# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Shi-Ping Yan' _publ_contact_author_email yansp@nankai.edu.cn _publ_author_name 'Shi-Ping Yan' data_a _database_code_depnum_ccdc_archive 'CCDC 801063' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H29 Dy N2 O6 ' _chemical_formula_weight 640.02 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 monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.5010(19) _cell_length_b 21.015(4) _cell_length_c 16.246(5) _cell_angle_alpha 90.00 _cell_angle_beta 116.52(2) _cell_angle_gamma 90.00 _cell_volume 2902.4(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 prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.465 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1276 _exptl_absorpt_coefficient_mu 2.613 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.461 _exptl_absorpt_correction_T_max 0.609 _exptl_absorpt_process_details crystalclear _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 P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20794 _diffrn_reflns_av_R_equivalents 0.0504 _diffrn_reflns_av_sigmaI/netI 0.0534 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6647 _reflns_number_gt 4853 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0344P)^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 6609 _refine_ls_number_parameters 331 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0656 _refine_ls_R_factor_gt 0.0396 _refine_ls_wR_factor_ref 0.0820 _refine_ls_wR_factor_gt 0.0763 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 0.76142(2) 0.846645(8) 0.340635(12) 0.03888(8) Uani 1 1 d . . . O1 O 0.8264(4) 0.95364(13) 0.3477(2) 0.0562(8) Uani 1 1 d . . . O2 O 0.7142(3) 0.89093(13) 0.45597(19) 0.0517(7) Uani 1 1 d . . . O3 O 0.7568(4) 0.86539(14) 0.1988(2) 0.0615(9) Uani 1 1 d . . . O4 O 0.5135(4) 0.88845(14) 0.2459(2) 0.0619(8) Uani 1 1 d . . . O5 O 0.8349(4) 0.75033(13) 0.2999(2) 0.0583(8) Uani 1 1 d . . . O6 O 0.5931(3) 0.76897(13) 0.3477(2) 0.0563(8) Uani 1 1 d . . . N1 N 1.0572(4) 0.85097(14) 0.3895(2) 0.0428(8) Uani 1 1 d . . . N2 N 0.9421(4) 0.79234(14) 0.4952(2) 0.0419(8) Uani 1 1 d . . . C1 C 1.1149(6) 0.8809(2) 0.3400(3) 0.0559(12) Uani 1 1 d . . . H1 H 1.0474 0.9061 0.2914 0.067 Uiso 1 1 calc R . . C2 C 1.2724(6) 0.8767(3) 0.3568(4) 0.0652(15) Uani 1 1 d . . . H2 H 1.3079 0.8984 0.3197 0.078 Uiso 1 1 calc R . . C3 C 1.3711(6) 0.8408(2) 0.4269(4) 0.0712(16) Uani 1 1 d . . . H3 H 1.4757 0.8370 0.4381 0.085 Uiso 1 1 calc R . . C4 C 1.3181(5) 0.8094(2) 0.4832(3) 0.0591(12) Uani 1 1 d . . . C5 C 1.4171(6) 0.7722(3) 0.5618(4) 0.0880(18) Uani 1 1 d . . . H5 H 1.5226 0.7671 0.5756 0.106 Uiso 1 1 calc R . . C6 C 1.3623(7) 0.7446(3) 0.6157(4) 