# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Org.Biomol.Chem. _journal_coden_cambridge 0177 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Yu Liu' _publ_contact_author_email yuliu@nankai.edu.cn loop_ _publ_author_name 'Fei Ding' 'Yu Liu' data_SC4A+MFM _database_code_depnum_ccdc_archive 'CCDC 820613' #TrackingRef 'SC4A+MFM.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H128.50 N20 O50.25 S8' _chemical_formula_sum 'C72 H128.50 N20 O50.25 S8' _chemical_formula_weight 2334.93 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 'C 1 c 1' 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' _cell_length_a 20.657(3) _cell_length_b 18.786(3) _cell_length_c 26.624(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.992(5) _cell_angle_gamma 90.00 _cell_volume 10231(3) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 17443 _cell_measurement_theta_min 1.50 _cell_measurement_theta_max 28.00 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.516 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4922 _exptl_absorpt_coefficient_mu 0.281 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9356 _exptl_absorpt_correction_T_max 0.9511 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator multilayer _diffrn_measurement_device_type 'Rigaku Saturn724 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.222 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 41401 _diffrn_reflns_av_R_equivalents 0.0664 _diffrn_reflns_av_sigmaI/netI 0.1103 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 26.00 _reflns_number_total 19429 _reflns_number_gt 15663 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r2 (Rigaku, 2009)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r2' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure 4.0' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2009)' _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^)+(0.0989P)^2^+13.6089P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.43(8) _refine_ls_number_reflns 19429 _refine_ls_number_parameters 1361 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1042 _refine_ls_R_factor_gt 0.0881 _refine_ls_wR_factor_ref 0.2279 _refine_ls_wR_factor_gt 0.2120 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.16025(9) 0.65217(10) 0.18152(7) 0.0322(4) Uani 1 1 d . . . S2 S -0.02649(8) 0.35026(10) 0.22427(7) 0.0303(4) Uani 1 1 d . . . S3 S 0.15323(7) 0.04296(9) 0.18745(6) 0.0245(3) Uani 1 1 d . . . S4 S 0.37598(8) 0.31334(11) 0.21829(7) 0.0330(4) Uani 1 1 d . . . O1 O 0.1298(2) 0.4303(3) 0.02207(19) 0.0322(11) Uani 1 1 d . . . H1 H 0.0892 0.4276 0.0109 0.039 Uiso 1 1 d R . . O2 O 0.0171(2) 0.3420(3) 0.00988(19) 0.0302(11) Uani 1 1 d . . . H2 H 0.0109 0.2995 -0.0007 0.036 Uiso 1 1 d R . . O3 O 0.1248(2) 0.2500(3) 0.01908(19) 0.0323(11) Uani 1 1 d . . . H3 H 0.1517 0.2379 -0.0008 0.039 Uiso 1 1 d R . . O4 O 0.2318(2) 0.3465(3) 0.00998(19) 0.0309(11) Uani 1 1 d . . . H4 H 0.2561 0.3313 -0.0110 0.037 Uiso 1 1 d R . . O5 O 0.0966(2) 0.6615(3) 0.1987(2) 0.0435(14) Uani 1 1 d . . . O6 O 0.2107(3) 0.6278(3) 0.2226(2) 0.0413(13) Uani 1 1 d . . . O7 O 0.1832(2) 0.7166(3) 0.1578(2) 0.0357(12) Uani 1 1 d . . . O8 O 0.0366(2) 0.3200(3) 0.24919(18) 0.0368(12) Uani 1 1 d . . . O9 O -0.0367(3) 0.4234(3) 0.2383(2) 0.0453(14) Uani 1 1 d . . . O10 O -0.0787(2) 0.3005(3) 0.2318(2) 0.0432(14) Uani 1 1 d . . . O11 O 0.1998(2) 0.0742(3) 0.2280(2) 0.0380(13) Uani 1 1 d . . . O12 O 0.0894(2) 0.0314(3) 0.20392(18) 0.0323(11) Uani 1 1 d . . . O13 O 0.1784(3) -0.0214(3) 0.1661(2) 0.0443(14) Uani 1 1 d . . . O14 O 0.3943(3) 0.2359(3) 0.2230(2) 0.0546(16) Uani 1 1 d . . . O15 O 0.4342(3) 0.3549(4) 0.2221(3) 0.063(2) Uani 1 1 d . . . O16 O 0.3305(3) 0.3309(4) 0.2525(2) 0.067(2) Uani 1 1 d . . . C1 C 0.1385(3) 0.4809(3) 0.0592(2) 0.0224(13) Uani 1 1 d . . . C2 C 0.2020(3) 0.5032(3) 0.0808(3) 0.0243(14) Uani 1 1 d . . . C3 C 0.2082(3) 0.5562(4) 0.1181(3) 0.0264(14) Uani 1 1 d . . . H3A H 0.2503 0.5728 0.1320 0.032 Uiso 1 1 calc R . . C4 C 0.1524(3) 0.5848(4) 0.1352(3) 0.0263(14) Uani 1 1 d . . . C5 C 0.0899(3) 0.5621(3) 0.1141(2) 0.0204(13) Uani 1 1 d . . . H5A H 0.0523 0.5824 0.1254 0.025 Uiso 1 1 calc R . . C6 C 0.0829(3) 0.5101(4) 0.0767(2) 0.0268(14) Uani 1 1 d . . . C7 C 0.0146(3) 0.4831(3) 0.0568(3) 0.0238(14) Uani 1 1 d . . . H7A H 0.0107 0.4757 0.0197 0.029 Uiso 1 1 calc R . . H7B H -0.0183 0.5189 0.0635 0.029 Uiso 1 1 calc R . . C8 C 0.0060(3) 0.3464(3) 0.0591(3) 0.0260(15) Uani 1 1 d . . . C9 C 0.0019(3) 0.4123(4) 0.0832(2) 0.0217(13) Uani 1 1 d . . . C10 C -0.0105(3) 0.4139(4) 0.1331(3) 0.0263(15) Uani 1 1 d . . . H10A H -0.0125 0.4583 0.1500 0.032 Uiso 1 1 calc R . . C11 C -0.0201(3) 0.3496(4) 0.1591(3) 0.0273(15) Uani 1 1 d . . . C12 C -0.0166(3) 0.2847(4) 0.1346(3) 0.0270(15) Uani 1 1 d . . . H12A H -0.0233 0.2417 0.1520 0.032 Uiso 1 1 calc R . . C13 C -0.0034(3) 0.2819(3) 0.0843(3) 0.0231(14) Uani 1 1 d . . . C14 C 0.0050(3) 0.2106(3) 0.0602(2) 0.0222(13) Uani 1 1 d . . . H14A H -0.0010 0.2159 0.0228 0.027 Uiso 1 1 calc R . . H14B H -0.0287 0.1773 0.0691 0.027 Uiso 1 1 calc R . . C15 C 0.1283(3) 0.2003(3) 0.0575(2) 0.0221(13) Uani 1 1 d . . . C16 C 0.0728(3) 0.1801(4) 0.0781(2) 0.0241(14) Uani 1 1 d . . . C17 C 0.0800(3) 0.1314(4) 0.1185(2) 0.0238(14) Uani 1 1 d . . . H17A H 0.0430 0.1167 0.1335 0.029 Uiso 1 1 calc R . . C18 C 0.1430(3) 0.1047(3) 0.1367(3) 0.0234(13) Uani 1 1 d . . . C19 C 0.1968(3) 0.1250(4) 0.1151(3) 0.0250(14) Uani 1 1 d . . . H19A H 0.2385 0.1057 0.1275 0.030 Uiso 1 1 calc R . . C20 C 0.1912(3) 0.1731(3) 0.0755(2) 0.0222(13) Uani 1 1 d . . . C21 C 0.2513(3) 0.1992(4) 0.0523(3) 0.0243(14) Uani 1 1 d . . . H21A H 0.2857 0.1620 0.0560 0.029 Uiso 1 1 calc R . . H21B H 0.2389 0.2089 0.0156 0.029 Uiso 1 1 calc R . . C22 C 0.2639(3) 0.3364(4) 0.0586(3) 0.0236(14) Uani 1 1 d . . . C23 C 0.2774(3) 0.2671(3) 0.0795(2) 0.0186(12) Uani 1 1 d . . . C24 C 0.3124(3) 0.2625(4) 0.1276(3) 0.0247(14) Uani 1 1 d . . . H24A H 0.3228 0.2169 0.1419 0.030 Uiso 1 1 calc R . . C25 C 0.3331(3) 0.3240(4) 0.1562(3) 0.0297(15) Uani 1 1 d . . . C26 C 0.3172(3) 0.3904(4) 0.1358(3) 0.0323(16) Uani 1 1 d . . . H26A H 0.3297 0.4318 0.1553 0.039 Uiso 1 1 calc R . . C27 C 0.2825(3) 0.3975(4) 0.0866(3) 0.0284(15) Uani 1 1 d . . . C28 C 0.2643(3) 0.4719(4) 0.0640(3) 0.0308(16) Uani 1 1 d . . . H28A H 0.3011 0.5050 0.0742 0.037 Uiso 1 1 calc R . . H28B H 0.2581 0.4685 0.0265 0.037 Uiso 1 1 calc R . . S5 S 0.03544(8) -0.16571(10) 0.41083(7) 0.0302(4) Uani 1 1 d . . . S6 S 0.23858(8) 0.15541(9) 0.37002(7) 0.0264(4) Uani 1 1 d . . . S7 S 0.02674(8) 0.46500(9) 0.40723(6) 0.0255(4) Uani 1 1 d . . . S8 S -0.17398(8) 0.15225(9) 0.36918(7) 0.0286(4) Uani 1 1 d . . . O17 O 0.0590(2) 0.0611(2) 0.56718(19) 0.0279(11) Uani 1 1 d . . . H17B H 0.0932 0.0864 0.5673 0.033 Uiso 1 1 d R . . O18 O 0.1647(2) 0.1517(2) 0.57746(18) 0.0270(11) Uani 1 1 d . . . H18A H 0.1327 0.1796 0.5791 0.032 Uiso 1 1 d R . . O19 O 0.0646(2) 0.2453(3) 0.56798(18) 0.0280(10) Uani 1 1 d . . . H19B H 0.0331 0.2281 0.5816 0.034 Uiso 1 1 d R . . O20 O -0.0421(2) 0.1588(2) 0.58171(19) 0.0269(11) Uani 1 1 d . . . H20A H -0.0425 0.1181 0.5955 0.032 Uiso 1 1 d R . . O21 O -0.0155(2) -0.1460(3) 0.3709(2) 0.0382(13) Uani 1 1 d . . . O22 O 0.0129(3) -0.2285(3) 0.4374(2) 0.0462(14) Uani 1 1 d . . . O23 O 0.0985(3) -0.1761(3) 0.3933(2) 0.0473(15) Uani 1 1 d . . . O24 O 0.1775(2) 0.1592(3) 0.33445(19) 0.0351(13) Uani 1 1 d . . . O25 O 0.2746(2) 0.0887(3) 0.3650(2) 0.0343(12) Uani 1 1 d . . . O26 O 0.2797(2) 0.2198(3) 0.36610(18) 0.0286(10) Uani 1 1 d . . . O27 O -0.0127(2) 0.4293(3) 0.36383(19) 0.0340(12) Uani 1 1 d . . . O28 O 0.0922(2) 0.4834(3) 0.39551(18) 0.0284(10) Uani 1 1 d . . . O29 O -0.0066(2) 0.5263(3) 0.42559(18) 0.0312(11) Uani 1 1 d . . . O30 O -0.1437(3) 0.0988(3) 0.3414(2) 0.0441(14) Uani 1 1 d . . . O31 O -0.1693(3) 0.2233(3) 0.34859(19) 0.0379(12) Uani 1 1 d . . . O32 O -0.2422(2) 0.1337(3) 0.3745(2) 0.0379(13) Uani 1 1 d . . . C29 C 0.0574(3) 0.0104(3) 0.5291(3) 0.0242(14) Uani 1 1 d . . . C30 C -0.0050(3) -0.0161(4) 0.5107(3) 0.0261(14) Uani 1 1 d . . . C31 C -0.0109(3) -0.0683(3) 0.4743(3) 0.0245(14) Uani 1 1 d . . . H31A H -0.0528 -0.0874 0.4623 0.029 Uiso 1 1 calc R . . C32 C 0.0438(3) -0.0937(3) 0.4548(3) 0.0231(13) Uani 1 1 d . . . C33 C 0.1070(3) -0.0670(4) 0.4735(3) 0.0277(15) Uani 1 1 d . . . H33A H 0.1445 -0.0853 0.4609 0.033 Uiso 1 1 calc R . . C34 C 0.1135(3) -0.0134(3) 0.5106(3) 0.0238(14) Uani 1 1 d . . . C35 C 0.1796(3) 0.0175(4) 0.5299(3) 0.0258(14) Uani 1 1 d . . . H35A H 0.2141 -0.0163 0.5228 0.031 Uiso 1 1 calc R . . H35B H 0.1835 0.0239 0.5671 0.031 Uiso 1 1 calc R . . C36 C 0.1817(3) 0.1547(3) 0.5287(2) 0.0209(13) Uani 1 1 d . . . C37 C 0.1904(3) 0.0894(4) 0.5049(3) 0.0242(14) Uani 1 1 d . . . C38 C 0.2097(3) 0.0914(3) 0.4571(2) 0.0225(13) Uani 1 1 d . . . H38A H 0.2182 0.0479 0.4410 0.027 Uiso 1 1 calc R . . C39 C 0.2171(3) 0.1548(3) 0.4321(2) 0.0207(13) Uani 1 1 d . . . C40 C 0.2055(3) 0.2195(4) 0.4566(3) 0.0245(14) Uani 1 1 d . . . H40A H 0.2101 0.2634 0.4396 0.029 Uiso 1 1 calc R . . C41 C 0.1876(3) 0.2200(3) 0.5051(2) 0.0212(13) Uani 1 1 d . . . C42 C 0.1765(3) 0.2934(3) 0.5295(3) 0.0251(14) Uani 1 1 d . . . H42A H 0.1820 0.2883 0.5669 0.030 Uiso 1 1 calc R . . H42B H 0.2097 0.3277 0.5209 0.030 Uiso 1 1 calc R . . C43 C 0.0523(3) 0.2960(3) 0.5312(2) 0.0201(13) Uani 1 1 d . . . C44 C 0.1092(3) 0.3216(3) 0.5110(3) 0.0237(14) Uani 1 1 d . . . C45 C 0.0999(3) 0.3737(4) 0.4743(3) 0.0248(14) Uani 1 1 d . . . H45A H 0.1369 0.3915 0.4608 0.030 Uiso 1 1 calc R . . C46 C 0.0384(3) 0.4014(4) 0.4560(3) 0.0246(14) Uani 1 1 d . . . C47 C -0.0158(3) 0.3752(4) 0.4759(2) 0.0250(14) Uani 1 1 d . . . H47A H -0.0579 0.3938 0.4639 0.030 Uiso 1 1 calc R . . C48 C -0.0097(3) 0.3218(3) 0.5131(3) 0.0230(14) Uani 1 1 d . . . C49 C -0.0692(3) 0.2908(3) 0.5329(3) 0.0246(14) Uani 1 1 d . . . H49A H -0.1066 0.3240 0.5255 0.029 Uiso 1 1 calc R . . H49B H -0.0598 0.2849 0.5702 0.029 Uiso 1 1 calc R . . C50 C -0.0717(3) 0.1536(3) 0.5319(3) 0.0231(14) Uani 1 1 d . . . C51 C -0.0873(3) 0.2184(4) 0.5080(2) 0.0240(14) Uani 1 1 d . . . C52 C -0.1191(3) 0.2180(4) 0.4568(2) 0.0246(14) Uani 1 1 d . . . H52A H -0.1315 0.2615 0.4400 0.030 Uiso 1 1 calc R . . C53 C -0.1317(3) 0.1537(4) 0.4318(3) 0.0242(14) Uani 1 1 d . . . C54 C -0.1151(3) 0.0896(4) 0.4565(3) 0.0283(15) Uani 1 1 d . . . H54A H -0.1250 0.0459 0.4391 0.034 Uiso 1 1 calc R . . C55 C -0.0839(3) 0.0888(4) 0.5066(3) 0.0266(15) Uani 1 1 d . . . C56 C -0.0650(3) 0.0149(4) 0.5302(3) 0.0268(15) Uani 1 1 d . . . H56A H -0.0561 0.0195 0.5676 0.032 Uiso 1 1 calc R . . H56B H -0.1023 -0.0182 0.5220 0.032 Uiso 1 1 calc R . . N1 N 0.1274(3) 0.3962(3) 0.3155(2) 0.0311(13) Uani 1 1 d . . . H1B H 0.1130 0.4303 0.3338 0.037 Uiso 1 1 calc R . . H1C H 0.1014 0.3776 0.2899 0.037 Uiso 1 1 calc R . . N2 N 0.2286(3) 0.3998(4) 0.3648(2) 0.0386(15) Uani 1 1 d . . . H2B H 0.2164 0.4339 0.3841 0.046 Uiso 1 1 calc R . . H2C H 0.2685 0.3826 0.3707 0.046 Uiso 1 1 calc R . . N3 N 0.2101(3) 0.3190(3) 0.2994(2) 0.0299(13) Uani 1 1 d . . . H3C H 0.2410 0.2922 0.3159 0.036 Uiso 1 1 calc R . . N4 N 0.1849(3) 0.2321(3) 0.2402(2) 0.0337(14) Uani 1 1 d . . . H4B H 0.1729 0.2166 0.2091 0.040 Uiso 1 1 calc R . . H4C H 0.1935 0.2015 0.2653 0.040 Uiso 1 1 calc R . . N5 N 0.1782(3) 0.3510(3) 0.2142(2) 0.0281(13) Uani 1 1 d . . . C57 C 0.1861(4) 0.3739(4) 0.3262(3) 0.0329(16) Uani 1 1 d . . . C58 C 0.1901(3) 0.3026(4) 0.2494(3) 0.0253(14) Uani 1 1 d . . . C59 C 0.1493(3) 0.3308(4) 0.1626(3) 0.0344(17) Uani 1 1 d . . . H59A H 0.1377 0.2802 0.1620 0.052 Uiso 1 1 calc R . . H59B H 0.1810 0.3394 0.1391 0.052 Uiso 1 1 calc R . . H59C H 0.1099 0.3593 0.1523 0.052 Uiso 1 1 calc R . . C60 C 0.1993(4) 0.4271(4) 0.2210(3) 0.0374(18) Uani 1 1 d . . . H60A H 0.2181 0.4351 0.2564 0.056 Uiso 1 1 calc R . . H60B H 0.1614 0.4583 0.2123 0.056 Uiso 1 1 calc R . . H60C H 0.2321 0.4376 0.1988 0.056 Uiso 1 1 calc R . . N6 N 0.0496(4) -0.0565(4) 0.3089(3) 0.054(2) Uani 1 1 d . . . H6A H 0.0872 -0.0565 0.2969 0.065 Uiso 1 1 calc R . . H6B H 0.0336 -0.0966 0.3191 0.065 Uiso 1 1 calc R . . N7 N -0.0388(3) 0.0048(4) 0.3314(3) 0.054(2) Uani 1 1 d . . . H7C H -0.0543 -0.0347 0.3429 0.065 Uiso 1 1 calc R . . H7D H -0.0602 0.0451 0.3330 0.065 Uiso 1 1 calc R . . N8 N 0.0425(3) 0.0632(4) 0.2957(3) 0.0470(18) Uani 1 1 d . . . H8A H 0.0754 0.0571 0.2784 0.056 Uiso 1 1 calc R . . N9 N 0.0135(4) 0.1708(4) 0.2619(3) 0.063(2) Uani 1 1 d . . . H9A H 0.0030 0.2160 0.2639 0.075 Uiso 1 1 calc R . . H9B H 0.0160 0.1513 0.2322 0.075 Uiso 1 1 calc R . . N10 N 0.0229(3) 0.1569(3) 0.3499(3) 0.0414(17) Uani 1 1 d . . . C61 C 0.0171(4) 0.0036(4) 0.3115(3) 0.0412(19) Uani 1 1 d . . . C62 C 0.0252(4) 0.1332(5) 0.3025(4) 0.042(2) Uani 1 1 d . . . C63 C 0.0489(4) 0.1221(5) 0.3967(3) 0.052(2) Uani 1 1 d . . . H63A H 0.0619 0.0734 0.3894 0.078 Uiso 1 1 calc R . . H63B H 0.0153 0.1207 0.4193 0.078 Uiso 1 1 calc R . . H63C H 0.0870 0.1485 0.4130 0.078 Uiso 1 1 calc R . . C64 C 0.0011(5) 0.2322(5) 0.3555(3) 0.052(2) Uani 1 1 d . . . H64A H -0.0153 0.2517 0.3220 0.078 Uiso 1 1 calc R . . H64B H 0.0380 0.2609 0.3712 0.078 Uiso 1 1 calc R . . H64C H -0.0339 0.2332 0.3769 0.078 Uiso 1 1 calc R . . N16 N 0.2995(3) -0.2263(3) 0.1377(2) 0.0339(14) Uani 1 1 d . . . H16A H 0.3227 -0.2396 0.1140 0.041 Uiso 1 1 calc R . . H16B H 0.2819 -0.2585 0.1556 0.041 Uiso 1 1 calc R . . N17 N 0.3171(3) -0.1076(4) 0.1200(2) 0.0359(15) Uani 1 1 d . . . H17C H 0.3405 -0.1194 0.0961 0.043 Uiso 1 1 calc R . . H17D H 0.3107 -0.0624 0.1266 0.043 Uiso 1 1 calc R . . N18 N 0.2529(3) -0.1383(3) 0.1831(2) 0.0240(12) Uani 1 1 d . . . H18B H 0.2322 -0.0974 0.1785 0.029 Uiso 1 1 calc R . . N19 N 0.2938(3) -0.2142(3) 0.2491(2) 0.0321(14) Uani 1 1 d . . . H19C H 0.2892 -0.2391 0.2764 0.039 Uiso 1 1 calc R . . H19D H 0.3315 -0.2143 0.2372 0.039 Uiso 1 1 calc R . . N20 N 0.1870(3) -0.1751(4) 0.2427(2) 0.0330(14) Uani 1 1 d . . . C69 C 0.2912(3) -0.1583(4) 0.1464(3) 0.0300(16) Uani 1 1 d . . . C70 C 0.2444(3) -0.1768(4) 0.2261(3) 0.0280(15) Uani 1 1 d . . . C71 C 0.1244(4) -0.1561(4) 0.2114(3) 0.043(2) Uani 1 1 d . . . H71A H 0.1333 -0.1353 0.1793 0.064 Uiso 1 1 calc R . . H71B H 0.1010 -0.1215 0.2296 0.064 Uiso 1 1 calc R . . H71C H 0.0977 -0.1990 0.2045 0.064 Uiso 1 1 calc R . . C72 C 0.1791(4) -0.2081(5) 0.2920(3) 0.0422(19) Uani 1 1 d . . . H72A H 0.2222 -0.2195 0.3105 0.063 Uiso 1 1 calc R . . H72B H 0.1533 -0.2518 0.2861 0.063 Uiso 1 1 calc R . . H72C H 0.1565 -0.1747 0.3119 0.063 Uiso 1 1 calc R . . N11 N 0.3360(3) 0.1058(3) 0.2506(2) 0.0337(14) Uani 1 1 d . . . H11A H 