# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1936 #=============================================================================== data_global #=============================================================================== _audit_creation_date 1-06-99 # 1. SUBMISSION DETAILS _publ_contact_author_name # Name of author for correspondance ; ; _publ_contact_author_address # Address of author for correspondance ; ; _publ_contact_author_phone 'xxxxxxxxxx' _publ_contact_author_fax 'xxxxxxxxxx' _publ_contact_author_email xxx@xx.xx.xx _publ_requested_journal 'Acta Crystallographica C' _publ_contact_letter ; Please consider this CIF submission for publication as a new structure paper in Acta Crystallographica Section C. The figures, chemical structure diagram (scheme), Transfert of Copyright Agreement form and structure factors will be sent on receipt of your acknowledgement letter ; _publ_requested_category FM #=============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #=============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; ? ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Dupont Karl' #<--'Last name, first name' ; Research School of Chemistry National Laboratory Ouchnock Islandia ; # 4. TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; ? ; _publ_section_references ; Burla, M.C., Camalli, M., Cascarano, G.,Giacovazzo, C., Polidori, G., Spagna, R. &Viterbo, D. (1989). SIR. J. Appl. Cryst. 22, 389-393. OpenMoleN, Interactive Intelligent Structure solution (1997) Nonius B.V., Delft, The Netherlands. KappaCCD Operation Manual (1997), Nonius B.V., Delft, The Nederlands. Otwinowski, Z. & Minor, W. (1997), Methods in Enzymology, 276, 307-326. ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #=============================================================================== # If more than one structure is reported, sections 5-10 should be filled in # per structure. For each data set, replace the ? in the data_? line below # by a unique identifier. data_st403 #=============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C38 H36 N6 O19 Tb2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C38 H36 N6 O19 Tb2' _chemical_formula_weight 1198.59 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 N ? 0.004 0.003 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 Tb ? -0.591 4.151 International_Tables_Vol_IV_Table_2.3.1 #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z _cell_length_a 13.6780(5) _cell_length_b 18.930(1) _cell_length_c 15.8188(9) _cell_angle_alpha 90 _cell_angle_beta 92.227(3) _cell_angle_gamma 90 _cell_volume 4092.