# Supplementary Material (ESI) for Perkin Transactions # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 188/285 data_000410b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C65 H86 N2 O7' _chemical_formula_weight 1007.36 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.401(17) _cell_length_b 13.436(10) _cell_length_c 22.040(18) _cell_angle_alpha 90.00 _cell_angle_beta 95.396(16) _cell_angle_gamma 90.00 _cell_volume 6309(9) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2458 _cell_measurement_theta_min 2.166 _cell_measurement_theta_max 19.145 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.061 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2184 _exptl_absorpt_coefficient_mu 0.068 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.724544 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 5.67 _diffrn_reflns_number 21932 _diffrn_reflns_av_R_equivalents 0.1342 _diffrn_reflns_av_sigmaI/netI 0.2145 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 25.03 _reflns_number_total 10972 _reflns_number_gt 3020 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1083P)^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 not refinement _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0062(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 10972 _refine_ls_number_parameters 668 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.2765 _refine_ls_R_factor_gt 0.0834 _refine_ls_wR_factor_ref 0.2755 _refine_ls_wR_factor_gt 0.1870 _refine_ls_goodness_of_fit_ref 0.895 _refine_ls_restrained_S_all 0.895 _refine_ls_shift/su_max 0.172 _refine_ls_shift/su_mean 0.011 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 N1 N 0.3426(3) 0.8063(4) 0.4097(2) 0.0806(15) Uani 1 1 d . . . N2 N 0.5334(2) 0.8592(4) 0.0657(2) 0.0773(15) Uani 1 1 d . . . O1 O 0.25216(16) 0.8969(2) 0.31365(16) 0.0609(10) Uani 1 1 d . . . O2 O 0.39410(15) 0.9559(2) 0.11706(15) 0.0572(10) Uani 1 1 d . . . O3 O 0.28426(16) 0.8239(2) 0.18426(16) 0.0614(10) Uani 1 1 d . . . O4 O 0.33891(18) 1.0569(3) 0.24816(17) 0.0673(11) Uani 1 1 d . . . O5 O 0.4968(2) 0.6930(5) 0.4460(2) 0.147(2) Uani 1 1 d . . . H5B H 0.5315 0.7136 0.4594 0.221 Uiso 1 1 calc R . . O6 O 0.6733(3) 0.7065(5) 0.0653(3) 0.187(3) Uani 1 1 d . . . H6A H 0.6706 0.6463 0.0596 0.281 Uiso 1 1 calc R . . O7 O 0.6442(4) 0.5021(5) 0.0347(3) 0.188(3) Uani 1 1 d . . . C1 C 0.2378(2) 1.1121(4) 0.3190(2) 0.0614(15) Uani 1 1 d . . . H1A H 0.2190 1.1522 0.3490 0.074 Uiso 1 1 calc R . . H1B H 0.2715 1.0734 0.3399 0.074 Uiso 1 1 calc