# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email tang@ciac.jl.cn _publ_contact_author_name 'Jinkui Tang' _publ_author_name 'Jinkui Tang' data_complex1Dy2 #TrackingRef 'web_deposit_cif_file_0_JinkuiTang_1323166039.Dy2.cif' _database_code_depnum_ccdc_archive 'CCDC 845737' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common complex1Dy2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C73 H60 Dy2 N8 O15' _chemical_formula_weight 1614.29 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 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 30.1750(18) _cell_length_b 14.9170(9) _cell_length_c 20.013(2) _cell_angle_alpha 90.00 _cell_angle_beta 125.9080(10) _cell_angle_gamma 90.00 _cell_volume 7296.1(10) _cell_formula_units_Z 4 _cell_measurement_temperature 185(2) _cell_measurement_reflns_used 8441 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 25.84 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.470 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3224 _exptl_absorpt_coefficient_mu 2.101 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6217 _exptl_absorpt_correction_T_max 0.7435 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 185(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19591 _diffrn_reflns_av_R_equivalents 0.0287 _diffrn_reflns_av_sigmaI/netI 0.0362 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 26.03 _reflns_number_total 7140 _reflns_number_gt 4963 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. 'comamands "isor 0.005 o8 o6 o7 o5 o9" have been used to restrain the anisotropic displacement parameters of the corresponding atoms' 'command "dfix o6 c37 1.3" has been used to refine the distance to be in the reasonable distance.' ; _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^)+(0.1252P)^2^+54.5106P] 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 7140 _refine_ls_number_parameters 439 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.1011 _refine_ls_R_factor_gt 0.0716 _refine_ls_wR_factor_ref 0.2323 _refine_ls_wR_factor_gt 0.2031 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.000 _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 0.01473(2) 0.30263(3) 0.17207(3) 0.0728(2) Uani 1 1 d . . . N1 N 0.0339(5) 0.3435(7) 0.0697(5) 0.095(3) Uani 1 1 d . . . N2 N -0.0115(5) 0.3812(7) -0.0034(6) 0.104(4) Uani 1 1 d . . . H2A H -0.0113 0.3906 -0.0466 0.125 Uiso 1 1 calc R . . N3 N 0.0305(3) 0.1375(5) 0.1965(5) 0.0635(18) Uani 1 1 d . . . N4 N -0.0062(3) 0.0836(5) 0.1296(5) 0.072(2) Uani 1 1 d . . . H4A H -0.0071 0.0250 0.1341 0.086 Uiso 1 1 calc R . . O1 O 0.1021(4) 0.2937(7) 0.2271(5) 0.120(4) Uani 1 1 d . . . O2 O -0.0520(4) 0.3930(5) 0.0590(5) 0.108(3) Uani 1 1 d . . . O3 O 0.0539(3) 0.2679(5) 0.3113(4) 0.0708(16) Uani 1 1 d . . . O4 O -0.0394(3) 0.2103(4) 0.0548(4) 0.0689(17) Uani 1 1 d . . . O5 O 0.0465(6) 0.4406(9) 0.2343(9) 0.072(3) Uani 0.50 1 d PU . . O6 O 0.0719(18) 0.542(3) 0.331(3) 0.30(2) Uani 0.50 1 d PDU . . O7 O 0.0001(8) 0.4435(12) 0.2879(11) 0.099(5) Uani 0.50 1 d PU . . O8 O 0.9909(7) 0.6038(11) 0.1195(11) 0.200(6) Uani 1 1 d U . . O9 O 0.9861(5) 0.9115(7) 0.1720(7) 0.142(4) Uani 1 1 d U . . C1 C 0.1382(6) 0.2787(10) 0.2142(7) 0.110(5) Uani 1 1 d . . . C2 C 0.1908(6) 0.2455(12) 0.2795(8) 0.121(6) Uani 1 1 d . . . H2 H 0.1978 0.2336 0.3316 0.145 Uiso 1 1 calc R . . C3 C 0.2289(8) 0.2313(12) 0.2702(9) 0.127(6) Uani 1 1 d . . . H3 H 0.2634 