# 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_name 'Yulin Yang' _publ_contact_author_email ylyang@hit.edu.cn loop_ _publ_author_name 'Xin Wang' 'Yulin Yang' 'Ping Wang' 'Liang Li' 'Ruiqing Fan' 'Wenwu Cao' 'Bing Yang' 'Hui Wang' 'Jingyao Liu' # Attachment '- Tb.CIF' data_w _database_code_depnum_ccdc_archive 'CCDC 740890' #TrackingRef '- Tb.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H36 N3 O16 Tb' _chemical_formula_weight 841.53 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' 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' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ORTHORHOMBIC _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.9674(11) _cell_length_b 10.6721(7) _cell_length_c 18.6477(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3376.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 17382 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 25.72 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.655 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1696 _exptl_absorpt_coefficient_mu 2.172 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5886 _exptl_absorpt_correction_T_max 0.6743 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Bruker Smart APEX CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 17329 _diffrn_reflns_av_R_equivalents 0.0208 _diffrn_reflns_av_sigmaI/netI 0.0153 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 25.72 _reflns_number_total 3208 _reflns_number_gt 2786 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXP-97 _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.0434P)^2^+35.2770P] 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 3208 _refine_ls_number_parameters 223 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0538 _refine_ls_R_factor_gt 0.0482 _refine_ls_wR_factor_ref 0.1248 _refine_ls_wR_factor_gt 0.1211 _refine_ls_goodness_of_fit_ref 0.967 _refine_ls_restrained_S_all 0.967 _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 Tb1 Tb 0.0000 -0.13046(4) -0.2500 0.03384(15) Uani 1 2 d S . . O1 O -0.0922(3) -0.0661(4) -0.3439(3) 0.0465(11) Uani 1 1 d . . . O2 O -0.2051(3) -0.0859(6) -0.4034(3) 0.0690(16) Uani 1 1 d . . . H2 H -0.2446 -0.1300 -0.4010 0.104 Uiso 1 1 calc R . . O3 O -0.0172(3) -0.2951(5) -0.1618(3) 0.0539(13) Uani 1 1 d . . . O4 O -0.0910(3) -0.4379(5) -0.1059(3) 0.0647(15) Uani 1 1 d . . . O5 O -0.0852(3) -0.0304(4) -0.1629(2) 0.0422(10) Uani 1 1 d . . . O6 O -0.1167(3) 0.1359(5) -0.0963(3) 0.0612(15) Uani 1 1 d . . . H6 H -0.1390 0.0824 -0.0722 0.092 Uiso 1 1 calc R . . N1 N -0.1284(3) -0.2480(5) -0.2555(3) 0.0400(12) Uani 1 1 d . . . N2 N 0.0000 0.1050(7) -0.2500 0.0354(16) Uani 1 2 d S . . C1 C -0.1581(4) -0.1165(7) -0.3553(4) 0.0449(16) Uani 1 1 d . . . C2 C -0.1814(4) -0.2213(7) -0.3060(4) 0.0441(16) Uani 1 1 d . . . C3 C -0.2519(5) -0.2854(8) -0.3111(4) 0.059(2) Uani 1 1 d . . . H3A H -0.2880 -0.2651 -0.3468 0.071 