Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_sad _database_code_CSD 162090 _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'L. R. MacGillivray' 'J. L. Reid' 'J. A. Ripmeester' _publ_contact_author_name 'L. R. MacGillivray' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C68 H68 N2 O8' _chemical_formula_weight 1069.31 _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' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 12.9078(8) _cell_length_b 13.7910(9) _cell_length_c 16.6485(10) _cell_angle_alpha 93.7700(10) _cell_angle_beta 102.7610(10) _cell_angle_gamma 91.189(2) _cell_volume 2882.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.23 _exptl_crystal_density_method ? _exptl_crystal_F_000 1136 _exptl_absorpt_coefficient_mu 0.071 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12675 _diffrn_reflns_av_R_equivalents 0.0476 _diffrn_reflns_av_sigmaI/netI 0.0909 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 22.50 _reflns_number_total 7512 _reflns_number_observed 4226 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 977 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0747P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6535 _refine_ls_number_parameters 738 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1281 _refine_ls_R_factor_obs 0.0589 _refine_ls_wR_factor_all 0.1622 _refine_ls_wR_factor_obs 0.1297 _refine_ls_goodness_of_fit_all 1.025 _refine_ls_goodness_of_fit_obs 1.156 _refine_ls_restrained_S_all 1.043 _refine_ls_restrained_S_obs 1.156 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group O1 O 0.2163(2) -0.3380(2) 0.1618(2) 0.0363(7) Uani 1 d . . H1 H 0.2721(17) -0.3540(15) 0.1940(12) 0.044 Uiso 1 calc R . O2 O 0.2174(2) -0.1073(2) 0.39085(15) 0.0350(7) Uani 1 d . . H2O H 0.2722(18) -0.1373(20) 0.4106(6) 0.042 Uiso 1 calc R . O3 O 0.0454(2) -0.3480(2) -0.0970(2) 0.0332(7) Uani 1 d . . H3 H 0.0428(23) -0.3947(12) -0.1325(14) 0.040 Uiso 1 calc R . O4 O -0.2318(2) -0.5419(2) -0.0269(2) 0.0335(7) Uani 1 d . . H4 H -0.2210(19) -0.5778(15) -0.0667(15) 0.040 Uiso 1 calc R . O5 O -0.0379(2) -0.5114(2) 0.22493(15) 0.0340(7) Uani 1 d . . H5O H 0.0145(18) -0.5294(18) 0.2596(8) 0.041 Uiso 1 calc R . O6 O -0.0459(2) -0.2863(2) 0.45549(15) 0.0321(7) Uani 1 d . . H6 H 0.0021(20) -0.3227(16) 0.4775(7) 0.038 Uiso 1 calc R . O7 O -0.2353(2) -0.0396(2) 0.4860(2) 0.0310(7) Uani 1 d . . H7O H -0.2262(19) 0.0033(16) 0.5254(13) 0.037 Uiso 1 calc R . O8 O 0.0386(2) 0.1551(2) 0.4127(2) 0.0306(7) Uani 1 d . . H8 H 0.0393(24) 0.1841(14) 0.4588(10) 0.037 Uiso 1 calc R . N1 N 0.4090(3) -0.4081(3) 0.2408(2) 0.0435(10) Uani 