0.0879(18) Uani 1 1 d . . . H6 H 1.4305 0.7215 0.6669 0.106 Uiso 1 1 calc R . . C7 C 1.1994(7) 0.7499(2) 0.5958(3) 0.0650(13) Uani 1 1 d . . . C8 C 1.1363(8) 0.7244(3) 0.6518(4) 0.0825(17) Uani 1 1 d . . . H8 H 1.2005 0.7012 0.7038 0.099 Uiso 1 1 calc R . . C9 C 0.9848(8) 0.7332(2) 0.6312(4) 0.0792(17) Uani 1 1 d . . . H9 H 0.9437 0.7172 0.6693 0.095 Uiso 1 1 calc R . . C10 C 0.8891(6) 0.7670(2) 0.5513(3) 0.0567(12) Uani 1 1 d . . . H10 H 0.7833 0.7720 0.5367 0.068 Uiso 1 1 calc R . . C11 C 1.0961(5) 0.78480(18) 0.5182(3) 0.0438(10) Uani 1 1 d . . . C12 C 1.1579(5) 0.81549(19) 0.4616(3) 0.0430(10) Uani 1 1 d . . . C13 C 0.8418(8) 1.0652(2) 0.3554(4) 0.0901(19) Uani 1 1 d . . . H13A H 0.9440 1.0792 0.3995 0.135 Uiso 1 1 calc R . . H13B H 0.7644 1.0960 0.3513 0.135 Uiso 1 1 calc R . . H13C H 0.8407 1.0605 0.2963 0.135 Uiso 1 1 calc R . . C14 C 0.8046(6) 1.0021(2) 0.3854(3) 0.0580(12) Uani 1 1 d . . . C15 C 0.7535(6) 1.0008(2) 0.4530(4) 0.0692(14) Uani 1 1 d . . . H15 H 0.7430 1.0396 0.4773 0.083 Uiso 1 1 calc R . . C16 C 0.7172(5) 0.9467(2) 0.4869(3) 0.0571(12) Uani 1 1 d . . . C17 C 0.6810(6) 0.9499(3) 0.5690(3) 0.0811(16) Uani 1 1 d . . . H17A H 0.5889 0.9251 0.5566 0.122 Uiso 1 1 calc R . . H17B H 0.6626 0.9934 0.5798 0.122 Uiso 1 1 calc R . . H17C H 0.7686 0.9334 0.6225 0.122 Uiso 1 1 calc R . . C18 C 0.7600(9) 0.9233(3) 0.0748(4) 0.117(3) Uani 1 1 d . . . H18A H 0.8258 0.9600 0.0992 0.175 Uiso 1 1 calc R . . H18B H 0.6798 0.9325 0.0141 0.175 Uiso 1 1 calc R . . H18C H 0.8226 0.8882 0.0723 0.175 Uiso 1 1 calc R . . C19 C 0.6836(7) 0.9061(3) 0.1366(3) 0.0717(15) Uani 1 1 d . . . C20 C 0.5444(7) 0.9349(3) 0.1233(4) 0.0919(19) Uani 1 1 d . . . H20 H 0.4995 0.9636 0.0750 0.110 Uiso 1 1 calc R . . C21 C 0.4669(7) 0.9241(3) 0.1765(4) 0.0836(17) Uani 1 1 d . . . C22 C 0.3082(8) 0.9581(4) 0.1517(5) 0.154(4) Uani 1 1 d . . . H22A H 0.2245 0.9275 0.1294 0.231 Uiso 1 1 calc R . . H22B H 0.2898 0.9894 0.1049 0.231 Uiso 1 1 calc R . . H22C H 0.3119 0.9786 0.2055 0.231 Uiso 1 1 calc R . . C23 C 0.9305(10) 0.6463(2) 0.3061(6) 0.121(3) Uani 1 1 d . . . H23A H 0.9058 0.6406 0.2424 0.181 Uiso 1 1 calc R . . H23B H 0.9233 0.6061 0.3321 0.181 Uiso 1 1 calc R . . H23C H 1.0354 0.6627 0.3387 0.181 Uiso 1 1 calc R . . C24 C 0.8166(7) 0.6923(2) 0.3138(3) 0.0670(14) Uani 1 1 d . . . C25 C 0.6972(8) 0.6709(2) 0.3350(4) 0.0763(16) Uani 1 1 d . . . H25 H 0.6896 0.6272 0.3413 0.092 Uiso 1 1 calc R . . C26 C 0.5909(6) 0.7085(2) 0.3472(3) 0.0653(13) Uani 1 1 d . . . C27 C 0.4592(7) 0.6778(3) 0.3606(5) 0.102(2) Uani 1 1 d . . . H27A H 0.4796 0.6818 0.4238 0.152 Uiso 1 1 calc R . . H27B H 0.4525 0.6336 0.3445 0.152 Uiso 1 1 calc R . . H27C H 0.3617 0.6985 0.3221 0.152 