Uiso 1 1 calc R . . C4 C -0.2679(5) -0.3779(8) -0.2637(3) 0.056(2) Uani 1 1 d . . . H4A H -0.3152 -0.4215 -0.2667 0.067 Uiso 1 1 calc R . . C5 C -0.2129(5) -0.4080(8) -0.2100(4) 0.062(2) Uani 1 1 d . . . H5A H -0.2228 -0.4708 -0.1766 0.074 Uiso 1 1 calc R . . C6 C -0.1427(4) -0.3394(6) -0.2089(4) 0.0441(16) Uani 1 1 d . . . C7 C -0.0792(4) -0.3606(6) -0.1538(4) 0.0433(16) Uani 1 1 d . . . C8 C -0.0843(4) 0.0857(6) -0.1482(3) 0.0393(14) Uani 1 1 d . . . C9 C -0.0401(4) 0.1675(6) -0.1996(3) 0.0371(14) Uani 1 1 d . . . C10 C -0.0415(5) 0.2968(7) -0.1984(4) 0.059(2) Uani 1 1 d . . . H10 H -0.0700 0.3389 -0.1633 0.071 Uiso 1 1 calc R . . C11 C 0.0000 0.3636(10) -0.2500 0.073(4) Uani 1 2 d S . . H11 H 0.0000 0.4507 -0.2500 0.087 Uiso 1 2 calc SR . . O7 O 0.0672(5) -0.3298(8) -0.0175(5) 0.117(3) Uani 1 1 d . . . H7A H 0.0348 -0.2972 0.0093 0.175 Uiso 1 1 calc R . . C12 C 0.0412(7) -0.4667(13) -0.0349(7) 0.110(4) Uani 1 1 d . . . H12A H -0.0086 -0.4649 -0.0604 0.132 Uiso 1 1 calc R . . H12B H 0.0333 -0.5123 0.0095 0.132 Uiso 1 1 calc R . . C13 C 0.1092(8) -0.5417(13) -0.0854(7) 0.121(5) Uani 1 1 d . . . H13A H 0.0915 -0.6254 -0.0952 0.182 Uiso 1 1 calc R . . H13B H 0.1583 -0.5447 -0.0599 0.182 Uiso 1 1 calc R . . H13C H 0.1164 -0.4974 -0.1297 0.182 Uiso 1 1 calc R . . O8 O -0.0956(9) 0.1365(11) -0.4929(6) 0.177(5) Uani 1 1 d . . . H8A H -0.0617 0.0890 -0.4774 0.265 Uiso 1 1 calc R . . C14 C -0.1651(5) 0.0650(7) -0.5123(4) 0.0492(17) Uani 1 1 d . . . H14A H -0.1507 0.0027 -0.5479 0.059 Uiso 1 1 calc R . . H14B H -0.1845 0.0213 -0.4703 0.059 Uiso 1 1 calc R . . C15 C -0.2272(7) 0.1436(11) -0.5410(6) 0.105(4) Uani 1 1 d . . . H15A H -0.2718 0.0925 -0.5534 0.157 Uiso 1 1 calc R . . H15B H -0.2085 0.1863 -0.5829 0.157 Uiso 1 1 calc R . . H15C H -0.2427 0.2040 -0.5055 0.157 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 Tb1 0.0282(2) 0.0273(2) 0.0460(3) 0.000 0.00331(19) 0.000 O1 0.038(2) 0.047(3) 0.055(3) -0.002(2) -0.002(2) 0.000(2) O2 0.051(3) 0.100(5) 0.055(3) 0.014(3) -0.014(3) -0.005(3) O3 0.041(3) 0.044(3) 0.076(4) 0.019(3) 0.005(2) -0.003(2) O4 0.065(3) 0.058(3) 0.071(4) 0.034(3) 0.006(3) -0.010(3) O5 0.042(2) 0.036(2) 0.048(3) 0.003(2) 0.010(2) -0.0013(19) O6 0.083(4) 0.052(3) 0.049(3) -0.004(2) 0.037(3) 0.003(3) N1 0.034(3) 0.035(3) 0.051(3) -0.010(3) 0.009(3) -0.003(2) N2 0.035(4) 0.032(4) 0.039(4) 0.000 0.015(3) 0.000 C1 0.036(3) 0.058(4) 0.041(4) -0.009(3) -0.004(3) 0.009(3) C2 0.035(3) 0.051(4) 0.046(4) -0.014(3) 0.007(3) -0.001(3) C3 0.045(4) 0.084(6) 0.048(4) -0.012(4) 0.001(4) -0.016(4) C4 0.062(5) 0.080(6) 0.026(4) -0.022(3) 0.011(3) -0.034(4) C5 0.071(5) 0.060(5) 0.055(5) -0.006(4) 0.022(4) -0.026(4) C6 0.042(4) 0.037(3) 0.053(4) -0.011(3) 0.008(3) -0.005(3) C7 0.050(4) 0.031(3) 0.049(4) 0.001(3) 0.014(3) 0.002(3) C8 0.040(3) 0.047(4) 0.032(3) 0.002(3) 0.007(3) 0.006(3) C9 0.042(3) 0.039(3) 0.030(3) -0.001(3) 0.004(3) 0.000(3) C10 0.085(6) 0.037(4) 