0.2957 0.1101 0.2350 0.040 Uiso 1 1 calc R . . H11B H 0.3638 0.1412 0.2500 0.040 Uiso 1 1 calc R . . N12 N 0.3151(3) -0.0087(3) 0.2769(2) 0.0363(15) Uani 1 1 d . . . H12B H 0.2745 -0.0059 0.2616 0.044 Uiso 1 1 calc R . . H12C H 0.3288 -0.0478 0.2933 0.044 Uiso 1 1 calc R . . N13 N 0.4186(3) 0.0366(3) 0.2982(2) 0.0318(14) Uani 1 1 d . . . H13A H 0.4262 -0.0022 0.3166 0.038 Uiso 1 1 calc R . . N14 N 0.5231(3) 0.0508(3) 0.2806(2) 0.0351(14) Uani 1 1 d . . . H14C H 0.5587 0.0761 0.2795 0.042 Uiso 1 1 calc R . . H14D H 0.5219 0.0058 0.2713 0.042 Uiso 1 1 calc R . . N15 N 0.4696(3) 0.1490(3) 0.3112(2) 0.0305(13) Uani 1 1 d . . . C65 C 0.3550(3) 0.0453(4) 0.2751(3) 0.0291(15) Uani 1 1 d . . . C66 C 0.4716(4) 0.0802(4) 0.2962(3) 0.0351(17) Uani 1 1 d . . . C67 C 0.4237(4) 0.1744(4) 0.3445(3) 0.0372(18) Uani 1 1 d . . . H67A H 0.3901 0.1381 0.3467 0.056 Uiso 1 1 calc R . . H67B H 0.4029 0.2184 0.3307 0.056 Uiso 1 1 calc R . . H67C H 0.4473 0.1836 0.3784 0.056 Uiso 1 1 calc R . . C68 C 0.5236(4) 0.1978(5) 0.3038(3) 0.0418(19) Uani 1 1 d . . . H68A H 0.5513 0.1755 0.2813 0.063 Uiso 1 1 calc R . . H68B H 0.5497 0.2079 0.3367 0.063 Uiso 1 1 calc R . . H68C H 0.5055 0.2423 0.2887 0.063 Uiso 1 1 calc R . . O33 O 0.4792(2) 0.4490(3) 0.15723(19) 0.0343(12) Uani 1 1 d . . . H33B H 0.4696 0.4171 0.1776 0.051 Uiso 1 1 d R . . H33C H 0.5046 0.4786 0.1742 0.051 Uiso 1 1 d R . . O34 O 0.3613(3) -0.1233(3) 0.3525(2) 0.0416(13) Uani 1 1 d . . . H34A H 0.4005 -0.1145 0.3652 0.062 Uiso 1 1 d R . . H34B H 0.3569 -0.1682 0.3507 0.062 Uiso 1 1 d R . . O35 O 0.3521(3) -0.1618(3) 0.0278(2) 0.0517(16) Uani 1 1 d . . . H35C H 0.3837 -0.1580 0.0107 0.078 Uiso 1 1 d R . . H35D H 0.3185 -0.1743 0.0077 0.078 Uiso 1 1 d R . . O36 O 0.4320(3) 0.4097(3) 0.6731(3) 0.0575(17) Uani 1 1 d . . . O37 O 0.3713(2) 0.0593(3) 0.4519(2) 0.0443(14) Uani 1 1 d . . . H37A H 0.3477 0.0736 0.4251 0.066 Uiso 1 1 d R . . H37B H 0.4090 0.0499 0.4443 0.066 Uiso 1 1 d R . . O38 O 0.3336(2) 0.0530(3) 0.0091(2) 0.0374(12) Uani 1 1 d . . . O39 O 0.2628(3) -0.1133(3) 0.4173(2) 0.0505(15) Uani 1 1 d . . . H39A H 0.2826 -0.1048 0.3920 0.076 Uiso 1 1 d R . . H39B H 0.2444 -0.1536 0.4126 0.076 Uiso 1 1 d R . . O40 O 0.6575(3) 0.0690(3) 0.3035(2) 0.0529(16) Uani 1 1 d . . . H40B H 0.6819 0.0812 0.3305 0.079 Uiso 1 1 d R . . H40C H 0.6751 0.0842 0.2785 0.079 Uiso 1 1 d R . . O41 O 0.3562(3) 0.3919(4) 0.3474(3) 0.0598(17) Uani 1 1 d . . . H41A H 0.3510 0.3817 0.3160 0.090 Uiso 1 1 d R . . H41B H 0.3838 0.3627 0.3625 0.090 Uiso 1 1 d R . . O42 O 0.7211(2) 0.0142(3) 0.4344(2) 0.0402(13) Uani 1 1 d . . . H42A H 0.7519 0.0438 0.4326 0.060 Uiso 1 1 d R . . H42B H 0.7091 0.0186 0.4635 0.060 Uiso 1 1 d R . . O43 O 0.3508(3) 0.3412(3) 0.5873(3) 0.0585(18) Uani 1 1 d . . . H43A H 0.3880 0.3541 0.6022 0.088 Uiso 1 1 d R . . H43B H 0.3300 0.3230 0.6096 0.088 Uiso 1 1 d R . . O44 O 0.7101(3) 0.2492(3) 0.4296(2) 0.0443(14) Uani 1 1 d . . . H44A H 0.7235 0.2092 0.4203 0.066 Uiso 1 1 d R . . H44B H 0.6695 0.2522 0.4187 0.066 Uiso 1 1 d R . . O45 O 0.3086(3) 0.3955(3) 0.4889(2) 0.0486(15) Uani 1 1 d . . . H45B H 0.2910 0.4291 0.4705 0.073 Uiso 1 1 d R . . H45C H 0.2861 0.3891 0.5129 0.073 Uiso 1 1 d R . . O46 O 0.1879(3) -0.0326(3) 0.3313(3) 0.0640(19) Uani 1 1 d . . . H46A H 0.2084 0.0067 0.3341 0.096 Uiso 1 1 d R . . H46B H 0.1894 -0.0502 0.3608 0.096 Uiso 1 1 d R . . O47 O 0.3699(3) 0.2801(3) 0.4472(2) 0.0556(18) Uani 1 1 d . . . H47B H 0.3432 0.2630 0.4223 0.083 Uiso 1 1 d R . . H47C H 0.4079 0.2656 0.4430 0.083 Uiso 1 1 d R . . O48 O 0.3500(3) 0.0459(3) 0.1192(2) 0.0566(17) Uani 1 1 d . . . H48A H 0.3482 0.0485 0.0868 0.085 Uiso 1 1 d R . . H48B H 0.3894 0.0539 0.1318 0.085 Uiso 1 1 d R . . O49 O 0.4565(3) 0.1397(4) 0.1667(3) 0.073(2) Uani 1 1 d . . . H49C H 0.4377 0.1765 0.1757 0.109 Uiso 1 1 d R . . H49D H 0.4976 0.1446 0.1765 0.109 Uiso 1 1 d R . . O50 O 0.8328(4) 0.0773(6) 0.2319(3) 0.075(3) Uani 0.75 1 d P . . O51 O 0.5955(8) 0.1460(8) 0.4162(6) 0.078(5) Uani 0.50 1 d P . . 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 0.0310(9) 0.0329(10) 0.0323(10) -0.0089(7) 0.0029(7) -0.0027(7) S2 0.0252(8) 0.0367(10) 0.0290(9) -0.0020(7) 0.0045(7) -0.0029(7) S3 0.0248(8) 0.0214(8) 0.0264(9) 0.0005(6) 0.0007(6) 0.0010(7) S4 0.0217(8) 0.0423(11) 0.0342(10) -0.0004(8) 0.0014(6) -0.0016(8) O1 0.025(2) 0.028(3) 0.042(3) -0.007(2) -0.002(2) 0.002(2) O2 0.042(3) 0.023(3) 0.026(3) 0.0002(19) 0.007(2) -0.004(2) O3 0.036(3) 0.028(3) 0.035(3) 0.009(2) 0.011(2) 0.004(2) O4 0.029(3) 0.038(3) 0.026(3) 0.006(2) 0.006(2) 0.009(2) O5 0.027(3) 0.057(4) 0.048(4) -0.015(3) 0.009(2) -0.006(2) O6 0.040(3) 0.053(4) 0.027(3) -0.003(3) -0.009(2) 0.002(3) O7 0.037(3) 0.026(3) 0.045(3) -0.003(2) 0.010(2) -0.011(2) O8 0.025(2) 0.066(4) 0.018(2) 0.003(2) -0.0042(18) -0.001(2) O9 0.055(3) 0.044(3) 0.038(3) -0.006(3) 0.010(3) 0.000(3) O10 0.033(3) 0.062(4) 0.036(3) -0.004(3) 0.011(2) -0.014(3) O11 0.034(3) 0.044(3) 0.033(3) 0.006(2) -0.009(2) -0.011(2) O12 0.031(3) 0.038(3) 0.027(3) 0.006(2) -0.0006(19) -0.006(2) O13 0.069(4) 0.023(3) 0.044(3) 0.002(2) 0.019(3) 0.012(3) O14 0.061(4) 0.042(4) 0.055(4) 0.010(3) -0.012(3) -0.001(3) O15 0.041(3) 0.085(5) 0.058(4) 0.034(4) -0.017(3) -0.027(3) O16 0.047(4) 0.120(6) 0.032(3) -0.012(4) 0.000(3) 0.025(4) C1 0.023(3) 0.015(3) 0.029(4) -0.001(3) 0.000(2) -0.005(3) C2 0.024(3) 0.016(3) 0.033(4) 0.000(3) 0.005(3) 0.003(3) C3 0.021(3) 0.027(4) 0.031(4) -0.001(3) 0.007(3) -0.006(3) C4 0.033(4) 0.020(3) 0.025(4) -0.003(3) 0.004(3) 0.000(3) C5 0.016(3) 0.023(3) 0.022(3) 0.000(2) 0.003(2) 0.003(2) C6 0.030(3) 0.029(4) 0.019(3) 0.005(3) 0.000(3) 0.002(3) C7 0.023(3) 0.017(3) 0.031(4) 0.002(3) 0.001(3) 0.006(3) C8 0.027(3) 0.017(3) 0.030(4) 0.004(3) -0.006(3) -0.001(3) C9 0.013(3) 0.024(3) 0.028(3) 0.002(3) 0.001(2) 0.005(2) C10 0.014(3) 0.026(4) 0.038(4) -0.007(3) 0.001(3) 0.001(3) C11 0.021(3) 0.034(4) 0.027(4) -0.003(3) 0.001(3) 0.002(3) C12 0.022(3) 0.030(4) 0.029(4) -0.001(3) 0.000(3) 0.006(3) C13 0.020(3) 0.020(3) 0.029(4) 0.001(3) 0.003(2) 0.003(3) C14 0.028(3) 0.020(3) 0.019(3) 0.003(2) 0.005(2) 0.002(3) C15 0.023(3) 0.021(3) 0.023(3) 0.000(3) 0.004(2) 0.002(3) C16 0.026(3) 0.024(4) 0.021(3) -0.003(3) -0.001(2) -0.002(3) C17 0.028(3) 0.021(3) 0.022(3) -0.002(3) 0.001(2) 0.001(3) C18 0.024(3) 0.018(3) 0.030(4) -0.001(3) 0.007(3) -0.002(3) C19 0.026(3) 0.020(3) 0.030(4) -0.003(3) 0.005(3) 0.007(3) C20 0.023(3) 0.019(3) 0.024(3) 0.000(3) 0.001(2) -0.001(3) C21 0.022(3) 0.023(3) 0.028(4) 0.000(3) 0.002(3) -0.001(3) C22 0.020(3) 0.024(3) 0.028(4) 0.003(3) 0.009(3) -0.002(3) C23 0.017(3) 0.019(3) 0.020(3) 0.003(2) 0.001(2) -0.001(2) C24 0.019(3) 0.024(3) 0.032(4) -0.003(3) 0.008(3) 0.001(3) C25 0.019(3) 0.038(4) 0.032(4) 0.002(3) 0.004(3) -0.006(3) C26 0.018(3) 0.039(4) 0.039(4) -0.008(3) 0.002(3) 0.003(3) C27 0.016(3) 0.026(4) 0.045(4) 0.004(3) 0.009(3) 0.002(3) C28 0.017(3) 0.027(4) 0.048(4) -0.006(3) 0.004(3) -0.008(3) S5 0.0272(8) 0.0349(10) 0.0264(9) -0.0033(7) -0.0029(7) 0.0052(7) S6 0.0274(8) 0.0262(9) 0.0256(9) 0.0014(7) 0.0038(6) -0.0031(7) S7 0.0263(8) 0.0235(9) 0.0263(9) 0.0026(7) 0.0024(6) 0.0013(7) S8 0.0255(8) 0.0284(10) 0.0311(9) -0.0024(7) 0.0010(7) 0.0018(7) O17 0.024(2) 0.015(2) 0.045(3) -0.008(2) 0.006(2) -0.0038(19) O18 0.032(3) 0.022(3) 0.027(3) 0.0029(19) 0.000(2) -0.0003(19) O19 