R . . C2 C 0.2646(3) 1.1805(4) 0.2719(2) 0.0594(15) Uani 1 1 d . . . C3 C 0.2367(3) 1.2742(4) 0.2610(3) 0.0643(16) Uani 1 1 d . . . H3A H 0.2057 1.2954 0.2849 0.077 Uiso 1 1 calc R . . C4 C 0.2547(3) 1.3349(4) 0.2155(3) 0.0677(16) Uani 1 1 d . . . C5 C 0.3001(3) 1.2989(4) 0.1794(3) 0.0676(17) Uani 1 1 d . . . H5A H 0.3121 1.3387 0.1480 0.081 Uiso 1 1 calc R . . C6 C 0.3285(3) 1.2044(4) 0.1887(3) 0.0583(15) Uani 1 1 d . . . C7 C 0.3678(3) 1.1619(4) 0.1418(2) 0.0659(16) Uani 1 1 d . . . H7A H 0.4016 1.1220 0.1616 0.079 Uiso 1 1 calc R . . H7B H 0.3861 1.2153 0.1197 0.079 Uiso 1 1 calc R . . C8 C 0.3259(2) 1.0974(4) 0.0977(2) 0.0536(14) Uani 1 1 d . . . C9 C 0.2720(3) 1.1383(4) 0.0670(2) 0.0622(15) Uani 1 1 d . . . H9A H 0.2641 1.2059 0.0715 0.075 Uiso 1 1 calc R . . C10 C 0.2301(2) 1.0818(4) 0.0302(3) 0.0608(15) Uani 1 1 d . . . C11 C 0.2415(2) 0.9821(4) 0.0284(2) 0.0595(15) Uani 1 1 d . . . H11A H 0.2121 0.9423 0.0061 0.071 Uiso 1 1 calc R . . C12 C 0.2936(3) 0.9363(4) 0.0573(2) 0.0547(14) Uani 1 1 d . . . C13 C 0.3003(2) 0.8232(4) 0.0581(2) 0.0601(15) Uani 1 1 d . . . H13A H 0.3380 0.8041 0.0833 0.072 Uiso 1 1 calc R . . H13B H 0.3034 0.7986 0.0171 0.072 Uiso 1 1 calc R . . C14 C 0.2430(2) 0.7792(4) 0.0838(3) 0.0547(14) Uani 1 1 d . . . C15 C 0.1940(3) 0.7377(4) 0.0460(3) 0.0631(16) Uani 1 1 d . . . H15A H 0.1992 0.7294 0.0049 0.076 Uiso 1 1 calc R . . C16 C 0.1371(3) 0.7080(4) 0.0676(3) 0.0636(16) Uani 1 1 d . . . C17 C 0.1324(3) 0.7176(4) 0.1281(3) 0.0676(17) Uani 1 1 d . . . H17A H 0.0954 0.6972 0.1433 0.081 Uiso 1 1 calc R . . C18 C 0.1801(3) 0.7567(4) 0.1692(3) 0.0570(15) Uani 1 1 d . . . C19 C 0.1708(3) 0.7736(4) 0.2346(3) 0.0666(16) Uani 1 1 d . . . H19A H 0.2084 0.7534 0.2597 0.080 Uiso 1 1 calc R . . H19B H 0.1364 0.7325 0.2457 0.080 Uiso 1 1 calc R . . C20 C 0.1567(3) 0.8822(4) 0.2478(2) 0.0556(14) Uani 1 1 d . . . C21 C 0.1013(3) 0.9261(5) 0.2217(3) 0.0665(16) Uani 1 1 d . . . H21A H 0.0726 0.8867 0.1983 0.080 Uiso 1 1 calc R . . C22 C 0.0873(3) 1.0260(5) 0.2291(3) 0.0662(16) Uani 1 1 d . . . C23 C 0.1320(3) 1.0828(4) 0.2607(3) 0.0657(16) Uani 1 1 d . . . H23A H 0.1249 1.1507 0.2644 0.079 Uiso 1 1 calc R . . C24 C 0.1887(2) 1.0426(4) 0.2880(2) 0.0552(14) Uani 1 1 d . . . C25 C 0.1985(2) 0.9409(4) 0.2832(2) 0.0535(14) Uani 1 1 d . . . C26 C 0.2360(3) 0.7834(3) 0.1459(3) 0.0543(14) Uani 1 1 d . . . C27 C 0.3379(2) 0.9972(4) 0.0901(2) 0.0530(14) Uani 1 1 d . . . C28 C 0.3110(3) 1.1480(4) 0.2371(3) 0.0581(15) Uani 1 1 d . . . C29 C 0.0236(3) 1.0697(5) 0.2036(4) 