# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_1 _database_code_depnum_ccdc_archive 'CCDC 912202' #TrackingRef '17648_web_deposit_cif_file_0_Hui-ZhongKou_1360546996.kou-rev.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C99 H133 Cl2 Dy4 N32 O38' _chemical_formula_weight 3100.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 49.845(10) _cell_length_b 22.258(5) _cell_length_c 34.838(7) _cell_angle_alpha 90.00 _cell_angle_beta 132.56(3) _cell_angle_gamma 90.00 _cell_volume 28469(10) _cell_formula_units_Z 8 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 46144 _cell_measurement_theta_min 2.1401 _cell_measurement_theta_max 29.1270 _exptl_crystal_description chip _exptl_crystal_colour orange _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.447 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 12424 _exptl_absorpt_coefficient_mu 2.193 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.7042 _exptl_absorpt_process_details 'Higashi, T. (1995)' _exptl_special_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_measurement_device_type 'Saturn724+ (2x2 bin mode)' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_decay_% ? _diffrn_reflns_number 135376 _diffrn_reflns_av_R_equivalents 0.0608 _diffrn_reflns_av_sigmaI/netI 0.0533 _diffrn_reflns_limit_h_min -61 _diffrn_reflns_limit_h_max 61 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 26.00 _reflns_number_total 27912 _reflns_number_gt 23042 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1990)' _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The DMF solvent molecules are not stable and show high temperature factors, and the occupancies of the atoms have been set as half of the original values. Some DMF molecules undergo site disorder,and therefore, constraints of planarity and bond distances have been used. The formula of the complex was confirmed by the micro-elementary analyses. Due to the weak diffraction of the crystal, the methanol solvents and the azide anions cannot be completely found from the difference Fourier map. The SQUEEZE function of PLATON was applied, giving available voids of 3322.6 \%A^3^. The corresponding residual electron counts were 2134 e- per unit cell, which should correspond to the missing solvent molecules and the azides. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0750P)^2^+689.8146P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 27912 _refine_ls_number_parameters 1582 _refine_ls_number_restraints 40 _refine_ls_R_factor_all 0.1033 _refine_ls_R_factor_gt 0.0866 _refine_ls_wR_factor_ref 0.2130 _refine_ls_wR_factor_gt 0.2025 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.008 _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 0.558854(11) 0.84633(2) 0.173313(16) 0.03511(12) Uani 1 1 d . . . Dy2 Dy 0.878823(11) 0.84701(2) 0.293447(17) 0.03689(12) Uani 1 1 d . . . Dy3 Dy 0.798437(11) 0.86542(2) 0.461376(18) 0.04037(13) Uani 1 1 d . . . Dy4 Dy 0.639995(11) 0.87440(2) 0.007040(17) 0.03659(12) Uani 1 1 d . . . Cl1 Cl 0.63810(15) 1.0958(2) 0.2624(2) 0.1197(17) Uani 1 1 d . . . Cl2 Cl 0.6965(2) 1.1242(4) 0.1141(3) 0.180(3) Uani 1 1 d . . . C1 C 0.7686(3) 0.9225(5) 0.1345(4) 0.053(3) Uani 1 1 d . . . H1A H 0.7462 0.9391 0.1035 0.080 Uiso 1 1 calc R . . H1B H 0.7863 0.9225 0.1314 0.080 Uiso 1 1 calc R . . H1C H 0.7774 0.9463 0.1640 0.080 Uiso 1 1 calc R . . C2 C 0.7621(3) 0.8570(5) 0.1420(4) 0.048(3) Uani 1 1 d . . . C3 C 0.7917(2) 0.8251(5) 0.1854(4) 0.044(2) Uani 1 1 d . . . C4 C 0.7857(3) 0.7657(5) 0.1940(4) 0.051(3) Uani 1 1 d . . . C5 C 0.7509(3) 0.7417(6) 0.1593(5) 0.068(4) Uani 1 1 d . . . H5A H 0.7471 0.7034 0.1655 0.082 Uiso 1 1 calc R . . C6 C 0.7215(3) 0.7728(5) 0.1154(4) 0.060(3) Uani 1 1 d . . . C7 C 0.7270(2) 0.8331(5) 0.1076(4) 0.045(3) Uani 1 1 d . . . C8 C 0.6863(3) 0.7433(5) 0.0798(4) 0.056(3) Uani 1 1 d . . . H8A H 0.6854 0.7037 0.0874 0.067 Uiso 1 1 calc R . . C9 C 0.5947(3) 0.7504(5) -0.0303(4) 0.043(2) Uani 1 1 d . . . C10 C 0.5618(3) 0.7105(5) -0.0592(4) 0.044(2) Uani 1 1 d . . . C11 C 0.5636(3) 0.6485(6) -0.0599(5) 0.075(4) Uani 1 1 d . . . H11A H 0.5857 0.6287 -0.0419 0.090 Uiso 1 1 calc R . . C12 C 0.5301(3) 0.6163(6) -0.0896(6) 0.075(4) Uani 1 1 d . . . H12A H 0.5306 0.5746 -0.0905 0.090 Uiso 1 1 calc R . . C13 C 0.4977(3) 0.7022(6) -0.1132(5) 0.063(3) Uani 1 1 d . . . H13A H 0.4756 0.7206 -0.1292 0.076 Uiso 1 1 calc R . . C14 C 0.5283(3) 0.7381(6) -0.0875(4) 0.054(3) Uani 1 1 d . . . H14A H 0.5264 0.7798 -0.0892 0.065 Uiso 1 1 calc R . . C15 C 0.8136(3) 0.7308(5) 0.2396(4) 0.053(3) Uani 1 1 d . . . H15A H 0.8073 0.6930 0.2426 0.064 Uiso 1 1 calc R . . C16 C 0.9033(3) 0.7242(5) 0.3586(4) 0.043(2) Uani 1 1 d . . . C17 C 0.9252(3) 0.6863(4) 0.4074(4) 0.042(2) Uani 1 1 d . . . C18 C 0.9103(3) 0.6473(6) 0.4191(5) 0.063(3) Uani 1 1 d . . . H18A H 0.8853 0.6409 0.3954 0.076 Uiso 1 1 calc R . . C19 C 0.9325(3) 0.6179(6) 0.4658(5) 0.067(4) Uani 1 1 d . . . H19A H 0.9219 0.5910 0.4726 0.080 Uiso 1 1 calc R . . C20 C 0.9827(3) 0.6630(5) 0.4916(4) 0.054(3) Uani 1 1 d . . . H20A H 1.0078 0.6690 0.5163 0.065 Uiso 1 1 calc R . . C21 C 0.9623(3) 0.6947(5) 0.4448(4) 0.048(3) Uani 1 1 d . . . H21A H 0.9736 0.7213 0.4390 0.058 Uiso 1 1 calc R . . C22 C 0.6703(3) 0.9172(5) 0.3344(4) 0.053(3) Uani 1 1 d . . . H22A H 0.6451 0.9281 0.3072 0.080 Uiso 1 1 calc R . . H22B H 0.6851 0.9437 0.3336 0.080 Uiso 1 1 calc R . . H22C H 0.6772 0.9203 0.3676 0.080 Uiso 1 1 calc R . . C23 C 0.6756(2) 0.8543(5) 0.3262(4) 0.040(2) Uani 1 1 d . . . C24 C 0.7110(2) 0.8288(4) 0.3611(4) 0.038(2) Uani 1 1 d . . . C25 C 0.7159(2) 0.7689(5) 0.3513(4) 0.039(2) Uani 1 1 d . . . C26 C 0.6865(3) 0.7379(5) 0.3084(4) 0.041(2) Uani 1 1 d . . . H26A H 0.6901 0.6991 0.3029 0.049 Uiso 1 1 calc R . . C27 C 0.6511(2) 0.7626(5) 0.2724(4) 0.041(2) Uani 1 1 d . . . C28 C 0.6459(3) 0.8226(5) 0.2838(4) 0.041(2) Uani 1 1 d . . . C29 C 0.6229(3) 0.7297(5) 0.2265(4) 0.044(2) Uani 1 1 d . . . H29A H 0.6289 0.6917 0.2232 0.053 Uiso 1 1 calc R . . C30 C 0.5346(3) 0.7257(5) 0.1063(4) 0.040(2) Uani 1 1 d . . . C31 C 0.5124(3) 0.6890(5) 0.0567(4) 0.044(2) Uani 1 1 d . . . C32 C 0.5288(3) 0.6580(5) 0.0427(4) 0.048(3) Uani 1 1 d . . . H32A H 0.5540 0.6557 0.0650 0.058 Uiso 1 1 calc R . . C33 C 0.5061(3) 0.6302(6) -0.0060(4) 0.059(3) Uani 1 1 d . . . H33A H 0.5168 0.6098 -0.0160 0.071 Uiso 1 1 calc R . . C34 C 0.4549(3) 0.6612(5) -0.0240(4) 0.056(3) Uani 1 1 d . . . H34A H 0.4297 0.6624 -0.0464 0.067 Uiso 1 1 calc R . . C35 C 0.4751(3) 0.6903(5) 0.0231(4) 0.052(3) Uani 1 1 d . . . H35A H 0.4637 0.7105 0.0320 0.063 Uiso 1 1 calc R . . C36 C 0.7508(2) 0.7380(4) 0.3844(4) 0.037(2) Uani 1 1 d . . . H36A H 0.7512 0.6991 0.3750 0.044 Uiso 1 1 calc R . . C37 C 0.8423(2) 0.7416(5) 0.4938(4) 0.039(2) Uani 1 1 d . . . C38 C 0.8751(2) 0.7014(5) 0.5209(4) 0.040(2) Uani 1 1 d . . . C39 C 0.8734(3) 0.6406(5) 0.5186(4) 0.047(3) Uani 1 1 d . . . H39A H 0.8510 0.6215 0.4989 0.057 Uiso 1 1 calc R . . C40 C 0.9051(3) 0.6063(6) 0.5454(4) 0.055(3) Uani 1 1 d . . . H40A H 0.9032 0.5647 0.5424 0.066 Uiso 1 1 calc R . . C41 C 0.9394(3) 0.6930(6) 0.5763(5) 0.067(4) Uani 1 1 d . . . H41A H 0.9620 0.7113 0.5948 0.080 Uiso 1 1 calc R . . C42 C 0.9089(3) 0.7292(6) 0.5509(5) 0.059(3) Uani 1 1 d . . . H42A H 0.9110 0.7708 0.5539 0.071 Uiso 1 1 calc R . . C43 C 0.8531(3) 0.7873(5) 0.3992(4) 0.046(2) Uani 1 1 d . . . H43A H 0.8655 0.7723 0.3889 0.069 Uiso 1 1 calc R . . H43B H 0.8320 0.7630 0.3837 0.069 Uiso 1 1 calc R . . H43C H 0.8691 0.7855 0.4365 0.069 Uiso 1 1 calc R . . C44 C 0.8416(3) 0.8514(4) 0.3813(4) 0.039(2) Uani 1 1 d . . . C45 C 0.8226(3) 0.8823(4) 0.3920(4) 0.042(2) Uani 1 1 d . . . C46 C 0.8107(3) 0.9426(5) 0.3743(4) 0.042(2) Uani 1 1 d . . . C47 C 0.8178(3) 0.9697(5) 0.3451(4) 0.044(2) Uani 1 1 d . . . H47A H 0.8097 1.0087 0.3329 0.053 Uiso 1 1 calc R . . C48 C 0.8361(2) 0.9403(4) 0.3342(4) 0.037(2) Uani 1 1 d . . . C49 C 0.8494(2) 0.8798(4) 0.3533(4) 0.036(2) Uani 1 1 d . . . C50 C 0.8402(2) 0.9712(5) 0.3023(4) 0.042(2) Uani 1 1 d . . . H50A H 0.8310 1.0100 0.2920 0.050 Uiso 1 1 calc R . . C51 C 0.8683(3) 0.9693(6) 0.2343(4) 0.058(3) Uani 1 1 d . . . C52 C 0.8619(4) 1.0108(7) 0.1950(5) 0.100(6) Uani 1 1 d D . . C53 C 0.8573(5) 1.0716(8) 0.1935(7) 0.226(18) Uani 1 1 d D . . H53A H 0.8579 1.0906 0.2178 0.271 Uiso 1 1 calc R . . C54 C 0.8518(7) 1.1039(9) 0.1550(9) 0.33(3) Uani 1 1 d D . . H54A H 0.8496 1.1454 0.1540 0.399 Uiso 1 1 calc R . . C55 C 0.8563(11) 1.0164(12) 0.1223(11) 0.31(3) Uani 1 1 d D . . H55A H 0.8583 0.9980 0.1004 0.372 Uiso 1 1 calc R . . C56 C 0.8599(7) 0.9842(8) 0.1587(7) 0.188(14) Uani 1 1 d D . . H56A H 0.8610 0.9425 0.1583 0.225 Uiso 1 1 calc R . . C57 C 0.7913(3) 0.9776(4) 0.3837(4) 0.046(3) Uani 1 1 d . . . H57A H 0.7838 1.0159 0.3692 0.055 Uiso 1 1 calc R . . C58 C 0.7625(3) 0.9942(5) 0.4491(5) 0.051(3) Uani 1 1 d . . . C59 C 0.7395(3) 1.0379(5) 0.4491(5) 0.053(3) Uani 1 1 d . . . C60 C 0.7088(4) 1.0634(7) 0.4038(5) 0.075(4) Uani 1 1 d . . . H60A H 0.7020 1.0549 0.3720 0.090 Uiso 1 1 calc R . . C61 C 0.6883(4) 1.1019(7) 0.4062(6) 0.081(5) Uani 1 1 d . . . H61A H 0.6676 1.1191 0.3754 0.097 Uiso 1 1 calc R . . C62 C 0.7256(3) 1.0891(6) 0.4940(5) 0.063(3) Uani 1 1 d . . . H62A H 0.7316 1.0970 0.5253 0.075 Uiso 1 1 calc R . . C63 C 0.7476(3) 1.0493(6) 0.4948(5) 0.059(3) Uani 1 1 d . . . H63A H 0.7674 1.0309 0.5257 0.071 Uiso 1 1 calc R . . C64 C 0.5823(3) 0.7959(5) 0.0634(4) 0.048(3) Uani 1 1 d . . . H64A H 0.5699 0.7796 0.0732 0.072 Uiso 1 1 calc R . . H64B H 0.6019 0.7697 0.0753 0.072 Uiso 1 1 calc R . . H64C H 0.5656 0.7995 0.0262 0.072 Uiso 1 1 calc R . . C65 C 0.5974(2) 0.8574(4) 0.0880(3) 0.034(2) Uani 1 1 d . . . C66 C 0.6170(2) 0.8882(4) 0.0783(3) 0.0316(19) Uani 1 1 d . . . C67 C 0.6316(2) 0.9470(4) 0.1011(4) 0.037(2) Uani 1 1 d . . . C68 C 0.6267(2) 0.9710(4) 0.1321(4) 0.039(2) Uani 1 1 d . . . H68A H 0.6365 1.0086 0.1469 0.047 Uiso 1 1 calc R . . C69 C 0.6075(3) 0.9406(4) 0.1421(4) 0.038(2) Uani 1 1 d . . . C70 C 0.5914(2) 0.8839(4) 0.1178(3) 0.034(2) Uani 1 1 d . . . C71 C 0.6039(2) 0.9693(5) 0.1754(4) 0.041(2) Uani 1 1 d . . . H71A H 0.6154 1.0062 0.1895 0.050 Uiso 1 1 calc R . . C72 C 0.5693(3) 0.9622(6) 0.2354(4) 0.053(3) Uani 1 1 d . . . C73 C 0.5735(3) 0.9917(8) 0.2773(5) 0.082(5) Uani 1 1 d . . . C74 C 0.5973(5) 1.0275(10) 0.3120(8) 0.122(8) Uani 1 1 d . . . H74A H 0.6151 1.0388 0.3117 0.147 Uiso 1 1 calc R . . C75 C 0.5998(5) 1.0523(12) 0.3514(8) 0.150(11) Uani 1 1 d . . . H75A H 0.6147 1.0852 0.3706 0.180 Uiso 1 1 calc R . . C76 C 0.5543(5) 0.9876(11) 0.3269(7) 0.134(9) Uani 1 1 d . . . H76A H 0.5391 0.9735 0.3316 0.160 Uiso 1 1 calc R . . C77 C 0.5509(5) 0.9685(10) 0.2857(7) 0.117(7) Uani 1 1 d . . . H77A H 0.5334 0.9397 0.2629 0.140 Uiso 1 1 calc R . . C78 C 0.6507(2) 0.9826(4) 0.0910(4) 0.040(2) Uani 1 1 d . . . H78A H 0.6602 1.0192 0.1083 0.048 Uiso 1 1 calc R . . C79 C 0.6771(2) 1.0004(5) 0.0224(4) 0.043(2) Uani 1 1 d . . . C80 C 0.6999(3) 1.0432(5) 0.0213(4) 0.043(2) Uani 1 1 d . . . C81 C 0.7314(3) 1.0672(5) 0.0662(5) 0.047(3) Uani 1 1 d . . . H81A H 0.7385 1.0587 0.0981 0.057 Uiso 1 1 calc R . . C82 C 0.7524(3) 1.1040(5) 0.0639(5) 0.057(3) Uani 1 1 d . . . H82A H 0.7741 1.1190 0.0948 0.069 Uiso 1 1 calc R . . C83 C 0.7129(4) 1.0952(6) -0.0237(5) 0.061(3) Uani 1 1 d . . . H83A H 0.7065 1.1045 -0.0550 0.073 Uiso 1 1 calc R . . C84 C 0.6903(3) 1.0571(5) -0.0251(5) 0.054(3) Uani 1 1 d . . . H84A H 0.6693 1.0414 -0.0564 0.065 Uiso 1 1 calc R . . C85 C 0.7285(4) 0.9997(7) 0.2273(6) 0.079(4) Uani 1 1 d . . . H85A H 0.7371 1.0140 0.2122 0.095 Uiso 1 1 calc R . . C86 C 0.7391(6) 0.8988(8) 0.2122(9) 0.120(7) Uani 1 1 d . . . H86A H 0.7461 0.9214 0.1967 0.181 Uiso 1 1 calc R . . H86B H 0.7195 0.8722 0.1868 0.181 Uiso 1 1 calc R . . H86C H 0.7596 0.8758 0.2409 0.181 Uiso 1 1 calc R . . C87 C 0.7140(5) 0.9139(8) 0.2546(7) 0.107(6) Uani 1 1 d . . . H87A H 0.7061 0.9456 0.2638 0.161 Uiso 1 1 calc R . . H87B H 0.7332 0.8917 0.2853 0.161 Uiso 1 1 calc R . . H87C H 0.6939 0.8875 0.2300 0.161 Uiso 1 1 calc R . . C88 C 0.7382(5) 0.7331(8) 0.2569(7) 0.098(5) Uani 1 1 d . . . H88A H 0.7583 0.7055 0.2758 0.147 Uiso 1 1 calc R . . H88B H 0.7336 0.7452 0.2785 0.147 Uiso 1 1 calc R . . H88C H 0.7440 0.7678 0.2474 0.147 Uiso 1 1 calc R . . C89 C 0.6738(5) 0.7421(9) 0.1790(9) 0.126(8) Uani 1 1 d . . . H89A H 0.6539 0.7205 0.1484 0.189 Uiso 1 1 calc R . . H89B H 0.6786 0.7777 0.1688 0.189 Uiso 1 1 calc R . . H89C H 0.6678 0.7532 0.1989 0.189 Uiso 1 1 calc R . . C90 C 0.7073(9) 0.6469(9) 0.2000(9) 0.195(15) Uani 1 1 d . . . H90A H 0.7294 0.6264 0.2211 0.234 Uiso 1 1 calc R . . C91 C 0.4735(4) 0.5328(7) 0.0455(6) 0.169(12) Uani 1 1 d D . . H91 H 0.4795 0.5503 0.0748 0.202 Uiso 1 1 calc R . . C92 C 0.4233(5) 0.4970(9) -0.0525(6) 0.116(7) Uani 1 1 d . . . H92A H 0.3972 0.4986 -0.0781 0.174 Uiso 1 1 calc R . . H92B H 0.4311 0.4559 -0.0466 0.174 Uiso 1 1 calc R . . H92C H 0.4328 0.5192 -0.0647 0.174 Uiso 1 1 calc R . . C93 C 0.4122(5) 0.5461(12) -0.0002(8) 