0.055(5) -0.006(3) 0.024(4) 0.003(4) C11 0.115(11) 0.030(5) 0.073(8) 0.000 0.050(8) 0.000 O7 0.115(6) 0.083(5) 0.152(8) -0.017(5) -0.041(6) -0.001(5) C12 0.095(8) 0.119(10) 0.116(10) 0.040(8) -0.002(8) 0.004(8) C13 0.121(10) 0.147(12) 0.095(9) -0.013(9) 0.029(8) -0.051(9) O8 0.222(14) 0.178(12) 0.131(9) 0.007(8) 0.009(9) -0.024(10) C14 0.064(5) 0.056(4) 0.028(3) -0.013(3) 0.008(3) -0.004(4) C15 0.127(10) 0.119(10) 0.068(7) 0.009(6) 0.036(7) 0.028(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O5 2.422(4) 3_554 ? Tb1 O5 2.422(4) . ? Tb1 O3 2.425(5) 3_554 ? Tb1 O3 2.425(5) . ? Tb1 O1 2.447(5) 3_554 ? Tb1 O1 2.447(5) . ? Tb1 N2 2.513(7) . ? Tb1 N1 2.515(5) 3_554 ? Tb1 N1 2.515(5) . ? O1 C1 1.258(8) . ? O2 C1 1.245(8) . ? O2 H2 0.8200 . ? O3 C7 1.271(8) . ? O4 C7 1.233(8) . ? O5 C8 1.269(8) . ? O6 C8 1.235(8) . ? O6 H6 0.8200 . ? N1 C6 1.328(9) . ? N1 C2 1.333(9) . ? N2 C9 1.338(7) . ? N2 C9 1.338(7) 3_554 ? C1 C2 1.500(10) . ? C2 C3 1.381(10) . ? C3 C4 1.353(11) . ? C3 H3A 0.9300 . ? C4 C5 1.406(12) . ? C4 H4A 0.9300 . ? C5 C6 1.399(10) . ? C5 H5A 0.9300 . ? C6 C7 1.507(10) . ? C8 C9 1.498(9) . ? C9 C10 1.380(10) . ? C10 C11 1.388(9) . ? C10 H10 0.9300 . ? C11 C10 1.388(9) 3_554 ? C11 H11 0.9300 . ? O7 C12 1.561(15) . ? O7 H7A 0.8200 . ? C12 C13 1.691(17) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? O8 C14 1.450(14) . ? O8 H8A 0.8200 . ? C14 C15 1.450(13) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? 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 Tb1 O5 127.7(2) 3_554 . ? O5 Tb1 O3 78.05(16) 3_554 3_554 ? O5 Tb1 O3 147.81(16) . 3_554 ? O5 Tb1 O3 147.81(16) 3_554 . ? O5 Tb1 O3 78.05(16) . . ? O3 Tb1 O3 87.1(3) 3_554 . ? O5 Tb1 O1 88.52(16) 3_554 3_554 ? O5 Tb1 O1 77.19(16) . 3_554 ? O3 Tb1 O1 127.73(16) 3_554 3_554 ? O3 Tb1 O1 78.17(17) . 3_554 ? O5 Tb1 O1 77.19(16) 3_554 . ? O5 Tb1 O1 88.52(16) . . ? O3 Tb1 O1 78.17(17) 3_554 . ? O3 Tb1 O1 127.73(16) . . ? O1 Tb1 O1 147.4(2) 3_554 . ? O5 Tb1 N2 63.83(10) 3_554 . ? O5 Tb1 N2 63.83(10) . . ? O3 Tb1 N2 136.44(13) 3_554 . ? O3 Tb1 N2 136.44(13) . . ? O1 Tb1 N2 73.69(11) 3_554 . ? O1 Tb1 N2 73.69(11) . . ? O5 Tb1 N1 74.36(16) 3_554 3_554 ? O5 Tb1 N1 135.19(17) . 3_554 ? O3 Tb1 N1 64.02(18) 3_554 3_554 ? O3 Tb1 N1 73.46(16) . 3_554 ? O1 Tb1 N1 63.71(17) 3_554 3_554 ? O1 Tb1 N1 136.30(17) . 3_554 ? N2 Tb1 N1 119.91(12) . 3_554 ? O5 Tb1 N1 135.19(17) 3_554 . ? O5 Tb1 N1 74.36(16) . . ? O3 Tb1 N1 73.46(16) 3_554 . ? O3 Tb1 N1 64.02(18) . . ? O1 Tb1 N1 136.30(17) 3_554 . ? O1 Tb1 N1 63.71(17) . . ? N2 Tb1 N1 119.91(12) . . ? N1 Tb1 N1 120.2(2) 3_554 . ? C1 O1 Tb1 124.6(5) . . ? C1 O2 H2 109.5 . . ? C7 O3 Tb1 125.3(5) . . ? C8 O5 Tb1 124.6(4) . . ? C8 O6 H6 109.5 . . ? C6 N1 C2 119.7(6) . . ? C6 N1 Tb1 119.9(5) . . ? C2 N1 Tb1 120.4(4) . . ? C9 N2 C9 120.2(8) . 