0.091(2) Uani 1 1 d . . . C30 C -0.0065(5) 1.0166(10) 0.1511(7) 0.310(11) Uani 1 1 d . . . H30A H -0.0456 1.0482 0.1379 0.466 Uiso 1 1 calc R . . H30B H -0.0141 0.9489 0.1623 0.466 Uiso 1 1 calc R . . H30C H 0.0204 1.0177 0.1187 0.466 Uiso 1 1 calc R . . C31 C -0.0198(5) 1.0601(11) 0.2543(6) 0.270(8) Uani 1 1 d . . . H31A H -0.0601 1.0877 0.2409 0.405 Uiso 1 1 calc R . . H31B H -0.0021 1.0954 0.2897 0.405 Uiso 1 1 calc R . . H31C H -0.0245 0.9911 0.2642 0.405 Uiso 1 1 calc R . . C32 C 0.0288(5) 1.1740(7) 0.1866(7) 0.266(8) Uani 1 1 d . . . H32A H -0.0118 1.1989 0.1717 0.399 Uiso 1 1 calc R . . H32B H 0.0568 1.1800 0.1552 0.399 Uiso 1 1 calc R . . H32C H 0.0448 1.2119 0.2216 0.399 Uiso 1 1 calc R . . C33 C 0.0840(3) 0.6649(6) 0.0240(3) 0.093(2) Uani 1 1 d . . . C34 C 0.1050(4) 0.5712(7) -0.0053(4) 0.182(4) Uani 1 1 d . . . H34A H 0.1160 0.5222 0.0255 0.274 Uiso 1 1 calc R . . H34B H 0.1409 0.5854 -0.0270 0.274 Uiso 1 1 calc R . . H34C H 0.0716 0.5463 -0.0333 0.274 Uiso 1 1 calc R . . C35 C 0.0683(4) 0.7362(8) -0.0285(5) 0.218(6) Uani 1 1 d . . . H35A H 0.0351 0.7087 -0.0558 0.326 Uiso 1 1 calc R . . H35B H 0.1048 0.7462 -0.0500 0.326 Uiso 1 1 calc R . . H35C H 0.0551 0.7988 -0.0130 0.326 Uiso 1 1 calc R . . C36 C 0.0258(4) 0.6365(8) 0.0539(4) 0.177(4) Uani 1 1 d . . . H36A H 0.0367 0.5900 0.0862 0.266 Uiso 1 1 calc R . . H36B H -0.0042 0.6066 0.0242 0.266 Uiso 1 1 calc R . . H36C H 0.0078 0.6950 0.0703 0.266 Uiso 1 1 calc R . . C37 C 0.1717(3) 1.1278(5) -0.0060(3) 0.088(2) Uani 1 1 d . . . C38 C 0.1638(5) 1.2364(7) 0.0062(5) 0.221(6) Uani 1 1 d . . . H38A H 0.1585 1.2461 0.0486 0.332 Uiso 1 1 calc R . . H38B H 0.1276 1.2610 -0.0181 0.332 Uiso 1 1 calc R . . H38C H 0.2004 1.2718 -0.0039 0.332 Uiso 1 1 calc R . . C39 C 0.1796(4) 1.1178(8) -0.0738(4) 0.180(4) Uani 1 1 d . . . H39A H 0.1437 1.1459 -0.0972 0.270 Uiso 1 1 calc R . . H39B H 0.1833 1.0488 -0.0840 0.270 Uiso 1 1 calc R . . H39C H 0.2168 1.1526 -0.0830 0.270 Uiso 1 1 calc R . . C40 C 0.1141(4) 1.0724(8) 0.0039(5) 0.186(5) Uani 1 1 d . . . H40A H 0.1066 1.0765 0.0461 0.279 Uiso 1 1 calc R . . H40B H 0.1190 1.0040 -0.0071 0.279 Uiso 1 1 calc R . . H40C H 0.0792 1.1007 -0.0207 0.279 Uiso 1 1 calc R . . C41 C 0.2221(3) 1.4350(5) 0.2017(3) 0.086(2) Uani 1 1 d . . . C42 C 0.2240(5) 1.4953(5) 0.2588(4) 0.184(5) Uani 1 1 d . . . H42A H 0.2669 1.5075 0.2739 0.276 Uiso 1 1 calc R . . H42B H 0.2033 1.4597 0.2889 0.276 Uiso 1 1 calc R . . H42C H 0.2031 1.5577 0.2502 0.276 Uiso 1 1 calc R . . C43 C 0.1539(4) 1.4168(5) 0.1789(4) 0.152(4) Uani 