# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email ecolacio@ugr.es _publ_contact_author_name 'Colacio, E.' _publ_author_name E.Colacio data_Compound1 _database_code_depnum_ccdc_archive 'CCDC 870818' #TrackingRef '- Compound1R.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H47 Dy N6 O15' _chemical_formula_weight 858.21 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7795(10) _cell_length_b 12.3752(13) _cell_length_c 15.1260(16) _cell_angle_alpha 76.3780(10) _cell_angle_beta 86.1800(10) _cell_angle_gamma 81.4960(10) _cell_volume 1758.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3870 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 22.07 _exptl_crystal_description Prismatic _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.621 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 874 _exptl_absorpt_coefficient_mu 2.200 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.619 _exptl_absorpt_correction_T_max 0.746 _exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Axs APEX automatic diffractometer' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17428 _diffrn_reflns_av_R_equivalents 0.0485 _diffrn_reflns_av_sigmaI/netI 0.0588 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6175 _reflns_number_gt 5368 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker smart' _computing_cell_refinement 'Bruker smart' _computing_data_reduction 'Bruker smart' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. Isotropic thermal parameters of all H atoms fixed to 1.2 times the equivalent isotropic thermal parameter of their parent atoms. We have used the command "HFIX 13 -1.20 N1A N3A". ; _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^)+(0.0422P)^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 6175 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0464 _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.0861 _refine_ls_wR_factor_gt 0.0817 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 0.20105(2) 0.183393(18) 0.216099(14) 0.02183(9) Uani 1 1 d . . . C1A C -0.0592(4) 0.3736(4) 0.2008(3) 0.0212(10) Uani 1 1 d . . . C1M C 0.5598(6) 0.4714(6) 0.3188(4) 0.0548(17) Uani 1 1 d . . . H1M1 H 0.5583 0.5269 0.2625 0.082 Uiso 1 1 d R . . H1M2 H 0.5348 0.4034 0.3084 0.082 Uiso 1 1 d R . . H1M3 H 0.6510 0.4573 0.3424 0.082 Uiso 1 1 d R . . C2A C 0.0136(5) 0.4194(4) 0.2557(3) 0.0249(11) Uani 1 1 d . . . C2M C 0.4612(6) 0.2437(4) 0.5407(4) 0.0473(15) Uani 1 1 d . . . H2M1 H 0.5588 0.2360 0.5265 0.071 Uiso 1 1 d R . . H2M2 H 0.4152 0.2133 0.4998 0.071 Uiso 1 1 d R . . H2M3 H 0.4446 0.2039 0.6022 0.071 Uiso 1 1 d R . . C3A C -0.0213(5) 0.5273(4) 0.2661(3) 0.0279(11) Uani 1 1 d . . . H3A H 0.0280 0.5543 0.3047 0.033 Uiso 1 1 calc R . . C4A C -0.1311(5) 0.5963(4) 0.2184(3) 0.0329(12) Uani 1 1 d . . . C5A C -0.2003(5) 0.5541(4) 0.1602(3) 0.0314(12) Uani 1 1 d . . . H5A H -0.2715 0.6004 0.1265 0.038 Uiso 1 1 calc R . . C6A C -0.1659(5) 0.4431(4) 0.1506(3) 0.0263(11) Uani 1 1 d . . . C7A C -0.2496(5) 0.3981(4) 0.0905(3) 0.0355(13) Uani 1 1 d . . . H7A1 H -0.2951 0.4602 0.0458 0.043 Uiso 1 1 calc R . . H7A2 H -0.3206 0.3596 0.1273 0.043 Uiso 1 1 calc R . . C8A C -0.2410(7) 0.2599(5) -0.0090(4) 0.0542(17) Uani 1 1 d . . . H8A1 H -0.3066 0.3154 -0.0466 0.065 Uiso 1 1 calc R . . H8A2 H -0.1781 0.2238 -0.0490 0.065 Uiso 1 1 calc R . . C9A C -0.3150(6) 0.1768(6) 0.0505(4) 0.0528(17) Uani 1 1 d . . . H9A1 H -0.3462 0.1303 0.0147 0.063 Uiso 1 1 calc R . . H9A2 H -0.3963 0.2150 0.0762 0.063 Uiso 1 1 calc R . . C10A C -0.3232(5) 0.0449(4) 0.1954(3) 0.0304(12) Uani 1 1 d . . . H10A H -0.3556 -0.0137 0.1728 0.036 Uiso 1 1 calc R . . H10B H -0.4032 0.0978 0.2052 0.036 Uiso 1 1 calc R . . C11A C -0.2550(5) -0.0068(4) 0.2852(3) 0.0251(11) Uani 1 1 d . . . H11A H -0.3254 -0.0295 0.3314 0.030 Uiso 1 1 calc R . . H11B H -0.1923 -0.0735 0.2796 0.030 Uiso 1 1 calc R . . C12A C -0.0891(5) 0.0149(4) 0.3963(3) 0.0266(11) Uani 1 1 d . . . H12A H -0.0385 0.0692 0.4119 0.032 Uiso 1 1 calc R . . H12B H -0.1494 -0.0115 0.4480 0.032 Uiso 1 1 calc R . . C13A C 0.0118(5) -0.0825(4) 0.3790(3) 0.0243(11) Uani 1 1 d . . . C14A