1 d . . N2 N 0.8899(2) -0.6075(3) 0.4501(2) 0.0356(9) Uani 1 d . . N3 N 0.3907(3) -0.1971(3) 0.4744(2) 0.0426(10) Uani 1 d . . N4 N 0.8569(3) -0.4185(3) 0.6836(2) 0.0396(9) Uani 1 d . . C1 C 0.1810(3) -0.2534(3) 0.1938(2) 0.0268(10) Uani 1 d . . C2 C 0.2151(3) -0.2237(3) 0.2766(2) 0.0287(10) Uani 1 d . . H2 H 0.2627(3) -0.2623(3) 0.3119(2) 0.034 Uiso 1 calc R . C3 C 0.1806(3) -0.1385(3) 0.3085(2) 0.0236(9) Uani 1 d . . C4 C 0.1101(3) -0.0803(3) 0.2588(2) 0.0216(9) Uani 1 d . . C5 C 0.0779(3) -0.1142(3) 0.1756(2) 0.0229(9) Uani 1 d . . H5 H 0.0291(3) -0.0764(3) 0.1404(2) 0.027 Uiso 1 calc R . C6 C 0.1112(3) -0.1980(3) 0.1407(2) 0.0220(9) Uani 1 d . . C7 C 0.0773(3) -0.2289(3) 0.0491(2) 0.0262(10) Uani 1 d . . H7 H 0.1419(3) -0.2537(3) 0.0318(2) 0.031 Uiso 1 calc R . C8 C 0.0407(3) -0.1440(3) -0.0032(2) 0.0351(11) Uani 1 d . . H8C H 0.0246(3) -0.1667(3) -0.0618(2) 0.042 Uiso 1 calc R . H8B H 0.0973(3) -0.0932(3) 0.0073(2) 0.042 Uiso 1 calc R . H8A H -0.0232(3) -0.1175(3) 0.0113(2) 0.042 Uiso 1 calc R . C9 C -0.0057(3) -0.3121(3) 0.0297(2) 0.0227(9) Uani 1 d . . C10 C -0.0197(3) -0.3691(3) -0.0450(2) 0.0260(10) Uani 1 d . . C11 C -0.0954(3) -0.4447(3) -0.0646(2) 0.0277(10) Uani 1 d . . H11 H -0.1047(3) -0.4821(3) -0.1158(2) 0.033 Uiso 1 calc R . C12 C -0.1575(3) -0.4656(3) -0.0093(2) 0.0258(10) Uani 1 d . . C13 C -0.1467(3) -0.4114(3) 0.0652(2) 0.0228(9) Uani 1 d . . C14 C -0.0710(3) -0.3357(3) 0.0824(2) 0.0246(9) Uani 1 d . . H14 H -0.0632(3) -0.2976(3) 0.1332(2) 0.030 Uiso 1 calc R . C15 C -0.2174(3) -0.4358(3) 0.1246(2) 0.0268(10) Uani 1 d . . H15 H -0.2198(3) -0.5082(3) 0.1260(2) 0.032 Uiso 1 calc R . C16 C -0.3309(3) -0.4058(3) 0.0898(2) 0.0357(11) Uani 1 d . . H16C H -0.3590(3) -0.4419(3) 0.0365(2) 0.043 Uiso 1 calc R . H16B H -0.3308(3) -0.3359(3) 0.0823(2) 0.043 Uiso 1 calc R . H16A H -0.3757(3) -0.4203(3) 0.1283(2) 0.043 Uiso 1 calc R . C17 C -0.1720(3) -0.3945(3) 0.2119(2) 0.0215(9) Uani 1 d . . C18 C -0.0824(3) -0.4347(3) 0.2592(2) 0.0218(9) Uani 1 d . . C19 C -0.0388(3) -0.3968(3) 0.3391(2) 0.0258(10) Uani 1 d . . H19 H 0.0236(3) -0.4236(3) 0.3700(2) 0.031 Uiso 1 calc R . C20 C -0.0857(3) -0.3200(3) 0.3744(2) 0.0246(9) Uani 1 d . . C21 C -0.1743(3) -0.2767(3) 0.3295(2) 0.0220(9) Uani 1 d . . C22 C -0.2143(3) -0.3166(3) 0.2490(2) 0.0234(9) Uani 1 d . . H22 H -0.2751(3) -0.2883(3) 0.2174(2) 0.028 Uiso 1 calc R . C23 C -0.2222(3) -0.1903(3) 0.3674(2) 0.0248(9) Uani 1 d . . H23 H -0.2311(3) -0.2077(3) 0.4230(2) 0.030 Uiso 1 calc R . C24 C -0.3320(3) -0.1656(3) 0.3179(3) 0.0342(11) Uani 1 d . . H24C H -0.3597(3) -0.1116(3) 0.3471(3) 0.041 