1 1 d . . . H43A H 0.1518 1.3777 0.1424 0.228 Uiso 1 1 calc R . . H43B H 0.1333 1.4794 0.1705 0.228 Uiso 1 1 calc R . . H43C H 0.1334 1.3818 0.2095 0.228 Uiso 1 1 calc R . . C44 C 0.2501(4) 1.4919(6) 0.1519(4) 0.158(4) Uani 1 1 d . . . H44A H 0.2934 1.5063 0.1643 0.237 Uiso 1 1 calc R . . H44B H 0.2275 1.5530 0.1443 0.237 Uiso 1 1 calc R . . H44C H 0.2473 1.4525 0.1154 0.237 Uiso 1 1 calc R . . C45 C 0.2389(3) 0.8622(4) 0.3728(3) 0.0773(18) Uani 1 1 d . . . H45A H 0.1963 0.8371 0.3715 0.093 Uiso 1 1 calc R . . H45B H 0.2439 0.9157 0.4024 0.093 Uiso 1 1 calc R . . C46 C 0.2853(4) 0.7807(5) 0.3892(3) 0.0774(19) Uani 1 1 d . . . C47 C 0.2687(4) 0.6812(6) 0.3810(3) 0.097(2) Uani 1 1 d . . . H47A H 0.2277 0.6643 0.3669 0.116 Uiso 1 1 calc R . . C48 C 0.3122(5) 0.6085(6) 0.3935(3) 0.107(2) Uani 1 1 d . . . H48A H 0.3011 0.5418 0.3893 0.128 Uiso 1 1 calc R . . C49 C 0.3724(4) 0.6352(6) 0.4124(3) 0.103(2) Uani 1 1 d . . . H49A H 0.4034 0.5867 0.4185 0.124 Uiso 1 1 calc R . . C50 C 0.3878(4) 0.7361(7) 0.4228(3) 0.094(2) Uani 1 1 d . . . C51 C 0.4508(4) 0.7734(6) 0.4472(4) 0.136(3) Uani 1 1 d . . . H51A H 0.4629 0.8288 0.4226 0.163 Uiso 1 1 calc R . . H51B H 0.4492 0.7968 0.4887 0.163 Uiso 1 1 calc R . . C52 C 0.4403(3) 0.9540(4) 0.0744(3) 0.0759(17) Uani 1 1 d . . . H52A H 0.4473 1.0211 0.0602 0.091 Uiso 1 1 calc R . . H52B H 0.4252 0.9140 0.0394 0.091 Uiso 1 1 calc R . . C53 C 0.5013(3) 0.9115(4) 0.1030(3) 0.0673(16) Uani 1 1 d . . . C54 C 0.5214(3) 0.9277(5) 0.1635(3) 0.104(2) Uani 1 1 d . . . H54A H 0.4971 0.9630 0.1890 0.125 Uiso 1 1 calc R . . C55 C 0.5798(4) 0.8886(6) 0.1844(4) 0.116(3) Uani 1 1 d . . . H55A H 0.5956 0.8985 0.2247 0.140 Uiso 1 1 calc R . . C56 C 0.6132(3) 0.8371(6) 0.1470(5) 0.103(3) Uani 1 1 d . . . H56A H 0.6523 0.8117 0.1612 0.124 Uiso 1 1 calc R . . C57 C 0.5902(3) 0.8218(5) 0.0877(4) 0.096(2) Uani 1 1 d . . . C58 C 0.6197(4) 0.7526(7) 0.0389(4) 0.167(5) Uani 1 1 d . . . H58A H 0.5893 0.7027 0.0239 0.201 Uiso 1 1 calc R . . H58B H 0.6300 0.7926 0.0046 0.201 Uiso 1 1 calc R . . C59 C 0.3309(4) 0.7519(5) 0.2069(4) 0.131(3) Uani 1 1 d . . . H59A H 0.3112 0.7028 0.2312 0.157 Uiso 1 1 calc R . . H59B H 0.3463 0.7176 0.1726 0.157 Uiso 1 1 calc R . . C60 C 0.3804(5) 0.7928(10) 0.2414(5) 0.216(5) Uani 1 1 d . . . H60A H 0.3659 0.8224 0.2777 0.260 Uiso 1 1 calc R . . H60B H 0.3987 0.8452 0.2184 0.260 Uiso 1 1 calc R . . C61 C 0.4317(4) 0.7120(9) 0.2603(4) 0.193(5) Uani 1 1 d . . . H61A H 0.4644 0.7411 0.2874 0.290 Uiso 1 1 calc R . . H61B H 0.4491 0.6876 0.2246 