# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2003 data_global _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_Cambridge 0440 loop_ _publ_author_name 'Yongzhong Bian' 'Daqi Wang' 'Rongming Wang' 'Linhong Weng' 'Jianmin Dou' 'Dongyuan Zhao' 'Dennis K. P. Ng' 'Jianzhuang Jiang' data_020318d _database_code_CSD 194117 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H68 La N12' _chemical_formula_weight 1384.41 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' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 28.368(5) _cell_length_b 26.078(4) _cell_length_c 11.0950(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8208(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2461 _cell_measurement_theta_min 2.331 _cell_measurement_theta_max 17.421 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.120 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2852 _exptl_absorpt_coefficient_mu 0.567 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.8711 _exptl_absorpt_correction_T_max 0.9560 _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 '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 39136 _diffrn_reflns_av_R_equivalents 0.2155 _diffrn_reflns_av_sigmaI/netI 0.2357 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 24.80 _reflns_number_total 6900 _reflns_number_gt 2421 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0550P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6900 _refine_ls_number_parameters 445 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2083 _refine_ls_R_factor_gt 0.0605 _refine_ls_wR_factor_ref 0.1694 _refine_ls_wR_factor_gt 0.1152 _refine_ls_goodness_of_fit_ref 0.882 _refine_ls_restrained_S_all 0.882 _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 La1 La 0.97673(3) 0.2500 0.79219(6) 0.0499(3) Uani 1 2 d S . . N1 N 0.8855(4) 0.2500 0.8305(7) 0.074(3) Uani 1 2 d S . . N2 N 0.8715(3) 0.3417(3) 0.8432(6) 0.0585(19) Uani 1 1 d . . . N3 N 0.9319(2) 0.3267(2) 0.6940(6) 0.0555(17) Uani 1 1 d . . . N4 N 0.9806(3) 0.3411(2) 0.5169(5) 0.0552(18) Uani 1 1 d . . . N5 N 0.9782(3) 0.2500 0.5629(9) 0.060(3) Uani 1 2 d S . . N6 N 1.0482(2) 0.3067(2) 0.7837(5) 0.0534(16) Uani 1 1 d . . . N7 N 0.9754(2) 0.3058(2) 0.9762(5) 0.0488(16) Uani 1 1 d . . . C1 C 0.8627(3) 0.2919(3) 0.8682(8) 0.059(2) Uani 1 1 d . . . C2 C 0.8241(3) 0.2775(3) 0.9452(7) 0.060(2) Uani 1 1 d . . . C3 C 0.7915(3) 0.3052(4) 1.0094(8) 0.076(3) Uani 1 1 d . . . C4 C 0.7568(4) 0.2768(3) 1.0753(8) 0.078(3) Uani 1 1 d . . . C5 C 0.7226(4) 0.3044(4) 1.1480(11) 0.113(4) Uani 1 1 d . . . C6 C 0.6910(5) 0.2786(4) 1.2150(12) 0.153(6) Uani 1 1 d . . . C7 C 0.9014(3) 0.3566(3) 0.7592(7) 0.054(2) Uani 1 1 d . . . C8 C 0.9041(3) 0.4077(3) 0.7164(7) 0.057(2) Uani 1 1 d . . . C9 C 0.8810(3) 0.4531(3) 0.7522(7) 0.066(3) Uani 1 1 d . . . C10 C 0.8901(3) 0.4995(3) 0.6875(8) 0.062(2) Uani 1 1 d . . . C11 C 0.8677(3) 0.5455(3) 0.7247(9) 0.081(3) Uani 1 1 d . . . C12 C 0.8781(4) 0.5910(4) 0.6613(9) 0.089(3) Uani 1 1 d . . . C13 C 0.9089(4) 0.5917(4) 0.5612(10) 0.087(3) Uani 1 1 d . . . C14 C 0.9309(4) 0.5438(3) 0.5219(8) 0.074(3) Uani 1 1 d . . . C15 C 0.9205(3) 0.4993(3) 0.5864(8) 0.061(2) Uani 1 1 d . . . C16 C 0.9451(4) 0.4523(3) 0.5488(7) 0.070(3) Uani 1 1 d . . . C17 C 0.9359(3) 0.4084(3) 0.6176(7) 0.063(2) Uani 1 1 d . . . C18 C 0.9513(3) 0.3556(3) 0.6076(7) 0.054(2) Uani 1 1 d . . . C19 C 0.9911(3) 0.2910(3) 0.4971(7) 0.061(2) Uani 1 1 d . . . C20 C 1.0169(3) 0.2776(3) 0.3869(7) 0.056(2) Uani 1 1 d . . . C21 C 1.0369(3) 0.3055(3) 0.2939(7) 0.055(2) Uani 1 1 d . . . C22 C 1.0608(3) 0.2772(3) 0.2013(7) 0.054(2) Uani 1 1 d . . . C23 C 1.0843(3) 0.3055(4) 0.1085(8) 0.072(3) Uani 1 1 d . . . C24 C 1.1090(3) 0.2770(3) 0.0206(8) 0.080(3) Uani 1 1 d . . . C25 C 1.1044(4) 0.2500 0.6816(9) 0.056(3) Uani 1 2 d S . . C26 C 1.0884(3) 0.2977(3) 0.7184(7) 0.051(2) Uani 1 1 d . . . C27 C 1.1153(3) 0.3459(3) 0.7063(8) 0.056(2) Uani 1 1 d . . . C28 C 1.0906(3) 0.3819(3) 0.7654(7) 0.059(2) Uani 1 1 d . . . C29 C 1.0481(3) 0.3581(3) 0.8172(7) 0.056(2) Uani 1 1 d . . . C30 C 1.0163(3) 0.3819(3) 0.8924(7) 0.053(2) Uani 1 1 d . . . C31 C 0.9842(3) 0.3587(3) 0.9703(7) 0.057(2) Uani 1 1 d . . . C32 C 0.9592(3) 0.3841(3) 1.0686(7) 0.054(2) Uani 1 1 d . . . C33 C 0.9335(4) 0.2500 1.1190(9) 0.056(3) Uani 1 2 d S . . C34 C 0.9479(3) 0.2976(3) 1.0763(7) 0.050(2) Uani 1 1 d . . . C35 C 0.9375(3) 0.3474(3) 1.1319(7) 0.058(2) Uani 1 1 d . . . C36 C 1.1623(4) 0.3505(4) 0.6469(8) 0.080(3) Uani 1 1 d . . . C37 C 1.2024(4) 0.3356(5) 0.7356(12) 0.126(4) Uani 1 1 d . . . C38 C 1.1049(3) 0.4371(3) 0.7874(9) 0.072(3) Uani 1 1 d . . . C39 C 1.1281(4) 0.4444(4) 0.9091(10) 0.105(4) Uani 1 1 d . . . C40 C 0.9620(4) 0.4412(3) 1.0935(8) 0.082(3) Uani 1 1 d . . . C41 C 1.0038(4) 0.4556(4) 1.1760(10) 0.106(4) Uani 1 1 d . . . C42 C 0.9103(4) 0.3540(3) 1.2508(9) 0.091(3) Uani 1 1 d . . . C43 C 0.8619(6) 0.3690(8) 1.2291(14) 0.206(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 La1 0.0574(5) 0.0489(4) 0.0433(4) 0.000 0.0005(4) 0.000 N1 0.112(10) 0.073(8) 0.037(6) 0.000 0.010(6) 0.000 N2 0.064(5) 0.047(5) 0.064(5) 0.000(4) 0.011(4) 0.003(4) N3 0.061(5) 0.054(4) 0.051(4) 0.005(4) 0.007(4) -0.006(3) N4 0.075(5) 0.046(4) 0.044(4) 0.000(3) -0.001(4) -0.007(4) N5 0.043(6) 0.023(5) 0.115(8) 0.000 0.002(6) 0.000 N6 0.054(4) 0.054(4) 0.052(4) 0.003(4) 0.003(4) 0.001(3) N7 0.051(4) 0.037(4) 0.058(4) 0.002(3) -0.007(4) -0.002(3) C1 0.047(6) 0.054(6) 0.075(6) 0.004(5) 0.001(5) 0.008(5) C2 0.049(6) 0.080(6) 0.051(5) 0.004(4) 0.009(4) 0.014(4) C3 0.063(7) 0.098(8) 0.066(6) 0.014(5) 0.015(5) 0.010(6) C4 0.075(8) 0.093(8) 0.067(6) 0.011(5) 0.021(5) 0.005(5) C5 0.080(9) 0.119(9) 0.138(10) 0.029(8) 0.061(8) 0.021(7) C6 0.132(12) 0.161(12) 0.166(11) -0.010(8) 0.113(10) 0.003(8) C7 0.058(6) 0.039(5) 0.065(6) -0.005(4) 0.012(5) 0.011(4) C8 0.066(6) 0.056(6) 0.050(5) 0.003(5) 0.001(5) 0.006(4) C9 0.068(7) 0.054(6) 0.076(6) 0.006(5) 0.021(5) 0.010(5) C10 0.074(7) 0.039(5) 0.071(6) 0.000(5) -0.004(5) 0.015(4) C11 0.089(8) 0.053(6) 0.101(7) -0.003(6) -0.009(6) 0.000(5) C12 0.128(10) 0.059(7) 0.079(7) -0.004(6) -0.026(7) 0.006(6) C13 0.085(9) 0.089(8) 0.086(7) -0.014(6) -0.015(6) 0.014(6) C14 0.098(8) 0.049(6) 0.074(6) 0.005(5) -0.013(6) 0.004(5) C15 0.081(8) 0.038(5) 0.066(6) 0.008(5) -0.009(5) 0.007(5) C16 0.101(8) 0.056(6) 0.052(5) 0.008(5) -0.009(5) -0.002(5) C17 0.082(8) 0.048(6) 0.060(6) 0.003(5) 0.000(5) 0.016(5) C18 0.064(6) 0.051(6) 0.045(5) -0.004(4) 0.001(5) 0.006(5) C19 0.081(7) 0.039(5) 0.062(6) -0.021(5) -0.001(5) 0.003(5) C20 0.069(7) 0.059(5) 0.041(4) 0.001(4) 0.003(5) 0.000(4) C21 0.059(6) 0.072(5) 0.034(4) 0.005(5) -0.001(4) -0.004(4) C22 0.054(6) 0.064(5) 0.043(4) -0.002(4) 0.007(4) 0.001(4) C23 0.069(7) 0.101(8) 0.046(5) 0.003(5) 0.005(5) -0.003(6) C24 0.060(7) 0.119(9) 0.060(5) 0.008(5) -0.006(5) 0.012(5) C25 0.084(10) 0.043(7) 0.040(7) 0.000 0.016(6) 0.000 C26 0.040(5) 0.051(5) 0.061(5) 0.012(5) 0.019(4) -0.008(4) C27 0.047(6) 0.064(6) 0.057(5) 0.005(5) 0.010(5) 0.001(4) C28 0.052(6) 0.056(6) 0.069(6) 0.011(5) -0.008(5) -0.009(4) C29 0.071(6) 0.040(5) 0.057(5) -0.003(4) -0.001(5) -0.003(4) C30 0.064(7) 0.045(5) 0.051(5) 0.009(4) 0.018(5) 0.000(5) C31 0.092(8) 0.033(5) 0.045(5) -0.006(4) -0.012(5) 0.004(5) C32 0.081(7) 0.038(5) 0.044(5) -0.012(4) 0.005(4) 0.002(4) C33 0.079(10) 0.046(8) 0.044(7) 0.000 0.003(6) 0.000 C34 0.052(6) 0.058(6) 0.039(5) -0.015(4) 0.004(4) -0.002(5) C35 0.065(7) 0.059(6) 0.051(5) 0.005(5) 0.009(5) 0.014(5) C36 0.073(8) 0.089(7) 0.079(7) 0.005(6) 0.008(6) -0.025(6) C37 0.085(9) 0.148(11) 0.144(11) 0.004(8) -0.002(8) -0.002(7) C38 0.087(7) 0.040(5) 0.088(6) -0.010(5) 0.009(6) -0.012(4) C39 0.100(10) 0.110(9) 0.105(8) -0.031(7) -0.031(7) -0.014(7) C40 0.122(10) 0.045(6) 0.081(7) -0.008(5) -0.001(6) 0.006(5) C41 0.096(9) 0.081(7) 0.142(10) -0.025(7) -0.028(7) -0.009(6) C42 0.102(9) 0.069(7) 0.103(8) -0.010(5) 0.044(7) 0.021(6) C43 0.110(13) 0.36(2) 0.144(13) -0.032(14) 0.025(10) 0.049(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 La1 N7 2.507(6) 7_565 ? La1 N7 2.507(6) . ? La1 N6 2.510(6) 7_565 ? La1 N6 2.510(6) . ? La1 N5 2.545(10) . ? La1 N3 2.608(6) . ? La1 N3 2.608(6) 7_565 ? La1 N1 2.622(12) . ? N1 C1 1.337(10) . ? N1 C1 1.337(10) 7_565 ? N2 C7 1.320(9) . ? N2 C1 1.351(9) . ? N3 C18 1.338(9) . ? N3 C7 1.371(9) . ? N4 C19 1.358(9) . ? N4 C18 1.359(9) . ? N5 C19 1.346(10) . ? N5 C19 1.346(10) 7_565 ? N6 C26 1.371(8) . ? N6 C29 1.391(8) . ? N7 C34 1.374(9) . ? N7 C31 1.404(8) . ? C1 C2 1.440(11) . ? C2 C3 1.372(11) . ? C2 C2 1.435(15) 7_565 ? C3 C4 1.434(12) . ? C4 C4 1.396(17) 7_565 ? C4 C5 1.453(13) . ? C5 C6 1.344(13) . ? C6 C6 1.49(2) 7_565 ? C7 C8 1.417(10) . ? C8 C9 1.409(10) . ? C8 C17 1.420(10) . ? C9 C10 1.430(10) . ? C10 C15 1.414(11) . ? C10 C11 1.420(11) . ? C11 C12 1.411(12) . ? C12 C13 1.413(13) . ? C13 C14 1.462(12) . ? C14 C15 1.394(10) . ? C15 C16 1.473(11) . ? C16 C17 1.401(10) . ? C17 C18 1.448(10) . ? C19 C20 1.468(10) . ? C20 C21 1.384(9) . ? C20 C20 1.441(14) 7_565 ? C21 C22 1.435(10) . ? C22 C22 1.419(13) 7_565 ? C22 C23 1.431(10) . ? C23 C24 1.412(11) . ? C24 C24 1.407(17) 7_565 ? C25 C26 1.386(9) 7_565 ? C25 C26 1.386(9) . ? C26 C27 1.478(10) . ? C27 C28 1.342(10) . ? C27 C36 1.491(11) . ? C28 C29 1.473(11) . ? C28 C38 1.517(10) . ? C29 C30 1.377(10) . ? C30 C31 1.393(10) . ? C31 C32 1.461(10) . ? C32 C35 1.339(10) . ? C32 C40 1.515(10) . ? C33 C34 1.390(9) 7_565 ? C33 C34 1.390(9) . ? C34 C35 1.467(10) . ? C35 C42 1.538(11) . ? C36 C37 1.554(14) . ? C38 C39 1.514(12) . ? C40 C41 1.544(13) . ? C42 C43 1.449(16) . ? 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 N7 La1 N7 70.9(3) 7_565 . ? N7 La1 N6 72.6(2) 7_565 7_565 ? N7 La1 N6 112.6(2) . 7_565 ? N7 La1 N6 112.6(2) 7_565 . ? N7 La1 N6 72.6(2) . . ? N6 La1 N6 72.1(3) 7_565 . ? N7 La1 N5 144.55(13) 7_565 . ? N7 La1 N5 144.55(13) . . ? N6 La1 N5 87.1(2) 7_565 . ? N6 La1 N5 87.1(2) . . ? N7 La1 N3 141.0(2) 7_565 . ? N7 La1 N3 83.59(19) . . ? N6 La1 N3 146.0(2) 7_565 . ? N6 La1 N3 85.80(19) . . ? N5 La1 N3 65.80(19) . . ? N7 La1 N3 83.59(19) 7_565 7_565 ? N7 La1 N3 141.0(2) . 7_565 ? N6 La1 N3 85.80(19) 7_565 7_565 ? N6 La1 N3 146.0(2) . 7_565 ? N5 La1 N3 65.80(19) . 7_565 ? N3 La1 N3 100.1(3) . 7_565 ? N7 La1 N1 81.6(2) 7_565 . ? N7 La1 N1 81.6(2) . . ? N6 La1 N1 143.41(14) 7_565 . ? N6 La1 N1 143.41(14) . . ? N5 La1 N1 100.3(3) . . ? N3 La1 N1 65.58(18) . . ? N3 La1 N1 65.58(18) 7_565 . ? C1 N1 C1 109.6(11) . 7_565 ? C1 N1 La1 121.9(6) . . ? C1 N1 La1 121.9(6) 7_565 . ? C7 N2 C1 123.1(7) . . ? C18 N3 C7 108.4(7) . . ? C18 N3 La1 122.1(5) . . ? C7 N3 La1 121.6(5) . . ? C19 N4 C18 121.4(7) . . ? C19 N5 C19 105.3(10) . 7_565 ? C19 N5 La1 123.1(5) . . ? C19 N5 La1 123.1(5) 7_565 . ? C26 N6 C29 107.9(6) . . ? C26 N6 La1 126.3(5) . . ? C29 N6 La1 123.7(5) . . ? C34 N7 C31 106.9(6) . . ? C34 N7 La1 125.3(5) . . ? C31 N7 La1 122.0(4) . . ? N1 C1 N2 129.2(8) . . ? N1 C1 C2 109.9(8) . . ? N2 C1 C2 120.8(8) . . ? C3 C2 C2 121.7(5) . 7_565 ? C3 C2 C1 133.1(8) . . ? C2 C2 C1 105.1(5) 7_565 . ? C2 C3 C4 117.1(9) . . ? C4 C4 C3 121.1(5) 7_565 . ? C4 C4 C5 119.8(6) 7_565 . ? C3 C4 C5 119.0(9) . . ? C6 C5 C4 120.1(11) . . ? C5 C6 C6 120.1(7) . 7_565 ? N2 C7 N3 127.6(7) . . ? N2 C7 C8 123.2(7) . . ? N3 C7 C8 109.0(7) . . ? C9 C8 C7 132.1(8) . . ? C9 C8 C17 120.2(7) . . ? C7 C8 C17 107.6(7) . . ? C8 C9 C10 118.9(7) . . ? C15 C10 C11 120.3(8) . . ? C15 C10 C9 120.5(7) . . ? C11 C10 C9 119.2(9) . . ? C12 C11 C10 118.2(9) . . ? C11 C12 C13 122.2(9) . . ? C12 C13 C14 119.1(9) . . ? C15 C14 C13 117.9(9) . . ? C14 C15 C10 122.3(8) . . ? C14 C15 C16 116.6(9) . . ? C10 C15 C16 121.0(8) . . ? C17 C16 C15 116.0(8) . . ? C16 C17 C8 123.3(8) . . ? C16 C17 C18 132.7(8) . . ? C8 C17 C18 103.9(7) . . ? N3 C18 N4 128.7(7) . . ? N3 C18 C17 110.9(7) . . ? N4 C18 C17 120.4(8) . . ? N5 C19 N4 128.1(8) . . ? N5 C19 C20 113.5(7) . . ? N4 C19 C20 118.3(7) . . ? C21 C20 C20 121.7(4) . 7_565 ? C21 C20 C19 134.5(7) . . ? C20 C20 C19 103.8(4) 7_565 . ? C20 C21 C22 117.2(7) . . ? C22 C22 C23 121.0(5) 7_565 . ? C22 C22 C21 120.9(4) 7_565 . ? C23 C22 C21 118.1(7) . . ? C24 C23 C22 117.2(8) . . ? C24 C24 C23 121.7(5) 7_565 . ? C26 C25 C26 127.7(10) 7_565 . ? N6 C26 C25 125.5(7) . . ? N6 C26 C27 109.5(7) . . ? C25 C26 C27 124.6(8) . . ? C28 C27 C26 106.2(7) . . ? C28 C27 C36 128.9(8) . . ? C26 C27 C36 124.8(8) . . ? C27 C28 C29 109.0(7) . . ? C27 C28 C38 126.9(8) . . ? C29 C28 C38 123.9(8) . . ? C30 C29 N6 126.8(8) . . ? C30 C29 C28 125.6(8) . . ? N6 C29 C28 107.4(7) . . ? C29 C30 C31 127.4(7) . . ? C30 C31 N7 124.9(7) . . ? C30 C31 C32 125.7(7) . . ? N7 C31 C32 109.0(7) . . ? C35 C32 C31 106.8(7) . . ? C35 C32 C40 129.2(8) . . ? C31 C32 C40 123.8(8) . . ? C34 C33 C34 126.5(11) 7_565 . ? N7 C34 C33 125.5(8) . . ? N7 C34 C35 108.5(7) . . ? C33 C34 C35 126.0(7) . . ? C32 C35 C34 108.7(7) . . ? C32 C35 C42 126.9(8) . . ? C34 C35 C42 124.2(7) . . ? C27 C36 C37 110.8(8) . . ? C39 C38 C28 112.4(7) . . ? C32 C40 C41 112.9(8) . . ? C43 C42 C35 111.3(10) . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 24.80 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 0.970 _refine_diff_density_min -0.680 _refine_diff_density_rms 0.075 data_f11101c _database_code_CSD 194118 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H38 N4 O0.25 Pr0.50' _chemical_formula_weight 709.25 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' Pr Pr -0.2180 2.8214 '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 Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 29.062(8) _cell_length_b 26.502(7) _cell_length_c 10.962(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8443(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 911 _cell_measurement_theta_min 2.511 _cell_measurement_theta_max 21.406 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.116 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2940 _exptl_absorpt_coefficient_mu 0.623 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8351 _exptl_absorpt_correction_T_max 0.9403 _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 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'OMEGA SCAN' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 5.54 _diffrn_reflns_number 33396 _diffrn_reflns_av_R_equivalents 0.1203 _diffrn_reflns_av_sigmaI/netI 0.0822 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 25.01 _reflns_number_total 7577 _reflns_number_gt 5057 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0943P)^2^+7.0280P] 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 const _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00019(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7577 _refine_ls_number_parameters 470 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1196 _refine_ls_R_factor_gt 0.0736 _refine_ls_wR_factor_ref 0.1949 _refine_ls_wR_factor_gt 0.1714 _refine_ls_goodness_of_fit_ref 1.115 _refine_ls_restrained_S_all 1.115 _refine_ls_shift/su_max 0.002 _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 Pr1 Pr 0.027281(18) 0.7500 0.69968(4) 0.03301(19) Uani 1 2 d S . . N1 N 0.0228(3) 0.7500 0.9325(6) 0.0362(18) Uani 1 2 d S . . N2 N 0.06819(18) 0.6753(2) 0.7972(5) 0.0401(13) Uani 1 1 d . . . N3 N 0.1139(3) 0.7500 0.6609(7) 0.0360(18) Uani 1 2 d S . . N4 N -0.04103(18) 0.6942(2) 0.7154(4) 0.0364(13) Uani 1 1 d . . . N5 N 0.02828(19) 0.6948(2) 0.5175(5) 0.0403(13) Uani 1 1 d . . . C1 C 0.0102(2) 0.7079(3) 0.9973(6) 0.0388(16) Uani 1 1 d . . . C2 C -0.0148(2) 0.7231(2) 1.1073(6) 0.0394(16) Uani 1 1 d . . . C3 C -0.0346(2) 0.6963(3) 1.1998(6) 