# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Yu Liu' _publ_contact_author_email YULIU@NANKAI.EDU.CN _publ_section_title ; Solid-state Supramolecular Architectures by p-Sulfonatocalix[5]arene with Bispyridinium Derivatives: Factors of Spacers and Terminal Groups ; loop_ _publ_author_name 'Yu Liu.' 'Dong-Sheng Guo.' 'Xin Su.' # Attachment 'revised_compound_4.cif' data_shelxl _database_code_depnum_ccdc_archive 'CCDC 728423' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C47 H56 N4 O26 S5' _chemical_formula_sum 'C47 H56 N4 O26 S5' _chemical_formula_weight 1253.26 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' S S 0.1246 0.1234 '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 'P 1 21/n 1' 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 11.4886(19) _cell_length_b 19.653(4) _cell_length_c 29.851(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.170(3) _cell_angle_gamma 90.00 _cell_volume 6654(2) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 16484 _cell_measurement_theta_min 1.2 _cell_measurement_theta_max 28.0 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.251 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2616 _exptl_absorpt_coefficient_mu 0.250 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9424 _exptl_absorpt_correction_T_max 0.9611 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 37529 _diffrn_reflns_av_R_equivalents 0.0535 _diffrn_reflns_av_sigmaI/netI 0.0599 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11636 _reflns_number_gt 8471 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.8' _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^)+(0.1423P)^2^+24.0761P] 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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0078(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 11636 _refine_ls_number_parameters 798 _refine_ls_number_restraints 114 _refine_ls_R_factor_all 0.1207 _refine_ls_R_factor_gt 0.1002 _refine_ls_wR_factor_ref 0.2875 _refine_ls_wR_factor_gt 0.2710 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.013 _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 S1 S 0.62745(12) 0.65845(7) 0.13337(4) 0.0305(3) Uani 1 1 d . . . S2 S 0.81809(17) 0.32496(8) 0.06913(5) 0.0473(5) Uani 1 1 d D . . S3 S 0.63587(14) -0.00828(7) 0.12830(5) 0.0400(4) Uani 1 1 d . . . S4 S 0.08316(12) 0.10845(8) 0.11935(5) 0.0371(4) Uani 1 1 d . . . S5 S 0.08775(12) 0.53387(10) 0.12067(5) 0.0493(5) Uani 1 1 d D . . O1 O 0.6399(3) 0.43560(18) 0.26661(12) 0.0324(8) Uani 1 1 d . . . H1A H 0.7035 0.4130 0.2682 0.049 Uiso 1 1 d R . . O2 O 0.8190(3) 0.32534(17) 0.26678(12) 0.0314(8) Uani 1 1 d . . . H2 H 0.7898 0.2871 0.2713 0.047 Uiso 1 1 d R . . O3 O 0.6429(3) 0.21010(18) 0.26381(12) 0.0323(8) Uani 1 1 d . A . H3G H 0.6350 0.1947 0.2898 0.048 Uiso 1 1 d R . . O4 O 0.3783(3) 0.2524(2) 0.26997(14) 0.0415(10) Uani 1 1 d . A . H4E H 0.4047 0.2892 0.2607 0.062 Uiso 1 1 d R . . O5 O 0.3692(4) 0.3882(2) 0.27443(14) 0.0448(10) Uani 1 1 d . A . H5 H 0.4208 0.4081 0.2923 0.067 Uiso 1 1 d R . . O6 O 0.6246(4) 0.7230(2) 0.15758(14) 0.0461(10) Uani 1 1 d . . . O7 O 0.7315(3) 0.65310(19) 0.11189(13) 0.0368(9) Uani 1 1 d . . . O8 O 0.5189(4) 0.6452(2) 0.10275(14) 0.0453(10) Uani 1 1 d . . . O9 O 0.8431(10) 0.3917(3) 0.0551(3) 0.056(2) Uani 0.698(14) 1 d PDU A 1 O10 O 0.8841(7) 0.2702(3) 0.0565(2) 0.055(3) Uani 0.698(14) 1 d PDU A 1 O11 O 0.6898(5) 0.3105(4) 0.0527(2) 0.064(3) Uani 0.698(14) 1 d PDU A 1 O9' O 0.7889(18) 0.3904(6) 0.0511(9) 0.070(8) Uani 0.302(14) 1 d PDU A 2 O10' O 0.9439(9) 0.3096(10) 0.0669(6) 0.075(6) Uani 0.302(14) 1 d PDU A 2 O11' O 0.7508(17) 0.2687(8) 0.0501(6) 0.083(7) Uani 0.302(14) 1 d PDU A 2 O12 O 0.7403(5) -0.0044(2) 0.10885(17) 0.0601(13) Uani 1 1 d . . . O13 O 0.6271(4) -0.0729(2) 0.15166(16) 0.0542(12) Uani 1 1 d . . . O14 O 0.5309(5) 0.0061(3) 0.09611(18) 0.0732(17) Uani 1 1 d . . . O15 O -0.0379(3) 0.1189(2) 0.12433(15) 0.0480(11) Uani 1 1 d . . . O16 O 0.1177(4) 0.0364(2) 0.12580(18) 0.0585(13) Uani 1 1 d . . . O17 O 0.1135(4) 0.1343(3) 0.07775(15) 0.0587(13) Uani 1 1 d . . . O18 O -0.0314(6) 0.5282(4) 0.1280(3) 0.030(2) Uani 0.574(13) 1 d PDU B 1 O19 O 0.1252(7) 0.6084(3) 0.1298(3) 0.058(3) Uani 0.574(13) 1 d PDU B 1 O20 O 0.1184(9) 0.5128(6) 0.0799(3) 0.071(3) Uani 0.574(13) 1 d PDU B 1 O18' O -0.0159(10) 0.5563(8) 0.1355(5) 0.047(4) Uani 0.426(13) 1 d PDU B 2 O19' O 0.1625(8) 0.5798(5) 0.1032(3) 0.043(3) Uani 0.426(13) 1 d PDU B 2 O20' O 0.0547(11) 0.4784(5) 0.0848(3) 0.058(4) Uani 0.426(13) 1 d PDU B 2 O21 O 0.9537(7) 0.7063(3) 0.1483(2) 0.095(2) Uani 1 1 d . . . O22 O 0.7783(9) 0.8237(4) 0.1335(3) 0.121(3) Uani 1 1 d . . . O23 O 0.9707(9) 0.9369(3) 0.1471(2) 0.132(4) Uani 1 1 d . . . O24 O 0.0366(8) 0.8179(5) 0.1233(3) 0.122(3) Uani 1 1 d . . . O25 O 0.2461(8) 0.8214(5) 0.1465(4) 0.142(3) Uani 1 1 d . . . O26 O 0.4852(9) 0.8236(5) 0.1149(4) 0.154(4) Uani 1 1 d . . . N1 N 0.4430(4) 0.3292(2) 0.13083(15) 0.0337(10) Uani 1 1 d . . . N2 N 0.4587(4) 0.4482(2) 0.06824(14) 0.0303(10) Uani 1 1 d . . . C1 C 0.6418(4) 0.4893(2) 0.23722(17) 0.0250(10) Uani 1 1 d . . . C2 C 0.5437(4) 0.5328(2) 0.22954(17) 0.0263(11) Uani 1 1 d . A . C3 C 0.5429(4) 0.5845(2) 0.19817(17) 0.0259(11) Uani 1 1 d . . . H3A H 0.4774 0.6145 0.1926 0.031 Uiso 1 1 calc R . . C4 C 0.6378(4) 0.5930(2) 0.17453(17) 0.0266(11) Uani 1 1 d . . . C5 C 0.7350(4) 0.5510(2) 0.18380(17) 0.0260(11) Uani 1 1 d . . . H5A H 0.8002 0.5580 0.1684 0.031 Uiso 1 1 calc R . . C6 C 0.7391(4) 0.4991(2) 0.21496(17) 0.0239(10) Uani 1 1 d . . . C7 C 0.8461(4) 0.4534(2) 0.22470(17) 0.0253(10) Uani 1 1 d . . . H7A H 0.8623 0.4436 0.2577 0.030 Uiso 1 1 calc R . . H7B H 0.9153 0.4778 0.2166 0.030 Uiso 1 1 calc R . . C8 C 0.8257(4) 0.3240(2) 0.22121(17) 0.0235(10) Uani 1 1 d . . . C9 C 0.8318(4) 0.3865(2) 0.19895(16) 0.0231(10) Uani 1 1 d . A . C10 C 0.8320(4) 0.3858(2) 0.15235(16) 0.0225(10) Uani 1 1 d . . . H10 H 0.8346 0.4276 0.1366 0.027 Uiso 1 1 calc R A . C11 C 0.8284(4) 0.3255(3) 0.12872(17) 0.0267(11) Uani 1 1 d . A . C12 C 0.8330(4) 0.2637(3) 0.15208(17) 0.0283(11) Uani 1 1 d . . . H12 H 0.8359 0.2221 0.1360 0.034 Uiso 1 1 calc R A . C13 C 0.8336(4) 0.2626(2) 0.19854(16) 0.0226(10) Uani 1 1 d . A . C14 C 0.8483(4) 0.1952(2) 0.22360(17) 0.0257(10) Uani 1 1 d . . . H14A H 0.8625 0.2041 0.2567 0.031 Uiso 1 1 calc R A . H14B H 0.9185 0.1716 0.2158 0.031 Uiso 1 1 calc R . . C15 C 0.6428(4) 0.1569(2) 0.23394(17) 0.0261(11) Uani 1 1 d . . . C16 C 0.7412(4) 0.1488(3) 0.21227(17) 0.0266(11) Uani 1 1 d . A . C17 C 0.7405(5) 0.0975(3) 0.18010(17) 0.0284(11) Uani 1 1 d . . . H17 H 0.8064 0.0914 0.1649 0.034 Uiso 1 1 calc R A . C18 C 0.6432(5) 0.0554(3) 0.17031(18) 0.0320(12) Uani 1 1 d . A . C19 C 0.5482(5) 0.0627(3) 0.19337(18) 0.0294(11) Uani 1 1 d . . . H19 H 0.4832 0.0324 0.1869 0.035 Uiso 1 1 calc R A . C20 C 0.5461(4) 0.1127(3) 0.22549(18) 0.0289(11) Uani 1 1 d . A . C21 C 0.4424(5) 0.1173(3) 0.25090(18) 0.0315(12) Uani 1 1 d . . . H21A H 0.4674 0.1414 0.2800 0.038 Uiso 1 1 calc R A . H21B H 0.4181 0.0707 0.2581 0.038 Uiso 1 1 calc R . . C22 C 0.3090(4) 0.2208(3) 0.23480(18) 0.0305(11) Uani 1 1 d . . . C23 C 0.3375(4) 0.1540(3) 0.22432(17) 0.0283(11) Uani 1 1 d . A . C24 C 0.2664(4) 0.1217(3) 0.18888(18) 0.0299(11) Uani 1 1 d . . . H24 H 0.2846 0.0763 0.1814 0.036 Uiso 1 1 calc R A . C25 C 0.1704(4) 0.1532(3) 0.16432(19) 0.0324(12) Uani 1 1 d . A . C26 C 0.1407(5) 0.2192(3) 0.17541(19) 0.0352(12) Uani 1 1 d . . . H26 H 0.0741 0.2407 0.1583 0.042 Uiso 1 1 calc R A . C27 C 0.2079(4) 0.2541(3) 0.21153(18) 0.0296(11) Uani 1 1 d . A . C28 C 0.1636(5) 0.3202(3) 0.2281(2) 0.0349(12) Uani 1 1 d . . . H28A H 0.1805 0.3194 0.2616 0.042 Uiso 1 1 calc R A . H28B H 0.0767 0.3203 0.2195 0.042 Uiso 1 1 calc R . . C29 C 0.3059(4) 0.4221(3) 0.23823(17) 0.0282(11) Uani 1 1 d . . . C30 C 0.2085(4) 0.3881(3) 0.21284(18) 0.0308(12) Uani 1 1 d . A . C31 C 0.1467(4) 0.4231(3) 0.17611(19) 0.0334(12) Uani 1 1 d . . . H31 H 0.0829 0.4009 0.1576 0.040 Uiso 1 1 calc R A . C32 C 0.1746(4) 0.4884(3) 0.16559(19) 0.0361(13) Uani 1 1 d . A . C33 C 0.2684(4) 0.5210(3) 0.19210(19) 0.0326(12) Uani 1 1 d . . . H33 H 0.2863 0.5667 0.1853 0.039 Uiso 1 1 calc R A . C34 C 0.3363(4) 0.4886(3) 0.22811(18) 0.0300(12) Uani 1 1 d . A . C35 C 0.4407(4) 0.5259(3) 0.25511(18) 0.0301(11) Uani 1 1 d . . . H35A H 0.4150 0.5718 0.2630 0.036 Uiso 1 1 calc R A . H35B H 0.4669 0.5010 0.2838 0.036 Uiso 1 1 calc R . . C36 C 0.3360(5) 0.3114(3) 0.1076(2) 0.0375(13) Uani 1 1 d . . . H36 H 0.2756 0.3448 0.1023 0.045 Uiso 1 1 calc R . . C37 C 0.3134(5) 0.2480(3) 0.0918(2) 0.0442(14) Uani 1 1 d . . . H37 H 0.2382 0.2374 0.0750 0.053 Uiso 1 1 calc R . . C38 C 0.4004(5) 0.1972(3) 0.10003(19) 0.0385(13) Uani 1 1 d . . . C39 C 0.5108(6) 0.2165(3) 0.1240(2) 0.0426(14) Uani 1 1 d . . . H39 H 0.5731 0.1843 0.1295 0.051 Uiso 1 1 calc R . . C40 C 0.5281(5) 0.2819(3) 0.1395(2) 0.0432(14) Uani 1 1 d . . . H40 H 0.6019 0.2941 0.1568 0.052 Uiso 1 1 calc R . . N3 N 0.3794(5) 0.1330(3) 0.08636(18) 0.0483(13) Uani 1 1 d . . . H3B H 0.4370 0.1189 0.0708 0.073 Uiso 1 1 calc R . . H3C H 0.3083 0.1307 0.0680 0.073 Uiso 1 1 calc R . . H3D H 0.3787 0.1058 0.1110 0.073 Uiso 1 1 calc R . . C41 C 0.4674(5) 0.3998(3) 0.14547(18) 0.0372(13) Uani 1 1 d . . . H41A H 0.5163 0.3999 0.1759 0.045 Uiso 1 1 calc R . . H41B H 0.3922 0.4231 0.1478 0.045 Uiso 1 1 calc R . . C42 C 0.5318(5) 0.4387(3) 0.11235(18) 0.0352(12) Uani 1 1 d . . . H42A H 0.5562 0.4837 0.1254 0.042 Uiso 1 1 calc R . . H42B H 0.6039 0.4134 0.1083 0.042 