0.023(2) 0.035(3) 0.028(3) 0.010(2) 0.0076(18) 0.002(2) O20 0.030(2) 0.021(2) 0.031(3) 0.0037(19) 0.007(2) -0.0002(19) O21 0.029(3) 0.043(3) 0.038(3) -0.001(2) -0.012(2) 0.001(2) O22 0.068(4) 0.034(3) 0.035(3) -0.005(2) 0.000(3) -0.007(3) O23 0.034(3) 0.064(4) 0.045(4) -0.015(3) 0.008(2) -0.005(3) O24 0.023(2) 0.051(4) 0.028(3) 0.004(2) -0.007(2) -0.013(2) O25 0.045(3) 0.016(2) 0.045(3) -0.007(2) 0.017(2) 0.002(2) O26 0.029(2) 0.025(3) 0.033(3) 0.005(2) 0.0053(19) 0.001(2) O27 0.032(3) 0.036(3) 0.031(3) 0.001(2) -0.007(2) -0.002(2) O28 0.026(2) 0.029(3) 0.030(3) 0.002(2) 0.0063(19) 0.002(2) O29 0.037(3) 0.027(3) 0.031(3) 0.007(2) 0.008(2) 0.010(2) O30 0.048(3) 0.053(4) 0.030(3) -0.008(3) 0.001(2) 0.016(3) O31 0.049(3) 0.037(3) 0.025(3) 0.004(2) -0.003(2) -0.005(2) O32 0.018(2) 0.038(3) 0.055(4) -0.009(3) -0.003(2) -0.008(2) C29 0.024(3) 0.019(3) 0.030(4) 0.001(3) 0.003(3) 0.007(3) C30 0.027(3) 0.020(3) 0.032(4) 0.008(3) 0.006(3) 0.009(3) C31 0.021(3) 0.019(3) 0.032(4) 0.000(3) -0.003(2) 0.001(3) C32 0.024(3) 0.021(3) 0.025(3) 0.005(3) 0.006(2) 0.004(3) C33 0.024(3) 0.026(4) 0.035(4) 0.007(3) 0.011(3) 0.005(3) C34 0.018(3) 0.020(3) 0.034(4) 0.005(3) 0.008(3) 0.002(3) C35 0.022(3) 0.028(4) 0.029(4) 0.007(3) 0.011(3) 0.001(3) C36 0.017(3) 0.025(4) 0.021(3) -0.005(2) 0.003(2) 0.000(2) C37 0.011(3) 0.025(4) 0.036(4) 0.006(3) 0.001(2) 0.005(2) C38 0.022(3) 0.017(3) 0.028(4) 0.002(3) 0.002(2) -0.004(2) C39 0.017(3) 0.027(4) 0.019(3) 0.000(2) 0.004(2) 0.006(2) C40 0.018(3) 0.020(3) 0.035(4) 0.005(3) -0.001(3) -0.003(3) C41 0.019(3) 0.023(3) 0.021(3) 0.001(3) -0.001(2) 0.001(3) C42 0.023(3) 0.014(3) 0.038(4) -0.003(3) 0.002(3) -0.001(3) C43 0.029(3) 0.018(3) 0.014(3) -0.001(2) 0.005(2) -0.001(3) C44 0.023(3) 0.019(3) 0.026(3) -0.004(3) -0.005(2) -0.001(3) C45 0.020(3) 0.019(3) 0.035(4) -0.007(3) 0.005(3) -0.003(3) C46 0.029(3) 0.019(3) 0.025(3) 0.000(3) 0.001(3) -0.002(3) C47 0.027(3) 0.027(4) 0.018(3) 0.003(3) -0.005(2) 0.001(3) C48 0.023(3) 0.013(3) 0.032(4) -0.005(3) 0.002(3) -0.001(3) C49 0.026(3) 0.015(3) 0.034(4) 0.002(3) 0.007(3) -0.003(3) C50 0.020(3) 0.023(4) 0.025(4) 0.003(3) 0.002(3) 0.001(3) C51 0.024(3) 0.023(4) 0.024(3) -0.005(3) 0.003(2) -0.002(3) C52 0.021(3) 0.029(4) 0.022(3) 0.001(3) -0.002(2) 0.003(3) C53 0.013(3) 0.033(4) 0.026(4) 0.007(3) 0.000(2) 0.000(3) C54 0.021(3) 0.022(4) 0.043(4) -0.004(3) 0.007(3) -0.001(3) C55 0.015(3) 0.025(4) 0.039(4) 0.002(3) 0.001(3) 0.001(3) C56 0.020(3) 0.023(4) 0.038(4) -0.002(3) 0.009(3) 0.001(3) N1 0.036(3) 0.029(3) 0.028(3) -0.005(2) 0.007(2) 0.006(3) N2 0.035(3) 0.040(4) 0.039(4) -0.010(3) -0.001(3) 0.009(3) N3 0.040(3) 0.020(3) 0.028(3) -0.002(2) -0.003(2) 0.005(3) N4 0.039(3) 0.027(3) 0.032(3) -0.002(3) -0.005(3) 0.002(3) N5 0.025(3) 0.038(4) 0.021(3) 0.003(2) 0.001(2) 0.004(2) C57 0.043(4) 0.034(4) 0.020(3) -0.007(3) -0.003(3) 0.010(3) C58 0.019(3) 0.033(4) 0.025(3) -0.002(3) 0.004(2) -0.002(3) C59 0.027(3) 0.048(5) 0.025(4) -0.009(3) -0.003(3) 0.004(3) C60 0.034(4) 0.020(4) 0.058(5) 0.008(3) 0.004(3) 0.004(3) N6 0.054(4) 0.036(4) 0.077(6) 0.013(4) 0.028(4) 0.016(3) N7 0.039(4) 0.036(4) 0.091(6) 0.001(4) 0.019(4) -0.005(3) N8 0.032(3) 0.037(4) 0.073(5) -0.008(4) 0.012(3) 0.010(3) N9 0.099(7) 0.050(5) 0.042(5) -0.001(4) 0.022(4) -0.002(5) N10 0.033(3) 0.034(4) 0.058(5) -0.001(3) 0.010(3) -0.010(3) C61 0.040(4) 0.037(5) 0.049(5) 0.012(4) 0.015(4) 0.000(4) C62 0.027(4) 0.040(5) 0.061(6) -0.010(4) 0.010(3) -0.004(3) C63 0.041(5) 0.056(6) 0.051(5) -0.010(4) -0.017(4) 0.013(4) C64 0.077(6) 0.040(5) 0.044(5) -0.002(4) 0.023(5) -0.006(5) N16 0.031(3) 0.031(3) 0.041(4) -0.005(3) 0.007(3) 0.008(3) N17 0.024(3) 0.043(4) 0.040(4) 0.008(3) 0.004(3) -0.002(3) N18 0.026(3) 0.018(3) 0.028(3) 0.003(2) 0.004(2) 0.005(2) N19 0.027(3) 0.041(4) 0.029(3) 0.003(3) 0.003(2) 0.004(3) N20 0.019(3) 0.047(4) 0.033(3) 0.002(3) 0.003(2) -0.001(3) C69 0.019(3) 0.034(4) 0.035(4) 0.007(3) -0.002(3) 0.006(3) C70 0.022(3) 0.024(4) 0.036(4) -0.001(3) -0.004(3) 0.000(3) C71 0.042(5) 0.043(5) 0.042(5) 0.007(4) 0.004(4) 0.008(4) C72 0.041(4) 0.043(5) 0.041(5) 0.002(4) 0.002(3) 0.000(4) N11 0.030(3) 0.034(4) 0.035(3) 0.006(3) -0.003(2) 0.000(3) N12 0.027(3) 0.035(4) 0.045(4) 0.002(3) 0.000(3) -0.002(3) N13 0.021(3) 0.032(3) 0.041(4) 0.003(3) 0.000(2) -0.004(2) N14 0.026(3) 0.030(4) 0.050(4) 0.001(3) 0.008(3) -0.003(3) N15 0.025(3) 0.033(3) 0.032(3) -0.003(3) -0.002(2) 0.002(2) C65 0.032(4) 0.024(4) 0.031(4) 0.002(3) 0.002(3) 0.000(3) C66 0.033(4) 0.042(5) 0.030(4) 0.004(3) 0.003(3) 0.000(3) C67 0.033(4) 0.036(4) 0.044(5) -0.007(3) 0.008(3) -0.006(3) C68 0.041(4) 0.046(5) 0.039(5) 0.001(4) 0.008(3) -0.012(4) O33 0.029(3) 0.033(3) 0.039(3) -0.002(2) 0.001(2) -0.010(2) O34 0.035(3) 0.036(3) 0.052(4) -0.004(3) 0.000(2) -0.007(2) O35 0.037(3) 0.071(5) 0.046(4) -0.005(3) 0.001(3) 0.001(3) O36 0.054(4) 0.055(4) 0.063(4) 0.003(3) 0.005(3) -0.001(3) O37 0.031(3) 0.065(4) 0.038(3) 0.013(3) 0.008(2) 0.008(3) O38 0.035(3) 0.027(3) 0.051(3) -0.009(2) 0.011(2) -0.006(2) O39 0.058(4) 0.036(3) 0.060(4) 0.002(3) 0.014(3) -0.012(3) O40 0.047(3) 0.070(5) 0.040(3) 0.012(3) 0.001(3) -0.021(3) O41 0.049(4) 0.066(5) 0.060(4) -0.002(3) -0.007(3) 0.009(3) O42 0.038(3) 0.048(3) 0.036(3) -0.014(3) 0.011(2) -0.010(3) O43 0.047(4) 0.046(4) 0.083(5) 0.020(3) 0.010(3) -0.012(3) O44 0.035(3) 0.049(4) 0.049(3) -0.002(3) 0.007(2) 0.006(3) O45 0.055(3) 0.051(4) 0.040(3) -0.003(3) 0.006(3) -0.013(3) O46 0.078(5) 0.043(4) 0.071(5) -0.002(3) 0.007(4) -0.030(3) O47 0.030(3) 0.066(4) 0.069(4) -0.033(3) 0.002(3) 0.007(3) O48 0.051(4) 0.063(4) 0.055(4) -0.006(3) 0.005(3) 0.003(3) O49 0.042(4) 0.086(6) 0.085(6) -0.020(4) -0.007(3) 0.008(4) O50 0.040(4) 0.149(10) 0.036(5) -0.003(6) 0.007(3) 0.043(5) O51 0.103(12) 0.056(10) 0.071(11) 0.012(7) 0.004(9) -0.008(8) _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 O5 1.462(5) . ? S1 O7 1.473(5) . ? S1 O6 1.475(5) . ? S1 C4 1.759(7) . ? S2 O9 1.447(6) . ? S2 O10 1.463(5) . ? S2 O8 1.489(5) . ? S2 C11 1.758(8) . ? S3 O13 1.463(5) . ? S3 O12 1.463(5) . ? S3 O11 1.465(5) . ? S3 C18 1.771(7) . ? S4 O15 1.426(6) . ? S4 O16 1.435(6) . ? S4 O14 1.504(6) . ? S4 C25 1.775(7) . ? O1 C1 1.364(8) . ? O1 H1 0.8500 . ? O2 C8 1.363(9) . ? O2 H2 0.8500 . ? O3 C15 1.378(8) . ? O3 H3 0.8500 . ? O4 C22 1.383(8) . ? O4 H4 0.8501 . ? C1 C6 1.411(9) . ? C1 C2 1.420(9) . ? C2 C3 1.400(9) . ? C2 C28 1.536(9) . ? C3 C4 1.404(9) . ? C3 H3A 0.9500 . ? C4 C5 1.400(9) . ? C5 C6 1.390(9) . ? C5 H5A 0.9500 . ? C6 C7 1.522(9) . ? C7 C9 1.545(9) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.402(9) . ? C8 C13 1.411(9) . ? C9 C10 1.388(9) . ? C10 C11 1.420(10) . ? C10 H10A 0.9500 . ? C11 C12 1.389(9) . ? C12 C13 1.405(9) . ? C12 H12A 0.9500 . ? C13 C14 1.507(9) . ? C14 C16 1.526(9) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.391(9) . ? C15 C20 1.417(8) . ? C16 C17 1.405(9) . ? C17 C18 1.416(9) . ? C17 H17A 0.9500 . ? C18 C19 1.377(9) . ? C19 C20 1.380(9) . ? C19 H19A 0.9500 . ? C20 C21 1.543(9) . ? C21 C23 1.529(9) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C27 1.393(10) . ? C22 C23 1.428(9) . ? C23 C24 1.382(9) . ? C24 C25 1.416(10) . ? C24 H24A 0.9500 . ? C25 C26 1.382(10) . ? C26 C27 1.409(10) . ? C26 H26A 0.9500 . ? C27 C28 1.549(10) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? S5 