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_special_details ; Cell parameters refined using Scalepack part of DENZO Z. Otwinowski, W. Minor, 1997 ; _exptl_crystal_description prism _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.95 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 2352 _exptl_absorpt_coefficient_mu 3.518 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? #=============================================================================== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\p scans' _diffrn_measurement_details ; 25474 reflections were collected using program Collect (Collect Software, Nonius, Delft (The Nederlands), 1997) The conditions were as follow : crystal to detector distance = 40. mm. Scan angle = 2.3 deg 1 scans of 104 sec per frame. Data collection was divided into 2 sets with the following starting angles and number of frames Set 1 Theta = 9.94 Omega = 180. Kappa = 0.00 76 frames Set 2 Theta = -7.63 Kappa = -173. Phi = -40. 17 frames Friedel pairs were not averaged. Internal R = 0.03 ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 25474 _diffrn_reflns_av_R_equivalents 0 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 32.04 _reflns_number_total 20627 _reflns_number_gt 15332 _reflns_threshold_expression >3.0\s(I) _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #=============================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme '4Fo^2^/(\s^2^(Fo^2^) + 0.0049 Fo^4^)' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 15332 _refine_ls_number_parameters 586 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.057 _refine_ls_R_factor_gt 0.037 _refine_ls_wR_factor_all 0.175 _refine_ls_wR_factor_ref 0.053 _refine_ls_goodness_of_fit_all 3.446 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_shift/su_max 0.003 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 2.020 _refine_diff_density_min -0.364 #=============================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol TB1 0.52379(1) -0.16921(1) 0.17101(1) 0.01871(7) Uani ? ? Tb TB2 0.92525(1) -0.01098(1) 0.29994(1) 0.01884(7) Uani ? ? Tb O1 0.4134(2) -0.0751(1) 0.1660(1) 0.031(1) Uani ? ? O C1 0.3813(2) -0.0439(2) 0.0992(2) 0.030(2) Uani ? ? C O2 0.3231(2) 0.0066(1) 0.0953(2) 0.041(1) Uani ? ? O C2 0.4223(2) -0.0695(2) 0.0169(2) 0.026(2) Uani ? ? C C3 0.3895(2) -0.0438(2) -0.0622(2) 0.033(2) Uani ? ? C C4 0.4342(3) -0.0701(2) -0.1337(2) 0.036(2) Uani ? ? C C5 0.5082(3) -0.1199(2) -0.1244(2) 0.030(2) Uani ? ? C C6 0.5373(2) -0.1423(2) -0.0425(2) 0.024(1) Uani ? ? C N1 0.4939(2) -0.1176(1) 0.0256(2) 0.025(1) Uani ? ? N C7 0.6130(2) -0.1966(2) -0.0258(2) 0.023(1) Uani ? ? C C8 0.6696(2) -0.2265(2) -0.0888(2) 