# Supplementary Material (ESI) for Organic & Biomolecular Chemistry # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Org.Biomol.Chem. _journal_coden_cambridge 0177 loop_ _publ_author_name _publ_author_address 'Coluccini, C.' 'Dept. of Organic Chemistry, University of Pavia, Italy' 'Dondi, D.' 'Dept. of General Chemistry, University of Pavia, Italy' M.Caricato 'Dept. of Organic Chemistry, University of Pavia, Italy' A.Taglietti 'Dept. of General Chemistry, University of Pavia, Italy' M.Boiocchi 'Centro Grandi Strumenti, University of Pavia, Italy' D.Pasini 'Dept. of Organic Chemistry, University of Pavia, Italy' _publ_contact_author ; Dario Pasini ; _publ_contact_author_email dario.pasini@unipv.it _publ_section_title ; Structurally-Variable, Rigid and Optically-Active D2 and D3 Macrocycles Possessing Recognition Properties towards C60 ; _publ_contact_author_name 'Dario Pasini' data_3b _database_code_depnum_ccdc_archive 'CCDC 746582' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ;bis(bis(2-methoxy-3-methyl-naphthyl)-isophthalate) bis(acetone) solvate ; _chemical_melting_point ? _chemical_formula_moiety 'C64 H48 O12, 2(C3 H6 O)' _chemical_formula_sum 'C70 H60 O14' _chemical_formula_weight 1125.18 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.423(2) _cell_length_b 10.230(3) _cell_length_c 27.358(6) _cell_angle_alpha 90.00 _cell_angle_beta 93.50(2) _cell_angle_gamma 90.00 _cell_volume 2911.7(12) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 6 _cell_measurement_theta_max 12 _exptl_crystal_description irregular _exptl_crystal_colour colorless _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.283 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1184 _exptl_absorpt_coefficient_mu 0.089 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.8952 _exptl_absorpt_correction_T_max 0.9865 _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4' _diffrn_measurement_method 'omega scans' _diffrn_standards_number 3 _diffrn_standards_interval_time 333 _diffrn_standards_decay_% 0 _diffrn_reflns_number 5970 _diffrn_reflns_av_R_equivalents 0.0382 _diffrn_reflns_av_sigmaI/netI 0.0854 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 25.08 _reflns_number_total 5506 _reflns_number_gt 2935 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SIR-97 (Altomare et al.,1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0940P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5506 _refine_ls_number_parameters 754 _refine_ls_number_restraints 37 _refine_ls_R_factor_all 0.1470 _refine_ls_R_factor_gt 0.0689 _refine_ls_wR_factor_ref 0.1980 _refine_ls_wR_factor_gt 0.1588 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.001 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 C1 C 0.9469(8) 0.5752(9) 0.6491(3) 0.054(2) Uani 1 1 d . . . C2 C 0.9970(8) 0.5025(9) 0.6929(3) 0.060(2) Uani 1 1 d . . . C3 C 1.0547(8) 0.3807(9) 0.6900(3) 0.057(2) Uani 1 1 d . . . H3 H 1.0658 0.3432 0.6596 0.068 Uiso 1 1 calc R . . C4 C 1.0957(8) 0.3151(9) 0.7323(3) 0.062(2) Uani 1 1 d . . . C5 C 1.0827(11) 0.3716(11) 0.7771(3) 0.084(3) Uani 1 1 d . . . H5 H 1.1107 0.3274 0.8055 0.101 Uiso 1 1 calc R . . C6 C 1.0281(13) 0.4939(12) 0.7802(4) 0.100(4) Uani 1 1 d . . . H6 H 1.0221 0.5343 0.8104 0.120 Uiso 1 1 calc R . . C7 C 0.9825(10) 0.5556(11) 0.7377(3) 0.084(3) Uani 1 1 d . . . H7 H 0.9408 0.6356 0.7398 0.101 Uiso 1 1 calc R . . C8 C 1.1544(9) 0.1819(10) 0.7280(3) 0.068(3) Uani 1 1 d . . . C9 C 1.2551(9) 0.0060(9) 0.7718(3) 0.071(3) Uani 1 1 d . . . H9A H 1.3407 0.0164 0.7603 0.085 Uiso 1 1 calc R . . H9B H 1.2086 -0.0571 0.7510 0.085 Uiso 1 1 calc R . . C10 C 1.2623(9) -0.0389(9) 0.8241(3) 0.062(2) Uani 1 1 d . . . C11 C 1.3577(8) 0.0090(9) 0.8555(3) 0.065(2) Uani 1 1 d . . . H11 H 1.4158 0.0695 0.8444 0.078 Uiso 1 1 calc R . . C12 C 1.3687(8) -0.0318(9) 0.9043(3) 0.059(2) Uani 1 1 d . . . C13 C 1.4690(8) 0.0209(11) 0.9379(3) 0.075(3) Uani 1 1 d . . . H13 H 1.5270 0.0812 0.9266 0.090 Uiso 1 1 calc R . . C14 C 1.4791(9) -0.0157(12) 0.9846(4) 0.083(3) Uani 1 1 d . . . H14 H 1.5436 0.0195 1.0056 0.100 Uiso 1 1 calc R . . C15 C 1.3945(8) -0.1057(12) 1.0021(3) 0.078(3) Uani 1 1 d . . . H15 H 1.4019 -0.1292 1.0350 0.094 Uiso 1 1 calc R . . C16 C 1.2997(8) -0.1612(9) 0.9718(3) 0.058(2) Uani 1 1 d . . . H16 H 1.2458 -0.2242 0.9840 0.069 Uiso 1 1 calc R . . C17 C 1.2837(7) -0.1227(9) 0.9220(3) 0.054(2) Uani 1 1 d . . . C18 C 1.1831(7) -0.1712(8) 0.8890(3) 0.050(2) Uani 1 1 d . . . C19 C 1.1758(8) -0.1326(8) 0.8420(3) 0.055(2) Uani 1 1 d . . . C20 C 1.0832(8) -0.2636(9) 0.9071(3) 0.051(2) Uani 1 1 d . . . C21 C 1.1105(9) -0.3986(9) 0.9143(3) 0.058(2) Uani 1 1 d . . . C22 C 1.2353(9) -0.4538(10) 0.9084(3) 0.065(3) Uani 1 1 d . . . H22 H 1.3033 -0.4003 0.9007 0.079 Uiso 1 1 calc R . . C23 C 1.2533(11) -0.5831(11) 0.9140(4) 0.084(3) Uani 1 1 d . . . H23 H 1.3349 -0.6165 0.9098 0.100 Uiso 1 1 calc R . . C24 C 1.1594(14) -0.6678(12) 0.9253(4) 0.101(4) Uani 1 1 d . . . H24 H 1.1761 -0.7569 0.9284 0.122 Uiso 1 1 calc R . . C25 C 1.0395(13) -0.6191(12) 0.9323(4) 0.094(4) Uani 1 1 d . . . H25 H 0.9751 -0.6761 0.9408 0.113 Uiso 1 1 calc R . . C26 C 1.0111(10) -0.4861(10) 0.9269(3) 0.070(3) Uani 1 1 d . . . C27 C 0.8885(9) -0.4329(12) 0.9344(3) 0.074(3) Uani 1 1 d . . . H27 H 0.8236 -0.4878 0.9441 0.089 Uiso 1 1 calc R . . C28 C 0.8638(9) -0.3061(11) 0.9280(3) 0.065(3) Uani 1 1 d . . . C29 C 0.9615(9) -0.2176(9) 0.9138(3) 0.058(2) Uani 1 1 d . . . C30 C 0.7304(8) -0.2508(12) 0.9348(3) 0.074(3) Uani 1 1 d . . . H30A H 0.6811 -0.3108 0.9537 0.089 Uiso 1 1 calc R . . H30B H 0.7369 -0.1678 0.9520 0.089 Uiso 1 1 calc R . . C31 C 0.5767(8) -0.3136(12) 0.8707(3) 0.068(3) Uani 1 1 d . . . C32 C 0.5323(8) -0.2912(10) 0.8188(3) 0.064(2) Uani 1 1 d . . . C33 C 0.5975(8) -0.2159(9) 0.7872(3) 0.059(2) Uani 1 1 d . . . H33 H 0.6722 -0.1733 0.7986 0.070 Uiso 1 1 calc R . . C34 C 0.5549(7) -0.2021(9) 0.7389(3) 0.056(2) Uani 1 1 d . . . C35 C 0.4436(10) -0.2641(13) 0.7224(4) 0.092(4) Uani 1 1 d . . . H35 H 0.4151 -0.2578 0.6896 0.110 Uiso 1 1 calc R . . C36 C 0.3752(10) -0.3346(14) 0.7539(4) 0.101(4) Uani 1 1 d . . . H36 H 0.2972 -0.3717 0.7429 0.121 Uiso 1 1 calc R . . C37 C 0.4194(9) -0.3521(13) 0.8019(3) 0.091(4) Uani 1 1 d . . . H37 H 0.3740 -0.4041 0.8228 0.110 Uiso 1 1 calc R . . C38 C 0.6339(9) -0.1268(10) 0.7058(3) 0.063(2) Uani 1 1 d . . . C39 C 0.6709(8) -0.0882(9) 0.6222(3) 0.062(2) Uani 1 1 d . . . H39A H 0.6860 -0.1522 0.5971 0.074 Uiso 1 1 calc R . . H39B H 0.7536 -0.0624 0.6374 0.074 Uiso 1 1 calc R . . C40 C 0.6043(7) 0.0312(7) 0.5988(3) 0.0438(18) Uani 1 1 d . . . C41 C 0.4742(7) 0.0537(8) 0.5996(3) 0.049(2) Uani 1 1 d . . . H41 H 0.4247 -0.0018 0.6177 0.059 Uiso 1 1 calc R . . C42 C 0.4148(7) 0.1564(8) 0.5741(2) 0.0464(19) Uani 1 1 d . . . C43 C 0.2810(7) 0.1807(9) 0.5747(3) 0.057(2) Uani 1 1 d . . . H43 H 0.2308 0.1282 0.5937 0.068 Uiso 1 1 calc R . . C44 C 0.2240(8) 0.2819(9) 0.5474(3) 0.060(2) Uani 1 1 d . . . H44 H 0.1368 0.2986 0.5493 0.072 Uiso 1 1 calc R . . C45 C 0.2956(7) 0.3579(9) 0.5174(3) 0.059(2) Uani 1 1 d . . . H45 H 0.2554 0.4224 0.4980 0.071 Uiso 1 1 calc R . . C46 C 0.4264(7) 0.3386(8) 0.5162(3) 0.0501(19) Uani 1 1 d . . . H46 H 0.4744 0.3911 0.4963 0.060 Uiso 1 1 calc R . . C47 C 0.4879(7) 0.2391(7) 0.5450(3) 0.0424(18) Uani 1 1 d . . . C48 C 0.6245(7) 0.2233(7) 0.5461(2) 0.0401(17) Uani 1 1 d . . . C49 C 0.6770(7) 0.1194(8) 0.5727(3) 0.0470(19) Uani 1 1 d . . . C50 C 0.7147(6) 0.3120(7) 0.5219(2) 0.0349(16) Uani 1 1 d . . . C51 C 0.7479(7) 0.2892(7) 0.4731(3) 0.0443(19) Uani 1 1 d . . . C52 C 0.6902(8) 0.1901(8) 0.4427(3) 0.054(2) Uani 1 1 d . . . H52 H 0.6304 0.1341 0.4555 0.065 Uiso 1 1 calc R . . C53 C 0.7201(8) 0.1757(9) 0.3961(3) 0.058(2) Uani 1 1 d . . . H53 H 0.6806 0.1100 0.3772 0.070 Uiso 1 1 calc R . . C54 C 0.8107(8) 0.2583(9) 0.3752(3) 0.060(2) Uani 1 1 d . . . H54 H 0.8283 0.2500 0.3424 0.073 Uiso 1 1 calc R . . C55 C 0.8714(7) 0.3502(9) 0.4041(3) 0.057(2) Uani 1 1 d . . . H55 H 0.9328 0.4030 