O21 1.436(5) . ? S5 O23 1.457(6) . ? S5 O22 1.483(6) . ? S5 C32 1.783(7) . ? S6 O24 1.471(5) . ? S6 O25 1.474(5) . ? S6 O26 1.490(5) . ? S6 C39 1.770(7) . ? S7 O29 1.460(5) . ? S7 O28 1.469(5) . ? S7 O27 1.478(5) . ? S7 C46 1.756(7) . ? S8 O30 1.439(5) . ? S8 O31 1.452(5) . ? S8 O32 1.477(5) . ? S8 C53 1.772(7) . ? O17 C29 1.388(8) . ? O17 H17B 0.8499 . ? O18 C36 1.393(8) . ? O18 H18A 0.8500 . ? O19 C43 1.364(7) . ? O19 H19B 0.8500 . ? O20 C50 1.384(8) . ? O20 H20A 0.8501 . ? C29 C34 1.396(9) . ? C29 C30 1.405(9) . ? C30 C31 1.373(9) . ? C30 C56 1.525(9) . ? C31 C32 1.390(9) . ? C31 H31A 0.9500 . ? C32 C33 1.422(9) . ? C33 C34 1.404(10) . ? C33 H33A 0.9500 . ? C34 C35 1.507(9) . ? C35 C37 1.536(9) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C41 1.392(9) . ? C36 C37 1.404(9) . ? C37 C38 1.385(9) . ? C38 C39 1.383(9) . ? C38 H38A 0.9500 . ? C39 C40 1.416(9) . ? C40 C41 1.392(9) . ? C40 H40A 0.9500 . ? C41 C42 1.554(9) . ? C42 C44 1.507(8) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C48 1.391(9) . ? C43 C44 1.441(9) . ? C44 C45 1.377(10) . ? C45 C46 1.397(9) . ? C45 H45A 0.9500 . ? C46 C47 1.392(9) . ? C47 C48 1.404(9) . ? C47 H47A 0.9500 . ? C48 C49 1.521(9) . ? C49 C51 1.537(9) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C51 1.391(9) . ? C50 C55 1.397(9) . ? C51 C52 1.428(9) . ? C52 C53 1.386(9) . ? C52 H52A 0.9500 . ? C53 C54 1.391(9) . ? C54 C55 1.399(10) . ? C54 H54A 0.9500 . ? C55 C56 1.552(9) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? N1 C57 1.276(9) . ? N1 H1B 0.8800 . ? N1 H1C 0.8800 . ? N2 C57 1.345(9) . ? N2 H2B 0.8800 . ? N2 H2C 0.8800 . ? N3 C58 1.373(9) . ? N3 C57 1.386(9) . ? N3 H3C 0.8800 . ? N4 C58 1.349(9) . ? N4 H4B 0.8800 . ? N4 H4C 0.8800 . ? N5 C58 1.305(9) . ? N5 C59 1.470(8) . ? N5 C60 1.497(9) . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? N6 C61 1.320(10) . ? N6 H6A 0.8800 . ? N6 H6B 0.8800 . ? N7 C61 1.337(10) . ? N7 H7C 0.8800 . ? N7 H7D 0.8800 . ? N8 C61 1.329(10) . ? N8 C62 1.382(10) . ? N8 H8A 0.8800 . ? N9 C62 1.284(12) . ? N9 H9A 0.8800 . ? N9 H9B 0.8800 . ? N10 C62 1.347(11) . ? N10 C63 1.441(11) . ? N10 C64 1.499(10) . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? N16 C69 1.313(9) . ? N16 H16A 0.8800 . ? N16 H16B 0.8800 . ? N17 C69 1.339(9) . ? N17 H17C 0.8800 . ? N17 H17D 0.8800 . ? N18 C70 1.388(9) . ? N18 C69 1.391(9) . ? N18 H18B 0.8800 . ? N19 C70 1.318(8) . ? N19 H19C 0.8800 . ? N19 H19D 0.8800 . ? N20 C70 1.322(9) . ? N20 C72 1.479(10) . ? N20 C71 1.481(9) . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? N11 C65 1.341(9) . ? N11 H11A 0.8800 . ? N11 H11B 0.8800 . ? N12 C65 1.314(9) . ? N12 H12B 0.8800 . ? N12 H12C 0.8800 . ? N13 C66 1.375(9) . ? N13 C65 1.380(8) . ? N13 H13A 0.8800 . ? N14 C66 1.318(9) . ? N14 H14C 0.8800 . ? N14 H14D 0.8800 . ? N15 C66 1.355(10) . ? N15 C67 1.465(9) . ? N15 C68 1.477(9) . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? O33 H33B 0.8500 . ? O33 H33C 0.8500 . ? O34 H34A 0.8499 . ? O34 H34B 0.8499 . ? O35 H35C 0.8500 . ? O35 H35D 0.8501 . ? O37 H37A 0.8500 . ? O37 H37B 0.8501 . ? O39 H39A 0.8501 . ? O39 H39B 0.8500 . ? O40 H40B 0.8500 . ? O40 H40C 0.8501 . ? O41 H41A 0.8500 . ? O41 H41B 0.8500 . ? O42 H42A 0.8501 . ? O42 H42B 0.8500 . ? O43 H43A 0.8499 . ? O43 H43B 0.8501 . ? O44 H44A 0.8501 . ? O44 H44B 0.8500 . ? O45 H45B 0.8500 . ? O45 H45C 0.8502 . ? O46 H46A 0.8499 . ? O46 H46B 0.8499 . ? O47 H47B 0.8630 . ? O47 H47C 0.8527 . ? O48 H48A 0.8589 . ? O48 H48B 0.8489 . ? O49 H49C 0.8430 . ? O49 H49D 0.8584 . ? 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 O5 S1 O7 113.1(3) . . ? O5 S1 O6 112.3(4) . . ? O7 S1 O6 109.6(3) . . ? O5 S1 C4 107.8(3) . . ? O7 S1 C4 107.2(3) . . ? O6 S1 C4 106.5(3) . . ? O9 S2 O10 115.8(3) . . ? O9 S2 O8 113.4(3) . . ? O10 S2 O8 108.1(3) . . ? O9 S2 C11 107.2(3) . . ? O10 S2 C11 106.7(3) . . ? O8 S2 C11 104.9(3) . . ? O13 S3 O12 112.2(3) . . ? O13 S3 O11 112.7(3) . . ? O12 S3 O11 111.4(3) . . ? O13 S3 C18 104.8(3) . . ? O12 S3 C18 107.9(3) . . ? O11 S3 C18 107.3(3) . . ? O15 S4 O16 116.7(5) . . ? O15 S4 O14 108.9(4) . . ? O16 S4 O14 110.4(4) . . ? O15 S4 C25 108.1(4) . . ? O16 S4 C25 106.2(3) . . ? O14 S4 C25 105.9(4) . . ? C1 O1 H1 108.6 . . ? C8 O2 H2 109.7 . . ? C15 O3 H3 108.1 . . ? C22 O4 H4 108.7 . . ? O1 C1 C6 118.6(5) . . ? O1 C1 C2 121.4(6) . . ? C6 C1 C2 120.0(6) . . ? C3 C2 C1 119.0(6) . . ? C3 C2 C28 118.8(6) . . ? C1 C2 C28 122.2(6) . . ? C2 C3 C4 120.3(6) . . ? C2 C3 H3A 119.8 . . ? C4 C3 H3A 119.8 . . ? C5 C4 C3 120.4(6) . . ? C5 C4 S1 119.4(5) . . ? C3 C4 S1 120.2(5) . . ? C6 C5 C4 120.0(6) . . ? C6 C5 H5A 120.0 . . ? C4 C5 H5A 120.0 . . ? C5 C6 C1 120.1(6) . . ? C5 C6 C7 118.9(6) . . ? C1 C6 C7 120.9(6) . . ? C6 C7 C9 109.7(5) . . ? C6 C7 H7A 109.7 . . ? C9 C7 H7A 109.7 . . ? C6 C7 H7B 109.7 . . ? C9 C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? O2 C8 C9 121.5(6) . . ? O2 C8 C13 117.2(6) . . ? C9 C8 C13 121.2(7) . . ? C10 C9 C8 119.3(6) . . ? C10 C9 C7 118.9(6) . . ? C8 C9 C7 121.7(6) . . ? C9 C10 C11 120.2(6) . . ? C9 C10 H10A 119.9 . . ? C11 C10 H10A 119.9 . . ? C12 C11 C10 119.9(7) . . ? C12 C11 S2 119.1(6) . . ? C10 C11 S2 120.6(5) . . ? C11 C12 C13 120.6(7) . . ? C11 C12 H12A 119.7 . . ? C13 C12 H12A 119.7 . . ? C12 C13 C8 118.7(6) . . ? C12 C13 C14 119.2(6) . . ? C8 C13 C14 122.0(6) . . ? C13 C14 C16 110.8(5) . . ? C13 C14 H14A 109.5 . . ? C16 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? C16 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? O3 C15 C16 121.1(6) . . ? O3 C15 C20 116.6(5) . . ? C16 C15 C20 122.3(6) . . ? C15 C16 C17 118.4(6) . . ? C15 C16 C14 123.0(6) . . ? C17 C16 C14 118.5(6) . . ? C16 C17 C18 119.1(6) . . ? C16 C17 H17A 120.5 . . ? C18 C17 H17A 120.5 . . ? C19 C18 C17 121.1(6) . . ? C19 C18 S3 118.9(5) . . ? C17 C18 S3 120.0(5) . . ? C18 C19 C20 120.9(6) . . ? C18 C19 H19A 119.5 . . ? C20 C19 H19A 119.5 . . ? C19 C20 C15 118.1(6) . . ? C19 C20 C21 121.8(6) . . ? C15 C20 C21 120.0(6) . . ? C23 C21 C20 108.9(5) . . ? C23 C21 H21A 109.9 . . ? C20 C21 H21A 109.9 . . ? C23 C21 H21B 109.9 . . ? C20 C21 H21B 109.9 . . ? H21A C21 H21B 108.3 . . ? O4 C22 C27 116.7(6) . . ? O4 C22 C23 122.1(6) . . ? C27 C22 C23 121.2(6) . . ? C24 C23 C22 117.8(6) . . ? C24 C23 C21 119.5(6) . . ? C22 C23 C21 122.6(5) . . ? C23 C24 C25 121.8(6) . . ? C23 C24 H24A 119.1 . . ? C25 C24 H24A 119.1 . . ? C26 C25 C24 119.2(7) . . ? C26 C25 S4 121.9(6) . . ? C24 C25 S4 118.9(6) . . ? C25 C26 C27 120.9(7) . . ? C25 C26 H26A 119.6 . . ? C27 C26 H26A 119.6 . . ? C22 C27 C26 119.1(6) . . ? C22 C27 C28 120.1(6) . . ? C26 C27 C28 120.8(6) . . ? C2 C28 C27 113.5(6) . . ? C2 C28 H28A 108.9 . . ? C27 C28 H28A 108.9 . . ? C2 C28 H28B 108.9 . . ? C27 C28 H28B 108.9 . . ? H28A C28 H28B 107.7 . . ? O21 S5 O23 113.1(4) . . ? O21 S5 O22 108.2(3) . . ? O23 S5 O22 113.6(4) . . ? O21 S5 C32 106.6(3) . . ? O23 S5 C32 107.7(3) . . ? O22 S5 C32 107.3(3) . . ? O24 S6 O25 112.5(3) . . ? O24 S6 O26 111.2(3) . . ? O25 S6 O26 112.6(3) . . ? O24 S6 C39 107.3(3) . . ? O25 S6 C39 106.0(3) . . ? O26 S6 C39 106.9(3) . . ? O29 S7 O28 112.2(3) . . ? O29 S7 O27 112.6(3) . . ? O28 S7 O27 111.3(3) . . ? O29 S7 C46 108.1(3) . . ? O28 S7 C46 106.3(3) . . ? O27 S7 C46 105.9(3) . . ? O30 S8 O31 113.0(3) . . ? O30 S8 O32 111.9(3) . . ? O31 S8 O32 