# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2071 data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H42 N0 O10' _chemical_formula_weight 682.74 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 monoclinic _symmetry_space_group_name_H-M P21/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 10.509(14) _cell_length_b 16.364(17) _cell_length_c 20.06(2) _cell_angle_alpha 90.00 _cell_angle_beta 94.735(10) _cell_angle_gamma 90.00 _cell_volume 3439(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.319 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1448 _exptl_absorpt_coefficient_mu 0.094 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8977 _diffrn_reflns_av_R_equivalents 0.0374 _diffrn_reflns_av_sigmaI/netI 0.0488 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 25.97 _reflns_number_total 5575 _reflns_number_gt 3338 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _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 w=1/[\s^2^(Fo^2^)+(0.2000P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.009(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5575 _refine_ls_number_parameters 456 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1358 _refine_ls_R_factor_gt 0.0828 _refine_ls_wR_factor_ref 0.2841 _refine_ls_wR_factor_gt 0.2401 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.084 _refine_ls_shift/su_mean 0.006 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C11 C 0.5546(4) 0.4929(2) 0.34065(17) 0.0550(10) Uani 1 d . . . C12 C 0.5515(4) 0.5464(2) 0.39511(19) 0.0648(11) Uani 1 d . . . H12 H 0.4770 0.5516 0.4167 0.078 Uiso 1 calc R . . C13 C 0.6583(5) 0.5916(2) 0.4170(2) 0.0730(12) Uani 1 d . . . H13 H 0.6552 0.6269 0.4532 0.088 Uiso 1 calc R . . C14 C 0.7680(5) 0.5843(2) 0.3856(2) 0.0643(11) Uani 1 d . . . H14 H 0.8390 0.6150 0.4010 0.077 Uiso 1 calc R . . C15 C 0.7771(4) 0.53163(18) 0.33056(16) 0.0507(9) Uani 1 d . . . C16 C 0.6658(4) 0.48688(19) 0.30920(17) 0.0503(9) Uani 1 d . . . C17 C 0.9001(4) 0.52458(19) 0.29834(19) 0.0550(9) Uani 1 d . . . H17A H 0.9508 0.5733 0.3084 0.066 Uiso 1 calc R . . H17B H 0.8818 0.5218 0.2502 0.066 Uiso 1 calc R . . C21 C 0.9773(4) 0.44999(19) 0.32170(18) 0.0507(9) Uani 1 d . . . C22 C 1.0546(4) 0.4518(2) 0.3818(2) 0.0637(11) Uani 1 d . . . H22 H 1.0604 0.4995 0.4071 0.076 Uiso 1 calc R . . C23 C 1.1226(5) 0.3829(3) 0.4042(2) 0.0718(12) Uani 1 d . . . H23 H 1.1750 0.3850 0.4439 0.086 Uiso 1 calc R . . C24 C 1.1126(4) 0.3123(2) 0.3682(2) 0.0643(11) Uani 1 d . . . H24 H 1.1593 0.2668 0.3837 0.077 Uiso 1 calc R . . C25 C 1.0351(3) 0.3061(2) 0.30903(17) 0.0485(8) Uani 1 d . . . C26 C 0.9725(3) 0.37656(19) 0.28593(15) 0.0437(8) Uani 1 d . . . C27 C 1.0172(4) 0.2244(2) 0.27245(18) 0.0545(9) Uani 1 d . . . H27A H 0.9936 0.2346 0.2254 0.065 Uiso 1 calc R . . H27B H 1.0978 0.1951 0.2759 0.065 Uiso 1 calc R . . C31 C 0.9156(4) 0.17124(19) 0.30040(17) 0.0506(9) Uani 1 d . . . C32 C 0.9497(5) 0.1185(2) 0.3539(2) 0.0680(11) Uani 1 d . . . H32 H 1.0342 0.1164 0.3718 0.082 Uiso 1 calc R . . C33 C 0.8590(6) 0.0694(2) 0.3805(2) 0.0758(13) Uani 1 d . . . H33 H 0.8830 0.0336 0.4152 0.091 Uiso 1 calc R . . C34 C 0.7359(5) 0.0738(2) 0.3558(2) 0.0723(13) Uani 1 d . . . H34 H 0.6763 0.0406 0.3744 0.087 Uiso 1 calc R . . C35 C 0.6943(4) 0.1259(2) 0.30346(18) 0.0574(10) Uani 1 d . . . C36 C 0.7885(4) 0.17192(18) 0.27461(16) 0.0493(9) Uani 1 d . . . C37 C 0.5510(4) 0.1396(2) 0.28739(18) 0.0621(10) Uani 1 d . . . H37A H 0.5339 0.1529 0.2404 0.075 Uiso 1 calc R . . H37B H 0.5048 0.0900 0.2963 0.075 Uiso 1 calc R . . C41 C 0.5060(4) 0.2087(2) 0.32973(17) 0.0543(9) Uani 1 d . . . C42 C 0.5029(4) 0.1998(2) 0.39870(19) 0.0614(10) Uani 1 d . . . H42 H 0.5183 0.1486 0.4178 0.074 Uiso 1 calc R . . C43 C 0.4778(4) 0.2644(2) 0.43923(18) 0.0617(10) Uani 1 d . . . H43 H 0.4742 0.2565 0.4849 0.074 Uiso 1 calc R . . C44 C 0.4578(4) 0.3408(2) 0.41188(17) 0.0574(9) Uani 1 d . . . H44 H 0.4447 0.3846 0.4400 0.069 Uiso 1 calc R . . C45 C 0.4566(4) 0.3544(2) 0.34396(16) 0.0519(9) Uani 1 d . . . C46 C 0.4760(4) 0.2863(2) 0.30276(16) 0.0518(9) Uani 1 d . . . C47 C 0.4407(4) 0.4405(2) 0.31664(19) 0.0598(10) Uani 1 d . . . H47A H 0.3633 0.4644 0.3313 0.072 Uiso 1 calc R . . H47B H 0.4327 0.4389 0.2682 0.072 Uiso 1 calc R . . O150 O 0.6611(3) 0.43537(17) 0.25555(14) 0.0682(8) Uani 1 d . . . H150 H 0.7326 0.4309 0.2424 0.082 Uiso 1 calc R . . O250 O 0.8966(2) 0.37561(13) 0.22514(10) 0.0481(6) Uani 1 d . . . C251 C 0.9674(4) 0.3906(2) 0.16904(17) 0.0616(10) Uani 1 d . . . H25A H 1.0199 0.3434 0.1613 0.074 Uiso 1 calc R . . H25B H 1.0237 0.4369 0.1785 0.074 Uiso 1 calc R . . C252 C 0.8826(5) 0.4077(3) 0.10816(19) 0.0663(11) Uani 1 d . . . O253 O 0.7616(4) 0.4004(3) 0.11630(18) 0.1195(15) Uani 1 d . . . O254 O 0.9220(4) 0.4228(3) 0.05554(17) 0.1258(16) Uani 1 d . . . C255 C 0.6707(7) 0.4120(5) 0.0594(3) 0.129(3) Uani 1 d . . . H25C H 0.7123 0.4117 0.0181 0.154 Uiso 1 calc R . . H25D H 0.6054 0.3700 0.0574 0.154 Uiso 1 calc R . . C256 C 0.623(2) 0.4831(11) 0.0705(10) 0.42(2) Uani 1 d . . . H25E H 0.5556 0.4774 0.0997 0.504 Uiso 1 calc R . . H25F H 0.5895 0.5068 0.0289 0.504 Uiso 1 calc R . . H25G H 0.6884 0.5179 0.0911 0.504 Uiso 1 calc R . . O350 O 0.7555(3) 0.22519(13) 0.22184(12) 0.0555(7) Uani 1 d . . . C351 C 0.7025(4) 0.1903(3) 0.16126(19) 0.0677(11) Uani 1 d . . . H35A H 0.6315 0.2238 0.1436 0.081 Uiso 1 calc R . . H35B H 0.6690 0.1366 0.1707 0.081 Uiso 1 calc R . . C352 C 0.7942(5) 0.1821(2) 0.10979(19) 0.0641(11) Uani 1 d . . . O353 O 0.7318(4) 0.1546(3) 0.05237(15) 0.1018(12) Uani 1 d . . . C355 C 0.8031(7) 0.1372(4) -0.0062(3) 0.1087(19) Uani 1 d . . . H35C H 0.8877 0.1176 0.0089 0.130 Uiso 1 calc R . . H35D H 0.7599 0.0942 -0.0325 0.130 Uiso 1 calc R . . O354 O 0.9080(3) 0.1936(2) 0.11601(16) 0.0857(10) Uani 1 d . . . C356 C 0.8137(8) 0.2032(5) -0.0447(4) 0.158(3) Uani 1 d . . . H35E H 0.8636 0.1899 -0.0811 0.190 Uiso 1 calc R . . H35F H 0.8548 0.2463 -0.0185 0.190 Uiso 1 calc R . . H35G H 0.7303 0.2208 -0.0619 0.190 Uiso 1 calc R . . O450 O 0.4681(3) 0.29646(16) 0.23361(11) 0.0592(7) Uani 1 d . . . C451 C 0.3403(4) 0.2854(3) 0.20621(19) 0.0724(12) Uani 1 d . . . H45A H 0.2843 0.3235 0.2265 0.087 Uiso 1 calc R . . H45B H 0.3119 0.2303 0.2150 0.087 Uiso 1 calc R . . C452 C 0.3356(5) 0.3000(3) 0.1322(2) 0.0667(11) Uani 1 d . . . O453 O 0.2144(3) 0.2998(2) 0.10727(14) 0.0824(10) Uani 1 d . . . O454 O 0.4246(4) 0.3033(3) 0.09962(16) 0.1122(14) Uani 1 d . . . C455 C 0.1873(7) 0.3029(5) 0.0358(3) 0.107(2) Uani 1 d . . . H45C H 0.2364 0.2614 0.0148 0.128 Uiso 1 calc R . . H45D H 0.0974 0.2922 0.0243 0.128 Uiso 1 calc R . . C456 C 0.2158(18) 0.3723(9) 0.0151(8) 0.290(11) Uani 1 d . . . H45E H 0.1486 0.4101 0.0225 0.348 Uiso 1 calc R . . H45F H 0.2268 0.3695 -0.0319 0.348 Uiso 1 calc R . . H45G H 0.2939 0.3904 0.0387 0.348 Uiso 1 calc R . . 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 C11 0.059(3) 0.059(2) 0.0477(19) 0.0081(15) 0.0085(17) 0.0188(17) C12 0.065(3) 0.075(2) 0.057(2) 0.0065(18) 0.020(2) 0.026(2) C13 0.096(4) 0.066(2) 0.058(2) -0.0130(18) 0.016(2) 0.015(2) C14 0.076(3) 0.0514(19) 0.066(2) -0.0104(16) 0.008(2) 0.0073(19) C15 0.065(3) 0.0389(16) 0.0490(18) 0.0022(13) 0.0091(17) 0.0074(16) C16 0.054(2) 0.0529(18) 0.0443(17) 0.0031(14) 0.0076(16) 0.0133(16) C17 0.064(3) 0.0417(17) 0.060(2) -0.0019(14) 0.0097(18) -0.0083(16) C21 0.048(2) 0.0516(18) 0.054(2) -0.0061(14) 0.0132(17) -0.0085(15) C22 0.059(3) 0.074(2) 0.058(2) -0.0241(18) 0.003(2) -0.017(2) C23 0.062(3) 0.085(3) 0.065(2) -0.010(2) -0.013(2) -0.001(2) C24 0.054(3) 0.075(2) 0.062(2) -0.0027(18) -0.006(2) 0.0082(19) C25 0.041(2) 0.0596(19) 0.0459(18) -0.0019(14) 0.0055(15) 0.0019(15) C26 0.038(2) 0.0536(18) 0.0400(16) -0.0045(13) 0.0068(14) -0.0053(14) C27 0.051(2) 0.0578(19) 0.056(2) -0.0061(15) 0.0101(17) 0.0101(16) C31 0.058(2) 0.0454(17) 0.0499(19) -0.0056(14) 0.0117(17) 0.0081(15) C32 0.078(3) 0.065(2) 0.060(2) 0.0029(18) 0.009(2) 0.019(2) C33 0.099(4) 0.061(2) 0.070(3) 0.0177(19) 0.026(3) 0.030(2) C34 0.100(4) 0.054(2) 0.067(3) 0.0048(18) 0.036(3) -0.001(2) C35 0.076(3) 0.0485(18) 0.0503(19) -0.0080(15) 0.0193(18) -0.0049(17) C36 0.061(3) 0.0417(17) 0.0468(18) -0.0056(13) 0.0108(17) -0.0022(15) C37 0.069(3) 0.070(2) 0.049(2) -0.0112(16) 0.0174(18) -0.0223(19) C41 0.049(2) 0.072(2) 0.0431(19) -0.0063(15) 0.0150(16) -0.0161(18) C42 0.065(3) 0.070(2) 0.050(2) 0.0092(17) 0.0102(18) -0.0114(19) C43 0.062(3) 0.085(3) 0.0397(18) -0.0033(17) 0.0130(17) 0.001(2) C44 0.053(2) 0.078(2) 0.0425(18) -0.0045(16) 0.0153(16) 0.0075(18) C45 0.041(2) 0.072(2) 0.0436(18) 0.0008(15) 0.0108(15) 0.0031(16) C46 0.042(2) 0.079(2) 0.0341(17) -0.0001(15) 0.0050(15) -0.0072(17) C47 0.046(2) 0.079(2) 0.056(2) 0.0045(17) 0.0108(18) 0.0193(18) O150 0.0542(18) 0.0863(17) 0.0658(17) -0.0253(13) 0.0160(14) -0.0025(14) O250 0.0486(16) 0.0580(13) 0.0385(12) 0.0010(9) 0.0078(11) -0.0014(10) C251 0.068(3) 0.073(2) 0.0455(19) 0.0010(16) 0.0151(18) -0.0038(19) C252 0.067(3) 0.083(3) 0.050(2) 0.0041(18) 0.010(2) -0.014(2) O253 0.081(3) 0.211(4) 0.064(2) 0.039(2) -0.003(2) -0.007(3) O254 0.109(3) 0.214(5) 0.055(2) 0.026(2) 0.012(2) -0.030(3) C255 0.097(5) 0.194(7) 0.092(4) 0.033(4) -0.013(4) 0.004(5) C256 0.56(4) 0.37(2) 0.31(2) -0.076(19) -0.11(3) 0.31(3) O350 0.0605(17) 0.0539(13) 0.0514(14) 0.0030(10) 0.0007(12) -0.0082(11) C351 0.062(3) 0.091(3) 0.050(2) -0.0016(19) 0.0060(19) -0.019(2) C352 0.068(3) 0.075(2) 0.051(2) 0.0075(17) 0.009(2) 0.002(2) O353 0.085(3) 0.171(3) 0.0505(17) -0.0018(19) 0.0107(17) -0.019(2) C355 0.124(5) 0.142(5) 0.063(3) 0.016(3) 0.022(3) 0.006(4) O354 0.050(2) 0.133(3) 0.075(2) -0.0091(18) 0.0138(16) 0.0049(18) C356 0.114(6) 0.212(8) 0.154(7) 0.076(6) 0.048(5) 0.062(6) O450 0.0458(17) 0.0962(18) 0.0363(12) -0.0016(11) 0.0074(11) -0.0097(13) C451 0.051(3) 0.120(3) 0.045(2) -0.002(2) -0.0006(19) -0.010(2) C452 0.059(3) 0.099(3) 0.042(2) -0.0109(19) 0.007(2) -0.006(2) O453 0.056(2) 0.136(3) 0.0538(16) -0.0104(15) -0.0062(15) 0.0152(17) O454 0.074(3) 0.216(4) 0.0469(17) 0.002(2) 0.0113(18) -0.018(3) C455 0.094(5) 0.149(5) 0.073(3) -0.012(4) -0.017(3) 0.026(4) C456 0.30(2) 0.258(15) 0.287(19) -0.113(15) -0.099(17) 0.110(15) _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 C11 C16 1.377(6) . ? C11 C12 1.402(5) . ? C11 C47 1.518(6) . ? C12 C13 1.385(7) . ? C13 C14 1.364(7) . ? C14 C15 1.411(5) . ? C15 C16 1.416(5) . ? C15 C17 1.497(6) . ? C16 O150 1.365(4) . ? C17 C21 1.518(5) . ? C21 C22 1.398(5) . ? C21 C26 1.398(5) . ? C22 C23 1.390(6) . ? C23 C24 1.364(5) . ? C24 C25 1.387(5) . ? C25 C26 1.388(5) . ? C25 C27 1.530(5) . ? C26 O250 1.401(4) . ? C27 C31 1.520(6) . ? C31 C36 1.393(6) . ? C31 C32 1.401(5) . ? C32 C33 1.386(7) . ? C33 C34 1.348(7) . ? C34 C35 1.395(6) . ? C35 C36 1.406(5) . ? C35 C37 1.530(7) . ? C36 O350 1.393(4) . ? C37 C41 1.514(5) . ? C41 C42 1.395(5) . ? C41 C46 1.406(5) . ? C42 C43 1.372(6) . ? C43 C44 1.375(5) . ? C44 C45 1.380(5) . ? C45 C46 1.412(5) . ? C45 C47 1.516(5) . ? C46 O450 1.393(4) . ? O250 C251 1.421(5) . ? C251 C252 1.478(6) . ? C252 O254 1.191(6) . ? C252 O253 1.300(6) . ? O253 C255 1.439(6) . ? C255 C256 1.294(14) . ? O350 C351 1.415(4) . ? C351 C352 1.476(6) . ? C352 O354 1.207(6) . ? C352 O353 1.355(5) . ? O353 C355 1.472(7) . ? C355 C356 1.338(8) . ? O450 C451 1.421(5) . ? C451 C452 1.500(6) . ? C452 O454 1.187(6) . ? C452 O453 1.330(6) . ? O453 C455 1.440(7) . ? C455 C456 1.254(17) . ? 