0.3906 0.068 Uiso 1 1 calc R . . C56 C 0.8454(7) 0.3683(8) 0.4529(3) 0.0488(19) Uani 1 1 d . . . C57 C 0.9102(7) 0.4630(8) 0.4842(3) 0.0483(19) Uani 1 1 d . . . H57 H 0.9790 0.5094 0.4728 0.058 Uiso 1 1 calc R . . C58 C 0.8735(7) 0.4861(8) 0.5298(3) 0.0479(19) Uani 1 1 d . . . C59 C 0.7685(7) 0.4141(8) 0.5476(2) 0.0422(18) Uani 1 1 d . . . C60 C 0.9419(8) 0.5873(8) 0.5623(3) 0.056(2) Uani 1 1 d . . . H60A H 1.0138 0.6235 0.5459 0.067 Uiso 1 1 calc R . . H60B H 0.8834 0.6580 0.5688 0.067 Uiso 1 1 calc R . . C61 C 0.9779(9) -0.1084(12) 0.7931(3) 0.091(4) Uani 1 1 d . . . H61A H 0.9103 -0.1199 0.8150 0.137 Uiso 1 1 calc R . . H61B H 0.9480 -0.1346 0.7606 0.137 Uiso 1 1 calc R . . H61C H 1.0028 -0.0181 0.7927 0.137 Uiso 1 1 calc R . . C62 C 0.9739(12) 0.0013(12) 0.9415(4) 0.111(4) Uani 1 1 d . . . H62A H 0.9047 0.0278 0.9609 0.167 Uiso 1 1 calc R . . H62B H 1.0073 0.0763 0.9254 0.167 Uiso 1 1 calc R . . H62C H 1.0409 -0.0377 0.9623 0.167 Uiso 1 1 calc R . . C63 C 0.8850(7) 0.1579(9) 0.6122(3) 0.063(2) Uani 1 1 d . . . H63A H 0.8803 0.2511 0.6084 0.095 Uiso 1 1 calc R . . H63B H 0.9729 0.1302 0.6117 0.095 Uiso 1 1 calc R . . H63C H 0.8515 0.1334 0.6428 0.095 Uiso 1 1 calc R . . C64 C 0.6313(9) 0.5382(10) 0.5949(4) 0.083(3) Uani 1 1 d . . . H64A H 0.6458 0.6068 0.5719 0.124 Uiso 1 1 calc R . . H64B H 0.6297 0.5744 0.6272 0.124 Uiso 1 1 calc R . . H64C H 0.5505 0.4966 0.5862 0.124 Uiso 1 1 calc R . . O1 O 0.9872(5) 0.5278(5) 0.60730(19) 0.0569(14) Uani 1 1 d . . . O2 O 0.8842(6) 0.6741(7) 0.6513(2) 0.0784(18) Uani 1 1 d . . . O3 O 1.1886(6) 0.1295(6) 0.77083(19) 0.0710(17) Uani 1 1 d . . . O4 O 1.1678(7) 0.1275(8) 0.6896(2) 0.092(2) Uani 1 1 d . . . O5 O 1.0864(6) -0.1870(6) 0.80919(19) 0.0664(17) Uani 1 1 d . . . O6 O 0.9282(6) -0.0904(7) 0.9061(2) 0.0733(17) Uani 1 1 d . . . O7 O 0.6670(6) -0.2327(7) 0.8851(2) 0.0770(19) Uani 1 1 d . . . O8 O 0.5360(7) -0.3965(10) 0.8968(2) 0.117(3) Uani 1 1 d . . . O9 O 0.5950(5) -0.1459(6) 0.65838(19) 0.0647(16) Uani 1 1 d . . . O10 O 0.7222(7) -0.0573(8) 0.7191(2) 0.095(2) Uani 1 1 d . . . O11 O 0.8095(5) 0.0956(5) 0.57214(18) 0.0541(14) Uani 1 1 d . . . O12 O 0.7320(5) 0.4445(5) 0.59382(18) 0.0532(14) Uani 1 1 d . . . C65 C 0.436(2) 0.368(3) 0.6879(10) 0.258(12) Uani 1 1 d U . . H65A H 0.3485 0.3408 0.6900 0.388 Uiso 1 1 calc R . . H65B H 0.4567 0.3705 0.6542 0.388 Uiso 1 1 calc R . . H65C H 0.4474 0.4535 0.7020 0.388 Uiso 1 1 calc R . . C66 C 0.526(2) 0.271(3) 0.7160(9) 0.186(8) Uani 1 1 d U . . C67 C 0.655(2) 0.284(3) 0.7043(7) 0.213(10) Uani 1 1 d U . . H67A H 0.7064 0.3105 0.7329 0.319 Uiso 1 1 calc R . . H67B H 0.6610 0.3489 0.6792 0.319 Uiso 1 1 calc R . . H67C H 0.6861 0.2019 0.6928 0.319 Uiso 1 1 calc R . . O13 O 0.504(2) 0.209(3) 0.7520(10) 0.387(18) Uani 1 1 d U . . C68 C 0.746(3) 0.138(3) 0.8299(8) 0.259(12) Uani 1 1 d U . . H68A H 0.8357 0.1332 0.8248 0.389 Uiso 1 1 calc R . . H68B H 0.6978 0.1463 0.7990 0.389 Uiso 1 1 calc R . . H68C H 0.7195 0.0595 0.8460 0.389 Uiso 1 1 calc R . . C69 C 0.722(2) 0.246(3) 0.8593(8) 0.193(9) Uani 1 1 d U . . C70 C 0.6552(13) 0.3634(13) 0.8374(5) 0.38(2) Uani 1 1 d U . . H70A H 0.5893 0.3912 0.8580 0.573 Uiso 1 1 calc R . . H70B H 0.6174 0.3417 0.8055 0.573 Uiso 1 1 calc R . . H70C H 0.7164 0.4327 0.8344 0.573 Uiso 1 1 calc R . . O14 O 0.7319(13) 0.2321(13) 0.9060(5) 0.192(5) Uani 1 1 d U . . 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 C1 0.046(5) 0.049(5) 0.066(6) -0.005(5) -0.004(4) -0.008(5) C2 0.064(6) 0.055(6) 0.060(5) -0.003(5) -0.008(4) -0.012(5) C3 0.064(5) 0.056(6) 0.050(5) -0.004(4) -0.002(4) -0.013(5) C4 0.065(6) 0.063(6) 0.055(5) 0.009(5) -0.013(4) -0.008(5) C5 0.135(9) 0.073(7) 0.043(5) 0.008(5) -0.014(5) -0.002(7) C6 0.157(12) 0.077(8) 0.065(7) -0.017(6) 0.001(7) -0.002(8) C7 0.109(8) 0.079(7) 0.064(6) -0.005(6) -0.005(5) 0.009(7) C8 0.082(6) 0.071(7) 0.049(5) 0.013(5) -0.005(5) -0.004(6) C9 0.083(7) 0.056(6) 0.073(6) 0.015(5) -0.004(5) -0.002(6) C10 0.068(6) 0.059(6) 0.058(5) 0.013(4) -0.004(4) -0.006(5) C11 0.066(6) 0.057(6) 0.071(6) 0.020(5) 0.004(5) -0.019(5) C12 0.046(5) 0.056(5) 0.072(6) -0.004(5) -0.014(4) -0.005(5) C13 0.062(6) 0.089(7) 0.073(6) -0.001(6) -0.006(5) -0.029(6) C14 0.053(6) 0.115(9) 0.080(7) -0.020(7) -0.012(5) -0.009(7) C15 0.058(6) 0.119(9) 0.056(5) -0.005(6) -0.013(4) 0.009(7) C16 0.055(5) 0.068(6) 0.050(4) 0.000(4) -0.005(4) -0.003(5) C17 0.043(5) 0.061(5) 0.057(5) 0.003(4) -0.008(4) 0.004(5) C18 0.046(4) 0.056(5) 0.045(4) 0.004(4) -0.009(3) -0.006(4) C19 0.061(5) 0.050(5) 0.051(4) 0.010(4) -0.014(4) -0.005(5) C20 0.052(5) 0.061(6) 0.041(4) 0.010(4) -0.008(4) -0.004(5) C21 0.059(5) 0.062(6) 0.051(5) -0.003(4) -0.012(4) -0.008(5) C22 0.069(6) 0.064(7) 0.062(5) 0.010(5) -0.004(5) -0.012(5) C23 0.085(8) 0.069(7) 0.096(8) -0.001(6) -0.003(6) 0.001(7) C24 0.126(11) 0.062(7) 0.115(9) 0.011(7) -0.008(8) -0.018(9) C25 0.094(9) 0.078(9) 0.110(9) 0.018(7) 0.002(7) -0.025(7) C26 0.076(7) 0.064(7) 0.069(6) 0.021(5) -0.018(5) -0.019(6) C27 0.058(6) 0.103(9) 0.059(5) 0.032(6) -0.004(4) -0.024(6) C28 0.056(6) 0.090(8) 0.047(5) 0.016(5) -0.014(4) -0.014(6) C29 0.060(6) 0.066(6) 0.046(5) -0.002(4) -0.008(4) -0.011(5) C30 0.052(5) 0.109(8) 0.058(5) 0.007(5) -0.010(4) -0.005(6) C31 0.038(5) 0.108(8) 0.057(5) 0.002(6) -0.009(4) -0.015(6) C32 0.043(5) 0.089(7) 0.059(5) 0.015(5) -0.002(4) -0.013(5) C33 0.043(5) 0.074(6) 0.057(5) 0.017(5) -0.015(4) -0.004(5) C34 0.040(5) 0.068(6) 0.060(5) 0.007(5) -0.006(4) -0.002(5) C35 0.077(7) 0.128(10) 0.067(6) 0.034(6) -0.017(5) -0.026(7) C36 0.072(7) 0.149(11) 0.080(7) 0.024(7) -0.007(5) -0.071(8) C37 0.060(6) 0.143(11) 0.070(6) 0.008(7) -0.003(5) -0.043(7) C38 0.062(6) 0.065(6) 0.059(5) 0.020(5) -0.013(4) 0.002(5) C39 0.069(5) 0.060(6) 0.057(5) 0.019(4) 0.003(4) 0.002(5) C40 0.051(5) 0.035(4) 0.044(4) 0.000(4) -0.006(3) -0.005(4) C41 0.044(5) 0.043(5) 0.060(5) 0.015(4) 0.002(4) -0.009(4) C42 0.043(4) 0.058(5) 0.037(4) 0.005(4) -0.004(3) -0.011(4) C43 0.039(5) 0.058(5) 0.073(5) 0.001(5) 0.004(4) -0.007(4) C44 0.036(4) 0.064(6) 0.080(6) 0.007(5) 0.003(4) 0.003(5) C45 0.035(4) 0.052(5) 0.089(6) 0.018(5) -0.010(4) -0.003(4) C46 0.053(5) 0.042(5) 0.055(4) 0.009(4) 0.000(4) -0.004(4) C47 0.042(4) 0.029(4) 0.055(4) 0.001(3) -0.007(3) 0.003(4) C48 0.038(4) 0.039(4) 0.042(4) -0.001(3) -0.007(3) -0.007(4) C49 0.046(5) 0.049(5) 0.044(4) -0.005(4) -0.004(3) 0.004(4) C50 0.027(3) 0.031(4) 0.046(4) 0.005(3) -0.004(3) 0.001(3) C51 0.037(4) 0.039(4) 0.055(5) 0.014(4) -0.010(3) 0.005(4) C52 0.053(5) 0.047(5) 0.061(5) -0.003(4) -0.012(4) -0.007(4) C53 0.067(6) 0.055(5) 0.052(5) 0.005(4) -0.011(4) 0.005(5) C54 0.062(6) 0.073(6) 0.045(4) 0.004(5) -0.005(4) 0.019(5) C55 0.045(5) 0.071(6) 0.055(5) 0.017(5) 0.008(4) 0.010(5) C56 0.045(4) 0.049(5) 0.053(4) 0.015(4) 0.002(4) 0.002(4) C57 0.046(4) 0.046(5) 0.052(5) 0.013(4) -0.006(4) -0.001(4) C58 0.047(5) 0.038(4) 0.058(5) 0.017(4) -0.004(4) -0.004(4) C59 0.045(4) 0.045(4) 0.037(4) 0.007(4) 0.001(3) 0.005(4) C60 0.065(5) 0.043(5) 0.058(5) 0.015(4) -0.010(4) -0.019(4) C61 0.078(7) 0.109(9) 0.082(6) 0.012(7) -0.039(5) -0.016(7) C62 0.129(10) 0.082(8) 0.118(9) -0.031(8) -0.029(8) 0.006(8) C63 0.042(5) 0.062(6) 0.082(6) -0.018(5) -0.015(4) 0.002(4) C64 0.061(6) 0.078(7) 0.108(8) -0.021(6) -0.008(5) 0.021(6) O1 0.056(3) 0.056(3) 0.057(3) 0.010(3) -0.011(3) -0.006(3) O2 0.079(4) 0.076(5) 0.079(4) 0.007(4) -0.005(3) 0.002(4) O3 0.090(4) 0.066(4) 0.055(3) 0.015(3) -0.007(3) 0.001(4) O4 0.138(6) 0.081(5) 0.056(4) 0.008(4) -0.005(4) 0.020(5) O5 0.078(4) 0.063(4) 0.056(3) 0.004(3) -0.020(3) -0.014(3) O6 0.068(4) 0.066(4) 0.084(4) 0.008(4) -0.012(3) 0.008(4) O7 0.071(4) 0.100(5) 0.057(3) 0.012(4) -0.015(3) -0.009(4) O8 0.096(5) 0.171(9) 0.079(5) 0.047(6) -0.022(4) -0.074(6) O9 0.070(4) 0.064(4) 0.058(3) 0.023(3) -0.010(3) -0.003(3) O10 0.090(5) 0.109(6) 0.083(4) 0.014(4) -0.013(4) -0.038(5) O11 0.043(3) 0.053(3) 0.065(3) 0.000(3) -0.005(2) 0.000(3) O12 0.052(3) 0.048(3) 0.060(3) -0.004(3) 0.002(3) 0.007(3) C65 0.17(2) 0.27(3) 0.33(3) -0.03(3) 