111.6(3) . . ? O30 S8 C53 107.6(3) . . ? O31 S8 C53 107.0(3) . . ? O32 S8 C53 105.3(3) . . ? C29 O17 H17B 108.8 . . ? C36 O18 H18A 108.8 . . ? C43 O19 H19B 119.6 . . ? C50 O20 H20A 108.7 . . ? O17 C29 C34 122.8(6) . . ? O17 C29 C30 115.2(5) . . ? C34 C29 C30 122.0(6) . . ? C31 C30 C29 119.2(6) . . ? C31 C30 C56 121.1(6) . . ? C29 C30 C56 119.7(6) . . ? C30 C31 C32 120.7(6) . . ? C30 C31 H31A 119.6 . . ? C32 C31 H31A 119.6 . . ? C31 C32 C33 120.2(6) . . ? C31 C32 S5 119.7(5) . . ? C33 C32 S5 119.8(5) . . ? C34 C33 C32 119.5(6) . . ? C34 C33 H33A 120.3 . . ? C32 C33 H33A 120.3 . . ? C29 C34 C33 118.4(6) . . ? C29 C34 C35 120.9(6) . . ? C33 C34 C35 120.7(6) . . ? C34 C35 C37 111.8(5) . . ? C34 C35 H35A 109.3 . . ? C37 C35 H35A 109.3 . . ? C34 C35 H35B 109.3 . . ? C37 C35 H35B 109.3 . . ? H35A C35 H35B 107.9 . . ? O18 C36 C41 120.4(5) . . ? O18 C36 C37 116.8(6) . . ? C41 C36 C37 122.8(6) . . ? C38 C37 C36 117.5(6) . . ? C38 C37 C35 119.9(6) . . ? C36 C37 C35 122.5(6) . . ? C39 C38 C37 122.0(6) . . ? C39 C38 H38A 119.0 . . ? C37 C38 H38A 119.0 . . ? C38 C39 C40 118.8(6) . . ? C38 C39 S6 120.9(5) . . ? C40 C39 S6 120.3(5) . . ? C41 C40 C39 121.1(6) . . ? C41 C40 H40A 119.5 . . ? C39 C40 H40A 119.5 . . ? C40 C41 C36 117.7(6) . . ? C40 C41 C42 117.9(6) . . ? C36 C41 C42 124.5(6) . . ? C44 C42 C41 111.0(5) . . ? C44 C42 H42A 109.4 . . ? C41 C42 H42A 109.4 . . ? C44 C42 H42B 109.4 . . ? C41 C42 H42B 109.4 . . ? H42A C42 H42B 108.0 . . ? O19 C43 C48 124.2(6) . . ? O19 C43 C44 114.9(5) . . ? C48 C43 C44 120.9(6) . . ? C45 C44 C43 117.5(6) . . ? C45 C44 C42 120.9(6) . . ? C43 C44 C42 121.6(6) . . ? C44 C45 C46 122.8(6) . . ? C44 C45 H45A 118.6 . . ? C46 C45 H45A 118.6 . . ? C47 C46 C45 118.4(6) . . ? C47 C46 S7 119.2(5) . . ? C45 C46 S7 122.4(5) . . ? C46 C47 C48 121.5(6) . . ? C46 C47 H47A 119.2 . . ? C48 C47 H47A 119.2 . . ? C43 C48 C47 118.8(6) . . ? C43 C48 C49 119.8(6) . . ? C47 C48 C49 121.4(6) . . ? C48 C49 C51 110.4(5) . . ? C48 C49 H49A 109.6 . . ? C51 C49 H49A 109.6 . . ? C48 C49 H49B 109.6 . . ? C51 C49 H49B 109.6 . . ? H49A C49 H49B 108.1 . . ? O20 C50 C51 114.9(6) . . ? O20 C50 C55 123.4(6) . . ? C51 C50 C55 121.8(6) . . ? C50 C51 C52 118.6(6) . . ? C50 C51 C49 123.4(6) . . ? C52 C51 C49 118.0(6) . . ? C53 C52 C51 119.6(6) . . ? C53 C52 H52A 120.2 . . ? C51 C52 H52A 120.2 . . ? C52 C53 C54 120.6(6) . . ? C52 C53 S8 120.0(5) . . ? C54 C53 S8 119.2(5) . . ? C53 C54 C55 120.7(6) . . ? C53 C54 H54A 119.7 . . ? C55 C54 H54A 119.7 . . ? C50 C55 C54 118.7(6) . . ? C50 C55 C56 124.5(6) . . ? C54 C55 C56 116.9(6) . . ? C30 C56 C55 112.0(5) . . ? C30 C56 H56A 109.2 . . ? C55 C56 H56A 109.2 . . ? C30 C56 H56B 109.2 . . ? C55 C56 H56B 109.2 . . ? H56A C56 H56B 107.9 . . ? C57 N1 H1B 120.0 . . ? C57 N1 H1C 120.0 . . ? H1B N1 H1C 120.0 . . ? C57 N2 H2B 120.0 . . ? C57 N2 H2C 120.0 . . ? H2B N2 H2C 120.0 . . ? C58 N3 C57 125.9(6) . . ? C58 N3 H3C 117.0 . . ? C57 N3 H3C 117.0 . . ? C58 N4 H4B 120.0 . . ? C58 N4 H4C 120.0 . . ? H4B N4 H4C 120.0 . . ? C58 N5 C59 120.1(6) . . ? C58 N5 C60 123.8(6) . . ? C59 N5 C60 115.7(6) . . ? N1 C57 N2 123.4(7) . . ? N1 C57 N3 121.8(6) . . ? N2 C57 N3 114.8(6) . . ? N5 C58 N4 123.5(7) . . ? N5 C58 N3 122.7(6) . . ? N4 C58 N3 113.7(6) . . ? N5 C59 H59A 109.5 . . ? N5 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? N5 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? N5 C60 H60A 109.5 . . ? N5 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? N5 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C61 N6 H6A 120.0 . . ? C61 N6 H6B 120.0 . . ? H6A N6 H6B 120.0 . . ? C61 N7 H7C 120.0 . . ? C61 N7 H7D 120.0 . . ? H7C N7 H7D 120.0 . . ? C61 N8 C62 129.8(7) . . ? C61 N8 H8A 115.1 . . ? C62 N8 H8A 115.1 . . ? C62 N9 H9A 120.0 . . ? C62 N9 H9B 120.0 . . ? H9A N9 H9B 120.0 . . ? C62 N10 C63 127.1(8) . . ? C62 N10 C64 117.0(7) . . ? C63 N10 C64 115.1(7) . . ? N6 C61 N8 118.5(7) . . ? N6 C61 N7 120.5(8) . . ? N8 C61 N7 120.8(8) . . ? N9 C62 N10 125.5(9) . . ? N9 C62 N8 115.9(9) . . ? N10 C62 N8 118.6(8) . . ? N10 C63 H63A 109.5 . . ? N10 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? N10 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? N10 C64 H64A 109.5 . . ? N10 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? N10 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C69 N16 H16A 120.0 . . ? C69 N16 H16B 120.0 . . ? H16A N16 H16B 120.0 . . ? C69 N17 H17C 120.0 . . ? C69 N17 H17D 120.0 . . ? H17C N17 H17D 120.0 . . ? C70 N18 C69 126.1(6) . . ? C70 N18 H18B 117.0 . . ? C69 N18 H18B 117.0 . . ? C70 N19 H19C 120.0 . . ? C70 N19 H19D 120.0 . . ? H19C N19 H19D 120.0 . . ? C70 N20 C72 120.1(6) . . ? C70 N20 C71 124.8(7) . . ? C72 N20 C71 113.9(6) . . ? N16 C69 N17 121.9(7) . . ? N16 C69 N18 119.2(7) . . ? N17 C69 N18 118.9(7) . . ? N19 C70 N20 122.0(7) . . ? N19 C70 N18 118.9(6) . . ? N20 C70 N18 119.1(6) . . ? N20 C71 H71A 109.5 . . ? N20 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? N20 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? N20 C72 H72A 109.5 . . ? N20 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? N20 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C65 N11 H11A 120.0 . . ? C65 N11 H11B 120.0 . . ? H11A N11 H11B 120.0 . . ? C65 N12 H12B 120.0 . . ? C65 N12 H12C 120.0 . . ? H12B N12 H12C 120.0 . . ? C66 N13 C65 128.7(6) . . ? C66 N13 H13A 115.6 . . ? C65 N13 H13A 115.6 . . ? C66 N14 H14C 120.0 . . ? C66 N14 H14D 120.0 . . ? H14C N14 H14D 120.0 . . ? C66 N15 C67 122.4(6) . . ? C66 N15 C68 119.9(6) . . ? C67 N15 C68 116.3(6) . . ? N12 C65 N11 121.9(6) . . ? N12 C65 N13 117.1(6) . . ? N11 C65 N13 120.9(6) . . ? N14 C66 N15 123.5(7) . . ? N14 C66 N13 116.4(7) . . ? N15 C66 N13 120.1(7) . . ? N15 C67 H67A 109.5 . . ? N15 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? N15 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? N15 C68 H68A 109.5 . . ? N15 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? N15 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? H33B O33 H33C 107.7 . . ? H34A O34 H34B 107.7 . . ? H35C O35 H35D 107.7 . . ? H37A O37 H37B 107.7 . . ? H39A O39 H39B 107.7 . . ? H40B O40 H40C 107.7 . . ? H41A O41 H41B 107.7 . . ? H42A O42 H42B 107.7 . . ? H43A O43 H43B 107.7 . . ? H44A O44 H44B 107.7 . . ? H45B O45 H45C 107.7 . . ? H46A O46 H46B 107.7 . . ? H47B O47 H47C 106.3 . . ? H48A O48 H48B 107.0 . . ? H49C O49 H49D 107.6 . . ? 