3_554 ? C9 N2 Tb1 119.9(4) . . ? C9 N2 Tb1 119.9(4) 3_554 . ? O2 C1 O1 125.4(7) . . ? O2 C1 C2 117.9(6) . . ? O1 C1 C2 116.7(6) . . ? N1 C2 C3 121.8(7) . . ? N1 C2 C1 114.5(6) . . ? C3 C2 C1 123.7(7) . . ? C4 C3 C2 119.4(8) . . ? C4 C3 H3A 120.3 . . ? C2 C3 H3A 120.3 . . ? C3 C4 C5 119.9(7) . . ? C3 C4 H4A 120.0 . . ? C5 C4 H4A 120.0 . . ? C6 C5 C4 117.1(7) . . ? C6 C5 H5A 121.4 . . ? C4 C5 H5A 121.4 . . ? N1 C6 C5 122.1(7) . . ? N1 C6 C7 115.2(6) . . ? C5 C6 C7 122.7(7) . . ? O3 C7 O4 126.0(7) . . ? O3 C7 C6 115.4(6) . . ? O4 C7 C6 118.6(6) . . ? O6 C8 O5 126.0(6) . . ? O6 C8 C9 118.1(6) . . ? O5 C8 C9 115.9(5) . . ? N2 C9 C10 121.2(6) . . ? N2 C9 C8 114.4(6) . . ? C10 C9 C8 124.3(6) . . ? C9 C10 C11 119.6(7) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? C10 C11 C10 118.2(9) 3_554 . ? C10 C11 H11 120.9 3_554 . ? C10 C11 H11 120.9 . . ? C12 O7 H7A 109.5 . . ? O7 C12 C13 111.5(9) . . ? O7 C12 H12A 109.3 . . ? C13 C12 H12A 109.3 . . ? O7 C12 H12B 109.3 . . ? C13 C12 H12B 109.3 . . ? H12A C12 H12B 108.0 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C14 O8 H8A 109.5 . . ? C15 C14 O8 112.3(9) . . ? C15 C14 H14A 109.1 . . ? O8 C14 H14A 109.1 . . ? C15 C14 H14B 109.1 . . ? O8 C14 H14B 109.1 . . ? H14A C14 H14B 107.9 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? 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 Tb1 O1 C1 155.8(5) 3_554 . . . ? O5 Tb1 O1 C1 -75.0(5) . . . . ? O3 Tb1 O1 C1 75.5(5) 3_554 . . . ? O3 Tb1 O1 C1 -1.4(6) . . . . ? O1 Tb1 O1 C1 -138.1(5) 3_554 . . . ? N2 Tb1 O1 C1 -138.1(5) . . . . ? N1 Tb1 O1 C1 105.4(5) 3_554 . . . ? N1 Tb1 O1 C1 -1.7(5) . . . . ? O5 Tb1 O3 C7 -138.5(5) 3_554 . . . ? O5 Tb1 O3 C7 74.8(5) . . . . ? O3 Tb1 O3 C7 -76.5(5) 3_554 . . . ? O1 Tb1 O3 C7 154.0(6) 3_554 . . . ? O1 Tb1 O3 C7 -3.8(6) . . . . ? N2 Tb1 O3 C7 103.5(5) . . . . ? N1 Tb1 O3 C7 -140.2(6) 3_554 . . . ? N1 Tb1 O3 C7 -3.5(5) . . . . ? O5 Tb1 O5 C8 -10.7(5) 3_554 . . . ? O3 Tb1 O5 C8 -148.0(5) 3_554 . . . ? O3 Tb1 O5 C8 147.6(5) . . . . ? O1 Tb1 O5 C8 67.2(5) 3_554 . . . ? O1 Tb1 O5 C8 -83.2(5) . . . . ? N2 Tb1 O5 C8 -10.7(5) . . . . ? N1 Tb1 O5 C8 96.4(5) 3_554 . . . ? N1 Tb1 O5 C8 -146.3(5) . . . . ? O5 Tb1 N1 C6 147.9(4) 3_554 . . . ? O5 Tb1 N1 C6 -83.9(5) . . . . ? O3 Tb1 N1 C6 95.2(5) 3_554 . . . ? O3 Tb1 N1 C6 0.2(4) . . . . ? O1 Tb1 N1 C6 -32.6(6) 3_554 . . . ? O1 Tb1 N1 C6 179.9(5) . . . . ? N2 Tb1 N1 C6 -130.3(4) . . . . ? N1 Tb1 N1 C6 49.7(4) 3_554 . . . ? O5 Tb1 N1 C2 -30.3(6) 3_554 . . . ? O5 Tb1 N1 C2 97.9(5) . . . . ? O3 Tb1 N1 C2 -83.1(5) 3_554 . . . ? O3 Tb1 N1 C2 -178.0(5) . . . . ? O1 Tb1 N1 C2 149.1(4) 3_554 . . . ? O1 Tb1 N1 C2 1.6(4) . . . . ? N2 Tb1 N1 C2 51.4(5) . . . . ? N1 Tb1 N1 C2 -128.6(5) 3_554 . . . ? O5 Tb1 N2 C9 -174.2(3) 3_554 . . . ? O5 Tb1 N2 C9 5.8(3) . . . . ? O3 Tb1 N2 C9 154.2(4) 3_554 . . . ? O3 Tb1 N2 C9 -25.8(4) . . . . ? O1 Tb1 N2 C9 -77.7(3) 3_554 . . . ? O1 Tb1 N2 C9 102.3(3) . . . . ? N1 Tb1 N2 C9 -123.2(4) 3_554 . . . ? N1 Tb1 N2 C9 56.8(4) . . . . ? O5 Tb1 N2 C9 5.8(3) 3_554 . . 3_554 ? O5 Tb1 N2 C9 -174.2(3) . . . 