0.0447(17) Uani 1 1 d . . . H3A H -0.0331 0.6612 1.2011 0.054 Uiso 1 1 calc R . . C4 C -0.0575(2) 0.7231(3) 1.2936(6) 0.0435(16) Uani 1 1 d . . . C5 C -0.0806(2) 0.6976(3) 1.3880(6) 0.054(2) Uani 1 1 d . . . H5A H -0.0807 0.6625 1.3895 0.064 Uiso 1 1 calc R . . C6 C -0.1030(3) 0.7237(3) 1.4775(6) 0.060(2) Uani 1 1 d . . . H6A H -0.1183 0.7063 1.5390 0.072 Uiso 1 1 calc R . . C7 C 0.02041(19) 0.6607(2) 0.9721(5) 0.0243(13) Uani 1 1 d . . . H7A H 0.0070 0.6357 1.0199 0.029 Uiso 1 1 calc R . . C8 C 0.0482(2) 0.6462(3) 0.8841(6) 0.0407(16) Uani 1 1 d . . . C9 C 0.0641(2) 0.5936(2) 0.8724(6) 0.0396(16) Uani 1 1 d . . . C10 C 0.0555(2) 0.5512(3) 0.9380(6) 0.0451(17) Uani 1 1 d . . . H10A H 0.0362 0.5523 1.0055 0.054 Uiso 1 1 calc R . . C11 C 0.0765(3) 0.5056(3) 0.9021(7) 0.0473(18) Uani 1 1 d . . . C12 C 0.0680(3) 0.4596(3) 0.9635(7) 0.058(2) Uani 1 1 d . . . H12A H 0.0488 0.4595 1.0315 0.070 Uiso 1 1 calc R . . C13 C 0.0871(3) 0.4157(3) 0.9256(8) 0.066(2) Uani 1 1 d . . . H13A H 0.0803 0.3857 0.9659 0.079 Uiso 1 1 calc R . . C14 C 0.1170(3) 0.4154(3) 0.8262(9) 0.070(3) Uani 1 1 d . . . H14A H 0.1304 0.3852 0.8016 0.083 Uiso 1 1 calc R . . C15 C 0.1266(3) 0.4579(3) 0.7657(8) 0.066(2) Uani 1 1 d . . . H15A H 0.1467 0.4569 0.6999 0.080 Uiso 1 1 calc R . . C16 C 0.1064(3) 0.5047(3) 0.8004(7) 0.0517(18) Uani 1 1 d . . . C17 C 0.1162(3) 0.5500(3) 0.7365(7) 0.0484(18) Uani 1 1 d . . . H17A H 0.1367 0.5501 0.6712 0.058 Uiso 1 1 calc R . . C18 C 0.0951(2) 0.5930(2) 0.7727(6) 0.0400(16) Uani 1 1 d . . . C19 C 0.0982(2) 0.6458(2) 0.7315(6) 0.0404(16) Uani 1 1 d . . . C20 C 0.1289(2) 0.6607(2) 0.6490(5) 0.0253(13) Uani 1 1 d . . . H20A H 0.1453 0.6359 0.6079 0.030 Uiso 1 1 calc R . . C21 C 0.1375(2) 0.7078(3) 0.6214(6) 0.0391(16) Uani 1 1 d . . . C22 C 0.1773(2) 0.7234(3) 0.5509(6) 0.0405(16) Uani 1 1 d . . . C23 C 0.2106(2) 0.6961(3) 0.4942(6) 0.0500(19) Uani 1 1 d . . . H23A H 0.2103 0.6610 0.4968 0.060 Uiso 1 1 calc R . . C24 C 0.2460(3) 0.7223(3) 0.4307(7) 0.054(2) Uani 1 1 d . . . C25 C 0.2818(3) 0.6975(4) 0.3674(8) 0.069(2) Uani 1 1 d . . . H25A H 0.2827 0.6624 0.3669 0.082 Uiso 1 1 calc R . . C26 C 0.3153(3) 0.7237(4) 0.3069(9) 0.087(3) Uani 1 1 d . . . H26A H 0.3382 0.7063 0.2653 0.105 Uiso 1 1 calc R . . C27 C 0.0555(2) 0.7028(3) 0.4167(6) 0.0423(17) Uani 1 1 d . . . C28 C 0.0648(2) 0.6542(3) 0.3578(7) 0.0480(18) Uani 1 1 d . . . C29 C 0.0437(2) 0.6183(3) 0.4244(7) 0.0473(18) Uani 1 1 d . . . C30 C 0.0197(2) 0.6441(2) 0.5226(6) 0.0382(16) Uani 1 1 d . . . C31 C -0.0118(2) 0.6213(3) 0.6030(6) 0.0417(16) Uani 1 1 d . . . H31A H -0.0125 0.5862 0.6015 0.050 Uiso 1 1 calc R . . C32 C -0.0415(2) 0.6441(3) 0.6836(6) 0.0386(16) Uani 1 1 d . . . C33 C -0.0810(3) 0.6201(3) 0.7392(6) 0.0447(17) Uani 1 1 d . . . C34 C -0.1048(2) 0.6562(3) 0.8014(6) 0.0447(16) Uani 1 1 d . . . C35 C -0.0796(2) 0.7025(2) 0.7833(5) 0.0380(15) Uani 1 1 d . . . C36 C 0.0680(3) 0.7500 0.3722(8) 0.045(2) Uani 1 2 d S . . H36A H 0.0871 0.7500 0.3041 0.054 Uiso 1 2 calc SR . . C37 C 0.0920(3) 0.6473(4) 0.2411(8) 0.071(3) Uani 1 1 d . . . H37A H 0.0798 0.6187 0.1965 0.086 Uiso 1 1 calc R . . H37B H 0.0885 0.6770 0.1905 0.086 Uiso 1 1 calc R . . C38 C 0.1425(4) 0.6387(7) 0.2658(11) 0.159(7) Uani 1 1 d . . . H38A H 0.1585 0.6346 0.1899 0.238 Uiso 1 1 calc R . . H38B H 0.1462 0.6088 0.3144 0.238 Uiso 1 1 calc R . . H38C H 0.1548 0.6672 0.3089 0.238 Uiso 1 1 calc R . . C39 C 0.0418(3) 0.5627(3) 0.3998(8) 0.061(2) Uani 1 1 d . . . H39A H 0.0413 0.5448 0.4769 0.074 Uiso 1 1 calc R . . H39B H 0.0694 0.5528 0.3564 0.074 Uiso 1 1 calc R . . C40 C -0.0001(4) 0.5473(4) 0.3254(9) 0.089(3) Uani 1 1 d . . . H40A H 0.0004 0.5115 0.3125 0.134 Uiso 1 1 calc R . . H40B H 0.0005 0.5643 0.2481 0.134 Uiso 1 1 calc R . . H40C H -0.0276 0.5564 0.3687 0.134 Uiso 1 1 calc R . . C41 C -0.0949(3) 0.5663(3) 0.7160(8) 0.062(2) Uani 1 1 d . . . H41A H -0.1153 0.5555 0.7810 0.075 Uiso 1 1 calc R . . H41B H -0.0677 0.5452 0.7190 0.075 Uiso 1 1 calc R . . C42 C -0.1190(4) 0.5582(4) 0.5941(9) 0.096(3) Uani 1 1 d . . . H42A H -0.1270 0.5232 0.5856 0.144 Uiso 1 1 calc R . . H42B H -0.0987 0.5678 0.5289 0.144 Uiso 1 1 calc R . . H42C H -0.1464 0.5784 0.5909 0.144 Uiso 1 1 calc R . . C43 C -0.1507(3) 0.6514(3) 0.8620(7) 0.059(2) Uani 1 1 d . . . H43A H -0.1512 0.6728 0.9337 0.071 Uiso 1 1 calc R . . H43B H -0.1548 0.6168 0.8889 0.071 Uiso 1 1 calc R . . C44 C -0.1906(3) 0.6657(4) 0.7796(9) 0.086(3) Uani 1 1 d . . . H44A H -0.2190 0.6625 0.8239 0.129 Uiso 1 1 calc R . . H44B H -0.1912 0.6436 0.7101 0.129 Uiso 1 1 calc R . . H44C H -0.1870 0.6999 0.7526 0.129 Uiso 1 1 calc R . . C45 C -0.0952(3) 0.7500 0.8221(9) 0.045(2) Uani 1 2 d S . . H45A H -0.1185 0.7500 0.8802 0.054 Uiso 1 2 calc SR . . O1 O 0.1602(13) 0.7500 -0.025(3) 0.28(3) Uani 0.50 2 d SPD . . C46 C 0.1885(9) 0.7088(14) -0.052(3) 0.191(18) Uani 0.50 1 d PD . . H46A H 0.1902 0.7038 -0.1397 0.229 Uiso 0.50 1 calc PR . . H46B H 0.1764 0.6784 -0.0150 0.229 Uiso 0.50 1 calc PR . . C47 C 0.2366(9) 0.72101(19) 0.000(3) 0.29(4) Uani 0.50 1 d PD . . H47A H 0.2402 0.7077 0.0815 0.346 Uiso 0.50 1 calc PR . . H47B H 0.2607 0.7077 -0.0521 0.346 Uiso 0.50 1 calc PR . . 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 Pr1 0.0351(3) 0.0344(3) 0.0295(3) 0.000 0.0016(3) 0.000 N1 0.047(5) 0.037(4) 0.025(4) 0.000 0.005(4) 0.000 N2 0.043(3) 0.037(3) 0.040(3) 0.000(3) 0.004(3) 0.001(2) N3 0.039(5) 0.032(4) 0.037(4) 0.000 0.005(3) 0.000 N4 0.039(3) 0.040(3) 0.031(3) -0.006(2) 0.006(2) 0.003(2) N5 0.042(3) 0.043(3) 0.035(3) 0.002(2) 0.002(3) -0.001(3) C1 0.038(4) 0.052(4) 0.026(3) -0.002(3) -0.004(3) -0.002(3) C2 0.042(4) 0.045(4) 0.031(3) 0.002(3) -0.004(3) 0.005(3) C3 0.052(5) 0.045(4) 0.037(4) 0.003(3) 0.002(4) 0.000(3) C4 0.035(4) 0.061(4) 0.034(3) 0.002(3) -0.005(3) 0.001(3) C5 0.049(5) 0.079(5) 0.033(4) 0.006(4) -0.001(3) -0.003(4) C6 0.049(4) 0.098(6) 0.032(4) 0.015(4) 0.001(3) -0.004(4) C7 0.034(4) 0.018(3) 0.022(3) 0.002(2) 0.008(3) -0.003(3) C8 0.037(4) 0.041(4) 0.044(4) 0.008(3) -0.007(3) -0.001(3) C9 0.046(4) 0.037(4) 0.036(4) -0.001(3) -0.001(3) -0.001(3) C10 0.052(5) 0.044(4) 0.039(4) 0.001(3) 0.002(3) -0.012(4) C11 0.059(5) 0.038(4) 0.045(4) 0.004(3) -0.006(4) 0.000(4) C12 0.069(6) 0.047(5) 0.059(5) 0.009(4) -0.010(4) -0.002(4) C13 0.090(7) 0.038(4) 0.070(6) 0.008(4) -0.023(5) -0.004(4) C14 0.090(7) 0.037(4) 0.082(7) 0.002(4) -0.012(5) 0.010(4) C15 0.081(6) 0.055(5) 0.064(5) -0.009(4) -0.003(5) 0.008(5) C16 0.054(4) 0.036(4) 0.065(5) 0.005(4) -0.009(4) 0.003(3) C17 0.053(5) 0.044(4) 0.048(4) -0.004(3) 0.008(3) 0.009(4) C18 0.049(4) 0.034(4) 0.038(4) 0.005(3) -0.003(3) -0.002(3) C19 0.048(4) 0.036(4) 0.037(4) 0.000(3) -0.005(3) 0.009(3) C20 0.027(3) 0.020(3) 0.028(3) 0.001(2) 0.006(3) 0.005(3) C21 0.032(4) 0.050(4) 0.035(4) 0.002(3) -0.001(3) 0.005(3) C22 0.036(4) 0.049(4) 0.036(4) 0.004(3) 0.002(3) -0.002(3) C23 0.049(5) 0.054(5) 0.047(4) 0.001(4) 0.004(4) 0.009(4) C24 0.048(4) 0.070(5) 0.045(4) -0.002(4) 0.004(4) 0.005(4) C25 0.052(5) 0.072(6) 0.082(6) -0.010(5) 0.024(5) 0.018(4) C26 0.064(6) 0.097(7) 0.100(7) -0.005(6) 0.041(6) 0.011(5) C27 0.053(4) 0.043(4) 0.031(4) -0.006(3) 0.001(3) 0.006(3) C28 0.042(4) 0.059(5) 0.043(4) -0.014(4) 0.006(3) 0.010(4) C29 0.048(4) 0.051(4) 0.043(4) -0.009(4) 0.003(3) 0.002(4) C30 0.046(4) 0.033(3) 0.035(4) -0.005(3) -0.002(3) -0.001(3) C31 0.049(4) 0.034(4) 0.042(4) -0.004(3) -0.002(3) -0.001(3) C32 0.036(4) 0.044(4) 0.036(4) 0.003(3) 0.002(3) -0.002(3) C33 0.051(4) 0.039(4) 0.044(4) 0.007(3) -0.002(3) -0.004(3) C34 0.047(4) 0.046(4) 0.041(4) 0.003(3) 0.006(4) -0.004(3) C35 0.042(4) 0.046(4) 0.026(3) 0.004(3) 0.000(3) -0.002(3) C36 0.047(6) 0.061(7) 0.028(5) 0.000 0.006(4) 0.000 C37 0.082(7) 0.069(6) 0.064(5) -0.019(5) 0.023(5) 0.007(5) C38 0.092(9) 0.30(2) 0.086(9) -0.014(11) 0.018(7) 0.041(12) C39 0.069(6) 0.050(5) 0.065(5) -0.018(4) 0.005(4) 0.010(4) C40 0.114(8) 0.057(6) 0.097(8) -0.025(5) -0.018(6) 0.001(6) C41 0.069(6) 0.051(5) 0.067(6) 0.004(4) 0.008(5) -0.013(4) C42 0.121(9) 0.074(7) 0.093(8) -0.016(6) -0.031(7) -0.022(6) C43 0.059(5) 0.054(5) 0.065(5) 0.007(4) 0.024(4) 0.001(4) C44 0.045(5) 0.119(9) 0.093(8) 0.003(6) 0.009(5) 0.003(5) C45 0.044(6) 0.048(6) 0.042(6) 0.000 0.010(5) 0.000 O1 0.12(3) 0.59(12) 0.14(3) 0.000 -0.09(3) 0.000 C46 0.15(4) 0.22(4) 0.20(4) -0.04(3) -0.12(3) 0.06(3) C47 0.25(4) 0.50(10) 0.12(2) -0.04(3) 0.00(2) 0.29(6) _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 Pr1 N5 2.476(5) 8_575 ? Pr1 N5 2.476(5) . ? Pr1 N4 2.481(5) 8_575 ? Pr1 N4 2.481(5) . ? Pr1 N2 2.545(5) 8_575 ? Pr1 N2 2.545(5) . ? Pr1 N3 2.553(8) . ? Pr1 N1 2.556(7) . ? N1 C1 1.372(8) 8_575 ? N1 C1 1.372(8) . ? N2 C8 1.356(8) . ? N2 C19 1.375(8) . ? N3 C21 1.381(8) 8_575 ? N3 C21 1.381(8) . ? N4 C35 1.364(8) . ? N4 C32 1.374(8) . ? N5 C30 1.367(8) . ? N5 C27 1.374(8) . ? C1 C7 1.316(8) . ? C1 C2 1.464(9) . ? C2 C3 1.365(9) . ? C2 C2 1.427(13) 8_575 ? C3 C4 1.416(9) . ? C4 C5 1.407(9) . ? C4 C4 1.427(14) 8_575 ? C5 C6 1.365(10) . ? C6 C6 1.392(17) 8_575 ? C7 C8 1.315(9) . ? C8 C9 1.475(9) . ? C9 C10 1.355(9) . ? C9 C18 1.418(9) . ? C10 C11 1.411(10) . ? C11 C16 1.412(10) . ? C11 C12 1.414(10) . ? C12 C13 1.355(11) . ? C13 C14 1.392(12) . ? C14 C15 1.337(12) . ? C15 C16 1.423(11) . ? C16 C17 1.420(10) . ? C17 C18 1.354(9) . ? C18 C19 1.474(9) . ? C19 C20 1.329(9) . ? C20 C21 1.309(8) . ? C21 C22 1.451(9) . ? C22 C23 1.360(9) . ? C22 C22 1.410(13) 8_575 ? C23 C24 1.423(10) . ? C24 C25 1.414(10) . ? C24 C24 1.468(15) 8_575 ? C25 C26 1.367(12) . ? C26 C26 1.39(2) 8_575 ? C27 C36 1.391(8) . ? C27 C28 1.467(9) . ? C28 C29 1.349(10) . ? C28 C37 1.514(10) . ? C29 C30 1.453(9) . ? C29 C39 1.498(10) . ? C30 C31 1.406(9) . ? C31 C32 1.376(9) . ? C32 C33 1.445(9) . ? C33 C34 1.364(10) . ? C33 C41 1.502(10) . ? C34 C35 1.444(9) . ? C34 C43 1.496(10) . ? C35 C45 1.404(8) . ? C36 C27 1.391(8) 8_575 ? C37 C38 1.508(14) . ? C39 C40 1.520(12) . ? C41 C42 1.524(12) . ? C43 C44 1.519(12) . ? C45 C35 1.404(8) 8_575 ? O1 C46 1.398(10) 8_575 ? O1 C46 1.398(10) . ? C46 C47 1.542(10) . ? C47 C47 1.537(10) 8_575 ? 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 N5 Pr1 N5 72.5(2) 8_575 . ? N5 Pr1 N4 73.34(17) 8_575 8_575 ? N5 Pr1 N4 114.68(18) . 8_575 ? N5 Pr1 N4 114.68(18) 8_575 . ? N5 Pr1 N4 73.34(17) . . ? N4 Pr1 N4 73.1(2) 8_575 . ? N5 Pr1 N2 82.74(18) 8_575 8_575 ? N5 Pr1 N2 142.49(18) . 8_575 ? N4 Pr1 N2 83.17(17) 8_575 8_575 ? N4 Pr1 N2 143.90(16) . 8_575 ? N5 Pr1 N2 142.49(18) 8_575 . ? N5 Pr1 N2 82.74(18) . . ? N4 Pr1 N2 143.90(17) 8_575 . ? N4 Pr1 N2 83.17(17) . . ? N2 Pr1 N2 102.1(2) 8_575 . ? N5 Pr1 N3 81.61(19) 8_575 . ? N5 Pr1 N3 81.61(19) . . ? N4 Pr1 N3 143.18(12) 8_575 . ? N4 Pr1 N3 143.18(12) . . ? N2 Pr1 N3 67.01(15) 8_575 . ? N2 Pr1 N3 67.01(15) . . ? N5 Pr1 N1 143.72(12) 8_575 . ? N5 Pr1 N1 143.72(12) . . ? N4 Pr1 N1 83.67(18) 8_575 . ? N4 Pr1 N1 83.67(18) . . ? N2 Pr1 N1 66.68(16) 8_575 . ? N2 Pr1 N1 66.68(15) . . ? N3 Pr1 N1 102.5(2) . . ? C1 N1 C1 108.8(7) 8_575 . ? C1 N1 Pr1 122.1(4) 8_575 . ? C1 N1 Pr1 122.1(4) . . ? C8 N2 C19 108.5(5) . . ? C8 N2 Pr1 122.5(4) . . ? C19 N2 Pr1 121.2(4) . . ? C21 N3 C21 108.1(7) 8_575 . ? C21 N3 Pr1 122.8(4) 8_575 . ? C21 N3 Pr1 122.8(4) . . ? C35 N4 C32 106.6(5) . . ? C35 N4 Pr1 126.8(4) . . ? C32 N4 Pr1 124.5(4) . . ? C30 N5 C27 106.8(5) . . ? C30 N5 Pr1 123.1(4) . . ? C27 N5 Pr1 124.3(4) . . ? C7 C1 N1 127.2(6) . . ? C7 C1 C2 123.1(6) . . ? N1 C1 C2 109.6(6) . . ? C3 C2 C2 121.4(4) . 8_575 ? C3 C2 C1 132.7(6) . . ? C2 C2 C1 105.9(4) 8_575 . ? C2 C3 C4 118.5(7) . . ? C5 C4 C3 121.2(7) . . ? C5 C4 C4 118.7(5) . 8_575 ? C3 C4 C4 120.1(4) . 8_575 ? C6 C5 C4 120.8(8) . . ? C5 C6 C6 120.5(5) . 8_575 ? C8 C7 C1 124.7(6) . . ? C7 C8 N2 127.8(6) . . ? C7 C8 C9 122.1(6) . . ? N2 C8 C9 110.1(6) . . ? C10 C9 C18 121.2(6) . . ? C10 C9 C8 132.8(6) . . ? C18 C9 C8 106.0(6) . . ? C9 C10 C11 118.9(7) . . ? C10 C11 C16 120.0(6) . . ? C10 C11 C12 122.0(7) . . ? C16 C11 C12 117.9(7) . . ? C13 C12 C11 121.5(8) . . ? C12 C13 C14 120.0(8) . . ? C15 C14 C13 120.9(8) . . ? C14 C15 C16 121.0(9) . . ? C11 C16 C17 119.9(6) . . ? C11 C16 C15 118.7(7) . . ? C17 C16 C15 121.4(8) . . ? C18 C17 C16 118.5(7) . . ? C17 C18 C9 121.5(6) . . ? C17 C18 C19 133.1(6) . . ? C9 C18 C19 105.4(6) . . ? C20 C19 N2 127.9(6) . . ? C20 C19 C18 122.1(6) . . ? N2 C19 C18 109.9(6) . . ? C21 C20 C19 124.6(6) . . ? C20 C21 N3 127.2(6) . . ? C20 C21 C22 123.2(6) . . ? N3 C21 C22 109.4(6) . . ? C23 C22 C22 122.2(4) . 8_575 ? C23 C22 C21 131.3(7) . . ? C22 C22 C21 106.5(4) 8_575 . ? C22 C23 C24 118.6(7) . . ? C25 C24 C23 123.0(7) . . ? C25 C24 C24 117.7(5) . 8_575 ? C23 C24 C24 119.2(4) . 8_575 ? C26 C25 C24 121.7(9) . . ? C25 C26 C26 120.6(5) . 8_575 ? N5 C27 C36 124.9(6) . . ? N5 C27 C28 109.0(6) . . ? C36 C27 C28 125.8(7) . . ? C29 C28 C27 107.3(6) . . ? C29 C28 C37 127.5(7) . . ? C27 C28 C37 125.2(7) . . ? C28 C29 C30 106.7(6) . . ? C28 C29 C39 127.9(7) . . ? C30 C29 C39 125.3(7) . . ? N5 C30 C31 124.5(6) . . ? N5 C30 C29 110.2(6) . . ? C31 C30 C29 125.0(6) . . ? C32 C31 C30 128.6(6) . . ? N4 C32 C31 125.5(6) . . ? N4 C32 C33 109.1(6) . . ? C31 C32 C33 125.2(6) . . ? C34 C33 C32 107.7(6) . . ? C34 C33 C41 127.8(7) . . ? C32 C33 C41 124.0(7) . . ? C33 C34 C35 105.7(6) . . ? C33 C34 C43 128.0(7) . . ? C35 C34 C43 125.8(7) . . ? N4 C35 C45 125.2(6) . . ? N4 C35 C34 110.8(6) . . ? C45 C35 C34 123.9(7) . . ? C27 C36 C27 128.0(9) 8_575 . ? C38 C37 C28 112.0(8) . . ? C29 C39 C40 113.0(7) . . ? C33 C41 C42 114.0(7) . . ? C34 C43 C44 113.3(7) . . ? C35 C45 C35 127.4(9) 8_575 . ? C46 O1 C46 103(5) 8_575 . ? O1 C46 C47 107(3) . . ? C47 C47 C46 102.1(14) 8_575 . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.978 _refine_diff_density_min -0.690 _refine_diff_density_rms 0.112 data_f11105a _database_code_CSD 194119 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C90 H76 N8 Nd O0.50' _chemical_formula_weight 1421.83 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' Nd Nd -0.1943 3.0179 '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 Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 28.618(8) _cell_length_b 26.329(8) _cell_length_c 10.987(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8278(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 978 _cell_measurement_theta_min 2.828 _cell_measurement_theta_max 21.756 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.141 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2944 _exptl_absorpt_coefficient_mu 0.674 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8495 _exptl_absorpt_correction_T_max 0.9671 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 5.48 _diffrn_reflns_number 32498 _diffrn_reflns_av_R_equivalents 0.1150 _diffrn_reflns_av_sigmaI/netI 0.0797 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 25.01 _reflns_number_total 7424 _reflns_number_gt 5384 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0785P)^2^+20.2423P] 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 const _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00037(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7424 _refine_ls_number_parameters 446 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1205 _refine_ls_R_factor_gt 0.0843 _refine_ls_wR_factor_ref 0.1973 _refine_ls_wR_factor_gt 0.1809 _refine_ls_goodness_of_fit_ref 1.186 _refine_ls_restrained_S_all 1.186 _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 Nd1 Nd 0.025398(18) 0.7500 0.69973(5) 0.03006(19) Uani 1 2 d S . . N1 N 0.0197(3) 0.7500 0.9327(7) 0.040(2) Uani 1 2 d S . . N2 N 0.0667(2) 0.6750(2) 0.7959(5) 0.0370(14) Uani 1 1 d . . . N3 N 0.1135(3) 0.7500 0.6610(7) 0.0327(19) Uani 1 2 d S . . N4 N -0.0430(2) 0.6936(2) 0.7171(5) 0.0330(13) Uani 1 1 d . . . N5 N 0.0276(2) 0.6945(2) 0.5195(5) 0.0353(13) Uani 1 1 d . . . C1 C 0.0079(2) 0.7078(3) 0.9954(7) 0.0381(17) Uani 1 1 d . . . C2 C -0.0164(2) 0.7231(3) 1.1067(6) 0.0355(17) Uani 1 1 d . . . C3 C -0.0365(2) 0.6962(3) 1.1999(7) 0.0406(17) Uani 1 1 d . . . H3A H -0.0356 0.6609 1.2002 0.049 Uiso 1 1 calc R . . C4 C -0.0586(2) 0.7227(3) 1.2949(7) 0.0416(17) Uani 1 1 d . . . C5 C -0.0818(3) 0.6970(3) 1.3899(7) 0.051(2) Uani 1 1 d . . . H5A H -0.0815 0.6617 1.3916 0.061 Uiso 1 1 calc R . . C6 C -0.1044(3) 0.7226(3) 1.4784(7) 0.058(2) Uani 1 1 d . . . H6A H -0.1200 0.7049 1.5394 0.070 Uiso 1 1 calc R . . C7 C 0.0182(2) 0.6600(2) 0.9727(5) 0.0204(13) Uani 1 1 d . . . H7A H 0.0048 0.6352 1.0219 0.025 Uiso 1 1 calc R . . C8 C 0.0462(3) 0.6453(3) 0.8846(7) 0.0386(18) Uani 1 1 d . . . C9 C 0.0636(3) 0.5927(3) 0.8719(7) 0.0384(17) Uani 1 1 d . . . C10 C 0.0558(3) 0.5498(3) 0.9398(7) 0.0457(19) Uani 1 1 d . . . H10A H 0.0365 0.5508 1.0079 0.055 Uiso 1 1 calc R . . C11 C 0.0774(3) 0.5046(3) 0.9047(7) 0.0454(19) Uani 1 1 d . . . C12 C 0.0702(3) 0.4587(3) 0.9686(8) 0.057(2) Uani 1 1 d . . . H12A H 0.0513 0.4583 1.0376 0.068 Uiso 1 1 calc R . . C13 C 0.0911(3) 0.4147(3) 0.9287(10) 0.065(3) Uani 1 1 d . . . H13A H 0.0851 0.3846 0.9700 0.078 Uiso 1 1 calc R . . C14 C 0.1204(3) 0.4139(3) 0.8299(9) 0.063(3) Uani 1 1 d . . . H14A H 0.1339 0.3835 0.8050 0.076 Uiso 1 1 calc R . . C15 C 0.1296(3) 0.4575(3) 0.7686(9) 0.062(2) Uani 1 1 d . . . H15A H 0.1501 0.4569 0.7030 0.074 Uiso 1 1 calc R . . C16 C 0.1083(3) 0.5042(3) 0.8038(8) 0.051(2) Uani 1 1 d . . . C17 C 0.1172(3) 0.5492(3) 0.7384(8) 0.047(2) Uani 1 1 d . . . H17A H 0.1378 0.5493 0.6730 0.057 Uiso 1 1 calc R . . C18 C 0.0949(2) 0.5927(3) 0.7730(7) 0.0388(18) Uani 1 1 d . . . C19 C 0.0975(2) 0.6454(3) 0.7304(6) 0.0360(17) Uani 1 1 d . . . C20 C 0.1280(2) 0.6601(2) 0.6483(6) 0.0214(13) Uani 1 1 d . . . H20A H 0.1445 0.6352 0.6065 0.026 Uiso 1 1 calc R . . C21 C 0.1365(2) 0.7076(3) 0.6217(7) 0.0391(17) Uani 1 1 d . . . C22 C 0.1766(2) 0.7232(3) 0.5483(6) 0.0363(17) Uani 1 1 d . . . C23 C 0.2103(3) 0.6961(3) 0.4913(7) 0.048(2) Uani 1 1 d . . . H23A H 0.2104 0.6608 0.4938 0.058 Uiso 1 1 calc R . . C24 C 0.2457(3) 0.7233(3) 0.4272(8) 0.054(2) Uani 1 1 d . . . C25 C 0.2813(3) 0.6976(4) 0.3638(10) 0.080(3) Uani 1 1 d . . . H25A H 0.2824 0.6623 0.3650 0.096 Uiso 1 1 calc R . . C26 C 0.3139(4) 0.7238(4) 0.3013(13) 0.113(5) Uani 1 1 d . . . H26A H 0.3366 0.7063 0.2576 0.135 Uiso 1 1 calc R . . C27 C 0.0545(2) 0.7025(3) 0.4184(7) 0.0374(17) Uani 1 1 d . . . C28 C 0.0640(3) 0.6538(3) 0.3579(7) 0.048(2) Uani 1 1 d . . . C29 C 0.0422(3) 0.6170(3) 0.4250(7) 0.0455(19) Uani 1 1 d . . . C30 C 0.0181(2) 0.6435(3) 0.5236(6) 0.0369(17) Uani 1 1 d . . . C31 C -0.0132(2) 0.6202(3) 0.6030(7) 0.0405(18) Uani 1 1 d . . . H31A H -0.0135 0.5849 0.6024 0.049 Uiso 1 1 calc R . . C32 C -0.0441(3) 0.6435(3) 0.6830(6) 0.0380(17) Uani 1 1 d . . . C33 C -0.0854(3) 0.6191(3) 0.7363(7) 0.0408(18) Uani 1 1 d . . . C34 C -0.1087(3) 0.6553(3) 0.7968(7) 0.0431(18) Uani 1 1 d . . . C35 C -0.0824(2) 0.7027(3) 0.7831(6) 0.0348(16) Uani 1 1 d . . . C36 C 0.0675(4) 0.7500 0.3761(9) 0.040(3) Uani 1 2 d S . . H36A H 0.0878 0.7500 0.3099 0.048 Uiso 1 2 calc SR . . C37 C 0.0919(4) 0.6469(4) 0.2427(9) 0.069(3) Uani 1 1 d . . . H37A H 0.0792 0.6182 0.1981 0.083 Uiso 1 1 calc R . . H37B H 0.0880 0.6768 0.1924 0.083 Uiso 1 1 calc R . . C38 C 0.1396(5) 0.6387(9) 0.2621(14) 0.189(10) Uani 1 1 d . . . H38A H 0.1551 0.6347 0.1852 0.283 Uiso 1 1 calc R . . H38B H 0.1439 0.6086 0.3100 0.283 Uiso 1 1 calc R . . H38C H 0.1527 0.6673 0.3045 0.283 Uiso 1 1 calc R . . C39 C 0.0399(3) 0.5619(3) 0.3987(9) 0.058(2) Uani 1 1 d . . . H39A H 0.0393 0.5435 0.4750 0.069 Uiso 1 1 calc R . . H39B H 0.0680 0.5520 0.3553 0.069 Uiso 1 1 calc R . . C40 C -0.0015(4) 0.5469(4) 0.3253(10) 0.081(3) Uani 1 1 d . . . H40A H -0.0011 0.5108 0.3123 0.122 Uiso 1 1 calc R . . H40B H -0.0007 0.5640 0.2482 0.122 Uiso 1 1 calc R . . H40C H -0.0295 0.5561 0.3681 0.122 Uiso 1 1 calc R . . C41 C -0.0994(3) 0.5649(3) 0.7131(8) 0.056(2) Uani 1 1 d . . . H41A H -0.1206 0.5538 0.7767 0.068 Uiso 1 1 calc R . . H41B H -0.0719 0.5434 0.7163 0.068 Uiso 1 1 calc R . . C42 C -0.1233(4) 0.5586(4) 0.5886(10) 0.087(3) Uani 1 1 d . . . H42A H -0.1319 0.5237 0.5772 0.130 Uiso 1 1 calc R . . H42B H -0.1021 0.5687 0.5254 0.130 Uiso 1 1 calc R . . H42C H -0.1508 0.5794 0.5856 0.130 Uiso 1 1 calc R . . C43 C -0.1557(3) 0.6510(3) 0.8558(9) 0.059(2) Uani 1 1 d . . . H43A H -0.1562 0.6722 0.9279 0.071 Uiso 1 1 calc R . . H43B H -0.1603 0.6161 0.8818 0.071 Uiso 1 1 calc R . . C44 C -0.1957(3) 0.6662(5) 0.7735(11) 0.093(4) Uani 1 1 d . . . H44A H -0.2247 0.6632 0.8171 0.140 Uiso 1 1 calc R . . H44B H -0.1964 0.6444 0.7036 0.140 Uiso 1 1 calc R . . H44C H -0.1915 0.7007 0.7476 0.140 Uiso 1 1 calc R . . C45 C -0.0980(4) 0.7500 0.8202(9) 0.040(3) Uani 1 2 d S . . H45A H -0.1219 0.7500 0.8774 0.048 Uiso 1 2 calc SR . . 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 Nd1 0.0305(3) 0.0314(3) 0.0283(3) 0.000 0.0023(3) 0.000 N1 0.049(5) 0.049(5) 0.023(4) 0.000 0.014(4) 0.000 N2 0.038(3) 0.038(3) 0.035(3) -0.003(3) 0.013(3) 0.003(3) N3 0.037(5) 0.034(5) 0.027(4) 0.000 0.011(4) 0.000 N4 0.035(3) 0.035(3) 0.029(3) -0.002(3) 0.003(3) -0.001(2) N5 0.032(3) 0.036(3) 0.038(3) -0.002(3) 0.001(3) -0.001(3) C1 0.036(4) 0.048(5) 0.030(4) 0.004(3) -0.006(3) -0.001(3) C2 0.038(4) 0.042(4) 0.027(4) 0.002(3) 0.003(3) -0.001(3) C3 0.036(4) 0.050(4) 0.037(4) 0.003(4) -0.004(4) 0.000(3) C4 0.036(4) 0.060(4) 0.029(4) 0.006(4) 0.000(4) -0.001(3) C5 0.045(5) 0.076(6) 0.031(4) 0.010(4) -0.007(4) -0.001(4) C6 0.046(5) 0.100(7) 0.029(4) 0.009(4) -0.001(4) -0.003(4) C7 0.026(3) 0.017(3) 0.018(3) 0.004(2) 0.007(3) 0.000(3) C8 0.036(4) 0.041(4) 0.039(4) 0.011(3) -0.008(4) -0.002(3) C9 0.047(4) 0.033(4) 0.036(4) -0.001(3) 0.000(4) 0.001(3) C10 0.053(5) 0.040(4) 0.044(5) 0.004(4) 0.001(4) -0.002(4) C11 0.052(5) 0.040(4) 0.044(5) 0.003(4) -0.007(4) -0.004(4) C12 0.068(6) 0.044(5) 0.059(6) 0.005(4) -0.014(5) -0.004(4) C13 0.083(7) 0.032(5) 0.079(7) 0.013(4) -0.019(6) -0.003(5) C14 0.078(7) 0.038(5) 0.073(7) -0.002(4) -0.010(6) 0.018(5) C15 0.069(6) 0.043(5) 0.072(6) -0.003(4) 0.005(5) 0.015(4) C16 0.054(5) 0.041(4) 0.057(5) 0.007(4) -0.007(5) 0.003(4) C17 0.050(5) 0.041(4) 0.051(5) 0.000(4) 0.010(4) 0.008(4) C18 0.034(4) 0.041(4) 0.041(5) 0.006(3) 0.003(3) 0.000(3) C19 0.036(4) 0.034(4) 0.038(4) 0.000(3) -0.008(3) 0.005(3) C20 0.016(3) 0.022(3) 0.026(3) -0.001(3) 0.012(3) 0.005(3) C21 0.032(4) 0.048(5) 0.037(4) -0.001(4) 0.002(3) 0.004(3) C22 0.031(4) 0.048(4) 0.030(4) 0.001(3) 0.006(3) -0.002(3) C23 0.042(4) 0.052(5) 0.051(5) 0.003(4) 0.007(4) 0.007(4) C24 0.042(4) 0.070(5) 0.050(5) 0.000(4) 0.009(4) 0.003(4) C25 0.060(6) 0.078(7) 0.103(8) 0.014(6) 0.041(6) 0.015(5) C26 0.077(7) 0.091(8) 0.171(13) -0.012(8) 0.077(9) 0.004(6) C27 0.034(4) 0.044(4) 0.034(4) -0.007(3) 0.007(3) -0.002(3) C28 0.051(5) 0.052(5) 0.039(4) -0.012(4) 0.006(4) 0.012(4) C29 0.055(5) 0.041(4) 0.041(5) -0.007(4) 0.006(4) 0.005(4) C30 0.039(4) 0.039(4) 0.032(4) -0.005(3) 0.001(3) 0.005(3) C31 0.044(5) 0.036(4) 0.041(4) -0.003(3) 0.001(4) -0.004(3) C32 0.041(4) 0.044(4) 0.029(4) 0.004(3) 0.002(3) -0.005(3) C33 0.048(5) 0.036(4) 0.038(4) 0.007(3) 0.000(4) -0.007(4) C34 0.045(4) 0.045(4) 0.039(4) 0.007(4) 0.005(4) 0.001(4) C35 0.038(4) 0.042(4) 0.025(4) -0.005(3) 0.001(3) -0.003(3) C36 0.036(6) 0.053(7) 0.032(6) 0.000 0.013(5) 0.000 C37 0.081(7) 0.072(6) 0.055(6) -0.014(5) 0.026(5) 0.016(5) C38 0.095(11) 0.38(3) 0.096(11) -0.026(15) 0.034(9) 0.046(15) C39 0.068(6) 0.048(5) 0.058(6) -0.011(4) 0.009(5) 0.012(4) C40 0.099(8) 0.060(6) 0.084(8) -0.022(5) -0.017(7) -0.004(6) C41 0.065(5) 0.037(4) 0.067(6) 0.003(4) 0.013(5) -0.014(4) C42 0.102(8) 0.074(7) 0.085(8) -0.023(6) -0.023(7) -0.031(6) C43 0.053(5) 0.057(5) 0.068(6) 0.000(5) 0.019(5) -0.008(4) C44 0.048(6) 0.128(10) 0.103(9) -0.007(8) 0.019(6) 0.005(6) C45 0.046(6) 0.049(6) 0.024(6) 0.000 0.017(5) 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 Nd1 N5 2.462(6) 7_575 ? Nd1 N5 2.462(6) . ? Nd1 N4 2.464(6) 7_575 ? Nd1 N4 2.464(6) . ? Nd1 N2 2.532(6) 7_575 ? Nd1 N2 2.532(6) . ? Nd1 N3 2.556(8) . ? Nd1 N1 2.565(8) . ? N1 C1 1.350(8) 7_575 ? N1 C1 1.350(8) . ? N2 C19 1.378(9) . ? N2 C8 1.381(9) . ? N3 C21 1.366(8) 7_575 ? N3 C21 1.366(8) . ? N4 C35 1.363(8) . ? N4 C32 1.373(9) . ? N5 C27 1.369(9) . ? N5 C30 1.371(9) . ? C1 C7 1.316(9) . ? C1 C2 1.464(10) . ? C2 C3 1.372(10) . ? C2 C2 1.414(13) 7_575 ? C3 C4 1.405(10) . ? C4 C5 1.410(10) . ? C4 C4 1.439(15) 7_575 ? C5 C6 1.347(11) . ? C6 C6 1.445(18) 7_575 ? C7 C8 1.316(9) . ? C8 C9 1.478(10) . ? C9 C10 1.372(10) . ? C9 C18 1.409(10) . ? C10 C11 1.394(10) . ? C11 C12 1.412(11) . ? C11 C16 1.418(11) . ? C12 C13 1.375(12) . ? C13 C14 1.372(13) . ? C14 C15 1.357(12) . ? C15 C16 1.426(11) . ? C16 C17 1.408(11) . ? C17 C18 1.364(10) . ? C18 C19 1.468(10) . ? C19 C20 1.313(9) . ? C20 C21 1.308(9) . ? C21 C22 1.460(9) . ? C22 C23 1.353(10) . ? C22 C22 1.412(14) 7_575 ? C23 C24 1.427(11) . ? C24 C24 1.405(17) 7_575 ? C24 C25 1.408(12) . ? C25 C26 1.347(13) . ? C26 C26 1.38(2) 7_575 ? C27 C36 1.385(8) . ? C27 C28 1.471(10) . ? C28 C29 1.368(11) . ? C28 C37 1.505(11) . ? C29 C30 1.462(10) . ? C29 C39 1.479(10) . ? C30 C31 1.392(10) . ? C31 C32 1.388(10) . ? C32 C33 1.467(10) . ? C33 C34 1.339(10) . ? C33 C41 1.504(10) . ? C34 C35 1.465(10) . ? C34 C43 1.498(11) . ? C35 C45 1.383(8) . ? C36 C27 1.385(8) 7_575 ? C37 C38 1.400(16) . ? C39 C40 1.487(13) . ? C41 C42 1.538(13) . ? C43 C44 1.514(14) . ? C45 C35 1.383(8) 7_575 ? 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 N5 Nd1 N5 72.9(3) 7_575 . ? N5 Nd1 N4 74.02(18) 7_575 7_575 ? N5 Nd1 N4 116.14(19) . 7_575 ? N5 Nd1 N4 116.14(19) 7_575 . ? N5 Nd1 N4 74.02(18) . . ? N4 Nd1 N4 74.1(3) 7_575 . ? N5 Nd1 N2 81.98(19) 7_575 7_575 ? N5 Nd1 N2 141.86(18) . 7_575 ? N4 Nd1 N2 82.45(18) 7_575 7_575 ? N4 Nd1 N2 143.95(18) . 7_575 ? N5 Nd1 N2 141.86(18) 7_575 . ? N5 Nd1 N2 81.98(19) . . ? N4 Nd1 N2 143.95(18) 7_575 . ? N4 Nd1 N2 82.45(18) . . ? N2 Nd1 N2 102.5(3) 7_575 . ? N5 Nd1 N3 80.84(19) 7_575 . ? N5 Nd1 N3 80.84(19) . . ? N4 Nd1 N3 142.74(13) 7_575 . ? N4 Nd1 N3 142.74(13) . . ? N2 Nd1 N3 66.98(16) 7_575 . ? N2 Nd1 N3 66.98(16) . . ? N5 Nd1 N1 143.53(13) 7_575 . ? N5 Nd1 N1 143.53(13) . . ? N4 Nd1 N1 82.7(2) 7_575 . ? N4 Nd1 N1 82.7(2) . . ? N2 Nd1 N1 67.24(17) 7_575 . ? N2 Nd1 N1 67.24(17) . . ? N3 Nd1 N1 103.2(3) . . ? C1 N1 C1 110.8(8) 7_575 . ? C1 N1 Nd1 121.7(4) 7_575 . ? C1 N1 Nd1 121.7(4) . . ? C19 N2 C8 108.6(6) . . ? C19 N2 Nd1 121.4(4) . . ? C8 N2 Nd1 122.5(4) . . ? C21 N3 C21 109.5(8) 7_575 . ? C21 N3 Nd1 121.9(4) 7_575 . ? C21 N3 Nd1 121.9(4) . . ? C35 N4 C32 107.2(6) . . ? C35 N4 Nd1 126.4(4) . . ? C32 N4 Nd1 125.2(4) . . ? C27 N5 C30 106.9(6) . . ? C27 N5 Nd1 125.1(4) . . ? C30 N5 Nd1 123.4(4) . . ? C7 C1 N1 129.4(7) . . ? C7 C1 C2 121.8(6) . . ? N1 C1 C2 108.5(6) . . ? C3 C2 C2 121.1(4) . 7_575 ? C3 C2 C1 132.9(7) . . ? C2 C2 C1 106.0(4) 7_575 . ? C2 C3 C4 119.2(7) . . ? C3 C4 C5 121.7(7) . . ? C3 C4 C4 119.7(4) . 7_575 ? C5 C4 C4 118.6(5) . 7_575 ? C6 C5 C4 121.4(8) . . ? C5 C6 C6 119.9(5) . 7_575 ? C8 C7 C1 123.8(6) . . ? C7 C8 N2 127.7(7) . . ? C7 C8 C9 123.4(6) . . ? N2 C8 C9 108.8(6) . . ? C10 C9 C18 121.5(7) . . ? C10 C9 C8 131.7(7) . . ? C18 C9 C8 106.7(6) . . ? C9 C10 C11 118.6(7) . . ? C10 C11 C12 121.8(8) . . ? C10 C11 C16 119.9(7) . . ? C12 C11 C16 118.3(7) . . ? C13 C12 C11 119.9(9) . . ? C14 C13 C12 122.1(8) . . ? C15 C14 C13 119.9(8) . . ? C14 C15 C16 120.7(9) . . ? C17 C16 C11 120.4(7) . . ? C17 C16 C15 120.6(8) . . ? C11 C16 C15 119.0(7) . . ? C18 C17 C16 118.7(7) . . ? C17 C18 C9 120.8(7) . . ? C17 C18 C19 133.0(7) . . ? C9 C18 C19 106.1(6) . . ? C20 C19 N2 128.1(6) . . ? C20 C19 C18 122.0(6) . . ? N2 C19 C18 109.7(6) . . ? C21 C20 C19 124.0(6) . . ? C20 C21 N3 128.3(7) . . ? C20 C21 C22 122.6(6) . . ? N3 C21 C22 108.9(6) . . ? C23 C22 C22 121.8(5) . 7_575 ? C23 C22 C21 131.9(7) . . ? C22 C22 C21 106.3(4) 7_575 . ? C22 C23 C24 118.1(7) . . ? C24 C24 C25 118.7(6) 7_575 . ? C24 C24 C23 120.1(5) 7_575 . ? C25 C24 C23 121.2(8) . . ? C26 C25 C24 120.5(10) . . ? C25 C26 C26 120.8(7) . 7_575 ? N5 C27 C36 124.3(7) . . ? N5 C27 C28 109.6(6) . . ? C36 C27 C28 125.9(7) . . ? C29 C28 C27 106.8(7) . . ? C29 C28 C37 127.5(8) . . ? C27 C28 C37 125.7(8) . . ? C28 C29 C30 106.1(7) . . ? C28 C29 C39 127.5(7) . . ? C30 C29 C39 126.2(7) . . ? N5 C30 C31 125.4(6) . . ? N5 C30 C29 110.4(6) . . ? C31 C30 C29 124.0(7) . . ? C32 C31 C30 127.7(7) . . ? N4 C32 C31 125.6(6) . . ? N4 C32 C33 109.3(6) . . ? C31 C32 C33 124.9(7) . . ? C34 C33 C32 106.7(7) . . ? C34 C33 C41 128.8(7) . . ? C32 C33 C41 124.2(7) . . ? C33 C34 C35 107.5(6) . . ? C33 C34 C43 127.4(7) . . ? C35 C34 C43 124.7(7) . . ? N4 C35 C45 125.6(7) . . ? N4 C35 C34 109.2(6) . . ? C45 C35 C34 124.9(7) . . ? C27 C36 C27 129.0(9) 7_575 . ? C38 C37 C28 114.0(10) . . ? C29 C39 C40 113.8(8) . . ? C33 C41 C42 111.8(7) . . ? C34 C43 C44 113.7(8) . . ? C35 C45 C35 128.3(9) 7_575 . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.818 _refine_diff_density_min -1.303 _refine_diff_density_rms 0.115 data_020319a _database_code_CSD 194120 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H68 N12 Tb' _chemical_formula_weight 1404.42 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' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 28.550(4) _cell_length_b 26.489(3) _cell_length_c 10.9353(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8269.7(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4615 _cell_measurement_theta_min 2.346 _cell_measurement_theta_max 20.413 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.128 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2884 _exptl_absorpt_coefficient_mu 0.902 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.7032 _exptl_absorpt_correction_T_max 0.9152 _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 '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 40241 _diffrn_reflns_av_R_equivalents 0.1071 _diffrn_reflns_av_sigmaI/netI 0.1034 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 24.82 _reflns_number_total 7097 _reflns_number_gt 3891 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0668P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7097 _refine_ls_number_parameters 445 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1155 _refine_ls_R_factor_gt 0.0521 _refine_ls_wR_factor_ref 0.1424 _refine_ls_wR_factor_gt 0.1153 _refine_ls_goodness_of_fit_ref 0.937 _refine_ls_restrained_S_all 0.937 _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 Tb1 Tb 0.527465(15) 0.2500 0.30084(4) 0.03929(16) Uani 1 2 d S . . N1 N 0.5215(2) 0.2500 0.0770(6) 0.0319(15) Uani 1 2 d S . . N2 N 0.51815(17) 0.33965(18) 0.0321(5) 0.0464(13) Uani 1 1 d . . . N3 N 0.56645(16) 0.32471(18) 0.2093(5) 0.0443(12) Uani 1 1 d . . . N4 N 0.62894(18) 0.34036(19) 0.3563(5) 0.0487(13) Uani 1 1 d . . . N5 N 0.6131(2) 0.2500 0.3452(6) 0.0436(18) Uani 1 2 d S . . N6 N 0.46018(16) 0.30544(18) 0.2797(4) 0.0418(13) Uani 1 1 d . . . N7 N 0.53018(17) 0.30478(18) 0.4780(4) 0.0411(12) Uani 1 1 d . . . C1 C 0.5080(2) 0.2912(2) 0.0103(5) 0.0413(15) Uani 1 1 d . . . C2 C 0.4834(2) 0.2769(2) -0.1034(5) 0.0452(16) Uani 1 1 d . . . C3 C 0.4645(2) 0.3041(2) -0.1986(6) 0.0516(16) Uani 1 1 d . . . C4 C 0.4427(2) 0.2768(2) -0.2957(6) 0.0505(16) Uani 1 1 d . . . C5 C 