0.2113 0.3167 0.153 Uiso 1 1 calc R . . C4 C 0.2225(8) 0.2437(11) 0.1942(10) 0.119(5) Uani 1 1 d . . . C5 C 0.2608(10) 0.2251(13) 0.1829(14) 0.150(7) Uani 1 1 d . . . H5 H 0.2955 0.2041 0.2282 0.179 Uiso 1 1 calc R . . C6 C 0.2519(13) 0.235(2) 0.1112(19) 0.182(9) Uani 1 1 d . . . H6 H 0.2805 0.2234 0.1056 0.219 Uiso 1 1 calc R . . C7 C 0.2020(14) 0.262(2) 0.0441(16) 0.180(10) Uani 1 1 d . . . H7 H 0.1956 0.2655 -0.0083 0.216 Uiso 1 1 calc R . . C8 C 0.1621(9) 0.2837(13) 0.0510(12) 0.139(6) Uani 1 1 d . . . H8 H 0.1281 0.3055 0.0048 0.167 Uiso 1 1 calc . . . C9 C 0.1712(8) 0.2738(10) 0.1267(10) 0.109(5) Uani 1 1 d . . . C10 C 0.1276(7) 0.2948(8) 0.1365(8) 0.107(5) Uani 1 1 d . . . C11 C 0.0772(7) 0.3317(9) 0.0709(7) 0.107(5) Uani 1 1 d . . . H11 H 0.0746 0.3497 0.0232 0.129 Uiso 1 1 calc R . . C12 C -0.0534(7) 0.4014(7) -0.0041(8) 0.105(5) Uani 1 1 d . . . C13 C -0.1022(5) 0.4382(6) -0.0822(6) 0.121(6) Uani 1 1 d G . . C14 C -0.1031(6) 0.4553(6) -0.1509(7) 0.144(7) Uani 1 1 d G . . H14 H -0.0714 0.4448 -0.1491 0.173 Uiso 1 1 calc R . . C15 C -0.1503(6) 0.4876(7) -0.2222(6) 0.176(10) Uani 1 1 d G . . H15 H -0.1509 0.4993 -0.2694 0.211 Uiso 1 1 calc R . . C16 C -0.1964(6) 0.5028(7) -0.2247(7) 0.160(8) Uani 1 1 d G . . H16 H -0.2288 0.5251 -0.2737 0.191 Uiso 1 1 calc R . . C17 C -0.1954(5) 0.4857(7) -0.1560(8) 0.153(7) Uani 1 1 d G . . H17 H -0.2271 0.4962 -0.1577 0.183 Uiso 1 1 calc R . . C18 C -0.1483(6) 0.4534(7) -0.0847(7) 0.147(7) Uani 1 1 d G . . H18 H -0.1476 0.4417 -0.0375 0.176 Uiso 1 1 calc R . . C19 C 0.0997(4) 0.2208(8) 0.3611(6) 0.072(3) Uani 1 1 d . . . C20 C 0.1406(5) 0.2583(10) 0.4376(7) 0.095(3) Uani 1 1 d . . . H20 H 0.1353 0.3161 0.4519 0.114 Uiso 1 1 calc R . . C21 C 0.1876(6) 0.2130(12) 0.4914(8) 0.117(5) Uani 1 1 d . . . H21 H 0.2142 0.2396 0.5433 0.140 Uiso 1 1 calc R . . C22 C 0.1985(5) 0.1299(13) 0.4741(8) 0.114(4) Uani 1 1 d . . . C23 C 0.2474(7) 0.0868(18) 0.5305(11) 0.172(9) Uani 1 1 d . . . H23 H 0.2733 0.1135 0.5827 0.206 Uiso 1 1 calc R . . C24 C 0.2587(8) 0.006(2) 0.5112(15) 0.205(11) Uani 1 1 d . . . H24 H 0.2930 -0.0223 0.5499 0.246 Uiso 1 1 calc R . . C25 C 0.2194(7) -0.0388(15) 0.4331(13) 0.180(9) Uani 1 1 d . . . H25 H 0.2267 -0.0967 0.4218 0.216 Uiso 1 1 calc R . . C26 C 0.1705(6) 0.0057(11) 0.3749(11) 0.148(7) Uani 1 1 d . . . H26 H 0.1458 -0.0194 0.3215 0.177 Uiso 1 1 calc R . . C27 C 0.1578(5) 0.0891(10) 0.3955(7) 0.100(4) Uani 1 1 d . . . C28 C 0.1081(4) 0.1375(7) 0.3399(6) 0.076(3) Uani 1 1 d . . . C29 C 0.0662(4) 0.0952(7) 0.2617(6) 0.075(3) Uani 1 1 d . . . H29 H 0.0657 0.0316 0.2593 0.091 Uiso 1 1 calc R . . C30 C -0.0396(3) 0.1259(6) 0.0589(5) 0.062(2) Uani 1 1 d . . . C31 C -0.0769(3) 0.0746(5) -0.0187(5) 0.079(3) Uani 1 1 d G . . C32 C -0.0660(4) -0.0132(5) -0.0248(6) 0.137(6) Uani 1 1 d G . . H32 H -0.0350 -0.0423 0.0212 0.164 Uiso 1 1 calc R . . C33 C -0.1000(5) -0.0590(6) -0.0977(7) 0.169(8) Uani 1 1 d G . . H33 H -0.0925 -0.1198 -0.1019 0.203 Uiso 1 1 calc R . . C34 C -0.1449(5) -0.0170(7) -0.1643(6) 0.151(7) Uani 1 1 d G . . H34 H -0.1685 -0.0486 -0.2146 0.181 Uiso 1 1 calc R . . C35 C -0.1558(4) 0.0709(7) -0.1581(5) 0.173(9) Uani 1 1 d G . . H35 H -0.1869 0.1000 -0.2042 0.207 Uiso 1 1 calc R . . C36 C -0.1218(4) 0.1167(5) -0.0853(5) 0.131(6) Uani 1 1 d G . . H36 H -0.1294 0.1774 -0.0810 0.157 Uiso 1 1 calc R . . C37 C 0.0386(11) 0.4728(12) 0.2835(11) 0.095(8) Uani 0.50 1 d PD . . 