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 0.04027(13) 0.03837(11) 0.03699(12) -0.00163(9) 0.01635(10) -0.00025(9) O1 0.064(2) 0.0441(17) 0.068(2) -0.0051(15) 0.0362(18) -0.0033(15) O2 0.053(2) 0.0523(17) 0.0553(19) -0.0083(14) 0.0289(17) 0.0009(15) O3 0.083(3) 0.0641(19) 0.0400(17) 0.0122(15) 0.0301(19) 0.0204(18) O4 0.051(2) 0.066(2) 0.061(2) 0.0209(17) 0.0186(18) 0.0111(17) O5 0.072(2) 0.0472(18) 0.061(2) -0.0084(15) 0.0349(19) 0.0032(16) O6 0.053(2) 0.0485(18) 0.063(2) -0.0062(15) 0.0217(17) -0.0114(15) N1 0.047(2) 0.0445(19) 0.0407(19) -0.0012(16) 0.0226(19) -0.0045(17) N2 0.045(2) 0.0436(19) 0.0362(19) 0.0035(15) 0.0172(18) -0.0003(16) C1 0.066(3) 0.062(3) 0.050(3) -0.005(2) 0.036(3) -0.016(3) C2 0.070(4) 0.076(3) 0.071(4) -0.022(3) 0.050(3) -0.029(3) C3 0.053(3) 0.087(4) 0.090(4) -0.027(3) 0.046(4) -0.020(3) C4 0.041(3) 0.068(3) 0.061(3) -0.016(3) 0.017(3) -0.004(2) C5 0.037(3) 0.107(5) 0.096(5) -0.005(4) 0.009(3) 0.016(3) C6 0.055(4) 0.097(4) 0.069(4) 0.015(3) -0.011(3) 0.022(3) C7 0.070(4) 0.060(3) 0.047(3) 0.007(2) 0.010(3) 0.007(3) C8 0.098(5) 0.076(4) 0.053(3) 0.021(3) 0.016(4) -0.005(4) C9 0.120(5) 0.074(4) 0.053(3) 0.009(3) 0.047(4) -0.019(4) C10 0.067(3) 0.061(3) 0.048(3) 0.005(2) 0.032(3) -0.005(2) C11 0.047(3) 0.043(2) 0.036(2) -0.0040(18) 0.014(2) -0.001(2) C12 0.041(3) 0.043(2) 0.045(3) -0.0102(19) 0.019(2) -0.0036(19) C13 0.110(5) 0.047(3) 0.114(5) -0.001(3) 0.051(4) -0.009(3) C14 0.057(3) 0.038(2) 0.067(3) -0.005(2) 0.017(3) 0.000(2) C15 0.082(4) 0.048(3) 0.082(4) -0.016(3) 0.040(3) 0.004(3) C16 0.049(3) 0.068(3) 0.050(3) -0.014(2) 0.018(2) 0.008(2) C17 0.088(4) 0.094(4) 0.069(4) -0.021(3) 0.043(3) 0.003(3) C18 0.162(7) 0.137(6) 0.085(5) 0.052(4) 0.086(5) 0.054(5) C19 0.091(4) 0.079(4) 0.048(3) 0.014(3) 0.033(3) 0.016(3) C20 0.097(5) 0.105(5) 0.074(4) 0.050(3) 0.038(4) 0.045(4) C21 0.072(4) 0.086(4) 0.087(4) 0.035(3) 0.030(4) 0.022(3) C22 0.112(6) 0.191(8) 0.176(8) 0.129(7) 0.080(6) 0.090(6) C23 0.171(8) 0.069(4) 0.152(7) -0.002(4) 0.099(7) 0.029(4) C24 0.088(4) 0.050(3) 0.060(3) -0.006(2) 0.031(3) 0.007(3) C25 0.104(5) 0.039(3) 0.091(4) -0.002(2) 0.048(4) -0.002(3) C26 0.072(4) 0.057(3) 0.055(3) -0.006(2) 0.018(3) -0.022(3) C27 0.091(5) 0.079(4) 0.134(6) 0.006(4) 0.049(5) -0.035(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O2 2.309(3) . ? Dy1 O3 2.318(3) . ? Dy1 O1 2.321(3) . ? Dy1 O6 2.324(3) . ? Dy1 O5 2.331(3) . ? Dy1 O4 2.335(3) . ? Dy1 N1 2.558(3) . ? Dy1 N2 2.589(3) . ? O1 C14 1.252(5) . ? O2 C16 1.271(5) . ? O3 C19 1.268(5) . ? O4 C21 1.257(6) . ? O5 C24 1.267(5) . ? O6 C26 1.271(5) . ? N1 C1 1.317(5) . ? N1 C12 1.358(5) . ? N2 C10 1.334(5) . ? N2 C11 1.348(5) . ? C1 C2 1.399(6) . ? C1 H1 0.9300 . ? C2 