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O9 C13 O8 124.6(3) . . ? O9 C13 C14 117.6(3) . . ? O8 C13 C14 117.7(3) . . ? C16 C14 C15 110.6(4) . . ? C16 C14 C17 109.0(3) . . ? C15 C14 C17 109.7(4) . . ? C16 C14 C13 107.7(3) . . ? C15 C14 C13 108.2(3) . . ? C17 C14 C13 111.7(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 . . ? O12 N1 O10 123.3(3) . . ? O12 N1 O11 120.1(3) . . ? O10 N1 O11 116.6(3) . . ? O12 N1 Dy1 173.4(3) . . ? O10 N1 Dy1 63.26(17) . . ? O11 N1 Dy1 53.37(15) . . ? N1 O10 Dy1 91.62(19) . . ? N1 O11 Dy1 101.30(18) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.578 _refine_diff_density_min -0.944 _refine_diff_density_rms 0.085 data_6 _database_code_depnum_ccdc_archive 'CCDC 858955' #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H66 Fe2 Ho2 N2 O24' _chemical_formula_weight 1328.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 12.6420(8) _cell_length_b 8.7461(5) _cell_length_c 22.2786(16) _cell_angle_alpha 90.00 _cell_angle_beta 96.566(5) _cell_angle_gamma 90.00 _cell_volume 2447.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 24171 _cell_measurement_theta_min 1.77 _cell_measurement_theta_max 27.25 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.803 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1324 _exptl_absorpt_coefficient_mu 3.860 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4577 _exptl_absorpt_correction_T_max 0.6140 _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 '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate ( 34 cm diameter )' _diffrn_detector_type STOE _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17021 _diffrn_reflns_av_R_equivalents 0.0265 _diffrn_reflns_av_sigmaI/netI 0.0223 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 26.75 _reflns_number_total 5178 _reflns_number_gt 4543 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0210P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5178 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0231 _refine_ls_R_factor_gt 0.0171 _refine_ls_wR_factor_ref 0.0361 _refine_ls_wR_factor_gt 0.0351 _refine_ls_goodness_of_fit_ref 0.972 _refine_ls_restrained_S_all 0.972 _refine_ls_shift/su_max 0.004 _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 Ho1 Ho 0.710873(7) 0.559511(10) 0.955308(4) 0.02006(3) Uani 1 1 d . . . Fe1 Fe 0.55321(2) 0.52196(3) 1.068560(13) 0.02140(6) Uani 1 1 d . . . O1 O 0.67461(11) 0.42122(16) 1.04051(6) 0.0232(3) Uani 1 1 d . . . O2 O 0.86833(12) 0.41463(18) 