0.4201(2) 0.3035(3) -0.3913(6) 0.0624(19) Uani 1 1 d . . . C6 C 0.3978(2) 0.2765(3) -0.4814(6) 0.062(2) Uani 1 1 d . . . C7 C 0.5467(2) 0.3542(2) 0.1221(6) 0.0437(15) Uani 1 1 d . . . C8 C 0.5629(2) 0.4060(2) 0.1296(6) 0.0460(16) Uani 1 1 d . . . C9 C 0.5546(2) 0.4484(2) 0.0625(6) 0.0531(17) Uani 1 1 d . . . C10 C 0.5774(2) 0.4940(2) 0.0999(6) 0.0551(17) Uani 1 1 d . . . C11 C 0.5684(3) 0.5400(3) 0.0329(7) 0.066(2) Uani 1 1 d . . . C12 C 0.5897(3) 0.5841(3) 0.0764(8) 0.075(2) Uani 1 1 d . . . C13 C 0.6202(3) 0.5845(3) 0.1754(8) 0.076(2) Uani 1 1 d . . . C14 C 0.6293(3) 0.5407(3) 0.2378(8) 0.072(2) Uani 1 1 d . . . C15 C 0.6083(2) 0.4942(2) 0.2014(7) 0.0544(17) Uani 1 1 d . . . C16 C 0.6175(2) 0.4496(2) 0.2674(6) 0.0576(19) Uani 1 1 d . . . C17 C 0.5946(2) 0.4067(2) 0.2296(6) 0.0503(17) Uani 1 1 d . . . C18 C 0.5971(2) 0.3542(2) 0.2744(6) 0.0457(16) Uani 1 1 d . . . C19 C 0.6369(2) 0.2917(2) 0.3825(6) 0.0453(15) Uani 1 1 d . . . C20 C 0.6770(2) 0.2767(2) 0.4567(6) 0.0494(17) Uani 1 1 d . . . C21 C 0.7114(2) 0.3038(3) 0.5151(6) 0.0592(19) Uani 1 1 d . . . C22 C 0.7457(2) 0.2768(2) 0.5786(6) 0.0582(19) Uani 1 1 d . . . C23 C 0.7818(3) 0.3032(3) 0.6451(8) 0.083(3) Uani 1 1 d . . . C24 C 0.8147(3) 0.2765(3) 0.7088(10) 0.112(3) Uani 1 1 d . . . C25 C 0.4047(3) 0.2500 0.1703(7) 0.045(2) Uani 1 2 d S . . C26 C 0.4210(2) 0.2975(2) 0.2112(5) 0.0427(15) Uani 1 1 d . . . C27 C 0.3949(2) 0.3438(2) 0.1967(6) 0.0482(15) Uani 1 1 d . . . C28 C 0.4181(2) 0.3797(2) 0.2589(6) 0.0499(17) Uani 1 1 d . . . C29 C 0.4591(2) 0.3556(2) 0.3102(5) 0.0424(15) Uani 1 1 d . . . C30 C 0.4894(2) 0.3793(2) 0.3934(6) 0.0480(16) Uani 1 1 d . . . C31 C 0.5215(2) 0.3562(2) 0.4738(5) 0.0431(15) Uani 1 1 d . . . C32 C 0.5443(2) 0.3812(2) 0.5731(6) 0.0520(17) Uani 1 1 d . . . C33 C 0.5662(2) 0.3453(3) 0.6417(6) 0.0576(19) Uani 1 1 d . . . C34 C 0.5566(2) 0.2974(2) 0.5803(6) 0.0465(16) Uani 1 1 d . . . C35 C 0.5703(3) 0.2500 0.6242(9) 0.050(2) Uani 1 2 d S . . C36 C 0.3477(2) 0.3475(3) 0.1340(7) 0.070(2) Uani 1 1 d . . . C37 C 0.3080(3) 0.3326(4) 0.2224(9) 0.101(3) Uani 1 1 d . . . C38 C 0.4035(3) 0.4338(2) 0.2820(7) 0.067(2) Uani 1 1 d . . . C39 C 0.3792(3) 0.4406(3) 0.4062(9) 0.095(3) Uani 1 1 d . . . C40 C 0.5426(3) 0.4379(2) 0.5988(7) 0.069(2) Uani 1 1 d . . . C41 C 0.4982(3) 0.4526(3) 0.6738(8) 0.094(3) Uani 1 1 d . . . C42 C 0.5912(3) 0.3516(3) 0.7617(8) 0.087(3) Uani 1 1 d . . . C43 C 0.6415(5) 0.3635(7) 0.7456(12) 0.197(7) 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 Tb1 0.0411(3) 0.0438(3) 0.0330(2) 0.000 -0.0028(2) 0.000 N1 0.036(4) 0.023(3) 0.036(4) 0.000 0.012(3) 0.000 N2 0.057(4) 0.041(3) 0.041(3) 0.007(2) -0.005(3) -0.002(2) N3 0.046(3) 0.051(3) 0.036(3) 0.003(3) -0.007(3) -0.008(2) N4 0.050(3) 0.048(3) 0.048(3) 0.004(3) -0.010(3) -0.006(3) N5 0.039(4) 0.049(4) 0.043(4) 0.000 -0.001(3) 0.000 N6 0.045(3) 0.044(3) 0.036(3) -0.007(2) -0.006(2) 0.009(2) N7 0.040(3) 0.053(3) 0.030(3) -0.005(2) -0.005(2) -0.006(2) C1 0.045(4) 0.044(4) 0.035(4) -0.003(3) -0.002(3) -0.003(3) C2 0.048(4) 0.054(4) 0.033(3) -0.002(3) -0.005(3) 0.002(3) C3 0.052(4) 0.066(4) 0.037(3) 0.002(3) -0.006(4) -0.001(3) C4 0.047(4) 0.070(4) 0.034(3) 0.000(3) -0.001(3) 0.000(3) C5 0.045(4) 0.106(6) 0.036(4) 0.006(4) 0.003(3) 0.000(4) C6 0.051(4) 0.093(5) 0.043(4) -0.002(3) 0.001(4) 0.005(4) C7 0.053(4) 0.043(4) 0.035(4) 0.000(3) -0.007(3) -0.004(3) C8 0.047(4) 0.052(4) 0.038(4) 0.000(3) -0.003(3) -0.005(3) C9 0.067(5) 0.039(4) 0.053(4) 0.005(3) 0.006(4) -0.002(3) C10 0.062(5) 0.051(4) 0.052(4) 0.003(4) 0.010(4) 0.001(3) C11 0.087(6) 0.043(4) 0.068(5) 0.014(4) 0.017(4) 0.003(4) C12 0.101(7) 0.047(5) 0.076(6) 0.009(4) 0.026(5) 0.007(4) C13 0.089(6) 0.058(5) 0.081(6) 0.007(4) 0.000(5) -0.008(4) C14 0.079(5) 0.048(4) 0.090(6) 0.000(4) 0.012(4) -0.012(4) C15 0.060(4) 0.047(4) 0.056(4) -0.010(4) 0.007(4) -0.001(3) C16 0.071(5) 0.038(4) 0.064(5) 0.002(3) 0.003(4) -0.006(3) C17 0.052(4) 0.045(4) 0.053(4) 0.007(3) -0.002(3) -0.003(3) C18 0.049(4) 0.044(4) 0.045(4) 0.001(3) 0.004(3) 0.000(3) C19 0.036(4) 0.054(4) 0.046(4) 0.007(3) -0.005(3) -0.002(3) C20 0.043(4) 0.061(4) 0.044(4) 0.000(3) -0.003(3) -0.005(3) C21 0.053(4) 0.071(5) 0.054(4) 0.004(4) -0.010(4) -0.012(4) C22 0.033(4) 0.083(5) 0.059(4) 0.000(4) -0.011(3) -0.003(3) C23 0.062(5) 0.100(6) 0.088(6) 0.006(5) -0.034(5) -0.010(5) C24 0.081(6) 0.113(7) 0.144(9) 0.000(6) -0.054(6) -0.003(5) C25 0.050(6) 0.051(6) 0.033(5) 0.000 0.003(4) 0.000 C26 0.043(4) 0.055(4) 0.030(3) 0.000(3) 0.004(3) 0.004(3) C27 0.060(4) 0.050(4) 0.035(3) 0.004(3) -0.003(4) 0.004(3) C28 0.060(4) 0.043(4) 0.047(4) 0.012(3) 0.003(3) 0.014(3) C29 0.047(4) 0.044(4) 0.037(3) 0.002(3) -0.003(3) 0.002(3) C30 0.055(4) 0.046(4) 0.043(4) -0.003(3) 0.000(3) -0.002(3) C31 0.058(4) 0.031(3) 0.040(4) 0.000(3) 0.003(3) 0.000(3) C32 0.059(4) 0.051(4) 0.046(4) -0.011(3) -0.002(3) -0.002(3) C33 0.066(5) 0.065(5) 0.041(4) -0.012(4) -0.011(4) -0.005(4) C34 0.046(4) 0.057(4) 0.037(4) -0.004(3) -0.003(3) 0.001(3) C35 0.044(6) 0.053(6) 0.053(6) 0.000 0.000(5) 0.000 C36 0.047(4) 0.088(6) 0.074(5) 0.021(4) -0.011(4) 0.010(4) C37 0.050(5) 0.149(9) 0.104(7) 0.024(6) -0.008(5) -0.006(5) C38 0.084(5) 0.051(4) 0.068(5) 0.000(4) -0.003(4) 0.022(4) C39 0.108(7) 0.086(6) 0.091(7) -0.016(5) 0.037(6) 0.013(5) C40 0.090(6) 0.050(4) 0.067(5) -0.018(4) -0.009(4) -0.013(4) C41 0.096(6) 0.083(6) 0.105(7) -0.034(5) 0.026(6) 0.005(5) C42 0.085(6) 0.094(6) 0.080(6) -0.026(5) -0.032(5) -0.008(5) C43 0.105(9) 0.38(2) 0.110(9) -0.029(12) -0.017(8) -0.075(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 N7 2.422(4) . ? Tb1 N7 2.422(4) 7_565 ? Tb1 N6 2.429(5) 7_565 ? Tb1 N6 2.429(5) . ? Tb1 N1 2.454(6) . ? Tb1 N3 2.481(5) 7_565 ? Tb1 N3 2.481(5) . ? Tb1 N5 2.493(7) . ? N1 C1 1.367(7) 7_565 ? N1 C1 1.367(7) . ? N2 C7 1.334(7) . ? N2 C1 1.338(7) . ? N3 C7 1.356(7) . ? N3 C18 1.372(7) . ? N4 C18 1.327(7) . ? N4 C19 1.340(7) . ? N5 C19 1.360(7) . ? N5 C19 1.360(7) 7_565 ? N6 C26 1.364(7) . ? N6 C29 1.371(7) . ? N7 C34 1.363(7) . ? N7 C31 1.384(7) . ? C1 C2 1.478(8) . ? C2 C3 1.376(8) . ? C2 C2 1.426(11) 7_565 ? C3 C4 1.428(8) . ? C4 C5 1.416(9) . ? C4 C4 1.422(12) 7_565 ? C5 C6 1.374(9) . ? C6 C6 1.404(14) 7_565 ? C7 C8 1.451(8) . ? C8 C9 1.362(8) . ? C8 C17 1.419(8) . ? C9 C10 1.432(9) . ? C10 C15 1.417(9) . ? C10 C11 1.445(9) . ? C11 C12 1.402(10) . ? C12 C13 1.389(11) . ? C13 C14 1.371(10) . ? C14 C15 1.428(9) . ? C15 C16 1.409(9) . ? C16 C17 1.375(8) . ? C17 C18 1.477(8) . ? C19 C20 1.457(8) . ? C20 C21 1.374(8) . ? C20 C20 1.417(12) 7_565 ? C21 C22 1.395(8) . ? C22 C22 1.421(13) 7_565 ? C22 C23 1.443(9) . ? C23 C24 1.367(11) . ? C24 C24 1.403(18) 7_565 ? C25 C26 1.413(7) . ? C25 C26 1.413(7) 7_565 ? C26 C27 1.446(8) . ? C27 C28 1.345(8) . ? C27 C36 1.515(9) . ? C28 C29 1.446(8) . ? C28 C38 1.512(9) . ? C29 C30 1.402(8) . ? C30 C31 1.411(8) . ? C31 C32 1.429(8) . ? C32 C33 1.362(9) . ? C32 C40 1.530(9) . ? C33 C34 1.463(8) . ? C33 C42 1.504(10) . ? C34 C35 1.400(7) . ? C35 C34 1.400(7) 7_565 ? C36 C37 1.539(11) . ? C38 C39 1.536(11) . ? C40 C41 1.559(11) . ? C42 C43 1.481(14) . ? 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 N7 Tb1 N7 73.6(2) . 7_565 ? N7 Tb1 N6 117.62(16) . 7_565 ? N7 Tb1 N6 74.87(16) 7_565 7_565 ? N7 Tb1 N6 74.87(16) . . ? N7 Tb1 N6 117.62(16) 7_565 . ? N6 Tb1 N6 74.4(2) 7_565 . ? N7 Tb1 N1 143.15(11) . . ? N7 Tb1 N1 143.15(11) 7_565 . ? N6 Tb1 N1 81.39(15) 7_565 . ? N6 Tb1 N1 81.39(15) . . ? N7 Tb1 N3 141.83(16) . 7_565 ? N7 Tb1 N3 80.23(16) 7_565 7_565 ? N6 Tb1 N3 80.46(16) 7_565 7_565 ? N6 Tb1 N3 143.00(16) . 7_565 ? N1 Tb1 N3 68.22(14) . 7_565 ? N7 Tb1 N3 80.23(16) . . ? N7 Tb1 N3 141.83(16) 7_565 . ? N6 Tb1 N3 143.00(16) 7_565 . ? N6 Tb1 N3 80.46(16) . . ? N1 Tb1 N3 68.22(14) . . ? N3 Tb1 N3 105.8(2) 7_565 . ? N7 Tb1 N5 79.22(17) . . ? N7 Tb1 N5 79.22(17) 7_565 . ? N6 Tb1 N5 142.58(12) 7_565 . ? N6 Tb1 N5 142.58(12) . . ? N1 Tb1 N5 105.2(2) . . ? N3 Tb1 N5 68.81(14) 7_565 . ? N3 Tb1 N5 68.81(14) . . ? C1 N1 C1 105.8(7) 7_565 . ? C1 N1 Tb1 123.5(3) 7_565 . ? C1 N1 Tb1 123.5(3) . . ? C7 N2 C1 122.7(5) . . ? C7 N3 C18 107.7(5) . . ? C7 N3 Tb1 123.8(4) . . ? C18 N3 Tb1 122.1(4) . . ? C18 N4 C19 121.7(5) . . ? C19 N5 C19 108.7(7) . 7_565 ? C19 N5 Tb1 123.3(4) . . ? C19 N5 Tb1 123.3(4) 7_565 . ? C26 N6 C29 105.4(5) . . ? C26 N6 Tb1 127.4(4) . . ? C29 N6 Tb1 125.5(4) . . ? C34 N7 C31 105.5(5) . . ? C34 N7 Tb1 126.0(4) . . ? C31 N7 Tb1 123.9(4) . . ? N2 C1 N1 127.6(5) . . ? N2 C1 C2 119.8(5) . . ? N1 C1 C2 112.3(5) . . ? C3 C2 C2 121.6(4) . 7_565 ? C3 C2 C1 133.6(6) . . ? C2 C2 C1 104.8(3) 7_565 . ? C2 C3 C4 117.9(6) . . ? C5 C4 C4 119.9(4) . 7_565 ? C5 C4 C3 119.7(6) . . ? C4 C4 C3 120.4(4) 7_565 . ? C6 C5 C4 118.7(7) . . ? C5 C6 C6 121.4(4) . 7_565 ? N2 C7 N3 127.4(5) . . ? N2 C7 C8 120.6(5) . . ? N3 C7 C8 111.8(5) . . ? C9 C8 C17 121.0(6) . . ? C9 C8 C7 133.9(6) . . ? C17 C8 C7 105.1(5) . . ? C8 C9 C10 117.5(6) . . ? C15 C10 C9 120.7(6) . . ? C15 C10 C11 120.3(6) . . ? C9 C10 C11 119.0(7) . . ? C12 C11 C10 117.0(7) . . ? C13 C12 C11 122.9(7) . . ? C14 C13 C12 120.0(7) . . ? C13 C14 C15 120.8(8) . . ? C16 C15 C10 120.9(6) . . ? C16 C15 C14 120.2(7) . . ? C10 C15 C14 118.9(6) . . ? C17 C16 C15 116.7(6) . . ? C16 C17 C8 123.1(6) . . ? C16 C17 C18 131.0(6) . . ? C8 C17 C18 105.9(5) . . ? N4 C18 N3 129.0(6) . . ? N4 C18 C17 121.1(6) . . ? N3 C18 C17 109.5(5) . . ? N4 C19 N5 129.2(6) . . ? N4 C19 C20 120.9(6) . . ? N5 C19 C20 109.8(6) . . ? C21 C20 C20 121.4(4) . 7_565 ? C21 C20 C19 132.8(6) . . ? C20 C20 C19 105.8(3) 7_565 . ? C20 C21 C22 117.8(6) . . ? C21 C22 C22 120.8(4) . 7_565 ? C21 C22 C23 120.3(6) . . ? C22 C22 C23 119.0(4) 7_565 . ? C24 C23 C22 119.8(8) . . ? C23 C24 C24 121.2(5) . 7_565 ? C26 C25 C26 125.6(8) . 7_565 ? N6 C26 C25 125.6(6) . . ? N6 C26 C27 110.6(5) . . ? C25 C26 C27 123.5(6) . . ? C28 C27 C26 106.9(6) . . ? C28 C27 C36 128.6(6) . . ? C26 C27 C36 124.2(6) . . ? C27 C28 C29 106.5(5) . . ? C27 C28 C38 128.1(6) . . ? C29 C28 C38 125.2(6) . . ? N6 C29 C30 125.3(5) . . ? N6 C29 C28 110.6(5) . . ? C30 C29 C28 123.6(6) . . ? C29 C30 C31 127.7(5) . . ? N7 C31 C30 124.3(5) . . ? N7 C31 C32 110.4(5) . . ? C30 C31 C32 124.7(5) . . ? C33 C32 C31 107.7(5) . . ? C33 C32 C40 126.8(6) . . ? C31 C32 C40 125.5(6) . . ? C32 C33 C34 105.5(6) . . ? C32 C33 C42 128.4(6) . . ? C34 C33 C42 125.9(6) . . ? N7 C34 C35 124.5(6) . . ? N7 C34 C33 110.8(5) . . ? C35 C34 C33 124.6(6) . . ? C34 C35 C34 127.3(8) 7_565 . ? C27 C36 C37 110.7(6) . . ? C28 C38 C39 112.6(6) . . ? C32 C40 C41 111.5(6) . . ? C43 C42 C33 112.4(8) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 24.82 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 1.025 _refine_diff_density_min -0.711 _refine_diff_density_rms 0.092 data_020405c _database_code_CSD 194121 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H68 Dy N12' _chemical_formula_weight 1408.00 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' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 28.589(13) _cell_length_b 26.655(13) _cell_length_c 10.922(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8323(7) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 1164 _cell_measurement_theta_min 2.347 _cell_measurement_theta_max 15.465 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.124 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2888 _exptl_absorpt_coefficient_mu 0.944 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7649 _exptl_absorpt_correction_T_max 0.9632 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 33102 _diffrn_reflns_av_R_equivalents 0.3429 _diffrn_reflns_av_sigmaI/netI 0.3976 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.28 _diffrn_reflns_theta_max 23.41 _reflns_number_total 5676 _reflns_number_gt 1647 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0000P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5676 _refine_ls_number_parameters 445 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2334 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.1017 _refine_ls_wR_factor_gt 0.0552 _refine_ls_goodness_of_fit_ref 0.701 _refine_ls_restrained_S_all 0.701 _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 0.02784(2) 0.2500 0.69738(7) 0.0501(3) Uani 1 2 d S . . N1 N 0.0229(4) 0.2500 0.9165(7) 0.021(2) Uani 1 2 d S . . N2 N 0.0181(3) 0.1613(3) 0.9658(7) 0.052(2) Uani 1 1 d . . . N3 N 0.0648(3) 0.1762(3) 0.7877(8) 0.057(2) Uani 1 1 d . . . N4 N 0.1280(3) 0.1588(3) 0.6369(7) 0.054(2) Uani 1 1 d . . . N5 N 0.1125(4) 0.2500 0.6466(9) 0.053(3) Uani 1 2 d S . . N6 N 0.0309(3) 0.1953(3) 0.5190(6) 0.048(2) Uani 1 1 d . . . N7 N -0.0388(3) 0.1951(3) 0.7182(7) 0.051(2) Uani 1 1 d . . . C1 C 0.0069(3) 0.2086(4) 0.9877(8) 0.043(3) Uani 1 1 d . . . C2 C -0.0164(3) 0.2230(3) 1.1007(9) 0.051(3) Uani 1 1 d . . . C3 C -0.0356(3) 0.1958(3) 1.1958(10) 0.054(3) Uani 1 1 d . . . C4 C -0.0560(3) 0.2236(3) 1.2949(11) 0.058(3) Uani 1 1 d . . . C5 C -0.0797(4) 0.1958(5) 1.3889(10) 0.077(4) Uani 1 1 d . . . C6 C -0.1022(4) 0.2237(4) 1.4814(11) 0.085(5) Uani 1 1 d . . . C7 C 0.0470(4) 0.1447(5) 0.8737(10) 0.068(4) Uani 1 1 d . . . C8 C 0.0644(4) 0.0956(5) 0.8680(10) 0.051(3) Uani 1 1 d . . . C9 C 0.0558(4) 0.0518(5) 0.9333(10) 0.065(3) Uani 1 1 d . . . C10 C 0.0778(4) 0.0079(5) 0.9021(10) 0.056(3) Uani 1 1 d . . . C11 C 0.0691(4) -0.0372(5) 0.9667(12) 0.086(4) Uani 1 1 d . . . C12 C 0.0888(5) -0.0834(6) 0.9191(13) 0.089(5) Uani 1 1 d . . . C13 C 0.1190(4) -0.0858(5) 0.8203(15) 0.094(4) Uani 1 1 d . . . C14 C 0.1300(4) -0.0403(5) 0.7635(11) 0.081(4) Uani 1 1 d . . . C15 C 0.1084(4) 0.0062(4) 0.8064(13) 0.065(3) Uani 1 1 d . . . C16 C 0.1186(4) 0.0518(4) 0.7305(11) 0.075(4) Uani 1 1 d . . . C17 C 0.0928(4) 0.0946(4) 0.7685(9) 0.061(3) Uani 1 1 d . . . C18 C 0.0975(3) 0.1465(4) 0.7211(10) 0.050(3) Uani 1 1 d . . . C19 C 0.1366(3) 0.2089(4) 0.6172(9) 0.050(3) Uani 1 1 d . . . C20 C 0.1771(4) 0.2229(4) 0.5463(9) 0.063(3) Uani 1 1 d . . . C21 C 0.2114(4) 0.1945(5) 0.4829(11) 0.083(4) Uani 1 1 d . . . C22 C 0.2464(3) 0.2239(4) 0.4206(9) 0.056(3) Uani 1 1 d . . . C23 C 0.2829(4) 0.1934(5) 0.3595(11) 0.086(4) Uani 1 1 d . . . C24 C 0.3180(5) 0.2207(4) 0.3043(16) 0.135(5) Uani 1 1 d . . . C25 C 0.0697(5) 0.2500 0.3777(11) 0.057(4) Uani 1 2 d S . . C26 C 0.0569(4) 0.2033(5) 0.4167(10) 0.061(3) Uani 1 1 d . . . C27 C 0.0658(4) 0.1545(5) 0.3572(10) 0.069(4) Uani 1 1 d . . . C28 C 0.0443(4) 0.1183(4) 0.4246(10) 0.059(3) Uani 1 1 d . . . C29 C 0.0208(4) 0.1426(4) 0.5246(10) 0.063(3) Uani 1 1 d . . . C30 C -0.0094(4) 0.1197(4) 0.6063(10) 0.057(3) Uani 1 1 d . . . C31 C -0.0386(4) 0.1452(4) 0.6933(11) 0.052(3) Uani 1 1 d . . . C32 C -0.0805(4) 0.1203(4) 0.7410(10) 0.065(3) Uani 1 1 d . . . C33 C -0.1038(4) 0.1563(4) 0.8075(11) 0.066(3) Uani 1 1 d . . . C34 C -0.0786(3) 0.2023(4) 0.7891(11) 0.055(3) Uani 1 1 d . . . C35 C -0.0941(4) 0.2500 0.8271(12) 0.043(4) Uani 1 2 d S . . C36 C 0.0918(5) 0.1502(5) 0.2344(13) 0.117(5) Uani 1 1 d . . . C37 C 0.1413(8) 0.1379(9) 0.2532(16) 0.240(10) Uani 1 1 d . . . C38 C 0.0438(5) 0.0636(4) 0.4059(11) 0.083(4) Uani 1 1 d . . . C39 C 0.0003(4) 0.0464(5) 0.3333(11) 0.104(5) Uani 1 1 d . . . C40 C -0.0924(4) 0.0655(4) 0.7223(11) 0.082(4) Uani 1 1 d . . . C41 C -0.1192(4) 0.0592(5) 0.5962(12) 0.101(5) Uani 1 1 d . . . C42 C -0.1496(4) 0.1516(5) 0.8688(10) 0.088(4) Uani 1 1 d . . . C43 C -0.1919(4) 0.1709(5) 0.7815(12) 0.106(4) 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 0.0470(4) 0.0535(5) 0.0497(4) 0.000 0.0027(5) 0.000 N1 0.048(7) 0.000(5) 0.016(5) 0.000 -0.013(6) 0.000 N2 0.066(7) 0.041(6) 0.050(6) 0.002(5) 0.012(5) 0.004(5) N3 0.050(6) 