C3 1.338(7) . ? C2 H2 0.9300 . ? C3 C4 1.393(6) . ? C3 H3 0.9300 . ? C4 C12 1.407(6) . ? C4 C5 1.433(7) . ? C5 C6 1.336(7) . ? C5 H5 0.9300 . ? C6 C7 1.437(8) . ? C6 H6 0.9300 . ? C7 C8 1.400(7) . ? C7 C11 1.409(6) . ? C8 C9 1.338(8) . ? C8 H8 0.9300 . ? C9 C10 1.401(7) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.445(5) . ? C13 C14 1.507(6) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.386(6) . ? C15 C16 1.373(6) . ? C15 H15 0.9300 . ? C16 C17 1.521(6) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.522(7) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.380(7) . ? C20 C21 1.382(7) . ? C20 H20 0.9300 . ? C21 C22 1.551(8) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C24 1.498(7) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C25 1.398(8) . ? C25 C26 1.365(7) . ? C25 H25 0.9300 . ? C26 C27 1.508(7) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 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 O2 Dy1 O3 144.47(10) . . ? O2 Dy1 O1 73.33(9) . . ? O3 Dy1 O1 76.77(10) . . ? O2 Dy1 O6 81.69(10) . . ? O3 Dy1 O6 117.43(11) . . ? O1 Dy1 O6 148.42(10) . . ? O2 Dy1 O5 140.52(10) . . ? O3 Dy1 O5 74.96(10) . . ? O1 Dy1 O5 138.44(10) . . ? O6 Dy1 O5 72.80(10) . . ? O2 Dy1 O4 83.03(11) . . ? O3 Dy1 O4 73.46(11) . . ? O1 Dy1 O4 80.56(11) . . ? O6 Dy1 O4 77.46(10) . . ? O5 Dy1 O4 118.78(11) . . ? O2 Dy1 N1 108.59(10) . . ? O3 Dy1 N1 80.38(11) . . ? O1 Dy1 N1 73.68(10) . . ? O6 Dy1 N1 134.00(10) . . ? O5 Dy1 N1 72.06(10) . . ? O4 Dy1 N1 146.76(10) . . ? O2 Dy1 N2 71.08(10) . . ? O3 Dy1 N2 138.47(11) . . ? O1 Dy1 N2 109.41(10) . . ? O6 Dy1 N2 79.36(10) . . ? O5 Dy1 N2 74.91(10) . . ? O4 Dy1 N2 147.35(10) . . ? N1 Dy1 N2 63.50(10) . . ? C14 O1 Dy1 135.5(3) . . ? C16 O2 Dy1 135.6(3) . . ? C19 O3 Dy1 131.8(3) . . ? C21 O4 Dy1 131.5(3) . . ? C24 O5 Dy1 134.6(3) . . ? C26 O6 Dy1 135.4(3) . . ? C1 N1 C12 117.6(4) . . ? C1 N1 Dy1 121.8(3) . . ? C12 N1 Dy1 120.1(2) . . ? C10 N2 C11 117.2(4) . . ? C10 N2 Dy1 123.3(3) . . ? C11 N2 Dy1 119.2(2) . . ? N1 C1 C2 123.5(5) . . ? N1 C1 H1 118.2 . . ? C2 C1 H1 118.2 . . ? C3 C2 C1 118.9(5) . . ? C3 C2 H2 120.6 . . ? C1 C2 H2 120.6 . . ? C2 C3 C4 120.3(5) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C3 C4 C12 117.5(5) . . ? C3 C4 C5 123.9(5) . . ? C12 C4 C5 118.6(5) . . ? C6 C5 C4 121.9(5) . . ? C6 C5 H5 119.1 . . ? C4 C5 H5 119.1 . . ? C5 C6 C7 121.0(5) . . ? C5 C6 H6 119.5 . . ? C7 C6 H6 119.5 . . ? C8 C7 C11 116.9(5) . . ? C8 C7 C6 123.6(5) . . ? C11 C7 C6 119.5(5) . . ? C9 C8 C7 120.7(5) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C8 C9 C10 118.8(5) . . ? C8 C9 H9 120.6 . . ? C10 C9 H9 120.6 . . ? N2 C10 C9 123.3(5) . . ? N2 C10 H10 118.3 . . ? C9 C10 H10 118.3 . . ? N2 C11 C7 123.0(4) . . ? N2 C11 C12 118.0(4) . . ? C7 C11 C12 118.9(4) . . ? N1 C12 C4 122.2(4) . . ? N1 C12 C11 117.6(4) . . ? C4 C12 C11 120.2(4) . . ? C14 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C14 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O1 C14 C15 124.4(4) . . ? O1 C14 C13 116.3(4) . . ? C15 C14 C13 119.2(4) . . ? C16 C15 C14 125.0(4) . . ? C16 C15 H15 117.5 . . ? C14 C15 H15 117.5 . . ? O2 C16 C15 124.8(4) . . ? O2 C16 C17 114.4(4) . . ? C15 C16 C17 120.7(4) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 H18A 109.5 . . ? C19 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C19 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O3 C19 C20 124.5(5) . . ? O3 C19 C18 115.6(5) . . ? C20 C19 C18 119.9(5) . . ? C21 C20 C19 124.8(5) . . ? C21 C20 H20 117.6 . . ? C19 C20 H20 117.6 . . ? O4 C21 C20 125.9(5) . . ? O4 C21 C22 114.8(5) . . ? C20 C21 C22 119.3(5) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C24 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O5 C24 C25 123.0(5) . . ? O5 C24 C23 116.4(5) . . ? C25 C24 C23 120.6(5) . . ? C26 C25 C24 125.7(4) . . ? C26 C25 H25 117.1 . . ? C24 C25 H25 117.1 . . ? O6 C26 C25 124.7(5) . . ? O6 C26 C27 116.0(5) . . ? C25 C26 C27 119.3(5) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.710 _refine_diff_density_min -0.788 _refine_diff_density_rms 0.100 # Attachment '- 2.cif' data_a2 _database_code_depnum_ccdc_archive 'CCDC 801064' #TrackingRef '- 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H25 Dy N6 O9' _chemical_formula_weight 764.05 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 Monoclinic _symmetry_space_group_name_H-M P2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 11.193(2) _cell_length_b 9.5690(19) _cell_length_c 15.559(5) _cell_angle_alpha 90.00 _cell_angle_beta 123.63(2) _cell_angle_gamma 90.00 _cell_volume 1387.5(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9686 _cell_measurement_theta_min 6.10 _cell_measurement_theta_max 55.39 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.829 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 758 _exptl_absorpt_coefficient_mu 2.762 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6081 _exptl_absorpt_correction_T_max 0.6081 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'rigaku saturn CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 8161 _diffrn_reflns_av_R_equivalents 0.0371 _diffrn_reflns_av_sigmaI/netI 0.0353 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2460 _reflns_number_gt 2356 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'crystalclear(Rigaku/MSC Inc., 2005)' _computing_cell_refinement crystalclear _computing_data_reduction