0.152(10) Uani 1 1 d . . . H93A H 0.3879 0.5400 -0.0332 0.227 Uiso 1 1 calc R . . H93B H 0.4164 0.5882 0.0078 0.227 Uiso 1 1 calc R . . H93C H 0.4150 0.5252 0.0265 0.227 Uiso 1 1 calc R . . C94 C 0.9897(6) 0.593(2) 0.3870(12) 0.25(2) Uani 1 1 d D . . H94 H 0.9658 0.6050 0.3596 0.305 Uiso 1 1 calc R . . C95 C 1.0380(4) 0.5473(10) 0.4744(7) 0.123(7) Uani 1 1 d . . . H95A H 1.0531 0.5675 0.4705 0.185 Uiso 1 1 calc R . . H95B H 1.0423 0.5048 0.4771 0.185 Uiso 1 1 calc R . . H95C H 1.0439 0.5614 0.5054 0.185 Uiso 1 1 calc R . . C96 C 0.9736(6) 0.5320(13) 0.4251(12) 0.220(18) Uani 1 1 d . . . H96A H 0.9504 0.5446 0.3926 0.330 Uiso 1 1 calc R . . H96B H 0.9754 0.5437 0.4533 0.330 Uiso 1 1 calc R . . H96C H 0.9756 0.4892 0.4251 0.330 Uiso 1 1 calc R . . N1 N 0.8470(2) 0.7485(4) 0.2769(3) 0.043(2) Uani 1 1 d . . . N2 N 0.8680(2) 0.7092(4) 0.3201(3) 0.0416(19) Uani 1 1 d . . . H2A H 0.8588 0.6777 0.3218 0.050 Uiso 1 1 calc R . . N3 N 0.9687(2) 0.6255(5) 0.5025(4) 0.058(3) Uani 1 1 d . . . N4 N 0.6562(2) 0.7664(4) 0.0388(3) 0.045(2) Uani 1 1 d . . . N5 N 0.6261(2) 0.7274(4) 0.0126(3) 0.054(2) Uani 1 1 d . . . H5B H 0.6278 0.6916 0.0233 0.064 Uiso 1 1 calc R . . N6 N 0.4983(3) 0.6438(5) -0.1160(4) 0.070(3) Uani 1 1 d . . . N7 N 0.58957(19) 0.7475(4) 0.1885(3) 0.0364(17) Uani 1 1 d . . . N8 N 0.5689(2) 0.7096(4) 0.1458(3) 0.0414(19) Uani 1 1 d . . . H8B H 0.5779 0.6772 0.1450 0.050 Uiso 1 1 calc R . . N9 N 0.4693(3) 0.6315(4) -0.0395(4) 0.056(2) Uani 1 1 d . . . N10 N 0.78118(19) 0.7598(4) 0.4256(3) 0.0367(18) Uani 1 1 d . . . N11 N 0.81091(19) 0.7213(4) 0.4500(3) 0.0404(19) Uani 1 1 d . . . H11H H 0.8090 0.6867 0.4374 0.048 Uiso 1 1 calc R . . N12 N 0.9379(2) 0.6319(5) 0.5752(4) 0.060(3) Uani 1 1 d . . . N13 N 0.7836(2) 0.9607(4) 0.4102(4) 0.049(2) Uani 1 1 d . . . N14 N 0.7635(2) 1.0025(4) 0.4126(4) 0.053(2) Uani 1 1 d . . . H14B H 0.7524 1.0321 0.3912 0.064 Uiso 1 1 calc R . . N15 N 0.6968(3) 1.1162(5) 0.4514(4) 0.066(3) Uani 1 1 d . . . N16 N 0.8557(2) 0.9503(4) 0.2865(3) 0.0384(18) Uani 1 1 d . . . N17 N 0.8533(2) 0.9888(4) 0.2529(3) 0.054(2) Uani 1 1 d . . . H17A H 0.8427 1.0232 0.2443 0.065 Uiso 1 1 calc R . . N18 N 0.8497(5) 1.0756(11) 0.1189(6) 0.264(18) Uani 1 1 d D . . N19 N 0.5862(2) 0.9485(4) 0.1876(3) 0.0411(19) Uani 1 1 d . . . N20 N 0.5876(2) 0.9839(4) 0.2226(3) 0.049(2) Uani 1 1 d . . . H20B H 0.5995 1.0172 0.2350 0.059 Uiso 1 1 calc R . . N21 N 0.5814(4) 1.0286(8) 0.3601(6) 0.123(6) Uani 1 1 d . . . N22 N 0.6558(2) 0.9682(4) 0.0601(3) 0.0390(18) Uani 1 1 d . . . N23 N 0.6757(2) 1.0107(4) 0.0582(3) 0.044(2) Uani 1 1 d . . . H23A H 0.6862 1.0411 0.0788 0.053 Uiso 1 1 calc R . . N24 N 0.7430(3) 1.1190(4) 0.0195(5) 0.067(3) Uani 1 1 d . . . N25 N 0.7273(3) 0.9400(6) 0.2311(5) 0.087(4) Uani 1 1 d . . . N26 N 0.7062(4) 0.7042(6) 0.2105(6) 0.100(4) Uani 1 1 d . . . N27 N 0.4371(3) 0.5241(6) -0.0024(5) 0.098(5) Uani 1 1 d D . . N28 N 1.0014(4) 0.5591(7) 0.4311(8) 0.148(8) Uani 1 1 d D . . O1 O 0.82403(17) 0.8479(3) 0.2157(3) 0.0495(19) Uani 1 1 d . . . O2 O 0.91745(17) 0.7677(3) 0.3560(3) 0.0423(16) Uani 1 1 d . . . O3 O 0.9049(2) 0.7973(5) 0.2646(3) 0.071(2) Uani 1 1 d . . . O4 O 0.93584(16) 0.8971(3) 0.3604(2) 0.0393(15) Uani 1 1 d . . . O5 O 0.69973(17) 0.8654(3) 0.0672(3) 0.052(2) Uani 1 1 d . . . O6 O 0.59156(16) 0.8022(3) -0.0459(3) 0.0420(16) Uani 1 1 d . . . O7 O 0.6426(2) 0.8376(4) -0.0551(3) 0.0519(19) Uani 1 1 d . . . O8 O 0.58566(18) 0.9291(4) -0.0607(3) 0.0518(19) Uani 1 1 d . . . O9 O 0.61352(16) 0.8455(3) 0.2528(2) 0.0473(18) Uani 1 1 d . . . O10 O 0.52021(16) 0.7706(3) 0.1080(2) 0.0395(15) Uani 1 1 d . . . O11 O 0.50379(15) 0.8994(3) 0.1052(2) 0.0385(15) Uani 1 1 d . . . O12 O 0.5318(2) 0.7940(5) 0.1990(4) 0.077(3) Uani 1 1 d . . . O13 O 0.73852(16) 0.8589(3) 0.4010(3) 0.0420(16) Uani 1 1 d . . . O14 O 0.84599(17) 0.7924(4) 0.5133(3) 0.0491(19) Uani 1 1 d . . . O15 O 0.7957(2) 0.8338(5) 0.5237(3) 0.074(3) Uani 1 1 d . . . O16 O 0.8528(2) 0.9199(4) 0.5285(4) 0.082(3) Uani 1 1 d . . . O17 O 0.77907(19) 0.9528(4) 0.4815(3) 0.056(2) Uani 1 1 d . . . O18 O 0.8164(2) 0.8552(3) 0.4186(3) 0.0484(18) Uani 1 1 d . . . O19 O 0.86857(17) 0.8520(3) 0.3461(3) 0.0390(15) Uani 1 1 d . . . O20 O 0.8845(2) 0.9208(4) 0.2480(3) 0.057(2) Uani 1 1 d . . . O21 O 0.65999(17) 0.9591(3) -0.0113(3) 0.0434(16) Uani 1 1 d . . . O22 O 0.62171(19) 0.8638(3) 0.0494(3) 0.0428(16) Uani 1 1 d . . . O23 O 0.57128(17) 0.8549(3) 0.1237(3) 0.0380(15) Uani 1 1 d . . . O24 O 0.55085(18) 0.9161(4) 0.2161(3) 0.0495(18) Uani 1 1 d . . . O25 O 0.7192(3) 1.0367(5) 0.2421(4) 0.090(3) Uani 1 1 d . . . O26 O 0.6786(9) 0.6207(7) 0.1616(8) 0.301(18) Uani 1 1 d . . . O27 O 0.4972(3) 0.5141(9) 0.0443(8) 0.237(11) Uani 1 1 d D . . O28 O 1.0167(5) 0.6044(11) 0.3901(8) 0.241(11) Uani 1 1 d D . . O1W O 0.9350(3) 1.0249(5) 0.3577(4) 0.107(4) Uani 1 1 d . . . O2W O 0.6786(2) 1.1323(4) 0.1772(3) 0.065(2) Uani 1 1 d . . . O3W O 0.6074(3) 0.6108(4) 0.1526(4) 0.094(4) Uani 1 1 d . . . O4W O 0.7184(3) 1.0766(5) 0.3162(5) 0.095(3) Uani 1 1 d . . . O5W O 0.6430(5) 0.5479(8) -0.0150(9) 0.202(9) Uani 1 1 d . . . O6W O 0.9258(5) 0.8852(9) 0.6086(8) 0.218(10) Uani 1 1 d . . . O7W O 0.978(2) 1.173(4) 0.296(3) 0.35(5) Uiso 0.49(6) 1 d P . . O7WA O 1.0089(13) 1.162(2) 0.358(2) 0.23(3) Uiso 0.51(6) 1 d P . . O8W O 0.6405(3) 0.6113(5) 0.0575(4) 0.132(6) Uani 1 1 d . . . O9W O 0.9201(8) 0.6779(11) 0.2816(10) 0.259(13) Uani 1 1 d . . . C101 C 0.8478(7) 0.7205(14) 0.6027(12) 0.160 Uani 0.50 1 d PD . . H10A H 0.8406 0.6810 0.6038 0.240 Uiso 0.50 1 calc PR . . H10B H 0.8379 0.7285 0.5682 0.240 Uiso 0.50 1 calc PR . . H10C H 0.8386 0.7497 0.6117 0.240 Uiso 0.50 1 calc PR . . C102 C 0.9039(10) 0.7771(13) 0.6452(17) 0.197 Uani 0.50 1 d PD . . H10D H 0.9297 0.7705 0.6707 0.296 Uiso 0.50 1 calc PR . . H10E H 0.8977 0.8084 0.6569 0.296 Uiso 0.50 1 calc PR . . H10F H 0.8966 0.7887 0.6127 0.296 Uiso 0.50 1 calc PR . . C103 C 0.9064(9) 0.6722(13) 0.6658(13) 0.128 Uani 0.50 1 d PD . . H103 H 0.8961 0.6358 0.6632 0.154 Uiso 0.50 1 calc PR . . N31 N 0.8858(7) 0.7240(10) 0.6381(9) 0.108 Uani 0.50 1 d PD . . O33 O 0.9414(9) 0.680(2) 0.6956(19) 0.434 Uiso 0.50 1 d PD . . N41 N 0.9537(13) 0.992(3) 0.251(2) 0.850 Uiso 0.50 1 d PD . . C119 C 0.951(2) 0.933(3) 0.234(3) 0.360 Uiso 0.50 1 d PD . . H11B H 0.9551 0.9047 0.2588 0.539 Uiso 0.50 1 calc PR . . H11C H 0.9684 0.9266 0.2313 0.539 Uiso 0.50 1 calc PR . . H11D H 0.9268 0.9265 0.2008 0.539 Uiso 0.50 1 calc PR . . C118 C 0.947(3) 1.041(3) 0.221(4) 0.359 Uiso 0.50 1 d PD . . H11E H 0.9533 1.0775 0.2407 0.538 Uiso 0.50 1 calc PR . . H11F H 0.9213 1.0426 0.1899 0.538 Uiso 0.50 1 calc PR . . H11G H 0.9608 1.0384 0.2115 0.538 Uiso 0.50 1 calc PR . . C120 C 0.9624(14) 1.011(3) 0.2937(19) 0.296 Uiso 0.50 1 d PD . . H120 H 0.9680 0.9827 0.3181 0.355 Uiso 0.50 1 calc PR . . O35 O 0.9635(17) 1.068(3) 0.303(3) 0.436 Uiso 0.50 1 d PD . . N30 N 0.8163(3) 1.0944(14) 0.2266(10) 0.230 Uiso 1 1 d D . . N32 N 0.78517(16) 1.0867(3) 0.2023(2) 0.016 Uani 1 1 d D . . N33 N 0.7561(5) 1.084(2) 0.1885(16) 0.366 Uiso 1 1 d 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 0.0195(2) 0.0577(3) 0.0237(2) 0.00211(18) 0.01288(18) 0.00242(18) Dy2 0.0204(2) 0.0542(3) 0.0277(2) 0.00136(19) 0.01284(19) -0.00190(18) Dy3 0.0218(2) 0.0633(3) 0.0321(2) -0.0067(2) 0.0166(2) 0.00328(19) Dy4 0.0194(2) 0.0541(3) 0.0283(2) 0.00752(19) 0.01296(19) -0.00253(17) Cl1 0.115(4) 0.110(4) 0.120(4) -0.021(3) 0.074(3) -0.021(3) Cl2 0.224(8) 0.171(7) 0.153(6) -0.016(5) 0.131(6) -0.052(6) C1 0.027(5) 0.054(7) 0.040(6) 0.011(5) 0.008(5) -0.002(4) C2 0.030(5) 0.044(6) 0.046(6) 0.003(5) 0.015(5) -0.007(4) C3 0.024(5) 0.052(6) 0.035(5) 0.005(5) 0.011(4) -0.001(4) C4 0.025(5) 0.055(7) 0.036(6) 0.014(5) 0.006(4) -0.002(4) C5 0.030(6) 0.055(7) 0.061(8) 0.012(6) 0.007(6) -0.011(5) C6 0.025(5) 0.061(7) 0.046(7) 0.020(5) 0.005(5) -0.007(5) C7 0.021(4) 0.049(6) 0.040(6) 0.008(5) 0.010(4) 0.000(4) C8 0.031(5) 0.045(6) 0.051(7) 0.014(5) 0.012(5) -0.006(4) C9 0.027(5) 0.060(6) 0.039(5) -0.002(5) 0.021(4) -0.013(4) C10 0.026(5) 0.051(6) 0.040(6) 0.005(5) 0.017(4) -0.011(4) C11 0.037(6) 0.069(9) 0.071(9) 0.006(7) 0.017(6) -0.012(6) C12 0.047(7) 0.066(8) 0.090(10) 0.002(7) 0.038(7) -0.015(6) C13 0.024(5) 0.086(9) 0.065(8) 0.000(7) 0.025(6) -0.014(5) C14 0.020(5) 0.067(7) 0.049(7) 0.002(5) 0.013(5) -0.001(5) C15 0.030(5) 0.052(6) 0.040(6) 0.004(5) 0.008(5) -0.002(4) C16 0.034(5) 0.051(6) 0.031(5) -0.005(4) 0.017(4) 0.006(4) C17 0.035(5) 0.038(5) 0.043(6) -0.003(4) 0.023(5) 0.001(4) C18 0.030(6) 0.076(8) 0.046(7) 0.016(6) 0.011(5) 0.001(5) C19 0.047(7) 0.080(9) 0.043(7) 0.015(6) 0.018(6) -0.007(6) C20 0.032(5) 0.061(7) 0.043(6) 0.003(5) 0.015(5) 0.004(5) C21 0.039(6) 0.050(6) 0.043(6) 0.001(5) 0.023(5) 0.001(5) C22 0.027(5) 0.062(7) 0.040(6) -0.004(5) 0.010(5) 0.010(5) C23 0.024(5) 0.060(6) 0.029(5) -0.005(4) 0.015(4) 0.005(4) C24 0.028(5) 0.047(5) 0.035(5) 0.003(4) 0.020(4) 0.007(4) C25 0.022(4) 0.054(6) 0.028(5) 0.006(4) 0.012(4) 0.008(4) C26 0.033(5) 0.047(6) 0.030(5) 0.000(4) 0.016(4) 0.007(4) C27 0.023(4) 0.055(6) 0.029(5) 0.005(4) 0.011(4) 0.007(4) C28 0.031(5) 0.057(6) 0.035(5) 0.006(4) 0.022(4) 0.011(4) C29 0.040(6) 0.049(6) 0.038(6) 0.000(4) 0.024(5) 0.004(4) C30 0.035(5) 0.047(6) 0.042(6) 0.004(4) 0.027(5) -0.006(4) C31 0.037(5) 0.047(6) 0.032(5) 0.005(4) 0.017(5) -0.005(4) C32 0.042(6) 0.055(7) 0.043(6) -0.003(5) 0.027(5) -0.002(5) C33 0.047(7) 0.066(8) 0.043(7) -0.002(5) 0.021(6) 0.003(5) C34 0.033(6) 0.065(8) 0.042(6) -0.006(5) 0.015(5) -0.012(5) C35 0.033(5) 0.063(7) 0.046(6) -0.001(5) 0.021(5) -0.006(5) C36 0.027(5) 0.046(5) 0.032(5) 0.006(4) 0.017(4) 0.010(4) C37 0.025(4) 0.060(6) 0.029(5) 0.004(4) 0.018(4) 0.008(4) C38 0.026(5) 0.059(6) 0.036(5) 0.003(4) 0.021(4) 0.004(4) C39 0.022(5) 0.065(7) 0.049(6) 0.003(5) 0.022(5) 0.004(4) C40 0.027(5) 0.062(7) 0.054(7) 0.009(6) 0.018(5) 0.008(5) C41 0.025(5) 0.066(8) 0.087(9) 0.003(7) 0.028(6) 0.000(5) C42 0.030(5) 0.062(7) 0.067(8) 0.005(6) 0.026(6) 0.005(5) C43 0.056(6) 0.045(6) 0.060(7) 0.015(5) 0.049(6) 0.012(5) C44 0.034(5) 0.045(5) 0.042(6) 0.005(4) 0.028(5) -0.001(4) C45 0.035(5) 0.041(5) 0.055(6) -0.006(5) 0.032(5) 0.000(4) C46 0.033(5) 0.050(6) 0.044(6) -0.008(5) 0.026(5) 0.002(4) C47 0.035(5) 0.042(6) 0.053(6) -0.001(5) 0.028(5) 0.001(4) C48 0.023(4) 0.045(5) 0.032(5) 0.002(4) 0.014(4) 0.003(4) C49 0.021(4) 0.050(6) 0.029(5) 0.004(4) 0.013(4) 0.003(4) C50 0.029(5) 0.047(6) 0.036(5) 0.009(4) 0.017(4) 0.006(4) C51 0.042(6) 0.082(9) 0.037(6) 0.006(6) 0.021(5) -0.013(6) C52 0.065(9) 0.161(17) 0.053(8) 0.037(10) 0.032(8) -0.028(10) C53 0.24(3) 0.25(3) 0.33(4) 0.25(3) 0.24(3) 0.15(3) C54 0.22(3) 0.51(7) 0.32(5) 0.36(5) 0.20(4) 0.19(4) C55 0.42(7) 0.29(5) 0.25(4) -0.08(4) 0.24(5) -0.12(5) C56 0.25(3) 0.27(3) 0.110(17) -0.043(18) 0.15(2) -0.13(3) C57 0.046(6) 0.029(5) 0.072(7) -0.007(5) 0.043(6) 0.000(4) C58 0.039(6) 0.061(7) 0.057(7) -0.024(6) 0.034(6) -0.006(5) C59 0.035(6) 0.063(7) 0.058(7) -0.020(6) 0.030(6) -0.005(5) C60 0.057(8) 0.111(12) 0.062(8) -0.010(8) 0.041(7) 0.019(8) C61 0.064(8) 0.115(12) 0.075(9) -0.020(8) 0.052(8) 0.024(8) C62 0.057(7) 0.073(8) 0.067(8) -0.014(6) 0.045(7) 0.002(6) C63 0.059(7) 0.061(7) 0.066(8) -0.004(6) 0.046(7) 0.006(6) C64 0.051(6) 0.051(6) 0.055(7) -0.006(5) 0.041(6) -0.011(5) C65 0.029(5) 0.044(5) 0.028(5) -0.003(4) 0.019(4) -0.008(4) C66 0.024(4) 0.043(5) 0.022(4) 0.004(4) 0.013(4) -0.002(4) C67 0.034(5) 0.039(5) 0.038(5) 0.006(4) 0.024(4) -0.001(4) C68 0.029(5) 0.043(5) 0.037(5) 0.000(4) 0.019(4) -0.006(4) C69 0.033(5) 0.047(6) 0.031(5) -0.006(4) 0.021(4) -0.002(4) C70 0.027(4) 0.041(5) 0.028(5) -0.005(4) 0.016(4) -0.008(4) C71 0.029(5) 0.050(6) 0.040(6) -0.010(4) 0.021(5) -0.005(4) C72 0.023(5) 0.090(9) 0.029(5) -0.007(5) 0.011(4) 0.018(5) C73 0.029(6) 0.132(14) 0.063(9) -0.039(9) 0.022(6) -0.001(7) C74 0.112(15) 0.16(2) 0.125(16) -0.064(15) 0.093(14) -0.021(14) C75 0.123(16) 0.27(3) 0.123(16) -0.109(18) 0.110(15) -0.097(18) C76 0.103(14) 0.22(3) 0.090(13) -0.068(15) 0.071(13) -0.039(15) C77 0.115(15) 0.16(2) 0.099(14) -0.031(13) 0.083(13) -0.014(14) C78 0.031(5) 0.039(5) 0.039(5) 0.004(4) 0.019(4) -0.007(4) C79 0.024(4) 0.048(6) 0.042(6) 0.017(4) 0.017(4) -0.002(4) C80 0.040(5) 0.041(5) 0.057(7) 0.008(5) 0.037(5) 0.003(4) C81 0.034(5) 0.047(6) 0.063(7) 0.001(5) 0.034(5) -0.008(4) C82 0.050(7) 0.057(7) 0.080(9) -0.009(6) 0.050(7) -0.010(5) C83 0.072(8) 0.061(7) 0.080(9) 0.008(6) 0.064(8) -0.004(6) C84 0.048(6) 0.054(7) 0.062(7) 0.008(6) 0.038(6) -0.004(5) C85 0.079(10) 0.083(10) 0.071(9) 0.002(8) 0.049(9) 0.010(8) C86 0.129(17) 0.084(12) 0.17(2) -0.033(13) 0.108(17) -0.023(11) C87 0.084(12) 0.097(13) 0.106(14) -0.010(11) 0.050(11) -0.007(10) C88 0.086(12) 0.085(11) 0.110(14) 0.006(10) 0.062(11) 0.005(9) C89 0.089(13) 0.115(15) 0.16(2) 0.045(14) 0.081(14) 0.013(11) C90 0.29(4) 0.071(13) 0.091(16) -0.006(11) 0.08(2) 0.002(17) C91 0.16(2) 0.082(12) 0.35(4) 0.118(18) 0.21(2) 0.064(13) C92 0.075(11) 0.125(16) 0.077(12) 0.008(11) 0.022(10) 0.012(11) C93 0.062(11) 