Supplementary Material (ESI) for Green Chemistry This journal is (C) The Royal Society of Chemistry 2001 data_3c _database_code_CSD 168122 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 2,8,14,20-tetra(p-butoxy-phenyl)pentacyclo-[19.3.1.13,7.19,13.115,19]octacosa- 1-(25),3,5,7(28),9,11,13(27),15,17,19(26),21,23-dodecaene- 4,6,10,12,16,18,22,24-octaol ; _chemical_name_common '2,8,14,20-tetra(p-butoxy-phenyl)resorcinarene DMF/acetone solvate ' _chemical_melting_point ? _chemical_formula_moiety ' C68H70O12.2(C3H8NO).2(C3H6O)' _chemical_formula_sum 'C80 H98 N2 O16' _chemical_formula_weight 1343.60 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2391(2) _cell_length_b 12.8890(2) _cell_length_c 14.4780(4) _cell_angle_alpha 90.7340(10) _cell_angle_beta 110.9560(10) _cell_angle_gamma 112.2100(10) _cell_volume 1786.48(6) _cell_formula_units_Z 1 _exptl_crystal_description rhombs _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.249 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 720 _exptl_absorpt_coefficient_mu 0.086 _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 Kappa CCD diffractometer' _diffrn_measurement_method '1 degree, phi and omega scans' _diffrn_reflns_number 30522 _diffrn_reflns_av_R_equivalents 0.0984 _diffrn_reflns_av_sigmaI/netI 0.1415 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 28.45 _reflns_number_total 8752 _reflns_number_gt 3850 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1140P)^2^+3.8815P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef none _refine_ls_number_reflns 8752 _refine_ls_number_parameters 428 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.2155 _refine_ls_R_factor_gt 0.0979 _refine_ls_wR_factor_ref 0.2877 _refine_ls_wR_factor_gt 0.2273 _refine_ls_goodness_of_fit_ref 0.938 _refine_ls_restrained_S_all 0.946 _refine_ls_shift/su_max 0.183 _refine_ls_shift/su_mean 0.008 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 O1 O 0.8350(3) 0.8511(2) 0.3455(2) 0.0356(7) Uani 1 1 d D . . O2 O 1.0333(3) 1.2568(2) 0.4597(2) 0.0371(7) Uani 1 1 d D . . C37' C 0.6009(4) 0.8168(3) 0.3907(3) 0.0269(9) Uani 1 1 d . . . H37' H 0.5928 0.7696 0.3316 0.032 Uiso 1 1 calc R . . C57' C 0.8155(4) 1.2415(3) 0.5170(3) 0.0275(9) Uani 1 1 d . . . H57' H 0.9147 1.2938 0.5584 0.033 Uiso 1 1 calc R . . O12 O 0.4612(3) 0.8834(3) 0.2147(2) 0.0423(8) Uani 1 1 d D . . O31' O 0.7757(3) 