# Supplementary Material (ESI) for Organic & Biomolecular Chemistry # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Org.Biomol.Chem. _journal_coden_Cambridge 0177 _publ_contact_author_name 'Maija Nissinen' _publ_contact_author_email MAIJA.NISSINEN@JYU.FI _publ_section_title ; Synthesis and structure of mono-bridged resorcinarene host: Ditopic receptor for ammonium guests ; _publ_author_name 'Maija Nissinen' # Attachment 'supplementary.cif' data_I _database_code_depnum_ccdc_archive 'CCDC 735046' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H66 O13' _chemical_formula_weight 851.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0492 0.0322 '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 10.7736(3) _cell_length_b 14.6309(4) _cell_length_c 16.0249(6) _cell_angle_alpha 68.9590(10) _cell_angle_beta 72.573(2) _cell_angle_gamma 83.647(2) _cell_volume 2249.32(12) _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 colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.256 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 916 _exptl_absorpt_coefficient_mu 0.739 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8368 _exptl_absorpt_correction_T_max 0.9298 _exptl_absorpt_process_details 'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11384 _diffrn_reflns_av_R_equivalents 0.0493 _diffrn_reflns_av_sigmaI/netI 0.0449 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 67.15 _reflns_number_total 7760 _reflns_number_gt 5763 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0940P)^2^+1.5649P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7760 _refine_ls_number_parameters 576 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0845 _refine_ls_R_factor_gt 0.0619 _refine_ls_wR_factor_ref 0.1856 _refine_ls_wR_factor_gt 0.1662 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_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_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8070(2) 0.26308(19) 0.15237(18) 0.0346(6) Uani 1 1 d . . . C2 C 0.8133(2) 0.33981(19) 0.18342(18) 0.0335(5) Uani 1 1 d . . . H2 H 0.8662 0.3944 0.1414 0.040 Uiso 1 1 calc R . . C3 C 0.7467(2) 0.34142(19) 0.27225(18) 0.0324(5) Uani 1 1 d . . . C4 C 0.6689(2) 0.2603(2) 0.33192(18) 0.0372(6) Uani 1 1 d . . . C5 C 0.6632(3) 0.1811(2) 0.30542(19) 0.0425(6) Uani 1 1 d . . . H5 H 0.6115 0.1259 0.3478 0.051 Uiso 1 1 calc R . . C6 C 0.7331(3) 0.1823(2) 0.21688(19) 0.0389(6) Uani 1 1 d . . . C7 C 0.7523(2) 0.42505(19) 0.30591(18) 0.0338(6) Uani 1 1 d . . . H7 H 0.6617 0.4356 0.3415 0.041 Uiso 1 1 calc R . . C8 C 0.8353(2) 0.39959(18) 0.37300(18) 0.0323(5) Uani 1 1 d . . . C9 C 0.9617(2) 0.36403(19) 0.34976(18) 0.0349(6) Uani 1 1 d . . . H9 H 0.9913 0.3494 0.2938 0.042 Uiso 1 1 calc R . . C10 C 1.0468(2) 0.34881(19) 0.40365(18) 0.0347(6) Uani 1 1 d . . . C11 C 1.0001(2) 0.36672(19) 0.48711(18) 0.0360(6) Uani 1 1 d . . . C12 C 0.8731(2) 0.3993(2) 0.51496(18) 0.0375(6) Uani 1 1 d . . . H12 H 0.8415 0.4090 0.5732 0.045 Uiso 1 1 calc R . . C13 C 0.7927(2) 0.41757(19) 0.45691(18) 0.0337(5) Uani 1 1 d . . . C14 C 1.1896(2) 0.3234(2) 0.36799(19) 0.0368(6) Uani 1 1 d . . . H14 H 1.2290 0.3072 0.4207 0.044 Uiso 1 1 calc R . . C15 C 1.2047(2) 0.2332(2) 0.33919(19) 0.0367(6) Uani 1 1 d . . . C16 C 1.2397(2) 0.2375(2) 0.24713(19) 0.0383(6) Uani 1 1 d . . . H16 H 1.2532 0.3001 0.1996 0.046 Uiso 1 1 calc R . . C17 C 1.2561(2) 0.1549(2) 0.22054(19) 0.0389(6) Uani 1 1 d . . . C18 C 1.2309(3) 0.0651(2) 0.2907(2) 0.0479(7) Uani 1 1 d . . . C19 C 1.1977(3) 0.0568(2) 0.3839(2) 0.0508(7) Uani 1 1 d . . . H19 H 1.1834 -0.0059 0.4313 0.061 Uiso 1 1 calc R . . C20 C 1.1855(3) 0.1408(2) 0.4075(2) 0.0433(7) Uani 1 1 d . . . C21 C 1.3071(3) 0.1601(2) 0.1199(2) 0.0427(7) Uani 1 1 d . . . H21 H 1.3672 0.1031 0.1193 0.051 Uiso 1 1 calc R . . C22 C 1.2024(2) 0.1497(2) 0.0780(2) 0.0408(6) Uani 1 1 d . . . C23 C 1.0848(2) 0.2000(2) 0.09025(19) 0.0396(6) Uani 1 1 d . . . H23 H 1.0662 0.2356 0.1319 0.048 Uiso 1 1 calc R . . C24 C 0.9928(2) 0.2010(2) 0.04476(18) 0.0374(6) Uani 1 1 d . . . C25 C 1.0224(3) 0.1481(2) -0.01660(19) 0.0421(6) Uani 1 1 d . . . C26 C 1.1383(3) 0.0953(2) -0.0291(2) 0.0465(7) Uani 1 1 d . . . H26 H 1.1567 0.0590 -0.0701 0.056 Uiso 1 1 calc R . . C27 C 1.2264(3) 0.0959(2) 0.0180(2) 0.0457(7) Uani 1 1 d . . . C28 C 0.8726(2) 0.2660(2) 0.05256(18) 0.0378(6) Uani 1 1 d . . . H28 H 0.8085 0.2397 0.0330 0.045 Uiso 1 1 calc R . . C29 C 0.7986(3) 0.5235(2) 0.22813(19) 0.0399(6) Uani 1 1 d . . . H29A H 0.8108 0.5700 0.2571 0.048 Uiso 1 1 calc R . . H29B H 0.8847 0.5132 0.1878 0.048 Uiso 1 1 calc R . . C30 C 0.7090(3) 0.5701(2) 0.1676(2) 0.0534(8) Uani 1 1 d . . . H30A H 0.6986 0.5259 0.1364 0.080 Uiso 1 1 calc R . . H30B H 0.7463 0.6321 0.1207 0.080 Uiso 1 1 calc R . . H30C H 0.6240 0.5824 0.2063 0.080 Uiso 1 1 calc R . . C31 C 1.2587(2) 0.4150(2) 0.2912(2) 0.0418(6) Uani 1 1 d . . . H31A H 1.2276 0.4282 0.2357 0.050 Uiso 1 1 calc R . . H31B H 1.2329 0.4716 0.3129 0.050 Uiso 1 1 calc R . . C32 C 1.4065(3) 0.4088(3) 0.2620(2) 0.0545(8) Uani 1 1 d . . . H32A H 1.4393 0.4030 0.3145 0.082 Uiso 1 1 calc R . . H32B H 1.4418 0.4681 0.2096 0.082 Uiso 1 1 calc R . . H32C H 1.4335 0.3514 0.2430 0.082 Uiso 1 1 calc R . . C33 C 1.3869(3) 0.2522(3) 0.0541(2) 0.0527(8) Uani 1 1 d . . . H33A H 1.4093 0.2523 -0.0105 0.063 Uiso 1 1 calc R . . H33B H 1.3326 0.3108 0.0569 0.063 Uiso 1 1 calc R . . C34 C 1.5110(3) 0.2597(3) 0.0771(3) 0.0694(10) Uani 1 1 d . . . H34A H 1.4908 0.2528 0.1429 0.104 Uiso 1 1 calc R . . H34B H 1.5514 0.3236 0.0382 0.104 Uiso 1 1 calc R . . H34C H 1.5712 0.2076 0.0651 0.104 Uiso 1 1 calc R . . C35 C 0.9104(3) 0.3686(2) -0.0188(2) 0.0475(7) Uani 1 1 d . . . H35A H 0.9675 0.3987 0.0024 0.057 Uiso 1 1 calc R . . H35B H 0.9620 0.3617 -0.0788 0.057 Uiso 1 1 calc R . . C36 C 0.7985(4) 0.4382(3) -0.0362(2) 0.0615(9) Uani 1 1 d . . . H36A H 0.7478 0.4141 -0.0656 0.092 Uiso 1 1 calc R . . H36B H 0.8328 0.5033 -0.0774 0.092 Uiso 1 1 calc R . . H36C H 0.7426 0.4422 0.0232 0.092 Uiso 1 1 calc R . . C37 C 0.6596(5) 0.0207(3) 0.2523(3) 0.0848(13) Uani 1 1 d . . . H37A H 0.6871 -0.0026 0.3095 0.127 Uiso 1 1 calc R . . H37B H 0.6731 -0.0313 0.2253 0.127 Uiso 1 1 calc R . . H37C H 0.5673 0.0386 0.2667 0.127 Uiso 1 1 calc R . . C38 C 0.6285(3) 0.4831(2) 0.5584(2) 0.0454(7) Uani 1 1 d . . . H38A H 0.6272 0.4248 0.6135 0.068 Uiso 1 1 calc R . . H38B H 0.5409 0.5115 0.5640 0.068 Uiso 1 1 calc R . . H38C H 0.6887 0.5314 0.5538 0.068 Uiso 1 1 calc R . . C39 C 1.1281(5) 0.0473(3) 0.5694(3) 0.0787(11) Uani 1 1 d . . . H39A H 1.0547 0.0170 0.5649 0.118 Uiso 1 1 calc R . . H39B H 1.1059 0.0564 0.6298 0.118 Uiso 1 1 calc R . . H39C H 1.2048 0.0048 0.5633 0.118 Uiso 1 1 calc R . . C40 C 1.3597(3) -0.0276(3) -0.0312(3) 0.0581(8) Uani 1 1 d . . . H40A H 1.2827 -0.0696 -0.0038 0.087 Uiso 1 1 calc R . . H40B H 1.4364 -0.0672 -0.0197 0.087 Uiso 1 1 calc R . . H40C H 1.3723 0.0033 -0.0985 0.087 Uiso 1 1 calc R . . C41 C 0.4957(3) 0.1966(2) 0.4719(2) 0.0500(7) Uani 1 1 d . . . H41A H 0.5319 0.1305 0.4970 0.060 Uiso 1 1 calc R . . H41B H 0.4414 0.1937 0.4329 0.060 Uiso 1 1 calc R . . C42 C 0.4153(3) 0.2293(3) 0.5501(2) 0.0519(7) Uani 1 1 d . . . H42A H 0.3970 0.3003 0.5259 0.062 Uiso 1 1 calc R . . H42B H 0.3313 0.1941 0.5784 0.062 Uiso 1 1 calc R . . C44 C 0.4139(3) 0.2429(3) 0.6927(2) 0.0553(8) Uani 1 1 d . . . H44A H 0.3238 0.2175 0.7176 0.066 Uiso 1 1 calc R . . H44B H 0.4096 0.3154 0.6696 0.066 Uiso 1 1 calc R . . C45 C 0.4806(3) 0.2082(3) 0.7683(2) 0.0585(8) Uani 1 1 d . . . H45A H 0.4216 0.2162 0.8259 0.070 Uiso 1 1 calc R . . H45B H 0.5022 0.1377 0.7816 0.070 Uiso 1 1 calc R . . C47 C 0.6592(3) 0.2308(3) 0.8118(2) 0.0628(9) Uani 1 1 d . . . H47A H 0.6768 0.1596 0.8284 0.075 Uiso 1 1 calc R . . H47B H 0.6024 0.2430 0.8681 0.075 Uiso 1 1 calc R . . C48 C 0.7864(4) 0.2857(3) 0.7789(3) 0.0660(9) Uani 1 1 d . . . H48A H 0.7732 0.3559 0.7453 0.079 Uiso 1 1 calc R . . H48B H 0.8161 0.2806 0.8332 0.079 Uiso 1 1 calc R . . C50 C 1.0106(4) 0.2746(3) 0.7036(3) 0.0688(10) Uani 1 1 d . . . H50A H 1.0711 0.2213 0.6926 0.083 Uiso 1 1 calc R . . H50B H 1.0169 0.2826 0.7610 0.083 Uiso 1 1 calc R . . C51 C 1.0541(3) 0.3663(2) 0.6247(2) 0.0503(7) Uani 1 1 d . . . H51A H 0.9834 0.4156 0.6266 0.060 Uiso 1 1 calc R . . H51B H 1.1301 0.3921 0.6318 0.060 Uiso 1 1 calc R . . O4 O 0.59872(18) 0.26511(15) 0.41753(13) 0.0444(5) Uani 1 1 d . . . O6 O 0.7346(2) 0.10426(15) 0.18725(14) 0.0532(5) Uani 1 1 d . . . O11 O 1.08851(18) 0.35374(16) 0.53719(14) 0.0478(5) Uani 1 1 d . . . O13 O 0.67005(16) 0.45640(15) 0.47699(13) 0.0419(5) Uani 1 1 d . . . O18 O 1.2411(3) -0.01708(17) 0.26562(18) 0.0656(6) Uani 1 1 d D . . H18 H 1.232(4) -0.067(2) 0.3174(19) 0.079 Uiso 1 1 d D . . O20 O 1.1552(2) 0.13852(16) 0.49777(14) 0.0528(5) Uani 1 1 d . . . O25 O 0.93556(19) 0.15112(16) -0.06430(15) 0.0495(5) Uani 1 1 d D . . H25 H 0.969(3) 0.119(2) -0.101(2) 0.059 Uiso 1 1 d D . . O27 O 1.34209(19) 0.04544(18) 0.00944(17) 0.0604(6) Uani 1 1 d . . . O43 O 0.48304(19) 0.20982(16) 0.61858(14) 