Uiso 1 calc R . H24B H -0.3805(3) -0.2226(3) 0.3114(3) 0.041 Uiso 1 calc R . H24A H -0.3260(3) -0.1467(3) 0.2633(3) 0.041 Uiso 1 calc R . C25 C -0.1495(3) -0.0992(3) 0.3810(2) 0.0227(9) Uani 1 d . . C26 C -0.1614(3) -0.0247(3) 0.4394(2) 0.0217(9) Uani 1 d . . C27 C -0.1000(3) 0.0606(3) 0.4489(2) 0.0242(9) Uani 1 d . . H27 H -0.1097(3) 0.1115(3) 0.4874(2) 0.029 Uiso 1 calc R . C28 C -0.0249(3) 0.0717(3) 0.4027(2) 0.0199(9) Uani 1 d . . C29 C -0.0090(3) -0.0004(3) 0.3448(2) 0.0219(9) Uani 1 d . . C30 C -0.0735(3) -0.0841(3) 0.3350(2) 0.0230(9) Uani 1 d . . H30 H -0.0653(3) -0.1338(3) 0.2947(2) 0.028 Uiso 1 calc R . C31 C 0.0737(3) 0.0141(3) 0.2939(2) 0.0221(9) Uani 1 d . . H31 H 0.1375(3) 0.0469(3) 0.3318(2) 0.027 Uiso 1 calc R . C32 C 0.0327(3) 0.0839(3) 0.2266(2) 0.0307(10) Uani 1 d . . H32C H 0.0253(3) 0.1485(3) 0.2525(2) 0.037 Uiso 1 calc R . H32B H -0.0365(3) 0.0594(3) 0.1937(2) 0.037 Uiso 1 calc R . H32A H 0.0833(3) 0.0882(3) 0.1908(2) 0.037 Uiso 1 calc R . C33 C 0.4684(4) -0.3683(4) 0.3107(3) 0.062(2) Uani 1 d . . H33 H 0.4439(4) -0.3118(4) 0.3355(3) 0.074 Uiso 1 calc R . C34 C 0.5633(3) -0.4040(3) 0.3492(3) 0.061(2) Uani 1 d . . H34 H 0.6026(3) -0.3714(3) 0.3990(3) 0.074 Uiso 1 calc R . C35 C 0.6033(3) -0.4863(3) 0.3170(3) 0.0321(10) Uani 1 d . . C36 C 0.5419(4) -0.5268(4) 0.2451(3) 0.0545(14) Uani 1 d . . H36 H 0.5644(4) -0.5836(4) 0.2193(3) 0.065 Uiso 1 calc R . C37 C 0.4463(4) -0.4861(4) 0.2084(3) 0.0590(15) Uani 1 d . . H37 H 0.4062(4) -0.5161(4) 0.1578(3) 0.071 Uiso 1 calc R . C38 C 0.7044(3) -0.5274(3) 0.3605(3) 0.0316(10) Uani 1 d . . C39 C 0.7641(3) -0.4821(3) 0.4330(3) 0.0407(11) Uani 1 d . . H39 H 0.7427(3) -0.4220(3) 0.4542(3) 0.049 Uiso 1 calc R . C40 C 0.8539(3) -0.5239(3) 0.4744(3) 0.0434(12) Uani 1 d . . H40 H 0.8931(3) -0.4905(3) 0.5239(3) 0.052 Uiso 1 calc R . C41 C 0.7441(3) -0.6126(3) 0.3328(3) 0.0442(12) Uani 1 d . . H41 H 0.7088(3) -0.6458(3) 0.2820(3) 0.053 Uiso 1 calc R . C42 C 0.8351(3) -0.6495(3) 0.3790(3) 0.0437(12) Uani 1 d . . H42 H 0.8599(3) -0.7085(3) 0.3587(3) 0.052 Uiso 1 calc R . C43 C 0.4861(4) -0.1573(3) 0.4808(3) 0.0439(12) Uani 1 d . . H43 H 0.4912(4) -0.0986(3) 0.4549(3) 0.053 Uiso 1 calc R . C44 C 0.5790(3) -0.1951(3) 0.5224(3) 0.0417(12) Uani 1 d . . H44 H 0.6454(3) -0.1630(3) 0.5242(3) 0.050 Uiso 1 calc R . C45 C 0.5751(3) -0.2801(3) 0.5616(2) 0.0325(10) Uani 1 d . . C46 C 0.4757(3) -0.3208(4) 0.5563(3) 0.063(2) Uani 1 d . . H46 H 0.4680(3) -0.3784(4) 0.5830(3) 0.076 Uiso 1 calc R . C47 C 0.3865(4) -0.2782(4) 0.5122(3) 0.070(2) Uani 1 d . . H47 H 0.3188(4) -0.3087(4) 0.5088(3) 0.084 Uiso 1 calc R . C48 C 