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 C16 C11 C12 118.5(4) . . ? C16 C11 C47 119.4(3) . . ? C12 C11 C47 122.1(4) . . ? C13 C12 C11 120.7(4) . . ? C14 C13 C12 120.0(4) . . ? C13 C14 C15 122.0(4) . . ? C14 C15 C16 116.4(4) . . ? C14 C15 C17 120.1(4) . . ? C16 C15 C17 123.4(3) . . ? O150 C16 C11 115.4(3) . . ? O150 C16 C15 122.3(4) . . ? C11 C16 C15 122.4(3) . . ? C15 C17 C21 112.8(3) . . ? C22 C21 C26 117.1(3) . . ? C22 C21 C17 120.4(3) . . ? C26 C21 C17 122.4(3) . . ? C21 C22 C23 120.5(3) . . ? C24 C23 C22 120.1(3) . . ? C23 C24 C25 122.0(4) . . ? C26 C25 C24 117.0(3) . . ? C26 C25 C27 122.0(3) . . ? C24 C25 C27 120.9(3) . . ? C25 C26 O250 120.1(3) . . ? C25 C26 C21 123.1(3) . . ? O250 C26 C21 116.8(3) . . ? C31 C27 C25 112.6(3) . . ? C36 C31 C32 117.8(4) . . ? C36 C31 C27 122.7(3) . . ? C32 C31 C27 119.5(4) . . ? C33 C32 C31 120.7(4) . . ? C34 C33 C32 119.9(4) . . ? C33 C34 C35 122.7(4) . . ? C34 C35 C36 116.7(4) . . ? C34 C35 C37 119.4(4) . . ? C36 C35 C37 123.3(3) . . ? C31 C36 O350 117.3(3) . . ? C31 C36 C35 122.0(3) . . ? O350 C36 C35 120.6(3) . . ? C41 C37 C35 109.8(3) . . ? C42 C41 C46 117.0(3) . . ? C42 C41 C37 120.8(3) . . ? C46 C41 C37 122.0(3) . . ? C43 C42 C41 121.9(4) . . ? C44 C43 C42 119.6(3) . . ? C43 C44 C45 122.0(4) . . ? C44 C45 C46 117.4(3) . . ? C44 C45 C47 120.0(3) . . ? C46 C45 C47 122.6(3) . . ? O450 C46 C41 118.9(3) . . ? O450 C46 C45 119.3(3) . . ? C41 C46 C45 121.7(3) . . ? C45 C47 C11 110.5(3) . . ? C26 O250 C251 112.9(3) . . ? O250 C251 C252 111.6(4) . . ? O254 C252 O253 123.0(4) . . ? O254 C252 C251 122.8(5) . . ? O253 C252 C251 114.1(4) . . ? C252 O253 C255 118.7(4) . . ? C256 C255 O253 103.0(10) . . ? C36 O350 C351 117.1(3) . . ? O350 C351 C352 113.8(4) . . ? O354 C352 O353 123.0(4) . . ? O354 C352 C351 127.8(4) . . ? O353 C352 C351 109.1(4) . . ? C352 O353 C355 120.1(4) . . ? C356 C355 O353 112.1(6) . . ? C46 O450 C451 110.3(3) . . ? O450 C451 C452 108.4(4) . . ? O454 C452 O453 124.5(4) . . ? O454 C452 C451 126.2(4) . . ? O453 C452 C451 108.9(4) . . ? C452 O453 C455 118.7(5) . . ? C456 C455 O453 109.2(9) . . ? _refine_diff_density_max 0.574 _refine_diff_density_min -0.412 _refine_diff_density_rms 0.063 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands ; #===END data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H41 N O12' _chemical_formula_weight 727.74 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 monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.193(15) _cell_length_b 21.08(2) _cell_length_c 14.730(15) _cell_angle_alpha 90.00 _cell_angle_beta 114.840(10) _cell_angle_gamma 90.00 _cell_volume 3717(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.301 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1536 _exptl_absorpt_coefficient_mu 0.096 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10799 _diffrn_reflns_av_R_equivalents 0.0264 _diffrn_reflns_av_sigmaI/netI 0.0396 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 25.91 _reflns_number_total 6060 _reflns_number_gt 3665 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _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 w=1/[\s^2^(Fo^2^)+(0.1821P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.006(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6060 _refine_ls_number_parameters 483 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1296 _refine_ls_R_factor_gt 0.0818 _refine_ls_wR_factor_ref 0.2843 _refine_ls_wR_factor_gt 0.2473 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.106 _refine_ls_shift/su_max 0.030 _refine_ls_shift/su_mean 0.006 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C11 C 0.9109(3) -0.03797(15) 0.6115(3) 0.0575(9) Uani 1 d . . . C12 C 0.9381(3) -0.08377(17) 0.6852(3) 0.0689(10) Uani 1 d . . . H12 H 0.9347 -0.1265 0.6683 0.083 Uiso 1 calc R . . C13 C 0.9703(3) -0.06628(19) 0.7841(3) 0.0700(11) Uani 1 d . . . C14 C 0.9763(3) -0.00380(18) 0.8108(3) 0.0668(10) Uani 1 d . . . H14 H 0.9966 0.0067 0.8775 0.080 Uiso 1 calc R . . C15 C 0.9528(3) 0.04380(16) 0.7409(2) 0.0596(9) Uani 1 d . . . C16 C 0.9203(3) 0.02639(15) 0.6411(2) 0.0548(8) Uani 1 d . . . C17 C 0.9620(3) 0.11285(17) 0.7724(3) 0.0656(10) Uani 1 d . . . H17A H 1.0021 0.1158 0.8445 0.079 Uiso 1 calc R . . H17B H 1.0042 0.1360 0.7428 0.079 Uiso 1 calc R . . C21 C 0.8478(3) 0.14267(16) 0.7398(3) 0.0598(9) Uani 1 d . . . C22 C 0.7830(4) 0.12890(19) 0.7912(3) 0.0728(11) Uani 1 d . . . H22 H 0.8115 0.1032 0.8478 0.087 Uiso 1 calc R . . C23 C 0.6762(4) 0.1533(2) 0.7584(3) 0.0762(11) Uani 1 d . . . H23 H 0.6334 0.1442 0.7934 0.091 Uiso 1 calc R . . C24 C 0.6326(3) 0.19101(18) 0.6743(3) 0.0688(10) Uani 1 d . . . H24 H 0.5602 0.2065 0.6527 0.083 Uiso 1 calc R . . C25 C 0.6937(3) 0.20608(15) 