0.0519(5) Uani 1 1 d . . . O46 O 0.5956(2) 0.26227(17) 0.74074(15) 0.0578(6) Uani 1 1 d . . . O49 O 0.8818(2) 0.24539(19) 0.71898(17) 0.0667(6) Uani 1 1 d . . . O100 O 0.9997(3) 0.04677(19) -0.18974(18) 0.0670(6) Uani 1 1 d D . . H101 H 0.931(3) 0.060(3) -0.211(3) 0.080 Uiso 1 1 d D . . H102 H 1.012(4) -0.0145(15) -0.167(3) 0.080 Uiso 1 1 d D . . O200 O 0.7640(3) 0.1727(2) 0.5829(2) 0.0822(8) Uani 1 1 d D . . H201 H 0.692(3) 0.204(3) 0.588(3) 0.099 Uiso 1 1 d D . . H202 H 0.817(3) 0.200(3) 0.594(3) 0.099 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0290(12) 0.0413(15) 0.0376(14) -0.0159(12) -0.0133(11) 0.0024(10) C2 0.0244(11) 0.0410(14) 0.0355(13) -0.0131(11) -0.0093(10) 0.0006(10) C3 0.0262(11) 0.0370(14) 0.0373(13) -0.0133(11) -0.0134(10) 0.0017(10) C4 0.0321(12) 0.0471(16) 0.0334(13) -0.0146(12) -0.0092(11) -0.0020(11) C5 0.0466(15) 0.0417(16) 0.0385(14) -0.0113(12) -0.0104(12) -0.0098(12) C6 0.0421(14) 0.0405(15) 0.0402(14) -0.0170(12) -0.0148(12) -0.0039(11) C7 0.0281(12) 0.0397(15) 0.0373(13) -0.0180(12) -0.0096(10) 0.0031(10) C8 0.0267(11) 0.0349(14) 0.0377(13) -0.0156(11) -0.0089(10) 0.0010(10) C9 0.0326(12) 0.0416(15) 0.0353(13) -0.0193(12) -0.0095(11) 0.0024(10) C10 0.0301(12) 0.0384(14) 0.0417(14) -0.0211(12) -0.0121(11) 0.0057(10) C11 0.0340(13) 0.0404(15) 0.0398(14) -0.0192(12) -0.0142(11) 0.0043(10) C12 0.0350(13) 0.0459(16) 0.0356(13) -0.0213(12) -0.0080(11) 0.0033(11) C13 0.0278(12) 0.0358(14) 0.0383(14) -0.0164(11) -0.0072(10) 0.0033(10) C14 0.0320(13) 0.0454(16) 0.0420(14) -0.0239(13) -0.0151(11) 0.0073(11) C15 0.0277(12) 0.0454(16) 0.0455(15) -0.0250(13) -0.0140(11) 0.0082(10) C16 0.0297(12) 0.0479(16) 0.0450(15) -0.0243(13) -0.0143(11) 0.0081(11) C17 0.0319(13) 0.0479(17) 0.0461(15) -0.0265(14) -0.0146(12) 0.0087(11) C18 0.0484(16) 0.0477(18) 0.0571(18) -0.0308(15) -0.0159(14) 0.0094(13) C19 0.0570(18) 0.0426(17) 0.0536(18) -0.0171(14) -0.0179(15) 0.0056(13) C20 0.0385(14) 0.0547(18) 0.0439(16) -0.0270(14) -0.0124(12) 0.0084(12) C21 0.0345(13) 0.0549(18) 0.0500(16) -0.0330(14) -0.0129(12) 0.0096(12) C22 0.0326(13) 0.0525(17) 0.0444(15) -0.0262(13) -0.0102(12) 0.0021(11) C23 0.0357(13) 0.0479(16) 0.0418(15) -0.0245(13) -0.0099(12) 0.0020(11) C24 0.0325(13) 0.0462(16) 0.0364(14) -0.0180(12) -0.0090(11) -0.0007(11) C25 0.0387(14) 0.0521(17) 0.0405(15) -0.0199(13) -0.0124(12) -0.0030(12) C26 0.0442(15) 0.0573(19) 0.0485(16) -0.0328(15) -0.0113(13) 0.0032(13) C27 0.0337(13) 0.0592(19) 0.0544(17) -0.0349(15) -0.0097(13) 0.0047(12) C28 0.0320(13) 0.0472(16) 0.0377(14) -0.0180(12) -0.0105(11) -0.0005(11) C29 0.0416(14) 0.0375(15) 0.0426(15) -0.0143(12) -0.0139(12) 0.0002(11) C30 0.0611(19) 0.0483(18) 0.0532(18) -0.0147(15) -0.0252(15) 0.0067(14) C31 0.0361(14) 0.0459(16) 0.0516(16) -0.0264(14) -0.0129(12) 0.0022(11) C32 0.0371(15) 0.069(2) 0.066(2) -0.0372(18) -0.0085(14) -0.0030(14) C33 0.0379(15) 0.079(2) 0.0502(17) -0.0389(17) -0.0042(13) -0.0024(14) C34 0.0409(17) 0.100(3) 0.086(3) -0.058(2) -0.0112(17) -0.0026(17) C35 0.0487(16) 0.0526(18) 0.0387(15) -0.0164(13) -0.0078(13) -0.0007(13) C36 0.072(2) 0.059(2) 0.0509(18) -0.0136(16) -0.0217(17) 0.0062(16) C37 0.141(4) 0.060(2) 0.056(2) -0.0239(19) -0.013(2) -0.040(2) C38 0.0357(14) 0.0595(19) 0.0474(16) -0.0319(15) -0.0088(12) 0.0118(12) C39 0.105(3) 0.080(3) 0.048(2) -0.0188(19) -0.014(2) -0.019(2) C40 0.0536(18) 0.063(2) 0.069(2) -0.0368(18) -0.0191(16) 0.0097(15) C41 0.0463(16) 0.0563(19) 0.0440(16) -0.0146(14) -0.0066(13) -0.0125(13) C42 0.0427(15) 0.063(2) 0.0467(17) -0.0153(15) -0.0096(13) -0.0055(14) C44 0.0479(17) 0.064(2) 0.0526(18) -0.0257(16) -0.0035(14) -0.0063(14) C45 0.0592(19) 0.067(2) 0.0466(17) -0.0225(16) -0.0033(15) -0.0104(16) C47 0.060(2) 0.080(3) 0.0468(18) -0.0197(17) -0.0155(16) 0.0004(17) C48 0.069(2) 0.071(2) 0.072(2) -0.030(2) -0.0357(19) 0.0072(18) C50 0.065(2) 0.072(2) 0.068(2) -0.0146(19) -0.0252(18) -0.0104(18) C51 0.0516(16) 0.0585(19) 0.0483(17) -0.0231(15) -0.0194(14) 0.0014(14) O4 0.0435(10) 0.0521(12) 0.0359(10) -0.0178(9) -0.0007(8) -0.0138(8) O6 0.0718(14) 0.0458(12) 0.0460(11) -0.0208(10) -0.0102(10) -0.0166(10) O11 0.0395(10) 0.0722(14) 0.0477(11) -0.0365(11) -0.0201(9) 0.0132(9) O13 0.0308(9) 0.0594(12) 0.0437(10) -0.0305(9) -0.0104(8) 0.0104(8) O18 0.0931(17) 0.0478(14) 0.0649(15) -0.0313(12) -0.0230(14) 0.0073(12) O20 0.0660(13) 0.0520(13) 0.0405(11) -0.0176(10) -0.0141(10) 0.0034(10) O25 0.0485(11) 0.0650(14) 0.0516(12) -0.0346(11) -0.0224(10) 0.0070(10) O27 0.0412(11) 0.0853(17) 0.0834(16) -0.0641(14) -0.0216(11) 0.0178(10) O43 0.0462(11) 0.0636(14) 0.0440(11) -0.0207(10) -0.0074(9) 0.0008(9) O46 0.0575(13) 0.0650(15) 0.0503(12) -0.0152(11) -0.0163(10) -0.0099(10) O49 0.0609(14) 0.0761(17) 0.0639(15) -0.0256(13) -0.0128(12) -0.0112(12) O100 0.0824(17) 0.0652(16) 0.0590(15) -0.0247(13) -0.0233(13) -0.0021(13) O200 0.0710(17) 0.0537(16) 0.117(2) -0.0245(16) -0.0250(17) 0.0009(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 C1 C6 1.392(4) . ? C1 C2 1.397(4) . ? C1 C28 1.530(4) . ? C2 C3 1.397(3) . ? C3 C4 1.397(4) . ? C3 C7 1.517(3) . ? C4 O4 1.376(3) . ? C4 C5 1.382(4) . ? C5 C6 1.388(4) . ? C6 O6 1.382(3) . ? C7 C8 1.519(3) . ? C7 C29 1.541(4) . ? C8 C9 1.394(3) . ? C8 C13 1.395(3) . ? C9 C10 1.388(3) . ? C10 C11 1.389(4) . ? C10 C14 1.527(3) . ? C11 O11 1.377(3) . ? C11 C12 1.394(4) . ? C12 C13 1.393(4) . ? C13 O13 1.372(3) . ? C14 C15 1.525(4) . ? C14 C31 1.534(4) . ? C15 C16 1.389(4) . ? C15 C20 1.390(4) . ? C16 C17 1.398(4) . ? C17 C18 1.378(4) . ? C17 C21 1.516(4) . ? C18 O18 1.383(4) . ? C18 C19 1.390(4) . ? C19 C20 1.394(4) . ? C20 O20 1.373(3) . ? C21 C22 1.519(4) . ? C21 C33 1.536(4) . ? C22 C23 1.391(4) . ? C22 C27 1.401(4) . ? C23 C24 1.391(4) . ? C24 C25 1.404(4) . ? C24 C28 1.520(4) . ? C25 O25 1.363(3) . ? C25 C26 1.394(4) . ? C26 C27 1.381(4) . ? C27 O27 1.373(3) . ? C28 C35 1.533(4) . ? C29 C30 1.510(4) . ? C31 C32 1.521(4) . ? C33 C34 1.513(4) . ? C35 C36 1.514(4) . ? C37 O6 1.425(4) . ? C38 O13 1.426(3) . ? C39 O20 1.403(4) . ? C40 O27 1.408(4) . ? C41 O4 1.426(3) . ? C41 C42 1.495(4) . ? C42 O43 1.425(4) . ? C44 O43 1.415(4) . ? C44 C45 1.497(5) . ? C45 O46 1.413(4) . ? C47 O46 1.414(4) . ? C47 C48 1.519(5) . ? C48 O49 1.417(4) . ? C50 O49 1.421(4) . ? C50 C51 1.479(5) . ? C51 O11 1.413(3) . ? 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 C6 C1 C2 116.5(2) . . ? C6 C1 C28 120.1(2) . . ? C2 C1 C28 123.4(2) . . ? C1 C2 C3 124.2(2) . . ? C2 C3 C4 116.3(2) . . ? C2 C3 C7 124.4(2) . . ? C4 C3 C7 119.3(2) . . ? O4 C4 C5 122.8(2) . . ? O4 C4 C3 115.7(2) . . ? C5 C4 C3 121.5(2) . . ? C4 C5 C6 120.0(3) . . ? O6 C6 C5 122.7(2) . . ? O6 C6 C1 115.9(2) . . ? C5 C6 C1 121.4(2) . . ? C3 C7 C8 111.9(2) . . ? C3 C7 C29 115.0(2) . . ? C8 C7 C29 108.9(2) . . ? C9 C8 C13 117.0(2) . . ? C9 C8 C7 121.0(2) . . ? C13 C8 C7 121.8(2) . . ? C10 C9 C8 123.8(2) . . ? C9 C10 C11 117.4(2) . . ? C9 C10 C14 121.1(2) . . ? C11 C10 C14 121.2(2) . . ? O11 C11 C10 115.7(2) . . ? O11 C11 C12 123.2(2) . . ? C10 C11 C12 121.1(2) . . ? C13 C12 C11 119.7(2) . . ? O13 C13 C12 122.6(2) . . ? O13 C13 C8 116.3(2) . . ? C12 C13 C8 121.1(2) . . ? C15 C14 C10 111.8(2) . . ? C15 C14 C31 114.4(2) . . ? C10 C14 C31 108.5(2) . . ? C16 C15 C20 117.1(2) . . ? C16 C15 C14 123.5(3) . . ? C20 C15 C14 119.3(2) . . ? C15 C16 C17 123.6(3) . . ? C18 C17 C16 117.1(3) . . ? C18 C17 C21 119.8(2) . . ? C16 C17 C21 122.9(3) . . ? C17 C18 O18 117.9(3) . . ? C17 C18 C19 121.4(3) . . ? O18 C18 C19 120.7(3) . . ? C18 C19 C20 119.6(3) . . ? O20 C20 C15 115.9(2) . . ? O20 C20 C19 123.1(3) . . ? C15 C20 C19 121.0(3) . . ? C17 C21 C22 114.0(2) . . ? C17 C21 C33 114.5(2) . . ? C22 C21 C33 108.4(2) . . ? C23 C22 C27 117.3(2) . . ? C23 C22 C21 121.9(2) . . ? C27 C22 C21 120.6(2) . . ? C22 C23 C24 123.6(2) . . ? C23 C24 C25 117.2(2) . . ? C23 C24 C28 121.2(2) . . ? C25 C24 C28 121.2(2) . . ? O25 C25 C26 121.2(2) . . ? O25 C25 C24 118.0(2) . . ? C26 C25 C24 120.8(2) . . ? C27 C26 C25 120.0(2) . . ? O27 C27 C26 123.2(2) . . ? O27 C27 C22 115.6(2) . . ? C26 C27 C22 121.2(2) . . ? C24 C28 C1 112.9(2) . . ? C24 C28 C35 108.0(2) . . ? C1 C28 C35 114.8(2) . . ? C30 C29 C7 115.5(2) . . ? C32 C31 C14 115.2(2) . . ? C34 C33 C21 113.6(3) . . ? C36 C35 C28 115.9(3) . . ? O4 C41 C42 108.3(3) . . ? O43 C42 C41 109.8(2) . . ? O43 C44 C45 109.8(3) . . ? O46 C45 C44 110.1(3) . . ? O46 C47 C48 110.0(3) . . ? O49 C48 C47 109.6(3) . . ? O49 C50 C51 115.1(3) . . ? O11 C51 C50 113.0(3) . . ? C4 O4 C41 117.7(2) . . ? C6 O6 C37 116.8(2) . . ? C11 O11 C51 122.1(2) . . ? C13 O13 C38 117.4(2) . . ? C20 O20 C39 118.0(3) . . ? C27 O27 C40 118.6(2) . . ? C44 O43 C42 112.4(2) . . ? C45 O46 C47 110.8(3) . . ? C48 O49 C50 113.4(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -2.7(4) . . . . ? C28 C1 C2 C3 175.3(2) . . . . ? C1 C2 C3 C4 -0.5(3) . . . . ? C1 C2 C3 C7 -179.4(2) . . . . ? C2 C3 C4 O4 -176.8(2) . . . . ? C7 C3 C4 O4 2.1(3) . . . . ? C2 C3 C4 C5 2.8(4) . . . . ? C7 C3 C4 C5 -178.2(2) . . . . ? O4 C4 C5 C6 177.8(2) . . . . ? C3 C4 C5 C6 -1.8(4) . . . . ? C4 