0.26(3) 0.119(17) 0.058(18) 0.055(12) 0.021(15) C94 0.12(2) 0.44(6) 0.14(2) -0.03(3) 0.06(2) -0.08(3) C95 0.070(11) 0.18(2) 0.112(15) -0.035(14) 0.057(11) -0.037(12) C96 0.094(15) 0.25(3) 0.31(4) -0.20(3) 0.13(2) -0.087(18) N1 0.031(4) 0.046(5) 0.038(5) 0.005(4) 0.017(4) -0.001(3) N2 0.028(4) 0.043(5) 0.034(4) 0.007(4) 0.014(4) 0.004(3) N3 0.039(5) 0.066(6) 0.036(5) 0.003(4) 0.012(4) -0.002(4) N4 0.023(4) 0.052(5) 0.040(5) 0.004(4) 0.013(4) -0.010(3) N5 0.026(4) 0.057(6) 0.050(5) 0.008(4) 0.014(4) -0.011(4) N6 0.031(5) 0.067(7) 0.067(7) -0.005(5) 0.015(5) -0.011(4) N7 0.023(4) 0.051(5) 0.023(4) -0.001(3) 0.011(3) -0.001(3) N8 0.029(4) 0.045(5) 0.032(4) -0.005(4) 0.014(4) -0.003(3) N9 0.055(6) 0.051(6) 0.044(5) -0.002(4) 0.026(5) -0.002(4) N10 0.019(4) 0.056(5) 0.031(4) 0.009(4) 0.015(3) 0.010(3) N11 0.021(4) 0.053(5) 0.039(5) 0.009(4) 0.017(4) 0.009(3) N12 0.029(5) 0.068(7) 0.062(6) 0.001(5) 0.023(5) 0.011(4) N13 0.040(5) 0.050(5) 0.071(6) -0.009(4) 0.044(5) 0.001(4) N14 0.047(5) 0.045(5) 0.075(7) -0.014(5) 0.044(5) 0.003(4) N15 0.060(6) 0.079(7) 0.078(7) -0.007(6) 0.055(6) 0.007(5) N16 0.029(4) 0.048(5) 0.030(4) 0.012(3) 0.016(4) 0.000(3) N17 0.044(5) 0.055(6) 0.045(5) 0.017(4) 0.022(4) -0.005(4) N18 0.090(13) 0.55(5) 0.055(10) 0.104(19) 0.010(9) -0.07(2) N19 0.030(4) 0.055(5) 0.029(4) -0.011(4) 0.016(4) 0.001(4) N20 0.041(5) 0.059(6) 0.043(5) -0.019(4) 0.027(4) 0.000(4) N21 0.092(11) 0.147(15) 0.082(10) -0.052(10) 0.039(9) -0.011(10) N22 0.026(4) 0.049(5) 0.032(4) 0.006(4) 0.015(4) -0.006(3) N23 0.029(4) 0.058(5) 0.035(5) 0.006(4) 0.017(4) -0.011(4) N24 0.071(7) 0.050(6) 0.111(9) 0.002(6) 0.074(7) -0.009(5) N25 0.069(8) 0.071(8) 0.085(9) -0.003(7) 0.037(7) 0.004(6) N26 0.098(10) 0.067(8) 0.102(10) 0.011(7) 0.055(9) 0.001(7) N27 0.044(6) 0.107(10) 0.086(9) 0.037(8) 0.021(6) 0.004(6) N28 0.062(9) 0.122(13) 0.197(19) -0.070(13) 0.062(11) -0.012(9) O1 0.020(3) 0.055(4) 0.034(4) 0.004(3) 0.002(3) -0.006(3) O2 0.028(3) 0.051(4) 0.040(4) 0.008(3) 0.020(3) 0.010(3) O3 0.054(5) 0.103(7) 0.059(5) -0.003(5) 0.040(5) 0.010(5) O4 0.022(3) 0.046(4) 0.035(4) 0.006(3) 0.014(3) 0.000(3) O5 0.016(3) 0.048(4) 0.053(5) 0.014(3) 0.008(3) -0.002(3) O6 0.022(3) 0.051(4) 0.040(4) 0.002(3) 0.015(3) -0.009(3) O7 0.048(4) 0.070(5) 0.056(5) 0.000(4) 0.043(4) -0.008(4) O8 0.034(4) 0.064(5) 0.046(4) 0.019(4) 0.022(3) 0.007(3) O9 0.018(3) 0.071(5) 0.024(3) -0.004(3) 0.002(3) 0.012(3) O10 0.020(3) 0.051(4) 0.034(4) -0.004(3) 0.013(3) -0.002(3) O11 0.018(3) 0.050(4) 0.032(3) 0.003(3) 0.011(3) -0.002(3) O12 0.069(6) 0.117(8) 0.076(6) 0.013(6) 0.061(6) -0.005(5) O13 0.021(3) 0.051(4) 0.036(4) 0.000(3) 0.012(3) 0.005(3) O14 0.023(3) 0.078(5) 0.032(4) -0.002(3) 0.013(3) 0.016(3) O15 0.074(6) 0.114(8) 0.048(5) 0.027(5) 0.047(5) 0.057(5) O16 0.037(4) 0.091(7) 0.081(6) -0.049(5) 0.024(5) -0.010(4) O17 0.031(4) 0.080(6) 0.051(5) -0.021(4) 0.025(4) 0.007(4) O18 0.065(5) 0.047(4) 0.072(5) 0.000(4) 0.061(5) 0.003(3) O19 0.035(4) 0.055(4) 0.040(4) 0.014(3) 0.031(3) 0.012(3) O20 0.045(4) 0.084(6) 0.041(4) -0.002(4) 0.028(4) -0.012(4) O21 0.033(3) 0.054(4) 0.037(4) 0.010(3) 0.021(3) -0.004(3) O22 0.053(4) 0.049(4) 0.045(4) -0.002(3) 0.041(4) -0.014(3) O23 0.036(4) 0.052(4) 0.039(4) -0.008(3) 0.031(3) -0.012(3) O24 0.031(4) 0.077(5) 0.035(4) -0.001(4) 0.020(3) 0.005(3) O25 0.097(8) 0.086(7) 0.078(7) 0.011(5) 0.056(7) 0.024(6) O26 0.51(4) 0.065(9) 0.144(16) 0.017(10) 0.15(2) -0.008(16) O27 0.175(18) 0.164(18) 0.23(2) 0.051(16) 0.081(17) -0.027(14) O28 0.122(15) 0.27(3) 0.24(2) -0.05(2) 0.086(16) -0.055(16) O1W 0.050(6) 0.083(7) 0.105(8) 0.001(6) 0.019(6) -0.011(5) O2W 0.043(5) 0.065(5) 0.059(5) -0.011(4) 0.023(4) 0.003(4) O3W 0.058(6) 0.071(6) 0.081(7) -0.021(5) 0.019(5) 0.013(5) O4W 0.125(9) 0.091(8) 0.113(9) 0.020(7) 0.098(8) 0.025(7) O5W 0.163(16) 0.130(13) 0.27(2) 0.069(14) 0.132(17) 0.082(12) O6W 0.154(16) 0.173(18) 0.180(18) 0.010(14) 0.054(14) -0.035(14) O8W 0.110(9) 0.072(7) 0.077(7) 0.022(6) 0.009(7) -0.031(7) O9W 0.34(3) 0.20(2) 0.26(3) 0.05(2) 0.21(3) 0.13(2) C101 0.305 0.098 0.294 -0.034 0.289 -0.040 C102 0.197 0.197 0.197 0.000 0.133 0.000 C103 0.128 0.128 0.128 0.000 0.087 0.000 N31 0.194 0.091 0.125 0.001 0.143 0.007 N32 0.016 0.016 0.016 0.000 0.011 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 O23 2.204(6) . ? Dy1 O9 2.210(6) . ? Dy1 O24 2.366(7) . ? Dy1 O12 2.368(8) . ? Dy1 O11 2.398(6) . ? Dy1 O10 2.409(6) . ? Dy1 N19 2.521(9) . ? Dy1 N7 2.522(8) . ? Dy2 O1 2.188(6) . ? Dy2 O19 2.216(6) . ? Dy2 O3 2.385(8) . ? Dy2 O4 2.408(6) . ? Dy2 O20 2.428(8) . ? Dy2 O2 2.429(6) . ? Dy2 N16 2.508(8) . ? Dy2 N1 2.534(8) . ? Dy3 O13 2.206(6) . ? Dy3 O18 2.210(6) . ? Dy3 O15 2.374(8) . ? Dy3 O16 2.389(8) . ? Dy3 O14 2.395(7) . ? Dy3 O17 2.474(7) . ? Dy3 N10 2.524(9) . ? Dy3 N13 2.537(10) . ? Dy4 O5 2.204(6) . ? Dy4 O22 2.209(6) . ? Dy4 O8 2.396(7) . ? Dy4 O7 2.401(7) . ? Dy4 O6 2.406(6) . ? Dy4 O21 2.412(6) . ? Dy4 N22 2.536(9) . ? Dy4 N4 2.539(9) . ? C1 C2 1.553(14) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C7 1.392(13) . ? C2 C3 1.396(14) . ? C3 O1 1.290(11) . ? C3 C4 1.433(15) . ? C4 C5 1.383(14) . ? C4 C15 1.440(14) . ? C5 C6 1.393(15) . ? C5 H5A 0.9300 . ? C6 C7 1.433(15) . ? C6 C8 1.450(14) . ? C7 O5 1.325(11) . ? C8 N4 1.287(12) . ? C8 H8A 0.9300 . ? C9 O6 1.241(12) . ? C9 N5 1.333(13) . ? C9 C10 1.503(12) . ? C10 C14 1.381(14) . ? C10 C11 1.384(17) . ? C11 C12 1.426(16) . ? C11 H11A 0.9300 . ? C12 N6 1.328(16) . ? C12 H12A 0.9300 . ? C13 N6 1.304(16) . ? C13 C14 1.386(14) . ? C13 H13A 0.9300 . ? C14 H14A 0.9300 . ? C15 N1 1.298(12) . ? C15 H15A 0.9300 . ? C16 O2 1.237(12) . ? C16 N2 1.347(12) . ? C16 C17 1.511(14) . ? C17 C18 1.370(16) . ? C17 C21 1.375(14) . ? C18 C19 1.367(16) . ? C18 H18A 0.9300 . ? C19 N3 1.340(14) . ? C19 H19A 0.9300 . ? C20 N3 1.301(15) . ? C20 C21 1.394(15) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C22 C23 1.487(14) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C28 1.383(14) . ? C23 C24 1.419(12) . ? C24 O13 1.297(11) . ? C24 C25 1.438(14) . ? C25 C26 1.376(13) . ? C25 C36 1.455(12) . ? C26 C27 1.412(12) . ? C26 H26A 0.9300 . ? C27 C29 1.425(14) . ? C27 C28 1.465(14) . ? C28 O9 1.294(11) . ? C29 N7 1.301(12) . ? C29 H29A 0.9300 . ? C30 O10 1.255(12) . ? C30 N8 1.329(12) . ? C30 C31 1.512(14) . ? C31 C35 1.372(14) . ? C31 C32 1.385(15) . ? C32 C33 1.395(15) . ? C32 H32A 0.9300 . ? C33 N9 1.352(15) . ? C33 H33A 0.9300 . ? C34 N9 1.327(15) . ? C34 C35 1.376(15) . ? C34 H34A 0.9300 . ? C35 H35A 0.9300 . ? C36 N10 1.284(12) . ? C36 H36A 0.9300 . ? C37 O14 1.266(12) . ? C37 N11 1.322(12) . ? C37 C38 1.509(13) . ? C38 C39 1.355(15) . ? C38 C42 1.390(14) . ? C39 C40 1.396(14) . ? C39 H39A 0.9300 . ? C40 N12 1.335(14) . ? C40 H40A 0.9300 . ? C41 N12 1.361(16) . ? C41 C42 1.387(15) . ? C41 H41A 0.9300 . ? C42 H42A 0.9300 . ? C43 C44 1.507(13) . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 C45 1.411(13) . ? C44 C49 1.419(13) . ? C45 O18 1.304(12) . ? C45 C46 1.427(14) . ? C46 C47 1.415(14) . ? C46 C57 1.443(13) . ? C47 C48 1.370(13) . ? C47 H47A 0.9300 . ? C48 C50 1.434(13) . ? C48 C49 1.450(13) . ? C49 O19 1.296(11) . ? C50 N16 1.301(13) . ? C50 H50A 0.9300 . ? C51 O20 1.235(15) . ? C51 N17 1.352(15) . ? C51 C52 1.495(15) . ? C52 C56 1.339(14) . ? C52 C53 1.368(15) . ? C53 C54 1.375(14) . ? C53 H53A 0.9300 . ? C54 N18 1.347(16) . ? C54 H54A 0.9300 . ? C55 N18 1.342(16) . ? C55 C56 1.358(16) . ? C55 H55A 0.9300 . ? C56 H56A 0.9300 . ? C57 N13 1.274(13) . ? C57 H57A 0.9300 . ? C58 O17 1.244(14) . ? C58 N14 1.318(14) . ? C58 C59 1.506(14) . ? C59 C63 1.373(16) . ? C59 C60 1.374(17) . ? C60 C61 1.381(16) . ? C60 H60A 0.9300 . ? C61 N15 1.364(16) . ? C61 H61A 0.9300 . ? C62 N15 1.322(16) . ? C62 C63 1.395(16) . ? C62 H62A 0.9300 . ? C63 H63A 0.9300 . ? C64 C65 1.518(13) . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? C65 C70 1.391(13) . ? C65 C66 1.408(12) . ? C66 O22 1.299(11) . ? C66 C67 1.444(13) . ? C67 C68 1.365(13) . ? C67 C78 1.453(12) . ? C68 C69 1.398(13) . ? C68 H68A 0.9300 . ? C69 C70 1.428(13) . ? C69 C71 1.435(13) . ? C70 O23 1.320(10) . ? C71 N19 1.298(12) . ? C71 H71A 0.9300 . ? C72 O24 1.231(14) . ? C72 N20 1.348(15) . ? C72 C73 1.482(16) . ? C73 C74 1.25(2) . ? C73 C77 1.44(2) . ? C74 C75 1.40(2) . ? C74 H74A 0.9300 . ? C75 N21 1.26(2) . ? C75 H75A 0.9300 . ? C76 N21 1.37(2) . ? C76 C77 1.39(2) . ? C76 H76A 0.9300 . ? C77 H77A 0.9300 . ? C78 N22 1.303(13) . ? C78 H78A 0.9300 . ? C79 O21 1.264(12) . ? C79 N23 1.314(13) . ? C79 C80 1.504(13) . ? C80 C81 1.369(14) . ? C80 C84 1.374(15) . ? C81 C82 1.375(14) . ? C81 H81A 0.9300 . ? C82 N24 1.319(16) . ? C82 H82A 0.9300 . ? C83 N24 1.319(16) . ? C83 C84 1.382(15) . ? C83 H83A 0.9300 . ? C84 H84A 0.9300 . ? C85 O25 1.216(16) . ? C85 N25 1.340(19) . ? C85 H85A 0.9300 . ? C86 N25 1.46(2) . ? C86 H86A 0.9600 . ? C86 H86B 0.9600 . ? C86 H86C 0.9600 . ? C87 N25 1.48(2) . ? C87 H87A 0.9600 . ? C87 H87B 0.9600 . ? C87 H87C 0.9600 . ? C88 N26 1.44(2) . ? C88 H88A 0.9600 . ? C88 H88B 0.9600 . ? C88 H88C 0.9600 . ? C89 N26 1.46(2) . ? C89 H89A 0.9600 . ? C89 H89B 0.9600 . ? C89 H89C 0.9600 . ? C90 O26 1.26(3) . ? C90 N26 1.34(2) . ? C90 H90A 0.9300 . ? C91 O27 1.279(10) . ? C91 N27 1.423(10) . ? C91 H91 0.9300 . ? C92 N27 1.50(2) . ? C92 H92A 0.9600 . ? C92 H92B 0.9600 . ? C92 H92C 0.9600 . ? C93 N27 1.38(2) . ? C93 H93A 0.9600 . ? C93 H93B 0.9600 . ? C93 H93C 0.9600 . ? C94 O28 1.300(10) . ? C94 N28 1.43(3) . ? C94 H94 0.9300 . ? C95 N28 1.40(2) . ? C95 H95A 0.9600 . ? C95 H95B 0.9600 . ? C95 H95C 0.9600 . ? C96 N28 1.39(3) . ? C96 H96A 0.9600 . ? C96 H96B 0.9600 . ? C96 H96C 0.9600 . ? N1 N2 1.414(11) . ? N2 H2A 0.8600 . ? N4 N5 1.409(10) . ? N5 H5B 0.8600 . ? N7 N8 1.383(10) . ? N8 H8B 0.8600 . ? N10 N11 1.395(10) . ? N11 H11H 0.8600 . ? N13 N14 1.409(11) . ? N14 H14B 0.8600 . ? N16 N17 1.387(11) . ? N17 H17A 0.8600 . ? N19 N20 1.412(11) . ? N20 H20B 0.8600 . ? N22 N23 1.404(10) . ? N23 H23A 0.8600 . ? O7W O7WA 1.62(8) . ? C101 N31 1.401(10) . ? C101 H10A 0.9600 . ? C101 H10B 0.9600 . ? C101 H10C 0.9600 . ? C102 N31 1.403(10) . ? C102 H10D 0.9600 . ? C102 H10E 0.9600 . ? C102 H10F 0.9600 . ? C103 O33 1.305(10) . ? C103 N31 1.404(17) . ? C103 H103 0.9300 . ? N41 C120 1.302(10) . ? N41 C119 1.403(10) . ? N41 C118 1.403(10) . ? C119 H11B 0.9600 . ? C119 H11C 0.9600 . ? C119 H11D 0.9600 . ? C118 H11E 0.9600 . ? C118 H11F 0.9600 . ? C118 H11G 0.9600 . ? C120 O35 1.303(10) . ? C120 H120 0.9300 . ? N30 N32 1.173(8) . ? N32 N33 1.177(9) . ? 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 O23 Dy1 O9 102.7(3) . . ? O23 Dy1 O24 133.9(3) . . ? O9 Dy1 O24 78.8(2) . . ? O23 Dy1 O12 150.8(3) . . ? O9 Dy1 O12 93.3(3) . . ? O24 Dy1 O12 72.7(3) . . ? O23 Dy1 O11 85.5(2) . . ? O9 Dy1 O11 149.3(2) . . ? O24 Dy1 O11 74.5(2) . . ? O12 Dy1 O11 93.1(3) . . ? O23 Dy1 O10 77.8(2) . . ? O9 Dy1 O10 134.3(2) . . ? O24 Dy1 O10 133.4(2) . . ? O12 Dy1 O10 73.6(3) . . ? O11 Dy1 O10 76.2(2) . . ? O23 Dy1 N19 71.1(2) . . ? O9 Dy1 N19 73.5(3) . . ? O24 Dy1 N19 65.3(3) . . ? O12 Dy1 N19 137.6(3) . . ? O11 Dy1 N19 81.6(2) . . ? O10 Dy1 N19 142.9(2) . . ? O23 Dy1 N7 77.8(3) . . ? O9 Dy1 N7 70.8(2) . . ? O24 Dy1 N7 141.0(2) . . ? O12 Dy1 N7 84.9(3) . . ? O11 Dy1 N7 139.8(2) . . ? O10 Dy1 N7 64.7(2) . . ? N19 Dy1 N7 125.1(2) . . ? O1 Dy2 O19 103.3(3) . . ? O1 Dy2 O3 93.6(3) . . ? O19 Dy2 O3 150.3(3) . . ? O1 Dy2 O4 149.6(2) . . ? O19 Dy2 O4 87.5(2) . . ? O3 Dy2 O4 90.1(3) . . ? O1 Dy2 O20 77.6(3) . . ? O19 Dy2 O20 134.5(3) . . ? O3 Dy2 O20 72.6(3) . . ? O4 Dy2 O20 74.7(2) . . ? O1 Dy2 O2 133.3(3) . . ? O19 Dy2 O2 77.3(2) . . ? O3 Dy2 O2 73.4(3) . . ? O4 Dy2 O2 76.5(2) . . ? O20 Dy2 O2 134.9(2) . . ? O1 Dy2 N16 76.4(3) . . ? O19 Dy2 N16 71.7(2) . . ? O3 Dy2 N16 136.8(3) . . ? O4 Dy2 N16 80.4(2) . . ? O20 Dy2 N16 64.3(3) . . ? O2 Dy2 N16 141.8(2) . . ? O1 Dy2 N1 70.2(3) . . ? O19 Dy2 N1 76.8(3) . . ? O3 Dy2 N1 86.5(3) . . ? O4 Dy2 N1 140.2(2) . . ? O20 Dy2 N1 140.2(3) . . ? O2 Dy2 N1 64.5(2) . . ? N16 Dy2 N1 126.5(3) . . ? O13 Dy3 O18 104.8(3) . . ? O13 Dy3 O15 88.5(3) . . ? O18 Dy3 O15 152.6(3) . . ? O13 Dy3 O16 151.0(3) . . ? O18 Dy3 O16 90.2(3) . . ? O15 Dy3 O16 89.1(4) . . ? O13 Dy3 O14 133.2(3) . . ? O18 Dy3 O14 78.1(3) . . ? O15 Dy3 O14 75.4(2) . . ? O16 Dy3 O14 73.6(3) . . ? O13 Dy3 O17 77.7(2) . . ? O18 Dy3 O17 133.3(3) . . ? O15 Dy3 O17 72.4(3) . . ? O16 Dy3 O17 74.1(3) . . ? O14 Dy3 O17 134.1(2) . . ? O13 Dy3 N10 71.2(2) . . ? O18 Dy3 N10 74.4(3) . . ? O15 Dy3 N10 87.9(3) . . ? O16 Dy3 N10 137.6(3) . . ? O14 Dy3 N10 64.7(2) . . ? O17 Dy3 N10 143.5(2) . . ? O13 Dy3 N13 79.7(3) . . ? O18 Dy3 N13 70.8(3) . . ? O15 Dy3 N13 136.1(3) . . ? O16 Dy3 N13 82.1(3) . . ? O14 Dy3 N13 140.1(3) . . ? O17 Dy3 N13 63.8(3) . . ? N10 Dy3 N13 126.3(3) . . ? O5 Dy4 O22 104.9(3) . . ? O5 Dy4 O8 152.0(3) . . ? O22 Dy4 O8 90.6(3) . . ? O5 Dy4 O7 88.0(3) . . ? O22 Dy4 O7 149.9(2) . . ? O8 Dy4 O7 90.0(3) . . ? O5 Dy4 O6 132.7(2) . . ? O22 Dy4 O6 77.7(2) . . ? O8 Dy4 O6 72.8(2) . . ? O7 Dy4 O6 73.7(2) . . ? O5 Dy4 O21 