Uiso 1 1 calc R . . C43 C 0.3835(5) 0.5016(3) 0.0603(2) 0.0410(14) Uani 1 1 d . . . H43 H 0.3817 0.5344 0.0836 0.049 Uiso 1 1 calc R . . C44 C 0.3108(6) 0.5096(3) 0.0203(2) 0.0446(15) Uani 1 1 d . . . H44 H 0.2603 0.5481 0.0156 0.053 Uiso 1 1 calc R . . C45 C 0.3099(5) 0.4607(3) -0.01447(19) 0.0410(14) Uani 1 1 d . . . C46 C 0.3893(6) 0.4058(3) -0.0056(2) 0.0469(15) Uani 1 1 d . . . H46 H 0.3926 0.3721 -0.0282 0.056 Uiso 1 1 calc R . . C47 C 0.4606(5) 0.4010(3) 0.03482(19) 0.0414(14) Uani 1 1 d . . . H47 H 0.5136 0.3636 0.0402 0.050 Uiso 1 1 calc R . . N4 N 0.2382(5) 0.4664(3) -0.05410(17) 0.0528(14) Uani 1 1 d . . . H4A H 0.1980 0.5064 -0.0549 0.079 Uiso 1 1 calc R . . H4B H 0.1862 0.4311 -0.0574 0.079 Uiso 1 1 calc R . . H4C H 0.2815 0.4656 -0.0771 0.079 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 S1 0.0340(7) 0.0241(7) 0.0316(7) -0.0004(5) -0.0006(5) 0.0016(5) S2 0.0788(12) 0.0377(9) 0.0283(7) 0.0046(6) 0.0169(7) 0.0128(8) S3 0.0541(9) 0.0245(7) 0.0408(8) -0.0040(6) 0.0054(7) -0.0002(6) S4 0.0294(7) 0.0404(9) 0.0407(8) -0.0103(6) 0.0034(6) -0.0052(6) S5 0.0243(8) 0.0765(12) 0.0465(9) 0.0218(8) 0.0031(6) 0.0064(7) O1 0.036(2) 0.0234(19) 0.038(2) 0.0031(15) 0.0051(16) 0.0051(15) O2 0.047(2) 0.0248(19) 0.0229(18) 0.0025(14) 0.0061(16) 0.0003(16) O3 0.034(2) 0.029(2) 0.033(2) -0.0025(15) 0.0043(15) 0.0012(15) O4 0.039(2) 0.034(2) 0.046(2) 0.0017(18) -0.0117(18) -0.0088(17) O5 0.049(2) 0.045(2) 0.036(2) -0.0105(18) -0.0084(18) 0.0055(19) O6 0.067(3) 0.025(2) 0.045(2) 0.0006(18) 0.006(2) 0.0103(19) O7 0.039(2) 0.031(2) 0.042(2) 0.0019(17) 0.0109(17) -0.0021(16) O8 0.040(2) 0.057(3) 0.035(2) 0.0083(19) -0.0057(18) -0.0050(19) O9 0.091(7) 0.048(4) 0.028(3) 0.016(3) 0.008(4) 0.007(4) O10 0.087(5) 0.050(4) 0.031(3) 0.004(3) 0.021(3) 0.028(4) O11 0.047(4) 0.103(6) 0.036(3) -0.015(3) -0.009(3) 0.015(4) O9' 0.071(11) 0.068(10) 0.072(11) 0.011(7) 0.013(8) 0.009(8) O10' 0.105(11) 0.067(10) 0.055(9) -0.003(7) 0.020(8) 0.012(8) O11' 0.104(12) 0.075(10) 0.069(9) -0.001(7) 0.013(8) -0.020(8) O12 0.085(4) 0.043(3) 0.060(3) -0.020(2) 0.035(3) -0.016(2) O13 0.082(3) 0.023(2) 0.058(3) -0.0041(19) 0.015(2) -0.002(2) O14 0.092(4) 0.054(3) 0.061(3) -0.029(3) -0.026(3) 0.021(3) O15 0.028(2) 0.056(3) 0.058(3) -0.023(2) 0.0030(19) -0.0050(18) O16 0.046(3) 0.043(3) 0.081(3) -0.016(2) -0.007(2) 0.004(2) O17 0.049(3) 0.089(4) 0.039(2) -0.013(2) 0.007(2) -0.022(2) O18 0.020(3) 0.027(4) 0.042(4) -0.002(4) 0.003(3) 0.002(3) O19 0.036(4) 0.055(5) 0.078(6) 0.023(4) -0.002(4) -0.008(4) O20 0.062(6) 0.104(7) 0.052(5) 0.014(5) 0.029(4) 0.019(5) O18' 0.037(6) 0.056(8) 0.050(6) 0.002(6) 0.009(5) 0.021(5) O19' 0.045(5) 0.046(6) 0.039(5) -0.003(4) 0.004(4) -0.001(4) O20' 0.068(7) 0.053(6) 0.047(6) 0.004(5) -0.011(5) -0.009(5) O21 0.145(6) 0.073(4) 0.056(3) 0.016(3) -0.020(4) -0.013(4) O22 0.199(9) 0.086(5) 0.073(5) 0.001(4) 0.005(5) 0.036(5) O23 0.263(10) 0.072(4) 0.049(3) 0.003(3) -0.016(5) -0.061(5) O24 0.117(6) 0.152(8) 0.096(6) 0.014(5) 0.014(5) -0.037(5) O25 0.115(7) 0.164(9) 0.153(9) 0.005(6) 0.036(6) 0.005(6) O26 0.112(7) 0.145(8) 0.197(11) 0.001(7) 0.001(7) 0.003(5) N1 0.033(3) 0.042(3) 0.025(2) -0.0004(19) 0.0031(18) -0.005(2) N2 0.031(2) 0.031(2) 0.028(2) -0.0029(18) 0.0033(18) -0.0018(19) C1 0.023(2) 0.023(3) 0.027(2) -0.0025(19) -0.0007(19) -0.0016(19) C2 0.025(3) 0.024(3) 0.029(3) -0.010(2) 0.002(2) 0.000(2) C3 0.021(2) 0.025(3) 0.031(3) -0.008(2) -0.0008(19) 0.0004(19) C4 0.028(3) 0.021(3) 0.030(3) -0.005(2) 0.000(2) -0.003(2) C5 0.028(3) 0.021(2) 0.029(3) -0.008(2) 0.004(2) -0.005(2) C6 0.020(2) 0.017(2) 0.032(3) -0.0073(19) -0.0031(19) 0.0001(18) C7 0.017(2) 0.021(3) 0.036(3) -0.003(2) -0.0018(19) 0.0011(18) C8 0.014(2) 0.027(3) 0.030(3) 0.000(2) 0.0018(18) 0.0006(18) C9 0.015(2) 0.024(3) 0.029(2) -0.001(2) 0.0001(18) 0.0011(18) C10 0.014(2) 0.021(2) 0.033(3) 0.0041(19) 0.0033(18) 0.0025(18) C11 0.026(3) 0.028(3) 0.027(3) 0.001(2) 0.006(2) 0.008(2) C12 0.034(3) 0.023(3) 0.028(3) 0.001(2) 0.004(2) 0.004(2) C13 0.017(2) 0.025(3) 0.026(2) 0.0018(19) -0.0001(18) 0.0034(18) C14 0.023(2) 0.025(3) 0.029(3) 0.004(2) 0.002(2) 0.004(2) C15 0.029(3) 0.019(2) 0.030(3) 0.007(2) 0.001(2) 0.0017(19) C16 0.029(3) 0.023(3) 0.027(2) 0.006(2) 0.001(2) 0.002(2) C17 0.034(3) 0.023(3) 0.028(3) 0.004(2) 0.006(2) 0.008(2) C18 0.042(3) 0.021(3) 0.031(3) 0.006(2) 0.001(2) 0.003(2) C19 0.029(3) 0.023(3) 0.034(3) 0.006(2) -0.002(2) 0.000(2) C20 0.028(3) 0.024(3) 0.033(3) 0.008(2) 0.001(2) 0.003(2) C21 0.034(3) 0.027(3) 0.032(3) 0.005(2) 0.002(2) 0.001(2) C22 0.028(3) 0.030(3) 0.034(3) 0.001(2) 0.006(2) -0.005(2) C23 0.026(3) 0.028(3) 0.031(3) 0.003(2) 0.005(2) -0.004(2) C24 0.027(3) 0.028(3) 0.037(3) 0.002(2) 0.011(2) -0.002(2) C25 0.022(3) 0.040(3) 0.037(3) -0.004(2) 0.011(2) -0.001(2) C26 0.023(3) 0.042(3) 0.040(3) -0.002(2) 0.004(2) -0.001(2) C27 0.020(2) 0.031(3) 0.039(3) -0.002(2) 0.007(2) -0.004(2) C28 0.025(3) 0.037(3) 0.045(3) -0.004(2) 0.010(2) -0.002(2) C29 0.024(3) 0.029(3) 0.032(3) -0.005(2) 0.004(2) 0.009(2) C30 0.022(3) 0.034(3) 0.039(3) -0.008(2) 0.011(2) 0.002(2) C31 0.014(2) 0.046(3) 0.039(3) -0.007(2) 0.002(2) 0.002(2) C32 0.014(2) 0.053(4) 0.041(3) 0.008(3) 0.004(2) 0.007(2) C33 0.022(3) 0.034(3) 0.043(3) 0.003(2) 0.011(2) 0.003(2) C34 0.021(3) 0.036(3) 0.035(3) -0.007(2) 0.011(2) 0.005(2) C35 0.029(3) 0.030(3) 0.032(3) -0.006(2) 0.007(2) 0.004(2) C36 0.029(3) 0.041(3) 0.042(3) -0.005(3) 0.007(2) -0.006(2) C37 0.039(3) 0.048(4) 0.044(3) -0.001(3) 0.002(3) -0.009(3) C38 0.042(3) 0.040(3) 0.033(3) 0.006(2) 0.005(2) -0.006(3) C39 0.049(4) 0.038(3) 0.038(3) 0.008(3) -0.003(3) -0.002(3) C40 0.041(3) 0.051(4) 0.035(3) 0.010(3) -0.002(3) -0.003(3) N3 0.053(3) 0.048(3) 0.044(3) -0.004(2) 0.007(2) -0.010(3) C41 0.044(3) 0.042(3) 0.023(3) -0.006(2) 0.002(2) -0.002(3) C42 0.033(3) 0.039(3) 0.031(3) -0.002(2) -0.001(2) -0.005(2) C43 0.046(3) 0.039(3) 0.034(3) -0.008(2) -0.005(3) 0.003(3) C44 0.051(4) 0.036(3) 0.043(3) -0.002(3) -0.007(3) 0.010(3) C45 0.041(3) 0.051(4) 0.029(3) 0.000(3) 0.000(2) 0.009(3) C46 0.061(4) 0.051(4) 0.028(3) -0.003(3) 0.003(3) 0.019(3) C47 0.048(4) 0.044(3) 0.031(3) -0.004(3) 0.004(3) 0.010(3) N4 0.063(4) 0.059(4) 0.033(3) -0.002(2) -0.005(2) 0.020(3) _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 S1 O8 1.447(4) . ? S1 O7 1.448(4) . ? S1 O6 1.463(4) . ? S1 C4 1.769(5) . ? S2 O10 1.403(5) . ? S2 O9' 1.415(9) . ? S2 O11' 1.415(9) . ? S2 O9 1.421(6) . ? S2 O10' 1.488(9) . ? S2 O11 1.505(6) . ? S2 C11 1.764(5) . ? S3 O12 1.416(5) . ? S3 O14 1.445(5) . ? S3 O13 1.459(4) . ? S3 C18 1.763(5) . ? S4 O17 1.435(5) . ? S4 O15 1.437(4) . ? S4 O16 1.475(5) . ? S4 C25 1.775(6) . ? S5 O20 1.384(6) . ? S5 O19' 1.403(7) . ? S5 O18' 1.407(7) . ? S5 O18 1.425(6) . ? S5 O20' 1.533(7) . ? S5 O19 1.539(7) . ? S5 C32 1.780(6) . ? O1 C1 1.374(6) . ? O1 H1A 0.8500 . ? O2 C8 1.375(6) . ? O2 H2 0.8432 . ? O3 C15 1.375(6) . ? O3 H3G 0.8501 . ? O4 C22 1.362(6) . ? O4 H4E 0.8499 . ? O5 C29 1.375(6) . ? O5 H5 0.8295 . ? N1 C40 1.343(8) . ? N1 C36 1.357(7) . ? N1 C41 1.468(7) . ? N2 C43 1.355(7) . ? N2 C47 1.366(7) . ? N2 C42 1.456(7) . ? C1 C6 1.401(7) . ? C1 C2 1.404(7) . ? C2 C3 1.381(7) . ? C2 C35 1.513(7) . ? C3 C4 1.400(7) . ? C3 H3A 0.9500 . ? C4 C5 1.381(7) . ? C5 C6 1.376(7) . ? C5 H5A 0.9500 . ? C6 C7 1.513(6) . ? C7 C9 1.518(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C13 1.394(7) . ? C8 C9 1.403(7) . ? C9 C10 1.391(7) . ? C10 C11 1.377(7) . ? C10 H10 0.9500 . ? C11 C12 1.397(7) . ? C12 C13 1.386(7) . ? C12 H12 0.9500 . ? C13 C14 1.517(7) . ? C14 C16 1.526(7) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.397(7) . ? C15 C20 1.400(7) . ? C16 C17 1.392(7) . ? C17 C18 1.384(8) . ? C17 H17 0.9500 . ? C18 C19 1.387(8) . ? C19 C20 1.377(7) . ? C19 H19 0.9500 . ? C20 C21 1.513(7) . ? C21 C23 1.516(7) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.400(7) . ? C22 C27 1.415(7) . ? C23 C24 1.384(7) . ? C24 C25 1.372(8) . ? C24 H24 0.9500 . ? C25 C26 1.393(8) . ? C26 C27 1.402(8) . ? C26 H26 0.9500 . ? C27 C28 1.507(7) . ? C28 C30 1.525(7) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C34 1.397(8) . ? C29 C30 1.415(7) . ? C30 C31 1.389(8) . ? C31 C32 1.372(8) . ? C31 H31 0.9500 . ? C32 C33 1.388(8) . ? C33 C34 1.380(8) . ? C33 H33 0.9500 . ? C34 C35 1.523(7) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.343(8) . ? C36 H36 0.9500 . ? C37 C38 1.406(9) . ? C37 H37 0.9500 . ? C38 N3 1.335(8) . ? C38 C39 1.406(8) . ? C39 C40 1.369(9) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? N3 H3B 0.9100 . ? N3 H3C 0.9100 . ? N3 H3D 0.9100 . ? C41 C42 1.530(8) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.353(8) . ? C43 H43 0.9500 . ? C44 C45 1.413(8) . ? C44 H44 0.9500 . ? C45 N4 1.334(7) . ? C45 C46 1.411(8) . ? C46 C47 1.350(8) . ? C46 H46 0.9500 . ? C47 H47 0.9500 . ? N4 H4A 0.9100 . ? N4 H4B 0.9100 . ? N4 H4C 0.9100 . ? 