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 0.0997(4) 0.0606(3) 0.0453(3) -0.00703(17) 0.0354(3) -0.0266(2) N1 0.130(8) 0.085(6) 0.051(5) -0.013(4) 0.042(6) -0.058(6) N2 0.147(10) 0.095(7) 0.060(6) -0.005(5) 0.055(7) -0.055(7) N3 0.057(4) 0.068(5) 0.050(4) -0.014(4) 0.022(3) -0.014(3) N4 0.057(4) 0.052(4) 0.066(5) -0.014(4) 0.014(4) -0.006(3) O1 0.112(6) 0.185(10) 0.051(4) -0.019(5) 0.040(5) -0.081(6) O2 0.174(8) 0.069(4) 0.071(5) 0.010(4) 0.066(6) 0.002(5) O3 0.077(4) 0.075(4) 0.046(3) -0.005(3) 0.029(3) -0.012(3) O4 0.090(4) 0.061(4) 0.044(3) -0.008(3) 0.032(3) -0.024(3) O5 0.080(5) 0.064(5) 0.068(5) -0.005(4) 0.040(4) -0.002(4) O6 0.30(2) 0.29(2) 0.29(2) -0.001(5) 0.172(13) 0.000(5) O7 0.100(6) 0.097(6) 0.098(6) 0.013(4) 0.057(5) 0.003(4) O8 0.218(7) 0.199(8) 0.188(7) 0.007(5) 0.122(5) -0.007(5) O9 0.154(5) 0.120(5) 0.136(5) -0.001(4) 0.076(4) -0.009(4) C1 0.122(11) 0.132(10) 0.053(6) -0.026(6) 0.039(7) -0.083(9) C2 0.104(10) 0.177(15) 0.066(8) -0.032(9) 0.041(8) -0.080(10) C3 0.146(13) 0.149(13) 0.081(9) -0.027(9) 0.063(10) -0.078(11) C4 0.154(14) 0.111(11) 0.100(11) -0.029(9) 0.080(12) -0.059(10) C5 0.194(19) 0.156(15) 0.150(17) -0.022(13) 0.130(17) -0.052(14) C6 0.22(3) 0.22(3) 0.16(2) -0.01(2) 0.14(2) -0.02(2) C7 0.26(3) 0.21(2) 0.139(19) -0.017(19) 0.15(2) -0.06(2) C8 0.180(17) 0.158(15) 0.118(13) -0.025(11) 0.108(14) -0.043(12) C9 0.154(13) 0.102(9) 0.093(10) -0.026(8) 0.084(11) -0.059(9) C10 0.148(12) 0.106(9) 0.067(7) -0.028(6) 0.062(9) -0.077(9) C11 0.156(13) 0.095(8) 0.056(7) -0.016(6) 0.054(8) -0.076(9) C12 0.168(14) 0.044(5) 0.074(8) 0.002(5) 0.054(9) -0.028(7) C13 0.190(16) 0.055(6) 0.080(9) 0.005(6) 0.059(10) -0.016(8) C14 0.26(2) 0.072(8) 0.084(9) 0.022(7) 0.090(12) 0.035(10) C15 0.32(3) 0.099(11) 0.099(12) 0.040(9) 0.117(17) 0.063(15) C16 0.22(2) 0.098(11) 0.094(12) 0.025(9) 0.056(13) 0.012(13) C17 0.193(18) 0.103(11) 0.124(14) 0.042(10) 0.072(13) 0.017(11) C18 0.195(18) 0.102(11) 0.089(11) 0.025(8) 0.054(12) -0.030(12) C19 0.069(6) 0.092(7) 0.045(5) -0.005(5) 0.027(5) -0.016(5) C20 0.088(8) 0.123(10) 0.055(6) -0.024(6) 0.031(6) -0.023(7) C21 0.087(9) 0.170(15) 0.056(7) -0.031(8) 0.021(7) -0.022(9) C22 0.081(8) 0.153(13) 0.073(8) -0.013(9) 0.025(7) -0.015(8) C23 0.095(11) 0.23(3) 0.090(11) 0.005(13) 0.000(9) 0.045(14) C24 0.081(11) 0.26(3) 0.17(2) 0.03(2) 0.012(13) 0.022(16) C25 0.112(12) 0.151(16) 0.171(19) 0.017(14) 0.024(13) 0.048(12) C26 0.093(9) 0.125(12) 0.135(13) -0.010(10) 0.017(9) 0.033(9) C27 0.074(7) 0.123(10) 0.064(7) 0.010(7) 0.018(6) 0.007(7) C28 0.066(6) 0.082(7) 0.055(5) -0.002(5) 0.021(5) -0.005(5) C29 0.072(6) 0.067(6) 0.065(6) -0.005(5) 0.027(5) 0.002(5) C30 0.057(5) 0.066(6) 0.051(5) -0.012(4) 0.025(4) -0.012(4) C31 0.075(6) 0.063(6) 0.076(7) -0.021(5) 0.032(5) -0.018(5) C32 0.165(14) 0.085(9) 0.094(10) -0.028(8) 0.039(10) -0.016(9) C33 0.24(2) 0.091(10) 0.105(12) -0.048(9) 0.058(14) -0.035(12) C34 0.163(15) 0.128(13) 0.080(10) -0.043(9) 0.025(10) -0.042(12) C35 0.197(18) 0.110(12) 0.083(10) -0.029(9) 0.010(11) -0.039(12) C36 0.150(12) 0.084(8) 0.070(8) -0.019(6) 0.015(8) -0.033(8) C37 0.125(19) 0.038(9) 0.042(10) -0.009(7) 0.003(11) -0.001(10) _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 2.185(11) . ? Dy1 O5 2.303(13) . ? Dy1 O3 2.339(7) 2 ? Dy1 O3 2.360(6) . ? Dy1 O4 2.362(6) . ? Dy1 O2 2.376(8) . ? Dy1 O7 2.383(18) 2 ? Dy1 N3 2.502(8) . ? Dy1 N1 2.508(10) . ? Dy1 Dy1 3.7112(10) 2 ? N1 