# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' # Attachment '- combined cif files.cif' # 1. SUBMISSION DETAILS _journal_coden_Cambridge 0222 _publ_contact_author ; Anjana Devi Lehrstuhl f\"ur Anorganische Chemie II Ruhr-Universit\"at Bochum Universit\"atsstrasse 150 44780 Bochum Bundesrepublik Deutschland ; _publ_contact_author_phone '049 234 32-24150' _publ_contact_author_fax '049 234 321-4174' _publ_contact_author_email anjana.devi@rub.de _publ_requested_coeditor_name ? _publ_contact_letter ; ; #============================================================================== # 2. TITLE AND AUTHOR LIST _publ_section_title ; Malonate Complexes of Dysprosium: Synthesis, Characterization an Application for Atomic Vapor Deposition of Dysprosium Containing Thin Films ; loop_ _publ_author_name _publ_author_address 'Anjana Devi' ; Lehrstuhl f\"ur Anorganische Chemie II Ruhr-Universit\"at Bochum Universit\"atsstrasse 150 44780 Bochum Bundesrepublik Deutschland ; 'Andrian P. Milanov' ; Lehrstuhl f\"ur Anorganische Chemie II Ruhr-Universit\"at Bochum Universit\"atsstrasse 150 44780 Bochum Bundesrepublik Deutschland ; 'R\"udiger W. Seidel' ; Lehrstuhl f\"ur Analytische Chemie Ruhr-Universit\"at Bochum Universit\"atsstrasse 150 44780 Bochum Bundesrepublik Deutschland ; 'Davide Barreca' ; CNR-ISTM and INSTM Department of Chemistry, Padova University Via Marzolo, 1 35131 Padova Italy ; 'Alberto Gasparotto' ; Department of Chemistry Padova University and INSTM Via Marzolo, 1 35131 Padova Italy ; 'Manuela Winter' ; Lehrstuhl f\"ur Anorganische Chemie II Ruhr-Universit\"at Bochum Universit\"atsstrasse 150 44780 Bochum Bundesrepublik Deutschland ; ; J.Feydt ; ; Center of Advanced European Studies and Research (CAESAR) 53175 Bonn Bundesrepublik Deutschland ; 'Hans-Werner Becker' ; Dynamitron-Tandem-Laboratorium Ruhr-Universit\"at Bochum Universit\"atsstrasse 150 44780 Bochum Bundesrepublik Deutschland ; #============================================================================== # 4. TEXT _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_experimental ; ; _publ_section_references ; ; _publ_section_figure_captions ; ; _publ_section_acknowledgements; ; ; _publ_contact_author_name 'Anjana Devi' #============================================================================== data_cvd265 _database_code_depnum_ccdc_archive 'CCDC 770257' #TrackingRef '- combined cif files.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18.50 H25 Dy O12' _chemical_formula_weight 601.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7969(3) _cell_length_b 10.1177(3) _cell_length_c 12.0404(4) _cell_angle_alpha 73.675(3) _cell_angle_beta 84.554(2) _cell_angle_gamma 88.970(2) _cell_volume 1140.14(6) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 1500 _cell_measurement_theta_min 2.674 _cell_measurement_theta_max 27.498 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.753 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 596 _exptl_absorpt_coefficient_mu 3.336 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.430 _exptl_absorpt_correction_T_max 0.510 _exptl_absorpt_process_details abspack _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Sapphire2-CCD, Oxford Diffraction' _diffrn_measurement_method '887 images at 1.0 deg. in \w and 17 sec.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17812 _diffrn_reflns_av_R_equivalents 0.0390 _diffrn_reflns_av_sigmaI/netI 0.0566 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 27.59 _reflns_number_total 5193 _reflns_number_gt 4313 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD 171_33_34d, Oxford Diffraction' _computing_cell_refinement 'CrysAlis RED 171_33_34d, Oxford Diffraction' _computing_data_reduction 'CrysAlis RED 171_33_34d, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0126P)^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 5193 _refine_ls_number_parameters 292 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0356 _refine_ls_R_factor_gt 0.0247 _refine_ls_wR_factor_ref 0.0400 _refine_ls_wR_factor_gt 0.0389 _refine_ls_goodness_of_fit_ref 0.916 _refine_ls_restrained_S_all 0.916 _refine_ls_shift/su_max 0.023 _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 Dy1 Dy 0.922234(15) 0.000465(14) 0.157973(13) 0.01569(4) Uani 1 1 d . . . O1 O 0.91900(19) -0.23108(18) 0.17699(15) 0.0185(4) Uani 1 1 d . . . O2 O 1.04150(19) -0.10008(18) 0.31608(16) 0.0200(4) Uani 1 1 d . . . O3 O 1.1239(2) -0.24558(19) 0.47201(16) 0.0245(5) Uani 1 1 d . . . O4 O 0.9394(2) -0.4604(2) 0.23227(19) 0.0392(6) Uani 1 1 d . . . O5 O 0.79236(18) 0.19374(18) 0.09326(15) 0.0178(4) Uani 1 1 d . . . O6 O 0.74642(19) -0.02283(18) 0.29721(15) 0.0171(4) Uani 1 1 d . . . O7 O 0.5329(2) -0.0311(2) 0.38280(17) 0.0213(5) Uani 1 1 d . . . O8 O 0.61482(19) 0.33898(19) 0.05974(16) 0.0230(5) Uani 1 1 d . . . O9 O 1.11955(18) 0.02837(18) 0.02839(15) 0.0157(4) Uani 1 1 d . . . O10 O 1.05163(19) 0.17171(18) 0.19233(16) 0.0186(4) Uani 1 1 d . . . O11 O 1.23386(19) 0.26240(19) 0.24367(16) 0.0219(5) Uani 1 1 d . . . O12 O 1.31826(19) 0.07232(19) -0.06969(16) 0.0190(4) Uani 1 1 d . . . C6 C 0.6308(3) 0.0327(3) 0.3001(2) 0.0177(7) Uani 1 1 d . . . C5 C 0.5901(3) 0.1559(3) 0.2244(2) 0.0171(6) Uani 1 1 d . . . H5A H 0.5030 0.1930 0.2404 0.020 Uiso 1 1 calc R . . C70 C 0.5720(3) -0.1578(3) 0.4624(3) 0.0285(8) Uani 1 1 d . . . H70A H 0.4938 -0.1957 0.5187 0.043 Uiso 1 1 calc R . . H70B H 0.6483 -0.1400 0.5034 0.043 Uiso 1 1 calc R . . H70C H 0.6006 -0.2240 0.4191 0.043 Uiso 1 1 calc R . . C4 C 0.6740(3) 0.2257(3) 0.1261(2) 0.0174(6) Uani 1 1 d . . . C8 C 1.2710(3) 0.1699(3) 0.0892(2) 0.0187(6) Uani 1 1 d . . . H8A H 1.3620 0.2052 0.0787 0.022 Uiso 1 1 calc R . . C7 C 1.2335(3) 0.0928(3) 0.0205(2) 0.0171(6) Uani 1 1 d . . . C9 C 1.1762(3) 0.1983(3) 0.1764(2) 0.0173(6) Uani 1 1 d . . . C3 C 1.0593(3) -0.2223(3) 0.3744(2) 0.0187(6) Uani 1 1 d . . . C1 C 0.9581(3) -0.3361(3) 0.2499(3) 0.0231(7) Uani 1 1 d . . . C120 C 1.4430(3) 0.1524(3) -0.1067(3) 0.0300(8) Uani 1 1 d . . . H12A H 1.4927 0.1259 -0.1715 0.045 Uiso 1 1 calc R . . H12B H 1.5005 0.1354 -0.0418 0.045 Uiso 1 1 calc R . . H12C H 1.4207 0.2505 -0.1318 0.045 Uiso 1 1 calc R . . C80 C 0.6879(3) 0.4072(3) -0.0503(2) 0.0276(7) Uani 1 1 d . . . H80A H 0.6356 0.4870 -0.0903 0.041 Uiso 1 1 calc R . . H80B H 0.7002 0.3431 -0.0981 0.041 Uiso 1 1 calc R . . H80C H 0.7779 0.4380 -0.0374 0.041 Uiso 1 1 calc R . . C40 C 0.8829(3) -0.4624(3) 0.1278(3) 0.0327(8) Uani 1 1 d . . . H40A H 0.8748 -0.5579 0.1252 0.049 Uiso 1 1 calc R . . H40B H 0.9430 -0.4105 0.0606 0.049 Uiso 1 1 calc R . . H40C H 0.7919 -0.4204 0.1260 0.049 Uiso 1 1 calc R . . C110 C 1.1453(3) 0.2838(3) 0.3405(3) 0.0272(7) Uani 1 1 d . . . H11A H 1.1969 0.3311 0.3841 0.041 Uiso 1 1 calc R . . H11B H 1.1121 0.1946 0.3917 0.041 Uiso 1 1 calc R . . H11C H 1.0671 0.3402 0.3111 0.041 Uiso 1 1 calc R . . C2 C 1.0224(3) -0.3413(3) 0.3489(3) 0.0282(7) Uani 1 1 d . . . H2A H 1.0416 -0.4283 0.4003 0.034 Uiso 1 1 calc R . . C30 C 1.1767(3) -0.1286(3) 0.4993(3) 0.0312(8) Uani 1 1 d . . . H30A H 1.2205 -0.1593 0.5720 0.047 Uiso 1 1 calc R . . H30B H 1.1014 -0.0662 0.5083 0.047 Uiso 1 1 calc R . . H30C H 1.2443 -0.0802 0.4364 0.047 Uiso 1 1 calc R . . C91 C 0.5082(5) 0.4956(6) 0.4459(4) 0.0336(17) Uani 0.50 1 d PGD A -1 C92 C 0.6135(4) 0.4680(5) 0.5185(4) 0.0323(8) Uani 0.50 1 d PGD A -1 H92A H 0.7020 0.4450 0.4902 0.039 Uiso 0.50 1 calc PR A -1 C93 C 0.5895(5) 0.4741(5) 0.6326(4) 0.0360(17) Uani 0.50 1 d PG A -1 H93A H 0.6616 0.4553 0.6822 0.043 Uiso 0.50 1 calc PR A -1 C94 C 0.4602(5) 0.5078(6) 0.6741(4) 0.0455(10) Uani 0.50 1 d PG A -1 H94A H 0.4438 0.5119 0.7521 0.055 Uiso 0.50 1 calc PR A -1 C95 C 0.3548(4) 0.5353(5) 0.6015(4) 0.0365(17) Uani 0.50 1 d PG A -1 H95A H 0.2663 0.5584 0.6298 0.044 Uiso 0.50 1 calc PR A -1 C96 C 0.3788(5) 0.5292(5) 0.4874(4) 0.0323(8) Uani 0.50 1 d PGD A -1 H96A H 0.3067 0.5481 0.4378 0.039 Uiso 0.50 1 calc PR A -1 C97 C 0.5345(9) 0.4875(10) 0.3235(7) 0.0455(10) Uani 0.50 1 d PD A -1 H97A H 0.6304 0.4626 0.3091 0.068 Uiso 0.50 1 calc PR A -1 H97B H 0.5163 0.5771 0.2696 0.068 Uiso 0.50 1 calc PR A -1 H97C H 0.4741 0.4174 0.3117 0.068 Uiso 0.50 1 calc PR A -1 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 0.01299(7) 0.01642(7) 0.01805(7) -0.00503(5) -0.00285(5) 0.00039(5) O1 0.0212(11) 0.0152(10) 0.0197(11) -0.0041(8) -0.0069(9) 0.0024(8) O2 0.0206(12) 0.0168(10) 0.0234(11) -0.0053(9) -0.0086(9) 0.0020(9) O3 0.0308(13) 0.0239(11) 0.0219(11) -0.0086(9) -0.0126(9) 0.0063(9) O4 0.0670(17) 0.0165(11) 0.0413(14) -0.0105(10) -0.0346(12) 0.0072(11) O5 0.0136(11) 0.0174(10) 0.0208(11) -0.0025(8) -0.0011(8) -0.0014(8) O6 0.0144(11) 0.0179(10) 0.0177(11) -0.0034(8) -0.0014(8) 0.0033(8) O7 0.0154(12) 0.0255(11) 0.0188(11) -0.0010(9) 0.0041(9) 0.0011(9) O8 0.0227(12) 0.0203(11) 0.0222(11) 0.0015(9) -0.0063(9) 0.0058(9) O9 0.0109(10) 0.0192(10) 0.0186(10) -0.0073(8) -0.0034(8) -0.0017(8) O10 0.0141(11) 0.0197(10) 0.0240(11) -0.0091(9) -0.0018(9) -0.0001(9) O11 0.0201(11) 0.0258(11) 0.0251(11) -0.0144(9) -0.0052(9) -0.0028(9) O12 0.0129(11) 0.0246(11) 0.0203(11) -0.0081(9) 0.0013(9) -0.0049(9) C6 0.0184(17) 0.0227(16) 0.0159(15) -0.0107(13) -0.0036(13) -0.0038(14) C5 0.0131(16) 0.0194(15) 0.0188(16) -0.0051(12) -0.0037(12) 0.0039(12) C70 0.032(2) 0.0212(17) 0.0268(18) -0.0004(14) 0.0069(15) -0.0039(15) C4 0.0191(17) 0.0150(14) 0.0214(16) -0.0078(12) -0.0096(13) 0.0028(12) C8 0.0106(15) 0.0238(16) 0.0230(16) -0.0083(13) -0.0030(12) -0.0025(12) C7 0.0126(16) 0.0177(15) 0.0185(15) 0.0004(12) -0.0050(12) 0.0016(12) C9 0.0198(17) 0.0120(14) 0.0205(15) -0.0034(12) -0.0080(13) 0.0020(12) C3 0.0120(16) 0.0275(17) 0.0185(15) -0.0098(13) -0.0009(12) 0.0045(13) C1 0.0260(18) 0.0174(15) 0.0278(17) -0.0084(13) -0.0056(14) 0.0019(13) C120 0.0194(18) 0.0333(18) 0.038(2) -0.0132(15) 0.0082(15) -0.0084(15) C80 0.0321(19) 0.0240(16) 0.0236(17) 0.0000(13) -0.0076(14) -0.0009(14) C40 0.043(2) 0.0252(17) 0.039(2) -0.0189(15) -0.0203(16) 0.0056(15) C110 0.0271(18) 0.0323(18) 0.0295(18) -0.0198(15) -0.0065(14) 0.0069(15) C2 0.040(2) 0.0197(16) 0.0245(17) -0.0038(13) -0.0111(15) 0.0059(15) C30 0.033(2) 0.0334(19) 0.0341(19) -0.0160(15) -0.0192(15) 0.0056(15) C91 0.055(5) 0.009(3) 0.033(4) 0.000(3) -0.001(4) -0.006(3) C92 0.028(2) 0.0204(17) 0.045(2) -0.0015(16) -0.0087(17) -0.0011(15) C93 0.035(4) 0.022(3) 0.046(4) 0.003(3) -0.017(3) -0.006(3) C94 0.067(3) 0.030(2) 0.036(2) -0.0058(17) -0.002(2) -0.002(2) C95 0.029(4) 0.023(4) 0.053(5) -0.005(3) -0.001(3) -0.002(3) C96 0.028(2) 0.0204(17) 0.045(2) -0.0015(16) -0.0087(17) -0.0011(15) C97 0.067(3) 0.030(2) 0.036(2) -0.0058(17) -0.002(2) -0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O6 2.2533(18) . ? Dy1 O1 2.2895(17) . ? Dy1 O5 2.3005(18) . ? Dy1 O2 2.3053(18) . ? Dy1 O10 2.3155(18) . ? Dy1 O9 2.3346(18) . ? Dy1 O9 2.4154(18) 2_755 ? Dy1 O12 2.8638(18) 2_755 ? Dy1 Dy1 3.9639(3) 2_755 ? O1 C1 1.254(3) . ? O2 C3 1.256(3) . ? O3 C3 1.349(3) . ? O3 C30 1.432(3) . ? O4 C1 1.351(3) . ? O4 C40 1.427(3) . ? O5 C4 1.256(3) . ? O6 C6 1.257(3) . ? O7 C6 1.344(3) . ? O7 C70 1.439(3) . ? O8 C4 1.355(3) . ? O8 C80 1.438(3) . ? O9 C7 1.285(3) . ? O9 Dy1 2.4154(18) 2_755 ? O10 C9 1.240(3) . ? O11 C9 1.338(3) . ? O11 C110 1.450(3) . ? O12 C7 1.364(3) . ? O12 C120 1.442(3) . ? O12 Dy1 2.8638(18) 2_755 ? C6 C5 1.399(4) . ? C5 C4 1.394(4) . ? C5 H5A 0.9500 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C8 C7 1.364(4) . ? C8 C9 1.423(4) . ? C8 H8A 0.9500 . ? C3 C2 1.386(4) . ? C1 C2 1.388(4) . ? C120 H12A 0.9800 . ? C120 H12B 0.9800 . ? C120 H12C 0.9800 . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C110 H11A 0.9800 . ? C110 H11B 0.9800 . ? C110 H11C 0.9800 . ? C2 H2A 0.9500 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C91 C92 1.3900 . ? C91 C96 1.3900 . ? C91 C97 1.497(6) . ? C92 C93 1.3900 . ? C92 H92A 0.9500 . ? C93 C94 1.3900 . ? C93 H93A 0.9500 . ? C94 C95 1.3900 . ? C94 H94A 0.9500 . ? C95 C96 1.3900 . ? C95 H95A 0.9500 . ? C96 H96A 0.9500 . ? C97 H97A 0.9800 . ? C97 H97B 0.9800 . ? C97 H97C 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 O6 Dy1 O1 91.09(6) . . ? O6 Dy1 O5 75.85(6) . . ? O1 Dy1 O5 140.32(6) . . ? O6 Dy1 O2 82.10(6) . . ? O1 Dy1 O2 74.23(6) . . ? O5 Dy1 O2 138.01(6) . . ? O6 Dy1 O10 101.43(6) . . ? O1 Dy1 O10 142.28(7) . . ? O5 Dy1 O10 77.40(6) . . ? O2 Dy1 O10 72.52(6) . . ? O6 Dy1 O9 173.80(7) . . ? O1 Dy1 O9 90.74(6) . . ? O5 Dy1 O9 106.27(6) . . ? O2 Dy1 O9 92.71(6) . . ? O10 Dy1 O9 73.65(6) . . ? O6 Dy1 O9 119.31(6) . 2_755 ? O1 Dy1 O9 72.57(6) . 2_755 ? O5 Dy1 O9 81.49(6) . 2_755 ? O2 Dy1 O9 140.37(6) . 2_755 ? O10 Dy1 O9 127.24(6) . 2_755 ? O9 Dy1 O9 66.88(7) . 2_755 ? O6 Dy1 O12 71.90(6) . 2_755 ? O1 Dy1 O12 69.83(6) . 2_755 ? O5 Dy1 O12 70.50(6) . 2_755 ? O2 Dy1 O12 134.57(6) . 2_755 ? O10 Dy1 O12 147.88(6) . 2_755 ? O9 Dy1 O12 114.28(6) . 2_755 ? O9 Dy1 O12 47.46(5) 2_755 2_755 ? O6 Dy1 Dy1 152.11(5) . 2_755 ? O1 Dy1 Dy1 79.92(4) . 2_755 ? O5 Dy1 Dy1 94.29(4) . 2_755 ? O2 Dy1 Dy1 119.82(5) . 2_755 ? O10 Dy1 Dy1 101.71(4) . 2_755 ? O9 Dy1 Dy1 34.08(4) . 2_755 ? O9 Dy1 Dy1 32.80(4) 2_755 2_755 ? O12 Dy1 Dy1 80.22(4) 2_755 2_755 ? C1 O1 Dy1 134.78(18) . . ? C3 O2 Dy1 134.08(18) . . ? C3 O3 C30 117.5(2) . . ? C1 O4 C40 117.4(2) . . ? C4 O5 Dy1 132.10(17) . . ? C6 O6 Dy1 133.28(18) . . ? C6 O7 C70 116.0(2) . . ? C4 O8 C80 116.8(2) . . ? C7 O9 Dy1 132.90(17) . . ? C7 O9 Dy1 110.40(16) . 2_755 ? Dy1 O9 Dy1 113.12(7) . 2_755 ? C9 O10 Dy1 132.56(17) . . ? C9 O11 C110 115.8(2) . . ? C7 O12 C120 119.1(2) . . ? C7 O12 Dy1 86.97(14) . 2_755 ? C120 O12 Dy1 141.42(16) . 2_755 ? O6 C6 O7 118.4(2) . . ? O6 C6 C5 126.9(3) . . ? O7 C6 C5 114.7(2) . . ? C4 C5 C6 121.7(3) . . ? C4 C5 H5A 119.2 . . ? C6 C5 H5A 119.2 . . ? O7 C70 H70A 109.5 . . ? O7 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? O7 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? O5 C4 O8 118.9(2) . . ? O5 C4 C5 127.7(3) . . ? O8 C4 C5 113.4(2) . . ? C7 C8 C9 121.1(3) . . ? C7 C8 H8A 119.5 . . ? C9 C8 H8A 119.5 . . ? O9 C7 O12 109.5(2) . . ? O9 C7 C8 127.9(3) . . ? O12 C7 C8 122.6(2) . . ? O10 C9 O11 120.3(2) . . ? O10 C9 C8 126.7(3) . . ? O11 C9 C8 113.1(2) . . ? O2 C3 O3 118.9(2) . . ? O2 C3 C2 127.3(3) . . ? O3 C3 C2 113.8(2) . . ? O1 C1 O4 118.3(3) . . ? O1 C1 C2 127.5(3) . . ? O4 C1 C2 114.2(3) . . ? O12 C120 H12A 109.5 . . ? O12 C120 H12B 109.5 . . ? H12A C120 H12B 109.5 . . ? O12 C120 H12C 109.5 . . ? H12A C120 H12C 109.5 . . ? H12B C120 H12C 109.5 . . ? O8 C80 H80A 109.5 . . ? O8 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? O8 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? O4 C40 H40A 109.5 . . ? O4 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? O4 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O11 C110 H11A 109.5 . . ? O11 C110 H11B 109.5 . . ? H11A C110 H11B 109.5 . . ? O11 C110 H11C 109.5 . . ? H11A C110 H11C 109.5 . . ? H11B C110 H11C 109.5 . . ? C3 C2 C1 121.3(3) . . ? C3 C2 H2A 119.3 . . ? C1 C2 H2A 119.3 . . ? O3 C30 H30A 109.5 . . ? O3 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? O3 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C92 C91 C96 120.0 . . ? C92 C91 C97 119.7(5) . . ? C96 C91 C97 120.3(5) . . ? C93 C92 C91 120.0 . . ? C93 C92 H92A 120.0 . . ? C91 C92 H92A 120.0 . . ? C92 C93 C94 120.0 . . ? C92 C93 H93A 120.0 . . ? C94 C93 H93A 120.0 . . ? C95 C94 C93 120.0 . . ? C95 C94 H94A 120.0 . . ? C93 C94 H94A 120.0 . . ? C96 C95 C94 120.0 . . ? C96 C95 H95A 120.0 . . ? C94 C95 H95A 120.0 . . ? C95 C96 C91 120.0 . . ? C95 C96 H96A 120.0 . . ? C91 C96 H96A 120.0 . . ? C91 C97 H97A 109.5 . . ? C91 C97 H97B 109.5 . . ? H97A C97 H97B 109.5 . . ? C91 C97 H97C 109.5 . . ? H97A C97 H97C 109.5 . . ? H97B C97 H97C 109.5 . . ? 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 O6 Dy1 O1 C1 -75.9(3) . . . . ? O5 Dy1 O1 C1 -144.8(2) . . . . ? O2 Dy1 O1 C1 5.6(3) . . . . ? O10 Dy1 O1 C1 34.6(3) . . . . ? O9 Dy1 O1 C1 98.2(3) . . . . ? O9 Dy1 O1 C1 163.7(3) 2_755 . . . ? O12 Dy1 O1 C1 -146.1(3) 2_755 . . . ? Dy1 Dy1 O1 C1 130.7(3) 2_755 . . . ? O6 Dy1 O2 C3 83.8(2) . . . . ? O1 Dy1 O2 C3 -9.6(2) . . . . ? O5 Dy1 O2 C3 142.2(2) . . . . ? O10 Dy1 O2 C3 -171.5(3) . . . . ? O9 Dy1 O2 C3 -99.6(2) . . . . ? O9 Dy1 O2 C3 -43.6(3) 2_755 . . . ? O12 Dy1 O2 C3 29.0(3) 2_755 . . . ? Dy1 Dy1 O2 C3 -77.8(2) 2_755 . . . ? O6 Dy1 O5 C4 -11.9(2) . . . . ? O1 Dy1 O5 C4 62.2(3) . . . . ? O2 Dy1 O5 C4 -72.4(2) . . . . ? O10 Dy1 O5 C4 -117.3(2) . . . . ? O9 Dy1 O5 C4 174.1(2) . . . . ? O9 Dy1 O5 C4 111.3(2) 2_755 . . . ? O12 Dy1 O5 C4 63.6(2) 2_755 . . . ? Dy1 Dy1 O5 C4 141.6(2) 2_755 . . . ? O1 Dy1 O6 C6 -124.9(2) . . . . ? O5 Dy1 O6 C6 17.2(2) . . . . ? O2 Dy1 O6 C6 161.2(2) . . . . ? O10 Dy1 O6 C6 90.9(2) . . . . ? O9 Dy1 O6 C6 127.9(6) . . . . ? O9 Dy1 O6 C6 -54.3(2) 2_755 . . . ? O12 Dy1 O6 C6 -56.5(2) 2_755 . . . ? Dy1 Dy1 O6 C6 -54.6(3) 2_755 . . . ? O6 Dy1 O9 C7 -26.0(7) . . . . ? O1 Dy1 O9 C7 -133.2(2) . . . . ? O5 Dy1 O9 C7 83.1(2) . . . . ? O2 Dy1 O9 C7 -59.0(2) . . . . ? O10 Dy1 O9 C7 11.9(2) . . . . ? O9 Dy1 O9 C7 156.1(3) 2_755 . . . ? O12 Dy1 O9 C7 158.6(2) 2_755 . . . ? Dy1 Dy1 O9 C7 156.1(3) 2_755 . . . ? O6 Dy1 O9 Dy1 177.9(6) . . . 2_755 ? O1 Dy1 O9 Dy1 70.65(8) . . . 2_755 ? O5 Dy1 O9 Dy1 -73.01(8) . . . 2_755 ? O2 Dy1 O9 Dy1 144.90(8) . . . 2_755 ? O10 Dy1 O9 Dy1 -144.20(9) . . . 2_755 ? O9 Dy1 O9 Dy1 0.0 2_755 . . 2_755 ? O12 Dy1 O9 Dy1 2.52(9) 2_755 . . 2_755 ? O6 Dy1 O10 C9 150.8(2) . . . . ? O1 Dy1 O10 C9 43.8(3) . . . . ? O5 Dy1 O10 C9 -136.7(2) . . . . ? O2 Dy1 O10 C9 73.0(2) . . . . ? O9 Dy1 O10 C9 -25.3(2) . . . . ? O9 Dy1 O10 C9 -67.8(3) 2_755 . . . ? O12 Dy1 O10 C9 -135.1(2) 2_755 . . . ? Dy1 Dy1 O10 C9 -44.9(2) 2_755 . . . ? Dy1 O6 C6 O7 160.12(15) . . . . ? Dy1 O6 C6 C5 -19.1(4) . . . . ? C70 O7 C6 O6 1.0(3) . . . . ? C70 O7 C6 C5 -179.7(3) . . . . ? O6 C6 C5 C4 6.9(4) . . . . ? O7 C6 C5 C4 -172.3(2) . . . . ? Dy1 O5 C4 O8 -169.93(16) . . . . ? Dy1 O5 C4 C5 8.4(4) . . . . ? C80 O8 C4 O5 5.8(4) . . . . ? C80 O8 C4 C5 -172.7(2) . . . . ? C6 C5 C4 O5 -1.8(4) . . . . ? C6 C5 C4 O8 176.6(2) . . . . ? Dy1 O9 C7 O12 177.70(15) . . . . ? Dy1 O9 C7 O12 -25.7(2) 2_755 . . . ? Dy1 O9 C7 C8 -1.6(4) . . . . ? Dy1 O9 C7 C8 154.9(2) 2_755 . . . ? C120 O12 C7 O9 170.1(2) . . . . ? Dy1 O12 C7 O9 20.10(19) 2_755 . . . ? C120 O12 C7 C8 -10.5(4) . . . . ? Dy1 O12 C7 C8 -160.5(3) 2_755 . . . ? C9 C8 C7 O9 -5.9(4) . . . . ? C9 C8 C7 O12 174.8(2) . . . . ? Dy1 O10 C9 O11 -151.98(18) . . . . ? Dy1 O10 C9 C8 29.3(4) . . . . ? C110 O11 C9 O10 6.2(4) . . . . ? C110 O11 C9 C8 -174.9(2) . . . . ? C7 C8 C9 O10 -7.9(4) . . . . ? C7 C8 C9 O11 173.2(2) . . . . ? Dy1 O2 C3 O3 -172.49(16) . . . . ? Dy1 O2 C3 C2 9.2(4) . . . . ? C30 O3 C3 O2 -4.0(4) . . . . ? C30 O3 C3 C2 174.5(2) . . . . ? Dy1 O1 C1 O4 -179.75(17) . . . . ? Dy1 O1 C1 C2 -0.9(5) . . . . ? C40 O4 C1 O1 3.3(4) . . . . ? C40 O4 C1 C2 -175.6(3) . . . . ? O2 C3 C2 C1 0.0(5) . . . . ? O3 C3 C2 C1 -178.4(3) . . . . ? O1 C1 C2 C3 -4.2(5) . . . . ? O4 C1 C2 C3 174.6(3) . . . . ? C96 C91 C92 C93 0.0 . . . . ? C97 C91 C92 C93 -179.4(7) . . . . ? C91 C92 C93 C94 0.0 . . . . ? C92 C93 C94 C95 0.0 . . . . ? C93 C94 C95 C96 0.0 . . . . ? C94 C95 C96 C91 0.0 . . . . ? C92 C91 C96 C95 0.0 . . . . ? C97 C91 C96 C95 179.4(7) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.59 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 2.096 _refine_diff_density_min -0.689 _refine_diff_density_rms 0.111 #=================================END data_cvd267 _database_code_depnum_ccdc_archive 'CCDC 770258' #TrackingRef '- combined cif files.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H66 Dy2 O24' _chemical_formula_weight 1279.95 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' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.6306(3) _cell_length_b 13.6562(2) _cell_length_c 14.2430(3) _cell_angle_alpha 86.873(2) _cell_angle_beta 86.606(2) _cell_angle_gamma 81.801(2) _cell_volume 2616.67(9) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 13341 _cell_measurement_theta_min 2.674 _cell_measurement_theta_max 27.498 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.625 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1284 _exptl_absorpt_coefficient_mu 2.912 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.420 _exptl_absorpt_correction_T_max 0.555 _exptl_absorpt_process_details abspack _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Sapphire2-CCD, Oxford Diffraction' _diffrn_measurement_method '887 images at 1.0 deg. in \w and 17 sec.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28755 _diffrn_reflns_av_R_equivalents 0.0439 _diffrn_reflns_av_sigmaI/netI 0.0621 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9156 _reflns_number_gt 6237 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD 171_33_34d, Oxford Diffraction' _computing_cell_refinement 'CrysAlis RED 171_33_34d, Oxford Diffraction' _computing_data_reduction 'CrysAlis RED 171_33_34d, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0254P)^2^+1.2139P] 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 9156 _refine_ls_number_parameters 613 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0677 _refine_ls_R_factor_gt 0.0321 _refine_ls_wR_factor_ref 0.0679 _refine_ls_wR_factor_gt 0.0588 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.019074(18) 0.391049(17) 0.095506(18) 0.01490(8) Uani 1 1 d . . . Dy2 Dy 0.476029(18) 0.106632(17) -0.409260(18) 0.01412(8) Uani 1 1 d . . . C110 C 0.0714(4) 0.1885(3) -0.1156(4) 0.0130(11) Uani 1 1 d U . . H11A H 0.1439 0.1794 -0.1302 0.017 Uiso 1 1 calc R . . H11B H 0.0381 0.1867 -0.1753 0.017 Uiso 1 1 calc R . . O3 O -0.0414(2) 0.0965(2) 0.2150(3) 0.0196(9) Uani 1 1 d . . . O16 O 0.1433(2) 0.1658(3) -0.3531(3) 0.0215(9) Uani 1 1 d . . . O15 O 0.3354(2) -0.0652(2) -0.1713(3) 0.0204(9) Uani 1 1 d . . . O4 O -0.2726(2) 0.2971(2) 0.0427(3) 0.0211(9) Uani 1 1 d . . . O13 O 0.3063(3) 0.1475(2) -0.3950(3) 0.0193(9) Uani 1 1 d . . . O12 O -0.1558(3) 0.5377(2) 0.3405(3) 0.0247(9) Uani 1 1 d . . . O11 O 0.0419(3) 0.2830(2) -0.0761(2) 0.0174(8) Uani 1 1 d . . . O17 O 0.4696(2) 0.2602(2) -0.3558(3) 0.0187(8) Uani 1 1 d . . . O20 O 0.4968(3) 0.4125(3) -0.3264(3) 0.0358(11) Uani 1 1 d . . . O14 O 0.4204(2) 0.0104(2) -0.2866(3) 0.0187(8) Uani 1 1 d . . . O5 O 0.1784(3) 0.3219(2) 0.0583(3) 0.0213(9) Uani 1 1 d . . . O6 O 0.1188(3) 0.4571(2) 0.1916(3) 0.0201(8) Uani 1 1 d . . . O7 O 0.2441(3) 0.5109(3) 0.2599(3) 0.0285(10) Uani 1 1 d . . . O24 O 0.6962(3) -0.0121(3) -0.1957(3) 0.0220(9) Uani 1 1 d . . . O18 O 0.5997(2) 0.1712(2) -0.4951(2) 0.0184(8) Uani 1 1 d . . . O8 O 0.3433(3) 0.2783(3) 0.0395(3) 0.0314(10) Uani 1 1 d . . . O19 O 0.7201(3) 0.2598(3) -0.5443(3) 0.0329(11) Uani 1 1 d . . . C10 C 0.2379(4) 0.1210(4) -0.3408(4) 0.0172(12) Uani 1 1 d . . . C3 C -0.0603(4) 0.1858(4) 0.1684(4) 0.0166(12) Uani 1 1 d . . . C12 C 0.3385(4) 0.0003(4) -0.2458(4) 0.0170(12) Uani 1 1 d . . . C7 C 0.0584(4) 0.3694(4) -0.1208(4) 0.0169(12) Uani 1 1 d . . . C4 C 0.2630(4) 0.3319(4) 0.0828(4) 0.0208(13) Uani 1 1 d . . . C9 C -0.1099(4) 0.5300(4) 0.2541(4) 0.0185(12) Uani 1 1 d . . . C230 C 0.3443(4) 0.2967(4) -0.6160(4) 0.0224(13) Uani 1 1 d . . . H23A H 0.2722 0.2942 -0.6174 0.027 Uiso 1 1 calc R . . H23B H 0.3715 0.3056 -0.6814 0.027 Uiso 1 1 calc R . . C18 C 0.3921(4) 0.1186(4) -0.6077(4) 0.0159(12) Uani 1 1 d . . . C5 C 0.2852(4) 0.3941(4) 0.1492(4) 0.0183(12) Uani 1 1 d . . . H5A H 0.3526 0.3964 0.1611 0.022 Uiso 1 1 calc R . . C8 C -0.0979(4) 0.6241(4) 0.2103(4) 0.0175(12) Uani 1 1 d . . . H8A H -0.1177 0.6826 0.2438 0.021 Uiso 1 1 calc R . . C1 C -0.1809(4) 0.2902(4) 0.0756(4) 0.0153(12) Uani 1 1 d . . . C30 C 0.0529(4) 0.0754(4) 0.2573(4) 0.0237(13) Uani 1 1 d . . . H30A H 0.0549 0.1190 0.3103 0.028 Uiso 1 1 calc R . . H30B H 0.1072 0.0869 0.2104 0.028 Uiso 1 1 calc R . . C11 C 0.2462(4) 0.0509(4) -0.2675(4) 0.0175(12) Uani 1 1 d . . . H11C H 0.1884 0.0371 -0.2314 0.021 Uiso 1 1 calc R . . C160 C 0.1275(4) 0.2352(4) -0.4328(4) 0.0247(13) Uani 1 1 d . . . H16A H 0.1846 0.2727 -0.4426 0.030 Uiso 1 1 calc R . . H16B H 0.0672 0.2830 -0.4197 0.030 Uiso 1 1 calc R . . C16 C 0.6488(4) -0.0107(4) -0.2753(4) 0.0172(12) Uani 1 1 d . . . C2 C -0.1524(4) 0.2044(4) 0.1304(4) 0.0198(12) Uani 1 1 d U . . H2A H -0.1974 0.1575 0.1419 0.024 Uiso 1 1 calc R . . C17 C 0.3477(4) 0.1061(4) -0.6886(4) 0.0164(12) Uani 1 1 d . . . H17A H 0.3137 0.1621 -0.7213 0.020 Uiso 1 1 calc R . . C150 C 0.4258(4) -0.1297(4) -0.1505(4) 0.0264(14) Uani 1 1 d . . . H15A H 0.4230 -0.1523 -0.0833 0.032 Uiso 1 1 calc R . . H15B H 0.4831 -0.0927 -0.1618 0.032 Uiso 1 1 calc R . . C240 C 0.6929(4) 0.0829(4) -0.1533(4) 0.0253(14) Uani 1 1 d . . . H24A H 0.6234 0.1110 -0.1370 0.030 Uiso 1 1 calc R . . H24B H 0.7224 0.1301 -0.1979 0.030 Uiso 1 1 calc R . . C120 C -0.1722(4) 0.4457(4) 0.3904(4) 0.0249(14) Uani 1 1 d . . . H12A H -0.1925 0.4003 0.3456 0.030 Uiso 1 1 calc R . . H12B H -0.2269 0.4591 0.4389 0.030 Uiso 1 1 calc R . . C15 C 0.6384(4) 0.2479(4) -0.4900(4) 0.0233(13) Uani 1 1 d . . . C14 C 0.6052(4) 0.3268(4) -0.4324(4) 0.0282(14) Uani 1 1 d . . . H14A H 0.6410 0.3818 -0.4351 0.034 Uiso 1 1 calc R . . C6 C 0.2109(4) 0.4534(4) 0.1990(4) 0.0205(13) Uani 1 1 d . . . C190 C 0.7625(4) 0.1775(4) -0.6002(4) 0.0287(14) Uani 1 1 d . . . H19A H 0.8040 0.2017 -0.6535 0.034 Uiso 1 1 calc R . . H19B H 0.7086 0.1478 -0.6265 0.034 Uiso 1 1 calc R . . C13 C 0.5223(4) 0.3277(4) -0.3716(4) 0.0260(14) Uani 1 1 d . . . C111 C 0.0466(4) 0.1088(4) -0.0526(4) 0.0269(14) Uani 1 1 d . . . H11D H 0.0679 0.0455 -0.0821 0.040 Uiso 1 1 calc R . . H11E H -0.0253 0.1169 -0.0390 0.040 Uiso 1 1 calc R . . H11F H 0.0804 0.1096 0.0061 0.040 Uiso 1 1 calc R . . C241 C 0.7505(5) 0.0654(5) -0.0670(4) 0.0365(16) Uani 1 1 d . . . H24C H 0.7497 0.1283 -0.0367 0.055 Uiso 1 1 calc R . . H24D H 0.8191 0.0378 -0.0841 0.055 Uiso 1 1 calc R . . H24E H 0.7205 0.0188 -0.0234 0.055 Uiso 1 1 calc R . . C151 C 0.4400(4) -0.2184(4) -0.2111(4) 0.0312(15) Uani 1 1 d . . . H15C H 0.5016 -0.2611 -0.1959 0.047 Uiso 1 1 calc R . . H15D H 0.4438 -0.1960 -0.2776 0.047 Uiso 1 1 calc R . . H15E H 0.3838 -0.2556 -0.1992 0.047 Uiso 1 1 calc R . . C40 C -0.3056(4) 0.3838(4) -0.0160(4) 0.0260(14) Uani 1 1 d . . . H40A H -0.2567 0.3914 -0.0692 0.031 Uiso 1 1 calc R . . H40B H -0.3131 0.4440 0.0211 0.031 Uiso 1 1 calc R . . C80 C 0.3218(4) 0.2169(5) -0.0343(5) 0.0383(17) Uani 1 1 d . . . H80A H 0.2895 0.2587 -0.0859 0.046 Uiso 1 1 calc R . . H80B H 0.2763 0.1702 -0.0092 0.046 Uiso 1 1 calc R . . C70 C 0.1725(4) 0.5802(4) 0.3105(4) 0.0311(15) Uani 1 1 d . . . H70A H 0.1944 0.5856 0.3748 0.037 Uiso 1 1 calc R . . H70B H 0.1075 0.5553 0.3161 0.037 Uiso 1 1 calc R . . C231 C 0.3632(5) 0.3805(4) -0.5579(5) 0.0382(17) Uani 1 1 d . . . H23C H 0.3311 0.4434 -0.5854 0.057 Uiso 1 1 calc R . . H23D H 0.4348 0.3819 -0.5571 0.057 Uiso 1 1 calc R . . H23E H 0.3360 0.3706 -0.4934 0.057 Uiso 1 1 calc R . . C191 C 0.8243(4) 0.1005(4) -0.5430(5) 0.0382(17) Uani 1 1 d . . . H19C H 0.8520 0.0458 -0.5826 0.057 Uiso 1 1 calc R . . H19D H 0.7830 0.0756 -0.4909 0.057 Uiso 1 1 calc R . . H19E H 0.8784 0.1294 -0.5177 0.057 Uiso 1 1 calc R . . C161 C 0.1159(4) 0.1829(4) -0.5202(4) 0.0313(15) Uani 1 1 d . . . H16C H 0.1053 0.2315 -0.5731 0.047 Uiso 1 1 calc R . . H16D H 0.0587 0.1466 -0.5109 0.047 Uiso 1 1 calc R . . H16E H 0.1760 0.1363 -0.5338 0.047 Uiso 1 1 calc R . . C31 C 0.0651(4) -0.0316(4) 0.2922(4) 0.0309(15) Uani 1 1 d . . . H31A H 0.1289 -0.0485 0.3216 0.046 Uiso 1 1 calc R . . H31B H 0.0632 -0.0739 0.2392 0.046 Uiso 1 1 calc R . . H31C H 0.0111 -0.0420 0.3386 0.046 Uiso 1 1 calc R . . C201 C 0.3880(5) 0.5260(4) -0.2376(5) 0.0463(19) Uani 1 1 d . . . H20A H 0.3276 0.5351 -0.1963 0.069 Uiso 1 1 calc R . . H20B H 0.3792 0.5706 -0.2937 0.069 Uiso 1 1 calc R . . H20C H 0.4442 0.5412 -0.2038 0.069 Uiso 1 1 calc R . . C121 C -0.0806(4) 0.3964(4) 0.4368(5) 0.0363(16) Uani 1 1 d . . . H12C H -0.0944 0.3346 0.4698 0.055 Uiso 1 1 calc R . . H12D H -0.0610 0.4407 0.4821 0.055 Uiso 1 1 calc R . . H12E H -0.0266 0.3819 0.3889 0.055 Uiso 1 1 calc R . . C71 C 0.1612(5) 0.6804(4) 0.2604(5) 0.0477(19) Uani 1 1 d . . . H71A H 0.1125 0.7261 0.2958 0.072 Uiso 1 1 calc R . . H71B H 0.1385 0.6752 0.1971 0.072 Uiso 1 1 calc R . . H71C H 0.2253 0.7054 0.2557 0.072 Uiso 1 1 calc R . . C200 C 0.4081(4) 0.4203(4) -0.2667(5) 0.0367(16) Uani 1 1 d . . . H20D H 0.4173 0.3744 -0.2107 0.044 Uiso 1 1 calc R . . H20E H 0.3520 0.4039 -0.3010 0.044 Uiso 1 1 calc R . . C41 C -0.4034(5) 0.3697(5) -0.0520(5) 0.050(2) Uani 1 1 d . . . H41A H -0.4281 0.4274 -0.0922 0.075 Uiso 1 1 calc R . . H41B H -0.4511 0.3624 0.0013 0.075 Uiso 1 1 calc R . . H41C H -0.3950 0.3100 -0.0885 0.075 Uiso 1 1 calc R . . O9 O 0.0328(2) 0.4408(2) -0.0650(2) 0.0173(8) Uani 1 1 d . . . O1 O -0.1315(2) 0.3593(2) 0.0541(2) 0.0167(8) Uani 1 1 d . . . O2 O 0.0060(2) 0.2418(2) 0.1645(2) 0.0164(8) Uani 1 1 d . . . O21 O 0.6072(2) 0.0691(2) -0.3092(3) 0.0183(8) Uani 1 1 d . . . O10 O -0.0861(2) 0.4479(2) 0.2221(2) 0.0180(8) Uani 1 1 d . . . O22 O 0.4385(2) 0.0500(2) -0.5552(2) 0.0153(8) Uani 1 1 d . . . O23 O 0.3935(2) 0.2070(2) -0.5716(2) 0.0182(8) Uani 1 1 d . . . C81 C 0.4164(5) 0.1618(5) -0.0695(6) 