0.6123(2) 0.7331(2) 0.0401(7) Uani 1 1 d . . . C22 C 0.9355(4) 1.0542(3) 0.4008(3) 0.0319(9) Uani 1 1 d . . . H22 H 1.0126 1.0628 0.3840 0.038 Uiso 1 1 calc R . . O51' O 0.6075(4) 1.4795(3) 0.2148(2) 0.0508(9) Uani 1 1 d . A 2 C14 C 0.4580(4) 0.8186(3) 0.3669(3) 0.0267(9) Uani 1 1 d . . . C26 C 0.8194(4) 1.1386(3) 0.4678(3) 0.0283(9) Uani 1 1 d . . . C34' C 0.7273(4) 0.6548(3) 0.6480(3) 0.0329(9) Uani 1 1 d . . . C25 C 0.7128(4) 1.0304(3) 0.4466(3) 0.0287(9) Uani 1 1 d . . . H25 H 0.6346 1.0222 0.4619 0.034 Uiso 1 1 calc R . . C31' C 0.6440(4) 0.7600(3) 0.4813(3) 0.0299(9) Uani 1 1 d . . . C32' C 0.7037(4) 0.8190(3) 0.5798(3) 0.0309(9) Uani 1 1 d . . . H32' H 0.7165 0.8960 0.5906 0.037 Uiso 1 1 calc R . . C24 C 0.7144(4) 0.9341(3) 0.4043(3) 0.0278(9) Uani 1 1 d . . . C36' C 0.6262(4) 0.6474(3) 0.4699(3) 0.0293(9) Uani 1 1 d . . . H36' H 0.5846 0.6049 0.4039 0.035 Uiso 1 1 calc R . . C12 C 0.2675(4) 0.8610(3) 0.2585(3) 0.0345(10) Uani 1 1 d . . . H12 H 0.2261 0.8866 0.1991 0.041 Uiso 1 1 calc R . . C13 C 0.3953(4) 0.8549(3) 0.2800(3) 0.0311(9) Uani 1 1 d . . . C56' C 0.8179(4) 1.4244(3) 0.4543(3) 0.0322(9) Uani 1 1 d . . . H56' H 0.8940 1.4644 0.5160 0.039 Uiso 1 1 calc R . . C15 C 0.3865(4) 0.7871(3) 0.4299(3) 0.0276(9) Uani 1 1 d . . . H15 H 0.4282 0.7620 0.4895 0.033 Uiso 1 1 calc R . . C51' C 0.7571(4) 1.3062(3) 0.4385(3) 0.0302(9) Uani 1 1 d . A . C33' C 0.7443(4) 0.7679(3) 0.6614(3) 0.0334(10) Uani 1 1 d . . . H33' H 0.7843 0.8099 0.7274 0.040 Uiso 1 1 calc R . . C23 C 0.8303(4) 0.9476(3) 0.3837(3) 0.0291(9) Uani 1 1 d . . . C54' C 0.6600(5) 1.4282(4) 0.2936(3) 0.0376(10) Uani 1 1 d . . . C35' C 0.6666(4) 0.5945(3) 0.5505(3) 0.0320(9) Uani 1 1 d . . . H35' H 0.6532 0.5173 0.5396 0.038 Uiso 1 1 calc R . . C21 C 0.9301(4) 1.1488(3) 0.4422(3) 0.0294(9) Uani 1 1 d . . . C55' C 0.7703(4) 1.4860(3) 0.3822(3) 0.0342(10) Uani 1 1 d . A . H55' H 0.8138 1.5667 0.3943 0.041 Uiso 1 1 calc R . . C52' C 0.6424(4) 1.2508(4) 0.3491(3) 0.0375(10) Uani 1 1 d . . . H52' H 0.5964 1.1702 0.3370 0.045 Uiso 1 1 calc R A . C53' C 0.5946(5) 1.3111(4) 0.2778(4) 0.0445(12) Uani 1 1 d . A . H53' H 0.5159 1.2717 0.2173 0.053 Uiso 1 1 calc R . . C39' C 0.8416(5) 0.4732(4) 0.8186(4) 0.0476(12) Uani 1 1 d . . . H39A H 0.8077 0.4885 0.8695 0.057 Uiso 1 1 calc R . . H39B H 0.8247 0.3918 0.8118 0.057 Uiso 1 1 calc R . . C59' C 0.6134(5) 1.6368(4) 0.1275(4) 