0.076(7) 0.045(6) -0.011(6) 0.007(5) -0.012(5) N4 0.045(6) 0.043(6) 0.075(6) 0.007(5) 0.028(5) -0.002(5) N5 0.057(9) 0.060(10) 0.042(8) 0.000 -0.001(6) 0.000 N6 0.046(5) 0.060(6) 0.037(5) 0.004(5) -0.001(5) 0.009(6) N7 0.066(6) 0.042(5) 0.045(5) 0.008(5) 0.003(5) 0.006(5) C1 0.046(7) 0.048(8) 0.034(6) 0.015(6) 0.011(5) 0.001(6) C2 0.044(7) 0.057(7) 0.052(7) -0.002(5) -0.005(5) 0.009(5) C3 0.034(6) 0.085(8) 0.042(6) 0.024(7) -0.002(6) 0.002(6) C4 0.049(6) 0.076(8) 0.049(6) -0.012(7) -0.022(6) 0.004(5) C5 0.072(9) 0.134(13) 0.024(6) 0.003(7) -0.007(6) -0.019(9) C6 0.054(8) 0.118(14) 0.084(9) 0.013(8) -0.019(7) 0.003(7) C7 0.075(10) 0.086(12) 0.043(8) -0.003(8) 0.003(7) -0.007(8) C8 0.050(8) 0.045(8) 0.058(8) -0.009(7) 0.006(6) 0.004(7) C9 0.087(9) 0.056(9) 0.051(8) 0.009(7) -0.010(7) 0.002(8) C10 0.076(9) 0.060(10) 0.032(7) 0.008(7) 0.013(6) -0.007(8) C11 0.094(10) 0.050(9) 0.113(12) -0.004(9) -0.035(9) -0.004(8) C12 0.098(12) 0.105(13) 0.064(9) 0.005(10) -0.028(8) -0.039(10) C13 0.086(10) 0.087(11) 0.109(12) 0.023(12) -0.039(10) -0.021(9) C14 0.086(9) 0.054(9) 0.103(11) 0.002(8) -0.044(7) -0.002(8) C15 0.087(9) 0.039(7) 0.069(8) -0.003(9) -0.032(9) 0.012(6) C16 0.066(8) 0.049(8) 0.110(11) 0.004(8) 0.001(7) 0.004(7) C17 0.064(8) 0.056(9) 0.061(8) -0.013(7) 0.022(6) -0.004(7) C18 0.035(7) 0.032(7) 0.083(9) 0.006(7) 0.015(6) 0.014(6) C19 0.031(7) 0.065(9) 0.054(7) 0.004(7) 0.018(5) 0.023(6) C20 0.073(8) 0.066(9) 0.049(7) -0.001(6) 0.010(6) 0.011(6) C21 0.049(8) 0.119(12) 0.081(9) 0.018(8) 0.008(7) 0.011(8) C22 0.030(6) 0.072(9) 0.065(7) 0.005(6) 0.017(6) 0.017(5) C23 0.075(9) 0.106(12) 0.077(9) 0.020(8) 0.032(7) 0.001(9) C24 0.170(14) 0.090(11) 0.146(12) -0.009(11) 0.016(13) 0.017(9) C25 0.092(13) 0.050(12) 0.028(9) 0.000 0.015(8) 0.000 C26 0.074(9) 0.062(9) 0.045(7) -0.005(7) 0.008(7) -0.027(7) C27 0.089(9) 0.067(10) 0.049(8) -0.011(7) 0.034(7) 0.005(7) C28 0.086(10) 0.047(8) 0.045(7) -0.004(7) -0.013(6) 0.003(7) C29 0.080(10) 0.046(8) 0.062(8) -0.022(7) -0.017(8) 0.016(8) C30 0.048(8) 0.063(9) 0.060(8) 0.006(7) 0.000(6) -0.023(6) C31 0.061(8) 0.037(7) 0.058(7) -0.001(7) -0.006(7) -0.011(6) C32 0.051(8) 0.059(9) 0.085(10) 0.021(7) -0.005(6) 0.020(7) C33 0.047(7) 0.088(10) 0.062(7) -0.014(9) 0.012(7) -0.010(7) C34 0.045(6) 0.046(7) 0.074(8) 0.021(8) 0.016(7) -0.025(6) C35 0.052(9) 0.036(9) 0.040(10) 0.000 0.027(8) 0.000 C36 0.128(13) 0.091(10) 0.131(13) 0.030(9) 0.074(11) 0.044(9) C37 0.147(16) 0.43(3) 0.143(18) 0.006(17) -0.010(13) 0.040(19) C38 0.129(13) 0.046(8) 0.073(9) -0.019(7) -0.015(8) -0.002(8) C39 0.091(9) 0.109(12) 0.113(12) -0.007(10) -0.005(9) 0.035(8) C40 0.097(9) 0.051(8) 0.098(11) 0.009(8) -0.009(8) -0.028(7) C41 0.089(11) 0.098(12) 0.117(11) -0.028(9) -0.012(8) -0.015(9) C42 0.078(10) 0.103(11) 0.083(9) 0.012(8) 0.022(8) -0.039(8) C43 0.084(9) 0.145(12) 0.090(10) -0.007(10) 0.007(8) 0.023(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 N1 2.398(8) . ? Dy1 N7 2.414(8) . ? Dy1 N7 2.414(8) 7_565 ? Dy1 N6 2.436(7) . ? Dy1 N6 2.436(7) 7_565 ? Dy1 N3 2.441(9) 7_565 ? Dy1 N3 2.441(9) . ? Dy1 N5 2.484(12) . ? N1 C1 1.424(10) . ? N1 C1 1.424(10) 7_565 ? N2 C1 1.323(11) . ? N2 C7 1.375(12) . ? N3 C7 1.358(12) . ? N3 C18 1.426(11) . ? N4 C18 1.310(11) . ? N4 C19 1.373(12) . ? N5 C19 1.334(10) . ? N5 C19 1.334(10) 7_565 ? N6 C26 1.358(11) . ? N6 C29 1.436(12) . ? N7 C31 1.356(9) . ? N7 C34 1.389(11) . ? C1 C2 1.454(12) . ? C2 C3 1.381(11) . ? C2 C2 1.439(18) 7_565 ? C3 C4 1.435(12) . ? C4 C4 1.410(17) 7_565 ? C4 C5 1.435(13) . ? C5 C6 1.409(13) . ? C6 C6 1.40(2) 7_565 ? C7 C8 1.401(15) . ? C8 C17 1.357(11) . ? C8 C9 1.391(14) . ? C9 C10 1.370(14) . ? C10 C15 1.363(14) . ? C10 C11 1.417(14) . ? C11 C12 1.449(16) . ? C12 C13 1.383(16) . ? C13 C14 1.398(14) . ? C14 C15 1.464(13) . ? C15 C16 1.499(13) . ? C16 C17 1.421(12) . ? C17 C18 1.482(13) . ? C19 C20 1.443(14) . ? C20 C21 1.418(13) . ? C20 C20 1.447(19) 7_565 ? C21 C22 1.442(13) . ? C22 C22 1.392(19) 7_565 ? C22 C23 1.480(13) . ? C23 C24 1.378(15) . ? C24 C24 1.56(2) 7_565 ? C25 C26 1.365(12) . ? C25 C26 1.365(12) 7_565 ? C26 C27 1.478(14) . ? C27 C28 1.360(13) . ? C27 C36 1.538(13) . ? C28 C29 1.435(13) . ? C28 C38 1.474(13) . ? C29 C30 1.384(13) . ? C30 C31 1.437(13) . ? C31 C32 1.464(13) . ? C32 C33 1.375(12) . ? C32 C40 1.515(12) . ? C33 C34 1.438(12) . ? C33 C42 1.476(13) . ? C34 C35 1.408(11) . ? C35 C34 1.408(11) 7_565 ? C36 C37 1.467(18) . ? C38 C39 1.544(14) . ? C40 C41 1.585(15) . ? C42 C43 1.624(16) . ? 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 N1 Dy1 N7 81.9(3) . . ? N1 Dy1 N7 81.9(3) . 7_565 ? N7 Dy1 N7 74.7(4) . 7_565 ? N1 Dy1 N6 143.21(19) . . ? N7 Dy1 N6 74.9(3) . . ? N7 Dy1 N6 117.8(3) 7_565 . ? N1 Dy1 N6 143.21(19) . 7_565 ? N7 Dy1 N6 117.8(3) . 7_565 ? N7 Dy1 N6 74.9(3) 7_565 7_565 ? N6 Dy1 N6 73.6(4) . 7_565 ? N1 Dy1 N3 67.8(2) . 7_565 ? N7 Dy1 N3 142.4(3) . 7_565 ? N7 Dy1 N3 79.3(3) 7_565 7_565 ? N6 Dy1 N3 142.2(3) . 7_565 ? N6 Dy1 N3 79.9(3) 7_565 7_565 ? N1 Dy1 N3 67.8(2) . . ? N7 Dy1 N3 79.3(3) . . ? N7 Dy1 N3 142.4(3) 7_565 . ? N6 Dy1 N3 79.9(3) . . ? N6 Dy1 N3 142.2(3) 7_565 . ? N3 Dy1 N3 107.4(3) 7_565 . ? N1 Dy1 N5 106.3(3) . . ? N7 Dy1 N5 142.22(19) . . ? N7 Dy1 N5 142.22(19) 7_565 . ? N6 Dy1 N5 77.7(3) . . ? N6 Dy1 N5 77.7(3) 7_565 . ? N3 Dy1 N5 70.7(2) 7_565 . ? N3 Dy1 N5 70.7(2) . . ? C1 N1 C1 101.5(11) . 7_565 ? C1 N1 Dy1 124.3(5) . . ? C1 N1 Dy1 124.3(5) 7_565 . ? C1 N2 C7 125.8(9) . . ? C7 N3 C18 104.8(10) . . ? C7 N3 Dy1 128.0(8) . . ? C18 N3 Dy1 121.7(7) . . ? C18 N4 C19 118.2(9) . . ? C19 N5 C19 110.6(13) . 7_565 ? C19 N5 Dy1 123.8(7) . . ? C19 N5 Dy1 123.8(7) 7_565 . ? C26 N6 C29 107.4(9) . . ? C26 N6 Dy1 125.7(7) . . ? C29 N6 Dy1 123.0(6) . . ? C31 N7 C34 104.6(9) . . ? C31 N7 Dy1 124.9(7) . . ? C34 N7 Dy1 127.9(6) . . ? N2 C1 N1 124.2(8) . . ? N2 C1 C2 121.0(9) . . ? N1 C1 C2 114.0(9) . . ? C3 C2 C2 121.7(6) . 7_565 ? C3 C2 C1 133.1(9) . . ? C2 C2 C1 105.3(5) 7_565 . ? C2 C3 C4 117.3(9) . . ? C4 C4 C5 121.0(7) 7_565 . ? C4 C4 C3 121.0(5) 7_565 . ? C5 C4 C3 117.7(9) . . ? C6 C5 C4 117.2(12) . . ? C6 C6 C5 121.8(7) 7_565 . ? N3 C7 N2 122.1(12) . . ? N3 C7 C8 114.4(11) . . ? N2 C7 C8 123.2(11) . . ? C17 C8 C9 120.0(12) . . ? C17 C8 C7 105.4(12) . . ? C9 C8 C7 134.4(12) . . ? C10 C9 C8 120.5(11) . . ? C15 C10 C9 120.9(12) . . ? C15 C10 C11 117.8(12) . . ? C9 C10 C11 121.3(12) . . ? C10 C11 C12 118.3(12) . . ? C13 C12 C11 124.2(14) . . ? C12 C13 C14 116.5(14) . . ? C13 C14 C15 119.9(13) . . ? C10 C15 C14 122.9(12) . . ? C10 C15 C16 121.5(11) . . ? C14 C15 C16 115.3(12) . . ? C17 C16 C15 112.8(10) . . ? C8 C17 C16 124.1(12) . . ? C8 C17 C18 108.4(11) . . ? C16 C17 C18 126.9(10) . . ? N4 C18 N3 131.0(10) . . ? N4 C18 C17 122.7(10) . . ? N3 C18 C17 106.3(9) . . ? N5 C19 N4 132.0(10) . . ? N5 C19 C20 109.3(11) . . ? N4 C19 C20 118.6(9) . . ? C21 C20 C19 132.8(10) . . ? C21 C20 C20 122.2(7) . 7_565 ? C19 C20 C20 105.0(6) . 7_565 ? C20 C21 C22 114.9(11) . . ? C22 C22 C21 122.9(6) 7_565 . ? C22 C22 C23 123.3(6) 7_565 . ? C21 C22 C23 113.9(10) . . ? C24 C23 C22 114.9(12) . . ? C23 C24 C24 121.8(8) . 7_565 ? C26 C25 C26 131.4(15) . 7_565 ? N6 C26 C25 123.2(12) . . ? N6 C26 C27 108.5(9) . . ? C25 C26 C27 128.3(11) . . ? C28 C27 C26 107.9(9) . . ? C28 C27 C36 129.7(12) . . ? C26 C27 C36 122.2(11) . . ? C27 C28 C29 107.7(10) . . ? C27 C28 C38 129.1(11) . . ? C29 C28 C38 123.2(11) . . ? C30 C29 C28 125.7(11) . . ? C30 C29 N6 125.8(10) . . ? C28 C29 N6 108.3(11) . . ? C29 C30 C31 125.5(10) . . ? N7 C31 C30 126.8(10) . . ? N7 C31 C32 111.7(10) . . ? C30 C31 C32 119.7(10) . . ? C33 C32 C31 105.6(10) . . ? C33 C32 C40 129.4(11) . . ? C31 C32 C40 124.9(10) . . ? C32 C33 C34 106.1(10) . . ? C32 C33 C42 127.7(11) . . ? C34 C33 C42 125.5(11) . . ? N7 C34 C35 123.3(9) . . ? N7 C34 C33 111.7(9) . . ? C35 C34 C33 124.8(10) . . ? C34 C35 C34 128.9(12) . 7_565 ? C37 C36 C27 111.2(14) . . ? C28 C38 C39 111.8(10) . . ? C32 C40 C41 109.1(9) . . ? C33 C42 C43 111.6(10) . . ? _diffrn_measured_fraction_theta_max 0.909 _diffrn_reflns_theta_full 23.41 _diffrn_measured_fraction_theta_full 0.909 _refine_diff_density_max 0.959 _refine_diff_density_min -0.378 _refine_diff_density_rms 0.064 data_020319b _database_code_CSD 194122 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H68 Ho N12' _chemical_formula_weight 1410.43 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' Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 28.546(5) _cell_length_b 26.529(5) _cell_length_c 10.915(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8266(3) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3679 _cell_measurement_theta_min 2.349 _cell_measurement_theta_max 18.728 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.133 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2892 _exptl_absorpt_coefficient_mu 1.004 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.6444 _exptl_absorpt_correction_T_max 0.8890 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 35753 _diffrn_reflns_av_R_equivalents 0.1111 _diffrn_reflns_av_sigmaI/netI 0.1022 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 23.38 _reflns_number_total 6077 _reflns_number_gt 3518 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.1069P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6077 _refine_ls_number_parameters 445 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1160 _refine_ls_R_factor_gt 0.0622 _refine_ls_wR_factor_ref 0.1860 _refine_ls_wR_factor_gt 0.1553 _refine_ls_goodness_of_fit_ref 0.955 _refine_ls_restrained_S_all 0.955 _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 Ho1 Ho 0.028158(19) 0.2500 0.69788(5) 0.0371(2) Uani 1 2 d S . . N1 N 0.0217(3) 0.2500 0.9224(7) 0.024(2) Uani 1 2 d S . . N2 N 0.0185(2) 0.1602(3) 0.9654(6) 0.0443(19) Uani 1 1 d . . . N3 N 0.0662(2) 0.1756(2) 0.7875(6) 0.0397(17) Uani 1 1 d . . . N4 N 0.1291(2) 0.1610(3) 0.6411(7) 0.0456(18) Uani 1 1 d . . . N5 N 0.1127(3) 0.2500 0.6503(8) 0.037(2) Uani 1 2 d S . . N6 N 0.0310(2) 0.1951(2) 0.5218(5) 0.0340(16) Uani 1 1 d . . . N7 N -0.0383(2) 0.1948(3) 0.7208(6) 0.0381(17) Uani 1 1 d . . . C1 C 0.0087(3) 0.2093(3) 0.9876(7) 0.036(2) Uani 1 1 d . . . C2 C -0.0163(3) 0.2240(3) 1.1007(7) 0.041(2) Uani 1 1 d . . . C3 C -0.0349(3) 0.1959(4) 1.1963(8) 0.047(2) Uani 1 1 d . . . C4 C -0.0569(3) 0.2230(3) 1.2941(8) 0.048(2) Uani 1 1 d . . . C5 C -0.0793(3) 0.1948(4) 1.3905(8) 0.060(3) Uani 1 1 d . . . C6 C -0.1013(3) 0.2218(4) 1.4821(8) 0.060(3) Uani 1 1 d . . . C7 C 0.0466(3) 0.1457(3) 0.8746(7) 0.040(2) Uani 1 1 d . . . C8 C 0.0629(3) 0.0944(3) 0.8682(8) 0.042(2) Uani 1 1 d . . . C9 C 0.0548(3) 0.0523(3) 0.9349(8) 0.052(2) Uani 1 1 d . . . C10 C 0.0770(3) 0.0070(3) 0.8976(8) 0.051(2) Uani 1 1 d . . . C11 C 0.0678(4) -0.0379(4) 0.9648(10) 0.066(3) Uani 1 1 d . . . C12 C 0.0895(4) -0.0832(4) 0.9229(11) 0.078(3) Uani 1 1 d . . . C13 C 0.1200(4) -0.0838(4) 0.8203(11) 0.080(3) Uani 1 1 d . . . C14 C 0.1291(4) -0.0400(4) 0.7570(10) 0.067(3) Uani 1 1 d . . . C15 C 0.1076(3) 0.0063(3) 0.7966(8) 0.050(2) Uani 1 1 d . . . C16 C 0.1179(3) 0.0509(3) 0.7298(9) 0.055(3) Uani 1 1 d . . . C17 C 0.0946(3) 0.0941(3) 0.7684(8) 0.048(2) Uani 1 1 d . . . C18 C 0.0971(3) 0.1468(3) 0.7228(7) 0.040(2) Uani 1 1 d . . . C19 C 0.1365(3) 0.2086(3) 0.6140(8) 0.041(2) Uani 1 1 d . . . C20 C 0.1768(3) 0.2233(3) 0.5419(8) 0.045(2) Uani 1 1 d . . . C21 C 0.2111(3) 0.1957(4) 0.4845(8) 0.058(3) Uani 1 1 d . . . C22 C 0.2464(3) 0.2226(3) 0.4202(9) 0.058(3) Uani 1 1 d . . . C23 C 0.2824(4) 0.1955(5) 0.3563(11) 0.087(4) Uani 1 1 d . . . C24 C 0.3159(4) 0.2237(5) 0.2940(12) 0.106(5) Uani 1 1 d . . . C25 C 0.0703(4) 0.2500 0.3730(11) 0.048(3) Uani 1 2 d S . . C26 C 0.0572(3) 0.2025(3) 0.4200(8) 0.043(2) Uani 1 1 d . . . C27 C 0.0663(3) 0.1554(4) 0.3571(8) 0.051(2) Uani 1 1 d . . . C28 C 0.0449(3) 0.1191(4) 0.4258(8) 0.051(2) Uani 1 1 d . . . C29 C 0.0224(3) 0.1459(3) 0.5265(7) 0.041(2) Uani 1 1 d . . . C30 C -0.0101(3) 0.1208(3) 0.6069(8) 0.045(2) Uani 1 1 d . . . C31 C -0.0397(3) 0.1452(3) 0.6887(7) 0.035(2) Uani 1 1 d . . . C32 C -0.0798(3) 0.1205(3) 0.7421(8) 0.048(2) Uani 1 1 d . . . C33 C -0.1037(3) 0.1571(3) 0.8053(8) 0.045(2) Uani 1 1 d . . . C34 C -0.0772(3) 0.2033(3) 0.7899(7) 0.042(2) Uani 1 1 d . . . C35 C -0.0929(4) 0.2500 0.8300(9) 0.040(3) Uani 1 2 d S . . C36 C 0.0924(4) 0.1489(5) 0.2359(11) 0.081(3) Uani 1 1 d . . . C37 C 0.1403(6) 0.1373(9) 0.2535(17) 0.177(9) Uani 1 1 d . . . C38 C 0.0432(4) 0.0623(4) 0.4017(10) 0.065(3) Uani 1 1 d . . . C39 C -0.0004(4) 0.0479(5) 0.3269(11) 0.089(4) Uani 1 1 d . . . C40 C -0.0946(4) 0.0665(4) 0.7211(8) 0.062(3) Uani 1 1 d . . . C41 C -0.1189(4) 0.0599(4) 0.5943(11) 0.089(4) Uani 1 1 d . . . C42 C -0.1502(3) 0.1523(4) 0.8673(9) 0.060(3) Uani 1 1 d . . . C43 C -0.1903(4) 0.1685(5) 0.7818(12) 0.091(4) 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 Ho1 0.0411(3) 0.0397(4) 0.0304(3) 0.000 0.0033(3) 0.000 N1 0.022(5) 0.026(5) 0.026(5) 0.000 -0.005(4) 0.000 N2 0.061(5) 0.033(4) 0.039(4) 0.009(3) 0.011(4) 0.002(4) N3 0.038(4) 0.039(4) 0.043(4) 0.005(3) 0.008(3) 0.006(3) N4 0.044(4) 0.047(5) 0.046(4) -0.001(4) 0.016(4) 0.007(4) N5 0.033(5) 0.037(6) 0.043(6) 0.000 -0.002(5) 0.000 N6 0.042(4) 0.032(4) 0.029(4) -0.005(3) 0.004(3) 0.001(3) N7 0.040(4) 0.042(4) 0.033(4) 0.001(3) 0.009(3) -0.001(3) C1 0.039(5) 0.042(6) 0.028(5) 0.003(4) 0.003(4) -0.001(4) C2 0.041(5) 0.053(5) 0.028(5) -0.002(4) 0.003(4) 0.005(4) C3 0.046(5) 0.059(6) 0.037(5) 0.003(5) 0.008(5) 0.003(4) C4 0.040(5) 0.070(6) 0.034(5) 0.001(4) -0.002(4) 0.002(4) C5 0.050(6) 0.103(8) 0.026(5) 0.016(5) -0.003(5) -0.003(6) C6 0.047(5) 0.098(8) 0.034(5) 0.000(5) -0.003(5) 0.001(5) C7 0.050(5) 0.041(6) 0.030(5) -0.003(4) 0.010(4) 0.003(4) C8 0.048(5) 0.042(6) 0.037(5) -0.003(4) 0.004(4) -0.002(4) C9 0.071(6) 0.033(6) 0.053(6) 0.001(5) -0.007(5) 0.002(5) C10 0.070(6) 0.032(5) 0.050(6) 0.008(4) -0.007(5) -0.003(5) C11 0.075(7) 0.045(7) 0.077(7) 0.010(6) -0.019(6) -0.001(6) C12 0.102(9) 0.059(8) 0.073(8) 0.004(6) -0.028(7) -0.013(7) C13 0.101(9) 0.064(8) 0.075(8) 0.006(6) -0.006(7) 0.011(7) C14 0.090(8) 0.033(6) 0.079(7) 0.003(5) -0.015(6) 0.002(6) C15 0.057(6) 0.042(6) 0.052(6) 0.004(5) -0.003(5) 0.004(5) C16 0.061(6) 0.039(6) 0.065(7) 0.003(5) 0.000(5) 0.008(5) C17 0.049(5) 0.051(6) 0.044(6) 0.005(4) 0.003(4) 0.006(5) C18 0.046(5) 0.030(5) 0.045(6) 0.000(4) -0.012(4) 0.005(4) C19 0.038(5) 0.039(6) 0.046(5) 0.011(4) 0.005(4) 0.001(4) C20 0.040(5) 0.056(6) 0.040(5) -0.004(4) 0.009(4) 0.008(4) C21 0.051(6) 0.075(7) 0.048(6) 0.002(5) 0.003(5) 0.010(5) C22 0.037(5) 0.080(7) 0.056(6) -0.002(5) 0.011(5) -0.003(5) C23 0.055(7) 0.108(10) 0.098(9) 0.005(7) 0.041(7) 0.012(7) C24 0.083(8) 0.116(11) 0.119(11) 0.000(8) 0.047(8) 0.010(7) C25 0.051(8) 0.050(9) 0.043(8) 0.000 -0.002(6) 0.000 C26 0.047(5) 0.047(6) 0.035(5) -0.007(4) 0.003(4) 0.003(5) C27 0.065(6) 0.053(6) 0.035(5) -0.003(5) 0.003(5) 0.000(5) C28 0.059(6) 0.054(6) 0.041(5) -0.005(5) 0.002(5) 0.008(5) C29 0.051(5) 0.037(5) 0.035(5) -0.011(4) -0.005(4) 0.007(5) C30 0.048(5) 0.050(6) 0.038(5) 0.004(4) -0.002(4) 0.003(4) C31 0.040(5) 0.034(5) 0.032(5) 0.001(4) 0.006(4) 0.006(4) C32 0.057(6) 0.043(6) 0.043(5) 0.007(4) -0.005(5) -0.015(5) C33 0.054(5) 0.045(5) 0.036(5) 0.007(5) 0.005(5) -0.006(5) C34 0.042(5) 0.052(6) 0.032(5) -0.006(4) -0.007(4) -0.007(4) C35 0.050(7) 0.049(8) 0.022(7) 0.000 0.007(5) 0.000 C36 0.069(8) 0.094(9) 0.081(8) -0.019(7) 0.032(6) 0.008(7) C37 0.105(12) 0.31(3) 0.118(13) -0.039(16) 0.014(11) 0.034(15) C38 0.090(8) 0.041(6) 0.065(7) -0.017(5) 0.014(6) 0.004(5) C39 0.097(9) 0.078(9) 0.093(9) -0.036(7) -0.024(7) -0.002(7) C40 0.079(7) 0.049(6) 0.057(7) 0.003(5) 0.007(6) -0.019(5) C41 0.102(9) 0.073(8) 0.091(9) -0.013(7) -0.033(8) -0.010(7) C42 0.042(5) 0.071(7) 0.066(7) 0.013(6) 0.016(5) -0.001(5) C43 0.051(7) 0.112(11) 0.110(10) 0.002(8) 0.009(7) -0.005(7) _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 Ho1 N7 2.409(6) . ? Ho1 N7 2.409(6) 7_565 ? Ho1 N6 2.413(6) . ? Ho1 N6 2.413(6) 7_565 ? Ho1 N3 2.455(6) 7_565 ? Ho1 N3 2.455(6) . ? Ho1 N1 2.458(8) . ? Ho1 N5 2.467(9) . ? N1 C1 1.346(9) . ? N1 C1 1.346(9) 7_565 ? N2 C7 1.332(10) . ? N2 C1 1.353(10) . ? N3 C7 1.360(10) . ? N3 C18 1.364(10) . ? N4 C19 1.314(10) . ? N4 C18 1.333(10) . ? N5 C19 1.351(9) . ? N5 C19 1.351(9) 7_565 ? N6 C29 1.329(10) . ? N6 C26 1.353(10) . ? N7 C31 1.361(10) . ? N7 C34 1.362(10) . ? C1 C2 1.478(11) . ? C2 C2 1.382(16) 7_565 ? C2 C3 1.387(11) . ? C3 C4 1.432(11) . ? C4 C4 1.434(18) 7_565 ? C4 C5 1.441(12) . ? C5 C6 1.381(12) . ? C6 C6 1.50(2) 7_565 ? C7 C8 1.440(11) . ? C8 C9 1.352(11) . ? C8 C17 1.417(11) . ? C9 C10 1.418(12) . ? C10 C15 1.406(12) . ? C10 C11 1.424(12) . ? C11 C12 1.427(14) . ? C12 C13 1.418(15) . ? C13 C14 1.378(14) . ? C14 C15 1.440(13) . ? C15 C16 1.420(12) . ? C16 C17 1.391(12) . ? C17 C18 1.486(11) . ? C19 C20 1.446(11) . ? C20 C21 1.375(11) . ? C20 C20 1.415(17) 7_565 ? C21 C22 1.421(12) . ? C22 C23 1.436(13) . ? C22 C22 1.454(19) 7_565 ? C23 C24 1.392(15) . ? C24 C24 1.39(3) 7_565 ? C25 C26 1.411(10) . ? C25 C26 1.411(10) 7_565 ? C26 C27 1.449(11) . ? C27 C28 1.366(12) . ? C27 C36 1.528(13) . ? C28 C29 1.458(11) . ? C28 C38 1.531(12) . ? C29 C30 1.438(11) . ? C30 C31 1.390(11) . ? C31 C32 1.442(11) . ? C32 C33 1.373(12) . ? C32 C40 1.511(12) . ? C33 C34 1.452(11) . ? C33 C42 1.494(11) . ? C34 C35 1.388(10) . ? C35 C34 1.388(10) 7_565 ? C36 C37 1.414(19) . ? C38 C39 1.536(15) . ? C40 C41 1.558(14) . ? C42 C43 1.538(14) . ? 