C11 1.305(19) . ? N1 N2 1.407(15) . ? N2 C12 1.292(18) . ? N3 C29 1.270(12) . ? N3 N4 1.388(10) . ? N4 C30 1.321(12) . ? O1 C1 1.278(19) . ? O2 C12 1.245(15) . ? O3 C19 1.335(12) . ? O3 Dy1 2.339(7) 2 ? O4 C30 1.261(10) . ? O5 O7 1.20(2) 2 ? O5 C37 1.24(3) . ? O6 C37 1.365(19) . ? O7 O5 1.20(2) 2 ? O7 C37 1.28(2) 2 ? O7 C37 1.29(3) . ? O7 O7 1.52(3) 2 ? O7 Dy1 2.383(18) 2 ? C1 C10 1.413(17) . ? C1 C2 1.43(2) . ? C2 C3 1.29(2) . ? C3 C4 1.43(2) . ? C4 C5 1.33(2) . ? C4 C9 1.40(2) . ? C5 C6 1.31(3) . ? C6 C7 1.36(4) . ? C7 C8 1.33(3) . ? C8 C9 1.38(2) . ? C9 C10 1.47(2) . ? C10 C11 1.41(2) . ? C12 C13 1.486(16) . ? C13 C18 1.382(6) . ? C13 C14 1.382(6) . ? C14 C15 1.382(6) . ? C15 C16 1.382(6) . ? C16 C17 1.382(6) . ? C17 C18 1.382(6) . ? C19 C28 1.383(15) . ? C19 C20 1.402(14) . ? C20 C21 1.356(19) . ? C21 C22 1.38(2) . ? C22 C23 1.38(2) . ? C22 C27 1.444(17) . ? C23 C24 1.37(3) . ? C24 C25 1.45(3) . ? C25 C26 1.40(2) . ? C26 C27 1.43(2) . ? C27 C28 1.433(15) . ? C28 C29 1.457(13) . ? C30 C31 1.487(10) . ? C31 C32 1.374(5) . ? C31 C36 1.374(5) . ? C32 C33 1.374(5) . ? C33 C34 1.374(5) . ? C34 C35 1.374(5) . ? C35 C36 1.374(5) . ? C37 O7 1.28(2) 2 ? C37 C37 1.89(5) 2 ? 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 O5 77.6(4) . . ? O1 Dy1 O3 145.2(3) . 2 ? O5 Dy1 O3 104.0(4) . 2 ? O1 Dy1 O3 76.7(3) . . ? O5 Dy1 O3 78.2(4) . . ? O3 Dy1 O3 69.9(3) 2 . ? O1 Dy1 O4 113.1(3) . . ? O5 Dy1 O4 152.2(4) . . ? O3 Dy1 O4 81.8(2) 2 . ? O3 Dy1 O4 128.4(2) . . ? O1 Dy1 O2 127.8(3) . . ? O5 Dy1 O2 81.9(4) . . ? O3 Dy1 O2 86.3(3) 2 . ? O3 Dy1 O2 143.8(3) . . ? O4 Dy1 O2 71.3(3) . . ? O1 Dy1 O7 107.0(5) . 2 ? O5 Dy1 O7 29.6(5) . 2 ? O3 Dy1 O7 78.0(5) 2 2 ? O3 Dy1 O7 81.9(5) . 2 ? O4 Dy1 O7 133.8(5) . 2 ? O2 Dy1 O7 66.3(5) . 2 ? O1 Dy1 N3 78.9(3) . . ? O5 Dy1 N3 143.4(4) . . ? O3 Dy1 N3 80.6(2) 2 . ? O3 Dy1 N3 69.3(2) . . ? O4 Dy1 N3 64.0(2) . . ? O2 Dy1 N3 134.6(3) . . ? O7 Dy1 N3 148.7(4) 2 . ? O1 Dy1 N1 68.9(3) . . ? O5 Dy1 N1 90.2(4) . . ? O3 Dy1 N1 144.8(3) 2 . ? O3 Dy1 N1 145.3(3) . . ? O4 Dy1 N1 71.7(2) . . ? O2 Dy1 N1 63.7(4) . . ? O7 Dy1 N1 103.8(5) 2 . ? N3 Dy1 N1 106.9(3) . . ? O1 Dy1 Dy1 112.9(2) . 2 ? O5 Dy1 Dy1 76.9(3) . 2 ? O3 Dy1 Dy1 38.04(15) 2 2 ? O3 Dy1 Dy1 37.65(17) . 2 ? O4 Dy1 Dy1 117.92(16) . 2 ? O2 Dy1 Dy1 108.3(2) . 2 ? O7 Dy1 Dy1 62.2(4) 2 2 ? N3 Dy1 Dy1 86.97(17) . 2 ? N1 Dy1 Dy1 165.9(2) . 2 ? C11 N1 N2 115.2(10) . . ? C11 N1 Dy1 131.3(8) . . ? N2 N1 Dy1 113.4(9) . . ? C12 N2 N1 117.0(11) . . ? C29 N3 N4 114.8(8) . . ? C29 N3 Dy1 129.7(6) . . ? N4 N3 Dy1 115.4(6) . . ? C30 N4 N3 115.6(8) . . ? C1 O1 Dy1 145.9(7) . . ? C12 O2 Dy1 122.0(10) . . ? C19 O3 Dy1 128.8(6) . 2 ? C19 O3 Dy1 125.3(6) . . ? Dy1 O3 Dy1 104.3(3) 2 . ? C30 O4 Dy1 123.0(6) . . ? O7 O5 C37 63.4(15) 2 . ? O7 O5 Dy1 78.9(11) 2 . ? C37 O5 Dy1 124.4(15) . . ? O5 O7 C37 59.7(19) 2 2 ? O5 O7 C37 153.0(19) 2 . ? C37 O7 C37 94(2) 2 . ? O5 O7 O7 108(2) 2 2 ? C37 O7 O7 54.3(17) 2 2 ? C37 O7 O7 53.5(13) . 2 ? O5 O7 Dy1 71.5(11) 2 2 ? C37 O7 Dy1 116.6(17) 2 2 ? C37 O7 Dy1 132.4(14) . 