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 O8 S1 O7 113.4(3) . . ? O8 S1 O6 112.5(3) . . ? O7 S1 O6 111.5(2) . . ? O8 S1 C4 105.3(2) . . ? O7 S1 C4 106.6(2) . . ? O6 S1 C4 106.9(2) . . ? O10 S2 O9' 134.5(11) . . ? O10 S2 O11' 64.9(9) . . ? O9' S2 O11' 118.4(10) . . ? O10 S2 O9 119.1(5) . . ? O9' S2 O9 25.1(8) . . ? O11' S2 O9 136.6(9) . . ? O10 S2 O10' 42.4(7) . . ? O9' S2 O10' 109.9(9) . . ? O11' S2 O10' 107.2(9) . . ? O9 S2 O10' 86.0(8) . . ? O10 S2 O11 108.1(4) . . ? O9' S2 O11 83.5(9) . . ? O11' S2 O11 43.7(8) . . ? O9 S2 O11 108.2(5) . . ? O10' S2 O11 148.8(8) . . ? O10 S2 C11 108.9(3) . . ? O9' S2 C11 110.6(12) . . ? O11' S2 C11 110.7(8) . . ? O9 S2 C11 107.9(4) . . ? O10' S2 C11 97.9(8) . . ? O11 S2 C11 103.6(3) . . ? O12 S3 O14 112.9(4) . . ? O12 S3 O13 111.7(3) . . ? O14 S3 O13 111.9(3) . . ? O12 S3 C18 107.9(3) . . ? O14 S3 C18 105.9(3) . . ? O13 S3 C18 106.0(3) . . ? O17 S4 O15 114.3(3) . . ? O17 S4 O16 110.8(3) . . ? O15 S4 O16 111.7(3) . . ? O17 S4 C25 107.0(3) . . ? O15 S4 C25 106.8(2) . . ? O16 S4 C25 105.6(3) . . ? O20 S5 O19' 67.0(6) . . ? O20 S5 O18' 136.0(7) . . ? O19' S5 O18' 121.0(7) . . ? O20 S5 O18 119.9(5) . . ? O19' S5 O18 140.1(6) . . ? O18' S5 O18 25.0(5) . . ? O20 S5 O20' 40.7(5) . . ? O19' S5 O20' 107.3(6) . . ? O18' S5 O20' 108.4(6) . . ? O18 S5 O20' 85.1(6) . . ? O20 S5 O19 109.7(5) . . ? O19' S5 O19 44.1(4) . . ? O18' S5 O19 82.7(6) . . ? O18 S5 O19 107.2(4) . . ? O20' S5 O19 146.3(5) . . ? O20 S5 C32 108.7(4) . . ? O19' S5 C32 107.5(4) . . ? O18' S5 C32 108.7(6) . . ? O18 S5 C32 106.4(4) . . ? O20' S5 C32 102.4(5) . . ? O19 S5 C32 103.7(4) . . ? C1 O1 H1A 109.6 . . ? C8 O2 H2 103.1 . . ? C15 O3 H3G 109.4 . . ? C22 O4 H4E 109.4 . . ? C29 O5 H5 120.8 . . ? C40 N1 C36 119.5(5) . . ? C40 N1 C41 119.8(5) . . ? C36 N1 C41 120.7(5) . . ? C43 N2 C47 118.9(5) . . ? C43 N2 C42 121.2(5) . . ? C47 N2 C42 119.9(5) . . ? O1 C1 C6 120.3(4) . . ? O1 C1 C2 118.5(4) . . ? C6 C1 C2 121.2(4) . . ? C3 C2 C1 118.5(4) . . ? C3 C2 C35 119.1(4) . . ? C1 C2 C35 122.4(5) . . ? C2 C3 C4 120.6(4) . . ? C2 C3 H3A 119.7 . . ? C4 C3 H3A 119.7 . . ? C5 C4 C3 119.8(5) . . ? C5 C4 S1 122.5(4) . . ? C3 C4 S1 117.8(4) . . ? C6 C5 C4 121.2(5) . . ? C6 C5 H5A 119.4 . . ? C4 C5 H5A 119.4 . . ? C5 C6 C1 118.6(4) . . ? C5 C6 C7 120.6(4) . . ? C1 C6 C7 120.8(4) . . ? C6 C7 C9 113.4(4) . . ? C6 C7 H7A 108.9 . . ? C9 C7 H7A 108.9 . . ? C6 C7 H7B 108.9 . . ? C9 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? O2 C8 C13 121.0(4) . . ? O2 C8 C9 117.8(4) . . ? C13 C8 C9 121.1(4) . . ? C10 C9 C8 118.2(4) . . ? C10 C9 C7 119.8(4) . . ? C8 C9 C7 121.8(4) . . ? C11 C10 C9 121.1(4) . . ? C11 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C10 C11 C12 119.8(5) . . ? C10 C11 S2 120.9(4) . . ? C12 C11 S2 119.3(4) . . ? C13 C12 C11 120.4(5) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C12 C13 C8 118.8(4) . . ? C12 C13 C14 119.3(4) . . ? C8 C13 C14 121.8(4) . . ? C13 C14 C16 113.0(4) . . ? C13 C14 H14A 109.0 . . ? C16 C14 H14A 109.0 . . ? C13 C14 H14B 109.0 . . ? C16 C14 H14B 109.0 . . ? H14A C14 H14B 107.8 . . ? O3 C15 C16 118.0(4) . . ? O3 C15 C20 120.4(4) . . ? C16 C15 C20 121.5(5) . . ? C17 C16 C15 119.0(5) . . ? C17 C16 C14 120.1(4) . . ? C15 C16 C14 120.8(4) . . ? C18 C17 C16 119.7(5) . . ? C18 C17 H17 120.2 . . ? C16 C17 H17 120.2 . . ? C17 C18 C19 120.4(5) . . ? C17 C18 S3 121.3(4) . . ? C19 C18 S3 118.3(4) . . ? C20 C19 C18 121.5(5) . . ? C20 C19 H19 119.3 . . ? C18 C19 H19 119.3 . . ? C19 C20 C15 117.8(5) . . ? C19 C20 C21 119.6(5) . . ? C15 C20 C21 122.6(5) . . ? C20 C21 C23 112.9(4) . . ? C20 C21 H21A 109.0 . . ? C23 C21 H21A 109.0 . . ? C20 C21 H21B 109.0 . . ? C23 C21 H21B 109.0 . . ? H21A C21 H21B 107.8 . . ? O4 C22 C23 118.1(5) . . ? O4 C22 C27 120.1(5) . . ? C23 C22 C27 121.8(5) . . ? C24 C23 C22 118.1(5) . . ? C24 C23 C21 120.3(5) . . ? C22 C23 C21 121.6(5) . . ? C25 C24 C23 121.8(5) . . ? C25 C24 H24 119.1 . . ? C23 C24 H24 119.1 . . ? C24 C25 C26 120.0(5) . . ? C24 C25 S4 119.3(4) . . ? C26 C25 S4 120.7(4) . . ? C25 C26 C27 120.9(5) . . ? C25 C26 H26 119.6 . . ? C27 C26 H26 119.6 . . ? C26 C27 C22 117.3(5) . . ? C26 C27 C28 120.1(5) . . ? C22 C27 C28 122.1(5) . . ? C27 C28 C30 120.6(4) . . ? C27 C28 H28A 107.2 . . ? C30 C28 H28A 107.2 . . ? C27 C28 H28B 107.2 . . ? C30 C28 H28B 107.2 . . ? H28A C28 H28B 106.8 . . ? O5 C29 C34 120.2(5) . . ? O5 C29 C30 117.8(5) . . ? C34 C29 C30 121.9(5) . . ? C31 C30 C29 116.8(5) . . ? C31 C30 C28 120.9(5) . . ? C29 C30 C28 122.0(5) . . ? C32 C31 C30 122.3(5) . . ? C32 C31 H31 118.8 . . ? C30 C31 H31 118.8 . . ? C31 C32 C33 119.4(5) . . ? C31 C32 S5 121.3(4) . . ? C33 C32 S5 119.3(5) . . ? C34 C33 C32 121.4(5) . . ? C34 C33 H33 119.3 . . ? C32 C33 H33 119.3 . . ? C33 C34 C29 118.1(5) . . ? C33 C34 C35 119.3(5) . . ? C29 C34 C35 122.6(5) . . ? C2 C35 C34 112.9(4) . . ? C2 C35 H35A 109.0 . . ? C34 C35 H35A 109.0 . . ? C2 C35 H35B 109.0 . . ? C34 C35 H35B 109.0 . . ? H35A C35 H35B 107.8 . . ? C37 C36 N1 121.8(6) . . ? C37 C36 H36 119.1 . . ? N1 C36 H36 119.1 . . ? C36 C37 C38 120.3(6) . . ? C36 C37 H37 119.8 . . ? C38 C37 H37 119.8 . . ? N3 C38 C39 121.0(6) . . ? N3 C38 C37 121.9(5) . . ? C39 C38 C37 117.1(6) . . ? C40 C39 C38 119.8(6) . . ? C40 C39 H39 120.1 . . ? C38 C39 H39 120.1 . . ? N1 C40 C39 121.4(6) . . ? N1 C40 H40 119.3 . . ? C39 C40 H40 119.3 . . ? C38 N3 H3B 109.5 . . ? C38 N3 H3C 109.5 . . ? H3B N3 H3C 109.5 . . ? C38 N3 H3D 109.5 . . ? H3B N3 H3D 109.5 . . ? H3C N3 H3D 109.5 . . ? N1 C41 C42 111.7(4) . . ? N1 C41 H41A 109.3 . . ? C42 C41 H41A 109.3 . . ? N1 C41 H41B 109.3 . . ? C42 C41 H41B 109.3 . . ? H41A C41 H41B 107.9 . . ? N2 C42 C41 112.4(4) . . ? N2 C42 H42A 109.1 . . ? C41 C42 H42A 109.1 . . ? N2 C42 H42B 109.1 . . ? C41 C42 H42B 109.1 . . ? H42A C42 H42B 107.9 . . ? C44 C43 N2 122.1(5) . . ? C44 C43 H43 119.0 . . ? N2 C43 H43 119.0 . . ? C43 C44 C45 120.0(6) . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? N4 C45 C46 121.3(6) . . ? N4 C45 C44 121.7(6) . . ? C46 C45 C44 117.0(5) . . ? C47 C46 C45 120.3(6) . . ? C47 C46 H46 119.9 . . ? C45 C46 H46 119.9 . . ? C46 C47 N2 121.8(6) . . ? C46 C47 H47 119.1 . . ? N2 C47 H47 119.1 . . ? C45 N4 H4A 109.5 . . ? C45 N4 H4B 109.5 . . ? H4A N4 H4B 109.5 . . ? C45 N4 H4C 109.5 . . ? H4A N4 H4C 109.5 . . ? H4B N4 H4C 109.5 . . ? 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 O1 C1 C2 C3 -176.5(4) . . . . ? C6 C1 C2 C3 2.3(7) . . . . ? O1 C1 C2 C35 4.9(7) . . . . ? C6 C1 C2 C35 -176.3(4) . . . . ? C1 C2 C3 C4 0.2(7) . . . . ? C35 C2 C3 C4 178.8(4) . . . . ? C2 C3 C4 C5 -2.3(7) . . . . ? C2 C3 C4 S1 177.6(4) . . . . ? O8 S1 C4 C5 124.8(4) . . . . ? O7 S1 C4 C5 4.1(5) . . . . ? O6 S1 C4 C5 -115.3(4) . . . . ? O8 S1 C4 C3 -55.1(4) . . . . ? O7 S1 C4 C3 -175.8(4) . . . . ? O6 S1 C4 C3 64.7(4) . . . . ? C3 C4 C5 C6 2.1(7) . . . . ? S1 C4 C5 C6 -177.9(4) . . . . ? C4 C5 C6 C1 0.3(7) . . . . ? C4 C5 C6 C7 179.9(4) . . . . ? O1 C1 C6 C5 176.3(4) . . . . ? C2 C1 C6 C5 -2.5(7) . . . . ? O1 C1 C6 C7 -3.3(7) . . . . ? C2 C1 C6 C7 177.9(4) . . . . ? C5 C6 C7 C9 -97.8(5) . . . . ? C1 C6 C7 C9 81.7(6) . . . . ? O2 C8 C9 C10 -176.5(4) . . . . ? C13 C8 C9 C10 7.4(7) . . . . ? O2 C8 C9 C7 7.6(6) . . . . ? C13 C8 C9 C7 -168.5(4) . . . . ? C6 C7 C9 C10 71.5(6) . . . . ? C6 C7 C9 C8 -112.7(5) . . . . ? C8 C9 C10 C11 -1.1(7) . . . . ? C7 C9 C10 C11 174.9(4) . . . . ? C9 C10 C11 C12 -4.6(7) . . . . ? C9 C10 C11 S2 175.5(4) . . . . ? O10 S2 C11 C10 144.3(5) . . . . ? O9' S2 C11 C10 -12.8(10) . . . . ? O11' S2 C11 C10 -146.2(11) . . . . ? O9 S2 C11 C10 13.7(6) . . . . ? O10' S2 C11 C10 102.0(9) . . . . ? O11 S2 C11 C10 -100.9(5) . . . . ? O10 S2 C11 C12 -35.6(6) . . . . ? O9' S2 C11 C12 167.3(10) . . . . ? O11' S2 C11 C12 33.9(11) . . . . ? O9 S2 C11 C12 -166.2(6) . . . . ? O10' S2 C11 C12 -77.9(9) . . . . ? O11 S2 C11 C12 79.2(5) . . . . ? C10 C11 C12 C13 4.2(7) . . . . ? S2 C11 C12 C13 -175.9(4) . . . . ? C11 C12 C13 C8 1.9(7) . . . . ? C11 C12 C13 C14 -175.3(4) . . . . ? O2 C8 C13 C12 176.2(4) . . . . ? C9 C8 C13 C12 -7.8(7) . . . . ? O2 C8 C13 C14 -6.7(7) . . . . ? C9 C8 C13 C14 169.3(4) . . . . ? C12 C13 C14 C16 -69.7(6) . . . . ? C8 C13 C14 C16 113.2(5) . . . . ? O3 C15 C16 C17 -176.6(4) . . . . ? C20 C15 C16 C17 2.8(7) . . . . ? O3 C15 C16 C14 3.5(7) . . . . ? C20 C15 C16 C14 -177.0(4) . . . . ? C13 C14 C16 C17 97.8(5) . . . . ? C13 C14 C16 C15 -82.3(6) . . . . ? C15 C16 C17 C18 -0.3(7) . . . . ? C14 C16 C17 C18 179.6(4) . . . . ? C16 C17 C18 C19 -2.0(7) . . . . ? C16 C17 C18 S3 177.6(4) . . . . ? O12 S3 C18 C17 -1.4(5) . . . . ? O14 S3 C18 C17 -122.5(5) . . . . ? O13 S3 C18 C17 118.4(5) . . . . ? O12 S3 C18 C19 178.3(4) . . . . ? O14 S3 C18 C19 57.1(5) . . . . ? O13 S3 C18 C19 -61.9(5) . . . . ? C17 C18 C19 C20 1.9(8) . . . . ? S3 C18 C19 C20 -177.8(4) . . . . ? C18 C19 C20 C15 0.6(7) . . . . ? C18 C19 C20 C21 -178.0(4) . . . . ? O3 C15 C20 C19 176.5(4) . . . . ? C16 C15 C20 C19 -3.0(7) . . . . ? O3 C15 C20 C21 -5.0(7) . . . . ? C16 C15 C20 C21 175.6(4) . . . . ? C19 C20 C21 C23 -81.7(6) . . . . ? C15 C20 C21 C23 99.7(6) . . . . ? O4 C22 C23 C24 179.3(5) . . . . ? C27 C22 C23 C24 2.7(7) . . . . ? O4 C22 C23 C21 -0.3(7) . . . . ? C27 C22 C23 C21 -176.9(5) . . . . ? C20 C21 C23 C24 76.1(6) . . . . ? C20 C21 C23 C22 -104.3(6) . . . . ? C22 C23 C24 C25 0.0(7) . . . . ? C21 C23 C24 C25 179.6(5) . . . . ? C23 C24 C25 C26 -1.3(8) . . . . ? C23 C24 C25 S4 -179.9(4) . . . . ? O17 S4 C25 C24 -103.5(5) . . . . ? O15 S4 C25 C24 133.8(4) . . . . ? O16 S4 C25 C24 14.7(5) . . . . ? O17 S4 C25 C26 77.9(5) . . . . ? O15 S4 C25 C26 -44.9(5) . . . . ? O16 S4 C25 C26 -163.9(5) . . . . ? C24 C25 C26 C27 0.0(8) . . . . ? S4 C25 C26 C27 178.6(4) . . . . ? C25 C26 C27 C22 2.5(8) . . . . ? C25 C26 C27 C28 -169.7(5) . . . . ? O4 C22 C27 C26 179.5(5) . . . . ? C23 C22 C27 C26 -3.9(7) . . . . ? O4 C22 C27 C28 -8.4(7) . . . . ? C23 C22 C27 C28 168.2(5) . . . . ? C26 C27 C28 C30 -98.9(6) . . . . ? C22 C27 C28 C30 89.2(7) . . . . ? O5 C29 C30 C31 -179.3(4) . . . . ? C34 C29 C30 C31 2.4(7) . . . . ? O5 C29 C30 C28 8.0(7) . . . . ? C34 C29 C30 C28 -170.3(5) . . . . ? C27 C28 C30 C31 94.9(6) . . . . ? C27 C28 C30 C29 -92.7(6) . . . . ? C29 C30 C31 C32 -2.6(7) . . . . ? C28 C30 C31 C32 