3_554 ? O3 Tb1 N2 C9 -25.8(4) 3_554 . . 3_554 ? O3 Tb1 N2 C9 154.2(4) . . . 3_554 ? O1 Tb1 N2 C9 102.3(3) 3_554 . . 3_554 ? O1 Tb1 N2 C9 -77.7(3) . . . 3_554 ? N1 Tb1 N2 C9 56.8(4) 3_554 . . 3_554 ? N1 Tb1 N2 C9 -123.2(4) . . . 3_554 ? Tb1 O1 C1 O2 -179.0(5) . . . . ? Tb1 O1 C1 C2 1.6(8) . . . . ? C6 N1 C2 C3 0.7(10) . . . . ? Tb1 N1 C2 C3 179.0(5) . . . . ? C6 N1 C2 C1 -179.8(6) . . . . ? Tb1 N1 C2 C1 -1.6(7) . . . . ? O2 C1 C2 N1 -179.4(6) . . . . ? O1 C1 C2 N1 0.0(9) . . . . ? O2 C1 C2 C3 0.0(11) . . . . ? O1 C1 C2 C3 179.5(7) . . . . ? N1 C2 C3 C4 0.0(11) . . . . ? C1 C2 C3 C4 -179.4(7) . . . . ? C2 C3 C4 C5 -0.1(12) . . . . ? C3 C4 C5 C6 -0.5(12) . . . . ? C2 N1 C6 C5 -1.3(10) . . . . ? Tb1 N1 C6 C5 -179.6(5) . . . . ? C2 N1 C6 C7 -179.5(6) . . . . ? Tb1 N1 C6 C7 2.2(7) . . . . ? C4 C5 C6 N1 1.2(11) . . . . ? C4 C5 C6 C7 179.2(7) . . . . ? Tb1 O3 C7 O4 -174.1(5) . . . . ? Tb1 O3 C7 C6 5.8(8) . . . . ? N1 C6 C7 O3 -5.0(9) . . . . ? C5 C6 C7 O3 176.8(7) . . . . ? N1 C6 C7 O4 174.9(6) . . . . ? C5 C6 C7 O4 -3.2(10) . . . . ? Tb1 O5 C8 O6 -166.7(6) . . . . ? Tb1 O5 C8 C9 13.7(8) . . . . ? C9 N2 C9 C10 0.3(6) 3_554 . . . ? Tb1 N2 C9 C10 -179.7(6) . . . . ? C9 N2 C9 C8 178.1(6) 3_554 . . . ? Tb1 N2 C9 C8 -1.9(6) . . . . ? O6 C8 C9 N2 173.4(6) . . . . ? O5 C8 C9 N2 -7.1(8) . . . . ? O6 C8 C9 C10 -8.9(11) . . . . ? O5 C8 C9 C10 170.6(7) . . . . ? N2 C9 C10 C11 -0.6(12) . . . . ? C8 C9 C10 C11 -178.1(6) . . . . ? C9 C10 C11 C10 0.3(6) . . . 3_554 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.72 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.549 _refine_diff_density_min -0.540 _refine_diff_density_rms 0.095 data_r _database_code_depnum_ccdc_archive 'CCDC 818568' #TrackingRef '- Dy.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H36 Dy N3 O16' _chemical_formula_weight 845.11 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+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.947(3) _cell_length_b 10.654(2) _cell_length_c 18.659(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3368.9(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.666 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1700 _exptl_absorpt_coefficient_mu 2.296 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.6567 _exptl_absorpt_correction_T_max 0.7702 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 31096 _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_av_sigmaI/netI 0.0200 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 27.46 _reflns_number_total 3839 _reflns_number_gt 2985 _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^)+(0.0424P)^2^+13.6043P] 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 3839 _refine_ls_number_parameters 227 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0476 _refine_ls_R_factor_gt 0.0351 _refine_ls_wR_factor_ref 0.0961 _refine_ls_wR_factor_gt 0.0887 _refine_ls_goodness_of_fit_ref 0.961 _refine_ls_restrained_S_all 0.982 _refine_ls_shift/su_max 0.006 _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 0.0013(6) 0.86978(3) 0.2568(2) 0.0227(5) Uani 0.50 1 d P . . O1 O 0.0907(2) 0.5621(3) 0.1064(2) 0.0616(10) Uani 1 1 d . . . H1 H 0.0522 0.5584 0.0798 0.092 Uiso 0.50 1 calc PR . . O2 O 0.01675(18) 0.7060(3) 0.1620(2) 0.0480(8) Uani 1 1 d . . . O3 O 0.2050(2) 0.9152(4) 0.4029(2) 0.0625(10) Uani 1 1 d . . . O4 O 0.09166(18) 0.9347(3) 0.34356(17) 0.0414(7) Uani 1 1 d . . . O5 O 0.08505(17) 0.9689(3) 0.16314(16) 0.0377(7) Uani 1 1 d . . . O6 O 0.1175(2) 1.1333(3) 0.0961(2) 0.0583(10) Uani 1 1 d . . . H6 H 0.1106 1.2095 0.0972 0.087 Uiso 0.50 1 calc PR . . O7 O 0.0921(6) 0.8663(8) -0.0083(4) 0.171(4) Uani 1 1 d . . . H7 H 0.0737 0.8306 0.0269 0.257 Uiso 1 1 calc R . . O8 O 0.0670(3) 1.3295(5) -0.0167(3) 0.1075(19) Uani 1 1 d . . . H8 H 0.0320 1.2973 0.0075 0.161 Uiso 1 1 calc R . . C1 C 0.1577(3) 0.8846(5) 0.3551(3) 0.0424(10) Uani 1 1 d . . . C2 C 0.1807(2) 0.7793(4) 0.3057(2) 0.0385(10) Uani 1 1 d . . . C3 C 0.2515(3) 0.7151(6) 0.3106(3) 0.0525(13) Uani 1 1 d . . . H3A H 0.2881 0.7357 0.3458 0.063 Uiso 1 1 calc R . . C4 C 0.2668(4) 0.6208(6) 0.2628(3) 0.0628(18) Uani 1 1 d . . . H4A H 0.3140 0.5764 0.2653 0.075 Uiso 1 1 calc R . . C5 C 0.2115(3) 0.5919(5) 0.2106(3) 0.0550(14) Uani 1 1 d . . . H5A H 0.2207 0.5279 0.1778 0.066 Uiso 1 1 calc R . . C6 C 0.1417(3) 0.6610(4) 0.2085(3) 0.0386(10) Uani 1 1 d . . . C7 C 0.0784(3) 0.6399(4) 0.1540(3) 0.0424(11) Uani 1 1 d . . . C8 C 0.0000 1.3587(6) 0.2500 0.080(4) Uani 1 2 d S . . H8 H 0.0000 1.4460 0.2500 0.096 Uiso 1 2 calc SR . . C9 C 0.0414(4) 1.2963(4) 0.1979(3) 0.0531(13) Uani 1 1 d . . . H9A H 0.0691 1.3395 0.1627 0.064 Uiso 1 1 calc R . . C10 C 0.0402(2) 1.1672(4) 0.1998(2) 0.0324(8) Uani 1 1 d . . . C11 C 0.0841(3) 1.0838(4) 0.1484(2) 0.0366(9) Uani 1 1 d . . . C12 C 0.2280(5) 0.8573(8) 0.0405(4) 0.104(3) Uani 1 1 d . . . H12A H 0.2726 0.9093 0.0515 0.157 Uiso 1 1 calc R . . H12B H 0.2428 0.7958 0.0054 0.157 Uiso 1 1 calc R . . H12C H 0.2104 0.8157 0.0833 0.157 Uiso 1 1 calc R . . C13 C 0.1649(3) 0.9344(5) 0.0125(2) 0.0469(12) Uani 1 1 d . . . H13A H 0.1845 0.9790 -0.0292 0.056 Uiso 1 1 calc R . . H13B H 0.1512 0.9966 0.0483 0.056 Uiso 1 1 calc R . . C14 C 0.1089(5) 1.5393(9) -0.0842(5) 0.114(3) Uani 1 1 d D . . H14A H 0.0914 1.6229 -0.0950 0.171 Uiso 1 1 calc R . . H14B H 0.1169 1.4939 -0.1281 0.171 Uiso 1 1 calc R . . H14C H 0.1576 1.5431 -0.0581 0.171 Uiso 1 1 calc R . . C15 C 0.0429(5) 1.4686(8) -0.0364(5) 0.098(3) Uani 1 1 d D . . H15A H 0.0345 1.5157 0.0075 0.118 Uiso 1 1 calc R . . H15B H -0.0066 1.4673 -0.0626 0.118 Uiso 1 1 calc R . . N1 N 0.1275(2) 0.7527(3) 0.2555(2) 0.0356(8) Uani 1 1 d . . . N2 N 0.0000 1.1036(4) 0.2500 0.0317(10) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.0233(5) 0.02236(14) 0.0224(14) 0.00057(19) 0.0000(14) 0.0004(3) O1 0.060(2) 0.049(2) 0.076(3) -0.029(2) 0.006(2) 