0.056(2) Uani 1 1 d . . . H81A H 0.4040 0.1195 -0.1197 0.084 Uiso 1 1 calc R . . H81B H 0.4475 0.1206 -0.0179 0.084 Uiso 1 1 calc R . . H81C H 0.4608 0.2087 -0.0944 0.084 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.01556(15) 0.01198(14) 0.01733(16) -0.00125(11) 0.00056(12) -0.00284(11) Dy2 0.01395(15) 0.01215(14) 0.01607(16) -0.00126(11) 0.00086(11) -0.00168(11) C110 0.0113(14) 0.0112(14) 0.0170(14) -0.0054(9) -0.0026(9) -0.0011(9) O3 0.019(2) 0.017(2) 0.023(2) 0.0047(16) -0.0034(17) -0.0028(16) O16 0.013(2) 0.027(2) 0.021(2) 0.0006(17) 0.0002(16) 0.0061(16) O15 0.019(2) 0.021(2) 0.020(2) 0.0066(16) 0.0018(16) -0.0021(16) O4 0.018(2) 0.021(2) 0.025(2) 0.0087(17) -0.0069(17) -0.0049(16) O13 0.017(2) 0.019(2) 0.021(2) 0.0031(16) 0.0004(17) -0.0006(16) O12 0.034(2) 0.019(2) 0.019(2) 0.0005(16) 0.0121(18) -0.0021(17) O11 0.028(2) 0.0083(18) 0.016(2) -0.0025(15) 0.0030(16) -0.0046(15) O17 0.017(2) 0.0131(19) 0.026(2) -0.0029(16) -0.0002(16) -0.0003(16) O20 0.029(2) 0.021(2) 0.059(3) -0.020(2) 0.002(2) -0.0022(18) O14 0.016(2) 0.019(2) 0.021(2) 0.0037(16) -0.0004(16) -0.0030(16) O5 0.017(2) 0.020(2) 0.027(2) -0.0059(17) 0.0010(17) -0.0024(16) O6 0.021(2) 0.020(2) 0.019(2) -0.0039(16) -0.0057(17) 0.0006(16) O7 0.028(2) 0.032(2) 0.027(2) -0.0135(19) -0.0109(19) 0.0006(18) O24 0.022(2) 0.023(2) 0.021(2) -0.0058(17) -0.0084(17) 0.0019(16) O18 0.019(2) 0.0155(19) 0.021(2) 0.0008(16) 0.0039(16) -0.0070(16) O8 0.016(2) 0.035(2) 0.043(3) -0.017(2) 0.0012(19) 0.0017(18) O19 0.028(2) 0.022(2) 0.050(3) -0.0018(19) 0.015(2) -0.0114(18) C10 0.015(3) 0.019(3) 0.018(3) -0.013(2) 0.000(2) 0.001(2) C3 0.022(3) 0.016(3) 0.010(3) -0.002(2) 0.003(2) 0.000(2) C12 0.024(3) 0.015(3) 0.013(3) -0.006(2) 0.003(2) -0.006(2) C7 0.017(3) 0.011(3) 0.023(3) -0.001(2) -0.003(2) -0.004(2) C4 0.021(3) 0.019(3) 0.022(3) 0.003(2) 0.001(3) -0.003(2) C9 0.016(3) 0.022(3) 0.016(3) -0.002(2) -0.001(2) 0.003(2) C230 0.025(3) 0.013(3) 0.028(3) 0.005(2) -0.007(3) 0.001(2) C18 0.012(3) 0.018(3) 0.017(3) -0.004(2) 0.008(2) -0.003(2) C5 0.014(3) 0.017(3) 0.024(3) 0.001(2) -0.005(2) 0.000(2) C8 0.018(3) 0.016(3) 0.017(3) -0.002(2) 0.000(2) 0.002(2) C1 0.010(3) 0.021(3) 0.015(3) -0.006(2) 0.002(2) -0.004(2) C30 0.024(3) 0.025(3) 0.022(3) 0.002(3) -0.007(3) -0.001(3) C11 0.013(3) 0.024(3) 0.015(3) -0.003(2) 0.006(2) -0.002(2) C160 0.024(3) 0.022(3) 0.026(4) -0.002(3) -0.007(3) 0.007(2) C16 0.009(3) 0.026(3) 0.017(3) -0.002(2) -0.001(2) -0.004(2) C2 0.0195(15) 0.0200(15) 0.0202(15) -0.0004(10) -0.0008(10) -0.0037(10) C17 0.013(3) 0.018(3) 0.016(3) -0.001(2) -0.002(2) 0.003(2) C150 0.022(3) 0.033(3) 0.022(3) 0.014(3) -0.004(3) -0.003(3) C240 0.024(3) 0.022(3) 0.030(4) -0.013(3) -0.006(3) 0.002(2) C120 0.029(3) 0.018(3) 0.025(3) 0.004(2) 0.010(3) -0.001(3) C15 0.018(3) 0.022(3) 0.028(4) 0.006(3) -0.002(3) 0.000(2) C14 0.024(3) 0.018(3) 0.046(4) -0.008(3) 0.000(3) -0.011(2) C6 0.028(3) 0.021(3) 0.012(3) 0.005(2) -0.008(2) -0.004(3) C190 0.021(3) 0.036(4) 0.029(4) -0.003(3) 0.010(3) -0.009(3) C13 0.026(3) 0.021(3) 0.032(4) -0.009(3) -0.011(3) 0.003(3) C111 0.049(4) 0.005(3) 0.027(4) 0.001(2) 0.006(3) -0.006(3) C241 0.041(4) 0.038(4) 0.031(4) -0.015(3) -0.012(3) 0.005(3) C151 0.023(3) 0.026(3) 0.042(4) 0.005(3) 0.006(3) -0.001(3) C40 0.025(3) 0.024(3) 0.028(4) 0.008(3) -0.009(3) -0.003(3) C80 0.020(3) 0.044(4) 0.054(5) -0.030(3) -0.002(3) -0.004(3) C70 0.036(4) 0.031(3) 0.027(4) -0.015(3) -0.006(3) -0.002(3) C231 0.059(5) 0.017(3) 0.037(4) -0.002(3) -0.019(3) 0.006(3) C191 0.022(3) 0.041(4) 0.050(5) -0.012(3) 0.003(3) 0.003(3) C161 0.026(3) 0.036(4) 0.031(4) -0.003(3) -0.004(3) 0.002(3) C31 0.024(3) 0.027(3) 0.041(4) 0.012(3) -0.001(3) -0.004(3) C201 0.048(4) 0.035(4) 0.056(5) -0.028(3) -0.015(4) 0.010(3) C121 0.042(4) 0.033(4) 0.034(4) 0.010(3) -0.005(3) -0.008(3) C71 0.040(4) 0.033(4) 0.069(6) -0.006(4) 0.001(4) -0.002(3) C200 0.032(4) 0.034(4) 0.043(4) -0.020(3) -0.003(3) 0.004(3) C41 0.041(4) 0.042(4) 0.069(6) 0.023(4) -0.027(4) -0.010(3) O9 0.023(2) 0.0096(18) 0.018(2) -0.0041(16) 0.0029(16) -0.0015(15) O1 0.017(2) 0.0139(19) 0.020(2) 0.0021(15) -0.0007(16) -0.0039(15) O2 0.0143(19) 0.0132(18) 0.022(2) -0.0004(15) -0.0018(16) -0.0031(15) O21 0.018(2) 0.0142(19) 0.024(2) -0.0014(16) -0.0036(16) -0.0024(16) O10 0.020(2) 0.017(2) 0.017(2) -0.0032(16) 0.0040(16) -0.0029(16) O22 0.0163(19) 0.0125(18) 0.016(2) 0.0007(15) -0.0012(16) 0.0020(15) O23 0.024(2) 0.0115(18) 0.017(2) 0.0005(15) -0.0053(16) 0.0021(15) C81 0.038(4) 0.063(5) 0.068(6) -0.037(4) -0.003(4) 0.006(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O2 2.240(3) . ? Dy1 O1 2.274(3) . ? Dy1 O5 2.285(3) . ? Dy1 O6 2.289(4) . ? Dy1 O9 2.329(3) 2_565 ? Dy1 O10 2.332(3) . ? Dy1 O9 2.354(3) . ? Dy1 O11 2.902(3) . ? Dy1 Dy1 3.9204(5) 2_565 ? Dy2 O17 2.258(3) . ? Dy2 O18 2.275(3) . ? Dy2 O14 2.287(3) . ? Dy2 O13 2.301(3) . ? Dy2 O21 2.334(3) . ? Dy2 O22 2.351(3) 2_654 ? Dy2 O22 2.365(3) . ? Dy2 O23 2.830(3) . ? Dy2 Dy2 3.9584(5) 2_654 ? C110 O11 1.431(5) . ? C110 C111 1.437(7) . ? C110 H11A 0.9900 . ? C110 H11B 0.9900 . ? O3 C3 1.354(6) . ? O3 C30 1.437(6) . ? O16 C10 1.363(6) . ? O16 C160 1.444(6) . ? O15 C12 1.353(6) . ? O15 C150 1.445(6) . ? O4 C1 1.349(6) . ? O4 C40 1.445(6) . ? O13 C10 1.255(6) . ? O12 C9 1.350(6) . ? O12 C120 1.449(6) . ? O11 C7 1.351(6) . ? O17 C13 1.251(6) . ? O20 C13 1.347(6) . ? O20 C200 1.431(7) . ? O14 C12 1.250(6) . ? O5 C4 1.252(6) . ? O6 C6 1.260(6) . ? O7 C6 1.340(6) . ? O7 C70 1.448(6) . ? O24 C16 1.337(6) . ? O24 C240 1.454(6) . ? O18 C15 1.245(6) . ? O8 C4 1.363(6) . ? O8 C80 1.448(7) . ? O19 C15 1.341(6) . ? O19 C190 1.446(7) . ? C10 C11 1.376(7) . ? C3 O2 1.262(6) . ? C3 C2 1.381(7) . ? C12 C11 1.390(7) . ? C7 O9 1.288(6) . ? C7 C8 1.357(7) 2_565 ? C4 C5 1.379(8) . ? C9 O10 1.227(6) . ? C9 C8 1.424(7) . ? C230 O23 1.443(6) . ? C230 C231 1.507(8) . ? C230 H23A 0.9900 . ? C230 H23B 0.9900 . ? C18 O22 1.284(6) . ? C18 O23 1.342(6) . ? C18 C17 1.362(7) . ? C5 C6 1.389(7) . ? C5 H5A 0.9500 . ? C8 C7 1.357(7) 2_565 ? C8 H8A 0.9500 . ? C1 O1 1.251(6) . ? C1 C2 1.393(7) . ? C30 C31 1.508(7) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C11 H11C 0.9500 . ? C160 C161 1.495(8) . ? C160 H16A 0.9900 . ? C160 H16B 0.9900 . ? C16 O21 1.241(6) . ? C16 C17 1.420(7) 2_654 ? C2 H2A 0.9500 . ? C17 C16 1.420(7) 2_654 ? C17 H17A 0.9500 . ? C150 C151 1.509(8) . ? C150 H15A 0.9900 . ? C150 H15B 0.9900 . ? C240 C241 1.487(8) . ? C240 H24A 0.9900 . ? C240 H24B 0.9900 . ? C120 C121 1.503(8) . ? C120 H12A 0.9900 . ? C120 H12B 0.9900 . ? C15 C14 1.398(8) . ? C14 C13 1.381(8) . ? C14 H14A 0.9500 . ? C190 C191 1.487(8) . ? C190 H19A 0.9900 . ? C190 H19B 0.9900 . ? C111 H11D 0.9800 . ? C111 H11E 0.9800 . ? C111 H11F 0.9800 . ? C241 H24C 0.9800 . ? C241 H24D 0.9800 . ? C241 H24E 0.9800 . ? C151 H15C 0.9800 . ? C151 H15D 0.9800 . ? C151 H15E 0.9800 . ? C40 C41 1.498(8) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C80 C81 1.473(8) . ? C80 H80A 0.9900 . ? C80 H80B 0.9900 . ? C70 C71 1.501(8) . ? C70 H70A 0.9900 . ? C70 H70B 0.9900 . ? C231 H23C 0.9800 . ? C231 H23D 0.9800 . ? C231 H23E 0.9800 . ? C191 H19C 0.9800 . ? C191 H19D 0.9800 . ? C191 H19E 0.9800 . ? C161 H16C 0.9800 . ? C161 H16D 0.9800 . ? C161 H16E 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C201 C200 1.506(8) . ? C201 H20A 0.9800 . ? C201 H20B 0.9800 . ? C201 H20C 0.9800 . ? C121 H12C 0.9800 . ? C121 H12D 0.9800 . ? C121 H12E 0.9800 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C200 H20D 0.9900 . ? C200 H20E 0.9900 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? O9 Dy1 2.329(3) 2_565 ? O22 Dy2 2.351(3) 2_654 ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Dy1 O1 76.31(12) . . ? O2 Dy1 O5 83.83(12) . . ? O1 Dy1 O5 133.27(12) . . ? O2 Dy1 O6 103.46(12) . . ? O1 Dy1 O6 152.34(12) . . ? O5 Dy1 O6 73.25(13) . . ? O2 Dy1 O9 154.24(12) . 2_565 ? O1 Dy1 O9 88.94(12) . 2_565 ? O5 Dy1 O9 121.05(12) . 2_565 ? O6 Dy1 O9 79.96(12) . 2_565 ? O2 Dy1 O10 83.61(12) . . ? O1 Dy1 O10 77.29(12) . . ? O5 Dy1 O10 142.12(13) . . ? O6 Dy1 O10 75.22(12) . . ? O9 Dy1 O10 72.48(11) 2_565 . ? O2 Dy1 O9 130.34(12) . . ? O1 Dy1 O9 81.79(12) . . ? O5 Dy1 O9 79.74(12) . . ? O6 Dy1 O9 115.70(12) . . ? O9 Dy1 O9 66.32(13) 2_565 . ? O10 Dy1 O9 133.76(11) . . ? O2 Dy1 O11 83.53(11) . . ? O1 Dy1 O11 70.11(11) . . ? O5 Dy1 O11 65.88(12) . . ? O6 Dy1 O11 137.55(11) . . ? O9 Dy1 O11 111.47(11) 2_565 . ? O10 Dy1 O11 146.94(11) . . ? O9 Dy1 O11 46.99(10) . . ? O2 Dy1 Dy1 157.47(9) . 2_565 ? O1 Dy1 Dy1 84.45(8) . 2_565 ? O5 Dy1 Dy1 101.51(9) . 2_565 ? O6 Dy1 Dy1 99.02(9) . 2_565 ? O9 Dy1 Dy1 33.35(8) 2_565 2_565 ? O10 Dy1 Dy1 103.67(8) . 2_565 ? O9 Dy1 Dy1 32.96(7) . 2_565 ? O11 Dy1 Dy1 78.93(6) . 2_565 ? O17 Dy2 O18 75.98(12) . . ? O17 Dy2 O14 106.51(12) . . ? O18 Dy2 O14 151.70(12) . . ? O17 Dy2 O13 81.48(12) . . ? O18 Dy2 O13 134.27(12) . . ? O14 Dy2 O13 73.00(12) . . ? O17 Dy2 O21 83.36(12) . . ? O18 Dy2 O21 78.72(12) . . ? O14 Dy2 O21 73.69(12) . . ? O13 Dy2 O21 137.44(12) . . ? O17 Dy2 O22 152.05(12) . 2_654 ? O18 Dy2 O22 86.63(11) . 2_654 ? O14 Dy2 O22 78.96(11) . 2_654 ? O13 Dy2 O22 125.62(12) . 2_654 ? O21 Dy2 O22 71.74(12) . 2_654 ? O17 Dy2 O22 132.16(12) . . ? O18 Dy2 O22 84.40(12) . . ? O14 Dy2 O22 110.93(12) . . ? O13 Dy2 O22 82.08(12) . . ? O21 Dy2 O22 135.01(11) . . ? O22 Dy2 O22 65.85(13) 2_654 . ? O17 Dy2 O23 84.48(11) . . ? O18 Dy2 O23 72.15(11) . . ? O14 Dy2 O23 135.83(11) . . ? O13 Dy2 O23 66.45(11) . . ? O21 Dy2 O23 150.37(11) . . ? O22 Dy2 O23 111.09(11) 2_654 . ? O22 Dy2 O23 47.83(10) . . ? O17 Dy2 Dy2 157.77(9) . 2_654 ? O18 Dy2 Dy2 84.65(9) . 2_654 ? O14 Dy2 Dy2 95.72(9) . 2_654 ? O13 Dy2 Dy2 105.28(9) . 2_654 ? O21 Dy2 Dy2 103.68(8) . 2_654 ? O22 Dy2 Dy2 33.03(8) 2_654 2_654 ? O22 Dy2 Dy2 32.82(7) . 2_654 ? O23 Dy2 Dy2 79.20(7) . 2_654 ? O11 C110 C111 111.9(4) . . ? O11 C110 H11A 109.2 . . ? C111 C110 H11A 109.2 . . ? O11 C110 H11B 109.2 . . ? C111 C110 H11B 109.2 . . ? H11A C110 H11B 107.9 . . ? C3 O3 C30 116.1(4) . . ? C10 O16 C160 117.4(4) . . ? C12 O15 C150 117.7(4) . . ? C1 O4 C40 117.1(4) . . ? C10 O13 Dy2 135.5(3) . . ? C9 O12 C120 116.3(4) . . ? C7 O11 C110 123.3(4) . . ? C7 O11 Dy1 86.2(3) . . ? C110 O11 Dy1 145.3(3) . . ? C13 O17 Dy2 133.7(3) . . ? C13 O20 C200 117.2(4) . . ? C12 O14 Dy2 136.4(3) . . ? C4 O5 Dy1 136.2(3) . . ? C6 O6 Dy1 135.8(3) . . ? C6 O7 C70 118.4(4) . . ? C16 O24 C240 115.9(4) . . ? C15 O18 Dy2 133.4(3) . . ? C4 O8 C80 115.6(4) . . ? C15 O19 C190 116.8(4) . . ? O13 C10 O16 118.3(5) . . ? O13 C10 C11 127.7(5) . . ? O16 C10 C11 114.1(4) . . ? O2 C3 O3 117.9(5) . . ? O2 C3 C2 127.5(5) . . ? O3 C3 C2 114.6(5) . . ? O14 C12 O15 119.1(5) . . ? O14 C12 C11 127.1(5) . . ? O15 C12 C11 113.8(4) . . ? O9 C7 O11 109.5(4) . . ? O9 C7 C8 127.1(5) . 2_565 ? O11 C7 C8 123.4(5) . 2_565 ? O5 C4 O8 118.4(5) . . ? O5 C4 C5 126.8(5) . . ? O8 C4 C5 114.8(5) . . ? O10 C9 O12 119.5(5) . . ? O10 C9 C8 128.1(5) . . ? O12 C9 C8 112.3(4) . . ? O23 C230 C231 106.4(4) . . ? O23 C230 H23A 110.5 . . ? C231 C230 H23A 110.5 . . ? O23 C230 H23B 110.5 . . ? C231 C230 H23B 110.5 . . ? H23A C230 H23B 108.6 . . ? O22 C18 O23 109.8(5) . . ? O22 C18 C17 126.4(5) . . ? O23 C18 C17 123.7(5) . . ? C4 C5 C6 121.3(5) . . ? C4 C5 H5A 119.3 . . ? C6 C5 H5A 119.3 . . ? C7 C8 C9 120.3(5) 2_565 . ? C7 C8 H8A 119.9 2_565 . ? C9 C8 H8A 119.9 . . ? O1 C1 O4 117.9(4) . . ? O1 C1 C2 127.5(5) . . ? O4 C1 C2 114.6(4) . . ? O3 C30 C31 107.4(4) . . ? O3 C30 H30A 110.2 . . ? C31 C30 H30A 110.2 . . ? O3 C30 H30B 110.2 . . ? C31 C30 H30B 110.2 . . ? H30A C30 H30B 108.5 . . ? C10 C11 C12 120.4(5) . . ? C10 C11 H11C 119.8 . . ? C12 C11 H11C 119.8 . . ? O16 C160 C161 111.1(5) . . ? O16 C160 H16A 109.4 . . ? C161 C160 H16A 109.4 . . ? O16 C160 H16B 109.4 . . ? C161 C160 H16B 109.4 . . ? H16A C160 H16B 108.0 . . ? O21 C16 O24 119.7(5) . . ? O21 C16 C17 127.2(5) . 2_654 ? O24 C16 C17 113.1(4) . 2_654 ? C3 C2 C1 121.7(5) . . ? C3 C2 H2A 119.1 . . ? C1 C2 H2A 119.1 . . ? C18 C17 C16 121.0(5) . 2_654 ? C18 C17 H17A 119.5 . . ? C16 C17 H17A 119.5 2_654 . ? O15 C150 C151 110.8(5) . . ? O15 C150 H15A 109.5 . . ? C151 C150 H15A 109.5 . . ? O15 C150 H15B 109.5 . . ? C151 C150 H15B 109.5 . . ? H15A C150 H15B 108.1 . . ? O24 C240 C241 107.4(4) . . ? O24 C240 H24A 110.2 . . ? C241 C240 H24A 110.2 . . ? O24 C240 H24B 110.2 . . ? C241 C240 H24B 110.2 . . ? H24A C240 H24B 108.5 . . ? O12 C120 C121 111.7(5) . . ? O12 C120 H12A 109.3 . . ? C121 C120 H12A 109.3 . . ? O12 C120 H12B 109.3 . . ? C121 C120 H12B 109.3 . . ? H12A C120 H12B 107.9 . . ? O18 C15 O19 119.3(5) . . ? O18 C15 C14 126.6(5) . . ? O19 C15 C14 114.1(5) . . ? C13 C14 C15 122.4(5) . . ? C13 C14 H14A 118.8 . . ? C15 C14 H14A 118.8 . . ? O6 C6 O7 119.3(5) . . ? O6 C6 C5 126.3(5) . . ? O7 C6 C5 114.4(5) . . ? O19 C190 C191 111.3(5) . . ? O19 C190 H19A 109.4 . . ? C191 C190 H19A 109.4 . . ? O19 C190 H19B 109.4 . . ? C191 C190 H19B 109.4 . . ? H19A C190 H19B 108.0 . . ? O17 C13 O20 118.2(5) . . ? O17 C13 C14 127.3(5) . . ? O20 C13 C14 114.5(5) . . ? C110 C111 H11D 109.5 . . ? C110 C111 H11E 109.5 . . ? H11D C111 H11E 109.5 . . ? C110 C111 H11F 109.5 . . ? H11D C111 H11F 109.5 . . ? H11E C111 H11F 109.5 . . ? C240 C241 H24C 109.5 . . ? C240 C241 H24D 109.5 . . ? H24C C241 H24D 109.5 . . ? C240 C241 H24E 109.5 . . ? H24C C241 H24E 109.5 . . ? H24D C241 H24E 109.5 . . ? C150 C151 H15C 109.5 . . ? C150 C151 H15D 109.5 . . ? H15C C151 H15D 109.5 . . ? C150 C151 H15E 109.5 . . ? H15C C151 H15E 109.5 . . ? H15D C151 H15E 109.5 . . ? O4 C40 C41 107.2(4) . . ? O4 C40 H40A 110.3 . . ? C41 C40 H40A 110.3 . . ? O4 C40 H40B 110.3 . . ? C41 C40 H40B 110.3 . . ? H40A C40 H40B 108.5 . . ? O8 C80 C81 107.8(5) . . ? O8 C80 H80A 110.2 . . ? C81 C80 H80A 110.2 . . ? O8 C80 H80B 110.2 . . ? C81 C80 H80B 110.2 . . ? H80A C80 H80B 108.5 . . ? O7 C70 C71 110.8(5) . . ? O7 C70 H70A 109.5 . . ? C71 C70 H70A 109.5 . . ? O7 C70 H70B 109.5 . . ? C71 C70 H70B 109.5 . . ? H70A C70 H70B 108.1 . . ? C230 C231 H23C 109.5 . . ? C230 C231 H23D 109.5 . . ? H23C C231 H23D 109.5 . . ? C230 C231 H23E 109.5 . . ? H23C C231 H23E 109.5 . . ? H23D C231 H23E 109.5 . . ? C190 C191 H19C 109.5 . . ? C190 C191 H19D 109.5 . . ? H19C C191 H19D 109.5 . . ? C190 C191 H19E 109.5 . . ? H19C C191 H19E 109.5 . . ? H19D C191 H19E 109.5 . . ? C160 C161 H16C 109.5 . . ? C160 C161 H16D 109.5 . . ? H16C C161 H16D 109.5 . . ? C160 C161 H16E 109.5 . . ? H16C C161 H16E 109.5 . . ? H16D C161 H16E 109.5 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C200 C201 H20A 109.5 . . ? C200 C201 H20B 109.5 . . ? H20A C201 H20B 109.5 . . ? C200 C201 H20C 109.5 . . ? H20A C201 H20C 109.5 . . ? H20B C201 H20C 109.5 . . ? C120 C121 H12C 109.5 . . ? C120 C121 H12D 109.5 . . ? H12C C121 H12D 109.5 . . ? C120 C121 H12E 109.5 . . ? H12C C121 H12E 109.5 . . ? H12D C121 H12E 109.5 . . ? C70 C71 H71A 109.5 . . ? C70 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C70 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? O20 C200 C201 106.5(5) . . ? O20 C200 H20D 110.4 . . ? C201 C200 H20D 110.4 . . ? O20 C200 H20E 110.4 . . ? C201 C200 H20E 110.4 . . ? H20D C200 H20E 108.6 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C7 O9 Dy1 131.3(3) . 2_565 ? C7 O9 Dy1 114.6(3) . . ? Dy1 O9 Dy1 113.68(13) 2_565 . ? C1 O1 Dy1 132.9(3) . . ? C3 O2 Dy1 133.8(3) . . ? C16 O21 Dy2 132.1(3) . . ? C9 O10 Dy1 133.0(3) . . ? C18 O22 Dy2 131.1(3) . 2_654 ? C18 O22 Dy2 112.9(3) . . ? Dy2 O22 Dy2 114.15(13) 2_654 . ? C18 O23 C230 121.1(4) . . ? C18 O23 Dy2 88.4(3) . . ? C230 O23 Dy2 149.0(3) . . ? C80 C81 H81A 109.5 . . ? C80 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C80 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? 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 O17 Dy2 O13 C10 -109.0(5) . . . . ? O18 Dy2 O13 C10 -169.8(4) . . . . ? O14 Dy2 O13 C10 1.3(5) . . . . ? O21 Dy2 O13 C10 -38.6(5) . . . . ? O22 Dy2 O13 C10 63.5(5) 2_654 . . . ? O22 Dy2 O13 C10 116.1(5) . . . . ? O23 Dy2 O13 C10 163.3(5) . . . . ? Dy2 Dy2 O13 C10 92.7(5) 2_654 . . . ? C111 C110 O11 C7 178.9(5) . . . . ? C111 C110 O11 Dy1 34.9(7) . . . . ? O2 Dy1 O11 C7 -175.3(3) . . . . ? O1 Dy1 O11 C7 106.9(3) . . . . ? O5 Dy1 O11 C7 -89.2(3) . . . . ? O6 Dy1 O11 C7 -72.4(3) . . . . ? O9 Dy1 O11 C7 26.3(3) 2_565 . . . ? O10 Dy1 O11 C7 117.0(3) . . . . ? O9 Dy1 O11 C7 9.5(3) . . . . ? Dy1 Dy1 O11 C7 18.9(3) 2_565 . . . ? O2 Dy1 O11 C110 -24.8(5) . . . . ? O1 Dy1 O11 C110 -102.6(5) . . . . ? O5 Dy1 O11 C110 61.3(5) . . . . ? O6 Dy1 O11 C110 78.1(5) . . . . ? O9 Dy1 O11 C110 176.8(5) 2_565 . . . ? O10 Dy1 O11 C110 -92.5(5) . . . . ? O9 Dy1 O11 C110 160.0(5) . . . . ? Dy1 Dy1 O11 C110 169.4(5) 2_565 . . . ? O18 Dy2 O17 C13 -5.3(5) . . . . ? O14 Dy2 O17 C13 145.4(5) . . . . ? O13 Dy2 O17 C13 -145.2(5) . . . . ? O21 Dy2 O17 C13 74.7(5) . . . . ? O22 Dy2 O17 C13 47.8(6) 2_654 . . . ? O22 Dy2 O17 C13 -74.1(5) . . . . ? O23 Dy2 O17 C13 -78.3(5) . . . . ? Dy2 Dy2 O17 C13 -35.5(6) 2_654 . . . ? O17 Dy2 O14 C12 74.2(5) . . . . ? O18 Dy2 O14 C12 165.3(4) . . . . ? O13 Dy2 O14 C12 -1.1(5) . . . . ? O21 Dy2 O14 C12 152.0(5) . . . . ? O22 Dy2 O14 C12 -134.0(5) 2_654 . . . ? O22 Dy2 O14 C12 -75.4(5) . . . . ? O23 Dy2 O14 C12 -25.0(5) . . . . ? Dy2 Dy2 O14 C12 -105.4(5) 2_654 . . . ? O2 Dy1 O5 C4 -110.2(5) . . . . ? O1 Dy1 O5 C4 -174.8(4) . . . . ? O6 Dy1 O5 C4 -4.1(5) . . . . ? O9 Dy1 O5 C4 62.7(5) 2_565 . . . ? O10 Dy1 O5 C4 -39.0(6) . . . . ? O9 Dy1 O5 C4 116.8(5) . . . . ? O11 Dy1 O5 C4 164.1(5) . . . . ? Dy1 Dy1 O5 C4 91.9(5) 2_565 . . . ? O2 Dy1 O6 C6 85.5(5) . . . . ? O1 Dy1 O6 C6 171.7(4) . . . . ? O5 Dy1 O6 C6 6.4(5) . . . . ? O9 Dy1 O6 C6 -120.5(5) 2_565 . . . ? O10 Dy1 O6 C6 165.1(5) . . . . ? O9 Dy1 O6 C6 -63.1(5) . . . . ? O11 Dy1 O6 C6 -9.6(5) . . . . ? Dy1 Dy1 O6 C6 -93.0(5) 2_565 . . . ? O17 Dy2 O18 C15 9.2(5) . . . . ? O14 Dy2 O18 C15 -89.7(5) . . . . ? O13 Dy2 O18 C15 72.0(5) . . . . ? O21 Dy2 O18 C15 -76.7(5) . . . . ? O22 Dy2 O18 C15 -148.7(5) 2_654 . . . ? O22 Dy2 O18 C15 145.2(5) . . . . ? O23 Dy2 O18 C15 97.8(5) . . . . ? Dy2 Dy2 O18 C15 178.2(5) 2_654 . . . ? Dy2 O13 C10 O16 177.9(3) . . . . ? Dy2 O13 C10 C11 -1.2(8) . . . . ? C160 O16 C10 O13 5.0(7) . . . . ? C160 O16 C10 C11 -175.7(5) . . . . ? C30 O3 C3 O2 1.2(7) . . . . ? C30 O3 C3 C2 -178.7(4) . . . . ? Dy2 O14 C12 O15 -178.2(3) . . . . ? Dy2 O14 C12 C11 0.9(8) . . . . ? C150 O15 C12 O14 -8.0(7) . . . . ? C150 O15 C12 C11 172.7(5) . . . . ? C110 O11 C7 O9 -173.9(4) . . . . ? Dy1 O11 C7 O9 -13.5(4) . . . . ? C110 O11 C7 C8 5.0(8) . . . 2_565 ? Dy1 O11 C7 C8 165.3(5) . . . 2_565 ? Dy1 O5 C4 O8 -176.8(3) . . . . ? Dy1 O5 C4 C5 1.9(9) . . . . ? C80 O8 C4 O5 2.3(7) . . . . ? C80 O8 C4 C5 -176.6(5) . . . . ? C120 O12 C9 O10 1.0(7) . . . . ? C120 O12 C9 C8 179.4(4) . . . . ? O5 C4 C5 C6 1.2(9) . . . . ? O8 C4 C5 C6 180.0(5) . . . . ? O10 C9 C8 C7 2.2(9) . . . 2_565 ? O12 C9 C8 C7 -176.2(5) . . . 2_565 ? C40 O4 C1 O1 0.8(7) . . . . ? C40 O4 C1 C2 -179.0(5) . . . . ? C3 O3 C30 C31 -171.8(4) . . . . ? O13 C10 C11 C12 0.2(9) . . . . ? O16 C10 C11 C12 -179.0(4) . . . . ? O14 C12 C11 C10 0.0(8) . . . . ? O15 C12 C11 C10 179.1(5) . . . . ? C10 O16 C160 C161 84.1(6) . . . . ? C240 O24 C16 O21 1.3(7) . . . . ? C240 O24 C16 C17 -178.2(4) . . . 2_654 ? O2 C3 C2 C1 4.1(9) . . . . ? O3 C3 C2 C1 -176.0(5) . . . . ? O1 C1 C2 C3 -0.4(9) . . . . ? O4 C1 C2 C3 179.3(5) . . . . ? O22 C18 C17 C16 -1.6(8) . . . 2_654 ? O23 C18 C17 C16 178.1(4) . . . 2_654 ? C12 O15 C150 C151 -82.9(6) . . . . ? C16 O24 C240 C241 -179.4(5) . . . . ? C9 O12 C120 C121 80.9(6) . . . . ? Dy2 O18 C15 O19 171.4(3) . . . . ? Dy2 O18 C15 C14 -8.9(9) . . . . ? C190 O19 C15 O18 -4.9(8) . . . . ? C190 O19 C15 C14 175.4(5) . . . . ? O18 C15 C14 C13 0.4(10) . . . . ? O19 C15 C14 C13 -179.9(5) . . . . ? Dy1 O6 C6 O7 173.5(3) . . . . ? Dy1 O6 C6 C5 -6.5(8) . . . . ? C70 O7 C6 O6 -4.0(7) . . . . ? C70 O7 C6 C5 175.9(5) . . . . ? C4 C5 C6 O6 1.0(9) . . . . ? C4 C5 C6 O7 -179.0(5) . . . . ? C15 O19 C190 C191 -80.6(6) . . . . ? Dy2 O17 C13 O20 -179.9(3) . . . . ? Dy2 O17 C13 C14 1.0(9) . . . . ? C200 O20 C13 O17 -2.8(8) . . . . ? C200 O20 C13 C14 176.4(5) . . . . ? C15 C14 C13 O17 3.7(10) . . . . ? C15 C14 C13 O20 -175.4(5) . . . . ? C1 O4 C40 C41 174.0(5) . . . . ? C4 O8 C80 C81 -177.6(5) . . . . ? C6 O7 C70 C71 -94.4(6) . . . . ? C13 O20 C200 C201 -171.3(5) . . . . ? O11 C7 O9 Dy1 -154.0(3) . . . 2_565 ? C8 C7 O9 Dy1 27.2(8) 2_565 . . 2_565 ? O11 C7 O9 Dy1 18.4(5) . . . . ? C8 C7 O9 Dy1 -160.4(5) 2_565 . . . ? O2 Dy1 O9 C7 -17.2(4) . . . . ? O1 Dy1 O9 C7 -81.3(3) . . . . ? O5 Dy1 O9 C7 55.6(3) . . . . ? O6 Dy1 O9 C7 121.2(3) . . . . ? O9 Dy1 O9 C7 -173.8(4) 2_565 . . . ? O10 Dy1 O9 C7 -144.8(3) . . . . ? O11 Dy1 O9 C7 -10.9(3) . . . . ? Dy1 Dy1 O9 C7 -173.8(4) 2_565 . . . ? O2 Dy1 O9 Dy1 156.60(13) . . . 2_565 ? O1 Dy1 O9 Dy1 92.45(15) . . . 2_565 ? O5 Dy1 O9 Dy1 -130.67(17) . . . 2_565 ? O6 Dy1 O9 Dy1 -65.01(17) . . . 2_565 ? O9 Dy1 O9 Dy1 0.0 2_565 . . 2_565 ? O10 Dy1 O9 Dy1 28.9(2) . . . 2_565 ? O11 Dy1 O9 Dy1 162.9(2) . . . 2_565 ? O4 C1 O1 Dy1 175.7(3) . . . . ? C2 C1 O1 Dy1 -4.6(8) . . . . ? O2 Dy1 O1 C1 4.4(4) . . . . ? O5 Dy1 O1 C1 72.0(5) . . . . ? O6 Dy1 O1 C1 -88.6(5) . . . . ? O9 Dy1 O1 C1 -154.3(4) 2_565 . . . ? O10 Dy1 O1 C1 -82.1(4) . . . . ? O9 Dy1 O1 C1 139.4(4) . . . . ? O11 Dy1 O1 C1 92.3(4) . . . . ? Dy1 Dy1 O1 C1 172.5(4) 2_565 . . . ? O3 C3 O2 Dy1 177.5(3) . . . . ? C2 C3 O2 Dy1 -2.6(8) . . . . ? O1 Dy1 O2 C3 -0.9(4) . . . . ? O5 Dy1 O2 C3 -138.3(5) . . . . ? O6 Dy1 O2 C3 150.6(4) . . . . ? O9 Dy1 O2 C3 55.8(6) 2_565 . . . ? O10 Dy1 O2 C3 77.5(4) . . . . ? O9 Dy1 O2 C3 -67.4(5) . . . . ? O11 Dy1 O2 C3 -72.0(4) . . . . ? Dy1 Dy1 O2 C3 -33.0(6) 2_565 . . . ? O24 C16 O21 Dy2 -155.8(3) . . . . ? C17 C16 O21 Dy2 23.7(7) 2_654 . . . ? O17 Dy2 O21 C16 162.2(4) . . . . ? O18 Dy2 O21 C16 -120.8(4) . . . . ? O14 Dy2 O21 C16 52.8(4) . . . . ? O13 Dy2 O21 C16 92.6(4) . . . . ? O22 Dy2 O21 C16 -30.6(4) 2_654 . . . ? O22 Dy2 O21 C16 -50.7(5) . . . . ? O23 Dy2 O21 C16 -131.4(4) . . . . ? Dy2 Dy2 O21 C16 -39.2(4) 2_654 . . . ? O12 C9 O10 Dy1 -165.6(3) . . . . ? C8 C9 O10 Dy1 16.2(8) . . . . ? O2 Dy1 O10 C9 165.6(5) . . . . ? O1 Dy1 O10 C9 -117.0(5) . . . . ? O5 Dy1 O10 C9 94.3(5) . . . . ? O6 Dy1 O10 C9 59.8(5) . . . . ? O9 Dy1 O10 C9 -24.1(5) 2_565 . . . ? O9 Dy1 O10 C9 -51.8(5) . . . . ? O11 Dy1 O10 C9 -126.7(4) . . . . ? Dy1 Dy1 O10 C9 -36.1(5) 2_565 . . . ? O23 C18 O22 Dy2 -152.4(3) . . . 2_654 ? C17 C18 O22 Dy2 27.4(7) . . . 2_654 ? O23 C18 O22 Dy2 10.9(5) . . . . ? C17 C18 O22 Dy2 -169.4(4) . . . . ? O17 Dy2 O22 C18 -12.1(4) . . . . ? O18 Dy2 O22 C18 -77.4(3) . . . . ? O14 Dy2 O22 C18 127.1(3) . . . . ? O13 Dy2 O22 C18 58.8(3) . . . . ? O21 Dy2 O22 C18 -145.4(3) . . . . ? O22 Dy2 O22 C18 -166.3(4) 2_654 . . . ? O23 Dy2 O22 C18 -6.5(3) . . . . ? Dy2 Dy2 O22 C18 -166.3(4) 2_654 . . . ? O17 Dy2 O22 Dy2 154.16(13) . . . 2_654 ? O18 Dy2 O22 Dy2 88.81(15) . . . 2_654 ? O14 Dy2 O22 Dy2 -66.66(16) . . . 2_654 ? O13 Dy2 O22 Dy2 -134.98(15) . . . 2_654 ? O21 Dy2 O22 Dy2 20.9(2) . . . 2_654 ? O22 Dy2 O22 Dy2 0.0 2_654 . . 2_654 ? O23 Dy2 O22 Dy2 159.7(2) . . . 2_654 ? O22 C18 O23 C230 -178.5(4) . . . . ? C17 C18 O23 C230 1.8(7) . . . . ? O22 C18 O23 Dy2 -8.4(4) . . . . ? C17 C18 O23 Dy2 171.9(4) . . . . ? C231 C230 O23 C18 -178.8(4) . . . . ? C231 C230 O23 Dy2 20.7(8) . . . . ? O17 Dy2 O23 C18 -178.4(3) . . . . ? O18 Dy2 O23 C18 104.6(3) . . . . ? O14 Dy2 O23 C18 -70.3(3) . . . . ? O13 Dy2 O23 C18 -95.3(3) . . . . ? O21 Dy2 O23 C18 115.5(3) . . . . ? O22 Dy2 O23 C18 25.5(3) 2_654 . . . ? O22 Dy2 O23 C18 5.7(2) . . . . ? Dy2 Dy2 O23 C18 16.8(2) 2_654 . . . ? O17 Dy2 O23 C230 -15.0(6) . . . . ? O18 Dy2 O23 C230 -92.0(6) . . . . ? O14 Dy2 O23 C230 93.1(6) . . . . ? O13 Dy2 O23 C230 68.1(6) . . . . ? O21 Dy2 O23 C230 -81.1(6) . . . . ? O22 Dy2 O23 C230 -171.1(6) 2_654 . . . ? O22 Dy2 O23 C230 169.1(6) . . . . ? Dy2 Dy2 O23 C230 -179.9(6) 2_654 . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 3.188 _refine_diff_density_min -1.178 _refine_diff_density_rms 0.137 #=================================END data_cvd266 _database_code_depnum_ccdc_archive 'CCDC 770259' #TrackingRef '- combined cif files.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H90 Dy2 O24' _chemical_formula_weight 1448.26 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' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.4112(2) _cell_length_b 16.1629(3) _cell_length_c 17.6679(2) _cell_angle_alpha 96.3730(10) _cell_angle_beta 97.3720(10) _cell_angle_gamma 100.0620(10) _cell_volume 3428.38(9) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 8500 _cell_measurement_theta_min 2.774 _cell_measurement_theta_max 27.499 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.403 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1476 _exptl_absorpt_coefficient_mu 2.232 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.455 _exptl_absorpt_correction_T_max 0.570 _exptl_absorpt_process_details abspack _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Sapphire2-CCD, Oxford Diffraction' _diffrn_measurement_method '887 images at 1.0 deg. in \w and 15 sec.