crystalclear _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^)+(0.0617P)^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 2460 _refine_ls_number_parameters 206 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0328 _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_ref 0.1034 _refine_ls_wR_factor_gt 0.1027 _refine_ls_goodness_of_fit_ref 1.318 _refine_ls_restrained_S_all 1.318 _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 0.5000 0.38597(3) 0.2500 0.02320(15) Uani 1 2 d S . . O4 O 0.7131(4) 0.3042(4) 0.2540(3) 0.0413(9) Uani 1 1 d . . . O5 O 0.5511(5) 0.3697(4) 0.1010(3) 0.0422(10) Uani 1 1 d . . . O6 O 0.7299(6) 0.2475(5) 0.1272(4) 0.0699(14) Uani 1 1 d . . . O10 O 0.5949(4) 0.1944(3) 0.3555(3) 0.0358(8) Uani 1 1 d . . . N1 N 0.3828(5) 0.6074(3) 0.2689(4) 0.0273(10) Uani 1 1 d . . . N2 N 0.2853(4) 0.4856(4) 0.0847(3) 0.0270(9) Uani 1 1 d . . . N5 N 0.6666(5) 0.3061(5) 0.1597(4) 0.0376(10) Uani 1 1 d . . . C1 C 0.4285(6) 0.6665(5) 0.3584(4) 0.0329(11) Uani 1 1 d . . . H1 H 0.5106 0.6309 0.4171 0.039 Uiso 1 1 calc R . . C2 C 0.3601(6) 0.7793(5) 0.3695(4) 0.0381(12) Uani 1 1 d . . . H2 H 0.3960 0.8178 0.4342 0.046 Uiso 1 1 calc R . . C3 C 0.2398(7) 0.8328(6) 0.2842(5) 0.0443(14) Uani 1 1 d . . . H3 H 0.1928 0.9085 0.2903 0.053 Uiso 1 1 calc R . . C4 C 0.1879(6) 0.7737(5) 0.1883(4) 0.0346(11) Uani 1 1 d . . . C5 C 0.0628(6) 0.8231(6) 0.0950(5) 0.0461(14) Uani 1 1 d . . . H5 H 0.0119 0.8976 0.0981 0.055 Uiso 1 1 calc R . . C6 C 0.2634(5) 0.6600(5) 0.1837(4) 0.0269(10) Uani 1 1 d . . . C7 C 0.0172(6) 0.7660(6) 0.0043(5) 0.0426(13) Uani 1 1 d . . . H7 H -0.0641 0.8012 -0.0551 0.051 Uiso 1 1 calc R . . C8 C 0.2121(6) 0.5978(5) 0.0865(4) 0.0276(11) Uani 1 1 d . . . C9 C 0.0918(6) 0.6513(6) -0.0027(4) 0.0333(11) Uani 1 1 d . . . C10 C 0.0454(6) 0.5871(6) -0.0961(5) 0.0403(14) Uani 1 1 d . . . H10 H -0.0353 0.6198 -0.1570 0.048 Uiso 1 1 calc R . . C11 C 0.1196(6) 0.4761(6) -0.0970(4) 0.0422(13) Uani 1 1 d . . . H11 H 0.0903 0.4322 -0.1591 0.051 Uiso 1 1 calc R . . C12 C 0.2384(6) 0.4280(6) -0.0062(4) 0.0347(11) Uani 1 1 d . . . H12 H 0.2878 0.3518 -0.0087 0.042 Uiso 1 1 calc R . . C25 C 0.6720(7) -0.0195(6) 0.4411(5) 0.0477(14) Uani 1 1 d . . . H25A H 0.6261 -0.0184 0.4780 0.071 Uiso 1 1 calc R . . H25B H 0.7667 0.0190 0.4839 0.071 Uiso 1 1 calc R . . H25C H 0.6781 -0.1139 0.4230 0.071 Uiso 1 1 calc R . . C26 C 0.5860(6) 0.0665(5) 0.3447(4) 0.0303(11) Uani 1 1 d . . . C27 C 0.5000 -0.0011(8) 0.2500 0.0371(17) Uani 1 2 d S . . H27 H 0.5000 -0.0983 0.2500 0.044 Uiso 1 2 calc SR . . O12 O 1.0000 0.0942(7) 0.2500 0.103(4) Uani 1 2 d S . . H12A H 0.9369 0.0402 0.1963 0.123 Uiso 1 1 d 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 