0.6221(3) 0.0589(9) Uani 1 d . . . C26 C 0.8019(3) 0.18206(15) 0.6561(2) 0.0556(9) Uani 1 d . . . C27 C 0.6428(3) 0.24696(15) 0.5284(3) 0.0660(10) Uani 1 d . . . H27A H 0.6118 0.2851 0.5436 0.079 Uiso 1 calc R . . H27B H 0.7010 0.2596 0.5082 0.079 Uiso 1 calc R . . C31 C 0.5517(3) 0.21214(16) 0.4427(3) 0.0605(9) Uani 1 d . . . C32 C 0.4402(3) 0.22530(17) 0.4167(3) 0.0674(10) Uani 1 d . . . H32 H 0.4210 0.2578 0.4493 0.081 Uiso 1 calc R . . C33 C 0.3575(3) 0.1909(2) 0.3434(3) 0.0746(11) Uani 1 d . . . H33 H 0.2828 0.2009 0.3252 0.089 Uiso 1 calc R . . C34 C 0.3857(3) 0.14196(18) 0.2974(3) 0.0662(10) Uani 1 d . . . H34 H 0.3289 0.1178 0.2503 0.079 Uiso 1 calc R . . C35 C 0.4957(3) 0.12684(16) 0.3182(2) 0.0571(9) Uani 1 d . . . C36 C 0.5783(3) 0.16514(15) 0.3892(2) 0.0537(8) Uani 1 d . . . C37 C 0.5238(3) 0.07015(17) 0.2697(2) 0.0630(9) Uani 1 d . . . H37A H 0.5749 0.0834 0.2415 0.076 Uiso 1 calc R . . H37B H 0.4560 0.0550 0.2154 0.076 Uiso 1 calc R . . C41 C 0.5765(3) 0.01609(16) 0.3431(2) 0.0576(9) Uani 1 d . . . C42 C 0.5140(3) -0.01751(17) 0.3827(3) 0.0667(10) Uani 1 d . . . H42 H 0.4385 -0.0082 0.3610 0.080 Uiso 1 calc R . . C43 C 0.5611(4) -0.06441(18) 0.4535(3) 0.0723(11) Uani 1 d . . . H43 H 0.5172 -0.0879 0.4768 0.087 Uiso 1 calc R . . C44 C 0.6735(3) -0.07593(17) 0.4890(3) 0.0656(10) Uani 1 d . . . H44 H 0.7057 -0.1061 0.5390 0.079 Uiso 1 calc R . . C45 C 0.7402(3) -0.04420(14) 0.4526(2) 0.0543(8) Uani 1 d . . . C46 C 0.6888(3) -0.00082(15) 0.3756(2) 0.0529(8) Uani 1 d . . . C47 C 0.8662(3) -0.05423(16) 0.5029(3) 0.0597(9) Uani 1 d . . . H47A H 0.8832 -0.0982 0.4954 0.072 Uiso 1 calc R . . H47B H 0.9017 -0.0277 0.4708 0.072 Uiso 1 calc R . . N100 N 0.9999(4) -0.1148(2) 0.8613(3) 0.0947(12) Uani 1 d . . . O101 O 1.0232(4) -0.09962(19) 0.9472(3) 0.1282(15) Uani 1 d . . . O102 O 1.0003(5) -0.1699(2) 0.8364(3) 0.1487(19) Uani 1 d . . . C251 C 0.9326(3) 0.24900(17) 0.6310(3) 0.0669(10) Uani 1 d . . . H25A H 0.9772 0.2494 0.7027 0.080 Uiso 1 calc R . . H25B H 0.8855 0.2864 0.6128 0.080 Uiso 1 calc R . . C252 C 1.0063(4) 0.2486(2) 0.5776(3) 0.0808(12) Uani 1 d . . . O253 O 1.0222(4) 0.2038(2) 0.5368(4) 0.1378(17) Uani 1 d . . . O254 O 1.0529(3) 0.30472(16) 0.5819(3) 0.1031(11) Uani 1 d . . . C255 C 1.1333(6) 0.3087(4) 0.5370(5) 0.146(3) Uani 1 d . . . H25C H 1.1946 0.2795 0.5706 0.175 Uiso 1 calc R . . H25D H 1.0971 0.2968 0.4669 0.175 Uiso 1 calc R . . C256 C 1.1749(10) 0.3717(6) 0.5460(8) 0.228(6) Uani 1 d . . . H25E H 1.2410 0.3719 0.5339 0.274 Uiso 1 calc R . . H25F H 1.1927 0.3872 0.6122 0.274 Uiso 1 calc R . . H25G H 1.1192 0.3984 0.4979 0.274 Uiso 1 calc R . . C351 C 0.7358(3) 0.16832(17) 0.3480(3) 0.0680(10) Uani 1 d . . . H35A H 0.6879 0.1504 0.2834 0.082 Uiso 1 calc R . . H35B H 0.8082 0.1479 0.3701 0.082 Uiso 1 calc R . . C352 C 0.7498(4) 0.2370(2) 0.3348(4) 0.0863(13) Uani 1 d . . . O353 O 0.7230(7) 0.2795(2) 0.3653(5) 0.207(3) Uani 1 d . . . O354 O 0.7996(6) 0.2443(2) 0.2768(4) 0.171(2) Uani 1 d . . . C355 C 0.8120(10) 0.3122(4) 0.2499(9) 0.210(5) Uani 1 d . . . H35C H 0.7430 0.3255 0.1952 0.252 Uiso 1 calc R . . H35D H 0.8242 0.3392 0.3069 0.252 Uiso 1 calc R . . C356 C 0.8848(10) 0.3191(5) 0.2268(11) 0.251(7) Uani 1 d . . . H35E H 0.9023 0.3634 0.2286 0.302 Uiso 1 calc R . . H35F H 0.8635 0.3031 0.1602 0.302 Uiso 1 calc R . . H35G H 0.9493 0.2964 0.2723 0.302 Uiso 1 calc R . . C451 C 0.7888(3) -0.00758(19) 0.2738(3) 0.0666(10) Uani 1 d . . . H45A H 0.8153 -0.0476 0.3082 0.080 Uiso 1 calc R . . H45B H 0.8522 0.0137 0.2702 0.080 Uiso 1 calc R . . C452 C 0.7055(4) -0.0214(2) 0.1699(3) 0.0845(13) Uani 1 d . . . O453 O 0.7530(3) -0.04413(18) 0.1172(2) 0.1031(11) Uani 1 d . . . O454 O 0.6045(3) -0.0166(3) 0.1404(3) 0.154(2) Uani 1 d . . . C455 C 0.6853(5) -0.0605(4) 0.0137(4) 0.127(2) Uani 1 d . . . H45C H 0.6534 -0.1025 0.0084 0.153 Uiso 1 calc R . . H45D H 0.6254 -0.0301 -0.0172 0.153 Uiso 1 calc R . . C456 C 0.7618(8) -0.0586(7) -0.0323(6) 0.273(8) Uani 1 d . . . H45E H 0.7754 -0.0152 -0.0439 0.327 Uiso 1 calc R . . H45F H 0.7303 -0.0809 -0.0949 0.327 Uiso 1 calc R . . H45G H 0.8309 -0.0782 0.0110 0.327 Uiso 1 calc R . . O150 O 0.8987(2) 0.06814(10) 0.56639(16) 0.0649(7) Uani 1 d . . . H150 H 0.8985 0.1042 0.5872 0.078 Uiso 1 calc R . . O250 O 0.8664(2) 0.19364(10) 0.60274(17) 0.0615(7) Uani 1 d . . . O350 O 0.69041(18) 0.15340(10) 0.41623(16) 0.0570(6) Uani 1 d . . . O450 O 0.74968(19) 0.03005(10) 0.33178(17) 0.0597(7) Uani 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 C11 0.060(2) 0.0498(19) 0.059(2) 0.0030(14) 0.0213(17) 0.0010(14) C12 0.071(2) 0.0481(19) 0.079(3) 0.0071(17) 0.023(2) 0.0033(16) C13 0.071(2) 0.069(2) 0.057(2) 0.0129(16) 0.0147(19) 0.0000(17) C14 0.071(2) 0.074(2) 0.0484(19) 0.0039(16) 0.0176(18) 0.0070(17) C15 0.057(2) 0.059(2) 0.0507(19) -0.0010(15) 0.0110(16) 0.0053(15) C16 0.0493(19) 0.0539(19) 0.0498(18) 0.0029(13) 0.0096(15) 0.0044(13) C17 0.065(2) 0.064(2) 0.054(2) -0.0059(15) 0.0118(18) 0.0011(16) C21 0.067(2) 0.0536(19) 0.0496(19) -0.0089(14) 0.0148(17) -0.0024(15) C22 0.088(3) 0.072(2) 0.054(2) 0.0011(17) 0.027(2) 0.006(2) C23 0.085(3) 0.088(3) 0.065(2) 0.004(2) 0.040(2) 0.004(2) C24 0.070(2) 0.066(2) 0.070(2) -0.0020(18) 0.029(2) 0.0032(17) C25 0.070(2) 0.0483(18) 0.0545(19) -0.0055(14) 0.0222(18) -0.0002(15) C26 0.064(2) 0.0484(18) 0.0468(18) -0.0121(13) 0.0159(17) -0.0061(14) C27 0.079(2) 0.0438(18) 