C5 C6 O6 178.0(2) . . . . ? C4 C5 C6 C1 -1.7(4) . . . . ? C2 C1 C6 O6 -175.9(2) . . . . ? C28 C1 C6 O6 6.0(3) . . . . ? C2 C1 C6 C5 3.8(4) . . . . ? C28 C1 C6 C5 -174.3(2) . . . . ? C2 C3 C7 C8 -105.5(3) . . . . ? C4 C3 C7 C8 75.6(3) . . . . ? C2 C3 C7 C29 19.5(3) . . . . ? C4 C3 C7 C29 -159.4(2) . . . . ? C3 C7 C8 C9 52.1(3) . . . . ? C29 C7 C8 C9 -76.1(3) . . . . ? C3 C7 C8 C13 -132.8(3) . . . . ? C29 C7 C8 C13 98.9(3) . . . . ? C13 C8 C9 C10 -2.0(4) . . . . ? C7 C8 C9 C10 173.3(2) . . . . ? C8 C9 C10 C11 2.6(4) . . . . ? C8 C9 C10 C14 -171.4(2) . . . . ? C9 C10 C11 O11 -178.1(2) . . . . ? C14 C10 C11 O11 -4.1(4) . . . . ? C9 C10 C11 C12 -0.4(4) . . . . ? C14 C10 C11 C12 173.6(2) . . . . ? O11 C11 C12 C13 175.2(3) . . . . ? C10 C11 C12 C13 -2.3(4) . . . . ? C11 C12 C13 O13 -175.2(2) . . . . ? C11 C12 C13 C8 2.9(4) . . . . ? C9 C8 C13 O13 177.4(2) . . . . ? C7 C8 C13 O13 2.2(4) . . . . ? C9 C8 C13 C12 -0.8(4) . . . . ? C7 C8 C13 C12 -176.1(2) . . . . ? C9 C10 C14 C15 -55.3(3) . . . . ? C11 C10 C14 C15 130.9(3) . . . . ? C9 C10 C14 C31 71.7(3) . . . . ? C11 C10 C14 C31 -102.0(3) . . . . ? C10 C14 C15 C16 104.1(3) . . . . ? C31 C14 C15 C16 -19.7(3) . . . . ? C10 C14 C15 C20 -77.3(3) . . . . ? C31 C14 C15 C20 158.9(2) . . . . ? C20 C15 C16 C17 0.1(4) . . . . ? C14 C15 C16 C17 178.7(2) . . . . ? C15 C16 C17 C18 2.5(4) . . . . ? C15 C16 C17 C21 -173.8(2) . . . . ? C16 C17 C18 O18 177.2(2) . . . . ? C21 C17 C18 O18 -6.3(4) . . . . ? C16 C17 C18 C19 -3.5(4) . . . . ? C21 C17 C18 C19 172.9(3) . . . . ? C17 C18 C19 C20 2.0(4) . . . . ? O18 C18 C19 C20 -178.8(3) . . . . ? C16 C15 C20 O20 177.9(2) . . . . ? C14 C15 C20 O20 -0.8(3) . . . . ? C16 C15 C20 C19 -1.7(4) . . . . ? C14 C15 C20 C19 179.6(2) . . . . ? C18 C19 C20 O20 -178.9(3) . . . . ? C18 C19 C20 C15 0.7(4) . . . . ? C18 C17 C21 C22 80.5(3) . . . . ? C16 C17 C21 C22 -103.2(3) . . . . ? C18 C17 C21 C33 -153.9(3) . . . . ? C16 C17 C21 C33 22.4(4) . . . . ? C17 C21 C22 C23 45.4(4) . . . . ? C33 C21 C22 C23 -83.4(3) . . . . ? C17 C21 C22 C27 -140.8(3) . . . . ? C33 C21 C22 C27 90.4(3) . . . . ? C27 C22 C23 C24 -1.5(4) . . . . ? C21 C22 C23 C24 172.6(3) . . . . ? C22 C23 C24 C25 -0.2(4) . . . . ? C22 C23 C24 C28 -173.2(3) . . . . ? C23 C24 C25 O25 -177.7(3) . . . . ? C28 C24 C25 O25 -4.6(4) . . . . ? C23 C24 C25 C26 1.4(4) . . . . ? C28 C24 C25 C26 174.5(3) . . . . ? O25 C25 C26 C27 178.1(3) . . . . ? C24 C25 C26 C27 -1.0(5) . . . . ? C25 C26 C27 O27 179.8(3) . . . . ? C25 C26 C27 C22 -0.7(5) . . . . ? C23 C22 C27 O27 -178.5(3) . . . . ? C21 C22 C27 O27 7.3(4) . . . . ? C23 C22 C27 C26 1.9(5) . . . . ? C21 C22 C27 C26 -172.3(3) . . . . ? C23 C24 C28 C1 -44.7(3) . . . . ? C25 C24 C28 C1 142.5(3) . . . . ? C23 C24 C28 C35 83.3(3) . . . . ? C25 C24 C28 C35 -89.5(3) . . . . ? C6 C1 C28 C24 -75.5(3) . . . . ? C2 C1 C28 C24 106.5(3) . . . . ? C6 C1 C28 C35 160.1(2) . . . . ? C2 C1 C28 C35 -17.9(3) . . . . ? C3 C7 C29 C30 66.1(3) . . . . ? C8 C7 C29 C30 -167.4(2) . . . . ? C15 C14 C31 C32 -66.5(3) . . . . ? C10 C14 C31 C32 167.9(2) . . . . ? C17 C21 C33 C34 63.5(3) . . . . ? C22 C21 C33 C34 -168.0(2) . . . . ? C24 C28 C35 C36 167.6(2) . . . . ? C1 C28 C35 C36 -65.5(3) . . . . ? O4 C41 C42 O43 -74.4(3) . . . . ? O43 C44 C45 O46 73.7(3) . . . . ? O46 C47 C48 O49 -77.8(4) . . . . ? O49 C50 C51 O11 -77.2(4) . . . . ? C5 C4 O4 C41 -14.2(4) . . . . ? C3 C4 O4 C41 165.4(2) . . . . ? C42 C41 O4 C4 -167.3(2) . . . . ? C5 C6 O6 C37 0.2(4) . . . . ? C1 C6 O6 C37 179.9(3) . . . . ? C10 C11 O11 C51 -178.0(3) . . . . ? C12 C11 O11 C51 4.4(4) . . . . ? C50 C51 O11 C11 91.6(3) . . . . ? C12 C13 O13 C38 3.3(4) . . . . ? C8 C13 O13 C38 -174.8(2) . . . . ? C15 C20 O20 C39 176.6(3) . . . . ? C19 C20 O20 C39 -3.8(4) . . . . ? C26 C27 O27 C40 -15.2(5) . . . . ? C22 C27 O27 C40 165.2(3) . . . . ? C45 C44 O43 C42 172.1(3) . . . . ? C41 C42 O43 C44 177.5(3) . . . . ? C44 C45 O46 C47 179.5(3) . . . . ? C48 C47 O46 C45 176.8(3) . . . . ? C47 C48 O49 C50 -165.0(3) . . . . ? C51 C50 O49 C48 -88.5(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O18 H18 O200 0.871(19) 1.79(2) 2.657(4) 172(4) 2_756 O25 H25 O100 0.859(18) 1.99(2) 2.826(3) 165(3) . O100 H101 O49 0.878(18) 2.60(4) 3.073(4) 115(3) 1_554 O100 H101 O18 0.878(18) 2.49(3) 3.304(4) 154(3) 2_755 O200 H201 O43 0.856(19) 2.15(3) 2.934(3) 152(4) . O200 H202 O49 0.824(19) 2.62(3) 3.335(4) 147(4) . _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 67.15 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 0.336 _refine_diff_density_min -0.333 _refine_diff_density_rms 0.053 #===END data_II _database_code_depnum_ccdc_archive 'CCDC 735047' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H70 O13' _chemical_formula_weight 879.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0492 0.0322 '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 10.8389(1) _cell_length_b 14.9945(1) _cell_length_c 16.0372(1) _cell_angle_alpha 74.018(1) _cell_angle_beta 70.853(1) _cell_angle_gamma 86.719(1) _cell_volume 2365.50(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 colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.234 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 948 _exptl_absorpt_coefficient_mu 0.718 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8134 _exptl_absorpt_correction_T_max 0.9317 _exptl_absorpt_process_details 'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12088 _diffrn_reflns_av_R_equivalents 0.0326 _diffrn_reflns_av_sigmaI/netI 0.0331 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 67.00 _reflns_number_total 8224 _reflns_number_gt 6947 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0653P)^2^+0.9829P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8224 _refine_ls_number_parameters 614 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0553 _refine_ls_R_factor_gt 0.0461 _refine_ls_wR_factor_ref 0.1273 _refine_ls_wR_factor_gt 0.1197 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_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_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.75906(15) 0.15036(11) 0.73624(11) 0.0258(3) Uani 1 1 d . . . C2 C 0.68619(15) 0.15449(12) 0.82445(11) 0.0262(3) Uani 1 1 d . . . H2 H 0.6231 0.1060 0.8614 0.031 Uiso 1 1 calc R . . C3 C 0.70014(16) 0.22550(12) 0.86191(11) 0.0267(3) Uani 1 1 d . . . C4 C 0.79214(16) 0.29707(12) 0.80526(11) 0.0286(4) Uani 1 1 d . . . C5 C 0.86628(17) 0.29610(12) 0.71626(12) 0.0307(4) Uani 1 1 d . . . H5 H 0.9282 0.3452 0.6787 0.037 Uiso 1 1 calc R . . C6 C 0.84963(16) 0.22357(12) 0.68261(11) 0.0278(4) Uani 1 1 d . . . C7 C 0.62664(16) 0.22538(12) 0.96083(11) 0.0281(4) Uani 1 1 d . . . H7 H 0.6893 0.2503 0.9835 0.034 Uiso 1 1 calc R . . C8 C 0.50998(16) 0.28811(12) 0.97116(11) 0.0276(4) Uani 1 1 d . . . C9 C 0.42011(16) 0.28744(12) 0.92644(11) 0.0282(4) Uani 1 1 d . . . H9 H 0.4385 0.2526 0.8827 0.034 Uiso 1 1 calc R . . C10 C 0.30412(16) 0.33537(12) 0.94241(11) 0.0284(4) Uani 1 1 d . . . C11 C 0.28090(16) 0.38760(12) 1.00527(11) 0.0292(4) Uani 1 1 d . . . C12 C 0.36956(17) 0.39172(13) 1.04983(11) 0.0320(4) Uani 1 1 d . . . H12 H 0.3536 0.4296 1.0908 0.038 Uiso 1 1 calc R . . C13 C 0.48179(17) 0.34054(12) 1.03468(11) 0.0297(4) Uani 1 1 d . . . C14 C 0.19816(16) 0.32045(12) 0.90446(11) 0.0293(4) Uani 1 1 d . . . H14 H 0.1371 0.3726 0.9106 0.035 Uiso 1 1 calc R . . C15 C 0.24796(16) 0.32328(12) 0.80323(11) 0.0271(4) Uani 1 1 d . . . C16 C 0.26361(15) 0.24324(12) 0.77294(11) 0.0264(3) Uani 1 1 d . . . H16 H 0.2485 0.1848 0.8177 0.032 Uiso 1 1 calc R . . C17 C 0.29998(15) 0.24391(12) 0.68116(11) 0.0254(3) Uani 1 1 d . . . C18 C 0.32299(16) 0.33059(12) 0.61660(11) 0.0275(4) Uani 1 1 d . . . C19 C 0.31066(17) 0.41179(12) 0.64328(12) 0.0305(4) Uani 1 1 d . . . H19 H 0.3274 0.4702 0.5985 0.037 Uiso 1 1 calc R . . C20 C 0.27369(16) 0.40751(12) 0.73606(12) 0.0293(4) Uani 1 1 d . . . C21 C 0.31511(16) 0.15659(12) 0.64824(11) 0.0264(3) Uani 1 1 d . . . H21 H 0.2766 0.1688 0.5976 0.032 Uiso 1 1 calc R . . C22 C 0.45881(16) 0.13674(11) 0.60807(11) 0.0250(3) Uani 1 1 d . . . C23 C 0.54076(16) 0.12254(11) 0.66092(11) 0.0257(3) Uani 1 1 d . . . H23 H 0.5077 0.1328 0.7200 0.031 Uiso 1 1 calc R . . C24 C 0.66840(16) 0.09413(11) 0.63230(11) 0.0254(3) Uani 1 1 d . . . C25 C 0.71541(16) 0.08098(11) 0.54438(11) 0.0267(3) Uani 1 1 d . . . C26 C 0.63880(16) 0.09945(12) 0.48747(11) 0.0282(4) Uani 1 1 d . . . H26 H 0.6740 0.0939 0.4266 0.034 Uiso 1 1 calc R . . C27 C 0.51093(16) 0.12592(11) 0.51951(11) 0.0263(3) Uani 1 1 d . A . C28 C 0.74872(16) 0.07035(11) 0.69713(11) 0.0264(3) Uani 1 1 d . . . H28 H 0.8394 0.0595 0.6598 0.032 Uiso 1 1 calc R . . C29 C 0.57876(18) 0.12883(13) 1.02645(12) 0.0341(4) Uani 1 1 d . . . H29A H 0.5248 0.1367 1.0870 0.041 Uiso 1 1 calc R . . H29B H 0.5215 0.1005 1.0029 0.041 Uiso 1 1 calc R . . C30 C 0.6853(2) 0.06164(15) 1.04025(14) 0.0452(5) Uani 1 1 d . . . H30A H 0.7433 0.0563 0.9805 0.068 Uiso 1 1 calc R . . H30B H 0.6455 0.0005 1.0779 0.068 Uiso 1 1 calc R . . H30C H 0.7359 0.0847 1.0712 0.068 Uiso 1 1 calc