2 ? O7 O7 Dy1 116.5(5) 2 2 ? O1 C1 C10 121.6(15) . . ? O1 C1 C2 119.8(12) . . ? C10 C1 C2 118.7(16) . . ? C3 C2 C1 122.2(15) . . ? C2 C3 C4 123.9(19) . . ? C5 C4 C9 118.7(17) . . ? C5 C4 C3 124(2) . . ? C9 C4 C3 116.8(17) . . ? C6 C5 C4 122(3) . . ? C5 C6 C7 121(3) . . ? C8 C7 C6 121(2) . . ? C7 C8 C9 119(2) . . ? C8 C9 C4 119.1(17) . . ? C8 C9 C10 120.4(18) . . ? C4 C9 C10 120.5(13) . . ? C1 C10 C11 121.0(15) . . ? C1 C10 C9 117.8(16) . . ? C11 C10 C9 121.2(13) . . ? N1 C11 C10 126.1(11) . . ? O2 C12 N2 120.9(14) . . ? O2 C12 C13 121.8(16) . . ? N2 C12 C13 117.2(13) . . ? C18 C13 C14 120.0 . . ? C18 C13 C12 117.1(11) . . ? C14 C13 C12 122.9(11) . . ? C13 C14 C15 120.0 . . ? C14 C15 C16 120.0 . . ? C17 C16 C15 120.0 . . ? C16 C17 C18 120.0 . . ? C13 C18 C17 120.0 . . ? O3 C19 C28 122.7(8) . . ? O3 C19 C20 117.8(11) . . ? C28 C19 C20 119.5(11) . . ? C21 C20 C19 120.6(13) . . ? C20 C21 C22 122.8(12) . . ? C21 C22 C23 120.7(16) . . ? C21 C22 C27 118.5(13) . . ? C23 C22 C27 120.8(18) . . ? C24 C23 C22 120(2) . . ? C23 C24 C25 121.5(19) . . ? C26 C25 C24 118(2) . . ? C25 C26 C27 120.1(16) . . ? C26 C27 C28 123.3(12) . . ? C26 C27 C22 118.6(12) . . ? C28 C27 C22 117.9(13) . . ? C19 C28 C27 120.7(10) . . ? C19 C28 C29 121.3(9) . . ? C27 C28 C29 118.0(10) . . ? N3 C29 C28 124.5(10) . . ? O4 C30 N4 121.1(8) . . ? O4 C30 C31 118.4(8) . . ? N4 C30 C31 120.5(8) . . ? C32 C31 C36 120.0 . . ? C32 C31 C30 120.6(6) . . ? C36 C31 C30 119.3(6) . . ? C31 C32 C33 120.0 . . ? C34 C33 C32 120.0 . . ? C35 C34 C33 120.0 . . ? C34 C35 C36 120.0 . . ? C31 C36 C35 120.0 . . ? O5 C37 O7 56.9(13) . 2 ? O5 C37 O7 121.6(18) . . ? O7 C37 O7 72(2) 2 . ? O5 C37 O6 117(3) . . ? O7 C37 O6 149(3) 2 . ? O7 C37 O6 122(3) . . ? O5 C37 C37 99.7(15) . 2 ? O7 C37 C37 43.1(11) 2 2 ? O7 C37 C37 42.6(15) . 2 ? O6 C37 C37 126(3) . 2 ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.03 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.737 _refine_diff_density_min -1.979 _refine_diff_density_rms 0.159 #===END data_complex2Dy2 #TrackingRef 'web_deposit_cif_file_0_JinkuiTang_1323166039.Dy2.cif' _database_code_depnum_ccdc_archive 'CCDC 845738' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common complex2Dy2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H39 Dy2 N11 O12' _chemical_formula_weight 1214.84 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 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 17.8580(6) _cell_length_b 10.8931(4) _cell_length_c 23.2797(8) _cell_angle_alpha 90.00 _cell_angle_beta 95.8582(4) _cell_angle_gamma 90.00 _cell_volume 4504.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used 9272 _cell_measurement_theta_min 2.74 _cell_measurement_theta_max 26.03 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.791 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2384 _exptl_absorpt_coefficient_mu 3.366 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4988 _exptl_absorpt_correction_T_max 0.5825 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 170(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12138 _diffrn_reflns_av_R_equivalents 0.0180 _diffrn_reflns_av_sigmaI/netI 0.0208 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 26.03 _reflns_number_total 4417 _reflns_number_gt 4100 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0205P)^2^+9.9215P] 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 4417 _refine_ls_number_parameters 306 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0210 _refine_ls_R_factor_gt 0.0188 _refine_ls_wR_factor_ref 0.0464 _refine_ls_wR_factor_gt 0.0454 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.081192(6) 0.590763(10) 0.468212(5) 0.01594(5) Uani 1 1 d . . . N1 N -0.10952(11) 0.2625(2) 0.44744(9) 0.0190(4) Uani 1 1 d . . . N2 N 0.00333(12) 0.42747(19) 0.35525(9) 