0.290 Uiso 1 1 calc R . . H61C H 0.4129 0.6579 0.2805 0.290 Uiso 1 1 calc R . . C62 C 0.3997(5) 1.0637(6) 0.2901(6) 0.195(5) Uani 1 1 d D . . H62A H 0.4273 1.1044 0.2679 0.234 Uiso 1 1 calc R . . H62B H 0.3891 1.1042 0.3241 0.234 Uiso 1 1 calc R . . C63 C 0.4404(9) 0.9841(11) 0.3180(9) 0.53(2) Uani 1 1 d D . . H63A H 0.4610 0.9478 0.2875 0.641 Uiso 1 1 calc R . . H63B H 0.4168 0.9378 0.3407 0.641 Uiso 1 1 calc R . . C64 C 0.4875(5) 1.0426(13) 0.3601(5) 0.261(8) Uani 1 1 d D . . H64A H 0.5010 1.0029 0.3951 0.391 Uiso 1 1 calc R . . H64B H 0.4681 1.1025 0.3731 0.391 Uiso 1 1 calc R . . H64C H 0.5231 1.0595 0.3388 0.391 Uiso 1 1 calc R . . C65 C 0.6512(9) 0.4812(11) -0.0271(5) 0.295(9) Uani 1 1 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 N1 0.086(4) 0.074(4) 0.082(4) 0.028(3) 0.007(3) 0.012(3) N2 0.060(3) 0.087(4) 0.086(4) 0.025(3) 0.015(3) 0.015(3) O1 0.063(2) 0.061(2) 0.060(3) 0.0135(19) 0.010(2) 0.007(2) O2 0.046(2) 0.061(2) 0.065(2) 0.0026(19) 0.006(2) 0.0019(19) O3 0.061(2) 0.053(2) 0.068(3) -0.0029(19) -0.007(2) -0.004(2) O4 0.066(3) 0.052(3) 0.081(3) 0.003(2) -0.002(2) 0.009(2) O5 0.101(4) 0.196(6) 0.146(5) 0.021(4) 0.020(3) 0.051(4) O6 0.189(7) 0.185(6) 0.188(7) 0.007(5) 0.019(5) 0.062(5) O7 0.255(8) 0.144(5) 0.163(6) 0.020(5) 0.010(6) 0.035(5) C1 0.069(4) 0.052(4) 0.063(4) -0.004(3) 0.006(3) 0.001(3) C2 0.055(4) 0.061(4) 0.060(4) -0.001(3) -0.011(3) -0.007(3) C3 0.067(4) 0.051(4) 0.074(4) -0.007(3) 0.002(3) 0.006(3) C4 0.078(4) 0.043(4) 0.080(5) -0.005(3) 0.003(4) 0.000(3) C5 0.084(5) 0.046(4) 0.070(4) 0.010(3) -0.009(4) -0.002(3) C6 0.060(4) 0.051(4) 0.061(4) -0.010(3) -0.009(3) -0.003(3) C7 0.065(4) 0.056(4) 0.076(4) -0.014(3) 0.002(3) -0.004(3) C8 0.049(3) 0.047(4) 0.064(4) 0.001(3) 0.002(3) -0.002(3) C9 0.069(4) 0.044(3) 0.072(4) 0.002(3) 0.000(3) -0.003(3) C10 0.047(3) 0.057(4) 0.077(4) 0.004(3) -0.003(3) 0.006(3) C11 0.049(3) 0.061(4) 0.068(4) -0.006(3) -0.002(3) -0.003(3) C12 0.055(4) 0.048(4) 0.063(4) -0.004(3) 0.014(3) -0.002(3) C13 0.058(4) 0.053(4) 0.070(4) -0.013(3) 0.009(3) -0.003(3) C14 0.059(4) 0.042(3) 0.063(4) -0.006(3) 0.005(3) -0.004(3) C15 0.067(4) 0.062(4) 0.059(4) -0.012(3) -0.003(3) -0.006(3) C16 0.064(4) 0.059(4) 0.067(4) -0.012(3) 0.000(3) -0.017(3) C17 0.062(4) 0.047(4) 0.094(5) 0.002(3) 0.010(4) -0.011(3) C18 0.069(4) 0.037(3) 0.066(4) -0.002(3) 0.014(3) -0.002(3) C19 0.073(4) 0.049(4) 0.078(5) 0.004(3) 0.007(3) -0.012(3) C20 0.065(4) 0.044(4) 0.060(4) 0.002(3) 0.016(3) -0.004(3) C21 0.048(4) 0.077(5) 0.074(4) -0.008(3) 