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45121 _diffrn_reflns_av_R_equivalents 0.0218 _diffrn_reflns_av_sigmaI/netI 0.0234 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12008 _reflns_number_gt 9863 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD 171_33_34d, Oxford Diffraction' _computing_cell_refinement 'CrysAlis RED 171_33_34d, Oxford Diffraction' _computing_data_reduction 'CrysAlis RED 171_33_34d, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0225P)^2^+2.0790P] 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 12008 _refine_ls_number_parameters 721 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0324 _refine_ls_R_factor_gt 0.0213 _refine_ls_wR_factor_ref 0.0483 _refine_ls_wR_factor_gt 0.0451 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.005 _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 Dy2 Dy 0.629830(9) 0.594603(7) 0.516245(7) 0.01329(4) Uani 1 1 d . . . Dy1 Dy 0.934184(9) 1.047228(7) 0.911277(6) 0.01333(4) Uani 1 1 d . . . O11 O 1.11292(16) 1.31874(11) 0.97289(11) 0.0247(4) Uani 1 1 d . . . O12 O 0.90703(14) 0.87335(11) 0.84513(9) 0.0173(4) Uani 1 1 d . . . O5 O 1.08315(14) 1.02399(11) 0.85533(9) 0.0170(4) Uani 1 1 d . . . O4 O 0.69163(16) 1.21167(12) 0.97568(11) 0.0252(4) Uani 1 1 d . . . O8 O 1.21357(14) 1.01948(12) 0.77908(10) 0.0211(4) Uani 1 1 d . . . O16 O 0.48924(16) 0.78359(12) 0.66194(10) 0.0235(4) Uani 1 1 d . . . O17 O 0.79525(14) 0.68080(11) 0.51836(10) 0.0173(4) Uani 1 1 d . . . O2 O 0.76601(14) 0.96958(11) 0.92353(10) 0.0187(4) Uani 1 1 d . . . O6 O 0.89227(14) 1.06851(11) 0.78817(10) 0.0178(4) Uani 1 1 d . . . O22 O 0.57886(14) 0.67572(11) 0.42148(10) 0.0174(4) Uani 1 1 d . . . O10 O 1.04379(15) 1.18271(11) 0.92608(10) 0.0190(4) Uani 1 1 d . . . O21 O 0.43987(14) 0.55011(11) 0.47400(10) 0.0161(4) Uani 1 1 d . . . O18 O 0.69510(14) 0.53831(11) 0.41168(10) 0.0176(4) Uani 1 1 d . . . O1 O 0.82541(15) 1.14346(11) 0.94315(11) 0.0215(4) Uani 1 1 d . . . O9 O 0.97520(14) 0.92329(11) 0.96323(9) 0.0149(4) Uani 1 1 d . . . O7 O 0.89924(15) 1.10523(13) 0.67008(10) 0.0243(4) Uani 1 1 d . . . O14 O 0.67212(15) 0.58835(11) 0.64519(10) 0.0204(4) Uani 1 1 d . . . O24 O 0.73616(14) 0.45530(11) 0.54975(10) 0.0194(4) Uani 1 1 d . . . O13 O 0.56493(15) 0.70357(11) 0.57918(10) 0.0202(4) Uani 1 1 d . . . O15 O 0.68185(18) 0.59918(12) 0.77406(10) 0.0295(5) Uani 1 1 d . . . O20 O 0.92726(16) 0.76853(12) 0.47407(11) 0.0256(5) Uani 1 1 d . . . O19 O 0.76687(19) 0.53233(14) 0.30141(12) 0.0402(6) Uani 1 1 d . . . C9 C 1.0822(2) 1.23692(16) 0.98257(15) 0.0184(6) Uani 1 1 d . . . O3 O 0.59552(15) 0.92159(11) 0.95086(11) 0.0246(4) Uani 1 1 d . . . O23 O 0.49162(15) 0.76775(12) 0.36453(11) 0.0251(4) Uani 1 1 d . . . C16 C 0.3651(2) 0.58868(16) 0.44538(14) 0.0158(6) Uani 1 1 d . . . C17 C 0.3831(2) 0.66206(16) 0.41300(15) 0.0177(6) Uani 1 1 d . . . H17A H 0.3224 0.6882 0.3978 0.023 Uiso 1 1 calc R . . C240 C 0.8370(2) 0.42784(18) 0.57936(17) 0.0230(6) Uani 1 1 d . . . H24A H 0.8278 0.4045 0.6287 0.028 Uiso 1 1 calc R . . C7 C 0.9276(2) 0.85510(16) 0.91795(14) 0.0157(6) Uani 1 1 d . . . C120 C 0.8474(2) 0.80920(17) 0.78192(14) 0.0207(6) Uani 1 1 d . . . H12A H 0.7863 0.7715 0.8004 0.025 Uiso 1 1 calc R . . C8 C 1.0999(2) 1.22394(17) 1.06119(15) 0.0187(6) Uani 1 1 d . . . H8A H 1.1313 1.2708 1.0997 0.022 Uiso 1 1 calc R . . C4 C 1.1137(2) 1.03569(16) 0.79183(15) 0.0170(6) Uani 1 1 d . . . C15 C 0.6454(2) 0.62311(17) 0.70563(15) 0.0204(6) Uani 1 1 d . . . C6 C 0.9478(2) 1.07921(16) 0.73394(14) 0.0177(6) Uani 1 1 d . . . C1 C 0.6780(2) 0.98636(17) 0.94475(15) 0.0181(6) Uani 1 1 d . . . C18 C 0.4909(2) 0.69946(16) 0.40191(14) 0.0172(6) Uani 1 1 d . . . C3 C 0.7293(2) 1.13879(17) 0.95914(15) 0.0189(6) Uani 1 1 d . . . C13 C 0.5470(2) 0.72229(16) 0.64697(15) 0.0182(6) Uani 1 1 d . . . C14 C 0.5827(2) 0.68578(17) 0.71123(15) 0.0215(6) Uani 1 1 d . . . H14A H 0.5635 0.7043 0.7598 0.026 Uiso 1 1 calc R . . C10 C 0.8495(2) 0.69661(16) 0.46446(15) 0.0184(6) Uani 1 1 d . . . C80 C 1.2733(2) 0.98088(18) 0.83867(15) 0.0206(6) Uani 1 1 d . . . H80A H 1.2623 1.0065 0.8906 0.025 Uiso 1 1 calc R . . C200 C 0.9324(2) 0.83159(17) 0.54090(16) 0.0238(6) Uani 1 1 d . . . H20A H 0.9087 0.8023 0.5847 0.029 Uiso 1 1 calc R . . C122 C 0.7997(2) 0.85898(19) 0.72305(16) 0.0287(7) Uani 1 1 d . . . H12B H 0.7494 0.8916 0.7457 0.043 Uiso 1 1 calc R . . H12C H 0.7589 0.8199 0.6781 0.043 Uiso 1 1 calc R . . H12D H 0.8599 0.8979 0.7071 0.043 Uiso 1 1 calc R . . C11 C 0.8408(2) 0.64717(17) 0.39365(16) 0.0224(6) Uani 1 1 d . . . H11A H 0.8885 0.6657 0.3584 0.027 Uiso 1 1 calc R . . C12 C 0.7645(2) 0.57132(17) 0.37261(15) 0.0216(6) Uani 1 1 d . . . C5 C 1.0545(2) 1.06471(17) 0.73070(15) 0.0196(6) Uani 1 1 d . . . H5A H 1.0877 1.0747 0.6862 0.024 Uiso 1 1 calc R . . C40 C 0.7663(3) 1.29170(18) 0.97831(18) 0.0308(7) Uani 1 1 d . . . H40A H 0.8124 1.2876 0.9361 0.037 Uiso 1 1 calc R . . C230 C 0.5973(2) 0.80949(18) 0.34539(18) 0.0279(7) Uani 1 1 d . . . H23A H 0.6593 0.7997 0.3833 0.033 Uiso 1 1 calc R . . C2 C 0.6532(2) 1.06581(17) 0.96255(15) 0.0198(6) Uani 1 1 d . . . H2A H 0.5833 1.0705 0.9773 0.024 Uiso 1 1 calc R . . C121 C 0.9262(3) 0.75710(19) 0.75110(17) 0.0295(7) Uani 1 1 d . . . H12E H 0.9549 0.7260 0.7913 0.044 Uiso 1 1 calc R . . H12F H 0.9879 0.7947 0.7355 0.044 Uiso 1 1 calc R . . H12G H 0.8870 0.7167 0.7065 0.044 Uiso 1 1 calc R . . C81 C 1.3936(2) 1.0025(2) 0.83082(17) 0.0276(7) Uani 1 1 d . . . H81A H 1.4178 1.0643 0.8383 0.041 Uiso 1 1 calc R . . H81B H 1.4044 0.9793 0.7793 0.041 Uiso 1 1 calc R . . H81C H 1.4373 0.9781 0.8697 0.041 Uiso 1 1 calc R . . C82 C 1.2284(2) 0.88656(18) 0.82793(17) 0.0283(7) Uani 1 1 d . . . H82A H 1.1499 0.8765 0.8337 0.042 Uiso 1 1 calc R . . H82B H 1.2695 0.8604 0.8668 0.042 Uiso 1 1 calc R . . H82C H 1.2366 0.8616 0.7764 0.042 Uiso 1 1 calc R . . C160 C 0.4496(2) 0.82569(19) 0.59805(16) 0.0256(7) Uani 1 1 d . . . H16A H 0.4309 0.7841 0.5498 0.031 Uiso 1 1 calc R . . C30 C 0.6141(2) 0.83521(17) 0.93731(17) 0.0256(7) Uani 1 1 d . . . H30A H 0.6718 0.8325 0.9030 0.031 Uiso 1 1 calc R . . C70 C 0.7911(2) 1.12715(19) 0.67290(16) 0.0255(7) Uani 1 1 d . . . H70A H 0.7447 1.0841 0.6977 0.031 Uiso 1 1 calc R . . C72 C 0.7405(3) 1.1233(2) 0.58964(16) 0.0331(7) Uani 1 1 d . . . H72A H 0.7345 1.0659 0.5627 0.050 Uiso 1 1 calc R . . H72B H 0.7875 1.1640 0.5648 0.050 Uiso 1 1 calc R . . H72C H 0.6666 1.1375 0.5875 0.050 Uiso 1 1 calc R . . C150 C 0.7216(3) 0.51950(19) 0.77288(17) 0.0326(7) Uani 1 1 d . . . H15A H 0.7532 0.5078 0.7244 0.039 Uiso 1 1 calc R . . C241 C 0.8607(3) 0.3604(2) 0.52131(19) 0.0334(7) Uani 1 1 d . . . H24B H 0.8007 0.3106 0.5138 0.050 Uiso 1 1 calc R . . H24C H 0.9307 0.3441 0.5402 0.050 Uiso 1 1 calc R . . H24D H 0.8661 0.3824 0.4722 0.050 Uiso 1 1 calc R . . C162 C 0.3457(2) 0.8532(2) 0.61830(17) 0.0318(7) Uani 1 1 d . . . H16B H 0.2915 0.8034 0.6242 0.048 Uiso 1 1 calc R . . H16C H 0.3147 0.8821 0.5771 0.048 Uiso 1 1 calc R . . H16D H 0.3634 0.8921 0.6667 0.048 Uiso 1 1 calc R . . C242 C 0.9253(2) 0.5074(2) 0.59493(19) 0.0333(7) Uani 1 1 d . . . H24E H 0.9051 0.5486 0.6330 0.050 Uiso 1 1 calc R . . H24F H 0.9318 0.5318 0.5470 0.050 Uiso 1 1 calc R . . H24G H 0.9964 0.4935 0.6149 0.050 Uiso 1 1 calc R . . C31 C 0.5049(2) 0.7825(2) 0.89751(19) 0.0337(8) Uani 1 1 d . . . H31A H 0.4841 0.8024 0.8483 0.051 Uiso 1 1 calc R . . H31B H 0.4477 0.7879 0.9302 0.051 Uiso 1 1 calc R . . H31C H 0.5119 0.7229 0.8881 0.051 Uiso 1 1 calc R . . C110 C 1.0945(3) 1.33919(19) 0.89460(17) 0.0299(7) Uani 1 1 d . . . H11B H 1.0229 1.3044 0.8667 0.036 Uiso 1 1 calc R . . C32 C 0.6523(3) 0.8088(2) 1.0136(2) 0.0406(8) Uani 1 1 d . . . H32A H 0.7233 0.8450 1.0368 0.061 Uiso 1 1 calc R . . H32B H 0.6614 0.7495 1.0059 0.061 Uiso 1 1 calc R . . H32C H 0.5972 0.8145 1.0480 0.061 Uiso 1 1 calc R . . C41 C 0.8402(3) 1.3138(2) 1.0550(2) 0.0407(8) Uani 1 1 d . . . H41A H 0.8865 1.2710 1.0612 0.061 Uiso 1 1 calc R . . H41B H 0.7948 1.3153 1.0963 0.061 Uiso 1 1 calc R . . H41C H 0.8876 1.3696 1.0572 0.061 Uiso 1 1 calc R . . C152 C 0.6247(3) 0.4501(2) 0.77597(19) 0.0426(9) Uani 1 1 d . . . H15B H 0.5696 0.4455 0.7300 0.064 Uiso 1 1 calc R . . H15C H 0.5914 0.4635 0.8221 0.064 Uiso 1 1 calc R . . H15D H 0.6501 0.3962 0.7779 0.064 Uiso 1 1 calc R . . C161 C 0.5379(3) 0.8978(2) 0.5878(2) 0.0432(9) Uani 1 1 d . . . H16E H 0.6029 0.8758 0.5748 0.065 Uiso 1 1 calc R . . H16F H 0.5586 0.9374 0.6358 0.065 Uiso 1 1 calc R . . H16G H 0.5100 0.9273 0.5461 0.065 Uiso 1 1 calc R . . C71 C 0.8031(3) 1.2136(2) 0.71833(19) 0.0429(9) Uani 1 1 d . . . H71A H 0.8361 1.2126 0.7716 0.064 Uiso 1 1 calc R . . H71B H 0.7301 1.2289 0.7178 0.064 Uiso 1 1 calc R . . H71C H 0.8510 1.2554 0.6952 0.064 Uiso 1 1 calc R . . C111 C 1.1881(3) 1.3208(2) 0.85280(19) 0.0420(9) Uani 1 1 d . . . H11C H 1.1892 1.2600 0.8485 0.063 Uiso 1 1 calc R . . H11D H 1.2586 1.3528 0.8816 0.063 Uiso 1 1 calc R . . H11E H 1.1775 1.3376 0.8011 0.063 Uiso 1 1 calc R . . C190 C 0.6859(3) 0.4548(2) 0.27241(19) 0.0423(9) Uani 1 1 d . . . H19A H 0.6183 0.4559 0.2975 0.051 Uiso 1 1 calc R . . C231 C 0.5947(3) 0.90244(19) 0.3528(2) 0.0400(8) Uani 1 1 d . . . H23B H 0.5868 0.9227 0.4058 0.060 Uiso 1 1 calc R . . H23C H 0.5318 0.9118 0.3174 0.060 Uiso 1 1 calc R . . H23D H 0.6636 0.9335 0.3401 0.060 Uiso 1 1 calc R . . C42 C 0.6918(3) 1.3548(2) 0.9639(2) 0.0423(9) Uani 1 1 d . . . H42A H 0.6456 1.3373 0.9134 0.063 Uiso 1 1 calc R . . H42B H 0.7371 1.4111 0.9650 0.063 Uiso 1 1 calc R . . H42C H 0.6443 1.3568 1.0041 0.063 Uiso 1 1 calc R . . C151 C 0.8111(3) 0.5316(2) 0.8413(2) 0.0445(9) Uani 1 1 d . . . H15E H 0.8715 0.5775 0.8358 0.067 Uiso 1 1 calc R . . H15F H 0.8395 0.4790 0.8442 0.067 Uiso 1 1 calc R . . H15G H 0.7807 0.5463 0.8884 0.067 Uiso 1 1 calc R . . C112 C 1.0866(3) 1.4318(2) 0.9039(2) 0.0452(9) Uani 1 1 d . . . H11F H 1.0246 1.4399 0.9313 0.068 Uiso 1 1 calc R . . H11G H 1.0744 1.4502 0.8529 0.068 Uiso 1 1 calc R . . H11H H 1.1556 1.4655 0.9333 0.068 Uiso 1 1 calc R . . C202 C 0.8561(4) 0.8900(2) 0.5208(2) 0.0529(10) Uani 1 1 d . . . H20B H 0.7800 0.8578 0.5081 0.079 Uiso 1 1 calc R . . H20C H 0.8769 0.9168 0.4764 0.079 Uiso 1 1 calc R . . H20D H 0.8610 0.9338 0.5648 0.079 Uiso 1 1 calc R . . C232 C 0.6092(3) 0.7721(2) 0.2662(2) 0.0549(11) Uani 1 1 d . . . H23E H 0.6103 0.7115 0.2654 0.082 Uiso 1 1 calc R . . H23F H 0.6784 0.8010 0.2520 0.082 Uiso 1 1 calc R . . H23G H 0.5466 0.7793 0.2293 0.082 Uiso 1 1 calc R . . C191 C 0.6569(4) 0.4570(3) 0.1881(2) 0.0621(12) Uani 1 1 d . . . H19B H 0.6259 0.5077 0.1802 0.093 Uiso 1 1 calc R . . H19C H 0.6021 0.4062 0.1653 0.093 Uiso 1 1 calc R . . H19D H 0.7236 0.4586 0.1637 0.093 Uiso 1 1 calc R . . C201 C 1.0516(3) 0.8741(3) 0.5614(3) 0.0662(14) Uani 1 1 d . . . H20E H 1.0966 0.8319 0.5739 0.099 Uiso 1 1 calc R . . H20F H 1.0601 0.9176 0.6062 0.099 Uiso 1 1 calc R . . H20G H 1.0760 0.9006 0.5177 0.099 Uiso 1 1 calc R . . C192 C 0.7331(4) 0.3816(3) 0.2914(3) 0.0719(13) Uani 1 1 d . . . H19E H 0.7499 0.3847 0.3475 0.108 Uiso 1 1 calc R . . H19F H 0.8013 0.3817 0.2689 0.108 Uiso 1 1 calc R . . H19G H 0.6798 0.3294 0.2705 0.108 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 Dy2 0.01354(7) 0.01221(7) 0.01479(7) 0.00387(5) 0.00331(5) 0.00216(5) Dy1 0.01368(7) 0.01410(7) 0.01222(7) 0.00257(5) 0.00235(5) 0.00190(5) O11 0.0344(12) 0.0146(10) 0.0240(10) 0.0062(8) 0.0027(9) 0.0011(9) O12 0.0207(10) 0.0156(9) 0.0134(9) -0.0002(7) 0.0012(7) 0.0003(8) O5 0.0169(9) 0.0208(10) 0.0140(9) 0.0033(8) 0.0033(7) 0.0041(8) O4 0.0274(11) 0.0162(10) 0.0353(12) 0.0035(9) 0.0124(9) 0.0079(9) O8 0.0163(10) 0.0334(11) 0.0171(10) 0.0095(8) 0.0056(8) 0.0083(8) O16 0.0303(11) 0.0234(11) 0.0190(10) 0.0008(8) 0.0045(8) 0.0117(9) O17 0.0151(9) 0.0168(10) 0.0194(10) 0.0028(8) 0.0037(8) 0.0000(8) O2 0.0144(10) 0.0170(10) 0.0250(10) 0.0024(8) 0.0053(8) 0.0024(8) O6 0.0177(10) 0.0229(10) 0.0142(9) 0.0053(8) 0.0027(8) 0.0055(8) O22 0.0155(9) 0.0179(10) 0.0215(10) 0.0073(8) 0.0061(8) 0.0050(8) O10 0.0205(10) 0.0170(10) 0.0184(10) 0.0038(8) 0.0043(8) -0.0014(8) O21 0.0153(9) 0.0141(9) 0.0206(10) 0.0066(8) 0.0033(7) 0.0044(8) O18 0.0189(10) 0.0144(9) 0.0200(10) 0.0023(8) 0.0064(8) 0.0020(8) O1 0.0216(10) 0.0169(10) 0.0277(11) 0.0031(8) 0.0095(8) 0.0041(8) O9 0.0163(9) 0.0135(9) 0.0131(9) 0.0004(7) 0.0015(7) -0.0001(8) O7 0.0255(11) 0.0365(12) 0.0163(10) 0.0117(9) 0.0035(8) 0.0149(9) O14 0.0254(10) 0.0202(10) 0.0167(10) 0.0037(8) 0.0022(8) 0.0074(8) O24 0.0142(9) 0.0178(10) 0.0277(10) 0.0090(8) 0.0032(8) 0.0032(8) O13 0.0239(10) 0.0203(10) 0.0183(10) 0.0023(8) 0.0051(8) 0.0081(8) O15 0.0489(13) 0.0254(11) 0.0161(10) 0.0049(9) 0.0009(9) 0.0144(10) O20 0.0251(11) 0.0196(10) 0.0285(11) -0.0042(9) 0.0118(9) -0.0068(9) O19 0.0479(14) 0.0321(13) 0.0316(12) -0.0135(10) 0.0239(10) -0.0186(11) C9 0.0163(14) 0.0145(14) 0.0249(15) 0.0028(12) 0.0051(11) 0.0029(11) O3 0.0155(10) 0.0159(10) 0.0425(12) 0.0006(9) 0.0100(9) 0.0011(8) O23 0.0228(11) 0.0204(10) 0.0381(12) 0.0188(9) 0.0098(9) 0.0075(8) C16 0.0152(13) 0.0147(13) 0.0168(13) -0.0007(11) 0.0035(11) 0.0022(11) C17 0.0163(13) 0.0171(14) 0.0225(14) 0.0066(11) 0.0043(11) 0.0076(11) C240 0.0127(14) 0.0252(16) 0.0319(16) 0.0075(13) 0.0013(12) 0.0053(12) C7 0.0116(13) 0.0194(14) 0.0168(14) 0.0007(11) 0.0037(10) 0.0051(11) C120 0.0223(15) 0.0213(15) 0.0130(13) -0.0035(11) -0.0021(11) -0.0037(12) C8 0.0218(14) 0.0143(14) 0.0177(14) -0.0023(11) 0.0012(11) 0.0014(11) C4 0.0174(14) 0.0143(13) 0.0182(14) 0.0007(11) 0.0038(11) 0.0003(11) C15 0.0226(15) 0.0175(14) 0.0183(14) 0.0050(12) 0.0000(11) -0.0030(12) C6 0.0230(15) 0.0148(14) 0.0143(13) 0.0031(11) -0.0003(11) 0.0021(11) C1 0.0158(14) 0.0192(14) 0.0176(14) 0.0017(11) -0.0001(11) 0.0010(11) C18 0.0260(15) 0.0151(14) 0.0121(13) 0.0027(11) 0.0052(11) 0.0058(12) C3 0.0241(15) 0.0193(14) 0.0147(13) 0.0022(11) 0.0036(11) 0.0070(12) C13 0.0162(14) 0.0141(14) 0.0227(15) -0.0008(11) 0.0030(11) 0.0002(11) C14 0.0288(16) 0.0204(15) 0.0154(14) 0.0002(11) 0.0068(12) 0.0040(12) C10 0.0126(13) 0.0171(14) 0.0256(15) 0.0043(12) 0.0036(11) 0.0020(11) C80 0.0195(14) 0.0279(16) 0.0168(14) 0.0059(12) 0.0026(11) 0.0092(12) C200 0.0252(15) 0.0196(15) 0.0246(15) -0.0023(12) 0.0091(12) -0.0016(12) C122 0.0308(17) 0.0303(17) 0.0205(15) 0.0029(13) -0.0029(12) -0.0016(14) C11 0.0215(15) 0.0224(15) 0.0230(15) 0.0015(12) 0.0117(12) -0.0015(12) C12 0.0241(15) 0.0207(15) 0.0209(15) 0.0009(12) 0.0066(12) 0.0052(12) C5 0.0227(15) 0.0252(15) 0.0132(13) 0.0055(11) 0.0063(11) 0.0062(12) C40 0.0407(19) 0.0169(15) 0.0398(18) 0.0078(13) 0.0193(15) 0.0070(14) C230 0.0241(16) 0.0242(16) 0.0409(18) 0.0183(14) 0.0136(13) 0.0047(13) C2 0.0167(14) 0.0207(15) 0.0232(15) 0.0021(12) 0.0058(11) 0.0051(12) C121 0.0353(18) 0.0279(17) 0.0225(15) -0.0052(13) 0.0040(13) 0.0044(14) C81 0.0200(15) 0.0352(18) 0.0281(16) 0.0043(14) 0.0037(12) 0.0064(13) C82 0.0247(16) 0.0306(17) 0.0313(17) 0.0072(14) 0.0053(13) 0.0073(13) C160 0.0317(17) 0.0295(17) 0.0179(14) 0.0004(12) 0.0003(12) 0.0159(14) C30 0.0213(15) 0.0178(15) 0.0392(18) 0.0001(13) 0.0135(13) 0.0032(12) C70 0.0266(16) 0.0322(17) 0.0216(15) 0.0091(13) 0.0030(12) 0.0133(13) C72 0.0340(18) 0.045(2) 0.0240(16) 0.0108(14) -0.0019(13) 0.0184(15) C150 0.053(2) 0.0252(17) 0.0239(16) 0.0096(13) 0.0046(14) 0.0164(15) C241 0.0235(16) 0.0325(18) 0.045(2) 0.0030(15) 0.0110(14) 0.0062(14) C162 0.0312(17) 0.0361(18) 0.0302(17) 0.0015(14) 0.0009(13) 0.0173(15) C242 0.0193(16) 0.0331(18) 0.046(2) 0.0044(15) 0.0030(14) 0.0021(14) C31 0.0278(17) 0.0272(17) 0.0419(19) -0.0075(15) 0.0096(14) -0.0016(14) C110 0.0386(18) 0.0233(16) 0.0260(16) 0.0112(13) 0.0012(13) -0.0007(14) C32 0.044(2) 0.0267(18) 0.050(2) 0.0029(16) 0.0017(16) 0.0096(16) C41 0.039(2) 0.0221(17) 0.058(2) -0.0039(16) 0.0042(17) 0.0059(15) C152 0.063(2) 0.0296(19) 0.0328(19) 0.0052(15) -0.0013(17) 0.0089(17) C161 0.039(2) 0.041(2) 0.058(2) 0.0234(18) 0.0128(17) 0.0179(17) C71 0.054(2) 0.042(2) 0.0366(19) 0.0039(16) -0.0034(16) 0.0282(18) C111 0.058(2) 0.0348(19) 0.040(2) 0.0195(16) 0.0193(17) 0.0084(17) C190 0.052(2) 0.0293(19) 0.0365(19) -0.0107(15) 0.0244(17) -0.0193(16) C231 0.051(2) 0.0232(17) 0.052(2) 0.0159(16) 0.0243(17) 0.0039(16) C42 0.061(2) 0.0243(17) 0.049(2) 0.0143(16) 0.0141(18) 0.0159(17) C151 0.053(2) 0.038(2) 0.043(2) 0.0142(16) -0.0057(17) 0.0158(17) C112 0.065(3) 0.0292(19) 0.046(2) 0.0181(16) 0.0073(18) 0.0124(17) C202 0.079(3) 0.046(2) 0.041(2) 0.0020(18) 0.007(2) 0.034(2) C232 0.068(3) 0.037(2) 0.065(3) 0.0075(19) 0.044(2) 0.0015(19) C191 0.075(3) 0.046(2) 0.049(2) -0.0060(19) 0.005(2) -0.022(2) C201 0.032(2) 0.059(3) 0.088(3) -0.045(2) 0.014(2) -0.0122(19) C192 0.081(3) 0.040(2) 0.083(3) 0.006(2) -0.003(3) -0.008(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy2 O17 2.2643(17) . ? Dy2 O18 2.2728(17) . ? Dy2 O14 2.2888(17) . ? Dy2 O13 2.2974(18) . ? Dy2 O22 2.3297(17) . ? Dy2 O21 2.3387(17) . ? Dy2 O21 2.3810(17) 2_666 ? Dy2 O24 2.8800(17) . ? Dy2 Dy2 3.9698(2) 2_666 ? Dy1 O6 2.2490(17) . ? Dy1 O5 2.2728(17) . ? Dy1 O2 2.2890(17) . ? Dy1 O1 2.3006(18) . ? Dy1 O9 2.3122(16) 2_777 ? Dy1 O10 2.3355(18) . ? Dy1 O9 2.3997(17) . ? Dy1 O12 2.8665(17) . ? Dy1 Dy1 3.9304(2) 2_777 ? O11 C9 1.347(3) . ? O11 C110 1.457(3) . ? O12 C7 1.354(3) . ? O12 C120 1.460(3) . ? O5 C4 1.253(3) . ? O4 C3 1.358(3) . ? O4 C40 1.446(3) . ? O8 C4 1.352(3) . ? O8 C80 1.468(3) . ? O16 C13 1.343(3) . ? O16 C160 1.457(3) . ? O17 C10 1.259(3) . ? O2 C1 1.263(3) . ? O6 C6 1.260(3) . ? O22 C18 1.240(3) . ? O10 C9 1.237(3) . ? O21 C16 1.287(3) . ? O21 Dy2 2.3810(17) 2_666 ? O18 C12 1.256(3) . ? O1 C3 1.252(3) . ? O9 C7 1.288(3) . ? O9 Dy1 2.3123(16) 2_777 ? O7 C6 1.354(3) . ? O7 C70 1.452(3) . ? O14 C15 1.261(3) . ? O24 C16 1.350(3) 2_666 ? O24 C240 1.455(3) . ? O13 C13 1.260(3) . ? O15 C15 1.357(3) . ? O15 C150 1.456(3) . ? O20 C10 1.354(3) . ? O20 C200 1.459(3) . ? O19 C12 1.349(3) . ? O19 C190 1.459(4) . ? C9 C8 1.423(4) . ? O3 C1 1.354(3) . ? O3 C30 1.453(3) . ? O23 C18 1.347(3) . ? O23 C230 1.465(3) . ? C16 O24 1.350(3) 2_666 ? C16 C17 1.369(4) . ? C17 C18 1.416(4) . ? C17 H17A 0.9500 . ? C240 C241 1.506(4) . ? C240 C242 1.511(4) . ? C240 H24A 1.0000 . ? C7 C8 1.367(4) 2_777 ? C120 C122 1.508(4) . ? C120 C121 1.512(4) . ? C120 H12A 1.0000 . ? C8 C7 1.367(4) 2_777 ? C8 H8A 0.9500 . ? C4 C5 1.398(4) . ? C15 C14 1.384(4) . ? C6 C5 1.392(4) . ? C1 C2 1.384(4) . ? C3 C2 1.389(4) . ? C13 C14 1.394(4) . ? C14 H14A 0.9500 . ? C10 C11 1.389(4) . ? C80 C81 1.501(4) . ? C80 C82 1.511(4) . ? C80 H80A 1.0000 . ? C200 C202 1.488(4) . ? C200 C201 1.498(4) . ? C200 H20A 1.0000 . ? C122 H12B 0.9800 . ? C122 H12C 0.9800 . ? C122 H12D 0.9800 . ? C11 C12 1.393(4) . ? C11 H11A 0.9500 . ? C5 H5A 0.9500 . ? C40 C41 1.504(5) . ? C40 C42 1.511(4) . ? C40 H40A 1.0000 . ? C230 C232 1.498(5) . ? C230 C231 1.500(4) . ? C230 H23A 1.0000 . ? C2 H2A 0.9500 . ? C121 H12E 0.9800 . ? C121 H12F 0.9800 . ? C121 H12G 0.9800 . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? C160 C161 1.498(4) . ? C160 C162 1.508(4) . ? C160 H16A 1.0000 . ? C30 C32 1.504(4) . ? C30 C31 1.509(4) . ? C30 H30A 1.0000 . ? C70 C71 1.505(4) . ? C70 C72 1.514(4) . ? C70 H70A 1.0000 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C150 C151 1.504(4) . ? C150 C152 1.505(5) . ? C150 H15A 1.0000 . ? C241 H24B 0.9800 . ? C241 H24C 0.9800 . ? C241 H24D 0.9800 . ? C162 H16B 0.9800 . ? C162 H16C 0.9800 . ? C162 H16D 0.9800 . ? C242 H24E 0.9800 . ? C242 H24F 0.9800 . ? C242 H24G 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C110 C111 1.509(4) . ? C110 C112 1.509(4) . ? C110 H11B 1.0000 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C152 H15B 0.9800 . ? C152 H15C 0.9800 . ? C152 H15D 0.9800 . ? C161 H16E 0.9800 . ? C161 H16F 0.9800 . ? C161 H16G 0.9800 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C111 H11C 0.9800 . ? C111 H11D 0.9800 . ? C111 H11E 0.9800 . ? C190 C192 1.461(5) . ? C190 C191 1.492(5) . ? C190 H19A 1.0000 . ? C231 H23B 0.9800 . ? C231 H23C 0.9800 . ? C231 H23D 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C151 H15E 0.9800 . ? C151 H15F 0.9800 . ? C151 H15G 0.9800 . ? C112 H11F 0.9800 . ? C112 H11G 0.9800 . ? C112 H11H 0.9800 . ? C202 H20B 0.9800 . ? C202 H20C 0.9800 . ? C202 H20D 0.9800 . ? C232 H23E 0.9800 . ? C232 H23F 0.9800 . ? C232 H23G 0.9800 . ? C191 H19B 0.9800 . ? C191 H19C 0.9800 . ? C191 H19D 0.9800 . ? C201 H20E 0.9800 . ? C201 H20F 0.9800 . ? C201 H20G 0.9800 . ? C192 H19E 0.9800 . ? C192 H19F 0.9800 . ? C192 H19G 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 O17 Dy2 O18 76.19(6) . . ? O17 Dy2 O14 90.27(6) . . ? O18 Dy2 O14 132.24(6) . . ? O17 Dy2 O13 90.69(6) . . ? O18 Dy2 O13 149.95(6) . . ? O14 Dy2 O13 73.61(6) . . ? O17 Dy2 O22 80.77(6) . . ? O18 Dy2 O22 76.62(6) . . ? O14 Dy2 O22 146.82(6) . . ? O13 Dy2 O22 74.63(6) . . ? O17 Dy2 O21 152.85(6) . . ? O18 Dy2 O21 99.25(6) . . ? O14 Dy2 O21 111.11(6) . . ? O13 Dy2 O21 80.13(6) . . ? O22 Dy2 O21 72.19(6) . . ? O17 Dy2 O21 138.48(6) . 2_666 ? O18 Dy2 O21 83.45(6) . 2_666 ? O14 Dy2 O21 77.18(6) . 2_666 ? O13 Dy2 O21 121.99(6) . 2_666 ? O22 Dy2 O21 129.12(6) . 2_666 ? O21 Dy2 O21 65.49(7) . 2_666 ? O17 Dy2 O24 91.43(6) . . ? O18 Dy2 O24 68.47(6) . . ? O14 Dy2 O24 66.30(6) . . ? O13 Dy2 O24 139.86(6) . . ? O22 Dy2 O24 145.08(6) . . ? O21 Dy2 O24 112.06(5) . . ? O21 Dy2 O24 47.21(5) 2_666 . ? O17 Dy2 Dy2 166.74(4) . 2_666 ? O18 Dy2 Dy2 91.50(4) . 2_666 ? O14 Dy2 Dy2 94.54(5) . 2_666 ? O13 Dy2 Dy2 102.52(5) . 2_666 ? O22 Dy2 Dy2 101.43(4) . 2_666 ? O21 Dy2 Dy2 33.08(4) . 2_666 ? O21 Dy2 Dy2 32.41(4) 2_666 2_666 ? O24 Dy2 Dy2 79.27(3) . 2_666 ? O6 Dy1 O5 75.14(6) . . ? O6 Dy1 O2 97.64(6) . . ? O5 Dy1 O2 136.57(6) . . ? O6 Dy1 O1 87.23(6) . . ? O5 Dy1 O1 146.07(6) . . ? O2 Dy1 O1 73.59(6) . . ? O6 Dy1 O9 156.69(6) . 2_777 ? O5 Dy1 O9 96.67(6) . 2_777 ? O2 Dy1 O9 102.94(6) . 2_777 ? O1 Dy1 O9 88.19(6) . 2_777 ? O6 Dy1 O10 84.43(6) . . ? O5 Dy1 O10 77.18(6) . . ? O2 Dy1 O10 145.73(6) . . ? O1 Dy1 O10 72.36(6) . . ? O9 Dy1 O10 72.41(6) 2_777 . ? O6 Dy1 O9 130.13(6) . . ? O5 Dy1 O9 78.02(6) . . ? O2 Dy1 O9 74.81(6) . . ? O1 Dy1 O9 133.61(6) . . ? O9 Dy1 O9 66.96(7) 2_777 . ? O10 Dy1 O9 128.84(6) . . ? O6 Dy1 O12 83.68(6) . . ? O5 Dy1 O12 68.85(6) . . ? O2 Dy1 O12 67.79(6) . . ? O1 Dy1 O12 138.59(6) . . ? O9 Dy1 O12 114.15(5) 2_777 . ? O10 Dy1 O12 145.85(6) . . ? O9 Dy1 O12 47.36(5) . . ? O6 Dy1 Dy1 159.03(5) . 2_777 ? O5 Dy1 Dy1 86.65(4) . 2_777 ? O2 Dy1 Dy1 88.38(4) . 2_777 ? O1 Dy1 Dy1 113.73(5) . 2_777 ? O9 Dy1 Dy1 34.18(4) 2_777 2_777 ? O10 Dy1 Dy1 101.83(4) . 2_777 ? O9 Dy1 Dy1 32.78(4) . 2_777 ? O12 Dy1 Dy1 80.04(3) . 2_777 ? C9 O11 C110 117.0(2) . . ? C7 O12 C120 121.8(2) . . ? C7 O12 Dy1 87.11(13) . . ? C120 O12 Dy1 144.37(15) . . ? C4 O5 Dy1 134.35(17) . . ? C3 O4 C40 118.6(2) . . ? C4 O8 C80 116.44(19) . . ? C13 O16 C160 117.9(2) . . ? C10 O17 Dy2 130.26(16) . . ? C1 O2 Dy1 135.39(17) . . ? C6 O6 Dy1 133.94(16) . . ? C18 O22 Dy2 131.76(16) . . ? C9 O10 Dy1 133.27(17) . . ? C16 O21 Dy2 132.30(16) . . ? C16 O21 Dy2 113.18(15) . 2_666 ? Dy2 O21 Dy2 114.51(7) . 2_666 ? C12 O18 Dy2 130.80(17) . . ? C3 O1 Dy1 135.34(17) . . ? C7 O9 Dy1 134.84(16) . 2_777 ? C7 O9 Dy1 111.27(15) . . ? Dy1 O9 Dy1 113.04(7) 2_777 . ? C6 O7 C70 116.9(2) . . ? C15 O14 Dy2 134.98(17) . . ? C16 O24 C240 122.0(2) 2_666 . ? C16 O24 Dy2 87.22(13) 2_666 . ? C240 O24 Dy2 147.48(15) . . ? C13 O13 Dy2 134.79(17) . . ? C15 O15 C150 118.0(2) . . ? C10 O20 C200 118.5(2) . . ? C12 O19 C190 118.2(2) . . ? O10 C9 O11 120.0(2) . . ? O10 C9 C8 127.3(2) . . ? O11 C9 C8 112.7(2) . . ? C1 O3 C30 118.8(2) . . ? C18 O23 C230 118.1(2) . . ? O21 C16 O24 109.6(2) . 2_666 ? O21 C16 C17 126.3(2) . . ? O24 C16 C17 124.1(2) 2_666 . ? C16 C17 C18 120.9(2) . . ? C16 C17 H17A 119.6 . . ? C18 C17 H17A 119.6 . . ? O24 C240 C241 109.6(2) . . ? O24 C240 C242 105.0(2) . . ? C241 C240 C242 113.5(2) . . ? O24 C240 H24A 109.5 . . ? C241 C240 H24A 109.5 . . ? C242 C240 H24A 109.5 . . ? O9 C7 O12 109.5(2) . . ? O9 C7 C8 126.3(2) . 2_777 ? O12 C7 C8 124.2(2) . 2_777 ? O12 C120 C122 104.7(2) . . ? O12 C120 C121 109.8(2) . . ? C122 C120 C121 112.5(2) . . ? O12 C120 H12A 109.9 . . ? C122 C120 H12A 109.9 . . ? C121 C120 H12A 109.9 . . ? C7 C8 C9 120.8(2) 2_777 . ? C7 C8 H8A 119.6 2_777 . ? C9 C8 H8A 119.6 . . ? O5 C4 O8 118.6(2) . . ? O5 C4 C5 126.6(2) . . ? O8 C4 C5 114.8(2) . . ? O14 C15 O15 118.5(2) . . ? O14 C15 C14 127.1(2) . . ? O15 C15 C14 114.3(2) . . ? O6 C6 O7 117.9(2) . . ? O6 C6 C5 127.1(2) . . ? O7 C6 C5 114.9(2) . . ? O2 C1 O3 119.0(2) . . ? O2 C1 C2 127.2(2) . . ? O3 C1 C2 113.8(2) . . ? O22 C18 O23 119.8(2) . . ? O22 C18 C17 127.6(2) . . ? O23 C18 C17 112.6(2) . . ? O1 C3 O4 118.8(2) . . ? O1 C3 C2 127.4(3) . . ? O4 C3 C2 113.9(2) . . ? O13 C13 O16 119.4(2) . . ? O13 C13 C14 126.3(2) . . ? O16 C13 C14 114.3(2) . . ? C15 C14 C13 121.3(2) . . ? C15 C14 H14A 119.4 . . ? C13 C14 H14A 119.4 . . ? O17 C10 O20 119.0(2) . . ? O17 C10 C11 127.3(2) . . ? O20 C10 C11 113.7(2) . . ? O8 C80 C81 106.4(2) . . ? O8 C80 C82 109.3(2) . . ? C81 C80 C82 113.3(2) . . ? O8 C80 H80A 109.2 . . ? C81 C80 H80A 109.2 . . ? C82 C80 H80A 109.2 . . ? O20 C200 C202 108.9(2) . . ? O20 C200 C201 105.8(2) . . ? C202 C200 C201 114.1(3) . . ? O20 C200 H20A 109.3 . . ? C202 C200 H20A 109.3 . . ? C201 C200 H20A 109.3 . . ? C120 C122 H12B 109.5 . . ? C120 C122 H12C 109.5 . . ? H12B C122 H12C 109.5 . . ? C120 C122 H12D 109.5 . . ? H12B C122 H12D 109.5 . . ? H12C C122 H12D 109.5 . . ? C10 C11 C12 122.2(2) . . ? C10 C11 H11A 118.9 . . ? C12 C11 H11A 118.9 . . ? O18 C12 O19 118.8(2) . . ? O18 C12 C11 127.1(2) . . ? O19 C12 C11 114.1(2) . . ? C6 C5 C4 121.1(2) . . ? C6 C5 H5A 119.4 . . ? C4 C5 H5A 119.4 . . ? O4 C40 C41 110.1(2) . . ? O4 C40 C42 104.9(3) . . ? C41 C40 C42 113.0(3) . . ? O4 C40 H40A 109.6 . . ? C41 C40 H40A 109.6 . . ? C42 C40 H40A 109.6 . . ? O23 C230 C232 108.7(3) . . ? O23 C230 C231 106.1(2) . . ? C232 C230 C231 113.7(3) . . ? O23 C230 H23A 109.4 . . ? C232 C230 H23A 109.4 . . ? C231 C230 H23A 109.4 . . ? C1 C2 C3 120.8(2) . . ? C1 C2 H2A 119.6 . . ? C3 C2 H2A 119.6 . . ? C120 C121 H12E 109.5 . . ? C120 C121 H12F 109.5 . . ? H12E C121 H12F 109.5 . . ? C120 C121 H12G 109.5 . . ? H12E C121 H12G 109.5 . . ? H12F C121 H12G 109.5 . . ? C80 C81 H81A 109.5 . . ? C80 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C80 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C80 C82 H82A 109.5 . . ? C80 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C80 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? O16 C160 C161 109.7(2) . . ? O16 C160 C162 105.5(2) . . ? C161 C160 C162 113.5(3) . . ? O16 C160 H16A 109.3 . . ? C161 C160 H16A 109.3 . . ? C162 C160 H16A 109.3 . . ? O3 C30 C32 108.4(2) . . ? O3 C30 C31 105.8(2) . . ? C32 C30 C31 113.0(3) . . ? O3 C30 H30A 109.8 . . ? C32 C30 H30A 109.8 . . ? C31 C30 H30A 109.8 . . ? O7 C70 C71 110.1(2) . . ? O7 C70 C72 105.3(2) . . ? C71 C70 C72 112.7(3) . . ? O7 C70 H70A 109.5 . . ? C71 C70 H70A 109.5 . . ? C72 C70 H70A 109.5 . . ? C70 C72 H72A 109.5 . . ? C70 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C70 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? O15 C150 C151 106.0(2) . . ? O15 C150 C152 107.9(3) . . ? C151 C150 C152 113.5(3) . . ? O15 C150 H15A 109.8 . . ? C151 C150 H15A 109.8 . . ? C152 C150 H15A 109.8 . . ? C240 C241 H24B 109.5 . . ? C240 C241 H24C 109.5 . . ? H24B C241 H24C 109.5 . . ? C240 C241 H24D 109.5 . . ? H24B C241 H24D 109.5 . . ? H24C C241 H24D 109.5 . . ? C160 C162 H16B 109.5 . . ? C160 C162 H16C 109.5 . . ? H16B C162 H16C 109.5 . . ? C160 C162 H16D 109.5 . . ? H16B C162 H16D 109.5 . . ? H16C C162 H16D 109.5 . . ? C240 C242 H24E 109.5 . . ? C240 C242 H24F 109.5 . . ? H24E C242 H24F 109.5 . . ? C240 C242 H24G 109.5 . . ? H24E C242 H24G 109.5 . . ? H24F C242 H24G 109.5 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O11 C110 C111 109.8(2) . . ? O11 C110 C112 105.0(2) . . ? C111 C110 C112 113.2(3) . . ? O11 C110 H11B 109.6 . . ? C111 C110 H11B 109.6 . . ? C112 C110 H11B 109.6 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C150 C152 H15B 109.5 . . ? C150 C152 H15C 109.5 . . ? H15B C152 H15C 109.5 . . ? C150 C152 H15D 109.5 . . ? H15B C152 H15D 109.5 . . ? H15C C152 H15D 109.5 . . ? C160 C161 H16E 109.5 . . ? C160 C161 H16F 109.5 . . ? H16E C161 H16F 109.5 . . ? C160 C161 H16G 109.5 . . ? H16E C161 H16G 109.5 . . ? H16F C161 H16G 109.5 . . ? C70 C71 H71A 109.5 . . ? C70 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C70 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C110 C111 H11C 109.5 . . ? C110 C111 H11D 109.5 . . ? H11C C111 H11D 109.5 . . ? C110 C111 H11E 109.5 . . ? H11C C111 H11E 109.5 . . ? H11D C111 H11E 109.5 . . ? O19 C190 C192 109.3(3) . . ? O19 C190 C191 105.6(3) . . ? C192 C190 C191 114.4(3) . . ? O19 C190 H19A 109.1 . . ? C192 C190 H19A 109.1 . . ? C191 C190 H19A 109.1 . . ? C230 C231 H23B 109.5 . . ? C230 C231 H23C 109.5 . . ? H23B C231 H23C 109.5 . . ? C230 C231 H23D 109.5 . . ? H23B C231 H23D 109.5 . . ? H23C C231 H23D 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C150 C151 H15E 109.5 . . ? C150 C151 H15F 109.5 . . ? H15E C151 H15F 109.5 . . ? C150 C151 H15G 109.5 . . ? H15E C151 H15G 109.5 . . ? H15F C151 H15G 109.5 . . ? C110 C112 H11F 109.5 . . ? C110 C112 H11G 109.5 . . ? H11F C112 H11G 109.5 . . ? C110 C112 H11H 109.5 . . ? H11F C112 H11H 109.5 . . ? H11G C112 H11H 109.5 . . ? C200 C202 H20B 109.5 . . ? C200 C202 H20C 109.5 . . ? H20B C202 H20C 109.5 . . ? C200 C202 H20D 109.5 . . ? H20B C202 H20D 109.5 . . ? H20C C202 H20D 109.5 . . ? C230 C232 H23E 109.5 . . ? C230 C232 H23F 109.5 . . ? H23E C232 H23F 109.5 . . ? C230 C232 H23G 109.5 . . ? H23E C232 H23G 109.5 . . ? H23F C232 H23G 109.5 . . ? C190 C191 H19B 109.5 . . ? C190 C191 H19C 109.5 . . ? H19B C191 H19C 109.5 . . ? C190 C191 H19D 109.5 . . ? H19B C191 H19D 109.5 . . ? H19C C191 H19D 109.5 . . ? C200 C201 H20E 109.5 . . ? C200 C201 H20F 109.5 . . ? H20E C201 H20F 109.5 . . ? C200 C201 H20G 109.5 . . ? H20E C201 H20G 109.5 . . ? H20F C201 H20G 109.5 . . ? C190 C192 H19E 109.5 . . ? C190 C192 H19F 109.5 . . ? H19E C192 H19F 109.5 . . ? C190 C192 H19G 109.5 . . ? H19E C192 H19G 109.5 . . ? H19F C192 H19G 109.5 . . ? 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 O6 Dy1 O12 C7 -177.91(14) . . . . ? O5 Dy1 O12 C7 105.61(14) . . . . ? O2 Dy1 O12 C7 -76.98(13) . . . . ? O1 Dy1 O12 C7 -99.39(15) . . . . ? O9 Dy1 O12 C7 17.73(14) 2_777 . . . ? O10 Dy1 O12 C7 111.79(15) . . . . ? O9 Dy1 O12 C7 12.52(13) . . . . ? Dy1 Dy1 O12 C7 15.36(12) 2_777 . . . ? O6 Dy1 O12 C120 -31.3(3) . . . . ? O5 Dy1 O12 C120 -107.8(3) . . . . ? O2 Dy1 O12 C120 69.6(3) . . . . ? O1 Dy1 O12 C120 47.2(3) . . . . ? O9 Dy1 O12 C120 164.3(2) 2_777 . . . ? O10 Dy1 O12 C120 -101.6(3) . . . . ? O9 Dy1 O12 C120 159.1(3) . . . . ? Dy1 Dy1 O12 C120 162.0(3) 2_777 . . . ? O6 Dy1 O5 C4 10.1(2) . . . . ? O2 Dy1 O5 C4 95.5(2) . . . . ? O1 Dy1 O5 C4 -51.0(3) . . . . ? O9 Dy1 O5 C4 -147.7(2) 2_777 . . . ? O10 Dy1 O5 C4 -77.5(2) . . . . ? O9 Dy1 O5 C4 147.6(2) . . . . ? O12 Dy1 O5 C4 99.0(2) . . . . ? Dy1 Dy1 O5 C4 179.6(2) 2_777 . . . ? O18 Dy2 O17 C10 25.3(2) . . . . ? O14 Dy2 O17 C10 159.0(2) . . . . ? O13 Dy2 O17 C10 -127.4(2) . . . . ? O22 Dy2 O17 C10 -53.1(2) . . . . ? O21 Dy2 O17 C10 -58.0(3) . . . . ? O21 Dy2 O17 C10 88.2(2) 2_666 . . . ? O24 Dy2 O17 C10 92.7(2) . . . . ? Dy2 Dy2 O17 C10 47.6(3) 2_666 . . . ? O6 Dy1 O2 C1 -90.7(2) . . . . ? O5 Dy1 O2 C1 -167.1(2) . . . . ? O1 Dy1 O2 C1 -5.8(2) . . . . ? O9 Dy1 O2 C1 78.3(2) 2_777 . . . ? O10 Dy1 O2 C1 0.7(3) . . . . ? O9 Dy1 O2 C1 139.7(2) . . . . ? O12 Dy1 O2 C1 -170.6(2) . . . . ? Dy1 Dy1 O2 C1 109.5(2) 2_777 . . . ? O5 Dy1 O6 C6 -14.5(2) . . . . ? O2 Dy1 O6 C6 -150.7(2) . . . . ? O1 Dy1 O6 C6 136.2(2) . . . . ? O9 Dy1 O6 C6 57.3(3) 2_777 . . . ? O10 Dy1 O6 C6 63.7(2) . . . . ? O9 Dy1 O6 C6 -74.2(2) . . . . ? O12 Dy1 O6 C6 -84.2(2) . . . . ? Dy1 Dy1 O6 C6 -45.1(3) 2_777 . . . ? O17 Dy2 O22 C18 -147.5(2) . . . . ? O18 Dy2 O22 C18 134.6(2) . . . . ? O14 Dy2 O22 C18 -71.4(3) . . . . ? O13 Dy2 O22 C18 -54.2(2) . . . . ? O21 Dy2 O22 C18 30.1(2) . . . . ? O21 Dy2 O22 C18 64.8(2) 2_666 . . . ? O24 Dy2 O22 C18 133.4(2) . . . . ? Dy2 Dy2 O22 C18 45.8(2) 2_666 . . . ? O6 Dy1 O10 C9 158.7(2) . . . . ? O5 Dy1 O10 C9 -125.3(2) . . . . ? O2 Dy1 O10 C9 63.3(3) . . . . ? O1 Dy1 O10 C9 69.9(2) . . . . ? O9 Dy1 O10 C9 -23.9(2) 2_777 . . . ? O9 Dy1 O10 C9 -62.4(2) . . . . ? O12 Dy1 O10 C9 -131.2(2) . . . . ? Dy1 Dy1 O10 C9 -41.5(2) 2_777 . . . ? O17 Dy2 O21 C16 -22.9(3) . . . . ? O18 Dy2 O21 C16 -100.7(2) . . . . ? O14 Dy2 O21 C16 116.9(2) . . . . ? O13 Dy2 O21 C16 48.9(2) . . . . ? O22 Dy2 O21 C16 -28.0(2) . . . . ? O21 Dy2 O21 C16 -179.0(3) 2_666 . . . ? O24 Dy2 O21 C16 -171.1(2) . . . . ? Dy2 Dy2 O21 C16 -179.0(3) 2_666 . . . ? O17 Dy2 O21 Dy2 156.12(10) . . . 2_666 ? O18 Dy2 O21 Dy2 78.39(8) . . . 2_666 ? O14 Dy2 O21 Dy2 -64.07(9) . . . 2_666 ? O13 Dy2 O21 Dy2 -132.09(8) . . . 2_666 ? O22 Dy2 O21 Dy2 151.02(9) . . . 2_666 ? O21 Dy2 O21 Dy2 0.0 2_666 . . 2_666 ? O24 Dy2 O21 Dy2 7.97(9) . . . 