0.068(2) -0.0024(15) 0.024(2) 0.0075(16) C31 0.071(2) 0.0491(18) 0.058(2) 0.0139(15) 0.0240(18) 0.0088(15) C32 0.077(3) 0.060(2) 0.062(2) 0.0141(17) 0.027(2) 0.0143(18) C33 0.067(2) 0.077(3) 0.077(3) 0.028(2) 0.027(2) 0.0171(19) C34 0.062(2) 0.067(2) 0.059(2) 0.0117(16) 0.0147(18) 0.0019(17) C35 0.059(2) 0.0579(19) 0.0483(18) 0.0069(14) 0.0163(16) -0.0008(15) C36 0.059(2) 0.0481(18) 0.0480(17) 0.0124(13) 0.0169(16) 0.0044(14) C37 0.063(2) 0.067(2) 0.0453(18) -0.0041(14) 0.0085(17) -0.0067(16) C41 0.060(2) 0.0511(18) 0.0525(19) -0.0107(14) 0.0147(17) -0.0074(15) C42 0.062(2) 0.058(2) 0.078(2) -0.0078(17) 0.0271(19) -0.0102(16) C43 0.085(3) 0.058(2) 0.085(3) -0.0010(18) 0.046(2) -0.0133(19) C44 0.074(2) 0.0515(19) 0.069(2) 0.0019(16) 0.028(2) -0.0042(16) C45 0.066(2) 0.0428(16) 0.0515(18) -0.0081(13) 0.0216(16) -0.0056(14) C46 0.059(2) 0.0456(17) 0.0526(19) -0.0093(13) 0.0224(16) -0.0123(14) C47 0.065(2) 0.0497(18) 0.059(2) -0.0050(14) 0.0209(17) 0.0050(15) N100 0.108(3) 0.082(3) 0.080(3) 0.025(2) 0.026(2) -0.008(2) O101 0.174(4) 0.119(3) 0.069(2) 0.0310(19) 0.028(2) 0.009(2) O102 0.231(5) 0.075(2) 0.119(3) 0.038(2) 0.052(3) -0.001(3) C251 0.073(2) 0.056(2) 0.068(2) -0.0141(16) 0.0258(19) -0.0143(16) C252 0.082(3) 0.069(3) 0.094(3) -0.020(2) 0.040(2) -0.019(2) O253 0.152(4) 0.105(3) 0.209(5) -0.065(3) 0.128(4) -0.043(2) O254 0.126(3) 0.092(2) 0.107(2) -0.0156(18) 0.065(2) -0.0436(19) C255 0.154(6) 0.178(7) 0.136(5) -0.031(5) 0.090(5) -0.074(5) C256 0.274(13) 0.249(12) 0.228(10) -0.047(9) 0.170(10) -0.138(10) C351 0.068(2) 0.059(2) 0.078(2) 0.0033(17) 0.031(2) -0.0050(17) C352 0.112(3) 0.067(3) 0.091(3) 0.001(2) 0.054(3) -0.017(2) O353 0.409(10) 0.061(2) 0.283(7) 0.019(3) 0.276(8) 0.006(4) O354 0.266(6) 0.111(3) 0.211(5) -0.013(3) 0.174(5) -0.071(4) C355 0.282(12) 0.121(6) 0.317(13) 0.028(7) 0.214(12) -0.055(7) C356 0.234(11) 0.176(9) 0.409(18) 0.149(11) 0.198(12) 0.008(8) C451 0.069(2) 0.073(2) 0.055(2) -0.0081(17) 0.0225(19) -0.0041(17) C452 0.080(3) 0.095(3) 0.060(2) -0.015(2) 0.011(2) 0.006(2) O453 0.107(2) 0.129(3) 0.0641(18) -0.0357(17) 0.0268(18) 0.007(2) O454 0.092(3) 0.243(6) 0.093(3) -0.071(3) 0.006(2) 0.022(3) C455 0.110(4) 0.185(6) 0.067(3) -0.055(3) 0.016(3) 0.002(4) C456 0.138(7) 0.55(3) 0.079(5) -0.094(8) -0.005(5) 0.058(10) O150 0.0916(18) 0.0444(12) 0.0530(13) 0.0009(10) 0.0249(13) 0.0047(12) O250 0.0715(15) 0.0508(13) 0.0586(14) -0.0114(10) 0.0238(12) -0.0128(11) O350 0.0563(14) 0.0533(13) 0.0551(13) 0.0056(10) 0.0174(11) 0.0008(10) O450 0.0672(15) 0.0572(13) 0.0559(13) -0.0069(10) 0.0271(12) -0.0097(11) _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 C11 C12 1.383(5) . ? C11 C16 1.415(5) . ? C11 C47 1.493(5) . ? C12 C13 1.385(6) . ? C13 C14 1.368(6) . ? C13 N100 1.457(5) . ? C14 C15 1.377(5) . ? C15 C16 1.396(5) . ? C15 C17 1.516(5) . ? C16 O150 1.343(4) . ? C17 C21 1.513(5) . ? C21 C22 1.390(6) . ? C21 C26 1.396(5) . ? C22 C23 1.382(6) . ? C23 C24 1.378(6) . ? C24 C25 1.366(5) . ? C25 C26 1.394(5) . ? C25 C27 1.522(5) . ? C26 O250 1.401(4) . ? C27 C31 1.518(5) . ? C31 C32 1.383(6) . ? C31 C36 1.399(5) . ? C32 C33 1.376(6) . ? C33 C34 1.369(6) . ? C34 C35 1.389(5) . ? C35 C36 1.406(5) . ? C35 C37 1.515(5) . ? C36 O350 1.383(4) . ? C37 C41 1.523(5) . ? C41 C42 1.387(5) . ? C41 C46 1.398(5) . ? C42 C43 1.381(5) . ? C43 C44 1.370(6) . ? C44 C45 1.380(5) . ? C45 C46 1.391(5) . ? C45 C47 1.524(5) . ? C46 O450 1.386(4) . ? N100 O101 1.213(5) . ? N100 O102 1.218(6) . ? C251 O250 1.412(4) . ? C251 C252 1.485(6) . ? C252 O253 1.184(5) . ? C252 O254 1.323(5) . ? O254 C255 1.470(7) . ? C255 C256 1.422(12) . ? C351 O350 1.405(5) . ? C351 C352 1.482(6) . ? C352 O353 1.124(6) . ? C352 O354 1.288(6) . ? O354 C355 1.511(9) . ? C355 C356 1.156(10) . ? C451 O450 1.413(4) . ? C451 C452 1.490(6) . ? C452 O454 1.220(6) . ? C452 O453 1.278(5) . ? O453 C455 1.449(5) . ? C455 C456 1.433(11) . ? 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 C12 C11 C16 117.8(3) . . ? C12 C11 C47 122.4(3) . . ? C16 C11 C47 119.7(3) . . ? C11 C12 C13 120.3(3) . . ? C14 C13 C12 121.0(3) . . ? C14 C13 N100 119.2(4) . . ? C12 C13 N100 119.9(4) . . ? C13 C14 C15 121.2(3) . . ? C14 C15 C16 118.0(3) . . ? C14 C15 C17 120.5(3) . . ? C16 C15 C17 121.6(3) . . ? O150 C16 C15 123.8(3) . . ? O150 C16 C11 114.5(3) . . ? C15 C16 C11 121.7(3) . . ? C21 C17 C15 111.1(3) . . ? C22 C21 C26 117.9(3) . . ? C22 C21 C17 119.9(3) . . ? C26 C21 C17 122.1(4) . . ? C23 C22 C21 120.1(4) . . ? C24 C23 C22 120.5(4) . . ? C25 C24 C23 121.2(4) . . ? C24 C25 C26 118.1(3) . . ? C24 C25 C27 120.1(3) . . ? C26 C25 C27 121.8(3) . . ? C25 C26 C21 122.1(3) . . ? C25 C26 O250 120.4(3) . . ? C21 C26 O250 117.3(3) . . ? C31 C27 C25 112.0(3) . . ? C32 C31 C36 118.4(3) . . ? C32 C31 C27 120.8(3) . . ? C36 C31 C27 120.8(3) . . ? C33 C32 C31 120.8(4) . . ? C34 C33 C32 119.7(4) . . ? C33 C34 C35 122.7(4) . . ? C34 C35 C36 116.3(3) . . ? C34 C35 C37 121.1(3) . . ? C36 C35 C37 122.5(3) . . ? O350 C36 C31 117.1(3) . . ? O350 C36 C35 120.8(3) . . ? C31 C36 C35 121.8(3) . . ? C35 C37 C41 112.6(3) . . ? C42 C41 C46 117.2(3) . . ? C42 C41 C37 120.4(3) . . ? C46 C41 C37 122.4(3) . . ? C43 C42 C41 121.6(4) . . ? C44 C43 C42 119.1(4) . . ? C43 C44 C45 122.0(3) . . ? C44 C45 C46 117.5(3) . . ? C44 C45 C47 119.1(3) . . ? C46 C45 C47 123.1(3) . . ? O450 C46 C45 120.5(3) . . ? O450 C46 C41 117.3(3) . . ? C45 C46 C41 122.0(3) . . ? C11 