1.00308(7) 0.0284(3) Uani 1 1 d . . . O3 O 0.77701(12) 0.36372(17) 0.88975(7) 0.0282(3) Uani 1 1 d . . . O4 O 0.58144(11) 0.37821(17) 0.92073(6) 0.0235(3) Uani 1 1 d . . . O6 O 0.62569(12) 0.64417(17) 0.86231(7) 0.0282(3) Uani 1 1 d . . . O7 O 0.45064(12) 0.60238(18) 0.85670(7) 0.0277(3) Uani 1 1 d . . . O8 O 0.76510(11) 0.70701(17) 1.04250(6) 0.0271(3) Uani 1 1 d . . . O9 O 0.64328(11) 0.68833(18) 1.10743(7) 0.0285(3) Uani 1 1 d . . . O5 O 0.45258(11) 0.36985(16) 1.01616(6) 0.0212(3) Uani 1 1 d . . . O10 O 0.86200(12) 0.68010(18) 0.92081(7) 0.0301(3) Uani 1 1 d . . . O11 O 0.74266(13) 0.84905(19) 0.93356(7) 0.0333(4) Uani 1 1 d . . . O12 O 0.89233(17) 0.9188(2) 0.90365(12) 0.0612(6) Uani 1 1 d . . . C1 C 0.74926(18) 0.3202(3) 1.07067(11) 0.0331(5) Uani 1 1 d . . . H1A H 0.7400 0.2170 1.0526 0.040 Uiso 1 1 calc R . . H1B H 0.7376 0.3130 1.1138 0.040 Uiso 1 1 calc R . . C2 C 0.86001(19) 0.3767(3) 1.06564(11) 0.0342(5) Uani 1 1 d . . . H2A H 0.8750 0.4682 1.0914 0.041 Uiso 1 1 calc R . . H2B H 0.9125 0.2965 1.0795 0.041 Uiso 1 1 calc R . . C3 C 0.91287(19) 0.2938(3) 0.97050(11) 0.0367(5) Uani 1 1 d . . . H3A H 0.8811 0.1945 0.9799 0.044 Uiso 1 1 calc R . . H3B H 0.9908 0.2882 0.9817 0.044 Uiso 1 1 calc R . . C4 C 0.88804(18) 0.3297(3) 0.90463(11) 0.0338(5) Uani 1 1 d . . . H4A H 0.9311 0.4185 0.8943 0.041 Uiso 1 1 calc R . . H4B H 0.9075 0.2413 0.8804 0.041 Uiso 1 1 calc R . . C5 C 0.71120(19) 0.2290(3) 0.87993(12) 0.0366(5) Uani 1 1 d . . . H5A H 0.7231 0.1594 0.9151 0.044 Uiso 1 1 calc R . . H5B H 0.7282 0.1735 0.8435 0.044 Uiso 1 1 calc R . . C6 C 0.59783(18) 0.2835(3) 0.87169(11) 0.0312(5) Uani 1 1 d . . . H6A H 0.5837 0.3411 0.8334 0.037 Uiso 1 1 calc R . . H6B H 0.5487 0.1950 0.8700 0.037 Uiso 1 1 calc R . . C8 C 0.53439(17) 0.6467(2) 0.83476(9) 0.0247(4) Uani 1 1 d . . . C9 C 0.52099(18) 0.7073(3) 0.76986(9) 0.0293(5) Uani 1 1 d . . . C10 C 0.4048(2) 0.7100(3) 0.74310(11) 0.0428(6) Uani 1 1 d . . . H10A H 0.3645 0.7774 0.7673 0.064 Uiso 1 1 calc R . . H10B H 0.3755 0.6063 0.7433 0.064 Uiso 1 1 calc R . . H10C H 0.3997 0.7480 0.7015 0.064 Uiso 1 1 calc R . . C11 C 0.5829(3) 0.6000(4) 0.73234(12) 0.0544(8) Uani 1 1 d . . . H11A H 0.6579 0.5979 0.7493 0.082 Uiso 1 1 calc R . . H11B H 0.5775 0.6368 0.6905 0.082 Uiso 1 1 calc R . . H11C H 0.5531 0.4967 0.7331 0.082 Uiso 1 1 calc R . . C12 C 0.5671(3) 0.8684(4) 0.77053(14) 0.0628(9) Uani 1 1 d . . . H12A H 0.6418 0.8659 0.7881 0.094 Uiso 1 1 calc R . . H12B H 0.5266 0.9352 0.7948 