0.0087(18) O2 0.0336(16) 0.0398(17) 0.071(2) -0.0181(17) 0.0005(15) 0.0026(13) O3 0.046(2) 0.087(3) 0.054(2) -0.013(2) -0.0150(18) 0.004(2) O4 0.0365(16) 0.0391(17) 0.0487(18) -0.0023(14) -0.0024(14) 0.0013(13) O5 0.0385(16) 0.0295(15) 0.0452(17) -0.0019(13) 0.0106(14) 0.0019(12) O6 0.079(3) 0.047(2) 0.049(2) 0.0049(16) 0.032(2) -0.0022(18) O7 0.210(9) 0.175(9) 0.129(6) 0.009(5) 0.034(6) -0.046(7) O8 0.104(4) 0.078(4) 0.140(5) 0.015(4) -0.036(4) -0.005(3) C1 0.033(2) 0.048(3) 0.046(3) 0.010(2) -0.001(2) -0.0049(19) C2 0.030(2) 0.046(3) 0.040(2) 0.0105(19) 0.0047(18) 0.0028(18) C3 0.038(2) 0.071(4) 0.048(3) 0.014(3) -0.001(2) 0.016(2) C4 0.050(3) 0.081(4) 0.058(4) 0.021(3) 0.011(3) 0.035(3) C5 0.056(3) 0.053(3) 0.056(3) 0.008(3) 0.017(3) 0.026(3) C6 0.037(2) 0.033(2) 0.045(3) 0.0072(19) 0.011(2) 0.0080(18) C7 0.046(3) 0.026(2) 0.055(3) -0.0017(19) 0.014(2) -0.0021(18) C8 0.142(10) 0.017(3) 0.080(6) 0.000 0.050(6) 0.000 C9 0.080(4) 0.030(2) 0.049(3) 0.006(2) 0.024(3) -0.004(2) C10 0.036(2) 0.030(2) 0.031(2) 0.0009(16) 0.0064(17) -0.0020(17) C11 0.035(2) 0.038(2) 0.037(2) -0.0006(18) 0.0066(18) -0.0041(18) C12 0.132(8) 0.122(7) 0.059(4) 0.011(4) 0.023(5) 0.040(6) C13 0.062(3) 0.051(3) 0.028(2) -0.006(2) 0.012(2) -0.001(2) C14 0.117(7) 0.137(8) 0.089(6) 0.018(6) 0.032(5) 0.050(6) C15 0.093(6) 0.094(6) 0.108(6) -0.032(5) -0.019(5) 0.006(5) N1 0.0292(17) 0.0312(17) 0.046(2) 0.0060(16) 0.0086(16) 0.0036(13) N2 0.032(2) 0.026(2) 0.037(2) 0.000 0.004(2) 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 Dy1 0.257(9) 3 ? Dy1 O2 2.331(5) 3 ? Dy1 O4 2.334(8) . ? Dy1 O5 2.343(8) 3 ? Dy1 N1 2.477(9) . ? Dy1 O5 2.487(7) . ? Dy1 N2 2.495(5) . ? Dy1 O2 2.498(5) . ? Dy1 N1 2.525(9) 3 ? Dy1 O4 2.543(7) 3 ? O1 C7 1.232(6) . ? O1 H1 0.8200 . ? O2 C7 1.269(5) . ? O2 Dy1 2.331(5) 3 ? O3 C1 1.244(6) . ? O4 C1 1.258(5) . ? O4 Dy1 2.543(7) 3 ? O5 C11 1.256(5) . ? O5 Dy1 2.343(8) 3 ? O6 C11 1.245(5) . ? O6 H6 0.8200 . ? O7 C13 1.483(10) . ? O7 H7 0.8200 . ? O8 C15 1.581(10) . ? O8 H8 0.8200 . ? C1 C2 1.503(7) . ? C2 N1 1.331(6) . ? C2 C3 1.384(6) . ? C3 C4 1.369(8) . ? C3 H3A 0.9300 . ? C4 C5 1.386(9) . ? C4 H4A 0.9300 . ? C5 C6 1.394(6) . ? C5 H5A 0.9300 . ? C6 N1 1.334(6) . ? C6 C7 1.496(7) . ? C8 C9 1.370(6) 3 ? C8 C9 1.370(6) . ? C8 H8 0.9300 . ? C9 C10 1.376(6) . ? C9 H9A 0.9300 . ? C10 N2 1.341(5) . ? C10 C11 1.505(6) . ? C12 C13 1.446(9) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.618(10) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? N1 Dy1 2.525(9) 3 ? N2 C10 1.341(5) 3 ? N2 Dy1 2.495(5) 3 ? 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 Dy1 Dy1 O2 128.2(14) 3 3 ? Dy1 Dy1 O4 143(4) 3 . ? O2 Dy1 O4 81.8(2) 3 . ? Dy1 Dy1 O5 122(4) 3 3 ? O2 Dy1 O5 80.8(2) 3 3 ? O4 Dy1 O5 80.43(16) . 