0.0485(12) Uani 1 1 d . A . H59A H 0.6679 1.7189 0.1317 0.058 Uiso 1 1 calc R . . H59B H 0.6137 1.5951 0.0697 0.058 Uiso 1 1 calc R . . C60' C 0.4683(6) 1.6170(5) 0.1098(4) 0.0587(14) Uani 1 1 d . . . H60A H 0.4673 1.6559 0.1688 0.070 Uiso 1 1 calc R . . H60B H 0.4125 1.5345 0.1023 0.070 Uiso 1 1 calc R . . C40' C 0.9969(5) 0.5445(5) 0.8555(4) 0.0541(13) Uani 1 1 d . . . H40A H 1.0451 0.5231 0.9191 0.065 Uiso 1 1 calc R . . H40B H 1.0152 0.6257 0.8697 0.065 Uiso 1 1 calc R . . C61' C 0.4005(7) 1.6611(5) 0.0148(4) 0.0756(18) Uani 1 1 d . . . H61A H 0.4614 1.7404 0.0183 0.113 Uiso 1 1 calc R . . H61B H 0.3097 1.6564 0.0109 0.113 Uiso 1 1 calc R . . H61C H 0.3875 1.6144 -0.0449 0.113 Uiso 1 1 calc R . . C41' C 1.0564(6) 0.5294(6) 0.7796(5) 0.083(2) Uani 1 1 d . . . H41A H 1.0291 0.4481 0.7593 0.124 Uiso 1 1 calc R . . H41B H 1.1585 0.5685 0.8100 0.124 Uiso 1 1 calc R . . H41C H 1.0200 0.5617 0.7205 0.124 Uiso 1 1 calc R . . C16 C 0.2581(4) 0.7901(3) 0.4112(3) 0.0278(9) Uani 1 1 d . . . C38' C 0.7585(5) 0.4957(4) 0.7193(4) 0.0453(12) Uani 1 1 d . . . H38A H 0.7926 0.4828 0.6677 0.054 Uiso 1 1 calc R . . H38B H 0.6585 0.4437 0.6966 0.054 Uiso 1 1 calc R . . C1A C -0.1018(8) 0.8041(6) 0.0426(6) 0.086(2) Uiso 1 1 d . . . C3A C -0.0834(9) 0.6958(7) 0.0465(6) 0.103(2) Uiso 1 1 d . . . H3A1 H -0.0175 0.6982 0.0160 0.155 Uiso 1 1 calc R . . H3A2 H -0.1737 0.6322 0.0094 0.155 Uiso 1 1 calc R . . H3A3 H -0.0469 0.6857 0.1165 0.155 Uiso 1 1 calc R . . O1A O -0.0438(4) 0.8783(3) 0.1148(3) 0.0724(11) Uiso 1 1 d . . . C2A C -0.2114(13) 0.8039(11) -0.0565(9) 0.181(5) Uiso 1 1 d . . . H2A1 H -0.3035 0.7728 -0.0528 0.272 Uiso 1 1 calc R . . H2A2 H -0.2124 0.7569 -0.1107 0.272 Uiso 1 1 calc R . . H2A3 H -0.1891 0.8819 -0.0699 0.272 Uiso 1 1 calc R . . C11 C 0.2010(4) 0.8297(3) 0.3238(3) 0.0327(10) Uani 1 1 d . . . O11 O 0.0738(3) 0.8347(3) 0.3039(2) 0.0391(7) Uani 1 1 d D . . C58' C 0.6831(5) 1.5990(4) 0.2226(4) 0.0462(12) Uani 1 1 d . . . H58A H 0.7808 1.6156 0.2325 0.055 Uiso 1 1 calc R A 2 H58B H 0.6844 1.6408 0.2810 0.055 Uiso 1 1 calc R A 2 H11O H 0.040(4) 0.857(3) 0.2394(19) 0.040(12) Uiso 1 1 d D . . H2O H 1.116(4) 1.251(5) 0.461(4) 0.073(17) Uiso 1 1 d D . . H1O H 0.932(3) 0.866(6) 0.364(5) 0.11(3) Uiso 1 1 d D . . H12O H 0.399(5) 0.901(5) 0.158(3) 0.079(19) Uiso 1 1 d D . . O1D O 0.3251(8) 0.9561(6) 0.0555(5) 0.091(2) Uiso 0.70 1 d PD B 1 N1D N 