77.8(2) . . ? O22 Dy4 O21 133.8(3) . . ? O8 Dy4 O21 74.7(2) . . ? O7 Dy4 O21 75.1(3) . . ? O6 Dy4 O21 134.3(2) . . ? O5 Dy4 N22 80.1(3) . . ? O22 Dy4 N22 70.5(2) . . ? O8 Dy4 N22 83.5(3) . . ? O7 Dy4 N22 139.4(2) . . ? O6 Dy4 N22 139.9(2) . . ? O21 Dy4 N22 64.5(2) . . ? O5 Dy4 N4 70.9(2) . . ? O22 Dy4 N4 76.1(3) . . ? O8 Dy4 N4 136.5(2) . . ? O7 Dy4 N4 82.8(3) . . ? O6 Dy4 N4 63.9(2) . . ? O21 Dy4 N4 142.1(2) . . ? N22 Dy4 N4 127.7(3) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C7 C2 C3 122.1(10) . . ? C7 C2 C1 119.8(9) . . ? C3 C2 C1 118.0(9) . . ? O1 C3 C2 120.5(9) . . ? O1 C3 C4 121.0(9) . . ? C2 C3 C4 118.5(9) . . ? C5 C4 C3 119.4(9) . . ? C5 C4 C15 117.4(10) . . ? C3 C4 C15 123.1(9) . . ? C4 C5 C6 122.3(11) . . ? C4 C5 H5A 118.9 . . ? C6 C5 H5A 118.9 . . ? C5 C6 C7 118.6(9) . . ? C5 C6 C8 118.7(10) . . ? C7 C6 C8 122.7(9) . . ? O5 C7 C2 119.8(9) . . ? O5 C7 C6 121.1(8) . . ? C2 C7 C6 119.0(9) . . ? N4 C8 C6 126.5(10) . . ? N4 C8 H8A 116.8 . . ? C6 C8 H8A 116.8 . . ? O6 C9 N5 123.5(9) . . ? O6 C9 C10 119.9(9) . . ? N5 C9 C10 116.5(9) . . ? C14 C10 C11 119.5(10) . . ? C14 C10 C9 117.3(10) . . ? C11 C10 C9 123.1(10) . . ? C10 C11 C12 117.1(12) . . ? C10 C11 H11A 121.5 . . ? C12 C11 H11A 121.5 . . ? N6 C12 C11 122.2(13) . . ? N6 C12 H12A 118.9 . . ? C11 C12 H12A 118.9 . . ? N6 C13 C14 123.5(11) . . ? N6 C13 H13A 118.2 . . ? C14 C13 H13A 118.2 . . ? C10 C14 C13 118.3(11) . . ? C10 C14 H14A 120.8 . . ? C13 C14 H14A 120.8 . . ? N1 C15 C4 124.6(10) . . ? N1 C15 H15A 117.7 . . ? C4 C15 H15A 117.7 . . ? O2 C16 N2 123.2(9) . . ? O2 C16 C17 120.3(9) . . ? N2 C16 C17 116.5(9) . . ? C18 C17 C21 117.1(10) . . ? C18 C17 C16 124.2(9) . . ? C21 C17 C16 118.4(10) . . ? C19 C18 C17 119.5(11) . . ? C19 C18 H18A 120.2 . . ? C17 C18 H18A 120.2 . . ? N3 C19 C18 123.8(12) . . ? N3 C19 H19A 118.1 . . ? C18 C19 H19A 118.1 . . ? N3 C20 C21 123.6(10) . . ? N3 C20 H20A 118.2 . . ? C21 C20 H20A 118.2 . . ? C17 C21 C20 119.3(11) . . ? C17 C21 H21A 120.4 . . ? C20 C21 H21A 120.4 . . ? C23 C22 H22A 109.5 . . ? C23 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C23 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C28 C23 C24 121.5(9) . . ? C28 C23 C22 119.0(9) . . ? C24 C23 C22 119.5(9) . . ? O13 C24 C23 120.8(9) . . ? O13 C24 C25 120.4(8) . . ? C23 C24 C25 118.8(9) . . ? C26 C25 C24 119.6(8) . . ? C26 C25 C36 116.7(9) . . ? C24 C25 C36 123.7(9) . . ? C25 C26 C27 123.0(9) . . ? C25 C26 H26A 118.5 . . ? C27 C26 H26A 118.5 . . ? C26 C27 C29 119.3(9) . . ? C26 C27 C28 117.2(9) . . ? C29 C27 C28 123.4(9) . . ? O9 C28 C23 121.3(10) . . ? O9 C28 C27 118.8(9) . . ? C23 C28 C27 119.8(9) . . ? N7 C29 C27 126.6(10) . . ? N7 C29 H29A 116.7 . . ? C27 C29 H29A 116.7 . . ? O10 C30 N8 122.8(9) . . ? O10 C30 C31 118.9(9) . . ? N8 C30 C31 118.3(9) . . ? C35 C31 C32 119.3(10) . . ? C35 C31 C30 119.1(10) . . ? C32 C31 C30 121.4(9) . . ? C31 C32 C33 117.7(11) . . ? C31 C32 H32A 121.2 . . ? C33 C32 H32A 121.2 . . ? N9 C33 C32 123.3(12) . . ? N9 C33 H33A 118.4 . . ? C32 C33 H33A 118.4 . . ? N9 C34 C35 123.9(11) . . ? N9 C34 H34A 118.0 . . ? C35 C34 H34A 118.0 . . ? C31 C35 C34 119.0(11) . . ? C31 C35 H35A 120.5 . . ? C34 C35 H35A 120.5 . . ? N10 C36 C25 125.5(9) . . ? N10 C36 H36A 117.2 . . ? C25 C36 H36A 117.2 . . ? O14 C37 N11 123.6(9) . . ? O14 C37 C38 119.4(8) . . ? N11 C37 C38 117.1(9) . . ? C39 C38 C42 118.9(9) . . ? C39 C38 C37 123.9(9) . . ? C42 C38 C37 117.1(10) . . ? C38 C39 C40 120.7(10) . . ? C38 C39 H39A 119.6 . . ? C40 C39 H39A 119.6 . . ? N12 C40 C39 121.5(11) . . ? N12 C40 H40A 119.3 . . ? C39 C40 H40A 119.3 . . ? N12 C41 C42 123.1(10) . . ? N12 C41 H41A 118.4 . . ? C42 C41 H41A 118.4 . . ? C41 C42 C38 118.0(11) . . ? C41 C42 H42A 121.0 . . ? C38 C42 H42A 121.0 . . ? C44 C43 H43A 109.5 . . ? C44 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C44 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C45 C44 C49 120.7(9) . . ? C45 C44 C43 119.2(8) . . ? C49 C44 C43 120.1(9) . . ? O18 C45 C44 119.0(9) . . ? O18 C45 C46 121.0(9) . . ? C44 C45 C46 120.0(9) . . ? C47 C46 C45 118.7(9) . . ? C47 C46 C57 117.6(10) . . ? C45 C46 C57 123.7(10) . . ? C48 C47 C46 122.1(10) . . ? C48 C47 H47A 118.9 . . ? C46 C47 H47A 118.9 . . ? C47 C48 C50 117.3(9) . . ? C47 C48 C49 120.0(9) . . ? C50 C48 C49 122.7(9) . . ? O19 C49 C44 120.0(9) . . ? O19 C49 C48 121.5(9) . . ? C44 C49 C48 118.5(9) . . ? N16 C50 C48 126.4(9) . . ? N16 C50 H50A 116.8 . . ? C48 C50 H50A 116.8 . . ? O20 C51 N17 121.7(10) . . ? O20 C51 C52 124.9(13) . . ? N17 C51 C52 113.4(12) . . ? C56 C52 C53 119.7(10) . . ? C56 C52 C51 115.2(14) . . ? C53 C52 C51 125.0(13) . . ? C52 C53 C54 118.3(13) . . ? C52 C53 H53A 120.9 . . ? C54 C53 H53A 120.9 . . ? N18 C54 C53 120.3(13) . . ? N18 C54 H54A 119.8 . . ? C53 C54 H54A 119.8 . . ? N18 C55 C56 118.1(14) . . ? N18 C55 H55A 120.9 . . ? C56 C55 H55A 120.9 . . ? C52 C56 C55 121.8(13) . . ? C52 C56 H56A 119.1 . . ? C55 C56 H56A 119.1 . . ? N13 C57 C46 125.7(10) . . ? N13 C57 H57A 117.2 . . ? C46 C57 H57A 117.2 . . ? O17 C58 N14 123.0(10) . . ? O17 C58 C59 121.0(10) . . ? N14 C58 C59 116.0(11) . . ? C63 C59 C60 118.9(11) . . ? C63 C59 C58 119.5(11) . . ? C60 C59 C58 121.4(11) . . ? C59 C60 C61 118.6(12) . . ? C59 C60 H60A 120.7 . . ? C61 C60 H60A 120.7 . . ? N15 C61 C60 123.5(14) . . ? N15 C61 H61A 118.2 . . ? C60 C61 H61A 118.2 . . ? N15 C62 C63 123.7(12) . . ? N15 C62 H62A 118.1 . . ? C63 C62 H62A 118.1 . . ? C59 C63 C62 118.9(12) . . ? C59 C63 H63A 120.6 . . ? C62 C63 H63A 120.6 . . ? C65 C64 H64A 109.5 . . ? C65 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C65 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C70 C65 C66 120.5(8) . . ? C70 C65 C64 121.8(8) . . ? C66 C65 C64 117.7(8) . . ? O22 C66 C65 120.0(8) . . ? O22 C66 C67 121.3(8) . . ? C65 C66 C67 118.8(8) . . ? C68 C67 C66 119.9(8) . . ? C68 C67 C78 118.2(9) . . ? C66 C67 C78 121.9(9) . . ? C67 C68 C69 121.8(9) . . ? C67 C68 H68A 119.1 . . ? C69 C68 H68A 119.1 . . ? C68 C69 C70 118.9(9) . . ? C68 C69 C71 117.9(9) . . ? C70 C69 C71 123.1(9) . . ? O23 C70 C65 118.7(8) . . ? O23 C70 C69 121.2(8) . . ? C65 C70 C69 120.0(8) . . ? N19 C71 C69 126.2(9) . . ? N19 C71 H71A 116.9 . . ? C69 C71 H71A 116.9 . . ? O24 C72 N20 122.8(9) . . ? O24 C72 C73 117.5(12) . . ? N20 C72 C73 119.6(12) . . ? C74 C73 C77 113.2(16) . . ? C74 C73 C72 130.0(15) . . ? C77 C73 C72 115.8(14) . . ? C73 C74 C75 126.5(19) . . ? C73 C74 H74A 116.7 . . ? C75 C74 H74A 116.7 . . ? N21 C75 C74 118(2) . . ? N21 C75 H75A 120.9 . . ? C74 C75 H75A 120.9 . . ? N21 C76 C77 115.8(19) . . ? N21 C76 H76A 122.1 . . ? C77 C76 H76A 122.1 . . ? C76 C77 C73 122.3(19) . . ? C76 C77 H77A 118.9 . . ? C73 C77 H77A 118.9 . . ? N22 C78 C67 126.4(9) . . ? N22 C78 H78A 116.8 . . ? C67 C78 H78A 116.8 . . ? O21 C79 N23 125.0(9) . . ? O21 C79 C80 118.9(9) . . ? N23 C79 C80 116.1(9) . . ? C81 C80 C84 118.3(10) . . ? C81 C80 C79 121.3(9) . . ? C84 C80 C79 120.4(10) . . ? C80 C81 C82 119.7(11) . . ? C80 C81 H81A 120.1 . . ? C82 C81 H81A 120.1 . . ? N24 C82 C81 122.5(12) . . ? N24 C82 H82A 118.7 . . ? C81 C82 H82A 118.7 . . ? N24 C83 C84 123.8(12) . . ? N24 C83 H83A 118.1 . . ? C84 C83 H83A 118.1 . . ? C80 C84 C83 118.0(11) . . ? C80 C84 H84A 121.0 . . ? C83 C84 H84A 121.0 . . ? O25 C85 N25 125.1(16) . . ? O25 C85 H85A 117.4 . . ? N25 C85 H85A 117.4 . . ? N25 C86 H86A 109.5 . . ? N25 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? N25 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? N25 C87 H87A 109.5 . . ? N25 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? N25 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? N26 C88 H88A 109.5 . . ? N26 C88 H88B 109.5 . . ? H88A C88 H88B 109.5 . . ? N26 C88 H88C 109.5 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? N26 C89 H89A 109.5 . . ? N26 C89 H89B 109.5 . . ? H89A C89 H89B 109.5 . . ? N26 C89 H89C 109.5 . . ? H89A C89 H89C 109.5 . . ? H89B C89 H89C 109.5 . . ? O26 C90 N26 120(3) . . ? O26 C90 H90A 119.9 . . ? N26 C90 H90A 119.9 . . ? O27 C91 N27 112.9(11) . . ? O27 C91 H91 123.5 . . ? N27 C91 H91 123.5 . . ? N27 C92 H92A 109.5 . . ? N27 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? N27 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? N27 C93 H93A 109.5 . . ? N27 C93 H93B 109.5 . . ? H93A C93 H93B 109.5 . . ? N27 C93 H93C 109.5 . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 109.5 . . ? O28 C94 N28 111(2) . . ? O28 C94 H94 124.3 . . ? N28 C94 H94 124.3 . . ? N28 C95 H95A 109.5 . . ? N28 C95 H95B 109.5 . . ? H95A C95 H95B 109.5 . . ? N28 C95 H95C 109.5 . . ? H95A C95 H95C 109.5 . . ? H95B C95 H95C 109.5 . . ? N28 C96 H96A 109.5 . . ? N28 C96 H96B 109.5 . . ? H96A C96 H96B 109.5 . . ? N28 C96 H96C 109.5 . . ? H96A C96 H96C 109.5 . . ? H96B C96 H96C 109.5 . . ? C15 N1 N2 113.7(9) . . ? C15 N1 Dy2 132.2(7) . . ? N2 N1 Dy2 113.2(5) . . ? C16 N2 N1 115.8(8) . . ? C16 N2 H2A 122.1 . . ? N1 N2 H2A 122.1 . . ? C20 N3 C19 116.5(10) . . ? C8 N4 N5 113.8(9) . . ? C8 N4 Dy4 130.6(7) . . ? N5 N4 Dy4 114.5(6) . . ? C9 N5 N4 114.8(9) . . ? C9 N5 H5B 122.6 . . ? N4 N5 H5B 122.6 . . ? C13 N6 C12 119.0(10) . . ? C29 N7 N8 114.6(8) . . ? C29 N7 Dy1 131.0(7) . . ? N8 N7 Dy1 113.7(5) . . ? C30 N8 N7 116.8(8) . . ? C30 N8 H8B 121.6 . . ? N7 N8 H8B 121.6 . . ? C34 N9 C33 116.8(10) . . ? C36 N10 N11 114.3(8) . . ? C36 N10 Dy3 130.9(6) . . ? N11 N10 Dy3 113.8(6) . . ? C37 N11 N10 115.7(8) . . ? C37 N11 H11H 122.1 . . ? N10 N11 H11H 122.1 . . ? C40 N12 C41 117.6(9) . . ? C57 N13 N14 115.0(9) . . ? C57 N13 Dy3 132.0(7) . . ? N14 N13 Dy3 113.0(7) . . ? C58 N14 N13 117.2(10) . . ? C58 N14 H14B 121.4 . . ? N13 N14 H14B 121.4 . . ? C62 N15 C61 116.2(11) . . ? C50 N16 N17 113.4(9) . . ? C50 N16 Dy2 130.7(6) . . ? N17 N16 Dy2 114.9(7) . . ? C51 N17 N16 116.5(10) . . ? C51 N17 H17A 121.8 . . ? N16 N17 H17A 121.8 . . ? C55 N18 C54 121.0(12) . . ? C71 N19 N20 115.8(9) . . ? C71 N19 Dy1 130.8(7) . . ? N20 N19 Dy1 112.3(6) . . ? C72 N20 N19 115.8(9) . . ? C72 N20 H20B 122.1 . . ? N19 N20 H20B 122.1 . . ? C75 N21 C76 122.6(17) . . ? C78 N22 N23 114.5(8) . . ? C78 N22 Dy4 131.7(6) . . ? N23 N22 Dy4 113.6(6) . . ? C79 N23 N22 114.9(9) . . ? C79 N23 H23A 122.6 . . ? N22 N23 H23A 122.6 . . ? C82 N24 C83 117.7(10) . . ? C85 N25 C86 121.3(16) . . ? C85 N25 C87 120.6(15) . . ? C86 N25 C87 118.1(14) . . ? C90 N26 C88 120.7(19) . . ? C90 N26 C89 125(2) . . ? C88 N26 C89 114.1(15) . . ? C93 N27 C91 111.5(15) . . ? C93 N27 C92 119.0(14) . . ? C91 N27 C92 129.5(13) . . ? C96 N28 C95 122(2) . . ? C96 N28 C94 115(2) . . ? C95 N28 C94 122.9(14) . . ? C3 O1 Dy2 146.3(7) . . ? C16 O2 Dy2 119.3(6) . . ? C7 O5 Dy4 144.7(6) . . ? C9 O6 Dy4 121.4(6) . . ? C28 O9 Dy1 146.5(7) . . ? C30 O10 Dy1 119.0(6) . . ? C24 O13 Dy3 145.6(6) . . ? C37 O14 Dy3 119.3(6) . . ? C58 O17 Dy3 118.1(7) . . ? C45 O18 Dy3 146.0(6) . . ? C49 O19 Dy2 142.8(6) . . ? C51 O20 Dy2 120.6(7) . . ? C79 O21 Dy4 117.5(6) . . ? C66 O22 Dy4 147.7(6) . . ? C70 O23 Dy1 144.2(6) . . ? C72 O24 Dy1 120.6(7) . . ? N31 C101 H10A 109.5 . . ? N31 C101 H10B 109.5 . . ? H10A C101 H10B 109.5 . . ? N31 C101 H10C 109.5 . . ? H10A C101 H10C 109.5 . . ? H10B C101 H10C 109.5 . . ? N31 C102 H10D 109.5 . . ? N31 C102 H10E 109.5 . . ? H10D C102 H10E 109.5 . . ? N31 C102 H10F 109.5 . . ? H10D C102 H10F 109.5 . . ? H10E C102 H10F 109.5 . . ? O33 C103 N31 113.2(15) . . ? O33 C103 H103 123.4 . . ? N31 C103 H103 123.4 . . ? C101 N31 C102 121.8(13) . . ? C101 N31 C103 118.9(10) . . ? C102 N31 C103 119.2(10) . . ? C120 N41 C119 130(5) . . ? C120 N41 C118 109(5) . . ? C119 N41 C118 121.5(14) . . ? N41 C119 H11B 109.5 . . ? N41 C119 H11C 109.5 . . ? H11B C119 H11C 109.5 . . ? N41 C119 H11D 109.5 . . ? H11B C119 H11D 109.5 . . ? H11C C119 H11D 109.5 . . ? N41 C118 H11E 109.5 . . ? N41 C118 H11F 109.5 . . ? H11E C118 H11F 109.5 . . ? N41 C118 H11G 109.5 . . ? H11E C118 H11G 109.5 . . ? H11F C118 H11G 109.5 . . ? N41 C120 O35 121.5(15) . . ? N41 C120 H120 119.3 . . ? O35 C120 H120 119.3 . . ? N30 N32 N33 164(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.625 _refine_diff_density_min -1.335 _refine_diff_density_rms 0.155 data_2 _database_code_depnum_ccdc_archive 'CCDC 912203' #TrackingRef '17648_web_deposit_cif_file_0_Hui-ZhongKou_1360546996.kou-rev.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C99 H147 Cl2 N29 O37 Tb4' _chemical_formula_weight 3042.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 50.118(7) _cell_length_b 22.465(3) _cell_length_c 35.211(5) _cell_angle_alpha 90.00 _cell_angle_beta 133.025(2) _cell_angle_gamma 90.00 _cell_volume 28983(7) _cell_formula_units_Z 8 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 47910 _cell_measurement_theta_min 2.1268 _cell_measurement_theta_max 29.1226 _exptl_crystal_description Chunk _exptl_crystal_colour 'red orange' _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.394 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 12272 _exptl_absorpt_coefficient_mu 2.041 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7691 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Higashi, T. (1995)' _exptl_special_details ; Higashi, T. (1995). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _diffrn_ambient_temperature 143(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Saturn724+ (2x2 bin mode)' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_decay_% ? _diffrn_reflns_number 104509 _diffrn_reflns_av_R_equivalents 0.0563 _diffrn_reflns_av_sigmaI/netI 0.0572 _diffrn_reflns_limit_h_min -61 _diffrn_reflns_limit_h_max 61 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 26.00 _reflns_number_total 28422 _reflns_number_gt 24333 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1990)' _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. There presents site disorder in one pyridine group of the ligand, and occupancies have been set as 0.6:0.4 during the structural refinement. The DMF solvent molecules are not stable and show high temperature factors, and the occupancies of the atoms have been set as half of the original values. Some pyridine groups and DMF molecules undergo site disorder,and therefore, constraints of planarity (command FLAT) and bond distances have been used. The formula of the complex was confirmed by the micro-elementary analyses. Due to the weak diffraction of the crystal, the methanol solvents and the azide anions cannot be completely found from the difference Fourier map. The SQUEEZE function of PLATON was applied, giving available voids of 3443.4 \%A^3^. The corresponding residual electron counts were 2609 e- per unit cell, which should correspond to the missing solvent molecules and the azides. ; _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^)+(0.0910P)^2^+685.9863P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 28422 _refine_ls_number_parameters 1559 _refine_ls_number_restraints 59 _refine_ls_R_factor_all 0.0972 _refine_ls_R_factor_gt 0.0852 _refine_ls_wR_factor_ref 0.2267 _refine_ls_wR_factor_gt 0.2184 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 Tb1 Tb 0.562314(11) 0.14873(2) 0.178091(16) 0.03928(13) Uani 1 1 d . . . Tb2 Tb 0.802782(12) 0.13515(2) 0.471334(18) 0.04402(13) Uani 1 1 d . . . Tb3 Tb 0.880401(11) 0.14982(2) 0.301433(16) 0.03746(12) Uani 1 1 d . . . Tb4 Tb 0.640584(11) 0.12084(2) 0.010167(16) 0.03454(12) Uani 1 1 d . . . Cl1 Cl 0.7862(3) -0.0893(5) 0.2057(4) 0.090(3) Uani 0.50 1 d P . . Cl1A Cl 0.8096(4) -0.0966(6) 0.2264(6) 0.126(4) Uani 0.50 1 d P . . Cl2 Cl 0.6422(2) -0.0982(3) 0.2675(3) 0.175(3) Uani 1 1 d . . . C1 C 0.5832(3) 0.1992(5) 0.0663(4) 0.049(2) Uani 1 1 d . . . H1A H 0.5713 0.2152 0.0766 0.074 Uiso 1 1 calc R . . H1B H 0.5662 0.1968 0.0291 0.074 Uiso 1 1 calc R . . H1C H 0.6031 0.2247 0.0785 0.074 Uiso 1 1 calc R . . C2 C 0.5979(2) 0.1366(4) 0.0897(4) 0.038(2) Uani 1 1 d . . . C3 C 0.5921(2) 0.1115(4) 0.1199(3) 0.0350(19) Uani 1 1 d . . . C4 C 0.6079(2) 0.0534(5) 0.1435(4) 0.044(2) Uani 1 1 d . . . C5 C 0.6262(3) 0.0233(5) 0.1325(4) 0.046(2) Uani 1 1 d . . . H5A H 0.6359 -0.0141 0.1471 0.055 Uiso 1 1 calc R . . C6 C 0.6306(3) 0.0469(5) 0.1002(4) 0.043(2) Uani 1 1 d . . . C7 C 0.6168(2) 0.1056(4) 0.0792(4) 0.039(2) Uani 1 1 d . . . C8 C 0.6054(3) 0.0253(5) 0.1780(4) 0.048(3) Uani 1 1 d . . . H8A H 0.6172 -0.0110 0.1924 0.058 Uiso 1 1 calc R . . C9 C 0.5733(3) 0.0337(7) 0.2396(4) 0.078(5) Uani 1 1 d . . . C10 C 0.6501(3) 0.0113(4) 0.0918(4) 0.044(2) Uani 1 1 d . . . H10A H 0.6596 -0.0250 0.1090 0.052 Uiso 1 1 calc R . . C11 C 0.6782(2) -0.0042(4) 0.0264(4) 0.040(2) Uani 1 1 d . . . C12 C 0.7023(3) -0.0459(4) 0.0277(4) 0.045(2) Uani 1 1 d . . . C13 C 0.7337(3) -0.0707(5) 0.0732(5) 0.052(3) Uani 1 1 d . . . H13A H 0.7404 -0.0627 0.1047 0.062 Uiso 1 1 calc R . . C14 C 0.6933(3) -0.0584(5) -0.0196(5) 0.056(3) Uani 1 1 d . . . H14 H 0.6728 -0.0419 -0.0511 0.068 Uiso 1 1 calc R . . C15 C 0.8594(3) 0.2075(5) 0.4121(5) 0.056(3) Uani 1 1 d . . . H15A H 0.8714 0.2224 0.4015 0.084 Uiso 1 1 calc R . . H15B H 0.8764 0.2067 0.4494 0.084 Uiso 1 1 calc R . . H15C H 0.8393 0.2330 0.3989 0.084 Uiso 1 1 calc R . . C16 C 0.8456(3) 0.1457(5) 0.3912(4) 0.045(2) Uani 1 1 d . . . C17 C 0.8274(3) 0.1156(5) 0.4030(4) 0.045(2) Uani 1 1 d . . . C18 C 0.8138(3) 0.0559(5) 0.3834(4) 0.045(2) Uani 1 1 d . . . C19 C 0.8197(3) 0.0298(5) 0.3541(4) 0.052(3) Uani 1 1 d . . . H19A H 0.8111 -0.0086 0.3417 0.062 Uiso 1 1 calc R . . C20 C 0.8377(2) 0.0581(4) 0.3424(4) 0.041(2) Uani 1 1 d . . . C21 C 0.8524(2) 0.1168(4) 0.3627(4) 0.040(2) Uani 1 1 d . . . C22 C 0.8408(2) 0.0268(5) 0.3093(4) 0.044(2) Uani 1 1 d . . . H22A H 0.8309 -0.0112 0.2983 0.053 Uiso 1 1 calc R . . C23 C 0.8687(3) 0.0280(6) 0.2428(4) 0.064(3) Uani 1 1 d . . . C24 C 0.7948(3) 0.0231(5) 0.3935(4) 0.051(2) Uani 1 1 d . . . H24A H 0.7860 -0.0142 0.3780 0.061 Uiso 1 1 calc R . . C25 C 0.7665(3) 0.0086(5) 0.4597(5) 0.054(3) Uani 1 1 d . . . C26 C 0.7433(3) -0.0355(5) 0.4593(5) 0.056(3) Uani 1 1 d . . . C27 C 0.7131(3) -0.0616(6) 0.4147(5) 0.062(3) Uani 1 1 d . . . H27A H 0.7066 -0.0541 0.3833 0.075 Uiso 1 1 calc R . . C28 C 0.6737(3) 0.0816(5) 0.3419(4) 0.062(3) Uani 1 1 d . . . H28A H 0.6485 0.0709 0.3149 0.092 Uiso 1 1 calc R . . H28B H 0.6807 0.0796 0.3749 0.092 Uiso 1 1 calc R . . H28C H 0.6884 0.0544 0.3417 0.092 Uiso 1 1 calc R . . C29 C 0.6794(3) 0.1440(5) 0.3329(4) 0.045(2) Uani 1 1 d . . . C30 C 0.7148(2) 0.1695(5) 0.3678(3) 0.040(2) Uani 1 1 d . . . C31 C 0.7197(2) 0.2281(5) 0.3578(4) 0.042(2) Uani 1 1 d . . . C32 C 0.6899(2) 0.2576(5) 0.3127(4) 0.045(2) Uani 1 1 d . . . H32A H 0.6934 0.2954 0.3059 0.054 Uiso 1 1 calc R . . C33 C 0.6552(3) 0.2326(5) 0.2774(4) 0.047(2) Uani 1 1 d . . . C34 C 0.6499(2) 0.1748(5) 0.2885(4) 0.043(2) Uani 1 1 d . . . C35 C 0.6267(3) 0.2643(5) 0.2307(3) 0.045(2) Uani 1 1 d . . . H35A H 0.6328 0.3014 0.2267 0.055 Uiso 1 1 calc R . . C36 C 0.5373(3) 0.2692(5) 0.1106(4) 0.046(2) Uani 1 1 d . . . C37 C 0.5155(3) 0.3067(5) 0.0621(4) 0.048(2) Uani 1 1 d . . . C38 C 0.5323(4) 0.3352(6) 0.0475(5) 0.066(3) Uani 1 1 d . . . H38A H 0.5574 0.3335 0.0680 0.079 Uiso 1 1 calc R . . C39 C 0.4785(3) 0.3080(5) 0.0300(4) 0.058(3) Uani 1 1 d . . . H39A H 0.4669 0.2891 0.0389 0.070 Uiso 1 1 calc R . . C40 C 0.7546(2) 0.2589(5) 0.3902(4) 0.045(2) Uani 1 1 d . . . H40A H 0.7552 0.2959 0.3790 0.054 Uiso 1 1 calc R . . C41 C 0.8456(3) 0.2588(5) 0.5008(4) 0.048(3) Uani 1 1 d . . . C42 C 0.8784(3) 0.2977(5) 0.5273(4) 0.050(3) Uani 1 1 d . . . C43 C 0.8758(3) 0.3600(6) 0.5234(5) 0.059(3) Uani 1 1 d . . . H43A H 0.8532 0.3787 0.5033 0.071 Uiso 1 1 calc R . . C44 C 0.9130(3) 0.2731(6) 0.5582(5) 0.067(3) Uani 1 1 d . . . H44A H 0.9162 0.2321 0.5626 0.080 Uiso 1 1 calc R . . C45 C 0.7702(3) 0.0749(5) 0.1403(4) 0.049(2) Uani 1 1 d . . . H45A H 0.7871 0.0764 0.1359 0.074 Uiso 1 1 calc R . . H45B H 0.7476 0.0578 0.1099 0.074 Uiso 1 1 calc R . . H45C H 0.7802 0.0511 0.1701 0.074 Uiso 1 1 calc R . . C46 C 0.7633(2) 0.1372(4) 0.1481(4) 0.040(2) Uani 1 1 d . . . C47 C 0.7925(2) 0.1694(5) 0.1920(3) 0.042(2) Uani 1 1 d . . . C48 C 0.7863(3) 0.2286(5) 0.2022(4) 0.046(2) Uani 1 1 d . . . C49 C 0.7504(3) 0.2511(5) 0.1665(4) 0.055(3) Uani 1 1 d . . . H49A H 0.7460 0.2884 0.1727 0.066 Uiso 1 1 calc R . . C50 C 0.7211(2) 0.2195(5) 0.1221(4) 0.047(2) Uani 1 1 d . . . C51 C 0.7273(2) 0.1607(4) 0.1123(4) 0.041(2) Uani 1 1 d . . . C52 C 0.6863(3) 0.2490(5) 0.0877(4) 0.052(3) Uani 1 1 d . . . H52A H 0.6849 0.2866 0.0972 0.063 Uiso 1 1 calc R . . C53 C 0.5952(2) 0.2449(5) -0.0257(3) 0.042(2) Uani 1 1 d . . . C54 C 0.5623(3) 0.2843(5) -0.0546(4) 0.048(2) Uani 1 1 d . . . C55 C 0.5643(3) 0.3459(6) -0.0536(5) 0.068(3) Uani 1 1 d . . . H55A H 0.5866 0.3653 -0.0345 0.082 Uiso 1 1 calc R . . C56 C 0.5285(3) 0.2582(5) -0.0834(4) 0.054(3) Uani 1 1 d . . . H56A H 0.5262 0.2170 -0.0859 0.065 Uiso 1 1 calc R . . C57 C 0.8135(3) 0.2632(5) 0.2468(4) 0.053(3) Uani 1 1 d . . . H57A H 0.8065 0.3000 0.2497 0.064 Uiso 1 1 calc R . . C58 C 0.9038(2) 0.2735(5) 0.3655(4) 0.041(2) Uani 1 1 d . . . C59 C 0.9257(3) 0.3124(5) 0.4125(4) 0.044(2) Uani 1 1 d . . . C60 C 0.9108(3) 0.3518(6) 0.4250(4) 0.065(4) Uani 1 1 d . . . H60A H 0.8857 0.3578 0.4019 0.078 Uiso 1 1 calc R . . C62 C 0.7548(3) -0.1074(6) 0.0716(5) 0.058(3) Uani 1 1 d . . . H62A H 0.7758 -0.1238 0.1025 0.070 Uiso 1 1 calc R . . C63 C 0.7168(3) -0.0968(5) -0.0165(5) 0.059(3) Uani 1 1 d . . . H63A H 0.7112 -0.1061 -0.0470 0.071 Uiso 1 1 calc R . . C64 C 0.6925(4) -0.0991(6) 0.4167(5) 0.065(3) Uani 1 1 d . . . H64A H 0.6717 -0.1160 0.3858 0.078 Uiso 1 1 calc R . . C65 C 0.7298(4) -0.0878(6) 0.5028(6) 0.072(4) Uani 1 1 d . . . H65A H 0.7362 -0.0974 0.5339 0.086 Uiso 1 1 calc R . . C66 C 0.7517(4) -0.0481(6) 0.5040(6) 0.067(3) Uani 1 1 d . . . H66A H 0.7719 -0.0305 0.5351 0.081 Uiso 1 1 calc R . . C67 C 0.8634(3) -0.0133(7) 0.2042(4) 0.094(6) Uani 1 1 d D . . C70 C 0.5093(4) 0.3664(6) 0.0007(4) 0.067(3) Uani 1 1 d . . . H70A H 0.5201 0.3878 -0.0084 0.080 Uiso 1 1 calc R . . C71 C 0.4584(3) 0.3393(6) -0.0173(4) 0.065(3) Uani 1 1 d . . . H71A H 0.4331 0.3398 -0.0397 0.078 Uiso 1 1 calc R . . C72 C 0.9079(3) 0.3937(6) 0.5504(5) 0.066(3) Uani 1 1 d . . . H72A H 0.9058 0.4349 0.5473 0.079 Uiso 1 1 calc R . . C73 C 0.9430(3) 0.3110(6) 0.5829(6) 0.078(4) Uani 1 1 d . . . H73A H 0.9659 0.2937 0.6025 0.094 Uiso 1 1 calc R . . C74 C 0.5316(3) 0.3776(6) -0.0823(5) 0.076(4) Uani 1 1 d . . . H74A H 0.5328 0.4189 -0.0823 0.091 Uiso 1 1 calc R . . C75 C 0.4985(3) 0.2937(6) -0.1085(5) 0.069(3) Uani 1 1 d . . . H75A H 0.4761 0.2752 -0.1260 0.083 Uiso 1 1 calc R . . C76 C 0.9339(4) 0.3812(7) 0.4718(5) 0.081(4) Uani 1 1 d . . . H76A H 0.9235 0.4064 0.4796 0.097 Uiso 1 1 calc R . . C77 C 0.9830(3) 0.3394(5) 0.4945(4) 0.052(3) Uani 1 1 d . . . H77A H 1.0083 0.3356 0.5189 0.063 Uiso 1 1 calc R . . C78 C 0.9637(3) 0.3064(5) 0.4501(4) 0.050(2) Uani 1 1 d . . . H78A H 0.9755 0.2806 0.4449 0.060 Uiso 1 1 calc R . . C83 C 0.7144(10) 0.057(2) 0.2597(14) 0.32(2) Uiso 1 1 d D . . H83A H 0.7135 0.0185 0.2706 0.476 Uiso 1 1 calc R . . H83B H 0.6904 0.0743 0.2363 0.476 Uiso 1 1 calc R . . H83C H 0.7307 0.0823 0.2895 0.476 Uiso 1 1 calc R . . C84 C 0.7346(7) 0.0869(14) 0.2072(11) 0.207(14) Uani 1 1 d D . . H84A H 0.7445 0.0621 0.1971 0.310 Uiso 1 1 calc R . . H84B H 0.7518 0.1176 0.2301 0.310 Uiso 1 1 calc R . . H84C H 0.7123 0.1047 0.1768 0.310 Uiso 1 1 calc R . . C85 C 0.7300(5) -0.0060(11) 0.2301(8) 0.166(10) Uiso 1 1 d D . . H85A H 0.7379 -0.0200 0.2143 0.199 Uiso 1 1 calc R . . C87 C 0.7070(11) 0.3465(18) 0.205(2) 0.76(9) Uiso 1 1 d D . . H87A H 0.7284 0.3689 0.2251 0.911 Uiso 1 1 calc R . . C89 C 0.7401(6) 0.2603(13) 0.2641(8) 0.170(12) Uani 1 1 d D . . H89A H 0.7600 0.2879 0.2855 0.255 Uiso 1 1 calc R . . H89B H 0.7466 0.2286 0.2535 0.255 Uiso 1 1 calc R . . H89C H 0.7346 0.2442 0.2835 0.255 Uiso 1 1 calc R . . C90 C 0.8580(5) -0.0729(8) 0.2025(7) 0.227(19) Uani 1 1 d D . . H90A H 0.8572 -0.0902 0.2257 0.272 Uiso 1 1 calc R . . C91 C 0.8539(7) -0.1070(9) 0.1673(9) 0.29(3) Uani 1 1 d D . . H91A H 0.8527 -0.1482 0.1680 0.353 Uiso 1 1 calc R . . C92 C 0.8622(10) -0.0246(12) 0.1373(11) 0.268(19) Uiso 1 1 d D . . H92A H 0.8684 -0.0098 0.1195 0.322 Uiso 1 1 calc R . . C93 C 0.8638(7) 0.0106(8) 0.1701(7) 0.203(16) Uani 1 1 d D . . H93A H 0.8651 0.0518 0.1687 0.243 Uiso 1 1 calc R . . C94 C 0.5765(6) 0.0131(10) 0.2833(8) 0.049(6) Uani 0.51(2) 1 d P . . C95 C 0.6043(9) -0.0277(17) 0.3192(12) 0.100(15) Uani 0.51(2) 1 d P . . C96 C 0.6026(5) -0.0421(9) 0.3593(6) 0.098(5) Uani 1 1 d . . . C97 C 0.5549(7) 0.0098(14) 0.3274(10) 0.078(9) Uani 0.51(2) 1 d P . . C98 C 0.5518(7) 0.0315(12) 0.2870(9) 0.061(7) Uani 0.51(2) 1 d P . . C94A C 0.5811(8) -0.0208(14) 0.2783(10) 0.069(9) Uani 0.49(2) 1 d P . . C95A C 0.5922(8) 0.006(2) 0.3234(8) 0.108(18) Uani 0.49(2) 1 d P . . C97A C 0.5865(11) -0.1167(18) 0.3116(15) 0.123(16) Uani 0.49(2) 1 d P . . C98A C 0.5798(10) -0.0817(16) 0.2733(12) 0.100(13) Uani 0.49(2) 1 d P . . C99 C 0.4724(6) 0.4838(10) 0.0240(9) 0.252(17) Uiso 1 1 d D . . H99A H 0.4850 0.4943 0.0142 0.303 Uiso 1 1 calc R . . C100 C 0.4150(8) 0.4675(13) 0.0024(11) 0.194(12) Uiso 1 1 d D . . H10B H 0.4309 0.4575 0.0385 0.290 Uiso 1 1 calc R . . H10C H 0.4006 0.4334 -0.0183 0.290 Uiso 1 1 calc R . . H10D H 0.3993 0.4996 -0.0056 0.290 Uiso 1 1 calc R . . C101 C 0.4270(7) 0.5041(12) -0.0565(8) 0.28(2) Uani 1 1 d D . . H10E H 0.4487 0.5113 -0.0498 0.417 Uiso 1 1 calc R . . H10F H 0.4128 0.5400 -0.0689 0.417 Uiso 1 1 calc R . . H10G H 0.4129 0.4734 -0.0822 0.417 Uiso 1 1 calc R . . C104 C 0.5383(5) 0.0451(12) -0.0293(7) 0.159(10) Uani 1 1 d D . . H10H H 0.5501 0.0612 -0.0400 0.239 Uiso 1 1 calc R . . H10I H 0.5429 0.0031 -0.0235 0.239 Uiso 1 1 calc R . . H10J H 0.5478 0.0642 0.0022 0.239 Uiso 1 1 calc R . . C105 C 0.4735(7) 0.0289(14) -0.0688(14) 0.32(3) Uani 1 1 d D . . H10K H 0.4493 0.0428 -0.0982 0.487 Uiso 1 1 calc R . . H10L H 0.4795 0.0399 -0.0374 0.487 Uiso 1 1 calc R . . H10M H 0.4743 -0.0136 -0.0705 0.487 Uiso 1 1 calc R . . N1 N 0.5884(2) 0.0455(4) 0.1903(3) 0.044(2) Uani 1 1 d . . . N2 N 0.5905(2) 