C 0.0240(5) -0.1873(4) 0.4396(3) 0.0226(10) Uani 1 1 d . . . H14A H -0.0365 -0.1992 0.4900 0.027 Uiso 1 1 calc R . . C15A C 0.1243(5) -0.2740(4) 0.4264(3) 0.0252(11) Uani 1 1 d . . . C16A C 0.2107(5) -0.2556(4) 0.3484(3) 0.0243(11) Uani 1 1 d . . . H16A H 0.2776 -0.3133 0.3379 0.029 Uiso 1 1 calc R . . C17A C 0.1982(5) -0.1529(4) 0.2867(3) 0.0237(11) Uani 1 1 d . . . C18A C 0.1012(4) -0.0618(4) 0.3020(3) 0.0218(10) Uani 1 1 d . . . C19A C -0.1709(6) 0.7147(4) 0.2315(4) 0.0491(16) Uani 1 1 d . . . H19A H -0.2150 0.7611 0.1783 0.074 Uiso 1 1 d R . . H19B H -0.0892 0.7442 0.2414 0.074 Uiso 1 1 d R . . H19C H -0.2333 0.7135 0.2834 0.074 Uiso 1 1 d R . . C20A C 0.1417(6) -0.3853(4) 0.4937(3) 0.0358(13) Uani 1 1 d . . . H20A H 0.1224 -0.3741 0.5543 0.054 Uiso 1 1 d R . . H20B H 0.2349 -0.4209 0.4891 0.054 Uiso 1 1 d R . . H20C H 0.0790 -0.4320 0.4807 0.054 Uiso 1 1 d R . . C21A C 0.2052(5) 0.3829(4) 0.3569(3) 0.0315(12) Uani 1 1 d . . . H21A H 0.2458 0.4468 0.3228 0.047 Uiso 1 1 d R . . H21B H 0.2770 0.3242 0.3814 0.047 Uiso 1 1 d R . . H21C H 0.1475 0.4036 0.4058 0.047 Uiso 1 1 d R . . C31A C -0.0559(6) 0.3729(4) -0.0209(3) 0.0399(14) Uani 1 1 d . . . H31A H -0.0051 0.3197 -0.0520 0.060 Uiso 1 1 d R . . H31B H 0.0064 0.3998 0.0127 0.060 Uiso 1 1 d R . . H31C H -0.1011 0.4346 -0.0647 0.060 Uiso 1 1 d R . . C32A C -0.1241(6) 0.0236(5) 0.0950(4) 0.0477(16) Uani 1 1 d . . . H32A H -0.0744 -0.0211 0.1466 0.072 Uiso 1 1 d R . . H32B H -0.0613 0.0634 0.0522 0.072 Uiso 1 1 d R . . H32C H -0.1663 -0.0241 0.0663 0.072 Uiso 1 1 d R . . C33A C -0.2680(5) 0.1716(4) 0.3353(3) 0.0290(11) Uani 1 1 d . . . H33A H -0.3190 0.2102 0.2824 0.043 Uiso 1 1 d R . . H33B H -0.2126 0.2213 0.3518 0.043 Uiso 1 1 d R . . H33C H -0.3312 0.1470 0.3849 0.043 Uiso 1 1 d R . . C41A C 0.4014(5) -0.2020(5) 0.2006(4) 0.0403(14) Uani 1 1 d . . . H41A H 0.4569 -0.2103 0.2525 0.060 Uiso 1 1 d R . . H41B H 0.4526 -0.1724 0.1461 0.060 Uiso 1 1 d R . . H41C H 0.3775 -0.2736 0.1981 0.060 Uiso 1 1 d R . . N1B N 0.3303(4) 0.0527(3) 0.3823(3) 0.0267(9) Uani 1 1 d . . . N1C N 0.2948(4) 0.1453(3) 0.0415(3) 0.0290(10) Uani 1 1 d . . . N1D N 0.3553(4) 0.3725(4) 0.1473(3) 0.0287(10) Uani 1 1 d . . . N1A N -0.1606(4) 0.3178(3) 0.0419(3) 0.0369(11) Uani 1 1 d . . . H1A H -0.1140 0.2637 0.0852 0.044 Uiso 1 1 calc R . . N3A N -0.1768(4) 0.0722(3) 0.3148(2) 0.0220(9) Uani 1 1 d . . . H3A1 H -0.1182 0.0981 0.2678 0.026 Uiso 1 1 calc R . . N2A N -0.2311(4) 0.1026(4) 0.1268(3) 0.0336(10) Uani 1 1 d . . . O1A O -0.0208(3) 0.2659(2) 0.1954(2) 0.0221(7) Uani 1 1 d . . . O1M O 0.4689(4) 0.5125(3) 0.3823(3) 0.0432(9) Uani 1 1 d . . . H1M H 0.5016 0.5491 0.4184 0.052 Uiso 1 1 d R . . O2A O 0.1238(3) 0.3441(3) 0.2979(2) 0.0243(7) Uani 1 1 d . . . O2B O 0.2230(3) 0.1266(3) 0.3820(2) 0.0290(8) Uani 1 1 d . . . O2C O 0.1679(3) 0.1706(3) 0.0564(2) 0.0267(7) Uani 1 1 d . . . O2D O 0.2454(3) 0.3631(3) 0.1113(2) 0.0268(7) Uani 1 1 d . . . O2M O 0.4078(4) 0.3576(3) 0.5336(3) 0.0485(10) Uani 1 1 d . . . H2M H 0.4506 0.4008 0.4775 0.058 Uiso 1 1 d R . . O3A O 0.0910(3) 0.0387(2) 0.2458(2) 0.0242(7) Uani 1 1 d . . . O3B O 0.3846(3) 0.0464(3) 0.3055(2) 0.0308(8) Uani 1 1 d . . . O3C O 0.3726(3) 0.1277(3) 0.1094(2) 0.0305(8) Uani 1 1 d . . . O3D O 0.3995(3) 0.2924(3) 0.2132(2) 0.0276(8) Uani 1 1 d . . . O4A O 0.2787(3) -0.1276(3) 0.2075(2) 0.0304(8) Uani 1 1 d . . . O4B O 0.3757(4) -0.0074(3) 0.4531(2) 0.0401(9) Uani 1 1 d . . . O4C O 0.3440(4) 0.1381(3) -0.0338(2) 0.0431(10) Uani 1 1 d . . . O4D O 0.4166(4) 0.4537(3) 0.1197(3) 0.0443(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.02048(13) 0.02090(14) 0.02233(14) -0.00144(9) -0.00507(9) -0.00082(9) C1A 0.021(2) 0.021(3) 0.019(2) -0.002(2) 0.0000(19) -0.001(2) C1M 0.044(4) 0.069(5) 0.057(4) -0.028(4) 0.003(3) -0.005(3) C2A 0.023(3) 0.022(3) 0.028(3) -0.002(2) -0.003(2) 0.001(2) C2M 0.066(4) 0.029(3) 0.049(4) -0.012(3) -0.017(3) 0.002(3) C3A 0.034(3) 0.024(3) 0.024(3) -0.006(2) -0.002(2) 0.001(2) C4A 0.039(3) 0.025(3) 0.029(3) -0.001(2) 0.001(2) 0.004(2) C5A 0.027(3) 0.030(3) 0.030(3) 0.000(2) -0.007(2) 0.011(2) C6A 0.022(3) 0.026(3) 