0.05(2) 0.00(2) C66 0.104(14) 0.25(3) 0.20(2) -0.009(18) 0.007(13) 0.019(16) C67 0.162(18) 0.29(3) 0.193(18) 0.032(19) 0.028(14) 0.01(2) O13 0.32(2) 0.46(4) 0.39(3) 0.22(3) 0.11(2) -0.04(3) C68 0.35(3) 0.21(2) 0.22(2) -0.10(2) -0.01(2) 0.10(2) C69 0.24(2) 0.19(2) 0.137(15) -0.049(16) -0.049(16) -0.016(18) C70 0.56(5) 0.23(3) 0.34(4) 0.05(3) -0.08(4) 0.17(4) O14 0.203(13) 0.173(12) 0.203(13) -0.037(11) 0.032(11) -0.035(10) _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 C1 O2 1.208(10) . ? C1 O1 1.334(10) . ? C1 C2 1.477(12) . ? C2 C7 1.358(12) . ? C2 C3 1.387(12) . ? C3 C4 1.383(11) . ? C3 H3 0.9300 . ? C4 C5 1.368(12) . ? C4 C8 1.501(13) . ? C5 C6 1.379(15) . ? C5 H5 0.9300 . ? C6 C7 1.381(14) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 O4 1.203(10) . ? C8 O3 1.319(9) . ? C9 O3 1.441(11) . ? C9 C10 1.500(11) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.365(11) . ? C10 C19 1.424(11) . ? C11 C12 1.396(11) . ? C11 H11 0.9300 . ? C12 C17 1.391(11) . ? C12 C13 1.453(11) . ? C13 C14 1.329(12) . ? C13 H13 0.9300 . ? C14 C15 1.380(14) . ? C14 H14 0.9300 . ? C15 C16 1.374(11) . ? C15 H15 0.9300 . ? C16 C17 1.418(10) . ? C16 H16 0.9300 . ? C17 C18 1.431(10) . ? C18 C19 1.342(10) . ? C18 C20 1.512(11) . ? C19 O5 1.372(9) . ? C20 C29 1.376(12) . ? C20 C21 1.421(12) . ? C21 C26 1.427(12) . ? C21 C22 1.436(12) . ? C22 C23 1.343(14) . ? C22 H22 0.9300 . ? C23 C24 1.358(15) . ? C23 H23 0.9300 . ? C24 C25 1.369(16) . ? C24 H24 0.9300 . ? C25 C26 1.398(16) . ? C25 H25 0.9300 . ? C26 C27 1.416(14) . ? C27 C28 1.332(14) . ? C27 H27 0.9300 . ? C28 C29 1.434(13) . ? C28 C30 1.523(13) . ? C29 O6 1.360(11) . ? C30 O7 1.488(9) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 O8 1.202(12) . ? C31 O7 1.296(11) . ? C31 C32 1.484(11) . ? C32 C33 1.370(11) . ? C32 C37 1.387(12) . ? C33 C34 1.374(10) . ? C33 H33 0.9300 . ? C34 C35 1.375(12) . ? C34 C38 1.479(12) . ? C35 C36 1.359(13) . ? C35 H35 0.9300 . ? C36 C37 1.377(12) . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? C38 O10 1.202(10) . ? C38 O9 1.348(9) . ? C39 O9 1.431(9) . ? C39 C40 1.526(11) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 C41 1.377(10) . ? C40 C49 1.402(10) . ? C41 C42 1.386(10) . ? C41 H41 0.9300 . ? C42 C47 1.416(10) . ? C42 C43 1.417(10) . ? C43 C44 1.389(12) . ? C43 H43 0.9300 . ? C44 C45 1.382(11) . ? C44 H44 0.9300 . ? C45 C46 1.381(10) . ? C45 H45 0.9300 . ? C46 C47 1.417(10) . ? C46 H46 0.9300 . ? C47 C48 1.431(9) . ? C48 C49 1.381(10) . ? C48 C50 1.491(10) . ? C49 O11 1.404(9) . ? C50 C59 1.360(10) . ? C50 C51 1.421(10) . ? C51 C52 1.420(11) . ? C51 C56 1.435(10) . ? C52 C53 1.339(10) . ? C52 H52 0.9300 . ? C53 C54 1.414(12) . ? C53 H53 0.9300 . ? C54 C55 1.358(12) . ? C54 H54 0.9300 . ? C55 C56 1.393(10) . ? C55 H55 0.9300 . ? C56 C57 1.434(11) . ? C57 C58 1.350(10) . ? C57 H57 0.9300 . ? C58 C59 1.428(10) . ? C58 C60 1.514(10) . ? C59 O12 1.378(8) . ? C60 O1 1.428(8) . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? C61 O5 1.435(11) . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? C62 O6 1.411(12) . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? C63 O11 1.455(9) . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? C64 O12 1.423(10) . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? C65 C66 1.54(3) . ? C65 H65A 0.9600 . ? C65 H65B 0.9600 . ? C65 H65C 0.9600 . ? C66 O13 1.20(3) . ? C66 C67 1.41(2) . ? C67 H67A 0.9600 . ? C67 H67B 0.9600 . ? C67 H67C 0.9600 . ? C68 C69 1.40(3) . ? C68 H68A 0.9600 . ? C68 H68B 0.9600 . ? C68 H68C 0.9600 . ? C69 O14 1.28(2) . ? C69 C70 1.49(3) . ? C70 H70A 0.9600 . ? C70 H70B 0.9600 . ? C70 H70C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 C1 O1 123.1(8) . . ? O2 C1 C2 123.2(9) . . ? O1 C1 C2 113.4(8) . . ? C7 C2 C3 118.8(8) . . ? C7 C2 C1 118.5(9) . . ? C3 C2 C1 122.7(8) . . ? C4 C3 C2 120.1(8) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C5 C4 C3 120.1(9) . . ? C5 C4 C8 121.2(8) . . ? C3 C4 C8 118.7(8) . . ? C4 C5 C6 120.1(9) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C5 C6 C7 119.0(10) . . ? C5 C6 H6 120.5 . . ? C7 C6 H6 120.5 . . ? C2 C7 C6 121.7(10) . . ? C2 C7 H7 119.2 . . ? C6 C7 H7 119.2 . . ? O4 C8 O3 123.2(9) . . ? O4 C8 C4 124.0(8) . . ? O3 C8 C4 112.8(8) . . ? O3 C9 C10 106.4(7) . . ? O3 C9 H9A 110.5 . . ? C10 C9 H9A 110.5 . . ? O3 C9 H9B 110.5 . . ? C10 C9 H9B 110.5 . . ? H9A C9 H9B 108.6 . . ? C11 C10 C19 118.5(7) . . ? C11 C10 C9 118.9(8) . . ? C19 C10 C9 122.6(8) . . ? C10 C11 C12 120.6(8) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C17 C12 C11 121.0(7) . . ? C17 C12 C13 118.5(8) . . ? C11 C12 C13 120.5(8) . . ? C14 C13 C12 121.0(9) . . ? C14 C13 H13 119.5 . . ? C12 C13 H13 119.5 . . ? C13 C14 C15 120.5(9) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C16 C15 C14 121.1(9) . . ? C16 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? C15 C16 C17 120.2(9) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C12 C17 C16 118.7(7) . . ? C12 C17 C18 118.0(7) . . ? C16 C17 C18 123.3(8) . . ? C19 C18 C17 119.9(8) . . ? C19 C18 C20 119.9(7) . . ? C17 C18 C20 120.2(7) . . ? C18 C19 O5 120.2(7) . . ? C18 C19 C10 121.9(7) . . ? O5 C19 C10 117.8(7) . . ? C29 C20 C21 119.5(8) . . ? C29 C20 C18 119.2(8) . . ? C21 C20 C18 121.2(8) . . ? C20 C21 C26 120.1(9) . . ? C20 C21 C22 122.8(9) . . ? C26 C21 C22 117.1(8) . . ? C23 C22 C21 119.7(10) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C22 C23 C24 123.8(12) . . ? C22 C23 H23 118.1 . . ? C24 C23 H23 118.1 . . ? C23 C24 C25 118.4(11) . . ? C23 C24 H24 120.8 . . ? C25 C24 H24 120.8 . . ? C24 C25 C26 121.9(11) . . ? C24 C25 H25 119.0 . . ? C26 C25 H25 119.0 . . ? C25 C26 C27 123.1(10) . . ? C25 C26 C21 118.9(10) . . ? C27 C26 C21 118.0(9) . . ? C28 C27 C26 121.6(9) . . ? C28 C27 H27 119.2 . . ? C26 C27 H27 119.2 . . ? C27 C28 C29 121.1(10) . . ? C27 C28 C30 121.1(10) . . ? C29 C28 C30 117.9(10) . . ? O6 C29 C20 122.4(8) . . ? O6 C29 C28 117.9(9) . . ? C20 C29 C28 119.7(9) . . ? O7 C30 C28 106.9(7) . . ? O7 C30 H30A 110.3 . . ? C28 C30 H30A 110.3 . . ? O7 C30 H30B 110.3 . . ? C28 C30 H30B 110.3 . . ? H30A C30 H30B 108.6 . . ? O8 C31 O7 123.2(8) . . ? O8 C31 C32 125.2(9) . . ? O7 C31 C32 111.6(9) . . ? C33 C32 C37 119.0(8) . . ? C33 C32 C31 123.7(8) . . ? C37 C32 C31 117.3(8) . . ? C32 C33 C34 121.4(8) . . ? C32 C33 H33 119.3 . . ? C34 C33 H33 119.3 . . ? C33 C34 C35 119.1(8) . . ? C33 C34 C38 118.9(7) . . ? C35 C34 C38 121.9(8) . . ? C36 C35 C34 120.1(9) . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C35 C36 C37 121.1(9) . . ? C35 C36 H36 119.5 . . ? C37 C36 H36 119.5 . . ? C36 C37 C32 119.2(9) . . ? C36 C37 H37 120.4 . . ? C32 C37 H37 120.4 . . ? O10 C38 O9 123.9(8) . . ? O10 C38 C34 124.5(8) . . ? O9 C38 C34 111.6(8) . . ? O9 C39 C40 111.4(7) . . ? O9 C39 H39A 109.4 . . ? C40 C39 H39A 109.4 . . ? O9 C39 H39B 109.4 . . ? C40 C39 H39B 109.4 . . ? H39A C39 H39B 108.0 . . ? C41 C40 C49 117.6(7) . . ? C41 C40 C39 123.4(7) . . ? C49 C40 C39 118.9(7) . . ? C40 C41 C42 122.0(7) . . ? C40 C41 H41 119.0 . . ? C42 C41 H41 119.0 . . ? C41 C42 C47 119.7(7) . . ? C41 C42 C43 122.5(7) . . ? C47 C42 C43 117.8(7) . . ? C44 C43 C42 120.9(8) . . ? C44 C43 H43 119.6 . . ? C42 C43 H43 119.6 . . ? C45 C44 C43 120.7(8) . . ? C45 C44 H44 119.6 . . ? C43 C44 H44 119.6 . . ? C46 C45 C44 120.3(8) . . ? C46 C45 H45 119.9 . . ? C44 C45 H45 119.9 . . ? C45 C46 C47 120.2(7) . . ? C45 C46 H46 119.9 . . ? C47 C46 H46 119.9 . . ? C42 C47 C46 120.1(7) . . ? C42 C47 C48 119.3(6) . . ? C46 C47 C48 120.6(7) . . ? C49 C48 C47 117.4(7) . . ? C49 C48 C50 117.5(6) . . ? C47 C48 C50 125.1(6) . . ? C48 C49 C40 123.6(7) . . ? C48 C49 O11 119.1(7) . . ? C40 C49 O11 117.2(7) . . ? C59 C50 C51 119.7(6) . . ? C59 C50 C48 119.3(6) . . ? C51 C50 C48 120.9(6) . . ? C52 C51 C50 123.3(7) . . ? C52 C51 C56 117.6(7) . . ? C50 C51 C56 119.1(7) . . ? C53 C52 C51 121.3(8) . . ? C53 C52 H52 119.3 . . ? C51 C52 H52 119.3 . . ? C52 C53 C54 121.3(8) . . ? C52 C53 H53 119.3 . . ? C54 C53 H53 119.3 . . ? C55 C54 C53 118.5(8) . . ? C55 C54 H54 120.8 . . ? C53 C54 H54 120.8 . . ? C54 C55 C56 122.6(8) . . ? C54 C55 H55 118.7 . . ? C56 C55 H55 118.7 . . ? C55 C56 C57 123.4(7) . . ? C55 C56 C51 118.5(7) . . ? C57 C56 C51 118.1(7) . . ? C58 C57 C56 121.4(7) . . ? C58 C57 H57 119.3 . . ? C56 C57 H57 119.3 . . ? C57 C58 C59 119.4(7) . . ? C57 C58 C60 120.8(7) . . ? C59 C58 C60 119.8(7) . . ? C50 C59 O12 121.2(7) . . ? C50 C59 C58 121.4(7) . . ? O12 C59 C58 117.1(7) . . ? O1 C60 C58 109.5(6) . . ? O1 C60 H60A 109.8 . . ? C58 C60 H60A 109.8 . . ? O1 C60 H60B 109.8 . . ? C58 C60 H60B 109.8 . . ? H60A C60 H60B 108.2 . . ? O5 C61 H61A 109.5 . . ? O5 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? O5 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? O6 C62 H62A 109.5 . . ? O6 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? O6 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? O11 C63 H63A 109.5 . . ? O11 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? O11 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? O12 C64 H64A 109.5 . . ? O12 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? O12 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C1 O1 C60 118.6(7) . . ? C8 O3 C9 118.5(7) . . ? C19 O5 C61 117.7(7) . . ? C29 O6 C62 117.3(7) . . ? C31 O7 C30 118.1(8) . . ? C38 O9 C39 117.2(7) . . ? C49 O11 C63 113.8(6) . . ? C59 O12 C64 114.6(6) . . ? C66 C65 H65A 109.5 . . ? C66 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C66 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? O13 C66 C67 118(3) . . ? O13 C66 C65 127(2) . . ? C67 C66 C65 112(3) . . ? C66 C67 H67A 109.5 . . ? C66 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C66 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C69 C68 H68A 109.5 . . ? C69 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C69 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? O14 C69 C68 118(2) . . ? O14 C69 C70 120(2) . . ? C68 C69 C70 120.0(16) . . ? C69 C70 H70A 109.5 . . ? C69 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C69 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C7 -6.5(13) . . . . ? O1 C1 C2 C7 167.9(8) . . . . ? O2 C1 C2 C3 171.6(8) . . . . ? O1 C1 C2 C3 -14.1(11) . . . . ? C7 C2 C3 C4 0.3(12) . . . . ? C1 C2 C3 C4 -177.7(8) . . . . ? C2 C3 C4 C5 -1.7(13) . . . . ? C2 C3 C4 C8 178.3(8) . . . . ? C3 C4 C5 C6 0.3(16) . . . . ? C8 C4 C5 C6 -179.8(10) . . . . ? C4 C5 C6 C7 2.6(18) . . . . ? C3 C2 C7 C6 2.6(15) . . . . ? C1 C2 C7 C6 -179.3(10) . . . . ? C5 C6 C7 C2 -4.1(18) . . . . ? C5 C4 C8 O4 179.7(10) . . . . ? C3 C4 C8 O4 -0.3(14) . . . . ? C5 C4 C8 O3 0.5(12) . . . . ? C3 C4 C8 O3 -179.5(8) . . . . ? O3 C9 C10 C11 -82.6(10) . . . . ? O3 C9 C10 C19 99.3(9) . . . . ? C19 C10 C11 C12 -0.8(14) . . . . ? C9 C10 C11 C12 -179.1(8) . . . . ? C10 C11 C12 C17 0.4(14) . . . . ? C10 C11 C12 C13 -179.0(9) . . . . ? C17 C12 C13 C14 -0.6(15) . . . . ? C11 C12 C13 C14 178.9(10) . . . . ? C12 C13 C14 C15 0.4(17) . . . . ? C13 C14 C15 C16 1.1(16) . . . . ? C14 C15 C16 C17 -2.5(15) . . . . ? C11 C12 C17 C16 179.7(8) . . . . ? C13 C12 C17 C16 -0.8(12) . . . . ? C11 C12 C17 C18 -1.2(12) . . . . ? C13 C12 C17 C18 178.3(8) . . . . ? C15 C16 C17 C12 2.3(13) . . . . ? C15 C16 C17 C18 -176.7(8) . . . . ? C12 C17 C18 C19 2.5(12) . . . . ? C16 C17 C18 C19 -178.5(8) . . . . ? C12 C17 C18 C20 -176.2(8) . . . . ? C16 C17 C18 C20 2.9(12) . . . . ? C17 C18 C19 O5 174.5(7) . . . . ? C20 C18 C19 O5 -6.9(12) . . . . ? C17 C18 C19 C10 -3.0(13) . . . . ? C20 C18 C19 C10 175.6(8) . . . . ? C11 C10 C19 C18 2.2(13) . . . . ? C9 C10 C19 C18 -179.6(9) . . . . ? C11 C10 C19 O5 -175.4(8) . . . . ? C9 C10 C19 O5 2.8(12) . . . . ? C19 C18 C20 C29 -73.4(10) . . . . ? C17 C18 C20 C29 105.3(9) . . . . ? C19 C18 C20 C21 102.4(9) . . . . ? C17 C18 C20 C21 -78.9(10) . . . . ? C29 C20 C21 C26 1.8(12) . . . . ? C18 C20 C21 C26 -174.0(7) . . . . ? C29 C20 C21 C22 -179.6(7) . . . . ? C18 C20 C21 C22 4.6(12) . . . . ? C20 C21 C22 C23 -177.6(9) . . . . ? C26 C21 C22 C23 1.1(13) . . . . ? C21 C22 C23 C24 -0.3(16) . . . . ? C22 C23 C24 C25 -1.0(18) . . . . ? C23 C24 C25 C26 1.4(18) . . . . ? C24 C25 C26 C27 -179.2(10) . . . . ? C24 C25 C26 C21 -0.6(16) . . . . ? C20 C21 C26 C25 178.0(9) . . . . ? C22 C21 C26 C25 -0.7(13) . . . . ? C20 C21 C26 C27 -3.3(12) . . . . ? C22 C21 C26 C27 178.0(8) . . . . ? C25 C26 C27 C28 -178.5(10) . . . . ? C21 C26 C27 C28 2.9(13) . . . . ? C26 C27 C28 C29 -1.0(14) . . . . ? C26 C27 C28 C30 178.3(7) . . . . ? C21 C20 C29 O6 -178.0(7) . . . . ? C18 C20 C29 O6 -2.1(11) . . . . ? C21 C20 C29 C28 0.2(11) . . . . ? C18 C20 C29 C28 176.1(7) . . . . ? C27 C28 C29 O6 177.6(8) . . . . ? C30 C28 C29 O6 -1.6(11) . . . . ? C27 C28 C29 C20 -0.6(12) . . . . ? C30 C28 C29 C20 -179.9(7) . . . . ? C27 C28 C30 O7 -101.5(10) . . . . ? C29 C28 C30 O7 77.7(10) . . . . ? O8 C31 C32 C33 -165.6(11) . . . . ? O7 C31 C32 C33 13.9(14) . . . . ? O8 C31 C32 C37 13.4(16) . . . . ? O7 C31 C32 C37 -167.1(10) . . . . ? C37 C32 C33 C34 -1.5(15) . . . . ? C31 C32 C33 C34 177.5(9) . . . . ? C32 C33 C34 C35 0.7(14) . . . . ? C32 C33 C34 C38 -175.9(9) . . . . ? C33 C34 C35 C36 2.0(17) . . . . ? C38 C34 C35 C36 178.6(11) . . . . ? C34 C35 C36 C37 -4(2) . . . . ? C35 C36 C37 C32 3(2) . . . . ? C33 C32 C37 C36 -0.5(17) . . . . ? C31 C32 C37 C36 -179.6(11) . . . . ? C33 C34 C38 O10 -13.5(14) . . . . ? C35 C34 C38 O10 169.9(11) . . . . ? C33 C34 C38 O9 166.4(8) . . . . ? C35 C34 C38 O9 -10.2(13) . . . . ? O9 C39 C40 C41 -20.5(10) . . . . ? O9 C39 C40 C49 163.3(7) . . . . ? C49 C40 C41 C42 2.3(11) . . . . ? C39 C40 C41 C42 -173.9(7) . . . . ? C40 C41 C42 C47 2.2(11) . . . . ? C40 C41 C42 C43 -179.9(7) . . . . ? C41 C42 C43 C44 -177.7(8) . . . . ? C47 C42 C43 C44 0.3(12) . . . . ? C42 C43 C44 C45 2.7(13) . . . . ? C43 C44 C45 C46 -3.4(13) . . . . ? C44 C45 C46 C47 1.1(12) . . . . ? C41 C42 C47 C46 175.5(7) . . . . ? C43 C42 C47 C46 -2.5(10) . . . . ? C41 C42 C47 C48 -6.2(10) . . . . ? C43 C42 C47 C48 175.7(7) . . . . ? C45 C46 C47 C42 1.9(11) . . . . ? C45 C46 C47 C48 -176.3(7) . . . . ? C42 C47 C48 C49 5.6(10) . . . . ? C46 C47 C48 C49 -176.2(7) . . . . ? C42 C47 C48 C50 -172.8(6) . . . . ? C46 C47 C48 C50 5.4(11) . . . . ? C47 C48 C49 C40 -1.1(11) . . . . ? C50 C48 C49 C40 177.5(6) . . . . ? C47 C48 C49 O11 176.0(6) . . . . ? C50 C48 C49 O11 -5.4(10) . . . . ? C41 C40 C49 C48 -2.9(11) . . . . ? C39 C40 C49 C48 173.6(7) . . . . ? C41 C40 C49 O11 180.0(6) . . . . ? C39 C40 C49 O11 -3.6(10) . . . . ? C49 C48 C50 C59 -86.7(8) . . . . ? C47 C48 C50 C59 91.7(8) . . . . ? C49 C48 C50 C51 91.4(8) . . . . ? C47 C48 C50 C51 -90.1(8) . . . . ? C59 C50 C51 C52 -175.9(7) . . . . ? C48 C50 C51 C52 6.0(10) . . . . ? C59 C50 C51 C56 4.8(9) . . . . ? C48 C50 C51 C56 -173.3(6) . . . . ? C50 C51 C52 C53 177.0(7) . . . . ? C56 C51 C52 C53 -3.7(11) . . . . ? C51 C52 C53 C54 0.1(12) . . . . ? C52 C53 C54 C55 2.7(12) . . . . ? C53 C54 C55 C56 -1.8(12) . . . . ? C54 C55 C56 C57 178.7(7) . . . . ? C54 C55 C56 C51 -1.8(11) . . . . ? C52 C51 C56 C55 4.5(10) . . . . ? C50 C51 C56 C55 -176.2(7) . . . . ? C52 C51 C56 C57 -176.0(7) . . . . ? C50 C51 C56 C57 3.3(10) . . . . ? C55 C56 C57 C58 173.5(8) . . . . ? C51 C56 C57 C58 -6.0(10) . . . . ? C56 C57 C58 C59 0.5(11) . . . . ? C56 C57 C58 C60 -179.4(7) . . . . ? C51 C50 C59 O12 175.5(6) . . . . ? C48 C50 C59 O12 -6.3(9) . . . . ? C51 C50 C59 C58 -10.6(9) . . . . ? C48 C50 C59 C58 167.5(6) . . . . ? C57 C58 C59 C50 8.1(10) . . . . ? C60 C58 C59 C50 -172.1(6) . . . . ? C57 C58 C59 O12 -177.9(7) . . . . ? C60 C58 C59 O12 2.0(10) . . . . ? C57 C58 C60 O1 -124.2(7) . . . . ? C59 C58 C60 O1 55.9(9) . . . . ? O2 C1 O1 C60 -7.6(11) . . . . ? C2 C1 O1 C60 178.0(6) . . . . ? C58 C60 O1 C1 -121.3(8) . . . . ? O4 C8 O3 C9 5.5(13) . . . . ? C4 C8 O3 C9 -175.3(7) . . . . ? C10 C9 O3 C8 -171.1(7) . . . . ? C18 C19 O5 C61 106.9(9) . . . . ? C10 C19 O5 C61 -75.4(10) . . . . ? C20 C29 O6 C62 -74.4(12) . . . . ? C28 C29 O6 C62 107.4(9) . . . . ? O8 C31 