0.0106(5) 0.2248(3) 0.061(3) Uani 1 1 d . . . H2 H 0.6017 -0.0230 0.2362 0.074 Uiso 1 1 calc R . . N3 N 0.6554(2) 0.0273(4) 0.0615(3) 0.0400(17) Uani 1 1 d . . . N4 N 0.6762(2) -0.0142(4) 0.0608(3) 0.0448(19) Uani 1 1 d . . . H4 H 0.6868 -0.0441 0.0816 0.054 Uiso 1 1 calc R . . N5 N 0.8561(2) 0.0474(4) 0.2939(3) 0.0419(18) Uani 1 1 d . . . N6 N 0.8531(2) 0.0091(4) 0.2600(3) 0.052(2) Uani 1 1 d . . . H6 H 0.8420 -0.0245 0.2506 0.062 Uiso 1 1 calc R . . N7 N 0.7884(2) 0.0394(4) 0.4218(4) 0.051(2) Uani 1 1 d . . . N8 N 0.7678(3) -0.0015(4) 0.4233(4) 0.058(2) Uani 1 1 d . . . H8 H 0.7567 -0.0311 0.4022 0.070 Uiso 1 1 calc R . . N9 N 0.5939(2) 0.2468(4) 0.1939(3) 0.0427(18) Uani 1 1 d . . . N10 N 0.5726(2) 0.2848(4) 0.1504(3) 0.048(2) Uani 1 1 d . . . H10 H 0.5815 0.3166 0.1492 0.058 Uiso 1 1 calc R . . N11 N 0.78490(19) 0.2388(4) 0.4333(3) 0.0423(19) Uani 1 1 d . . . N12 N 0.8144(2) 0.2776(4) 0.4568(3) 0.048(2) Uani 1 1 d . . . H12 H 0.8122 0.3113 0.4434 0.057 Uiso 1 1 calc R . . N13 N 0.6568(2) 0.2272(4) 0.0447(3) 0.0425(18) Uani 1 1 d . . . N14 N 0.6266(2) 0.2654(4) 0.0180(3) 0.050(2) Uani 1 1 d . . . H14A H 0.6284 0.3004 0.0295 0.060 Uiso 1 1 calc R . . N15 N 0.8476(2) 0.2476(4) 0.2842(3) 0.0435(18) Uani 1 1 d . . . N16 N 0.8683(2) 0.2869(4) 0.3255(3) 0.0435(19) Uani 1 1 d . . . H16 H 0.8589 0.3188 0.3256 0.052 Uiso 1 1 calc R . . N17 N 0.7463(3) -0.1205(4) 0.0271(4) 0.062(3) Uani 1 1 d . . . N18 N 0.4992(3) 0.3534(5) -0.1093(4) 0.070(3) Uani 1 1 d . . . N19 N 0.4731(3) 0.3679(5) -0.0319(4) 0.065(3) Uani 1 1 d . . . N20 N 0.9685(2) 0.3763(5) 0.5052(3) 0.060(3) Uani 1 1 d . . . N21 N 0.9410(2) 0.3699(5) 0.5802(4) 0.068(3) Uani 1 1 d . . . N22 N 0.7002(3) -0.1124(4) 0.4595(5) 0.068(3) Uani 1 1 d . . . N23 N 0.7273(4) 0.0510(10) 0.2336(7) 0.41(3) Uani 1 1 d D . . N28 N 0.8517(5) -0.0806(11) 0.1313(5) 0.225(14) Uani 1 1 d D . . N29 N 0.5821(6) -0.0295(11) 0.3622(8) 0.094(7) Uani 0.60 1 d P . . N29A N 0.5949(8) -0.0959(13) 0.3526(10) 0.069(7) Uani 0.40 1 d P . . N30 N 0.4368(5) 0.4855(7) -0.0089(7) 0.180(10) Uani 1 1 d D . . N31 N 0.4994(5) 0.0555(10) -0.0696(9) 0.196(10) Uiso 1 1 d D . . O1 O 0.57265(18) 0.1392(3) 0.1263(3) 0.0420(15) Uani 1 1 d . . . O2 O 0.5553(2) 0.0789(4) 0.2217(3) 0.064(2) Uani 1 1 d . . . O3 O 0.62001(18) 0.1298(3) 0.0487(3) 0.0422(15) Uani 1 1 d . . . O4 O 0.66174(18) 0.0375(3) -0.0065(3) 0.0459(16) Uani 1 1 d . . . O5 O 0.87128(18) 0.1439(3) 0.3550(3) 0.0447(16) Uani 1 1 d . . . O6 O 0.8858(2) 0.0758(4) 0.2567(3) 0.0553(19) Uani 1 1 d . . . O7 O 0.8232(2) 0.1423(3) 0.4318(3) 0.0556(19) Uani 1 1 d . . . O8 O 0.78227(19) 0.0501(4) 0.4906(3) 0.057(2) Uani 1 1 d . . . O9 O 0.61762(18) 0.1507(3) 0.2578(2) 0.0513(19) Uani 1 1 d . . . O10 O 0.52349(17) 0.2247(3) 0.1130(3) 0.0459(16) Uani 1 1 d . . . O11 O 0.74251(17) 0.1409(3) 0.4099(3) 0.0493(17) Uani 1 1 d . . . O12 O 0.84972(18) 0.2100(4) 0.5218(3) 0.056(2) Uani 1 1 d . . . O13 O 0.70085(16) 0.1302(3) 0.0724(2) 0.0442(16) Uani 1 1 d . . . O14 O 0.59182(16) 0.1942(3) -0.0433(2) 0.0437(16) Uani 1 1 d . . . O15 O 0.82508(17) 0.1473(3) 0.2227(3) 0.0501(18) Uani 1 1 d . . . O16 O 0.91840(16) 0.2297(3) 0.3639(2) 0.0449(16) Uani 1 1 d . . . O17 O 0.7215(6) -0.0432(10) 0.2487(7) 0.246(12) Uani 1 1 d D . . O18 O 0.4895(5) 0.4668(8) 0.0707(8) 0.280(15) Uani 1 1 d D . . O1W O 0.50589(15) 0.0962(3) 0.1097(2) 0.0409(15) Uani 1 1 d . . . O2W O 0.5354(2) 0.2002(5) 0.2043(3) 0.080(3) Uani 1 1 d . . . O3W O 0.8578(2) 0.0835(5) 0.5429(4) 0.105(4) Uani 1 1 d . . . O4W O 0.7970(3) 0.1711(5) 0.5302(4) 0.081(3) Uani 1 1 d . . . O5W O 0.93843(16) 0.1017(3) 0.3690(2) 0.0434(15) Uani 1 1 d . . . O6W O 0.9061(2) 0.2005(4) 0.2724(3) 0.067(2) Uani 1 1 d . . . O7W O 0.6449(2) 0.1589(3) -0.0493(3) 0.0528(18) Uani 1 1 d . . . O8W O 0.58591(19) 0.0673(3) -0.0602(3) 0.057(2) Uani 1 1 d . . . O9W O 0.7281(8) -0.0876(8) 0.3345(14) 0.34(2) Uani 1 1 d . . . O10W O 0.6778(3) -0.1281(6) 0.1801(5) 0.165(8) Uani 1 1 d . . . O11W O 0.6121(4) 0.3837(6) 0.1597(4) 0.146(6) Uani 1 1 d . . . O12W O 0.9354(4) -0.0271(7) 0.3599(7) 0.187(8) Uani 1 1 d . . . O13W O 0.6923(3) -0.1307(4) 0.1112(3) 0.074(3) Uani 1 1 d . . . O14W O 0.9228(6) 0.3156(9) 0.2923(9) 0.096(7) Uani 0.50 1 d P . . O15W O 0.9330(11) 0.1176(15) 0.614(2) 0.23(2) Uani 0.50 1 d P . . O16W O 1.0031(13) 0.168(2) 0.6678(19) 0.24(2) Uiso 0.50 1 d P . . O17W O 0.6504(16) 0.349(3) -0.042(2) 0.27(2) Uiso 0.50 1 d P . . O18W O 0.6337(5) 0.3723(8) 0.0799(7) 0.164(6) Uiso 1 1 d . . . C103 C 0.4932(8) 0.0835(13) -0.1075(10) 0.30(2) Uiso 1 1 d D . . H10N H 0.4695 0.0947 -0.1368 0.363 Uiso 1 1 calc R . . N27 N 0.7080(7) 0.2912(15) 0.2183(9) 0.304(18) Uiso 1 1 d D . . O19 O 0.5199(12) 0.0959(16) -0.1045(16) 0.44(3) Uiso 1 1 d D . . C88 C 0.6779(9) 0.2491(14) 0.1869(12) 0.212(14) Uiso 1 1 d D . . H88A H 0.6565 0.2689 0.1568 0.317 Uiso 1 1 calc R . . H88B H 0.6730 0.2334 0.2071 0.317 Uiso 1 1 calc R . . H88C H 0.6842 0.2171 0.1763 0.317 Uiso 1 1 calc R . . C109 C 0.8237(9) 0.1872(14) 0.1256(12) 0.17(3) Uani 0.50 1 d PD . . H10O H 0.8071 0.1658 0.0934 0.259 Uiso 0.50 1 calc PR . . H10P H 0.8300 0.1631 0.1532 0.259 Uiso 0.50 1 calc PR . . H10Q H 0.8454 0.1965 0.1326 0.259 Uiso 0.50 1 calc PR . . C108 C 0.8269(10) 0.2820(13) 0.1655(13) 0.120(13) Uiso 0.50 1 d PD . . H10R H 0.8115 0.3147 0.1579 0.181 Uiso 0.50 1 calc PR . . H10S H 0.8477 0.2968 0.1721 0.181 Uiso 0.50 1 calc PR . . H10T H 0.8349 0.2612 0.1957 0.181 Uiso 0.50 1 calc PR . . C107 C 0.7728(7) 0.2556(14) 0.0837(10) 0.19(3) Uani 0.50 1 d PD . . H10U H 0.7589 0.2307 0.0548 0.225 Uiso 0.50 1 calc PR . . O23 O 0.7568(10) 0.3017(17) 0.0829(16) 0.24(2) Uiso 0.50 1 d PD . . O24 O 0.5493(7) 0.1850(12) 0.2911(17) 0.27(3) Uani 0.50 1 d PD . . N32 N 0.8066(7) 0.2418(11) 0.1219(9) 0.131(15) Uani 0.50 1 d PD . . N33 N 0.6062(8) 0.2230(16) 0.3495(10) 0.115(11) Uani 0.50 1 d PD . . C115 C 0.5845(8) 0.1781(14) 0.3239(14) 0.18(2) Uiso 0.50 1 d PD . . H11J H 0.5941 0.1405 0.3291 0.221 Uiso 0.50 1 calc PR . . C116 C 0.6435(11) 0.202(3) 0.384(2) 0.23(3) Uiso 0.50 1 d PD . . H11D H 0.6597 0.2345 0.3949 0.342 Uiso 0.50 1 calc PR . . H11E H 0.6458 0.1729 0.3663 0.342 Uiso 0.50 1 calc PR . . H11F H 0.6499 0.1835 0.4140 0.342 Uiso 0.50 1 calc PR . . C117 C 0.591(3) 0.281(2) 0.344(3) 0.35(6) Uiso 0.50 1 d PD . . H11G H 0.5650 0.2793 0.3173 0.527 Uiso 0.50 1 calc PR . . H11H H 0.5998 0.3098 0.3340 0.527 Uiso 0.50 1 calc PR . . H11I H 0.5987 0.2928 0.3761 0.527 Uiso 0.50 1 calc PR . . O22 O 0.6761(11) 0.3701(15) 0.1641(15) 0.41(2) Uiso 1 1 d 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 0.0235(2) 0.0712(3) 0.0237(2) -0.00390(19) 0.01633(18) -0.00617(19) Tb2 0.0243(2) 0.0749(3) 0.0334(2) 0.0010(2) 0.0199(2) -0.0077(2) Tb3 0.0229(2) 0.0610(3) 0.0253(2) -0.00095(18) 0.01522(18) 0.00126(18) Tb4 0.0206(2) 0.0543(3) 0.0279(2) -0.00669(18) 0.01622(17) -0.00172(17) Cl1 0.103(7) 0.085(6) 0.085(6) -0.016(5) 0.066(6) -0.019(6) Cl1A 0.114(9) 0.101(8) 0.139(11) -0.028(7) 0.077(9) -0.014(8) Cl2 0.197(7) 0.140(5) 0.167(6) 0.053(5) 0.117(6) 0.046(5) C1 0.060(6) 0.054(6) 0.060(6) 0.012(5) 0.051(6) 0.016(5) C2 0.031(5) 0.049(5) 0.040(5) 0.002(4) 0.027(4) 0.004(4) C3 0.026(4) 0.051(5) 0.032(4) 0.001(4) 0.022(4) 0.005(4) C4 0.030(5) 0.063(6) 0.044(5) 0.011(5) 0.027(4) 0.007(4) C5 0.040(5) 0.053(6) 0.047(6) 0.013(5) 0.030(5) 0.013(4) C6 0.039(5) 0.055(6) 0.049(5) 0.005(4) 0.035(5) 0.010(4) C7 0.030(4) 0.050(5) 0.039(5) -0.001(4) 0.025(4) 0.003(4) C8 0.036(5) 0.059(6) 0.057(6) 0.025(5) 0.034(5) 0.011(4) C9 0.043(6) 0.156(13) 0.023(5) 0.001(6) 0.018(5) -0.045(7) C10 0.035(5) 0.046(5) 0.051(6) 0.005(4) 0.030(5) 0.007(4) C11 0.026(4) 0.045(5) 0.039(5) -0.013(4) 0.019(4) -0.003(4) C12 0.037(5) 0.048(5) 0.057(6) -0.012(5) 0.035(5) -0.002(4) C13 0.034(5) 0.059(6) 0.062(7) -0.006(5) 0.033(5) 0.001(5) C14 0.052(6) 0.065(7) 0.070(7) -0.012(6) 0.049(6) -0.001(5) C15 0.063(7) 0.063(7) 0.066(7) -0.011(6) 0.053(7) -0.012(6) C16 0.039(5) 0.057(6) 0.044(5) 0.004(5) 0.030(5) -0.002(4) C17 0.036(5) 0.065(6) 0.045(5) 0.006(5) 0.032(5) 0.003(5) C18 0.033(5) 0.054(6) 0.054(6) 0.003(5) 0.033(5) 0.004(4) C19 0.050(6) 0.052(6) 0.061(7) -0.008(5) 0.041(6) -0.010(5) C20 0.032(5) 0.051(5) 0.039(5) -0.001(4) 0.023(4) -0.002(4) C21 0.030(5) 0.055(6) 0.037(5) -0.003(4) 0.023(4) -0.001(4) C22 0.028(5) 0.052(6) 0.041(5) -0.008(4) 0.019(4) -0.001(4) C23 0.042(6) 0.099(9) 0.035(5) -0.007(6) 0.020(5) 0.025(6) C24 0.041(5) 0.056(6) 0.058(6) -0.002(5) 0.035(5) -0.006(5) C25 0.050(6) 0.063(7) 0.072(7) 0.025(6) 0.050(6) 0.012(5) C26 0.043(6) 0.064(7) 0.071(7) 0.023(6) 0.043(6) 0.013(5) C27 0.057(7) 0.077(8) 0.077(8) 0.012(7) 0.055(7) 0.001(6) C28 0.031(5) 0.079(8) 0.043(6) 0.015(5) 0.013(5) -0.013(5) C29 0.035(5) 0.062(6) 0.035(5) -0.003(4) 0.023(4) -0.012(4) C30 0.027(4) 0.056(6) 0.029(4) -0.005(4) 0.016(4) -0.006(4) C31 0.032(5) 0.054(6) 0.037(5) -0.011(4) 0.022(4) -0.012(4) C32 0.029(5) 0.052(6) 0.039(5) -0.005(4) 0.017(4) -0.008(4) C33 0.036(5) 0.064(6) 0.035(5) -0.004(5) 0.021(4) -0.011(5) C34 0.029(5) 0.064(6) 0.035(5) -0.002(4) 0.022(4) -0.011(4) C35 0.035(5) 0.062(6) 0.031(5) -0.001(4) 0.019(4) -0.006(4) C36 0.038(5) 0.065(6) 0.031(5) -0.004(4) 0.022(4) 0.004(5) C37 0.048(6) 0.056(6) 0.035(5) -0.001(4) 0.026(5) 0.006(5) C38 0.068(8) 0.066(7) 0.052(7) -0.006(6) 0.037(7) 0.000(6) C39 0.048(6) 0.072(8) 0.044(6) 0.002(5) 0.027(5) 0.011(5) C40 0.030(5) 0.057(6) 0.039(5) -0.009(4) 0.020(4) -0.010(4) C41 0.040(5) 0.072(7) 0.044(5) -0.023(5) 0.033(5) -0.022(5) C42 0.031(5) 0.081(8) 0.045(6) -0.017(5) 0.029(5) -0.015(5) C43 0.026(5) 0.076(8) 0.064(7) -0.023(6) 0.026(5) -0.010(5) C44 0.035(6) 0.081(8) 0.075(8) -0.017(7) 0.034(6) -0.010(6) C45 0.036(5) 0.052(6) 0.042(5) -0.008(5) 0.020(5) 0.003(4) C46 0.019(4) 0.049(5) 0.032(5) -0.005(4) 0.010(4) 0.002(4) C47 0.026(4) 0.052(6) 0.030(4) 0.000(4) 0.013(4) 0.003(4) C48 0.029(5) 0.049(6) 0.037(5) -0.004(4) 0.013(4) 0.003(4) C49 0.035(5) 0.055(6) 0.046(6) -0.010(5) 0.016(5) 0.007(5) C50 0.027(5) 0.054(6) 0.042(5) -0.009(4) 0.016(4) 0.002(4) C51 0.024(4) 0.051(6) 0.036(5) -0.007(4) 0.016(4) -0.004(4) C52 0.029(5) 0.057(6) 0.044(6) -0.008(5) 0.014(5) 0.003(4) C53 0.026(4) 0.064(6) 0.032(5) 0.007(4) 0.019(4) 0.007(4) C54 0.027(5) 0.072(7) 0.037(5) 0.001(5) 0.019(4) 0.009(5) C55 0.033(6) 0.066(8) 0.075(8) 0.005(6) 0.025(6) 0.006(5) C56 0.027(5) 0.070(7) 0.045(6) 0.002(5) 0.017(5) 0.003(5) C57 0.031(5) 0.058(6) 0.045(6) -0.012(5) 0.016(5) -0.005(5) C58 0.032(5) 0.054(6) 0.034(5) -0.009(4) 0.020(4) -0.010(4) C59 0.035(5) 0.057(6) 0.032(5) -0.005(4) 0.020(4) -0.011(4) C60 0.026(5) 0.119(11) 0.023(5) -0.001(6) 0.007(4) 0.016(6) C62 0.048(6) 0.076(8) 0.067(7) 0.000(6) 0.045(6) 0.012(6) C63 0.067(7) 0.055(6) 0.086(9) -0.008(6) 0.064(7) 0.002(6) C64 0.071(8) 0.067(8) 0.081(9) -0.003(7) 0.062(8) -0.009(6) C65 0.080(9) 0.077(9) 0.089(9) 0.003(7) 0.070(9) -0.013(7) C66 0.069(8) 0.071(8) 0.092(9) 0.020(7) 0.067(8) 0.007(6) C67 0.059(8) 0.165(17) 0.043(7) -0.035(9) 0.028(6) 0.015(9) C70 0.061(8) 0.074(8) 0.041(6) 0.003(6) 0.025(6) -0.008(6) C71 0.051(7) 0.077(8) 0.043(6) 0.007(6) 0.022(6) 0.014(6) C72 0.038(6) 0.064(7) 0.073(8) -0.013(6) 0.029(6) -0.011(5) C73 0.033(6) 0.081(9) 0.113(11) -0.014(8) 0.046(7) -0.009(6) C74 0.046(7) 0.069(8) 0.078(9) 0.009(7) 0.028(7) 0.008(6) C75 0.036(6) 0.074(8) 0.073(8) 0.001(7) 0.028(6) 0.008(5) C76 0.056(8) 0.121(12) 0.041(6) -0.016(7) 0.023(6) 0.017(8) C77 0.032(5) 0.066(7) 0.036(5) -0.007(5) 0.015(4) -0.011(5) C78 0.037(5) 0.061(6) 0.043(5) -0.008(5) 0.024(5) -0.004(5) C84 0.18(3) 0.22(3) 0.24(3) 0.08(3) 0.15(3) 0.02(2) C89 0.15(2) 0.30(4) 0.094(14) 0.020(19) 0.096(16) 0.05(2) C90 0.22(3) 0.25(3) 0.34(4) -0.25(3) 0.24(3) -0.16(3) C91 0.23(3) 0.37(5) 0.38(5) -0.29(5) 0.24(4) -0.16(3) C93 0.30(4) 0.25(3) 0.107(16) 0.059(18) 0.16(2) 0.16(3) C94 0.048(12) 0.062(16) 0.039(14) -0.011(12) 0.030(11) -0.024(12) C95 0.10(3) 0.17(4) 0.08(3) 0.07(2) 0.08(2) 0.06(3) C96 0.085(11) 0.139(15) 0.073(10) 0.031(10) 0.056(9) 0.013(10) C97 0.076(18) 0.11(2) 0.053(14) 0.034(14) 0.047(14) 0.004(15) C98 0.065(15) 0.091(18) 0.048(13) 0.005(12) 0.046(13) 0.002(13) C94A 0.08(2) 0.09(2) 0.056(19) -0.023(18) 0.053(18) -0.05(2) C95A 0.061(19) 0.24(5) 0.018(13) -0.010(18) 0.025(13) -0.07(3) C97A 0.14(3) 0.13(3) 0.11(3) 0.09(3) 0.09(3) 0.03(3) C98A 0.15(3) 0.11(3) 0.08(2) 0.000(18) 0.09(2) -0.04(2) C101 0.16(2) 0.19(3) 0.112(19) 0.053(18) -0.057(16) -0.01(2) C104 0.095(14) 0.23(3) 0.081(13) -0.031(15) 0.030(12) -0.051(16) C105 0.14(2) 0.37(5) 0.48(6) -0.31(5) 0.21(3) -0.12(3) N1 0.027(4) 0.067(5) 0.031(4) 0.013(4) 0.016(3) -0.002(4) N2 0.035(4) 0.093(7) 0.044(5) 0.030(5) 0.022(4) 0.000(5) N3 0.029(4) 0.050(5) 0.042(4) -0.002(4) 0.025(4) 0.005(3) N4 0.039(4) 0.046(4) 0.056(5) -0.001(4) 0.035(4) 0.008(4) N5 0.035(4) 0.054(5) 0.032(4) -0.011(3) 0.020(3) 0.000(4) N6 0.042(5) 0.066(6) 0.037(4) -0.013(4) 0.023(4) 0.004(4) N7 0.048(5) 0.057(5) 0.070(6) 0.007(4) 0.049(5) -0.002(4) N8 0.060(6) 0.057(5) 0.082(7) 0.007(5) 0.058(6) -0.004(4) N9 0.034(4) 0.060(5) 0.027(4) -0.001(3) 