2_666 ? O17 Dy2 O18 C12 -23.0(2) . . . . ? O14 Dy2 O18 C12 -100.5(2) . . . . ? O13 Dy2 O18 C12 43.4(3) . . . . ? O22 Dy2 O18 C12 60.6(2) . . . . ? O21 Dy2 O18 C12 129.7(2) . . . . ? O21 Dy2 O18 C12 -166.6(2) 2_666 . . . ? O24 Dy2 O18 C12 -120.2(2) . . . . ? Dy2 Dy2 O18 C12 162.0(2) 2_666 . . . ? O6 Dy1 O1 C3 101.5(2) . . . . ? O5 Dy1 O1 C3 159.4(2) . . . . ? O2 Dy1 O1 C3 2.7(2) . . . . ? O9 Dy1 O1 C3 -101.3(2) 2_777 . . . ? O10 Dy1 O1 C3 -173.4(3) . . . . ? O9 Dy1 O1 C3 -46.1(3) . . . . ? O12 Dy1 O1 C3 24.3(3) . . . . ? Dy1 Dy1 O1 C3 -78.0(2) 2_777 . . . ? O6 Dy1 O9 C7 -27.77(18) . . . . ? O5 Dy1 O9 C7 -86.32(16) . . . . ? O2 Dy1 O9 C7 59.45(16) . . . . ? O1 Dy1 O9 C7 107.92(16) . . . . ? O9 Dy1 O9 C7 171.0(2) 2_777 . . . ? O10 Dy1 O9 C7 -148.81(15) . . . . ? O12 Dy1 O9 C7 -14.14(14) . . . . ? Dy1 Dy1 O9 C7 171.0(2) 2_777 . . . ? O6 Dy1 O9 Dy1 161.22(7) . . . 2_777 ? O5 Dy1 O9 Dy1 102.66(8) . . . 2_777 ? O2 Dy1 O9 Dy1 -111.57(8) . . . 2_777 ? O1 Dy1 O9 Dy1 -63.09(11) . . . 2_777 ? O9 Dy1 O9 Dy1 0.000(1) 2_777 . . 2_777 ? O10 Dy1 O9 Dy1 40.18(10) . . . 2_777 ? O12 Dy1 O9 Dy1 174.84(11) . . . 2_777 ? O17 Dy2 O14 C15 101.9(2) . . . . ? O18 Dy2 O14 C15 173.4(2) . . . . ? O13 Dy2 O14 C15 11.3(2) . . . . ? O22 Dy2 O14 C15 28.6(3) . . . . ? O21 Dy2 O14 C15 -60.9(2) . . . . ? O21 Dy2 O14 C15 -118.0(2) 2_666 . . . ? O24 Dy2 O14 C15 -166.6(2) . . . . ? Dy2 Dy2 O14 C15 -90.4(2) 2_666 . . . ? O17 Dy2 O24 C16 174.51(14) . . . 2_666 ? O18 Dy2 O24 C16 -110.94(14) . . . 2_666 ? O14 Dy2 O24 C16 84.85(14) . . . 2_666 ? O13 Dy2 O24 C16 81.74(16) . . . 2_666 ? O22 Dy2 O24 C16 -109.64(15) . . . 2_666 ? O21 Dy2 O24 C16 -19.42(15) . . . 2_666 ? O21 Dy2 O24 C16 -9.52(13) 2_666 . . 2_666 ? Dy2 Dy2 O24 C16 -15.00(13) 2_666 . . 2_666 ? O17 Dy2 O24 C240 19.1(3) . . . . ? O18 Dy2 O24 C240 93.6(3) . . . . ? O14 Dy2 O24 C240 -70.6(3) . . . . ? O13 Dy2 O24 C240 -73.7(3) . . . . ? O22 Dy2 O24 C240 94.9(3) . . . . ? O21 Dy2 O24 C240 -174.8(3) . . . . ? O21 Dy2 O24 C240 -164.9(3) 2_666 . . . ? Dy2 Dy2 O24 C240 -170.4(3) 2_666 . . . ? O17 Dy2 O13 C13 -104.9(2) . . . . ? O18 Dy2 O13 C13 -167.8(2) . . . . ? O14 Dy2 O13 C13 -14.9(2) . . . . ? O22 Dy2 O13 C13 174.8(2) . . . . ? O21 Dy2 O13 C13 100.7(2) . . . . ? O21 Dy2 O13 C13 48.0(2) 2_666 . . . ? O24 Dy2 O13 C13 -11.9(3) . . . . ? Dy2 Dy2 O13 C13 76.2(2) 2_666 . . . ? Dy1 O10 C9 O11 -158.96(17) . . . . ? Dy1 O10 C9 C8 21.3(4) . . . . ? C110 O11 C9 O10 2.3(4) . . . . ? C110 O11 C9 C8 -177.9(2) . . . . ? Dy2 O21 C16 O24 -162.69(14) . . . 2_666 ? Dy2 O21 C16 O24 18.3(2) 2_666 . . 2_666 ? Dy2 O21 C16 C17 18.7(4) . . . . ? Dy2 O21 C16 C17 -160.3(2) 2_666 . . . ? O21 C16 C17 C18 5.8(4) . . . . ? O24 C16 C17 C18 -172.7(2) 2_666 . . . ? C16 O24 C240 C241 81.6(3) 2_666 . . . ? Dy2 O24 C240 C241 -127.7(3) . . . . ? C16 O24 C240 C242 -156.1(2) 2_666 . . . ? Dy2 O24 C240 C242 -5.5(4) . . . . ? Dy1 O9 C7 O12 -167.89(14) 2_777 . . . ? Dy1 O9 C7 O12 23.8(2) . . . . ? Dy1 O9 C7 C8 12.9(4) 2_777 . . 2_777 ? Dy1 O9 C7 C8 -155.4(2) . . . 2_777 ? C120 O12 C7 O9 -176.2(2) . . . . ? Dy1 O12 C7 O9 -18.37(18) . . . . ? C120 O12 C7 C8 3.0(4) . . . 2_777 ? Dy1 O12 C7 C8 160.9(2) . . . 2_777 ? C7 O12 C120 C122 156.3(2) . . . . ? Dy1 O12 C120 C122 16.6(4) . . . . ? C7 O12 C120 C121 -82.6(3) . . . . ? Dy1 O12 C120 C121 137.7(2) . . . . ? O10 C9 C8 C7 -1.0(4) . . . 2_777 ? O11 C9 C8 C7 179.2(2) . . . 2_777 ? Dy1 O5 C4 O8 175.45(15) . . . . ? Dy1 O5 C4 C5 -4.4(4) . . . . ? C80 O8 C4 O5 6.1(3) . . . . ? C80 O8 C4 C5 -174.1(2) . . . . ? Dy2 O14 C15 O15 175.51(16) . . . . ? Dy2 O14 C15 C14 -5.6(4) . . . . ? C150 O15 C15 O14 -17.4(4) . . . . ? C150 O15 C15 C14 163.6(2) . . . . ? Dy1 O6 C6 O7 -168.59(16) . . . . ? Dy1 O6 C6 C5 13.6(4) . . . . ? C70 O7 C6 O6 6.3(3) . . . . ? C70 O7 C6 C5 -175.6(2) . . . . ? Dy1 O2 C1 O3 -174.48(16) . . . . ? Dy1 O2 C1 C2 6.3(4) . . . . ? C30 O3 C1 O2 3.7(4) . . . . ? C30 O3 C1 C2 -177.0(2) . . . . ? Dy2 O22 C18 O23 157.58(17) . . . . ? Dy2 O22 C18 C17 -23.4(4) . . . . ? C230 O23 C18 O22 2.6(4) . . . . ? C230 O23 C18 C17 -176.5(2) . . . . ? C16 C17 C18 O22 -3.4(4) . . . . ? C16 C17 C18 O23 175.6(2) . . . . ? Dy1 O1 C3 O4 179.90(16) . . . . ? Dy1 O1 C3 C2 0.1(4) . . . . ? C40 O4 C3 O1 -3.4(4) . . . . ? C40 O4 C3 C2 176.4(2) . . . . ? Dy2 O13 C13 O16 -167.90(16) . . . . ? Dy2 O13 C13 C14 12.8(4) . . . . ? C160 O16 C13 O13 0.1(3) . . . . ? C160 O16 C13 C14 179.5(2) . . . . ? O14 C15 C14 C13 -4.4(4) . . . . ? O15 C15 C14 C13 174.5(2) . . . . ? O13 C13 C14 C15 0.8(4) . . . . ? O16 C13 C14 C15 -178.5(2) . . . . ? Dy2 O17 C10 O20 159.27(17) . . . . ? Dy2 O17 C10 C11 -21.7(4) . . . . ? C200 O20 C10 O17 -10.1(4) . . . . ? C200 O20 C10 C11 170.8(2) . . . . ? C4 O8 C80 C81 -156.5(2) . . . . ? C4 O8 C80 C82 80.8(3) . . . . ? C10 O20 C200 C202 -87.8(3) . . . . ? C10 O20 C200 C201 149.1(3) . . . . ? O17 C10 C11 C12 1.8(5) . . . . ? O20 C10 C11 C12 -179.2(3) . . . . ? Dy2 O18 C12 O19 -161.62(19) . . . . ? Dy2 O18 C12 C11 16.7(4) . . . . ? C190 O19 C12 O18 1.9(4) . . . . ? C190 O19 C12 C11 -176.7(3) . . . . ? C10 C11 C12 O18 0.8(5) . . . . ? C10 C11 C12 O19 179.2(3) . . . . ? O6 C6 C5 C4 -0.6(4) . . . . ? O7 C6 C5 C4 -178.5(2) . . . . ? O5 C4 C5 C6 -4.0(4) . . . . ? O8 C4 C5 C6 176.2(2) . . . . ? C3 O4 C40 C41 -81.5(3) . . . . ? C3 O4 C40 C42 156.7(2) . . . . ? C18 O23 C230 C232 92.3(3) . . . . ? C18 O23 C230 C231 -145.0(3) . . . . ? O2 C1 C2 C3 -0.8(4) . . . . ? O3 C1 C2 C3 179.9(2) . . . . ? O1 C3 C2 C1 -2.3(4) . . . . ? O4 C3 C2 C1 177.9(2) . . . . ? C13 O16 C160 C161 -86.3(3) . . . . ? C13 O16 C160 C162 151.1(2) . . . . ? C1 O3 C30 C32 94.8(3) . . . . ? C1 O3 C30 C31 -143.8(2) . . . . ? C6 O7 C70 C71 77.6(3) . . . . ? C6 O7 C70 C72 -160.6(2) . . . . ? C15 O15 C150 C151 147.9(3) . . . . ? C15 O15 C150 C152 -90.1(3) . . . . ? C9 O11 C110 C111 -82.5(3) . . . . ? C9 O11 C110 C112 155.5(3) . . . . ? C12 O19 C190 C192 -91.9(4) . . . . ? C12 O19 C190 C191 144.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.530 _refine_diff_density_min -0.793 _refine_diff_density_rms 0.078 #=================================END data_cvd178mp _database_code_depnum_ccdc_archive 'CCDC 770260' #TrackingRef '- combined cif files.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H114 Dy2 O24' _chemical_formula_weight 1616.57 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' 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(1)/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 16.6894(8) _cell_length_b 12.5519(6) _cell_length_c 21.8342(14) _cell_angle_alpha 90.00 _cell_angle_beta 112.437(5) _cell_angle_gamma 90.00 _cell_volume 4227.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 16219 _cell_measurement_theta_min 2.636 _cell_measurement_theta_max 36.829 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.270 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1668 _exptl_absorpt_coefficient_mu 1.817 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.600 _exptl_absorpt_correction_T_max 0.670 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Sapphire2-CCD, Oxford Diffraction' _diffrn_measurement_method '560 images at 1.0 deg. in \w and 15 sec.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41846 _diffrn_reflns_av_R_equivalents 0.0624 _diffrn_reflns_av_sigmaI/netI 0.0534 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 27.57 _reflns_number_total 9651 _reflns_number_gt 6163 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD 1.171.13, Oxford Diffraction' _computing_cell_refinement 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_data_reduction 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0514P)^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 9651 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0546 _refine_ls_R_factor_gt 0.0331 _refine_ls_wR_factor_ref 0.0847 _refine_ls_wR_factor_gt 0.0800 _refine_ls_goodness_of_fit_ref 0.871 _refine_ls_restrained_S_all 0.871 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 1.126443(8) 0.496536(12) 0.525995(7) 0.01251(5) Uani 1 1 d . . . C1 C 1.2275(2) 0.5958(3) 0.67605(17) 0.0191(7) Uani 1 1 d . . . C2 C 1.2169(2) 0.4022(3) 0.67750(17) 0.0181(7) Uani 1 1 d . . . O5 O 0.99609(14) 0.39602(16) 0.50070(11) 0.0142(4) Uani 1 1 d . . . O1 O 1.16581(15) 0.39410(18) 0.61799(11) 0.0197(5) Uani 1 1 d . . . O2 O 1.18100(15) 0.60993(17) 0.61634(11) 0.0189(5) Uani 1 1 d . . . O3 O 1.26461(17) 0.67928(19) 0.71551(12) 0.0274(6) Uani 1 1 d . . . O4 O 1.23862(18) 0.30459(19) 0.70622(12) 0.0291(6) Uani 1 1 d . . . C4 C 1.0073(2) 0.2934(2) 0.50562(16) 0.0157(6) Uani 1 1 d . . . O7 O 0.84265(15) 0.17415(17) 0.55018(12) 0.0218(5) Uani 1 1 d . . . O8 O 1.08211(14) 0.26995(17) 0.49842(11) 0.0183(5) Uani 1 1 d . . . O6 O 0.84708(15) 0.34560(17) 0.52109(11) 0.0184(5) Uani 1 1 d . . . C3 C 1.2478(2) 0.4982(3) 0.71013(16) 0.0222(7) Uani 1 1 d . . . H3A H 1.2831 0.4977 0.7561 0.027 Uiso 1 1 calc R . . C6 C 0.8786(2) 0.2553(3) 0.52930(17) 0.0182(7) Uani 1 1 d . . . C5 C 0.9536(2) 0.2219(3) 0.51831(17) 0.0189(7) Uani 1 1 d . . . H5A H 0.9666 0.1481 0.5198 0.023 Uiso 1 1 calc R . . O9 O 1.11024(14) 0.45133(18) 0.42089(11) 0.0179(5) Uani 1 1 d . . . O10 O 1.26274(14) 0.46166(19) 0.53371(12) 0.0188(5) Uani 1 1 d . . . O12 O 1.13276(16) 0.4322(2) 0.32618(11) 0.0254(6) Uani 1 1 d . . . O11 O 1.38332(15) 0.4351(2) 0.51263(12) 0.0292(6) Uani 1 1 d . . . C7 C 1.1626(2) 0.4426(3) 0.39267(17) 0.0193(7) Uani 1 1 d . . . C9 C 1.2961(2) 0.4477(3) 0.49140(17) 0.0182(7) Uani 1 1 d . . . C41 C 1.3007(3) 0.1571(3) 0.77113(19) 0.0310(9) Uani 1 1 d . . . H41A H 1.2425 0.1294 0.7626 0.046 Uiso 1 1 calc R . . H41B H 1.3413 0.1297 0.8137 0.046 Uiso 1 1 calc R . . H41C H 1.3192 0.1342 0.7356 0.046 Uiso 1 1 calc R . . C80 C 1.1225(2) 0.1632(3) 0.50412(19) 0.0211(7) Uani 1 1 d . . . C110 C 1.4402(2) 0.4421(4) 0.58241(19) 0.0298(9) Uani 1 1 d . . . C70 C 0.7767(2) 0.1934(3) 0.57846(18) 0.0225(8) Uani 1 1 d . . . C8 C 1.2528(2) 0.4416(3) 0.42313(17) 0.0204(7) Uani 1 1 d . . . H8A H 1.2858 0.4365 0.3962 0.024 Uiso 1 1 calc R . . C81 C 1.0662(2) 0.0926(3) 0.44845(19) 0.0266(8) Uani 1 1 d . . . H81A H 1.0552 0.1277 0.4059 0.040 Uiso 1 1 calc R . . H81B H 1.0110 0.0797 0.4533 0.040 Uiso 1 1 calc R . . H81C H 1.0957 0.0246 0.4500 0.040 Uiso 1 1 calc R . . C30 C 1.2612(2) 0.7881(3) 0.69000(18) 0.0248(8) Uani 1 1 d . . . C121 C 0.9937(3) 0.3397(3) 0.3038(2) 0.0370(10) Uani 1 1 d . . . H12A H 0.9938 0.3532 0.3481 0.055 Uiso 1 1 calc R . . H12B H 1.0241 0.2728 0.3042 0.055 Uiso 1 1 calc R . . H12C H 0.9338 0.3347 0.2718 0.055 Uiso 1 1 calc R . . C40 C 1.2992(2) 0.2790(3) 0.77349(18) 0.0264(8) Uani 1 1 d . . . C120 C 1.0393(2) 0.4305(3) 0.28444(17) 0.0254(8) Uani 1 1 d . . . C82 C 1.1443(2) 0.1167(3) 0.57318(19) 0.0317(9) Uani 1 1 d . . . H82A H 1.1810 0.1670 0.6065 0.047 Uiso 1 1 calc R . . H82B H 1.1754 0.0493 0.5770 0.047 Uiso 1 1 calc R . . H82C H 1.0907 0.1041 0.5804 0.047 Uiso 1 1 calc R . . C122 C 0.9985(3) 0.5374(4) 0.2879(2) 0.0398(11) Uani 1 1 d . . . H12D H 0.9990 0.5478 0.3325 0.060 Uiso 1 1 calc R . . H12E H 0.9386 0.5389 0.2556 0.060 Uiso 1 1 calc R . . H12F H 1.0316 0.5946 0.2779 0.060 Uiso 1 1 calc R . . C71 C 0.7646(3) 0.0833(3) 0.6027(2) 0.0329(9) Uani 1 1 d . . . H71A H 0.7412 0.0349 0.5648 0.049 Uiso 1 1 calc R . . H71B H 0.7243 0.0878 0.6255 0.049 Uiso 1 1 calc R . . H71C H 0.8207 0.0564 0.6334 0.049 Uiso 1 1 calc R . . C72 C 0.6926(2) 0.2336(3) 0.5261(2) 0.0317(9) Uani 1 1 d . . . H72A H 0.6717 0.1822 0.4896 0.047 Uiso 1 1 calc R . . H72B H 0.7029 0.3025 0.5091 0.047 Uiso 1 1 calc R . . H72C H 0.6491 0.2422 0.5457 0.047 Uiso 1 1 calc R . . C32 C 1.1695(3) 0.8302(3) 0.66692(19) 0.0303(9) Uani 1 1 d . . . H32A H 1.1323 0.7897 0.6281 0.045 Uiso 1 1 calc R . . H32B H 1.1689 0.9056 0.6552 0.045 Uiso 1 1 calc R . . H32C H 1.1479 0.8225 0.7026 0.045 Uiso 1 1 calc R . . C83 C 1.2055(2) 0.1911(3) 0.4952(2) 0.0351(10) Uani 1 1 d . . . H83A H 1.1916 0.2211 0.4509 0.053 Uiso 1 1 calc R . . H83B H 1.2407 0.1268 0.5003 0.053 Uiso 1 1 calc R . . H83C H 1.2380 0.2437 0.5287 0.053 Uiso 1 1 calc R . . C111 C 1.4381(3) 0.5562(4) 0.6081(3) 0.0594(15) Uani 1 1 d . . . H11A H 1.3810 0.5702 0.6093 0.089 Uiso 1 1 calc R . . H11B H 1.4493 0.6075 0.5784 0.089 Uiso 1 1 calc R . . H11C H 1.4827 0.5634 0.6528 0.089 Uiso 1 1 calc R . . C43 C 1.2640(3) 0.3165(3) 0.8241(2) 0.0361(10) Uani 1 1 d . . . H43A H 1.2634 0.3945 0.8249 0.054 Uiso 1 1 calc R . . H43B H 1.3009 0.2896 0.8680 0.054 Uiso 1 1 calc R . . H43C H 1.2049 0.2895 0.8123 0.054 Uiso 1 1 calc R . . C33 C 1.3207(3) 0.8491(3) 0.7500(2) 0.0361(10) Uani 1 1 d . . . H33A H 1.2975 0.8464 0.7850 0.054 Uiso 1 1 calc R . . H33B H 1.3245 0.9235 0.7376 0.054 Uiso 1 1 calc R . . H33C H 1.3786 0.8170 0.7662 0.054 Uiso 1 1 calc R . . C42 C 1.3898(3) 0.3194(4) 0.7859(2) 0.0414(11) Uani 1 1 d . . . H42A H 1.3902 0.3974 0.7876 0.062 Uiso 1 1 calc R . . H42B H 1.4071 0.2957 0.7500 0.062 Uiso 1 1 calc R . . H42C H 1.4305 0.2912 0.8282 0.062 Uiso 1 1 calc R . . C31 C 1.2977(3) 0.7923(3) 0.6355(2) 0.0344(9) Uani 1 1 d . . . H31A H 1.2593 0.7530 0.5967 0.052 Uiso 1 1 calc R . . H31B H 1.3555 0.7601 0.6518 0.052 Uiso 1 1 calc R . . H31C H 1.3016 0.8667 0.6233 0.052 Uiso 1 1 calc R . . C73 C 0.8124(3) 0.2690(3) 0.63654(19) 0.0338(9) Uani 1 1 d . . . H73A H 0.8663 0.2400 0.6691 0.051 Uiso 1 1 calc R . . H73B H 0.7699 0.2778 0.6571 0.051 Uiso 1 1 calc R . . H73C H 0.8241 0.3383 0.6210 0.051 Uiso 1 1 calc R . . C123 C 1.0402(3) 0.4121(4) 0.21573(18) 0.0383(10) Uani 1 1 d . . . H12G H 1.0700 0.4715 0.2043 0.057 Uiso 1 1 calc R . . H12H H 0.9805 0.4076 0.1832 0.057 Uiso 1 1 calc R . . H12I H 1.0707 0.3454 0.2155 0.057 Uiso 1 1 calc R . . C112 C 1.4184(3) 0.3592(4) 0.6235(2) 0.0474(13) Uani 1 1 d . . . H11D H 1.3616 0.3751 0.6248 0.071 Uiso 1 1 calc R . . H11E H 1.4626 0.3597 0.6686 0.071 Uiso 1 1 calc R . . H11F H 1.4168 0.2887 0.6037 0.071 Uiso 1 1 calc R . . C113 C 1.5289(2) 0.4191(5) 0.5811(2) 0.0516(14) Uani 1 1 d . . . H11G H 1.5303 0.3459 0.5660 0.077 Uiso 1 1 calc R . . H11H H 1.5734 0.4279 0.6257 0.077 Uiso 1 1 calc R . . H11I H 1.5403 0.4688 0.5507 0.077 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.01373(7) 0.01107(8) 0.01393(8) -0.00012(7) 0.00663(5) 0.00008(7) C1 0.0231(18) 0.0173(17) 0.0178(19) -0.0030(14) 0.0088(16) -0.0038(14) C2 0.0231(18) 0.0174(17) 0.0149(18) 0.0037(14) 0.0084(15) 0.0006(14) O5 0.0187(10) 0.0069(9) 0.0186(11) -0.0010(10) 0.0088(8) -0.0005(10) O1 0.0274(13) 0.0147(11) 0.0141(13) 0.0010(10) 0.0047(11) -0.0004(10) O2 0.0250(13) 0.0128(11) 0.0152(13) -0.0023(9) 0.0034(10) -0.0001(9) O3 0.0413(16) 0.0155(12) 0.0200(13) -0.0040(10) 0.0054(12) -0.0063(11) O4 0.0474(17) 0.0153(12) 0.0215(14) 0.0045(11) 0.0095(12) 0.0024(12) C4 0.0202(16) 0.0124(14) 0.0155(17) -0.0017(14) 0.0080(14) 0.0011(13) O7 0.0272(13) 0.0119(11) 0.0349(15) 0.0035(10) 0.0215(12) 0.0007(10) O8 0.0216(12) 0.0089(11) 0.0285(13) -0.0011(10) 0.0141(11) 0.0006(9) O6 0.0250(12) 0.0113(11) 0.0237(13) 0.0012(10) 0.0147(11) 0.0017(9) C3 0.0266(16) 0.0197(16) 0.0144(15) 0.0032(16) 0.0014(12) 0.0016(16) C6 0.0209(16) 0.0167(16) 0.0186(17) 0.0006(14) 0.0095(14) -0.0017(13) C5 0.0254(17) 0.0102(15) 0.0244(19) -0.0011(14) 0.0132(15) -0.0021(13) O9 0.0206(12) 0.0192(12) 0.0143(12) -0.0029(10) 0.0071(10) -0.0037(10) O10 0.0175(11) 0.0213(12) 0.0180(12) 0.0010(10) 0.0074(10) -0.0021(9) O12 0.0259(13) 0.0359(15) 0.0147(13) -0.0019(11) 0.0081(10) -0.0038(11) O11 0.0160(12) 0.0504(17) 0.0210(14) 0.0062(13) 0.0067(11) 0.0047(12) C7 0.0264(18) 0.0113(16) 0.0207(18) 0.0011(14) 0.0097(15) -0.0017(13) C9 0.0179(16) 0.0141(16) 0.0239(19) 0.0011(14) 0.0093(14) 0.0004(13) C41 0.045(2) 0.0213(19) 0.029(2) 0.0090(17) 0.0164(19) 0.0113(17) C80 0.0213(17) 0.0115(16) 0.034(2) 0.0022(15) 0.0147(16) 0.0061(13) C110 0.0128(17) 0.050(3) 0.024(2) 0.0120(19) 0.0040(15) 0.0077(16) C70 0.0281(18) 0.0194(17) 0.030(2) 0.0034(15) 0.0226(17) 0.0015(15) C8 0.0227(17) 0.0192(18) 0.0248(19) -0.0007(15) 0.0152(15) 0.0018(14) C81 0.034(2) 0.0149(17) 0.035(2) -0.0059(16) 0.0170(18) -0.0004(15) C30 0.038(2) 0.0139(16) 0.0234(19) -0.0012(15) 0.0125(17) -0.0064(15) C121 0.042(2) 0.040(2) 0.027(2) -0.0061(19) 0.0115(19) -0.020(2) C40 0.034(2) 0.0220(19) 0.0220(19) 0.0090(15) 0.0098(16) 0.0033(16) C120 0.0292(19) 0.032(2) 0.0142(18) -0.0001(16) 0.0071(15) -0.0066(16) C82 0.032(2) 0.0230(19) 0.037(2) 0.0065(17) 0.0087(18) 0.0074(16) C122 0.036(2) 0.037(2) 0.034(2) 0.0016(19) -0.0002(19) 0.0025(18) C71 0.039(2) 0.0225(19) 0.051(3) 0.0080(18) 0.033(2) 0.0005(17) C72 0.0244(19) 0.033(2) 0.042(2) 0.0068(19) 0.0174(18) -0.0001(17) C32 0.042(2) 0.0184(18) 0.030(2) 0.0004(16) 0.0145(18) -0.0031(16) C83 0.033(2) 0.0169(18) 0.068(3) -0.0005(19) 0.033(2) 0.0032(16) C111 0.040(3) 0.055(3) 0.059(3) -0.018(3) -0.009(2) -0.014(2) C43 0.056(3) 0.025(2) 0.033(2) 0.0052(18) 0.024(2) 0.0046(19) C33 0.050(3) 0.0216(19) 0.032(2) -0.0084(17) 0.010(2) -0.0164(18) C42 0.040(2) 0.037(2) 0.043(3) 0.013(2) 0.012(2) -0.002(2) C31 0.046(2) 0.027(2) 0.036(2) -0.0070(18) 0.022(2) -0.0146(18) C73 0.057(3) 0.026(2) 0.028(2) 0.0002(17) 0.027(2) -0.0018(19) C123 0.037(2) 0.056(3) 0.021(2) 0.000(2) 0.0097(18) -0.013(2) C112 0.027(2) 0.071(3) 0.044(3) 0.035(3) 0.014(2) 0.014(2) C113 0.018(2) 0.102(4) 0.034(3) 0.029(3) 0.0102(18) 0.006(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O10 2.259(2) . ? Dy1 O1 2.261(2) . ? Dy1 O9 2.278(2) . ? Dy1 O2 2.318(2) . ? Dy1 O5 2.330(2) 3_766 ? Dy1 O6 2.351(2) 3_766 ? Dy1 O5 2.390(2) . ? Dy1 Dy1 3.9309(3) 3_766 ? C1 O2 1.250(4) . ? C1 O3 1.348(4) . ? C1 C3 1.406(5) . ? C2 O1 1.257(4) . ? C2 O4 1.361(4) . ? C2 C3 1.395(5) . ? O5 C4 1.301(4) . ? O5 Dy1 2.330(2) 3_766 ? O3 C30 1.468(4) . ? O4 C40 1.466(4) . ? C4 O8 1.348(4) . ? C4 C5 1.370(4) . ? O7 C6 1.347(4) . ? O7 C70 1.473(4) . ? O8 C80 1.483(4) . ? O6 C6 1.234(4) . ? O6 Dy1 2.351(2) 3_766 ? C3 H3A 0.9500 . ? C6 C5 1.423(5) . ? C5 H5A 0.9500 . ? O9 C7 1.252(4) . ? O10 C9 1.260(4) . ? O12 C7 1.349(4) . ? O12 C120 1.476(4) . ? O11 C9 1.357(4) . ? O11 C110 1.458(4) . ? C7 C8 1.394(5) . ? C9 C8 1.389(5) . ? C41 C40 1.531(5) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C80 C81 1.508(5) . ? C80 C83 1.511(5) . ? C80 C82 1.526(5) . ? C110 C112 1.507(6) . ? C110 C113 1.519(5) . ? C110 C111 1.543(7) . ? C70 C73 1.513(5) . ? C70 C72 1.519(5) . ? C70 C71 1.520(5) . ? C8 H8A 0.9500 . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? C30 C32 1.513(5) . ? C30 C33 1.515(5) . ? C30 C31 1.529(5) . ? C121 C120 1.518(5) . ? C121 H12A 0.9800 . ? C121 H12B 0.9800 . ? C121 H12C 0.9800 . ? C40 C43 1.512(5) . ? C40 C42 1.517(5) . ? C120 C122 1.521(6) . ? C120 C123 1.523(5) . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? C122 H12D 0.9800 . ? C122 H12E 0.9800 . ? C122 H12F 0.9800 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C83 H83A 0.9800 . ? C83 H83B 0.9800 . ? C83 H83C 0.9800 . ? C111 H11A 0.9800 . ? C111 H11B 0.9800 . ? C111 H11C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C123 H12G 0.9800 . ? C123 H12H 0.9800 . ? C123 H12I 0.9800 . ? C112 H11D 0.9800 . ? C112 H11E 0.9800 . ? C112 H11F 0.9800 . ? C113 H11G 0.9800 . ? C113 H11H 0.9800 . ? C113 H11I 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 O10 Dy1 O1 83.14(9) . . ? O10 Dy1 O9 75.87(8) . . ? O1 Dy1 O9 129.49(8) . . ? O10 Dy1 O2 89.90(8) . . ? O1 Dy1 O2 72.94(8) . . ? O9 Dy1 O2 150.14(8) . . ? O10 Dy1 O5 153.31(8) . 3_766 ? O1 Dy1 O5 118.75(8) . 3_766 ? O9 Dy1 O5 97.86(8) . 3_766 ? O2 Dy1 O5 83.09(8) . 3_766 ? O10 Dy1 O6 81.02(8) . 3_766 ? O1 Dy1 O6 145.95(8) . 3_766 ? O9 Dy1 O6 74.88(8) . 3_766 ? O2 Dy1 O6 77.07(8) . 3_766 ? O5 Dy1 O6 72.32(7) 3_766 3_766 ? O10 Dy1 O5 135.80(8) . . ? O1 Dy1 O5 80.52(8) . . ? O9 Dy1 O5 83.58(8) . . ? O2 Dy1 O5 123.23(8) . . ? O5 Dy1 O5 67.25(8) 3_766 . ? O6 Dy1 O5 130.57(8) 3_766 . ? O10 Dy1 Dy1 164.92(6) . 3_766 ? O1 Dy1 Dy1 100.66(6) . 3_766 ? O9 Dy1 Dy1 90.75(6) . 3_766 ? O2 Dy1 Dy1 105.18(6) . 3_766 ? O5 Dy1 Dy1 34.11(5) 3_766 3_766 ? O6 Dy1 Dy1 102.44(5) 3_766 3_766 ? O5 Dy1 Dy1 33.14(5) . 3_766 ? O2 C1 O3 120.5(3) . . ? O2 C1 C3 127.2(3) . . ? O3 C1 C3 112.3(3) . . ? O1 C2 O4 111.1(3) . . ? O1 C2 C3 124.8(3) . . ? O4 C2 C3 124.1(3) . . ? C4 O5 Dy1 132.8(2) . 3_766 ? C4 O5 Dy1 114.4(2) . . ? Dy1 O5 Dy1 112.75(8) 3_766 . ? C2 O1 Dy1 136.5(2) . . ? C1 O2 Dy1 133.4(2) . . ? C1 O3 C30 122.6(3) . . ? C2 O4 C40 128.3(3) . . ? O5 C4 O8 108.5(3) . . ? O5 C4 C5 125.5(3) . . ? O8 C4 C5 126.0(3) . . ? C6 O7 C70 121.3(3) . . ? C4 O8 C80 126.8(2) . . ? C6 O6 Dy1 134.2(2) . 3_766 ? C2 C3 C1 121.0(3) . . ? C2 C3 H3A 119.5 . . ? C1 C3 H3A 119.5 . . ? O6 C6 O7 121.5(3) . . ? O6 C6 C5 126.9(3) . . ? O7 C6 C5 111.6(3) . . ? C4 C5 C6 121.8(3) . . ? C4 C5 H5A 119.1 . . ? C6 C5 H5A 119.1 . . ? C7 O9 Dy1 132.9(2) . . ? C9 O10 Dy1 133.4(2) . . ? C7 O12 C120 122.4(3) . . ? C9 O11 C110 122.4(3) . . ? O9 C7 O12 119.8(3) . . ? O9 C7 C8 126.5(3) . . ? O12 C7 C8 113.6(3) . . ? O10 C9 O11 118.8(3) . . ? O10 C9 C8 126.8(3) . . ? O11 C9 C8 114.3(3) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? O8 C80 C81 109.8(3) . . ? O8 C80 C83 100.9(3) . . ? C81 C80 C83 110.6(3) . . ? O8 C80 C82 111.0(3) . . ? C81 C80 C82 114.3(3) . . ? C83 C80 C82 109.3(3) . . ? O11 C110 C112 111.8(3) . . ? O11 C110 C113 102.7(3) . . ? C112 C110 C113 109.8(3) . . ? O11 C110 C111 109.8(3) . . ? C112 C110 C111 112.4(4) . . ? C113 C110 C111 109.9(4) . . ? O7 C70 C73 109.6(3) . . ? O7 C70 C72 111.2(3) . . ? C73 C70 C72 112.2(3) . . ? O7 C70 C71 102.5(3) . . ? C73 C70 C71 109.9(3) . . ? C72 C70 C71 110.9(3) . . ? C9 C8 C7 122.5(3) . . ? C9 C8 H8A 118.8 . . ? C7 C8 H8A 118.8 . . ? C80 C81 H81A 109.5 . . ? C80 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C80 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? O3 C30 C32 109.8(3) . . ? O3 C30 C33 103.0(3) . . ? C32 C30 C33 110.9(3) . . ? O3 C30 C31 111.0(3) . . ? C32 C30 C31 112.4(3) . . ? C33 C30 C31 109.3(3) . . ? C120 C121 H12A 109.5 . . ? C120 C121 H12B 109.5 . . ? H12A C121 H12B 109.5 . . ? C120 C121 H12C 109.5 . . ? H12A C121 H12C 109.5 . . ? H12B C121 H12C 109.5 . . ? O4 C40 C43 110.6(3) . . ? O4 C40 C42 111.4(3) . . ? C43 C40 C42 113.8(3) . . ? O4 C40 C41 101.5(3) . . ? C43 C40 C41 110.6(3) . . ? C42 C40 C41 108.2(3) . . ? O12 C120 C121 111.3(3) . . ? O12 C120 C122 110.1(3) . . ? C121 C120 C122 111.5(3) . . ? O12 C120 C123 101.9(3) . . ? C121 C120 C123 110.8(3) . . ? C122 C120 C123 110.8(3) . . ? C80 C82 H82A 109.5 . . ? C80 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C80 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? C120 C122 H12D 109.5 . . ? C120 C122 H12E 109.5 . . ? H12D C122 H12E 109.5 . . ? C120 C122 H12F 109.5 . . ? H12D C122 H12F 109.5 . . ? H12E C122 H12F 109.5 . . ? C70 C71 H71A 109.5 . . ? C70 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C70 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C70 C72 H72A 109.5 . . ? C70 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C70 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C80 C83 H83A 109.5 . . ? C80 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C80 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? C110 C111 H11A 109.5 . . ? C110 C111 H11B 109.5 . . ? H11A C111 H11B 109.5 . . ? C110 C111 H11C 109.5 . . ? H11A C111 H11C 109.5 . . ? H11B C111 H11C 109.5 . . ? C40 C43 H43A 109.5 . . ? C40 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C70 C73 H73A 109.5 . . ? C70 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C70 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C120 C123 H12G 109.5 . . ? C120 C123 H12H 109.5 . . ? H12G C123 H12H 109.5 . . ? C120 C123 H12I 109.5 . . ? H12G C123 H12I 109.5 . . ? H12H C123 H12I 109.5 . . ? C110 C112 H11D 109.5 . . ? C110 C112 H11E 109.5 . . ? H11D C112 H11E 109.5 . . ? C110 C112 H11F 109.5 . . ? H11D C112 H11F 109.5 . . ? H11E C112 H11F 109.5 . . ? C110 C113 H11G 109.5 . . ? C110 C113 H11H 109.5 . . ? H11G C113 H11H 109.5 . . ? C110 C113 H11I 109.5 . . ? H11G C113 H11I 109.5 . . ? H11H C113 H11I 109.5 . . ? 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 O10 Dy1 O5 C4 17.8(3) . . . . ? O1 Dy1 O5 C4 -52.0(2) . . . . ? O9 Dy1 O5 C4 79.9(2) . . . . ? O2 Dy1 O5 C4 -114.3(2) . . . . ? O5 Dy1 O5 C4 -178.8(3) 3_766 . . . ? O6 Dy1 O5 C4 143.6(2) 3_766 . . . ? Dy1 Dy1 O5 C4 -178.8(3) 3_766 . . . ? O10 Dy1 O5 Dy1 -163.41(9) . . . 3_766 ? O1 Dy1 O5 Dy1 126.79(11) . . . 3_766 ? O9 Dy1 O5 Dy1 -101.33(10) . . . 3_766 ? O2 Dy1 O5 Dy1 64.49(12) . . . 3_766 ? O5 Dy1 O5 Dy1 0.0 3_766 . . 3_766 ? O6 Dy1 O5 Dy1 -37.56(14) 3_766 . . 3_766 ? O4 C2 O1 Dy1 -158.1(2) . . . . ? C3 C2 O1 Dy1 21.7(6) . . . . ? O10 Dy1 O1 C2 69.3(3) . . . . ? O9 Dy1 O1 C2 134.6(3) . . . . ? O2 Dy1 O1 C2 -22.7(3) . . . . ? O5 Dy1 O1 C2 -94.5(3) 3_766 . . . ? O6 Dy1 O1 C2 6.6(4) 3_766 . . . ? O5 Dy1 O1 C2 -151.9(3) . . . . ? Dy1 Dy1 O1 C2 -125.4(3) 3_766 . . . ? O3 C1 O2 Dy1 166.1(2) . . . . ? C3 C1 O2 Dy1 -14.0(6) . . . . ? O10 Dy1 O2 C1 -64.6(3) . . . . ? O1 Dy1 O2 C1 18.2(3) . . . . ? O9 Dy1 O2 C1 -125.1(3) . . . . ? O5 Dy1 O2 C1 141.2(3) 3_766 . . . ? O6 Dy1 O2 C1 -145.5(3) 3_766 . . . ? O5 Dy1 O2 C1 84.2(3) . . . . ? Dy1 Dy1 O2 C1 115.0(3) 3_766 . . . ? O2 C1 O3 C30 -7.2(5) . . . . ? C3 C1 O3 C30 173.0(3) . . . . ? O1 C2 O4 C40 176.9(3) . . . . ? C3 C2 O4 C40 -2.9(6) . . . . ? Dy1 O5 C4 O8 157.79(19) 3_766 . . . ? Dy1 O5 C4 O8 -23.7(3) . . . . ? Dy1 O5 C4 C5 -24.3(5) 3_766 . . . ? Dy1 O5 C4 C5 154.2(3) . . . . ? O5 C4 O8 C80 176.5(3) . . . . ? C5 C4 O8 C80 -1.4(5) . . . . ? O1 C2 C3 C1 -4.4(6) . . . . ? O4 C2 C3 C1 175.4(3) . . . . ? O2 C1 C3 C2 1.4(6) . . . . ? O3 C1 C3 C2 -178.8(3) . . . . ? Dy1 O6 C6 O7 -170.8(2) 3_766 . . . ? Dy1 O6 C6 C5 8.6(6) 3_766 . . . ? C70 O7 C6 O6 -14.0(5) . . . . ? C70 O7 C6 C5 166.5(3) . . . . ? O5 C4 C5 C6 -1.6(6) . . . . ? O8 C4 C5 C6 175.9(3) . . . . ? O6 C6 C5 C4 9.6(6) . . . . ? O7 C6 C5 C4 -171.0(3) . . . . ? O10 Dy1 O9 C7 -14.8(3) . . . . ? O1 Dy1 O9 C7 -83.3(3) . . . . ? O2 Dy1 O9 C7 48.9(4) . . . . ? O5 Dy1 O9 C7 138.7(3) 3_766 . . . ? O6 Dy1 O9 C7 69.5(3) 3_766 . . . ? O5 Dy1 O9 C7 -155.4(3) . . . . ? Dy1 Dy1 O9 C7 172.2(3) 3_766 . . . ? O1 Dy1 O10 C9 145.5(3) . . . . ? O9 Dy1 O10 C9 11.8(3) . . . . ? O2 Dy1 O10 C9 -141.7(3) . . . . ? O5 Dy1 O10 C9 -67.4(4) 3_766 . . . ? O6 Dy1 O10 C9 -64.8(3) 3_766 . . . ? O5 Dy1 O10 C9 76.7(3) . . . . ? Dy1 Dy1 O10 C9 39.8(5) 3_766 . . . ? Dy1 O9 C7 O12 -168.5(2) . . . . ? Dy1 O9 C7 C8 12.1(5) . . . . ? C120 O12 C7 O9 0.0(5) . . . . ? C120 O12 C7 C8 179.5(3) . . . . ? Dy1 O10 C9 O11 175.4(2) . . . . ? Dy1 O10 C9 C8 -5.8(5) . . . . ? C110 O11 C9 O10 -3.0(5) . . . . ? C110 O11 C9 C8 178.1(3) . . . . ? C4 O8 C80 C81 66.4(4) . . . . ? C4 O8 C80 C83 -176.7(3) . . . . ? C4 O8 C80 C82 -60.9(4) . . . . ? C9 O11 C110 C112 60.5(5) . . . . ? C9 O11 C110 C113 178.1(4) . . . . ? C9 O11 C110 C111 -65.0(4) . . . . ? C6 O7 C70 C73 -56.1(4) . . . . ? C6 O7 C70 C72 68.6(4) . . . . ? C6 O7 C70 C71 -172.8(3) . . . . ? O10 C9 C8 C7 -4.9(6) . . . . ? O11 C9 C8 C7 173.9(3) . . . . ? O9 C7 C8 C9 1.7(6) . . . . ? O12 C7 C8 C9 -177.8(3) . . . . ? C1 O3 C30 C32 69.1(4) . . . . ? C1 O3 C30 C33 -172.7(3) . . . . ? C1 O3 C30 C31 -55.8(4) . . . . ? C2 O4 C40 C43 68.4(4) . . . . ? C2 O4 C40 C42 -59.3(5) . . . . ? C2 O4 C40 C41 -174.3(3) . . . . ? C7 O12 C120 C121 -59.2(4) . . . . ? C7 O12 C120 C122 65.0(4) . . . . ? C7 O12 C120 C123 -177.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.57 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 3.064 _refine_diff_density_min -1.288 _refine_diff_density_rms 0.119 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.000 0.500 328 37 ' ' 2 0.500 0.500 1.000 328 37 ' ' _platon_squeeze_details ; ; #=================================END data_cvd157a _database_code_depnum_ccdc_archive 'CCDC 770261' #TrackingRef '- combined cif files.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H114 Dy2 O24 Si12' _chemical_formula_weight 1809.53 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' Si Si 0.0817 0.0704 '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(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.4612(6) _cell_length_b 17.0739(8) _cell_length_c 21.1623(12) _cell_angle_alpha 90.00 _cell_angle_beta 96.932(4) _cell_angle_gamma 90.00 _cell_volume 4469.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 11444 _cell_measurement_theta_min 2.565 _cell_measurement_theta_max 36.961 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.345 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1860 _exptl_absorpt_coefficient_mu 1.879 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.640 _exptl_absorpt_correction_T_max 0.700 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Sapphire2-CCD, Oxford Diffraction' _diffrn_measurement_method '560 images at 1.0 deg. in \w and 15 sec.