# 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 'Murale Murugesu' _publ_contact_author_email 'm.murugesu@uOttawa.ca, muralee.murugesu@gmail.com' _publ_author_name 'Murale Murugesu' data_sad _database_code_depnum_ccdc_archive 'CCDC 885487' #TrackingRef '- 09063_PL2957.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H62 Dy2 N14 O24' _chemical_formula_weight 1472.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _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 9.5597(18) _cell_length_b 10.0626(19) _cell_length_c 16.895(3) _cell_angle_alpha 78.919(3) _cell_angle_beta 80.042(3) _cell_angle_gamma 64.022(3) _cell_volume 1426.5(5) _cell_formula_units_Z 1 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 5708 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 25.68 _exptl_crystal_description cube _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas n/a _exptl_crystal_density_diffrn 1.714 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 736 _exptl_absorpt_coefficient_mu 2.690 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6152 _exptl_absorpt_correction_T_max 0.7747 _exptl_absorpt_process_details 'SADABS, (Bruker 2000)' _exptl_special_details ; One of the coordinated DMF molecules was disordered and was modeled over two positions as an 83:17 mixture. Only the major component of the disordered molecule was refined with anisotropic thermal parameters. All other non-hydrogen atoms were refined with anisotropic thermal parameters. ; _diffrn_ambient_temperature 203(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 'CCD area detector' _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 14934 _diffrn_reflns_av_R_equivalents 0.0253 _diffrn_reflns_av_sigmaI/netI 0.0295 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 25.72 _reflns_number_total 5414 _reflns_number_gt 4848 _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, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.0409P)^2^+3.3921P] 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 5414 _refine_ls_number_parameters 392 _refine_ls_number_restraints 37 _refine_ls_R_factor_all 0.0396 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0940 _refine_ls_wR_factor_gt 0.0909 _refine_ls_goodness_of_fit_ref 1.164 _refine_ls_restrained_S_all 1.160 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.68264(3) 1.05763(3) 0.266259(14) 0.03282(9) Uani 1 1 d . A . N1 N 0.8438(5) 1.1992(5) 0.2759(2) 0.0324(9) Uani 1 1 d . . . N2 N 0.7758(5) 1.3006(5) 0.3333(2) 0.0370(10) Uani 1 1 d . . . H2A H 0.8108 1.3661 0.3359 0.044 Uiso 1 1 calc R . . N3 N 0.7974(8) 0.8283(6) 0.4032(3) 0.0557(14) Uani 1 1 d . . . N4 N 0.5127(6) 1.2918(6) 0.1435(3) 0.0504(12) Uani 1 1 d . . . N5 N 0.7156(7) 0.6925(5) 0.1338(3) 0.0552(13) Uani 1 1 d . . . N6 N 0.2581(7) 1.0047(7) 0.3682(4) 0.0610(14) Uani 1 1 d . . . N7 N 0.1257(6) 0.5353(6) 0.3139(4) 0.0593(14) Uani 1 1 d D . . O1 O 1.0759(5) 0.8252(4) 0.0663(2) 0.0464(9) Uani 1 1 d . . . O2 O 0.8897(4) 0.9955(4) 0.1764(2) 0.0388(8) Uani 1 1 d . . . O3 O 0.6070(4) 1.1969(4) 0.3794(2) 0.0414(9) Uani 1 1 d . . . O4 O 0.8850(5) 0.8806(5) 0.3545(3) 0.0569(11) Uani 1 1 d . . . O5 O 0.8499(7) 0.7307(6) 0.4598(3) 0.0855(17) Uani 1 1 d . . . O6 O 0.6578(6) 0.8822(5) 0.3901(3) 0.0563(11) Uani 1 1 d . . . O7 O 0.5566(5) 1.1572(5) 0.1370(2) 0.0482(9) Uani 1 1 d . . . O8 O 0.4369(7) 1.3918(6) 0.0946(4) 0.0868(17) Uani 1 1 d . . . O9 O 0.5497(5) 1.3187(4) 0.2056(3) 0.0511(10) Uani 1 1 d . . . O10 O 0.6757(5) 0.8521(4) 0.2219(3) 0.0497(10) Uani 1 1 d . . . O11 O 0.4173(5) 1.1079(5) 0.3005(3) 0.0540(10) Uani 1 1 d . . . O12 O -0.0793(7) 0.4879(7) 0.3117(4) 0.099(2) Uani 1 1 d . . . C1 C 1.1795(8) 0.7285(7) 0.0091(4) 0.0567(16) Uani 1 1 d . . . H1A H 1.1333 0.6660 -0.0019 0.085 Uiso 1 1 calc R . . H1B H 1.2784 0.6661 0.0312 0.085 Uiso 1 1 calc R . . H1C H 1.1969 0.7878 -0.0409 0.085 Uiso 1 1 calc R . . C2 C 1.1241(6) 0.9211(6) 0.0872(3) 0.0396(12) Uani 1 1 d . . . C3 C 1.2587(7) 0.9347(8) 0.0561(4) 0.0537(15) Uani 1 1 d . . . H3A H 1.3266 0.8740 0.0174 0.064 Uiso 1 1 calc R . . C4 C 1.2978(8) 1.0380(9) 0.0811(4) 0.066(2) Uani 1 1 d . . . H4A H 1.3911 1.0466 0.0589 0.079 Uiso 1 1 calc R . . C5 C 1.1994(8) 1.1268(8) 0.1380(4) 0.0579(17) Uani 1 1 d . . . H5A H 1.2249 1.1971 0.1543 0.069 Uiso 1 1 calc R . . C6 C 1.0605(6) 1.1126(6) 0.1720(3) 0.0398(12) Uani 1 1 d . . . C7 C 1.0187(6) 1.0105(6) 0.1476(3) 0.0348(11) Uani 1 1 d . . . C8 C 0.9672(6) 1.2038(6) 0.2345(3) 0.0400(12) Uani 1 1 d . . . H8A H 1.0003 1.2729 0.2459 0.048 Uiso 1 1 calc R . . C9 C 0.6556(6) 