0.018(3) -0.004(4) N10 0.037(4) 0.059(5) 0.029(4) 0.000(4) 0.015(4) -0.003(4) N11 0.025(4) 0.062(5) 0.038(4) -0.017(4) 0.021(3) -0.013(3) N12 0.027(4) 0.064(5) 0.046(5) -0.021(4) 0.022(4) -0.018(4) N13 0.025(4) 0.052(5) 0.042(4) 0.003(4) 0.020(4) 0.010(3) N14 0.030(4) 0.055(5) 0.047(5) -0.007(4) 0.020(4) 0.006(4) N15 0.033(4) 0.050(5) 0.033(4) -0.009(3) 0.017(4) -0.004(3) N16 0.028(4) 0.048(5) 0.034(4) -0.011(3) 0.013(3) -0.007(3) N17 0.061(6) 0.055(5) 0.094(8) 0.007(5) 0.062(6) 0.013(5) N18 0.034(5) 0.090(8) 0.066(7) 0.002(6) 0.026(5) 0.008(5) N19 0.066(7) 0.071(6) 0.037(5) 0.000(4) 0.027(5) -0.002(5) N20 0.041(5) 0.081(7) 0.028(4) -0.008(4) 0.011(4) 0.000(5) N21 0.028(5) 0.075(7) 0.083(7) -0.020(6) 0.031(5) -0.012(4) N22 0.076(7) 0.056(6) 0.107(9) -0.003(6) 0.076(7) -0.002(5) N23 0.074(12) 0.44(5) 0.27(3) 0.29(3) -0.061(14) -0.095(19) N28 0.107(13) 0.46(4) 0.052(9) -0.091(16) 0.032(9) -0.001(19) N29 0.094(15) 0.121(18) 0.087(14) 0.029(13) 0.070(14) 0.000(13) N29A 0.09(2) 0.076(17) 0.057(15) -0.010(13) 0.057(16) -0.021(15) N30 0.086(11) 0.152(16) 0.22(2) -0.106(16) 0.070(14) -0.028(11) O1 0.041(4) 0.058(4) 0.041(4) 0.005(3) 0.033(3) 0.007(3) O2 0.051(4) 0.115(7) 0.038(4) -0.008(4) 0.034(4) -0.020(4) O3 0.050(4) 0.054(4) 0.050(4) 0.008(3) 0.044(4) 0.014(3) O4 0.041(4) 0.055(4) 0.048(4) -0.009(3) 0.033(3) 0.002(3) O5 0.044(4) 0.062(4) 0.044(4) -0.014(3) 0.036(3) -0.015(3) O6 0.047(4) 0.089(6) 0.035(4) 0.005(4) 0.030(3) 0.015(4) O7 0.064(5) 0.062(5) 0.075(5) 0.000(4) 0.061(5) -0.006(4) O8 0.039(4) 0.083(5) 0.046(4) 0.005(4) 0.027(3) -0.012(4) O9 0.029(3) 0.077(5) 0.021(3) 0.006(3) 0.007(3) -0.015(3) O10 0.036(3) 0.062(4) 0.039(4) -0.002(3) 0.025(3) 0.000(3) O11 0.027(3) 0.062(4) 0.046(4) 0.001(3) 0.020(3) -0.010(3) O12 0.034(4) 0.093(6) 0.042(4) -0.006(4) 0.026(3) -0.020(4) O13 0.017(3) 0.056(4) 0.038(3) -0.011(3) 0.010(3) -0.003(3) O14 0.027(3) 0.060(4) 0.031(3) -0.007(3) 0.015(3) 0.006(3) O15 0.021(3) 0.063(4) 0.033(3) -0.007(3) 0.005(3) 0.006(3) O16 0.023(3) 0.065(4) 0.034(3) -0.005(3) 0.015(3) -0.005(3) O17 0.23(2) 0.30(3) 0.174(18) -0.049(18) 0.124(18) -0.14(2) O18 0.192(19) 0.148(16) 0.27(3) -0.098(16) 0.071(19) 0.045(14) O1W 0.017(3) 0.061(4) 0.025(3) -0.003(3) 0.007(2) 0.001(3) O2W 0.075(6) 0.132(8) 0.058(5) -0.011(5) 0.055(5) 0.001(6) O3W 0.036(5) 0.143(10) 0.079(6) 0.056(7) 0.017(5) -0.006(5) O4W 0.092(7) 0.116(7) 0.079(6) -0.051(6) 0.075(6) -0.066(6) O5W 0.024(3) 0.055(4) 0.037(3) 0.001(3) 0.015(3) 0.001(3) O6W 0.056(5) 0.102(7) 0.050(4) 0.001(4) 0.039(4) -0.005(4) O7W 0.061(5) 0.058(4) 0.063(5) 0.009(4) 0.052(4) 0.016(4) O8W 0.038(4) 0.069(5) 0.046(4) -0.027(4) 0.021(3) -0.013(3) O9W 0.55(4) 0.179(16) 0.75(5) -0.27(3) 0.62(5) -0.23(2) O10W 0.081(8) 0.150(12) 0.117(10) 0.077(9) 0.010(7) -0.036(8) O11W 0.113(10) 0.109(9) 0.078(8) 0.020(7) 0.011(7) -0.059(8) O12W 0.098(10) 0.118(12) 0.194(17) 0.014(11) 0.040(11) 0.000(9) O13W 0.107(7) 0.058(5) 0.070(6) 0.028(4) 0.065(6) 0.048(5) O14W 0.098(15) 0.067(12) 0.106(16) 0.022(11) 0.064(14) -0.017(11) O15W 0.17(3) 0.12(3) 0.37(6) 0.07(3) 0.17(4) 0.05(2) C109 0.10(3) 0.37(9) 0.06(2) -0.04(4) 0.05(2) -0.06(4) C107 0.23(6) 0.21(6) 0.13(4) 0.09(4) 0.12(4) -0.04(5) O24 0.12(3) 0.09(2) 0.45(7) -0.07(3) 0.15(4) 0.002(19) N32 0.24(5) 0.08(2) 0.15(3) 0.02(2) 0.16(4) -0.02(2) N33 0.12(2) 0.15(3) 0.11(2) -0.04(2) 0.09(2) -0.04(2) _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 O1 2.220(6) . ? Tb1 O9 2.224(6) . ? Tb1 O2 2.384(8) . ? Tb1 O2W 2.390(8) . ? Tb1 O10 2.422(7) . ? Tb1 O1W 2.428(6) . ? Tb1 N9 2.542(8) . ? Tb1 N1 2.551(9) . ? Tb2 O11 2.214(6) . ? Tb2 O7 2.224(7) . ? Tb2 O12 2.411(7) . ? Tb2 O3W 2.411(9) . ? Tb2 O4W 2.419(8) . ? Tb2 O8 2.473(7) . ? Tb2 N11 2.525(9) . ? Tb2 N7 2.543(9) . ? Tb3 O15 2.210(6) . ? Tb3 O5 2.226(6) . ? Tb3 O6W 2.406(8) . ? Tb3 O5W 2.418(6) . ? Tb3 O6 2.430(7) . ? Tb3 O16 2.444(7) . ? Tb3 N5 2.533(8) . ? Tb3 N15 2.555(8) . ? Tb4 O3 2.204(6) . ? Tb4 O13 2.222(6) . ? Tb4 O7W 2.402(7) . ? Tb4 O4 2.413(6) . ? Tb4 O8W 2.414(6) . ? Tb4 O14 2.441(6) . ? Tb4 N3 2.530(8) . ? Tb4 N13 2.550(8) . ? Cl1 Cl1A 0.876(13) . ? C1 C2 1.540(13) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.402(12) . ? C2 C7 1.413(12) . ? C3 O1 1.298(10) . ? C3 C4 1.457(13) . ? C4 C5 1.390(13) . ? C4 C8 1.447(13) . ? C5 C6 1.402(13) . ? C5 H5A 0.9300 . ? C6 C7 1.436(14) . ? C6 C10 1.441(12) . ? C7 O3 1.307(11) . ? C8 N1 1.272(13) . ? C8 H8A 0.9300 . ? C9 O2 1.211(18) . ? C9 N2 1.378(18) . ? C9 C94 1.51(2) . ? C9 C94A 1.67(4) . ? C10 N3 1.316(12) . ? C10 H10A 0.9300 . ? C11 O4 1.264(12) . ? C11 N4 1.299(12) . ? C11 C12 1.506(12) . ? C12 C13 1.382(15) . ? C12 C14 1.427(15) . ? C13 C62 1.373(14) . ? C13 H13A 0.9300 . ? C14 C63 1.401(14) . ? C14 H14 0.9300 . ? C15 C16 1.502(15) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C17 1.405(13) . ? C16 C21 1.419(14) . ? C17 O7 1.314(12) . ? C17 C18 1.449(15) . ? C18 C19 1.382(14) . ? C18 C24 1.431(13) . ? C19 C20 1.377(13) . ? C19 H19A 0.9300 . ? C20 C21 1.440(14) . ? C20 C22 1.457(13) . ? C21 O5 1.300(11) . ? C22 N5 1.284(12) . ? C22 H22A 0.9300 . ? C23 O6 1.247(15) . ? C23 N6 1.340(16) . ? C23 C67 1.511(15) . ? C24 N7 1.289(13) . ? C24 H24A 0.9300 . ? C25 O8 1.225(14) . ? C25 N8 1.347(14) . ? C25 C26 1.520(14) . ? C26 C66 1.353(16) . ? C26 C27 1.363(17) . ? C27 C64 1.372(15) . ? C27 H27A 0.9300 . ? C28 C29 1.508(14) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C34 1.399(14) . ? C29 C30 1.415(12) . ? C30 O11 1.315(11) . ? C30 C31 1.427(14) . ? C31 C32 1.399(14) . ? C31 C40 1.455(12) . ? C32 C33 1.392(13) . ? C32 H32A 0.9300 . ? C33 C35 1.430(14) . ? C33 C34 1.432(14) . ? C34 O9 1.300(11) . ? C35 N9 1.278(12) . ? C35 H35A 0.9300 . ? C36 O10 1.252(12) . ? C36 N10 1.352(12) . ? C36 C37 1.509(14) . ? C37 C39 1.365(15) . ? C37 C38 1.402(17) . ? C38 C70 1.393(17) . ? C38 H38A 0.9300 . ? C39 C71 1.414(16) . ? C39 H39A 0.9300 . ? C40 N11 1.291(12) . ? C40 H40A 0.9300 . ? C41 O12 1.259(13) . ? C41 N12 1.311(13) . ? C41 C42 1.499(13) . ? C42 C44 1.385(15) . ? C42 C43 1.404(16) . ? C43 C72 1.404(14) . ? C43 H43A 0.9300 . ? C44 C73 1.398(16) . ? C44 H44A 0.9300 . ? C45 C46 1.511(13) . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 C47 1.402(12) . ? C46 C51 1.421(12) . ? C47 O15 1.292(11) . ? C47 C48 1.465(14) . ? C48 C49 1.410(13) . ? C48 C57 1.416(13) . ? C49 C50 1.404(13) . ? C49 H49A 0.9300 . ? C50 C52 1.439(13) . ? C50 C51 1.450(14) . ? C51 O13 1.288(11) . ? C52 N13 1.289(12) . ? C52 H52A 0.9300 . ? C53 O14 1.250(12) . ? C53 N14 1.326(12) . ? C53 C54 1.501(13) . ? C54 C56 1.375(14) . ? C54 C55 1.385(16) . ? C55 C74 1.399(16) . ? C55 H55A 0.9300 . ? C56 C75 1.367(15) . ? C56 H56A 0.9300 . ? C57 N15 1.307(12) . ? C57 H57A 0.9300 . ? C58 O16 1.249(12) . ? C58 N16 1.350(12) . ? C58 C59 1.493(13) . ? C59 C78 1.399(13) . ? C59 C60 1.406(15) . ? C60 C76 1.374(16) . ? C60 H60A 0.9300 . ? C62 N17 1.348(15) . ? C62 H62A 0.9300 . ? C63 N17 1.315(16) . ? C63 H63A 0.9300 . ? C64 N22 1.307(16) . ? C64 H64A 0.9300 . ? C65 N22 1.320(17) . ? C65 C66 1.394(16) . ? C65 H65A 0.9300 . ? C66 H66A 0.9300 . ? C67 C93 1.327(14) . ? C67 C90 1.359(15) . ? C70 N19 1.330(16) . ? C70 H70A 0.9300 . ? C71 N19 1.317(16) . ? C71 H71A 0.9300 . ? C72 N21 1.329(15) . ? C72 H72A 0.9300 . ? C73 N21 1.326(16) . ? C73 H73A 0.9300 . ? C74 N18 1.314(16) . ? C74 H74A 0.9300 . ? C75 N18 1.344(16) . ? C75 H75A 0.9300 . ? C76 N20 1.273(15) . ? C76 H76A 0.9300 . ? C77 N20 1.316(15) . ? C77 C78 1.366(14) . ? C77 H77A 0.9300 . ? C78 H78A 0.9300 . ? C83 N23 1.447(10) . ? C83 H83A 0.9600 . ? C83 H83B 0.9600 . ? C83 H83C 0.9600 . ? C84 N23 1.453(10) . ? C84 H84A 0.9600 . ? C84 H84B 0.9600 . ? C84 H84C 0.9600 . ? C85 O17 1.300(10) . ? C85 N23 1.301(10) . ? C85 H85A 0.9300 . ? C87 O22 1.31(2) . ? C87 N27 1.31(2) . ? C87 H87A 0.9300 . ? C89 N27 1.459(10) . ? C89 H89A 0.9600 . ? C89 H89B 0.9600 . ? C89 H89C 0.9600 . ? C90 C91 1.351(14) . ? C90 H90A 0.9300 . ? C91 N28 1.333(16) . ? C91 H91A 0.9300 . ? C92 N28 1.323(16) . ? C92 C93 1.360(16) . ? C92 H92A 0.9300 . ? C93 H93A 0.9300 . ? C94 C94A 0.85(4) . ? C94 C95A 1.06(3) . ? C94 C98 1.39(3) . ? C94 C95 1.41(4) . ? C95 C95A 1.03(6) . ? C95 C94A 1.08(4) . ? C95 C96 1.51(3) . ? C95 C98A 1.70(6) . ? C96 N29 1.14(2) . ? C96 N29A 1.24(3) . ? C96 C95A 1.46(4) . ? C97 N29 1.36(3) . ? C97 C98 1.41(3) . ? C97 C95A 1.97(4) . ? C98 C95A 1.59(5) . ? C94A C98A 1.37(5) . ? C94A C95A 1.41(5) . ? C95A N29 1.92(3) . ? C97A N29A 1.29(5) . ? C97A C98A 1.39(3) . ? C99 O18 1.290(10) . ? C99 N30 1.307(10) . ? C99 H99A 0.9300 . ? C100 N30 1.452(10) . ? C100 H10B 0.9600 . ? C100 H10C 0.9600 . ? C100 H10D 0.9600 . ? C101 N30 1.447(10) . ? C101 H10E 0.9600 . ? C101 H10F 0.9600 . ? C101 H10G 0.9600 . ? C104 N31 1.448(10) . ? C104 H10H 0.9600 . ? C104 H10I 0.9600 . ? C104 H10J 0.9600 . ? C105 N31 1.446(10) . ? C105 H10K 0.9600 . ? C105 H10L 0.9600 . ? C105 H10M 0.9600 . ? N1 N2 1.390(11) . ? N2 H2 0.8600 . ? N3 N4 1.409(10) . ? N4 H4 0.8600 . ? N5 N6 1.397(11) . ? N6 H6 0.8600 . ? N7 N8 1.410(11) . ? N8 H8 0.8600 . ? N9 N10 1.409(11) . ? N10 H10 0.8600 . ? N11 N12 1.401(10) . ? N12 H12 0.8600 . ? N13 N14 1.402(10) . ? N14 H14A 0.8600 . ? N15 N16 1.383(10) . ? N16 H16 0.8600 . ? N29 N29A 1.75(4) . ? N31 C103 1.307(10) . ? C103 O19 1.302(10) . ? C103 H10N 0.9300 . ? N27 C88 1.456(10) . ? C88 H88A 0.9600 . ? C88 H88B 0.9600 . ? C88 H88C 0.9600 . ? C109 N32 1.449(10) . ? C109 H10O 0.9600 . ? C109 H10P 0.9600 . ? C109 H10Q 0.9600 . ? C108 N32 1.442(10) . ? C108 H10R 0.9600 . ? C108 H10S 0.9600 . ? C108 H10T 0.9600 . ? C107 N32 1.293(10) . ? C107 O23 1.296(10) . ? C107 H10U 0.9300 . ? O24 C115 1.300(10) . ? N33 C115 1.296(10) . ? N33 C116 1.450(10) . ? N33 C117 1.452(10) . ? C115 H11J 0.9300 . ? C116 H11D 0.9600 . ? C116 H11E 0.9600 . ? C116 H11F 0.9600 . ? C117 H11G 0.9600 . ? C117 H11H 0.9600 . ? C117 H11I 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Tb1 O9 104.5(3) . . ? O1 Tb1 O2 133.3(3) . . ? O9 Tb1 O2 78.7(3) . . ? O1 Tb1 O2W 150.9(3) . . ? O9 Tb1 O2W 92.8(3) . . ? O2 Tb1 O2W 72.5(3) . . ? O1 Tb1 O10 77.1(2) . . ? O9 Tb1 O10 133.3(3) . . ? O2 Tb1 O10 134.2(3) . . ? O2W Tb1 O10 74.0(3) . . ? O1 Tb1 O1W 84.6(2) . . ? O9 Tb1 O1W 150.1(2) . . ? O2 Tb1 O1W 74.6(2) . . ? O2W Tb1 O1W 92.0(3) . . ? O10 Tb1 O1W 76.3(2) . . ? O1 Tb1 N9 78.7(2) . . ? O9 Tb1 N9 69.7(2) . . ? O2 Tb1 N9 140.6(2) . . ? O2W Tb1 N9 85.8(3) . . ? O10 Tb1 N9 64.8(2) . . ? O1W Tb1 N9 140.2(2) . . ? O1 Tb1 N1 70.8(2) . . ? O9 Tb1 N1 75.6(3) . . ? O2 Tb1 N1 65.0(3) . . ? O2W Tb1 N1 137.3(3) . . ? O10 Tb1 N1 142.0(2) . . ? O1W Tb1 N1 80.9(2) . . ? N9 Tb1 N1 125.4(3) . . ? O11 Tb2 O7 106.7(3) . . ? O11 Tb2 O12 132.4(3) . . ? O7 Tb2 O12 77.1(3) . . ? O11 Tb2 O3W 150.9(3) . . ? O7 Tb2 O3W 90.2(3) . . ? O12 Tb2 O3W 73.7(3) . . ? O11 Tb2 O4W 86.3(3) . . ? O7 Tb2 O4W 152.5(3) . . ? O12 Tb2 O4W 76.3(2) . . ? O3W Tb2 O4W 89.1(4) . . ? O11 Tb2 O8 76.6(2) . . ? O7 Tb2 O8 132.9(3) . . ? O12 Tb2 O8 135.7(2) . . ? O3W Tb2 O8 74.6(3) . . ? O4W Tb2 O8 73.0(3) . . ? O11 Tb2 N11 71.0(2) . . ? O7 Tb2 N11 75.5(3) . . ? O12 Tb2 N11 64.1(3) . . ? O3W Tb2 N11 137.5(3) . . ? O4W Tb2 N11 86.5(3) . . ? O8 Tb2 N11 142.5(2) . . ? O11 Tb2 N7 79.7(3) . . ? O7 Tb2 N7 70.6(3) . . ? O12 Tb2 N7 140.6(3) . . ? O3W Tb2 N7 84.1(4) . . ? O4W Tb2 N7 136.6(3) . . ? O8 Tb2 N7 63.8(3) . . ? N11 Tb2 N7 125.7(3) . . ? O15 Tb3 O5 104.7(3) . . ? O15 Tb3 O6W 93.2(3) . . ? O5 Tb3 O6W 150.1(3) . . ? O15 Tb3 O5W 149.3(2) . . ? O5 Tb3 O5W 86.8(2) . . ? O6W Tb3 O5W 89.8(3) . . ? O15 Tb3 O6 76.7(2) . . ? O5 Tb3 O6 133.3(3) . . ? O6W Tb3 O6 73.7(3) . . ? O5W Tb3 O6 75.0(2) . . ? O15 Tb3 O16 133.5(2) . . ? O5 Tb3 O16 76.4(2) . . ? O6W Tb3 O16 73.8(3) . . ? O5W Tb3 O16 76.5(2) . . ? O6 Tb3 O16 136.3(2) . . ? O15 Tb3 N5 75.1(3) . . ? O5 Tb3 N5 70.8(2) . . ? O6W Tb3 N5 138.1(3) . . ? O5W Tb3 N5 82.3(2) . . ? O6 Tb3 N5 64.5(3) . . ? O16 Tb3 N5 141.7(2) . . ? O15 Tb3 N15 70.8(2) . . ? O5 Tb3 N15 77.5(3) . . ? O6W Tb3 N15 86.3(3) . . ? O5W Tb3 N15 139.9(2) . . ? O6 Tb3 N15 140.6(2) . . ? O16 Tb3 N15 64.0(2) . . ? N5 Tb3 N15 124.8(3) . . ? O3 Tb4 O13 106.0(3) . . ? O3 Tb4 O7W 149.5(2) . . ? O13 Tb4 O7W 87.5(3) . . ? O3 Tb4 O4 133.5(2) . . ? O13 Tb4 O4 77.7(2) . . ? O7W Tb4 O4 75.5(2) . . ? O3 Tb4 O8W 89.9(3) . . ? O13 Tb4 O8W 152.5(2) . . ? O7W Tb4 O8W 89.8(3) . . ? O4 Tb4 O8W 75.1(2) . . ? O3 Tb4 O14 76.8(2) . . ? O13 Tb4 O14 131.9(2) . . ? O7W Tb4 O14 74.0(2) . . ? O4 Tb4 O14 135.3(2) . . ? O8W Tb4 O14 72.9(2) . . ? O3 Tb4 N3 70.7(2) . . ? O13 Tb4 N3 80.5(3) . . ? O7W Tb4 N3 139.5(2) . . ? O4 Tb4 N3 64.2(2) . . ? O8W Tb4 N3 83.9(3) . . ? O14 Tb4 N3 139.9(2) . . ? O3 Tb4 N13 75.6(3) . . ? O13 Tb4 N13 70.4(2) . . ? O7W Tb4 N13 83.9(3) . . ? O4 Tb4 N13 142.5(2) . . ? O8W Tb4 N13 136.5(2) . . ? O14 Tb4 N13 63.9(2) . . ? N3 Tb4 N13 126.6(3) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 C7 121.6(9) . . ? C3 C2 C1 120.2(8) . . ? C7 C2 C1 118.2(8) . . ? O1 C3 C2 120.5(8) . . ? O1 C3 C4 120.8(8) . . ? C2 C3 C4 118.7(8) . . ? C5 C4 C8 118.3(9) . . ? C5 C4 C3 118.8(8) . . ? C8 