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36031 _diffrn_reflns_av_R_equivalents 0.0624 _diffrn_reflns_av_sigmaI/netI 0.0812 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7847 _reflns_number_gt 5018 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD 1.171.13, Oxford Diffraction' _computing_cell_refinement 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_data_reduction 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0256P)^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 7847 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0627 _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_ref 0.0581 _refine_ls_wR_factor_gt 0.0544 _refine_ls_goodness_of_fit_ref 0.854 _refine_ls_restrained_S_all 0.854 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.939167(14) 0.605512(11) 0.019064(9) 0.01889(6) Uani 1 1 d . . . Si4 Si 1.32711(8) 0.49838(7) -0.10953(5) 0.0234(3) Uani 1 1 d . . . Si2 Si 1.26498(9) 0.80048(7) 0.07012(5) 0.0288(3) Uani 1 1 d . . . Si5 Si 0.72544(9) 0.53222(7) -0.18707(5) 0.0258(3) Uani 1 1 d . . . C9 C 0.7472(3) 0.7363(2) -0.00794(19) 0.0248(10) Uani 1 1 d . . . C4 C 1.0593(3) 0.6853(2) -0.09771(18) 0.0230(9) Uani 1 1 d . . . C40 C 1.3686(3) 0.3950(2) -0.09772(19) 0.0323(10) Uani 1 1 d . . . H40A H 1.3923 0.3857 -0.0525 0.048 Uiso 1 1 calc R . . H40B H 1.4282 0.3837 -0.1226 0.048 Uiso 1 1 calc R . . H40C H 1.3072 0.3608 -0.1119 0.048 Uiso 1 1 calc R . . C3 C 1.1131(3) 0.7083(2) 0.1174(2) 0.0239(10) Uani 1 1 d . . . C41 C 1.4333(3) 0.5670(2) -0.0741(2) 0.0313(10) Uani 1 1 d . . . H41A H 1.4085 0.6210 -0.0816 0.047 Uiso 1 1 calc R . . H41B H 1.4996 0.5586 -0.0938 0.047 Uiso 1 1 calc R . . H41C H 1.4478 0.5574 -0.0282 0.047 Uiso 1 1 calc R . . C8 C 0.7005(3) 0.7028(2) -0.06528(18) 0.0231(9) Uani 1 1 d . . . H8A H 0.6446 0.7307 -0.0902 0.028 Uiso 1 1 calc R . . C1 C 0.9775(3) 0.6415(2) 0.17292(19) 0.0257(10) Uani 1 1 d . . . C30 C 1.0415(3) 0.8716(3) -0.2192(2) 0.0460(13) Uani 1 1 d . . . H30A H 1.0657 0.8389 -0.2529 0.069 Uiso 1 1 calc R . . H30B H 1.1043 0.8962 -0.1946 0.069 Uiso 1 1 calc R . . H30C H 0.9925 0.9123 -0.2384 0.069 Uiso 1 1 calc R . . C42 C 1.2812(3) 0.5186(2) -0.19474(18) 0.0328(11) Uani 1 1 d . . . H42A H 1.2601 0.5738 -0.1999 0.049 Uiso 1 1 calc R . . H42B H 1.2191 0.4852 -0.2092 0.049 Uiso 1 1 calc R . . H42C H 1.3402 0.5076 -0.2201 0.049 Uiso 1 1 calc R . . C7 C 0.7321(3) 0.6311(2) -0.08717(18) 0.0251(10) Uani 1 1 d . . . C32 C 0.8562(3) 0.7565(3) -0.2124(2) 0.0380(12) Uani 1 1 d . . . H32A H 0.8839 0.7258 -0.2460 0.057 Uiso 1 1 calc R . . H32B H 0.8025 0.7942 -0.2315 0.057 Uiso 1 1 calc R . . H32C H 0.8223 0.7213 -0.1840 0.057 Uiso 1 1 calc R . . C2 C 1.0641(3) 0.6934(2) 0.17263(17) 0.0220(9) Uani 1 1 d . . . H2A H 1.0907 0.7196 0.2110 0.026 Uiso 1 1 calc R . . C22 C 1.3561(3) 0.8714(3) 0.1169(2) 0.0432(13) Uani 1 1 d . . . H22A H 1.3127 0.9103 0.1365 0.065 Uiso 1 1 calc R . . H22B H 1.4013 0.8978 0.0886 0.065 Uiso 1 1 calc R . . H22C H 1.4024 0.8434 0.1502 0.065 Uiso 1 1 calc R . . C51 C 0.6882(3) 0.4415(2) -0.1476(2) 0.0338(11) Uani 1 1 d . . . H51A H 0.7343 0.4354 -0.1070 0.051 Uiso 1 1 calc R . . H51B H 0.6981 0.3965 -0.1750 0.051 Uiso 1 1 calc R . . H51C H 0.6123 0.4445 -0.1397 0.051 Uiso 1 1 calc R . . C52 C 0.8725(3) 0.5351(2) -0.19482(19) 0.0329(11) Uani 1 1 d . . . H52A H 0.8896 0.5837 -0.2161 0.049 Uiso 1 1 calc R . . H52B H 0.8916 0.4901 -0.2200 0.049 Uiso 1 1 calc R . . H52C H 0.9139 0.5329 -0.1524 0.049 Uiso 1 1 calc R . . C10 C 0.9631(4) 0.7742(3) 0.3005(2) 0.0456(13) Uani 1 1 d . . . H10A H 1.0254 0.7914 0.2799 0.068 Uiso 1 1 calc R . . H10B H 0.9703 0.7936 0.3444 0.068 Uiso 1 1 calc R . . H10C H 0.8965 0.7948 0.2770 0.068 Uiso 1 1 calc R . . C70 C 0.8891(4) 0.8873(3) 0.0789(2) 0.0577(14) Uani 1 1 d . . . H70A H 0.9314 0.8401 0.0910 0.087 Uiso 1 1 calc R . . H70B H 0.9047 0.9273 0.1119 0.087 Uiso 1 1 calc R . . H70C H 0.9085 0.9073 0.0384 0.087 Uiso 1 1 calc R . . C20 C 1.1692(3) 0.8521(3) 0.0112(2) 0.0442(12) Uani 1 1 d . . . H20A H 1.1285 0.8907 0.0330 0.066 Uiso 1 1 calc R . . H20B H 1.1190 0.8142 -0.0110 0.066 Uiso 1 1 calc R . . H20C H 1.2092 0.8788 -0.0196 0.066 Uiso 1 1 calc R . . C21 C 1.3446(3) 0.7257(2) 0.0329(2) 0.0392(12) Uani 1 1 d . . . H21A H 1.2954 0.6890 0.0084 0.059 Uiso 1 1 calc R . . H21B H 1.3904 0.6971 0.0661 0.059 Uiso 1 1 calc R . . H21C H 1.3902 0.7514 0.0044 0.059 Uiso 1 1 calc R . . Si1 Si 0.95788(9) 0.66588(7) 0.30099(5) 0.0315(3) Uani 1 1 d . . . Si3 Si 0.96981(9) 0.80992(7) -0.16586(6) 0.0295(3) Uani 1 1 d . . . Si6 Si 0.74337(10) 0.86317(7) 0.07025(6) 0.0399(3) Uani 1 1 d . . . O1 O 0.93661(18) 0.60109(15) 0.12604(11) 0.0222(6) Uani 1 1 d . . . O12 O 0.68634(18) 0.60970(15) -0.14585(11) 0.0235(6) Uani 1 1 d . . . O7 O 1.22096(18) 0.50542(14) -0.06583(11) 0.0181(6) Uani 1 1 d . . . O5 O 0.97880(19) 0.68282(15) -0.06740(11) 0.0233(6) Uani 1 1 d . . . O6 O 1.06730(19) 0.53528(14) -0.03149(11) 0.0189(6) Uani 1 1 d . . . O9 O 0.79915(19) 0.58298(13) -0.05820(11) 0.0204(6) Uani 1 1 d . . . O2 O 1.08763(19) 0.67976(15) 0.06256(12) 0.0221(6) Uani 1 1 d . . . O11 O 0.7063(2) 0.80664(15) 0.00599(12) 0.0306(7) Uani 1 1 d . . . O3 O 1.1968(2) 0.75983(15) 0.12624(12) 0.0292(7) Uani 1 1 d . . . O10 O 0.82380(19) 0.70879(14) 0.03058(11) 0.0229(6) Uani 1 1 d . . . O8 O 1.0682(2) 0.74544(15) -0.13807(12) 0.0278(7) Uani 1 1 d . . . O4 O 0.9304(2) 0.63070(15) 0.22674(11) 0.0274(7) Uani 1 1 d . . . C6 C 1.1427(3) 0.5601(2) -0.06414(17) 0.0224(10) Uani 1 1 d . . . C5 C 1.1446(3) 0.6308(2) -0.09502(18) 0.0226(10) Uani 1 1 d . . . H5A H 1.2062 0.6435 -0.1154 0.027 Uiso 1 1 calc R . . C50 C 0.6434(3) 0.5487(3) -0.2653(2) 0.0415(12) Uani 1 1 d . . . H50A H 0.6669 0.5972 -0.2842 0.062 Uiso 1 1 calc R . . H50B H 0.5669 0.5530 -0.2592 0.062 Uiso 1 1 calc R . . H50C H 0.6532 0.5046 -0.2936 0.062 Uiso 1 1 calc R . . C71 C 0.7072(4) 0.8162(3) 0.1434(2) 0.0604(15) Uani 1 1 d . . . H71A H 0.7538 0.7706 0.1537 0.091 Uiso 1 1 calc R . . H71B H 0.6315 0.7993 0.1367 0.091 Uiso 1 1 calc R . . H71C H 0.7171 0.8538 0.1787 0.091 Uiso 1 1 calc R . . C12 C 1.0842(4) 0.6189(3) 0.3382(2) 0.0459(12) Uani 1 1 d . . . H12A H 1.1452 0.6370 0.3169 0.069 Uiso 1 1 calc R . . H12B H 1.0776 0.5619 0.3341 0.069 Uiso 1 1 calc R . . H12C H 1.0965 0.6330 0.3834 0.069 Uiso 1 1 calc R . . C31 C 0.9215(3) 0.8690(2) -0.1010(2) 0.0371(11) Uani 1 1 d . . . H31A H 0.9828 0.8966 -0.0775 0.056 Uiso 1 1 calc R . . H31B H 0.8884 0.8343 -0.0720 0.056 Uiso 1 1 calc R . . H31C H 0.8679 0.9072 -0.1194 0.056 Uiso 1 1 calc R . . C11 C 0.8396(4) 0.6342(3) 0.3400(2) 0.0617(16) Uani 1 1 d . . . H11A H 0.8362 0.5769 0.3405 0.093 Uiso 1 1 calc R . . H11B H 0.7732 0.6550 0.3163 0.093 Uiso 1 1 calc R . . H11C H 0.8467 0.6541 0.3838 0.093 Uiso 1 1 calc R . . C72 C 0.6587(5) 0.9519(3) 0.0482(3) 0.0726(18) Uani 1 1 d . . . H72A H 0.6807 0.9753 0.0095 0.109 Uiso 1 1 calc R . . H72B H 0.6688 0.9900 0.0830 0.109 Uiso 1 1 calc R . . H72C H 0.5824 0.9367 0.0406 0.109 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.01487(9) 0.02156(10) 0.01959(9) 0.00029(11) -0.00059(6) 0.00004(11) Si4 0.0177(6) 0.0258(7) 0.0274(7) 0.0002(5) 0.0057(5) 0.0004(5) Si2 0.0228(6) 0.0336(7) 0.0301(7) 0.0003(6) 0.0030(5) -0.0080(6) Si5 0.0224(6) 0.0286(7) 0.0252(6) -0.0018(6) -0.0021(5) 0.0002(5) C9 0.020(2) 0.025(2) 0.030(2) 0.004(2) 0.0089(19) 0.0021(19) C4 0.020(2) 0.025(2) 0.022(2) 0.001(2) -0.0052(18) -0.0022(19) C40 0.020(2) 0.031(2) 0.047(3) 0.000(3) 0.0102(18) 0.003(2) C3 0.016(2) 0.020(2) 0.034(3) 0.001(2) -0.0020(19) -0.0001(18) C41 0.022(2) 0.031(2) 0.041(3) 0.001(2) 0.0052(19) -0.003(2) C8 0.017(2) 0.025(2) 0.025(2) 0.000(2) -0.0039(17) 0.0074(19) C1 0.021(2) 0.027(2) 0.028(3) 0.002(2) -0.0014(19) 0.0031(19) C30 0.033(3) 0.054(3) 0.052(3) 0.030(3) 0.008(2) 0.007(2) C42 0.034(3) 0.037(3) 0.030(2) -0.004(2) 0.012(2) -0.001(2) C7 0.016(2) 0.037(3) 0.023(2) 0.004(2) 0.0037(18) -0.0057(19) C32 0.040(3) 0.038(3) 0.034(3) 0.012(2) 0.001(2) -0.002(2) C2 0.022(2) 0.027(2) 0.017(2) -0.0052(19) 0.0005(17) -0.0043(19) C22 0.040(3) 0.051(3) 0.041(3) -0.004(2) 0.011(2) -0.020(2) C51 0.026(2) 0.035(3) 0.039(3) -0.003(2) -0.001(2) -0.001(2) C52 0.035(3) 0.035(3) 0.030(3) -0.003(2) 0.006(2) 0.003(2) C10 0.039(3) 0.058(3) 0.037(3) -0.013(2) -0.006(2) 0.008(2) C70 0.055(3) 0.062(4) 0.054(3) -0.017(3) -0.002(2) -0.012(3) C20 0.036(3) 0.042(3) 0.054(3) 0.008(3) 0.004(2) -0.004(2) C21 0.031(3) 0.044(3) 0.044(3) -0.001(2) 0.006(2) -0.005(2) Si1 0.0286(7) 0.0427(8) 0.0225(7) -0.0068(6) 0.0007(5) -0.0071(6) Si3 0.0242(6) 0.0301(7) 0.0342(7) 0.0120(6) 0.0030(5) 0.0037(6) Si6 0.0428(8) 0.0314(7) 0.0451(8) -0.0104(6) 0.0038(6) 0.0016(6) O1 0.0198(13) 0.0258(15) 0.0199(14) -0.0014(14) -0.0019(11) -0.0056(13) O12 0.0180(12) 0.0323(15) 0.0183(13) -0.0010(14) -0.0050(10) 0.0003(14) O7 0.0159(14) 0.0193(15) 0.0195(15) 0.0017(12) 0.0036(11) 0.0034(12) O5 0.0196(14) 0.0292(16) 0.0213(15) 0.0033(13) 0.0027(12) 0.0024(13) O6 0.0170(13) 0.0240(14) 0.0156(15) -0.0005(12) 0.0010(11) -0.0021(12) O9 0.0206(14) 0.0209(16) 0.0190(14) -0.0001(12) -0.0004(11) -0.0003(12) O2 0.0208(14) 0.0259(16) 0.0192(15) -0.0011(13) 0.0010(12) -0.0037(12) O11 0.0318(16) 0.0231(16) 0.0357(17) -0.0029(14) -0.0008(13) 0.0113(14) O3 0.0226(15) 0.0356(17) 0.0290(16) -0.0043(14) 0.0011(12) -0.0135(13) O10 0.0203(14) 0.0242(15) 0.0234(15) -0.0022(13) -0.0011(12) 0.0046(12) O8 0.0277(16) 0.0267(16) 0.0302(16) 0.0145(14) 0.0077(13) 0.0044(13) O4 0.0258(15) 0.0389(18) 0.0182(15) -0.0041(13) 0.0047(12) -0.0129(13) C6 0.018(2) 0.035(3) 0.014(2) -0.003(2) 0.0011(17) 0.006(2) C5 0.017(2) 0.028(3) 0.023(2) 0.0032(19) 0.0066(17) -0.0025(18) C50 0.041(3) 0.045(3) 0.037(3) -0.003(2) -0.004(2) 0.002(2) C71 0.078(4) 0.055(4) 0.048(3) -0.019(3) 0.006(3) -0.010(3) C12 0.055(3) 0.042(3) 0.037(3) -0.006(2) -0.011(2) 0.004(3) C31 0.034(2) 0.034(3) 0.042(3) 0.006(2) 0.000(2) 0.005(2) C11 0.061(3) 0.095(4) 0.031(3) -0.009(3) 0.011(2) -0.027(3) C72 0.089(4) 0.038(3) 0.090(5) -0.024(3) 0.010(4) 0.013(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 Dy1 O1 2.269(2) . ? Dy1 O9 2.275(2) . ? Dy1 O10 2.307(2) . ? Dy1 O2 2.338(2) . ? Dy1 O6 2.355(2) . ? Dy1 O5 2.356(2) . ? Dy1 O6 2.421(2) 3_765 ? Si4 O7 1.707(3) . ? Si4 C40 1.848(4) . ? Si4 C41 1.856(4) . ? Si4 C42 1.857(4) . ? Si2 O3 1.690(3) . ? Si2 C20 1.842(4) . ? Si2 C21 1.851(4) . ? Si2 C22 1.862(4) . ? Si5 O12 1.688(3) . ? Si5 C51 1.846(4) . ? Si5 C50 1.859(4) . ? Si5 C52 1.861(4) . ? C9 O10 1.268(4) . ? C9 O11 1.351(4) . ? C9 C8 1.403(5) . ? C4 O5 1.255(4) . ? C4 O8 1.349(4) . ? C4 C5 1.409(5) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C3 O2 1.262(4) . ? C3 O3 1.361(4) . ? C3 C2 1.406(5) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C8 C7 1.383(5) . ? C8 H8A 0.9500 . ? C1 O1 1.264(4) . ? C1 O4 1.355(4) . ? C1 C2 1.397(5) . ? C30 Si3 1.850(4) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C7 O9 1.275(4) . ? C7 O12 1.353(4) . ? C32 Si3 1.863(4) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C2 H2A 0.9500 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C10 Si1 1.850(5) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C70 Si6 1.850(5) . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? Si1 O4 1.678(3) . ? Si1 C11 1.855(4) . ? Si1 C12 1.856(4) . ? Si3 O8 1.699(3) . ? Si3 C31 1.860(4) . ? Si6 O11 1.686(3) . ? Si6 C71 1.847(5) . ? Si6 C72 1.872(5) . ? O7 C6 1.353(4) . ? O6 C6 1.303(4) . ? O6 Dy1 2.421(2) 3_765 ? C6 C5 1.375(5) . ? C5 H5A 0.9500 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 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 O1 Dy1 O9 127.54(8) . . ? O1 Dy1 O10 80.57(9) . . ? O9 Dy1 O10 76.79(8) . . ? O1 Dy1 O2 74.39(8) . . ? O9 Dy1 O2 151.21(8) . . ? O10 Dy1 O2 91.00(8) . . ? O1 Dy1 O6 121.89(8) . . ? O9 Dy1 O6 95.20(8) . . ? O10 Dy1 O6 154.53(8) . . ? O2 Dy1 O6 84.68(8) . . ? O1 Dy1 O5 145.37(9) . . ? O9 Dy1 O5 75.59(8) . . ? O10 Dy1 O5 81.11(8) . . ? O2 Dy1 O5 76.82(8) . . ? O6 Dy1 O5 73.46(8) . . ? O1 Dy1 O6 81.60(8) . 3_765 ? O9 Dy1 O6 82.96(8) . 3_765 ? O10 Dy1 O6 135.92(8) . 3_765 ? O2 Dy1 O6 122.06(8) . 3_765 ? O6 Dy1 O6 64.97(9) . 3_765 ? O5 Dy1 O6 130.81(8) . 3_765 ? O7 Si4 C40 102.49(15) . . ? O7 Si4 C41 107.32(16) . . ? C40 Si4 C41 111.96(18) . . ? O7 Si4 C42 110.17(16) . . ? C40 Si4 C42 110.95(19) . . ? C41 Si4 C42 113.32(19) . . ? O3 Si2 C20 109.41(17) . . ? O3 Si2 C21 110.90(17) . . ? C20 Si2 C21 112.2(2) . . ? O3 Si2 C22 102.70(17) . . ? C20 Si2 C22 110.6(2) . . ? C21 Si2 C22 110.6(2) . . ? O12 Si5 C51 108.63(16) . . ? O12 Si5 C50 100.33(17) . . ? C51 Si5 C50 112.9(2) . . ? O12 Si5 C52 111.93(16) . . ? C51 Si5 C52 111.50(19) . . ? C50 Si5 C52 111.05(19) . . ? O10 C9 O11 117.6(3) . . ? O10 C9 C8 127.3(4) . . ? O11 C9 C8 115.0(3) . . ? O5 C4 O8 118.8(3) . . ? O5 C4 C5 127.1(4) . . ? O8 C4 C5 114.1(3) . . ? Si4 C40 H40A 109.5 . . ? Si4 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? Si4 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O2 C3 O3 118.7(3) . . ? O2 C3 C2 127.5(3) . . ? O3 C3 C2 113.9(3) . . ? Si4 C41 H41A 109.5 . . ? Si4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? Si4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C7 C8 C9 123.1(4) . . ? C7 C8 H8A 118.5 . . ? C9 C8 H8A 118.5 . . ? O1 C1 O4 114.3(3) . . ? O1 C1 C2 125.6(4) . . ? O4 C1 C2 120.2(4) . . ? Si3 C30 H30A 109.5 . . ? Si3 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si3 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Si4 C42 H42A 109.5 . . ? Si4 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? Si4 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O9 C7 O12 116.5(3) . . ? O9 C7 C8 127.3(4) . . ? O12 C7 C8 116.2(3) . . ? Si3 C32 H32A 109.5 . . ? Si3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C1 C2 C3 122.1(4) . . ? C1 C2 H2A 119.0 . . ? C3 C2 H2A 119.0 . . ? Si2 C22 H22A 109.5 . . ? Si2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si5 C51 H51A 109.5 . . ? Si5 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? Si5 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? Si5 C52 H52A 109.5 . . ? Si5 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? Si5 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? Si1 C10 H10A 109.5 . . ? Si1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? Si1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? Si6 C70 H70A 109.5 . . ? Si6 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? Si6 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? Si2 C20 H20A 109.5 . . ? Si2 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si2 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si2 C21 H21A 109.5 . . ? Si2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O4 Si1 C10 110.85(17) . . ? O4 Si1 C11 103.26(18) . . ? C10 Si1 C11 108.9(2) . . ? O4 Si1 C12 108.03(17) . . ? C10 Si1 C12 113.9(2) . . ? C11 Si1 C12 111.4(2) . . ? O8 Si3 C30 101.45(16) . . ? O8 Si3 C31 112.34(17) . . ? C30 Si3 C31 111.4(2) . . ? O8 Si3 C32 109.66(17) . . ? C30 Si3 C32 110.4(2) . . ? C31 Si3 C32 111.2(2) . . ? O11 Si6 C71 110.90(18) . . ? O11 Si6 C70 112.19(18) . . ? C71 Si6 C70 110.5(2) . . ? O11 Si6 C72 99.8(2) . . ? C71 Si6 C72 111.9(3) . . ? C70 Si6 C72 111.2(3) . . ? C1 O1 Dy1 135.4(2) . . ? C7 O12 Si5 124.8(2) . . ? C6 O7 Si4 132.1(2) . . ? C4 O5 Dy1 132.2(2) . . ? C6 O6 Dy1 130.4(2) . . ? C6 O6 Dy1 114.6(2) . 3_765 ? Dy1 O6 Dy1 115.03(9) . 3_765 ? C7 O9 Dy1 129.6(2) . . ? C3 O2 Dy1 132.1(2) . . ? C9 O11 Si6 127.6(2) . . ? C3 O3 Si2 127.6(3) . . ? C9 O10 Dy1 130.2(2) . . ? C4 O8 Si3 127.0(2) . . ? C1 O4 Si1 132.7(2) . . ? O6 C6 O7 111.0(3) . . ? O6 C6 C5 126.3(4) . . ? O7 C6 C5 122.7(3) . . ? C6 C5 C4 122.9(3) . . ? C6 C5 H5A 118.5 . . ? C4 C5 H5A 118.5 . . ? Si5 C50 H50A 109.5 . . ? Si5 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? Si5 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? Si6 C71 H71A 109.5 . . ? Si6 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? Si6 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? Si1 C12 H12A 109.5 . . ? Si1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si3 C31 H31A 109.5 . . ? Si3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si1 C11 H11A 109.5 . . ? Si1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si6 C72 H72A 109.5 . . ? Si6 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? Si6 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? 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 O10 C9 C8 C7 1.7(6) . . . . ? O11 C9 C8 C7 -179.9(3) . . . . ? C9 C8 C7 O9 5.8(6) . . . . ? C9 C8 C7 O12 -174.4(3) . . . . ? O1 C1 C2 C3 2.5(6) . . . . ? O4 C1 C2 C3 -178.0(3) . . . . ? O2 C3 C2 C1 0.9(6) . . . . ? O3 C3 C2 C1 -179.3(3) . . . . ? O4 C1 O1 Dy1 162.3(2) . . . . ? C2 C1 O1 Dy1 -18.1(6) . . . . ? O9 Dy1 O1 C1 -139.6(3) . . . . ? O10 Dy1 O1 C1 -74.4(3) . . . . ? O2 Dy1 O1 C1 19.3(3) . . . . ? O6 Dy1 O1 C1 92.6(3) . . . . ? O5 Dy1 O1 C1 -15.5(4) . . . . ? O6 Dy1 O1 C1 146.1(3) 3_765 . . . ? O9 C7 O12 Si5 -9.9(4) . . . . ? C8 C7 O12 Si5 170.3(2) . . . . ? C51 Si5 O12 C7 69.7(3) . . . . ? C50 Si5 O12 C7 -171.7(3) . . . . ? C52 Si5 O12 C7 -53.8(3) . . . . ? C40 Si4 O7 C6 -165.4(3) . . . . ? C41 Si4 O7 C6 76.6(3) . . . . ? C42 Si4 O7 C6 -47.3(4) . . . . ? O8 C4 O5 Dy1 -168.3(2) . . . . ? C5 C4 O5 Dy1 12.1(6) . . . . ? O1 Dy1 O5 C4 99.2(3) . . . . ? O9 Dy1 O5 C4 -123.5(3) . . . . ? O10 Dy1 O5 C4 157.9(3) . . . . ? O2 Dy1 O5 C4 64.8(3) . . . . ? O6 Dy1 O5 C4 -23.5(3) . . . . ? O6 Dy1 O5 C4 -56.4(3) 3_765 . . . ? O1 Dy1 O6 C6 -117.2(3) . . . . ? O9 Dy1 O6 C6 101.8(3) . . . . ? O10 Dy1 O6 C6 31.8(4) . . . . ? O2 Dy1 O6 C6 -49.3(3) . . . . ? O5 Dy1 O6 C6 28.5(3) . . . . ? O6 Dy1 O6 C6 -178.5(3) 3_765 . . . ? O1 Dy1 O6 Dy1 61.28(13) . . . 3_765 ? O9 Dy1 O6 Dy1 -79.73(10) . . . 3_765 ? O10 Dy1 O6 Dy1 -149.70(15) . . . 3_765 ? O2 Dy1 O6 Dy1 129.19(11) . . . 3_765 ? O5 Dy1 O6 Dy1 -153.01(12) . . . 3_765 ? O6 Dy1 O6 Dy1 0.0 3_765 . . 3_765 ? O12 C7 O9 Dy1 154.6(2) . . . . ? C8 C7 O9 Dy1 -25.7(5) . . . . ? O1 Dy1 O9 C7 92.4(3) . . . . ? O10 Dy1 O9 C7 25.5(3) . . . . ? O2 Dy1 O9 C7 -41.6(4) . . . . ? O6 Dy1 O9 C7 -130.0(3) . . . . ? O5 Dy1 O9 C7 -58.6(3) . . . . ? O6 Dy1 O9 C7 166.1(3) 3_765 . . . ? O3 C3 O2 Dy1 -169.7(2) . . . . ? C2 C3 O2 Dy1 10.0(6) . . . . ? O1 Dy1 O2 C3 -14.8(3) . . . . ? O9 Dy1 O2 C3 128.8(3) . . . . ? O10 Dy1 O2 C3 65.1(3) . . . . ? O6 Dy1 O2 C3 -140.1(3) . . . . ? O5 Dy1 O2 C3 145.7(3) . . . . ? O6 Dy1 O2 C3 -84.1(3) 3_765 . . . ? O10 C9 O11 Si6 -1.2(5) . . . . ? C8 C9 O11 Si6 -179.7(3) . . . . ? C71 Si6 O11 C9 -67.4(4) . . . . ? C70 Si6 O11 C9 56.6(4) . . . . ? C72 Si6 O11 C9 174.5(3) . . . . ? O2 C3 O3 Si2 8.0(5) . . . . ? C2 C3 O3 Si2 -171.8(3) . . . . ? C20 Si2 O3 C3 56.7(3) . . . . ? C21 Si2 O3 C3 -67.7(3) . . . . ? C22 Si2 O3 C3 174.2(3) . . . . ? O11 C9 O10 Dy1 -167.2(2) . . . . ? C8 C9 O10 Dy1 11.1(6) . . . . ? O1 Dy1 O10 C9 -151.1(3) . . . . ? O9 Dy1 O10 C9 -18.7(3) . . . . ? O2 Dy1 O10 C9 134.9(3) . . . . ? O6 Dy1 O10 C9 55.2(4) . . . . ? O5 Dy1 O10 C9 58.4(3) . . . . ? O6 Dy1 O10 C9 -83.7(3) 3_765 . . . ? O5 C4 O8 Si3 -14.3(5) . . . . ? C5 C4 O8 Si3 165.4(3) . . . . ? C30 Si3 O8 C4 -178.5(3) . . . . ? C31 Si3 O8 C4 62.5(3) . . . . ? C32 Si3 O8 C4 -61.8(3) . . . . ? O1 C1 O4 Si1 176.4(2) . . . . ? C2 C1 O4 Si1 -3.2(6) . . . . ? C10 Si1 O4 C1 54.3(4) . . . . ? C11 Si1 O4 C1 170.8(4) . . . . ? C12 Si1 O4 C1 -71.2(4) . . . . ? Dy1 O6 C6 O7 158.4(2) . . . . ? Dy1 O6 C6 O7 -20.1(3) 3_765 . . . ? Dy1 O6 C6 C5 -23.3(5) . . . . ? Dy1 O6 C6 C5 158.2(3) 3_765 . . . ? Si4 O7 C6 O6 169.1(2) . . . . ? Si4 O7 C6 C5 -9.3(5) . . . . ? O6 C6 C5 C4 -3.4(6) . . . . ? O7 C6 C5 C4 174.8(3) . . . . ? O5 C4 C5 C6 9.4(6) . . . . ? O8 C4 C5 C6 -170.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.728 _refine_diff_density_min -0.702 _refine_diff_density_rms 0.093 #=================================END data_cvd301a _database_code_depnum_ccdc_archive 'CCDC 770262' #TrackingRef '- combined cif files.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H41 Dy N2 O12' _chemical_formula_weight 796.16 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' 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(1)/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 11.0467(3) _cell_length_b 23.9085(7) _cell_length_c 12.9670(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.412(3) _cell_angle_gamma 90.00 _cell_volume 3409.45(17) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 7306 _cell_measurement_theta_min 2.553 _cell_measurement_theta_max 28.611 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.551 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1612 _exptl_absorpt_coefficient_mu 2.254 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.650 _exptl_absorpt_correction_T_max 0.870 _exptl_absorpt_process_details abspack _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Sapphire2-CCD, Oxford Diffraction' _diffrn_measurement_method '460 images at 1.0 deg. in \w and 40 sec.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23807 _diffrn_reflns_av_R_equivalents 0.0486 _diffrn_reflns_av_sigmaI/netI 0.0761 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5994 _reflns_number_gt 4012 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD 171_33_34d, Oxford Diffraction' _computing_cell_refinement 'CrysAlis RED 171_33_34d, Oxford Diffraction' _computing_data_reduction 'CrysAlis RED 171_33_34d, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0165P)^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 5994 _refine_ls_number_parameters 410 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0512 _refine_ls_R_factor_gt 0.0269 _refine_ls_wR_factor_ref 0.0451 _refine_ls_wR_factor_gt 0.0432 _refine_ls_goodness_of_fit_ref 0.804 _refine_ls_restrained_S_all 0.804 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.337665(17) 0.387727(7) 0.774323(13) 0.02975(6) Uani 1 1 d . . . N1 N 0.5278(2) 0.38422(13) 0.90716(19) 0.0321(7) Uani 1 1 d . . . O1 O 0.1446(2) 0.35472(9) 0.72817(18) 0.0382(6) Uiso 1 1 d . . . C1 C 0.0590(3) 0.37214(14) 0.6675(3) 0.0364(10) Uiso 1 1 d . . . N2 N 0.4749(3) 0.47519(11) 0.7856(2) 0.0302(8) Uani 1 1 d . . . O2 O 0.2795(2) 0.42428(9) 0.60926(17) 0.0361(6) Uani 1 1 d . . . O3 O 0.1665(2) 0.46258(11) 0.47397(19) 0.0487(7) Uani 1 1 d . . . O4 O -0.0560(2) 0.35447(11) 0.6804(2) 0.0530(8) Uani 1 1 d . . . O5 O 0.2589(2) 0.37568(9) 0.93329(16) 0.0343(6) Uani 1 1 d . . . O6 O 0.2267(2) 0.46733(9) 0.80771(18) 0.0368(6) Uani 1 1 d . . . O7 O 0.0676(2) 0.52131(10) 0.83408(19) 0.0422(7) Uani 1 1 d . . . O8 O 0.1040(2) 0.36015(10) 1.0302(2) 0.0497(7) Uani 1 1 d . . . O9 O 0.4863(2) 0.35540(9) 0.67174(17) 0.0351(6) Uani 1 1 d . . . O10 O 0.3547(2) 0.29173(10) 0.80170(18) 0.0443(7) Uani 1 1 d . A . O12 O 0.6006(2) 0.30360(10) 0.5735(2) 0.0481(7) Uani 1 1 d . . . C2 C 0.0661(3) 0.40845(15) 0.5835(3) 0.0395(10) Uani 1 1 d . . . H2 H -0.0059 0.4183 0.5415 0.047 Uiso 1 1 calc R . . C3 C 0.1777(4) 0.43043(15) 0.5607(3) 0.0361(10) Uani 1 1 d . . . C4 C 0.1597(3) 0.39175(16) 0.9622(2) 0.0327(8) Uani 1 1 d . . . C6 C 0.1362(4) 0.47478(15) 0.8563(3) 0.0348(9) Uani 1 1 d . . . C7 C 0.5230(3) 0.30757(16) 0.6483(3) 0.0365(10) Uani 1 1 d . . . C8 C 0.4928(4) 0.25627(15) 0.6888(3) 0.0495(12) Uani 1 1 d . A . H8 H 0.5286 0.2230 0.6653 0.059 Uiso 1 1 calc R . . C31 C 0.2734(4) 0.48893(18) 0.4429(3) 0.0568(12) Uani 1 1 d . . . H31A H 0.3392 0.4610 0.4398 0.068 Uiso 1 1 calc R . . H31B H 0.3018 0.5183 0.4934 0.068 Uiso 1 1 calc R . . C32 C 0.2423(4) 0.51432(16) 0.3383(3) 0.0565(12) Uani 1 1 d . . . H32A H 0.2179 0.4848 0.2882 0.085 Uiso 1 1 calc R . . H32B H 0.3135 0.5340 0.3166 0.085 Uiso 1 1 calc R . . H32C H 0.1752 0.5409 0.3416 0.085 Uiso 1 1 calc R . . C5 C 0.0959(3) 0.44097(15) 0.9334(3) 0.0387(10) Uani 1 1 d . . . H35 H 0.0258 0.4511 0.9663 0.046 Uiso 1 1 calc R . . C41 C -0.0688(4) 0.3215(2) 0.7724(3) 0.0760(16) Uani 1 1 d . . . H41A H -0.0033 0.2931 0.7805 0.091 Uiso 1 1 calc R . . H41B H -0.0603 0.3461 0.8341 0.091 Uiso 1 1 calc R . . C42 C -0.1785(6) 0.2956(3) 0.7664(4) 0.143(3) Uani 1 1 d . . . H42A H -0.2429 0.3237 0.7686 0.214 Uiso 1 1 calc R . . H42B H -0.1811 0.2699 0.8250 0.214 Uiso 1 1 calc R . . H42C H -0.1908 0.2746 0.7014 0.214 Uiso 1 1 calc R . . C71 C 0.0997(4) 0.55378(16) 0.7473(3) 0.0571(12) Uani 1 1 d . . . H71A H 0.0925 0.5306 0.6838 0.069 Uiso 1 1 calc R . . H71B H 0.1849 0.5669 0.7599 0.069 Uiso 1 1 calc R . . C72 C 0.0160(4) 0.60243(16) 0.7343(3) 0.0603(12) Uani 1 1 d . . . H72A H -0.0676 0.5891 0.7185 0.090 Uiso 1 1 calc R . . H72B H 0.0388 0.6259 0.6772 0.090 Uiso 1 1 calc R . . H72C H 0.0216 0.6244 0.7984 0.090 Uiso 1 1 calc R . . C81 C 0.1548(4) 0.30555(17) 1.0542(3) 0.0625(13) Uani 1 1 d . . . H81A H 0.2060 0.2939 0.9993 0.075 Uiso 1 1 calc R . . H81B H 0.2068 0.3070 1.1206 0.075 Uiso 1 1 calc R . . C82 C 0.0592(5) 0.2658(2) 1.0616(5) 0.135(3) Uani 1 1 d . . . H82A H -0.0032 0.2821 1.1015 0.202 Uiso 1 1 calc R . . H82B H 0.0922 0.2320 1.0965 0.202 Uiso 1 1 calc R . . H82C H 0.0230 0.2562 0.9920 0.202 Uiso 1 1 calc R . . C111 C 0.5639(4) 0.33672(15) 0.9558(3) 0.0386(10) Uani 1 1 d . . . H111 H 0.5093 0.3059 0.9523 0.046 Uiso 1 1 calc R . . C112 C 0.6759(4) 0.33028(16) 1.0105(3) 0.0478(11) Uani 1 1 d . . . H112 H 0.6980 0.2958 1.0435 0.057 Uiso 1 1 calc R . . C113 C 0.7548(4) 0.37442(16) 1.0165(3) 0.0512(12) Uani 1 1 d . . . H113 H 0.8333 0.3707 1.0526 0.061 Uiso 1 1 calc R . . C114 C 0.7195(4) 0.42446(15) 0.9698(3) 0.0434(10) Uani 1 1 d . . . H114 H 0.7726 0.4558 0.9742 0.052 Uiso 1 1 calc R . . C115 C 0.6050(3) 0.42799(15) 0.9164(3) 0.0331(9) Uani 1 1 d . . . C121 C 0.6448(4) 0.35473(15) 0.5315(3) 0.0472(11) Uani 1 1 d . . . H12A H 0.6920 0.3764 0.5866 0.057 Uiso 1 1 calc R . . H12B H 0.5757 0.3780 0.5022 0.057 Uiso 1 1 calc R . . C122 C 0.7238(4) 0.33900(18) 0.4487(3) 0.0610(13) Uani 1 1 d . . . H12C H 0.7935 0.3173 0.4792 0.092 Uiso 1 1 calc R . . H12D H 0.7528 0.3730 0.4166 0.092 Uiso 1 1 calc R . . H12E H 0.6768 0.3164 0.3961 0.092 Uiso 1 1 calc R . . C211 C 0.4384(3) 0.52124(15) 0.7331(3) 0.0369(10) Uani 1 1 d . . . H211 H 0.3770 0.5177 0.6770 0.044 Uiso 1 1 calc R . . C212 C 0.4857(3) 0.57363(14) 0.7566(3) 0.0415(10) Uani 1 1 d . . . H212 H 0.4595 0.6052 0.7160 0.050 Uiso 1 1 calc R . . C213 C 0.5710(4) 0.57924(15) 0.8393(3) 0.0458(11) Uani 1 1 d . . . H213 H 0.6030 0.6150 0.8588 0.055 Uiso 1 1 calc R . . C214 C 0.6100(3) 0.53223(14) 0.8941(3) 0.0384(10) Uani 1 1 d . . . H214 H 0.6690 0.5352 0.9521 0.046 Uiso 1 1 calc R . . C215 C 0.5623(3) 0.48063(14) 0.8639(3) 0.0290(9) Uani 1 1 d . . . C9 C 0.4117(4) 0.25315(16) 0.7622(3) 0.0492(12) Uani 1 1 d . . . O11 O 0.3718(6) 0.19972(19) 0.7759(6) 0.033(2) Uiso 0.494(13) 1 d P A 1 C11 C 0.2713(13) 0.1895(4) 0.8407(9) 0.063(3) Uiso 0.494(13) 1 d P A 1 H11A H 0.2116 0.2205 0.8321 0.076 Uiso 0.494(13) 1 calc PR A 1 H11B H 0.2291 0.1542 0.8194 0.076 Uiso 0.494(13) 1 calc PR A 1 C12 C 0.3207(12) 0.1858(5) 0.9476(11) 0.091(5) Uiso 0.494(13) 1 d P A 1 H12F H 0.3758 0.1537 0.9563 0.136 Uiso 0.494(13) 1 calc PR A 1 H12G H 0.2543 0.1811 0.9919 0.136 Uiso 0.494(13) 1 calc PR A 1 H12H H 0.3656 0.2201 0.9671 0.136 Uiso 0.494(13) 1 calc PR A 1 O119 O 0.4200(7) 0.20075(19) 0.8196(6) 0.036(2) Uiso 0.506(13) 1 d P A 2 C119 C 0.3401(9) 0.1927(4) 0.8976(9) 0.049(3) Uiso 0.506(13) 1 d P A 2 H11C H 0.3459 0.2257 0.9439 0.059 Uiso 0.506(13) 1 calc PR A 2 H11D H 0.3683 0.1598 0.9396 0.059 Uiso 0.506(13) 1 calc PR A 2 C129 C 0.2152(14) 0.1844(5) 0.8610(11) 0.104(5) Uiso 0.506(13) 1 d P A 2 H12I H 0.1799 0.2199 0.8353 0.155 Uiso 0.506(13) 1 calc PR A 2 H12J H 0.1707 0.1708 0.9179 0.155 Uiso 0.506(13) 1 calc PR A 2 H12K H 0.2094 0.1569 0.8048 0.155 Uiso 0.506(13) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.03257(9) 0.02317(9) 0.03505(9) -0.00198(10) 0.01121(7) -0.00035(11) N1 0.0367(17) 0.0269(17) 0.0342(16) 0.0039(16) 0.0119(14) 0.0015(17) N2 0.0331(19) 0.0258(18) 0.0326(18) 0.0025(14) 0.0081(16) -0.0039(15) O2 0.0359(16) 0.0380(15) 0.0355(15) 0.0010(12) 0.0091(13) -0.0016(13) O3 0.0412(18) 0.0659(19) 0.0405(16) 0.0213(14) 0.0116(14) -0.0056(15) O4 0.0393(17) 0.067(2) 0.0536(17) 0.0101(15) 0.0082(15) -0.0163(15) O5 0.0347(15) 0.0334(16) 0.0360(14) -0.0020(11) 0.0098(12) 0.0022(12) O6 0.0385(17) 0.0281(15) 0.0461(16) 0.0020(12) 0.0171(14) 0.0049(13) O7 0.0452(17) 0.0330(15) 0.0508(17) 0.0069(13) 0.0165(14) 0.0127(13) O8 0.0568(19) 0.0322(16) 0.0652(18) 0.0126(13) 0.0326(16) 0.0066(14) O9 0.0380(16) 0.0267(14) 0.0432(15) 0.0001(12) 0.0182(13) 0.0004(12) O10 0.0536(19) 0.0231(14) 0.0611(19) -0.0020(12) 0.0308(16) 0.0011(14) O12 0.0564(19) 0.0395(17) 0.0541(17) 0.0007(13) 0.0342(16) 0.0064(14) C2 0.034(2) 0.049(3) 0.036(2) 0.0048(18) 0.0027(19) 0.000(2) C3 0.045(3) 0.035(2) 0.030(2) -0.0040(18) 0.011(2) 0.000(2) C4 0.038(2) 0.034(2) 0.0268(19) -0.009(2) 0.0077(17) -0.005(2) C6 0.035(2) 0.029(2) 0.041(2) -0.0043(19) 0.007(2) -0.002(2) C7 0.031(2) 0.035(2) 0.045(2) -0.011(2) 0.013(2) 0.002(2) C8 0.066(3) 0.021(2) 0.068(3) -0.005(2) 0.042(3) 0.005(2) C31 0.052(3) 0.062(3) 0.059(3) 0.018(2) 0.019(3) -0.006(2) C32 0.071(3) 0.057(3) 0.045(3) 0.012(2) 0.024(2) -0.006(2) C5 0.036(2) 0.032(2) 0.051(3) -0.011(2) 0.018(2) 0.003(2) C41 0.065(4) 0.101(4) 0.063(3) 0.018(3) 0.013(3) -0.042(3) C42 0.156(7) 0.193(7) 0.076(4) 0.050(4) -0.007(4) -0.096(6) C71 0.071(3) 0.042(3) 0.062(3) 0.011(2) 0.021(3) 0.020(2) C72 0.075(3) 0.047(3) 0.059(3) 0.006(2) 0.009(2) 0.014(3) C81 0.068(3) 0.044(3) 0.080(3) 0.026(2) 0.029(3) 0.014(3) C82 0.119(6) 0.041(3) 0.243(8) 0.040(4) 0.011(5) -0.009(4) C111 0.048(3) 0.029(2) 0.040(2) 0.0023(19) 0.015(2) 0.000(2) C112 0.057(3) 0.039(3) 0.047(3) 0.013(2) 0.000(2) 0.008(2) C113 0.047(3) 0.049(3) 0.056(3) 0.006(2) -0.005(2) 0.001(2) C114 0.044(3) 0.032(2) 0.053(3) 0.003(2) -0.002(2) -0.006(2) C115 0.040(2) 0.028(2) 0.032(2) 0.0000(17) 0.009(2) -0.0002(19) C121 0.053(3) 0.041(3) 0.051(3) 0.007(2) 0.023(2) -0.002(2) C122 0.059(3) 0.071(3) 0.059(3) 0.015(2) 0.033(3) 0.013(3) C211 0.037(2) 0.032(2) 0.041(2) 0.0071(19) 0.002(2) -0.001(2) C212 0.046(3) 0.023(2) 0.055(3) 0.0077(19) 0.007(2) -0.001(2) C213 0.058(3) 0.023(2) 0.058(3) -0.003(2) 0.012(2) -0.008(2) C214 0.048(3) 