0.0192(5) Uani 1 1 d . . . N3 N 0.05303(11) 0.5272(2) 0.36683(9) 0.0187(4) Uani 1 1 d . . . N4 N 0.21178(13) 0.4371(2) 0.49392(10) 0.0246(5) Uani 1 1 d . . . N5 N 0.0429(2) -0.0355(3) 0.39828(16) 0.0604(9) Uani 1 1 d . . . N6 N 0.0000 1.1042(5) 0.2500 0.096(2) Uani 1 2 d S . . O1 O -0.01482(10) 0.44845(17) 0.45210(7) 0.0203(4) Uani 1 1 d . . . O2 O 0.14690(10) 0.70724(17) 0.41748(7) 0.0218(4) Uani 1 1 d . . . O3 O 0.16655(12) 0.41861(19) 0.44891(9) 0.0334(5) Uani 1 1 d . . . O4 O 0.18943(12) 0.5142(2) 0.52928(8) 0.0354(5) Uani 1 1 d . . . O5 O 0.27201(12) 0.3857(2) 0.50211(10) 0.0418(6) Uani 1 1 d . . . O6 O -0.00715(10) 0.74962(18) 0.44519(8) 0.0274(4) Uani 1 1 d . . . H6 H -0.0046 0.7849 0.4081 0.033 Uiso 1 1 calc R . . C1 C -0.15481(15) 0.1650(2) 0.44796(11) 0.0231(6) Uani 1 1 d . . . H1 H -0.1763 0.1460 0.4826 0.028 Uiso 1 1 calc R . . C2 C -0.17183(16) 0.0902(3) 0.40010(13) 0.0270(6) Uani 1 1 d . . . H2 H -0.2040 0.0212 0.4020 0.032 Uiso 1 1 calc R . . C3 C -0.14111(16) 0.1182(3) 0.34961(12) 0.0273(6) Uani 1 1 d . . . H3 H -0.1517 0.0685 0.3163 0.033 Uiso 1 1 calc R . . C4 C -0.09490(15) 0.2193(2) 0.34817(11) 0.0231(6) Uani 1 1 d . . . H4 H -0.0738 0.2409 0.3137 0.028 Uiso 1 1 calc R . . C5 C -0.07982(13) 0.2886(2) 0.39766(10) 0.0178(5) Uani 1 1 d . . . C6 C -0.02731(14) 0.3951(2) 0.40114(11) 0.0175(5) Uani 1 1 d . . . C7 C 0.08344(14) 0.5605(2) 0.32108(11) 0.0184(5) Uani 1 1 d . . . H7 H 0.0697 0.5148 0.2869 0.022 Uiso 1 1 calc R . . C8 C 0.13613(14) 0.6599(2) 0.31664(11) 0.0182(5) Uani 1 1 d . . . C9 C 0.16344(14) 0.7310(2) 0.36503(11) 0.0193(5) Uani 1 1 d . . . C10 C 0.21110(15) 0.8334(3) 0.35746(12) 0.0238(6) Uani 1 1 d . . . H10 H 0.2286 0.8823 0.3899 0.029 Uiso 1 1 calc R . . C11 C 0.23194(15) 0.8623(3) 0.30476(12) 0.0247(6) Uani 1 1 d . . . H11 H 0.2637 0.9312 0.3011 0.030 Uiso 1 1 calc R . . C12 C 0.20756(15) 0.7923(2) 0.25500(11) 0.0230(6) Uani 1 1 d . . . C13 C 0.23019(16) 0.8241(3) 0.20027(12) 0.0275(6) Uani 1 1 d . . . H13 H 0.2633 0.8916 0.1973 0.033 Uiso 1 1 calc R . . C14 C 0.20525(16) 0.7593(3) 0.15161(12) 0.0299(6) Uani 1 1 d . . . H14 H 0.2207 0.7816 0.1152 0.036 Uiso 1 1 calc R . . C15 C 0.15669(16) 0.6599(3) 0.15641(12) 0.0286(6) Uani 1 1 d . . . H15 H 0.1389 0.6151 0.1228 0.034 Uiso 1 1 calc R . . C16 C 0.13434(15) 0.6260(3) 0.20877(11) 0.0238(6) Uani 1 1 d . . . H16 H 0.1014 0.5580 0.2106 0.029 Uiso 1 1 calc R . . C17 C 0.15924(14) 0.6902(2) 0.26019(11) 0.0195(5) Uani 1 1 d . . . C18 C -0.06361(18) 0.8021(3) 0.47690(14) 0.0388(8) Uani 1 1 d . . . H18A H -0.0887 0.7368 0.4967 0.058 Uiso 1 1 calc R . . H18B H -0.1007 0.8453 0.4503 0.058 Uiso 1 1 calc R . . H18C H -0.0402 0.8600 0.5055 0.058 Uiso 1 1 calc R . . C19 C 0.0767(2) 0.0467(4) 0.38527(16) 0.0449(8) Uani 1 1 d . . . C20 C 0.1191(2) 0.1502(4) 0.36788(18) 0.0518(9) Uani 1 1 d . . . H20A H 0.1560 0.1223 0.3424 0.078 Uiso 1 1 calc R . . H20B H 0.1453 0.1894 0.4021 0.078 Uiso 1 1 calc R . . H20C H 0.0848 0.2095 0.3473 0.078 Uiso 1 1 calc R . . C21 C 0.0000 0.9992(6) 0.2500 0.0613(15) Uani 1 2 d S . . C22 C 0.0000 0.8705(6) 0.2500 0.128(4) Uani 1 2 d S . . H22A H 0.0126 0.8405 0.2895 0.192 Uiso 0.50 1 calc P . . H22B H 0.0374 0.8405 0.2254 0.192 Uiso 0.50 1 calc P . . H22C H -0.0500 0.8405 0.2351 0.192 Uiso 0.50 1 calc P . . 