0.6728(3) -0.3265(3) 0.6053(2) 0.0352(11) Uani 1 d . . C49 C 0.7720(3) -0.2841(3) 0.6151(3) 0.0400(11) Uani 1 d . . H49 H 0.7802(3) -0.2219(3) 0.5955(3) 0.048 Uiso 1 calc R . C50 C 0.8605(3) -0.3323(3) 0.6535(3) 0.0432(12) Uani 1 d . . H50 H 0.9283(3) -0.3014(3) 0.6587(3) 0.052 Uiso 1 calc R . C51 C 0.6687(3) -0.4183(4) 0.6347(3) 0.068(2) Uani 1 d . . H51 H 0.6024(3) -0.4524(4) 0.6284(3) 0.082 Uiso 1 calc R . C52 C 0.7611(4) -0.4594(4) 0.6728(3) 0.070(2) Uani 1 d . . H52 H 0.7556(4) -0.5219(4) 0.6927(3) 0.084 Uiso 1 calc R . C53 C 0.3910(4) -0.2576(4) 0.8885(3) 0.0504(13) Uani 1 d . . C54 C 0.4271(4) -0.2027(3) 0.8320(3) 0.0538(14) Uani 1 d . . H54 H 0.5010(4) -0.1992(3) 0.8331(3) 0.065 Uiso 1 calc R . C55 C 0.3573(4) -0.1527(3) 0.7739(3) 0.0532(13) Uani 1 d . . C56 C 0.2499(4) -0.1583(3) 0.7744(3) 0.0515(13) Uani 1 d . . H56 H 0.2008(4) -0.1239(3) 0.7363(3) 0.062 Uiso 1 calc R . C57 C 0.2138(4) -0.2129(4) 0.8293(3) 0.0534(13) Uani 1 d . . H57 H 0.1399(4) -0.2165(4) 0.8281(3) 0.064 Uiso 1 calc R . C58 C 0.2831(4) -0.2629(4) 0.8864(3) 0.0558(14) Uani 1 d . . H58 H 0.2569(4) -0.3007(4) 0.9238(3) 0.067 Uiso 1 calc R . C59 C 0.4680(4) -0.3090(4) 0.9524(3) 0.079(2) Uani 1 d . . H59C H 0.4910(4) -0.2655(4) 1.0025(3) 0.094 Uiso 1 calc R . H59B H 0.5299(4) -0.3271(4) 0.9305(3) 0.094 Uiso 1 calc R . H59A H 0.4329(4) -0.3677(4) 0.9656(3) 0.094 Uiso 1 calc R . C60 C 0.3999(5) -0.0971(4) 0.7129(4) 0.085(2) Uani 1 d . . H60C H 0.4600(5) -0.1309(4) 0.6985(4) 0.102 Uiso 1 calc R . H60B H 0.4236(5) -0.0316(4) 0.7374(4) 0.102 Uiso 1 calc R . H60A H 0.3438(5) -0.0924(4) 0.6631(4) 0.102 Uiso 1 calc R . C61 C 0.2725(7) 0.1450(8) 1.1110(13) 0.165(6) Uani 1 d . . C62 C 0.3139(6) 0.0528(9) 1.1575(7) 0.129(3) Uani 1 d . . H62 H 0.3180(6) 0.0485(9) 1.2149(7) 0.155 Uiso 1 calc R . C63 C 0.3448(13) -0.0235(24) 1.1071(8) 0.366(23) Uani 1 d . . C64 C 0.3336(7) -0.0088(7) 1.0329(11) 0.194(8) Uani 1 d . . H64 H 0.3533(7) -0.0620(7) 1.0011(11) 0.233 Uiso 1 calc R . C65 C 0.2932(10) 0.0803(12) 0.9801(12) 0.215(11) Uani 1 d . . C66 C 0.2692(7) 0.1438(12) 1.0310(8) 0.165(8) Uani 1 d . . H66 H 0.2439(7) 0.2019(12) 1.0070(8) 0.199 Uiso 1 calc R . C67 C 0.2594(9) 0.2232(13) 1.1589(10) 0.167(6) Uani 0.67 d P . H67C H 0.3206(9) 0.2323(13) 1.2058(10) 0.201 Uiso 0.67 calc PR . H67B H 0.1945(9) 0.2140(13) 1.1792(10) 0.201 Uiso 0.67 calc PR . H67A H 0.2536(9) 0.2806(13) 1.1268(10) 0.201 Uiso 0.67 calc PR . C68 C 0.3916(11) -0.1026(12) 1.1523(13) 0.267(15) Uani 0.67 d P . H68C H 0.3722(11) -0.1005(12) 1.2060(13) 0.320 Uiso 0.67 calc PR . H68B H 0.4691(11) -0.0970(12) 1.1606(13) 0.320 Uiso 0.67 calc PR . H68A H 0.3656(11) -0.1643(12) 1.1211(13) 0.320 Uiso 0.67 calc PR . C69 C 0.2862(13) 0.0919(11) 0.9032(7) 0.160(7) Uani 0.67 d P . H69C H 0.2126(13) 0.0787(11) 0.8727(7) 0.192 Uiso 0.67 calc PR . H69B H 0.3330(13) 0.0470(11) 0.8816(7) 0.192 Uiso 0.67 calc PR . H69A H 0.3077(13) 0.1590(11) 0.8966(7) 0.192 Uiso 0.67 calc PR . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.036(2) 0.035(2) 0.033(2) -0.0085(14) -0.0019(13) 0.0151(14) O2 0.037(2) 0.039(2) 0.024(2) -0.0031(14) -0.0018(13) 0.0175(14) O3 0.041(2) 0.035(2) 0.024(2) -0.0057(13) 0.0109(15) -0.0018(14) O4 0.040(2) 0.032(2) 0.028(2) -0.0074(13) 0.0085(14) -0.0010(15) O5 0.038(2) 0.037(2) 0.024(2) -0.0012(14) 0.0007(13) 0.0157(14) O6 0.039(2) 0.030(2) 0.022(2) -0.0034(13) -0.0034(13) 0.0103(13) O7 0.040(2) 0.029(2) 0.028(2) -0.0050(13) 0.0167(14) 0.0002(14) O8 0.039(2) 0.024(2) 0.029(2) -0.0060(13) 0.0102(14) -0.0057(14) N1 0.044(2) 0.041(2) 0.046(3) 0.009(2) 0.007(2) 0.008(2) N2 0.034(2) 0.037(2) 0.033(2) 0.002(2) 0.001(2) 0.007(2) N3 0.036(2) 0.054(3) 0.036(2) 0.010(2) 0.002(2) 0.013(2) N4 0.034(2) 0.044(3) 0.042(2) 0.012(2) 0.008(2) 0.004(2) C1 0.027(2) 0.022(2) 0.031(3) -0.002(2) 0.007(2) 0.004(2) C2 0.032(2) 0.030(3) 0.022(2) 0.000(2) 0.001(2) 0.011(2) C3 0.028(2) 0.028(2) 0.014(2) -0.004(2) 0.004(2) 0.002(2) C4 0.027(2) 0.023(2) 0.016(2) -0.001(2) 0.006(2) 0.001(2) C5 0.023(2) 0.022(2) 0.025(2) 0.007(2) 0.005(2) 0.004(2) C6 0.023(2) 0.024(2) 0.019(2) 0.001(2) 0.004(2) 0.000(2) C7 0.030(2) 0.026(2) 0.022(2) -0.003(2) 0.005(2) 0.004(2) C8 0.046(3) 0.034(3) 0.025(2) 0.004(2) 0.007(2) 0.001(2) C9 0.027(2) 0.023(2) 0.016(2) -0.001(2) -0.002(2) 0.002(2) C10 0.030(2) 0.026(2) 0.022(2) 0.004(2) 0.004(2) 0.010(2) C11 0.034(2) 0.027(2) 0.020(2) -0.002(2) 0.002(2) 0.008(2) C12 0.025(2) 0.024(2) 0.026(2) 0.000(2) 0.002(2) 0.001(2) C13 0.027(2) 0.023(2) 0.017(2) -0.002(2) 0.001(2) 0.008(2) C14 0.029(2) 0.026(2) 0.016(2) -0.003(2) 0.001(2) 0.005(2) C15 0.027(2) 0.027(2) 0.024(2) 0.002(2) 0.001(2) 0.003(2) C16 0.033(2) 0.039(3) 0.033(3) -0.001(2) 0.004(2) 0.002(2) C17 0.027(2) 0.017(2) 0.021(2) 0.003(2) 0.006(2) 0.000(2) C18 0.026(2) 0.023(2) 0.018(2) 0.002(2) 0.009(2) 0.002(2) C19 0.027(2) 0.021(2) 0.029(2) 0.003(2) 0.003(2) 0.005(2) C20 0.028(2) 0.025(2) 0.019(2) 0.001(2) 0.001(2) -0.001(2) C21 0.027(2) 0.020(2) 0.019(2) 0.001(2) 0.007(2) -0.001(2) C22 0.026(2) 0.023(2) 0.023(2) 0.007(2) 0.007(2) 0.000(2) C23 0.028(2) 0.025(2) 0.022(2) 0.000(2) 0.007(2) 0.002(2) C24 0.030(2) 0.028(2) 0.044(3) -0.002(2) 0.008(2) 0.002(2) C25 0.026(2) 0.021(2) 0.019(2) 0.004(2) 0.000(2) 0.006(2) C26 0.024(2) 0.022(2) 