R . . C31 C 0.12043(17) 0.23093(14) 0.96751(12) 0.0354(4) Uani 1 1 d . . . H31A H 0.1750 0.1773 0.9571 0.042 Uiso 1 1 calc R . . H31B H 0.1030 0.2311 1.0320 0.042 Uiso 1 1 calc R . . C32 C -0.0087(2) 0.21759(18) 0.95383(15) 0.0495(5) Uani 1 1 d . . . H32A H -0.0657 0.2685 0.9674 0.074 Uiso 1 1 calc R . . H32B H -0.0509 0.1584 0.9951 0.074 Uiso 1 1 calc R . . H32C H 0.0072 0.2173 0.8901 0.074 Uiso 1 1 calc R . . C33 C 0.24378(17) 0.06962(12) 0.72163(12) 0.0308(4) Uani 1 1 d . . . H33A H 0.2676 0.0154 0.6964 0.037 Uiso 1 1 calc R . . H33B H 0.2749 0.0592 0.7750 0.037 Uiso 1 1 calc R . . C34 C 0.09510(18) 0.07465(15) 0.75473(14) 0.0418(5) Uani 1 1 d . . . H34A H 0.0702 0.1278 0.7805 0.063 Uiso 1 1 calc R . . H34B H 0.0570 0.0173 0.8020 0.063 Uiso 1 1 calc R . . H34C H 0.0627 0.0821 0.7030 0.063 Uiso 1 1 calc R . . C35 C 0.69575(17) -0.02182(12) 0.76962(12) 0.0306(4) Uani 1 1 d . . . H35A H 0.6092 -0.0114 0.8113 0.037 Uiso 1 1 calc R . . H35B H 0.6824 -0.0670 0.7382 0.037 Uiso 1 1 calc R . . C36 C 0.7823(2) -0.06470(14) 0.82709(13) 0.0396(4) Uani 1 1 d . . . H36A H 0.8674 -0.0774 0.7869 0.059 Uiso 1 1 calc R . . H36B H 0.7408 -0.1228 0.8713 0.059 Uiso 1 1 calc R . . H36C H 0.7944 -0.0215 0.8601 0.059 Uiso 1 1 calc R . . C37 C 0.9093(2) 0.43375(14) 0.79179(14) 0.0446(5) Uani 1 1 d . . . H37A H 0.9922 0.4023 0.7765 0.067 Uiso 1 1 calc R . . H37B H 0.9130 0.4754 0.8286 0.067 Uiso 1 1 calc R . . H37C H 0.8942 0.4699 0.7352 0.067 Uiso 1 1 calc R . . C38 C 0.1690(2) 0.52736(14) 0.98345(15) 0.0453(5) Uani 1 1 d . . . H38A H 0.2318 0.5596 0.9982 0.068 Uiso 1 1 calc R . . H38B H 0.0825 0.5532 1.0033 0.068 Uiso 1 1 calc R . . H38C H 0.1970 0.5355 0.9171 0.068 Uiso 1 1 calc R . . C39 C 0.3764(2) 0.41409(14) 0.45829(13) 0.0456(5) Uani 1 1 d . . . H39A H 0.2941 0.4468 0.4675 0.068 Uiso 1 1 calc R . . H39B H 0.4041 0.4024 0.3977 0.068 Uiso 1 1 calc R . . H39C H 0.4437 0.4523 0.4621 0.068 Uiso 1 1 calc R . . C40 C 0.88373(19) 0.02656(14) 0.43323(12) 0.0381(4) Uani 1 1 d . . . H40A H 0.8220 -0.0177 0.4317 0.057 Uiso 1 1 calc R . . H40B H 0.9698 -0.0008 0.4250 0.057 Uiso 1 1 calc R . . H40C H 0.8905 0.0836 0.3838 0.057 Uiso 1 1 calc R . . C41 C 1.03529(18) 0.27717(14) 0.54665(12) 0.0363(4) Uani 1 1 d . . . H41A H 1.0904 0.2744 0.5857 0.044 Uiso 1 1 calc R . . H41B H 1.0091 0.3421 0.5280 0.044 Uiso 1 1 calc R . . C42 C 1.11022(18) 0.24579(15) 0.46347(12) 0.0396(4) Uani 1 1 d . . . H42A H 1.2011 0.2715 0.4393 0.047 Uiso 1 1 calc R . . H42B H 1.1131 0.1772 0.4803 0.047 Uiso 1 1 calc R . . C44 C 1.1147(2) 0.24586(17) 0.31652(13) 0.0463(5) Uani 1 1 d . . . H44A H 1.1104 0.1772 0.3327 0.056 Uiso 1 1 calc R . . H44B H 1.2079 0.2667 0.2928 0.056 Uiso 1 1 calc R . . C45 C 1.0522(2) 0.28465(17) 0.24455(14) 0.0521(6) Uani 1 1 d . . . H45A H 1.0404 0.3519 0.2377 0.063 Uiso 1 1 calc R . . H45B H 1.1102 0.2767 0.1851 0.063 Uiso 1 1 calc R . . C47 C 0.8728(2) 0.26711(19) 0.19810(14) 0.0558(6) Uani 1 1 d D . . H47A H 0.9352 0.2569 0.1409 0.067 Uiso 0.804(3) 1 calc PR A 1 H47B H 0.8574 0.3344 0.1868 0.067 Uiso 0.804(3) 1 calc PR A 1 H47C H 0.9035 0.3321 0.1648 0.067 Uiso 0.196(3) 1 calc PR A 2 H47D H 0.9121 0.2295 0.1546 0.067 Uiso 0.196(3) 1 calc PR A 2 C48A C 0.7454(4) 0.2157(3) 0.2202(3) 0.0508(9) Uani 0.804(3) 1 d PD A 1 H48A H 0.7173 0.2318 0.1651 0.061 Uiso 0.804(3) 1 calc PR A 1 H48B H 0.7589 0.1481 0.2362 0.061 Uiso 0.804(3) 1 calc PR A 1 O49A O 0.6466(2) 0.23740(19) 0.29319(12) 0.0496(6) Uani 0.804(3) 1 d PD A 1 C48B C 0.7511(12) 0.2642(10) 0.2129(9) 0.036(3) Uani 0.196(3) 1 d PD A 2 H48C H 0.7359 0.2640 0.1554 0.043 Uiso 0.196(3) 1 calc PR A 2 H48D H 0.7143 0.3216 0.2289 0.043 Uiso 0.196(3) 1 calc PR A 2 O49B O 0.6803(6) 0.1845(5) 0.2854(5) 0.0251(16) Uani 0.196(3) 1 d PD A 2 C50 C 0.5227(2) 0.20676(17) 0.30351(14) 0.0520(6) Uani 1 1 d D . . H50A H 0.5261 0.1928 0.2460 0.062 Uiso 0.804(3) 1 calc PR A 1 H50B H 0.4629 0.2586 0.3108 0.062 Uiso 0.804(3) 1 calc PR A 1 H50C H 0.5001 0.2653 0.3214 0.062 Uiso 0.196(3) 1 calc PR A 2 H50D H 0.4966 0.2090 0.2493 0.062 Uiso 0.196(3) 1 calc PR A 2 C51 C 0.46411(18) 0.12351(13) 0.38139(11) 0.0321(4) Uani 1 1 d . A . H51A H 0.3858 0.1009 0.3734 0.038 Uiso 1 1 calc R . . H51B H 0.5279 0.0735 0.3797 0.038 Uiso 1 1 calc R . . O4 O 0.80511(12) 0.36634(8) 0.84292(8) 0.0344(3) Uani 1 1 d . . . O6 O 0.92182(12) 0.21707(9) 0.59636(8) 0.0339(3) Uani 1 1 d . . . O11 O 0.16261(12) 0.43100(9) 1.02959(8) 0.0337(3) Uani 1 1 d . . . O13 O 0.56631(13) 0.33767(10) 1.08240(9) 0.0380(3) Uani 1 1 d . . . H13 H 0.542(2) 0.3718(16) 1.1175(16) 0.046 Uiso 1 1 d . . . O18 O 0.35794(13) 0.32861(8) 0.52684(8) 0.0345(3) Uani 1 1 d . . . O20 O 0.26029(14) 0.48844(9) 0.76270(9) 0.0373(3) Uani 1 1 d . . . H20 H 0.263(2) 0.5368(16) 0.7135(16) 0.045 Uiso 1 1 d . . . O25 O 0.83869(11) 0.04770(9) 0.51904(8) 0.0339(3) Uani 1 1 d . . . O27 O 0.42778(12) 0.14195(9) 0.46870(8) 0.0352(3) Uani 1 1 d . . . O43 O 1.04921(13) 0.27632(10) 0.39538(9) 0.0415(3) Uani 1 1 d . . . O46 O 0.92922(14) 0.23962(10) 0.26767(9) 0.0462(3) Uani 1 1 d . A . O20A O 0.6969(3) 0.36188(13) 0.37976(13) 0.0540(6) Uani 0.804(3) 1 d PD A 1 H20A H 0.680(3) 0.314(3) 0.361(2) 0.065 Uiso 0.804(3) 1 d P A 1 O20B O 0.7854(11) 0.3731(5) 0.3698(5) 0.0540(6) Uani 0.196(3) 1 d PD A 2 H20B H 0.790(14) 0.344(8) 0.330(7) 0.065 Uiso 0.196(3) 1 d PD A 2 C201 C 0.7269(2) 0.33413(16) 0.46324(16) 0.0544(6) Uani 1 1 d D . . H21B H 0.6486 0.3376 0.5145 0.082 Uiso 0.804(3) 1 calc PR A 1 H21C H 0.7962 0.3755 0.4598 0.082 Uiso 0.804(3) 1 calc PR A 1 H21D H 0.7563 0.2702 0.4727 0.082 Uiso 0.804(3) 1 calc PR A 1 H21E H 0.6320 0.3402 0.4793 0.082 Uiso 0.196(3) 1 calc PR A 2 H21F H 0.7603 0.3664 0.4974 0.082 Uiso 0.196(3) 1 calc PR A 2 H21G H 0.7470 0.2683 0.4791 0.082 Uiso 0.196(3) 1 calc PR A 2 O100 O 0.51563(15) 0.44064(10) 0.20853(10) 0.0459(3) Uani 1 1 d . . . H100 H 0.589(3) 0.4667(18) 0.2075(16) 0.055 Uiso 1 1 d . . . C101 C 0.4153(2) 0.50446(16) 0.22104(15) 0.0501(5) Uani 1 1 d . . . H10A H 0.3306 0.4707 0.2521 0.075 Uiso 1 1 calc R . . H10B H 0.4164 0.5448 0.1612 0.075 Uiso 1 1 calc R . . H10C H 0.4290 0.5423 0.2585 0.075 Uiso 1 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 C1 0.0210(8) 0.0311(9) 0.0278(8) -0.0084(7) -0.0116(7) 0.0034(6) C2 0.0212(8) 0.0307(8) 0.0273(8) -0.0059(7) -0.0103(7) 0.0004(6) C3 0.0229(8) 0.0327(9) 0.0263(8) -0.0076(7) -0.0113(7) 0.0031(7) C4 0.0277(8) 0.0306(9) 0.0314(9) -0.0104(7) -0.0135(7) 0.0038(7) C5 0.0270(9) 0.0317(9) 0.0313(9) -0.0057(7) -0.0084(7) -0.0030(7) C6 0.0242(8) 0.0349(9) 0.0247(8) -0.0082(7) -0.0086(7) 0.0023(7) C7 0.0248(8) 0.0359(9) 0.0256(8) -0.0098(7) -0.0099(7) 0.0012(7) C8 0.0274(8) 0.0320(9) 0.0219(8) -0.0061(7) -0.0066(7) -0.0014(7) C9 0.0288(9) 0.0340(9) 0.0239(8) -0.0114(7) -0.0086(7) 0.0023(7) C10 0.0280(9) 0.0337(9) 0.0226(8) -0.0072(7) -0.0073(7) 0.0006(7) C11 0.0267(8) 0.0328(9) 0.0259(8) -0.0090(7) -0.0052(7) 0.0017(7) C12 0.0334(9) 0.0377(10) 0.0277(9) -0.0153(7) -0.0083(7) 0.0015(7) C13 0.0293(9) 0.0346(9) 0.0264(8) -0.0078(7) -0.0106(7) -0.0016(7) C14 0.0255(8) 0.0386(9) 0.0267(8) -0.0140(7) -0.0092(7) 0.0073(7) C15 0.0230(8) 0.0363(9) 0.0258(8) -0.0121(7) -0.0105(7) 0.0047(7) C16 0.0236(8) 0.0304(9) 0.0266(8) -0.0079(7) -0.0105(7) 0.0039(6) C17 0.0210(8) 0.0314(9) 0.0277(8) -0.0114(7) -0.0108(6) 0.0036(6) C18 0.0252(8) 0.0335(9) 0.0255(8) -0.0100(7) -0.0092(7) 0.0021(7) C19 0.0340(9) 0.0293(9) 0.0291(9) -0.0067(7) -0.0123(7) 0.0012(7) C20 0.0283(9) 0.0316(9) 0.0341(9) -0.0146(7) -0.0139(7) 0.0049(7) C21 0.0248(8) 0.0317(9) 0.0272(8) -0.0117(7) -0.0121(7) 0.0051(7) C22 0.0258(8) 0.0237(8) 0.0268(8) -0.0082(6) -0.0094(7) 0.0021(6) C23 0.0263(8) 0.0277(8) 0.0239(8) -0.0098(6) -0.0071(7) 0.0016(6) C24 0.0243(8) 0.0250(8) 0.0274(8) -0.0078(6) -0.0087(7) 0.0010(6) C25 0.0245(8) 0.0265(8) 0.0285(8) -0.0083(7) -0.0072(7) 0.0019(6) C26 0.0299(9) 0.0316(9) 0.0237(8) -0.0108(7) -0.0071(7) 0.0038(7) C27 0.0282(8) 0.0255(8) 0.0286(8) -0.0090(7) -0.0126(7) 0.0032(6) C28 0.0230(8) 0.0312(9) 0.0266(8) -0.0100(7) -0.0088(7) 0.0034(6) C29 0.0357(10) 0.0389(10) 0.0262(8) -0.0078(7) -0.0089(7) 0.0002(8) C30 0.0488(12) 0.0442(11) 0.0404(11) -0.0032(9) -0.0190(9) 0.0057(9) C31 0.0309(9) 0.0484(11) 0.0269(9) -0.0136(8) -0.0068(7) 0.0011(8) C32 0.0332(10) 0.0708(15) 0.0465(12) -0.0208(11) -0.0105(9) -0.0048(10) C33 0.0299(9) 0.0310(9) 0.0330(9) -0.0112(7) -0.0103(7) 0.0002(7) C34 0.0310(10) 0.0477(11) 0.0468(11) -0.0184(9) -0.0072(8) -0.0041(8) C35 0.0314(9) 0.0306(9) 0.0328(9) -0.0096(7) -0.0134(7) 0.0016(7) C36 0.0430(11) 0.0370(10) 0.0411(10) -0.0071(8) -0.0204(9) 0.0058(8) C37 0.0490(12) 0.0408(11) 0.0436(11) -0.0133(9) -0.0103(9) -0.0128(9) C38 0.0437(11) 0.0410(11) 0.0483(12) -0.0140(9) -0.0108(9) 0.0094(9) C39 0.0667(14) 0.0388(11) 0.0277(9) -0.0058(8) -0.0126(9) -0.0021(10) C40 0.0340(10) 0.0511(11) 0.0301(9) -0.0170(8) -0.0086(8) 0.0138(8) C41 0.0287(9) 0.0438(10) 0.0314(9) -0.0082(8) -0.0035(7) -0.0064(8) C42 0.0297(9) 0.0532(12) 0.0335(10) -0.0112(9) -0.0074(8) -0.0003(8) C44 0.0362(10) 0.0635(14) 