0.030(2) 0.037(2) -0.0021(18) 0.002(2) -0.005(2) C215 0.031(2) 0.024(2) 0.034(2) 0.0005(17) 0.0147(19) -0.0021(17) C9 0.061(3) 0.015(2) 0.076(3) -0.002(2) 0.030(3) -0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O1 2.300(2) . ? Dy1 O6 2.327(2) . ? Dy1 O10 2.327(2) . ? Dy1 O5 2.330(2) . ? Dy1 O9 2.340(2) . ? Dy1 O2 2.345(2) . ? Dy1 N2 2.579(3) . ? Dy1 N1 2.589(3) . ? N1 C111 1.341(4) . ? N1 C115 1.348(4) . ? O1 C1 1.244(4) . ? C1 O4 1.364(4) . ? C1 C2 1.400(4) . ? N2 C211 1.337(4) . ? N2 C215 1.340(4) . ? O2 C3 1.245(4) . ? O3 C3 1.359(4) . ? O3 C31 1.430(4) . ? O4 C41 1.448(4) . ? O5 C4 1.251(4) . ? O6 C6 1.244(4) . ? O7 C6 1.361(4) . ? O7 C71 1.439(4) . ? O8 C4 1.352(4) . ? O8 C81 1.443(4) . ? O9 C7 1.260(4) . ? O10 C9 1.253(4) . ? O12 C7 1.357(4) . ? O12 C121 1.442(4) . ? C2 C3 1.397(5) . ? C2 H2 0.9500 . ? C4 C5 1.404(5) . ? C6 C5 1.391(5) . ? C7 C8 1.387(5) . ? C8 C9 1.370(5) . ? C8 H8 0.9500 . ? C31 C32 1.496(5) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C5 H35 0.9500 . ? C41 C42 1.357(6) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C71 C72 1.486(5) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C81 C82 1.431(6) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? C111 C112 1.376(5) . ? C111 H111 0.9500 . ? C112 C113 1.366(5) . ? C112 H112 0.9500 . ? C113 C114 1.381(5) . ? C113 H113 0.9500 . ? C114 C115 1.386(5) . ? C114 H114 0.9500 . ? C115 C215 1.486(4) . ? C121 C122 1.494(5) . ? C121 H12A 0.9900 . ? C121 H12B 0.9900 . ? C122 H12C 0.9800 . ? C122 H12D 0.9800 . ? C122 H12E 0.9800 . ? C211 C212 1.380(4) . ? C211 H211 0.9500 . ? C212 C213 1.366(5) . ? C212 H212 0.9500 . ? C213 C214 1.376(4) . ? C213 H213 0.9500 . ? C214 C215 1.383(4) . ? C214 H214 0.9500 . ? C9 O11 1.368(6) . ? C9 O119 1.455(6) . ? O11 C11 1.475(14) . ? C11 C12 1.443(18) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12F 0.9800 . ? C12 H12G 0.9800 . ? C12 H12H 0.9800 . ? O119 C119 1.417(12) . ? C119 C129 1.430(18) . ? C119 H11C 0.9900 . ? C119 H11D 0.9900 . ? C129 H12I 0.9800 . ? C129 H12J 0.9800 . ? C129 H12K 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 O1 Dy1 O6 80.63(8) . . ? O1 Dy1 O10 76.16(8) . . ? O6 Dy1 O10 144.56(9) . . ? O1 Dy1 O5 76.88(8) . . ? O6 Dy1 O5 71.89(8) . . ? O10 Dy1 O5 76.98(8) . . ? O1 Dy1 O9 114.97(8) . . ? O6 Dy1 O9 141.84(8) . . ? O10 Dy1 O9 73.15(8) . . ? O5 Dy1 O9 143.41(8) . . ? O1 Dy1 O2 73.92(8) . . ? O6 Dy1 O2 76.19(8) . . ? O10 Dy1 O2 121.20(8) . . ? O5 Dy1 O2 139.52(8) . . ? O9 Dy1 O2 75.56(8) . . ? O1 Dy1 N2 144.97(8) . . ? O6 Dy1 N2 69.12(9) . . ? O10 Dy1 N2 138.79(9) . . ? O5 Dy1 N2 108.47(8) . . ? O9 Dy1 N2 81.93(8) . . ? O2 Dy1 N2 81.86(8) . . ? O1 Dy1 N1 146.75(9) . . ? O6 Dy1 N1 108.14(9) . . ? O10 Dy1 N1 79.50(9) . . ? O5 Dy1 N1 75.81(8) . . ? O9 Dy1 N1 78.38(8) . . ? O2 Dy1 N1 138.98(8) . . ? N2 Dy1 N1 63.43(9) . . ? C111 N1 C115 117.3(3) . . ? C111 N1 Dy1 121.8(2) . . ? C115 N1 Dy1 120.0(2) . . ? C1 O1 Dy1 132.9(2) . . ? O1 C1 O4 118.7(3) . . ? O1 C1 C2 127.2(4) . . ? O4 C1 C2 114.1(3) . . ? C211 N2 C215 117.9(3) . . ? C211 N2 Dy1 119.4(2) . . ? C215 N2 Dy1 120.0(2) . . ? C3 O2 Dy1 131.5(2) . . ? C3 O3 C31 118.0(3) . . ? C1 O4 C41 115.7(3) . . ? C4 O5 Dy1 129.7(2) . . ? C6 O6 Dy1 132.4(2) . . ? C6 O7 C71 115.6(3) . . ? C4 O8 C81 117.0(3) . . ? C7 O9 Dy1 134.1(2) . . ? C9 O10 Dy1 134.4(3) . . ? C7 O12 C121 118.0(3) . . ? C3 C2 C1 120.8(4) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? O2 C3 O3 119.5(4) . . ? O2 C3 C2 128.5(4) . . ? O3 C3 C2 112.0(3) . . ? O5 C4 O8 119.3(3) . . ? O5 C4 C5 127.5(4) . . ? O8 C4 C5 113.2(3) . . ? O6 C6 O7 117.9(3) . . ? O6 C6 C5 127.4(4) . . ? O7 C6 C5 114.7(4) . . ? O9 C7 O12 118.4(3) . . ? O9 C7 C8 128.1(4) . . ? O12 C7 C8 113.5(3) . . ? C9 C8 C7 120.5(4) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? O3 C31 C32 108.0(3) . . ? O3 C31 H31A 110.1 . . ? C32 C31 H31A 110.1 . . ? O3 C31 H31B 110.1 . . ? C32 C31 H31B 110.1 . . ? H31A C31 H31B 108.4 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C6 C5 C4 119.5(4) . . ? C6 C5 H35 120.3 . . ? C4 C5 H35 120.3 . . ? C42 C41 O4 110.9(4) . . ? C42 C41 H41A 109.5 . . ? O4 C41 H41A 109.5 . . ? C42 C41 H41B 109.5 . . ? O4 C41 H41B 109.5 . . ? H41A C41 H41B 108.0 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O7 C71 C72 108.3(3) . . ? O7 C71 H71A 110.0 . . ? C72 C71 H71A 110.0 . . ? O7 C71 H71B 110.0 . . ? C72 C71 H71B 110.0 . . ? H71A C71 H71B 108.4 . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C82 C81 O8 109.9(4) . . ? C82 C81 H81A 109.7 . . ? O8 C81 H81A 109.7 . . ? C82 C81 H81B 109.7 . . ? O8 C81 H81B 109.7 . . ? H81A C81 H81B 108.2 . . ? C81 C82 H82A 109.5 . . ? C81 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C81 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? N1 C111 C112 123.4(4) . . ? N1 C111 H111 118.3 . . ? C112 C111 H111 118.3 . . ? C113 C112 C111 118.7(4) . . ? C113 C112 H112 120.6 . . ? C111 C112 H112 120.6 . . ? C112 C113 C114 119.5(4) . . ? C112 C113 H113 120.3 . . ? C114 C113 H113 120.3 . . ? C113 C114 C115 118.6(4) . . ? C113 C114 H114 120.7 . . ? C115 C114 H114 120.7 . . ? N1 C115 C114 122.4(3) . . ? N1 C115 C215 116.5(3) . . ? C114 C115 C215 121.0(3) . . ? O12 C121 C122 107.4(3) . . ? O12 C121 H12A 110.2 . . ? C122 C121 H12A 110.2 . . ? O12 C121 H12B 110.2 . . ? C122 C121 H12B 110.2 . . ? H12A C121 H12B 108.5 . . ? C121 C122 H12C 109.5 . . ? C121 C122 H12D 109.5 . . ? H12C C122 H12D 109.5 . . ? C121 C122 H12E 109.5 . . ? H12C C122 H12E 109.5 . . ? H12D C122 H12E 109.5 . . ? N2 C211 C212 123.0(3) . . ? N2 C211 H211 118.5 . . ? C212 C211 H211 118.5 . . ? C213 C212 C211 118.8(3) . . ? C213 C212 H212 120.6 . . ? C211 C212 H212 120.6 . . ? C212 C213 C214 118.9(3) . . ? C212 C213 H213 120.5 . . ? C214 C213 H213 120.5 . . ? C213 C214 C215 119.3(3) . . ? C213 C214 H214 120.3 . . ? C215 C214 H214 120.3 . . ? N2 C215 C214 121.9(3) . . ? N2 C215 C115 116.1(3) . . ? C214 C215 C115 122.0(3) . . ? O10 C9 O11 117.0(4) . . ? O10 C9 C8 129.1(4) . . ? O11 C9 C8 112.3(4) . . ? O10 C9 O119 115.8(4) . . ? O11 C9 O119 30.2(2) . . ? C8 C9 O119 112.8(4) . . ? C9 O11 C11 119.8(6) . . ? C12 C11 O11 108.7(14) . . ? C12 C11 H11A 110.0 . . ? O11 C11 H11A 110.0 . . ? C12 C11 H11B 110.0 . . ? O11 C11 H11B 110.0 . . ? H11A C11 H11B 108.3 . . ? C119 O119 C9 117.9(6) . . ? O119 C119 C129 115.4(14) . . ? O119 C119 H11C 108.4 . . ? C129 C119 H11C 108.4 . . ? O119 C119 H11D 108.4 . . ? C129 C119 H11D 108.4 . . ? H11C C119 H11D 107.5 . . ? C119 C129 H12I 109.5 . . ? C119 C129 H12J 109.5 . . ? H12I C129 H12J 109.5 . . ? C119 C129 H12K 109.5 . . ? H12I C129 H12K 109.5 . . ? H12J C129 H12K 109.5 . . ? 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 Dy1 N1 C111 35.1(3) . . . . ? O6 Dy1 N1 C111 135.9(2) . . . . ? O10 Dy1 N1 C111 -8.4(2) . . . . ? O5 Dy1 N1 C111 70.7(2) . . . . ? O9 Dy1 N1 C111 -83.1(2) . . . . ? O2 Dy1 N1 C111 -134.5(2) . . . . ? N2 Dy1 N1 C111 -169.8(3) . . . . ? O1 Dy1 N1 C115 -156.2(2) . . . . ? O6 Dy1 N1 C115 -55.4(3) . . . . ? O10 Dy1 N1 C115 160.4(3) . . . . ? O5 Dy1 N1 C115 -120.5(3) . . . . ? O9 Dy1 N1 C115 85.6(2) . . . . ? O2 Dy1 N1 C115 34.3(3) . . . . ? N2 Dy1 N1 C115 -1.1(2) . . . . ? O6 Dy1 O1 C1 53.7(3) . . . . ? O10 Dy1 O1 C1 -153.3(3) . . . . ? O5 Dy1 O1 C1 127.1(3) . . . . ? O9 Dy1 O1 C1 -89.7(3) . . . . ? O2 Dy1 O1 C1 -24.5(3) . . . . ? N2 Dy1 O1 C1 23.6(4) . . . . ? N1 Dy1 O1 C1 162.6(3) . . . . ? Dy1 O1 C1 O4 -158.8(2) . . . . ? Dy1 O1 C1 C2 22.1(5) . . . . ? O1 Dy1 N2 C211 -16.1(3) . . . . ? O6 Dy1 N2 C211 -48.1(2) . . . . ? O10 Dy1 N2 C211 159.2(2) . . . . ? O5 Dy1 N2 C211 -109.6(3) . . . . ? O9 Dy1 N2 C211 106.6(3) . . . . ? O2 Dy1 N2 C211 30.1(3) . . . . ? N1 Dy1 N2 C211 -172.4(3) . . . . ? O1 Dy1 N2 C215 144.7(2) . . . . ? O6 Dy1 N2 C215 112.7(3) . . . . ? O10 Dy1 N2 C215 -39.9(3) . . . . ? O5 Dy1 N2 C215 51.3(3) . . . . ? O9 Dy1 N2 C215 -92.6(2) . . . . ? O2 Dy1 N2 C215 -169.1(3) . . . . ? N1 Dy1 N2 C215 -11.6(2) . . . . ? O1 Dy1 O2 C3 19.4(3) . . . . ? O6 Dy1 O2 C3 -64.7(3) . . . . ? O10 Dy1 O2 C3 81.6(3) . . . . ? O5 Dy1 O2 C3 -26.1(4) . . . . ? O9 Dy1 O2 C3 141.2(3) . . . . ? N2 Dy1 O2 C3 -135.1(3) . . . . ? N1 Dy1 O2 C3 -166.5(3) . . . . ? O1 C1 O4 C41 6.8(5) . . . . ? C2 C1 O4 C41 -173.9(3) . . . . ? O1 Dy1 O5 C4 -49.4(3) . . . . ? O6 Dy1 O5 C4 34.9(3) . . . . ? O10 Dy1 O5 C4 -127.9(3) . . . . ? O9 Dy1 O5 C4 -163.8(3) . . . . ? O2 Dy1 O5 C4 -4.7(3) . . . . ? N2 Dy1 O5 C4 94.6(3) . . . . ? N1 Dy1 O5 C4 149.8(3) . . . . ? O1 Dy1 O6 C6 48.9(3) . . . . ? O10 Dy1 O6 C6 -0.6(4) . . . . ? O5 Dy1 O6 C6 -30.3(3) . . . . ? O9 Dy1 O6 C6 167.7(3) . . . . ? O2 Dy1 O6 C6 124.5(3) . . . . ? N2 Dy1 O6 C6 -149.1(3) . . . . ? N1 Dy1 O6 C6 -98.1(3) . . . . ? O1 Dy1 O9 C7 -56.8(3) . . . . ? O6 Dy1 O9 C7 -164.4(3) . . . . ? O10 Dy1 O9 C7 8.5(3) . . . . ? O5 Dy1 O9 C7 45.1(4) . . . . ? O2 Dy1 O9 C7 -121.0(3) . . . . ? N2 Dy1 O9 C7 155.4(3) . . . . ? N1 Dy1 O9 C7 91.0(3) . . . . ? O1 Dy1 O10 C9 115.4(4) . . . . ? O6 Dy1 O10 C9 166.0(3) . . . . ? O5 Dy1 O10 C9 -165.1(4) . . . . ? O9 Dy1 O10 C9 -6.5(4) . . . . ? O2 Dy1 O10 C9 54.3(4) . . . . ? N2 Dy1 O10 C9 -61.8(4) . . . . ? N1 Dy1 O10 C9 -87.4(4) . . . . ? O1 C1 C2 C3 -1.3(6) . . . . ? O4 C1 C2 C3 179.5(3) . . . . ? Dy1 O2 C3 O3 167.3(2) . . . . ? Dy1 O2 C3 C2 -12.0(6) . . . . ? C31 O3 C3 O2 -1.0(5) . . . . ? C31 O3 C3 C2 178.5(3) . . . . ? C1 C2 C3 O2 -3.4(6) . . . . ? C1 C2 C3 O3 177.2(3) . . . . ? Dy1 O5 C4 O8 147.2(2) . . . . ? Dy1 O5 C4 C5 -33.8(5) . . . . ? C81 O8 C4 O5 -8.4(5) . . . . ? C81 O8 C4 C5 172.4(3) . . . . ? Dy1 O6 C6 O7 -158.2(2) . . . . ? Dy1 O6 C6 C5 22.6(5) . . . . ? C71 O7 C6 O6 7.0(5) . . . . ? C71 O7 C6 C5 -173.7(3) . . . . ? Dy1 O9 C7 O12 170.5(2) . . . . ? Dy1 O9 C7 C8 -8.4(6) . . . . ? C121 O12 C7 O9 5.2(5) . . . . ? C121 O12 C7 C8 -175.6(3) . . . . ? O9 C7 C8 C9 1.5(7) . . . . ? O12 C7 C8 C9 -177.5(4) . . . . ? C3 O3 C31 C32 171.5(3) . . . . ? O6 C6 C5 C4 -1.0(6) . . . . ? O7 C6 C5 C4 179.8(3) . . . . ? O5 C4 C5 C6 7.2(5) . . . . ? O8 C4 C5 C6 -173.7(3) . . . . ? C1 O4 C41 C42 -166.0(5) . . . . ? C6 O7 C71 C72 179.8(3) . . . . ? C4 O8 C81 C82 -140.3(4) . . . . ? C115 N1 C111 C112 -2.4(5) . . . . ? Dy1 N1 C111 C112 166.7(3) . . . . ? N1 C111 C112 C113 0.4(6) . . . . ? C111 C112 C113 C114 1.4(6) . . . . ? C112 C113 C114 C115 -1.1(6) . . . . ? C111 N1 C115 C114 2.7(5) . . . . ? Dy1 N1 C115 C114 -166.6(3) . . . . ? C111 N1 C115 C215 -178.7(3) . . . . ? Dy1 N1 C115 C215 12.1(4) . . . . ? C113 C114 C115 N1 -1.0(6) . . . . ? C113 C114 C115 C215 -179.6(3) . . . . ? C7 O12 C121 C122 -177.9(3) . . . . ? C215 N2 C211 C212 -0.6(5) . . . . ? Dy1 N2 C211 C212 160.6(3) . . . . ? N2 C211 C212 C213 -2.2(6) . . . . ? C211 C212 C213 C214 2.3(6) . . . . ? C212 C213 C214 C215 0.3(6) . . . . ? C211 N2 C215 C214 3.3(5) . . . . ? Dy1 N2 C215 C214 -157.8(3) . . . . ? C211 N2 C215 C115 -176.7(3) . . . . ? Dy1 N2 C215 C115 22.2(4) . . . . ? C213 C214 C215 N2 -3.1(5) . . . . ? C213 C214 C215 C115 176.8(3) . . . . ? N1 C115 C215 N2 -22.4(4) . . . . ? C114 C115 C215 N2 156.3(3) . . . . ? N1 C115 C215 C214 157.6(3) . . . . ? C114 C115 C215 C214 -23.7(5) . . . . ? Dy1 O10 C9 O11 -160.7(5) . . . . ? Dy1 O10 C9 C8 4.1(7) . . . . ? Dy1 O10 C9 O119 165.6(4) . . . . ? C7 C8 C9 O10 0.8(7) . . . . ? C7 C8 C9 O11 166.1(5) . . . . ? C7 C8 C9 O119 -161.2(5) . . . . ? O10 C9 O11 C11 -4.0(11) . . . . ? C8 C9 O11 C11 -171.2(8) . . . . ? O119 C9 O11 C11 91.5(10) . . . . ? C9 O11 C11 C12 -84.8(10) . . . . ? O10 C9 O119 C119 15.7(10) . . . . ? O11 C9 O119 C119 -84.3(10) . . . . ? C8 C9 O119 C119 -179.8(7) . . . . ? C9 O119 C119 C129 70.8(10) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.671 _refine_diff_density_min -0.497 _refine_diff_density_rms 0.077 #=================================END data_cvd186d _database_code_depnum_ccdc_archive 'CCDC 770263' #TrackingRef '- combined cif files.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60.50 H85 Dy N2 O12' _chemical_formula_weight 1194.81 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' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.5760(6) _cell_length_b 20.7443(8) _cell_length_c 20.4233(6) _cell_angle_alpha 90.00 _cell_angle_beta 109.574(3) _cell_angle_gamma 90.00 _cell_volume 6217.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.276 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2496 _exptl_absorpt_coefficient_mu 1.260 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 53231 _diffrn_reflns_av_R_equivalents 0.0688 _diffrn_reflns_av_sigmaI/netI 0.0784 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 25.50 _reflns_number_total 11566 _reflns_number_gt 7320 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0537P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11566 _refine_ls_number_parameters 683 _refine_ls_number_restraints 199 _refine_ls_R_factor_all 0.0825 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.0973 _refine_ls_wR_factor_gt 0.0898 _refine_ls_goodness_of_fit_ref 0.872 _refine_ls_restrained_S_all 0.868 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.324820(14) 0.824271(10) 0.214126(10) 0.02888(7) Uani 1 1 d . . . N1A N 0.1748(2) 0.86331(17) 0.11933(18) 0.0332(9) Uani 1 1 d . . . O1 O 0.21923(19) 0.74009(14) 0.18747(14) 0.0329(7) Uani 1 1 d . . . O2 O 0.34456(19) 0.77248(14) 0.12009(14) 0.0344(7) Uani 1 1 d . . . O3 O 0.3664(2) 0.68997(14) 0.05482(16) 0.0410(8) Uani 1 1 d . . . O4 O 0.1343(2) 0.65337(14) 0.13911(15) 0.0384(8) Uani 1 1 d . . . O5 O 0.30018(19) 0.80296(14) 0.31887(14) 0.0327(7) Uani 1 1 d . . . O6 O 0.42405(19) 0.73962(14) 0.26465(15) 0.0344(7) Uani 1 1 d . . . O7 O 0.4818(2) 0.64856(15) 0.32499(16) 0.0399(8) Uani 1 1 d . . . O8 O 0.2701(2) 0.74351(15) 0.40192(16) 0.0435(8) Uani 1 1 d . . . O9 O 0.45126(19) 0.87498(14) 0.29022(14) 0.0355(7) Uani 1 1 d . . . O10 O 0.3610(2) 0.90926(15) 0.15211(15) 0.0385(8) Uani 1 1 d . . . O11 O 0.4080(3) 1.00541(17) 0.12387(19) 0.0661(12) Uani 1 1 d . A . O12 O 0.5532(2) 0.95005(16) 0.34953(17) 0.0574(10) Uani 1 1 d . . . N1B N 0.2436(2) 0.92265(17) 0.24203(18) 0.0331(8) Uani 1 1 d . . . C1 C 0.2062(3) 0.6931(2) 0.1473(2) 0.0327(11) Uani 1 1 d . . . C2 C 0.2586(3) 0.6758(2) 0.1065(2) 0.0343(10) Uani 1 1 d . . . H2 H 0.2490 0.6347 0.0849 0.041 Uiso 1 1 calc R . . C3 C 0.3242(3) 0.7161(2) 0.0960(2) 0.0331(10) Uani 1 1 d . . . C4 C 0.3131(3) 0.7527(2) 0.3551(2) 0.0342(11) Uani 1 1 d . . . C5 C 0.3697(3) 0.7015(2) 0.3529(2) 0.0350(11) Uani 1 1 d . . . H5 H 0.3713 0.6653 0.3818 0.042 Uiso 1 1 calc R . . C6 C 0.4239(3) 0.7000(2) 0.3114(2) 0.0308(10) Uani 1 1 d . . . C7 C 0.4895(3) 0.9282(2) 0.2909(2) 0.0376(11) Uani 1 1 d . . . C8 C 0.4718(3) 0.9707(2) 0.2358(2) 0.0429(12) Uani 1 1 d . . . H8 H 0.5035 1.0106 0.2432 0.052 Uiso 1 1 calc R . . C9 C 0.4102(3) 0.9579(2) 0.1702(2) 0.0425(12) Uani 1 1 d . . . C21A C 0.1303(3) 0.9158(2) 0.1285(2) 0.0343(11) Uani 1 1 d . . . C22A C 0.0482(3) 0.9347(2) 0.0795(2) 0.0502(14) Uani 1 1 d . . . H22A H 0.0164 0.9712 0.0878 0.060 Uiso 1 1 calc R . . C23A C 0.0137(4) 0.9001(3) 0.0192(3) 0.0566(15) Uani 1 1 d . . . H23A H -0.0419 0.9127 -0.0150 0.068 Uiso 1 1 calc R . . C24A C 0.0596(3) 0.8474(3) 0.0087(3) 0.0501(14) Uani 1 1 d . . . H24A H 0.0370 0.8230 -0.0330 0.060 Uiso 1 1 calc R . . C25A C 0.1391(3) 0.8304(2) 0.0596(2) 0.0371(11) Uani 1 1 d . . . H25A H 0.1708 0.7934 0.0523 0.045 Uiso 1 1 calc R . . C21B C 0.1736(3) 0.9525(2) 0.1939(2) 0.0337(11) Uani 1 1 d . . . C22B C 0.1463(3) 1.0140(2) 0.2045(3) 0.0444(12) Uani 1 1 d . . . H22B H 0.0985 1.0352 0.1695 0.053 Uiso 1 1 calc R . . C23B C 0.1910(3) 1.0438(2) 0.2678(3) 0.0536(15) Uani 1 1 d . . . H23B H 0.1716 1.0851 0.2773 0.064 Uiso 1 1 calc R . . C24B C 0.2610(3) 1.0146(2) 0.3153(2) 0.0434(12) Uani 1 1 d . . . H24B H 0.2932 1.0354 0.3579 0.052 Uiso 1 1 calc R . . C25B C 0.2852(3) 0.9537(2) 0.3013(2) 0.0380(11) Uani 1 1 d . . . H25B H 0.3340 0.9327 0.3356 0.046 Uiso 1 1 calc R . . C31 C 0.4108(4) 0.7296(3) 0.0166(2) 0.0493(13) Uani 1 1 d . . . C32 C 0.4370(4) 0.6802(3) -0.0289(3) 0.0725(18) Uani 1 1 d . . . H32A H 0.3819 0.6591 -0.0596 0.109 Uiso 1 1 calc R . . H32B H 0.4775 0.6478 0.0008 0.109 Uiso 1 1 calc R . . H32C H 0.4684 0.7020 -0.0569 0.109 Uiso 1 1 calc R . . C33 C 0.3415(4) 0.7769(3) -0.0285(3) 0.079(2) Uani 1 1 d . . . H33A H 0.2883 0.7531 -0.0583 0.119 Uiso 1 1 calc R . . H33B H 0.3690 0.8012 -0.0575 0.119 Uiso 1 1 calc R . . H33C H 0.3223 0.8067 0.0012 0.119 Uiso 1 1 calc R . . C34 C 0.4951(4) 0.7627(3) 0.0648(3) 0.084(2) Uani 1 1 d . . . H34A H 0.5376 0.7301 0.0923 0.126 Uiso 1 1 calc R . . H34B H 0.4777 0.7918 0.0960 0.126 Uiso 1 1 calc R . . H34C H 0.5244 0.7874 0.0373 0.126 Uiso 1 1 calc R . . C41 C 0.0671(3) 0.6635(2) 0.1736(2) 0.0382(11) Uani 1 1 d . . . C42 C 0.1110(3) 0.6528(3) 0.2514(2) 0.0517(14) Uani 1 1 d . . . H42A H 0.1383 0.6097 0.2598 0.078 Uiso 1 1 calc R . . H42B H 0.0645 0.6564 0.2738 0.078 Uiso 1 1 calc R . . H42C H 0.1583 0.6853 0.2707 0.078 Uiso 1 1 calc R . . C43 C -0.0022(3) 0.6117(3) 0.1421(3) 0.0530(14) Uani 1 1 d . . . H43A H 0.0266 0.5693 0.1535 0.080 Uiso 1 1 calc R . . H43B H -0.0261 0.6170 0.0916 0.080 Uiso 1 1 calc R . . H43C H -0.0523 0.6151 0.1609 0.080 Uiso 1 1 calc R . . C44 C 0.0229(3) 0.7291(3) 0.1561(3) 0.0596(15) Uani 1 1 d . . . H44A H 0.0682 0.7627 0.1765 0.089 Uiso 1 1 calc R . . H44B H -0.0270 0.7326 0.1750 0.089 Uiso 1 1 calc R . . H44C H -0.0011 0.7344 0.1055 0.089 Uiso 1 1 calc R . . C71 C 0.5548(3) 0.6416(2) 0.2953(2) 0.0396(11) Uani 1 1 d . . . C72 C 0.5184(4) 0.6317(3) 0.2181(3) 0.0683(18) Uani 1 1 d . . . H72A H 0.4871 0.6709 0.1956 0.102 Uiso 1 1 calc R . . H72B H 0.4755 0.5955 0.2072 0.102 Uiso 1 1 calc R . . H72C H 0.5690 0.6222 0.2012 0.102 Uiso 1 1 calc R . . C73 C 0.6194(4) 0.6983(3) 0.3154(3) 0.0671(17) Uani 1 1 d . . . H73A H 0.6415 0.7031 0.3660 0.101 Uiso 1 1 calc R . . H73B H 0.5874 0.7376 0.2939 0.101 Uiso 1 1 calc R . . H73C H 0.6711 0.6908 0.2992 0.101 Uiso 1 1 calc R . . C74 C 0.6040(4) 0.5812(3) 0.3316(3) 0.078(2) Uani 1 1 d . . . H74A H 0.6276 0.5885 0.3819 0.117 Uiso 1 1 calc R . . H74B H 0.6548 0.5714 0.3150 0.117 Uiso 1 1 calc R . . H74C H 0.5614 0.5448 0.3213 0.117 Uiso 1 1 calc R . . C81 C 0.2202(3) 0.7940(2) 0.4231(3) 0.0433(12) Uani 1 1 d . . . C82 C 0.1389(3) 0.8168(3) 0.3625(3) 0.0600(15) Uani 1 1 d . . . H82A H 0.0999 0.7799 0.3419 0.090 Uiso 1 1 calc R . . H82B H 0.1603 0.8369 0.3274 0.090 Uiso 1 1 calc R . . H82C H 0.1040 0.8483 0.3791 0.090 Uiso 1 1 calc R . . C83 C 0.2835(4) 0.8481(3) 0.4573(3) 0.0643(16) Uani 1 1 d . . . H83A H 0.3041 0.8700 0.4228 0.097 Uiso 1 1 calc R . . H83B H 0.3362 0.8308 0.4944 0.097 Uiso 1 1 calc R . . H83C H 0.2513 0.8789 0.4772 0.097 Uiso 1 1 calc R . . C84 C 0.1880(4) 0.7594(3) 0.4767(3) 0.0700(18) Uani 1 1 d . . . H84A H 0.1468 0.7241 0.4540 0.105 Uiso 1 1 calc R . . H84B H 0.1558 0.7899 0.4967 0.105 Uiso 1 1 calc R . . H84C H 0.2408 0.7418 0.5135 0.105 Uiso 1 1 calc R . . C111 C 0.3494(4) 1.0071(3) 0.0526(3) 0.0619(16) Uani 1 1 d D . . C112 C 0.3822(18) 1.0606(8) 0.0164(16) 0.067(6) Uani 0.50 1 d PDU A 1 H11A H 0.4393 1.0475 0.0099 0.101 Uiso 0.50 1 calc PR A 1 H11B H 0.3925 1.0997 0.0448 0.101 Uiso 0.50 1 calc PR A 1 H11C H 0.3361 1.0691 -0.0290 0.101 Uiso 0.50 1 calc PR A 1 C113 C 0.3375(13) 0.9452(7) 0.0103(11) 0.092(6) Uani 0.50 1 d PDU A 1 H11D H 0.3951 0.9341 0.0036 0.138 Uiso 0.50 1 calc PR A 1 H11E H 0.2901 0.9514 -0.0350 0.138 Uiso 0.50 1 calc PR A 1 H11F H 0.3195 0.9101 0.0352 0.138 Uiso 0.50 1 calc PR A 1 C114 C 0.2606(8) 1.0255(11) 0.0621(11) 0.094(8) Uani 0.50 1 d PDU A 1 H11G H 0.2404 0.9905 0.0857 0.140 Uiso 0.50 1 calc PR A 1 H11H H 0.2143 1.0333 0.0165 0.140 Uiso 0.50 1 calc PR A 1 H11I H 0.2692 1.0648 0.0902 0.140 Uiso 0.50 1 calc PR A 1 C02' C 0.372(2) 1.0739(8) 0.0337(18) 0.112(12) Uani 0.50 1 d PDU A 2 H02A H 0.4375 1.0778 0.0441 0.168 Uiso 0.50 1 calc PR A 2 H02B H 0.3513 1.1059 0.0607 0.168 Uiso 0.50 1 calc PR A 2 H02C H 0.3402 1.0814 -0.0160 0.168 Uiso 0.50 1 calc PR A 2 C03' C 0.3926(14) 0.9551(8) 0.0221(10) 0.119(9) Uani 0.50 1 d PDU A 2 H03A H 0.4581 0.9633 0.0349 0.179 Uiso 0.50 1 calc PR A 2 H03B H 0.3648 0.9552 -0.0286 0.179 Uiso 0.50 1 calc PR A 2 H03C H 0.3829 0.9130 0.0403 0.179 Uiso 0.50 1 calc PR A 2 C04' C 0.2489(9) 0.9975(12) 0.0363(11) 0.105(10) Uani 0.50 1 d PDU A 2 H04A H 0.2246 1.0321 0.0576 0.157 Uiso 0.50 1 calc PR A 2 H04B H 0.2381 0.9558 0.0548 0.157 Uiso 0.50 1 calc PR A 2 H04C H 0.2185 0.9982 -0.0142 0.157 Uiso 0.50 1 calc PR A 2 C121 C 0.5852(4) 0.9153(2) 0.4149(3) 0.0480(13) Uani 1 1 d . . . C122 C 0.6311(5) 0.8545(3) 0.4064(3) 0.092(2) Uani 1 1 d . . . H12A H 0.6809 0.8645 0.3888 0.139 Uiso 1 1 calc R . . H12B H 0.5869 0.8263 0.3733 0.139 Uiso 1 1 calc R . . H12C H 0.6556 0.8326 0.4514 0.139 Uiso 1 1 calc R . . C123 C 0.6513(5) 0.9623(3) 0.4618(3) 0.100(3) Uani 1 1 d . . . H12D H 0.7014 0.9703 0.4439 0.150 Uiso 1 1 calc R . . H12E H 0.6758 0.9443 0.5087 0.150 Uiso 1 1 calc R . . H12F H 0.6199 1.0029 0.4632 0.150 Uiso 1 1 calc R . . C124 C 0.5102(5) 0.9025(4) 0.4423(3) 0.091(2) Uani 1 1 d . . . H12G H 0.4818 0.9434 0.4478 0.137 Uiso 1 1 calc R . . H12H H 0.5344 0.8809 0.4874 0.137 Uiso 1 1 calc R . . H12I H 0.4646 0.8748 0.4097 0.137 Uiso 1 1 calc R . . C11 C 0.7533(4) 0.8749(5) 0.2147(5) 0.083(5) Uiso 0.68(3) 1 d PGD B 1 C12 C 0.7729(8) 0.8641(5) 0.1541(3) 0.080(4) Uiso 0.68(3) 1 d PGD B 1 H12 H 0.7258 0.8513 0.1129 0.096 Uiso 0.68(3) 1 calc PR B 1 C13 C 0.8613(10) 0.8718(5) 0.1537(6) 0.091(4) Uiso 0.68(3) 1 d PGD B 1 H13 H 0.8747 0.8644 0.1123 0.109 Uiso 0.68(3) 1 calc PR B 1 C14 C 0.9302(5) 0.8905(5) 0.2140(8) 0.084(4) Uiso 0.68(3) 1 d PGD B 1 H14 H 0.9907 0.8958 0.2138 0.100 Uiso 0.68(3) 1 calc PR B 1 C15 C 0.9106(5) 0.9013(5) 0.2747(6) 0.094(4) Uiso 0.68(3) 1 d PGD B 1 H15 H 0.9577 0.9141 0.3159 0.113 Uiso 0.68(3) 1 calc PR B 1 C16 C 0.8222(7) 0.8936(6) 0.2750(4) 0.083(5) Uiso 0.68(3) 1 d PGD B 1 H16 H 0.8088 0.9010 0.3165 0.100 Uiso 0.68(3) 1 calc PR B 1 C17 C 0.6619(7) 0.8641(7) 0.2149(9) 0.108(5) Uiso 0.68(3) 1 d PD B 1 H17A H 0.6588 0.8745 0.2608 0.162 Uiso 0.68(3) 1 calc PR B 1 H17B H 0.6455 0.8188 0.2041 0.162 Uiso 0.68(3) 1 calc PR B 1 H17C H 0.6194 0.8917 0.1798 0.162 Uiso 0.68(3) 1 calc PR B 1 C11' C 0.7551(9) 0.8767(12) 0.2016(12) 0.089(12) Uiso 0.32(3) 1 d PGD B 2 C12' C 0.8026(17) 0.8724(10) 0.1550(7) 0.063(6) Uiso 0.32(3) 1 d PGD B 2 H12' H 0.7717 0.8603 0.1082 0.075 Uiso 0.32(3) 1 calc PR B 2 C13' C 0.8954(17) 0.8858(11) 0.1771(14) 0.081(8) Uiso 0.32(3) 1 d PGD B 2 H13' H 0.9279 0.8829 0.1452 0.097 Uiso 0.32(3) 1 calc PR B 2 C14' C 0.9406(9) 0.9035(11) 0.2456(16) 0.081(8) Uiso 0.32(3) 1 d PGD B 2 H14' H 1.0040 0.9127 0.2607 0.097 Uiso 0.32(3) 1 calc PR B 2 C15' C 0.8931(18) 0.9078(14) 0.2922(8) 0.143(13) Uiso 0.32(3) 1 d PGD B 2 H15' H 0.9240 0.9199 0.3391 0.172 Uiso 0.32(3) 1 calc PR B 2 C16' C 0.8003(18) 0.8943(15) 0.2702(11) 0.16(2) Uiso 0.32(3) 1 d PGD B 2 H16' H 0.7678 0.8973 0.3020 0.198 Uiso 0.32(3) 1 calc PR B 2 C17' C 0.6589(12) 0.8676(15) 0.180(2) 0.127(12) Uiso 0.32(3) 1 d PD B 2 H17D H 0.6383 0.8723 0.2202 0.191 Uiso 0.32(3) 1 calc PR B 2 H17E H 0.6436 0.8243 0.1603 0.191 Uiso 0.32(3) 1 calc PR B 2 H17F H 0.6286 0.8999 0.1449 0.191 Uiso 0.32(3) 1 calc PR B 2 C21 C 0.8347(7) 0.5982(5) 0.2764(5) 0.091(5) Uiso 0.536(9) 1 d PGD C 1 C22 C 0.7718(8) 0.5850(4) 0.2113(6) 0.071(4) Uiso 0.536(9) 1 d PGD C 1 H22 H 0.7487 0.5425 0.2002 0.085 Uiso 0.536(9) 1 calc PR C 1 C23 C 0.7429(8) 0.6339(5) 0.1622(5) 0.079(9) Uiso 0.536(9) 1 d PGD C 1 H23 H 0.6999 0.6249 0.1177 0.095 Uiso 0.536(9) 1 calc PR C 1 C24 C 0.7768(8) 0.6960(5) 0.1784(5) 0.087(5) Uiso 0.536(9) 1 d PGD C 1 H24 H 0.7569 0.7295 0.1449 0.104 Uiso 0.536(9) 1 calc PR C 1 C25 C 0.8396(7) 0.7093(4) 0.2435(5) 0.072(4) Uiso 0.536(9) 1 d PGD C 1 H25 H 0.8628 0.7517 0.2545 0.087 Uiso 0.536(9) 1 calc PR C 1 C26 C 0.8686(7) 0.6604(5) 0.2925(4) 0.086(4) Uiso 0.536(9) 1 d PGD C 1 H26 H 0.9116 0.6694 0.3371 0.103 Uiso 0.536(9) 1 calc PR C 1 C27 C 0.8552(12) 0.5480(8) 0.3261(8) 0.143(6) Uiso 0.536(9) 1 d PD C 1 H27A H 0.9004 0.5632 0.3695 0.215 Uiso 0.536(9) 1 calc PR C 1 H27B H 0.8798 0.5110 0.3084 0.215 Uiso 0.536(9) 1 calc PR C 1 H27C H 0.7996 0.5351 0.3350 0.215 Uiso 0.536(9) 1 calc PR C 1 C22' C 0.7770(12) 0.6345(10) 0.2073(9) 0.075(8) Uiso 0.247(10) 1 d PGD D 2 H22' H 0.7300 0.6252 0.1647 0.091 Uiso 0.247(10) 1 calc PR D 2 C21' C 0.8153(13) 0.5852(7) 0.2540(10) 0.057(8) Uiso 0.247(10) 1 d PGD D 2 C26' C 0.8841(14) 0.5988(8) 0.3162(10) 0.095(11) Uiso 0.247(10) 1 d PGD D 2 H26' H 0.9103 0.5651 0.3482 0.114 Uiso 0.247(10) 1 calc PR D 2 C25' C 0.9146(14) 0.6618(10) 0.3318(10) 0.079(9) Uiso 0.247(10) 1 d PGD D 2 H25' H 0.9616 0.6711 0.3744 0.095 Uiso 0.247(10) 1 calc PR D 2 C24' C 0.8763(17) 0.7112(7) 0.2851(13) 0.104(11) Uiso 0.247(10) 1 d PGD D 2 H24' H 0.8971 0.7542 0.2957 0.125 Uiso 0.247(10) 1 calc PR D 2 C23' C 0.8075(17) 0.6975(8) 0.2228(12) 0.098(12) Uiso 0.247(10) 1 d PGD D 2 H23' H 0.7813 0.7312 0.1909 0.118 Uiso 0.247(10) 1 calc PR D 2 C27' C 0.784(2) 0.5218(11) 0.2341(16) 0.143(6) Uiso 0.247(10) 1 d PD D 2 H27D H 0.7369 0.5227 0.1882 0.215 Uiso 0.247(10) 1 calc PR D 2 H27E H 0.7595 0.5035 0.2681 0.215 Uiso 0.247(10) 1 calc PR D 2 H27F H 0.8354 0.4952 0.2320 0.215 Uiso 0.247(10) 1 calc PR D 2 C1'' C 0.8509(12) 0.6780(8) 0.2624(9) 0.038(6) Uiso 0.218(10) 1 d PGD E 3 C2'' C 0.8691(12) 0.6191(10) 0.2967(8) 0.044(7) Uiso 0.218(10) 1 d PGD E 3 H2'' H 0.9123 0.6166 0.3423 0.053 Uiso 0.218(10) 1 calc PR E 3 C3'' C 0.8241(16) 0.5638(8) 0.2643(11) 0.070(10) Uiso 0.218(10) 1 d PGD E 3 H3'' H 0.8365 0.5236 0.2878 0.084 Uiso 0.218(10) 1 calc PR E 3 C4'' C 0.7609(19) 0.5675(11) 0.1976(12) 0.100(14) Uiso 0.218(10) 1 d PGD E 3 H4'' H 0.7302 0.5297 0.1755 0.120 Uiso 0.218(10) 1 calc PR E 3 C5'' C 0.743(2) 0.6264(14) 0.1633(10) 0.13(4) Uiso 0.218(10) 1 d PGD E 3 H5'' H 0.6996 0.6289 0.1177 0.161 Uiso 0.218(10) 1 calc PR E 3 C6'' C 0.7877(17) 0.6816(11) 0.1957(10) 0.067(9) Uiso 0.218(10) 1 d PGD E 3 H6'' H 0.7753 0.7219 0.1722 0.081 Uiso 0.218(10) 1 calc PR E 3 C7'' C 0.899(3) 0.7319(13) 0.2989(17) 0.143(6) Uiso 0.218(10) 1 d PD E 3 H7'1 H 0.8814 0.7703 0.2695 0.215 Uiso 0.218(10) 1 calc PR E 3 H7'2 H 0.9643 0.7246 0.3115 0.215 Uiso 0.218(10) 1 calc PR E 3 H7'3 H 0.8832 0.7383 0.3412 0.215 Uiso 0.218(10) 1 calc PR E 3 C51 C 0.4534(11) 0.5080(9) 0.0352(8) 0.064(4) Uani 0.50 1 d PGU F -1 C52 C 0.4157(13) 0.4900(9) -0.0342(8) 0.077(5) Uani 0.50 1 d PGU F -1 H52 H 0.3526 0.4802 -0.0532 0.092 Uiso 0.50 1 calc PR F -1 C53 C 0.4703(16) 0.4863(9) -0.0757(9) 0.112(9) Uani 0.50 1 d PGU F -1 H53 H 0.4445 0.4740 -0.1231 0.134 Uiso 0.50 1 calc PR F -1 C54 C 0.5626(16) 0.5006(11) -0.0479(11) 0.098(8) Uani 0.50 1 d PGU F -1 H54 H 0.6000 0.4980 -0.0763 0.117 Uiso 0.50 1 calc PR F -1 C55 C 0.6004(12) 0.5185(11) 0.0215(12) 0.112(9) Uani 0.50 1 d PGU F -1 H55 H 0.6635 0.5283 0.0405 0.135 Uiso 0.50 1 calc PR F -1 C56 C 0.5458(11) 0.5223(11) 0.0630(9) 0.082(7) Uani 0.50 1 d PGU F -1 H56 H 0.5716 0.5345 0.1104 0.099 Uiso 0.50 1 calc PR F -1 C57 C 0.3951(8) 0.5112(7) 0.0804(7) 0.073(4) Uani 0.50 1 d PU F -1 H57A H 0.4323 0.5245 0.1274 0.110 Uiso 0.50 1 calc PR F -1 H57B H 0.3687 0.4687 0.0824 0.110 Uiso 0.50 1 calc PR F -1 H57C H 0.3460 0.5426 0.0611 0.110 Uiso 0.50 1 calc PR F -1 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 0.03203(11) 0.02473(10) 0.02922(11) 0.00038(11) 0.00939(8) 0.00020(11) N1A 0.033(2) 0.031(2) 0.036(2) 0.0043(17) 0.0112(18) 0.0010(17) O1 0.0335(17) 0.0282(17) 0.0379(17) -0.0034(14) 0.0131(14) -0.0009(13) O2 0.0359(17) 0.0345(18) 0.0349(17) -0.0043(14) 0.0147(14) -0.0025(14) O3 0.0467(19) 0.039(2) 0.0459(19) -0.0071(15) 0.0267(16) -0.0013(15) O4 0.0454(19) 0.0308(17) 0.0404(18) -0.0042(14) 0.0163(16) -0.0075(14) O5 0.0341(16) 0.0318(17) 0.0321(17) 0.0030(13) 0.0110(14) 0.0037(13) O6 0.0354(17) 0.0294(17) 0.0379(18) 0.0058(14) 0.0116(14) 0.0068(14) O7 0.0351(17) 0.0335(17) 0.051(2) 0.0089(15) 0.0142(16) 0.0105(14) O8 0.054(2) 0.041(2) 0.0450(19) 0.0075(16) 0.0287(17) 0.0078(16) O9 0.0383(17) 0.0298(17) 0.0362(17) 0.0000(14) 0.0098(15) -0.0040(14) O10 0.0424(18) 0.0313(18) 0.0415(18) 0.0048(15) 0.0137(15) -0.0041(15) O11 0.073(3) 0.049(2) 0.058(2) 0.0255(19) -0.002(2) -0.020(2) O12 0.062(2) 0.037(2) 0.051(2) 0.0069(17) -0.0105(19) -0.0169(17) N1B 0.035(2) 0.0282(19) 0.038(2) -0.0005(18) 0.0155(18) 0.0009(16) C1 0.032(2) 0.031(3) 0.031(2) 0.005(2) 0.005(2) 0.0020(19) C2 0.038(2) 0.028(2) 0.035(2) -0.004(2) 0.010(2) -0.004(2) C3 0.036(3) 0.036(3) 0.028(2) 0.003(2) 0.011(2) 0.005(2) C4 0.031(2) 0.037(3) 0.034(3) -0.001(2) 0.011(2) -0.006(2) C5 0.038(3) 0.031(2) 0.036(3) 0.006(2) 0.013(2) 0.002(2) C6 0.025(2) 0.027(2) 0.034(3) -0.003(2) 0.002(2) -0.0008(19) C7 0.035(3) 0.034(3) 0.040(3) -0.003(2) 0.009(2) 0.001(2) C8 0.042(3) 0.035(3) 0.045(3) 0.003(2) 0.006(2) -0.010(2) C9 0.045(3) 0.035(3) 0.048(3) 0.012(2) 0.016(3) 0.006(2) C21A 0.036(3) 0.028(2) 0.039(3) 0.006(2) 0.013(2) 0.002(2) C22A 0.053(3) 0.044(3) 0.047(3) 0.000(3) 0.008(3) 0.014(3) C23A 0.051(3) 0.055(4) 0.048(3) 0.001(3) -0.004(3) 0.014(3) C24A 0.054(3) 0.049(3) 0.037(3) -0.002(2) 0.001(3) 0.000(3) C25A 0.039(2) 0.034(3) 0.036(2) 0.000(2) 0.009(2) 0.002(2) C21B 0.030(2) 0.033(3) 0.039(3) 0.004(2) 0.012(2) 0.001(2) C22B 0.037(3) 0.043(3) 0.050(3) 0.004(2) 0.009(2) 0.010(2) C23B 0.045(3) 0.044(3) 0.056(3) -0.029(3) -0.003(3) 