0.021(2) 0.007(2) 0.008(2) 0.004(2) C27 0.031(2) 0.022(2) 0.021(2) -0.003(2) 0.009(2) 0.005(2) C28 0.024(2) 0.017(2) 0.018(2) 0.004(2) 0.001(2) 0.002(2) C29 0.025(2) 0.022(2) 0.019(2) 0.004(2) 0.004(2) 0.004(2) C30 0.028(2) 0.023(2) 0.020(2) 0.003(2) 0.008(2) 0.006(2) C31 0.027(2) 0.020(2) 0.018(2) 0.001(2) 0.003(2) 0.005(2) C32 0.039(2) 0.025(2) 0.029(2) 0.002(2) 0.010(2) 0.003(2) C33 0.042(3) 0.048(3) 0.086(4) -0.023(3) 0.000(3) 0.016(3) C34 0.037(3) 0.048(3) 0.086(4) -0.024(3) -0.006(3) 0.011(3) C35 0.028(2) 0.032(3) 0.040(3) 0.010(2) 0.012(2) 0.000(2) C36 0.058(3) 0.063(3) 0.037(3) -0.005(3) 0.000(3) 0.032(3) C37 0.058(3) 0.077(4) 0.041(3) -0.001(3) 0.007(3) 0.038(3) C38 0.027(2) 0.035(3) 0.036(3) 0.015(2) 0.010(2) 0.004(2) C39 0.050(3) 0.037(3) 0.036(3) 0.005(2) 0.009(2) 0.016(2) C40 0.053(3) 0.041(3) 0.032(3) 0.003(2) 0.001(2) 0.011(3) C41 0.046(3) 0.043(3) 0.036(3) -0.008(2) -0.006(2) 0.008(2) C42 0.039(3) 0.037(3) 0.048(3) -0.006(2) -0.006(2) 0.012(2) C43 0.046(3) 0.039(3) 0.048(3) 0.017(2) 0.008(3) 0.014(3) C44 0.041(3) 0.041(3) 0.044(3) 0.012(2) 0.008(2) 0.002(2) C45 0.031(3) 0.039(3) 0.029(2) 0.010(2) 0.007(2) 0.007(2) C46 0.032(3) 0.074(4) 0.083(4) 0.051(3) 0.000(3) 0.002(3) C47 0.037(3) 0.092(5) 0.083(4) 0.050(4) 0.007(3) 0.002(3) C48 0.036(3) 0.036(3) 0.037(3) 0.009(2) 0.016(2) 0.005(2) C49 0.033(3) 0.025(3) 0.059(3) 0.012(2) 0.001(2) -0.002(2) C50 0.032(3) 0.032(3) 0.061(3) 0.000(2) 0.004(2) -0.003(2) C51 0.026(3) 0.072(4) 0.108(5) 0.054(4) 0.006(3) -0.003(3) C52 0.042(3) 0.067(4) 0.106(5) 0.059(3) 0.012(3) 0.011(3) C53 0.040(3) 0.057(3) 0.050(3) 0.007(3) -0.003(3) 0.007(3) C54 0.044(3) 0.049(3) 0.068(4) 0.014(3) 0.006(3) 0.005(3) C55 0.066(4) 0.037(3) 0.054(3) 0.012(3) 0.005(3) 0.006(3) C56 0.050(3) 0.046(3) 0.050(3) -0.003(3) -0.005(3) 0.021(3) C57 0.049(3) 0.060(4) 0.052(3) 0.002(3) 0.011(3) 0.013(3) C58 0.053(3) 0.058(3) 0.055(3) 0.007(3) 0.007(3) 0.010(3) C59 0.071(4) 0.082(4) 0.074(4) 0.023(3) -0.009(3) 0.006(3) C60 0.106(5) 0.063(4) 0.090(5) 0.033(4) 0.021(4) 0.018(4) C61 0.047(5) 0.108(9) 0.343(22) -0.025(11) 0.061(9) 0.000(5) C62 0.071(5) 0.180(10) 0.141(9) 0.068(8) 0.025(6) -0.040(6) C63 0.134(13) 0.830(66) 0.117(11) 0.004(20) 0.024(10) -0.254(25) C64 0.084(6) 0.050(5) 0.435(25) -0.018(9) 0.038(10) -0.004(5) C65 0.142(11) 0.216(17) 0.300(21) -0.147(18) 0.134(14) -0.088(11) C66 0.054(5) 0.277(19) 0.159(10) 0.137(13) -0.020(7) -0.067(8) C67 0.079(9) 0.208(18) 0.225(18) 0.057(15) 0.042(10) 0.016(10) C68 0.131(12) 0.218(17) 0.430(33) 0.279(22) -0.058(15) -0.026(11) C69 0.262(18) 0.138(13) 0.069(8) 0.005(9) 