0.028(3) -0.001(2) -0.001(2) -0.002(2) C7A 0.025(3) 0.041(3) 0.034(3) 0.005(3) -0.008(2) -0.004(2) C8A 0.059(4) 0.055(4) 0.053(4) -0.013(3) -0.030(3) -0.008(3) C9A 0.052(4) 0.082(5) 0.026(3) 0.004(3) -0.015(3) -0.035(4) C10A 0.030(3) 0.027(3) 0.033(3) 0.002(2) -0.009(2) -0.012(2) C11A 0.025(3) 0.022(3) 0.026(3) -0.002(2) -0.007(2) -0.002(2) C12A 0.035(3) 0.026(3) 0.018(2) -0.007(2) -0.009(2) 0.005(2) C13A 0.028(3) 0.019(3) 0.027(3) -0.008(2) -0.004(2) 0.000(2) C14A 0.026(3) 0.021(3) 0.020(2) -0.005(2) -0.0024(19) -0.002(2) C15A 0.030(3) 0.023(3) 0.023(3) -0.004(2) -0.010(2) -0.001(2) C16A 0.024(3) 0.023(3) 0.027(3) -0.009(2) -0.005(2) 0.000(2) C17A 0.020(2) 0.031(3) 0.021(3) -0.005(2) -0.0047(19) -0.006(2) C18A 0.018(2) 0.025(3) 0.022(3) -0.006(2) -0.0053(19) -0.001(2) C19A 0.062(4) 0.029(3) 0.053(4) -0.013(3) -0.013(3) 0.015(3) C20A 0.044(3) 0.025(3) 0.033(3) 0.000(2) 0.002(2) 0.001(2) C21A 0.027(3) 0.037(3) 0.033(3) -0.014(2) -0.013(2) -0.001(2) C31A 0.059(4) 0.030(3) 0.024(3) 0.001(2) -0.004(3) 0.004(3) C32A 0.050(4) 0.065(4) 0.044(4) -0.029(3) 0.013(3) -0.038(3) C33A 0.031(3) 0.019(3) 0.032(3) -0.001(2) -0.003(2) 0.007(2) C41A 0.030(3) 0.060(4) 0.030(3) -0.015(3) 0.002(2) 0.003(3) N1B 0.024(2) 0.027(2) 0.029(2) -0.0044(19) -0.0098(18) -0.0014(18) N1C 0.030(2) 0.032(2) 0.027(2) -0.0078(19) -0.0027(19) -0.0037(19) N1D 0.023(2) 0.035(3) 0.028(2) -0.006(2) -0.0018(18) -0.005(2) N1A 0.047(3) 0.023(2) 0.043(3) -0.007(2) -0.031(2) 0.002(2) N3A 0.023(2) 0.021(2) 0.020(2) -0.0031(17) -0.0011(16) 0.0012(17) N2A 0.036(3) 0.040(3) 0.027(2) -0.004(2) -0.0058(19) -0.018(2) O1A 0.0192(16) 0.0200(17) 0.0265(18) -0.0030(14) -0.0066(13) -0.0024(13) O1M 0.043(2) 0.044(2) 0.047(2) -0.0209(19) -0.0092(18) 0.0014(18) O2A 0.0224(17) 0.0229(17) 0.0289(18) -0.0086(14) -0.0101(14) 0.0013(14) O2B 0.0281(19) 0.0274(19) 0.0287(19) -0.0045(15) -0.0051(15) 0.0042(15) O2C 0.0187(18) 0.034(2) 0.0262(18) -0.0051(15) -0.0032(14) -0.0006(15) O2D 0.0224(18) 0.0270(19) 0.0301(19) -0.0025(15) -0.0062(14) -0.0051(14) O2M 0.056(3) 0.027(2) 0.062(3) -0.0075(19) -0.008(2) -0.0040(19) O3A 0.0266(18) 0.0176(17) 0.0252(18) 0.0024(14) -0.0064(14) -0.0023(14) O3B 0.0289(19) 0.033(2) 0.027(2) -0.0066(16) -0.0031(15) 0.0046(15) O3C 0.0231(18) 0.041(2) 0.0272(19) -0.0089(16) -0.0095(15) 0.0033(15) O3D 0.0265(18) 0.0290(19) 0.0241(18) 0.0008(15) -0.0069(14) -0.0014(15) O4A 0.0274(19) 0.031(2) 0.0280(19) -0.0028(16) 0.0042(15) 0.0023(15) O4B 0.043(2) 0.043(2) 0.026(2) 0.0036(17) -0.0165(17) 0.0067(18) O4C 0.041(2) 0.067(3) 0.027(2) -0.0202(19) 0.0022(17) -0.011(2) O4D 0.040(2) 0.040(2) 0.049(2) 0.0066(19) -0.0065(18) -0.0208(19) _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 O3A 2.166(3) . ? Dy1 O1A 2.265(3) . ? Dy1 O3C 2.391(3) . ? Dy1 O2B 2.456(3) . ? Dy1 O2D 2.486(3) . ? Dy1 O2C 2.503(3) . ? Dy1 O3B 2.504(3) . ? Dy1 O3D 2.514(3) . ? Dy1 O2A 2.579(3) . ? Dy1 N1C 2.859(4) . ? Dy1 N1B 2.905(4) . ? Dy1 N1D 2.919(4) . ? C1A O1A 1.351(5) . ? C1A C6A 1.391(6) . ? C1A C2A 1.392(6) . ? C1M O1M 1.397(6) . ? C2A C3A 1.371(6) . ? C2A O2A 1.396(5) . ? C2M O2M 1.410(6) . ? C3A C4A 1.394(7) . ? C4A C5A 1.379(7) . ? C4A C19A 1.515(7) . ? C5A C6A 1.405(7) . ? C6A C7A 1.510(7) . ? C7A N1A 1.512(6) . ? C8A C9A 1.445(8) . ? C8A N1A 1.494(6) . ? C9A N2A 1.501(7) . ? C10A N2A 1.454(6) . ? C10A C11A 1.512(6) . ? C11A N3A 1.487(6) . ? C12A C13A 1.502(6) . ? C12A N3A 1.519(5) . ? C13A C14A 1.396(6) . ? C13A C18A 1.406(6) . ? C14A C15A 1.384(6) . ? C15A C16A 1.399(6) . ? C15A C20A 1.502(6) . ? C16A C17A 1.383(6) . ? C17A O4A 1.386(5) . ? C17A C18A 1.414(6) . ? C18A O3A 1.325(5) . ? C21A O2A 1.439(5) . ? C31A N1A 1.479(6) . ? C32A N2A 1.462(7) . ? C33A N3A 1.491(5) . ? C41A O4A 1.415(6) . ? N1B O4B 1.220(5) . ? N1B O3B 1.260(5) . ? N1B O2B 1.285(5) . ? N1C O4C 1.224(5) . ? N1C O2C 1.253(5) . ? N1C O3C 1.277(5) . ? N1D O4D 1.221(5) . ? N1D O2D 1.269(5) . ? N1D O3D 1.276(5) . ? 