0.018(2) C24B 0.041(3) 0.044(3) 0.045(3) -0.011(2) 0.015(2) 0.005(2) C25B 0.041(3) 0.035(3) 0.038(3) 0.001(2) 0.014(2) 0.000(2) C31 0.057(3) 0.053(3) 0.042(3) -0.005(2) 0.023(3) -0.007(3) C32 0.084(4) 0.076(4) 0.081(4) -0.026(4) 0.059(4) -0.016(4) C33 0.090(5) 0.094(5) 0.062(4) 0.023(4) 0.036(4) 0.014(4) C34 0.062(4) 0.110(6) 0.093(5) -0.041(4) 0.044(4) -0.035(4) C41 0.038(3) 0.038(3) 0.042(3) -0.004(2) 0.017(2) -0.007(2) C42 0.052(3) 0.058(3) 0.050(3) -0.007(3) 0.023(3) -0.014(3) C43 0.046(3) 0.060(4) 0.054(3) -0.004(3) 0.017(3) -0.016(3) C44 0.048(3) 0.052(3) 0.090(4) 0.008(3) 0.037(3) 0.005(3) C71 0.042(3) 0.038(3) 0.040(3) 0.000(2) 0.016(2) 0.005(2) C72 0.055(3) 0.091(5) 0.061(4) -0.019(3) 0.022(3) 0.020(3) C73 0.046(3) 0.054(4) 0.106(5) -0.016(3) 0.032(3) -0.009(3) C74 0.071(4) 0.066(4) 0.109(5) 0.032(4) 0.047(4) 0.042(3) C81 0.046(3) 0.044(3) 0.051(3) -0.004(2) 0.031(3) 0.000(2) C82 0.042(3) 0.074(4) 0.062(3) -0.005(3) 0.015(3) 0.010(3) C83 0.074(4) 0.067(4) 0.060(4) -0.020(3) 0.033(3) -0.014(3) C84 0.087(4) 0.066(4) 0.084(4) 0.004(3) 0.065(4) 0.002(3) C111 0.065(4) 0.068(4) 0.050(3) 0.022(3) 0.016(3) -0.006(3) C112 0.061(10) 0.076(11) 0.068(16) 0.036(9) 0.026(10) 0.001(8) C113 0.115(15) 0.083(12) 0.082(11) 0.006(9) 0.037(12) -0.040(11) C114 0.054(10) 0.14(2) 0.078(16) 0.062(13) 0.009(9) 0.034(11) C02' 0.16(3) 0.098(16) 0.065(16) 0.054(14) 0.019(13) -0.022(16) C03' 0.21(3) 0.112(16) 0.065(13) 0.005(10) 0.079(17) -0.049(16) C04' 0.077(12) 0.16(2) 0.058(13) 0.049(13) -0.009(9) -0.047(12) C121 0.052(3) 0.036(3) 0.042(3) 0.001(2) -0.003(3) 0.002(2) C122 0.096(5) 0.094(5) 0.062(4) -0.005(4) -0.008(4) 0.054(4) C123 0.114(6) 0.068(5) 0.065(4) 0.009(3) -0.042(4) -0.031(4) C124 0.081(5) 0.148(7) 0.042(4) -0.002(4) 0.016(3) -0.003(5) C51 0.073(8) 0.052(10) 0.064(9) -0.001(8) 0.019(7) -0.012(8) C52 0.092(11) 0.058(10) 0.074(9) -0.035(9) 0.019(8) -0.018(10) C53 0.168(19) 0.078(15) 0.112(14) -0.023(13) 0.077(12) -0.018(16) C54 0.156(17) 0.058(13) 0.118(13) 0.006(10) 0.098(13) 0.003(13) C55 0.098(12) 0.15(2) 0.105(12) 0.033(13) 0.056(10) 0.026(15) C56 0.065(7) 0.12(2) 0.054(8) 0.003(10) 0.014(7) -0.006(10) C57 0.060(7) 0.076(9) 0.083(8) -0.018(7) 0.023(7) 0.004(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O2 2.309(3) . ? Dy1 O9 2.313(3) . ? Dy1 O1 2.335(3) . ? Dy1 O6 2.338(3) . ? Dy1 O5 2.339(3) . ? Dy1 O10 2.347(3) . ? Dy1 N1B 2.564(4) . ? Dy1 N1A 2.614(3) . ? N1A C21A 1.337(5) . ? N1A C25A 1.345(5) . ? O1 C1 1.247(5) . ? O2 C3 1.268(5) . ? O3 C3 1.343(5) . ? O3 C31 1.457(6) . ? O4 C1 1.355(5) . ? O4 C41 1.458(5) . ? O5 C4 1.255(5) . ? O6 C6 1.260(5) . ? O7 C6 1.364(5) . ? O7 C71 1.464(5) . ? O8 C4 1.351(5) . ? O8 C81 1.453(5) . ? O9 C7 1.253(5) . ? O10 C9 1.246(5) . ? O11 C9 1.358(5) . ? O11 C111 1.436(6) . ? O12 C7 1.351(5) . ? O12 C121 1.451(6) . ? N1B C25B 1.332(5) . ? N1B C21B 1.349(5) . ? C1 C2 1.393(6) . ? C2 C3 1.392(6) . ? C4 C5 1.391(6) . ? C5 C6 1.384(6) . ? C7 C8 1.382(6) . ? C8 C9 1.388(6) . ? C21A C22A 1.391(6) . ? C21A C21B 1.490(6) . ? C22A C23A 1.371(7) . ? C23A C24A 1.363(7) . ? C24A C25A 1.370(6) . ? C21B C22B 1.383(6) . ? C22B C23B 1.392(6) . ? C23B C24B 1.338(6) . ? C24B C25B 1.375(6) . ? C31 C34 1.515(7) . ? C31 C33 1.519(7) . ? C31 C32 1.528(7) . ? C41 C43 1.506(6) . ? C41 C44 1.513(7) . ? C41 C42 1.522(6) . ? C71 C72 1.499(6) . ? C71 C73 1.512(7) . ? C71 C74 1.527(7) . ? C81 C83 1.504(7) . ? C81 C82 1.520(7) . ? C81 C84 1.526(7) . ? C111 C04' 1.500(12) . ? C111 C114 1.509(12) . ? C111 C02' 1.510(12) . ? C111 C03' 1.512(12) . ? C111 C112 1.514(12) . ? C111 C113 1.524(12) . ? C121 C124 1.479(8) . ? C121 C122 1.489(7) . ? C121 C123 1.505(7) . ? C11 C12 1.3900 . ? C11 C16 1.3900 . ? C11 C17 1.441(10) . ? C12 C13 1.3900 . ? C13 C14 1.3900 . ? C14 C15 1.3900 . ? C15 C16 1.3900 . ? C11' C12' 1.3900 . ? C11' C16' 1.3900 . ? C11' C17' 1.426(14) . ? C12' C13' 1.3900 . ? C13' C14' 1.3900 . ? C14' C15' 1.3900 . ? C15' C16' 1.3900 . ? C21 C22 1.3900 . ? C21 C26 1.3900 . ? C21 C27 1.414(12) . ? C22 C23 1.3900 . ? C23 C24 1.3900 . ? C24 C25 1.3900 . ? C25 C26 1.3900 . ? C22' C21' 1.3900 . ? C22' C23' 1.3900 . ? C21' C26' 1.3900 . ? C21' C27' 1.412(15) . ? C26' C25' 1.3900 . ? C25' C24' 1.3900 . ? C24' C23' 1.3900 . ? C1'' C2'' 1.3900 . ? C1'' C6'' 1.3900 . ? C1'' C7'' 1.410(16) . ? C2'' C3'' 1.3900 . ? C3'' C4'' 1.3900 . ? C4'' C5'' 1.3900 . ? C5'' C6'' 1.3900 . ? C51 C52 1.3900 . ? C51 C56 1.3900 . ? C51 C57 1.50(2) . ? C52 C53 1.3900 . ? C53 C54 1.3900 . ? C54 C55 1.3900 . ? C55 C56 1.3900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Dy1 O9 116.73(10) . . ? O2 Dy1 O1 74.80(10) . . ? O9 Dy1 O1 150.64(10) . . ? O2 Dy1 O6 76.42(10) . . ? O9 Dy1 O6 75.93(10) . . ? O1 Dy1 O6 81.43(10) . . ? O2 Dy1 O5 141.37(11) . . ? O9 Dy1 O5 80.51(10) . . ? O1 Dy1 O5 75.71(10) . . ? O6 Dy1 O5 75.00(10) . . ? O2 Dy1 O10 77.16(11) . . ? O9 Dy1 O10 73.54(10) . . ? O1 Dy1 O10 135.54(10) . . ? O6 Dy1 O10 124.02(10) . . ? O5 Dy1 O10 141.11(10) . . ? O2 Dy1 N1B 140.20(11) . . ? O9 Dy1 N1B 82.02(11) . . ? O1 Dy1 N1B 106.60(11) . . ? O6 Dy1 N1B 143.32(10) . . ? O5 Dy1 N1B 72.70(11) . . ? O10 Dy1 N1B 75.38(11) . . ? O2 Dy1 N1A 82.14(11) . . ? O9 Dy1 N1A 134.87(11) . . ? O1 Dy1 N1A 70.97(10) . . ? O6 Dy1 N1A 148.66(11) . . ? O5 Dy1 N1A 110.86(10) . . ? O10 Dy1 N1A 71.60(10) . . ? N1B Dy1 N1A 62.15(11) . . ? C21A N1A C25A 117.7(4) . . ? C21A N1A Dy1 121.7(3) . . ? C25A N1A Dy1 120.6(3) . . ? C1 O1 Dy1 133.2(3) . . ? C3 O2 Dy1 131.8(3) . . ? C3 O3 C31 121.8(4) . . ? C1 O4 C41 123.4(3) . . ? C4 O5 Dy1 130.8(3) . . ? C6 O6 Dy1 131.0(3) . . ? C6 O7 C71 123.0(3) . . ? C4 O8 C81 123.3(4) . . ? C7 O9 Dy1 134.7(3) . . ? C9 O10 Dy1 133.1(3) . . ? C9 O11 C111 125.6(4) . . ? C7 O12 C121 125.0(4) . . ? C25B N1B C21B 117.9(4) . . ? C25B N1B Dy1 117.4(3) . . ? C21B N1B Dy1 122.8(3) . . ? O1 C1 O4 120.1(4) . . ? O1 C1 C2 126.6(4) . . ? O4 C1 C2 113.3(4) . . ? C3 C2 C1 123.1(4) . . ? O2 C3 O3 120.3(4) . . ? O2 C3 C2 126.5(4) . . ? O3 C3 C2 113.2(4) . . ? O5 C4 O8 121.0(4) . . ? O5 C4 C5 126.3(4) . . ? O8 C4 C5 112.6(4) . . ? C6 C5 C4 124.2(4) . . ? O6 C6 O7 119.7(4) . . ? O6 C6 C5 127.3(4) . . ? O7 C6 C5 113.0(4) . . ? O9 C7 O12 120.7(4) . . ? O9 C7 C8 126.1(4) . . ? O12 C7 C8 113.3(4) . . ? C7 C8 C9 123.3(4) . . ? O10 C9 O11 120.8(4) . . ? O10 C9 C8 126.7(4) . . ? O11 C9 C8 112.5(4) . . ? N1A C21A C22A 121.7(4) . . ? N1A C21A C21B 116.2(4) . . ? C22A C21A C21B 122.1(4) . . ? C23A C22A C21A 119.1(5) . . ? C24A C23A C22A 119.7(5) . . ? C23A C24A C25A 118.3(5) . . ? N1A C25A C24A 123.5(5) . . ? N1B C21B C22B 121.7(4) . . ? N1B C21B C21A 115.5(4) . . ? C22B C21B C21A 122.7(4) . . ? C21B C22B C23B 118.1(4) . . ? C24B C23B C22B 120.3(4) . . ? C23B C24B C25B 118.6(5) . . ? N1B C25B C24B 123.3(4) . . ? O3 C31 C34 111.8(4) . . ? O3 C31 C33 108.7(4) . . ? C34 C31 C33 112.8(5) . . ? O3 C31 C32 102.6(4) . . ? C34 C31 C32 110.4(5) . . ? C33 C31 C32 110.1(5) . . ? O4 C41 C43 102.7(4) . . ? O4 C41 C44 111.0(4) . . ? C43 C41 C44 109.7(4) . . ? O4 C41 C42 109.9(4) . . ? C43 C41 C42 110.4(4) . . ? C44 C41 C42 112.8(4) . . ? O7 C71 C72 112.2(4) . . ? O7 C71 C73 110.5(4) . . ? C72 C71 C73 112.0(5) . . ? O7 C71 C74 102.3(4) . . ? C72 C71 C74 110.5(5) . . ? C73 C71 C74 109.0(4) . . ? O8 C81 C83 110.2(4) . . ? O8 C81 C82 111.4(4) . . ? C83 C81 C82 112.5(5) . . ? O8 C81 C84 102.2(4) . . ? C83 C81 C84 109.8(4) . . ? C82 C81 C84 110.2(4) . . ? O11 C111 C04' 118.9(10) . . ? O11 C111 C114 100.1(9) . . ? C04' C111 C114 29.4(12) . . ? O11 C111 C02' 99.2(15) . . ? C04' C111 C02' 112.1(14) . . ? C114 C111 C02' 95.6(16) . . ? O11 C111 C03' 100.4(9) . . ? C04' C111 C03' 112.9(11) . . ? C114 C111 C03' 141.9(12) . . ? C02' C111 C03' 112.3(12) . . ? O11 C111 C112 108.0(13) . . ? C04' C111 C112 119.1(17) . . ? C114 C111 C112 110.5(12) . . ? C02' C111 C112 19.7(19) . . ? C03' C111 C112 93.0(13) . . ? O11 C111 C113 118.0(10) . . ? C04' C111 C113 80.9(11) . . ? C114 C111 C113 110.1(10) . . ? C02' C111 C113 128.6(16) . . ? C03' C111 C113 32.0(9) . . ? C112 C111 C113 109.7(12) . . ? O12 C121 C124 111.4(4) . . ? O12 C121 C122 110.1(5) . . ? C124 C121 C122 111.3(6) . . ? O12 C121 C123 102.4(4) . . ? C124 C121 C123 109.6(5) . . ? C122 C121 C123 111.8(5) . . ? C12 C11 C16 120.0 . . ? C12 C11 C17 119.2(8) . . ? C16 C11 C17 120.7(8) . . ? C11 C12 C13 120.0 . . ? C12 C13 C14 120.0 . . ? C15 C14 C13 120.0 . . ? C14 C15 C16 120.0 . . ? C15 C16 C11 120.0 . . ? C12' C11' C16' 120.0 . . ? C12' C11' C17' 121.7(13) . . ? C16' C11' C17' 118.1(13) . . ? C11' C12' C13' 120.0 . . ? C12' C13' C14' 120.0 . . ? C13' C14' C15' 120.0 . . ? C14' C15' C16' 120.0 . . ? C15' C16' C11' 120.0 . . ? C22 C21 C26 120.0 . . ? C22 C21 C27 117.3(9) . . ? C26 C21 C27 122.4(9) . . ? C21 C22 C23 120.0 . . ? C24 C23 C22 120.0 . . ? C23 C24 C25 120.0 . . ? C26 C25 C24 120.0 . . ? C25 C26 C21 120.0 . . ? C21' C22' C23' 120.0 . . ? C22' C21' C26' 120.0 . . ? C22' C21' C27' 117.5(13) . . ? C26' C21' C27' 122.5(13) . . ? C25' C26' C21' 120.0 . . ? C24' C25' C26' 120.0 . . ? C25' C24' C23' 120.0 . . ? C24' C23' C22' 120.0 . . ? C2'' C1'' C6'' 120.0 . . ? C2'' C1'' C7'' 116.7(14) . . ? C6'' C1'' C7'' 123.3(14) . . ? C1'' C2'' C3'' 120.0 . . ? C4'' C3'' C2'' 120.0 . . ? C3'' C4'' C5'' 120.0 . . ? C6'' C5'' C4'' 120.0 . . ? C5'' C6'' C1'' 120.0 . . ? C52 C51 C56 120.0 . . ? C52 C51 C57 120.2(8) . . ? C56 C51 C57 119.8(8) . . ? C51 C52 C53 120.0 . . ? C54 C53 C52 120.0 . . ? C53 C54 C55 120.0 . . ? C56 C55 C54 120.0 . . ? C55 C56 C51 120.0 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.898 _refine_diff_density_min -0.705 _refine_diff_density_rms 0.097 #=================================END data_cvd194a _database_code_depnum_ccdc_archive 'CCDC 770264' #TrackingRef '- combined cif files.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H65 Dy N2 O12 Si6' _chemical_formula_weight 1060.95 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.5397(4) _cell_length_b 15.2934(6) _cell_length_c 17.4762(8) _cell_angle_alpha 65.409(4) _cell_angle_beta 72.152(4) _cell_angle_gamma 73.604(3) _cell_volume 2626.51(18) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 7293 _cell_measurement_theta_min 2.581 _cell_measurement_theta_max 36.799 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.342 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1094 _exptl_absorpt_coefficient_mu 1.611 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.560 _exptl_absorpt_correction_T_max 0.660 _exptl_absorpt_process_details abspack _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Sapphire2-CCD, Oxford Diffraction' _diffrn_measurement_method '560 images at 1.0 deg. in \w and 15 sec.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13076 _diffrn_reflns_av_R_equivalents 0.0373 _diffrn_reflns_av_sigmaI/netI 0.0949 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8915 _reflns_number_gt 6456 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD 1.171.13, Oxford Diffraction' _computing_cell_refinement 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_data_reduction 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0216P)^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 8915 _refine_ls_number_parameters 523 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0628 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.0670 _refine_ls_wR_factor_gt 0.0623 _refine_ls_goodness_of_fit_ref 0.860 _refine_ls_restrained_S_all 0.860 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.79250(2) 0.798134(16) 0.726294(15) 0.02211(7) Uani 1 1 d . . . Si1 Si 0.66538(12) 0.62294(9) 0.57913(9) 0.0307(3) Uani 1 1 d . . . Si6 Si 1.11821(12) 0.48396(9) 0.70540(8) 0.0300(3) Uani 1 1 d . . . Si4 Si 0.75124(13) 1.19698(10) 0.73914(10) 0.0379(4) Uani 1 1 d . . . Si2 Si 0.37148(13) 1.00720(10) 0.79343(10) 0.0410(4) Uani 1 1 d . . . O1 O 0.6906(3) 0.7250(2) 0.67808(18) 0.0224(7) Uani 1 1 d . . . O9 O 0.7078(2) 0.6943(2) 0.86148(18) 0.0230(7) Uani 1 1 d . . . O10 O 0.9179(2) 0.6455(2) 0.74077(17) 0.0236(7) Uani 1 1 d . . . O5 O 0.7829(3) 0.9601(2) 0.70458(18) 0.0253(7) Uani 1 1 d . . . O2 O 0.5847(3) 0.87145(19) 0.74787(18) 0.0255(7) Uani 1 1 d . . . O11 O 0.9805(3) 0.4837(2) 0.77326(18) 0.0271(7) Uani 1 1 d . . . O4 O 0.5540(3) 0.6799(2) 0.6401(2) 0.0317(8) Uani 1 1 d . . . O6 O 0.9031(3) 0.8000(2) 0.81809(18) 0.0252(7) Uani 1 1 d . . . O8 O 0.7431(3) 1.1001(2) 0.72214(18) 0.0295(8) Uani 1 1 d . . . O3 O 0.3790(3) 0.9069(2) 0.77343(19) 0.0305(8) Uani 1 1 d . . . C3 C 0.4864(4) 0.8529(3) 0.7455(3) 0.0236(11) Uani 1 1 d . . . N1 N 0.7977(3) 0.8977(2) 0.5642(2) 0.0224(9) Uani 1 1 d . . . N2 N 1.0043(3) 0.8188(2) 0.6238(2) 0.0237(9) Uani 1 1 d . . . C9 C 0.9031(4) 0.5597(3) 0.7924(3) 0.0228(11) Uani 1 1 d . . . C4 C 0.7940(4) 1.0039(3) 0.7477(3) 0.0229(10) Uani 1 1 d . . . C1 C 0.5790(4) 0.7310(3) 0.6783(3) 0.0228(11) Uani 1 1 d . . . Si3 Si 1.03617(12) 0.72537(10) 0.96284(9) 0.0302(3) Uani 1 1 d . . . Si5 Si 0.54624(12) 0.63036(10) 1.03172(8) 0.0320(3) Uani 1 1 d . . . O12 O 0.6612(2) 0.5655(2) 0.98010(18) 0.0273(7) Uani 1 1 d . . . O7 O 0.9599(3) 0.8356(2) 0.9119(2) 0.0458(9) Uani 1 1 d . . . C7 C 0.7271(4) 0.6033(3) 0.8988(3) 0.0230(11) Uani 1 1 d . . . C2 C 0.4759(4) 0.7881(3) 0.7129(3) 0.0248(11) Uani 1 1 d . . . H2A H 0.3956 0.7820 0.7139 0.030 Uiso 1 1 calc R . . C92 C 1.2249(4) 0.7729(3) 0.6063(3) 0.0304(12) Uani 1 1 d . . . H92A H 1.2945 0.7392 0.6318 0.036 Uiso 1 1 calc R . . C97 C 0.9041(4) 0.9612(3) 0.4177(3) 0.0294(11) Uani 1 1 d . . . H97A H 0.9804 0.9676 0.3766 0.035 Uiso 1 1 calc R . . C8 C 0.8135(4) 0.5348(3) 0.8680(3) 0.0253(11) Uani 1 1 d . . . H8A H 0.8112 0.4674 0.9004 0.030 Uiso 1 1 calc R . . C94 C 1.1357(4) 0.8652(3) 0.4843(3) 0.0311(12) Uani 1 1 d . . . H94A H 1.1444 0.8978 0.4238 0.037 Uiso 1 1 calc R . . C95 C 1.0188(4) 0.8631(3) 0.5380(3) 0.0237(11) Uani 1 1 d . . . C96 C 0.9040(4) 0.9096(3) 0.5044(3) 0.0241(11) Uani 1 1 d . . . C91 C 1.1059(4) 0.7760(3) 0.6563(3) 0.0278(11) Uani 1 1 d . . . H91A H 1.0956 0.7461 0.7172 0.033 Uiso 1 1 calc R . . C6 C 0.9052(4) 0.8629(3) 0.8449(3) 0.0311(12) Uani 1 1 d . . . C98 C 0.7948(5) 1.0029(3) 0.3910(3) 0.0352(13) Uani 1 1 d . . . H98A H 0.7945 1.0387 0.3317 0.042 Uiso 1 1 calc R . . C99 C 0.6851(5) 0.9922(3) 0.4519(3) 0.0332(12) Uani 1 1 d . . . H99A H 0.6074 1.0199 0.4358 0.040 Uiso 1 1 calc R . . C93 C 1.2392(4) 0.8198(3) 0.5190(3) 0.0332(12) Uani 1 1 d . . . H93A H 1.3195 0.8212 0.4826 0.040 Uiso 1 1 calc R . . C90 C 0.6922(4) 0.9401(3) 0.5365(3) 0.0297(12) Uani 1 1 d . . . H90A H 0.6168 0.9336 0.5785 0.036 Uiso 1 1 calc R . . C5 C 0.8527(4) 0.9622(3) 0.8159(3) 0.0352(12) Uani 1 1 d . . . H5A H 0.8576 1.0020 0.8440 0.042 Uiso 1 1 calc R . . C61 C 1.2246(4) 0.5178(3) 0.7445(3) 0.0400(13) Uani 1 1 d . . . H61A H 1.1985 0.5866 0.7387 0.060 Uiso 1 1 calc R . . H61B H 1.3088 0.5078 0.7103 0.060 Uiso 1 1 calc R . . H61C H 1.2229 0.4768 0.8052 0.060 Uiso 1 1 calc R . . C11 C 0.7622(4) 0.5187(3) 0.6448(3) 0.0395(13) Uani 1 1 d . . . H11A H 0.8103 0.5425 0.6673 0.059 Uiso 1 1 calc R . . H11B H 0.8187 0.4820 0.6093 0.059 Uiso 1 1 calc R . . H11C H 0.7094 0.4760 0.6930 0.059 Uiso 1 1 calc R . . C62 C 1.1074(4) 0.5635(4) 0.5933(3) 0.0420(13) Uani 1 1 d . . . H62A H 1.0805 0.6318 0.5893 0.063 Uiso 1 1 calc R . . H62B H 1.0473 0.5448 0.5762 0.063 Uiso 1 1 calc R . . H62C H 1.1886 0.5562 0.5548 0.063 Uiso 1 1 calc R . . C31 C 1.0725(4) 0.7518(3) 1.0462(3) 0.0408(13) Uani 1 1 d . . . H31A H 0.9954 0.7704 1.0839 0.061 Uiso 1 1 calc R . . H31B H 1.1192 0.8056 1.0183 0.061 Uiso 1 1 calc R . . H31C H 1.1222 0.6934 1.0804 0.061 Uiso 1 1 calc R . . C51 C 0.6033(5) 0.7225(4) 1.0470(3) 0.0478(15) Uani 1 1 d . . . H51A H 0.6288 0.7726 0.9909 0.072 Uiso 1 1 calc R . . H51B H 0.6742 0.6905 1.0746 0.072 Uiso 1 1 calc R . . H51C H 0.5371 0.7532 1.0836 0.072 Uiso 1 1 calc R . . C12 C 0.7623(5) 0.7090(4) 0.4914(3) 0.0462(14) Uani 1 1 d . . . H12A H 0.8111 0.7293 0.5162 0.069 Uiso 1 1 calc R . . H12B H 0.7090 0.7665 0.4595 0.069 Uiso 1 1 calc R . . H12C H 0.8181 0.6766 0.4522 0.069 Uiso 1 1 calc R . . C63 C 1.1694(5) 0.3539(3) 0.7157(3) 0.0481(15) Uani 1 1 d . . . H63A H 1.1129 0.3354 0.6954 0.072 Uiso 1 1 calc R . . H63B H 1.1689 0.3127 0.7762 0.072 Uiso 1 1 calc R . . H63C H 1.2533 0.3449 0.6809 0.072 Uiso 1 1 calc R . . C52 C 0.4218(4) 0.6860(4) 0.9717(3) 0.0449(14) Uani 1 1 d . . . H52A H 0.3940 0.6348 0.9656 0.067 Uiso 1 1 calc R . . H52B H 0.4527 0.7321 0.9145 0.067 Uiso 1 1 calc R . . H52C H 0.3523 0.7209 1.0030 0.067 Uiso 1 1 calc R . . C53 C 0.4971(4) 0.5345(4) 1.1369(3) 0.0490(15) Uani 1 1 d . . . H53A H 0.4669 0.4867 1.1276 0.073 Uiso 1 1 calc R . . H53B H 0.4308 0.5646 1.1739 0.073 Uiso 1 1 calc R . . H53C H 0.5676 0.5017 1.1647 0.073 Uiso 1 1 calc R . . C33 C 1.1723(5) 0.6887(4) 0.8885(3) 0.0568(17) Uani 1 1 d . . . H33A H 1.1462 0.6760 0.8464 0.085 Uiso 1 1 calc R . . H33B H 1.2228 0.6292 0.9208 0.085 Uiso 1 1 calc R . . H33C H 1.2212 0.7411 0.8585 0.085 Uiso 1 1 calc R . . C21 C 0.4464(5) 1.0967(3) 0.6933(4) 0.0543(16) Uani 1 1 d . . . H21A H 0.4069 1.1099 0.6463 0.081 Uiso 1 1 calc R . . H21B H 0.5344 1.0699 0.6782 0.081 Uiso 1 1 calc R . . H21C H 0.4374 1.1576 0.7023 0.081 Uiso 1 1 calc R . . C41 C 0.6230(5) 1.2883(4) 0.6946(4) 0.0645(19) Uani 1 1 d . . . H41A H 0.5443 1.2670 0.7288 0.097 Uiso 1 1 calc R . . H41B H 0.6328 1.2954 0.6347 0.097 Uiso 1 1 calc R . . H41C H 0.6235 1.3513 0.6966 0.097 Uiso 1 1 calc R . . C13 C 0.5721(5) 0.5827(4) 0.5343(3) 0.0507(15) Uani 1 1 d . . . H13A H 0.5214 0.5374 0.5815 0.076 Uiso 1 1 calc R . . H13B H 0.6274 0.5498 0.4954 0.076 Uiso 1 1 calc R . . H13C H 0.5182 0.6397 0.5023 0.076 Uiso 1 1 calc R . . C23 C 0.4413(5) 0.9792(4) 0.8845(3) 0.0598(17) Uani 1 1 d . . . H23A H 0.5308 0.9575 0.8688 0.090 Uiso 1 1 calc R . . H23B H 0.4049 0.9273 0.9348 0.090 Uiso 1 1 calc R . . H23C H 0.4254 1.0380 0.8983 0.090 Uiso 1 1 calc R . . C32 C 0.9367(5) 0.6330(4) 1.0111(4) 0.066(2) Uani 1 1 d . . . H32A H 0.9187 0.6210 0.9654 0.099 Uiso 1 1 calc R . . H32B H 0.8591 0.6564 1.0456 0.099 Uiso 1 1 calc R . . H32C H 0.9790 0.5721 1.0482 0.099 Uiso 1 1 calc R . . C22 C 0.2017(5) 1.0498(4) 0.8206(4) 0.073(2) Uani 1 1 d . . . H22A H 0.1662 1.0641 0.7715 0.110 Uiso 1 1 calc R . . H22B H 0.1855 1.1092 0.8336 0.110 Uiso 1 1 calc R . . H22C H 0.1639 0.9987 0.8709 0.110 Uiso 1 1 calc R . . C42 C 0.9029(5) 1.2334(4) 0.6792(5) 0.079(2) Uani 1 1 d . . . H42A H 0.9686 1.1832 0.7051 0.118 Uiso 1 1 calc R . . H42B H 0.9045 1.2959 0.6817 0.118 Uiso 1 1 calc R . . H42C H 0.9162 1.2404 0.6189 0.118 Uiso 1 1 calc R . . C43 C 0.7306(6) 1.1749(4) 0.8526(4) 0.0731(19) Uani 1 1 d . . . H43A H 0.6498 1.1561 0.8840 0.110 Uiso 1 1 calc R . . H43B H 0.7349 1.2346 0.8590 0.110 Uiso 1 1 calc R . . H43C H 0.7961 1.1221 0.8761 0.110 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.02352(13) 0.01860(11) 0.02027(12) -0.00462(9) -0.00414(9) -0.00230(9) Si1 0.0331(8) 0.0297(8) 0.0339(8) -0.0167(6) -0.0077(6) -0.0040(6) Si6 0.0283(8) 0.0261(7) 0.0277(8) -0.0097(6) -0.0011(6) 0.0015(6) Si4 0.0383(9) 0.0259(8) 0.0546(10) -0.0220(7) -0.0128(7) 0.0012(7) Si2 0.0371(9) 0.0326(8) 0.0553(11) -0.0252(8) -0.0132(7) 0.0086(7) O1 0.0240(19) 0.0221(17) 0.0222(18) -0.0097(14) -0.0054(14) -0.0028(14) O9 0.0164(17) 0.0205(17) 0.0244(18) -0.0058(14) -0.0004(13) 0.0002(13) O10 0.0212(17) 0.0222(16) 0.0212(17) -0.0028(14) -0.0016(13) -0.0054(14) O5 0.0302(19) 0.0187(16) 0.0256(19) -0.0075(14) -0.0085(14) -0.0004(14) O2 0.0221(18) 0.0219(17) 0.0303(19) -0.0098(14) -0.0063(14) 0.0005(14) O11 0.0286(19) 0.0172(16) 0.0283(19) -0.0072(14) -0.0040(14) 0.0027(14) O4 0.0277(19) 0.0349(19) 0.043(2) -0.0254(17) -0.0060(15) -0.0060(15) O6 0.0266(18) 0.0216(17) 0.0265(19) -0.0085(14) -0.0058(14) -0.0032(14) O8 0.042(2) 0.0187(17) 0.0250(19) -0.0084(14) -0.0104(15) 0.0038(15) O3 0.0224(18) 0.0276(18) 0.039(2) -0.0168(16) -0.0041(15) 0.0045(15) C3 0.023(3) 0.017(2) 0.020(3) -0.002(2) -0.003(2) 0.003(2) N1 0.025(2) 0.022(2) 0.021(2) -0.0071(17) -0.0052(17) -0.0049(17) N2 0.025(2) 0.019(2) 0.026(2) -0.0051(17) -0.0069(17) -0.0049(17) C9 0.021(3) 0.020(3) 0.028(3) -0.006(2) -0.011(2) -0.001(2) C4 0.026(3) 0.018(2) 0.019(3) -0.009(2) 0.003(2) 0.000(2) C1 0.031(3) 0.017(2) 0.021(3) -0.005(2) -0.008(2) -0.004(2) Si3 0.0300(8) 0.0314(8) 0.0305(8) -0.0114(6) -0.0134(6) 0.0006(6) Si5 0.0239(8) 0.0414(8) 0.0264(8) -0.0120(7) -0.0026(6) -0.0027(7) O12 0.0212(17) 0.0285(17) 0.0203(18) -0.0030(14) 0.0010(13) -0.0017(14) O7 0.071(3) 0.033(2) 0.044(2) -0.0158(17) -0.042(2) 0.0102(18) C7 0.023(3) 0.027(3) 0.017(3) -0.002(2) -0.005(2) -0.009(2) C2 0.019(3) 0.027(3) 0.030(3) -0.015(2) -0.004(2) -0.001(2) C92 0.020(3) 0.031(3) 0.039(3) -0.013(2) -0.005(2) -0.005(2) C97 0.039(3) 0.024(3) 0.019(3) -0.004(2) -0.004(2) -0.002(2) C8 0.029(3) 0.015(2) 0.025(3) -0.004(2) -0.004(2) -0.001(2) C94 0.032(3) 0.034(3) 0.022(3) -0.007(2) 0.001(2) -0.010(2) C95 0.027(3) 0.018(2) 0.024(3) -0.006(2) -0.001(2) -0.007(2) C96 0.032(3) 0.015(2) 0.025(3) -0.009(2) -0.003(2) -0.003(2) C91 0.030(3) 0.023(3) 0.026(3) -0.006(2) -0.004(2) -0.006(2) C6 0.034(3) 0.031(3) 0.024(3) -0.006(2) -0.006(2) -0.004(2) C98 0.053(4) 0.027(3) 0.021(3) -0.001(2) -0.013(3) -0.006(3) C99 0.041(3) 0.025(3) 0.032(3) -0.003(2) -0.018(3) -0.004(2) C93 0.026(3) 0.031(3) 0.039(3) -0.016(2) 0.010(2) -0.013(2) C90 0.031(3) 0.026(3) 0.029(3) -0.005(2) -0.007(2) -0.009(2) C5 0.054(3) 0.024(3) 0.035(3) -0.014(2) -0.025(3) 0.005(2) C61 0.033(3) 0.035(3) 0.041(3) -0.005(3) -0.008(2) -0.004(2) C11 0.041(3) 0.033(3) 0.042(3) -0.016(3) -0.003(2) -0.005(3) C62 0.043(3) 0.048(3) 0.029(3) -0.016(3) -0.001(2) -0.004(3) C31 0.047(3) 0.037(3) 0.034(3) -0.014(3) -0.018(3) 0.010(3) C51 0.044(4) 0.053(4) 0.049(4) -0.027(3) -0.012(3) 0.003(3) C12 0.061(4) 0.040(3) 0.035(3) -0.015(3) -0.005(3) -0.010(3) C63 0.047(4) 0.036(3) 0.049(4) -0.021(3) 0.003(3) 0.005(3) C52 0.028(3) 0.059(4) 0.042(3) -0.021(3) -0.009(2) 0.006(3) C53 0.039(3) 0.069(4) 0.026(3) -0.013(3) 0.006(2) -0.009(3) C33 0.041(3) 0.093(5) 0.045(4) -0.039(4) -0.018(3) 0.007(3) C21 0.060(4) 0.029(3) 0.077(5) -0.014(3) -0.032(3) 0.001(3) C41 0.066(4) 0.027(3) 0.114(6) -0.031(3) -0.047(4) 0.010(3) C13 0.052(4) 0.061(4) 0.058(4) -0.043(3) -0.013(3) -0.003(3) C23 0.078(5) 0.061(4) 0.047(4) -0.032(3) -0.013(3) -0.003(3) C32 0.064(4) 0.059(4) 0.068(5) 0.007(3) -0.042(3) -0.017(3) C22 0.055(4) 0.065(4) 0.108(6) -0.059(4) -0.012(4) 0.014(3) C42 0.054(4) 0.041(4) 0.135(7) -0.034(4) -0.004(4) -0.015(3) C43 0.090(5) 0.067(4) 0.079(5) -0.054(4) -0.034(4) 0.020(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O5 2.319(3) . ? Dy1 O9 2.323(3) . ? Dy1 O2 2.330(3) . ? Dy1 O10 2.331(3) . ? Dy1 O1 2.341(3) . ? Dy1 O6 2.349(3) . ? Dy1 N2 2.562(3) . ? Dy1 N1 2.590(3) . ? Si1 O4 1.687(3) . ? Si1 C11 1.834(5) . ? Si1 C12 1.853(4) . ? Si1 C13 1.855(4) . ? Si6 O11 1.666(3) . ? Si6 C61 1.846(5) . ? Si6 C62 1.848(5) . ? Si6 C63 1.855(5) . ? Si4 O8 1.659(3) . ? Si4 C43 1.818(6) . ? Si4 C41 1.839(5) . ? Si4 C42 1.847(5) . ? Si2 O3 1.683(3) . ? Si2 C23 1.842(5) . ? Si2 C21 1.852(5) . ? Si2 C22 1.859(6) . ? O1 C1 1.264(5) . ? O9 C7 1.254(5) . ? O10 C9 1.270(4) . ? O5 C4 1.250(5) . ? O2 C3 1.262(5) . ? O11 C9 1.347(5) . ? O4 C1 1.349(5) . ? O6 C6 1.241(5) . ? O8 C4 1.355(5) . ? O3 C3 1.358(5) . ? C3 C2 1.379(6) . ? N1 C90 1.337(5) . ? N1 C96 1.346(5) . ? N2 C91 1.339(5) . ? N2 C95 1.341(5) . ? C9 C8 1.388(6) . ? C4 C5 1.380(6) . ? C1 C2 1.398(6) . ? Si3 O7 1.674(3) . ? Si3 C33 1.824(5) . ? Si3 C32 1.832(5) . ? Si3 C31 1.849(5) . ? Si5 O12 1.681(3) . ? Si5 C52 1.838(5) . ? Si5 C53 1.853(5) . ? Si5 C51 1.854(5) . ? O12 C7 1.354(5) . ? O7 C6 1.357(5) . ? C7 C8 1.390(6) . ? C2 H2A 0.9500 . ? C92 C93 1.368(6) . ? C92 C91 1.384(6) . ? C92 H92A 0.9500 . ? C97 C98 1.369(6) . ? C97 C96 1.386(6) . ? C97 H97A 0.9500 . ? C8 H8A 0.9500 . ? C94 C93 1.378(6) . ? C94 C95 1.387(6) . ? C94 H94A 0.9500 . ? C95 C96 1.485(6) . ? C91 H91A 0.9500 . ? C6 C5 1.399(6) . ? C98 C99 1.381(6) . ? C98 H98A 0.9500 . ? C99 C90 1.374(6) . ? C99 H99A 0.9500 . ? C93 H93A 0.9500 . ? C90 H90A 0.9500 . ? C5 H5A 0.9500 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Dy1 O9 119.29(10) . . ? O5 Dy1 O2 72.04(9) . . ? O9 Dy1 O2 76.93(10) . . ? O5 Dy1 O10 146.34(9) . . ? O9 Dy1 O10 75.08(10) . . ? O2 Dy1 O10 141.03(9) . . ? O5 Dy1 O1 132.03(10) . . ? O9 Dy1 O1 83.35(9) . . ? O2 Dy1 O1 73.53(10) . . ? O10 Dy1 O1 76.77(10) . . ? O5 Dy1 O6 72.29(10) . . ? O9 Dy1 O6 75.91(9) . . ? O2 Dy1 O6 115.06(10) . . ? O10 Dy1 O6 83.55(10) . . ? O1 Dy1 O6 154.47(9) . . ? O5 Dy1 N2 82.55(10) . . ? O9 Dy1 N2 139.22(10) . . ? O2 Dy1 N2 143.66(10) . . ? O10 Dy1 N2 70.09(10) . . ? O1 Dy1 N2 108.03(10) . . ? O6 Dy1 N2 79.68(10) . . ? O5 Dy1 N1 72.93(10) . . ? O9 Dy1 N1 152.89(10) . . ? O2 Dy1 N1 85.34(11) . . ? O10 Dy1 N1 108.77(11) . . ? O1 Dy1 N1 71.94(10) . . ? O6 Dy1 N1 130.78(9) . . ? N2 Dy1 N1 62.18(11) . . ? O4 Si1 C11 111.3(2) . . ? O4 Si1 C12 111.2(2) . . ? C11 Si1 C12 110.3(2) . . ? O4 Si1 C13 101.6(2) . . ? C11 Si1 C13 111.6(2) . . ? C12 Si1 C13 110.6(2) . . ? O11 Si6 C61 109.1(2) . . ? O11 Si6 C62 112.18(19) . . ? C61 Si6 C62 112.4(2) . . ? O11 Si6 C63 102.73(19) . . ? C61 Si6 C63 109.1(2) . . ? C62 Si6 C63 110.9(2) . . ? O8 Si4 C43 112.9(2) . . ? O8 Si4 C41 102.4(2) . . ? C43 Si4 C41 111.0(3) . . ? O8 Si4 C42 108.6(2) . . ? C43 Si4 C42 109.8(3) . . ? C41 Si4 C42 112.0(3) . . ? O3 Si2 C23 112.5(2) . . ? O3 Si2 C21 108.2(2) . . ? C23 Si2 C21 111.7(2) . . ? O3 Si2 C22 101.9(2) . . ? C23 Si2 C22 110.7(3) . . ? C21 Si2 C22 111.4(3) . . ? C1 O1 Dy1 134.7(3) . . ? C7 O9 Dy1 133.0(3) . . ? C9 O10 Dy1 132.3(3) . . ? C4 O5 Dy1 135.3(3) . . ? C3 O2 Dy1 134.4(3) . . ? C9 O11 Si6 127.8(3) . . ? C1 O4 Si1 122.7(3) . . ? C6 O6 Dy1 133.3(3) . . ? C4 O8 Si4 136.3(3) . . ? C3 O3 Si2 123.9(3) . . ? O2 C3 O3 116.3(4) . . ? O2 C3 C2 127.3(4) . . ? O3 C3 C2 116.3(4) . . ? C90 N1 C96 117.0(4) . . ? C90 N1 Dy1 120.3(3) . . ? C96 N1 Dy1 122.6(3) . . ? C91 N2 C95 118.2(4) . . ? C91 N2 Dy1 118.5(3) . . ? C95 N2 Dy1 123.1(3) . . ? O10 C9 O11 118.1(4) . . ? O10 C9 C8 126.6(4) . . ? O11 C9 C8 115.2(4) . . ? O5 C4 O8 114.5(4) . . ? O5 C4 C5 125.4(4) . . ? O8 C4 C5 120.2(4) . . ? O1 C1 O4 118.4(4) . . ? O1 C1 C2 126.6(4) . . ? O4 C1 C2 115.1(4) . . ? O7 Si3 C33 110.4(2) . . ? O7 Si3 C32 111.3(2) . . ? C33 Si3 C32 109.6(3) . . ? O7 Si3 C31 99.71(19) . . ? C33 Si3 C31 114.0(2) . . ? C32 Si3 C31 111.5(2) . . ? O12 Si5 C52 108.8(2) . . ? O12 Si5 C53 102.1(2) . . ? C52 Si5 C53 111.3(2) . . ? O12 Si5 C51 111.4(2) . . ? C52 Si5 C51 112.2(2) . . ? C53 Si5 C51 110.6(2) . . ? C7 O12 Si5 124.9(3) . . ? C6 O7 Si3 128.4(3) . . ? O9 C7 O12 117.7(4) . . ? O9 C7 C8 127.5(4) . . ? O12 C7 C8 114.7(4) . . ? C3 C2 C1 122.4(4) . . ? C3 C2 H2A 118.8 . . ? C1 C2 H2A 118.8 . . ? C93 C92 C91 117.9(4) . . ? C93 C92 H92A 121.1 . . ? C91 C92 H92A 121.1 . . ? C98 C97 C96 120.3(4) . . ? C98 C97 H97A 119.9 . . ? C96 C97 H97A 119.9 . . ? C9 C8 C7 123.3(4) . . ? C9 C8 H8A 118.3 . . ? C7 C8 H8A 118.3 . . ? C93 C94 C95 119.9(4) . . ? C93 C94 H94A 120.0 . . ? C95 C94 H94A 120.0 . . ? N2 C95 C94 121.1(4) . . ? N2 C95 C96 116.5(4) . . ? C94 C95 C96 122.4(4) . . ? N1 C96 C97 121.5(4) . . ? N1 C96 C95 115.3(4) . . ? C97 C96 C95 123.2(4) . . ? N2 C91 C92 123.7(4) . . ? N2 C91 H91A 118.2 . . ? C92 C91 H91A 118.2 . . ? O6 C6 O7 119.0(4) . . ? O6 C6 C5 127.5(4) . . ? O7 C6 C5 113.5(4) . . ? C97 C98 C99 118.8(4) . . ? C97 C98 H98A 120.6 . . ? C99 C98 H98A 120.6 . . ? C90 C99 C98 117.6(4) . . ? C90 C99 H99A 121.2 . . ? C98 C99 H99A 121.2 . . ? C92 C93 C94 119.3(4) . . ? C92 C93 H93A 120.4 . . ? C94 C93 H93A 120.4 . . ? N1 C90 C99 124.8(4) . . ? N1 C90 H90A 117.6 . . ? C99 C90 H90A 117.6 . . ? C4 C5 C6 122.0(4) . . ? C4 C5 H5A 119.0 . . ? C6 C5 H5A 119.0 . . ? Si6 C61 H61A 109.5 . . ? Si6 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? Si6 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? Si1 C11 H11A 109.5 . . ? Si1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si6 C62 H62A 109.5 . . ? Si6 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? Si6 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? Si3 C31 H31A 109.5 . . ? Si3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si5 C51 H51A 109.5 . . ? Si5 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? Si5 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? Si1 C12 H12A 109.5 . . ? Si1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si6 C63 H63A 109.5 . . ? Si6 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? Si6 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? Si5 C52 H52A 109.5 . . ? Si5 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? Si5 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? Si5 C53 H53A 109.5 . . ? Si5 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? Si5 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? Si3 C33 H33A 109.5 . . ? Si3 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Si3 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Si2 C21 H21A 109.5 . . ? Si2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si4 C41 H41A 109.5 . . ? Si4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? Si4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? Si1 C13 H13A 109.5 . . ? Si1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si2 C23 H23A 109.5 . . ? Si2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si3 C32 H32A 109.5 . . ? Si3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Si2 C22 H22A 109.5 . . ? Si2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si4 C42 H42A 109.5 . . ? Si4 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? Si4 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? Si4 C43 H43A 109.5 . . ? Si4 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? Si4 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? 