0.022(10) -0.052(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C1 1.379(4) . ? O2 C3 1.384(4) . ? O3 C10 1.374(4) . ? O4 C12 1.381(4) . ? O5 C18 1.365(4) . ? O6 C20 1.380(4) . ? O7 C26 1.376(4) . ? O8 C28 1.378(4) . ? N1 C37 1.318(5) . ? N1 C33 1.322(5) . ? N2 C40 1.324(5) . ? N2 C42 1.326(5) . ? N3 C43 1.317(5) . ? N3 C47 1.325(6) . ? N4 C52 1.319(5) . ? N4 C50 1.323(5) . ? C1 C2 1.384(5) . ? C1 C6 1.393(5) . ? C2 C3 1.380(5) . ? C3 C4 1.393(5) . ? C4 C5 1.400(5) . ? C4 C31 1.518(5) . ? C5 C6 1.379(5) . ? C6 C7 1.521(5) . ? C7 C9 1.521(5) . ? C7 C8 1.525(5) . ? C9 C14 1.393(5) . ? C9 C10 1.401(5) . ? C10 C11 1.386(5) . ? C11 C12 1.387(5) . ? C12 C13 1.384(5) . ? C13 C14 1.386(5) . ? C13 C15 1.535(5) . ? C15 C17 1.510(5) . ? C15 C16 1.529(5) . ? C17 C22 1.385(5) . ? C17 C18 1.396(5) . ? C18 C19 1.387(5) . ? C19 C20 1.392(5) . ? C20 C21 1.390(5) . ? C21 C22 1.396(5) . ? C21 C23 1.518(5) . ? C23 C25 1.526(5) . ? C23 C24 1.532(5) . ? C25 C30 1.392(5) . ? C25 C26 1.402(5) . ? C26 C27 1.385(5) . ? C27 C28 1.376(5) . ? C28 C29 1.389(5) . ? C29 C30 1.389(5) . ? C29 C31 1.520(5) . ? C31 C32 1.537(5) . ? C33 C34 1.369(6) . ? C34 C35 1.382(6) . ? C35 C36 1.360(6) . ? C35 C38 1.488(5) . ? C36 C37 1.397(6) . ? C38 C39 1.383(5) . ? C38 C41 1.384(5) . ? C39 C40 1.371(5) . ? C41 C42 1.381(5) . ? C43 C44 1.377(5) . ? C44 C45 1.384(6) . ? C45 C46 1.372(6) . ? C45 C48 1.489(5) . ? C46 C47 1.387(6) . ? C48 C49 1.368(5) . ? C48 C51 1.391(6) . ? C49 C50 1.386(5) . ? C51 C52 1.374(6) . ? C53 C58 1.385(6) . ? C53 C54 1.396(6) . ? C53 C59 1.511(6) . ? C54 C55 1.396(6) . ? C55 C56 1.389(6) . ? C55 C60 1.501(7) . ? C56 C57 1.373(6) . ? C57 C58 1.383(6) . ? C61 C66 1.32(2) . ? C61 C67 1.33(2) . ? C61 C62 1.57(2) . ? C62 C63 1.42(3) . ? C63 C64 1.24(2) . ? C63 C68 1.43(3) . ? C64 C65 1.59(2) . ? C65 C66 1.27(2) . ? C65 C69 1.28(2) . ? 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 C37 N1 C33 116.2(4) . . ? C40 N2 C42 115.7(4) . . ? C43 N3 C47 116.2(4) . . ? C52 N4 C50 115.3(4) . . ? O1 C1 C2 120.6(3) . . ? O1 C1 C6 118.6(3) . . ? C2 C1 C6 120.8(3) . . ? C3 C2 C1 120.6(3) . . ? C2 C3 O2 120.5(3) . . ? C2 C3 C4 121.3(3) . . ? O2 C3 C4 118.1(3) . . ? C3 C4 C5 115.6(3) . . ? C3 C4 C31 121.1(3) . . ? C5 C4 C31 123.3(3) . . ? C6 C5 C4 125.2(3) . . ? C5 C6 C1 116.4(3) . . ? C5 C6 C7 123.0(3) . . ? C1 C6 C7 120.6(3) . . ? C6 C7 C9 113.2(3) . . ? C6 C7 C8 112.6(3) . . ? C9 C7 C8 110.8(3) . . ? C14 C9 C10 116.6(3) . . ? C14 C9 C7 123.6(3) . . ? C10 C9 C7 119.7(3) . . ? O3 C10 C11 121.6(3) . . ? O3 C10 C9 117.4(3) . . ? C11 C10 C9 121.0(4) . . ? C10 C11 C12 119.9(4) . . ? O4 C12 C13 117.9(3) . . ? O4 