3 ? Dy1 Dy1 N1 98(4) 3 . ? O2 Dy1 N1 75.06(18) 3 . ? O4 Dy1 N1 65.7(3) . . ? O5 Dy1 N1 140.6(3) 3 . ? Dy1 Dy1 O5 53(4) 3 . ? O2 Dy1 O5 148.1(4) 3 . ? O4 Dy1 O5 89.2(3) . . ? O5 Dy1 O5 127.84(14) 3 . ? N1 Dy1 O5 73.4(3) . . ? Dy1 Dy1 N2 87.05(10) 3 . ? O2 Dy1 N2 141.2(2) 3 . ? O4 Dy1 N2 75.22(14) . . ? O5 Dy1 N2 64.97(12) 3 . ? N1 Dy1 N2 120.7(4) . . ? O5 Dy1 N2 62.96(12) . . ? Dy1 Dy1 O2 47.1(13) 3 . ? O2 Dy1 O2 87.21(19) 3 . ? O4 Dy1 O2 129.0(4) . . ? O5 Dy1 O2 146.3(4) 3 . ? N1 Dy1 O2 63.31(18) . . ? O5 Dy1 O2 74.9(2) . . ? N2 Dy1 O2 131.5(2) . . ? Dy1 Dy1 N1 76(4) 3 3 ? O2 Dy1 N1 64.9(2) 3 3 ? O4 Dy1 N1 141.0(3) . 3 ? O5 Dy1 N1 75.0(3) 3 3 ? N1 Dy1 N1 119.80(16) . 3 ? O5 Dy1 N1 129.8(2) . 3 ? N2 Dy1 N1 118.8(3) . 3 ? O2 Dy1 N1 71.41(17) . 3 ? Dy1 Dy1 O4 34(4) 3 3 ? O2 Dy1 O4 127.0(4) 3 3 ? O4 Dy1 O4 146.81(15) . 3 ? O5 Dy1 O4 87.7(3) 3 3 ? N1 Dy1 O4 131.7(2) . 3 ? O5 Dy1 O4 73.79(15) . 3 ? N2 Dy1 O4 71.68(13) . 3 ? O2 Dy1 O4 74.56(17) . 3 ? N1 Dy1 O4 62.1(2) 3 3 ? C7 O1 H1 109.5 . . ? C7 O2 Dy1 126.9(4) . 3 ? C7 O2 Dy1 123.9(4) . . ? Dy1 O2 Dy1 4.6(2) 3 . ? C1 O4 Dy1 125.2(3) . . ? C1 O4 Dy1 124.1(3) . 3 ? Dy1 O4 Dy1 3.5(3) . 3 ? C11 O5 Dy1 124.9(3) . 3 ? C11 O5 Dy1 124.1(3) . . ? Dy1 O5 Dy1 5.0(3) 3 . ? C11 O6 H6 109.5 . . ? C13 O7 H7 109.5 . . ? C15 O8 H8 109.5 . . ? O3 C1 O4 125.8(5) . . ? O3 C1 C2 117.9(4) . . ? O4 C1 C2 116.3(4) . . ? N1 C2 C3 121.9(5) . . ? N1 C2 C1 114.5(4) . . ? C3 C2 C1 123.6(4) . . ? C4 C3 C2 119.0(5) . . ? C4 C3 H3A 120.5 . . ? C2 C3 H3A 120.5 . . ? C3 C4 C5 119.5(5) . . ? C3 C4 H4A 120.2 . . ? C5 C4 H4A 120.2 . . ? C4 C5 C6 118.4(5) . . ? C4 C5 H5A 120.8 . . ? C6 C5 H5A 120.8 . . ? N1 C6 C5 121.4(5) . . ? N1 C6 C7 115.4(4) . . ? C5 C6 C7 123.2(5) . . ? O1 C7 O2 126.7(5) . . ? O1 C7 C6 118.0(4) . . ? O2 C7 C6 115.3(4) . . ? C9 C8 C9 122.0(6) 3 . ? C9 C8 H8 119.0 3 . ? C9 C8 H8 119.0 . . ? C8 C9 C10 117.3(5) . . ? C8 C9 H9A 121.3 . . ? C10 C9 H9A 121.3 . . ? N2 C10 C9 122.0(4) . . ? N2 C10 C11 113.5(4) . . ? C9 C10 C11 124.5(4) . . ? O6 C11 O5 125.4(4) . . ? O6 C11 C10 118.4(4) . . ? O5 C11 C10 116.2(4) . . ? C13 C12 H12A 109.5 . . ? C13 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C13 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C12 C13 O7 115.6(7) . . ? C12 C13 H13A 108.4 . . ? O7 C13 H13A 108.4 . . ? C12 C13 H13B 108.4 . . ? O7 C13 H13B 108.4 . . ? H13A C13 H13B 107.4 . . ? C15 C14 H14A 109.5 . . ? C15 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C15 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O8 C15 C14 112.7(6) . . ? O8 C15 H15A 109.0 . . ? C14 C15 H15A 109.0 . . ? O8 C15 H15B 109.0 . . ? C14 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? C2 N1 C6 119.8(4) . . ? C2 N1 Dy1 118.1(3) . . ? C6 N1 Dy1 122.0(3) . . ? C2 N1 Dy1 123.0(3) . 3 ? C6 N1 Dy1 117.2(3) . 3 ? Dy1 N1 Dy1 5.78(19) . 3 ? C10 N2 C10 119.3(5) 3 . ? C10 N2 Dy1 122.4(3) 3 3 ? C10 N2 Dy1 118.3(3) . 3 ? C10 N2 Dy1 118.3(3) 3 . ? C10 N2 Dy1 122.4(3) . . ? Dy1 N2 Dy1 5.9(2) 3 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.562 _refine_diff_density_min -0.739 _refine_diff_density_rms 0.103