0.094 Uiso 1 1 calc R . . H12C H 0.5625 0.9077 0.7291 0.094 Uiso 1 1 calc R . . C13 C 0.72953(16) 0.7407(2) 1.09066(10) 0.0245(4) Uani 1 1 d . . . C14 C 0.79202(17) 0.8501(3) 1.13457(10) 0.0279(5) Uani 1 1 d . . . C15 C 0.8714(2) 0.9406(3) 1.10229(13) 0.0391(6) Uani 1 1 d . . . H15A H 0.8330 1.0037 1.0706 0.059 Uiso 1 1 calc R . . H15B H 0.9186 0.8698 1.0840 0.059 Uiso 1 1 calc R . . H15C H 0.9138 1.0065 1.1314 0.059 Uiso 1 1 calc R . . C16 C 0.7152(2) 0.9570(3) 1.16185(12) 0.0372(6) Uani 1 1 d . . . H16A H 0.6779 1.0204 1.1299 0.056 Uiso 1 1 calc R . . H16B H 0.7551 1.0229 1.1920 0.056 Uiso 1 1 calc R . . H16C H 0.6633 0.8966 1.1812 0.056 Uiso 1 1 calc R . . C17 C 0.8522(2) 0.7515(3) 1.18438(11) 0.0424(6) Uani 1 1 d . . . H17A H 0.8932 0.8178 1.2139 0.064 Uiso 1 1 calc R . . H17B H 0.9007 0.6821 1.1664 0.064 Uiso 1 1 calc R . . H17C H 0.8011 0.6917 1.2046 0.064 Uiso 1 1 calc R . . C7 C 0.48193(18) 0.2095(2) 1.01911(11) 0.0302(5) Uani 1 1 d . . . H7A H 0.4294 0.1501 0.9930 0.045 Uiso 1 1 calc R . . H7B H 0.4839 0.1733 1.0609 0.045 Uiso 1 1 calc R . . H7C H 0.5524 0.1967 1.0054 0.045 Uiso 1 1 calc R . . N1 N 0.83292(15) 0.8207(2) 0.91882(9) 0.0317(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ho1 0.01665(5) 0.02347(5) 0.02028(5) 0.00106(4) 0.00308(3) -0.00043(4) Fe1 0.01790(14) 0.02579(15) 0.02066(14) 0.00089(11) 0.00291(11) -0.00181(11) O1 0.0190(7) 0.0271(8) 0.0235(7) 0.0045(6) 0.0023(5) 0.0021(6) O2 0.0253(8) 0.0332(8) 0.0274(8) 0.0040(6) 0.0063(6) 0.0063(6) O3 0.0207(7) 0.0307(8) 0.0334(8) -0.0036(6) 0.0039(6) 0.0023(6) O4 0.0211(7) 0.0251(7) 0.0250(7) -0.0027(6) 0.0054(6) -0.0002(6) O6 0.0237(8) 0.0353(9) 0.0252(7) 0.0058(6) 0.0012(6) -0.0031(7) O7 0.0223(7) 0.0370(8) 0.0236(7) 0.0067(6) 0.0022(6) -0.0001(6) O8 0.0253(8) 0.0318(8) 0.0246(7) -0.0037(6) 0.0048(6) -0.0051(6) O9 0.0229(8) 0.0346(8) 0.0286(8) -0.0061(6) 0.0059(6) -0.0069(7) O5 0.0195(7) 0.0217(7) 0.0229(7) 0.0024(6) 0.0040(5) -0.0007(6) O10 0.0246(8) 0.0306(8) 0.0361(9) 0.0041(7) 0.0075(6) -0.0013(7) O11 0.0284(8) 0.0349(9) 0.0373(9) 0.0007(7) 0.0070(7) 0.0029(7) O12 0.0476(12) 0.0402(11) 0.1002(18) 0.0133(11) 0.0271(12) -0.0140(9) C1 0.0255(11) 0.0402(13) 0.0338(12) 0.0139(10) 0.0042(9) 0.0085(10) C2 0.0261(12) 0.0467(14) 0.0292(12) 0.0078(10) 0.0011(9) 0.0060(10) C3 0.0283(12) 0.0412(14) 0.0408(14) -0.0015(11) 0.0054(10) 0.0112(10) C4 0.0225(11) 0.0420(13) 0.0374(13) -0.0030(10) 0.0062(9) 0.0065(10) C5 0.0306(12) 0.0308(12) 0.0490(15) -0.0112(11) 0.0070(10) 