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 0.01484(7) 0.01798(7) 0.01520(7) -0.00159(4) 0.00249(4) -0.00325(5) N1 0.0163(10) 0.0198(11) 0.0209(11) -0.0010(9) 0.0020(8) -0.0022(9) N2 0.0194(11) 0.0175(11) 0.0206(11) -0.0011(8) 0.0017(9) -0.0046(8) N3 0.0162(10) 0.0189(11) 0.0208(11) -0.0007(9) 0.0010(8) -0.0032(9) N4 0.0222(12) 0.0232(12) 0.0284(12) 0.0025(10) 0.0031(10) -0.0012(10) N5 0.062(2) 0.047(2) 0.075(2) 0.0184(18) 0.0233(18) 0.0048(17) N6 0.194(8) 0.052(4) 0.051(3) 0.000 0.052(4) 0.000 O1 0.0217(9) 0.0230(9) 0.0167(9) -0.0049(7) 0.0039(7) -0.0068(8) O2 0.0232(10) 0.0245(10) 0.0179(9) -0.0013(7) 0.0040(7) -0.0070(8) O3 0.0342(12) 0.0337(12) 0.0309(11) -0.0094(9) -0.0042(9) 0.0079(9) O4 0.0340(12) 0.0416(13) 0.0285(11) -0.0101(9) -0.0064(9) 0.0108(10) O5 0.0259(12) 0.0463(14) 0.0527(14) 0.0041(11) 0.0006(10) 0.0138(10) O6 0.0246(10) 0.0320(11) 0.0260(10) 0.0020(8) 0.0051(8) 0.0055(8) C1 0.0241(14) 0.0221(14) 0.0239(13) 0.0011(11) 0.0057(11) -0.0057(11) C2 0.0246(15) 0.0219(14) 0.0349(16) -0.0038(12) 0.0043(12) -0.0068(11) C3 0.0294(15) 0.0241(15) 0.0283(14) -0.0100(11) 0.0030(12) -0.0064(12) C4 0.0226(13) 0.0235(14) 0.0236(13) -0.0039(11) 0.0050(11) -0.0039(11) C5 0.0155(12) 0.0162(12) 0.0214(12) -0.0010(10) 0.0014(10) -0.0005(10) C6 0.0160(12) 0.0172(13) 0.0188(12) -0.0016(10) -0.0002(10) 0.0013(10) C7 0.0185(13) 0.0185(13) 0.0179(12) -0.0010(10) 0.0010(10) -0.0010(10) C8 0.0159(12) 0.0187(13) 0.0203(12) 0.0021(10) 0.0032(10) 0.0013(10) C9 0.0161(12) 0.0221(13) 0.0200(12) 0.0008(10) 0.0042(10) 0.0003(10) C10 0.0215(13) 0.0248(14) 0.0253(13) -0.0030(11) 0.0036(11) -0.0042(11) C11 0.0216(14) 0.0220(14) 0.0309(14) 0.0018(11) 0.0052(11) -0.0072(11) C12 0.0210(13) 0.0238(15) 0.0247(14) 0.0048(11) 0.0053(11) 0.0012(11) C13 0.0267(15) 0.0272(15) 0.0302(15) 0.0082(12) 0.0108(12) -0.0020(12) C14 0.0330(16) 0.0329(17) 0.0255(14) 0.0089(12) 0.0109(12) 0.0041(13) C15 0.0333(16) 0.0318(16) 0.0210(13) 0.0014(12) 0.0042(11) 0.0039(13) C16 0.0262(14) 0.0239(14) 0.0219(13) 0.0015(11) 0.0052(11) -0.0002(11) C17 0.0163(12) 0.0206(13) 0.0219(13) 0.0040(10) 0.0035(10) 0.0030(10) C18 0.0361(18) 0.0373(19) 0.0452(19) 0.0028(14) 0.0152(14) 0.0136(14) C19 0.045(2) 0.044(2) 0.048(2) 0.0065(17) 0.0111(16) 0.0099(17) C20 0.046(2) 0.044(2) 0.068(3) -0.0022(19) 0.0153(18) -0.0052(17) C21 0.052(3) 0.059(4) 0.074(4) 0.000 0.013(3) 0.000 C22 0.065(5) 0.035(4) 0.266(13) 0.000 -0.063(6) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O2 2.1598(17) . ? Dy1 O1 2.3135(17) . ? Dy1 O1 2.3404(17) 5_566 ? Dy1 O6 2.3659(19) . ? Dy1 O4 2.427(2) . ? Dy1 N3 2.462(2) . ? Dy1 O3 2.486(2) . ? Dy1 N1 2.543(2) 5_566 ? Dy1 Dy1 3.9225(2) 5_566 ? N1 C1 1.335(3) . ? N1 C5 1.353(3) . ? N1 Dy1 2.543(2) 5_566 ? N2 C6 1.298(3) . ? N2 N3 1.412(3) . ? N3 C7 1.295(3) . ? N4 O5 1.210(3) . ? N4 O4 1.268(3) . ? N4 O3 1.272(3) . ? N5 C19 1.137(5) . ? N6 C21 1.143(8) . ? O1 C6 1.320(3) . ? O1 Dy1 2.3404(17) 5_566 ? O2 C9 1.311(3) . ? O6 C18 1.428(3) . ? O6 H6 0.9500 . ? C1 C2 1.389(4) . ? C1 H1 0.9500 . ? C2 C3 1.381(4) . ? C2 H2 0.9500 . ? C3 C4 1.378(4) . ? C3 H3 0.9500 . ? C4 C5 1.381(3) . ? C4 H4 0.9500 . ? C5 C6 1.489(3) . ? C7 C8 1.445(4) . ? C7 H7 0.9500 . ? C8 C9 1.412(4) . ? C8 C17 1.455(3) . ? C9 C10 1.425(4) . ? C10 C11 1.355(4) . ? C10 H10 0.9500 . ? C11 C12 1.418(4) . ? C11 H11 0.9500 . ? C12 C13 1.419(4) . ? C12 C17 1.420(4) . ? C13 C14 1.370(4) . ? C13 H13 0.9500 . ? C14 C15 1.399(4) . ? C14 H14 0.9500 . ? C15 C16 1.372(4) . ? C15 H15 0.9500 . ? C16 C17 1.418(4) . ? C16 H16 0.9500 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.440(5) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.403(9) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 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 137.73(6) . . ? O2 Dy1 O1 152.63(6) . 