O7 C30 5.2(15) . . . . ? C32 C31 O7 C30 -174.3(8) . . . . ? C28 C30 O7 C31 106.5(9) . . . . ? O10 C38 O9 C39 5.5(13) . . . . ? C34 C38 O9 C39 -174.4(7) . . . . ? C40 C39 O9 C38 -105.7(8) . . . . ? C48 C49 O11 C63 92.9(8) . . . . ? C40 C49 O11 C63 -89.8(8) . . . . ? C50 C59 O12 C64 -92.3(8) . . . . ? C58 C59 O12 C64 93.6(8) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.08 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.203 _refine_diff_density_min -0.237 _refine_diff_density_rms 0.048 #===END data_3c _database_code_depnum_ccdc_archive 'CCDC 746583' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ;bis(bis(2-methoxy-3-methyl-naphthyl)-terephthalate) bis(acetone) solvate ; _chemical_melting_point ? _chemical_formula_moiety 'C64 H48 O12, 2(C3 H6 O)' _chemical_formula_sum 'C70 H60 O14' _chemical_formula_weight 1125.18 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.4141(18) _cell_length_b 20.620(3) _cell_length_c 12.643(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.474(15) _cell_angle_gamma 90.00 _cell_volume 2974.7(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 12 _exptl_crystal_description IRREGULAR _exptl_crystal_colour COLORLESS _exptl_crystal_size_max 0.86 _exptl_crystal_size_mid 0.58 _exptl_crystal_size_min 0.43 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.256 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1184 _exptl_absorpt_coefficient_mu 0.087 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.872 _exptl_absorpt_correction_T_max 0.959 _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4' _diffrn_measurement_method 'omega scans' _diffrn_standards_number 3 _diffrn_standards_interval_time 250 _diffrn_standards_decay_% 0 _diffrn_reflns_number 6900 _diffrn_reflns_av_R_equivalents 0.0147 _diffrn_reflns_av_sigmaI/netI 0.0351 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 25.05 _reflns_number_total 5419 _reflns_number_gt 3884 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SIR-97 (Altomare et al.,1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0763P)^2^+0.2482P] 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 5419 _refine_ls_number_parameters 757 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0760 _refine_ls_R_factor_gt 0.0482 _refine_ls_wR_factor_ref 0.1371 _refine_ls_wR_factor_gt 0.1202 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.024 _refine_ls_shift/su_mean 0.001 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 C1 C 0.7544(5) 0.7489(3) 0.6169(4) 0.0751(14) Uani 1 1 d . . . C2 C 0.7386(4) 0.7325(3) 0.7297(4) 0.0637(12) Uani 1 1 d . . . C3 C 0.8117(5) 0.7610(3) 0.8053(4) 0.0770(15) Uani 1 1 d . . . H3 H 0.8722 0.7880 0.7842 0.092 Uiso 1 1 calc R . . C4 C 0.7958(5) 0.7500(3) 0.9107(4) 0.0743(14) Uani 1 1 d . . . H4 H 0.8455 0.7696 0.9606 0.089 Uiso 1 1 calc R . . C5 C 0.7059(4) 0.7097(2) 0.9441(4) 0.0619(12) Uani 1 1 d . . . C6 C 0.6348(5) 0.6814(2) 0.8682(4) 0.0701(14) Uani 1 1 d . . . H6 H 0.5753 0.6537 0.8889 0.084 Uiso 1 1 calc R . . C7 C 0.6492(4) 0.6930(3) 0.7627(4) 0.0702(13) Uani 1 1 d . . . H7 H 0.5984 0.6741 0.7130 0.084 Uiso 1 1 calc R . . C8 C 0.6912(5) 0.7013(2) 1.0590(4) 0.0657(12) Uani 1 1 d . . . C9 C 0.5943(5) 0.6416(3) 1.1901(4) 0.0743(14) Uani 1 1 d . . . H9A H 0.5304 0.6704 1.2080 0.089 Uiso 1 1 calc R . . H9B H 0.6613 0.6519 1.2358 0.089 Uiso 1 1 calc R . . C10 C 0.5582(4) 0.5718(2) 1.2060(3) 0.0620(12) Uani 1 1 d . . . C11 C 0.6228(4) 0.5319(3) 1.2672(4) 0.0659(13) Uani 1 1 d . . . H11 H 0.6894 0.5483 1.3017 0.079 Uiso 1 1 calc R . . C12 C 0.5942(4) 0.4660(2) 1.2817(3) 0.0546(11) Uani 1 1 d . . . C13 C 0.6611(4) 0.4239(3) 1.3478(3) 0.0674(14) Uani 1 1 d . . . H13 H 0.7265 0.4400 1.3845 0.081 Uiso 1 1 calc R . . C14 C 0.6315(4) 0.3602(3) 1.3587(4) 0.0665(13) Uani 1 1 d . . . H14 H 0.6754 0.3333 1.4035 0.080 Uiso 1 1 calc R . . C15 C 0.5353(4) 0.3360(3) 1.3025(3) 0.0635(12) Uani 1 1 d . . . H15 H 0.5167 0.2922 1.3082 0.076 Uiso 1 1 calc R . . C16 C 0.4677(4) 0.3747(2) 1.2393(3) 0.0550(11) Uani 1 1 d . . . H16 H 0.4025 0.3572 1.2041 0.066 Uiso 1 1 calc R . . C17 C 0.4943(3) 0.4406(2) 1.2261(3) 0.0501(10) Uani 1 1 d . . . C18 C 0.4233(4) 0.4833(2) 1.1608(3) 0.0513(10) Uani 1 1 d . . . C19 C 0.4555(4) 0.5473(2) 1.1540(3) 0.0573(11) Uani 1 1 d . . . C20 C 0.3222(4) 0.4572(2) 1.0984(3) 0.0499(10) Uani 1 1 d . . . C21 C 0.2125(4) 0.4445(2) 1.1462(4) 0.0554(10) Uani 1 1 d . . . C22 C 0.1949(4) 0.4553(3) 1.2551(4) 0.0719(13) Uani 1 1 d . . . H22 H 0.2560 0.4716 1.2973 0.086 Uiso 1 1 calc R . . C23 C 0.0898(5) 0.4422(4) 1.2990(6) 0.0959(19) Uani 1 1 d . . . H23 H 0.0798 0.4499 1.3706 0.115 Uiso 1 1 calc R . . C24 C -0.0028(5) 0.4174(3) 1.2374(6) 0.101(2) Uani 1 1 d . . . H24 H -0.0742 0.4086 1.2683 0.121 Uiso 1 1 calc R . . C25 C 0.0102(5) 0.4059(3) 1.1320(6) 0.0904(18) Uani 1 1 d . . . H25 H -0.0521 0.3894 1.0915 0.109 Uiso 1 1 calc R . . C26 C 0.1191(4) 0.4191(2) 1.0839(5) 0.0689(13) Uani 1 1 d . . . C27 C 0.1377(5) 0.4052(2) 0.9745(4) 0.0719(14) Uani 1 1 d . . . H27 H 0.0761 0.3887 0.9333 0.086 Uiso 1 1 calc R . . C28 C 0.2430(5) 0.4156(2) 0.9290(4) 0.0615(12) Uani 1 1 d . . . C29 C 0.3339(4) 0.4425(2) 0.9934(3) 0.0548(10) Uani 1 1 d . . . C30 C 0.2629(5) 0.3960(3) 0.8173(4) 0.0788(16) Uani 1 1 d . . . H30A H 0.3460 0.3888 0.8079 0.095 Uiso 1 1 calc R . . H30B H 0.2225 0.3555 0.8027 0.095 Uiso 1 1 calc R . . C31 C 0.1155(6) 0.4383(3) 0.7020(4) 0.0818(17) Uani 1 1 d . . . C32 C 0.0778(4) 0.4893(2) 0.6263(3) 0.0593(12) Uani 1 1 d . . . C33 C 0.1529(4) 0.5333(2) 0.5828(4) 0.0645(12) Uani 1 1 d . . . H33 H 0.2322 0.5323 0.6015 0.077 Uiso 1 1 calc R . . C34 C 0.1114(4) 0.5793(2) 0.5114(4) 0.0640(12) Uani 1 1 d . . . H34 H 0.1633 0.6084 0.4816 0.077 Uiso 1 1 calc R . . C35 C -0.0058(4) 0.5822(2) 0.4840(3) 0.0528(10) Uani 1 1 d . . . C36 C -0.0804(4) 0.5373(3) 0.5261(4) 0.0708(14) Uani 1 1 d . . . H36 H -0.1595 0.5377 0.5064 0.085 Uiso 1 1 calc R . . C37 C -0.0391(5) 0.4922(3) 0.5968(4) 0.0789(16) Uani 1 1 d . . . H37 H -0.0910 0.4627 0.6257 0.095 Uiso 1 1 calc R . . C38 C -0.0563(4) 0.6313(2) 0.4100(4) 0.0552(11) Uani 1 1 d . . . C39 C -0.0218(4) 0.7274(2) 0.3143(4) 0.0651(13) Uani 1 1 d . . . H39A H -0.0581 0.7588 0.3601 0.078 Uiso 1 1 calc R . . H39B H -0.0794 0.7133 0.2615 0.078 Uiso 1 1 calc R . . C40 C 0.0827(3) 0.7570(2) 0.2618(3) 0.0522(10) Uani 1 1 d . . . C41 C 0.0853(4) 0.7582(2) 0.1539(4) 0.0554(11) Uani 1 1 d . . . H41 H 0.0211 0.7428 0.1147 0.067 Uiso 1 1 calc R . . C42 C 0.1833(4) 0.7822(2) 0.1007(3) 0.0555(10) Uani 1 1 d . . . C43 C 0.1872(5) 0.7828(3) -0.0109(4) 0.0745(14) Uani 1 1 d . . . H43 H 0.1225 0.7686 -0.0508 0.089 Uiso 1 1 calc R . . C44 C 0.2838(6) 0.8036(4) -0.0603(4) 0.100(2) Uani 1 1 d . . . H44 H 0.2854 0.8036 -0.1338 0.120 Uiso 1 1 calc R . . C45 C 0.3815(6) 0.8253(4) -0.0011(4) 0.097(2) Uani 1 1 d . . . H45 H 0.4477 0.8396 -0.0355 0.116 Uiso 1 1 calc R . . C46 C 0.3802(5) 0.8254(3) 0.1060(4) 0.0758(15) Uani 1 1 d . . . H46 H 0.4459 0.8400 0.1439 0.091 Uiso 1 1 calc R . . C47 C 0.2817(4) 0.8040(2) 0.1613(3) 0.0533(10) Uani 1 1 d . . . C48 C 0.2774(3) 0.8043(2) 0.2735(3) 0.0496(10) Uani 1 1 d . . . C49 C 0.1785(3) 0.7823(2) 0.3221(3) 0.0496(10) Uani 1 1 d . . . C50 C 0.3817(3) 0.8266(2) 0.3372(3) 0.0507(10) Uani 1 1 d . . . C51 C 0.4021(4) 0.8939(3) 0.3552(3) 0.0564(11) Uani 1 1 d . . . C52 C 0.3235(4) 0.9423(3) 0.3187(4) 0.0662(12) Uani 1 1 d . . . H52 H 0.2573 0.9303 0.2790 0.079 Uiso 1 1 calc R . . C53 C 0.3425(6) 1.0064(3) 0.3403(5) 0.0826(16) Uani 1 1 d . . . H53 H 0.2895 1.0371 0.3144 0.099 Uiso 1 1 calc R . . C54 C 0.4395(7) 1.0264(4) 0.4002(5) 0.100(2) Uani 1 1 d . . . H54 H 0.4499 1.0700 0.4166 0.121 Uiso 1 1 calc R . . C55 C 0.5185(6) 0.9821(4) 0.4344(5) 0.0885(18) Uani 1 1 d . . . H55 H 0.5840 0.9961 0.4733 0.106 Uiso 1 1 calc R . . C56 C 0.5051(4) 0.9143(3) 0.4130(4) 0.0698(14) Uani 1 1 d . . . C57 C 0.5873(4) 0.8679(4) 0.4421(4) 0.0786(17) Uani 1 1 d . . . H57 H 0.6562 0.8812 0.4765 0.094 Uiso 1 1 calc R . . C58 C 0.5711(4) 0.8026(3) 0.4223(3) 