1.2913(5) 0.3833(3) 0.0322(10) Uani 1 1 d . . . C10 C 0.5789(6) 1.4008(6) 0.4431(3) 0.0333(11) Uani 1 1 d . . . C11 C 0.5986(6) 1.5317(6) 0.4369(3) 0.0370(11) Uani 1 1 d . . . H11 H 0.6656 1.5535 0.3940 0.044 Uiso 1 1 calc R . . C12 C 0.4794(6) 1.3705(6) 0.5069(3) 0.0392(12) Uani 1 1 d . . . H12 H 0.4652 1.2824 0.5117 0.047 Uiso 1 1 calc R . . C13 C 0.7402(7) 0.7966(6) 0.1584(4) 0.0491(14) Uani 1 1 d . . . H13A H 0.8110 0.8309 0.1258 0.059 Uiso 1 1 calc R . . C14 C 0.6085(11) 0.6368(9) 0.1798(5) 0.081(2) Uani 1 1 d . . . H14A H 0.6071 0.6403 0.2369 0.121 Uiso 1 1 calc R . . H14B H 0.6409 0.5345 0.1710 0.121 Uiso 1 1 calc R . . H14C H 0.5047 0.6975 0.1629 0.121 Uiso 1 1 calc R . . C15 C 0.7982(13) 0.6293(11) 0.0598(6) 0.102(3) Uani 1 1 d . . . H15A H 0.8450 0.6929 0.0274 0.152 Uiso 1 1 calc R . . H15B H 0.7252 0.6223 0.0292 0.152 Uiso 1 1 calc R . . H15C H 0.8795 0.5307 0.0735 0.152 Uiso 1 1 calc R . . C16 C 0.3201(9) 1.1029(9) 0.3559(5) 0.0536(18) Uani 0.83 1 d PU A 1 H16A H 0.2865 1.1729 0.3926 0.064 Uiso 0.83 1 calc PR A 1 C17 C 0.1399(11) 1.0054(13) 0.4345(6) 0.082(3) Uani 0.83 1 d PU A 1 H17A H 0.1088 1.0919 0.4618 0.123 Uiso 0.83 1 calc PR A 1 H17B H 0.1819 0.9154 0.4725 0.123 Uiso 0.83 1 calc PR A 1 H17C H 0.0496 1.0093 0.4135 0.123 Uiso 0.83 1 calc PR A 1 C18 C 0.3133(12) 0.8888(11) 0.3169(7) 0.077(3) Uani 0.83 1 d PU A 1 H18A H 0.3859 0.9056 0.2728 0.116 Uiso 0.83 1 calc PR A 1 H18B H 0.2253 0.8901 0.2950 0.116 Uiso 0.83 1 calc PR A 1 H18C H 0.3660 0.7927 0.3485 0.116 Uiso 0.83 1 calc PR A 1 C16A C 0.351(5) 1.031(5) 0.308(3) 0.070(10) Uiso 0.17 1 d PU A 2 H16B H 0.3673 0.9807 0.2637 0.085 Uiso 0.17 1 calc PR A 2 C17A C 0.212(7) 1.065(6) 0.431(3) 0.086(13) Uiso 0.17 1 d PU A 2 H17D H 0.1872 0.9991 0.4748 0.129 Uiso 0.17 1 calc PR A 2 H17E H 0.1201 1.1577 0.4220 0.129 Uiso 0.17 1 calc PR A 2 H17F H 0.2945 1.0860 0.4449 0.129 Uiso 0.17 1 calc PR A 2 C18A C 0.176(6) 0.913(6) 0.369(3) 0.085(13) Uiso 0.17 1 d PU A 2 H18D H 0.1472 0.8805 0.4249 0.127 Uiso 0.17 1 calc PR A 2 H18E H 0.2436 0.8270 0.3421 0.127 Uiso 0.17 1 calc PR A 2 H18F H 0.0827 0.9707 0.3415 0.127 Uiso 0.17 1 calc PR A 2 C19 C 0.0188(9) 0.4872(8) 0.3470(5) 0.0683(19) Uani 1 1 d . . . H19 H 0.0196 0.4496 0.4024 0.082 Uiso 1 1 calc R . . C20 C 0.1327(11) 0.5973(12) 0.2350(6) 0.110(4) Uani 1 1 d D . . H20A H 0.1261 0.5340 0.2005 0.165 Uiso 1 1 calc R . . H20B H 0.2307 0.6072 0.2202 0.165 Uiso 1 1 calc R . . H20C H 0.0461 0.6950 0.2280 0.165 Uiso 1 1 calc R . . C21 C 0.2322(14) 0.5336(17) 0.3624(9) 0.153(6) Uani 1 1 d D . . H21A H 0.1806 0.5541 0.4162 0.229 Uiso 1 1 calc R . . H21B H 0.2696 0.6092 0.3383 0.229 Uiso 1 1 calc R . . H21C H 0.3200 0.4363 0.3661 0.229 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.03691(15) 0.03270(14) 0.03448(14) -0.01430(9) 0.00787(9) -0.01983(10) N1 0.038(2) 0.034(2) 0.028(2) -0.0150(17) 0.0070(17) -0.0168(19) N2 0.047(3) 0.040(2) 0.036(2) -0.0240(19) 0.0130(19) -0.028(2) N3 0.088(4) 0.038(3) 0.040(3) 0.000(2) 0.001(3) -0.030(3) N4 0.047(3) 0.053(3) 0.049(3) -0.010(3) 0.001(2) -0.019(3) N5 0.076(4) 0.040(3) 0.058(3) -0.020(2) -0.009(3) -0.025(3) N6 0.052(3) 0.070(4) 0.068(4) -0.006(3) 0.001(3) -0.035(3) N7 0.048(3) 0.049(3) 0.083(4) 0.005(3) -0.016(3) -0.023(3) O1 0.054(2) 0.043(2) 0.041(2) -0.0223(17) 0.0132(17) -0.0191(19) O2 0.039(2) 0.042(2) 0.041(2) -0.0211(16) 0.0112(15) -0.0207(17) O3 0.053(2) 0.044(2) 0.039(2) -0.0211(16) 0.0158(16) -0.0329(19) O4 0.054(3) 0.056(3) 0.056(3) 0.002(2) -0.003(2) -0.024(2) O5 0.115(5) 0.066(3) 0.056(3) 0.013(3) -0.006(3) -0.029(3) O6 0.061(3) 0.056(3) 0.054(3) -0.002(2) 0.005(2) -0.033(2) O7 0.050(2) 0.051(2) 0.046(2) -0.0170(19) 0.0037(18) -0.022(2) O8 0.087(4) 0.068(3) 0.079(4) 0.006(3) -0.031(3) -0.007(3) O9 0.054(3) 0.040(2) 0.064(3) -0.0104(19) -0.010(2) -0.0208(19) O10 0.058(3) 0.047(2) 0.058(2) -0.025(2) 0.008(2) -0.032(2) O11 0.045(2) 0.064(3) 0.062(3) -0.020(2) 0.009(2) -0.031(2) O12 0.092(4) 0.115(5) 0.130(5) -0.075(4) 0.045(4) -0.078(4) C1 0.064(4) 0.050(4) 0.051(3) -0.025(3) 0.008(3) -0.016(3) C2 0.040(3) 0.040(3) 0.033(3) -0.011(2) 0.003(2) -0.011(2) C3 0.048(3) 0.066(4) 0.044(3) -0.028(3) 0.017(3) -0.020(3) C4 0.049(4) 0.093(5) 0.068(4) -0.041(4) 0.027(3) -0.040(4) C5 0.060(4) 0.079(5) 0.053(4) -0.030(3) 0.020(3) -0.046(4) C6 0.041(3) 0.049(3) 0.034(3) -0.013(2) 0.007(2) -0.023(3) C7 0.035(3) 0.038(3) 0.029(2) -0.011(2) 0.006(2) -0.013(2) C8 0.044(3) 0.044(3) 0.042(3) -0.018(2) 0.006(2) -0.027(3) C9 0.035(3) 0.035(3) 0.029(2) -0.015(2) 0.0073(19) -0.016(2) C10 0.037(3) 0.034(3) 0.031(2) -0.016(2) 