# 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_Compound1 _database_code_depnum_ccdc_archive 'CCDC 871379' #TrackingRef 'Compound 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Compound1 _chemical_melting_point ? _chemical_formula_moiety 'C26 H53 Dy2 O16' _chemical_formula_sum 'C26 H53 Dy2 O16' _chemical_formula_weight 946.68 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' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.710(6) _cell_length_b 13.941(6) _cell_length_c 8.914(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.046(8) _cell_angle_gamma 90.00 _cell_volume 1810.0(13) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Rod _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.737 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 938 _exptl_absorpt_coefficient_mu 4.160 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6351 _exptl_absorpt_correction_T_max 0.7059 _exptl_absorpt_process_details 'multi-scan absorption' _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 ? _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 3659 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0013 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 26.24 _reflns_number_total 3659 _reflns_number_gt 3657 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^ > 2\s(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^)+(0.0309P)^2^+4.4662P] 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 3659 _refine_ls_number_parameters 153 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0242 _refine_ls_R_factor_gt 0.0242 _refine_ls_wR_factor_ref 0.0650 _refine_ls_wR_factor_gt 0.0650 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.103 _refine_ls_shift/su_max 0.102 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3084(3) 0.4638(3) 1.2156(4) 0.0428(9) Uani 1 1 d . . . C2 C 0.2496(4) 0.5000(4) 1.3228(6) 0.0771(17) Uani 1 1 d . . . H2A H 0.2540 0.5693 1.3295 0.092 Uiso 1 1 calc R . . H2B H 0.2690 0.4734 1.4227 0.092 Uiso 1 1 calc R . . C3 C 0.1516(7) 0.4703(9) 1.2664(13) 0.149(4) Uiso 1 1 d . . . H3A H 0.1503 0.4016 1.2499 0.179 Uiso 1 1 calc R . . H3B H 0.1142 0.4838 1.3453 0.179 Uiso 1 1 calc R . . C4 C 0.1103(8) 0.5168(12) 1.1285(12) 0.238(10) Uani 1 1 d . . . H4A H 0.0557 0.4828 1.0874 0.357 Uiso 1 1 calc R . . H4B H 0.1529 0.5166 1.0562 0.357 Uiso 1 1 calc R . . H4C H 0.0949 0.5817 1.1502 0.357 Uiso 1 1 calc R . . C5 C 0.2630(3) 0.3627(3) 0.7609(5) 0.0451(9) Uiso 1 1 d . . . C6 C 0.1793(3) 0.3312(4) 0.6430(6) 0.0655(13) Uiso 1 1 d . . . H6A H 0.1755 0.3730 0.5554 0.079 Uiso 1 1 calc R . . H6B H 0.1898 0.2664 0.6095 0.079 