0.0706(15) Uani 1 1 d . . . C59 C 0.4639(4) 0.7834(3) 0.3721(3) 0.0596(12) Uani 1 1 d . . . C60 C 0.6656(5) 0.7544(4) 0.4457(4) 0.095(2) Uani 1 1 d . . . H60A H 0.6547 0.7168 0.4005 0.114 Uiso 1 1 calc R . . H60B H 0.7412 0.7735 0.4307 0.114 Uiso 1 1 calc R . . C61 C 0.2899(6) 0.6171(4) 1.1397(6) 0.112(2) Uani 1 1 d . . . H61A H 0.2346 0.5837 1.1557 0.168 Uiso 1 1 calc R . . H61B H 0.2536 0.6480 1.0924 0.168 Uiso 1 1 calc R . . H61C H 0.3146 0.6386 1.2039 0.168 Uiso 1 1 calc R . . C62 C 0.4589(6) 0.5039(4) 0.8843(5) 0.102(2) Uani 1 1 d . . . H62A H 0.4032 0.5027 0.8261 0.153 Uiso 1 1 calc R . . H62B H 0.5369 0.5038 0.8577 0.153 Uiso 1 1 calc R . . H62C H 0.4470 0.5426 0.9249 0.153 Uiso 1 1 calc R . . C63 C 0.1066(5) 0.8275(4) 0.4786(4) 0.097(2) Uani 1 1 d . . . H63A H 0.1316 0.8701 0.4586 0.145 Uiso 1 1 calc R . . H63B H 0.1134 0.8231 0.5541 0.145 Uiso 1 1 calc R . . H63C H 0.0264 0.8212 0.4561 0.145 Uiso 1 1 calc R . . C64 C 0.4060(6) 0.6824(3) 0.4410(5) 0.0959(19) Uani 1 1 d . . . H64A H 0.4632 0.6848 0.4978 0.144 Uiso 1 1 calc R . . H64B H 0.3944 0.6379 0.4210 0.144 Uiso 1 1 calc R . . H64C H 0.3333 0.7004 0.4636 0.144 Uiso 1 1 calc R . . O1 O 0.6640(3) 0.7345(2) 0.5567(3) 0.0836(11) Uani 1 1 d . . . O2 O 0.8396(4) 0.7762(4) 0.5848(3) 0.144(2) Uani 1 1 d . . . O3 O 0.6241(3) 0.65061(16) 1.0800(2) 0.0718(9) Uani 1 1 d . . . O4 O 0.7345(5) 0.7349(2) 1.1261(3) 0.1104(16) Uani 1 1 d . . . O5 O 0.3893(3) 0.58906(17) 1.0907(3) 0.0751(9) Uani 1 1 d . . . O6 O 0.4433(3) 0.4487(2) 0.9496(3) 0.0755(10) Uani 1 1 d . . . O7 O 0.2210(3) 0.44555(16) 0.7421(2) 0.0692(9) Uani 1 1 d . . . O8 O 0.0519(5) 0.3947(3) 0.7272(4) 0.150(3) Uani 1 1 d . . . O9 O 0.0222(3) 0.67202(16) 0.3759(3) 0.0676(9) Uani 1 1 d . . . O10 O -0.1587(3) 0.63460(19) 0.3851(3) 0.0904(13) Uani 1 1 d . . . O11 O 0.1769(2) 0.78123(17) 0.4307(2) 0.0635(8) Uani 1 1 d . . . O12 O 0.4462(3) 0.71792(19) 0.3530(3) 0.0771(10) Uani 1 1 d . . . C65 C 0.2339(11) 0.6661(5) 0.7421(8) 0.145(4) Uani 1 1 d D . . C66 C 0.2236(14) 0.6282(6) 0.8373(9) 0.226(7) Uani 1 1 d D . . H66A H 0.2160 0.5832 0.8192 0.339 Uiso 1 1 calc R . . H66B H 0.1556 0.6420 0.8745 0.339 Uiso 1 1 calc R . . H66C H 0.2922 0.6343 0.8817 0.339 Uiso 1 1 calc R . . C67 C 0.1446(16) 0.7046(6) 0.7026(10) 0.271(11) Uani 1 1 d D . . H67A H 0.1686 0.7249 0.6383 0.407 Uiso 1 1 calc R . . H67B H 0.1265 0.7374 0.7535 0.407 Uiso 1 1 calc R . . H67C H 0.0764 0.6785 0.6884 0.407 Uiso 1 1 calc R . . O13 O 0.3270(9) 0.6615(7) 0.6988(9) 0.257(6) Uani 1 1 d D . . C68 C 0.8851(15) 0.5461(9) 0.9729(17) 0.33(2) Uani 1 1 d D . . C69 C 0.9415(14) 0.5871(10) 1.043(2) 0.42(2) Uani 1 1 d D . . H69A H 1.0244 0.5854 1.0325 0.627 Uiso 1 1 calc R . . H69B H 0.9256 0.5740 1.1142 0.627 Uiso 1 1 calc R . . H69C H 0.9140 0.6307 1.0320 0.627 Uiso 1 1 calc R . . C70 C 0.7865(15) 0.5042(9) 0.9854(12) 0.278(11) Uani 1 1 d D . . H70A H 0.7990 0.4645 0.9479 0.416 Uiso 1 1 calc R . . H70B H 0.7171 0.5251 0.9577 0.416 Uiso 1 1 calc R . . H70C H 0.7772 0.4950 1.0592 0.416 Uiso 1 1 calc R . . O14 O 0.9132(18) 0.5450(14) 0.8825(14) 0.438(15) Uani 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 C1 0.063(3) 0.099(4) 0.063(3) -0.002(3) -0.003(2) -0.002(3) C2 0.055(3) 0.069(3) 0.066(3) 0.004(2) -0.011(2) 0.005(2) C3 0.068(3) 0.084(4) 0.078(3) 0.013(3) -0.013(3) -0.021(3) C4 0.083(3) 0.070(3) 0.068(3) 0.008(3) -0.021(3) -0.025(3) C5 0.071(3) 0.050(3) 0.064(3) 0.005(2) -0.018(2) -0.004(2) C6 0.080(3) 0.062(3) 0.067(3) 0.005(2) -0.013(3) -0.021(3) C7 0.077(3) 0.071(3) 0.062(3) -0.004(2) -0.017(2) -0.014(3) C8 0.085(3) 0.047(3) 0.064(3) 0.002(2) -0.012(2) -0.014(3) C9 0.099(4) 0.068(3) 0.057(3) -0.012(3) 0.008(3) -0.019(3) C10 0.076(3) 0.066(3) 0.045(2) -0.012(2) 0.008(2) -0.017(3) C11 0.064(3) 0.086(4) 0.048(3) -0.004(3) -0.003(2) -0.019(3) C12 0.050(2) 0.071(3) 0.043(2) 0.000(2) 0.0030(18) -0.005(2) C13 0.048(2) 0.105(4) 0.049(3) 0.001(3) -0.005(2) -0.006(3) C14 0.059(3) 0.081(4) 0.059(3) 0.012(3) -0.001(2) 0.006(3) C15 0.063(3) 0.072(3) 0.056(3) 0.011(2) 0.005(2) 0.000(2) C16 0.051(2) 0.061(3) 0.053(2) 0.003(2) 0.0015(19) -0.006(2) C17 0.048(2) 0.062(3) 0.040(2) -0.0013(19) 0.0044(17) -0.003(2) C18 0.052(2) 0.060(3) 0.041(2) -0.0024(19) 0.0017(18) 0.004(2) C19 0.071(3) 0.056(3) 0.044(2) -0.002(2) -0.002(2) 0.004(2) C20 0.052(2) 0.049(2) 0.049(2) -0.0003(19) -0.0039(18) 0.0078(19) C21 0.050(2) 0.050(2) 0.066(3) -0.004(2) -0.002(2) 0.004(2) C22 0.065(3) 0.078(4) 0.073(3) -0.006(3) 0.007(2) 0.000(3) C23 0.076(4) 0.105(5) 0.107(5) -0.007(4) 0.027(3) 0.002(4) C24 0.069(4) 0.103(5) 0.133(6) 0.019(4) 0.033(4) 0.001(4) C25 0.063(3) 0.082(4) 0.126(5) -0.002(4) -0.008(3) -0.001(3) C26 0.054(3) 0.058(3) 0.094(4) 0.005(3) -0.018(3) 0.003(2) C27 0.079(3) 0.057(3) 0.077(3) -0.003(3) -0.033(3) 0.000(3) C28 0.077(3) 0.051(3) 0.055(3) -0.003(2) -0.020(2) 0.012(2) C29 0.056(3) 0.056(3) 0.052(2) 0.003(2) -0.001(2) 0.015(2) C30 0.113(4) 0.066(3) 0.057(3) -0.005(2) -0.031(3) 0.023(3) C31 0.107(4) 0.059(3) 0.077(3) 0.014(3) -0.043(3) -0.028(3) C32 0.066(3) 0.054(3) 0.056(3) 0.009(2) -0.016(2) -0.016(2) C33 0.048(2) 0.067(3) 0.077(3) 0.011(3) -0.007(2) -0.007(2) C34 0.048(2) 0.070(3) 0.074(3) 0.019(3) 0.001(2) -0.005(2) C35 0.050(2) 0.055(2) 0.053(2) 0.003(2) -0.0024(18) -0.007(2) C36 0.046(2) 0.081(4) 0.085(3) 0.026(3) -0.007(2) -0.016(2) C37 0.066(3) 0.084(4) 0.086(4) 0.035(3) -0.012(3) -0.027(3) C38 0.043(2) 0.054(3) 0.069(3) 0.007(2) 0.000(2) -0.004(2) C39 0.047(2) 0.069(3) 0.079(3) 0.019(3) -0.008(2) 0.001(2) C40 0.042(2) 0.051(2) 0.063(3) 0.012(2) -0.0059(19) 0.0030(19) C41 0.054(2) 0.044(2) 0.067(3) 0.005(2) -0.016(2) 0.000(2) C42 0.073(3) 0.045(2) 0.049(2) 0.003(2) -0.005(2) 0.002(2) C43 0.090(4) 0.075(3) 0.058(3) -0.006(3) -0.006(3) -0.017(3) C44 0.131(5) 0.120(5) 0.051(3) -0.005(3) 0.010(3) -0.029(4) C45 0.112(5) 0.125(5) 0.054(3) -0.008(3) 0.022(3) -0.042(4) C46 0.084(3) 0.089(4) 0.055(3) -0.003(3) 0.016(3) -0.024(3) C47 0.057(3) 0.052(2) 0.051(2) 0.002(2) 0.006(2) -0.006(2) C48 0.048(2) 0.052(2) 0.049(2) 0.0019(19) -0.0007(18) -0.0028(19) C49 0.046(2) 0.055(2) 0.047(2) 0.011(2) -0.0015(18) 0.001(2) C50 0.044(2) 0.064(3) 0.044(2) -0.001(2) 0.0083(18) 0.003(2) C51 0.049(2) 0.075(3) 0.045(2) -0.007(2) 0.0102(19) -0.015(2) C52 0.062(3) 0.067(3) 0.070(3) -0.005(3) 0.015(2) -0.005(3) C53 0.093(4) 0.061(3) 0.095(4) -0.003(3) 0.020(3) -0.004(3) C54 0.125(6) 0.083(5) 0.094(5) -0.020(4) 0.020(4) -0.037(4) C55 0.083(4) 0.109(5) 0.074(4) -0.012(4) 0.009(3) -0.043(4) C56 0.060(3) 0.097(4) 0.052(3) -0.001(3) 0.007(2) -0.019(3) C57 0.050(3) 0.139(6) 0.046(3) 0.000(3) -0.001(2) -0.017(3) C58 0.051(3) 0.117(5) 0.044(2) 0.001(3) 0.004(2) 0.012(3) C59 0.059(3) 0.079(3) 0.041(2) -0.004(2) 0.0107(19) 0.008(3) C60 0.067(3) 0.170(6) 0.049(3) -0.003(3) 0.002(2) 0.038(4) C61 0.116(5) 0.092(5) 0.128(6) -0.005(4) -0.009(4) 0.038(4) C62 0.104(5) 0.112(6) 0.092(4) 0.000(4) 0.033(4) -0.004(4) C63 0.081(4) 0.143(6) 0.066(3) -0.018(4) -0.005(3) 0.030(4) C64 0.100(4) 0.086(4) 0.102(5) 0.020(4) 0.012(4) 0.020(3) O1 0.0548(18) 0.138(3) 0.0574(19) -0.003(2) -0.0063(15) 0.018(2) O2 0.108(3) 0.249(7) 0.076(3) 0.030(4) -0.009(2) -0.072(4) O3 0.096(2) 0.058(2) 0.0617(19) -0.0080(16) 0.0048(17) -0.0209(19) O4 0.176(4) 0.088(3) 0.066(2) 0.000(2) -0.021(3) -0.065(3) O5 0.094(2) 0.063(2) 0.068(2) 0.0001(17) -0.0046(18) 0.010(2) O6 0.069(2) 0.099(3) 0.0586(19) 0.001(2) 0.0054(16) 0.022(2) O7 0.087(2) 0.0613(19) 0.0583(18) 0.0043(16) -0.0259(17) 0.0046(18) O8 0.171(5) 0.116(4) 0.156(5) 0.080(4) -0.102(4) -0.087(4) O9 0.0459(16) 0.071(2) 0.086(2) 0.0317(18) -0.0042(15) -0.0038(15) O10 0.0486(19) 0.084(3) 0.138(3) 0.041(2) -0.019(2) -0.0141(18) O11 0.0545(16) 0.088(2) 0.0477(16) 0.0132(17) 0.0019(13) 0.0093(17) O12 0.085(2) 0.077(3) 0.069(2) -0.0002(19) 0.0027(18) 0.021(2) C65 0.189(10) 0.132(8) 0.116(7) -0.060(6) 0.028(7) -0.047(8) C66 0.36(2) 0.157(11) 0.155(10) 0.006(9) 0.013(11) 0.102(12) C67 0.45(3) 0.163(11) 0.195(12) -0.062(9) -0.162(16) 0.131(15) O13 0.210(9) 0.322(15) 