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 O5 Dy1 O1 C1 -50.4(4) . . . . ? O9 Dy1 O1 C1 73.5(3) . . . . ? O2 Dy1 O1 C1 -4.8(3) . . . . ? O10 Dy1 O1 C1 149.7(4) . . . . ? O6 Dy1 O1 C1 109.1(4) . . . . ? N2 Dy1 O1 C1 -146.7(3) . . . . ? N1 Dy1 O1 C1 -95.2(4) . . . . ? O5 Dy1 O9 C7 -156.9(3) . . . . ? O2 Dy1 O9 C7 142.6(4) . . . . ? O10 Dy1 O9 C7 -10.0(3) . . . . ? O1 Dy1 O9 C7 68.1(4) . . . . ? O6 Dy1 O9 C7 -96.9(4) . . . . ? N2 Dy1 O9 C7 -41.9(4) . . . . ? N1 Dy1 O9 C7 92.2(4) . . . . ? O5 Dy1 O10 C9 136.6(3) . . . . ? O9 Dy1 O10 C9 15.7(3) . . . . ? O2 Dy1 O10 C9 -29.8(4) . . . . ? O1 Dy1 O10 C9 -70.9(4) . . . . ? O6 Dy1 O10 C9 92.8(4) . . . . ? N2 Dy1 O10 C9 174.1(4) . . . . ? N1 Dy1 O10 C9 -136.2(4) . . . . ? O9 Dy1 O5 C4 39.0(4) . . . . ? O2 Dy1 O5 C4 102.0(4) . . . . ? O10 Dy1 O5 C4 -69.1(4) . . . . ? O1 Dy1 O5 C4 148.0(4) . . . . ? O6 Dy1 O5 C4 -22.9(4) . . . . ? N2 Dy1 O5 C4 -104.4(4) . . . . ? N1 Dy1 O5 C4 -167.5(4) . . . . ? O5 Dy1 O2 C3 157.8(4) . . . . ? O9 Dy1 O2 C3 -75.1(4) . . . . ? O10 Dy1 O2 C3 -30.1(4) . . . . ? O1 Dy1 O2 C3 11.7(3) . . . . ? O6 Dy1 O2 C3 -142.5(3) . . . . ? N2 Dy1 O2 C3 109.9(4) . . . . ? N1 Dy1 O2 C3 84.2(4) . . . . ? C61 Si6 O11 C9 62.9(4) . . . . ? C62 Si6 O11 C9 -62.3(4) . . . . ? C63 Si6 O11 C9 178.5(4) . . . . ? C11 Si1 O4 C1 68.7(3) . . . . ? C12 Si1 O4 C1 -54.8(4) . . . . ? C13 Si1 O4 C1 -172.4(3) . . . . ? O5 Dy1 O6 C6 17.7(4) . . . . ? O9 Dy1 O6 C6 -109.8(4) . . . . ? O2 Dy1 O6 C6 -41.8(4) . . . . ? O10 Dy1 O6 C6 174.0(4) . . . . ? O1 Dy1 O6 C6 -146.4(4) . . . . ? N2 Dy1 O6 C6 103.1(4) . . . . ? N1 Dy1 O6 C6 64.7(4) . . . . ? C43 Si4 O8 C4 -49.0(5) . . . . ? C41 Si4 O8 C4 -168.4(4) . . . . ? C42 Si4 O8 C4 73.0(5) . . . . ? C23 Si2 O3 C3 -65.5(4) . . . . ? C21 Si2 O3 C3 58.4(4) . . . . ? C22 Si2 O3 C3 175.9(4) . . . . ? Dy1 O2 C3 O3 171.5(2) . . . . ? Dy1 O2 C3 C2 -12.7(6) . . . . ? Si2 O3 C3 O2 11.2(5) . . . . ? Si2 O3 C3 C2 -165.1(3) . . . . ? O5 Dy1 N1 C90 -86.7(3) . . . . ? O9 Dy1 N1 C90 34.9(4) . . . . ? O2 Dy1 N1 C90 -14.0(3) . . . . ? O10 Dy1 N1 C90 128.7(3) . . . . ? O1 Dy1 N1 C90 60.1(3) . . . . ? O6 Dy1 N1 C90 -133.4(3) . . . . ? N2 Dy1 N1 C90 -177.2(3) . . . . ? O5 Dy1 N1 C96 93.3(3) . . . . ? O9 Dy1 N1 C96 -145.1(3) . . . . ? O2 Dy1 N1 C96 166.0(3) . . . . ? O10 Dy1 N1 C96 -51.3(3) . . . . ? O1 Dy1 N1 C96 -119.9(3) . . . . ? O6 Dy1 N1 C96 46.6(4) . . . . ? N2 Dy1 N1 C96 2.8(3) . . . . ? O5 Dy1 N2 C91 106.9(3) . . . . ? O9 Dy1 N2 C91 -20.2(4) . . . . ? O2 Dy1 N2 C91 152.2(3) . . . . ? O10 Dy1 N2 C91 -53.2(3) . . . . ? O1 Dy1 N2 C91 -121.3(3) . . . . ? O6 Dy1 N2 C91 33.6(3) . . . . ? N1 Dy1 N2 C91 -178.5(3) . . . . ? O5 Dy1 N2 C95 -79.2(3) . . . . ? O9 Dy1 N2 C95 153.6(3) . . . . ? O2 Dy1 N2 C95 -33.9(4) . . . . ? O10 Dy1 N2 C95 120.7(3) . . . . ? O1 Dy1 N2 C95 52.6(3) . . . . ? O6 Dy1 N2 C95 -152.5(3) . . . . ? N1 Dy1 N2 C95 -4.6(3) . . . . ? Dy1 O10 C9 O11 165.7(2) . . . . ? Dy1 O10 C9 C8 -14.0(7) . . . . ? Si6 O11 C9 O10 18.5(6) . . . . ? Si6 O11 C9 C8 -161.7(3) . . . . ? Dy1 O5 C4 O8 -159.8(2) . . . . ? Dy1 O5 C4 C5 20.6(7) . . . . ? Si4 O8 C4 O5 -165.2(3) . . . . ? Si4 O8 C4 C5 14.4(6) . . . . ? Dy1 O1 C1 O4 176.9(2) . . . . ? Dy1 O1 C1 C2 -1.5(6) . . . . ? Si1 O4 C1 O1 -9.8(5) . . . . ? Si1 O4 C1 C2 168.7(3) . . . . ? C52 Si5 O12 C7 61.4(4) . . . . ? C53 Si5 O12 C7 179.2(3) . . . . ? C51 Si5 O12 C7 -62.8(4) . . . . ? C33 Si3 O7 C6 62.0(4) . . . . ? C32 Si3 O7 C6 -60.0(5) . . . . ? C31 Si3 O7 C6 -177.7(4) . . . . ? Dy1 O9 C7 O12 179.0(2) . . . . ? Dy1 O9 C7 C8 2.1(7) . . . . ? Si5 O12 C7 O9 5.8(5) . . . . ? Si5 O12 C7 C8 -176.9(3) . . . . ? O2 C3 C2 C1 1.3(7) . . . . ? O3 C3 C2 C1 177.1(4) . . . . ? O1 C1 C2 C3 5.8(7) . . . . ? O4 C1 C2 C3 -172.6(4) . . . . ? O10 C9 C8 C7 -1.4(7) . . . . ? O11 C9 C8 C7 178.8(4) . . . . ? O9 C7 C8 C9 7.6(7) . . . . ? O12 C7 C8 C9 -169.4(4) . . . . ? C91 N2 C95 C94 -0.4(6) . . . . ? Dy1 N2 C95 C94 -174.3(3) . . . . ? C91 N2 C95 C96 179.9(4) . . . . ? Dy1 N2 C95 C96 6.0(5) . . . . ? C93 C94 C95 N2 1.1(7) . . . . ? C93 C94 C95 C96 -179.3(4) . . . . ? C90 N1 C96 C97 -1.7(6) . . . . ? Dy1 N1 C96 C97 178.3(3) . . . . ? C90 N1 C96 C95 178.8(4) . . . . ? Dy1 N1 C96 C95 -1.2(5) . . . . ? C98 C97 C96 N1 1.1(7) . . . . ? C98 C97 C96 C95 -179.5(4) . . . . ? N2 C95 C96 N1 -3.0(6) . . . . ? C94 C95 C96 N1 177.3(4) . . . . ? N2 C95 C96 C97 177.5(4) . . . . ? C94 C95 C96 C97 -2.2(7) . . . . ? C95 N2 C91 C92 -1.6(6) . . . . ? Dy1 N2 C91 C92 172.6(3) . . . . ? C93 C92 C91 N2 2.9(7) . . . . ? Dy1 O6 C6 O7 166.2(3) . . . . ? Dy1 O6 C6 C5 -11.3(7) . . . . ? Si3 O7 C6 O6 4.2(7) . . . . ? Si3 O7 C6 C5 -178.0(3) . . . . ? C96 C97 C98 C99 -0.4(7) . . . . ? C97 C98 C99 C90 0.3(7) . . . . ? C91 C92 C93 C94 -2.1(7) . . . . ? C95 C94 C93 C92 0.2(7) . . . . ? C96 N1 C90 C99 1.7(6) . . . . ? Dy1 N1 C90 C99 -178.3(3) . . . . ? C98 C99 C90 N1 -1.0(7) . . . . ? O5 C4 C5 C6 -1.2(7) . . . . ? O8 C4 C5 C6 179.3(4) . . . . ? O6 C6 C5 C4 -3.1(8) . . . . ? O7 C6 C5 C4 179.4(4) . . . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 1.878 _refine_diff_density_min -0.651 _refine_diff_density_rms 0.095 #=================================END data_cvd190b _database_code_depnum_ccdc_archive 'CCDC 770265' #TrackingRef '- combined cif files.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H62 Dy N O12 Si6' _chemical_formula_weight 983.87 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' Si Si 0.0817 0.0704 '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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.8588(6) _cell_length_b 21.5855(7) _cell_length_c 22.2231(8) _cell_angle_alpha 90.00 _cell_angle_beta 109.218(3) _cell_angle_gamma 90.00 _cell_volume 9901.3(6) _cell_formula_units_Z 8 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 10000 _cell_measurement_theta_min 2.637 _cell_measurement_theta_max 27.500 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.320 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4056 _exptl_absorpt_coefficient_mu 1.703 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.460 _exptl_absorpt_correction_T_max 0.680 _exptl_absorpt_process_details abspack _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Sapphire2-CCD, Oxford Diffraction' _diffrn_measurement_method '1109 images at 1.0 deg. in \w and 15 sec.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 91209 _diffrn_reflns_av_R_equivalents 0.0388 _diffrn_reflns_av_sigmaI/netI 0.0217 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.71 _diffrn_reflns_theta_max 27.58 _reflns_number_total 11441 _reflns_number_gt 9220 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD 1.171.13, Oxford Diffraction' _computing_cell_refinement 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_data_reduction 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0245P)^2^+24.4031P] 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 11441 _refine_ls_number_parameters 469 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0454 _refine_ls_R_factor_gt 0.0280 _refine_ls_wR_factor_ref 0.0674 _refine_ls_wR_factor_gt 0.0597 _refine_ls_goodness_of_fit_ref 1.172 _refine_ls_restrained_S_all 1.172 _refine_ls_shift/su_max 0.005 _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 0.727683(6) 0.570212(5) 0.850067(5) 0.01558(4) Uani 1 1 d . . . Si1 Si 0.92984(3) 0.43517(4) 0.87816(3) 0.02099(15) Uani 1 1 d . . . Si3 Si 0.56785(4) 0.70050(4) 0.92574(4) 0.02622(17) Uani 1 1 d . . . Si2 Si 0.58090(4) 0.48265(4) 0.63917(4) 0.02845(18) Uani 1 1 d . . . Si5 Si 0.90206(4) 0.71181(4) 0.82280(4) 0.02849(17) Uani 1 1 d . . . Si6 Si 0.81817(4) 0.55074(4) 1.09616(4) 0.03018(19) Uani 1 1 d . . . Si7 Si 0.67071(4) 0.35655(4) 0.91472(4) 0.02952(18) Uani 1 1 d . . . O8 O 0.64652(10) 0.42230(9) 0.94094(9) 0.0253(4) Uani 1 1 d . . . O1 O 0.80630(9) 0.50182(8) 0.84472(8) 0.0210(4) Uani 1 1 d . . . O9 O 0.81231(9) 0.63622(9) 0.86151(8) 0.0218(4) Uani 1 1 d . . . O4 O 0.85609(9) 0.41763(8) 0.82563(9) 0.0220(4) Uani 1 1 d . . . O2 O 0.68697(8) 0.52471(8) 0.75229(8) 0.0200(4) Uani 1 1 d . . . O5 O 0.68198(9) 0.48445(8) 0.87921(8) 0.0214(4) Uani 1 1 d . . . O11 O 0.86365(9) 0.57158(10) 1.05113(9) 0.0286(4) Uani 1 1 d . . . O7 O 0.58491(10) 0.62555(9) 0.94488(9) 0.0267(4) Uani 1 1 d . . . O6 O 0.64676(9) 0.60958(8) 0.88330(8) 0.0208(4) Uani 1 1 d . . . O10 O 0.78331(9) 0.57142(9) 0.95761(8) 0.0215(4) Uani 1 1 d . . . N1 N 0.68737(11) 0.65993(10) 0.77188(11) 0.0231(5) Uani 1 1 d . . . O12 O 0.91464(9) 0.66952(10) 0.88946(9) 0.0276(4) Uani 1 1 d . . . O3 O 0.65330(9) 0.45033(9) 0.67892(9) 0.0258(4) Uani 1 1 d . . . C2 C 0.75218(12) 0.43582(12) 0.75758(12) 0.0192(5) Uani 1 1 d . . . H2A H 0.7544 0.3968 0.7387 0.023 Uiso 1 1 calc R . . C7 C 0.86796(13) 0.63921(12) 0.90384(13) 0.0215(5) Uani 1 1 d . . . C6 C 0.61958(12) 0.58683(13) 0.92113(12) 0.0201(5) Uani 1 1 d . . . C9 C 0.84103(13) 0.58543(13) 0.98864(12) 0.0217(5) Uani 1 1 d . . . C3 C 0.69732(12) 0.47278(12) 0.73149(11) 0.0181(5) Uani 1 1 d . . . C1 C 0.80391(12) 0.45457(12) 0.81060(12) 0.0187(5) Uani 1 1 d . . . C5 C 0.62139(13) 0.52610(13) 0.94088(13) 0.0222(5) Uani 1 1 d . . . H5A H 0.6010 0.5159 0.9713 0.027 Uiso 1 1 calc R . . C4 C 0.65161(13) 0.47909(12) 0.91845(12) 0.0207(5) Uani 1 1 d . . . C8 C 0.88524(13) 0.61519(13) 0.96541(12) 0.0228(6) Uani 1 1 d . . . H8A H 0.9289 0.6193 0.9926 0.027 Uiso 1 1 calc R . . C21 C 0.54092(15) 0.42021(16) 0.58321(15) 0.0381(8) Uani 1 1 d . . . H21A H 0.5652 0.4124 0.5539 0.057 Uiso 1 1 calc R . . H21B H 0.4966 0.4327 0.5588 0.057 Uiso 1 1 calc R . . H21C H 0.5398 0.3824 0.6072 0.057 Uiso 1 1 calc R . . C111 C 0.69863(16) 0.65892(14) 0.71633(14) 0.0310(7) Uani 1 1 d . . . H11A H 0.7131 0.6213 0.7033 0.037 Uiso 1 1 calc R . . C11 C 0.92694(15) 0.43362(16) 0.96053(14) 0.0347(7) Uani 1 1 d . . . H11B H 0.9114 0.3930 0.9690 0.052 Uiso 1 1 calc R . . H11C H 0.8974 0.4659 0.9654 0.052 Uiso 1 1 calc R . . H11D H 0.9704 0.4411 0.9908 0.052 Uiso 1 1 calc R . . C32 C 0.51527(18) 0.72105(15) 0.97334(16) 0.0382(8) Uani 1 1 d . . . H32A H 0.5404 0.7186 1.0188 0.057 Uiso 1 1 calc R . . H32B H 0.4788 0.6921 0.9635 0.057 Uiso 1 1 calc R . . H32C H 0.4989 0.7633 0.9628 0.057 Uiso 1 1 calc R . . C12 C 0.95869(15) 0.51043(14) 0.85792(16) 0.0327(7) Uani 1 1 d . . . H12A H 0.9594 0.5091 0.8141 0.049 Uiso 1 1 calc R . . H12B H 1.0025 0.5186 0.8872 0.049 Uiso 1 1 calc R . . H12C H 0.9295 0.5435 0.8618 0.049 Uiso 1 1 calc R . . C13 C 0.97864(14) 0.37108(14) 0.86283(14) 0.0297(6) Uani 1 1 d . . . H13A H 0.9788 0.3737 0.8189 0.044 Uiso 1 1 calc R . . H13B H 0.9598 0.3314 0.8692 0.044 Uiso 1 1 calc R . . H13C H 1.0231 0.3741 0.8923 0.044 Uiso 1 1 calc R . . C114 C 0.65716(16) 0.76664(15) 0.75143(17) 0.0364(7) Uani 1 1 d . . . H11E H 0.6427 0.8039 0.7652 0.044 Uiso 1 1 calc R . . C115 C 0.66658(14) 0.71343(14) 0.78857(15) 0.0296(6) Uani 1 1 d . . . H11F H 0.6578 0.7151 0.8277 0.036 Uiso 1 1 calc R . . C113 C 0.66910(16) 0.76450(15) 0.69461(16) 0.0380(8) Uani 1 1 d . . . H11G H 0.6628 0.8001 0.6682 0.046 Uiso 1 1 calc R . . C51 C 0.87867(18) 0.66096(17) 0.75128(16) 0.0430(8) Uani 1 1 d . . . H51A H 0.8357 0.6433 0.7449 0.065 Uiso 1 1 calc R . . H51B H 0.9104 0.6274 0.7575 0.065 Uiso 1 1 calc R . . H51C H 0.8776 0.6853 0.7138 0.065 Uiso 1 1 calc R . . C31 C 0.52226(18) 0.70450(17) 0.83897(16) 0.0429(8) Uani 1 1 d . . . H31A H 0.5511 0.6935 0.8149 0.064 Uiso 1 1 calc R . . H31B H 0.5059 0.7467 0.8278 0.064 Uiso 1 1 calc R . . H31C H 0.4858 0.6755 0.8285 0.064 Uiso 1 1 calc R . . C71 C 0.75889(18) 0.35639(17) 0.9291(2) 0.0489(9) Uani 1 1 d . . . H71A H 0.7694 0.3878 0.9023 0.073 Uiso 1 1 calc R . . H71B H 0.7721 0.3155 0.9187 0.073 Uiso 1 1 calc R . . H71C H 0.7819 0.3657 0.9741 0.073 Uiso 1 1 calc R . . C61 C 0.87896(16) 0.5528(2) 1.17712(14) 0.0482(10) Uani 1 1 d . . . H61A H 0.9127 0.5219 1.1802 0.072 Uiso 1 1 calc R . . H61B H 0.8578 0.5435 1.2087 0.072 Uiso 1 1 calc R . . H61C H 0.8986 0.5941 1.1854 0.072 Uiso 1 1 calc R . . C62 C 0.75252(16) 0.60792(18) 1.08644(15) 0.0396(8) Uani 1 1 d . . . H62A H 0.7216 0.6052 1.0431 0.059 Uiso 1 1 calc R . . H62B H 0.7710 0.6497 1.0939 0.059 Uiso 1 1 calc R . . H62C H 0.7302 0.5991 1.1172 0.059 Uiso 1 1 calc R . . C53 C 0.84206(17) 0.77308(15) 0.81986(17) 0.0386(8) Uani 1 1 d . . . H53A H 0.8572 0.7981 0.8588 0.058 Uiso 1 1 calc R . . H53B H 0.8004 0.7540 0.8166 0.058 Uiso 1 1 calc R . . H53C H 0.8367 0.7996 0.7827 0.058 Uiso 1 1 calc R . . C52 C 0.98319(17) 0.74542(19) 0.83535(18) 0.0466(9) Uani 1 1 d . . . H52A H 0.9952 0.7722 0.8731 0.070 Uiso 1 1 calc R . . H52B H 0.9823 0.7699 0.7979 0.070 Uiso 1 1 calc R . . H52C H 1.0150 0.7120 0.8417 0.070 Uiso 1 1 calc R . . C112 C 0.69027(18) 0.71002(16) 0.67674(15) 0.0409(8) Uani 1 1 d . . . H11H H 0.6991 0.7073 0.6377 0.049 Uiso 1 1 calc R . . C73 C 0.64961(19) 0.29681(16) 0.96557(18) 0.0452(9) Uani 1 1 d . . . H73A H 0.6754 0.3038 1.0103 0.068 Uiso 1 1 calc R . . H73B H 0.6589 0.2555 0.9525 0.068 Uiso 1 1 calc R . . H73C H 0.6035 0.2999 0.9605 0.068 Uiso 1 1 calc R . . C72 C 0.6240(2) 0.34680(17) 0.82920(17) 0.0521(10) Uani 1 1 d . . . H72A H 0.6366 0.3790 0.8045 0.078 Uiso 1 1 calc R . . H72B H 0.5776 0.3503 0.8229 0.078 Uiso 1 1 calc R . . H72C H 0.6330 0.3059 0.8149 0.078 Uiso 1 1 calc R . . C33 C 0.64343(19) 0.74635(17) 0.95147(19) 0.0478(9) Uani 1 1 d . . . H33A H 0.6644 0.7418 0.9976 0.072 Uiso 1 1 calc R . . H33B H 0.6333 0.7901 0.9412 0.072 Uiso 1 1 calc R . . H33C H 0.6727 0.7315 0.9293 0.072 Uiso 1 1 calc R . . C22 C 0.53677(18) 0.4989(3) 0.69531(18) 0.0696(15) Uani 1 1 d . . . H22A H 0.5588 0.5321 0.7245 0.104 Uiso 1 1 calc R . . H22B H 0.5356 0.4614 0.7198 0.104 Uiso 1 1 calc R . . H22D H 0.4924 0.5118 0.6715 0.104 Uiso 1 1 calc R . . C23 C 0.5910(2) 0.55294(17) 0.59680(18) 0.0554(11) Uani 1 1 d . . . H23A H 0.6123 0.5851 0.6278 0.083 Uiso 1 1 calc R . . H23D H 0.5484 0.5678 0.5699 0.083 Uiso 1 1 calc R . . H23B H 0.6176 0.5435 0.5701 0.083 Uiso 1 1 calc R . . C63 C 0.7870(2) 0.47131(19) 1.0764(2) 0.0582(11) Uani 1 1 d . . . H63D H 0.7549 0.4707 1.0335 0.087 Uiso 1 1 calc R . . H63A H 0.7666 0.4575 1.1073 0.087 Uiso 1 1 calc R . . H63B H 0.8228 0.4435 1.0779 0.087 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.01643(6) 0.01533(6) 0.01481(6) -0.00025(5) 0.00491(4) 0.00084(5) Si1 0.0158(3) 0.0230(4) 0.0210(3) -0.0036(3) 0.0018(3) 0.0032(3) Si3 0.0339(4) 0.0220(4) 0.0274(4) 0.0009(3) 0.0163(3) 0.0072(3) Si2 0.0209(4) 0.0403(5) 0.0190(4) -0.0059(3) -0.0004(3) 0.0092(3) Si5 0.0278(4) 0.0302(4) 0.0301(4) 0.0021(3) 0.0131(3) -0.0051(3) Si6 0.0230(4) 0.0486(5) 0.0180(4) 0.0041(3) 0.0055(3) -0.0018(4) Si7 0.0414(5) 0.0173(4) 0.0354(4) 0.0013(3) 0.0202(4) -0.0009(3) O8 0.0305(11) 0.0190(10) 0.0309(10) 0.0022(8) 0.0160(8) -0.0006(8) O1 0.0177(9) 0.0212(10) 0.0214(9) -0.0029(7) 0.0029(7) 0.0032(7) O9 0.0209(9) 0.0224(10) 0.0208(9) 0.0016(7) 0.0050(7) -0.0028(7) O4 0.0155(9) 0.0228(10) 0.0240(9) -0.0026(7) 0.0014(7) 0.0048(7) O2 0.0187(9) 0.0206(9) 0.0175(9) -0.0010(7) 0.0015(7) 0.0051(7) O5 0.0252(10) 0.0176(9) 0.0234(9) -0.0014(7) 0.0109(8) -0.0005(7) O11 0.0214(10) 0.0483(13) 0.0148(9) 0.0019(9) 0.0045(7) -0.0001(9) O7 0.0328(11) 0.0229(10) 0.0303(10) 0.0016(8) 0.0184(9) 0.0069(8) O6 0.0230(10) 0.0170(9) 0.0233(9) 0.0017(7) 0.0090(8) 0.0026(7) O10 0.0197(9) 0.0274(10) 0.0173(8) -0.0014(8) 0.0060(7) -0.0037(8) N1 0.0227(12) 0.0195(12) 0.0250(11) 0.0022(9) 0.0051(9) 0.0005(9) O12 0.0223(10) 0.0327(11) 0.0289(10) 0.0018(8) 0.0098(8) -0.0057(8) O3 0.0197(10) 0.0298(10) 0.0217(9) -0.0079(8) -0.0015(8) 0.0041(8) C2 0.0173(12) 0.0191(13) 0.0195(12) -0.0032(10) 0.0039(10) 0.0029(10) C7 0.0200(13) 0.0168(13) 0.0266(13) -0.0050(10) 0.0063(11) -0.0012(10) C6 0.0136(12) 0.0305(15) 0.0155(12) -0.0019(10) 0.0037(9) 0.0038(10) C9 0.0227(13) 0.0267(14) 0.0159(12) -0.0040(10) 0.0066(10) 0.0030(11) C3 0.0174(12) 0.0211(13) 0.0152(11) -0.0003(9) 0.0045(9) -0.0014(10) C1 0.0172(12) 0.0198(13) 0.0207(12) 0.0021(10) 0.0084(10) 0.0028(10) C5 0.0217(13) 0.0247(14) 0.0223(13) 0.0012(10) 0.0101(11) 0.0009(11) C4 0.0189(13) 0.0200(13) 0.0210(12) 0.0000(10) 0.0034(10) -0.0002(10) C8 0.0185(13) 0.0280(15) 0.0211(13) -0.0041(11) 0.0055(10) -0.0003(11) C21 0.0270(16) 0.048(2) 0.0309(16) -0.0058(14) -0.0021(13) -0.0021(14) C111 0.0421(18) 0.0237(15) 0.0270(15) 0.0052(12) 0.0111(13) 0.0014(13) C11 0.0288(15) 0.049(2) 0.0235(14) -0.0013(14) 0.0040(12) 0.0070(14) C32 0.053(2) 0.0290(17) 0.0427(18) 0.0027(14) 0.0299(16) 0.0145(15) C12 0.0294(16) 0.0268(16) 0.0436(18) -0.0057(13) 0.0144(14) -0.0030(12) C13 0.0202(14) 0.0312(16) 0.0327(15) -0.0049(12) 0.0022(12) 0.0065(12) C114 0.0343(18) 0.0230(15) 0.052(2) 0.0059(14) 0.0136(15) 0.0064(13) C115 0.0307(16) 0.0250(15) 0.0339(16) 0.0039(12) 0.0116(13) 0.0041(12) C113 0.0395(18) 0.0281(17) 0.0414(18) 0.0158(14) 0.0067(15) 0.0003(14) C51 0.051(2) 0.048(2) 0.0327(17) -0.0045(15) 0.0178(16) -0.0053(17) C31 0.046(2) 0.047(2) 0.0358(18) 0.0063(15) 0.0146(15) 0.0242(17) C71 0.053(2) 0.0359(19) 0.070(3) 0.0150(18) 0.036(2) 0.0164(17) C61 0.0298(17) 0.096(3) 0.0187(15) 0.0046(16) 0.0075(13) 0.0071(18) C62 0.0297(17) 0.063(2) 0.0279(16) 0.0002(15) 0.0120(13) 0.0023(16) C53 0.0397(19) 0.0310(17) 0.0473(19) 0.0088(14) 0.0175(15) -0.0016(14) C52 0.0366(19) 0.057(2) 0.052(2) 0.0049(18) 0.0235(17) -0.0138(17) C112 0.061(2) 0.0346(18) 0.0289(16) 0.0095(14) 0.0171(15) -0.0006(16) C73 0.061(2) 0.0268(17) 0.052(2) 0.0081(15) 0.0235(18) 0.0008(16) C72 0.081(3) 0.038(2) 0.041(2) -0.0116(16) 0.0248(19) -0.026(2) C33 0.058(2) 0.038(2) 0.056(2) -0.0180(17) 0.0299(19) -0.0119(17) C22 0.0278(19) 0.141(5) 0.037(2) -0.023(2) 0.0063(16) 0.021(2) C23 0.070(3) 0.039(2) 0.0366(19) -0.0011(15) -0.0111(18) 0.0048(18) C63 0.054(2) 0.052(2) 0.057(2) 0.0141(19) 0.004(2) -0.008(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O2 2.2814(17) . ? Dy1 O9 2.2819(18) . ? Dy1 O6 2.2926(18) . ? Dy1 O5 2.2958(18) . ? Dy1 O10 2.2974(17) . ? Dy1 O1 2.2981(18) . ? Dy1 N1 2.557(2) . ? Si1 O4 1.6929(19) . ? Si1 C13 1.846(3) . ? Si1 C12 1.851(3) . ? Si1 C11 1.853(3) . ? Si3 O7 1.683(2) . ? Si3 C33 1.848(4) . ? Si3 C32 1.854(3) . ? Si3 C31 1.858(3) . ? Si2 O3 1.689(2) . ? Si2 C23 1.837(4) . ? Si2 C22 1.844(4) . ? Si2 C21 1.847(3) . ? Si5 O12 1.684(2) . ? Si5 C53 1.849(3) . ? Si5 C52 1.850(3) . ? Si5 C51 1.859(3) . ? Si6 O11 1.687(2) . ? Si6 C63 1.844(4) . ? Si6 C62 1.851(4) . ? Si6 C61 1.852(3) . ? Si7 O8 1.684(2) . ? Si7 C71 1.847(4) . ? Si7 C72 1.850(4) . ? Si7 C73 1.870(3) . ? O8 C4 1.342(3) . ? O1 C1 1.262(3) . ? O9 C7 1.271(3) . ? O4 C1 1.341(3) . ? O2 C3 1.261(3) . ? O5 C4 1.263(3) . ? O11 C9 1.345(3) . ? O7 C6 1.347(3) . ? O6 C6 1.277(3) . ? O10 C9 1.259(3) . ? N1 C111 1.336(4) . ? N1 C115 1.337(4) . ? O12 C7 1.336(3) . ? O3 C3 1.336(3) . ? C2 C3 1.397(4) . ? C2 C1 1.398(4) . ? C2 H2A 0.9500 . ? C7 C8 1.394(4) . ? C6 C5 1.379(4) . ? C9 C8 1.393(4) . ? C5 C4 1.390(4) . ? C5 H5A 0.9500 . ? C8 H8A 0.9500 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C111 C112 1.385(4) . ? C111 H11A 0.9500 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C11 H11D 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C114 C113 1.372(5) . ? C114 C115 1.390(4) . ? C114 H11E 0.9500 . ? C115 H11F 0.9500 . ? C113 C112 1.370(5) . ? C113 H11G 0.9500 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C112 H11H 0.9500 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22D 0.9800 . ? C23 H23A 0.9800 . ? C23 H23D 0.9800 . ? C23 H23B 0.9800 . ? C63 H63D 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Dy1 O9 115.01(7) . . ? O2 Dy1 O6 111.47(6) . . ? O9 Dy1 O6 114.57(7) . . ? O2 Dy1 O5 81.49(6) . . ? O9 Dy1 O5 152.15(7) . . ? O6 Dy1 O5 75.79(6) . . ? O2 Dy1 O10 154.51(6) . . ? O9 Dy1 O10 75.22(6) . . ? O6 Dy1 O10 82.01(6) . . ? O5 Dy1 O10 81.15(6) . . ? O2 Dy1 O1 74.81(6) . . ? O9 Dy1 O1 79.30(7) . . ? O6 Dy1 O1 157.54(7) . . ? O5 Dy1 O1 84.19(7) . . ? O10 Dy1 O1 84.97(6) . . ? O2 Dy1 N1 74.92(7) . . ? O9 Dy1 N1 71.83(7) . . ? O6 Dy1 N1 78.95(7) . . ? O5 Dy1 N1 135.87(7) . . ? O10 Dy1 N1 130.11(7) . . ? O1 Dy1 N1 123.21(7) . . ? O4 Si1 C13 100.49(11) . . ? O4 Si1 C12 110.61(13) . . ? C13 Si1 C12 110.43(15) . . ? O4 Si1 C11 110.05(13) . . ? C13 Si1 C11 112.24(15) . . ? C12 Si1 C11 112.41(15) . . ? O7 Si3 C33 109.61(16) . . ? O7 Si3 C32 102.31(13) . . ? C33 Si3 C32 110.75(17) . . ? O7 Si3 C31 107.78(14) . . ? C33 Si3 C31 114.56(18) . . ? C32 Si3 C31 111.06(16) . . ? O3 Si2 C23 111.07(16) . . ? O3 Si2 C22 109.48(15) . . ? C23 Si2 C22 111.6(2) . . ? O3 Si2 C21 101.83(13) . . ? C23 Si2 C21 111.57(16) . . ? C22 Si2 C21 110.9(2) . . ? O12 Si5 C53 109.11(13) . . ? O12 Si5 C52 102.07(14) . . ? C53 Si5 C52 111.01(17) . . ? O12 Si5 C51 110.56(14) . . ? C53 Si5 C51 113.57(17) . . ? C52 Si5 C51 109.92(17) . . ? O11 Si6 C63 110.53(17) . . ? O11 Si6 C62 109.78(14) . . ? C63 Si6 C62 112.36(19) . . ? O11 Si6 C61 101.26(13) . . ? C63 Si6 C61 110.16(19) . . ? C62 Si6 C61 112.21(17) . . ? O8 Si7 C71 111.72(15) . . ? O8 Si7 C72 108.74(16) . . ? C71 Si7 C72 111.7(2) . . ? O8 Si7 C73 101.78(14) . . ? C71 Si7 C73 110.17(17) . . ? C72 Si7 C73 112.32(17) . . ? C4 O8 Si7 124.54(17) . . ? C1 O1 Dy1 131.81(16) . . ? C7 O9 Dy1 131.11(17) . . ? C1 O4 Si1 125.28(17) . . ? C3 O2 Dy1 132.15(16) . . ? C4 O5 Dy1 130.16(17) . . ? C9 O11 Si6 125.68(18) . . ? C6 O7 Si3 127.15(18) . . ? C6 O6 Dy1 130.19(16) . . ? C9 O10 Dy1 131.62(16) . . ? C111 N1 C115 116.9(2) . . ? C111 N1 Dy1 119.23(19) . . ? C115 N1 Dy1 122.56(19) . . ? C7 O12 Si5 124.02(18) . . ? C3 O3 Si2 126.06(17) . . ? C3 C2 C1 122.0(2) . . ? C3 C2 H2A 119.0 . . ? C1 C2 H2A 119.0 . . ? O9 C7 O12 117.9(2) . . ? O9 C7 C8 126.3(3) . . ? O12 C7 C8 115.8(2) . . ? O6 C6 O7 117.6(2) . . ? O6 C6 C5 127.2(2) . . ? O7 C6 C5 115.2(2) . . ? O10 C9 O11 118.3(2) . . ? O10 C9 C8 126.9(2) . . ? O11 C9 C8 114.9(2) . . ? O2 C3 O3 118.6(2) . . ? O2 C3 C2 126.0(2) . . ? O3 C3 C2 115.4(2) . . ? O1 C1 O4 117.9(2) . . ? O1 C1 C2 127.1(2) . . ? O4 C1 C2 115.1(2) . . ? C6 C5 C4 123.2(2) . . ? C6 C5 H5A 118.4 . . ? C4 C5 H5A 118.4 . . ? O5 C4 O8 117.9(2) . . ? O5 C4 C5 126.9(2) . . ? O8 C4 C5 115.2(2) . . ? C9 C8 C7 122.6(2) . . ? C9 C8 H8A 118.7 . . ? C7 C8 H8A 118.7 . . ? Si2 C21 H21A 109.5 . . ? Si2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N1 C111 C112 123.2(3) . . ? N1 C111 H11A 118.4 . . ? C112 C111 H11A 118.4 . . ? Si1 C11 H11B 109.5 . . ? Si1 C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si1 C11 H11D 109.5 . . ? H11B C11 H11D 109.5 . . ? H11C C11 H11D 109.5 . . ? Si3 C32 H32A 109.5 . . ? Si3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Si1 C12 H12A 109.5 . . ? Si1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si1 C13 H13A 109.5 . . ? Si1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C113 C114 C115 118.9(3) . . ? C113 C114 H11E 120.6 . . ? C115 C114 H11E 120.6 . . ? N1 C115 C114 123.1(3) . . ? N1 C115 H11F 118.4 . . ? C114 C115 H11F 118.4 . . ? C112 C113 C114 118.7(3) . . ? C112 C113 H11G 120.6 . . ? C114 C113 H11G 120.6 . . ? Si5 C51 H51A 109.5 . . ? Si5 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? Si5 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? Si3 C31 H31A 109.5 . . ? Si3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si7 C71 H71A 109.5 . . ? Si7 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? Si7 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? Si6 C61 H61A 109.5 . . ? Si6 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? Si6 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? Si6 C62 H62A 109.5 . . ? Si6 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? Si6 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? Si5 C53 H53A 109.5 . . ? Si5 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? Si5 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? Si5 C52 H52A 109.5 . . ? Si5 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? Si5 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C113 C112 C111 119.1(3) . . ? C113 C112 H11H 120.5 . . ? C111 C112 H11H 120.5 . . ? Si7 C73 H73A 109.5 . . ? Si7 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? Si7 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? Si7 C72 H72A 109.5 . . ? Si7 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? Si7 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? Si3 C33 H33A 109.5 . . ? Si3 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Si3 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Si2 C22 H22A 109.5 . . ? Si2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si2 C22 H22D 109.5 . . ? H22A C22 H22D 109.5 . . ? H22B C22 H22D 109.5 . . ? Si2 C23 H23A 109.5 . . ? Si2 C23 H23D 109.5 . . ? H23A C23 H23D 109.5 . . ? Si2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? H23D C23 H23B 109.5 . . ? Si6 C63 H63D 109.5 . . ? Si6 C63 H63A 109.5 . . ? H63D C63 H63A 109.5 . . ? Si6 C63 H63B 109.5 . . ? H63D C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? 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 C71 Si7 O8 C4 62.5(3) . . . . ? C72 Si7 O8 C4 -61.2(3) . . . . ? C73 Si7 O8 C4 -179.9(2) . . . . ? O2 Dy1 O1 C1 -21.0(2) . . . . ? O9 Dy1 O1 C1 -140.8(2) . . . . ? O6 Dy1 O1 C1 88.7(3) . . . . ? O5 Dy1 O1 C1 61.8(2) . . . . ? O10 Dy1 O1 C1 143.4(2) . . . . ? N1 Dy1 O1 C1 -81.0(2) . . . . ? O2 Dy1 O9 C7 -128.7(2) . . . . ? O6 Dy1 O9 C7 100.2(2) . . . . ? O5 Dy1 O9 C7 -6.5(3) . . . . ? O10 Dy1 O9 C7 26.4(2) . . . . ? O1 Dy1 O9 C7 -61.2(2) . . . . ? N1 Dy1 O9 C7 168.4(2) . . . . ? C13 Si1 O4 C1 -170.1(2) . . . . ? C12 Si1 O4 C1 -53.4(2) . . . . ? C11 Si1 O4 C1 71.4(2) . . . . ? O9 Dy1 O2 C3 96.5(2) . . . . ? O6 Dy1 O2 C3 -131.0(2) . . . . ? O5 Dy1 O2 C3 -60.0(2) . . . . ? O10 Dy1 O2 C3 -12.5(3) . . . . ? O1 Dy1 O2 C3 26.3(2) . . . . ? N1 Dy1 O2 C3 157.6(2) . . . . ? O2 Dy1 O5 C4 -140.7(2) . . . . ? O9 Dy1 O5 C4 90.2(3) . . . . ? O6 Dy1 O5 C4 -25.9(2) . . . . ? O10 Dy1 O5 C4 58.1(2) . . . . ? O1 Dy1 O5 C4 143.9(2) . . . . ? N1 Dy1 O5 C4 -82.8(2) . . . . ? C63 Si6 O11 C9 72.8(3) . . . . ? C62 Si6 O11 C9 -51.7(3) . . . . ? C61 Si6 O11 C9 -170.5(3) . . . . ? C33 Si3 O7 C6 -65.6(3) . . . . ? C32 Si3 O7 C6 176.8(2) . . . . ? C31 Si3 O7 C6 59.7(3) . . . . ? O2 Dy1 O6 C6 98.5(2) . . . . ? O9 Dy1 O6 C6 -128.7(2) . . . . ? O5 Dy1 O6 C6 23.8(2) . . . . ? O10 Dy1 O6 C6 -59.0(2) . . . . ? O1 Dy1 O6 C6 -3.9(3) . . . . ? N1 Dy1 O6 C6 167.3(2) . . . . ? O2 Dy1 O10 C9 95.7(3) . . . . ? O9 Dy1 O10 C9 -21.9(2) . . . . ? O6 Dy1 O10 C9 -140.0(2) . . . . ? O5 Dy1 O10 C9 143.2(2) . . . . ? O1 Dy1 O10 C9 58.4(2) . . . . ? N1 Dy1 O10 C9 -71.8(2) . . . . ? O2 Dy1 N1 C111 -41.9(2) . . . . ? O9 Dy1 N1 C111 81.4(2) . . . . ? O6 Dy1 N1 C111 -157.9(2) . . . . ? O5 Dy1 N1 C111 -102.0(2) . . . . ? O10 Dy1 N1 C111 132.6(2) . . . . ? O1 Dy1 N1 C111 18.1(2) . . . . ? O2 Dy1 N1 C115 151.4(2) . . . . ? O9 Dy1 N1 C115 -85.3(2) . . . . ? O6 Dy1 N1 C115 35.3(2) . . . . ? O5 Dy1 N1 C115 91.2(2) . . . . ? O10 Dy1 N1 C115 -34.2(2) . . . . ? O1 Dy1 N1 C115 -148.7(2) . . . . ? C53 Si5 O12 C7 58.2(2) . . . . ? C52 Si5 O12 C7 175.7(2) . . . . ? C51 Si5 O12 C7 -67.4(3) . . . . ? C23 Si2 O3 C3 71.7(3) . . . . ? C22 Si2 O3 C3 -51.9(3) . . . . ? C21 Si2 O3 C3 -169.4(2) . . . . ? Dy1 O9 C7 O12 160.09(17) . . . . ? Dy1 O9 C7 C8 -21.8(4) . . . . ? Si5 O12 C7 O9 8.4(3) . . . . ? Si5 O12 C7 C8 -169.88(19) . . . . ? Dy1 O6 C6 O7 163.88(16) . . . . ? Dy1 O6 C6 C5 -16.3(4) . . . . ? Si3 O7 C6 O6 5.4(3) . . . . ? Si3 O7 C6 C5 -174.45(19) . . . . ? Dy1 O10 C9 O11 -168.65(17) . . . . ? Dy1 O10 C9 C8 12.3(4) . . . . ? Si6 O11 C9 O10 -13.7(4) . . . . ? Si6 O11 C9 C8 165.4(2) . . . . ? Dy1 O2 C3 O3 159.70(17) . . . . ? Dy1 O2 C3 C2 -21.8(4) . . . . ? Si2 O3 C3 O2 -4.7(4) . . . . ? Si2 O3 C3 C2 176.70(19) . . . . ? C1 C2 C3 O2 -1.9(4) . . . . ? C1 C2 C3 O3 176.7(2) . . . . ? Dy1 O1 C1 O4 -169.02(16) . . . . ? Dy1 O1 C1 C2 11.2(4) . . . . ? Si1 O4 C1 O1 -11.5(3) . . . . ? Si1 O4 C1 C2 168.23(18) . . . . ? C3 C2 C1 O1 7.1(4) . . . . ? C3 C2 C1 O4 -172.6(2) . . . . ? O6 C6 C5 C4 -3.7(4) . . . . ? O7 C6 C5 C4 176.2(2) . . . . ? Dy1 O5 C4 O8 -160.57(17) . . . . ? Dy1 O5 C4 C5 20.4(4) . . . . ? Si7 O8 C4 O5 -6.9(3) . . . . ? Si7 O8 C4 C5 172.21(19) . . . . ? C6 C5 C4 O5 1.5(4) . . . . ? C6 C5 C4 O8 -177.5(2) . . . . ? O10 C9 C8 C7 6.6(4) . . . . ? O11 C9 C8 C7 -172.5(2) . . . . ? O9 C7 C8 C9 -1.7(4) . . . . ? O12 C7 C8 C9 176.4(2) . . . . ? C115 N1 C111 C112 0.5(5) . . . . ? Dy1 N1 C111 C112 -167.0(3) . . . . ? C111 N1 C115 C114 -0.6(4) . . . . ? Dy1 N1 C115 C114 166.4(2) . . . . ? C113 C114 C115 N1 0.6(5) . . . . ? C115 C114 C113 C112 -0.4(5) . . . . ? C114 C113 C112 C111 0.3(5) . . . . ? N1 C111 C112 C113 -0.4(5) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.943 _refine_diff_density_min -0.764 _refine_diff_density_rms 0.093 #=================================END