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 O3A Dy1 O1A 78.53(11) . . ? O3A Dy1 O3C 99.54(11) . . ? O1A Dy1 O3C 130.29(11) . . ? O3A Dy1 O2B 80.21(11) . . ? O1A Dy1 O2B 104.81(10) . . ? O3C Dy1 O2B 124.02(10) . . ? O3A Dy1 O2D 148.64(11) . . ? O1A Dy1 O2D 81.28(10) . . ? O3C Dy1 O2D 75.88(11) . . ? O2B Dy1 O2D 128.46(11) . . ? O3A Dy1 O2C 81.26(11) . . ? O1A Dy1 O2C 78.95(10) . . ? O3C Dy1 O2C 52.11(10) . . ? O2B Dy1 O2C 159.89(11) . . ? O2D Dy1 O2C 71.46(10) . . ? O3A Dy1 O3B 82.45(11) . . ? O1A Dy1 O3B 152.18(11) . . ? O3C Dy1 O3B 72.74(10) . . ? O2B Dy1 O3B 51.56(10) . . ? O2D Dy1 O3B 123.82(10) . . ? O2C Dy1 O3B 118.03(10) . . ? O3A Dy1 O3D 157.42(11) . . ? O1A Dy1 O3D 123.02(10) . . ? O3C Dy1 O3D 72.43(11) . . ? O2B Dy1 O3D 86.96(10) . . ? O2D Dy1 O3D 51.38(10) . . ? O2C Dy1 O3D 107.82(10) . . ? O3B Dy1 O3D 75.03(10) . . ? O3A Dy1 O2A 119.27(11) . . ? O1A Dy1 O2A 64.46(10) . . ? O3C Dy1 O2A 141.17(11) . . ? O2B Dy1 O2A 66.28(10) . . ? O2D Dy1 O2A 71.50(10) . . ? O2C Dy1 O2A 130.83(10) . . ? O3B Dy1 O2A 109.16(10) . . ? O3D Dy1 O2A 70.94(10) . . ? O3A Dy1 N1C 92.02(11) . . ? O1A Dy1 N1C 104.22(11) . . ? O3C Dy1 N1C 26.26(10) . . ? O2B Dy1 N1C 147.70(11) . . ? O2D Dy1 N1C 70.02(11) . . ? O2C Dy1 N1C 25.96(10) . . ? O3B Dy1 N1C 96.50(11) . . ? O3D Dy1 N1C 88.97(11) . . ? O2A Dy1 N1C 141.15(11) . . ? O3A Dy1 N1B 78.87(11) . . ? O1A Dy1 N1B 128.94(11) . . ? O3C Dy1 N1B 98.30(11) . . ? O2B Dy1 N1B 26.06(10) . . ? O2D Dy1 N1B 132.35(10) . . ? O2C Dy1 N1B 140.50(11) . . ? O3B Dy1 N1B 25.59(10) . . ? O3D Dy1 N1B 81.45(10) . . ? O2A Dy1 N1B 88.66(10) . . ? N1C Dy1 N1B 121.74(11) . . ? O3A Dy1 N1D 171.04(11) . . ? O1A Dy1 N1D 102.09(11) . . ? O3C Dy1 N1D 73.13(11) . . ? O2B Dy1 N1D 108.06(11) . . ? O2D Dy1 N1D 25.59(10) . . ? O2C Dy1 N1D 90.06(11) . . ? O3B Dy1 N1D 99.86(11) . . ? O3D Dy1 N1D 25.81(10) . . ? O2A Dy1 N1D 68.31(10) . . ? N1C Dy1 N1D 79.14(11) . . ? N1B Dy1 N1D 106.94(11) . . ? O1A C1A C6A 122.7(4) . . ? O1A C1A C2A 119.2(4) . . ? C6A C1A C2A 118.0(4) . . ? C3A C2A C1A 122.5(4) . . ? C3A C2A O2A 124.6(4) . . ? C1A C2A O2A 112.9(4) . . ? C2A C3A C4A 119.8(5) . . ? C5A C4A C3A 118.6(4) . . ? C5A C4A C19A 121.9(5) . . ? C3A C4A C19A 119.5(5) . . ? C4A C5A C6A 121.7(4) . . ? C1A C6A C5A 119.3(4) . . ? C1A C6A C7A 120.5(4) . . ? C5A C6A C7A 120.0(4) . . ? C6A C7A N1A 112.0(4) . . ? C9A C8A N1A 112.7(5) . . ? C8A C9A N2A 114.0(5) . . ? N2A C10A C11A 113.1(4) . . ? N3A C11A C10A 112.2(4) . . ? C13A C12A N3A 112.8(4) . . ? C14A C13A C18A 120.8(4) . . ? C14A C13A C12A 121.9(4) . . ? C18A C13A C12A 117.2(4) . . ? C15A C14A C13A 121.4(4) . . ? C14A C15A C16A 118.3(4) . . ? C14A C15A C20A 121.5(4) . . ? C16A C15A C20A 120.2(4) . . ? C17A C16A C15A 121.0(4) . . ? C16A C17A O4A 124.8(4) . . ? C16A C17A C18A 121.2(4) . . ? O4A C17A C18A 114.0(4) . . ? O3A C18A C13A 120.4(4) . . ? O3A C18A C17A 122.4(4) . . ? C13A C18A C17A 117.2(4) . . ? O4B N1B O3B 122.6(4) . . ? O4B N1B O2B 121.5(4) . . ? O3B N1B O2B 115.9(4) . . ? O4B N1B Dy1 174.7(3) . . ? O3B N1B Dy1 59.1(2) . . ? O2B N1B Dy1 57.1(2) . . ? O4C N1C O2C 122.8(4) . . ? O4C N1C O3C 120.7(4) . . ? O2C N1C O3C 116.5(4) . . ? O4C N1C Dy1 172.9(3) . . ? O2C N1C Dy1 60.9(2) . . ? O3C N1C Dy1 56.0(2) . . ? O4D N1D O2D 121.6(4) . . ? O4D N1D O3D 121.5(4) . . ? O2D N1D O3D 116.8(4) . . ? O4D N1D Dy1 178.0(3) . . ? O2D N1D Dy1 57.8(2) . . ? O3D N1D Dy1 59.1(2) . . ? C31A N1A C8A 108.9(4) . . ? C31A N1A C7A 112.3(4) . . ? C8A N1A C7A 113.9(4) . . ? C11A N3A C33A 112.8(4) . . ? C11A N3A C12A 112.2(3) . . ? C33A N3A C12A 109.5(3) . . ? C10A N2A C32A 111.6(4) . . ? C10A N2A C9A 109.2(4) . . ? C32A N2A C9A 112.3(4) . . ? C1A O1A Dy1 121.2(3) . . ? C2A O2A C21A 117.3(3) . . ? C2A O2A Dy1 112.4(2) . . ? C21A O2A Dy1 126.7(3) . . ? N1B O2B Dy1 96.9(2) . . ? N1C O2C Dy1 93.1(2) . . ? N1D O2D Dy1 96.6(3) . . ? C18A O3A Dy1 137.8(3) . . ? N1B O3B Dy1 95.3(2) . . ? N1C O3C Dy1 97.8(2) . . ? N1D O3D Dy1 95.1(2) . . ? C17A O4A C41A 116.7(4) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.212 _refine_diff_density_min -0.535 _refine_diff_density_rms 0.115 # Attachment '- compound1.cif' data_Dy_Y _database_code_depnum_ccdc_archive 'CCDC 883706' #TrackingRef '- compound1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H47 Dy0.11 N6 O15 Y0.89' _chemical_formula_weight 792.71 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' Y Y -2.7962 3.5667 '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 9.7740(18) _cell_length_b 12.368(2) _cell_length_c 15.119(3) _cell_angle_alpha 76.302(3) _cell_angle_beta 86.088(3) _cell_angle_gamma 81.445(3) _cell_volume 1754.