0.005(2) -0.015(2) C11 0.044(3) 0.041(3) 0.030(2) -0.014(2) 0.014(2) -0.025(2) C12 0.049(3) 0.040(3) 0.036(3) -0.020(2) 0.014(2) -0.027(3) C13 0.056(4) 0.040(3) 0.056(4) -0.016(3) 0.000(3) -0.022(3) C14 0.122(7) 0.066(5) 0.084(5) -0.007(4) -0.018(5) -0.065(5) C15 0.143(9) 0.091(6) 0.092(6) -0.061(5) 0.018(6) -0.060(6) C16 0.046(4) 0.066(5) 0.054(4) -0.016(4) 0.006(3) -0.030(4) C17 0.062(6) 0.112(8) 0.075(6) 0.012(6) 0.004(5) -0.053(6) C18 0.085(7) 0.065(6) 0.093(7) -0.009(5) -0.006(5) -0.044(5) C19 0.067(5) 0.062(4) 0.078(5) -0.021(4) 0.005(4) -0.029(4) C20 0.078(6) 0.106(7) 0.108(8) 0.000(6) 0.031(5) -0.024(5) C21 0.108(9) 0.174(13) 0.198(15) -0.017(11) -0.068(10) -0.062(9) _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 2.203(3) . ? Dy1 O11 2.346(4) . ? Dy1 O10 2.361(4) . ? Dy1 O3 2.409(3) . ? Dy1 O9 2.461(4) . ? Dy1 O4 2.468(4) . ? Dy1 O7 2.498(4) . ? Dy1 O6 2.515(4) . ? Dy1 N1 2.555(4) . ? Dy1 N4 2.902(5) . ? Dy1 N3 2.914(5) . ? N1 C8 1.278(7) . ? N1 N2 1.408(5) . ? N2 C9 1.330(6) . ? N2 H2A 0.8700 . ? N3 O5 1.227(7) . ? N3 O6 1.243(7) . ? N3 O4 1.280(7) . ? N4 O8 1.212(7) . ? N4 O7 1.251(6) . ? N4 O9 1.273(6) . ? N5 C13 1.320(7) . ? N5 C14 1.424(9) . ? N5 C15 1.454(9) . ? N6 C17A 1.24(6) . ? N6 C16A 1.29(5) . ? N6 C16 1.328(9) . ? N6 C18 1.442(11) . ? N6 C18A 1.44(5) . ? N6 C17 1.445(10) . ? N7 C19 1.312(9) . ? N7 C20 1.364(10) . ? N7 C21 1.406(10) . ? O1 C2 1.359(7) . ? O1 C1 1.432(6) . ? O2 C7 1.307(6) . ? O3 C9 1.243(6) . ? O10 C13 1.243(7) . ? O11 C16A 1.18(5) . ? O11 C16 1.210(8) . ? O12 C19 1.192(10) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C1 H1C 0.9700 . ? C2 C3 1.358(8) . ? C2 C7 1.439(7) . ? C3 C4 1.400(9) . ? C3 H3A 0.9400 . ? C4 C5 1.375(9) . ? C4 H4A 0.9400 . ? C5 C6 1.409(8) . ? C5 H5A 0.9400 . ? C6 C7 1.402(7) . ? C6 C8 1.444(7) . ? C8 H8A 0.9400 . ? C9 C10 1.496(6) . ? C10 C12 1.390(7) . ? C10 C11 1.393(7) . ? C11 C12 1.378(7) 2_686 ? C11 H11 0.9400 . ? C12 C11 1.378(7) 2_686 ? C12 H12 0.9400 . ? C13 H13A 0.9400 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 H14C 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 H15C 0.9700 . ? C16 H16A 0.9400 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 H17C 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? C16A H16B 0.9400 . ? C17A H17D 0.9700 . ? C17A H17E 0.9700 . ? C17A H17F 0.9700 . ? C18A H18D 0.9700 . ? C18A H18E 0.9700 . ? C18A H18F 0.9700 . ? C19 H19 0.9400 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 H20C 0.9700 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C21 H21C 0.9700 . ? 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 O11 149.09(15) . . ? O2 Dy1 O10 79.17(13) . . ? O11 Dy1 O10 79.70(14) . . ? O2 Dy1 O3 132.55(12) . . ? O11 Dy1 O3 76.06(14) . . ? O10 Dy1 O3 143.24(13) . . ? O2 Dy1 O9 96.75(14) . . ? O11 Dy1 O9 77.25(15) . . ? O10 Dy1 O9 124.62(15) . . ? O3 Dy1 O9 76.07(14) . . ? O2 Dy1 O4 79.94(14) . . ? O11 Dy1 O4 121.79(15) . . ? O10 Dy1 O4 88.67(15) . . ? O3 Dy1 O4 81.24(15) . . ? O9 Dy1 O4 145.61(14) . . ? O2 Dy1 O7 79.09(13) . . ? O11 Dy1 O7 73.59(14) . . ? O10 Dy1 O7 74.15(14) . . ? O3 Dy1 O7 123.28(13) . . ? O9 Dy1 O7 51.22(13) . . ? O4 Dy1 O7 155.00(14) . . ? O2 Dy1 O6 122.35(15) . . ? O11 Dy1 O6 71.29(16) . . ? O10 Dy1 O6 72.40(15) . . ? O3 Dy1 O6 73.86(14) . . ? O9 Dy1 O6 140.61(15) . . ? O4 Dy1 O6 50.97(15) . . ? O7 Dy1 O6 134.82(15) . . ? O2 Dy1 N1 69.82(12) . . ? O11 Dy1 N1 132.85(14) . . ? O10 Dy1 N1 147.33(13) . . ? O3 Dy1 N1 63.52(12) . . ? O9 Dy1 N1 70.57(14) . . ? O4 Dy1 N1 76.30(14) . . ? O7 Dy1 N1 108.66(13) . . ? O6 Dy1 N1 115.94(14) . . ? O2 Dy1 N4 87.99(14) . . ? O11 Dy1 N4 73.42(15) . . ? O10 Dy1 N4 99.15(15) . . ? O3 Dy1 N4 99.89(14) . . ? O9 Dy1 N4 25.82(14) . . ? O4 Dy1 N4 164.17(15) . . ? O7 Dy1 N4 25.40(13) . . ? O6 Dy1 N4 144.63(15) . . ? N1 Dy1 N4 89.99(14) . . ? O2 Dy1 N3 101.68(16) . . ? O11 Dy1 N3 96.22(17) . . ? O10 Dy1 N3 79.24(15) . . ? O3 Dy1 N3 76.42(14) . . ? O9 Dy1 N3 152.49(14) . . ? O4 Dy1 N3 25.86(16) . . ? O7 Dy1 N3 152.76(15) . . ? O6 Dy1 N3 25.12(15) . . ? N1 Dy1 N3 96.84(15) . . ? N4 Dy1 N3 169.62(16) . . ? C8 N1 N2 114.1(4) . . ? C8 N1 Dy1 132.3(3) . . ? N2 N1 Dy1 113.4(3) . . ? C9 N2 N1 116.8(4) . . ? C9 N2 H2A 121.6 . . ? N1 N2 H2A 121.6 . . ? O5 N3 O6 122.5(6) . . ? O5 N3 O4 121.1(7) . . ? O6 N3 O4 116.4(5) . . ? O5 N3 Dy1 178.2(5) . . ? O6 N3 Dy1 59.2(3) . . ? O4 N3 Dy1 57.2(3) . . ? O8 N4 O7 122.4(6) . . ? O8 N4 O9 121.4(6) . . ? O7 N4 O9 116.2(5) . . ? O8 N4 Dy1 177.4(5) . . ? O7 N4 Dy1 58.9(3) . . ? O9 N4 Dy1 57.3(3) . . ? C13 N5 C14 120.8(6) . . ? C13 N5 C15 