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 N7 Ho1 N7 74.9(3) . 7_565 ? N7 Ho1 N6 75.1(2) . . ? N7 Ho1 N6 118.5(2) 7_565 . ? N7 Ho1 N6 118.5(2) . 7_565 ? N7 Ho1 N6 75.1(2) 7_565 7_565 ? N6 Ho1 N6 74.3(3) . 7_565 ? N7 Ho1 N3 142.7(2) . 7_565 ? N7 Ho1 N3 79.5(2) 7_565 7_565 ? N6 Ho1 N3 142.0(2) . 7_565 ? N6 Ho1 N3 79.5(2) 7_565 7_565 ? N7 Ho1 N3 79.5(2) . . ? N7 Ho1 N3 142.7(2) 7_565 . ? N6 Ho1 N3 79.5(2) . . ? N6 Ho1 N3 142.0(2) 7_565 . ? N3 Ho1 N3 107.0(3) 7_565 . ? N7 Ho1 N1 80.6(2) . . ? N7 Ho1 N1 80.6(2) 7_565 . ? N6 Ho1 N1 142.81(15) . . ? N6 Ho1 N1 142.81(15) 7_565 . ? N3 Ho1 N1 68.65(18) 7_565 . ? N3 Ho1 N1 68.65(18) . . ? N7 Ho1 N5 142.30(16) . . ? N7 Ho1 N5 142.30(16) 7_565 . ? N6 Ho1 N5 78.4(2) . . ? N6 Ho1 N5 78.4(2) 7_565 . ? N3 Ho1 N5 69.61(19) 7_565 . ? N3 Ho1 N5 69.61(19) . . ? N1 Ho1 N5 106.4(3) . . ? C1 N1 C1 106.8(9) . 7_565 ? C1 N1 Ho1 123.2(5) . . ? C1 N1 Ho1 123.2(5) 7_565 . ? C7 N2 C1 122.4(7) . . ? C7 N3 C18 107.5(7) . . ? C7 N3 Ho1 124.5(5) . . ? C18 N3 Ho1 122.0(5) . . ? C19 N4 C18 122.2(7) . . ? C19 N5 C19 108.6(9) . 7_565 ? C19 N5 Ho1 123.7(5) . . ? C19 N5 Ho1 123.7(5) 7_565 . ? C29 N6 C26 106.1(7) . . ? C29 N6 Ho1 123.8(5) . . ? C26 N6 Ho1 125.8(5) . . ? C31 N7 C34 106.2(7) . . ? C31 N7 Ho1 125.7(5) . . ? C34 N7 Ho1 126.7(5) . . ? N1 C1 N2 128.3(7) . . ? N1 C1 C2 111.3(7) . . ? N2 C1 C2 120.2(7) . . ? C2 C2 C3 122.5(5) 7_565 . ? C2 C2 C1 105.3(5) 7_565 . ? C3 C2 C1 132.2(8) . . ? C2 C3 C4 117.3(8) . . ? C3 C4 C4 120.1(5) . 7_565 ? C3 C4 C5 118.6(9) . . ? C4 C4 C5 121.3(6) 7_565 . ? C6 C5 C4 117.5(10) . . ? C5 C6 C6 121.2(6) . 7_565 ? N2 C7 N3 126.8(8) . . ? N2 C7 C8 120.3(7) . . ? N3 C7 C8 112.6(7) . . ? C9 C8 C17 121.2(8) . . ? C9 C8 C7 134.3(8) . . ? C17 C8 C7 104.4(7) . . ? C8 C9 C10 118.0(8) . . ? C15 C10 C9 120.8(8) . . ? C15 C10 C11 120.5(9) . . ? C9 C10 C11 118.7(9) . . ? C10 C11 C12 117.3(10) . . ? C13 C12 C11 122.0(10) . . ? C14 C13 C12 120.1(11) . . ? C13 C14 C15 119.2(10) . . ? C10 C15 C16 121.3(8) . . ? C10 C15 C14 120.8(9) . . ? C16 C15 C14 117.8(9) . . ? C17 C16 C15 115.6(8) . . ? C16 C17 C8 122.8(8) . . ? C16 C17 C18 130.7(8) . . ? C8 C17 C18 106.4(8) . . ? N4 C18 N3 129.2(7) . . ? N4 C18 C17 121.5(8) . . ? N3 C18 C17 108.9(7) . . ? N4 C19 N5 129.3(8) . . ? N4 C19 C20 120.6(8) . . ? N5 C19 C20 110.0(8) . . ? C21 C20 C20 122.3(6) . 7_565 ? C21 C20 C19 132.1(8) . . ? C20 C20 C19 105.6(5) 7_565 . ? C20 C21 C22 117.5(9) . . ? C21 C22 C23 119.8(9) . . ? C21 C22 C22 120.2(5) . 7_565 ? C23 C22 C22 120.0(6) . 7_565 ? C24 C23 C22 117.4(11) . . ? C23 C24 C24 122.6(7) . 7_565 ? C26 C25 C26 126.5(11) . 7_565 ? N6 C26 C25 125.1(8) . . ? N6 C26 C27 111.3(8) . . ? C25 C26 C27 123.3(8) . . ? C28 C27 C26 105.5(8) . . ? C28 C27 C36 127.9(9) . . ? C26 C27 C36 126.6(9) . . ? C27 C28 C29 105.5(8) . . ? C27 C28 C38 127.9(8) . . ? C29 C28 C38 126.5(8) . . ? N6 C29 C30 126.6(7) . . ? N6 C29 C28 111.6(8) . . ? C30 C29 C28 121.2(8) . . ? C31 C30 C29 124.6(8) . . ? N7 C31 C30 126.7(7) . . ? N7 C31 C32 111.0(7) . . ? C30 C31 C32 122.1(8) . . ? C33 C32 C31 106.1(8) . . ? C33 C32 C40 127.4(8) . . ? C31 C32 C40 126.3(9) . . ? C32 C33 C34 106.2(7) . . ? C32 C33 C42 127.5(8) . . ? C34 C33 C42 126.0(8) . . ? N7 C34 C35 126.0(8) . . ? N7 C34 C33 110.5(7) . . ? C35 C34 C33 123.2(8) . . ? C34 C35 C34 126.3(11) . 7_565 ? C37 C36 C27 112.2(12) . . ? C28 C38 C39 111.2(9) . . ? C32 C40 C41 111.6(8) . . ? C33 C42 C43 111.1(8) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 23.38 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.929 _refine_diff_density_min -0.877 _refine_diff_density_rms 0.128 data_020320a _database_code_CSD 194123 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H68 Er N12' _chemical_formula_weight 1412.76 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' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 28.617(5) _cell_length_b 26.626(5) _cell_length_c 10.918(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8319(3) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2663 _cell_measurement_theta_min 2.346 _cell_measurement_theta_max 17.075 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.128 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2896 _exptl_absorpt_coefficient_mu 1.055 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.7090 _exptl_absorpt_correction_T_max 0.9018 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 27634 _diffrn_reflns_av_R_equivalents 0.1422 _diffrn_reflns_av_sigmaI/netI 0.1611 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.28 _diffrn_reflns_theta_max 23.38 _reflns_number_total 5904 _reflns_number_gt 2881 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0315P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5904 _refine_ls_number_parameters 445 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1310 _refine_ls_R_factor_gt 0.0500 _refine_ls_wR_factor_ref 0.1076 _refine_ls_wR_factor_gt 0.0848 _refine_ls_goodness_of_fit_ref 0.861 _refine_ls_restrained_S_all 0.861 _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 Er1 Er 0.028813(15) 0.2500 0.69720(4) 0.04426(18) Uani 1 2 d S . . N1 N 0.0222(2) 0.2500 0.9205(6) 0.0282(17) Uani 1 2 d S . . N2 N 0.0191(2) 0.1605(2) 0.9660(5) 0.0526(16) Uani 1 1 d . . . N3 N 0.06655(18) 0.1752(2) 0.7871(6) 0.0470(15) Uani 1 1 d . . . N4 N 0.1290(2) 0.1604(3) 0.6402(6) 0.0550(17) Uani 1 1 d . . . N5 N 0.1135(3) 0.2500 0.6499(7) 0.048(2) Uani 1 2 d S . . N6 N 0.03170(19) 0.1949(2) 0.5211(5) 0.0448(14) Uani 1 1 d . . . N7 N -0.03739(19) 0.1949(2) 0.7202(5) 0.0460(15) Uani 1 1 d . . . C1 C 0.0089(2) 0.2096(3) 0.9858(6) 0.0421(18) Uani 1 1 d . . . C2 C -0.0166(2) 0.2228(2) 1.0996(6) 0.050(2) Uani 1 1 d . . . C3 C -0.0350(2) 0.1961(3) 1.1959(7) 0.0534(18) Uani 1 1 d . . . C4 C -0.0559(2) 0.2233(2) 1.2937(7) 0.0521(19) Uani 1 1 d . . . C5 C -0.0786(2) 0.1964(3) 1.3911(7) 0.065(2) Uani 1 1 d . . . C6 C -0.1009(2) 0.2238(3) 1.4819(7) 0.068(3) Uani 1 1 d . . . C7 C 0.0474(2) 0.1470(3) 0.8737(7) 0.0450(19) Uani 1 1 d . . . C8 C 0.0637(2) 0.0954(3) 0.8673(7) 0.050(2) Uani 1 1 d . . . C9 C 0.0547(3) 0.0534(3) 0.9342(7) 0.060(2) Uani 1 1 d . . . C10 C 0.0774(3) 0.0074(3) 0.8975(7) 0.060(2) Uani 1 1 d . . . C11 C 0.0674(3) -0.0381(3) 0.9657(9) 0.075(3) Uani 1 1 d . . . C12 C 0.0877(3) -0.0812(4) 0.9266(9) 0.081(3) Uani 1 1 d . . . C13 C 0.1161(3) -0.0834(3) 0.8253(11) 0.090(3) Uani 1 1 d . . . C14 C 0.1286(3) -0.0398(3) 0.7591(8) 0.081(3) Uani 1 1 d . . . C15 C 0.1071(2) 0.0072(3) 0.7968(9) 0.062(2) Uani 1 1 d . . . C16 C 0.1173(3) 0.0517(3) 0.7261(7) 0.062(2) Uani 1 1 d . . . C17 C 0.0950(2) 0.0945(3) 0.7660(6) 0.0480(19) Uani 1 1 d . . . C18 C 0.0975(3) 0.1467(3) 0.7226(7) 0.052(2) Uani 1 1 d . . . C19 C 0.1380(2) 0.2088(3) 0.6156(7) 0.0487(19) Uani 1 1 d . . . C20 C 0.1777(2) 0.2236(2) 0.5416(7) 0.052(2) Uani 1 1 d . . . C21 C 0.2119(3) 0.1955(3) 0.4852(7) 0.069(2) Uani 1 1 d . . . C22 C 0.2474(2) 0.2234(3) 0.4195(7) 0.062(2) Uani 1 1 d . . . C23 C 0.2829(3) 0.1975(4) 0.3571(8) 0.089(3) Uani 1 1 d . . . C24 C 0.3167(3) 0.2224(3) 0.2918(10) 0.119(4) Uani 1 1 d . . . C25 C 0.0710(4) 0.2500 0.3726(10) 0.057(3) Uani 1 2 d S . . C26 C 0.0572(2) 0.2040(3) 0.4164(7) 0.051(2) Uani 1 1 d . . . C27 C 0.0672(3) 0.1562(3) 0.3566(7) 0.060(2) Uani 1 1 d . . . C28 C 0.0453(2) 0.1195(3) 0.4256(7) 0.054(2) Uani 1 1 d . . . C29 C 0.0228(3) 0.1450(3) 0.5239(6) 0.0480(19) Uani 1 1 d . . . C30 C -0.0080(2) 0.1218(3) 0.6070(7) 0.052(2) Uani 1 1 d . . . C31 C -0.0382(2) 0.1455(3) 0.6890(7) 0.0429(17) Uani 1 1 d . . . C32 C -0.0794(3) 0.1214(3) 0.7426(6) 0.054(2) Uani 1 1 d . . . C33 C -0.1019(2) 0.1569(3) 0.8061(7) 0.0485(18) Uani 1 1 d . . . C34 C -0.0761(2) 0.2033(3) 0.7882(7) 0.0464(18) Uani 1 1 d . . . C35 C -0.0913(3) 0.2500 0.8284(8) 0.045(3) Uani 1 2 d S . . C36 C 0.0920(3) 0.1493(3) 0.2363(8) 0.097(3) Uani 1 1 d . . . C37 C 0.1429(5) 0.1412(7) 0.2501(13) 0.217(8) Uani 1 1 d . . . C38 C 0.0428(3) 0.0631(3) 0.4012(8) 0.073(2) Uani 1 1 d . . . C39 C 0.0005(3) 0.0478(3) 0.3273(10) 0.110(4) Uani 1 1 d . . . C40 C -0.0937(3) 0.0670(3) 0.7194(8) 0.076(2) Uani 1 1 d . . . C41 C -0.1193(3) 0.0612(3) 0.5961(9) 0.099(3) Uani 1 1 d . . . C42 C -0.1489(3) 0.1520(3) 0.8692(7) 0.080(3) Uani 1 1 d . . . C43 C -0.1893(3) 0.1684(4) 0.7822(10) 0.104(3) 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 Er1 0.0438(3) 0.0508(3) 0.0382(3) 0.000 0.0033(3) 0.000 N1 0.046(5) 0.035(5) 0.004(4) 0.000 -0.003(3) 0.000 N2 0.061(4) 0.047(4) 0.050(4) 0.008(3) 0.006(3) 0.002(3) N3 0.041(3) 0.054(4) 0.046(4) 0.001(4) 0.010(3) 0.003(3) N4 0.042(4) 0.062(5) 0.061(4) 0.008(4) 0.012(3) 0.005(3) N5 0.034(5) 0.059(6) 0.053(6) 0.000 0.012(4) 0.000 N6 0.038(3) 0.053(4) 0.044(4) 0.000(3) 0.003(3) 0.003(3) N7 0.057(4) 0.051(4) 0.030(4) 0.003(3) 0.012(3) -0.005(3) C1 0.051(4) 0.053(6) 0.022(4) 0.006(4) 0.010(3) 0.001(4) C2 0.055(5) 0.058(5) 0.036(4) -0.005(4) 0.006(4) 0.001(3) C3 0.058(4) 0.076(5) 0.026(4) 0.005(4) 0.008(4) -0.003(4) C4 0.051(4) 0.071(5) 0.035(4) -0.006(4) -0.016(4) 0.001(3) C5 0.050(5) 0.104(7) 0.040(5) 0.012(5) 0.006(4) -0.006(5) C6 0.052(5) 0.100(7) 0.052(5) 0.001(4) -0.003(4) -0.010(4) C7 0.050(5) 0.040(5) 0.045(5) -0.002(4) 0.006(4) -0.005(4) C8 0.045(5) 0.053(6) 0.053(5) -0.002(4) 0.003(4) 0.010(4) C9 0.068(5) 0.045(5) 0.066(6) 0.014(5) -0.017(4) -0.011(5) C10 0.064(6) 0.066(7) 0.052(5) 0.009(5) 0.001(4) 0.002(5) C11 0.089(7) 0.047(6) 0.090(7) -0.002(6) -0.018(5) -0.003(5) C12 0.094(7) 0.084(8) 0.066(7) -0.002(6) -0.002(6) -0.007(6) C13 0.099(7) 0.056(6) 0.113(9) 0.014(7) -0.030(7) 0.006(5) C14 0.092(6) 0.049(6) 0.103(8) -0.001(5) -0.021(5) 0.012(5) C15 0.061(5) 0.048(5) 0.077(6) -0.010(6) 0.000(5) 0.006(4) C16 0.063(5) 0.051(5) 0.073(6) 0.004(5) -0.001(4) 0.005(4) C17 0.051(5) 0.037(5) 0.055(5) 0.004(4) -0.002(4) 0.002(4) C18 0.046(5) 0.058(6) 0.051(6) 0.005(5) -0.001(4) 0.003(4) C19 0.040(5) 0.057(6) 0.048(5) 0.001(5) 0.000(4) 0.009(4) C20 0.038(4) 0.068(6) 0.049(5) -0.003(4) 0.012(4) 0.001(3) C21 0.048(5) 0.097(7) 0.063(6) 0.020(5) 0.005(4) 0.012(5) C22 0.031(4) 0.105(7) 0.051(5) -0.004(4) 0.010(4) 0.007(4) C23 0.071(6) 0.118(8) 0.077(7) -0.004(6) 0.029(5) 0.006(6) C24 0.096(7) 0.148(10) 0.112(8) 0.002(7) 0.052(6) -0.008(6) C25 0.072(8) 0.055(8) 0.045(7) 0.000 -0.007(6) 0.000 C26 0.043(4) 0.068(6) 0.041(5) -0.008(5) -0.004(4) -0.003(4) C27 0.067(5) 0.071(6) 0.042(5) -0.008(5) 0.014(4) 0.010(5) C28 0.060(5) 0.052(6) 0.048(5) -0.011(5) -0.004(4) 0.009(4) C29 0.069(5) 0.035(5) 0.040(5) -0.004(4) -0.005(4) -0.007(4) C30 0.060(5) 0.052(5) 0.044(5) 0.007(4) -0.005(4) -0.002(4) C31 0.045(5) 0.045(5) 0.038(4) -0.003(4) 0.003(4) 0.003(4) C32 0.060(5) 0.051(5) 0.052(5) 0.009(4) -0.005(4) -0.008(4) C33 0.052(5) 0.052(5) 0.042(4) 0.007(5) -0.001(4) -0.005(4) C34 0.055(5) 0.051(5) 0.034(4) 0.009(4) -0.009(4) 0.005(4) C35 0.060(6) 0.052(7) 0.023(6) 0.000 0.008(5) 0.000 C36 0.088(7) 0.114(8) 0.088(8) -0.017(6) 0.030(6) 0.012(6) C37 0.122(11) 0.39(2) 0.136(13) -0.046(13) 0.002(9) 0.088(12) C38 0.080(6) 0.067(6) 0.072(6) -0.016(5) 0.017(5) 0.008(5) C39 0.108(7) 0.085(7) 0.138(10) -0.041(7) -0.025(7) -0.004(6) C40 0.097(6) 0.054(5) 0.076(7) -0.011(5) -0.003(5) -0.033(5) C41 0.109(7) 0.097(7) 0.090(7) -0.016(6) -0.021(6) -0.018(6) C42 0.049(5) 0.127(8) 0.063(6) 0.019(5) 0.016(4) -0.002(5) C43 0.053(5) 0.137(9) 0.123(9) 0.028(7) 0.013(6) -0.004(5) _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 Er1 N7 2.409(5) 7_565 ? Er1 N7 2.409(5) . ? Er1 N6 2.419(5) . ? Er1 N6 2.419(5) 7_565 ? Er1 N1 2.445(6) . ? Er1 N3 2.468(6) 7_565 ? Er1 N3 2.468(6) . ? Er1 N5 2.477(7) . ? N1 C1 1.347(7) . ? N1 C1 1.347(7) 7_565 ? N2 C7 1.342(8) . ? N2 C1 1.356(8) . ? N3 C7 1.326(8) . ? N3 C18 1.362(8) . ? N4 C18 1.325(8) . ? N4 C19 1.339(8) . ? N5 C19 1.355(8) 7_565 ? N5 C19 1.355(8) . ? N6 C29 1.355(8) . ? N6 C26 1.377(8) . ? N7 C34 1.351(8) . ? N7 C31 1.361(7) . ? C1 C2 1.483(9) . ? C2 C3 1.375(9) . ? C2 C2 1.447(13) 7_565 ? C3 C4 1.423(9) . ? C4 C4 1.421(13) 7_565 ? C4 C5 1.438(9) . ? C5 C6 1.386(10) . ? C6 C6 1.395(16) 7_565 ? C7 C8 1.454(9) . ? C8 C9 1.361(9) . ? C8 C17 1.423(9) . ? C9 C10 1.441(10) . ? C10 C15 1.389(10) . ? C10 C11 1.453(10) . ? C11 C12 1.355(11) . ? C12 C13 1.375(11) . ? C13 C14 1.415(11) . ? C14 C15 1.453(10) . ? C15 C16 1.446(10) . ? C16 C17 1.376(9) . ? C17 C18 1.471(9) . ? C19 C20 1.450(9) . ? C20 C21 1.377(9) . ? C20 C20 1.405(13) 7_565 ? C21 C22 1.449(9) . ? C22 C23 1.405(10) . ? C22 C22 1.419(15) 7_565 ? C23 C24 1.372(11) . ? C24 C24 1.468(18) 7_565 ? C25 C26 1.374(8) . ? C25 C26 1.374(8) 7_565 ? C26 C27 1.458(10) . ? C27 C28 1.383(9) . ? C27 C36 1.505(10) . ? C28 C29 1.424(9) . ? C28 C38 1.528(10) . ? C29 C30 1.406(9) . ? C30 C31 1.395(9) . ? C31 C32 1.463(9) . ? C32 C33 1.336(9) . ? C32 C40 1.527(9) . ? C33 C34 1.451(8) . ? C33 C42 1.518(10) . ? C34 C35 1.390(8) . ? C35 C34 1.390(8) 7_565 ? C36 C37 1.480(14) . ? C38 C39 1.511(11) . ? C40 C41 1.539(11) . ? C42 C43 1.559(12) . ? 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 N7 Er1 N7 75.0(3) 7_565 . ? N7 Er1 N6 118.60(17) 7_565 . ? N7 Er1 N6 74.99(19) . . ? N7 Er1 N6 74.99(19) 7_565 7_565 ? N7 Er1 N6 118.60(17) . 7_565 ? N6 Er1 N6 74.6(3) . 7_565 ? N7 Er1 N1 80.52(18) 7_565 . ? N7 Er1 N1 80.52(18) . . ? N6 Er1 N1 142.66(14) . . ? N6 Er1 N1 142.66(14) 7_565 . ? N7 Er1 N3 79.15(18) 7_565 7_565 ? N7 Er1 N3 142.52(19) . 7_565 ? N6 Er1 N3 142.2(2) . 7_565 ? N6 Er1 N3 79.19(19) 7_565 7_565 ? N1 Er1 N3 68.73(17) . 7_565 ? N7 Er1 N3 142.52(19) 7_565 . ? N7 Er1 N3 79.15(18) . . ? N6 Er1 N3 79.19(19) . . ? N6 Er1 N3 142.2(2) 7_565 . ? N1 Er1 N3 68.73(17) . . ? N3 Er1 N3 107.5(3) 7_565 . ? N7 Er1 N5 142.28(14) 7_565 . ? N7 Er1 N5 142.28(14) . . ? N6 Er1 N5 78.52(19) . . ? N6 Er1 N5 78.52(19) 7_565 . ? N1 Er1 N5 106.4(2) . . ? N3 Er1 N5 69.82(16) 7_565 . ? N3 Er1 N5 69.82(16) . . ? C1 N1 C1 106.1(8) . 