C47 C45 110.4(3) . . ? O101 N100 O102 122.3(4) . . ? O101 N100 C13 119.8(4) . . ? O102 N100 C13 117.9(4) . . ? O250 C251 C252 107.5(3) . . ? O253 C252 O254 124.0(5) . . ? O253 C252 C251 124.7(4) . . ? O254 C252 C251 111.3(4) . . ? C252 O254 C255 115.9(5) . . ? C256 C255 O254 109.5(7) . . ? O350 C351 C352 115.3(4) . . ? O353 C352 O354 120.2(5) . . ? O353 C352 C351 130.5(5) . . ? O354 C352 C351 109.3(5) . . ? C352 O354 C355 115.4(6) . . ? C356 C355 O354 113.0(10) . . ? O450 C451 C452 115.6(4) . . ? O454 C452 O453 123.8(4) . . ? O454 C452 C451 125.0(5) . . ? O453 C452 C451 111.0(4) . . ? C452 O453 C455 119.1(4) . . ? C456 C455 O453 104.2(5) . . ? C26 O250 C251 115.2(3) . . ? C36 O350 C351 118.7(3) . . ? C46 O450 C451 116.7(3) . . ? _refine_diff_density_max 0.433 _refine_diff_density_min -0.379 _refine_diff_density_rms 0.054 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands ; #===END data_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H47 N O14' _chemical_formula_weight 813.83 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 monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.868(17) _cell_length_b 14.587(18) _cell_length_c 20.29(2) _cell_angle_alpha 90.00 _cell_angle_beta 110.322(10) _cell_angle_gamma 90.00 _cell_volume 4126(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.310 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1720 _exptl_absorpt_coefficient_mu 0.098 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13134 _diffrn_reflns_av_R_equivalents 0.0673 _diffrn_reflns_av_sigmaI/netI 0.1000 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 26.12 _reflns_number_total 7723 _reflns_number_gt 2736 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _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 w=1/[\s^2^(Fo^2^)+(0.1523P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0033(11) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7723 _refine_ls_number_parameters 537 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2285 _refine_ls_R_factor_gt 0.0843 _refine_ls_wR_factor_ref 0.2906 _refine_ls_wR_factor_gt 0.2219 _refine_ls_goodness_of_fit_ref 0.925 _refine_ls_restrained_S_all 0.925 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C11 C -0.1684(3) 0.1934(4) 0.1803(2) 0.0681(13) Uani 1 d . . . C12 C -0.2452(3) 0.2365(3) 0.1905(2) 0.0727(14) Uani 1 d . . . H12 H -0.2849 0.2749 0.1559 0.087 Uiso 1 calc R . . C13 C -0.2626(3) 0.2225(3) 0.2520(2) 0.0687(13) Uani 1 d . . . C14 C -0.2034(3) 0.1673(3) 0.3055(2) 0.0676(13) Uani 1 d . . . H14 H -0.2161 0.1603 0.3470 0.081 Uiso 1 calc R . . C15 C -0.1266(3) 0.1233(3) 0.2972(3) 0.0700(13) Uani 1 d . . . C16 C -0.1112(3) 0.1362(4) 0.2330(3) 0.0693(13) Uani 1 d . . . C17 C -0.0596(4) 0.0686(4) 0.3572(3) 0.0835(15) Uani 1 d . . . H17A H -0.0042 0.0499 0.3457 0.100 Uiso 1 calc R . . H17B H -0.0920 0.0138 0.3642 0.100 Uiso 1 calc R . . C21 C -0.0267(4) 0.1245(4) 0.4244(3) 0.0756(14) Uani 1 d . . . C22 C -0.0530(4) 0.1019(4) 0.4823(3) 0.0929(17) Uani 1 d . . . H22 H -0.0881 0.0488 0.4813 0.111 Uiso 1 calc R . . C23 C -0.0272(4) 0.1582(5) 0.5412(3) 0.0961(18) Uani 1 d . . . H23 H -0.0410 0.1407 0.5808 0.115 Uiso 1 calc R . . C24 C 0.0184(4) 0.2392(5) 0.5406(3) 0.0888(17) Uani 1 d . . . H24 H 0.0312 0.2783 0.5790 0.107 Uiso 1 calc R . . C25 C 0.0465(3) 0.2655(4) 0.4847(2) 0.0708(13) Uani 1 d . . . C26 C 0.0255(3) 0.2044(4) 0.4281(2) 0.0688(13) Uani 1 d . . . C27 C 0.0811(4) 0.3620(4) 0.4814(2) 0.0773(14) Uani 1 d . . . H27A H 0.1441 0.3602 0.4772 0.093 Uiso 1 calc R . . H27B H 0.0867 0.3939 0.5246 0.093 Uiso 1 calc R . . C31 C 0.0126(4) 0.4138(3) 0.4195(3) 0.0701(13) Uani 1 d . . . C32 C -0.0838(4) 0.4200(4) 0.4137(3) 0.0803(15) Uani 1 d . . . H32 H -0.1037 0.3973 0.4492 0.096 Uiso 1 calc R . . C33 C -0.1496(4) 0.4604(4) 0.3543(3) 0.0912(17) Uani 1 d . . . H33 H -0.2127 0.4687 0.3518 0.109 Uiso 1 calc R . . C34 C -0.1227(4) 0.4880(4) 0.2996(3) 0.0872(16) Uani 1 d . . . H34 H -0.1689 0.5103 0.2589 0.105 Uiso 1 calc R . . C35 C -0.0274(4) 0.4832(3) 0.3037(2) 0.0726(13) Uani 1 d . . . C36 C 0.0402(4) 0.4488(3) 0.3660(2) 0.0687(13) Uani 1 d . . . C37 C 0.0002(4) 0.5075(4) 0.2402(2) 0.0804(15) Uani 1 d . . . H37A H -0.0035 0.5734 0.2333 0.096 Uiso 1 calc R . . H37B H 0.0658 0.4886 0.2487 0.096 Uiso 1 calc R . . C41 C -0.0663(4) 0.4603(4) 0.1744(3) 0.0755(14) Uani 1 d . . . C42 C -0.1382(4) 0.5095(5) 0.1249(3) 0.0951(18) Uani 1 d . . . H42 H -0.1410 0.5728 0.1298 0.114 Uiso 1 calc R . . C43 C -0.2056(5) 0.4669(6) 0.0688(3) 0.108(2) Uani 1 d . . . H43 H -0.2513 0.5011 0.0346 0.130 Uiso 1 calc R . . C44 C -0.2043(4) 0.3722(6) 0.0640(3) 0.0993(19) Uani 1 d . . . H44 H -0.2515 0.3428 0.0273 0.119 Uiso 1 calc R . . C45 C -0.1341(4) 0.3202(4) 0.1128(2) 0.0748(14) Uani 1 d . . . C46 C -0.0615(4) 0.3677(4) 0.1646(2) 0.0705(13) Uani 1 d . . . C47 C -0.1429(4) 0.2168(4) 0.1161(2) 0.0835(16) Uani 1 d . . . H47A H -0.1924 0.1947 0.0739 0.100 Uiso 1 calc R . . H47B H -0.0827 0.1880 0.1194 0.100 Uiso 1 calc R . . O150 O -0.0312(2) 0.0958(3) 0.22488(19) 0.0875(11) Uani 1 d . . . C151 C -0.0488(4) 0.0138(4) 0.1837(3) 0.0902(16) Uani 1 d . . . H15A H -0.1091 0.0189 0.1447 0.108 Uiso 1 calc R . . H15B H -0.0531 -0.0382 0.2123 0.108 Uiso 1 calc R . . C152 C 0.0303(5) 0.0000(5) 0.1571(3) 0.0943(17) Uani 1 d . . . O154 O 0.0948(4) 0.0516(4) 0.1633(3) 0.1381(19) Uani 1 d . . . O153 O 