0.030(2) Uani ? ? C C9 0.7312(2) -0.2812(2) -0.0669(2) 0.036(2) Uani ? ? C C10 0.7373(2) -0.3062(2) 0.0156(2) 0.033(2) Uani ? ? C C11 0.6813(2) -0.2728(2) 0.0741(2) 0.026(2) Uani ? ? C N2 0.6212(2) -0.2188(1) 0.0549(2) 0.021(1) Uani ? ? N C12 0.6773(2) -0.2978(2) 0.1648(2) 0.032(2) Uani ? ? C O3 0.6267(2) -0.2614(1) 0.2134(1) 0.033(1) Uani ? ? O O4 0.7201(2) -0.3530(2) 0.1836(2) 0.061(2) Uani ? ? O O5 0.4205(2) -0.2548(1) 0.1118(1) 0.027(1) Uani ? ? O C13 0.3600(2) -0.2929(2) 0.1505(2) 0.024(1) Uani ? ? C O6 0.3134(2) -0.3431(1) 0.1190(2) 0.034(1) Uani ? ? O C14 0.3473(2) -0.2734(2) 0.2431(2) 0.022(1) Uani ? ? C C15 0.2771(2) -0.3042(2) 0.2924(2) 0.027(2) Uani ? ? C C16 0.2733(2) -0.2828(2) 0.3764(2) 0.030(2) Uani ? ? C C17 0.3386(2) -0.2329(2) 0.4078(2) 0.029(2) Uani ? ? C C18 0.4059(2) -0.2040(2) 0.3550(2) 0.023(1) Uani ? ? C N3 0.4100(2) -0.2234(1) 0.2728(2) 0.022(1) Uani ? ? N C19 0.4810(2) -0.1503(2) 0.3824(2) 0.022(1) Uani ? ? C C20 0.4888(2) -0.1233(2) 0.4643(2) 0.025(2) Uani ? ? C C21 0.5607(2) -0.0740(2) 0.4839(2) 0.028(2) Uani ? ? C C22 0.6257(2) -0.0541(2) 0.4227(2) 0.028(2) Uani ? ? C C23 0.6129(2) -0.0835(2) 0.3427(2) 0.022(1) Uani ? ? C N4 0.5421(2) -0.1303(1) 0.3225(2) 0.021(1) Uani ? ? N C24 0.6819(2) -0.0690(2) 0.2727(2) 0.022(1) Uani ? ? C O7 0.6581(1) -0.0921(1) 0.1999(1) 0.025(1) Uani ? ? O O8 0.7582(2) -0.0353(1) 0.2929(2) 0.030(1) Uani ? ? O O9 0.9486(2) -0.0679(1) 0.4316(2) 0.035(1) Uani ? ? O C25 0.9746(2) -0.1315(2) 0.4419(2) 0.028(2) Uani ? ? C O10 1.0047(2) -0.1585(1) 0.5109(2) 0.038(1) Uani ? ? O C26 0.9698(2) -0.1778(2) 0.3637(2) 0.023(1) Uani ? ? C C27 0.9921(2) -0.2488(2) 0.3654(2) 0.030(2) Uani ? ? C C28 0.9786(3) -0.2874(2) 0.2903(2) 0.035(2) Uani ? ? C C29 0.9471(3) -0.2527(2) 0.2172(2) 0.031(2) Uani ? ? C C30 0.9295(2) -0.1803(2) 0.2200(2) 0.022(1) Uani ? ? C N5 0.9394(2) -0.1438(1) 0.2925(2) 0.021(1) Uani ? ? N C31 0.9033(2) -0.1369(2) 0.1432(2) 0.021(1) Uani ? ? C C32 0.8923(3) -0.1654(2) 0.0623(2) 0.027(2) Uani ? ? C C33 0.8752(3) -0.1205(2) -0.0051(2) 0.029(2) Uani ? ? C C34 0.8713(2) -0.0482(2) 0.0089(2) 0.027(2) Uani ? ? C C35 0.8836(2) -0.0239(2) 0.0912(2) 0.022(1) Uani ? ? C N6 0.8977(2) -0.0673(1) 0.1573(2) 0.020(1) Uani ? ? N C36 0.8854(2) 0.0543(2) 0.1130(2) 0.023(1) Uani ? ? C O11 0.8945(2) 0.0687(1) 0.1919(1) 0.027(1) Uani ? ? O O12 0.8785(2) 0.0985(1) 0.0559(2) 0.033(1) Uani ? ? O O13 1.0797(2) -0.0328(1) 0.2420(2) 0.030(1) Uani ? ? O O14 1.0515(2) 0.0626(2) 0.3638(2) 0.042(1) Uani ? ? O O15 0.8547(2) 0.0831(1) 0.3819(2) 0.039(1) Uani ? ? O O16 0.1912(2) 0.0729(2) 0.1910(2) 0.039(1) Uani ? ? O O17 0.4027(2) 0.0189(2) 0.3060(2) 0.061(2) Uani ? ? O C37 0.8263(3) 