121.4(6) . . ? C14 N5 C15 117.8(6) . . ? C17A N6 C16A 126(4) . . ? C17A N6 C16 76(3) . . ? C16A N6 C16 50(2) . . ? C17A N6 C18 159(3) . . ? C16A N6 C18 71(2) . . ? C16 N6 C18 120.1(7) . . ? C17A N6 C18A 108(4) . . ? C16A N6 C18A 126(3) . . ? C16 N6 C18A 170(2) . . ? C18 N6 C18A 58(2) . . ? C17A N6 C17 47(3) . . ? C16A N6 C17 169(2) . . ? C16 N6 C17 121.9(8) . . ? C18 N6 C17 117.9(7) . . ? C18A N6 C17 61(2) . . ? C19 N7 C20 123.0(7) . . ? C19 N7 C21 119.5(9) . . ? C20 N7 C21 117.3(9) . . ? C2 O1 C1 116.4(5) . . ? C7 O2 Dy1 146.6(3) . . ? C9 O3 Dy1 122.7(3) . . ? N3 O4 Dy1 96.9(4) . . ? N3 O6 Dy1 95.7(3) . . ? N4 O7 Dy1 95.7(3) . . ? N4 O9 Dy1 96.8(3) . . ? C13 O10 Dy1 128.2(4) . . ? C16A O11 C16 55(2) . . ? C16A O11 Dy1 131(2) . . ? C16 O11 Dy1 144.3(5) . . ? O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 O1 125.1(5) . . ? C3 C2 C7 121.1(5) . . ? O1 C2 C7 113.8(5) . . ? C2 C3 C4 120.9(5) . . ? C2 C3 H3A 119.5 . . ? C4 C3 H3A 119.5 . . ? C5 C4 C3 119.9(6) . . ? C5 C4 H4A 120.1 . . ? C3 C4 H4A 120.1 . . ? C4 C5 C6 120.1(6) . . ? C4 C5 H5A 120.0 . . ? C6 C5 H5A 120.0 . . ? C7 C6 C5 121.0(5) . . ? C7 C6 C8 122.0(5) . . ? C5 C6 C8 117.0(5) . . ? O2 C7 C6 123.1(4) . . ? O2 C7 C2 119.9(5) . . ? C6 C7 C2 117.0(5) . . ? N1 C8 C6 125.9(5) . . ? N1 C8 H8A 117.0 . . ? C6 C8 H8A 117.0 . . ? O3 C9 N2 121.2(4) . . ? O3 C9 C10 121.2(4) . . ? N2 C9 C10 117.6(4) . . ? C12 C10 C11 118.9(4) . . ? C12 C10 C9 117.4(4) . . ? C11 C10 C9 123.6(4) . . ? C12 C11 C10 120.4(5) 2_686 . ? C12 C11 H11 119.8 2_686 . ? C10 C11 H11 119.8 . . ? C11 C12 C10 120.6(5) 2_686 . ? C11 C12 H12 119.7 2_686 . ? C10 C12 H12 119.7 . . ? O10 C13 N5 124.2(6) . . ? O10 C13 H13A 117.9 . . ? N5 C13 H13A 117.9 . . ? N5 C14 H14A 109.5 . . ? N5 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N5 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N5 C15 H15A 109.5 . . ? N5 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N5 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O11 C16 N6 124.1(7) . . ? O11 C16 H16A 118.0 . . ? N6 C16 H16A 118.0 . . ? N6 C17 H17A 109.5 . . ? N6 C17 H17B 109.5 . . ? N6 C17 H17C 109.5 . . ? N6 C18 H18A 109.5 . . ? N6 C18 H18B 109.5 . . ? N6 C18 H18C 109.5 . . ? O11 C16A N6 130(4) . . ? O11 C16A H16B 114.8 . . ? N6 C16A H16B 114.8 . . ? N6 C17A H17D 109.5 . . ? N6 C17A H17E 109.5 . . ? H17D C17A H17E 109.5 . . ? N6 C17A H17F 109.5 . . ? H17D C17A H17F 109.5 . . ? H17E C17A H17F 109.5 . . ? N6 C18A H18D 109.5 . . ? N6 C18A H18E 109.5 . . ? H18D C18A H18E 109.5 . . ? N6 C18A H18F 109.5 . . ? H18D C18A H18F 109.5 . . ? H18E C18A H18F 109.5 . . ? O12 C19 N7 124.6(8) . . ? O12 C19 H19 117.7 . . ? N7 C19 H19 117.7 . . ? N7 C20 H20A 109.5 . . ? N7 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N7 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N7 C21 H21A 109.5 . . ? N7 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N7 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.72 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.214 _refine_diff_density_min -0.658 _refine_diff_density_rms 0.112 # Attachment '- mm129.cif' data_mm129 _database_code_depnum_ccdc_archive 'CCDC 885486' #TrackingRef '- mm129.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H27 Dy N6 O11' _chemical_formula_weight 701.99 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 7.60440(10) _cell_length_b 10.2506(2) _cell_length_c 18.9048(3) _cell_angle_alpha 104.1310(10) _cell_angle_beta 90.7570(10) _cell_angle_gamma 107.6510(10) _cell_volume 1355.67(4) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 9895 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 28.26 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas n/a _exptl_crystal_density_diffrn 1.720 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 698 _exptl_absorpt_coefficient_mu 2.823 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6454 _exptl_absorpt_correction_T_max 0.6768 _exptl_absorpt_process_details 'SADABS, Bruker (2003)' _exptl_special_details ; Data collection is performed with four batch runs at phi = 0.00 deg (600 frames), at phi = 90.00 deg (600 frames), at phi = 180.00 deg (600 frames), and at phi = 270.00 deg (600 frames). A fifth batch run is collected at phi = 0.00 deg (50 frames) to monitor crystal and diffractometer stability. Frame width = 0.30 deg in omega. Data is merged, corrected for decay (if any), and treated with multi-scan absorption corrections (if required). All symmetry-equivalent reflections are merged for centrosymmetric data. Friedel pairs are not merged for noncentrosymmetric data. ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 19100 _diffrn_reflns_av_R_equivalents 0.0266 _diffrn_reflns_av_sigmaI/netI 0.0301 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 28.31 _reflns_number_total 6664 _reflns_number_gt 6034 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II, Bruker (2009)' _computing_cell_refinement 'APEX II, Bruker (2009)' _computing_data_reduction 'XPREP, Bruker (2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL, Bruker (2004)' _computing_publication_material 'SHELXTL, Bruker (2004)' _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^)+(0.0401P)^2^+0.1003P] 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 6664 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0315 _refine_ls_R_factor_gt 0.0262 _refine_ls_wR_factor_ref 0.0649 _refine_ls_wR_factor_gt 0.0628 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.821150(16) 0.970152(13) 0.745081(7) 0.02978(5) Uani 1 1 d . . . N1 N 0.5558(3) 1.0624(2) 0.78637(13) 0.0330(5) Uani 1 1 d . . . N2 N 0.4559(3) 1.0014(3) 0.83716(13) 0.0362(5) Uani 1 1 d . . . H2A H 0.3506 1.0154 0.8496 0.043 Uiso 1 1 calc R . . N3 N 0.5807(5) 0.7467(3) 0.62767(17) 0.0535(7) Uani 1 1 d . . . N4 N 1.0909(4) 1.1860(4) 0.85917(15) 0.0512(7) Uani 1 1 d . . . N5 N 1.0294(4) 0.6149(3) 0.77836(16) 0.0459(6) Uani 1 1 d . . . N6 N 1.2257(3) 1.0151(3) 0.58052(14) 0.0415(6) Uani 1 1 d . . . O1 O 0.9291(4) 1.2826(2) 0.5926(1) 0.0536(6) Uani 1 1 d . . . O2 O 0.7869(3) 1.1145(2) 0.6785(1) 0.0367(4) Uani 1 1 d . . . O3 O 0.6776(3) 0.9022(2) 0.8476(1) 0.0419(5) Uani 1 1 d . . . O4 O 0.9675(3) 1.2118(3) 0.8260(1) 0.0544(6) Uani 1 1 d . . . O5 O 1.2111(4) 1.2794(4) 0.9032(2) 0.0946(12) Uani 1 1 d . . . O6 O 1.0861(3) 1.0574(3) 0.8453(1) 0.0494(5) Uani 1 1 d . . . O7 O 0.7450(4) 0.8083(3) 0.6192(1) 0.0570(6) Uani 1 1 d . . . O8 O 0.4742(5) 0.6564(3) 0.5785(2) 0.0821(10) Uani 1 1 d . . . O9 O 0.5309(3) 0.7836(2) 0.6915(1) 0.0509(6) Uani 1 1 d . . . O10 O 1.0959(3) 1.0062(3) 0.6870(1) 0.0463(5) Uani 1 1 d . . . O11 O 0.9060(4) 0.7752(2) 0.7554(1) 0.0546(6) Uani 1 1 d . . . C1 C 0.7145(4) 1.2118(3) 0.67468(16) 0.0359(6) Uani 1 1 d . . . C2 C 0.7797(4) 1.3031(3) 0.62780(18) 0.0409(7) Uani 1 1 d . . . C3 C 0.6972(5) 1.4009(3) 0.6198(2) 0.0570(9) Uani 1 1 d . . . H3A H 0.7430 1.4590 0.5876 0.068 Uiso 1 1 calc R . . C4 C 0.5448(6) 1.4161(4) 0.6589(3) 0.0710(12) Uani 1 1 d . . . H4A H 0.4860 1.4828 0.6529 0.085 Uiso 1 1 calc R . . C5 C 0.4848(5) 1.3344(4) 0.7047(3) 0.0616(10) Uani 1 1 d . . . H5A H 0.3820 1.3442 0.7310 0.074 Uiso 1 1 calc R . . C6 C 0.5685(4) 1.2339(3) 0.71554(18) 0.0398(7) Uani 1 1 d . . . C7 C 1.0173(7) 1.3835(5) 0.5522(3) 0.0758(13) Uani 1 1 d . . . H7A H 1.1220 1.3586 0.5296 0.114 Uiso 1 1 calc R . . H7B H 1.0623 1.4788 0.5856 0.114 Uiso 1 1 calc R . . H7C H 0.9277 1.3816 0.5139 0.114 Uiso 1 1 calc R . . C8 C 0.4958(4) 1.1552(3) 0.76794(18) 0.0388(6) Uani 1 1 d . . . H8A H 0.3929 1.1737 0.7913 0.047 Uiso 1 1 calc R . . C9 C 0.5278(4) 0.9196(3) 0.86654(16) 0.0366(6) Uani 1 1 d . . . C10 C 0.4234(4) 0.8503(3) 0.92008(16) 0.0385(6) Uani 1 1 d . . . C11 C 0.2584(5) 0.8693(4) 0.94293(18) 0.0488(8) Uani 1 1 d . . . H11A H 0.2081 0.9298 0.9242 0.059 Uiso 1 1 calc R . . C12 C 0.1668(5) 0.8012(5) 0.9926(2) 0.0625(10) Uani 1 1 d . . . H12A H 0.0546 0.8158 1.0084 0.075 Uiso 1 1 calc R . . C13 C 0.2368(6) 0.7121(5) 1.0194(2) 0.0641(10) Uani 1 1 d . . . H13A H 0.1719 0.6631 1.0526 0.077 Uiso 1 1 calc R . . C14 C 0.4040(6) 0.6946(5) 0.9973(2) 0.0669(11) Uani 1 1 d . . . H14A H 0.4549 0.6352 1.0168 0.080 Uiso 1 1 calc R . . C15 C 0.4964(5) 0.7620(4) 0.9478(2) 0.0552(9) Uani 1 1 d . . . H15A H 0.6095 0.7483 0.9325 0.066 Uiso 1 1 calc R . . C16 C 1.0256(6) 0.7177(4) 0.7480(2) 0.0552(9) Uani 1 1 d . . . H16A H 1.1222 0.7485 0.7187 0.066 Uiso 1 1 calc R . . C17 C 0.8949(7) 0.5643(5) 0.8244(3) 0.0786(13) Uani 1 1 d . . . H17A H 0.8082 0.6192 0.8306 0.118 Uiso 1 1 calc R . . H17B H 0.9562 0.5745 0.8722 0.118 Uiso 1 1 calc R . . H17C H 0.8271 0.4640 0.8022 0.118 Uiso 1 1 calc R . . C18 C 1.1735(6) 0.5479(5) 0.7627(3) 0.0818(15) Uani 1 1 d . . . H18A H 1.2575 0.5938 0.7308 0.123 Uiso 1 1 calc R . . H18B H 1.1164 0.4471 0.7382 0.123 Uiso 1 1 calc R . . H18C H 1.2435 0.5578 0.8087 0.123 Uiso 1 1 calc R . . C19 C 1.1211(4) 1.0523(4) 0.63153(17) 0.0430(7) Uani 1 1 d . . . H19A H 1.0611 1.1184 0.6257 0.052 Uiso 1 1 calc R . . C20 C 1.3197(5) 0.9149(4) 0.58535(19) 0.0504(8) Uani 1 1 d . . . H20A H 1.2850 0.8788 0.6283 0.076 Uiso 1 1 calc R . . H20B H 1.4540 0.9616 0.5900 0.076 Uiso 1 1 calc R . . H20C H 1.2841 0.8359 0.5410 0.076 Uiso 1 1 calc R . . C21 C 1.2601(5) 1.0814(4) 0.52011(19) 0.0549(9) Uani 1 1 d . . . H21A H 1.1886 1.1474 0.5234 0.082 Uiso 1 1 calc R . . H21B H 1.2224 1.0083 0.4735 0.082 Uiso 1 1 calc R . . H21C H 1.3925 1.1333 0.5227 0.082 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Dy1 0.02805(7) 0.03752(8) 0.03206(8) 0.01481(5) 0.00797(5) 0.01752(5) N1 0.0250(10) 0.0411(12) 0.0372(12) 0.0131(10) 0.0043(9) 0.0142(9) N2 0.0262(11) 0.0459(13) 0.0425(13) 0.0171(11) 0.0114(10) 0.0154(10) N4 0.076(2) 0.0326(13) 0.0507(18) 0.0131(12) -0.0085(15) 0.0138(14) N3 0.0292(13) 0.075(2) 0.0431(15) 0.0007(14) 0.0037(11) 0.0186(13) N5 0.0525(16) 0.0329(12) 0.0545(17) 0.0109(12) -0.0069(13) 0.0175(11) N6 0.0315(12) 0.0647(16) 0.0353(13) 0.0211(12) 0.0092(10) 0.0185(12) O1 0.0386(10) 0.0422(10) 0.0412(11) 0.0208(9) 0.0088(8) 0.0219(9) O2 0.0623(15) 0.0529(13) 0.0566(15) 0.0352(11) 0.0177(12) 0.0171(11) O3 0.0333(10) 0.0645(13) 0.0400(11) 0.0256(10) 0.0118(8) 0.0231(10) O4 0.0519(14) 0.0438(12) 0.0568(15) 0.0175(11) -0.0014(11) 0.0115(10) O5 0.0837(19) 0.0500(13) 0.0378(12) 0.0144(10) 0.0091(12) 0.0195(13) O6 0.120(3) 0.0427(14) 0.0650(18) 0.0054(13) -0.0331(18) 0.0076(15) O7 0.0413(12) 0.0557(14) 0.0626(16) 0.0032(12) -0.0043(11) 0.0204(11) O8 0.0350(11) 0.0793(17) 0.0436(12) 0.0237(12) 0.0084(9) 0.0260(11) O9 0.0478(16) 0.117(3) 0.083(2) -0.025(2) -0.0188(15) 0.0160(17) O10 0.0730(16) 0.0552(13) 0.0598(15) 0.0288(11) 0.0187(12) 0.0439(13) O11 0.0349(11) 0.0791(15) 0.0433(12) 0.0334(11) 0.0171(9) 0.0301(11) C1 0.0350(14) 0.0310(13) 0.0405(15) 0.0110(11) -0.0050(12) 0.0077(11) C2 0.0439(16) 0.0330(14) 0.0454(17) 0.0167(12) -0.0041(13) 0.0070(12) C3 0.062(2) 0.0399(16) 0.075(3) 0.0299(17) -0.0020(19) 0.0125(15) C4 0.063(2) 0.055(2) 0.116(4) 0.044(2) 0.008(2) 0.0323(19) C5 0.050(2) 0.0510(19) 0.101(3) 0.034(2) 0.011(2) 0.0299(17) C6 0.0355(14) 0.0346(14) 0.0544(18) 0.0141(13) 0.0014(13) 0.0166(12) C7 0.092(3) 0.068(2) 0.078(3) 0.049(2) 0.027(2) 0.017(2) C8 0.0288(13) 0.0368(14) 0.0535(18) 0.0124(13) 0.0066(12) 0.0138(11) C9 0.0326(14) 0.0462(15) 0.0310(14) 0.0083(12) 0.0031(11) 0.0138(12) C10 0.0368(14) 0.0443(15) 0.0301(14) 0.0077(12) 0.0008(11) 0.0084(12) C11 0.0425(17) 0.065(2) 0.0420(17) 0.0168(15) 0.0112(14) 0.0194(15) C12 0.051(2) 0.087(3) 0.050(2) 0.026(2) 0.0199(16) 0.016(2) C13 0.065(2) 0.078(3) 0.047(2) 0.0286(19) 0.0170(18) 0.010(2) C14 0.072(3) 0.081(3) 0.059(2) 0.036(2) 0.014(2) 0.028(2) C15 0.053(2) 0.072(2) 0.053(2) 0.0316(18) 0.0139(16) 0.0256(18) C16 0.067(2) 0.0541(19) 0.053(2) 0.0186(16) 0.0097(17) 0.0281(18) C17 0.092(3) 0.070(3) 0.067(3) 0.019(2) 0.007(2) 0.014(2) C18 0.070(3) 0.075(3) 0.107(4) 0.014(3) -0.006(3) 0.040(3) C19 0.0311(14) 0.067(2) 0.0421(16) 0.0253(15) 0.0111(12) 0.0228(14) C20 0.0458(18) 0.066(2) 0.0433(18) 0.0122(16) 0.0081(14) 0.0252(16) C21 0.0493(19) 0.079(2) 0.0441(18) 0.0302(17) 0.0196(15) 0.0197(18) _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 2.2305(19) . ? Dy1 O10 2.327(2) . ? Dy1 O11 2.345(2) . ? Dy1 O3 2.384(2) . ? Dy1 O4 2.447(2) . ? Dy1 O7 2.479(2) . ? Dy1 O5 2.491(2) . ? Dy1 N1 2.533(2) . ? Dy1 O8 2.535(2) . ? Dy1 N4 2.896(3) . ? Dy1 N3 2.925(3) . ? N1 C8 1.286(4) . ? N1 N2 1.384(3) . ? N2 C9 1.345(4) . ? N4 O6 1.218(4) . ? N4 O5 1.250(4) . ? N4 O4 1.273(4) . ? N3 O9 1.227(4) . ? N3 O7 1.249(4) . ? N3 O8 1.269(4) . ? N5 C16 1.324(4) . ? N5 C17 1.412(6) . ? N5 C18 1.457(5) . ? N6 C19 1.316(4) . ? N6 C20 1.437(4) . ? N6 C21 1.454(4) . ? O1 C1 1.293(3) . ? O2 C2 1.369(4) . ? O2 C7 1.443(4) . ? O3 C9 1.250(3) . ? O10 C16 1.218(4) . ? O11 C19 1.246(4) . ? C1 C6 1.404(4) . ? C1 C2 1.429(4) . ? C2 C3 1.369(5) . ? C3 C4 1.411(6) . ? C4 C5 1.339(6) . ? C5 C6 1.416(4) . ? C6 C8 1.440(4) . ? C9 C10 1.480(4) . ? C10 C11 1.386(4) . ? C10 C15 1.389(5) . ? C11 C12 1.378(5) . ? C12 C13 1.374(6) . ? C13 C14 1.393(6) . ? C14 C15 1.374(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 O1 Dy1 O10 149.88(8) . . ? O1 Dy1 O11 78.78(7) . . ? O10 Dy1 O11 79.03(9) . . ? O1 Dy1 O3 133.73(7) . . ? O10 Dy1 O3 74.25(8) . . ? O11 Dy1 O3 144.17(7) . . ? O1 Dy1 O4 94.21(8) . . ? O10 Dy1 O4 81.44(9) . . ? O11 Dy1 O4 123.57(9) . . ? O3 Dy1 O4 75.57(8) . . ? O1 Dy1 O7 75.57(8) . . ? O10 Dy1 O7 122.88(9) . . ? O11 Dy1 O7 86.38(8) . . ? O3 Dy1 O7 88.46(8) . . ? O4 Dy1 O7 146.37(8) . . ? O1 Dy1 O5 78.02(8) . . ? O10 Dy1 O5 76.12(9) . . ? O11 Dy1 O5 72.73(9) . . ? O3 Dy1 O5 121.85(8) . . ? O4 Dy1 O5 51.25(9) . . ? O7 Dy1 O5 149.00(9) . . ? O1 Dy1 N1 70.34(7) . . ? O10 Dy1 N1 134.25(8) . . ? O11 Dy1 N1 146.70(8) . . ? O3 