170.2(5) . . . . ? C30 C31 C32 C33 0.6(8) . . . . ? C30 C31 C32 S5 -175.7(4) . . . . ? O20 S5 C32 C31 -79.7(7) . . . . ? O19' S5 C32 C31 -150.7(6) . . . . ? O18' S5 C32 C31 76.7(8) . . . . ? O18 S5 C32 C31 50.6(6) . . . . ? O20' S5 C32 C31 -37.9(7) . . . . ? O19 S5 C32 C31 163.6(6) . . . . ? O20 S5 C32 C33 104.0(7) . . . . ? O19' S5 C32 C33 33.0(7) . . . . ? O18' S5 C32 C33 -99.5(8) . . . . ? O18 S5 C32 C33 -125.6(5) . . . . ? O20' S5 C32 C33 145.8(7) . . . . ? O19 S5 C32 C33 -12.7(6) . . . . ? C31 C32 C33 C34 1.8(8) . . . . ? S5 C32 C33 C34 178.1(4) . . . . ? C32 C33 C34 C29 -1.9(7) . . . . ? C32 C33 C34 C35 177.9(5) . . . . ? O5 C29 C34 C33 -178.5(4) . . . . ? C30 C29 C34 C33 -0.2(7) . . . . ? O5 C29 C34 C35 1.6(7) . . . . ? C30 C29 C34 C35 180.0(4) . . . . ? C3 C2 C35 C34 81.9(6) . . . . ? C1 C2 C35 C34 -99.6(6) . . . . ? C33 C34 C35 C2 -73.0(6) . . . . ? C29 C34 C35 C2 106.9(5) . . . . ? C40 N1 C36 C37 -1.8(8) . . . . ? C41 N1 C36 C37 176.6(5) . . . . ? N1 C36 C37 C38 1.5(9) . . . . ? C36 C37 C38 N3 177.4(6) . . . . ? C36 C37 C38 C39 -1.6(9) . . . . ? N3 C38 C39 C40 -176.9(6) . . . . ? C37 C38 C39 C40 2.1(9) . . . . ? C36 N1 C40 C39 2.3(8) . . . . ? C41 N1 C40 C39 -176.1(5) . . . . ? C38 C39 C40 N1 -2.5(9) . . . . ? C40 N1 C41 C42 81.1(6) . . . . ? C36 N1 C41 C42 -97.2(6) . . . . ? C43 N2 C42 C41 85.8(6) . . . . ? C47 N2 C42 C41 -90.6(6) . . . . ? N1 C41 C42 N2 66.5(6) . . . . ? C47 N2 C43 C44 -0.3(9) . . . . ? C42 N2 C43 C44 -176.8(6) . . . . ? N2 C43 C44 C45 1.4(10) . . . . ? C43 C44 C45 N4 179.0(6) . . . . ? C43 C44 C45 C46 -1.6(10) . . . . ? N4 C45 C46 C47 -179.7(7) . . . . ? C44 C45 C46 C47 1.0(10) . . . . ? C45 C46 C47 N2 0.0(10) . . . . ? C43 N2 C47 C46 -0.4(9) . . . . ? C42 N2 C47 C46 176.1(6) . . . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.011 0.000 0.000 757 126 ' ' 2 -0.015 0.500 0.500 757 126 ' ' 3 0.132 0.212 0.316 17 3 ' ' 4 0.367 0.712 0.184 18 3 ' ' 5 0.632 0.288 0.816 17 3 ' ' 6 0.867 0.788 0.684 18 3 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.388 _refine_diff_density_min -0.850 _refine_diff_density_rms 0.115 # Attachment 'revised_compound_3.cif' data_060208c _database_code_depnum_ccdc_archive 'CCDC 728424' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H88 N2 O46 S10' _chemical_formula_weight 2182.16 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 31.666(5) _cell_length_b 19.154(3) _cell_length_c 22.704(4) _cell_angle_alpha 90.00 _cell_angle_beta 111.471(3) _cell_angle_gamma 90.00 _cell_volume 12816(4) _cell_formula_units_Z 4 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 6573 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 26.39 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.131 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4536 _exptl_absorpt_coefficient_mu 0.246 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.645891 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 34434 _diffrn_reflns_av_R_equivalents 0.0624 _diffrn_reflns_av_sigmaI/netI 0.0965 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 26.51 _reflns_number_total 13180 _reflns_number_gt 4274 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1364P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13180 _refine_ls_number_parameters 710 _refine_ls_number_restraints 164 _refine_ls_R_factor_all 0.1942 _refine_ls_R_factor_gt 0.0810 _refine_ls_wR_factor_ref 0.2588 _refine_ls_wR_factor_gt 0.2109 _refine_ls_goodness_of_fit_ref 0.854 _refine_ls_restrained_S_all 0.872 _refine_ls_shift/su_max 0.008 _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 S1 S 0.11854(7) 0.73191(13) 0.50500(10) 0.1280(7) Uani 1 1 d D . . S2 S 0.11725(5) 0.32827(9) 0.47825(7) 0.0951(5) Uani 1 1 d D . . S3 S 0.15679(7) 0.13549(9) 0.27718(10) 0.1164(6) Uani 1 1 d D . . S4 S 0.05696(5) 0.48328(9) 0.13576(7) 0.0935(5) Uani 1 1 d D . . S5 S 0.12006(8) 0.84566(11) 0.19938(11) 0.1323(7) Uani 1 1 d D . . O1 O 0.26796(12) 0.59724(17) 0.45229(14) 0.0927(10) Uani 1 1 d . A . H1C H 0.2708 0.5550 0.4645 0.139 Uiso 1 1 d R . . O2 O 0.0997(11) 0.7882(16) 0.4632(15) 0.302(16) Uani 0.50 1 d PD A 1 O3 O 0.0836(6) 0.6813(10) 0.4843(17) 0.323(14) Uani 0.50 1 d PD A 1 O4 O 0.1332(7) 0.7419(15) 0.5712(4) 0.230(9) Uani 0.50 1 d PD A 1 O2' O 0.0804(3) 0.7294(9) 0.4467(5) 0.137(4) Uani 0.50 1 d PD A 2 O3' O 0.1039(4) 0.6858(6) 0.5413(7) 0.128(4) Uani 0.50 1 d PD A 2 O4' O 0.1329(6) 0.8020(6) 0.5206(13) 0.218(11) Uani 0.50 1 d PD A 2 O5 O 0.28723(12) 0.45783(19) 0.48455(16) 0.1036(11) Uani 1 1 d . A . H5C H 0.3042 0.4651 0.5229 0.155 Uiso 1 1 d R . . O6 O 0.08148(15) 0.3793(3) 0.4480(2) 0.1514(17) Uani 1 1 d D . . O7 O 0.12010(14) 0.3139(3) 0.53966(17) 0.164(2) Uani 1 1 d D . . O8 O 0.10761(18) 0.2722(3) 0.4356(3) 0.185(2) Uani 1 1 d D . . O9 O 0.26280(11) 0.39428(17) 0.32237(14) 0.0845(9) Uani 1 1 d . A . H9A H 0.2602 0.4146 0.2879 0.127 Uiso 1 1 d R . . O10 O 0.1122(3) 0.1589(5) 0.2524(6) 0.139(3) Uani 0.50 1 d PDU B 1 O11 O 0.1679(4) 0.1060(5) 0.3423(3) 0.127(3) Uani 0.50 1 d PDU B 1 O12 O 0.1757(3) 0.0886(4) 0.2446(4) 0.099(2) Uani 0.50 1 d PDU B 1 O10' O 0.1230(3) 0.1467(6) 0.3035(6) 0.134(3) Uani 0.50 1 d PDU B 2 O11' O 0.1834(3) 0.0754(4) 0.3026(6) 0.129(3) Uani 0.50 1 d PDU B 2 O12' O 0.1325(4) 0.1258(5) 0.2086(4) 0.147(3) Uani 0.50 1 d PDU B 2 O13 O 0.25586(10) 0.48534(15) 0.21496(14) 0.0767(8) Uani 1 1 d . A . H13A H 0.2655 0.5210 0.2015 0.115 Uiso 1 1 d R . . O14 O 0.04454(15) 0.4156(3) 0.1493(3) 0.167(2) Uani 1 1 d D . . O15 O 0.03712(13) 0.4972(3) 0.07005(17) 0.1558(19) Uani 1 1 d D . . O16 O 0.04585(15) 0.5333(3) 0.1737(3) 0.176(2) Uani 1 1 d D . . O17 O 0.24780(11) 0.61904(17) 0.31468(13) 0.0853(9) Uani 1 1 d . A . H17C H 0.2686 0.6190 0.2993 0.128 Uiso 1 1 d R . . O18 O 0.0801(4) 0.8182(7) 0.2057(9) 0.190(5) Uani 0.50 1 d PDU C 1 O19 O 0.1159(3) 0.8513(5) 0.1334(3) 0.130(3) Uani 0.50 1 d PDU C 1 O20 O 0.1341(7) 0.9052(7) 0.2389(8) 0.219(7) Uani 0.50 1 d PDU C 1 O18' O 0.0978(5) 0.8617(8) 0.2425(6) 0.166(4) Uani 0.50 1 d PDU C 2 O19' O 0.0857(5) 0.8185(7) 0.1440(7) 0.200(5) Uani 0.50 1 d PDU C 2 O20' O 0.1475(4) 0.9090(5) 0.2089(7) 0.156(4) Uani 0.50 1 d PDU C 2 C1 C 0.23984(18) 0.7277(2) 0.39878(19) 0.0854(15) Uani 1 1 d . . . H1A H 0.2451 0.7760 0.4124 0.102 Uiso 1 1 calc R . . H1B H 0.2692 0.7062 0.4070 0.102 Uiso 1 1 calc R . . C2 C 0.21670(17) 0.6906(3) 0.43793(19) 0.0728(13) Uani 1 1 d . A . C3 C 0.18173(19) 0.7212(3) 0.4498(2) 0.0888(15) Uani 1 1 d . . . H3 H 0.1709 0.7644 0.4320 0.107 Uiso 1 1 calc R A . C4 C 0.16222(18) 0.6888(3) 0.4882(2) 0.0864(15) Uani 1 1 d . A . C5 C 0.18010(17) 0.6265(3) 0.5176(2) 0.0787(13) Uani 1 1 d . . . H5 H 0.1676 0.6058 0.5445 0.094 Uiso 1 1 calc R A . C6 C 0.21592(17) 0.5942(2) 0.50804(19) 0.0720(12) Uani 1 1 d . A . C7 C 0.23356(17) 0.6267(3) 0.46626(19) 0.0745(13) Uani 1 1 d . . . C8 C 0.23700(19) 0.5294(3) 0.5449(2) 0.0898(15) Uani 1 1 d . . . H8A H 0.2697 0.5328 0.5572 0.108 Uiso 1 1 calc R A . H8B H 0.2305 0.5289 0.5835 0.108 Uiso 1 1 calc R . . C9 C 0.22192(18) 0.4608(2) 0.51171(19) 0.0740(13) Uani 1 1 d . A . C10 C 0.18227(18) 0.4304(3) 0.51020(19) 0.0824(14) Uani 1 1 d . . . H10 H 0.1645 0.4531 0.5290 0.099 Uiso 1 1 calc R A . C11 C 0.16821(16) 0.3661(3) 0.48090(19) 0.0748(13) Uani 1 1 d . A . C12 C 0.19584(18) 0.3316(2) 0.4542(2) 0.0798(14) Uani 1 1 d . . . H12 H 0.1865 0.2885 0.4348 0.096 Uiso 1 1 calc R A . C13 C 0.23665(17) 0.3594(3) 0.4555(2) 0.0743(13) Uani 1 1 d . A . C14 C 0.24858(18) 0.4240(3) 0.4838(2) 0.0791(13) Uani 1 1 d . . . C15 C 0.26560(17) 0.3185(3) 0.4272(2) 0.0849(15) Uani 1 1 d . . . H15A H 0.2907 0.3476 0.4271 0.102 Uiso 1 1 calc R A . H15B H 0.2783 0.2782 0.4537 0.102 Uiso 1 1 calc R . . C16 C 0.23957(16) 0.2944(3) 0.3611(2) 0.0732(13) Uani 1 1 d . A . C17 C 0.21509(19) 0.2319(3) 0.3489(3) 0.0892(16) Uani 1 1 d . . . H17 H 0.2164 0.2037 0.3829 0.107 Uiso 1 1 calc R A . C18 C 0.18903(18) 0.2104(2) 0.2885(3) 0.0829(14) Uani 1 1 d . A . C19 C 0.18940(17) 0.2520(2) 0.2378(2) 0.0799(14) Uani 1 1 d . . . H19 H 0.1728 0.2375 0.1968 0.096 Uiso 1 1 calc R A . C20 C 0.21348(16) 0.3137(2) 0.2466(2) 0.0691(12) Uani 1 1 d . A . C21 C 0.23834(16) 0.3338(2) 0.3086(2) 0.0700(12) Uani 1 1 d . . . C22 C 0.21311(16) 0.3554(2) 0.1914(2) 0.0740(12) Uani 1 1 d . . . H22A H 0.1995 0.3278 0.1534 0.089 Uiso 1 1 calc R A . H22B H 0.2442 0.3654 0.1960 0.089 Uiso 1 1 calc R . . C23 C 0.18711(17) 0.4247(2) 0.18339(17) 0.0636(12) Uani 1 1 d . A . C24 C 0.14004(16) 0.4245(2) 0.16516(17) 0.0654(11) Uani 1 1 d . . . H24 H 0.1247 0.3821 0.1588 0.079 Uiso 1 1 calc R A . C25 C 0.11609(15) 0.4853(3) 0.15648(18) 0.0645(11) Uani 1 1 d . A . C26 C 0.13878(17) 0.5480(2) 0.16320(17) 0.0651(11) Uani 1 1 d . . . H26 H 0.1222 0.5892 0.1559 0.078 Uiso 1 1 calc R A . C27 C 0.18531(16) 0.5516(2) 0.18040(16) 0.0574(10) Uani 1 1 d . A . C28 C 0.20982(16) 0.4886(2) 0.19336(17) 0.0587(11) Uani 1 1 d . . . C29 C 0.20849(16) 0.6209(2) 0.1830(2) 0.0713(12) Uani 1 1 d . . . H29A H 0.1997 0.6392 0.1404 0.086 Uiso 1 1 calc R A . H29B H 0.2410 0.6135 0.1989 0.086 Uiso 1 1 calc R . . C30 C 0.19756(15) 0.6748(2) 0.22408(19) 0.0618(11) Uani 1 1 d . A . C31 C 0.16783(17) 0.7283(2) 0.1974(2) 0.0781(13) Uani 1 1 d . . . H31 H 0.1532 0.7300 0.1537 0.094 Uiso 1 1 calc R A . C32 C 0.15912(16) 0.7797(2) 0.2344(2) 0.0748(13) Uani 1 1 d . A . C33 C 0.18281(18) 0.7780(2) 0.2998(2) 0.0792(14) Uani 1 1 d . . . H33 H 0.1780 0.8133 0.3247 0.095 Uiso 1 1 calc R A . C34 C 0.21286(17) 0.7260(2) 0.32802(19) 0.0698(12) Uani 1 1 d . A . C35 C 0.21933(15) 0.6740(2) 0.28995(19) 0.0629(11) Uani 