0.1805(3) -0.1224(3) 0.066(3) Uani ? ? C O18 0.8800(2) 0.1187(1) -0.1117(2) 0.037(1) Uani ? ? O C38 1.2246(3) -0.0684(3) 0.4139(3) 0.068(3) Uani ? ? C O19 1.2267(3) 0.0042(2) 0.4072(3) 0.082(2) Uani ? ? O H1 0.3386 -0.0098 -0.0671 0.0433 Uiso calc C3 H H2 0.4139 -0.0538 -0.1884 0.0483 Uiso calc C4 H H3 0.5387 -0.1386 -0.1725 0.0408 Uiso calc C5 H H4 0.6653 -0.2092 -0.1452 0.0401 Uiso calc C8 H H5 0.7701 -0.3022 -0.1085 0.0474 Uiso calc C9 H H6 0.7785 -0.3448 0.0311 0.0440 Uiso calc C10 H H7 0.2331 -0.3386 0.2696 0.0349 Uiso calc C15 H H8 0.2259 -0.3025 0.4120 0.0395 Uiso calc C16 H H9 0.3372 -0.2185 0.4653 0.0391 Uiso calc C17 H H10 0.4454 -0.1386 0.5060 0.0345 Uiso calc C20 H H11 0.5656 -0.0538 0.5389 0.0379 Uiso calc C21 H H12 0.6772 -0.0217 0.4353 0.0360 Uiso calc C22 H H13 1.0159 -0.2709 0.4160 0.0391 Uiso calc C27 H H14 0.9908 -0.3368 0.2896 0.0480 Uiso calc C28 H H15 0.9377 -0.2779 0.1656 0.0423 Uiso calc C29 H H16 0.8965 -0.2150 0.0538 0.0360 Uiso calc C32 H H17 0.8661 -0.1389 -0.0607 0.0397 Uiso calc C33 H H18 0.8605 -0.0162 -0.0368 0.0356 Uiso calc C34 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol TB1 0.02070(7) 0.02156(6) 0.01467(6) -0.00281(5) 0.00069(6) 0.00013(5) Tb TB2 0.01843(7) 0.01927(6) 0.01884(6) -0.00126(5) 0.00039(6) -0.00448(5) Tb O1 0.033(1) 0.030(1) 0.029(1) 0.005(1) 0.004(1) -0.000(1) O C1 0.026(2) 0.029(2) 0.035(2) -0.001(1) -0.001(1) -0.001(1) C O2 0.036(1) 0.038(1) 0.049(2) 0.013(1) -0.002(1) 0.003(1) O C2 0.025(2) 0.025(1) 0.029(2) -0.004(1) -0.005(1) 0.003(1) C C3 0.030(2) 0.031(2) 0.038(2) -0.004(1) -0.010(1) 0.011(1) C C4 0.046(2) 0.038(2) 0.027(2) -0.008(2) -0.013(1) 0.012(1) C C5 0.037(2) 0.036(2) 0.021(1) -0.004(2) -0.001(1) 0.006(1) C C6 0.026(2) 0.030(2) 0.017(1) -0.005(1) 0.001(1) 0.004(1) C N1 0.027(1) 0.025(1) 0.021(1) -0.004(1) -0.003(1) 0.002(1) N C7 0.025(2) 0.027(1) 0.019(1) -0.007(1) 0.002(1) -0.002(1) C C8 0.034(2) 0.039(2) 0.020(1) -0.006(2) 0.003(1) -0.006(1) C C9 0.030(2) 0.045(2) 0.035(2) -0.005(2) 0.009(1) -0.016(2) C C10 0.028(2) 0.034(2) 0.040(2) 0.002(2) 0.001(2) -0.007(2) C C11 0.023(2) 0.026(1) 0.029(2) -0.002(1) -0.002(1) -0.000(1) C N2 0.018(1) 0.027(1) 0.020(1) -0.002(1) 0.001(1) 0.000(1) N C12 0.033(2) 0.031(2) 0.032(2) 0.004(2) -0.004(1) 0.007(1) C O3 0.043(1) 0.037(1) 0.023(1) 0.010(1) 0.000(1) 0.006(1) O O4 0.085(2) 0.056(2) 0.049(2) 0.041(1) 0.003(2) 0.012(1) O O5 0.030(1) 0.037(1) 0.017(1) -0.011(1) 0.0024(9) -0.002(1) O C13 0.024(2) 0.027(2) 0.022(1) -0.002(1) 0.001(1) -0.000(1) C O6 0.034(1) 0.039(1) 0.030(1) -0.016(1) 0.004(1) -0.009(1) O C14 0.019(1) 0.028(1) 0.021(1) -0.002(1) 0.001(1) 0.000(1) C C15 0.027(2) 0.028(1) 0.026(2) -0.007(1) 