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4433 _cell_measurement_theta_min 2.438 _cell_measurement_theta_max 23.865 _exptl_crystal_description Prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.500 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 826 _exptl_absorpt_coefficient_mu 1.789 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.859188 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Axs APEX automatic diffractometer' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17475 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_av_sigmaI/netI 0.0507 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6161 _reflns_number_gt 5281 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker smart' _computing_cell_refinement 'Bruker smart' _computing_data_reduction 'Bruker smart' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. Isotropic thermal parameters of all H atoms fixed to 1.2 times the equivalent isotropic thermal parameter of their parent atoms. We have used EADP for Dy1 and Y1 atoms to fix thermal parameters. We have used EXYZ for Dy1 and Y1 atoms to fix x, y and z values of these atoms. We have fixed the occupancy factors to 0.11 and 0.89 for Dy1 and Y1, respectively, according to magnetic properties We have used the command "HFIX 13 -1.20 N1A N3A". ; _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^)+(0.0607P)^2^+1.7022P] 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 6161 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0559 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.1188 _refine_ls_wR_factor_gt 0.1121 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 0.20110(3) 0.18340(3) 0.21644(2) 0.02226(12) Uani 0.11 1 d P . . Y1 Y 0.20110(3) 0.18340(3) 0.21644(2) 0.02226(12) Uani 0.89 1 d P . . C1A C -0.0588(4) 0.3731(3) 0.2009(2) 0.0199(8) Uani 1 1 d . . . C1M C 0.5593(5) 0.4708(5) 0.3200(3) 0.0523(13) Uani 1 1 d . . . H1M1 H 0.5584 0.5267 0.2638 0.078 Uiso 1 1 d R . . H1M2 H 0.5305 0.4040 0.3097 0.078 Uiso 1 1 d R . . H1M3 H 0.6513 0.4535 0.3427 0.078 Uiso 1 1 d R . . C2A C 0.0142(4) 0.4190(3) 0.2560(2) 0.0204(8) Uani 1 1 d . . . C2M C 0.4654(5) 0.2430(3) 0.5396(3) 0.0422(11) Uani 1 1 d . . . H2M1 H 0.5630 0.2386 0.5252 0.063 Uiso 1 1 d R . . H2M2 H 0.4214 0.2135 0.4974 0.063 Uiso 1 1 d R . . H2M3 H 0.4505 0.2000 0.6004 0.063 Uiso 1 1 d R . . C3A C -0.0223(4) 0.5274(3) 0.2674(2) 0.0260(9) Uani 1 1 d . . . H3A H 0.0261 0.5547 0.3064 0.031 Uiso 1 1 calc R . . C4A C -0.1332(4) 0.5954(3) 0.2193(3) 0.0290(9) Uani 1 1 d . . . C5A C -0.2003(4) 0.5536(3) 0.1604(3) 0.0292(9) Uani 1 1 d . . . H5A H -0.2707 0.6003 0.1261 0.035 Uiso 1 1 calc R . . C6A C -0.1663(4) 0.4429(3) 0.1505(3) 0.0248(8) Uani 1 1 d . . . C7A C -0.2488(4) 0.3967(3) 0.0904(3) 0.0329(10) Uani 1 1 d . . . H7A1 H -0.2957 0.4587 0.0460 0.039 Uiso 1 1 calc R . . H7A2 H -0.3190 0.3573 0.1275 0.039 Uiso 1 1 calc R . . C8A C -0.2386(5) 0.2591(4) -0.0104(3) 0.0426(11) Uani 1 1 d . . . H8A1 H -0.3025 0.3143 -0.0498 0.051 Uiso 1 1 calc R . . H8A2 H -0.1746 0.2208 -0.0486 0.051 Uiso 1 1 calc R . . C9A C -0.3165(5) 0.1769(4) 0.0515(3) 0.0439(12) Uani 1 1 d . . . H9A1 H -0.3508 0.1307 0.0166 0.053 Uiso 1 1 calc R . . H9A2 H -0.3958 0.2169 0.0778 0.053 Uiso 1 1 calc R . . C10A C -0.3230(4) 0.0446(3) 0.1955(3) 0.0259(8) Uani 1 1 d . . . H10A H -0.3552 -0.0143 0.1732 0.031 Uiso 1 1 calc R . . H10B H -0.4033 0.0973 0.2054 0.031 Uiso 1 1 calc R . . C11A C -0.2546(4) -0.0067(3) 0.2852(2) 0.0221(8) Uani 1 1 d . . . H11A H -0.3250 -0.0294 0.3315 0.026 Uiso 1 1 calc R . . H11B H -0.1921 -0.0736 0.2795 0.026 Uiso 1 1 calc R . . C12A C -0.0889(4) 0.0133(3) 0.3970(2) 0.0224(8) Uani 1 1 d . . . H12A H -0.0393 0.0673 0.4140 0.027 Uiso 1 1 calc R . . H12B H -0.1499 -0.0144 0.4480 0.027 Uiso 1 1 calc R . . C13A C 0.0133(3) -0.0831(3) 0.3788(2) 0.0176(7) Uani 1 1 d . . . C14A C 0.0252(4) -0.1879(3) 