1 1 d . . . C36 C 0.1613(2) 0.5112(5) 0.3367(3) 0.189(4) Uani 1 1 d D . . H36A H 0.1504 0.5582 0.3353 0.284 Uiso 1 1 calc R . . H36B H 0.1752 0.5059 0.3058 0.284 Uiso 1 1 calc R . . H36C H 0.1833 0.5017 0.3781 0.284 Uiso 1 1 calc R . . C37 C 0.12338(15) 0.4623(3) 0.32277(18) 0.146(3) Uani 1 1 d GD . . C38 C 0.08269(19) 0.4828(2) 0.32773(19) 0.138(3) Uani 1 1 d GD . . H38 H 0.0792 0.5282 0.3396 0.166 Uiso 1 1 calc R . . C39 C 0.04728(14) 0.4352(3) 0.31501(18) 0.128(2) Uani 1 1 d G . . H39 H 0.0201 0.4489 0.3183 0.154 Uiso 1 1 calc R . . N1 N 0.05256(15) 0.3673(3) 0.29732(17) 0.1247(17) Uani 1 1 d G . . C40 C 0.09325(19) 0.3469(2) 0.29235(18) 0.153(3) Uani 1 1 d G . . H40 H 0.0968 0.3014 0.2805 0.183 Uiso 1 1 calc R . . C41 C 0.12866(14) 0.3944(3) 0.30508(19) 0.189(5) Uani 1 1 d GD . . H41 H 0.1559 0.3807 0.3018 0.227 Uiso 1 1 calc R . . C42 C 0.0150(3) 0.3172(4) 0.2842(3) 0.170(3) Uani 1 1 d . . . H42A H -0.0028 0.3290 0.3096 0.203 Uiso 1 1 calc R . . H42B H 0.0273 0.2707 0.2962 0.203 Uiso 1 1 calc R . . O21 O 0.07376(17) 0.4955(3) 0.9891(2) 0.178(2) Uani 1 1 d . . . O22 O 0.1473(2) 0.9654(3) 0.3429(3) 0.208(2) Uani 1 1 d . . . O23 O 0.0419(3) 0.5924(4) 0.4099(4) 0.249(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.1133(15) 0.1553(19) 0.1261(15) 0.0233(15) 0.0564(13) 0.0215(14) S2 0.1053(12) 0.1113(11) 0.0772(9) -0.0115(9) 0.0434(8) -0.0165(10) S3 0.1343(16) 0.0959(12) 0.1450(16) -0.0106(12) 0.0821(14) -0.0192(12) S4 0.0719(9) 0.1234(12) 0.0820(9) 0.0093(9) 0.0245(8) 0.0010(9) S5 0.1454(18) 0.1052(15) 0.1301(16) -0.0102(12) 0.0310(14) 0.0348(14) O1 0.110(3) 0.093(2) 0.088(2) 0.0024(19) 0.051(2) -0.005(2) O2 0.36(3) 0.28(3) 0.38(3) 0.24(2) 0.28(3) 0.22(2) O3 0.184(17) 0.26(2) 0.39(3) -0.09(3) -0.057(19) -0.023(16) O4 0.248(18) 0.37(2) 0.082(7) 0.023(10) 0.070(9) 0.177(17) O2' 0.120(8) 0.141(11) 0.133(8) 0.061(8) 0.026(7) 0.061(8) O3' 0.107(8) 0.183(11) 0.140(9) 0.035(8) 0.098(8) 0.025(7) O4' 0.172(14) 0.105(10) 0.43(3) -0.142(15) 0.175(18) -0.060(10) O5 0.096(3) 0.114(3) 0.102(2) -0.002(2) 0.039(2) -0.013(2) O6 0.104(3) 0.187(5) 0.152(4) 0.032(3) 0.033(3) -0.009(3) O7 0.126(3) 0.292(6) 0.078(2) 0.033(3) 0.042(2) -0.063(4) O8 0.173(5) 0.203(5) 0.219(5) -0.108(5) 0.117(4) -0.092(4) O9 0.102(3) 0.078(2) 0.075(2) 0.0062(17) 0.0347(18) -0.001(2) O10 0.102(6) 0.136(6) 0.169(7) 0.007(6) 0.039(6) -0.004(5) O11 0.173(7) 0.105(5) 0.114(5) 0.013(5) 0.066(5) -0.034(5) O12 0.112(5) 0.081(4) 0.108(5) -0.019(4) 0.044(4) -0.003(4) O10' 0.119(6) 0.146(7) 0.155(7) -0.015(6) 0.070(6) -0.011(5) O11' 0.125(6) 0.093(6) 0.185(7) 0.008(5) 0.077(6) 0.003(5) O12' 0.180(7) 0.116(6) 0.150(7) -0.021(5) 0.066(6) -0.056(6) O13 0.063(2) 0.085(2) 0.083(2) 0.0111(16) 0.0290(17) 0.0080(17) O14 0.099(3) 0.176(5) 0.217(5) 0.070(4) 0.046(3) -0.019(3) O15 0.079(3) 0.295(6) 0.078(3) 0.037(3) 0.009(2) 0.027(3) O16 0.093(3) 0.261(6) 0.181(4) -0.087(4) 0.062(3) 0.010(3) O17 0.094(2) 0.086(2) 0.076(2) 0.0138(18) 0.0309(18) 0.007(2) O18 0.165(8) 0.194(9) 0.212(9) 0.010(7) 0.070(7) 0.036(7) O19 0.123(6) 0.145(7) 0.105(6) 0.031(5) 0.023(5) 0.044(5) O20 0.248(11) 0.184(10) 0.212(10) -0.026(8) 0.069(8) 0.024(8) O18' 0.147(7) 0.180(8) 0.188(8) 0.004(7) 0.080(6) 0.038(6) O19' 0.194(9) 0.167(8) 0.194(9) -0.019(7) 0.019(7) 0.062(7) O20' 0.170(8) 0.092(6) 0.203(9) 0.009(6) 0.063(7) 0.020(6) C1 0.117(4) 0.079(3) 0.060(3) -0.005(2) 0.032(3) -0.031(3) C2 0.093(4) 0.076(3) 0.045(2) -0.010(2) 0.021(2) -0.020(3) C3 0.111(4) 0.093(4) 0.059(3) 0.002(3) 0.028(3) -0.013(3) C4 0.101(4) 0.100(4) 0.061(3) 0.000(3) 0.034(3) -0.009(3) C5 0.084(4) 0.091(4) 0.060(3) 0.000(3) 0.025(3) -0.014(3) C6 0.095(4) 0.070(3) 0.048(2) -0.009(2) 0.022(3) -0.013(3) C7 0.083(3) 0.087(4) 0.051(3) -0.011(3) 0.022(3) -0.011(3) C8 0.113(4) 0.101(4) 0.059(3) 0.003(3) 0.035(3) -0.006(3) C9 0.097(4) 0.077(3) 0.050(2) 0.010(2) 0.030(3) 0.005(3) C10 0.110(4) 0.096(4) 0.054(3) 0.006(3) 0.045(3) -0.009(3) C11 0.094(4) 0.083(3) 0.052(2) 0.000(2) 0.032(3) -0.007(3) C12 0.113(4) 0.072(3) 0.060(3) 0.006(2) 0.039(3) 0.007(3) C13 0.093(4) 0.078(3) 0.056(3) 0.019(3) 0.031(3) 0.007(3) C14 0.091(4) 0.081(4) 0.065(3) 0.018(3) 0.029(3) 0.006(3) C15 0.107(4) 0.085(3) 0.069(3) 0.023(3) 0.039(3) 0.033(3) C16 0.082(3) 0.076(3) 0.068(3) 0.010(3) 0.035(3) 0.019(3) C17 0.114(4) 0.071(4) 0.104(4) 0.015(3) 0.065(4) 0.016(3) C18 0.090(4) 0.066(3) 0.106(4) -0.003(3) 0.052(3) 0.003(3) C19 0.102(4) 0.061(3) 0.088(3) -0.014(3) 0.048(3) 0.007(3) C20 0.084(3) 0.068(3) 0.063(3) -0.002(2) 0.035(3) 0.016(3) C21 0.081(3) 0.062(3) 0.074(3) 0.005(3) 0.037(3) 0.010(3) C22 0.095(3) 0.067(3) 0.071(3) 0.004(2) 0.044(3) 0.016(3) C23 0.093(4) 0.054(3) 0.047(2) -0.001(2) 0.029(2) 0.009(3) C24 0.071(3) 0.071(3) 0.052(2) -0.008(2) 0.019(2) -0.014(3) C25 0.068(3) 0.070(3) 0.053(2) 0.011(2) 0.019(2) 0.007(3) C26 0.074(3) 0.070(3) 0.050(2) 0.006(2) 0.022(2) 0.014(3) C27 0.073(3) 0.061(3) 0.036(2) 0.0055(19) 0.018(2) -0.001(2) C28 0.077(3) 0.058(3) 0.041(2) 0.002(2) 0.020(2) 0.002(3) C29 0.095(3) 0.063(3) 0.066(3) 0.006(2) 0.042(3) 0.005(3) C30 0.081(3) 0.046(2) 0.061(3) 0.006(2) 0.029(2) 0.002(2) C31 0.098(4) 0.066(3) 0.067(3) -0.005(3) 0.027(3) -0.009(3) C32 0.086(3) 0.059(3) 0.073(3) -0.005(2) 0.022(3) 0.008(3) C33 0.116(4) 0.052(3) 0.074(3) -0.008(3) 0.039(3) -0.011(3) C34 0.100(4) 0.058(3) 0.051(2) -0.001(2) 0.028(3) -0.018(3) C35 0.077(3) 0.055(3) 0.052(3) 0.008(2) 0.018(2) -0.003(2) C36 0.123(6) 0.342(13) 0.089(5) -0.010(6) 0.024(4) -0.070(7) C37 0.109(6) 0.279(11) 0.055(3) 0.018(5) 0.035(4) 0.002(7) C38 0.128(6) 0.198(8) 0.097(4) -0.003(5) 0.051(4) -0.028(6) C39 0.148(7) 0.156(6) 0.092(4) 0.009(4) 0.057(4) 0.048(6) N1 0.119(5) 0.164(5) 0.086(3) 0.021(4) 0.031(3) 0.028(4) C40 0.131(6) 0.235(9) 0.090(4) 0.021(5) 0.038(5) 0.095(7) C41 0.104(6) 0.385(17) 0.074(5) 0.023(7) 0.027(4) 0.061(8) C42 0.178(9) 0.142(6) 0.163(7) 0.022(5) 0.032(7) -0.026(6) O21 0.133(4) 0.255(6) 0.147(4) 0.032(4) 0.054(3) -0.006(4) O22 0.237(7) 0.142(4) 0.221(6) -0.027(4) 0.056(5) -0.032(4) O23 0.217(7) 0.226(7) 0.274(8) -0.013(6) 0.053(6) -0.036(6) _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 S1 O3' 1.398(7) . ? S1 O4 1.414(8) . ? S1 O2 1.415(8) . ? S1 O3 1.415(9) . ? S1 O4' 1.419(7) . ? S1 O2' 1.429(8) . ? S1 C4 1.768(5) . ? S2 O7 1.391(3) . ? S2 O8 1.403(4) . ? S2 O6 1.463(4) . ? S2 C11 1.750(5) . ? S3 O10 1.388(7) . ? S3 O11' 1.418(7) . ? S3 O10' 1.421(7) . ? S3 O12 1.427(6) . ? S3 O12' 1.475(7) . ? S3 O11 1.499(6) . ? S3 C18 1.726(5) . ? S4 O15 1.416(4) . ? S4 O16 1.416(4) . ? S4 O14 1.420(4) . ? S4 C25 1.756(5) . ? S5 O20 1.419(9) . ? S5 O18 1.424(9) . ? S5 O19' 1.426(8) . ? S5 O18' 1.434(7) . ? S5 O19 1.459(7) . ? S5 O20' 1.461(8) . ? S5 C32 1.743(5) . ? O1 C7 1.363(5) . ? O1 H1C 0.8500 . ? O5 C14 1.379(6) . ? O5 H5C 0.8501 . ? O9 C21 1.364(5) . ? O9 H9A 0.8500 . ? O13 C28 1.359(5) . ? O13 H13A 0.8499 . ? O17 C35 1.366(5) . ? O17 H17C 0.8498 . ? C1 C34 1.519(6) . ? C1 C2 1.520(6) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.365(6) . ? C2 C7 1.395(6) . ? C3 C4 1.386(6) . ? C3 H3 0.9300 . ? C4 C5 1.384(6) . ? C5 C6 1.376(6) . ? C5 H5 0.9300 . ? C6 C7 1.409(6) . ? C6 C8 1.510(6) . ? C8 C9 1.502(6) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.373(6) . ? C9 C14 1.415(6) . ? C10 C11 1.394(6) . ? C10 H10 0.9300 . ? C11 C12 1.400(6) . ? C12 C13 1.388(6) . ? C12 H12 0.9300 . ? C13 C14 1.381(6) . ? C13 C15 1.516(6) . ? C15 C16 1.497(6) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.397(6) . ? C16 C21 1.401(6) . ? C17 C18 1.380(7) . ? C17 H17 0.9300 . ? C18 C19 1.402(6) . ? C19 C20 1.381(6) . ? C19 H19 0.9300 . ? C20 C21 1.392(6) . ? C20 C22 1.482(5) . ? C22 C23 1.536(5) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.393(6) . ? C23 C28 1.395(5) . ? C24 C25 1.364(6) . ? C24 H24 0.9300 . ? C25 C26 1.379(6) . ? C26 C27 1.381(6) . ? C26 H26 0.9300 . ? C27 C28 1.408(6) . ? C27 C29 1.507(6) . ? C29 C30 1.514(5) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.373(6) . ? C30 C35 1.399(5) . ? C31 C32 1.386(6) . ? C31 H31 0.9300 . ? C32 C33 1.397(6) . ? C33 C34 1.365(6) . ? C33 H33 0.9300 . ? C34 C35 1.382(5) . ? C36 C37 1.464(6) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 C38 1.3900 . ? C37 C41 1.3900 . ? C38 C39 1.3900 . ? C38 H38 0.9300 . ? C39 N1 1.3900 . ? C39 H39 0.9300 . ? N1 C40 1.3900 . ? N1 C42 1.471(8) . ? C40 C41 1.3900 . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? C42 C42 1.494(14) 2 ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? 