0.004(1) 0.003(1) C C16 0.034(2) 0.030(2) 0.027(2) -0.003(1) 0.006(1) 0.001(1) C C17 0.035(2) 0.036(2) 0.020(1) -0.002(2) 0.007(1) 0.002(1) C C18 0.024(2) 0.026(1) 0.019(1) -0.002(1) 0.003(1) 0.001(1) C N3 0.023(1) 0.024(1) 0.019(1) -0.002(1) 0.002(1) 0.001(1) N C19 0.021(2) 0.029(1) 0.018(1) 0.000(1) 0.000(1) 0.000(1) C C20 0.030(2) 0.035(2) 0.015(1) 0.005(1) 0.002(1) -0.002(1) C C21 0.033(2) 0.033(2) 0.020(1) 0.004(1) -0.003(1) -0.004(1) C C22 0.026(2) 0.029(2) 0.028(2) -0.002(1) -0.001(1) -0.006(1) C C23 0.022(1) 0.023(1) 0.021(1) -0.000(1) -0.002(1) -0.000(1) C N4 0.020(1) 0.025(1) 0.018(1) 0.000(1) 0.000(1) 0.002(1) N C24 0.017(1) 0.022(1) 0.029(2) -0.000(1) 0.000(1) 0.001(1) C O7 0.024(1) 0.034(1) 0.019(1) -0.008(1) 0.0002(9) -0.0018(9) O O8 0.022(1) 0.036(1) 0.032(1) -0.006(1) 0.0017(9) -0.008(1) O O9 0.057(2) 0.029(1) 0.026(1) -0.001(1) -0.001(1) -0.006(1) O C25 0.033(2) 0.031(2) 0.022(1) -0.006(1) 0.002(1) 0.001(1) C O10 0.057(2) 0.040(1) 0.024(1) -0.004(1) -0.009(1) 0.004(1) O C26 0.026(2) 0.023(1) 0.022(1) -0.001(1) 0.001(1) -0.000(1) C C27 0.032(2) 0.028(2) 0.030(2) 0.002(1) 0.002(1) 0.003(1) C C28 0.051(2) 0.023(2) 0.037(2) 0.007(2) 0.002(2) -0.002(1) C C29 0.046(2) 0.023(1) 0.027(2) 0.004(2) -0.003(1) -0.004(1) C C30 0.027(2) 0.020(1) 0.021(1) -0.001(1) 0.002(1) -0.003(1) C N5 0.024(1) 0.020(1) 0.020(1) -0.001(1) 0.001(1) -0.003(1) N C31 0.021(1) 0.019(1) 0.023(1) -0.003(1) 0.001(1) -0.004(1) C C32 0.035(2) 0.023(1) 0.025(2) -0.003(1) -0.001(1) -0.008(1) C C33 0.041(2) 0.030(2) 0.020(1) -0.002(2) -0.002(1) -0.004(1) C C34 0.030(2) 0.033(2) 0.019(1) 0.001(1) -0.001(1) -0.004(1) C C35 0.018(1) 0.024(1) 0.025(1) 0.001(1) -0.003(1) -0.003(1) C N6 0.020(1) 0.021(1) 0.019(1) 0.001(1) -0.001(1) -0.003(1) N C36 0.023(2) 0.024(1) 0.024(1) 0.002(1) 0.002(1) -0.002(1) C O11 0.037(1) 0.023(1) 0.023(1) -0.001(1) 0.0008(9) -0.0047(9) O O12 0.055(1) 0.027(1) 0.024(1) 0.008(1) 0.002(1) 0.001(1) O O13 0.021(1) 0.038(1) 0.032(1) -0.000(1) 0.0029(9) -0.011(1) O O14 0.028(1) 0.055(2) 0.048(1) -0.009(1) 0.007(1) -0.028(1) O O15 0.033(1) 0.043(1) 0.040(1) 0.012(1) -0.005(1) -0.021(1) O O16 0.044(1) 0.045(1) 0.029(1) -0.009(1) 0.001(1) -0.004(1) O O17 0.082(2) 0.072(2) 0.038(2) 0.020(2) -0.007(2) -0.009(2) O C37 0.064(3) 0.066(3) 0.067(3) 0.037(2) 0.016(2) 0.020(2) C O18 0.040(1) 0.042(1) 0.029(1) 0.012(1) 0.001(1) -0.005(1) O C38 0.072(3) 0.068(3) 0.065(3) 0.009(3) -0.012(2) 0.021(3) C O19 0.073(2) 0.080(3) 0.094(3) 0.002(2) -0.043(2) -0.003(2) O # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag TB1 O1 2.334(2) . . ? TB1 N1 2.518(3) . . ? TB1 N2 2.494(3) . . ? TB1 O3 2.324(3) . . ? TB1 O5 2.324(2) . . ? TB1 N3 