0.2546(7) 0.9058(5) -0.1077(5) 0.0938(18) Uiso 1 1 d . B 1 C1D C 0.3055(9) 0.9038(7) -0.0170(7) 0.099(2) Uiso 1 1 d D B 1 H1D H 0.3360 0.8440 -0.0043 0.119 Uiso 1 1 calc R B 1 C2D C 0.0991(12) 0.8789(10) -0.1473(9) 0.099(3) Uiso 0.67 1 d P B 2 H2D1 H 0.0684 0.8704 -0.0914 0.148 Uiso 0.67 1 calc PR B 2 H2D2 H 0.0467 0.8081 -0.1962 0.148 Uiso 0.67 1 calc PR B 2 H2D3 H 0.0824 0.9411 -0.1799 0.148 Uiso 0.67 1 calc PR B 2 C3D C 0.2828(13) 0.8676(10) -0.1842(9) 0.100(3) Uiso 0.67 1 d P B 3 H3D1 H 0.3648 0.8501 -0.1552 0.151 Uiso 0.67 1 calc PR B 3 H3D2 H 0.3013 0.9269 -0.2253 0.151 Uiso 0.67 1 calc PR B 3 H3D3 H 0.2021 0.7990 -0.2262 0.151 Uiso 0.67 1 calc PR B 3 C4D C 0.2648(16) 1.0302(12) -0.1308(12) 0.141(5) Uiso 0.67 1 d P B 4 H4D1 H 0.1714 1.0255 -0.1712 0.211 Uiso 0.67 1 calc PR B 4 H4D2 H 0.3254 1.0584 -0.1677 0.211 Uiso 0.67 1 calc PR B 4 H4D3 H 0.3039 1.0824 -0.0674 0.211 Uiso 0.67 1 calc PR B 4 O1DA O 0.2560(13) 0.8874(11) 0.0287(10) 0.057(3) Uiso 0.30 1 d PD C 5 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 O1 0.0283(16) 0.0342(16) 0.0476(18) 0.0012(13) 0.0171(14) 0.0144(13) O2 0.0240(15) 0.0306(15) 0.0545(19) 0.0026(13) 0.0191(14) 0.0056(12) C37' 0.0222(19) 0.028(2) 0.031(2) 0.0019(16) 0.0103(17) 0.0115(16) C57' 0.0174(18) 0.028(2) 0.031(2) 0.0030(16) 0.0061(16) 0.0063(15) O12 0.0347(17) 0.061(2) 0.0412(19) 0.0195(15) 0.0202(15) 0.0250(15) O31' 0.0421(18) 0.0405(17) 0.0379(17) 0.0126(14) 0.0125(14) 0.0197(14) C22 0.025(2) 0.039(2) 0.036(2) 0.0095(18) 0.0134(18) 0.0166(18) O51' 0.060(2) 0.0363(18) 0.047(2) 0.0102(15) 0.0123(17) 0.0180(16) C14 0.0200(18) 0.0226(19) 0.034(2) 0.0013(16) 0.0094(17) 0.0060(15) C26 0.0221(19) 0.027(2) 0.032(2) 0.0030(17) 0.0086(17) 0.0084(16) C34' 0.024(2) 0.037(2) 0.039(2) 0.0084(19) 0.0142(19) 0.0134(17) C25 0.0226(19) 0.031(2) 0.033(2) 0.0043(17) 0.0124(17) 0.0099(16) C31' 0.0213(19) 0.033(2) 0.036(2) 0.0046(18) 0.0110(17) 0.0115(16) C32' 0.027(2) 0.028(2) 0.038(2) 0.0038(18) 0.0134(19) 0.0114(17) C24 0.0210(19) 0.029(2) 0.031(2) 0.0048(17) 0.0092(17) 0.0094(16) C36' 0.0211(19) 0.031(2) 0.033(2) 0.0020(17) 0.0102(17) 0.0087(16) C12 0.030(2) 0.039(2) 0.037(2) 0.0116(19) 0.0122(19) 0.0171(18) C13 0.028(2) 0.028(2) 0.035(2) 0.0045(17) 0.0133(19) 0.0085(17) C56' 0.027(2) 0.033(2) 0.035(2) 0.0011(18) 0.0135(18) 0.0097(17) C15 0.0220(19) 0.025(2) 0.031(2) -0.0001(16) 0.0073(17) 0.0073(15) C51' 