Dy1 N1 63.55(7) . . ? O4 Dy1 N1 72.03(8) . . ? O7 Dy1 N1 74.37(7) . . ? O5 Dy1 N1 111.37(9) . . ? O1 Dy1 O8 119.56(8) . . ? O10 Dy1 O8 72.37(9) . . ? O11 Dy1 O8 73.26(7) . . ? O3 Dy1 O8 76.17(7) . . ? O4 Dy1 O8 145.63(8) . . ? O7 Dy1 O8 50.57(8) . . ? O5 Dy1 O8 137.08(9) . . ? N1 Dy1 O8 111.46(7) . . ? O1 Dy1 N4 84.84(8) . . ? O10 Dy1 N4 78.39(9) . . ? O11 Dy1 N4 98.06(10) . . ? O3 Dy1 N4 99.44(9) . . ? O4 Dy1 N4 25.85(9) . . ? O7 Dy1 N4 158.71(8) . . ? O5 Dy1 N4 25.42(9) . . ? N1 Dy1 N4 91.40(9) . . ? O8 Dy1 N4 150.55(8) . . ? O1 Dy1 N3 96.85(9) . . ? O10 Dy1 N3 97.99(9) . . ? O11 Dy1 N3 77.61(8) . . ? O3 Dy1 N3 82.90(8) . . ? O4 Dy1 N3 157.81(9) . . ? O7 Dy1 N3 25.02(8) . . ? O5 Dy1 N3 150.34(9) . . ? N1 Dy1 N3 93.71(8) . . ? O8 Dy1 N3 25.62(8) . . ? N4 Dy1 N3 174.89(8) . . ? C8 N1 N2 114.0(2) . . ? C8 N1 Dy1 131.4(2) . . ? N2 N1 Dy1 114.55(16) . . ? C9 N2 N1 116.6(2) . . ? O6 N4 O5 122.7(4) . . ? O6 N4 O4 121.6(4) . . ? O5 N4 O4 115.7(3) . . ? O6 N4 Dy1 177.0(3) . . ? O5 N4 Dy1 58.84(16) . . ? O4 N4 Dy1 56.99(15) . . ? O9 N3 O7 122.2(4) . . ? O9 N3 O8 121.1(3) . . ? O7 N3 O8 116.6(3) . . ? O9 N3 Dy1 175.5(3) . . ? O7 N3 Dy1 57.10(15) . . ? O8 N3 Dy1 59.75(15) . . ? C16 N5 C17 122.2(4) . . ? C16 N5 C18 119.6(4) . . ? C17 N5 C18 118.1(3) . . ? C19 N6 C20 121.1(3) . . ? C19 N6 C21 121.0(3) . . ? C20 N6 C21 117.8(3) . . ? C1 O1 Dy1 144.92(19) . . ? C2 O2 C7 116.7(3) . . ? C9 O3 Dy1 123.47(19) . . ? N4 O4 Dy1 97.2(2) . . ? N4 O5 Dy1 95.74(19) . . ? N3 O7 Dy1 97.9(2) . . ? N3 O8 Dy1 94.63(17) . . ? C16 O10 Dy1 146.5(3) . . ? C19 O11 Dy1 124.60(18) . . ? O1 C1 C6 122.5(3) . . ? O1 C1 C2 121.2(3) . . ? C6 C1 C2 116.3(3) . . ? O2 C2 C3 124.3(3) . . ? O2 C2 C1 113.8(3) . . ? C3 C2 C1 121.9(3) . . ? C2 C3 C4 120.5(3) . . ? C5 C4 C3 118.5(3) . . ? C4 C5 C6 122.6(4) . . ? C1 C6 C5 120.0(3) . . ? C1 C6 C8 122.3(3) . . ? C5 C6 C8 117.7(3) . . ? N1 C8 C6 126.8(3) . . ? O3 C9 N2 119.9(3) . . ? O3 C9 C10 121.8(3) . . ? N2 C9 C10 118.2(3) . . ? C11 C10 C15 119.5(3) . . ? C11 C10 C9 123.1(3) . . ? C15 C10 C9 117.4(3) . . ? C12 C11 C10 120.4(4) . . ? C13 C12 C11 120.4(4) . . ? C12 C13 C14 119.2(4) . . ? C15 C14 C13 120.8(4) . . ? C14 C15 C10 119.6(4) . . ? O10 C16 N5 124.1(4) . . ? O11 C19 N6 124.1(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Dy1 N1 C8 -6.0(3) . . . . ? O10 Dy1 N1 C8 -165.1(2) . . . . ? O11 Dy1 N1 C8 17.0(3) . . . . ? O3 Dy1 N1 C8 170.1(3) . . . . ? O4 Dy1 N1 C8 -107.4(3) . . . . ? O7 Dy1 N1 C8 73.9(3) . . . . ? O5 Dy1 N1 C8 -73.9(3) . . . . ? O8 Dy1 N1 C8 109.0(3) . . . . ? N4 Dy1 N1 C8 -90.0(3) . . . . ? N3 Dy1 N1 C8 89.9(3) . . . . ? O1 Dy1 N1 N2 173.14(19) . . . . ? O10 Dy1 N1 N2 14.0(2) . . . . ? O11 Dy1 N1 N2 -163.87(16) . . . . ? O3 Dy1 N1 N2 -10.73(16) . . . . ? O4 Dy1 N1 N2 71.73(18) . . . . ? O7 Dy1 N1 N2 -106.93(19) . . . . ? O5 Dy1 N1 N2 105.26(18) . . . . ? O8 Dy1 N1 N2 -71.87(19) . . . . ? N4 Dy1 N1 N2 89.12(18) . . . . ? N3 Dy1 N1 N2 -90.90(18) . . . . ? C8 N1 N2 C9 -170.5(3) . . . . ? Dy1 N1 N2 C9 10.2(3) . . . . ? O1 Dy1 N4 O6 -48(5) . . . . ? O10 Dy1 N4 O6 157(5) . . . . ? O11 Dy1 N4 O6 -126(5) . . . . ? O3 Dy1 N4 O6 85(5) . . . . ? O4 Dy1 N4 O6 63(5) . . . . ? O7 Dy1 N4 O6 -25(6) . . . . ? O5 Dy1 N4 O6 -121(5) . . . . ? N1 Dy1 N4 O6 22(5) . . . . ? O8 Dy1 N4 O6 164(5) . . . . ? N3 Dy1 N4 O6 -158(5) . . . . ? O1 Dy1 N4 O5 72.80(19) . . . . ? O10 Dy1 N4 O5 -82.04(19) . . . . ? O11 Dy1 N4 O5 -5.07(19) . . . . ? O3 Dy1 N4 O5 -153.68(18) . . . . ? O4 Dy1 N4 O5 -176.4(3) . . . . ? O7 Dy1 N4 O5 95.8(3) . . . . ? N1 Dy1 N4 O5 142.92(19) . . . . ? O8 Dy1 N4 O5 -75.1(2) . . . . ? N3 Dy1 N4 O5 -36.8(10) . . . . ? O1 Dy1 N4 O4 -110.83(18) . . . . ? O10 Dy1 N4 O4 94.33(18) . . . . ? O11 Dy1 N4 O4 171.30(17) . . . . ? O3 Dy1 N4 O4 22.69(19) . . . . ? O7 Dy1 N4 O4 -87.9(3) . . . . ? O5 Dy1 N4 O4 176.4(3) . . . . ? N1 Dy1 N4 O4 -40.71(18) . . . . ? O8 Dy1 N4 O4 101.2(2) . . . . ? N3 Dy1 N4 O4 139.5(9) . . . . ? O1 Dy1 N3 O9 -51(4) . . . . ? O10 Dy1 N3 O9 103(4) . . . . ? O11 Dy1 N3 O9 26(4) . . . . ? O3 Dy1 N3 O9 176(4) . . . . ? O4 Dy1 N3 O9 -170(4) . . . . ? O7 Dy1 N3 O9 -83(4) . . . . ? O5 Dy1 N3 O9 27(4) . . . . ? N1 Dy1 N3 O9 -122(4) . . . . ? O8 Dy1 N3 O9 103(4) . . . . ? N4 Dy1 N3 O9 58(4) . . . . ? O1 Dy1 N3 O7 31.7(2) . . . . ? O10 Dy1 N3 O7 -174.6(2) . . . . ? O11 Dy1 N3 O7 108.5(2) . . . . ? O3 Dy1 N3 O7 -101.7(2) . . . . ? O4 Dy1 N3 O7 -87.7(3) . . . . ? O5 Dy1 N3 O7 109.5(2) . . . . ? N1 Dy1 N3 O7 -39.0(2) . . . . ? O8 Dy1 N3 O7 -174.4(3) . . . . ? N4 Dy1 N3 O7 140.8(9) . . . . ? O1 Dy1 N3 O8 -153.93(17) . . . . ? O10 Dy1 N3 