0.0369(10) -0.0196(10) -0.0028(9) -0.0054(9) C45 0.0615(14) 0.0553(13) 0.0336(10) -0.0079(9) -0.0082(10) -0.0153(11) C47 0.0556(14) 0.0731(16) 0.0318(10) -0.0033(10) -0.0135(10) -0.0028(12) C48A 0.059(2) 0.060(2) 0.049(2) -0.029(2) -0.0292(19) 0.020(2) O49A 0.0518(13) 0.0598(15) 0.0364(10) -0.0126(10) -0.0108(9) -0.0148(12) C48B 0.035(6) 0.036(6) 0.032(6) -0.003(6) -0.010(4) -0.003(6) O49B 0.025(3) 0.024(4) 0.020(4) -0.004(3) -0.001(3) 0.011(3) C50 0.0588(14) 0.0593(14) 0.0391(11) -0.0025(10) -0.0237(10) -0.0145(11) C51 0.0359(9) 0.0374(9) 0.0285(9) -0.0136(7) -0.0139(7) 0.0019(7) O4 0.0370(7) 0.0331(7) 0.0340(6) -0.0127(5) -0.0088(5) -0.0039(5) O6 0.0302(6) 0.0413(7) 0.0266(6) -0.0119(5) -0.0009(5) -0.0068(5) O11 0.0299(6) 0.0377(7) 0.0348(6) -0.0153(5) -0.0086(5) 0.0069(5) O13 0.0368(7) 0.0513(8) 0.0386(7) -0.0248(6) -0.0194(6) 0.0074(6) O18 0.0464(7) 0.0332(7) 0.0232(6) -0.0086(5) -0.0098(5) 0.0015(5) O20 0.0520(8) 0.0312(7) 0.0353(7) -0.0147(6) -0.0188(6) 0.0059(6) O25 0.0271(6) 0.0476(7) 0.0311(6) -0.0188(6) -0.0100(5) 0.0117(5) O27 0.0346(7) 0.0508(8) 0.0288(6) -0.0190(6) -0.0169(5) 0.0138(6) O43 0.0415(7) 0.0496(8) 0.0316(7) -0.0131(6) -0.0082(6) 0.0043(6) O46 0.0451(8) 0.0543(9) 0.0348(7) -0.0042(6) -0.0137(6) 0.0009(7) O20A 0.0818(18) 0.0351(9) 0.0482(10) -0.0102(8) -0.0249(12) -0.0057(11) O20B 0.0818(18) 0.0351(9) 0.0482(10) -0.0102(8) -0.0249(12) -0.0057(11) C201 0.0659(15) 0.0423(12) 0.0577(14) -0.0099(10) -0.0276(12) 0.0063(11) O100 0.0475(8) 0.0475(8) 0.0537(9) -0.0234(7) -0.0235(7) 0.0066(7) C101 0.0557(13) 0.0463(12) 0.0473(12) -0.0109(10) -0.0181(10) 0.0086(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.392(2) . ? C1 C6 1.399(2) . ? C1 C28 1.523(2) . ? C2 C3 1.396(2) . ? C3 C4 1.401(2) . ? C3 C7 1.523(2) . ? C4 O4 1.371(2) . ? C4 C5 1.393(2) . ? C5 C6 1.384(2) . ? C6 O6 1.375(2) . ? C7 C8 1.524(2) . ? C7 C29 1.537(2) . ? C8 C9 1.388(2) . ? C8 C13 1.399(2) . ? C9 C10 1.396(2) . ? C10 C11 1.392(2) . ? C10 C14 1.517(2) . ? C11 C12 1.386(2) . ? C11 O11 1.391(2) . ? C12 C13 1.389(3) . ? C13 O13 1.365(2) . ? C14 C15 1.523(2) . ? C14 C31 1.535(3) . ? C15 C20 1.388(2) . ? C15 C16 1.396(2) . ? C16 C17 1.390(2) . ? C17 C18 1.396(2) . ? C17 C21 1.523(2) . ? C18 O18 1.372(2) . ? C18 C19 1.384(2) . ? C19 C20 1.392(2) . ? C20 O20 1.379(2) . ? C21 C22 1.524(2) . ? C21 C33 1.535(2) . ? C22 C23 1.388(2) . ? C22 C27 1.397(2) . ? C23 C24 1.389(2) . ? C24 C25 1.399(2) . ? C24 C28 1.523(2) . ? C25 O25 1.371(2) . ? C25 C26 1.390(2) . ? C26 C27 1.387(2) . ? C27 O27 1.372(2) . ? C28 C35 1.536(2) . ? C29 C30 1.520(3) . ? C31 C32 1.518(3) . ? C33 C34 1.527(2) . ? C35 C36 1.521(2) . ? C37 O4 1.427(2) . ? C38 O11 1.424(2) . ? C39 O18 1.414(2) . ? C40 O25 1.419(2) . ? C41 O6 1.431(2) . ? C41 C42 1.501(3) . ? C42 O43 1.415(2) . ? C44 O43 1.416(2) . ? C44 C45 1.492(3) . ? C45 O46 1.418(3) . ? C47 C48B 1.263(13) . ? C47 O46 1.398(3) . ? C47 C48A 1.509(5) . ? C48A O49A 1.404(4) . ? O49A C50 1.387(3) . ? C48B O49B 1.458(14) . ? O49B C50 1.666(7) . ? C50 C51 1.494(3) . ? C51 O27 1.425(2) . ? O20A C201 1.426(3) . ? O20B C201 1.388(7) . ? O100 C101 1.408(3) . ? 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 C2 C1 C6 116.82(15) . . ? C2 C1 C28 124.02(15) . . ? C6 C1 C28 119.13(14) . . ? C1 C2 C3 124.06(15) . . ? C2 C3 C4 116.75(15) . . ? C2 C3 C7 123.33(15) . . ? C4 C3 C7 119.83(15) . . ? O4 C4 C5 122.75(15) . . ? O4 C4 C3 116.20(15) . . ? C5 C4 C3 121.05(15) . . ? C6 C5 C4 119.96(16) . . ? O6 C6 C5 122.96(15) . . ? O6 C6 C1 115.67(15) . . ? C5 C6 C1 121.35(15) . . ? C3 C7 C8 113.76(13) . . ? C3 C7 C29 114.58(14) . . ? C8 C7 C29 107.71(14) . . ? C9 C8 C13 117.47(16) . . ? C9 C8 C7 121.64(15) . . ? C13 C8 C7 120.48(14) . . ? C8 C9 C10 123.35(15) . . ? C11 C10 C9 117.21(15) . . ? C11 C10 C14 120.45(15) . . ? C9 C10 C14 121.73(15) . . ? C12 C11 O11 118.67(15) . . ? C12 C11 C10 121.19(16) . . ? O11 C11 C10 119.96(15) . . ? C11 C12 C13 120.04(15) . . ? O13 C13 C12 121.53(15) . . ? O13 C13 C8 117.79(15) . . ? C12 C13 C8 120.66(15) . . ? C10 C14 C15 114.16(13) . . ? C10 C14 C31 107.52(14) . . ? C15 C14 C31 114.17(14) . . ? C20 C15 C16 116.65(15) . . ? C20 C15 C14 120.61(15) . . ? C16 C15 C14 122.66(15) . . ? C17 C16 C15 123.92(16) . . ? C16 C17 C18 116.98(15) . . ? C16 C17 C21 123.90(15) . . ? C18 C17 C21 119.13(14) . . ? O18 C18 C19 123.45(15) . . ? O18 C18 C17 115.38(14) . . ? C19 C18 C17 121.17(15) . . ? C18 C19 C20 119.70(16) . . ? O20 C20 C15 118.72(15) . . ? O20 C20 C19 119.70(16) . . ? C15 C20 C19 121.56(15) . . ? C17 C21 C22 111.13(13) . . ? C17 C21 C33 114.44(13) . . ? C22 C21 C33 109.42(13) . . ? C23 C22 C27 117.45(15) . . ? C23 C22 C21 120.71(14) . . ? C27 C22 C21 121.70(14) . . ? C22 C23 C24 123.73(15) . . ? C23 C24 C25 116.99(14) . . ? C23 C24 C28 121.12(14) . . ? C25 C24 C28 121.68(14) . . ? O25 C25 C26 122.62(14) . . ? O25 C25 C24 116.41(14) . . ? C26 C25 C24 120.96(15) . . ? C27 C26 C25 120.05(15) . . ? O27 C27 C26 123.46(14) . . ? O27 C27 C22 115.86(14) . . ? C26 C27 C22 120.67(15) . . ? C24 C28 C1 112.25(13) . . ? C24 C28 C35 109.24(13) . . ? C1 C28 C35 114.53(13) . . ? C30 C29 C7 115.55(16) . . ? C32 C31 C14 114.45(16) . . ? C34 C33 C21 114.35(15) . . ? C36 C35 C28 115.23(14) . . ? O6 C41 C42 108.15(15) . . ? O43 C42 C41 109.68(16) . . ? O43 C44 C45 109.62(18) . . ? O46 C45 C44 111.06(17) . . ? C48B C47 O46 123.3(6) . . ? O46 C47 C48A 113.4(2) . . ? O49A C48A C47 112.0(3) . . ? C50 O49A C48A 113.6(3) . . ? C47 C48B O49B 115.0(10) . . ? C48B O49B C50 105.2(7) . . ? O49A C50 C51 117.15(19) . . ? C51 C50 O49B 99.1(3) . . ? O27 C51 C50 113.01(16) . . ? C4 O4 C37 117.65(14) . . ? C6 O6 C41 118.09(13) . . ? C11 O11 C38 113.88(14) . . ? C18 O18 C39 118.23(14) . . ? C25 O25 C40 117.16(13) . . ? C27 O27 C51 121.35(13) . . ? C42 O43 C44 111.56(15) . . ? C47 O46 C45 113.12(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -1.2(2) . . . . ? C28 C1 C2 C3 176.73(15) . . . . ? C1 C2 C3 C4 1.2(2) . . . . ? C1 C2 C3 C7 -175.43(15) . . . . ? C2 C3 C4 O4 -179.88(14) . . . . ? C7 C3 C4 O4 -3.1(2) . . . . ? C2 C3 C4 C5 -0.6(2) . . . . ? C7 C3 C4 C5 176.20(15) . . . . ? O4 C4 C5 C6 179.23(15) . . . . ? C3 C4 C5 C6 0.0(3) . . . . ? C4 C5 C6 O6 -178.29(15) . . . . ? C4 C5 C6 C1 0.1(3) . . . . ? C2 C1 C6 O6 178.97(14) . . . . ? C28 C1 C6 O6 1.0(2) . . . . ? C2 C1 C6 C5 0.5(2) . . . . ? C28 C1 C6 C5 -177.51(15) . . . . ? C2 C3 C7 C8 -101.83(18) . . . . ? C4 C3 C7 C8 81.64(19) . . . . ? C2 C3 C7 C29 22.7(2) . . . . ? C4 C3 C7 C29 -153.83(15) . . . . ? C3 C7 C8 C9 46.6(2) . . . . ? C29 C7 C8 C9 -81.51(19) . . . . ? C3 C7 C8 C13 -140.85(16) . . . . ? C29 C7 C8 C13 91.00(18) . . . . ? C13 C8 C9 C10 -0.6(3) . . . . ? C7 C8 C9 C10 172.15(15) . . . . ? C8 C9 C10 C11 1.4(3) . . . . ? C8 C9 C10 C14 -169.67(16) . . . . ? C9 C10 C11 C12 0.1(2) . . . . ? C14 C10 C11 C12 171.28(16) . . . . ? C9 C10 C11 O11 -174.95(15) . . . . ? C14 C10 C11 O11 -3.8(2) . . . . ? O11 C11 C12 C13 172.75(15) . . . . ? C10 C11 C12 C13 -2.4(3) . . . . ? C11 C12 C13 O13 -175.15(16) . . . . ? C11 C12 C13 C8 3.2(3) . . . . ? C9 C8 C13 O13 176.66(15) . . . . ? C7 C8 C13 O13 3.9(2) . . . . ? C9 C8 C13 C12 -1.8(2) . . . . ? C7 C8 C13 C12 -174.56(15) . . . . ? C11 C10 C14 C15 141.31(16) . . . . ? C9 C10 C14 C15 -47.9(2) . . . . ? C11 C10 C14 C31 -90.93(19) . . . . ? C9 C10 C14 C31 79.85(19) . . . . ? C10 C14 C15 C20 -80.7(2) . . . . ? C31 C14 C15 C20 155.05(16) . . . . ? C10 C14 C15 C16 102.73(18) . . . . ? C31 C14 C15 C16 -21.5(2) . . . . ? C20 C15 C16 C17 -1.4(2) . . . . ? C14 C15 C16 C17 175.27(15) . . . . ? C15 C16 C17 C18 0.7(2) . . . . ? C15 C16 C17 C21 -179.07(15) . . . . ? C16 C17 C18 O18 -179.64(14) . . . . ? C21 C17 C18 O18 0.1(2) . . . . ? C16 C17 C18 C19 0.4(2) . . . . ? C21 C17 C18 C19 -179.89(15) . . . . ? O18 C18 C19 C20 179.48(15) . . . . ? C17 C18 C19 C20 -0.5(3) . . . . ? C16 C15 C20 O20 -179.63(14) . . . . ? C14 C15 C20 O20 3.6(2) . . . . ? C16 C15 C20 C19 1.3(2) . . . . ? C14 C15 C20 C19 -175.53(15) . . . . ? C18 C19 C20 O20 -179.43(15) . . . . ? C18 C19 C20 C15 -0.3(3) . . . . ? C16 C17 C21 C22 -104.50(17) . . . . ? C18 C17 C21 C22 75.77(18) . . . . ? C16 C17 C21 C33 20.0(2) . . . . ? C18 C17 C21 C33 -159.68(14) . . . . ? C17 C21 C22 C23 59.37(19) . . . . ? C33 C21 C22 C23 -67.97(19) . . . . ? C17 C21 C22 C27 -125.03(16) . . . . ? C33 C21 C22 C27 107.63(17) . . . . ? C27 C22 C23 C24 -3.2(2) . . . . ? C21 C22 C23 C24 172.59(15) . . . . ? C22 C23 C24 C25 1.1(2) . . . . ? C22 C23 C24 C28 -173.74(15) . . . . ? C23 C24 C25 O25 -176.27(14) . . . . ? C28 C24 C25 O25 -1.5(2) . . . . ? C23 C24 C25 C26 2.6(2) . . . . ? C28 C24 C25 C26 177.35(15) . . . . ? O25 C25 C26 C27 174.81(15) . . . . ? C24 C25 C26 C27 -4.0(3) . . . . ? C25 C26 C27 O27 -177.48(15) . . . . ? C25 C26 C27 C22 1.7(2) . . . . ? C23 C22 C27 O27 -178.99(14) . . . . ? C21 C22 C27 O27 5.3(2) . . . . ? C23 C22 C27 C26 1.7(2) . . . . ? C21 C22 C27 C26 -173.99(15) . . . . ? C23 C24 C28 C1 -56.6(2) . . . . ? C25 C24 C28 C1 128.86(16) . . . . ? C23 C24 C28 C35 71.56(19) . . . . ? C25 C24 C28 C35 -102.99(17) . . . . ? C2 