0.003(3) -0.011(3) C22 0.059(4) 0.062(4) 0.077(4) 0.004(3) 0.006(3) 0.013(3) C23 0.064(4) 0.046(4) 0.088(5) -0.009(3) 0.011(3) 0.005(3) C24 0.056(4) 0.051(4) 0.059(4) -0.001(3) 0.011(3) -0.004(3) C25 0.047(3) 0.047(4) 0.066(4) 0.006(3) 0.007(3) 0.004(3) C26 0.056(4) 0.033(3) 0.073(4) -0.005(3) 0.004(3) -0.004(3) C27 0.048(3) 0.047(4) 0.063(4) -0.001(3) 0.004(3) -0.001(3) C28 0.062(4) 0.043(4) 0.067(4) -0.004(3) -0.004(3) 0.007(3) C29 0.048(4) 0.088(5) 0.133(6) -0.005(4) -0.008(4) 0.013(4) C30 0.186(11) 0.285(16) 0.42(2) -0.195(16) -0.189(14) 0.138(11) C31 0.114(8) 0.44(2) 0.268(15) 0.129(15) 0.084(9) 0.150(11) C32 0.158(10) 0.124(9) 0.48(2) 0.113(11) -0.152(12) 0.005(7) C33 0.074(5) 0.096(5) 0.107(6) -0.017(5) 0.002(4) -0.036(4) C34 0.167(9) 0.167(10) 0.207(10) -0.096(8) -0.018(8) -0.061(7) C35 0.175(10) 0.244(12) 0.207(11) 0.117(10) -0.126(8) -0.100(9) C36 0.106(7) 0.282(12) 0.142(8) -0.040(8) 0.002(6) -0.093(8) C37 0.069(5) 0.091(5) 0.102(6) 0.003(4) -0.015(4) 0.012(4) C38 0.189(10) 0.128(8) 0.314(14) -0.082(8) -0.152(9) 0.104(7) C39 0.192(10) 0.246(12) 0.092(7) 0.038(7) -0.041(7) 0.072(9) C40 0.064(6) 0.206(10) 0.281(13) 0.058(9) -0.025(7) 0.011(6) C41 0.092(5) 0.054(4) 0.112(6) 0.001(4) 0.013(4) 0.014(4) C42 0.360(15) 0.069(6) 0.118(7) -0.027(5) -0.009(8) 0.057(7) C43 0.111(7) 0.094(6) 0.238(11) -0.001(6) -0.052(7) 0.034(5) C44 0.202(10) 0.094(6) 0.188(9) 0.052(6) 0.069(8) 0.042(6) C45 0.091(5) 0.079(4) 0.062(4) 0.011(3) 0.007(4) 0.019(4) C46 0.095(6) 0.075(5) 0.062(4) 0.002(4) 0.007(4) -0.011(4) C47 0.125(6) 0.087(6) 0.076(5) 0.001(4) -0.003(4) -0.001(5) C48 0.136(7) 0.078(6) 0.101(6) 0.002(4) -0.015(5) 0.015(6) C49 0.132(8) 0.090(7) 0.086(6) 0.015(4) 0.004(5) 0.034(6) C50 0.105(6) 0.094(6) 0.082(5) 0.026(4) 0.010(4) 0.019(5) C51 0.088(6) 0.139(8) 0.177(9) 0.045(6) -0.005(6) 0.009(6) C52 0.057(4) 0.088(5) 0.083(5) 0.013(4) 0.008(4) 0.008(3) C53 0.058(4) 0.071(4) 0.071(5) 0.005(3) -0.003(4) -0.002(3) C54 0.080(5) 0.138(7) 0.091(6) -0.012(5) -0.008(4) 0.034(5) C55 0.094(6) 0.134(7) 0.115(7) 0.007(5) -0.021(5) 0.009(5) C56 0.065(5) 0.120(7) 0.123(8) 0.050(6) -0.005(5) 0.013(5) C57 0.074(5) 0.102(6) 0.112(7) 0.036(5) 0.015(5) 0.022(4) C58 0.114(7) 0.218(10) 0.177(9) 0.074(8) 0.054(6) 0.130(7) C59 0.138(7) 0.089(6) 0.147(8) 0.017(5) -0.082(6) -0.026(5) C60 0.144(10) 0.289(15) 0.207(12) 0.039(11) -0.030(9) 0.062(10) C61 0.127(8) 0.328(14) 0.125(8) 0.062(8) 0.015(6) 0.122(9) C62 0.224(11) 0.060(6) 0.285(15) -0.007(7) -0.058(11) 0.059(7) C63 0.69(6) 0.48(4) 0.41(4) 0.24(3) -0.05(4) -0.26(4) C64 