Uiso 1 1 calc R . . C7 C 0.0863(8) 0.3341(10) 0.7069(15) 0.160(4) Uiso 1 1 d . . . H7A H 0.0937 0.3115 0.8108 0.192 Uiso 1 1 calc R . . H7B H 0.0619 0.3989 0.7037 0.192 Uiso 1 1 calc R . . C8 C 0.0235(11) 0.2684(12) 0.6050(17) 0.220(7) Uiso 1 1 d . . . H8A H -0.0389 0.2791 0.6209 0.330 Uiso 1 1 calc R . . H8B H 0.0399 0.2029 0.6281 0.330 Uiso 1 1 calc R . . H8C H 0.0295 0.2814 0.5011 0.330 Uiso 1 1 calc R . . C9 C 0.4285(3) 0.6089(3) 0.7945(5) 0.0406(8) Uiso 1 1 d . . . C10 C 0.3399(4) 0.6155(4) 0.6944(7) 0.0731(15) Uiso 1 1 d . . . H10A H 0.3205 0.5525 0.6563 0.088 Uiso 1 1 calc R . . H10B H 0.3455 0.6570 0.6089 0.088 Uiso 1 1 calc R . . C11 C 0.2626(8) 0.6613(9) 0.7997(13) 0.150(4) Uiso 1 1 d . . . H11A H 0.2608 0.6228 0.8899 0.180 Uiso 1 1 calc R . . H11B H 0.2789 0.7265 0.8302 0.180 Uiso 1 1 calc R . . C12 C 0.1734(16) 0.6592(18) 0.703(3) 0.340(12) Uiso 1 1 d . . . H12A H 0.1274 0.6855 0.7581 0.510 Uiso 1 1 calc R . . H12B H 0.1579 0.5942 0.6752 0.510 Uiso 1 1 calc R . . H12C H 0.1766 0.6967 0.6140 0.510 Uiso 1 1 calc R . . C13 C 0.39163(19) 0.1121(2) 0.9558(4) 0.0221(6) Uiso 1 1 d . . . H13A H 0.3356 0.0793 0.9674 0.033 Uiso 1 1 calc R . . H13B H 0.4398 0.0906 1.0324 0.033 Uiso 1 1 calc R . . H13C H 0.4080 0.0985 0.8575 0.033 Uiso 1 1 calc R . . Dy1 Dy 0.407635(12) 0.390341(9) 0.983166(14) 0.03045(7) Uani 1 1 d . . . O1 O 0.3442(2) 0.5173(2) 1.1245(3) 0.0474(7) Uani 1 1 d . . . O2 O 0.3256(2) 0.37276(16) 1.2064(3) 0.0355(6) Uani 1 1 d . . . O3 O 0.2458(3) 0.3968(3) 0.8909(5) 0.0804(12) Uani 1 1 d . . . O4 O 0.33851(18) 0.36338(18) 0.7254(3) 0.0348(5) Uani 1 1 d . . . O5 O 0.4496(2) 0.53361(16) 0.8730(2) 0.0381(6) Uani 1 1 d . . . O6 O 0.4846(2) 0.67741(19) 0.8093(3) 0.0444(6) Uani 1 1 d . . . O7 O 0.3772(2) 0.22662(17) 0.9729(3) 0.0471(7) Uani 1 1 d . . . O8 O 0.5315(2) 0.33671(18) 0.8610(3) 0.0460(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 C1 0.055(2) 0.0333(19) 0.037(2) 0.0076(16) -0.0023(16) 0.0038(16) C2 0.122(5) 0.060(3) 0.059(3) 0.013(3) 0.052(3) 0.012(3) C4 0.215(12) 0.40(2) 0.122(8) 0.091(11) 0.093(8) 0.217(15) Dy1 0.07042(14) 0.01069(9) 0.01159(9) -0.00051(4) 0.01041(7) -0.00249(6) O1 0.0681(18) 0.0415(15) 0.0352(14) 0.0027(12) 0.0159(13) 0.0008(13) O2 0.0720(17) 0.0198(10) 0.0159(10) 0.0035(8) 0.0107(10) 0.0037(11) O3 0.089(3) 0.077(3) 0.080(3) -0.023(2) 0.028(2) -0.007(2) O4 0.0573(15) 0.0281(12) 0.0199(11) -0.0045(9) 0.0080(10) -0.0047(11) O5 0.0862(19) 0.0148(10) 0.0134(10) 0.0051(8) 0.0075(11) -0.0014(11) O6 0.0661(17) 0.0308(13) 0.0328(13) 0.0007(11) -0.0049(12) 0.0028(12) O7 0.104(2) 0.0167(11) 0.0250(12) -0.0040(9) 