C1 C28 C24 102.23(18) . . . . ? C6 C1 C28 C24 -79.93(18) . . . . ? C2 C1 C28 C35 -23.1(2) . . . . ? C6 C1 C28 C35 154.77(15) . . . . ? C3 C7 C29 C30 64.0(2) . . . . ? C8 C7 C29 C30 -168.36(15) . . . . ? C10 C14 C31 C32 165.83(16) . . . . ? C15 C14 C31 C32 -66.4(2) . . . . ? C17 C21 C33 C34 65.06(19) . . . . ? C22 C21 C33 C34 -169.49(14) . . . . ? C24 C28 C35 C36 168.01(15) . . . . ? C1 C28 C35 C36 -65.1(2) . . . . ? O6 C41 C42 O43 77.78(19) . . . . ? O43 C44 C45 O46 -73.1(2) . . . . ? C48B C47 C48A O49A -50.7(14) . . . . ? O46 C47 C48A O49A 66.9(4) . . . . ? C47 C48A O49A C50 167.7(2) . . . . ? O46 C47 C48B O49B -37.5(15) . . . . ? C48A C47 C48B O49B 39.3(9) . . . . ? C47 C48B O49B C50 170.2(9) . . . . ? C48A O49A C50 C51 105.1(3) . . . . ? C48A O49A C50 O49B 44.4(4) . . . . ? C48B O49B C50 O49A -48.8(7) . . . . ? C48B O49B C50 C51 -177.0(7) . . . . ? O49A C50 C51 O27 70.8(3) . . . . ? O49B C50 C51 O27 98.5(3) . . . . ? C5 C4 O4 C37 -7.3(2) . . . . ? C3 C4 O4 C37 172.01(16) . . . . ? C5 C6 O6 C41 12.7(2) . . . . ? C1 C6 O6 C41 -165.79(15) . . . . ? C42 C41 O6 C6 169.83(15) . . . . ? C12 C11 O11 C38 84.8(2) . . . . ? C10 C11 O11 C38 -100.08(19) . . . . ? C19 C18 O18 C39 -3.0(3) . . . . ? C17 C18 O18 C39 176.96(16) . . . . ? C26 C25 O25 C40 -4.0(2) . . . . ? C24 C25 O25 C40 174.85(15) . . . . ? C26 C27 O27 C51 6.2(2) . . . . ? C22 C27 O27 C51 -173.04(15) . . . . ? C50 C51 O27 C27 -93.9(2) . . . . ? C41 C42 O43 C44 -178.30(16) . . . . ? C45 C44 O43 C42 -176.40(16) . . . . ? C48B C47 O46 C45 -153.5(9) . . . . ? C48A C47 O46 C45 176.9(2) . . . . ? C44 C45 O46 C47 -173.99(19) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O13 H13 O100 0.83(2) 1.95(2) 2.7698(19) 168(2) 1_556 O20 H20 O20B 0.91(2) 1.81(3) 2.685(8) 162(2) 2_666 O20 H20 O20A 0.91(2) 1.77(2) 2.659(2) 166(2) 2_666 O20A H20A O49A 0.91(4) 1.90(4) 2.784(3) 165(3) . O20B H20B O46 0.85(2) 2.32(10) 2.982(9) 136(12) . O100 H100 O20 0.89(3) 2.05(3) 2.923(2) 167(2) 2_666 _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 67.00 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 0.265 _refine_diff_density_min -0.287 _refine_diff_density_rms 0.041 #===END data_III _database_code_depnum_ccdc_archive 'CCDC 735048' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H74 N4 O11' _chemical_formula_weight 979.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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 10.8272(4) _cell_length_b 16.3070(5) _cell_length_c 17.0285(8) _cell_angle_alpha 72.658(2) _cell_angle_beta 81.115(2) _cell_angle_gamma 70.302(3) _cell_volume 2697.05(18) _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 needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.206 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1052 _exptl_absorpt_coefficient_mu 0.676 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8491 _exptl_absorpt_correction_T_max 0.9670 _exptl_absorpt_process_details 'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14021 _diffrn_reflns_av_R_equivalents 0.0444 _diffrn_reflns_av_sigmaI/netI 0.0479 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 66.83 _reflns_number_total 9311 _reflns_number_gt 6723 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0749P)^2^+2.4285P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9311 _refine_ls_number_parameters 656 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0924 _refine_ls_R_factor_gt 0.0643 _refine_ls_wR_factor_ref 0.1804 _refine_ls_wR_factor_gt 0.1614 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.087 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_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_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7506(3) 0.26379(18) 0.37974(17) 0.0306(6) Uani 1 1 d . . . C2 C 0.8244(3) 0.17535(18) 0.37987(17) 0.0302(6) Uani 1 1 d . . . H2 H 0.8820 0.1415 0.4231 0.036 Uiso 1 1 calc R . . C3 C 0.8192(3) 0.13360(19) 0.32098(17) 0.0310(6) Uani 1 1 d . . . C4 C 0.7346(3) 0.1850(2) 0.25731(18) 0.0331(6) Uani 1 1 d . . . C5 C 0.6577(3) 0.27312(19) 0.25467(19) 0.0355(7) Uani 1 1 d . . . H5 H 0.5994 0.3066 0.2118 0.043 Uiso 1 1 calc R . . C6 C 0.6663(3) 0.31205(19) 0.31475(18) 0.0330(6) Uani 1 1 d . . . C7 C 0.8938(3) 0.03607(19) 0.32266(18) 0.0336(6) Uani 1 1 d . . . H7 H 0.8327 0.0120 0.3044 0.040 Uiso 1 1 calc R . . C8 C 1.0139(3) 0.02609(19) 0.26215(19) 0.0347(7) Uani 1 1 d . . . C9 C 1.1135(3) 0.06148(19) 0.26362(18) 0.0336(6) Uani 1 1 d . . . H9 H 1.1018 0.0977 0.3004 0.040 Uiso 1 1 calc R . . C10 C 1.2302(3) 0.04649(19) 0.21376(18) 0.0346(6) Uani 1 1 d . . . C11 C 1.2444(3) -0.0058(2) 0.16021(19) 0.0382(7) Uani 1 1 d . . . C12 C 1.1466(3) -0.0421(2) 0.1567(2) 0.0465(8) Uani 1 1 d . . . H12 H 1.1571 -0.0773 0.1192 0.056 Uiso 1 1 calc R . . C13 C 1.0332(3) -0.0264(2) 0.2085(2) 0.0408(7) Uani 1 1 d . . . C14 C 1.3419(3) 0.07776(19) 0.22594(19) 0.0343(6) Uani 1 1 d . . . H14 H 1.4090 0.0682 0.1794 0.041 Uiso 1 1 calc R . . C15 C 1.2990(3) 0.17799(19) 0.22111(17) 0.0303(6) Uani 1 1 d . . . C16 C 1.2705(3) 0.21289(19) 0.28908(18) 0.0315(6) Uani 1 1 d . . . H16 H 1.2766 0.1713 0.3421 0.038 Uiso 1 1 calc R . . C17 C 1.2336(3) 0.30406(19) 0.28557(18) 0.0312(6) Uani 1 1 d . . . C18 C 1.2237(3) 0.36453(19) 0.20601(18) 0.0330(6) Uani 1 1 d . . . C19 C 1.2518(3) 0.3330(2) 0.13632(18) 0.0352(7) Uani 1 1 d . . . H19 H 1.2464 0.3745 0.0832 0.042 Uiso 1 1 calc R . . C20 C 1.2881(3) 0.2406(2) 0.14366(18) 0.0344(6) Uani 1 1 d . . . C21 C 1.2053(3) 0.34206(18) 0.36011(17) 0.0306(6) Uani 1 1 d . . . H21 H 1.2486 0.3903 0.3472 0.037 Uiso 1 1 calc R . . C22 C 1.0591(3) 0.38669(18) 0.37718(17) 0.0298(6) Uani 1 1 d . . . C23 C 0.9710(3) 0.33695(18) 0.39285(17) 0.0297(6) Uani 1 1 d . . . H23 H 1.0020 0.2782 0.3844 0.036 Uiso 1 1 calc R . . C24 C 0.8407(3) 0.36889(18) 0.42013(17) 0.0300(6) Uani 1 1 d . . . C25 C 0.7970(3) 0.45549(19) 0.43099(17) 0.0309(6) Uani 1 1 d . . . C26 C 0.8799(3) 0.50911(19) 0.41224(17) 0.0322(6) Uani 1 1 d . . . H26 H 0.8474 0.5693 0.4174 0.039 Uiso 1 1 calc R . . C27 C 1.0101(3) 0.47414(18) 0.38603(17) 0.0308(6) Uani 1 1 d . A . C28 C 0.7523(3) 0.30831(18) 0.44530(17) 0.0311(6) Uani 1 1 d . . . H28 H 0.6607 0.3482 0.4531 0.037 Uiso 1 1 calc R . . C29 C 0.9348(3) -0.0254(2) 0.40818(18) 0.0373(7) Uani 1 1 d . . . H29A H 0.9895 -0.0859 0.4022 0.045 Uiso 1 1 calc R . . H29B H 0.9900 -0.0007 0.4300 0.045 Uiso 1 1 calc R . . C30 C 0.8204(3) -0.0363(2) 0.4709(2) 0.0489(8) Uani 1 1 d . . . H30A H 0.7651 0.0232 0.4772 0.073 Uiso 1 1 calc R . . H30B H 0.8547 -0.0747 0.5241 0.073 Uiso 1 1 calc R . . H30C H 0.7679 -0.0643 0.4516 0.073 Uiso 1 1 calc R . . C31 C 1.4077(3) 0.0158(2) 0.3054(2) 0.0385(7) Uani 1 1 d . . . H31A H 1.3466 0.0283 0.3531 0.046 Uiso 1 1 calc R . . H31B H 1.4225 -0.0477 0.3061 0.046 Uiso 1 1 calc R . . C32 C 1.5383(3) 0.0263(2) 0.3163(2) 0.0526(9) Uani 1 1 d . . . H32A H 1.6008 0.0122 0.2704 0.079 Uiso 1 1 calc R . . H32B H 1.5735 -0.0152 0.3683 0.079 Uiso 1 1 calc R . . H32C H 1.5246 0.0886 0.3172 0.079 Uiso 1 1 calc R . . C33 C 1.2620(3) 0.2725(2) 0.44018(18) 0.0349(6) Uani 1 1 d . . . H33A H 1.2293 0.3009 0.4865 0.042 Uiso 1 1 calc R . . H33B H 1.2277 0.2208 0.4512 0.042 Uiso 1 1 calc R . . C34 C 1.4111(3) 0.2368(2) 0.4391(2) 0.0456(8) Uani 1 1 d . . . H34A H 1.4448 0.2055 0.3955 0.068 Uiso 1 1 calc R . . H34B H 1.4381 0.1946 0.4925 0.068 Uiso 1 1 calc R . . H34C H 1.4465 0.2873 0.4285 0.068 Uiso 1 1 calc R . . C35 C 0.7911(3) 0.2426(2) 0.52998(18) 0.0352(7) Uani 1 1 d . . . H35A H 0.8809 0.2012 0.5237 0.042 Uiso 1 1 calc R . . H35B H 0.7943 0.2778 0.5676 0.042 Uiso 1 1 calc R . . C36 C 0.6992(3) 0.1859(2) 0.5703(2) 0.0432(8) Uani 1 1 d . . . H36A H 0.6100 0.2260 0.5773 0.065 Uiso 1 1 calc R . . H36B H 0.7301 0.1473 0.6243 0.065 Uiso 1 1 calc R . . H36C H 0.6989 0.1481 0.5352 0.065 Uiso 1 1 calc R . . C37 C 0.6439(4) 0.1880(3) 0.1365(2) 0.0521(9) Uani 1 1 d . . . H37A H 0.5547 0.2026 0.1624 0.078 Uiso 1 1 calc R . . H37B H 0.6522 0.1486 0.1010 0.078 Uiso 1 1 calc R . . H37C H 0.6613 0.2438 0.1032 0.078 Uiso 1 1 calc R . . C38 C 1.3720(4) -0.0636(3) 0.0490(2) 0.0542(9) Uani 1 1 d . . . H38A H 1.3591 -0.1230 0.0725 0.081 Uiso 1 1 calc R . . H38B H 1.4594 -0.0708 0.0207 0.081 Uiso 1 1 calc R . . H38C H 1.3049 -0.0257 0.0097 0.081 Uiso 1 1 calc R . . C39 C 1.1716(4) 0.5179(2) 0.1250(2) 0.0553(9) Uani 1 1 d . . . H39A H 1.2570 0.5078 0.0939 0.083 Uiso 1 1 calc R . . H39B H 1.1414 0.5792 0.1321 0.083 Uiso 1 1 calc R . . H39C H 1.1077 0.5105 0.0948 0.083 Uiso 1 1 calc R . . C40 C 0.6239(3) 0.5699(2) 0.4778(2) 0.0449(8) Uani 1 1 d . . . H40A H 0.6778 0.5713 0.5184 0.067 Uiso 1 1 calc R . . H40B H 0.5321 0.5818 0.4995 0.067 Uiso 1 1 calc R . . H40C H 0.6300 0.6163 0.4266 0.067 Uiso 1 1 calc R . . C41 C 0.4941(3) 0.4475(2) 0.25875(19) 0.0384(7) Uani 1 1 d . . . H41A H 0.4347 0.4113 0.2632 0.046 Uiso 1 1 calc R . . H41B H 0.5331 0.4595 0.2016 0.046 Uiso 1 1 calc R . . C42 C 0.4192(3) 0.5341(2) 0.2796(2) 0.0424(8) Uani 1 1 d . . . H42A H 0.3338 0.5600 0.2537 0.051 Uiso 1 1 calc R . . H42B