C12 C11 120.9(4) . . ? C13 C12 C11 121.3(4) . . ? C12 C13 C14 117.3(4) . . ? C12 C13 C15 120.0(3) . . ? C14 C13 C15 122.7(3) . . ? C13 C14 C9 123.9(4) . . ? C17 C15 C16 113.6(3) . . ? C17 C15 C13 112.5(3) . . ? C16 C15 C13 109.5(3) . . ? C22 C17 C18 116.7(3) . . ? C22 C17 C15 123.5(3) . . ? C18 C17 C15 119.8(3) . . ? O5 C18 C19 120.7(3) . . ? O5 C18 C17 118.7(3) . . ? C19 C18 C17 120.6(3) . . ? C18 C19 C20 120.5(3) . . ? O6 C20 C21 118.6(3) . . ? O6 C20 C19 120.3(3) . . ? C21 C20 C19 121.0(3) . . ? C20 C21 C22 116.2(3) . . ? C20 C21 C23 120.6(3) . . ? C22 C21 C23 123.2(3) . . ? C17 C22 C21 124.9(3) . . ? C21 C23 C25 112.4(3) . . ? C21 C23 C24 113.7(3) . . ? C25 C23 C24 108.8(3) . . ? C30 C25 C26 117.5(3) . . ? C30 C25 C23 122.7(3) . . ? C26 C25 C23 119.7(3) . . ? O7 C26 C27 121.9(3) . . ? O7 C26 C25 117.9(3) . . ? C27 C26 C25 120.2(3) . . ? C28 C27 C26 120.3(4) . . ? C27 C28 O8 121.0(3) . . ? C27 C28 C29 121.8(4) . . ? O8 C28 C29 117.1(3) . . ? C30 C29 C28 116.7(3) . . ? C30 C29 C31 122.4(3) . . ? C28 C29 C31 120.9(3) . . ? C29 C30 C25 123.5(4) . . ? C4 C31 C29 113.7(3) . . ? C4 C31 C32 112.2(3) . . ? C29 C31 C32 109.7(3) . . ? N1 C33 C34 123.5(4) . . ? C33 C34 C35 121.3(5) . . ? C36 C35 C34 114.8(4) . . ? C36 C35 C38 123.8(4) . . ? C34 C35 C38 121.4(4) . . ? C35 C36 C37 121.1(4) . . ? N1 C37 C36 123.1(5) . . ? C39 C38 C41 115.7(4) . . ? C39 C38 C35 121.1(4) . . ? C41 C38 C35 123.3(4) . . ? C40 C39 C38 120.1(4) . . ? N2 C40 C39 124.5(4) . . ? C42 C41 C38 120.1(4) . . ? N2 C42 C41 123.9(4) . . ? N3 C43 C44 124.4(4) . . ? C43 C44 C45 119.6(4) . . ? C46 C45 C44 116.1(4) . . ? C46 C45 C48 121.6(4) . . ? C44 C45 C48 122.3(4) . . ? C45 C46 C47 120.3(4) . . ? N3 C47 C46 123.3(4) . . ? C49 C48 C51 116.0(4) . . ? C49 C48 C45 122.3(4) . . ? C51 C48 C45 121.6(4) . . ? C48 C49 C50 119.8(4) . . ? N4 C50 C49 124.5(4) . . ? C52 C51 C48 119.7(4) . . ? N4 C52 C51 124.7(4) . . ? C58 C53 C54 119.0(4) . . ? C58 C53 C59 120.1(5) . . ? C54 C53 C59 120.9(4) . . ? C53 C54 C55 121.6(4) . . ? C56 C55 C54 117.9(5) . . ? C56 C55 C60 122.6(5) . . ? C54 C55 C60 119.5(5) . . ? C57 C56 C55 120.7(4) . . ? C56 C57 C58 121.2(5) . . ? C57 C58 C53 119.5(5) . . ? C66 C61 C67 125.2(19) . . ? C66 C61 C62 118.2(12) . . ? C67 C61 C62 115.8(18) . . ? C63 C62 C61 114.8(15) . . ? C64 C63 C62 115.8(27) . . ? C64 C63 C68 130.4(29) . . ? C62 C63 C68 113.7(15) . . ? C63 C64 C65 133.5(20) . . ? C66 C65 C69 124.4(22) . . ? C66 C65 C64 105.2(16) . . ? C69 C65 C64 130.4(15) . . ? C65 C66 C61 132.5(18) . . ? _refine_diff_density_max 0.320 _refine_diff_density_min -0.304 _refine_diff_density_rms 0.047