0.116(8) 0.49(3) 0.169(11) 0.101(13) -0.053(7) -0.081(12) C65 0.51(3) 0.285(16) 0.106(9) 0.050(10) 0.095(13) 0.120(17) _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 N1 C46 1.312(7) . ? N1 C50 1.362(8) . ? N2 C53 1.322(7) . ? N2 C57 1.363(8) . ? O1 C25 1.405(6) . ? O1 C45 1.437(6) . ? O2 C27 1.406(6) . ? O2 C52 1.428(6) . ? O3 C26 1.383(6) . ? O3 C59 1.445(8) . ? O4 C28 1.374(6) . ? O4 C62 1.526(11) . ? O5 C51 1.465(8) . ? O6 C58 1.384(8) . ? O7 C65 1.413(11) . ? C1 C2 1.536(7) . ? C1 C24 1.519(7) . ? C2 C28 1.382(7) . ? C2 C3 1.404(7) . ? C3 C4 1.374(7) . ? C4 C5 1.399(7) . ? C4 C41 1.531(8) . ? C5 C6 1.414(7) . ? C6 C28 1.387(7) . ? C6 C7 1.505(7) . ? C7 C8 1.527(7) . ? C8 C27 1.383(6) . ? C8 C9 1.394(7) . ? C9 C10 1.380(7) . ? C10 C11 1.363(7) . ? C10 C37 1.548(8) . ? C11 C12 1.376(7) . ? C12 C27 1.401(7) . ? C12 C13 1.527(7) . ? C13 C14 1.519(7) . ? C14 C15 1.391(7) . ? C14 C26 1.392(7) . ? C15 C16 1.407(7) . ? C16 C17 1.354(7) . ? C16 C33 1.530(8) . ? C17 C18 1.401(7) . ? C18 C26 1.393(7) . ? C18 C19 1.492(7) . ? C19 C20 1.523(7) . ? C20 C25 1.378(7) . ? C20 C21 1.399(7) . ? C21 C22 1.389(7) . ? C22 C23 1.363(7) . ? C22 C29 1.540(8) . ? C23 C24 1.410(7) . ? C24 C25 1.388(7) . ? C29 C32 1.459(10) . ? C29 C30 1.456(11) . ? C29 C31 1.523(11) . ? C33 C36 1.512(9) . ? C33 C35 1.516(10) . ? C33 C34 1.504(10) . ? C37 C40 1.474(9) . ? C37 C38 1.496(9) . ? C37 C39 1.526(10) . ? C41 C42 1.493(9) . ? C41 C43 1.519(9) . ? C41 C44 1.508(9) . ? C45 C46 1.499(8) . ? C46 C47 1.391(8) . ? C47 C48 1.359(9) . ? C48 C49 1.364(9) . ? C49 C50 1.408(9) . ? C50 C51 1.490(10) . ? C52 C53 1.507(7) . ? C53 C54 1.379(8) . ? C54 C55 1.395(9) . ? C55 C56 1.335(9) . ? C56 C57 1.366(9) . ? C57 C58 1.596(10) . ? C59 C60 1.360(11) . ? C60 C61 1.573(12) . ? C62 C63 1.478(10) . ? C63 C64 1.523(10) . ? 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 C46 N1 C50 120.9(6) . . ? C53 N2 C57 118.2(6) . . ? C25 O1 C45 110.4(4) . . ? C27 O2 C52 110.4(4) . . ? C26 O3 C59 113.6(4) . . ? C28 O4 C62 112.6(4) . . ? C2 C1 C24 110.5(4) . . ? C28 C2 C3 120.3(5) . . ? C28 C2 C1 121.4(5) . . ? C3 C2 C1 118.1(5) . . ? C4 C3 C2 120.9(6) . . ? C3 C4 C5 117.8(5) . . ? C3 C4 C41 120.9(6) . . ? C5 C4 C41 121.2(6) . . ? C4 C5 C6 122.7(5) . . ? C28 C6 C5 117.3(5) . . ? C28 C6 C7 121.9(5) . . ? C5 C6 C7 120.1(6) . . ? C6 C7 C8 108.6(4) . . ? C27 C8 C9 118.6(5) . . ? C27 C8 C7 121.6(5) . . ? C9 C8 C7 119.6(5) . . ? C10 C9 C8 122.1(5) . . ? C11 C10 C9 116.7(5) . . ? C11 C10 C37 121.1(5) . . ? C9 C10 C37 