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 178.9(6) . . . . ? C6 C1 C2 C3 -2.3(10) . . . . ? O1 C1 C2 C28 -0.1(10) . . . . ? C6 C1 C2 C28 178.6(6) . . . . ? C1 C2 C3 C4 2.3(10) . . . . ? C28 C2 C3 C4 -178.6(6) . . . . ? C2 C3 C4 C5 -1.7(10) . . . . ? C2 C3 C4 S1 -179.2(5) . . . . ? O5 S1 C4 C5 13.4(7) . . . . ? O7 S1 C4 C5 -108.7(6) . . . . ? O6 S1 C4 C5 134.0(6) . . . . ? O5 S1 C4 C3 -169.2(6) . . . . ? O7 S1 C4 C3 68.8(6) . . . . ? O6 S1 C4 C3 -48.5(7) . . . . ? C3 C4 C5 C6 1.1(10) . . . . ? S1 C4 C5 C6 178.6(5) . . . . ? C4 C5 C6 C1 -1.1(10) . . . . ? C4 C5 C6 C7 176.2(6) . . . . ? O1 C1 C6 C5 -179.5(6) . . . . ? C2 C1 C6 C5 1.7(10) . . . . ? O1 C1 C6 C7 3.3(9) . . . . ? C2 C1 C6 C7 -175.5(6) . . . . ? C5 C6 C7 C9 -98.6(7) . . . . ? C1 C6 C7 C9 78.6(8) . . . . ? O2 C8 C9 C10 179.0(6) . . . . ? C13 C8 C9 C10 1.2(9) . . . . ? O2 C8 C9 C7 -4.6(9) . . . . ? C13 C8 C9 C7 177.6(6) . . . . ? C6 C7 C9 C10 74.7(7) . . . . ? C6 C7 C9 C8 -101.8(7) . . . . ? C8 C9 C10 C11 -1.2(9) . . . . ? C7 C9 C10 C11 -177.8(5) . . . . ? C9 C10 C11 C12 0.5(9) . . . . ? C9 C10 C11 S2 172.6(5) . . . . ? O9 S2 C11 C12 -173.6(5) . . . . ? O10 S2 C11 C12 -49.0(6) . . . . ? O8 S2 C11 C12 65.6(6) . . . . ? O9 S2 C11 C10 14.2(6) . . . . ? O10 S2 C11 C10 138.8(5) . . . . ? O8 S2 C11 C10 -106.6(6) . . . . ? C10 C11 C12 C13 0.2(10) . . . . ? S2 C11 C12 C13 -172.0(5) . . . . ? C11 C12 C13 C8 -0.3(9) . . . . ? C11 C12 C13 C14 175.5(6) . . . . ? O2 C8 C13 C12 -178.3(6) . . . . ? C9 C8 C13 C12 -0.4(9) . . . . ? O2 C8 C13 C14 6.0(9) . . . . ? C9 C8 C13 C14 -176.1(6) . . . . ? C12 C13 C14 C16 -78.3(7) . . . . ? C8 C13 C14 C16 97.4(7) . . . . ? O3 C15 C16 C17 -177.4(6) . . . . ? C20 C15 C16 C17 0.7(10) . . . . ? O3 C15 C16 C14 0.0(10) . . . . ? C20 C15 C16 C14 178.1(6) . . . . ? C13 C14 C16 C15 -81.2(8) . . . . ? C13 C14 C16 C17 96.1(7) . . . . ? C15 C16 C17 C18 -0.3(10) . . . . ? C14 C16 C17 C18 -177.8(6) . . . . ? C16 C17 C18 C19 -0.6(10) . . . . ? C16 C17 C18 S3 -179.7(5) . . . . ? O13 S3 C18 C19 -61.2(6) . . . . ? O12 S3 C18 C19 179.0(5) . . . . ? O11 S3 C18 C19 58.8(6) . . . . ? O13 S3 C18 C17 117.9(6) . . . . ? O12 S3 C18 C17 -1.9(6) . . . . ? O11 S3 C18 C17 -122.0(5) . . . . ? C17 C18 C19 C20 1.0(10) . . . . ? S3 C18 C19 C20 -179.8(5) . . . . ? C18 C19 C20 C15 -0.6(10) . . . . ? C18 C19 C20 C21 177.3(6) . . . . ? O3 C15 C20 C19 177.9(6) . . . . ? C16 C15 C20 C19 -0.3(10) . . . . ? O3 C15 C20 C21 0.0(9) . . . . ? C16 C15 C20 C21 -178.2(6) . . . . ? C19 C20 C21 C23 -91.8(7) . . . . ? C15 C20 C21 C23 86.0(7) . . . . ? O4 C22 C23 C24 177.1(5) . . . . ? C27 C22 C23 C24 -3.1(9) . . . . ? O4 C22 C23 C21 -6.7(9) . . . . ? C27 C22 C23 C21 173.1(6) . . . . ? C20 C21 C23 C24 75.6(7) . . . . ? C20 C21 C23 C22 -100.6(7) . . . . ? C22 C23 C24 C25 1.6(9) . . . . ? C21 C23 C24 C25 -174.8(6) . . . . ? C23 C24 C25 C26 0.9(10) . . . . ? C23 C24 C25 S4 178.4(5) . . . . ? O15 S4 C25 C26 -53.6(7) . . . . ? O16 S4 C25 C26 72.4(7) . . . . ? O14 S4 C25 C26 -170.2(6) . . . . ? O15 S4 C25 C24 128.9(6) . . . . ? O16 S4 C25 C24 -105.1(6) . . . . ? O14 S4 C25 C24 12.3(6) . . . . ? C24 C25 C26 C27 -1.9(10) . . . . ? S4 C25 C26 C27 -179.4(5) . . . . ? O4 C22 C27 C26 -178.1(6) . . . . ? C23 C22 C27 C26 2.1(9) . . . . ? O4 C22 C27 C28 2.8(9) . . . . ? C23 C22 C27 C28 -177.0(6) . . . . ? C25 C26 C27 C22 0.4(10) . . . . ? C25 C26 C27 C28 179.6(6) . . . . ? C3 C2 C28 C27 102.9(7) . . . . ? C1 C2 C28 C27 -78.0(8) . . . . ? C22 C27 C28 C2 96.6(7) . . . . ? C26 C27 C28 C2 -82.6(7) . . . . ? O17 C29 C30 C31 -177.6(6) . . . . ? C34 C29 C30 C31 1.7(10) . . . . ? O17 C29 C30 C56 4.1(9) . . . . ? C34 C29 C30 C56 -176.6(6) . . . . ? C29 C30 C31 C32 -1.6(10) . . . . ? C56 C30 C31 C32 176.7(6) . . . . ? C30 C31 C32 C33 1.7(10) . . . . ? C30 C31 C32 S5 175.7(5) . . . . ? O21 S5 C32 C31 52.9(6) . . . . ? O23 S5 C32 C31 174.5(6) . . . . ? O22 S5 C32 C31 -62.8(6) . . . . ? O21 S5 C32 C33 -133.1(5) . . . . ? O23 S5 C32 C33 -11.5(6) . . . . ? O22 S5 C32 C33 111.2(6) . . . . ? C31 C32 C33 C34 -1.9(10) . . . . ? S5 C32 C33 C34 -175.8(5) . . . . ? O17 C29 C34 C33 177.4(6) . . . . ? C30 C29 C34 C33 -1.8(10) . . . . ? O17 C29 C34 C35 -2.6(10) . . . . ? C30 C29 C34 C35 178.1(6) . . . . ? C32 C33 C34 C29 1.9(10) . . . . ? C32 C33 C34 C35 -178.1(6) . . . . ? C29 C34 C35 C37 -79.7(8) . . . . ? C33 C34 C35 C37 100.2(7) . . . . ? O18 C36 C37 C38 -177.6(5) . . . . ? C41 C36 C37 C38 4.0(9) . . . . ? O18 C36 C37 C35 2.2(8) . . . . ? C41 C36 C37 C35 -176.1(5) . . . . ? C34 C35 C37 C38 -81.1(7) . . . . ? C34 C35 C37 C36 99.1(7) . . . . ? C36 C37 C38 C39 -3.3(9) . . . . ? C35 C37 C38 C39 176.9(5) . . . . ? C37 C38 C39 C40 1.1(9) . . . . ? C37 C38 C39 S6 -177.4(5) . . . . ? O24 S6 C39 C38 94.0(6) . . . . ? O25 S6 C39 C38 -26.3(6) . . . . ? O26 S6 C39 C38 -146.6(5) . . . . ? O24 S6 C39 C40 -84.5(6) . . . . ? O25 S6 C39 C40 155.2(5) . . . . ? O26 S6 C39 C40 34.9(6) . . . . ? C38 C39 C40 C41 0.5(9) . . . . ? S6 C39 C40 C41 179.1(5) . . . . ? C39 C40 C41 C36 0.2(9) . . . . ? C39 C40 C41 C42 179.4(5) . . . . ? O18 C36 C41 C40 179.2(5) . . . . ? C37 C36 C41 C40 -2.5(9) . . . . ? O18 C36 C41 C42 0.0(9) . . . . ? C37 C36 C41 C42 178.3(5) . . . . ? C40 C41 C42 C44 81.9(7) . . . . ? C36 C41 C42 C44 -98.9(7) . . . . ? O19 C43 C44 C45 -179.0(6) . . . . ? C48 C43 C44 C45 1.9(9) . . . . ? O19 C43 C44 C42 0.2(9) . . . . ? C48 C43 C44 C42 -179.0(6) . . . . ? C41 C42 C44 C45 -101.8(7) . . . . ? C41 C42 C44 C43 79.1(8) . . . . ? C43 C44 C45 C46 -0.8(10) . . . . ? C42 C44 C45 C46 -179.9(6) . . . . ? C44 C45 C46 C47 0.1(10) . . . . ? C44 C45 C46 S7 -177.1(5) . . . . ? O29 S7 C46 C47 57.9(6) . . . . ? O28 S7 C46 C47 178.5(5) . . . . ? O27 S7 C46 C47 -63.0(6) . . . . ? O29 S7 C46 C45 -125.0(6) . . . . ? O28 S7 C46 C45 -4.3(7) . . . . ? O27 S7 C46 C45 114.1(6) . . . . ? C45 C46 C47 C48 -0.4(10) . . . . ? S7 C46 C47 C48 176.9(5) . . . . ? O19 C43 C48 C47 178.7(6) . . . . ? C44 C43 C48 C47 -2.2(9) . . . . ? O19 C43 C48 C49 -2.7(10) . . . . ? C44 C43 C48 C49 176.4(6) . . . . ? C46 C47 C48 C43 1.5(10) . . . . ? C46 C47 C48 C49 -177.1(6) . . . . ? C43 C48 C49 C51 -77.5(8) . . . . ? C47 C48 C49 C51 101.0(7) . . . . ? O20 C50 C51 C52 -178.8(5) . . . . ? C55 C50 C51 C52 2.6(10) . . . . ? O20 C50 C51 C49 4.0(9) . . . . ? C55 C50 C51 C49 -174.5(6) . . . . ? C48 C49 C51 C50 101.4(7) . . . . ? C48 C49 C51 C52 -75.7(7) . . . . ? C50 C51 C52 C53 -2.0(9) . . . . ? C49 C51 C52 C53 175.3(6) . . . . ? C51 C52 C53 C54 1.5(10) . . . . ? C51 C52 C53 S8 177.6(5) . . . . ? O30 S8 C53 C52 140.5(6) . . . . ? O31 S8 C53 C52 18.7(6) . . . . ? O32 S8 C53 C52 -100.1(6) . . . . ? O30 S8 C53 C54 -43.4(6) . . . . ? O31 S8 C53 C54 -165.1(5) . . . . ? O32 S8 C53 C54 76.1(6) . . . . ? C52 C53 C54 C55 -1.5(10) . . . . ? S8 C53 C54 C55 -177.6(5) . . . . ? O20 C50 C55 C54 179.0(6) . . . . ? C51 C50 C55 C54 -2.6(10) . . . . ? O20 C50 C55 C56 -1.2(10) . . . . ? C51 C50 C55 C56 177.2(6) . . . . ? C53 C54 C55 C50 2.0(10) . . . . ? C53 C54 C55 C56 -177.8(6) . . . . ? C31 C30 C56 C55 -102.3(7) . . . . ? C29 C30 C56 C55 76.0(8) . . . . ? C50 C55 C56 C30 -103.9(8) . . . . ? C54 C55 C56 C30 75.9(7) . . . . ? C58 N3 C57 N1 29.4(12) . . . . ? C58 N3 C57 N2 -152.3(7) . . . . ? C59 N5 C58 N4 8.5(10) . . . . ? C60 N5 C58 N4 -164.2(6) . . . . ? C59 N5 C58 N3 -172.5(6) . . . . ? C60 N5 C58 N3 14.9(10) . . . . ? C57 N3 C58 N5 41.4(10) . . . . ? C57 N3 C58 N4 -139.4(7) . . . . ? C62 N8 C61 N6 -167.2(9) . . . . ? C62 N8 C61 N7 10.1(15) . . . . ? C63 N10 C62 N9 -165.4(9) . . . . ? C64 N10 C62 N9 3.9(12) . . . . ? C63 N10 C62 N8 13.3(12) . . . . ? C64 N10 C62 N8 -177.4(7) . . . . ? C61 N8 C62 N9 -126.6(10) . . . . ? C61 N8 C62 N10 54.5(12) . . . . ? C70 N18 C69 N16 29.5(10) . . . . ? C70 N18 C69 N17 -152.1(6) . . . . ? C72 N20 C70 N19 8.1(11) . . . . ? C71 N20 C70 N19 -158.2(7) . . . . ? C72 N20 C70 N18 -172.2(7) . . . . ? C71 N20 C70 N18 21.5(11) . . . . ? C69 N18 C70 N19 34.8(10) . . . . ? C69 N18 C70 N20 -144.9(7) . . . . ? C66 N13 C65 N12 170.7(7) . . . . ? C66 N13 C65 N11 -7.1(12) . . . . ? C67 N15 C66 N14 -157.7(7) . . . . ? C68 N15 C66 N14 8.5(11) . . . . ? C67 N15 C66 N13 20.5(10) . . . . ? C68 N15 C66 N13 -173.3(7) . . . . ? C65 N13 C66 N14 -124.2(8) . . . . ? C65 N13 C66 N15 57.5(11) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.741 _refine_diff_density_min -0.645 _refine_diff_density_rms 0.093 # Attachment 'SC4A+PFM.cif' data_SC4A+PFM _database_code_depnum_ccdc_archive 'CCDC 820614' #TrackingRef 'SC4A+PFM.