0.4398(2) 0.0202(8) Uani 1 1 d . . . H14A H -0.0354 -0.1996 0.4903 0.024 Uiso 1 1 calc R . . C15A C 0.1261(4) -0.2749(3) 0.4264(2) 0.0212(8) Uani 1 1 d . . . C16A C 0.2118(4) -0.2563(3) 0.3482(2) 0.0207(8) Uani 1 1 d . . . H16A H 0.2784 -0.3143 0.3375 0.025 Uiso 1 1 calc R . . C17A C 0.1999(4) -0.1535(3) 0.2861(2) 0.0189(7) Uani 1 1 d . . . C18A C 0.1019(4) -0.0632(3) 0.3021(2) 0.0187(8) Uani 1 1 d . . . C19A C -0.1746(5) 0.7139(3) 0.2336(3) 0.0427(11) Uani 1 1 d . . . H19A H -0.2253 0.7592 0.1825 0.064 Uiso 1 1 d R . . H19B H -0.0929 0.7460 0.2391 0.064 Uiso 1 1 d R . . H19C H -0.2315 0.7111 0.2881 0.064 Uiso 1 1 d R . . C20A C 0.1429(4) -0.3866(3) 0.4942(3) 0.0317(9) Uani 1 1 d . . . H20A H 0.1218 -0.3751 0.5545 0.048 Uiso 1 1 d R . . H20B H 0.2366 -0.4225 0.4907 0.048 Uiso 1 1 d R . . H20C H 0.0810 -0.4333 0.4805 0.048 Uiso 1 1 d R . . C21A C 0.2046(4) 0.3828(3) 0.3573(3) 0.0267(9) Uani 1 1 d . . . H21A H 0.2422 0.4487 0.3239 0.040 Uiso 1 1 d R . . H21B H 0.2789 0.3250 0.3805 0.040 Uiso 1 1 d R . . H21C H 0.1466 0.4007 0.4071 0.040 Uiso 1 1 d R . . C31A C -0.0551(5) 0.3730(3) -0.0215(3) 0.0355(10) Uani 1 1 d . . . H31A H -0.0018 0.3199 -0.0519 0.053 Uiso 1 1 d R . . H31B H 0.0052 0.4011 0.0126 0.053 Uiso 1 1 d R . . H31C H -0.1007 0.4342 -0.0658 0.053 Uiso 1 1 d R . . C32A C -0.1240(5) 0.0239(4) 0.0950(3) 0.0425(12) Uani 1 1 d . . . H32A H -0.0735 -0.0220 0.1460 0.064 Uiso 1 1 d R . . H32B H -0.0620 0.0649 0.0525 0.064 Uiso 1 1 d R . . H32C H -0.1659 -0.0231 0.0655 0.064 Uiso 1 1 d R . . C33A C -0.2673(4) 0.1713(3) 0.3355(3) 0.0257(8) Uani 1 1 d . . . H33A H -0.3161 0.2114 0.2819 0.039 Uiso 1 1 d R . . H33B H -0.2127 0.2199 0.3540 0.039 Uiso 1 1 d R . . H33C H -0.3327 0.1463 0.3836 0.039 Uiso 1 1 d R . . C41A C 0.4034(4) -0.2031(4) 0.2000(3) 0.0339(10) Uani 1 1 d . . . H41A H 0.4573 -0.2125 0.2528 0.051 Uiso 1 1 d R . . H41B H 0.4561 -0.1727 0.1463 0.051 Uiso 1 1 d R . . H41C H 0.3803 -0.2746 0.1962 0.051 Uiso 1 1 d R . . N1B N 0.3296(3) 0.0534(3) 0.3818(2) 0.0234(7) Uani 1 1 d . . . N1C N 0.2950(3) 0.1451(3) 0.0418(2) 0.0249(7) Uani 1 1 d . . . N1D N 0.3552(3) 0.3712(3) 0.1487(2) 0.0243(7) Uani 1 1 d . . . N1A N -0.1598(4) 0.3175(3) 0.0409(2) 0.0318(8) Uani 1 1 d . . . H1A H -0.1129 0.2633 0.0840 0.038 Uiso 1 1 calc R . . N3A N -0.1753(3) 0.0720(2) 0.3154(2) 0.0190(6) Uani 1 1 d . . . H3A1 H -0.1161 0.0978 0.2687 0.023 Uiso 1 1 calc R . . N2A N -0.2316(3) 0.1026(3) 0.1266(2) 0.0299(8) Uani 1 1 d . . . O1A O -0.0195(2) 0.26578(19) 0.19505(16) 0.0189(5) Uani 1 1 d . . . O1M O 0.4699(3) 0.5113(2) 0.3830(2) 0.0422(8) Uani 1 1 d . . . H1M H 0.5026 0.5479 0.4192 0.051 Uiso 1 1 d R . . O2A O 0.1242(2) 0.3439(2) 0.29791(16) 0.0217(5) Uani 1 1 d . . . O2B O 0.2227(2) 0.1274(2) 0.38162(17) 0.0235(6) Uani 1 1 d . . . O2C O 0.1669(2) 0.1715(2) 0.05771(17) 0.0237(6) Uani 1 1 d . . . O2D O 0.2454(2) 0.3620(2) 0.11230(17) 0.0228(6) Uani 1 1 d . . . O2M O 0.4082(3) 0.3571(2) 0.5336(2) 0.0468(8) Uani 1 1 d . . . H2M H 0.4510 0.4003 0.4774 0.056 Uiso 1 1 d R . . O3A O 0.0927(2) 0.03861(19) 0.24562(16) 0.0211(5) Uani 1 1 d . . . O3B O 0.3841(2) 0.0467(2) 0.30470(16) 0.0244(6) Uani 1 1 d . . . O3C O 0.3725(3) 0.1275(2) 0.11024(17) 0.0264(6) Uani 1 1 d . . . O3D O 0.3985(2) 0.2912(2) 0.21501(17) 0.0236(6) Uani 1 1 d . . . O4A O 0.2804(3) -0.1287(2) 0.20714(17) 0.0255(6) Uani 1 1 d . . . O4B O 0.3752(3) -0.0065(2) 0.45322(18) 0.0319(7) Uani 1 1 d . . . O4C O 0.3423(3) 0.1374(3) -0.03350(18) 0.0373(7) Uani 1 1 d . . . O4D O 0.4165(3) 0.4529(2) 0.1212(2) 0.0407(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.01997(19) 0.02140(19) 0.0239(2) -0.00264(13) -0.00431(13) -0.00054(13) Y1 0.01997(19) 0.02140(19) 0.0239(2) -0.00264(13) -0.00431(13) -0.00054(13) C1A 0.0190(18) 0.0193(19) 0.0183(18) 0.0006(15) 0.0006(14) -0.0015(15) C1M 0.040(3) 0.064(3) 0.055(3) -0.020(3) -0.004(2) -0.004(3) C2A 0.0176(18) 0.0212(19) 0.0190(19) -0.0004(15) -0.0007(14) 0.0014(15) C2M 0.055(3) 0.026(2) 0.047(3) -0.010(2) -0.015(2) -0.001(2) C3A 0.031(2) 0.023(2) 0.022(2) -0.0040(16) -0.0025(16) 0.0004(17) C4A 0.031(2) 0.022(2) 0.029(2) -0.0013(17) 0.0009(17) 