0.0238(13) -0.0149(13) O8 0.0760(19) 0.0208(12) 0.0443(15) -0.0039(11) 0.0195(13) 0.0027(12) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.270(5) . ? C1 O2 1.299(4) . ? C1 C2 1.465(6) . ? C1 Dy1 2.885(4) . ? C2 C3 1.516(12) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.446(13) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 O4 1.197(5) . ? C5 O3 1.310(6) . ? C5 C6 1.566(7) . ? C5 Dy1 2.724(4) . ? C6 C7 1.555(12) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.511(16) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 O6 1.258(5) . ? C9 O5 1.276(4) . ? C9 C10 1.475(7) . ? C9 Dy1 2.899(4) 3_667 ? C10 C11 1.697(12) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.46(2) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 O7 1.621(4) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? Dy1 O7 2.325(3) . ? Dy1 O5 2.346(2) . ? Dy1 O8 2.371(3) . ? Dy1 O3 2.410(5) . ? Dy1 O4 2.409(3) . ? Dy1 O1 2.433(3) . ? Dy1 O6 2.451(3) 3_667 ? Dy1 O2 2.480(3) . ? Dy1 O5 2.534(3) 3_667 ? Dy1 C9 2.899(4) 3_667 ? O5 Dy1 2.534(3) 3_667 ? O6 Dy1 2.451(3) 3_667 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 O2 115.5(4) . . ? O1 C1 C2 123.4(4) . . ? O2 C1 C2 121.0(4) . . ? O1 C1 Dy1 56.8(2) . . ? O2 C1 Dy1 59.0(2) . . ? C2 C1 Dy1 174.3(4) . . ? C1 C2 C3 108.1(6) . . ? C1 C2 H2A 110.1 . . ? C3 C2 H2A 110.1 . . ? C1 C2 H2B 110.1 . . ? C3 C2 H2B 110.1 . . ? H2A C2 H2B 108.4 . . ? C4 C3 C2 115.3(11) . . ? C4 C3 H3A 108.5 . . ? C2 C3 H3A 108.5 . . ? C4 C3 H3B 108.5 . . ? C2 C3 H3B 108.5 . . ? H3A C3 H3B 107.5 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O4 C5 O3 122.2(4) . . ? O4 C5 C6 119.7(4) . . ? O3 C5 C6 117.6(4) . . ? O4 C5 Dy1 62.1(2) . . ? O3 C5 Dy1 62.2(3) . . ? C6 C5 Dy1 171.4(3) . . ? C7 C6 C5 113.4(6) . . ? C7 C6 H6A 108.9 . . ? C5 C6 H6A 108.9 . . ? C7 C6 H6B 108.9 . . ? C5 C6 H6B 108.9 . . ? H6A C6 H6B 107.7 . . ? C8 C7 C6 105.0(10) . . ? C8 C7 H7A 110.8 . . ? C6 C7 H7A 110.8 . . ? C8 C7 H7B 110.7 . . ? C6 C7 H7B 110.7 . . ? H7A C7 H7B 108.8 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.4 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O6 C9 O5 117.5(4) . . ? O6 C9 C10 121.8(4) . . ? O5 C9 C10 120.7(4) . . ? O6 C9 Dy1 56.93(19) . 3_667 ? O5 C9 Dy1 60.8(2) . 3_667 ? C10 C9 Dy1 173.1(3) . 