0.022(2) 0.030(2) 0.038(2) 0.0032(18) 0.0135(18) 0.0092(16) C33' 0.032(2) 0.035(2) 0.033(2) 0.0012(18) 0.0119(19) 0.0148(18) C23 0.025(2) 0.032(2) 0.033(2) 0.0062(17) 0.0117(18) 0.0145(17) C54' 0.039(2) 0.034(2) 0.038(3) 0.0108(19) 0.015(2) 0.0128(19) C35' 0.024(2) 0.028(2) 0.041(3) 0.0039(18) 0.0139(19) 0.0076(16) C21 0.022(2) 0.029(2) 0.034(2) 0.0060(17) 0.0099(17) 0.0094(16) C55' 0.033(2) 0.028(2) 0.042(3) 0.0029(19) 0.019(2) 0.0093(18) C52' 0.031(2) 0.030(2) 0.044(3) 0.0043(19) 0.008(2) 0.0105(18) C53' 0.037(3) 0.039(3) 0.042(3) 0.003(2) 0.003(2) 0.011(2) C39' 0.049(3) 0.050(3) 0.048(3) 0.012(2) 0.014(2) 0.027(2) C59' 0.061(3) 0.045(3) 0.048(3) 0.011(2) 0.026(3) 0.026(2) C60' 0.068(4) 0.057(3) 0.047(3) 0.001(2) 0.017(3) 0.026(3) C40' 0.044(3) 0.076(4) 0.043(3) 0.006(3) 0.012(2) 0.031(3) C61' 0.079(4) 0.078(4) 0.058(4) 0.012(3) 0.005(3) 0.041(4) C41' 0.058(4) 0.127(6) 0.062(4) -0.003(4) 0.020(3) 0.040(4) C16 0.0221(19) 0.026(2) 0.031(2) -0.0014(16) 0.0092(17) 0.0078(15) C38' 0.047(3) 0.035(2) 0.050(3) 0.011(2) 0.011(2) 0.019(2) C11 0.024(2) 0.032(2) 0.039(2) 0.0021(18) 0.0101(19) 0.0117(17) O11 0.0284(16) 0.0551(19) 0.0381(18) 0.0107(15) 0.0118(14) 0.0224(14) C58' 0.055(3) 0.037(3) 0.052(3) 0.013(2) 0.027(3) 0.019(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C23 1.382(5) . ? O2 C21 1.381(5) . ? C37' C24 1.519(5) . ? C37' C14 1.527(5) . ? C37' C31' 1.525(6) . ? C57' C16 1.517(6) 2_676 ? C57' C26 1.520(5) . ? C57' C51' 1.525(6) . ? O12 C13 1.371(5) . ? O31' C34' 1.369(5) . ? O31' C38' 1.443(5) . ? C22 C23 1.379(5) . ? C22 C21 1.382(5) . ? O51' C54' 1.386(5) . ? O51' C58' 1.429(5) . ? C14 C13 1.389(6) . ? C14 C15 1.388(5) . ? C26 C21 1.382(5) . ? C26 C25 1.391(5) . ? C34' C33' 1.398(6) . ? C34' C35' 1.395(6) . ? C25 C24 1.386(5) . ? C31' C36' 1.388(5) . ? C31' C32' 1.401(6) . ? C32' C33' 1.378(6) . ? C24 C23 1.386(5) . ? C36' C35' 1.382(6) . ? C12 C11 1.379(6) . ? C12 C13 1.390(6) . ? C56' C51' 1.389(5) . ? C56' C55' 1.397(6) . ? C15 C16 1.386(5) . ? C51' C52' 1.391(6) . ? C54' C55' 1.370(6) . ? C54' C53' 1.379(6) . ? C52' C53' 1.377(6) . ? C39' C40' 1.512(7) . ? C39' C38' 1.510(6) . ? C59' C60' 1.475(7) . ? C59' C58' 1.511(7) . ? C60' C61' 1.546(8) . ? C40' C41' 1.522(8) . ? C16 C11 1.400(6) . ? C16 C57' 1.517(6) 2_676 ? C1A O1A 1.203(7) . ? C1A C3A 1.485(10) . ? C1A C2A 1.520(13) . ? C11 O11 1.380(5) . ? O1D C1D 1.144(9) . ? N1D C1D 1.236(9) . ? N1D C3D 1.387(12) . ? N1D C2D 1.524(12) . ? N1D C4D 1.612(15) . ? 