0.0213(2) 0.0214(2) 0.0187(2) 0.000 0.00592(16) 0.000 O4 0.033(2) 0.052(2) 0.029(2) -0.0037(16) 0.0107(17) 0.0003(17) O5 0.041(3) 0.043(2) 0.029(2) -0.0014(15) 0.011(2) -0.0015(17) O6 0.070(3) 0.089(4) 0.076(3) -0.011(3) 0.055(3) 0.012(3) O10 0.041(2) 0.0269(19) 0.0284(19) 0.0028(14) 0.0123(17) 0.0017(15) N1 0.032(3) 0.027(2) 0.026(2) 0.0025(15) 0.019(2) 0.0024(15) N2 0.025(2) 0.031(2) 0.022(2) 0.0039(16) 0.0111(18) 0.0030(17) N5 0.032(3) 0.042(3) 0.039(3) -0.008(2) 0.020(2) -0.006(2) C1 0.039(3) 0.033(3) 0.028(3) 0.001(2) 0.020(2) -0.001(2) C2 0.049(3) 0.036(3) 0.039(3) -0.003(2) 0.030(3) 0.003(2) C3 0.056(4) 0.033(3) 0.062(4) 0.001(3) 0.043(4) 0.010(3) C4 0.032(3) 0.031(3) 0.046(3) 0.004(2) 0.025(3) 0.004(2) C5 0.039(3) 0.036(3) 0.060(4) 0.007(3) 0.026(3) 0.015(3) C6 0.025(3) 0.026(2) 0.030(3) 0.007(2) 0.015(2) 0.001(2) C7 0.031(3) 0.039(3) 0.045(3) 0.014(3) 0.013(3) 0.011(2) C8 0.023(3) 0.029(2) 0.031(3) 0.0069(19) 0.015(2) -0.0004(19) C9 0.024(3) 0.036(2) 0.034(3) 0.012(2) 0.012(2) 0.001(2) C10 0.029(3) 0.049(3) 0.028(3) 0.013(2) 0.006(3) -0.002(2) C11 0.039(3) 0.054(4) 0.021(3) 0.001(2) 0.008(2) -0.003(3) C12 0.033(3) 0.039(3) 0.025(3) 0.000(2) 0.011(2) 0.003(2) C25 0.058(4) 0.033(3) 0.037(3) 0.009(2) 0.017(3) 0.010(3) C26 0.031(3) 0.029(3) 0.030(3) 0.004(2) 0.016(2) 0.004(2) C27 0.044(5) 0.030(4) 0.031(4) 0.000 0.017(4) 0.000 O12 0.066(6) 0.036(4) 0.167(11) 0.000 0.040(7) 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 O10 2.292(3) 2_655 ? Dy1 O10 2.292(3) . ? Dy1 O4 2.479(4) 2_655 ? Dy1 O4 2.479(4) . ? Dy1 N2 2.540(4) 2_655 ? Dy1 N2 2.540(4) . ? Dy1 N1 2.593(4) 2_655 ? Dy1 N1 2.593(4) . ? Dy1 O5 2.682(4) 2_655 ? Dy1 O5 2.682(4) . ? O4 N5 1.256(6) . ? O5 N5 1.252(6) . ? O6 N5 1.213(6) . ? O10 C26 1.232(6) . ? N1 C1 1.317(7) . ? N1 C6 1.354(7) . ? N2 C12 1.326(6) . ? N2 C8 1.360(6) . ? C1 C2 1.387(7) . ? C1 H1 0.9300 . ? C2 C3 1.363(8) . ? C2 H2 0.9300 . ? C3 C4 1.388(8) . ? C3 H3 0.9300 . ? C4 C6 1.403(7) . ? C4 C5 1.428(8) . ? C5 C7 1.324(8) . ? C5 H5 0.9300 . ? C6 C8 1.418(8) . ? C7 C9 1.419(8) . ? C7 H7 0.9300 . ? C8 C9 1.390(8) . ? C9 C10 1.386(8) . ? C10 C11 1.353(8) . ? C10 H10 0.9300 . ? C11 C12 1.376(8) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C25 C26 1.501(7) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C27 1.394(6) . ? C27 C26 1.394(6) 2_655 ? C27 H27 0.9300 . ? O12 H12A 0.9001 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O10 Dy1 O10 73.76(18) 2_655 . ? O10 Dy1 O4 70.84(13) 2_655 2_655 ? O10 Dy1 O4 79.82(13) . 2_655 ? O10 Dy1 O4 79.82(13) 2_655 . ? O10 Dy1 O4 70.84(13) . . ? O4 Dy1 O4 143.20(18) 2_655 . ? O10 Dy1 N2 145.98(13) 2_655 2_655 ? O10 Dy1 N2 76.81(13) . 