O8 -0.22(18) . . . . ? O11 Dy1 N3 O8 -77.06(17) . . . . ? O3 Dy1 N3 O8 72.70(17) . . . . ? O4 Dy1 N3 O8 86.7(3) . . . . ? O7 Dy1 N3 O8 174.4(3) . . . . ? O5 Dy1 N3 O8 -76.1(3) . . . . ? N1 Dy1 N3 O8 135.44(17) . . . . ? N4 Dy1 N3 O8 -44.8(10) . . . . ? O10 Dy1 O1 C1 166.4(3) . . . . ? O11 Dy1 O1 C1 -150.4(3) . . . . ? O3 Dy1 O1 C1 12.1(4) . . . . ? O4 Dy1 O1 C1 86.2(3) . . . . ? O7 Dy1 O1 C1 -61.3(3) . . . . ? O5 Dy1 O1 C1 135.1(3) . . . . ? N1 Dy1 O1 C1 16.9(3) . . . . ? O8 Dy1 O1 C1 -87.2(3) . . . . ? N4 Dy1 O1 C1 110.3(3) . . . . ? N3 Dy1 O1 C1 -74.6(3) . . . . ? O1 Dy1 O3 C9 17.1(3) . . . . ? O10 Dy1 O3 C9 -149.7(2) . . . . ? O11 Dy1 O3 C9 167.0(2) . . . . ? O4 Dy1 O3 C9 -64.7(2) . . . . ? O7 Dy1 O3 C9 85.4(2) . . . . ? O5 Dy1 O3 C9 -87.7(2) . . . . ? N1 Dy1 O3 C9 12.1(2) . . . . ? O8 Dy1 O3 C9 135.0(2) . . . . ? N4 Dy1 O3 C9 -74.7(2) . . . . ? N3 Dy1 O3 C9 109.9(2) . . . . ? O6 N4 O4 Dy1 -176.9(3) . . . . ? O5 N4 O4 Dy1 3.4(3) . . . . ? O1 Dy1 O4 N4 68.97(18) . . . . ? O10 Dy1 O4 N4 -81.03(18) . . . . ? O11 Dy1 O4 N4 -10.4(2) . . . . ? O3 Dy1 O4 N4 -156.86(19) . . . . ? O7 Dy1 O4 N4 139.1(2) . . . . ? O5 Dy1 O4 N4 -2.00(17) . . . . ? N1 Dy1 O4 N4 136.72(19) . . . . ? O8 Dy1 O4 N4 -121.32(19) . . . . ? N3 Dy1 O4 N4 -171.2(2) . . . . ? O6 N4 O5 Dy1 176.9(3) . . . . ? O4 N4 O5 Dy1 -3.4(3) . . . . ? O1 Dy1 O5 N4 -103.44(19) . . . . ? O10 Dy1 O5 N4 92.13(19) . . . . ? O11 Dy1 O5 N4 174.7(2) . . . . ? O3 Dy1 O5 N4 31.0(2) . . . . ? O4 Dy1 O5 N4 2.03(17) . . . . ? O7 Dy1 O5 N4 -135.46(19) . . . . ? N1 Dy1 O5 N4 -40.3(2) . . . . ? O8 Dy1 O5 N4 135.75(19) . . . . ? N3 Dy1 O5 N4 173.81(18) . . . . ? O9 N3 O7 Dy1 174.8(3) . . . . ? O8 N3 O7 Dy1 -5.4(3) . . . . ? O1 Dy1 O7 N3 -147.4(2) . . . . ? O10 Dy1 O7 N3 6.3(2) . . . . ? O11 Dy1 O7 N3 -68.1(2) . . . . ? O3 Dy1 O7 N3 76.4(2) . . . . ? O4 Dy1 O7 N3 137.03(19) . . . . ? O5 Dy1 O7 N3 -115.1(2) . . . . ? N1 Dy1 O7 N3 139.3(2) . . . . ? O8 Dy1 O7 N3 3.13(18) . . . . ? N4 Dy1 O7 N3 -171.1(2) . . . . ? O9 N3 O8 Dy1 -174.9(3) . . . . ? O7 N3 O8 Dy1 5.3(3) . . . . ? O1 Dy1 O8 N3 30.10(19) . . . . ? O10 Dy1 O8 N3 179.77(19) . . . . ? O11 Dy1 O8 N3 96.26(18) . . . . ? O3 Dy1 O8 N3 -102.65(18) . . . . ? O4 Dy1 O8 N3 -138.09(19) . . . . ? O7 Dy1 O8 N3 -3.06(17) . . . . ? O5 Dy1 O8 N3 135.13(18) . . . . ? N1 Dy1 O8 N3 -48.79(19) . . . . ? N4 Dy1 O8 N3 172.67(18) . . . . ? O1 Dy1 O10 C16 52.9(5) . . . . ? O11 Dy1 O10 C16 9.7(5) . . . . ? O3 Dy1 O10 C16 -146.2(5) . . . . ? O4 Dy1 O10 C16 136.5(5) . . . . ? O7 Dy1 O10 C16 -68.7(5) . . . . ? O5 Dy1 O10 C16 84.4(5) . . . . ? N1 Dy1 O10 C16 -169.1(4) . . . . ? O8 Dy1 O10 C16 -66.1(5) . . . . ? N4 Dy1 O10 C16 110.4(5) . . . . ? N3 Dy1 O10 C16 -66.0(5) . . . . ? O1 Dy1 O11 C19 -17.7(3) . . . . ? O10 Dy1 O11 C19 141.8(3) . . . . ? O3 Dy1 O11 C19 -176.0(2) . . . . ? O4 Dy1 O11 C19 69.9(3) . . . . ? O7 Dy1 O11 C19 -93.7(3) . . . . ? O5 Dy1 O11 C19 63.1(3) . . . . ? N1 Dy1 O11 C19 -39.8(3) . . . . ? O8 Dy1 O11 C19 -143.5(3) . . . . ? N4 Dy1 O11 C19 65.3(3) . . . . ? N3 Dy1 O11 C19 -117.4(3) . . . . ? Dy1 O1 C1 C6 -19.1(5) . . . . ? Dy1 O1 C1 C2 161.2(2) . . . . ? C7 O2 C2 C3 8.2(5) . . . . ? C7 O2 C2 C1 -172.0(3) . . . . ? O1 C1 C2 O2 -3.9(4) . . . . ? C6 C1 C2 O2 176.3(3) . . . . ? O1 C1 C2 C3 175.9(3) . . . . ? C6 C1 C2 C3 -3.8(4) . . . . ? O2 C2 C3 C4 -179.2(3) . . . . ? C1 C2 C3 C4 0.9(5) . . . . ? C2 C3 C4 C5 1.0(6) . . . . ? C3 C4 C5 C6 0.2(7) . . . . ? O1 C1 C6 C5 -174.9(3) . . . . ? C2 C1 C6 C5 4.8(4) . . . . ? O1 C1 C6 C8 3.8(5) . . . . ? C2 C1 C6 C8 -176.5(3) . . . . ? C4 C5 C6 C1 -3.2(6) . . . . ? C4 C5 C6 C8 178.1(4) . . . . ? N2 N1 C8 C6 -178.7(3) . . . . ? Dy1 N1 C8 C6 0.5(5) . . . . ? C1 C6 C8 N1 3.0(5) . . . . ? C5 C6 C8 N1 -178.3(3) . . . . ? Dy1 O3 C9 N2 -11.8(4) . . . . ? Dy1 O3 C9 C10 167.0(2) . . . . ? N1 N2 C9 O3 0.0(4) . . . . ? N1 N2 C9 C10 -178.9(2) . . . . ? O3 C9 C10 C11 179.0(3) . . . . ? N2 C9 C10 C11 -2.1(4) . . . . ? O3 C9 C10 C15 -1.2(4) . . . . ? N2 C9 C10 C15 177.6(3) . . . . ? C15 C10 C11 C12 -0.1(5) . . . . ? C9 C10 C11 C12 179.6(3) . . . . ? C10 C11 C12 C13 -0.8(6) . . . . ? C11 C12 C13 C14 1.7(6) . . . . ? C12 C13 C14 C15 -1.8(7) . . . . ? C13 C14 C15 C10 0.9(6) . . . . ? C11 C10 C15 C14 0.1(5) . . . . ? C9 C10 C15 C14 -179.6(3) . . . . ? Dy1 O10 C16 N5 162.7(3) . . . . ? C17 N5 C16 O10 -1.7(6) . . . . ? C18 N5 C16 O10 176.6(4) . . . . ? Dy1 O11 C19 N6 -147.4(3) . . . . ? C20 N6 C19 O11 0.4(5) . . . . ? C21 N6 C19 O11 -175.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.339 _refine_diff_density_min -0.764 _refine_diff_density_rms 0.082