0.0199(3) -0.0784(3) 0.1230(3) 0.1238(16) Uani 1 d . . . C155 C 0.0943(6) -0.1024(7) 0.0914(6) 0.178(4) Uani 1 d . . . H15C H 0.1176 -0.0464 0.0770 0.214 Uiso 1 calc R . . H15D H 0.1481 -0.1317 0.1268 0.214 Uiso 1 calc R . . C156 C 0.0617(9) -0.1566(12) 0.0373(6) 0.271(8) Uani 1 d . . . H15E H 0.0342 -0.2102 0.0503 0.326 Uiso 1 calc R . . H15F H 0.1133 -0.1746 0.0219 0.326 Uiso 1 calc R . . H15G H 0.0135 -0.1252 -0.0001 0.326 Uiso 1 calc R . . O250 O 0.0474(2) 0.2267(2) 0.36897(15) 0.0718(9) Uani 1 d . . . C251 C 0.1450(4) 0.2354(4) 0.3763(3) 0.0792(15) Uani 1 d . . . H25A H 0.1795 0.2642 0.4211 0.095 Uiso 1 calc R . . H25B H 0.1503 0.2748 0.3394 0.095 Uiso 1 calc R . . C252 C 0.1908(5) 0.1432(5) 0.3727(3) 0.0926(18) Uani 1 d . . . O254 O 0.1640(3) 0.0696(3) 0.3793(2) 0.1159(15) Uani 1 d . . . O253 O 0.2719(4) 0.1609(4) 0.3613(4) 0.168(3) Uani 1 d . . . C255 C 0.3273(10) 0.0844(8) 0.3531(9) 0.229(7) Uani 1 d . . . H25C H 0.2843 0.0344 0.3315 0.275 Uiso 1 calc R . . H25D H 0.3606 0.1016 0.3214 0.275 Uiso 1 calc R . . C256 C 0.3934(13) 0.0544(11) 0.4152(8) 0.291(10) Uani 1 d . . . H25E H 0.4357 0.1038 0.4374 0.349 Uiso 1 calc R . . H25F H 0.4299 0.0049 0.4059 0.349 Uiso 1 calc R . . H25G H 0.3607 0.0333 0.4457 0.349 Uiso 1 calc R . . O350 O 0.1372(2) 0.4466(2) 0.37277(17) 0.0779(10) Uani 1 d . . . C351 C 0.1798(4) 0.5338(4) 0.3786(3) 0.0849(16) Uani 1 d . . . H35A H 0.1309 0.5787 0.3554 0.102 Uiso 1 calc R . . H35B H 0.2265 0.5333 0.3551 0.102 Uiso 1 calc R . . C352 C 0.2287(4) 0.5613(5) 0.4547(3) 0.0837(16) Uani 1 d . . . O354 O 0.2557(3) 0.5118(3) 0.5044(2) 0.1169(15) Uani 1 d . . . O353 O 0.2406(3) 0.6511(3) 0.4575(2) 0.1163(15) Uani 1 d . . . C355 C 0.2915(6) 0.6920(6) 0.5252(4) 0.140(3) Uani 1 d . . . H35C H 0.3448 0.6533 0.5518 0.168 Uiso 1 calc R . . H35D H 0.2489 0.6990 0.5518 0.168 Uiso 1 calc R . . C356 C 0.3261(8) 0.7802(7) 0.5128(4) 0.172(4) Uani 1 d . . . H35E H 0.3722 0.7721 0.4899 0.207 Uiso 1 calc R . . H35F H 0.3557 0.8110 0.5568 0.207 Uiso 1 calc R . . H35G H 0.2733 0.8162 0.4834 0.207 Uiso 1 calc R . . N100 N -0.3437(3) 0.2702(4) 0.2616(3) 0.0942(14) Uani 1 d . . . O101 O -0.3852(4) 0.3297(4) 0.2188(3) 0.139(2) Uani 1 d . . . O102 O -0.3660(3) 0.2505(3) 0.3122(2) 0.1244(17) Uani 1 d . . . O450 O 0.0128(2) 0.3182(2) 0.21247(16) 0.0742(9) Uani 1 d . . . C451 C 0.0773(4) 0.2757(4) 0.1836(3) 0.0851(16) Uani 1 d . . . H45A H 0.0483 0.2750 0.1328 0.102 Uiso 1 calc R . . H45B H 0.0876 0.2126 0.1996 0.102 Uiso 1 calc R . . C452 C 0.1719(5) 0.3237(5) 0.2040(3) 0.0927(17) Uani 1 d . . . O454 O 0.1972(3) 0.3871(4) 0.2425(3) 0.1183(15) Uani 1 d . . . O453 O 0.2274(4) 0.2844(5) 0.1756(4) 0.172(3) Uani 1 d . . . C455 C 0.3201(9) 0.3312(11) 0.1860(8) 0.219(7) Uani 1 d . . . H45C H 0.3268 0.3458 0.1412 0.263 Uiso 1 calc R . . H45D H 0.3256 0.3872 0.2129 0.263 Uiso 1 calc R . . C456 C 0.3759(12) 0.2786(12) 0.2163(12) 0.332(14) Uani 1 d . . . H45E H 0.3513 0.2179 0.2028 0.398 Uiso 1 calc R . . H45F H 0.3897 0.2866 0.2658 0.398 Uiso 1 calc R . . H45G H 0.4335 0.2869 0.2058 0.398 Uiso 1 calc R . . 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 C11 0.061(3) 0.079(3) 0.062(3) -0.019(3) 0.019(2) -0.011(3) C12 0.065(3) 0.077(3) 0.065(3) -0.007(3) 0.010(2) -0.004(3) C13 0.073(3) 0.076(3) 0.058(3) -0.001(3) 0.024(2) 0.001(3) C14 0.072(3) 0.068(3) 0.060(3) -0.008(2) 0.019(2) 0.001(3) C15 0.065(3) 0.059(3) 0.080(3) -0.005(3) 0.017(3) -0.005(2) C16 0.061(3) 0.081(3) 0.068(3) -0.019(3) 0.025(2) -0.011(3) C17 0.082(3) 0.064(3) 0.095(4) -0.003(3) 0.019(3) 0.003(3) C21 0.073(3) 0.068(3) 0.078(3) 0.012(3) 0.017(3) 0.005(3) C22 0.081(4) 0.088(4) 0.108(5) 0.038(4) 0.031(3) 0.016(3) C23 0.098(4) 0.113(5) 0.080(4) 0.024(4) 0.034(3) 0.022(4) C24 0.098(4) 0.103(5) 0.062(3) 0.016(3) 0.023(3) 0.020(4) C25 0.069(3) 0.084(4) 0.053(3) 0.004(3) 0.013(2) 0.016(3) C26 0.073(3) 0.068(3) 0.057(3) 0.013(2) 0.013(2) 0.011(3) C27 0.088(3) 0.080(4) 0.056(3) -0.004(3) 0.014(3) 0.006(3) C31 0.079(3) 0.062(3) 0.066(3) -0.016(2) 0.021(3) 0.009(3) C32 0.094(4) 0.081(4) 0.065(3) 0.004(3) 0.027(3) 0.012(3) C33 0.079(4) 0.098(4) 0.103(4) 0.013(4) 0.039(3) 0.020(3) C34 0.085(4) 0.081(4) 0.090(4) 0.004(3) 0.023(3) 0.015(3) C35 0.085(4) 0.058(3) 0.069(3) -0.006(2) 0.020(3) 0.002(3) C36 0.081(3) 0.061(3) 0.061(3) -0.010(2) 0.020(3) 0.011(3) C37 0.102(4) 0.067(3) 0.075(3) 0.000(3) 0.034(3) 0.001(3) C41 0.079(3) 0.077(4) 0.065(3) 0.007(3) 0.018(3) 0.000(3) C42 0.103(4) 0.095(4) 0.079(4) 0.016(3) 0.020(3) 0.013(4) C43 0.103(5) 0.137(7) 0.075(4) 0.030(4) 0.018(4) 0.022(5) C44 0.086(4) 0.142(6) 0.058(3) 0.003(4) 0.009(3) -0.003(4) C45 0.072(3) 0.099(4) 0.054(3) -0.003(3) 0.023(3) -0.007(3) C46 0.078(3) 0.078(4) 0.054(3) 0.006(3) 0.021(3) -0.003(3) C47 0.073(3) 0.113(5) 0.061(3) -0.022(3) 0.020(3) -0.018(3) O150 0.065(2) 0.096(3) 0.101(3) -0.031(2) 0.0279(18) -0.0059(19) C151 0.091(4) 0.074(4) 0.109(4) -0.020(3) 0.040(3) 0.002(3) C152 0.094(4) 0.078(4) 0.120(5) -0.019(4) 0.049(4) 0.004(4) O154 0.122(4) 0.108(4) 0.221(6) -0.038(4) 0.106(4) -0.015(3) O153 0.112(3) 0.111(3) 0.160(4) -0.057(3) 0.062(3) -0.007(3) C155 0.122(6) 0.220(10) 0.226(10) -0.111(9) 0.102(7) -0.002(6) C156 0.262(14) 0.43(2) 0.152(9) -0.078(12) 0.104(9) 0.085(15) O250 0.074(2) 0.077(2) 0.0597(19) -0.0001(17) 0.0169(16) 0.0045(17) C251 0.098(4) 0.075(4) 0.068(3) -0.005(3) 0.033(3) 0.003(3) C252 0.082(4) 0.093(5) 0.102(4) -0.027(4) 0.030(3) 