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 C24 C37' C14 112.7(3) . . ? C24 C37' C31' 110.5(3) . . ? C14 C37' C31' 112.3(3) . . ? C16 C57' C26 111.9(3) 2_676 . ? C16 C57' C51' 113.6(3) 2_676 . ? C26 C57' C51' 111.0(3) . . ? C34' O31' C38' 116.7(3) . . ? C23 C22 C21 120.7(4) . . ? C54' O51' C58' 117.4(3) . . ? C13 C14 C15 117.2(4) . . ? C13 C14 C37' 120.0(4) . . ? C15 C14 C37' 122.9(3) . . ? C21 C26 C25 117.0(3) . . ? C21 C26 C57' 121.0(3) . . ? C25 C26 C57' 121.9(3) . . ? O31' C34' C33' 116.7(4) . . ? O31' C34' C35' 124.7(4) . . ? C33' C34' C35' 118.6(4) . . ? C24 C25 C26 123.6(4) . . ? C36' C31' C32' 116.8(4) . . ? C36' C31' C37' 121.4(4) . . ? C32' C31' C37' 121.8(3) . . ? C33' C32' C31' 121.6(4) . . ? C23 C24 C25 117.4(3) . . ? C23 C24 C37' 121.1(3) . . ? C25 C24 C37' 121.3(3) . . ? C31' C36' C35' 122.6(4) . . ? C11 C12 C13 119.8(4) . . ? O12 C13 C14 118.7(4) . . ? O12 C13 C12 120.4(4) . . ? C14 C13 C12 120.9(4) . . ? C51' C56' C55' 121.8(4) . . ? C16 C15 C14 124.2(4) . . ? C56' C51' C52' 117.4(4) . . ? C56' C51' C57' 120.5(3) . . ? C52' C51' C57' 122.1(4) . . ? C32' C33' C34' 120.6(4) . . ? C22 C23 O1 122.1(3) . . ? C22 C23 C24 120.4(4) . . ? O1 C23 C24 117.6(3) . . ? C55' C54' C53' 120.2(4) . . ? C55' C54' O51' 124.3(4) . . ? C53' C54' O51' 115.6(4) . . ? C36' C35' C34' 119.8(4) . . ? C26 C21 O2 117.0(3) . . ? C26 C21 C22 120.8(4) . . ? O2 C21 C22 122.2(4) . . ? C54' C55' C56' 119.0(4) . . ? C53' C52' C51' 121.0(4) . . ? C52' C53' C54' 120.5(4) . . ? C40' C39' C38' 113.4(4) . . ? C60' C59' C58' 112.5(4) . . ? C59' C60' C61' 111.9(5) . . ? C39' C40' C41' 112.2(4) . . ? C15 C16 C11 116.4(4) . . ? C15 C16 C57' 123.0(4) . 2_676 ? C11 C16 C57' 120.6(3) . 2_676 ? O31' C38' C39' 107.9(4) . . ? O1A C1A C3A 122.0(7) . . ? O1A C1A C2A 124.9(8) . . ? C3A C1A C2A 112.8(8) . . ? C12 C11 O11 120.8(4) . . ? C12 C11 C16 121.6(4) . . ? O11 C11 C16 117.6(4) . . ? O51' C58' C59' 109.1(4) . . ? C1D N1D C3D 128.4(8) . . ? C1D N1D C2D 113.2(8) . . ? C3D N1D C2D 108.4(8) . . ? C1D N1D C4D 112.8(8) . . ? C3D N1D C4D 101.6(9) . . ? C2D N1D C4D 82.1(8) . . ? O1D C1D N1D 135.8(9) . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 28.45 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.796 _refine_diff_density_min -0.631 _refine_diff_density_rms 0.075