2.503(3) . . ? TB1 N4 2.511(3) . . ? TB1 O7 2.377(2) . . ? TB2 O8 2.329(2) . . ? TB2 O9 2.355(3) . . ? TB2 N5 2.524(3) . . ? TB2 N6 2.511(3) . . ? TB2 O11 2.306(2) . . ? TB2 O13 2.372(2) . . ? TB2 O14 2.410(3) . . ? TB2 O15 2.425(2) . . ? O1 C1 1.273(4) . . ? C1 O2 1.242(4) . . ? C1 C2 1.518(5) . . ? C2 C3 1.400(5) . . ? C2 N1 1.339(4) . . ? C3 C4 1.398(6) . . ? C4 C5 1.388(5) . . ? C5 C6 1.405(4) . . ? C6 N1 1.335(4) . . ? C6 C7 1.475(5) . . ? C7 C8 1.405(5) . . ? C7 N2 1.344(4) . . ? C8 C9 1.372(6) . . ? C9 C10 1.386(6) . . ? C10 C11 1.377(5) . . ? C11 N2 1.339(4) . . ? C11 C12 1.514(5) . . ? C12 O3 1.259(5) . . ? C12 O4 1.228(5) . . ? O5 C13 1.273(4) . . ? C13 O6 1.238(4) . . ? C13 C14 1.527(4) . . ? C14 C15 1.389(4) . . ? C14 N3 1.350(4) . . ? C15 C16 1.392(5) . . ? C16 C17 1.380(5) . . ? C17 C18 1.379(5) . . ? C18 N3 1.354(4) . . ? C18 C19 1.499(5) . . ? C19 C20 1.392(4) . . ? C19 N4 1.341(4) . . ? C20 C21 1.382(5) . . ? C21 C22 1.392(5) . . ? C22 C23 1.388(5) . . ? C23 N4 1.342(4) . . ? C23 C24 1.508(4) . . ? C24 O7 1.262(4) . . ? C24 O8 1.255(4) . . ? O9 C25 1.264(4) . . ? C25 O10 1.259(4) . . ? C25 C26 1.515(5) . . ? C26 C27 1.377(5) . . ? C26 N5 1.350(4) . . ? C27 C28 1.402(5) . . ? C28 C29 1.385(5) . . ? C29 C30 1.392(5) . . ? C30 N5 1.341(4) . . ? C30 C31 1.499(5) . . ? C31 C32 1.391(4) . . ? C31 N6 1.339(4) . . ? C32 C33 1.376(5) . . ? C33 C34 1.389(5) . . ? C34 C35 1.384(4) . . ? C35 N6 1.338(4) . . ? C35 C36 1.520(5) . . ? C36 O11 1.280(4) . . ? C36 O12 1.232(4) . . ? C37 O18 1.389(5) . . ? C38 O19 1.377(7) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 TB1 N1 65.87(9) . . . ? O1 TB1 N2 128.72(9) . . . ? O1 TB1 O3 165.08(9) . . . ? O1 TB1 O5 97.84(9) . . . ? O1 TB1 N3 85.25(9) . . . ? O1 TB1 N4 81.29(9) . . . ? O1 TB1 O7 91.82(9) . . . ? N1 TB1 N2 62.97(9) . . . ? N1 TB1 O3 129.03(9) . . . ? N1 TB1 O5 80.05(9) . . . ? N1 TB1 N3 131.59(9) . . . ? N1 TB1 N4 139.91(9) . . . ? N1 TB1 O7 92.00(8) . . . ? N2 TB1 O3 66.11(9) . . . ? N2 TB1 O5 76.97(8) . . . ? N2 TB1 N3 133.08(9) . . . ? N2 TB1 N4 141.01(8) . . . ? N2 TB1 O7 86.66(8) . . . ? O3 TB1 O5 86.8(1) . . . ? O3 TB1 N3 83.76(9) . . . ? O3 TB1 N4 84.74(9) . . . ? O3 TB1 O7 87.17(9) . . . ? O5 TB1 N3 65.79(8) . . . ? O5 TB1 N4 128.76(8) . . . ? O5 TB1 O7 163.62(8) . . . ? N3 TB1 N4 63.08(9) . . . ? N3 TB1 O7 128.55(8) . . . ? N4 TB1 O7 65.70(8) . . . ? O8 TB2 O9 92.93(9) . . . ? O8 TB2 N5 82.95(9) . . . ? O8 TB2 N6 76.11(8) . . . ? O8 TB2 O11 86.76(9) . . . ? O8 TB2 O13 146.52(8) . . . ? O8 TB2 O14 145.11(9) . . . ? O8 TB2 O15 76.19(9) . . . ? O9 TB2 N5 65.04(9) . . . ? O9 TB2 N6 127.66(9) . . . ? O9 TB2 O11 165.69(9) . . . ? O9 TB2 O13 