0.243(10) -0.076(10) 0.058(8) -0.084(10) C68 0.194(19) 0.30(3) 0.49(5) 0.22(3) 0.15(3) 0.13(2) C69 0.234(19) 0.34(3) 0.67(5) -0.33(3) -0.26(3) 0.158(18) C70 0.29(2) 0.32(3) 0.218(15) -0.076(16) -0.093(15) 0.15(2) O14 0.39(3) 0.58(4) 0.35(2) 0.08(3) 0.102(18) -0.04(3) _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 C1 O2 1.203(7) . ? C1 O1 1.301(6) . ? C1 C2 1.482(7) . ? C2 C7 1.379(7) . ? C2 C3 1.383(7) . ? C3 C4 1.369(7) . ? C3 H3 0.9300 . ? C4 C5 1.395(7) . ? C4 H4 0.9300 . ? C5 C6 1.370(6) . ? C5 C8 1.478(7) . ? C6 C7 1.369(7) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 O4 1.193(6) . ? C8 O3 1.327(6) . ? C9 O3 1.453(6) . ? C9 C10 1.512(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.339(7) . ? C10 C19 1.422(6) . ? C11 C12 1.410(7) . ? C11 H11 0.9300 . ? C12 C13 1.415(7) . ? C12 C17 1.425(6) . ? C13 C14 1.364(7) . ? C13 H13 0.9300 . ? C14 C15 1.386(7) . ? C14 H14 0.9300 . ? C15 C16 1.356(6) . ? C15 H15 0.9300 . ? C16 C17 1.404(6) . ? C16 H16 0.9300 . ? C17 C18 1.441(6) . ? C18 C19 1.374(6) . ? C18 C20 1.483(6) . ? C19 O5 1.386(5) . ? C20 C29 1.372(6) . ? C20 C21 1.428(6) . ? C21 C26 1.410(6) . ? C21 C22 1.414(7) . ? C22 C23 1.361(7) . ? C22 H22 0.9300 . ? C23 C24 1.394(9) . ? C23 H23 0.9300 . ? C24 C25 1.365(9) . ? C24 H24 0.9300 . ? C25 C26 1.423(8) . ? C25 H25 0.9300 . ? C26 C27 1.435(8) . ? C27 C28 1.362(7) . ? C27 H27 0.9300 . ? C28 C29 1.416(6) . ? C28 C30 1.492(7) . ? C29 O6 1.385(5) . ? C30 O7 1.468(6) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 O8 1.204(7) . ? C31 O7 1.303(6) . ? C31 C32 1.479(7) . ? C32 C33 1.373(6) . ? C32 C37 1.376(6) . ? C33 C34 1.384(6) . ? C33 H33 0.9300 . ? C34 C35 1.374(6) . ? C34 H34 0.9300 . ? C35 C36 1.374(6) . ? C35 C38 1.485(6) . ? C36 C37 1.366(7) . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? C38 O10 1.205(5) . ? C38 O9 1.310(5) . ? C39 O9 1.465(5) . ? C39 C40 1.507(6) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 C41 1.366(6) . ? C40 C49 1.417(6) . ? C41 C42 1.411(6) . ? C41 H41 0.9300 . ? C42 C43 1.413(6) . ? C42 C47 1.416(6) . ? C43 C44 1.352(8) . ? C43 H43 0.9300 . ? C44 C45 1.400(8) . ? C44 H44 0.9300 . ? C45 C46 1.354(7) . ? C45 H45 0.9300 . ? C46 C47 1.410(6) . ? C46 H46 0.9300 . ? C47 C48 1.421(6) . ? C48 C49 1.375(6) . ? C48 C50 1.493(6) . ? C49 O11 1.375(5) . ? C50 C59 1.360(6) . ? C50 C51 1.424(7) . ? C51 C52 1.413(7) . ? C51 C56 1.432(6) . ? C52 C53 1.364(7) . ? C52 H52 0.9300 . ? C53 C54 1.389(9) . ? C53 H53 0.9300 . ? C54 C55 1.345(9) . ? C54 H54 0.9300 . ? C55 C56 1.432(9) . ? C55 H55 0.9300 . ? C56 C57 1.382(8) . ? C57 C58 1.382(8) . ? C57 H57 0.9300 . ? C58 C59 1.419(7) . ? C58 C60 1.490(8) . ? C59 O12 1.386(6) . ? C60 O1 1.463(6) . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? C61 O5 1.430(8) . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? C62 O6 1.420(8) . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? C63 O11 1.396(7) . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? C64 O12 1.418(7) . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? C65 O13 1.211(11) . ? C65 C67 1.377(14) . ? C65 C66 1.443(14) . ? C66 H66A 0.9600 . ? C66 H66B 0.9600 . ? C66 H66C 0.9600 . ? C67 H67A 0.9600 . ? C67 H67B 0.9600 . ? C67 H67C 0.9600 . ? C68 O14 1.195(18) . ? C68 C69 1.38(2) . ? C68 C70 1.431(19) . ? C69 H69A 0.9600 . ? C69 H69B 0.9600 . ? C69 H69C 0.9600 . ? C70 H70A 0.9600 . ? C70 H70B 0.9600 . ? C70 H70C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 C1 O1 123.1(5) . . ? O2 C1 C2 123.4(5) . . ? O1 C1 C2 113.4(5) . . ? C7 C2 C3 118.7(5) . . ? C7 C2 C1 122.3(4) . . ? C3 C2 C1 118.8(5) . . ? C4 C3 C2 120.6(5) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C3 C4 C5 120.7(5) . . ? C3 C4 H4 119.6 . . ? C5 C4 H4 119.6 . . ? C6 C5 C4 117.9(5) . . ? C6 C5 C8 124.0(5) . . ? C4 C5 C8 118.1(4) . . ? C7 C6 C5 121.6(5) . . ? C7 C6 H6 119.2 . . ? C5 C6 H6 119.2 . . ? C6 C7 C2 120.4(4) . . ? C6 C7 H7 119.8 . . ? C2 C7 H7 119.8 . . ? O4 C8 O3 123.1(5) . . ? O4 C8 C5 125.2(5) . . ? O3 C8 C5 111.7(4) . . ? O3 C9 C10 108.6(4) . . ? O3 C9 H9A 110.0 . . ? C10 C9 H9A 110.0 . . ? O3 C9 H9B 110.0 . . ? C10 C9 H9B 110.0 . . ? H9A C9 H9B 108.3 . . ? C11 C10 C19 118.9(5) . . ? C11 C10 C9 120.9(5) . . ? C19 C10 C9 120.1(5) . . ? C10 C11 C12 122.8(4) . . ? C10 C11 H11 118.6 . . ? C12 C11 H11 118.6 . . ? C11 C12 C13 123.0(4) . . ? C11 C12 C17 118.4(4) . . ? C13 C12 C17 118.6(4) . . ? C14 C13 C12 121.3(4) . . ? C14 C13 H13 119.3 . . ? C12 C13 H13 119.3 . . ? C13 C14 C15 119.3(5) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C16 C15 C14 121.5(5) . . ? C16 C15 H15 119.3 . . ? C14 C15 H15 119.3 . . ? C15 C16 C17 121.2(4) . . ? C15 C16 H16 119.4 . . ? C17 C16 H16 119.4 . . ? C16 C17 C12 118.1(4) . . ? C16 C17 C18 122.6(4) . . ? C12 C17 C18 119.3(4) . . ? C19 C18 C17 118.4(4) . . ? C19 C18 C20 121.4(4) . . ? C17 C18 C20 120.1(4) . . ? C18 C19 O5 119.4(4) . . ? C18 C19 C10 122.1(4) . . ? O5 C19 C10 118.4(4) . . ? C29 C20 C21 118.5(4) . . ? C29 C20 C18 120.1(4) . . ? C21 C20 C18 121.3(4) . . ? C26 C21 C22 118.5(4) . . ? C26 C21 C20 119.4(4) . . ? C22 C21 C20 122.1(4) . . ? C23 C22 C21 121.0(5) . . ? C23 C22 H22 119.5 . . ? C21 C22 H22 119.5 . . ? C22 C23 C24 120.6(6) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? C25 C24 C23 120.5(6) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C24 C25 C26 120.2(6) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C21 C26 C25 119.2(5) . . ? C21 C26 C27 118.9(5) . . ? C25 C26 C27 121.8(5) . . ? C28 C27 C26 122.0(4) . . ? C28 C27 H27 119.0 . . ? C26 C27 H27 119.0 . . ? C27 C28 C29 117.4(4) . . ? C27 C28 C30 121.0(5) . . ? C29 C28 C30 121.6(5) . . ? C20 C29 O6 118.6(4) . . ? C20 C29 C28 123.7(4) . . ? O6 C29 C28 117.5(4) . . ? O7 C30 C28 111.7(4) . . ? O7 C30 H30A 109.3 . . ? C28 C30 H30A 109.3 . . ? O7 C30 H30B 109.3 . . ? C28 C30 H30B 109.3 . . ? H30A C30 H30B 107.9 . . ? O8 C31 O7 122.7(5) . . ? O8 C31 C32 122.4(5) . . ? O7 C31 C32 114.9(5) . . ? C33 C32 C37 118.4(4) . . ? C33 C32 C31 123.7(4) . . ? C37 C32 C31 118.0(4) . . ? C32 C33 C34 120.4(4) . . ? C32 C33 H33 119.8 . . ? C34 C33 H33 119.8 . . ? C35 C34 C33 120.6(4) . . ? C35 C34 H34 119.7 . . ? C33 C34 H34 119.7 . . ? C36 C35 C34 118.9(4) . . ? C36 C35 C38 117.9(4) . . ? C34 C35 C38 123.2(4) . . ? C37 C36 C35 120.3(4) . . ? C37 C36 H36 119.8 . . ? C35 C36 H36 119.8 . . ? C36 C37 C32 121.4(5) . . ? C36 C37 H37 119.3 . . ? C32 C37 H37 119.3 . . ? O10 C38 O9 123.1(4) . . ? O10 C38 C35 124.2(4) . . ? O9 C38 C35 112.8(3) . . ? O9 C39 C40 106.6(3) . . ? O9 C39 H39A 110.4 . . ? C40 C39 H39A 110.4 . . ? O9 C39 H39B 110.4 . . ? C40 C39 H39B 110.4 . . ? H39A C39 H39B 108.6 . . ? C41 C40 C49 119.6(4) . . ? C41 C40 C39 119.0(4) . . ? C49 C40 C39 121.4(4) . . ? C40 C41 C42 121.4(4) . . ? C40 C41 H41 119.3 . . ? C42 C41 H41 119.3 . . ? C41 C42 C43 121.6(4) . . ? C41 C42 C47 118.8(4) . . ? C43 C42 C47 119.6(4) . . ? C44 C43 C42 120.7(5) . . ? C44 C43 H43 119.7 . . ? C42 C43 H43 119.7 . . ? C43 C44 C45 120.1(5) . . ? C43 C44 H44 119.9 . . ? C45 C44 H44 119.9 . . ? C46 C45 C44 120.5(5) . . ? C46 C45 H45 119.8 . . ? C44 C45 H45 119.8 . . ? C45 C46 C47 121.6(5) . . ? C45 C46 H46 119.2 . . ? C47 C46 H46 119.2 . . ? C46 C47 C42 117.5(4) . . ? C46 C47 C48 122.9(4) . . ? C42 C47 C48 119.6(4) . . ? C49 C48 C47 119.7(4) . . ? C49 C48 C50 120.9(4) . . ? C47 C48 C50 119.4(4) . . ? C48 C49 O11 118.9(3) . . ? C48 C49 C40 120.8(4) . . ? O11 C49 C40 120.1(4) . . ? C59 C50 C51 118.5(4) . . ? C59 C50 C48 120.5(4) . . ? C51 C50 C48 120.8(4) . . ? C52 C51 C50 122.4(4) . . ? C52 C51 C56 117.8(5) . . ? C50 C51 C56 119.8(5) . . ? C53 C52 C51 121.5(5) . . ? C53 C52 H52 119.2 . . ? C51 C52 H52 119.2 . . ? C52 C53 C54 121.1(6) . . ? C52 C53 H53 119.4 . . ? C54 C53 H53 119.4 . . ? C55 C54 C53 119.5(6) . . ? C55 C54 H54 120.3 . . ? C53 C54 H54 120.3 . . ? C54 C55 C56 122.3(6) . . ? C54 C55 H55 118.8 . . ? C56 C55 H55 118.8 . . ? C57 C56 C55 123.9(6) . . ? C57 C56 C51 118.4(5) . . ? C55 C56 C51 117.7(6) . . ? C56 C57 C58 122.6(5) . . ? C56 