5_566 ? O1 Dy1 O1 65.12(7) . 5_566 ? O2 Dy1 O6 80.41(7) . . ? O1 Dy1 O6 89.28(7) . . ? O1 Dy1 O6 86.16(6) 5_566 . ? O2 Dy1 O4 94.45(7) . . ? O1 Dy1 O4 113.41(7) . . ? O1 Dy1 O4 84.86(7) 5_566 . ? O6 Dy1 O4 148.95(7) . . ? O2 Dy1 N3 73.14(7) . . ? O1 Dy1 N3 65.21(6) . . ? O1 Dy1 N3 129.66(6) 5_566 . ? O6 Dy1 N3 85.54(7) . . ? O4 Dy1 N3 122.51(7) . . ? O2 Dy1 O3 88.10(7) . . ? O1 Dy1 O3 85.59(7) . . ? O1 Dy1 O3 112.03(7) 5_566 . ? O6 Dy1 O3 156.58(7) . . ? O4 Dy1 O3 51.72(7) . . ? N3 Dy1 O3 71.56(7) . . ? O2 Dy1 N1 88.66(7) . 5_566 ? O1 Dy1 N1 129.22(6) . 5_566 ? O1 Dy1 N1 65.14(6) 5_566 5_566 ? O6 Dy1 N1 77.91(7) . 5_566 ? O4 Dy1 N1 71.34(7) . 5_566 ? N3 Dy1 N1 157.26(7) . 5_566 ? O3 Dy1 N1 122.45(7) . 5_566 ? O2 Dy1 Dy1 165.09(5) . 5_566 ? O1 Dy1 Dy1 32.77(4) . 5_566 ? O1 Dy1 Dy1 32.35(4) 5_566 5_566 ? O6 Dy1 Dy1 87.28(5) . 5_566 ? O4 Dy1 Dy1 100.42(6) . 5_566 ? N3 Dy1 Dy1 97.67(5) . 5_566 ? O3 Dy1 Dy1 100.28(5) . 5_566 ? N1 Dy1 Dy1 97.01(5) 5_566 5_566 ? C1 N1 C5 117.8(2) . . ? C1 N1 Dy1 124.46(17) . 5_566 ? C5 N1 Dy1 117.69(16) . 5_566 ? C6 N2 N3 111.2(2) . . ? C7 N3 N2 111.5(2) . . ? C7 N3 Dy1 130.37(17) . . ? N2 N3 Dy1 117.54(14) . . ? O5 N4 O4 122.5(2) . . ? O5 N4 O3 122.4(2) . . ? O4 N4 O3 115.1(2) . . ? C6 O1 Dy1 119.70(15) . . ? C6 O1 Dy1 125.41(15) . 5_566 ? Dy1 O1 Dy1 114.88(7) . 5_566 ? C9 O2 Dy1 144.28(16) . . ? N4 O3 Dy1 94.64(15) . . ? N4 O4 Dy1 97.57(15) . . ? C18 O6 Dy1 131.69(17) . . ? C18 O6 H6 114.2 . . ? Dy1 O6 H6 114.2 . . ? N1 C1 C2 122.8(2) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C3 C2 C1 118.7(3) . . ? C3 C2 H2 120.7 . . ? C1 C2 H2 120.7 . . ? C4 C3 C2 119.2(3) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C3 C4 C5 118.9(2) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? N1 C5 C4 122.7(2) . . ? N1 C5 C6 114.7(2) . . ? C4 C5 C6 122.7(2) . . ? N2 C6 O1 125.0(2) . . ? N2 C6 C5 118.9(2) . . ? O1 C6 C5 116.1(2) . . ? N3 C7 C8 126.8(2) . . ? N3 C7 H7 116.6 . . ? C8 C7 H7 116.6 . . ? C9 C8 C7 121.9(2) . . ? C9 C8 C17 119.3(2) . . ? C7 C8 C17 118.8(2) . . ? O2 C9 C8 122.9(2) . . ? O2 C9 C10 117.6(2) . . ? C8 C9 C10 119.5(2) . . ? C11 C10 C9 121.1(2) . . ? C11 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C10 C11 C12 121.7(2) . . ? C10 C11 H11 119.1 . . ? C12 C11 H11 119.1 . . ? C11 C12 C13 120.7(3) . . ? C11 C12 C17 119.3(2) . . ? C13 C12 C17 119.9(2) . . ? C14 C13 C12 121.2(3) . . ? C14 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? C13 C14 C15 119.0(3) . . ? C13 C14 H14 120.5 . . ? C15 C14 H14 120.5 . . ? C16 C15 C14 121.2(3) . . ? C16 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? C15 C16 C17 121.5(3) . . ? C15 C16 H16 119.2 . . ? C17 C16 H16 119.2 . . ? C16 C17 C12 117.1(2) . . ? C16 C17 C8 123.9(2) . . ? C12 C17 C8 119.0(2) . . ? O6 C18 H18A 109.5 . . ? O6 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? O6 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N5 C19 C20 179.1(5) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N6 C21 C22 180.000(4) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.03 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.580 _refine_diff_density_min -0.569 _refine_diff_density_rms 0.079