99.76(9) . . . ? O9 TB2 O14 79.8(1) . . . ? O9 TB2 O15 84.6(1) . . . ? N5 TB2 N6 62.89(9) . . . ? N5 TB2 O11 128.97(8) . . . ? N5 TB2 O13 74.79(9) . . . ? N5 TB2 O14 122.7(1) . . . ? N5 TB2 O15 142.10(9) . . . ? N6 TB2 O11 66.12(8) . . . ? N6 TB2 O13 71.59(8) . . . ? N6 TB2 O14 134.60(8) . . . ? N6 TB2 O15 138.02(9) . . . ? O11 TB2 O13 88.13(9) . . . ? O11 TB2 O14 92.3(1) . . . ? O11 TB2 O15 81.42(9) . . . ? O13 TB2 O14 68.14(8) . . . ? O13 TB2 O15 135.49(9) . . . ? O14 TB2 O15 69.19(9) . . . ? O1 C1 O2 126.8(4) . . . ? O1 C1 C2 115.8(3) . . . ? O2 C1 C2 117.4(3) . . . ? C1 C2 C3 122.6(3) . . . ? C1 C2 N1 115.0(3) . . . ? C3 C2 N1 122.3(3) . . . ? C2 C3 C4 117.7(3) . . . ? C3 C4 C5 119.8(3) . . . ? C4 C5 C6 118.8(3) . . . ? C5 C6 N1 121.3(3) . . . ? C5 C6 C7 123.2(3) . . . ? N1 C6 C7 115.5(3) . . . ? C2 N1 C6 120.1(3) . . . ? C6 C7 C8 123.7(3) . . . ? C6 C7 N2 114.9(3) . . . ? C8 C7 N2 121.4(3) . . . ? C7 C8 C9 118.3(3) . . . ? C8 C9 C10 120.6(3) . . . ? C9 C10 C11 117.5(4) . . . ? C10 C11 N2 123.4(3) . . . ? C10 C11 C12 122.4(3) . . . ? N2 C11 C12 114.1(3) . . . ? C7 N2 C11 118.7(3) . . . ? C11 C12 O3 116.7(3) . . . ? C11 C12 O4 117.4(4) . . . ? O3 C12 O4 125.8(4) . . . ? O5 C13 O6 125.1(3) . . . ? O5 C13 C14 115.1(3) . . . ? O6 C13 C14 119.8(3) . . . ? C13 C14 C15 123.0(3) . . . ? C13 C14 N3 114.2(3) . . . ? C15 C14 N3 122.8(3) . . . ? C14 C15 C16 117.9(3) . . . ? C15 C16 C17 119.7(3) . . . ? C16 C17 C18 119.4(3) . . . ? C17 C18 N3 121.9(3) . . . ? C17 C18 C19 124.1(3) . . . ? N3 C18 C19 114.1(3) . . . ? C14 N3 C18 118.4(3) . . . ? C18 C19 C20 123.0(3) . . . ? C18 C19 N4 115.2(3) . . . ? C20 C19 N4 121.8(3) . . . ? C19 C20 C21 119.0(3) . . . ? C20 C21 C22 119.6(3) . . . ? C21 C22 C23 117.7(3) . . . ? C22 C23 N4 123.1(3) . . . ? C22 C23 C24 122.4(3) . . . ? N4 C23 C24 114.4(3) . . . ? C19 N4 C23 118.8(3) . . . ? C23 C24 O7 117.4(3) . . . ? C23 C24 O8 116.4(3) . . . ? O7 C24 O8 126.2(3) . . . ? O9 C25 O10 125.3(3) . . . ? O9 C25 C26 116.3(3) . . . ? O10 C25 C26 118.3(3) . . . ? C25 C26 C27 123.1(3) . . . ? C25 C26 N5 114.0(3) . . . ? C27 C26 N5 122.8(3) . . . ? C26 C27 C28 118.1(3) . . . ? C27 C28 C29 119.1(3) . . . ? C28 C29 C30 119.3(3) . . . ? C29 C30 N5 121.6(3) . . . ? C29 C30 C31 123.3(3) . . . ? N5 C30 C31 115.1(3) . . . ? C26 N5 C30 119.0(3) . . . ? C30 C31 C32 123.1(3) . . . ? C30 C31 N6 114.7(3) . . . ? C32 C31 N6 122.0(3) . . . ? C31 C32 C33 118.8(3) . . . ? C32 C33 C34 119.4(3) . . . ? C33 C34 C35 118.3(3) . . . ? C34 C35 N6 122.6(3) . . . ? C34 C35 C36 122.5(3) . . . ? N6 C35 C36 114.8(3) . . . ? C31 N6 C35 118.8(3) . . . ? C35 C36 O11 115.4(3) . . . ? C35 C36 O12 119.6(3) . . . ? O11 C36 O12 125.0(3) . . . ?