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 O3' S1 O4 60.7(10) . . ? O3' S1 O2 136.7(10) . . ? O4 S1 O2 120.2(15) . . ? O3' S1 O3 51.3(12) . . ? O4 S1 O3 111.0(15) . . ? O2 S1 O3 102.3(16) . . ? O3' S1 O4' 126.6(10) . . ? O4 S1 O4' 69.9(11) . . ? O2 S1 O4' 57.6(14) . . ? O3 S1 O4' 150.5(11) . . ? O3' S1 O2' 100.0(8) . . ? O4 S1 O2' 145.6(9) . . ? O2 S1 O2' 53.1(15) . . ? O3 S1 O2' 51.5(11) . . ? O4' S1 O2' 110.3(11) . . ? O3' S1 C4 106.6(4) . . ? O4 S1 C4 108.3(5) . . ? O2 S1 C4 112.4(7) . . ? O3 S1 C4 100.7(10) . . ? O4' S1 C4 106.9(5) . . ? O2' S1 C4 104.3(5) . . ? O7 S2 O8 117.3(4) . . ? O7 S2 O6 111.0(3) . . ? O8 S2 O6 104.6(3) . . ? O7 S2 C11 109.1(2) . . ? O8 S2 C11 107.8(3) . . ? O6 S2 C11 106.6(2) . . ? O10 S3 O11' 142.2(5) . . ? O10 S3 O10' 46.4(5) . . ? O11' S3 O10' 112.2(6) . . ? O10 S3 O12 123.4(6) . . ? O11' S3 O12 53.2(5) . . ? O10' S3 O12 146.8(5) . . ? O10 S3 O12' 63.4(6) . . ? O11' S3 O12' 109.3(6) . . ? O10' S3 O12' 106.3(7) . . ? O12 S3 O12' 61.9(5) . . ? O10 S3 O11 110.9(6) . . ? O11' S3 O11 53.4(5) . . ? O10' S3 O11 65.3(6) . . ? O12 S3 O11 106.4(6) . . ? O12' S3 O11 146.9(5) . . ? O10 S3 C18 104.5(5) . . ? O11' S3 C18 112.6(4) . . ? O10' S3 C18 107.9(4) . . ? O12 S3 C18 105.3(3) . . ? O12' S3 C18 108.3(4) . . ? O11 S3 C18 104.7(4) . . ? O15 S4 O16 113.6(4) . . ? O15 S4 O14 110.4(3) . . ? O16 S4 O14 109.6(3) . . ? O15 S4 C25 107.2(2) . . ? O16 S4 C25 107.5(3) . . ? O14 S4 C25 108.3(3) . . ? O20 S5 O18 108.5(11) . . ? O20 S5 O19' 144.3(9) . . ? O18 S5 O19' 62.3(8) . . ? O20 S5 O18' 60.9(8) . . ? O18 S5 O18' 48.2(7) . . ? O19' S5 O18' 105.8(9) . . ? O20 S5 O19 118.7(10) . . ? O18 S5 O19 112.4(8) . . ? O19' S5 O19 50.9(7) . . ? O18' S5 O19 143.5(6) . . ? O20 S5 O20' 37.6(9) . . ? O18 S5 O20' 142.5(9) . . ? O19' S5 O20' 130.8(9) . . ? O18' S5 O20' 97.8(9) . . ? O19 S5 O20' 85.1(8) . . ? O20 S5 C32 106.8(8) . . ? O18 S5 C32 101.2(6) . . ? O19' S5 C32 108.9(5) . . ? O18' S5 C32 106.7(5) . . ? O19 S5 C32 107.7(4) . . ? O20' S5 C32 104.5(5) . . ? C7 O1 H1C 108.4 . . ? C14 O5 H5C 108.3 . . ? C21 O9 H9A 108.8 . . ? C28 O13 H13A 108.2 . . ? C35 O17 H17C 109.0 . . ? C34 C1 C2 113.8(4) . . ? C34 C1 H1A 108.8 . . ? C2 C1 H1A 108.8 . . ? C34 C1 H1B 108.8 . . ? C2 C1 H1B 108.8 . . ? H1A C1 H1B 107.7 . . ? C3 C2 C7 119.2(4) . . ? C3 C2 C1 121.0(5) . . ? C7 C2 C1 119.7(5) . . ? C2 C3 C4 120.8(5) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C5 C4 C3 119.4(5) . . ? C5 C4 S1 120.9(4) . . ? C3 C4 S1 119.4(4) . . ? C6 C5 C4 121.8(4) . . ? C6 C5 H5 119.1 . . ? C4 C5 H5 119.1 . . ? C5 C6 C7 117.4(5) . . ? C5 C6 C8 120.3(4) . . ? C7 C6 C8 122.2(5) . . ? O1 C7 C2 117.3(4) . . ? O1 C7 C6 121.4(5) . . ? C2 C7 C6 121.2(4) . . ? C9 C8 C6 116.4(4) . . ? C9 C8 H8A 108.2 . . ? C6 C8 H8A 108.2 . . ? C9 C8 H8B 108.2 . . ? C6 C8 H8B 108.2 . . ? H8A C8 H8B 107.3 . . ? C10 C9 C14 117.9(5) . . ? C10 C9 C8 120.2(4) . . ? C14 C9 C8 121.9(5) . . ? C9 C10 C11 121.1(4) . . ? C9 C10 H10 119.5 . . ? C11 C10 H10 119.5 . . ? C10 C11 C12 118.9(4) . . ? C10 C11 S2 120.8(4) . . ? C12 C11 S2 120.3(4) . . ? C13 C12 C11 122.2(5) . . ? C13 C12 H12 118.9 . . ? C11 C12 H12 118.9 . . ? C14 C13 C12 116.7(4) . . ? C14 C13 C15 123.7(5) . . ? C12 C13 C15 119.6(5) . . ? O5 C14 C13 121.1(4) . . ? O5 C14 C9 115.6(5) . . ? C13 C14 C9 123.2(5) . . ? C16 C15 C13 112.8(4) . . ? C16 C15 H15A 109.0 . . ? C13 C15 H15A 109.0 . . ? C16 C15 H15B 109.0 . . ? C13 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? C17 C16 C21 116.9(5) . . ? C17 C16 C15 121.7(4) . . ? C21 C16 C15 121.4(5) . . ? C18 C17 C16 122.6(5) . . ? C18 C17 H17 118.7 . . ? C16 C17 H17 118.7 . . ? C17 C18 C19 117.7(5) . . ? C17 C18 S3 120.1(4) . . ? C19 C18 S3 122.2(5) . . ? C20 C19 C18 122.5(5) . . ? C20 C19 H19 118.7 . . ? C18 C19 H19 118.7 . . ? C19 C20 C21 117.4(4) . . ? C19 C20 C22 120.4(4) . . ? C21 C20 C22 122.1(4) . . ? O9 C21 C20 122.1(4) . . ? O9 C21 C16 115.2(4) . . ? C20 C21 C16 122.7(5) . . ? C20 C22 C23 113.8(3) . . ? C20 C22 H22A 108.8 . . ? C23 C22 H22A 108.8 . . ? C20 C22 H22B 108.8 . . ? C23 C22 H22B 108.8 . . ? H22A C22 H22B 107.7 . . ? C24 C23 C28 118.8(4) . . ? C24 C23 C22 120.1(4) . . ? C28 C23 C22 121.1(4) . . ? C25 C24 C23 121.2(4) . . ? C25 C24 H24 119.4 . . ? C23 C24 H24 119.4 . . ? C24 C25 C26 119.2(4) . . ? C24 C25 S4 120.1(4) . . ? C26 C25 S4 120.6(4) . . ? C25 C26 C27 122.3(4) . . ? C25 C26 H26 118.9 . . ? C27 C26 H26 118.9 . . ? C26 C27 C28 117.7(4) . . ? C26 C27 C29 120.6(4) . . ? C28 C27 C29 121.6(4) . . ? O13 C28 C23 116.1(4) . . ? O13 C28 C27 123.4(4) . . ? C23 C28 C27 120.5(4) . . ? C27 C29 C30 114.0(3) . . ? C27 C29 H29A 108.8 . . ? C30 C29 H29A 108.8 . . ? C27 C29 H29B 108.8 . . ? C30 C29 H29B 108.8 . . ? H29A C29 H29B 107.6 . . ? C31 C30 C35 118.0(4) . . ? C31 C30 C29 120.8(4) . . ? C35 C30 C29 121.1(4) . . ? C30 C31 C32 121.3(4) . . ? C30 C31 H31 119.3 . . ? C32 C31 H31 119.3 . . ? C31 C32 C33 118.6(4) . . ? C31 C32 S5 120.3(4) . . ? C33 C32 S5 121.2(4) . . ? C34 C33 C32 121.9(4) . . ? C34 C33 H33 119.1 . . ? C32 C33 H33 119.1 . . ? C33 C34 C35 118.0(4) . . ? C33 C34 C1 120.5(4) . . ? C35 C34 C1 121.5(4) . . ? O17 C35 C34 121.7(4) . . ? O17 C35 C30 116.1(4) . . ? C34 C35 C30 122.2(4) . . ? C37 C36 H36A 109.5 . . ? C37 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C37 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 C41 120.0 . . ? C38 C37 C36 121.0(4) . . ? C41 C37 C36 119.0(4) . . ? C37 C38 C39 120.0 . . ? C37 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? N1 C39 C38 120.0 . . ? N1 C39 H39 120.0 . . ? C38 C39 H39 120.0 . . ? C39 N1 C40 120.0 . . ? C39 N1 C42 119.7(5) . . ? C40 N1 C42 120.3(5) . . ? C41 C40 N1 120.0 . . ? C41 C40 H40 120.0 . . ? N1 C40 H40 120.0 . . ? C40 C41 C37 120.0 . . ? C40 C41 H41 120.0 . . ? C37 C41 H41 120.0 . . ? N1 C42 C42 111.7(7) . 2 ? N1 C42 H42A 109.3 . . ? C42 C42 H42A 109.3 2 . ? N1 C42 H42B 109.3 . . ? C42 C42 H42B 109.3 2 . ? H42A C42 H42B 107.9 . . ? 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 C34 C1 C2 C3 -77.4(6) . . . . ? C34 C1 C2 C7 107.6(5) . . . . ? C7 C2 C3 C4 -1.7(7) . . . . ? C1 C2 C3 C4 -176.7(4) . . . . ? C2 C3 C4 C5 3.6(7) . . . . ? C2 C3 C4 S1 177.5(4) . . . . ? O3' S1 C4 C5 -9.5(9) . . . . ? O4 S1 C4 C5 54.4(15) . . . . ? O2 S1 C4 C5 -170(2) . . . . ? O3 S1 C4 C5 -62.1(16) . . . . ? O4' S1 C4 C5 128.4(13) . . . . ? O2' S1 C4 C5 -114.8(8) . . . . ? O3' S1 C4 C3 176.7(8) . . . . ? O4 S1 C4 C3 -119.3(15) . . . . ? O2 S1 C4 C3 16(2) . . . . ? O3 S1 C4 C3 124.2(16) . . . . ? O4' S1 C4 C3 -45.4(13) . . . . ? O2' S1 C4 C3 71.5(8) . . . . ? C3 C4 C5 C6 -2.3(7) . . . . ? S1 C4 C5 C6 -176.1(4) . . . . ? C4 C5 C6 C7 -0.8(7) . . . . ? C4 C5 C6 C8 175.0(4) . . . . ? C3 C2 C7 O1 178.9(4) . . . . ? C1 C2 C7 O1 -6.0(6) . . . . ? C3 C2 C7 C6 -1.6(6) . . . . ? C1 C2 C7 C6 173.5(4) . . . . ? C5 C6 C7 O1 -177.7(4) . . . . ? C8 C6 C7 O1 6.5(6) . . . . ? C5 C6 C7 C2 2.8(6) . . . . ? C8 C6 C7 C2 -172.9(4) . . . . ? C5 C6 C8 C9 98.8(5) . . . . ? C7 C6 C8 C9 -85.6(6) . . . . ? C6 C8 C9 C10 -82.3(5) . . . . ? C6 C8 C9 C14 100.7(5) . . . . ? C14 C9 C10 C11 -1.4(6) . . . . ? C8 C9 C10 C11 -178.5(4) . . . . ? C9 C10 C11 C12 1.7(7) . . . . ? C9 C10 C11 S2 -179.1(3) . . . . ? O7 S2 C11 C10 -63.5(5) . . . . ? O8 S2 C11 C10 168.2(4) . . . . ? O6 S2 C11 C10 56.4(4) . . . . ? O7 S2 C11 C12 115.8(4) . . . . ? O8 S2 C11 C12 -12.6(5) . . . . ? O6 S2 C11 C12 -124.3(4) . . . . ? C10 C11 C12 C13 -0.4(7) . . . . ? S2 C11 C12 C13 -179.6(3) . . . . ? C11 C12 C13 C14 -1.1(6) . . . . ? C11 C12 C13 C15 178.4(4) . . . . ? C12 C13 C14 O5 -176.5(4) . . . . ? C15 C13 C14 O5 4.0(7) . . . . ? C12 C13 C14 C9 1.4(6) . . . . ? C15 C13 C14 C9 -178.1(4) . . . . ? C10 C9 C14 O5 177.8(4) . . . . ? C8 C9 C14 O5 -5.2(6) . . . . ? C10 C9 C14 C13 -0.2(7) . . . . ? C8 C9 C14 C13 176.9(4) . . . . ? C14 C13 C15 C16 -129.1(5) . . . . ? C12 C13 C15 C16 51.4(6) . . . . ? C13 C15 C16 C17 -86.0(5) . . . . ? C13 C15 C16 C21 93.5(5) . . . . ? C21 C16 C17 C18 -2.8(7) . . . . ? C15 C16 C17 C18 176.7(4) . . . . ? C16 C17 C18 C19 3.2(7) . . . . ? C16 C17 C18 S3 -175.8(3) . . . . ? O10 S3 C18 C17 113.2(7) . . . . ? O11' S3 C18 C17 -59.6(7) . . . . ? O10' S3 C18 C17 64.9(8) . . . . ? O12 S3 C18 C17 -115.5(6) . . . . ? O12' S3 C18 C17 179.5(6) . . . . ? O11 S3 C18 C17 -3.5(7) . . . . ? O10 S3 C18 C19 -65.8(7) . . . . ? O11' S3 C18 C19 121.5(7) . . . . ? O10' S3 C18 C19 -114.1(7) . . . . ? O12 S3 C18 C19 65.5(6) . . . . ? O12' S3 C18 C19 0.6(7) . . . . ? O11 S3 C18 C19 177.5(6) . . . . ? C17 C18 C19 C20 -2.0(7) . . . . ? S3 C18 C19 C20 177.0(3) . . . . ? C18 C19 C20 C21 0.6(6) . . . . ? C18 C19 C20 C22 179.4(4) . . . . ? C19 C20 C21 O9 -179.1(4) . . . . ? C22 C20 C21 O9 2.0(6) . . . . ? C19 C20 C21 C16 -0.2(6) . . . . ? C22 C20 C21 C16 -179.0(4) . . . . ? C17 C16 C21 O9 -179.7(4) . . . . ? C15 C16 C21 O9 0.8(6) . . . . ? C17 C16 C21 C20 1.2(6) . . . . ? C15 C16 C21 C20 -178.2(4) . . . . ? C19 C20 C22 C23 110.3(5) . . . . ? C21 C20 C22 C23 -70.9(5) . . . . ? C20 C22 C23 C24 -69.6(5) . . . . ? C20 C22 C23 C28 111.2(4) . . . . ? C28 C23 C24 C25 0.6(5) . . . . ? C22 C23 C24 C25 -178.7(3) . . . . ? C23 C24 C25 C26 2.9(6) . . . . ? C23 C24 C25 S4 -178.1(3) . . . . ? O15 S4 C25 C24 -102.1(4) . . . . ? O16 S4 C25 C24 135.4(4) . . . . ? O14 S4 C25 C24 17.1(4) . . . . ? O15 S4 C25 C26 76.9(4) . . . . ? O16 S4 C25 C26 -45.6(4) . . . . ? O14 S4 C25 C26 -164.0(4) . . . . ? C24 C25 C26 C27 -2.1(6) . . . . ? S4 C25 C26 C27 179.0(3) . . . . ? C25 C26 C27 C28 -2.2(5) . . . . ? C25 C26 C27 C29 175.9(3) . . . . ? C24 C23 C28 O13 175.9(3) . . . . ? C22 C23 C28 O13 -4.8(5) . . . . ? C24 C23 C28 C27 -4.9(5) . . . . ? C22 C23 C28 C27 174.3(3) . . . . ? C26 C27 C28 O13 -175.3(3) . . . . ? C29 C27 C28 O13 6.7(5) . . . . ? C26 C27 C28 C23 5.7(5) . . . . ? C29 C27 C28 C23 -172.4(3) . . . . ? C26 C27 C29 C30 54.2(5) . . . . ? C28 C27 C29 C30 -127.7(4) . . . . ? C27 C29 C30 C31 -103.7(5) . . . . ? C27 C29 C30 C35 80.0(5) . . . . ? C35 C30 C31 C32 -0.7(6) . . . . ? C29 C30 C31 C32 -177.0(4) . . . . ? C30 C31 C32 C33 2.8(7) . . . . ? C30 C31 C32 S5 -178.3(3) . . . . ? O20 S5 C32 C31 -151.0(11) . . . . ? O18 S5 C32 C31 95.5(9) . . . . ? O19' S5 C32 C31 31.2(10) . . . . ? O18' S5 C32 C31 145.0(9) . . . . ? O19 S5 C32 C31 -22.6(7) . . . . ? O20' S5 C32 C31 -112.0(7) . . . . ? O20 S5 C32 C33 27.9(11) . . . . ? O18 S5 C32 C33 -85.6(9) . . . . ? O19' S5 C32 C33 -149.9(10) . . . . ? O18' S5 C32 C33 -36.1(9) . . . . ? O19 S5 C32 C33 156.3(6) . . . . ? O20' S5 C32 C33 66.9(8) . . . . ? C31 C32 C33 C34 -2.3(7) . . . . ? S5 C32 C33 C34 178.7(4) . . . . ? C32 C33 C34 C35 -0.2(7) . . . . ? C32 C33 C34 C1 176.8(4) . . . . ? C2 C1 C34 C33 90.7(5) . . . . ? C2 C1 C34 C35 -92.3(5) . . . . ? C33 C34 C35 O17 -178.1(4) . . . . ? C1 C34 C35 O17 4.9(6) . . . . ? C33 C34 C35 C30 2.5(6) . . . . ? C1 C34 C35 C30 -174.5(4) . . . . ? C31 C30 C35 O17 178.5(4) . . . . ? C29 C30 C35 O17 -5.1(6) . . . . ? C31 C30 C35 C34 -2.0(6) . . . . ? C29 C30 C35 C34 174.3(4) . . . . ? C41 C37 C38 C39 0.0 . . . . ? C36 C37 C38 C39 -179.2(5) . . . . ? C37 C38 C39 N1 0.0 . . . . ? C38 C39 N1 C40 0.0 . . . . ? C38 C39 N1 C42 179.7(4) . . . . ? C39 N1 C40 C41 0.0 . . . . ? C42 N1 C40 C41 -179.7(4) . . . . ? N1 C40 C41 C37 0.0 . . . . ? C38 C37 C41 C40 0.0 . . . . ? C36 C37 C41 C40 179.2(4) . . . . ? C39 N1 C42 C42 91.3(8) . . . 