122.2(5) . . ? C10 C11 C12 124.4(5) . . ? C11 C12 C27 117.2(5) . . ? C11 C12 C13 121.4(5) . . ? C27 C12 C13 121.1(5) . . ? C12 C13 C14 108.3(4) . . ? C15 C14 C26 117.4(5) . . ? C15 C14 C13 121.5(5) . . ? C26 C14 C13 121.0(5) . . ? C14 C15 C16 122.6(5) . . ? C17 C16 C15 116.9(5) . . ? C17 C16 C33 122.4(6) . . ? C15 C16 C33 120.8(6) . . ? C16 C17 C18 123.8(5) . . ? C17 C18 C26 117.3(5) . . ? C17 C18 C19 121.8(5) . . ? C26 C18 C19 120.9(5) . . ? C18 C19 C20 112.2(4) . . ? C25 C20 C21 118.1(5) . . ? C25 C20 C19 121.7(5) . . ? C21 C20 C19 120.1(5) . . ? C20 C21 C22 123.0(5) . . ? C23 C22 C21 116.8(5) . . ? C23 C22 C29 121.9(6) . . ? C21 C22 C29 121.2(6) . . ? C22 C23 C24 122.6(5) . . ? C25 C24 C23 118.3(5) . . ? C25 C24 C1 122.5(5) . . ? C23 C24 C1 119.2(5) . . ? C24 C25 C20 120.8(5) . . ? C24 C25 O1 120.0(5) . . ? C20 C25 O1 119.2(5) . . ? O3 C26 C14 118.3(5) . . ? O3 C26 C18 119.6(5) . . ? C14 C26 C18 121.8(5) . . ? C8 C27 C12 120.5(5) . . ? C8 C27 O2 119.6(5) . . ? C12 C27 O2 119.9(5) . . ? C2 C28 C6 121.0(5) . . ? C2 C28 O4 120.3(5) . . ? C6 C28 O4 118.7(5) . . ? C32 C29 C30 107.8(9) . . ? C32 C29 C31 109.7(9) . . ? C30 C29 C31 106.7(9) . . ? C32 C29 C22 111.9(6) . . ? C30 C29 C22 114.4(6) . . ? C31 C29 C22 106.2(6) . . ? C36 C33 C35 111.0(7) . . ? C36 C33 C34 105.6(7) . . ? C35 C33 C34 104.7(8) . . ? C36 C33 C16 114.6(6) . . ? C35 C33 C16 109.8(6) . . ? C34 C33 C16 110.6(6) . . ? C40 C37 C38 110.9(8) . . ? C40 C37 C39 105.8(7) . . ? C38 C37 C39 106.7(7) . . ? C40 C37 C10 111.6(6) . . ? C38 C37 C10 113.3(6) . . ? C39 C37 C10 108.1(6) . . ? C42 C41 C43 108.4(7) . . ? C42 C41 C44 110.9(7) . . ? C43 C41 C44 106.0(7) . . ? C42 C41 C4 109.5(6) . . ? C43 C41 C4 109.3(5) . . ? C44 C41 C4 112.7(6) . . ? O1 C45 C46 105.9(5) . . ? N1 C46 C47 121.0(7) . . ? N1 C46 C45 117.9(6) . . ? C47 C46 C45 121.1(7) . . ? C48 C47 C46 120.1(8) . . ? C47 C48 C49 118.9(8) . . ? C48 C49 C50 120.1(7) . . ? N1 C50 C49 118.8(7) . . ? N1 C50 C51 116.3(8) . . ? C49 C50 C51 124.9(8) . . ? O5 C51 C50 109.5(7) . . ? O2 C52 C53 111.0(5) . . ? N2 C53 C54 123.5(6) . . ? N2 C53 C52 115.0(6) . . ? C54 C53 C52 121.5(6) . . ? C53 C54 C55 116.6(7) . . ? C56 C55 C54 120.5(8) . . ? C55 C56 C57 120.2(7) . . ? N2 C57 C56 120.9(7) . . ? N2 C57 C58 111.7(7) . . ? C56 C57 C58 127.1(8) . . ? O6 C58 C57 109.9(8) . . ? C60 C59 O3 113.5(7) . . ? C59 C60 C61 110.9(11) . . ? C63 C62 O4 130.1(9) . . ? C62 C63 C64 102.1(11) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.321 _refine_diff_density_min -0.214 _refine_diff_density_rms 0.051