3_667 ? C9 C10 C11 107.0(6) . . ? C9 C10 H10A 110.3 . . ? C11 C10 H10A 110.3 . . ? C9 C10 H10B 110.3 . . ? C11 C10 H10B 110.3 . . ? H10A C10 H10B 108.6 . . ? C12 C11 C10 106.5(12) . . ? C12 C11 H11A 110.4 . . ? C10 C11 H11A 110.4 . . ? C12 C11 H11B 110.4 . . ? C10 C11 H11B 110.4 . . ? H11A C11 H11B 108.6 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O7 C13 H13A 109.5 . . ? O7 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O7 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O7 Dy1 O5 151.60(8) . . ? O7 Dy1 O8 80.11(10) . . ? O5 Dy1 O8 79.16(9) . . ? O7 Dy1 O3 81.25(13) . . ? O5 Dy1 O3 97.51(13) . . ? O8 Dy1 O3 129.89(13) . . ? O7 Dy1 O4 75.88(9) . . ? O5 Dy1 O4 80.47(8) . . ? O8 Dy1 O4 76.19(10) . . ? O3 Dy1 O4 54.22(12) . . ? O7 Dy1 O1 130.45(10) . . ? O5 Dy1 O1 74.93(9) . . ? O8 Dy1 O1 147.40(10) . . ? O3 Dy1 O1 73.57(12) . . ? O4 Dy1 O1 117.80(10) . . ? O7 Dy1 O6 75.64(10) . 3_667 ? O5 Dy1 O6 117.63(10) . 3_667 ? O8 Dy1 O6 76.58(10) . 3_667 ? O3 Dy1 O6 140.88(13) . 3_667 ? O4 Dy1 O6 143.33(9) . 3_667 ? O1 Dy1 O6 98.26(10) . 3_667 ? O7 Dy1 O2 79.75(8) . . ? O5 Dy1 O2 127.31(8) . . ? O8 Dy1 O2 146.02(9) . . ? O3 Dy1 O2 73.08(13) . . ? O4 Dy1 O2 124.22(9) . . ? O1 Dy1 O2 52.50(9) . . ? O6 Dy1 O2 72.06(10) 3_667 . ? O7 Dy1 O5 124.88(10) . 3_667 ? O5 Dy1 O5 66.89(9) . 3_667 ? O8 Dy1 O5 74.26(10) . 3_667 ? O3 Dy1 O5 150.01(11) . 3_667 ? O4 Dy1 O5 139.20(8) . 3_667 ? O1 Dy1 O5 77.55(10) . 3_667 ? O6 Dy1 O5 51.46(9) 3_667 3_667 ? O2 Dy1 O5 95.58(9) . 3_667 ? O7 Dy1 C5 72.90(12) . . ? O5 Dy1 C5 92.33(11) . . ? O8 Dy1 C5 101.15(12) . . ? O3 Dy1 C5 28.74(13) . . ? O4 Dy1 C5 26.05(11) . . ? O1 Dy1 C5 99.36(12) . . ? O6 Dy1 C5 148.35(11) 3_667 . ? O2 Dy1 C5 98.71(12) . . ? O5 Dy1 C5 159.15(11) 3_667 . ? O7 Dy1 C1 105.24(10) . . ? O5 Dy1 C1 100.82(10) . . ? O8 Dy1 C1 160.19(11) . . ? O3 Dy1 C1 69.90(13) . . ? O4 Dy1 C1 123.52(10) . . ? O1 Dy1 C1 25.89(10) . . ? O6 Dy1 C1 86.18(11) 3_667 . ? O2 Dy1 C1 26.68(9) . . ? O5 Dy1 C1 87.43(10) 3_667 . ? C5 Dy1 C1 98.65(12) . . ? O7 Dy1 C9 99.65(11) . 3_667 ? O5 Dy1 C9 92.32(10) . 3_667 ? O8 Dy1 C9 72.32(11) . 3_667 ? O3 Dy1 C9 157.03(14) . 3_667 ? O4 Dy1 C9 148.49(10) . 3_667 ? O1 Dy1 C9 89.17(11) . 3_667 ? O6 Dy1 C9 25.47(10) 3_667 3_667 ? O2 Dy1 C9 84.44(11) . 3_667 ? O5 Dy1 C9 26.06(9) 3_667 3_667 ? C5 Dy1 C9 171.11(12) . 3_667 ? C1 Dy1 C9 87.92(12) . 3_667 ? C1 O1 Dy1 97.3(2) . . ? C1 O2 Dy1 94.3(2) . . ? C5 O3 Dy1 89.1(3) . . ? C5 O4 Dy1 91.8(2) . . ? C9 O5 Dy1 150.7(3) . . ? C9 O5 Dy1 93.1(2) . 3_667 ? Dy1 O5 Dy1 113.11(9) . 3_667 ? C9 O6 Dy1 97.6(2) . 3_667 ? C13 O7 Dy1 160.7(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 107.4(7) . . . . ? O2 C1 C2 C3 -71.2(7) . . . . ? Dy1 C1 C2 C3 18(3) . . . . ? C1 C2 C3 C4 -68.4(11) . . . . ? O4 C5 C6 C7 179.9(7) . . . . ? O3 C5 C6 C7 -6.9(8) . . . . ? Dy1 C5 C6 C7 80(2) . . . . ? C5 C6 C7 C8 -159.1(9) . . . . ? O6 C9 C10 C11 -88.8(7) . . . . ? O5 C9 C10 C11 89.1(7) . . . . ? Dy1 C9 C10 C11 -11(3) 