7_565 ? C1 N1 Er1 123.4(4) . . ? C1 N1 Er1 123.4(4) 7_565 . ? C7 N2 C1 120.5(6) . . ? C7 N3 C18 108.8(6) . . ? C7 N3 Er1 124.0(5) . . ? C18 N3 Er1 121.9(5) . . ? C18 N4 C19 122.1(7) . . ? C19 N5 C19 108.2(9) 7_565 . ? C19 N5 Er1 124.3(4) 7_565 . ? C19 N5 Er1 124.3(4) . . ? C29 N6 C26 106.8(6) . . ? C29 N6 Er1 124.8(4) . . ? C26 N6 Er1 124.9(5) . . ? C34 N7 C31 106.4(6) . . ? C34 N7 Er1 127.0(5) . . ? C31 N7 Er1 125.2(4) . . ? N1 C1 N2 128.6(6) . . ? N1 C1 C2 113.2(7) . . ? N2 C1 C2 117.9(6) . . ? C3 C2 C2 121.2(4) . 7_565 ? C3 C2 C1 134.9(6) . . ? C2 C2 C1 103.7(4) 7_565 . ? C2 C3 C4 118.1(6) . . ? C4 C4 C3 120.7(4) 7_565 . ? C4 C4 C5 119.9(4) 7_565 . ? C3 C4 C5 119.4(6) . . ? C6 C5 C4 118.3(8) . . ? C5 C6 C6 121.8(5) . 7_565 ? N3 C7 N2 129.3(7) . . ? N3 C7 C8 111.6(7) . . ? N2 C7 C8 118.9(7) . . ? C9 C8 C17 121.6(7) . . ? C9 C8 C7 133.6(7) . . ? C17 C8 C7 104.8(7) . . ? C8 C9 C10 117.5(7) . . ? C15 C10 C9 120.0(8) . . ? C15 C10 C11 121.5(8) . . ? C9 C10 C11 118.5(8) . . ? C12 C11 C10 117.4(9) . . ? C11 C12 C13 123.0(9) . . ? C12 C13 C14 121.7(9) . . ? C13 C14 C15 117.0(9) . . ? C10 C15 C16 122.8(7) . . ? C10 C15 C14 119.3(8) . . ? C16 C15 C14 117.9(8) . . ? C17 C16 C15 114.6(7) . . ? C16 C17 C8 123.5(7) . . ? C16 C17 C18 131.1(7) . . ? C8 C17 C18 105.4(7) . . ? N4 C18 N3 129.8(7) . . ? N4 C18 C17 120.8(7) . . ? N3 C18 C17 109.2(7) . . ? N4 C19 N5 128.6(6) . . ? N4 C19 C20 121.6(7) . . ? N5 C19 C20 109.8(7) . . ? C21 C20 C20 123.0(4) . 7_565 ? C21 C20 C19 131.1(7) . . ? C20 C20 C19 105.8(4) 7_565 . ? C20 C21 C22 116.1(7) . . ? C23 C22 C22 119.4(5) . 7_565 ? C23 C22 C21 119.8(7) . . ? C22 C22 C21 120.8(4) 7_565 . ? C24 C23 C22 121.6(9) . . ? C23 C24 C24 119.0(5) . 7_565 ? C26 C25 C26 126.3(11) . 7_565 ? C25 C26 N6 126.7(8) . . ? C25 C26 C27 124.4(7) . . ? N6 C26 C27 108.9(7) . . ? C28 C27 C26 106.4(7) . . ? C28 C27 C36 127.1(8) . . ? C26 C27 C36 126.2(8) . . ? C27 C28 C29 106.3(7) . . ? C27 C28 C38 128.4(7) . . ? C29 C28 C38 125.3(7) . . ? N6 C29 C30 124.3(7) . . ? N6 C29 C28 111.4(7) . . ? C30 C29 C28 124.2(7) . . ? C31 C30 C29 127.2(7) . . ? N7 C31 C30 125.9(6) . . ? N7 C31 C32 109.7(6) . . ? C30 C31 C32 124.0(7) . . ? C33 C32 C31 106.6(6) . . ? C33 C32 C40 128.9(7) . . ? C31 C32 C40 124.4(7) . . ? C32 C33 C34 106.7(7) . . ? C32 C33 C42 126.9(7) . . ? C34 C33 C42 125.8(7) . . ? N7 C34 C35 125.3(7) . . ? N7 C34 C33 110.5(6) . . ? C35 C34 C33 124.0(7) . . ? C34 C35 C34 127.1(9) 7_565 . ? C37 C36 C27 113.2(9) . . ? C39 C38 C28 113.2(7) . . ? C32 C40 C41 111.6(7) . . ? C33 C42 C43 110.9(7) . . ? _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 23.38 _diffrn_measured_fraction_theta_full 0.949 _refine_diff_density_max 1.147 _refine_diff_density_min -0.592 _refine_diff_density_rms 0.077 data_f11121b _database_code_CSD 194124 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C88 H72 N8 Tm' _chemical_formula_weight 1410.47 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' Tm Tm -0.3139 5.2483 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 28.632(14) _cell_length_b 26.669(13) _cell_length_c 10.938(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8352(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1323 _cell_measurement_theta_min 3.671 _cell_measurement_theta_max 18.375 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.122 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2900 _exptl_absorpt_coefficient_mu 1.107 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7324 _exptl_absorpt_correction_T_max 0.8974 _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 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'OMEGA SCAN' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 4.30 _diffrn_reflns_number 35772 _diffrn_reflns_av_R_equivalents 0.0876 _diffrn_reflns_av_sigmaI/netI 0.0587 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 26.01 _reflns_number_total 8392 _reflns_number_gt 6416 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0859P)^2^+21.3441P] 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 const _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00053(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8392 _refine_ls_number_parameters 446 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1013 _refine_ls_R_factor_gt 0.0752 _refine_ls_wR_factor_ref 0.2009 _refine_ls_wR_factor_gt 0.1885 _refine_ls_goodness_of_fit_ref 1.236 _refine_ls_restrained_S_all 1.236 _refine_ls_shift/su_max 0.002 _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 Tm1 Tm 0.028567(15) 0.7500 0.69709(4) 0.03179(16) Uani 1 2 d S . . N1 N 0.0188(3) 0.7500 0.9211(8) 0.042(2) Uani 1 2 d S . . N2 N 0.0663(2) 0.6763(2) 0.7853(5) 0.0351(13) Uani 1 1 d . . . N3 N 0.1122(3) 0.7500 0.6526(8) 0.0358(19) Uani 1 2 d S . . N4 N -0.03718(19) 0.6947(2) 0.7203(5) 0.0337(13) Uani 1 1 d . . . N5 N 0.0311(2) 0.6952(2) 0.5226(5) 0.0363(13) Uani 1 1 d . . . C1 C 0.0079(2) 0.7081(3) 0.9868(6) 0.0347(15) Uani 1 1 d . . . C2 C -0.0163(2) 0.7237(3) 1.1001(7) 0.0385(16) Uani 1 1 d . . . C3 C -0.0344(2) 0.6966(3) 1.1964(7) 0.0429(17) Uani 1 1 d . . . H3A H -0.0322 0.6618 1.1978 0.052 Uiso 1 1 calc R . . C4 C -0.0564(2) 0.7228(3) 1.2929(7) 0.0431(18) Uani 1 1 d . . . C5 C -0.0785(3) 0.6975(4) 1.3913(7) 0.053(2) Uani 1 1 d . . . H5A H -0.0783 0.6626 1.3936 0.063 Uiso 1 1 calc R . . C6 C -0.0998(3) 0.7235(4) 1.4819(7) 0.056(2) Uani 1 1 d . . . H6A H -0.1146 0.7063 1.5449 0.067 Uiso 1 1 calc R . . C7 C 0.0182(2) 0.6611(2) 0.9638(5) 0.0239(13) Uani 1 1 d . . . H7A H 0.0050 0.6365 1.0131 0.029 Uiso 1 1 calc R . . C8 C 0.0464(3) 0.6467(3) 0.8748(6) 0.0362(16) Uani 1 1 d . . . C9 C 0.0634(3) 0.5947(3) 0.8648(7) 0.0387(16) Uani 1 1 d . . . C10 C 0.0551(3) 0.5525(3) 0.9326(7) 0.0456(18) Uani 1 1 d . . . H10A H 0.0356 0.5535 1.0006 0.055 Uiso 1 1 calc R . . C11 C 0.0769(3) 0.5076(3) 0.8964(8) 0.0482(19) Uani 1 1 d . . . C12 C 0.0684(3) 0.4613(3) 0.9602(9) 0.059(2) Uani 1 1 d . . . H12A H 0.0488 0.4613 1.0280 0.071 Uiso 1 1 calc R . . C13 C 0.0884(4) 0.4174(3) 0.9231(10) 0.066(3) Uani 1 1 d . . . H13A H 0.0822 0.3877 0.9648 0.079 Uiso 1 1 calc R . . C14 C 0.1178(4) 0.4173(3) 0.8237(11) 0.073(3) Uani 1 1 d . . . H14A H 0.1315 0.3873 0.7993 0.087 Uiso 1 1 calc R . . C15 C 0.1275(3) 0.4601(3) 0.7598(10) 0.062(2) Uani 1 1 d . . . H15A H 0.1476 0.4587 0.6930 0.074 Uiso 1 1 calc R . . C16 C 0.1076(3) 0.5062(3) 0.7935(8) 0.0492(19) Uani 1 1 d . . . C17 C 0.1167(3) 0.5511(3) 0.7300(8) 0.048(2) Uani 1 1 d . . . H17A H 0.1374 0.5514 0.6644 0.058 Uiso 1 1 calc R . . C18 C 0.0949(3) 0.5941(3) 0.7659(7) 0.0420(17) Uani 1 1 d . . . C19 C 0.0971(3) 0.6465(3) 0.7221(7) 0.0400(17) Uani 1 1 d . . . C20 C 0.1283(2) 0.6610(2) 0.6394(6) 0.0255(13) Uani 1 1 d . . . H20A H 0.1454 0.6364 0.5989 0.031 Uiso 1 1 calc R . . C21 C 0.1364(2) 0.7077(3) 0.6121(7) 0.0378(16) Uani 1 1 d . . . C22 C 0.1774(2) 0.7232(3) 0.5408(7) 0.0406(17) Uani 1 1 d . . . C23 C 0.2114(3) 0.6960(3) 0.4834(8) 0.048(2) Uani 1 1 d . . . H23A H 0.2114 0.6611 0.4853 0.058 Uiso 1 1 calc R . . C24 C 0.2467(3) 0.7232(4) 0.4209(8) 0.058(2) Uani 1 1 d . . . C25 C 0.2833(3) 0.6973(4) 0.3558(11) 0.079(3) Uani 1 1 d . . . H25A H 0.2839 0.6625 0.3538 0.095 Uiso 1 1 calc R . . C26 C 0.3165(4) 0.7239(5) 0.2982(12) 0.101(5) Uani 1 1 d . . . H26A H 0.3402 0.7070 0.2572 0.122 Uiso 1 1 calc R . . C27 C 0.0570(3) 0.7039(3) 0.4185(7) 0.0398(17) Uani 1 1 d . . . C28 C 0.0663(3) 0.6561(3) 0.3561(8) 0.0491(19) Uani 1 1 d . . . C29 C 0.0453(3) 0.6191(3) 0.4246(7) 0.0460(19) Uani 1 1 d . . . C30 C 0.0220(2) 0.6454(3) 0.5263(6) 0.0354(16) Uani 1 1 d . . . C31 C -0.0087(3) 0.6221(3) 0.6055(6) 0.0382(16) Uani 1 1 d . . . H31A H -0.0095 0.5872 0.6032 0.046 Uiso 1 1 calc R . . C32 C -0.0386(2) 0.6454(3) 0.6884(6) 0.0333(15) Uani 1 1 d . . . C33 C -0.0794(3) 0.6209(3) 0.7436(7) 0.0411(17) Uani 1 1 d . . . C34 C -0.1026(3) 0.6568(3) 0.8063(7) 0.0425(17) Uani 1 1 d . . . C35 C -0.0761(2) 0.7033(3) 0.7895(6) 0.0335(15) Uani 1 1 d . . . C36 C 0.0705(4) 0.7500 0.3738(10) 0.047(3) Uani 1 2 d S . . H36A H 0.0906 0.7500 0.3070 0.056 Uiso 1 2 calc SR . . C37 C 0.0929(4) 0.6488(4) 0.2373(10) 0.072(3) Uani 1 1 d . . . H37A H 0.0785 0.6217 0.1917 0.086 Uiso 1 1 calc R . . H37B H 0.0903 0.6791 0.1887 0.086 Uiso 1 1 calc R . . C38 C 0.1406(6) 0.6377(10) 0.2547(17) 0.194(11) Uani 1 1 d . . . H38A H 0.1555 0.6338 0.1767 0.291 Uiso 1 1 calc R . . H38B H 0.1435 0.6071 0.3004 0.291 Uiso 1 1 calc R . . H38C H 0.1552 0.6645 0.2989 0.291 Uiso 1 1 calc R . . C39 C 0.0427(3) 0.5641(3) 0.3999(9) 0.060(2) Uani 1 1 d . . . H39A H 0.0428 0.5463 0.4773 0.072 Uiso 1 1 calc R . . H39B H 0.0704 0.5540 0.3550 0.072 Uiso 1 1 calc R . . C40 C -0.0002(5) 0.5484(4) 0.3277(12) 0.089(4) Uani 1 1 d . . . H40A H 0.0003 0.5128 0.3150 0.133 Uiso 1 1 calc R . . H40B H -0.0003 0.5652 0.2501 0.133 Uiso 1 1 calc R . . H40C H -0.0278 0.5574 0.3724 0.133 Uiso 1 1 calc R . . C41 C -0.0940(3) 0.5675(3) 0.7192(8) 0.057(2) Uani 1 1 d . . . H41A H -0.1144 0.5565 0.7846 0.068 Uiso 1 1 calc R . . H41B H -0.0664 0.5463 0.7208 0.068 Uiso 1 1 calc R . . C42 C -0.1188(4) 0.5601(4) 0.5979(11) 0.087(4) Uani 1 1 d . . . H42A H -0.1270 0.5254 0.5884 0.130 Uiso 1 1 calc R . . H42B H -0.0986 0.5701 0.5323 0.130 Uiso 1 1 calc R . . H42C H -0.1467 0.5802 0.5963 0.130 Uiso 1 1 calc R . . C43 C -0.1495(3) 0.6530(4) 0.8675(9) 0.058(2) Uani 1 1 d . . . H43A H -0.1497 0.6745 0.9390 0.069 Uiso 1 1 calc R . . H43B H -0.1541 0.6188 0.8951 0.069 Uiso 1 1 calc R . . C44 C -0.1897(3) 0.6676(5) 0.7851(11) 0.084(3) Uani 1 1 d . . . H44A H -0.2185 0.6645 0.8292 0.126 Uiso 1 1 calc R . . H44B H -0.1903 0.6459 0.7151 0.126 Uiso 1 1 calc R . . H44C H -0.1857 0.7017 0.7587 0.126 Uiso 1 1 calc R . . C45 C -0.0919(3) 0.7500 0.8302(9) 0.039(2) Uani 1 2 d S . . H45A H -0.1150 0.7500 0.8898 0.047 Uiso 1 2 calc SR . . 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 Tm1 0.0304(2) 0.0349(2) 0.0301(2) 0.000 0.0034(2) 0.000 N1 0.033(5) 0.061(6) 0.032(5) 0.000 -0.001(4) 0.000 N2 0.031(3) 0.039(3) 0.035(3) -0.001(3) 0.004(2) 0.004(2) N3 0.029(4) 0.037(5) 0.042(5) 0.000 0.005(4) 0.000 N4 0.031(3) 0.039(3) 0.031(3) -0.002(2) -0.001(2) 0.003(2) N5 0.036(3) 0.040(3) 0.033(3) 0.004(2) 0.001(3) -0.004(3) C1 0.034(4) 0.041(4) 0.028(3) 0.000(3) -0.003(3) -0.002(3) C2 0.035(4) 0.047(4) 0.034(4) 0.000(3) 0.002(3) 0.005(3) C3 0.038(4) 0.053(4) 0.037(4) 0.006(3) 0.002(4) 0.003(3) C4 0.031(4) 0.067(5) 0.031(4) 0.005(3) -0.005(3) -0.003(3) C5 0.049(5) 0.075(6) 0.034(4) 0.007(4) -0.003(4) -0.004(4) C6 0.043(4) 0.099(7) 0.026(4) 0.001(4) 0.007(3) -0.007(4) C7 0.030(3) 0.021(3) 0.021(3) 0.002(2) 0.006(2) 0.001(2) C8 0.042(4) 0.036(4) 0.030(4) 0.006(3) -0.005(3) 0.000(3) C9 0.043(4) 0.038(4) 0.035(4) 0.001(3) -0.002(3) 0.004(3) C10 0.054(5) 0.044(4) 0.039(4) 0.004(3) 0.001(4) 0.002(4) C11 0.059(5) 0.037(4) 0.049(5) 0.004(3) -0.008(4) -0.003(4) C12 0.074(6) 0.044(5) 0.060(5) 0.009(4) -0.008(5) -0.006(4) C13 0.087(7) 0.042(5) 0.068(6) 0.012(4) -0.014(6) 0.004(5) C14 0.089(8) 0.038(5) 0.091(8) -0.003(5) -0.023(6) 0.015(5) C15 0.066(6) 0.047(5) 0.071(6) -0.003(4) -0.001(5) 0.015(4) C16 0.053(5) 0.042(4) 0.052(5) 0.001(4) -0.005(4) 0.003(4) C17 0.048(5) 0.043(4) 0.054(5) 0.002(4) 0.007(4) 0.010(4) C18 0.041(4) 0.041(4) 0.044(4) 0.003(3) 0.003(3) 0.003(3) C19 0.044(4) 0.034(4) 0.041(4) 0.001(3) -0.003(3) 0.006(3) C20 0.022(3) 0.027(3) 0.027(3) 0.000(3) 0.006(3) 0.004(2) C21 0.026(3) 0.052(4) 0.036(4) -0.003(3) 0.003(3) 0.003(3) C22 0.032(4) 0.048(4) 0.042(4) 0.000(3) 0.008(3) 0.002(3) C23 0.038(4) 0.057(5) 0.050(5) 0.005(4) 0.008(4) 0.009(4) C24 0.036(4) 0.090(6) 0.047(5) -0.002(4) 0.015(4) 0.004(4) C25 0.058(6) 0.080(7) 0.099(8) 0.012(6) 0.042(6) 0.022(5) C26 0.067(7) 0.113(9) 0.125(11) -0.013(8) 0.059(7) 0.014(6) C27 0.042(4) 0.046(4) 0.031(4) -0.007(3) 0.002(3) 0.004(3) C28 0.054(5) 0.050(5) 0.044(4) -0.008(4) 0.006(4) 0.005(4) C29 0.051(4) 0.048(5) 0.039(4) -0.007(4) -0.001(4) 0.009(4) C30 0.036(4) 0.039(4) 0.031(3) -0.006(3) -0.002(3) 0.008(3) C31 0.045(4) 0.034(4) 0.035(4) -0.002(3) -0.002(3) -0.004(3) C32 0.022(3) 0.041(4) 0.036(4) -0.001(3) -0.002(3) 0.001(3) C33 0.045(4) 0.035(4) 0.044(4) 0.006(3) -0.001(4) -0.008(3) C34 0.046(4) 0.043(4) 0.038(4) 0.009(3) 0.007(4) -0.007(3) C35 0.030(3) 0.042(4) 0.028(3) 0.004(3) 0.002(3) -0.005(3) C36 0.049(7) 0.060(7) 0.031(6) 0.000 0.010(5) 0.000 C37 0.079(7) 0.068(6) 0.067(6) -0.019(5) 0.033(6) 0.008(5) C38 0.094(12) 0.37(4) 0.117(13) -0.032(19) 0.039(11) 0.035(17) C39 0.071(6) 0.049(5) 0.060(5) -0.010(4) 0.008(5) 0.011(4) C40 0.100(9) 0.066(7) 0.101(9) -0.025(6) -0.015(7) 0.005(6) C41 0.059(5) 0.042(5) 0.068(6) 0.005(4) 0.013(5) -0.010(4) C42 0.096(8) 0.071(7) 0.093(8) -0.026(6) -0.018(7) -0.020(6) C43 0.046(5) 0.060(5) 0.067(6) 0.006(5) 0.019(4) -0.009(4) C44 0.047(5) 0.115(10) 0.090(8) -0.004(7) 0.012(6) 0.004(6) C45 0.029(5) 0.050(6) 0.039(6) 0.000 0.010(4) 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 Tm1 N5 2.405(6) . ? Tm1 N5 2.405(6) 7_575 ? Tm1 N4 2.406(6) . ? Tm1 N4 2.406(6) 7_575 ? Tm1 N2 2.441(6) 7_575 ? Tm1 N2 2.441(6) . ? Tm1 N3 2.444(8) . ? Tm1 N1 2.466(9) . ? N1 C1 1.366(8) . ? N1 C1 1.366(8) 7_575 ? N2 C19 1.375(9) . ? N2 C8 1.380(9) . ? N3 C21 1.395(9) 7_575 ? N3 C21 1.395(9) . ? N4 C32 1.360(9) . ? N4 C35 1.365(8) . ? N5 C30 1.354(9) . ? N5 C27 1.378(9) . ? C1 C7 1.311(9) . ? C1 C2 1.480(10) . ? C2 C3 1.379(10) . ? C2 C2 1.401(15) 7_575 ? C3 C4 1.413(11) . ? C4 C5 1.419(11) . ? C4 C4 1.452(17) 7_575 ? C5 C6 1.356(12) . ? C6 C6 1.412(19) 7_575 ? C7 C8 1.322(9) . ? C8 C9 1.472(10) . ? C9 C10 1.368(10) . ? C9 C18 1.410(11) . ? C10 C11 1.409(11) . ? C11 C16 1.428(12) . ? C11 C12 1.439(11) . ? C12 C13 1.367(13) . ? C13 C14 1.374(15) . ? C14 C15 1.367(14) . ? C15 C16 1.405(12) . ? C16 C17 1.409(12) . ? C17 C18 1.364(11) . ? C18 C19 1.478(10) . ? C19 C20 1.329(10) . ? C20 C21 1.303(10) . ? C21 C22 1.469(10) . ? C22 C23 1.367(10) . ? C22 C22 1.428(15) 7_575 ? C23 C24 1.419(11) . ? C24 C24 1.43(2) 7_575 ? C24 C25 1.443(12) . ? C25 C26 1.343(15) . ? C26 C26 1.39(3) 7_575 ? C27 C36 1.379(9) . ? C27 C28 1.469(10) . ? C28 C29 1.377(12) . ? C28 C37 1.518(12) . ? C29 C30 1.475(10) . ? C29 C39 1.494(11) . ? C30 C31 1.383(10) . ? C31 C32 1.393(10) . ? C32 C33 1.470(10) . ? C33 C34 1.352(11) . ? C33 C41 1.507(11) . ? C34 C35 1.467(10) . ? C34 C43 1.503(11) . ? C35 C45 1.399(8) . ? C36 C27 1.379(9) 7_575 ? C37 C38 1.411(19) . ? C39 C40 1.518(15) . ? C41 C42 1.519(14) . ? C43 C44 1.512(14) . ? C45 C35 1.399(8) 7_575 ? 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 N5 Tm1 N5 74.8(3) . 7_575 ? N5 Tm1 N4 74.62(19) . . ? N5 Tm1 N4 118.7(2) 7_575 . ? N5 Tm1 N4 118.7(2) . 7_575 ? N5 Tm1 N4 74.62(19) 7_575 7_575 ? N4 Tm1 N4 75.7(3) . 7_575 ? N5 Tm1 N2 142.13(19) . 7_575 ? N5 Tm1 N2 79.1(2) 7_575 7_575 ? N4 Tm1 N2 142.97(19) . 7_575 ? N4 Tm1 N2 79.05(19) 7_575 7_575 ? N5 Tm1 N2 79.11(19) . . ? N5 Tm1 N2 142.13(19) 7_575 . ? N4 Tm1 N2 79.05(19) . . ? N4 Tm1 N2 142.97(19) 7_575 . ? N2 Tm1 N2 107.3(3) 7_575 . ? N5 Tm1 N3 79.2(2) . . ? N5 Tm1 N3 79.2(2) 7_575 . ? N4 Tm1 N3 141.99(14) . . ? N4 Tm1 N3 141.99(14) 7_575 . ? N2 Tm1 N3 69.24(17) 7_575 . ? N2 Tm1 N3 69.24(17) . . ? N5 Tm1 N1 142.38(14) . . ? N5 Tm1 N1 142.38(14) 7_575 . ? N4 Tm1 N1 78.8(2) . . ? N4 Tm1 N1 78.8(2) 7_575 . ? N2 Tm1 N1 69.98(17) 7_575 . ? N2 Tm1 N1 69.98(17) . . ? N3 Tm1 N1 108.0(3) . . ? C1 N1 C1 109.9(8) . 