C57 H57 118.7 . . ? C58 C57 H57 118.7 . . ? C57 C58 C59 117.5(5) . . ? C57 C58 C60 121.4(5) . . ? C59 C58 C60 121.0(6) . . ? C50 C59 O12 119.0(4) . . ? C50 C59 C58 122.9(5) . . ? O12 C59 C58 118.0(5) . . ? O1 C60 C58 110.5(4) . . ? O1 C60 H60A 109.6 . . ? C58 C60 H60A 109.6 . . ? O1 C60 H60B 109.6 . . ? C58 C60 H60B 109.6 . . ? H60A C60 H60B 108.1 . . ? O5 C61 H61A 109.5 . . ? O5 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? O5 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? O6 C62 H62A 109.5 . . ? O6 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? O6 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? O11 C63 H63A 109.5 . . ? O11 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? O11 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? O12 C64 H64A 109.5 . . ? O12 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? O12 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C1 O1 C60 117.9(5) . . ? C8 O3 C9 116.3(4) . . ? C19 O5 C61 115.3(4) . . ? C29 O6 C62 115.8(4) . . ? C31 O7 C30 117.1(4) . . ? C38 O9 C39 116.6(3) . . ? C49 O11 C63 116.4(4) . . ? C59 O12 C64 114.5(4) . . ? O13 C65 C67 122.1(14) . . ? O13 C65 C66 115.3(14) . . ? C67 C65 C66 122.7(13) . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C65 C67 H67A 109.5 . . ? C65 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C65 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? O14 C68 C69 120(2) . . ? O14 C68 C70 109(2) . . ? C69 C68 C70 131(2) . . ? C68 C69 H69A 109.5 . . ? C68 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C68 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C68 C70 H70A 109.5 . . ? C68 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C68 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C7 -170.1(7) . . . . ? O1 C1 C2 C7 14.0(8) . . . . ? O2 C1 C2 C3 13.8(9) . . . . ? O1 C1 C2 C3 -162.1(5) . . . . ? C7 C2 C3 C4 0.2(8) . . . . ? C1 C2 C3 C4 176.4(5) . . . . ? C2 C3 C4 C5 0.2(9) . . . . ? C3 C4 C5 C6 0.3(8) . . . . ? C3 C4 C5 C8 -178.1(5) . . . . ? C4 C5 C6 C7 -1.2(8) . . . . ? C8 C5 C6 C7 177.1(5) . . . . ? C5 C6 C7 C2 1.7(8) . . . . ? C3 C2 C7 C6 -1.1(8) . . . . ? C1 C2 C7 C6 -177.2(5) . . . . ? C6 C5 C8 O4 -163.5(6) . . . . ? C4 C5 C8 O4 14.8(8) . . . . ? C6 C5 C8 O3 17.4(7) . . . . ? C4 C5 C8 O3 -164.3(5) . . . . ? O3 C9 C10 C11 113.8(5) . . . . ? O3 C9 C10 C19 -64.9(6) . . . . ? C19 C10 C11 C12 0.7(7) . . . . ? C9 C10 C11 C12 -178.1(4) . . . . ? C10 C11 C12 C13 -178.9(4) . . . . ? C10 C11 C12 C17 2.0(7) . . . . ? C11 C12 C13 C14 -179.2(5) . . . . ? C17 C12 C13 C14 0.0(7) . . . . ? C12 C13 C14 C15 1.2(7) . . . . ? C13 C14 C15 C16 -2.1(7) . . . . ? C14 C15 C16 C17 1.7(7) . . . . ? C15 C16 C17 C12 -0.4(6) . . . . ? C15 C16 C17 C18 -179.1(4) . . . . ? C11 C12 C17 C16 178.8(4) . . . . ? C13 C12 C17 C16 -0.4(6) . . . . ? C11 C12 C17 C18 -2.5(6) . . . . ? C13 C12 C17 C18 178.3(4) . . . . ? C16 C17 C18 C19 179.1(4) . . . . ? C12 C17 C18 C19 0.5(6) . . . . ? C16 C17 C18 C20 -4.2(6) . . . . ? C12 C17 C18 C20 177.2(4) . . . . ? C17 C18 C19 O5 179.2(4) . . . . ? C20 C18 C19 O5 2.6(6) . . . . ? C17 C18 C19 C10 2.3(6) . . . . ? C20 C18 C19 C10 -174.4(4) . . . . ? C11 C10 C19 C18 -2.9(7) . . . . ? C9 C10 C19 C18 175.9(4) . . . . ? C11 C10 C19 O5 -179.9(4) . . . . ? C9 C10 C19 O5 -1.1(6) . . . . ? C19 C18 C20 C29 78.9(5) . . . . ? C17 C18 C20 C29 -97.7(5) . . . . ? C19 C18 C20 C21 -103.5(5) . . . . ? C17 C18 C20 C21 79.9(5) . . . . ? C29 C20 C21 C26 -1.8(6) . . . . ? C18 C20 C21 C26 -179.4(4) . . . . ? C29 C20 C21 C22 176.9(4) . . . . ? C18 C20 C21 C22 -0.7(7) . . . . ? C26 C21 C22 C23 -0.6(8) . . . . ? C20 C21 C22 C23 -179.3(5) . . . . ? C21 C22 C23 C24 0.4(9) . . . . ? C22 C23 C24 C25 -0.1(11) . . . . ? C23 C24 C25 C26 0.1(10) . . . . ? C22 C21 C26 C25 0.6(7) . . . . ? C20 C21 C26 C25 179.4(5) . . . . ? C22 C21 C26 C27 -177.2(5) . . . . ? C20 C21 C26 C27 1.6(7) . . . . ? C24 C25 C26 C21 -0.3(8) . . . . ? C24 C25 C26 C27 177.4(6) . . . . ? C21 C26 C27 C28 0.2(7) . . . . ? C25 C26 C27 C28 -177.5(5) . . . . ? C26 C27 C28 C29 -1.7(7) . . . . ? C26 C27 C28 C30 175.2(4) . . . . ? C21 C20 C29 O6 -173.7(4) . . . . ? C18 C20 C29 O6 3.9(6) . . . . ? C21 C20 C29 C28 0.3(6) . . . . ? C18 C20 C29 C28 178.0(4) . . . . ? C27 C28 C29 C20 1.4(7) . . . . ? C30 C28 C29 C20 -175.5(4) . . . . ? C27 C28 C29 O6 175.5(4) . . . . ? C30 C28 C29 O6 -1.3(6) . . . . ? C27 C28 C30 O7 83.9(6) . . . . ? C29 C28 C30 O7 -99.3(5) . . . . ? O8 C31 C32 C33 -169.0(7) . . . . ? O7 C31 C32 C33 13.4(8) . . . . ? O8 C31 C32 C37 10.1(9) . . . . ? O7 C31 C32 C37 -167.5(5) . . . . ? C37 C32 C33 C34 0.1(8) . . . . ? C31 C32 C33 C34 179.2(5) . . . . ? C32 C33 C34 C35 1.0(8) . . . . ? C33 C34 C35 C36 -2.1(7) . . . . ? C33 C34 C35 C38 178.4(5) . . . . ? C34 C35 C36 C37 2.3(8) . . . . ? C38 C35 C36 C37 -178.2(5) . . . . ? C35 C36 C37 C32 -1.3(9) . . . . ? C33 C32 C37 C36 0.1(9) . . . . ? C31 C32 C37 C36 -179.1(6) . . . . ? C36 C35 C38 O10 0.6(7) . . . . ? C34 C35 C38 O10 -180.0(5) . . . . ? C36 C35 C38 O9 179.1(4) . . . . ? C34 C35 C38 O9 -1.4(7) . . . . ? O9 C39 C40 C41 117.8(4) . . . . ? O9 C39 C40 C49 -61.0(6) . . . . ? C49 C40 C41 C42 2.1(6) . . . . ? C39 C40 C41 C42 -176.8(4) . . . . ? C40 C41 C42 C43 179.1(4) . . . . ? C40 C41 C42 C47 1.5(7) . . . . ? C41 C42 C43 C44 -177.3(5) . . . . ? C47 C42 C43 C44 0.2(8) . . . . ? C42 C43 C44 C45 -0.2(10) . . . . ? C43 C44 C45 C46 0.0(11) . . . . ? C44 C45 C46 C47 0.1(10) . . . . ? C45 C46 C47 C42 -0.1(8) . . . . ? C45 C46 C47 C48 -179.4(6) . . . . ? C41 C42 C47 C46 177.5(4) . . . . ? C43 C42 C47 C46 -0.1(7) . . . . ? C41 C42 C47 C48 -3.1(6) . . . . ? C43 C42 C47 C48 179.2(4) . . . . ? C46 C47 C48 C49 -179.6(5) . . . . ? C42 C47 C48 C49 1.1(6) . . . . ? C46 C47 C48 C50 -1.3(7) . . . . ? C42 C47 C48 C50 179.4(4) . . . . ? C47 C48 C49 O11 178.3(4) . . . . ? C50 C48 C49 O11 0.0(6) . . . . ? C47 C48 C49 C40 2.6(6) . . . . ? C50 C48 C49 C40 -175.7(4) . . . . ? C41 C40 C49 C48 -4.2(6) . . . . ? C39 C40 C49 C48 174.6(4) . . . . ? C41 C40 C49 O11 -179.8(4) . . . . ? C39 C40 C49 O11 -1.0(6) . . . . ? C49 C48 C50 C59 85.9(5) . . . . ? C47 C48 C50 C59 -92.4(5) . . . . ? C49 C48 C50 C51 -99.3(5) . . . . ? C47 C48 C50 C51 82.4(5) . . . . ? C59 C50 C51 C52 177.9(4) . . . . ? C48 C50 C51 C52 2.9(6) . . . . ? C59 C50 C51 C56 -2.6(6) . . . . ? C48 C50 C51 C56 -177.6(4) . . . . ? C50 C51 C52 C53 177.5(5) . . . . ? C56 C51 C52 C53 -2.0(7) . . . . ? C51 C52 C53 C54 -0.7(8) . . . . ? C52 C53 C54 C55 2.4(9) . . . . ? C53 C54 C55 C56 -1.3(10) . . . . ? C54 C55 C56 C57 176.5(5) . . . . ? C54 C55 C56 C51 -1.5(8) . . . . ? C52 C51 C56 C57 -175.1(4) . . . . ? C50 C51 C56 C57 5.4(6) . . . . ? C52 C51 C56 C55 3.0(6) . . . . ? C50 C51 C56 C55 -176.5(4) . . . . ? C55 C56 C57 C58 178.7(5) . . . . ? C51 C56 C57 C58 -3.3(7) . . . . ? C56 C57 C58 C59 -1.5(7) . . . . ? C56 C57 C58 C60 174.3(4) . . . . ? C51 C50 C59 O12 -178.6(4) . . . . ? C48 C50 C59 O12 -3.6(6) . . . . ? C51 C50 C59 C58 -2.4(6) . . . . ? C48 C50 C59 C58 172.6(4) . . . . ? C57 C58 C59 C50 4.5(7) . . . . ? C60 C58 C59 C50 -171.3(4) . . . . ? C57 C58 C59 O12 -179.2(4) . . . . ? C60 C58 C59 O12 4.9(6) . . . . ? C57 C58 C60 O1 84.5(7) . . . . ? C59 C58 C60 O1 -99.9(6) . . . . ? O2 C1 O1 C60 -1.8(9) . . . . ? C2 C1 O1 C60 174.0(5) . . . . ? C58 C60 O1 C1 -115.8(6) . . . . ? O4 C8 O3 C9 6.7(8) . . . . ? C5 C8 O3 C9 -174.1(4) . . . . ? C10 C9 O3 C8 -159.5(4) . . . . ? C18 C19 O5 C61 85.3(6) . . . . ? C10 C19 O5 C61 -97.6(6) . . . . ? C20 C29 O6 C62 -104.2(5) . . . . ? C28 C29 O6 C62 81.4(6) . . . . ? O8 C31 O7 C30 2.8(9) . . . . ? C32 C31 O7 C30 -179.7(4) . . . . ? C28 C30 O7 C31 -94.8(6) . . . . ? O10 C38 O9 C39 6.7(7) . . . . ? C35 C38 O9 C39 -171.9(4) . . . . ? C40 C39 O9 C38 -166.1(4) . . . . ? C48 C49 O11 C63 107.9(5) . . . . ? C40 C49 O11 C63 -76.4(6) . . . . ? C50 C59 O12 C64 -101.4(5) . . . . ? C58 C59 O12 C64 82.2(5) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.224 _refine_diff_density_min -0.134 _refine_diff_density_rms 0.032