2 ? C40 N1 C42 C42 -88.9(7) . . . 2 ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 1968 730 ' ' 2 0.500 0.500 0.247 1968 730 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.51 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.438 _refine_diff_density_min -0.316 _refine_diff_density_rms 0.057 # Attachment 'revised_compound_5.cif' data_060321c _database_code_depnum_ccdc_archive 'CCDC 728425' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H44 N O23 S5' _chemical_formula_weight 1091.08 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 31.878(4) _cell_length_b 19.919(2) _cell_length_c 11.1685(13) _cell_angle_alpha 90.00 _cell_angle_beta 96.582(2) _cell_angle_gamma 90.00 _cell_volume 7044.9(14) _cell_formula_units_Z 4 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 3629 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 22.49 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.029 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2268 _exptl_absorpt_coefficient_mu 0.224 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.522 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17640 _diffrn_reflns_av_R_equivalents 0.0422 _diffrn_reflns_av_sigmaI/netI 0.0541 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6308 _reflns_number_gt 2720 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0035(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6308 _refine_ls_number_parameters 398 _refine_ls_number_restraints 445 _refine_ls_R_factor_all 0.2369 _refine_ls_R_factor_gt 0.1508 _refine_ls_wR_factor_ref 0.4337 _refine_ls_wR_factor_gt 0.3620 _refine_ls_goodness_of_fit_ref 1.347 _refine_ls_restrained_S_all 1.421 _refine_ls_shift/su_max 0.004 _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 S1 S 0.12308(9) 0.19204(16) 0.3504(2) 0.1197(10) Uani 1 1 d DU . . S2 S 0.14728(11) 0.34748(14) 0.9000(3) 0.1424(13) Uani 1 1 d DU . . S3 S 0.07263(10) 0.0000 0.9816(5) 0.1230(13) Uani 1 2 d SDU . . O1 O 0.2743(2) 0.0709(4) 0.6135(6) 0.130(2) Uani 1 1 d U A . H1E H 0.2756 0.0832 0.6867 0.156 Uiso 0.50 1 d PR . . H1C H 0.2718 0.0285 0.6088 0.195 Uiso 0.50 1 d PR . . O2 O 0.0902(5) 0.1447(9) 0.3641(18) 0.164(6) Uani 0.50 1 d PDU A 1 O3 O 0.1300(4) 0.2011(8) 0.2289(8) 0.111(4) Uani 0.50 1 d PDU A 1 O4 O 0.1171(6) 0.2580(6) 0.3983(16) 0.149(5) Uani 0.50 1 d PDU A 1 O2' O 0.0909(4) 0.1856(10) 0.4261(14) 0.147(5) Uani 0.50 1 d PDU A 2 O3' O 0.1131(6) 0.1646(10) 0.2326(11) 0.154(6) Uani 0.50 1 d PDU A 2 O4' O 0.1354(6) 0.2596(7) 0.324(2) 0.183(7) Uani 0.50 1 d PDU A 2 O5 O 0.25521(15) 0.1100(2) 0.8767(4) 0.0880(15) Uani 1 1 d U A . H5D H 0.2430 0.0765 0.9045 0.106 Uiso 0.50 1 d PR . . H5B H 0.2589 0.1029 0.8036 0.132 Uiso 0.50 1 d PR . . O6 O 0.1146(3) 0.3376(5) 0.8014(9) 0.204(4) Uani 1 1 d DU . . O7 O 0.1726(3) 0.4060(4) 0.8940(10) 0.193(4) Uani 1 1 d DU . . O8 O 0.1246(4) 0.3405(6) 1.0077(10) 0.226(4) Uani 1 1 d DU . . O9 O 0.25676(19) 0.0000 1.0898(6) 0.0766(17) Uani 1 2 d SU A . H9A H 0.2665 -0.0273 1.0414 0.115 Uiso 0.50 1 d PR . . O10 O 0.0552(6) 0.0000 1.0924(12) 0.124(5) Uani 0.50 2 d SPDU . . O11 O 0.0571(5) 0.0637(6) 1.0214(17) 0.157(5) Uani 0.50 1 d PDU . . O12 O 0.0625(5) 0.0613(7) 0.9171(16) 0.152(5) Uani 0.50 1 d PDU . . O13 O 0.0638(6) 0.0000 0.8529(10) 0.137(6) Uani 0.50 2 d SPDU . . C1 C 0.2348(4) 0.0000 0.4053(11) 0.113(4) Uani 1 2 d SU . . H1A H 0.2297 0.0000 0.3179 0.136 Uiso 1 2 calc SR . . H1B H 0.2652 0.0000 0.4263 0.136 Uiso 1 2 calc SR . . C2 C 0.2182(3) 0.0650(5) 0.4486(6) 0.094(2) Uani 1 1 d U A . C3 C 0.1822(3) 0.0946(5) 0.3893(6) 0.090(2) Uani 1 1 d U . . H3 H 0.1670 0.0728 0.3247 0.109 Uiso 1 1 calc R A . C4 C 0.1694(3) 0.1548(5) 0.4251(6) 0.093(2) Uani 1 1 d U A . C5 C 0.1907(3) 0.1921(5) 0.5184(7) 0.100(3) Uani 1 1 d U . . H5A H 0.1813 0.2344 0.5385 0.120 Uiso 1 1 calc R A . C6 C 0.2276(3) 0.1625(5) 0.5822(7) 0.093(2) Uani 1 1 d U A . C7 C 0.2395(3) 0.1004(5) 0.5480(7) 0.093(2) Uani 1 1 d U . . C8 C 0.2516(3) 0.2029(5) 0.6801(7) 0.103(3) Uani 1 1 d U . . H8A H 0.2585 0.2461 0.6476 0.124 Uiso 1 1 calc R A . H8B H 0.2779 0.1801 0.7067 0.124 Uiso 1 1 calc R . . C9 C 0.2275(2) 0.2142(4) 0.7882(6) 0.085(2) Uani 1 1 d U A . C10 C 0.2023(3) 0.2688(4) 0.7982(7) 0.093(2) Uani 1 1 d U . . H10 H 0.2004 0.3012 0.7379 0.112 Uiso 1 1 calc R A . C11 C 0.1789(3) 0.2776(4) 0.8974(8) 0.093(2) Uani 1 1 d U A . C12 C 0.1845(2) 0.2319(3) 0.9894(6) 0.0756(18) Uani 1 1 d U . . H12 H 0.1708 0.2387 1.0574 0.091 Uiso 1 1 calc R A . C13 C 0.2100(2) 0.1760(3) 0.9847(5) 0.0649(16) Uani 1 1 d U A . C14 C 0.2308(2) 0.1664(3) 0.8834(6) 0.0703(18) Uani 1 1 d U . . C15 C 0.2156(2) 0.1272(3) 1.0871(5) 0.0657(16) Uani 1 1 d U . . H15A H 0.2055 0.1478 1.1572 0.079 Uiso 1 1 calc R A . H15B H 0.2455 0.1182 1.1068 0.079 Uiso 1 1 calc R . . C16 C 0.19258(19) 0.0607(3) 1.0620(5) 0.0588(15) Uani 1 1 d U A . C17 C 0.1495(2) 0.0598(3) 1.0371(6) 0.0692(17) Uani 1 1 d U . . H17 H 0.1347 0.1002 1.0310 0.083 Uiso 1 1 calc R A . C18 C 0.1275(3) 0.0000 1.0210(9) 0.079(3) Uani 1 2 d SU . . C19 C 0.2141(3) 0.0000 1.0699(6) 0.054(2) Uani 1 2 d SU . . N1 N 0.0980(3) 0.0000 0.5797(8) 0.103(3) Uani 1 2 d SU . . C20 C 0.1660(4) 0.0000 0.7437(13) 0.116(4) Uani 1 2 d SU . . H20 H 0.1903 0.0000 0.7985 0.139 Uiso 1 2 calc SR . . C21 C 0.1494(3) 0.0578(6) 0.7062(8) 0.120(3) Uani 1 1 d U . . H21 H 0.1618 0.0978 0.7349 0.144 Uiso 1 1 calc R . . C22 C 0.1139(3) 0.0590(6) 0.6250(9) 0.122(3) Uani 1 1 d U . . H22 H 0.1009 0.0995 0.6014 0.146 Uiso 1 1 calc R . . C23 C 0.0610(4) 0.0000 0.4882(13) 0.128(4) Uani 1 2 d SU . . H23A H 0.0642 -0.0341 0.4292 0.154 Uiso 0.50 1 d PR . . H23B H 0.0587 0.0427 0.4480 0.154 Uiso 0.50 1 d PR . . C24 C 0.0189(4) -0.0140(13) 0.5504(13) 0.101(6) Uani 0.50 1 d PU . . H24A H 0.0147 0.0205 0.6077 0.121 Uiso 0.50 1 d PR . . H24B H 0.0207 -0.0566 0.5909 0.121 Uiso 0.50 1 d PR . . O14 O 0.0689(6) 0.2172(10) 1.0310(18) 0.184(6) Uani 0.50 1 d PU . . O16 O 0.1558(8) 0.5000 0.693(2) 0.177(9) Uani 0.50 2 d SPU . . O17 O 0.1619(11) 0.5000 1.108(3) 0.236(13) Uani 0.50 2 d SPU . . O15 O 0.0165(7) 0.1072(11) 0.202(2) 0.212(8) Uani 0.50 1 d PU . . 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 S1 0.128(2) 0.151(2) 0.0776(14) -0.0044(14) 0.0009(13) -0.0004(16) S2 0.146(2) 0.0856(18) 0.184(3) 0.0227(17) -0.035(2) 0.0116(16) S3 0.0748(19) 0.111(3) 0.182(4) 0.000 0.011(2) 0.000 O1 0.122(4) 0.157(5) 0.104(4) 0.010(4) -0.021(3) -0.011(4) O2 0.157(8) 0.164(8) 0.166(8) 0.017(7) 0.005(6) -0.008(6) O3 0.119(6) 0.122(7) 0.092(6) 0.029(5) 0.009(5) 0.002(6) O4 0.152(7) 0.147(8) 0.146(7) -0.024(6) 0.009(6) 0.034(6) O2' 0.139(7) 0.161(8) 0.143(8) 0.004(6) 0.027(6) 0.025(6) O3' 0.154(8) 0.161(9) 0.144(8) -0.007(6) 0.003(6) 0.007(6) O4' 0.182(9) 0.177(9) 0.189(9) 0.030(7) 0.014(7) 0.001(7) O5 0.098(3) 0.086(3) 0.080(3) -0.004(2) 0.012(3) -0.002(3) O6 0.181(6) 0.192(6) 0.229(7) -0.008(5) -0.022(5) 0.035(5) O7 0.186(6) 0.141(5) 0.245(7) 0.001(5) -0.013(5) 0.005(5) O8 0.224(7) 0.211(7) 0.248(7) -0.001(6) 0.043(6) 0.053(6) O9 0.073(4) 0.073(4) 0.082(4) 0.000 -0.003(3) 0.000 O10 0.117(8) 0.128(8) 0.131(8) 0.000 0.027(6) 0.000 O11 0.136(7) 0.162(8) 0.171(8) -0.024(6) 0.013(6) 0.026(6) O12 0.132(7) 0.155(8) 0.165(8) 0.027(6) 0.003(6) 0.004(6) O13 0.122(8) 0.160(9) 0.128(8) 0.000 0.003(6) 0.000 C1 0.113(7) 0.145(8) 0.084(6) 0.000 0.016(6) 0.000 C2 0.109(5) 0.122(6) 0.054(4) 0.004(4) 0.020(4) -0.015(5) C3 0.102(5) 0.116(6) 0.053(4) 0.003(4) 0.009(4) -0.013(4) C4 0.098(5) 0.120(6) 0.060(4) 0.004(4) 0.007(4) -0.019(5) C5 0.112(5) 0.116(6) 0.074(4) 0.011(4) 0.024(4) -0.027(5) C6 0.096(5) 0.115(6) 0.068(4) 0.019(4) 0.010(4) -0.032(5) C7 0.100(5) 0.116(6) 0.062(4) 0.013(4) 0.008(4) -0.019(5) C8 0.109(5) 0.129(6) 0.070(4) 0.005(4) 0.009(4) -0.045(5) C9 0.089(4) 0.097(5) 0.064(4) 0.001(4) -0.011(3) -0.036(4) C10 0.106(5) 0.077(5) 0.087(5) 0.019(4) -0.026(4) -0.024(4) C11 0.114(5) 0.065(4) 0.094(5) 0.005(4) -0.018(4) -0.009(4) C12 0.081(4) 0.062(4) 0.080(4) 0.000(3) -0.005(3) -0.010(3) C13 0.078(4) 0.058(4) 0.056(3) -0.004(3) 0.000(3) -0.019(3) C14 0.082(4) 0.066(4) 0.060(4) 0.000(3) -0.003(3) -0.020(3) C15 0.085(4) 0.057(3) 0.053(3) -0.001(3) 0.000(3) -0.009(3) C16 0.074(4) 0.059(4) 0.042(3) 0.000(3) 0.003(2) 0.003(3) C17 0.070(4) 0.064(4) 0.075(4) 0.004(3) 0.014(3) 0.014(3) C18 0.073(5) 0.082(6) 0.084(6) 0.000 0.018(4) 0.000 C19 0.061(5) 0.061(5) 0.040(4) 0.000 0.003(3) 0.000 N1 0.088(5) 0.145(7) 0.075(5) 0.000 0.007(4) 0.000 C20 0.103(7) 0.144(9) 0.101(7) 0.000 0.011(6) 0.000 C21 0.113(6) 0.150(7) 0.097(5) 0.006(5) 0.011(5) -0.043(6) C22 0.112(6) 0.135(7) 0.117(6) 0.020(5) 0.007(5) -0.017(5) C23 0.100(7) 0.157(9) 0.121(8) 0.000 -0.017(6) 0.000 C24 0.096(7) 0.102(13) 0.101(7) -0.002(8) -0.002(6) 0.000(7) O14 0.177(9) 0.188(9) 0.183(9) 0.008(7) 0.000(6) 0.013(7) O16 0.178(10) 0.178(11) 0.173(10) 0.000 0.012(7) 0.000 O17 0.238(15) 0.235(15) 0.238(15) 