H 0.4016 0.5230 0.3400 0.051 Uiso 1 1 calc R . . C44 C 0.4255(3) 0.6787(2) 0.2723(2) 0.0463(8) Uani 1 1 d . . . H44A H 0.4174 0.6673 0.3330 0.056 Uiso 1 1 calc R . . H44B H 0.3358 0.7031 0.2521 0.056 Uiso 1 1 calc R . . C45 C 0.4974(3) 0.7463(2) 0.2356(2) 0.0494(8) Uani 1 1 d . A . H45A H 0.5234 0.7475 0.1770 0.059 Uiso 1 1 calc R . . H45B H 0.4388 0.8072 0.2379 0.059 Uiso 1 1 calc R . . C47 C 0.6770(4) 0.7906(2) 0.2498(3) 0.0571(10) Uani 1 1 d . A . H47A H 0.6150 0.8501 0.2533 0.069 Uiso 1 1 calc R . . H47B H 0.7069 0.7946 0.1912 0.069 Uiso 1 1 calc R . . C48 C 0.7908(4) 0.7687(3) 0.2981(3) 0.0722(12) Uani 1 1 d D . . H48A H 0.8203 0.8225 0.2870 0.087 Uiso 0.765(6) 1 calc PR A 1 H48B H 0.7657 0.7507 0.3576 0.087 Uiso 0.765(6) 1 calc PR A 1 H48C H 0.8436 0.8077 0.2651 0.087 Uiso 0.235(6) 1 calc PR A 2 H48D H 0.7549 0.7908 0.3477 0.087 Uiso 0.235(6) 1 calc PR A 2 C50 C 1.0171(4) 0.6837(3) 0.3038(3) 0.0655(11) Uani 1 1 d D . . H50A H 1.0127 0.7416 0.3133 0.079 Uiso 0.765(6) 1 calc PR A 1 H50B H 1.0854 0.6729 0.2589 0.079 Uiso 0.765(6) 1 calc PR A 1 H50C H 1.0520 0.6640 0.2529 0.079 Uiso 0.235(6) 1 calc PR A 2 H50D H 1.0370 0.7396 0.3008 0.079 Uiso 0.235(6) 1 calc PR A 2 C51 C 1.0630(3) 0.61033(19) 0.3804(2) 0.0388(7) Uani 1 1 d . A . H51A H 1.1401 0.6179 0.3987 0.047 Uiso 1 1 calc R . . H51B H 0.9923 0.6161 0.4247 0.047 Uiso 1 1 calc R . . O4 O 0.7359(2) 0.14308(14) 0.19845(13) 0.0399(5) Uani 1 1 d . . . O6 O 0.59553(19) 0.39921(13) 0.31549(13) 0.0390(5) Uani 1 1 d . . . O11 O 1.3612(2) -0.02208(16) 0.11297(15) 0.0494(6) Uani 1 1 d . . . O13 O 0.9377(2) -0.06523(18) 0.20917(18) 0.0579(7) Uani 1 1 d . . . H13 H 0.949(4) -0.078(3) 0.154(3) 0.069 Uiso 1 1 d . . . O18 O 1.1842(2) 0.45421(13) 0.20359(12) 0.0394(5) Uani 1 1 d . . . O20 O 1.3162(2) 0.20800(16) 0.07561(14) 0.0462(6) Uani 1 1 d . . . H20 H 1.289(4) 0.244(3) 0.034(3) 0.055 Uiso 1 1 d . . . O25 O 0.66964(19) 0.48397(13) 0.46204(13) 0.0390(5) Uani 1 1 d . . . O27 O 1.09803(19) 0.52262(13) 0.36809(13) 0.0393(5) Uani 1 1 d . . . O43 O 0.4924(2) 0.59634(14) 0.25096(14) 0.0425(5) Uani 1 1 d . . . O46 O 0.6113(2) 0.72428(15) 0.27900(15) 0.0525(5) Uani 1 1 d . . . O49A O 0.8971(3) 0.6949(2) 0.2753(3) 0.0525(5) Uani 0.765(6) 1 d PD A 1 O49B O 0.8706(9) 0.6932(6) 0.3231(9) 0.0525(5) Uani 0.235(6) 1 d PD A 2 N100 N 0.7539(4) 0.4204(3) 0.0781(2) 0.0824(11) Uani 1 1 d . . . C101 C 0.8326(4) 0.3786(3) 0.1240(3) 0.0609(10) Uani 1 1 d . . . C102 C 0.9319(4) 0.3251(3) 0.1840(3) 0.0653(11) Uani 1 1 d . . . H10A H 0.9102 0.3480 0.2330 0.098 Uiso 1 1 calc R . . H10B H 1.0183 0.3295 0.1596 0.098 Uiso 1 1 calc R . . H10C H 0.9337 0.2618 0.1995 0.098 Uiso 1 1 calc R . . N200 N 0.9299(5) -0.1150(4) 0.0700(3) 0.1191(18) Uani 1 1 d . . . C201 C 0.9612(5) -0.1495(4) 0.0187(3) 0.0782(13) Uani 1 1 d . . . C202 C 0.9974(5) -0.1923(3) -0.0475(3) 0.0780(13) Uani 1 1 d . . . H20A H 0.9184 -0.1833 -0.0746 0.117 Uiso 1 1 calc R . . H20B H 1.0405 -0.2571 -0.0256 0.117 Uiso 1 1 calc R . . H20C H 1.0579 -0.1658 -0.0877 0.117 Uiso 1 1 calc R . . N300 N 0.2622(5) 0.7230(3) 0.0918(3) 0.0960(13) Uani 1 1 d . . . C301 C 0.3606(5) 0.6786(3) 0.0682(3) 0.0713(12) Uani 1 1 d . . . C302 C 0.4803(5) 0.6225(4) 0.0380(3) 0.1017(19) Uani 1 1 d . . . H30D H 0.5328 0.5820 0.0845 0.152 Uiso 1 1 calc R . . H30E H 0.5303 0.6605 0.0012 0.152 Uiso 1 1 calc R . . H30F H 0.4597 0.5867 0.0077 0.152 Uiso 1 1 calc R . . N400 N 0.7757(4) 0.6561(3) 0.0696(2) 0.0849(12) Uani 1 1 d . . . C401 C 0.7935(4) 0.6095(3) 0.1339(2) 0.0589(10) Uani 1 1 d . . . C402 C 0.8161(4) 0.5510(3) 0.2165(2) 0.0587(10) Uani 1 1 d . . . H40D H 0.8009 0.5878 0.2553 0.088 Uiso 1 1 calc R . . H40E H 0.9070 0.5109 0.2184 0.088 Uiso 1 1 calc R . . H40F H 0.7557 0.5148 0.2315 0.088 Uiso 1 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 C1 0.0234(13) 0.0310(14) 0.0358(15) -0.0015(12) -0.0017(11) -0.0128(11) C2 0.0249(14) 0.0307(14) 0.0322(15) -0.0008(12) -0.0034(11) -0.0111(11) C3 0.0236(14) 0.0337(15) 0.0334(15) -0.0012(12) -0.0028(11) -0.0123(11) C4 0.0284(15) 0.0387(16) 0.0352(16) -0.0069(13) -0.0026(12) -0.0165(12) C5 0.0282(15) 0.0349(16) 0.0381(16) 0.0020(13) -0.0073(12) -0.0109(12) C6 0.0247(14) 0.0302(15) 0.0419(17) -0.0030(12) -0.0035(12) -0.0107(12) C7 0.0299(15) 0.0334(15) 0.0389(16) -0.0064(13) -0.0053(12) -0.0129(12) C8 0.0318(15) 0.0315(15) 0.0404(16) -0.0069(13) -0.0070(13) -0.0095(12) C9 0.0324(15) 0.0323(15) 0.0370(16) -0.0083(12) -0.0038(12) -0.0112(12) C10 0.0323(15) 0.0320(15) 0.0391(16) -0.0072(13) -0.0032(13) -0.0109(12) C11 0.0329(16) 0.0366(16) 0.0440(17) -0.0134(14) 0.0011(13) -0.0084(13) C12 0.052(2) 0.0480(19) 0.0478(19) -0.0222(16) 0.0001(16) -0.0198(16) C13 0.0379(17) 0.0422(17) 0.0470(18) -0.0123(14) -0.0047(14) -0.0168(14) C14 0.0291(15) 0.0340(15) 0.0393(16) -0.0089(13) -0.0003(12) -0.0104(12) C15 0.0233(13) 0.0341(15) 0.0353(15) -0.0081(12) -0.0014(11) -0.0121(11) C16 0.0242(14) 0.0327(15) 0.0356(15) -0.0008(12) -0.0037(11) -0.0126(11) C17 0.0212(13) 0.0335(15) 0.0379(16) -0.0064(12) 0.0006(11) -0.0110(11) C18 0.0270(14) 0.0332(15) 0.0380(16) -0.0064(12) -0.0006(12) -0.0115(12) C19 0.0322(15) 0.0382(16) 0.0314(15) -0.0018(12) -0.0036(12) -0.0120(12) C20 0.0279(15) 0.0419(17) 0.0357(16) -0.0112(13) -0.0003(12) -0.0135(12) C21 0.0265(14) 0.0303(14) 0.0355(15) -0.0055(12) -0.0009(11) -0.0128(11) C22 0.0271(14) 0.0325(15) 0.0287(14) -0.0024(11) -0.0033(11) -0.0122(11) C23 0.0286(14) 0.0281(14) 0.0305(14) -0.0046(11) -0.0022(11) -0.0091(11) C24 0.0284(14) 0.0308(14) 0.0299(14) -0.0024(11) -0.0040(11) -0.0119(11) C25 0.0260(14) 0.0327(15) 0.0314(15) -0.0049(12) -0.0015(11) -0.0090(12) C26 0.0322(15) 0.0273(14) 0.0339(15) -0.0038(12) -0.0005(12) -0.0095(12) C27 0.0302(15) 0.0317(15) 0.0318(15) -0.0033(12) -0.0027(12) -0.0152(12) C28 0.0232(13) 0.0295(14) 0.0372(16) -0.0047(12) -0.0018(11) -0.0076(11) C29 0.0397(17) 0.0309(15) 0.0383(17) -0.0023(13) -0.0071(13) -0.0108(13) C30 0.054(2) 0.0436(19) 0.0456(19) 0.0028(15) -0.0046(16) -0.0232(16) C31 0.0304(15) 0.0333(15) 0.0487(18) -0.0063(13) -0.0045(13) -0.0089(12) C32 0.0409(19) 0.0462(19) 0.070(2) -0.0071(17) -0.0189(17) -0.0126(15) C33 0.0304(15) 0.0372(16) 0.0369(16) -0.0072(13) -0.0040(12) -0.0116(12) C34 0.0349(17) 0.0496(19) 0.0489(19) -0.0092(15) -0.0109(14) -0.0085(14) C35 0.0356(16) 0.0355(16) 0.0335(16) -0.0028(12) -0.0032(12) -0.0146(13) C36 0.0479(19) 0.0433(18) 0.0387(17) -0.0042(14) 0.0016(14) -0.0221(15) C37 0.055(2) 0.060(2) 0.0440(19) -0.0088(16) -0.0199(16) -0.0175(17) C38 0.053(2) 0.059(2) 0.054(2) -0.0260(18) 0.0110(17) -0.0183(17) C39 0.075(3) 0.0359(18) 0.046(2) 0.0033(15) -0.0069(18) -0.0170(17) C40 0.0355(17) 0.0381(17) 0.059(2) -0.0158(15) 0.0113(15) -0.0126(13) C41 0.0289(15) 0.0387(16) 0.0406(17) 0.0012(13) -0.0079(13) -0.0091(13) C42 0.0297(16) 0.0400(17) 0.0462(18) 0.0025(14) -0.0042(13) -0.0077(13) C44 0.0339(17) 0.0450(19) 0.056(2) -0.0153(16) -0.0068(15) -0.0036(14) C45 0.0458(19) 0.0393(18) 0.055(2) -0.0058(15) -0.0084(16) -0.0058(15) C47 0.052(2) 0.0360(18) 0.075(3) 0.0002(17) -0.0103(19) -0.0132(16) C48 0.064(3) 0.073(3) 0.087(3) -0.019(2) 0.001(2) -0.036(2) C50 0.064(2) 0.044(2) 0.083(3) 0.0109(19) -0.028(2) -0.0245(18) C51 0.0385(17) 0.0353(16) 0.0463(18) -0.0098(14) -0.0033(14) -0.0168(13) O4 0.0391(12) 0.0434(12) 0.0373(11) -0.0074(9) -0.0111(9) -0.0120(9) O6 0.0318(11) 0.0328(11) 0.0459(12) -0.0019(9) -0.0143(9) -0.0039(9) O11 0.0440(13) 0.0547(14) 0.0592(15) -0.0310(12) 0.0107(11) -0.0196(11) O13 0.0561(15) 0.0726(17) 0.0681(17) -0.0380(14) 0.0092(13) -0.0380(13) O18 0.0452(12) 0.0306(11) 0.0367(11) -0.0007(9) -0.0012(9) -0.0122(9) O20 0.0543(14) 0.0481(14) 0.0357(12) -0.0111(10) -0.0039(10) -0.0145(11) O25 0.0275(10) 0.0355(11) 0.0530(13) -0.0135(10) 0.0072(9) -0.0112(8) O27 0.0351(11) 0.0347(11) 0.0522(13) -0.0124(10) 0.0062(9) -0.0190(9) O43 0.0349(11) 0.0357(11) 0.0499(13) -0.0057(10) -0.0010(10) -0.0074(9) O46 0.0507(11) 0.0446(10) 0.0560(13) 0.0027(9) -0.0146(10) -0.0160(8) O49A 0.0507(11) 0.0446(10) 0.0560(13) 0.0027(9) -0.0146(10) -0.0160(8) O49B 0.0507(11) 0.0446(10) 0.0560(13) 0.0027(9) -0.0146(10) -0.0160(8) N100 0.085(3) 0.086(3) 0.057(2) 0.003(2) -0.004(2) -0.021(2) C101 0.064(3) 0.063(2) 0.056(2) -0.011(2) 0.008(2) -0.029(2) C102 0.051(2) 0.079(3) 0.068(3) -0.018(2) 0.001(2) -0.027(2) N200 0.133(4) 0.162(5) 0.093(3) -0.074(4) -0.012(3) -0.046(4) C201 0.085(3) 0.102(4) 0.064(3) -0.037(3) -0.010(2) -0.033(3) C202 0.076(3) 0.085(3) 0.071(3) -0.027(2) -0.008(2) -0.014(2) N300 0.104(4) 0.091(3) 0.087(3) -0.019(3) -0.014(3) -0.025(3) C301 0.077(3) 0.078(3) 0.058(3) 0.003(2) -0.018(2) -0.034(3) C302 0.065(3) 0.125(5) 0.077(3) 0.012(3) -0.005(3) -0.015(3) N400 0.118(3) 0.078(3) 0.052(2) -0.005(2) -0.021(2) -0.025(2) C401 0.067(2) 0.058(2) 0.047(2) -0.0128(19) -0.0092(18) -0.0117(19) C402 0.059(2) 0.062(2) 0.045(2) -0.0067(17) -0.0117(17) -0.0077(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.393(4) . ? C1 C6 1.409(4) . ? C1 C28 1.507(4) . ? C2 C3 1.387(4) . ? C3 C4 1.401(4) . ? C3 C7 1.515(4) . ? C4 O4 