3_667 . . . ? C9 C10 C11 C12 -174.9(12) . . . . ? O4 C5 Dy1 O7 -92.7(3) . . . . ? O3 C5 Dy1 O7 103.3(3) . . . . ? C6 C5 Dy1 O7 12(2) . . . . ? O4 C5 Dy1 O5 62.6(2) . . . . ? O3 C5 Dy1 O5 -101.4(3) . . . . ? C6 C5 Dy1 O5 167(2) . . . . ? O4 C5 Dy1 O8 -16.9(3) . . . . ? O3 C5 Dy1 O8 179.2(3) . . . . ? C6 C5 Dy1 O8 88(2) . . . . ? O4 C5 Dy1 O3 164.0(4) . . . . ? C6 C5 Dy1 O3 -91(2) . . . . ? O3 C5 Dy1 O4 -164.0(4) . . . . ? C6 C5 Dy1 O4 105(2) . . . . ? O4 C5 Dy1 O1 137.7(2) . . . . ? O3 C5 Dy1 O1 -26.3(3) . . . . ? C6 C5 Dy1 O1 -118(2) . . . . ? O4 C5 Dy1 O6 -99.3(3) . . . 3_667 ? O3 C5 Dy1 O6 96.7(3) . . . 3_667 ? C6 C5 Dy1 O6 5(2) . . . 3_667 ? O4 C5 Dy1 O2 -169.1(2) . . . . ? O3 C5 Dy1 O2 26.9(3) . . . . ? C6 C5 Dy1 O2 -64(2) . . . . ? O4 C5 Dy1 O5 58.1(4) . . . 3_667 ? O3 C5 Dy1 O5 -105.9(4) . . . 3_667 ? C6 C5 Dy1 O5 162.9(19) . . . 3_667 ? O4 C5 Dy1 C1 163.9(2) . . . . ? O3 C5 Dy1 C1 -0.1(3) . . . . ? C6 C5 Dy1 C1 -91(2) . . . . ? O4 C5 Dy1 C9 -58.9(8) . . . 3_667 ? O3 C5 Dy1 C9 137.1(7) . . . 3_667 ? C6 C5 Dy1 C9 46(2) . . . 3_667 ? O1 C1 Dy1 O7 -168.2(2) . . . . ? O2 C1 Dy1 O7 17.7(2) . . . . ? C2 C1 Dy1 O7 -75(3) . . . . ? O1 C1 Dy1 O5 0.4(3) . . . . ? O2 C1 Dy1 O5 -173.7(2) . . . . ? C2 C1 Dy1 O5 94(3) . . . . ? O1 C1 Dy1 O8 88.5(4) . . . . ? O2 C1 Dy1 O8 -85.7(4) . . . . ? C2 C1 Dy1 O8 -178(3) . . . . ? O1 C1 Dy1 O3 -93.7(3) . . . . ? O2 C1 Dy1 O3 92.2(2) . . . . ? C2 C1 Dy1 O3 0(3) . . . . ? O1 C1 Dy1 O4 -85.2(3) . . . . ? O2 C1 Dy1 O4 100.6(2) . . . . ? C2 C1 Dy1 O4 8(3) . . . . ? O2 C1 Dy1 O1 -174.2(4) . . . . ? C2 C1 Dy1 O1 94(3) . . . . ? O1 C1 Dy1 O6 117.9(2) . . . 3_667 ? O2 C1 Dy1 O6 -56.3(2) . . . 3_667 ? C2 C1 Dy1 O6 -149(3) . . . 3_667 ? O1 C1 Dy1 O2 174.2(4) . . . . ? C2 C1 Dy1 O2 -92(3) . . . . ? O1 C1 Dy1 O5 66.3(2) . . . 3_667 ? O2 C1 Dy1 O5 -107.8(2) . . . 3_667 ? C2 C1 Dy1 O5 160(3) . . . 3_667 ? O1 C1 Dy1 C5 -93.6(3) . . . . ? O2 C1 Dy1 C5 92.2(2) . . . . ? C2 C1 Dy1 C5 0(3) . . . . ? O1 C1 Dy1 C9 92.4(2) . . . 3_667 ? O2 C1 Dy1 C9 -81.8(2) . . . 3_667 ? C2 C1 Dy1 C9 -174(3) . . . 3_667 ? O2 C1 O1 Dy1 5.5(4) . . . . ? C2 C1 O1 Dy1 -173.1(4) . . . . ? O7 Dy1 O1 C1 15.1(3) . . . . ? O5 Dy1 O1 C1 -179.6(3) . . . . ? O8 Dy1 O1 C1 -141.0(2) . . . . ? O3 Dy1 O1 C1 77.7(3) . . . . ? O4 Dy1 O1 C1 110.1(2) . . . . ? O6 Dy1 O1 C1 -63.1(2) 3_667 . . . ? O2 Dy1 O1 C1 -3.3(2) . . . . ? O5 Dy1 O1 C1 -110.5(2) 3_667 . . . ? C5 Dy1 O1 C1 90.5(3) . . . . ? C9 Dy1 O1 C1 -86.9(2) 3_667 . . . ? O1 C1 O2 Dy1 -5.4(4) . . . . ? C2 C1 O2 Dy1 173.3(4) . . . . ? O7 Dy1 O2 C1 -162.7(2) . . . . ? O5 Dy1 O2 C1 7.8(3) . . . . ? O8 Dy1 O2 C1 142.8(2) . . . . ? O3 