C4 C3 122.9(9) . . ? C4 C5 C6 122.8(9) . . ? C4 C5 H5A 118.6 . . ? C6 C5 H5A 118.6 . . ? C5 C6 C7 118.6(8) . . ? C5 C6 C10 117.4(9) . . ? C7 C6 C10 124.0(9) . . ? O3 C7 C2 119.2(8) . . ? O3 C7 C6 121.3(8) . . ? C2 C7 C6 119.4(8) . . ? N1 C8 C4 126.3(9) . . ? N1 C8 H8A 116.9 . . ? C4 C8 H8A 116.9 . . ? O2 C9 N2 123.9(10) . . ? O2 C9 C94 108.1(15) . . ? N2 C9 C94 127.7(16) . . ? O2 C9 C94A 135.8(15) . . ? N2 C9 C94A 99.8(16) . . ? C94 C9 C94A 30.6(12) . . ? N3 C10 C6 123.9(9) . . ? N3 C10 H10A 118.1 . . ? C6 C10 H10A 118.1 . . ? O4 C11 N4 124.5(8) . . ? O4 C11 C12 119.8(9) . . ? N4 C11 C12 115.8(9) . . ? C13 C12 C14 118.6(9) . . ? C13 C12 C11 122.7(9) . . ? C14 C12 C11 118.7(9) . . ? C62 C13 C12 119.6(11) . . ? C62 C13 H13A 120.2 . . ? C12 C13 H13A 120.2 . . ? C63 C14 C12 116.7(11) . . ? C63 C14 H14 121.7 . . ? C12 C14 H14 121.7 . . ? C16 C15 H15A 109.5 . . ? C16 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C16 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C21 120.5(10) . . ? C17 C16 C15 118.3(9) . . ? C21 C16 C15 121.1(9) . . ? O7 C17 C16 119.2(10) . . ? O7 C17 C18 121.3(8) . . ? C16 C17 C18 119.5(9) . . ? C19 C18 C24 119.1(10) . . ? C19 C18 C17 118.6(9) . . ? C24 C18 C17 122.3(9) . . ? C20 C19 C18 123.1(10) . . ? C20 C19 H19A 118.5 . . ? C18 C19 H19A 118.5 . . ? C19 C20 C21 119.4(9) . . ? C19 C20 C22 117.8(9) . . ? C21 C20 C22 122.8(9) . . ? O5 C21 C16 119.7(9) . . ? O5 C21 C20 121.5(8) . . ? C16 C21 C20 118.8(9) . . ? N5 C22 C20 125.5(9) . . ? N5 C22 H22A 117.2 . . ? C20 C22 H22A 117.2 . . ? O6 C23 N6 123.5(10) . . ? O6 C23 C67 122.2(12) . . ? N6 C23 C67 114.3(12) . . ? N7 C24 C18 127.2(10) . . ? N7 C24 H24A 116.4 . . ? C18 C24 H24A 116.4 . . ? O8 C25 N8 123.4(9) . . ? O8 C25 C26 122.1(10) . . ? N8 C25 C26 114.5(11) . . ? C66 C26 C27 118.1(11) . . ? C66 C26 C25 119.7(12) . . ? C27 C26 C25 122.1(10) . . ? C26 C27 C64 119.2(12) . . ? C26 C27 H27A 120.4 . . ? C64 C27 H27A 120.4 . . ? C29 C28 H28A 109.5 . . ? C29 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C29 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C34 C29 C30 120.9(9) . . ? C34 C29 C28 119.1(9) . . ? C30 C29 C28 119.9(9) . . ? O11 C30 C29 121.0(9) . . ? O11 C30 C31 120.0(8) . . ? C29 C30 C31 118.9(9) . . ? C32 C31 C30 119.1(8) . . ? C32 C31 C40 116.5(9) . . ? C30 C31 C40 124.3(9) . . ? C33 C32 C31 122.5(10) . . ? C33 C32 H32A 118.8 . . ? C31 C32 H32A 118.8 . . ? C32 C33 C35 118.9(10) . . ? C32 C33 C34 118.4(9) . . ? C35 C33 C34 122.7(9) . . ? O9 C34 C29 119.4(9) . . ? O9 C34 C33 120.5(9) . . ? C29 C34 C33 120.0(8) . . ? N9 C35 C33 126.7(10) . . ? N9 C35 H35A 116.7 . . ? C33 C35 H35A 116.7 . . ? O10 C36 N10 122.0(9) . . ? O10 C36 C37 121.1(9) . . ? N10 C36 C37 116.9(9) . . ? C39 C37 C38 120.3(11) . . ? C39 C37 C36 118.3(10) . . ? C38 C37 C36 121.2(10) . . ? C70 C38 C37 116.4(12) . . ? C70 C38 H38A 121.8 . . ? C37 C38 H38A 121.8 . . ? C37 C39 C71 117.2(12) . . ? C37 C39 H39A 121.4 . . ? C71 C39 H39A 121.4 . . ? N11 C40 C31 125.1(10) . . ? N11 C40 H40A 117.5 . . ? C31 C40 H40A 117.5 . . ? O12 C41 N12 124.0(9) . . ? O12 C41 C42 118.3(10) . . ? N12 C41 C42 117.7(10) . . ? C44 C42 C43 117.3(10) . . ? C44 C42 C41 120.6(11) . . ? C43 C42 C41 122.1(10) . . ? C72 C43 C42 118.9(10) . . ? C72 C43 H43A 120.6 . . ? C42 C43 H43A 120.6 . . ? C42 C44 C73 118.8(13) . . ? C42 C44 H44A 120.6 . . ? C73 C44 H44A 120.6 . . ? C46 C45 H45A 109.5 . . ? C46 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C46 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C47 C46 C51 121.7(9) . . ? C47 C46 C45 118.7(8) . . ? C51 C46 C45 119.5(8) . . ? O15 C47 C46 119.9(9) . . ? O15 C47 C48 120.0(8) . . ? C46 C47 C48 120.0(8) . . ? C49 C48 C57 118.0(9) . . ? C49 C48 C47 117.5(9) . . ? C57 C48 C47 124.5(9) . . ? C50 C49 C48 122.7(10) . . ? C50 C49 H49A 118.6 . . ? C48 C49 H49A 118.6 . . ? C49 C50 C52 116.9(9) . . ? C49 C50 C51 119.6(9) . . ? C52 C50 C51 123.5(9) . . ? O13 C51 C46 120.6(9) . . ? O13 C51 C50 121.1(8) . . ? C46 C51 C50 118.3(8) . . ? N13 C52 C50 125.1(10) . . ? N13 C52 H52A 117.4 . . ? C50 C52 H52A 117.4 . . ? O14 C53 N14 123.0(8) . . ? O14 C53 C54 119.2(8) . . ? N14 C53 C54 117.8(9) . . ? C56 C54 C55 118.5(10) . . ? C56 C54 C53 118.5(10) . . ? C55 C54 C53 123.0(9) . . ? C54 C55 C74 117.4(11) . . ? C54 C55 H55A 121.3 . . ? C74 C55 H55A 121.3 . . ? C75 C56 C54 119.2(12) . . ? C75 C56 H56A 120.4 . . ? C54 C56 H56A 120.4 . . ? N15 C57 C48 125.3(10) . . ? N15 C57 H57A 117.4 . . ? C48 C57 H57A 117.4 . . ? O16 C58 N16 121.5(8) . . ? O16 C58 C59 120.1(8) . . ? N16 C58 C59 118.4(9) . . ? C78 C59 C60 115.8(9) . . ? C78 C59 C58 119.2(9) . . ? C60 C59 C58 124.7(9) . . ? C76 C60 C59 119.0(10) . . ? C76 C60 H60A 120.5 . . ? C59 C60 H60A 120.5 . . ? N17 C62 C13 122.6(11) . . ? N17 C62 H62A 118.7 . . ? C13 C62 H62A 118.7 . . ? N17 C63 C14 124.0(11) . . ? N17 C63 H63A 118.0 . . ? C14 C63 H63A 118.0 . . ? N22 C64 C27 123.9(13) . . ? N22 C64 H64A 118.0 . . ? C27 C64 H64A 118.0 . . ? N22 C65 C66 122.9(13) . . ? N22 C65 H65A 118.6 . . ? C66 C65 H65A 118.6 . . ? C26 C66 C65 119.0(14) . . ? C26 C66 H66A 120.5 . . ? C65 C66 H66A 120.5 . . ? C93 C67 C90 118.9(10) . . ? C93 C67 C23 117.5(14) . . ? C90 C67 C23 123.6(13) . . ? N19 C70 C38 125.0(13) . . ? N19 C70 H70A 117.5 . . ? C38 C70 H70A 117.5 . . ? N19 C71 C39 124.5(12) . . ? N19 C71 H71A 117.8 . . ? C39 C71 H71A 117.8 . . ? N21 C72 C43 123.7(12) . . ? N21 C72 H72A 118.1 . . ? C43 C72 H72A 118.1 . . ? N21 C73 C44 124.6(11) . . ? N21 C73 H73A 117.7 . . ? C44 C73 H73A 117.7 . . ? N18 C74 C55 124.9(13) . . ? N18 C74 H74A 117.5 . . ? C55 C74 H74A 117.5 . . ? N18 C75 C56 124.1(12) . . ? N18 C75 H75A 117.9 . . ? C56 C75 H75A 117.9 . . ? N20 C76 C60 124.6(12) . . ? N20 C76 H76A 117.7 . . ? C60 C76 H76A 117.7 . . ? N20 C77 C78 124.9(10) . . ? N20 C77 H77A 117.6 . . ? C78 C77 H77A 117.6 . . ? C77 C78 C59 118.3(10) . . ? C77 C78 H78A 120.9 . . ? C59 C78 H78A 120.9 . . ? N23 C83 H83A 109.5 . . ? N23 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? N23 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? N23 C84 H84A 109.5 . . ? N23 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? N23 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? O17 C85 N23 119.8(17) . . ? O17 C85 H85A 120.1 . . ? N23 C85 H85A 120.1 . . ? O22 C87 N27 120(3) . . ? O22 C87 H87A 119.9 . . ? N27 C87 H87A 119.9 . . ? N27 C89 H89A 109.5 . . ? N27 C89 H89B 109.5 . . ? H89A C89 H89B 109.5 . . ? N27 C89 H89C 109.5 . . ? H89A C89 H89C 109.5 . . ? H89B C89 H89C 109.5 . . ? C91 C90 C67 120.0(12) . . ? C91 C90 H90A 120.0 . . ? C67 C90 H90A 120.0 . . ? N28 C91 C90 118.9(13) . . ? N28 C91 H91A 120.5 . . ? C90 C91 H91A 120.5 . . ? N28 C92 C93 118.4(15) . . ? N28 C92 H92A 120.8 . . ? C93 C92 H92A 120.8 . . ? C67 C93 C92 120.4(13) . . ? C67 C93 H93A 119.8 . . ? C92 C93 H93A 119.8 . . ? C94A C94 C95A 94(5) . . ? C94A C94 C98 132(4) . . ? C95A C94 C98 80(3) . . ? C94A C94 C95 50(3) . . ? C95A C94 C95 47(3) . . ? C98 C94 C95 121(2) . . ? C94A C94 C9 85(3) . . ? C95A C94 C9 151(3) . . ? C98 C94 C9 121(2) . . ? C95 C94 C9 118(2) . . ? C95A C95 C94A 84(4) . . ? C95A C95 C94 49(2) . . ? C94A C95 C94 37(2) . . ? C95A C95 C96 67(3) . . ? C94A C95 C96 126(3) . . ? C94 C95 C96 109(3) . . ? C95A C95 C98A 123(4) . . ? C94A C95 C98A 54(4) . . ? C94 C95 C98A 89(3) . . ? C96 C95 C98A 106(3) . . ? N29 C96 N29A 94(2) . . ? N29 C96 C95A 95(2) . . ? N29A C96 C95A 132(2) . . ? N29 C96 C95 132(2) . . ? N29A C96 C95 104(2) . . ? C95A C96 C95 41(2) . . ? N29 C97 C98 119(2) . . ? N29 C97 C95A 67.5(18) . . ? C98 C97 C95A 53.1(17) . . ? C94 C98 C97 120(2) . . ? C94 C98 C95A 40.9(15) . . ? C97 C98 C95A 81.9(19) . . ? C94 C94A C95 93(4) . . ? C94 C94A C98A 157(4) . . ? C95 C94A C98A 87(4) . . ? C94 C94A C95A 49(3) . . ? C95 C94A C95A 47(3) . . ? C98A C94A C95A 121(4) . . ? C94 C94A C9 64(3) . . ? C95 C94A C9 129(3) . . ? C98A C94A C9 132(2) . . ? C95A C94A C9 108(3) . . ? C95 C95A C94 84(4) . . ? C95 C95A C94A 50(3) . . ? C94 C95A C94A 37(2) . . ? C95 C95A C96 72(4) . . ? C94 C95A C96 141(5) . . ? C94A C95A C96 108(4) . . ? C95 C95A C98 134(4) . . ? C94 C95A C98 59(3) . . ? C94A C95A C98 86(3) . . ? C96 C95A C98 118(2) . . ? C95 C95A N29 106(4) . . ? C94 C95A N29 134(2) . . ? C94A C95A N29 122(3) . . ? C96 C95A N29 36.2(10) . . ? C98 C95A N29 85.1(16) . . ? C95 C95A C97 136(4) . . ? C94 C95A C97 102(3) . . ? C94A C95A C97 116(2) . . ? C96 C95A C97 76.6(15) . . ? C98 C95A C97 45.1(14) . . ? N29 C95A C97 41.0(10) . . ? N29A C97A C98A 124(4) . . ? C94A C98A C97A 119(3) . . ? C94A C98A C95 39.4(19) . . ? C97A C98A C95 87(3) . . ? O18 C99 N30 117.0(17) . . ? O18 C99 H99A 121.5 . . ? N30 C99 H99A 121.5 . . ? N30 C100 H10B 109.5 . . ? N30 C100 H10C 109.5 . . ? H10B C100 H10C 109.5 . . ? N30 C100 H10D 109.5 . . ? H10B C100 H10D 109.5 . . ? H10C C100 H10D 109.5 . . ? N30 C101 H10E 109.5 . . ? N30 C101 H10F 109.5 . . ? H10E C101 H10F 109.5 . . ? N30 C101 H10G 109.5 . . ? H10E C101 H10G 109.5 . . ? H10F C101 H10G 109.5 . . ? N31 C104 H10H 109.5 . . ? N31 C104 H10I 109.5 . . ? H10H C104 H10I 109.5 . . ? N31 C104 H10J 109.5 . . ? H10H C104 H10J 109.5 . . ? H10I C104 H10J 109.5 . . ? N31 C105 H10K 109.5 . . ? N31 C105 H10L 109.5 . . ? H10K C105 H10L 109.5 . . ? N31 C105 H10M 109.5 . . ? H10K C105 H10M 109.5 . . ? H10L C105 H10M 109.5 . . ? C8 N1 N2 115.4(9) . . ? C8 N1 Tb1 130.7(7) . . ? N2 N1 Tb1 112.6(7) . . ? C9 N2 N1 115.1(10) . . ? C9 N2 H2 122.4 . . ? N1 N2 H2 122.4 . . ? C10 N3 N4 113.3(8) . . ? C10 N3 Tb4 133.0(6) . . ? N4 N3 Tb4 113.5(6) . . ? C11 N4 N3 115.3(8) . . ? C11 N4 H4 122.3 . . ? N3 N4 H4 122.3 . . ? C22 N5 N6 113.2(9) . . ? C22 N5 Tb3 131.7(7) . . ? N6 N5 Tb3 114.2(6) . . ? C23 N6 N5 116.0(10) . . ? C23 N6 H6 122.0 . . ? N5 N6 H6 122.0 . . ? C24 N7 N8 114.6(9) . . ? C24 N7 Tb2 131.8(7) . . ? N8 N7 Tb2 113.4(6) . . ? C25 N8 N7 116.0(10) . . ? C25 N8 H8 122.0 . . ? N7 N8 H8 122.0 . . ? C35 N9 N10 114.4(8) . . ? C35 N9 Tb1 131.8(7) . . ? N10 N9 Tb1 113.0(5) . . ? C36 N10 N9 117.0(9) . . ? C36 N10 H10 121.5 . . ? N9 N10 H10 121.5 . . ? C40 N11 N12 113.4(9) . . ? C40 N11 Tb2 130.8(7) . . ? N12 N11 Tb2 114.2(6) . . ? C41 N12 N11 115.2(9) . . ? C41 N12 H12 122.4 . . ? N11 N12 H12 122.4 . . ? C52 N13 N14 113.7(8) . . ? C52 N13 Tb4 130.7(7) . . ? N14 N13 Tb4 114.1(6) . . ? C53 N14 N13 116.6(8) . . ? C53 N14 H14A 121.7 . . ? N13 N14 H14A 121.7 . . ? C57 N15 N16 114.5(8) . . ? C57 N15 Tb3 131.1(7) . . ? N16 N15 Tb3 113.6(5) . . ? C58 N16 N15 117.6(8) . . ? C58 N16 H16 121.2 . . ? N15 N16 H16 121.2 . . ? C63 N17 C62 118.6(9) . . ? C74 N18 C75 115.8(11) . . ? C71 N19 C70 116.5(10) . . ? C76 N20 C77 117.4(10) . . ? C73 N21 C72 116.6(10) . . ? C64 N22 C65 116.9(11) . . ? C85 N23 C83 106(2) . . ? C85 N23 C84 114(3) . . ? C83 N23 C84 140(3) . . ? C92 N28 C91 120.3(12) . . ? C96 N29 C97 119(2) . . ? C96 N29 N29A 45.2(16) . . ? C97 N29 N29A 131(2) . . ? C96 N29 C95A 49.0(19) . . ? C97 N29 C95A 71.5(18) . . ? N29A N29 C95A 84.4(19) . . ? C96 N29A C97A 113(3) . . ? C96 N29A N29 40.6(13) . . ? C97A N29A N29 130(3) . . ? C99 N30 C101 102.5(18) . . ? C99 N30 C100 125(2) . . ? C101 N30 C100 132(2) . . ? C103 N31 C105 129(3) . . ? C103 N31 C104 107.5(19) . . ? C105 N31 C104 123(2) . . ? C3 O1 Tb1 144.2(6) . . ? C9 O2 Tb1 120.0(7) . . ? C7 O3 Tb4 146.9(6) . . ? C11 O4 Tb4 118.2(6) . . ? C21 O5 Tb3 143.5(6) . . ? C23 O6 Tb3 119.5(7) . . ? C17 O7 Tb2 146.7(7) . . ? C25 O8 Tb2 118.8(6) . . ? C34 O9 Tb1 146.1(6) . . ? C36 O10 Tb1 120.1(6) . . ? C30 O11 Tb2 144.9(6) . . ? C41 O12 Tb2 119.2(6) . . ? C51 O13 Tb4 145.2(6) . . ? C53 O14 Tb4 120.4(5) . . ? C47 O15 Tb3 145.8(6) . . ? C58 O16 Tb3 119.9(5) . . ? O19 C103 N31 120(2) . . ? O19 C103 H10N 119.8 . . ? N31 C103 H10N 119.8 . . ? C87 N27 C88 125(3) . . ? C87 N27 C89 126(3) . . ? C88 N27 C89 109(3) . . ? N27 C88 H88A 109.5 . . ? N27 C88 H88B 109.5 . . ? H88A C88 H88B 109.5 . . ? N27 C88 H88C 109.5 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? N32 C109 H10O 109.5 . . ? N32 C109 H10P 109.5 . . ? H10O C109 H10P 109.5 . . ? N32 C109 H10Q 109.5 . . ? H10O C109 H10Q 109.5 . . ? H10P C109 H10Q 109.5 . . ? N32 C108 H10R 109.5 . . ? N32 C108 H10S 109.5 . . ? H10R C108 H10S 109.5 . . ? N32 C108 H10T 109.5 . . ? H10R C108 H10T 109.5 . . ? H10S C108 H10T 109.5 . . ? N32 C107 O23 125(2) . . ? N32 C107 H10U 117.7 . . ? O23 C107 H10U 117.7 . . ? C107 N32 C108 115(2) . . ? C107 N32 C109 125(3) . . ? C108 N32 C109 119.4(12) . . ? C115 N33 C116 109(4) . . ? C115 N33 C117 119(5) . . ? C116 N33 C117 132(5) . . ? N33 C115 O24 121(2) . . ? N33 C115 H11J 119.5 . . ? O24 C115 H11J 119.5 . . ? N33 C116 H11D 109.5 . . ? N33 C116 H11E 109.5 . . ? H11D C116 H11E 109.5 . . ? N33 C116 H11F 109.5 . . ? H11D C116 H11F 109.5 . . ? H11E C116 H11F 109.5 . . ? N33 C117 H11G 109.5 . . ? N33 C117 H11H 109.5 . . ? H11G C117 H11H 109.5 . . ? N33 C117 H11I 109.5 . . ? H11G C117 H11I 109.5 . . ? H11H C117 H11I 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.832 _refine_diff_density_min -1.327 _refine_diff_density_rms 0.163