1.367(4) . ? C4 C5 1.388(4) . ? C5 C6 1.383(4) . ? C6 O6 1.371(3) . ? C7 C8 1.524(4) . ? C7 C29 1.534(4) . ? C8 C13 1.377(4) . ? C8 C9 1.391(4) . ? C9 C10 1.400(4) . ? C10 C11 1.383(4) . ? C10 C14 1.524(4) . ? C11 O11 1.380(4) . ? C11 C12 1.393(4) . ? C12 C13 1.393(5) . ? C13 O13 1.380(4) . ? C14 C15 1.521(4) . ? C14 C31 1.535(4) . ? C15 C16 1.387(4) . ? C15 C20 1.400(4) . ? C16 C17 1.388(4) . ? C17 C18 1.413(4) . ? C17 C21 1.520(4) . ? C18 O18 1.368(3) . ? C18 C19 1.383(4) . ? C19 C20 1.394(4) . ? C20 O20 1.367(4) . ? C21 C22 1.526(4) . ? C21 C33 1.546(4) . ? C22 C27 1.390(4) . ? C22 C23 1.397(4) . ? C23 C24 1.388(4) . ? C24 C25 1.389(4) . ? C24 C28 1.527(4) . ? C25 O25 1.374(3) . ? C25 C26 1.395(4) . ? C26 C27 1.388(4) . ? C27 O27 1.378(3) . ? C28 C35 1.538(4) . ? C29 C30 1.527(4) . ? C31 C32 1.525(4) . ? C33 C34 1.519(4) . ? C35 C36 1.532(4) . ? C37 O4 1.419(4) . ? C38 O11 1.415(4) . ? C39 O18 1.421(4) . ? C40 O25 1.414(4) . ? C41 O6 1.432(3) . ? C41 C42 1.489(5) . ? C42 O43 1.422(4) . ? C44 O43 1.419(4) . ? C44 C45 1.494(5) . ? C45 O46 1.422(4) . ? C47 O46 1.418(4) . ? C47 C48 1.471(6) . ? C48 O49B 1.237(9) . ? C48 O49A 1.459(6) . ? C50 O49A 1.391(5) . ? C50 C51 1.501(5) . ? C50 O49B 1.533(10) . ? C51 O27 1.422(4) . ? N100 C101 1.139(5) . ? C101 C102 1.462(6) . ? N200 C201 1.126(6) . ? C201 C202 1.437(6) . ? N300 C301 1.159(6) . ? C301 C302 1.434(8) . ? N400 C401 1.133(5) . ? C401 C402 1.448(5) . ? 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 C2 C1 C6 116.4(3) . . ? C2 C1 C28 124.3(3) . . ? C6 C1 C28 119.2(2) . . ? C3 C2 C1 124.2(3) . . ? C2 C3 C4 117.0(3) . . ? C2 C3 C7 124.8(3) . . ? C4 C3 C7 118.2(3) . . ? O4 C4 C5 123.3(3) . . ? O4 C4 C3 115.5(3) . . ? C5 C4 C3 121.2(3) . . ? C6 C5 C4 119.8(3) . . ? O6 C6 C5 123.2(3) . . ? O6 C6 C1 115.3(3) . . ? C5 C6 C1 121.5(3) . . ? C3 C7 C8 113.0(2) . . ? C3 C7 C29 114.6(3) . . ? C8 C7 C29 109.1(2) . . ? C13 C8 C9 117.2(3) . . ? C13 C8 C7 120.2(3) . . ? C9 C8 C7 122.3(3) . . ? C8 C9 C10 123.4(3) . . ? C11 C10 C9 117.2(3) . . ? C11 C10 C14 121.9(3) . . ? C9 C10 C14 120.5(3) . . ? O11 C11 C10 116.7(3) . . ? O11 C11 C12 122.2(3) . . ? C10 C11 C12 121.1(3) . . ? C13 C12 C11 119.5(3) . . ? C8 C13 O13 117.7(3) . . ? C8 C13 C12 121.5(3) . . ? O13 C13 C12 120.7(3) . . ? C15 C14 C10 112.8(2) . . ? C15 C14 C31 114.4(2) . . ? C10 C14 C31 108.9(2) . . ? C16 C15 C20 116.5(3) . . ? C16 C15 C14 124.4(3) . . ? C20 C15 C14 119.1(3) . . ? C15 C16 C17 125.0(3) . . ? C16 C17 C18 116.3(3) . . ? C16 C17 C21 124.9(3) . . ? C18 C17 C21 118.8(2) . . ? O18 C18 C19 123.5(3) . . ? O18 C18 C17 115.6(3) . . ? C19 C18 C17 120.9(3) . . ? C18 C19 C20 120.2(3) . . ? O20 C20 C19 121.2(3) . . ? O20 C20 C15 117.7(3) . . ? C19 C20 C15 121.1(3) . . ? C17 C21 C22 112.9(2) . . ? C17 C21 C33 114.2(2) . . ? C22 C21 C33 108.6(2) . . ? C27 C22 C23 117.3(2) . . ? C27 C22 C21 122.1(2) . . ? C23 C22 C21 120.3(2) . . ? C24 C23 C22 123.4(3) . . ? C23 C24 C25 117.3(2) . . ? C23 C24 C28 121.4(2) . . ? C25 C24 C28 121.1(2) . . ? O25 C25 C24 116.3(2) . . ? O25 C25 C26 122.6(3) . . ? C24 C25 C26 121.2(3) . . ? C27 C26 C25 119.7(3) . . ? O27 C27 C26 122.8(3) . . ? O27 C27 C22 116.2(2) . . ? C26 C27 C22 121.0(2) . . ? C1 C28 C24 112.9(2) . . ? C1 C28 C35 114.7(2) . . ? C24 C28 C35 108.2(2) . . ? C30 C29 C7 114.6(3) . . ? C32 C31 C14 114.6(3) . . ? C34 C33 C21 115.1(2) . . ? C36 C35 C28 115.0(2) . . ? O6 C41 C42 108.0(3) . . ? O43 C42 C41 110.0(2) . . ? O43 C44 C45 110.9(3) . . ? O46 C45 C44 110.6(3) . . ? O46 C47 C48 111.4(3) . . ? O49B C48 C47 126.6(6) . . ? O49A C48 C47 109.3(4) . . ? O49A C50 C51 118.5(3) . . ? C51 C50 O49B 95.7(5) . . ? O27 C51 C50 112.4(3) . . ? C4 O4 C37 118.4(2) . . ? C6 O6 C41 118.0(2) . . ? C11 O11 C38 118.3(2) . . ? C18 O18 C39 117.8(3) . . ? C25 O25 C40 117.9(2) . . ? C27 O27 C51 121.8(2) . . ? C44 O43 C42 111.4(2) . . ? C47 O46 C45 112.2(2) . . ? C50 O49A C48 112.8(4) . . ? C48 O49B C50 117.7(8) . . ? N100 C101 C102 179.0(5) . . ? N200 C201 C202 178.4(6) . . ? N300 C301 C302 178.4(6) . . ? N400 C401 C402 179.3(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 0.0(4) . . . . ? C28 C1 C2 C3 177.7(2) . . . . ? C1 C2 C3 C4 0.6(4) . . . . ? C1 C2 C3 C7 -176.8(2) . . . . ? C2 C3 C4 O4 177.4(2) . . . . ? C7 C3 C4 O4 -5.0(4) . . . . ? C2 C3 C4 C5 -1.3(4) . . . . ? C7 C3 C4 C5 176.3(2) . . . . ? O4 C4 C5 C6 -177.2(2) . . . . ? C3 C4 C5 C6 1.4(4) . . . . ? C4 C5 C6 O6 178.7(2) . . . . ? C4 C5 C6 C1 -0.8(4) . . . . ? C2 C1 C6 O6 -179.4(2) . . . . ? C28 C1 C6 O6 2.8(4) . . . . ? C2 C1 C6 C5 0.1(4) . . . . ? C28 C1 C6 C5 -177.7(2) . . . . ? C2 C3 C7 C8 -103.4(3) . . . . ? C4 C3 C7 C8 79.2(3) . . . . ? C2 C3 C7 C29 22.4(4) . . . . ? C4 C3 C7 C29 -154.9(2) . . . . ? C3 C7 C8 C13 -129.7(3) . . . . ? C29 C7 C8 C13 101.5(3) . . . . ? C3 C7 C8 C9 56.5(4) . . . . ? C29 C7 C8 C9 -72.3(3) . . . . ? C13 C8 C9 C10 0.1(4) . . . . ? C7 C8 C9 C10 174.1(3) . . . . ? C8 C9 C10 C11 0.6(4) . . . . ? C8 C9 C10 C14 -172.6(3) . . . . ? C9 C10 C11 O11 -178.3(3) . . . . ? C14 C10 C11 O11 -5.3(4) . . . . ? C9 C10 C11 C12 -0.3(5) . . . . ? C14 C10 C11 C12 172.8(3) . . . . ? O11 C11 C12 C13 177.2(3) . . . . ? C10 C11 C12 C13 -0.7(5) . . . . ? C9 C8 C13 O13 177.1(3) . . . . ? C7 C8 C13 O13 3.0(4) . . . . ? C9 C8 C13 C12 -1.2(5) . . . . ? C7 C8 C13 C12 -175.3(3) . . . . ? C11 C12 C13 C8 1.5(5) . . . . ? C11 C12 C13 O13 -176.8(3) . . . . ? C11 C10 C14 C15 131.9(3) . . . . ? C9 C10 C14 C15 -55.2(4) . . . . ? C11 C10 C14 C31 -100.0(3) . . . . ? C9 C10 C14 C31 72.8(3) . . . . ? C10 C14 C15 C16 100.4(3) . . . . ? C31 C14 C15 C16 -24.7(4) . . . . ? C10 C14 C15 C20 -80.3(3) . . . . ? C31 C14 C15 C20 154.5(3) . . . . ? C20 C15 C16 C17 -0.6(4) . . . . ? C14 C15 C16 C17 178.7(3) . . . . ? C15 C16 C17 C18 0.7(4) . . . . ? C15 C16 C17 C21 -178.6(2) . . . . ? C16 C17 C18 O18 178.5(2) . . . . ? C21 C17 C18 O18 -2.2(4) . . . . ? C16 C17 C18 C19 -1.1(4) . . . . ? C21 C17 C18 C19 178.3(2) . . . . ? O18 C18 C19 C20 -178.2(3) . . . . ? C17 C18 C19 C20 1.3(4) . . . . ? C18 C19 C20 O20 180.0(3) . . . . ? C18 C19 C20 C15 -1.1(4) . . . . ? C16 C15 C20 O20 179.7(2) . . . . ? C14 C15 C20 O20 0.4(4) . . . . ? C16 C15 C20 C19 0.7(4) . . . . ? C14 C15 C20 C19 -178.6(2) . . . . ? C16 C17 C21 C22 -106.1(3) . . . . ? C18 C17 C21 C22 74.5(3) . . . . ? C16 C17 C21 C33 18.7(4) . . . . ? C18 C17 C21 C33 -160.7(2) . . . . ? C17 C21 C22 C27 -127.3(3) . . . . ? C33 C21 C22 C27 104.9(3) . . . . ? C17 C21 C22 C23 59.3(3) . . . . ? C33 C21 C22 C23 -68.5(3) . . . . ? C27 C22 C23 C24 -3.1(4) . . . . ? C21 C22 C23 C24 170.6(3) . . . . ? C22 C23 C24 C25 0.9(4) . . . . ? C22 C23 C24 C28 -173.3(3) . . . . ? C23 C24 C25 O25 -176.8(2) . . . . ? C28 C24 C25 O25 -2.6(4) . . . . ? C23 C24 C25 C26 2.3(4) . . . . ? C28 C24 C25 C26 176.5(3) . . . . ? O25 C25 C26 C27 175.9(3) . . . . ? C24 C25 C26 C27 -3.2(4) . . . . ? C25 C26 C27 O27 -178.6(3) . . . . ? C25 C26 C27 C22 0.8(4) . . . . ? C23 C22 C27 O27 -178.3(2) . . . . ? C21 C22 C27 O27 8.1(4) . . . . ? C23 C22 C27 C26 2.2(4) . . . . ? C21 C22 C27 C26 -171.4(3) . . . . ? C2 C1 C28 C24 99.3(3) . . . . ? C6 C1 C28 C24 -83.1(3) . . . . ? C2 C1 C28 C35 -25.3(4) . . . . ? C6 C1 C28 C35 152.4(2) . . . . ? C23 C24 C28 C1 -53.2(3) . . . . ? C25 C24 C28 C1 132.9(3) . . . . ? C23 C24 C28 C35 74.8(3) . . . . ? C25 C24 C28 C35 -99.1(3) . . . . ? C3 C7 C29 C30 63.5(3) . . . . ? C8 C7 C29 C30 -168.6(3) . . . . ? C15 C14 C31 C32 -65.0(3) . . . . ? C10 C14 C31 C32 167.8(3) . . . . ? C17 C21 C33 C34 65.5(3) . . . . ? C22 C21 C33 C34 -167.4(3) . . . . ? C1 C28 C35 C36 -61.4(3) . . . . ? C24 C28 C35 C36 171.6(3) . . . . ? O6 C41 C42 O43 76.5(3) . . . . ? O43 C44 C45 O46 -74.5(4) . . . . ? O46 C47 C48 O49B 41.1(10) . . . . ? O46 C47 C48 O49A 74.5(4) . . . . ? O49A C50 C51 O27 69.4(5) . . . . ? O49B C50 C51 O27 93.0(6) . . . . ? C5 C4 O4 C37 -7.1(4) . . . . ? C3 C4 O4 C37 174.2(3) . . . . ? C5 C6 O6 C41 9.7(4) . . . . ? C1 C6 O6 C41 -170.9(2) . . . . ? C42 C41 O6 C6 171.7(2) . . . . ? C10 C11 O11 C38 -170.8(3) . . . . ? C12 C11 O11 C38 11.2(5) . . . . ? C19 C18 O18 C39 0.1(4) . . . . ? C17 C18 O18 C39 -179.5(3) . . . . ? C24 C25 O25 C40 176.9(3) . . . . ? C26 C25 O25 C40 -2.2(4) . . . . ? C26 C27 O27 C51 4.1(4) . . . . ? C22 C27 O27 C51 -175.3(3) . . . . ? C50 C51 O27 C27 -94.3(3) . . . . ? C45 C44 O43 C42 -175.0(3) . . . . ? C41 C42 O43 C44 -178.1(3) . . . . ? C48 C47 O46 C45 177.3(3) . . . . ? C44 C45 O46 C47 -175.7(3) . . . . ? C51 C50 O49A C48 100.0(4) . . . . ? O49B C50 O49A C48 51.2(7) . . . . ? O49B C48 O49A C50 -66.1(9) . . . . ? C47 C48 O49A C50 166.3(3) . . . . ? O49A C48 O49B C50 59.7(9) . . . . ? C47 C48 O49B C50 128.3(8) . . . . ? O49A C50 O49B C48 -73.1(11) . . . . ? C51 C50 O49B C48 148.6(10) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O13 H13 N200 1.00(4) 1.77(4) 2.744(5) 163(4) . O20 H20 N400 0.79(4) 2.04(4) 2.833(4) 175(4) 2_765 _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 66.83 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.344 _refine_diff_density_min -0.478 _refine_diff_density_rms 0.053 #===END