0.0007(10) C6 0.0263(11) 0.0335(12) 0.0345(12) -0.0107(10) 0.0061(9) -0.0019(9) C8 0.0258(11) 0.0244(11) 0.0242(10) 0.0022(8) 0.0038(8) 0.0002(8) C9 0.0291(11) 0.0371(13) 0.0213(10) 0.0053(9) 0.0017(8) -0.0002(9) C10 0.0345(13) 0.0641(18) 0.0284(12) 0.0094(12) -0.0029(10) 0.0063(13) C11 0.0518(17) 0.085(2) 0.0283(13) 0.0017(14) 0.0111(12) 0.0224(16) C12 0.083(2) 0.0519(18) 0.0491(18) 0.0264(14) -0.0118(16) -0.0240(17) C13 0.0202(10) 0.0246(10) 0.0285(11) 0.0015(8) 0.0021(8) -0.0013(8) C14 0.0236(11) 0.0284(11) 0.0319(11) -0.0074(9) 0.0038(9) -0.0035(9) C15 0.0307(12) 0.0336(12) 0.0552(15) -0.0131(12) 0.0139(11) -0.0081(11) C16 0.0343(13) 0.0347(13) 0.0444(14) -0.0123(11) 0.0126(10) -0.0041(10) C17 0.0359(14) 0.0551(16) 0.0340(13) -0.0080(12) -0.0048(10) 0.0028(12) C7 0.0283(11) 0.0261(11) 0.0364(12) 0.0013(9) 0.0049(9) 0.0002(9) N1 0.0277(10) 0.0317(10) 0.0360(11) 0.0041(8) 0.0051(8) -0.0050(8) _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 Ho1 O5 2.3143(14) 3_667 ? Ho1 O1 2.3399(14) . ? Ho1 O6 2.3431(15) . ? Ho1 O4 2.3446(15) . ? Ho1 O8 2.3670(15) . ? Ho1 O10 2.3852(15) . ? Ho1 O3 2.4585(15) . ? Ho1 O2 2.4933(15) . ? Ho1 O11 2.6179(17) . ? Ho1 N1 2.9237(19) . ? Ho1 Fe1 3.3957(4) 3_667 ? Ho1 Fe1 3.4054(4) . ? Fe1 O1 1.9343(14) . ? Fe1 O4 1.9519(14) 3_667 ? Fe1 O9 1.9844(15) . ? Fe1 O7 1.9941(15) 3_667 ? Fe1 O5 2.1004(15) . ? Fe1 O5 2.1053(14) 3_667 ? Fe1 Ho1 3.3958(4) 3_667 ? O1 C1 1.406(3) . ? O2 C3 1.433(3) . ? O2 C2 1.448(3) . ? O3 C4 1.436(3) . ? O3 C5 1.445(3) . ? O4 C6 1.405(3) . ? O4 Fe1 1.9519(14) 3_667 ? O6 C8 1.244(3) . ? O7 C8 1.276(3) . ? O7 Fe1 1.9941(15) 3_667 ? O8 C13 1.245(3) . ? O9 C13 1.277(3) . ? O5 C7 1.451(3) . ? O5 Fe1 2.1052(14) 3_667 ? O5 Ho1 2.3143(13) 3_667 ? O10 N1 1.283(2) . ? O11 N1 1.248(2) . ? O12 N1 1.214(3) . ? C1 C2 1.501(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.498(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.502(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C8 C9 1.531(3) . ? C9 C10 1.520(3) . ? C9 C12 1.524(4) . ? C9 C11 1.531(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.523(3) . ? C14 C15 1.522(3) . ? C14 C16 1.524(3) . ? C14 C17 1.536(3) . ? 