0.0055(17) C5A 0.023(2) 0.025(2) 0.030(2) 0.0028(17) -0.0048(17) 0.0109(17) C6A 0.0187(19) 0.027(2) 0.025(2) -0.0009(16) -0.0046(15) 0.0012(16) C7A 0.024(2) 0.033(2) 0.037(2) 0.0044(18) -0.0129(18) -0.0023(18) C8A 0.043(3) 0.043(3) 0.044(3) -0.010(2) -0.015(2) -0.007(2) C9A 0.045(3) 0.059(3) 0.030(2) -0.002(2) -0.013(2) -0.023(2) C10A 0.022(2) 0.025(2) 0.030(2) -0.0021(17) -0.0037(16) -0.0087(16) C11A 0.0187(19) 0.0182(19) 0.029(2) -0.0042(16) -0.0016(15) -0.0024(15) C12A 0.024(2) 0.0195(19) 0.0207(19) -0.0027(15) -0.0052(15) 0.0047(15) C13A 0.0153(17) 0.0164(18) 0.0218(19) -0.0061(15) -0.0038(14) 0.0002(14) C14A 0.0224(19) 0.0207(19) 0.0171(18) -0.0031(15) -0.0006(14) -0.0033(15) C15A 0.0213(19) 0.0171(18) 0.025(2) -0.0028(15) -0.0060(15) -0.0020(15) C16A 0.0196(19) 0.0167(18) 0.025(2) -0.0054(15) -0.0054(15) 0.0031(15) C17A 0.0169(18) 0.0233(19) 0.0175(18) -0.0055(15) -0.0037(14) -0.0037(15) C18A 0.0187(18) 0.0164(18) 0.0210(19) -0.0027(15) -0.0074(14) -0.0020(14) C19A 0.052(3) 0.025(2) 0.045(3) -0.007(2) -0.007(2) 0.012(2) C20A 0.039(2) 0.022(2) 0.029(2) -0.0011(17) 0.0000(18) 0.0044(18) C21A 0.023(2) 0.029(2) 0.030(2) -0.0097(17) -0.0098(16) 0.0009(17) C31A 0.050(3) 0.027(2) 0.025(2) -0.0004(18) -0.0074(19) 0.006(2) C32A 0.041(3) 0.060(3) 0.039(3) -0.024(2) 0.011(2) -0.032(2) C33A 0.026(2) 0.022(2) 0.025(2) -0.0064(16) 0.0001(16) 0.0072(16) C41A 0.025(2) 0.049(3) 0.025(2) -0.0101(19) 0.0033(17) 0.0062(19) N1B 0.0214(17) 0.0224(17) 0.0254(18) -0.0017(14) -0.0074(14) -0.0027(14) N1C 0.0265(18) 0.0225(17) 0.0265(18) -0.0061(14) -0.0021(14) -0.0054(14) N1D 0.0209(17) 0.0272(18) 0.0237(17) -0.0045(14) 0.0009(13) -0.0033(14) N1A 0.040(2) 0.0214(17) 0.035(2) -0.0059(15) -0.0230(16) 0.0021(15) N3A 0.0192(16) 0.0159(15) 0.0206(16) -0.0043(12) 0.0004(12) 0.0017(12) N2A 0.0310(19) 0.039(2) 0.0222(17) -0.0034(15) -0.0037(14) -0.0173(16) O1A 0.0158(12) 0.0147(12) 0.0244(13) -0.0015(10) -0.0052(10) 0.0007(10) O1M 0.0390(18) 0.0410(18) 0.052(2) -0.0252(15) -0.0129(15) 0.0042(14) O2A 0.0201(13) 0.0211(13) 0.0234(13) -0.0048(11) -0.0076(10) 0.0015(11) O2B 0.0212(14) 0.0204(13) 0.0265(14) -0.0040(11) -0.0052(11) 0.0052(11) O2C 0.0185(14) 0.0263(14) 0.0255(14) -0.0048(11) -0.0031(11) -0.0014(11) O2D 0.0173(13) 0.0228(14) 0.0270(14) -0.0017(11) -0.0061(11) -0.0025(11) O2M 0.052(2) 0.0289(17) 0.061(2) -0.0111(15) -0.0097(16) -0.0043(15) O3A 0.0215(13) 0.0162(13) 0.0232(13) 0.0004(10) -0.0049(10) -0.0012(10) O3B 0.0209(14) 0.0286(15) 0.0205(14) -0.0018(11) -0.0017(11) 0.0009(11) O3C 0.0190(13) 0.0339(15) 0.0246(14) -0.0059(12) -0.0072(11) 0.0034(11) O3D 0.0202(13) 0.0243(14) 0.0238(14) -0.0008(11) -0.0067(11) 0.0001(11) O4A 0.0211(14) 0.0277(14) 0.0236(14) -0.0020(11) 0.0035(11) 0.0007(11) O4B 0.0313(16) 0.0312(16) 0.0273(15) 0.0021(12) -0.0114(12) 0.0055(12) O4C 0.0314(16) 0.060(2) 0.0261(16) -0.0206(14) 0.0055(12) -0.0081(14) O4D 0.0345(17) 0.0362(17) 0.0482(19) 0.0071(14) -0.0060(14) -0.0202(14) _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 O3A 2.156(2) . ? Dy1 O1A 2.253(2) . ? Dy1 O3C 2.383(3) . ? Dy1 O2B 2.443(2) . ? Dy1 O2D 2.468(2) . ? Dy1 O2C 2.487(2) . ? Dy1 O3B 2.489(2) . ? Dy1 O3D 2.500(2) . ? Dy1 O2A 2.571(2) . ? Dy1 N1C 2.859(3) . ? Dy1 N1B 2.887(3) . ? Dy1 N1D 2.901(3) . ? C1A O1A 1.348(4) . ? C1A C6A 1.399(5) . ? C1A C2A 1.396(5) . ? C1M O1M 1.380(5) . ? C2A C3A 1.384(5) . ? C2A O2A 1.392(4) . ? C2M O2M 1.422(5) . ? C3A C4A 1.399(5) . ? C4A C5A 1.375(6) . ? C4A C19A 1.523(5) . ? C5A C6A 1.401(5) . ? C6A C7A 1.512(5) . ? C7A N1A 1.509(5) . ? C8A C9A 1.474(6) . ? C8A N1A 1.493(5) . ? C9A N2A 1.493(5) . ? C10A N2A 1.452(5) . ? C10A C11A 1.509(5) . ? C11A N3A 1.497(4) . ? C12A C13A 1.503(5) . ? C12A N3A 1.515(4) . ? C13A C14A 1.395(5) . ? C13A C18A 1.394(5) . ? C14A C15A 1.391(5) . ? C15A C16A 1.395(5) . ? C15A C20A 1.506(5) . ? C16A C17A 1.385(5) . ? C17A O4A 1.382(4) . ? C17A C18A 1.414(5) . ? C18A O3A 1.339(4) . ? C21A O2A 1.439(4) . ? C31A N1A 1.476(5) . ? C32A N2A 1.459(6) . ? C33A N3A 1.490(4) . ? C41A O4A 1.416(4) . ? N1B O4B 1.226(4) . ? N1B O3B 1.264(4) . ? N1B O2B 1.281(4) . ? N1C O4C 1.219(4) . ? N1C O2C 