2_655 ? O4 Dy1 N2 120.09(12) 2_655 2_655 ? O4 Dy1 N2 74.67(12) . 2_655 ? O10 Dy1 N2 76.81(13) 2_655 . ? O10 Dy1 N2 145.98(13) . . ? O4 Dy1 N2 74.67(12) 2_655 . ? O4 Dy1 N2 120.09(12) . . ? N2 Dy1 N2 135.90(18) 2_655 . ? O10 Dy1 N1 129.45(13) 2_655 2_655 ? O10 Dy1 N1 132.21(14) . 2_655 ? O4 Dy1 N1 142.70(13) 2_655 2_655 ? O4 Dy1 N1 73.77(13) . 2_655 ? N2 Dy1 N1 63.49(14) 2_655 2_655 ? N2 Dy1 N1 80.38(14) . 2_655 ? O10 Dy1 N1 132.21(14) 2_655 . ? O10 Dy1 N1 129.45(13) . . ? O4 Dy1 N1 73.77(13) 2_655 . ? O4 Dy1 N1 142.70(13) . . ? N2 Dy1 N1 80.38(14) 2_655 . ? N2 Dy1 N1 63.49(13) . . ? N1 Dy1 N1 70.40(18) 2_655 . ? O10 Dy1 O5 109.66(12) 2_655 2_655 ? O10 Dy1 O5 64.56(12) . 2_655 ? O4 Dy1 O5 48.72(13) 2_655 2_655 ? O4 Dy1 O5 128.53(13) . 2_655 ? N2 Dy1 O5 71.43(13) 2_655 2_655 ? N2 Dy1 O5 111.23(13) . 2_655 ? N1 Dy1 O5 120.58(12) 2_655 2_655 ? N1 Dy1 O5 65.57(12) . 2_655 ? O10 Dy1 O5 64.56(12) 2_655 . ? O10 Dy1 O5 109.66(12) . . ? O4 Dy1 O5 128.53(13) 2_655 . ? O4 Dy1 O5 48.72(13) . . ? N2 Dy1 O5 111.23(13) 2_655 . ? N2 Dy1 O5 71.43(13) . . ? N1 Dy1 O5 65.57(12) 2_655 . ? N1 Dy1 O5 120.58(12) . . ? O5 Dy1 O5 173.33(15) 2_655 . ? N5 O4 Dy1 101.3(3) . . ? N5 O5 Dy1 91.5(3) . . ? C26 O10 Dy1 136.6(3) . . ? C1 N1 C6 118.1(4) . . ? C1 N1 Dy1 123.1(4) . . ? C6 N1 Dy1 118.7(3) . . ? C12 N2 C8 117.5(4) . . ? C12 N2 Dy1 121.2(3) . . ? C8 N2 Dy1 121.2(3) . . ? O6 N5 O5 121.8(5) . . ? O6 N5 O4 121.4(5) . . ? O5 N5 O4 116.9(4) . . ? N1 C1 C2 123.2(5) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C3 C2 C1 119.2(5) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? C2 C3 C4 119.5(5) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C3 C4 C6 117.8(5) . . ? C3 C4 C5 123.3(5) . . ? C6 C4 C5 119.0(5) . . ? C7 C5 C4 121.9(5) . . ? C7 C5 H5 119.0 . . ? C4 C5 H5 119.0 . . ? N1 C6 C4 122.3(5) . . ? N1 C6 C8 119.0(4) . . ? C4 C6 C8 118.7(5) . . ? C5 C7 C9 120.4(5) . . ? C5 C7 H7 119.8 . . ? C9 C7 H7 119.8 . . ? N2 C8 C9 122.2(5) . . ? N2 C8 C6 117.4(5) . . ? C9 C8 C6 120.4(5) . . ? C10 C9 C8 118.4(5) . . ? C10 C9 C7 121.9(5) . . ? C8 C9 C7 119.6(5) . . ? C11 C10 C9 118.9(5) . . ? C11 C10 H10 120.5 . . ? C9 C10 H10 120.5 . . ? C10 C11 C12 120.0(5) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? N2 C12 C11 122.9(5) . . ? N2 C12 H12 118.5 . . ? C11 C12 H12 118.5 . . ? C26 C25 H25A 109.5 . . ? C26 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C26 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O10 C26 C27 124.1(5) . . ? O10 C26 C25 116.7(4) . . ? C27 C26 C25 119.2(5) . . ? C26 C27 C26 124.8(7) . 2_655 ? C26 C27 H27 117.6 . . ? C26 C27 H27 117.6 2_655 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.751 _refine_diff_density_min -1.342 _refine_diff_density_rms 0.266