0.000 0.034(8) 0.000 O15 0.213(10) 0.210(10) 0.213(10) -0.015(7) 0.028(7) 0.001(7) _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 S1 O2' 1.407(9) . ? S1 O3 1.411(8) . ? S1 O3' 1.426(9) . ? S1 O2 1.431(9) . ? S1 O4 1.439(9) . ? S1 O4' 1.441(10) . ? S1 C4 1.773(9) . ? S2 O7 1.424(7) . ? S2 O6 1.440(8) . ? S2 O8 1.479(8) . ? S2 C11 1.721(9) . ? S3 O10 1.413(9) . ? S3 O13 1.433(10) . ? S3 O12 1.436(9) 6 ? S3 O12 1.436(9) . ? S3 O11 1.451(9) 6 ? S3 O11 1.451(9) . ? S3 C18 1.753(11) . ? O1 C7 1.386(10) . ? O1 H1E 0.8500 . ? O1 H1C 0.8502 . ? O5 C14 1.372(8) . ? O5 H5D 0.8500 . ? O5 H5B 0.8500 . ? O9 C19 1.351(10) . ? O9 H9A 0.8499 . ? O10 O11 1.501(19) 6 ? O13 O12 1.419(18) 6 ? C1 C2 1.499(10) 6 ? C1 C2 1.499(10) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.389(11) . ? C2 C7 1.421(11) . ? C3 C4 1.343(11) . ? C3 H3 0.9300 . ? C4 C5 1.391(11) . ? C5 C6 1.432(12) . ? C5 H5A 0.9300 . ? C6 C7 1.361(11) . ? C6 C8 1.494(11) . ? C8 C9 1.519(11) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.364(11) . ? C9 C14 1.422(10) . ? C10 C11 1.415(11) . ? C10 H10 0.9300 . ? C11 C12 1.369(10) . ? C12 C13 1.383(9) . ? C12 H12 0.9300 . ? C13 C14 1.389(9) . ? C13 C15 1.496(8) . ? C15 C16 1.526(8) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C17 1.371(8) . ? C16 C19 1.388(7) . ? C17 C18 1.383(8) . ? C17 H17 0.9300 . ? C18 C17 1.383(8) 6 ? C19 C16 1.388(7) 6 ? N1 C22 1.355(11) 6 ? N1 C22 1.355(11) . ? N1 C23 1.468(15) . ? C20 C21 1.316(12) 6 ? C20 C21 1.316(12) . ? C20 H20 0.9300 . ? C21 C22 1.366(13) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.607(19) 6 ? C23 C24 1.607(19) . ? C23 H23A 0.9601 . ? C23 H23B 0.9601 . ? C24 C24 0.56(5) 6 ? C24 C24 1.55(3) 2_556 ? C24 C24 1.65(3) 5_556 ? C24 H24A 0.9601 . ? C24 H24B 0.9600 . ? 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 O2' S1 O3 142.6(10) . . ? O2' S1 O3' 114.7(11) . . ? O3 S1 O3' 37.3(7) . . ? O2' S1 O2 44.2(8) . . ? O3 S1 O2 112.5(11) . . ? O3' S1 O2 75.9(12) . . ? O2' S1 O4 73.9(11) . . ? O3 S1 O4 106.5(10) . . ? O3' S1 O4 131.9(10) . . ? O2 S1 O4 115.6(12) . . ? O2' S1 O4' 116.2(13) . . ? O3 S1 O4' 67.0(10) . . ? O3' S1 O4' 102.0(12) . . ? O2 S1 O4' 149.0(12) . . ? O4 S1 O4' 43.5(9) . . ? O2' S1 C4 107.7(7) . . ? O3 S1 C4 107.0(6) . . ? O3' S1 C4 111.1(8) . . ? O2 S1 C4 104.8(8) . . ? O4 S1 C4 110.2(7) . . ? O4' S1 C4 104.7(8) . . ? O7 S2 O6 116.1(7) . . ? O7 S2 O8 116.6(7) . . ? O6 S2 O8 103.4(7) . . ? O7 S2 C11 108.9(5) . . ? O6 S2 C11 104.5(5) . . ? O8 S2 C11 106.2(5) . . ? O10 S3 O13 145.7(11) . . ? O10 S3 O12 110.5(8) . 6 ? O13 S3 O12 59.3(8) . 6 ? O10 S3 O12 110.5(8) . . ? O13 S3 O12 59.3(8) . . ? O12 S3 O12 116.5(15) 6 . ? O10 S3 O11 63.2(8) . 6 ? O13 S3 O11 105.8(9) . 6 ? O12 S3 O11 49.0(8) 6 6 ? O12 S3 O11 146.4(9) . 6 ? O10 S3 O11 63.2(8) . . ? O13 S3 O11 105.8(9) . . ? O12 S3 O11 146.4(9) 6 . ? O12 S3 O11 49.0(8) . . ? O11 S3 O11 122.1(15) 6 . ? O10 S3 C18 105.2(9) . . ? O13 S3 C18 109.1(9) . . ? O12 S3 C18 106.6(6) 6 . ? O12 S3 C18 106.6(6) . . ? O11 S3 C18 106.8(7) 6 . ? O11 S3 C18 106.8(7) . . ? C7 O1 H1E 109.6 . . ? C7 O1 H1C 109.1 . . ? H1E O1 H1C 109.8 . . ? C14 O5 H5D 109.6 . . ? C14 O5 H5B 109.3 . . ? H5D O5 H5B 109.8 . . ? C19 O9 H9A 109.1 . . ? S3 O10 O11 59.6(6) . 6 ? O12 O13 S3 60.5(6) 6 . ? C2 C1 C2 119.5(10) 6 . ? C2 C1 H1A 107.5 6 . ? C2 C1 H1A 107.5 . . ? C2 C1 H1B 107.5 6 . ? C2 C1 H1B 107.5 . . ? H1A C1 H1B 107.0 . . ? C3 C2 C7 117.1(8) . . ? C3 C2 C1 121.0(8) . . ? C7 C2 C1 121.9(9) . . ? C4 C3 C2 120.0(8) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 124.1(8) . . ? C3 C4 S1 119.9(6) . . ? C5 C4 S1 116.0(8) . . ? C4 C5 C6 117.1(9) . . ? C4 C5 H5A 121.4 . . ? C6 C5 H5A 121.4 . . ? C7 C6 C5 118.3(8) . . ? C7 C6 C8 124.0(8) . . ? C5 C6 C8 117.7(9) . . ? C6 C7 O1 118.0(8) . . ? C6 C7 C2 123.2(8) . . ? O1 C7 C2 118.8(9) . . ? C6 C8 C9 113.5(6) . . ? C6 C8 H8A 108.9 . . ? C9 C8 H8A 108.9 . . ? C6 C8 H8B 108.9 . . ? C9 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? C10 C9 C14 117.7(7) . . ? C10 C9 C8 122.6(8) . . ? C14 C9 C8 119.6(8) . . ? C9 C10 C11 122.1(7) . . ? C9 C10 H10 118.9 . . ? C11 C10 H10 118.9 . . ? C12 C11 C10 118.0(7) . . ? C12 C11 S2 123.5(7) . . ? C10 C11 S2 118.5(6) . . ? C11 C12 C13 122.3(7) . . ? C11 C12 H12 118.9 . . ? C13 C12 H12 118.9 . . ? C12 C13 C14 118.6(6) . . ? C12 C13 C15 120.9(6) . . ? C14 C13 C15 120.5(6) . . ? O5 C14 C13 118.9(6) . . ? O5 C14 C9 120.0(6) . . ? C13 C14 C9 121.1(7) . . ? C13 C15 C16 114.2(5) . . ? C13 C15 H15A 108.7 . . ? C16 C15 H15A 108.7 . . ? C13 C15 H15B 108.7 . . ? C16 C15 H15B 108.7 . . ? H15A C15 H15B 107.6 . . ? C17 C16 C19 118.7(6) . . ? C17 C16 C15 119.9(5) . . ? C19 C16 C15 121.4(5) . . ? C16 C17 C18 121.2(6) . . ? C16 C17 H17 119.4 . . ? C18 C17 H17 119.4 . . ? C17 C18 C17 118.9(9) . 6 ? C17 C18 S3 120.6(4) . . ? C17 C18 S3 120.6(4) 6 . ? O9 C19 C16 119.4(4) . 6 ? O9 C19 C16 119.4(4) . . ? C16 C19 C16 121.1(7) 6 . ? C22 N1 C22 120.4(12) 6 . ? C22 N1 C23 119.7(6) 6 . ? C22 N1 C23 119.7(6) . . ? C21 C20 C21 122.0(15) 6 . ? C21 C20 H20 119.0 6 . ? C21 C20 H20 119.0 . . ? C20 C21 C22 120.0(12) . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? N1 C22 C21 118.5(11) . . ? N1 C22 H22 120.7 . . ? C21 C22 H22 120.7 . . ? N1 C23 C24 110.1(11) . 6 ? N1 C23 C24 110.1(11) . . ? C24 C23 C24 20.0(18) 6 . ? N1 C23 H23A 109.8 . . ? C24 C23 H23A 125.5 6 . ? C24 C23 H23A 109.5 . . ? N1 C23 H23B 109.8 . . ? C24 C23 H23B 91.3 6 . ? C24 C23 H23B 109.4 . . ? H23A C23 H23B 108.3 . . ? C24 C24 C24 90.013(4) 6 2_556 ? C24 C24 C23 80.0(9) 6 . ? C24 C24 C23 107.7(14) 2_556 . ? C24 C24 C24 70.2(17) 6 5_556 ? C24 C24 C24 19.8(17) 2_556 5_556 ? C23 C24 C24 103.1(15) . 5_556 ? C24 C24 H24A 44.2 6 . ? C24 C24 H24A 109.2 2_556 . ? C23 C24 H24A 110.5 . . ? C24 C24 H24A 93.8 5_556 . ? C24 C24 H24B 152.1 6 . ? C24 C24 H24B 110.1 2_556 . ? C23 C24 H24B 110.4 . . ? C24 C24 H24B 128.5 5_556 . ? H24A C24 H24B 109.0 . . ? 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 O13 S3 O10 O11 78.5(9) . . . 6 ? O12 S3 O10 O11 13.3(13) 6 . . 6 ? O12 S3 O10 O11 143.8(10) . . . 6 ? O11 S3 O10 O11 157.0(17) . . . 6 ? C18 S3 O10 O11 -101.5(9) . . . 6 ? O10 S3 O13 O12 -81.6(9) . . . 6 ? O12 S3 O13 O12 -163.1(17) . . . 6 ? O11 S3 O13 O12 -16.2(12) 6 . . 6 ? O11 S3 O13 O12 -147.0(10) . . . 6 ? C18 S3 O13 O12 98.4(9) . . . 6 ? C2 C1 C2 C3 -87.4(12) 6 . . . ? C2 C1 C2 C7 95.5(12) 6 . . . ? C7 C2 C3 C4 1.2(10) . . . . ? C1 C2 C3 C4 -175.9(7) . . . . ? C2 C3 C4 C5 1.8(12) . . . . ? C2 C3 C4 S1 -179.2(5) . . . . ? O2' S1 C4 C3 105.0(11) . . . . ? O3 S1 C4 C3 -60.7(10) . . . . ? O3' S1 C4 C3 -21.4(12) . . . . ? O2 S1 C4 C3 59.0(11) . . . . ? O4 S1 C4 C3 -176.1(11) . . . . ? O4' S1 C4 C3 -130.7(12) . . . . ? O2' S1 C4 C5 -75.9(11) . . . . ? O3 S1 C4 C5 118.3(9) . . . . ? O3' S1 C4 C5 157.7(11) . . . . ? O2 S1 C4 C5 -122.0(11) . . . . ? O4 S1 C4 C5 2.9(11) . . . . ? O4' S1 C4 C5 48.3(12) . . . . ? C3 C4 C5 C6 -2.5(11) . . . . ? S1 C4 C5 C6 178.5(5) . . . . ? C4 C5 C6 C7 0.0(10) . . . . ? C4 C5 C6 C8 178.1(6) . . . . ? C5 C6 C7 O1 -177.3(6) . . . . ? C8 C6 C7 O1 4.7(11) . . . . ? C5 C6 C7 C2 3.1(11) . . . . ? C8 C6 C7 C2 -174.9(7) . . . . ? C3 C2 C7 C6 -3.7(11) . . . . ? C1 C2 C7 C6 173.4(7) . . . . ? C3 C2 C7 O1 176.6(6) . . . . ? C1 C2 C7 O1 -6.2(11) . . . . ? C7 C6 C8 C9 -114.6(9) . . . . ? C5 C6 C8 C9 67.4(9) . . . . ? C6 C8 C9 C10 -91.3(9) . . . . ? C6 C8 C9 C14 88.3(9) . . . . ? C14 C9 C10 C11 -1.8(10) . . . . ? C8 C9 C10 C11 177.8(7) . . . . ? C9 C10 C11 C12 4.8(11) . . . . ? C9 C10 C11 S2 -178.8(5) . . . . ? O7 S2 C11 C12 118.3(8) . . . . ? O6 S2 C11 C12 -117.0(8) . . . . ? O8 S2 C11 C12 -8.1(9) . . . . ? O7 S2 C11 C10 -57.9(8) . . . . ? O6 S2 C11 C10 66.8(8) . . . . ? O8 S2 C11 C10 175.7(8) . . . . ? C10 C11 C12 C13 -4.1(10) . . . . ? S2 C11 C12 C13 179.7(5) . . . . ? C11 C12 C13 C14 0.6(9) . . . . ? C11 C12 C13 C15 179.7(6) . . . . ? C12 C13 C14 O5 -178.3(5) . . . . ? C15 C13 C14 O5 2.6(8) . . . . ? C12 C13 C14 C9 2.5(9) . . . . ? C15 C13 C14 C9 -176.6(6) . . . . ? C10 C9 C14 O5 178.9(6) . . . . ? C8 C9 C14 O5 -0.6(9) . . . . ? C10 C9 C14 C13 -1.9(9) . . . . ? C8 C9 C14 C13 178.5(6) . . . . ? C12 C13 C15 C16 106.7(6) . . . . ? C14 C13 C15 C16 -74.2(7) . . . . ? C13 C15 C16 C17 -61.3(7) . . . . ? C13 C15 C16 C19 122.2(7) . . . . ? C19 C16 C17 C18 0.5(10) . . . . ? C15 C16 C17 C18 -176.1(6) . . . . ? C16 C17 C18 C17 3.7(13) . . . 6 ? C16 C17 C18 S3 -176.7(6) . . . . ? O10 S3 C18 C17 -89.8(7) . . . . ? O13 S3 C18 C17 90.2(7) . . . . ? O12 S3 C18 C17 152.8(10) 6 . . . ? O12 S3 C18 C17 27.6(12) . . . . ? O11 S3 C18 C17 -155.9(11) 6 . . . ? O11 S3 C18 C17 -23.7(12) . . . . ? O10 S3 C18 C17 89.8(7) . . . 6 ? O13 S3 C18 C17 -90.2(7) . . . 6 ? O12 S3 C18 C17 -27.6(12) 6 . . 6 ? O12 S3 C18 C17 -152.8(10) . . . 6 ? O11 S3 C18 C17 23.7(12) 6 . . 6 ? O11 S3 C18 C17 155.9(11) . . . 6 ? C17 C16 C19 O9 177.5(6) . . . . ? C15 C16 C19 O9 -5.9(9) . . . . ? C17 C16 C19 C16 -4.8(11) . . . 6 ? C15 C16 C19 C16 171.7(4) . . . 6 ? C21 C20 C21 C22 -1(2) 6 . . . ? C22 N1 C22 C21 8.0(17) 6 . . . ? C23 N1 C22 C21 -177.2(9) . . . . ? C20 C21 C22 N1 -3.7(15) . . . . ? C22 N1 C23 C24 98.1(12) 6 . . 6 ? C22 N1 C23 C24 -76.7(14) . . . 6 ? C22 N1 C23 C24 76.8(14) 6 . . . ? C22 N1 C23 C24 -98.1(12) . . . . ? N1 C23 C24 C24 93.7(4) . . . 6 ? N1 C23 C24 C24 -179.5(3) . . . 2_556 ? C24 C23 C24 C24 86.8(4) 6 . . 2_556 ? N1 C23 C24 C24 160.4(16) . . . 5_556 ? C24 C23 C24 C24 66.7(19) 6 . . 5_556 ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.696 _refine_diff_density_min -0.405 _refine_diff_density_rms 0.145