1.268(4) . ? N1C O3C 1.282(4) . ? N1D O4D 1.225(4) . ? N1D O2D 1.271(4) . ? N1D O3D 1.275(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3A Dy1 O1A 78.93(9) . . ? O3A Dy1 O3C 99.03(9) . . ? O1A Dy1 O3C 130.09(8) . . ? O3A Dy1 O2B 80.54(9) . . ? O1A Dy1 O2B 105.06(8) . . ? O3C Dy1 O2B 123.98(8) . . ? O3A Dy1 O2D 148.70(9) . . ? O1A Dy1 O2D 81.14(8) . . ? O3C Dy1 O2D 76.00(9) . . ? O2B Dy1 O2D 128.22(8) . . ? O3A Dy1 O2C 81.03(9) . . ? O1A Dy1 O2C 78.30(8) . . ? O3C Dy1 O2C 52.54(8) . . ? O2B Dy1 O2C 160.20(8) . . ? O2D Dy1 O2C 71.42(8) . . ? O3A Dy1 O3B 82.20(9) . . ? O1A Dy1 O3B 152.64(8) . . ? O3C Dy1 O3B 72.34(8) . . ? O2B Dy1 O3B 51.94(8) . . ? O2D Dy1 O3B 123.70(8) . . ? O2C Dy1 O3B 118.10(8) . . ? O3A Dy1 O3D 156.88(8) . . ? O1A Dy1 O3D 123.12(8) . . ? O3C Dy1 O3D 72.80(9) . . ? O2B Dy1 O3D 86.31(8) . . ? O2D Dy1 O3D 51.76(8) . . ? O2C Dy1 O3D 108.48(8) . . ? O3B Dy1 O3D 74.72(8) . . ? O3A Dy1 O2A 119.78(9) . . ? O1A Dy1 O2A 64.71(8) . . ? O3C Dy1 O2A 141.16(9) . . ? O2B Dy1 O2A 66.11(8) . . ? O2D Dy1 O2A 71.42(8) . . ? O2C Dy1 O2A 130.53(8) . . ? O3B Dy1 O2A 109.39(8) . . ? O3D Dy1 O2A 70.62(8) . . ? O3A Dy1 N1C 91.58(9) . . ? O1A Dy1 N1C 103.92(9) . . ? O3C Dy1 N1C 26.37(8) . . ? O2B Dy1 N1C 147.80(8) . . ? O2D Dy1 N1C 70.13(8) . . ? O2C Dy1 N1C 26.27(8) . . ? O3B Dy1 N1C 96.20(8) . . ? O3D Dy1 N1C 89.51(8) . . ? O2A Dy1 N1C 141.18(8) . . ? O3A Dy1 N1B 78.89(9) . . ? O1A Dy1 N1B 129.26(9) . . ? O3C Dy1 N1B 98.18(9) . . ? O2B Dy1 N1B 26.16(8) . . ? O2D Dy1 N1B 132.23(8) . . ? O2C Dy1 N1B 140.85(9) . . ? O3B Dy1 N1B 25.86(8) . . ? O3D Dy1 N1B 80.92(8) . . ? O2A Dy1 N1B 88.61(8) . . ? N1C Dy1 N1B 121.73(9) . . ? O3A Dy1 N1D 170.94(9) . . ? O1A Dy1 N1D 102.15(8) . . ? O3C Dy1 N1D 73.28(9) . . ? O2B Dy1 N1D 107.63(9) . . ? O2D Dy1 N1D 25.80(8) . . ? O2C Dy1 N1D 90.34(8) . . ? O3B Dy1 N1D 99.61(9) . . ? O3D Dy1 N1D 25.97(8) . . ? O2A Dy1 N1D 68.15(8) . . ? N1C Dy1 N1D 79.41(9) . . ? N1B Dy1 N1D 106.61(9) . . ? O1A C1A C6A 122.6(3) . . ? O1A C1A C2A 119.2(3) . . ? C6A C1A C2A 118.2(3) . . ? C3A C2A O2A 124.7(3) . . ? C3A C2A C1A 122.5(3) . . ? O2A C2A C1A 112.8(3) . . ? C2A C3A C4A 118.9(4) . . ? C5A C4A C3A 119.1(3) . . ? C5A C4A C19A 122.2(4) . . ? C3A C4A C19A 118.7(4) . . ? C4A C5A C6A 122.2(3) . . ? C1A C6A C5A 118.9(3) . . ? C1A C6A C7A 120.0(3) . . ? C5A C6A C7A 121.0(3) . . ? C6A C7A N1A 112.7(3) . . ? C9A C8A N1A 111.6(4) . . ? C8A C9A N2A 113.0(4) . . ? N2A C10A C11A 113.1(3) . . ? N3A C11A C10A 113.0(3) . . ? C13A C12A N3A 112.7(3) . . ? C14A C13A C18A 120.7(3) . . ? C14A C13A C12A 120.9(3) . . ? C18A C13A C12A 118.2(3) . . ? C15A C14A C13A 121.1(3) . . ? C14A C15A C16A 118.2(3) . . ? C14A C15A C20A 121.2(3) . . ? C16A C15A C20A 120.6(3) . . ? C17A C16A C15A 121.4(3) . . ? O4A C17A C16A 124.9(3) . . ? O4A C17A C18A 114.8(3) . . ? C16A C17A C18A 120.3(3) . . ? O3A C18A C13A 120.3(3) . . ? O3A C18A C17A 121.6(3) . . ? C13A C18A C17A 118.1(3) . . ? O4B N1B O3B 122.7(3) . . ? O4B N1B O2B 121.2(3) . . ? O3B N1B O2B 116.2(3) . . ? O4B N1B Dy1 174.8(2) . . ? O3B N1B Dy1 59.21(16) . . ? O2B N1B Dy1 57.22(16) . . ? O4C N1C O2C 122.7(3) . . ? O4C N1C O3C 121.8(3) . . ? O2C N1C O3C 115.6(3) . . ? O4C N1C Dy1 173.7(2) . . ? O2C N1C Dy1 60.25(16) . . ? O3C N1C Dy1 55.62(16) . . ? O4D N1D O2D 121.5(3) . . ? O4D N1D O3D 121.7(3) . . ? O2D N1D O3D 116.8(3) . . ? O4D N1D Dy1 177.7(3) . . ? O2D N1D Dy1 57.68(16) . . ? O3D N1D Dy1 59.15(16) . . ? C31A N1A C8A 108.8(3) . . ? C31A N1A C7A 112.5(3) . . ? C8A N1A C7A 114.6(3) . . ? C33A N3A C11A 112.1(3) . . ? C33A N3A C12A 110.1(3) . . ? C11A N3A C12A 111.9(3) . . ? C10A N2A C32A 111.5(3) . . ? C10A N2A C9A 109.0(3) . . ? C32A N2A C9A 113.2(3) . . ? C1A O1A Dy1 121.4(2) . . ? C2A O2A C21A 117.0(3) . . ? C2A O2A Dy1 112.42(19) . . ? C21A O2A Dy1 127.1(2) . . ? N1B O2B Dy1 96.62(19) . . ? N1C O2C Dy1 93.48(19) . . ? N1D O2D Dy1 96.51(19) . . ? C18A O3A Dy1 138.4(2) . . ? N1B O3B Dy1 94.94(19) . . ? N1C O3C Dy1 98.01(19) . . ? N1D O3D Dy1 94.88(19) . . ? C17A O4A C41A 117.0(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.237 _refine_diff_density_min -0.413 _refine_diff_density_rms 0.085