0.004(4) O254 0.105(3) 0.082(3) 0.151(4) -0.008(3) 0.032(3) 0.009(3) O253 0.151(5) 0.111(4) 0.298(8) -0.050(4) 0.150(5) -0.008(3) C255 0.241(14) 0.139(10) 0.39(2) -0.040(12) 0.215(16) 0.015(9) C256 0.39(3) 0.229(17) 0.30(2) 0.012(13) 0.166(18) 0.160(17) O350 0.075(2) 0.070(2) 0.086(2) -0.0067(17) 0.0235(18) 0.0012(18) C351 0.099(4) 0.074(4) 0.078(3) -0.009(3) 0.025(3) -0.023(3) C352 0.074(3) 0.091(5) 0.084(4) -0.006(4) 0.024(3) -0.016(3) O354 0.129(3) 0.120(3) 0.085(3) -0.001(3) 0.016(2) -0.029(3) O353 0.134(4) 0.104(3) 0.089(3) -0.023(2) 0.012(2) -0.028(3) C355 0.163(7) 0.133(7) 0.113(5) -0.052(5) 0.035(5) -0.058(6) C356 0.218(10) 0.146(8) 0.136(7) -0.054(6) 0.040(6) -0.050(7) N100 0.091(3) 0.119(4) 0.073(3) -0.002(3) 0.028(3) 0.021(3) O101 0.142(4) 0.182(5) 0.100(3) 0.038(3) 0.049(3) 0.083(4) O102 0.125(3) 0.172(5) 0.097(3) 0.026(3) 0.065(3) 0.050(3) O450 0.072(2) 0.080(2) 0.0660(19) 0.0009(17) 0.0188(17) 0.0046(18) C451 0.078(3) 0.087(4) 0.090(4) -0.015(3) 0.029(3) -0.002(3) C452 0.090(4) 0.094(5) 0.098(4) -0.020(4) 0.039(4) -0.014(4) O454 0.090(3) 0.122(4) 0.146(4) -0.034(3) 0.046(3) -0.024(3) O453 0.103(3) 0.206(6) 0.243(6) -0.108(5) 0.103(4) -0.058(4) C455 0.152(11) 0.264(19) 0.284(16) -0.083(13) 0.129(12) -0.035(10) C456 0.183(16) 0.232(18) 0.50(3) -0.13(2) 0.019(17) -0.011(13) _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 C11 C12 1.381(7) . ? C11 C16 1.389(7) . ? C11 C47 1.517(7) . ? C12 C13 1.375(7) . ? C13 C14 1.393(7) . ? C13 N100 1.463(7) . ? C14 C15 1.372(6) . ? C15 C16 1.411(7) . ? C15 C17 1.507(7) . ? C16 O150 1.387(6) . ? C17 C21 1.516(7) . ? C21 C26 1.388(7) . ? C21 C22 1.400(8) . ? C22 C23 1.389(8) . ? C23 C24 1.364(8) . ? C24 C25 1.393(7) . ? C25 C26 1.400(7) . ? C25 C27 1.509(7) . ? C26 O250 1.386(6) . ? C27 C31 1.516(7) . ? C31 C36 1.385(7) . ? C31 C32 1.399(7) . ? C32 C33 1.392(7) . ? C33 C34 1.363(7) . ? C34 C35 1.392(7) . ? C35 C36 1.406(7) . ? C35 C37 1.524(7) . ? C36 O350 1.401(6) . ? C37 C41 1.523(7) . ? C41 C46 1.372(7) . ? C41 C42 1.385(7) . ? C42 C43 1.377(8) . ? C43 C44 1.385(9) . ? C44 C45 1.390(8) . ? C45 C46 1.400(7) . ? C45 C47 1.517(8) . ? C46 O450 1.392(6) . ? O150 C151 1.431(6) . ? C151 C152 1.469(8) . ? C152 O154 1.191(7) . ? C152 O153 1.317(7) . ? O153 C155 1.501(8) . ? C155 C156 1.301(12) . ? O250 C251 1.412(6) . ? C251 C252 1.521(8) . ? C252 O254 1.168(7) . ? C252 O253 1.329(8) . ? O253 C255 1.431(11) . ? C255 C256 1.373(17) . ? O350 C351 1.407(6) . ? C351 C352 1.514(7) . ? C352 O354 1.190(6) . ? C352 O353 1.322(7) . ? O353 C355 1.446(7) . ? C355 C356 1.439(11) . ? N100 O102 1.217(6) . ? N100 O101 1.232(6) . ? O450 C451 1.428(6) . ? C451 C452 1.495(8) . ? C452 O454 1.186(7) . ? C452 O453 1.293(7) . ? O453 C455 1.486(13) . ? C455 C456 1.141(19) . ? 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 C12 C11 C16 118.4(5) . . ? C12 C11 C47 119.5(5) . . ? C16 C11 C47 121.9(5) . . ? C13 C12 C11 119.6(5) . . ? C12 C13 C14 121.8(5) . . ? C12 C13 N100 118.4(5) . . ? C14 C13 N100 119.8(5) . . ? C15 C14 C13 120.1(5) . . ? C14 C15 C16 117.4(4) . . ? C14 C15 C17 119.5(5) . . ? C16 C15 C17 122.9(5) . . ? O150 C16 C11 119.0(5) . . ? O150 C16 C15 118.2(5) . . ? C11 C16 C15 122.6(5) . . ? C15 C17 C21 111.0(4) . . ? C26 C21 C22 117.8(5) . . ? C26 C21 C17 119.9(5) . . ? C22 C21 C17 122.1(5) . . ? C23 C22 C21 120.6(6) . . ? C24 C23 C22 119.6(6) . . ? C23 C24 C25 122.4(6) . . ? C24 C25 C26 116.7(5) . . ? C24 C25 C27 119.7(5) . . ? C26 C25 C27 122.7(5) . . ? O250 C26 C21 116.5(4) . . ? O250 C26 C25 120.5(5) . . ? C21 C26 C25 122.6(5) . . ? C25 C27 C31 111.2(4) . . ? C36 C31 C32 118.9(5) . . ? C36 C31 C27 122.5(5) . . ? C32 C31 C27 118.4(5) . . ? C33 C32 C31 119.4(5) . . ? C34 C33 C32 120.9(5) . . ? C33 C34 C35 121.1(5) . . ? C34 C35 C36 117.8(5) . . ? C34 C35 C37 120.4(5) . . ? C36 C35 C37 121.6(5) . . ? C31 C36 O350 119.3(4) . . ? C31 C36 C35 121.5(5) . . ? O350 C36 C35 119.2(5) . . ? C41 C37 C35 110.6(4) . . ? C46 C41 C42 118.1(5) . . ? C46 C41 C37 121.5(5) . . ? C42 C41 C37 120.3(5) . . ? C43 C42 C41 121.5(6) . . ? C42 C43 C44 119.0(6) . . ? C43 C44 C45 121.3(6) . . ? C44 C45 C46 117.2(6) . . ? C44 C45 C47 121.3(5) . . ? C46 C45 C47 121.0(5) . . ? C41 C46 O450 118.6(4) . . ? C41 C46 C45 122.1(5) . . ? O450 C46 C45 119.0(5) . . ? C11 C47 C45 108.2(4) . . ? C16 O150 C151 115.7(4) . . ? O150 C151 C152 108.7(5) . . ? O154 C152 O153 123.2(6) . . ? O154 C152 C151 126.4(6) . . ? O153 C152 C151 110.4(6) . . ? C152 O153 C155 117.2(6) . . ? C156 C155 O153 112.8(8) . . ? C26 O250 C251 118.1(4) . . ? O250 C251 C252 112.1(5) . . ? O254 C252 O253 124.4(6) . . ? O254 C252 C251 129.1(6) . . ? O253 C252 C251 106.5(6) . . ? C252 O253 C255 117.5(7) . . ? C256 C255 O253 113.5(14) . . ? C36 O350 C351 113.9(4) . . ? O350 C351 C352 111.6(4) . . ? O354 C352 O353 124.3(6) . . ? O354 C352 C351 127.2(6) . . ? O353 C352 C351 108.5(5) . . ? C352 O353 C355 117.9(5) . . ? O353 C355 C356 107.7(7) . . ? O102 N100 O101 123.0(5) . . ? O102 N100 C13 118.7(5) . . ? O101 N100 C13 118.3(5) . . ? C46 O450 C451 114.9(4) . . ? O450 C451 C452 112.6(5) . . ? O454 C452 O453 122.3(6) . . ? O454 C452 C451 126.9(6) . . ? O453 C452 C451 110.7(6) . . ? C452 O453 C455 115.9(7) . . ? C456 C455 O453 103.4(18) . . ? _refine_diff_density_max 0.218 _refine_diff_density_min -0.207 _refine_diff_density_rms 0.052 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands ; #===END