7_575 ? C1 N1 Tm1 123.3(4) . . ? C1 N1 Tm1 123.3(4) 7_575 . ? C19 N2 C8 106.9(6) . . ? C19 N2 Tm1 123.4(5) . . ? C8 N2 Tm1 124.0(4) . . ? C21 N3 C21 107.8(8) 7_575 . ? C21 N3 Tm1 123.3(4) 7_575 . ? C21 N3 Tm1 123.3(4) . . ? C32 N4 C35 106.3(6) . . ? C32 N4 Tm1 126.0(4) . . ? C35 N4 Tm1 126.4(5) . . ? C30 N5 C27 107.0(6) . . ? C30 N5 Tm1 124.5(4) . . ? C27 N5 Tm1 124.8(5) . . ? C7 C1 N1 129.0(7) . . ? C7 C1 C2 122.4(6) . . ? N1 C1 C2 108.5(6) . . ? C3 C2 C2 121.7(5) . 7_575 ? C3 C2 C1 131.8(7) . . ? C2 C2 C1 106.4(4) 7_575 . ? C2 C3 C4 118.6(8) . . ? C3 C4 C5 122.0(8) . . ? C3 C4 C4 119.6(5) . 7_575 ? C5 C4 C4 118.4(5) . 7_575 ? C6 C5 C4 120.7(9) . . ? C5 C6 C6 120.9(6) . 7_575 ? C1 C7 C8 123.9(6) . . ? C7 C8 N2 127.4(6) . . ? C7 C8 C9 122.0(6) . . ? N2 C8 C9 110.5(6) . . ? C10 C9 C18 121.2(7) . . ? C10 C9 C8 132.6(7) . . ? C18 C9 C8 106.1(6) . . ? C9 C10 C11 118.0(7) . . ? C10 C11 C16 121.1(7) . . ? C10 C11 C12 121.2(8) . . ? C16 C11 C12 117.7(8) . . ? C13 C12 C11 121.4(9) . . ? C12 C13 C14 119.6(9) . . ? C15 C14 C13 121.8(9) . . ? C14 C15 C16 121.0(10) . . ? C15 C16 C17 122.7(8) . . ? C15 C16 C11 118.6(8) . . ? C17 C16 C11 118.7(7) . . ? C18 C17 C16 119.2(8) . . ? C17 C18 C9 121.6(7) . . ? C17 C18 C19 133.0(7) . . ? C9 C18 C19 105.4(6) . . ? C20 C19 N2 127.3(7) . . ? C20 C19 C18 121.6(7) . . ? N2 C19 C18 110.9(6) . . ? C21 C20 C19 123.6(6) . . ? C20 C21 N3 127.8(7) . . ? C20 C21 C22 122.2(6) . . ? N3 C21 C22 109.7(7) . . ? C23 C22 C22 122.1(5) . 7_575 ? C23 C22 C21 131.5(7) . . ? C22 C22 C21 106.3(4) 7_575 . ? C22 C23 C24 117.1(8) . . ? C23 C24 C24 120.7(5) . 7_575 ? C23 C24 C25 120.7(9) . . ? C24 C24 C25 118.5(6) 7_575 . ? C26 C25 C24 119.6(11) . . ? C25 C26 C26 121.8(7) . 7_575 ? N5 C27 C36 126.4(7) . . ? N5 C27 C28 109.6(7) . . ? C36 C27 C28 123.9(7) . . ? C29 C28 C27 106.8(7) . . ? C29 C28 C37 126.3(8) . . ? C27 C28 C37 126.9(8) . . ? C28 C29 C30 105.5(7) . . ? C28 C29 C39 128.9(8) . . ? C30 C29 C39 125.5(8) . . ? N5 C30 C31 125.6(6) . . ? N5 C30 C29 110.9(6) . . ? C31 C30 C29 123.1(7) . . ? C30 C31 C32 126.7(7) . . ? N4 C32 C31 125.5(6) . . ? N4 C32 C33 110.4(6) . . ? C31 C32 C33 123.8(7) . . ? C34 C33 C32 106.5(6) . . ? C34 C33 C41 128.5(7) . . ? C32 C33 C41 124.6(7) . . ? C33 C34 C35 106.3(6) . . ? C33 C34 C43 128.1(7) . . ? C35 C34 C43 125.1(7) . . ? N4 C35 C45 126.1(7) . . ? N4 C35 C34 110.5(6) . . ? C45 C35 C34 123.1(7) . . ? C27 C36 C27 126.3(10) 7_575 . ? C38 C37 C28 113.4(11) . . ? C29 C39 C40 113.9(8) . . ? C33 C41 C42 114.0(8) . . ? C34 C43 C44 113.4(8) . . ? C35 C45 C35 126.0(9) 7_575 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.419 _refine_diff_density_min -1.318 _refine_diff_density_rms 0.147 data_020605a _database_code_CSD 194125 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H68 N12 Yb' _chemical_formula_weight 1418.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Yb Yb -0.3850 5.5486 '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' 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 28.739(6) _cell_length_b 26.832(5) _cell_length_c 10.866(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8379(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1986 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 15.446 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.125 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2904 _exptl_absorpt_coefficient_mu 1.162 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.6865 _exptl_absorpt_correction_T_max 0.9442 _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 '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 31602 _diffrn_reflns_av_R_equivalents 0.2362 _diffrn_reflns_av_sigmaI/netI 0.2538 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 23.40 _reflns_number_total 5449 _reflns_number_gt 2012 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0000P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5449 _refine_ls_number_parameters 445 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1665 _refine_ls_R_factor_gt 0.0422 _refine_ls_wR_factor_ref 0.0715 _refine_ls_wR_factor_gt 0.0440 _refine_ls_goodness_of_fit_ref 0.644 _refine_ls_restrained_S_all 0.644 _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 Yb1 Yb 0.030603(16) 0.2500 0.80222(5) 0.05096(17) Uani 1 2 d S . . N1 N 0.0248(2) 0.2500 0.5828(5) 0.0195(16) Uani 1 2 d S . . N2 N 0.0194(2) 0.1622(2) 0.5342(5) 0.0573(18) Uani 1 1 d . . . N3 N 0.0681(2) 0.1769(2) 0.7129(6) 0.0562(16) Uani 1 1 d . . . N4 N 0.1297(2) 0.1608(3) 0.8612(5) 0.0622(18) Uani 1 1 d . . . N5 N 0.1146(3) 0.2500 0.8456(6) 0.048(2) Uani 1 2 d S . . N6 N 0.0322(2) 0.1963(2) 0.9775(5) 0.0479(14) Uani 1 1 d . . . N7 N -0.0345(2) 0.19642(19) 0.7776(5) 0.0509(14) Uani 1 1 d . . . C1 C 0.0086(2) 0.2103(3) 0.5138(7) 0.047(2) Uani 1 1 d . . . C2 C -0.0163(2) 0.2237(2) 0.4013(8) 0.053(2) Uani 1 1 d . . . C3 C -0.0331(2) 0.1959(2) 0.3077(7) 0.0597(18) Uani 1 1 d . . . C4 C -0.0547(2) 0.22519(19) 0.2052(7) 0.0460(18) Uani 1 1 d . . . C5 C -0.0774(2) 0.1968(3) 0.1114(7) 0.059(2) Uani 1 1 d . . . C6 C -0.0994(3) 0.2226(3) 0.0141(8) 0.078(3) Uani 1 1 d . . . C7 C 0.0491(3) 0.1466(3) 0.6263(7) 0.056(2) Uani 1 1 d . . . C8 C 0.0639(2) 0.0957(3) 0.6325(7) 0.0475(19) Uani 1 1 d . . . C9 C 0.0543(3) 0.0542(3) 0.5669(7) 0.062(2) Uani 1 1 d . . . C10 C 0.0760(3) 0.0100(3) 0.6046(7) 0.054(2) Uani 1 1 d . . . C11 C 0.0654(3) -0.0360(3) 0.5408(8) 0.076(3) Uani 1 1 d . . . C12 C 0.0854(3) -0.0800(3) 0.5878(10) 0.088(3) Uani 1 1 d . . . C13 C 0.1170(3) -0.0816(3) 0.6863(10) 0.090(3) Uani 1 1 d . . . C14 C 0.1262(3) -0.0381(4) 0.7506(8) 0.089(3) Uani 1 1 d . . . C15 C 0.1059(3) 0.0084(3) 0.7066(10) 0.067(2) Uani 1 1 d . . . C16 C 0.1174(3) 0.0526(3) 0.7760(8) 0.073(2) Uani 1 1 d . . . C17 C 0.0941(3) 0.0966(3) 0.7369(7) 0.064(2) Uani 1 1 d . . . C18 C 0.0988(3) 0.1472(3) 0.7806(7) 0.048(2) Uani 1 1 d . . . C19 C 0.1372(2) 0.2099(3) 0.8856(6) 0.055(2) Uani 1 1 d . . . C20 C 0.1782(3) 0.2227(3) 0.9602(7) 0.072(3) Uani 1 1 d . . . C21 C 0.2125(3) 0.1965(3) 1.0181(7) 0.070(3) Uani 1 1 d . . . C22 C 0.2466(3) 0.2243(3) 1.0809(7) 0.072(3) Uani 1 1 d . . . C23 C 0.2834(3) 0.1974(3) 1.1437(8) 0.083(3) Uani 1 1 d . . . C24 C 0.3172(3) 0.2219(3) 1.2032(10) 0.117(4) Uani 1 1 d . . . C25 C 0.0706(4) 0.2500 1.1290(10) 0.069(3) Uani 1 2 d S . . C26 C 0.0585(2) 0.2033(3) 1.0812(8) 0.056(2) Uani 1 1 d . . . C27 C 0.0680(3) 0.1554(3) 1.1464(7) 0.074(3) Uani 1 1 d . . . C28 C 0.0480(3) 0.1209(3) 1.0740(9) 0.082(3) Uani 1 1 d . . . C29 C 0.0247(3) 0.1448(3) 0.9763(6) 0.048(2) Uani 1 1 d . . . C30 C -0.0054(2) 0.1230(3) 0.8927(7) 0.051(2) Uani 1 1 d . . . C31 C -0.0366(3) 0.1469(2) 0.8074(7) 0.0465(17) Uani 1 1 d . . . C32 C -0.0763(3) 0.1234(3) 0.7572(7) 0.062(2) Uani 1 1 d . . . C33 C -0.0975(2) 0.1575(3) 0.6905(7) 0.0508(19) Uani 1 1 d . . . C34 C -0.0735(2) 0.2036(3) 0.7077(8) 0.0500(19) Uani 1 1 d . . . C35 C -0.0877(3) 0.2500 0.6697(8) 0.047(3) Uani 1 2 d S . . C36 C 0.0937(4) 0.1496(4) 1.2654(10) 0.122(4) Uani 1 1 d . . . C37 C 0.1417(5) 0.1401(5) 1.2441(11) 0.205(6) Uani 1 1 d . . . C38 C 0.0457(3) 0.0642(3) 1.1009(8) 0.085(3) Uani 1 1 d . . . C39 C 0.0034(3) 0.0494(3) 1.1718(9) 0.120(4) Uani 1 1 d . . . C40 C -0.0912(3) 0.0683(3) 0.7759(7) 0.076(2) Uani 1 1 d . . . C41 C -0.1132(3) 0.0636(3) 0.8984(9) 0.098(3) Uani 1 1 d . . . C42 C -0.1450(3) 0.1524(3) 0.6221(7) 0.071(2) Uani 1 1 d . . . C43 C -0.1847(3) 0.1700(3) 0.7109(9) 0.100(3) 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 Yb1 0.0495(3) 0.0572(3) 0.0461(3) 0.000 -0.0021(3) 0.000 N1 0.021(4) 0.024(4) 0.013(4) 0.000 0.011(4) 0.000 N2 0.066(5) 0.057(5) 0.050(4) 0.004(3) -0.010(3) -0.008(4) N3 0.044(4) 0.075(5) 0.050(4) 0.019(4) -0.004(4) 0.006(3) N4 0.079(5) 0.056(5) 0.051(4) 0.004(4) -0.005(4) 0.001(4) N5 0.055(6) 0.042(6) 0.047(6) 0.000 -0.003(4) 0.000 N6 0.050(4) 0.062(5) 0.032(3) 0.006(3) -0.002(3) 0.010(4) N7 0.063(4) 0.051(4) 0.038(4) -0.004(3) 0.009(4) 0.003(4) C1 0.057(5) 0.031(5) 0.052(5) -0.004(4) -0.001(4) -0.023(4) C2 0.058(5) 0.041(5) 0.060(6) -0.015(4) 0.012(4) -0.008(4) C3 0.047(4) 0.111(6) 0.021(4) -0.006(5) 0.007(5) -0.012(5) C4 0.055(4) 0.052(5) 0.032(4) -0.004(4) 0.017(4) 0.000(3) C5 0.026(4) 0.105(7) 0.047(5) -0.033(5) 0.008(4) -0.005(4) C6 0.043(5) 0.108(8) 0.084(7) -0.012(5) 0.003(5) 0.001(5) C7 0.068(6) 0.053(6) 0.046(5) 0.008(4) -0.021(4) 0.001(5) C8 0.041(5) 0.057(6) 0.045(5) -0.008(4) 0.003(4) 0.003(4) C9 0.068(6) 0.049(6) 0.069(6) -0.008(5) 0.010(5) -0.013(5) C10 0.054(6) 0.058(6) 0.050(5) -0.004(5) 0.006(4) -0.014(5) C11 0.075(6) 0.057(6) 0.095(7) 0.000(6) 0.023(5) 0.002(5) C12 0.088(7) 0.063(7) 0.114(9) 0.017(6) 0.024(6) 0.004(6) C13 0.093(7) 0.083(7) 0.095(8) -0.004(7) -0.004(7) -0.006(6) C14 0.109(7) 0.067(7) 0.091(8) 0.007(5) 0.023(6) 0.012(6) C15 0.061(5) 0.042(5) 0.098(7) -0.004(6) 0.003(6) -0.011(4) C16 0.080(6) 0.051(6) 0.090(7) 0.000(5) -0.011(5) 0.000(5) C17 0.066(6) 0.056(6) 0.071(6) -0.007(5) 0.006(5) 0.012(5) C18 0.046(5) 0.053(6) 0.046(6) -0.005(4) -0.004(4) -0.004(4) C19 0.036(5) 0.081(7) 0.048(5) 0.001(5) -0.021(4) 0.013(5) C20 0.060(5) 0.093(7) 0.063(5) 0.021(4) -0.010(5) -0.008(5) C21 0.044(5) 0.117(8) 0.049(5) 0.004(5) -0.020(4) 0.013(5) C22 0.062(5) 0.082(7) 0.073(6) -0.023(4) -0.036(5) 0.015(4) C23 0.048(5) 0.125(8) 0.076(7) 0.009(5) -0.017(5) 0.013(6) C24 0.105(7) 0.156(10) 0.092(7) 0.004(6) -0.048(7) -0.007(6) C25 0.067(8) 0.063(9) 0.077(9) 0.000 0.020(7) 0.000 C26 0.036(5) 0.071(6) 0.060(6) 0.023(5) -0.004(4) -0.004(5) C27 0.115(7) 0.056(6) 0.051(6) 0.004(5) -0.028(5) -0.006(6) C28 0.090(7) 0.063(7) 0.094(8) 0.013(6) -0.020(6) 0.008(6) C29 0.054(5) 0.058(6) 0.031(5) 0.011(4) -0.003(4) 0.010(5) C30 0.056(5) 0.052(5) 0.044(5) 0.002(4) -0.003(4) 0.012(4) C31 0.067(5) 0.029(4) 0.044(4) 0.000(4) 0.003(5) 0.004(4) C32 0.073(6) 0.062(6) 0.053(6) 0.000(4) 0.009(4) -0.020(5) C33 0.050(5) 0.054(5) 0.048(5) -0.016(5) -0.015(5) -0.001(4) C34 0.024(4) 0.063(6) 0.063(5) -0.002(5) -0.008(4) 0.013(4) C35 0.044(6) 0.081(9) 0.015(6) 0.000 -0.010(5) 0.000 C36 0.102(8) 0.147(9) 0.118(10) -0.003(7) -0.043(7) 0.030(7) C37 0.106(9) 0.376(19) 0.134(12) -0.005(11) -0.024(8) 0.064(11) C38 0.094(7) 0.057(6) 0.105(7) 0.024(5) -0.020(6) -0.004(5) C39 0.119(7) 0.102(8) 0.138(10) 0.050(7) 0.015(8) -0.010(6) C40 0.088(6) 0.070(6) 0.068(7) 0.002(5) 0.001(5) -0.036(5) C41 0.099(7) 0.076(7) 0.119(8) 0.021(6) 0.014(6) -0.005(6) C42 0.065(6) 0.067(6) 0.082(6) 0.002(5) -0.027(5) -0.003(5) C43 0.060(5) 0.146(8) 0.095(7) -0.021(7) -0.035(6) 0.028(5) _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 Yb1 N7 2.375(6) . ? Yb1 N7 2.375(6) 7_565 ? Yb1 N6 2.389(5) 7_565 ? Yb1 N6 2.389(5) . ? Yb1 N1 2.390(6) . ? Yb1 N3 2.440(6) 7_565 ? Yb1 N3 2.440(6) . ? Yb1 N5 2.458(8) . ? N1 C1 1.383(7) . ? N1 C1 1.383(7) 7_565 ? N2 C1 1.346(8) . ? N2 C7 1.380(8) . ? N3 C7 1.358(8) . ? N3 C18 1.398(8) . ? N4 C18 1.300(8) . ? N4 C19 1.361(8) . ? N5 C19 1.332(8) 7_565 ? N5 C19 1.332(8) . ? N6 C26 1.370(8) . ? N6 C29 1.399(8) . ? N7 C34 1.367(8) . ? N7 C31 1.370(6) . ? C1 C2 1.461(10) . ? C2 C3 1.351(8) . ? C2 C2 1.411(11) 7_565 ? C3 C4 1.496(9) . ? C4 C4 1.331(10) 7_565 ? C4 C5 1.431(8) . ? C5 C6 1.413(10) . ? C6 C6 1.472(15) 7_565 ? C7 C8 1.433(9) . ? C8 C9 1.350(9) . ? C8 C17 1.428(8) . ? C9 C10 1.402(9) . ? C10 C15 1.402(10) . ? C10 C11 1.448(10) . ? C11 C12 1.410(10) . ? C12 C13 1.405(11) . ? C13 C14 1.387(10) . ? C14 C15 1.457(9) . ? C15 C16 1.442(9) . ? C16 C17 1.424(9) . ? C17 C18 1.444(8) . ? C19 C20 1.471(10) . ? C20 C21 1.365(9) . ? C20 C20 1.463(14) 7_565 ? C21 C22 1.406(9) . ? C22 C22 1.381(14) 7_565 ? C22 C23 1.451(9) . ? C23 C24 1.341(10) . ? C24 C24 1.509(16) 7_565 ? C25 C26 1.400(9) . ? C25 C26 1.400(9) 7_565 ? C26 C27 1.493(9) . ? C27 C28 1.343(10) . ? C27 C36 1.496(11) . ? C28 C29 1.410(9) . ? C28 C38 1.551(10) . ? C29 C30 1.384(9) . ? C30 C31 1.440(9) . ? C31 C32 1.412(9) . ? C32 C33 1.318(8) . ? C32 C40 1.553(9) . ? C33 C34 1.427(8) . ? C33 C42 1.559(9) . ? C34 C35 1.375(7) . ? C35 C34 1.375(7) 7_565 ? C36 C37 1.422(12) . ? C38 C39 1.493(10) . ? C40 C41 1.478(10) . ? C42 C43 1.567(11) . ? 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 N7 Yb1 N7 74.5(3) . 7_565 ? N7 Yb1 N6 118.08(18) . 7_565 ? N7 Yb1 N6 74.9(2) 7_565 7_565 ? N7 Yb1 N6 74.9(2) . . ? N7 Yb1 N6 118.08(18) 7_565 . ? N6 Yb1 N6 74.2(3) 7_565 . ? N7 Yb1 N1 80.36(17) . . ? N7 Yb1 N1 80.36(17) 7_565 . ? N6 Yb1 N1 142.80(14) 7_565 . ? N6 Yb1 N1 142.80(14) . . ? N7 Yb1 N3 142.2(2) . 7_565 ? N7 Yb1 N3 79.44(19) 7_565 7_565 ? N6 Yb1 N3 79.8(2) 7_565 7_565 ? N6 Yb1 N3 142.5(2) . 7_565 ? N1 Yb1 N3 68.53(17) . 7_565 ? N7 Yb1 N3 79.44(19) . . ? N7 Yb1 N3 142.2(2) 7_565 . ? N6 Yb1 N3 142.5(2) 7_565 . ? N6 Yb1 N3 79.8(2) . . ? N1 Yb1 N3 68.53(17) . . ? N3 Yb1 N3 107.0(3) 7_565 . ? N7 Yb1 N5 142.64(14) . . ? N7 Yb1 N5 142.64(14) 7_565 . ? N6 Yb1 N5 80.1(2) 7_565 . ? N6 Yb1 N5 80.1(2) . . ? N1 Yb1 N5 105.1(2) . . ? N3 Yb1 N5 69.04(17) 7_565 . ? N3 Yb1 N5 69.04(17) . . ? C1 N1 C1 100.7(8) . 7_565 ? C1 N1 Yb1 124.4(4) . . ? C1 N1 Yb1 124.4(4) 7_565 . ? C1 N2 C7 123.6(7) . . ? C7 N3 C18 106.1(6) . . ? C7 N3 Yb1 125.4(5) . . ? C18 N3 Yb1 121.8(5) . . ? C18 N4 C19 120.7(7) . . ? C19 N5 C19 107.9(9) 7_565 . ? C19 N5 Yb1 122.9(5) 7_565 . ? C19 N5 Yb1 122.9(5) . . ? C26 N6 C29 103.3(6) . . ? C26 N6 Yb1 125.7(5) . . ? C29 N6 Yb1 125.9(4) . . ? C34 N7 C31 103.3(6) . . ? C34 N7 Yb1 128.6(5) . . ? C31 N7 Yb1 126.6(5) . . ? N2 C1 N1 124.9(7) . . ? N2 C1 C2 119.2(6) . . ? N1 C1 C2 115.4(6) . . ? C3 C2 C2 123.5(4) . 7_565 ? C3 C2 C1 132.0(6) . . ? C2 C2 C1 104.3(4) 7_565 . ? C2 C3 C4 114.8(6) . . ? C4 C4 C5 122.2(4) 7_565 . ? C4 C4 C3 121.6(3) 7_565 . ? C5 C4 C3 116.1(6) . . ? C6 C5 C4 118.4(7) . . ? C5 C6 C6 119.3(4) . 7_565 ? N3 C7 N2 124.7(7) . . ? N3 C7 C8 114.8(7) . . ? N2 C7 C8 120.4(7) . . ? C9 C8 C17 123.9(8) . . ? C9 C8 C7 134.5(8) . . ? C17 C8 C7 101.5(7) . . ? C8 C9 C10 116.9(8) . . ? C9 C10 C15 122.0(8) . . ? C9 C10 C11 119.1(8) . . ? C15 C10 C11 118.8(8) . . ? C12 C11 C10 117.0(8) . . ? C13 C12 C11 124.5(9) . . ? C14 C13 C12 118.7(9) . . ? C13 C14 C15 118.7(9) . . ? C10 C15 C16 121.9(8) . . ? C10 C15 C14 122.0(8) . . ? C16 C15 C14 116.1(9) . . ? C17 C16 C15 114.7(8) . . ? C16 C17 C8 120.5(8) . . ? C16 C17 C18 129.6(8) . . ? C8 C17 C18 109.6(7) . . ? N4 C18 N3 128.8(7) . . ? N4 C18 C17 123.3(8) . . ? N3 C18 C17 107.6(7) . . ? N5 C19 N4 129.9(7) . . ? N5 C19 C20 112.5(8) . . ? N4 C19 C20 117.5(7) . . ? C21 C20 C20 121.0(5) . 7_565 ? C21 C20 C19 135.4(8) . . ? C20 C20 C19 103.6(5) 7_565 . ? C20 C21 C22 117.0(8) . . ? C22 C22 C21 121.9(5) 7_565 . ? C22 C22 C23 119.9(5) 7_565 . ? C21 C22 C23 118.2(7) . . ? C24 C23 C22 120.7(9) . . ? C23 C24 C24 119.4(5) . 7_565 ? C26 C25 C26 127.0(11) . 7_565 ? N6 C26 C25 124.5(8) . . ? N6 C26 C27 111.8(7) . . ? C25 C26 C27 123.3(8) . . ? C28 C27 C26 103.8(8) . . ? C28 C27 C36 130.2(9) . . ? C26 C27 C36 126.0(8) . . ? C27 C28 C29 109.3(8) . . ? C27 C28 C38 125.8(8) . . ? C29 C28 C38 124.5(8) . . ? C30 C29 N6 121.4(7) . . ? C30 C29 C28 126.9(8) . . ? N6 C29 C28 111.6(7) . . ? C29 C30 C31 128.5(7) . . ? N7 C31 C32 112.2(7) . . ? N7 C31 C30 123.8(7) . . ? C32 C31 C30 123.5(7) . . ? C33 C32 C31 106.0(7) . . ? C33 C32 C40 127.2(8) . . ? C31 C32 C40 126.7(8) . . ? C32 C33 C34 107.8(7) . . ? C32 C33 C42 127.3(7) . . ? C34 C33 C42 124.2(7) . . ? N7 C34 C35 122.5(8) . . ? N7 C34 C33 110.4(6) . . ? C35 C34 C33 126.9(7) . . ? C34 C35 C34 130.0(9) 7_565 . ? C37 C36 C27 110.9(10) . . ? C39 C38 C28 113.2(7) . . ? C41 C40 C32 108.4(6) . . ? C33 C42 C43 108.5(6) . . ? _diffrn_measured_fraction_theta_max 0.868 _diffrn_reflns_theta_full 23.40 _diffrn_measured_fraction_theta_full 0.868 _refine_diff_density_max 0.981 _refine_diff_density_min -0.345 _refine_diff_density_rms 0.053