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 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 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 O5 Ho1 O1 69.59(5) 3_667 . ? O5 Ho1 O6 79.86(5) 3_667 . ? O1 Ho1 O6 140.16(5) . . ? O5 Ho1 O4 70.08(5) 3_667 . ? O1 Ho1 O4 73.91(5) . . ? O6 Ho1 O4 71.96(5) . . ? O5 Ho1 O8 79.23(5) 3_667 . ? O1 Ho1 O8 71.41(5) . . ? O6 Ho1 O8 127.88(5) . . ? O4 Ho1 O8 139.82(5) . . ? O5 Ho1 O10 138.05(5) 3_667 . ? O1 Ho1 O10 136.75(5) . . ? O6 Ho1 O10 83.08(5) . . ? O4 Ho1 O10 138.40(5) . . ? O8 Ho1 O10 81.71(5) . . ? O5 Ho1 O3 136.39(5) 3_667 . ? O1 Ho1 O3 103.50(5) . . ? O6 Ho1 O3 81.25(5) . . ? O4 Ho1 O3 66.78(5) . . ? O8 Ho1 O3 141.34(5) . . ? O10 Ho1 O3 77.13(5) . . ? O5 Ho1 O2 135.46(5) 3_667 . ? O1 Ho1 O2 67.16(5) . . ? O6 Ho1 O2 143.31(5) . . ? O4 Ho1 O2 106.84(5) . . ? O8 Ho1 O2 77.55(5) . . ? O10 Ho1 O2 74.48(5) . . ? O3 Ho1 O2 65.82(5) . . ? O5 Ho1 O11 87.33(5) 3_667 . ? O1 Ho1 O11 134.31(5) . . ? O6 Ho1 O11 66.14(5) . . ? O4 Ho1 O11 135.20(5) . . ? O8 Ho1 O11 65.70(5) . . ? O10 Ho1 O11 50.73(5) . . ? O3 Ho1 O11 119.60(5) . . ? O2 Ho1 O11 116.02(5) . . ? O5 Ho1 N1 112.58(5) 3_667 . ? O1 Ho1 N1 142.00(5) . . ? O6 Ho1 N1 73.20(5) . . ? O4 Ho1 N1 143.88(5) . . ? O8 Ho1 N1 71.92(5) . . ? O10 Ho1 N1 25.48(5) . . ? O3 Ho1 N1 98.80(5) . . ? O2 Ho1 N1 95.44(5) . . ? O11 Ho1 N1 25.26(5) . . ? O5 Ho1 Fe1 37.46(4) 3_667 3_667 ? O1 Ho1 Fe1 74.83(4) . 3_667 ? O6 Ho1 Fe1 65.39(4) . 3_667 ? O4 Ho1 Fe1 33.89(3) . 3_667 ? O8 Ho1 Fe1 115.48(3) . 3_667 ? O10 Ho1 Fe1 148.40(4) . 3_667 ? O3 Ho1 Fe1 98.97(4) . 3_667 ? O2 Ho1 Fe1 133.07(4) . 3_667 ? O11 Ho1 Fe1 110.06(4) . 3_667 ? N1 Ho1 Fe1 131.39(4) . 3_667 ? O5 Ho1 Fe1 37.41(3) 3_667 . ? O1 Ho1 Fe1 33.23(3) . . ? O6 Ho1 Fe1 115.90(4) . . ? O4 Ho1 Fe1 74.49(3) . . ? O8 Ho1 Fe1 65.40(3) . . ? O10 Ho1 Fe1 147.10(4) . . ? O3 Ho1 Fe1 129.84(4) . . ? O2 Ho1 Fe1 98.11(3) . . ? O11 Ho1 Fe1 110.22(3) . . ? N1 Ho1 Fe1 130.81(4) . . ? Fe1 Ho1 Fe1 56.462(10) 3_667 . ? O1 Fe1 O4 168.10(6) . 3_667 ? O1 Fe1 O9 92.19(6) . . ? O4 Fe1 O9 94.79(6) 3_667 . ? O1 Fe1 O7 96.75(6) . 3_667 ? O4 Fe1 O7 92.11(6) 3_667 3_667 ? O9 Fe1 O7 95.92(6) . 3_667 ? O1 Fe1 O5 89.11(6) . . ? O4 Fe1 O5 82.53(6) 3_667 . ? O9 Fe1 O5 171.05(6) . . ? O7 Fe1 O5 92.72(6) 3_667 . ? O1 Fe1 O5 82.10(6) . 3_667 ? O4 Fe1 O5 88.12(6) 3_667 3_667 ? O9 Fe1 O5 91.21(6) . 3_667 ? O7 Fe1 O5 172.82(6) 3_667 3_667 ? O5 Fe1 O5 80.19(6) . 3_667 ? O1 Fe1 Ho1 131.00(4) . 3_667 ? O4 Fe1 Ho1 42.05(4) 3_667 3_667 ? O9 Fe1 Ho1 136.63(4) . 3_667 ? O7 Fe1 Ho1 84.19(4) 3_667 3_667 ? O5 Fe1 Ho1 42.08(4) . 