Dy1 O2 C1 -78.8(2) . . . . ? O4 Dy1 O2 C1 -97.7(2) . . . . ? O1 Dy1 O2 C1 3.2(2) . . . . ? O6 Dy1 O2 C1 119.2(2) 3_667 . . . ? O5 Dy1 O2 C1 72.8(2) 3_667 . . . ? C5 Dy1 O2 C1 -91.9(2) . . . . ? C9 Dy1 O2 C1 96.4(2) 3_667 . . . ? O4 C5 O3 Dy1 -16.8(5) . . . . ? C6 C5 O3 Dy1 170.3(4) . . . . ? O7 Dy1 O3 C5 -70.3(3) . . . . ? O5 Dy1 O3 C5 81.1(3) . . . . ? O8 Dy1 O3 C5 -1.0(3) . . . . ? O4 Dy1 O3 C5 8.6(2) . . . . ? O1 Dy1 O3 C5 152.9(3) . . . . ? O6 Dy1 O3 C5 -124.3(3) 3_667 . . . ? O2 Dy1 O3 C5 -152.1(3) . . . . ? O5 Dy1 O3 C5 136.8(3) 3_667 . . . ? C1 Dy1 O3 C5 179.9(3) . . . . ? C9 Dy1 O3 C5 -164.4(3) 3_667 . . . ? O3 C5 O4 Dy1 16.8(5) . . . . ? C6 C5 O4 Dy1 -170.4(4) . . . . ? O7 Dy1 O4 C5 79.9(3) . . . . ? O5 Dy1 O4 C5 -115.9(3) . . . . ? O8 Dy1 O4 C5 163.0(3) . . . . ? O3 Dy1 O4 C5 -9.4(3) . . . . ? O1 Dy1 O4 C5 -48.7(3) . . . . ? O6 Dy1 O4 C5 119.9(3) 3_667 . . . ? O2 Dy1 O4 C5 13.0(3) . . . . ? O5 Dy1 O4 C5 -152.5(2) 3_667 . . . ? C1 Dy1 O4 C5 -19.2(3) . . . . ? C9 Dy1 O4 C5 165.3(3) 3_667 . . . ? O6 C9 O5 Dy1 159.9(3) . . . . ? C10 C9 O5 Dy1 -18.1(8) . . . . ? Dy1 C9 O5 Dy1 154.1(5) 3_667 . . . ? O6 C9 O5 Dy1 5.8(4) . . . 3_667 ? C10 C9 O5 Dy1 -172.2(4) . . . 3_667 ? O7 Dy1 O5 C9 87.1(5) . . . . ? O8 Dy1 O5 C9 130.9(5) . . . . ? O3 Dy1 O5 C9 1.6(5) . . . . ? O4 Dy1 O5 C9 53.3(5) . . . . ? O1 Dy1 O5 C9 -69.1(5) . . . . ? O6 Dy1 O5 C9 -160.6(5) 3_667 . . . ? O2 Dy1 O5 C9 -72.8(5) . . . . ? O5 Dy1 O5 C9 -151.7(5) 3_667 . . . ? C5 Dy1 O5 C9 30.0(5) . . . . ? C1 Dy1 O5 C9 -69.3(5) . . . . ? C9 Dy1 O5 C9 -157.6(4) 3_667 . . . ? O7 Dy1 O5 Dy1 -121.2(2) . . . 3_667 ? O8 Dy1 O5 Dy1 -77.37(12) . . . 3_667 ? O3 Dy1 O5 Dy1 153.33(13) . . . 3_667 ? O4 Dy1 O5 Dy1 -155.00(12) . . . 3_667 ? O1 Dy1 O5 Dy1 82.66(12) . . . 3_667 ? O6 Dy1 O5 Dy1 -8.89(14) 3_667 . . 3_667 ? O2 Dy1 O5 Dy1 78.92(15) . . . 3_667 ? O5 Dy1 O5 Dy1 0.0 3_667 . . 3_667 ? C5 Dy1 O5 Dy1 -178.28(12) . . . 3_667 ? C1 Dy1 O5 Dy1 82.46(13) . . . 3_667 ? C9 Dy1 O5 Dy1 -5.86(12) 3_667 . . 3_667 ? O5 C9 O6 Dy1 -6.0(4) . . . 3_667 ? C10 C9 O6 Dy1 171.9(4) . . . 3_667 ? O5 Dy1 O7 C13 61.0(7) . . . . ? O8 Dy1 O7 C13 17.3(6) . . . . ? O3 Dy1 O7 C13 150.6(6) . . . . ? O4 Dy1 O7 C13 95.4(6) . . . . ? O1 Dy1 O7 C13 -149.9(5) . . . . ? O6 Dy1 O7 C13 -61.2(6) 3_667 . . . ? O2 Dy1 O7 C13 -135.2(6) . . . . ? O5 Dy1 O7 C13 -45.5(6) 3_667 . . . ? C5 Dy1 O7 C13 122.3(6) . . . . ? C1 Dy1 O7 C13 -143.1(6) . . . . ? C9 Dy1 O7 C13 -52.7(6) 3_667 . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.24 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.172 _refine_diff_density_min -0.890 _refine_diff_density_rms 0.096