3_667 ? O5 Fe1 Ho1 91.21(4) 3_667 3_667 ? O1 Fe1 Ho1 41.52(4) . . ? O4 Fe1 Ho1 129.79(4) 3_667 . ? O9 Fe1 Ho1 84.11(4) . . ? O7 Fe1 Ho1 138.04(4) 3_667 . ? O5 Fe1 Ho1 91.03(4) . . ? O5 Fe1 Ho1 41.90(4) 3_667 . ? Ho1 Fe1 Ho1 123.537(10) 3_667 . ? C1 O1 Fe1 130.22(13) . . ? C1 O1 Ho1 121.96(12) . . ? Fe1 O1 Ho1 105.24(6) . . ? C3 O2 C2 113.24(18) . . ? C3 O2 Ho1 119.95(13) . . ? C2 O2 Ho1 112.64(12) . . ? C4 O3 C5 113.39(18) . . ? C4 O3 Ho1 113.38(13) . . ? C5 O3 Ho1 115.40(12) . . ? C6 O4 Fe1 124.54(13) . 3_667 ? C6 O4 Ho1 119.66(12) . . ? Fe1 O4 Ho1 104.06(6) 3_667 . ? C8 O6 Ho1 138.48(13) . . ? C8 O7 Fe1 125.89(14) . 3_667 ? C13 O8 Ho1 137.47(13) . . ? C13 O9 Fe1 127.00(14) . . ? C7 O5 Fe1 116.86(13) . . ? C7 O5 Fe1 117.25(12) . 3_667 ? Fe1 O5 Fe1 99.81(6) . 3_667 ? C7 O5 Ho1 118.53(12) . 3_667 ? Fe1 O5 Ho1 100.45(6) . 3_667 ? Fe1 O5 Ho1 100.70(6) 3_667 3_667 ? N1 O10 Ho1 101.43(12) . . ? N1 O11 Ho1 91.21(12) . . ? O1 C1 C2 109.78(19) . . ? O1 C1 H1A 109.7 . . ? C2 C1 H1A 109.7 . . ? O1 C1 H1B 109.7 . . ? C2 C1 H1B 109.7 . . ? H1A C1 H1B 108.2 . . ? O2 C2 C1 108.56(19) . . ? O2 C2 H2A 110.0 . . ? C1 C2 H2A 110.0 . . ? O2 C2 H2B 110.0 . . ? C1 C2 H2B 110.0 . . ? H2A C2 H2B 108.4 . . ? O2 C3 C4 106.93(19) . . ? O2 C3 H3A 110.3 . . ? C4 C3 H3A 110.3 . . ? O2 C3 H3B 110.3 . . ? C4 C3 H3B 110.3 . . ? H3A C3 H3B 108.6 . . ? O3 C4 C3 111.06(18) . . ? O3 C4 H4A 109.4 . . ? C3 C4 H4A 109.4 . . ? O3 C4 H4B 109.4 . . ? C3 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? O3 C5 C6 106.55(18) . . ? O3 C5 H5A 110.4 . . ? C6 C5 H5A 110.4 . . ? O3 C5 H5B 110.4 . . ? C6 C5 H5B 110.4 . . ? H5A C5 H5B 108.6 . . ? O4 C6 C5 108.40(19) . . ? O4 C6 H6A 110.0 . . ? C5 C6 H6A 110.0 . . ? O4 C6 H6B 110.0 . . ? C5 C6 H6B 110.0 . . ? H6A C6 H6B 108.4 . . ? O6 C8 O7 124.69(19) . . ? O6 C8 C9 117.93(18) . . ? O7 C8 C9 117.38(19) . . ? C10 C9 C12 109.9(2) . . ? C10 C9 C8 111.92(18) . . ? C12 C9 C8 108.0(2) . . ? C10 C9 C11 109.1(2) . . ? C12 C9 C11 110.7(2) . . ? C8 C9 C11 107.18(19) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O8 C13 O9 124.8(2) . . ? O8 C13 C14 119.36(18) . . ? O9 C13 C14 115.79(18) . . ? C13 C14 C15 110.17(19) . . ? C13 C14 C16 109.53(18) . . ? C15 C14 C16 110.73(19) . . ? C13 C14 C17 106.80(19) . . ? C15 C14 C17 109.5(2) . . ? C16 C14 C17 110.0(2) . . ? 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 . . ? O5 C7 H7A 109.5 . . ? O5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O12 N1 O11 123.1(2) . . ? O12 N1 O10 120.2(2) . . ? O11 N1 O10 116.63(17) . . ? O12 N1 Ho1 173.25(17) . . ? O11 N1 Ho1 63.53(11) . . ? O10 N1 Ho1 53.10(9) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.412 _refine_diff_density_min -0.529 _refine_diff_density_rms 0.064