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H71 N10 O24.50 S4' _chemical_formula_weight 1308.39 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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.129(3) _cell_length_b 12.140(2) _cell_length_c 33.206(7) _cell_angle_alpha 90.00 _cell_angle_beta 100.51(3) _cell_angle_gamma 90.00 _cell_volume 5997(2) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.449 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2756 _exptl_absorpt_coefficient_mu 0.248 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.9475 _exptl_absorpt_correction_T_max 0.9614 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'rigaku saturn CCD area detector' _diffrn_measurement_method '\w and \f scans' _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 36360 _diffrn_reflns_av_R_equivalents 0.1004 _diffrn_reflns_av_sigmaI/netI 0.1296 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 25.02 _reflns_number_total 10489 _reflns_number_gt 6294 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'crystalclear(Rigaku/MSC Inc., 2005)' _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 '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^)+(0.1229P)^2^+38.5880P] 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 0.0169(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10489 _refine_ls_number_parameters 797 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1352 _refine_ls_R_factor_gt 0.1116 _refine_ls_wR_factor_ref 0.3058 _refine_ls_wR_factor_gt 0.2946 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _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 S1 S 0.54241(8) 0.57943(10) 0.18267(4) 0.0233(3) Uani 1 1 d . . . S2 S 0.04013(9) 0.34687(10) 0.12479(4) 0.0259(3) Uani 1 1 d . . . S3 S -0.13412(8) 0.94204(11) 0.10848(4) 0.0274(3) Uani 1 1 d . . . S4 S 0.35379(8) 1.17462(10) 0.16275(4) 0.0217(3) Uani 1 1 d . . . O1 O 0.3280(2) 0.6959(3) 0.02206(11) 0.0264(9) Uani 1 1 d . . . H1 H 0.3192 0.7640 0.0194 0.040 Uiso 1 1 calc R . . O2 O 0.6212(2) 0.6509(3) 0.18757(12) 0.0339(10) Uani 1 1 d . . . O3 O 0.4919(2) 0.5967(3) 0.21572(11) 0.0269(9) Uani 1 1 d . . . O4 O 0.5637(3) 0.4641(3) 0.17828(12) 0.0354(10) Uani 1 1 d . . . O5 O 0.1631(2) 0.6227(3) 0.00008(11) 0.0271(9) Uani 1 1 d . . . H5 H 0.2193 0.6249 0.0028 0.041 Uiso 1 1 calc R . . O6 O 0.1166(3) 0.3188(3) 0.15652(12) 0.0355(11) Uani 1 1 d . . . O7 O 0.0079(2) 0.2508(3) 0.09990(12) 0.0299(10) Uani 1 1 d . . . O8 O -0.0325(3) 0.4026(3) 0.13974(12) 0.0351(10) Uani 1 1 d . . . O9 O 0.1094(2) 0.8322(3) -0.00549(11) 0.0252(9) Uani 1 1 d . . . H9 H 0.1159 0.7639 -0.0079 0.038 Uiso 1 1 calc R . . O10 O -0.1590(3) 0.8422(3) 0.12691(16) 0.0571(13) Uani 1 1 d . . . O11 O -0.2076(3) 0.9957(4) 0.08191(14) 0.0448(12) Uani 1 1 d . . . O12 O -0.0880(2) 1.0200(3) 0.13858(11) 0.0280(9) Uani 1 1 d . . . O13 O 0.2774(2) 0.9036(3) 0.01335(10) 0.0262(9) Uani 1 1 d . . . H13 H 0.2224 0.8897 0.0062 0.039 Uiso 1 1 calc R . . O14 O 0.2876(2) 1.1507(3) 0.18850(11) 0.0291(10) Uani 1 1 d . . . O15 O 0.3450(2) 1.2867(3) 0.14768(12) 0.0321(10) Uani 1 1 d . . . O16 O 0.4451(2) 1.1493(3) 0.18287(11) 0.0299(10) Uani 1 1 d . . . N1 N 0.2927(3) 0.9200(4) 0.27459(15) 0.0363(13) Uani 1 1 d . . . H1C H 0.3077 0.9011 0.3005 0.044 Uiso 1 1 calc R . . N2 N 0.1464(3) 0.9344(4) 0.28410(13) 0.0301(12) Uani 1 1 d . . . H2 H 0.1668 0.9072 0.3105 0.036 Uiso 1 1 d R . . H2A H 0.0879 0.9487 0.2742 0.036 Uiso 1 1 d R . . N3 N 0.1879(3) 1.0058(4) 0.22519(13) 0.0255(11) Uani 1 1 d . . . H3 H 0.2308 1.0456 0.2178 0.031 Uiso 1 1 calc R . . N4 N 0.0442(3) 0.9311(3) 0.20183(13) 0.0251(11) Uani 1 1 d . . . H4A H 0.0046 0.9391 0.1812 0.030 Uiso 1 1 d R . . H4B H 0.0499 0.8631 0.2201 0.030 Uiso 1 1 d R . . N5 N 0.0937(3) 1.0819(3) 0.17138(13) 0.0243(9) Uiso 1 1 d . . . H5A H 0.0388 1.0786 0.1524 0.029 Uiso 1 1 d R . . H5B H 0.1345 1.1354 0.1701 0.029 Uiso 1 1 d R . . N6 N 0.3492(3) 0.6900(3) 0.87784(13) 0.0235(10) Uani 1 1 d . . . H6 H 0.3098 0.6447 0.8854 0.028 Uiso 1 1 calc R . . N7 N 0.3730(3) 0.8034(4) 0.82411(15) 0.0328(12) Uani 1 1 d . . . H7 H 0.4174 0.7986 0.8279 0.039 Uiso 1 1 d R . . H7A H 0.3466 0.8473 0.8033 0.039 Uiso 1 1 d R . . N8 N 0.2288(3) 0.7620(4) 0.83524(13) 0.0252(11) Uani 1 1 d . . . H8 H 0.1978 0.7540 0.8551 0.030 Uiso 1 1 calc R . . N9 N 0.2084(3) 0.7540(4) 0.76308(13) 0.0266(11) Uani 1 1 d . . . H9A H 0.2531 0.7086 0.7556 0.032 Uiso 1 1 d R . . H9B H 0.1744 0.7855 0.7412 0.032 Uiso 1 1 d R . . N10 N 0.1035(3) 0.8371(4) 0.79559(14) 0.0280(10) Uiso 1 1 d . . . H10A H 0.1042 0.8969 0.8161 0.034 Uiso 1 1 d R . . H10B H 0.0540 0.8191 0.7770 0.034 Uiso 1 1 d R . . C1 C 0.4439(3) 0.8681(4) 0.06512(16) 0.0230(12) Uani 1 1 d . . . H1A H 0.5050 0.8958 0.0764 0.028 Uiso 1 1 calc R . . H1B H 0.4382 0.8634 0.0350 0.028 Uiso 1 1 calc R . . C2 C 0.4332(3) 0.7523(4) 0.08222(16) 0.0226(12) Uani 1 1 d . . . C3 C 0.4831(3) 0.7226(4) 0.11988(16) 0.0225(12) Uani 1 1 d . . . H3A H 0.5241 0.7736 0.1349 0.027 Uiso 1 1 calc R . . C4 C 0.4735(3) 0.6176(4) 0.13592(15) 0.0228(12) Uani 1 1 d . . . C5 C 0.4137(3) 0.5434(4) 0.11463(15) 0.0221(12) Uani 1 1 d . . . H5D H 0.4069 0.4730 0.1262 0.026 Uiso 1 1 calc R . . C6 C 0.3630(3) 0.5691(4) 0.07649(15) 0.0190(11) Uani 1 1 d . . . C7 C 0.3732(3) 0.6738(4) 0.06057(15) 0.0202(12) Uani 1 1 d . . . C8 C 0.2999(3) 0.4863(4) 0.05184(16) 0.0231(12) Uani 1 1 d . . . H8A H 0.3214 0.4111 0.0600 0.028 Uiso 1 1 calc R . . H8B H 0.3026 0.4955 0.0225 0.028 Uiso 1 1 calc R . . C9 C 0.2015(3) 0.4965(4) 0.05723(16) 0.0232(12) Uani 1 1 d . . . C10 C 0.1708(3) 0.4339(4) 0.08673(16) 0.0236(13) Uani 1 1 d . . . H10 H 0.2111 0.3863 0.1039 0.028 Uiso 1 1 calc R . . C11 C 0.0805(3) 0.4402(4) 0.09152(16) 0.0237(13) Uani 1 1 d . . . C12 C 0.0222(3) 0.5123(4) 0.06763(16) 0.0240(13) Uani 1 1 d . . . H12 H -0.0383 0.5179 0.0715 0.029 Uiso 1 1 calc R . . C13 C 0.0515(3) 0.5762(4) 0.03824(15) 0.0202(12) Uani 1 1 d . . . C14 C 0.1396(3) 0.5656(4) 0.03231(15) 0.0225(12) Uani 1 1 d . . . C15 C -0.0117(3) 0.6597(4) 0.01337(16) 0.0214(12) Uani 1 1 d . . . H15A H 0.0024 0.6649 -0.0145 0.026 Uiso 1 1 calc R . . H15B H -0.0744 0.6333 0.0108 0.026 Uiso 1 1 calc R . . C16 C -0.0041(3) 0.7732(4) 0.03280(15) 0.0216(12) Uani 1 1 d . . . C17 C -0.0593(3) 0.8021(4) 0.06067(15) 0.0222(12) Uani 1 1 d . . . H17 H -0.1002 0.7494 0.0678 0.027 Uiso 1 1 calc R . . C18 C -0.0553(3) 0.9054(4) 0.07795(16) 0.0215(12) Uani 1 1 d . . . C19 C 0.0057(3) 0.9825(4) 0.06894(15) 0.0218(12) Uani 1 1 d . . . H19 H 0.0083 1.0535 0.0811 0.026 Uiso 1 1 calc R . . C20 C 0.0637(3) 0.9558(4) 0.04188(14) 0.0184(11) Uani 1 1 d . . . C21 C 0.0570(3) 0.8524(4) 0.02375(14) 0.0183(11) Uani 1 1 d . . . C22 C 0.1314(3) 1.0409(4) 0.03281(15) 0.0232(13) Uani 1 1 d . . . H22A H 0.1378 1.0333 0.0038 0.028 Uiso 1 1 calc R . . H22B H 0.1070 1.1153 0.0362 0.028 Uiso 1 1 calc R . . C23 C 0.2238(3) 1.0326(4) 0.05941(15) 0.0185(11) Uani 1 1 d . . . C24 C 0.2450(3) 1.0951(4) 0.09470(15) 0.0190(11) Uani 1 1 d . . . H24 H 0.2016 1.1437 0.1023 0.023 Uiso 1 1 calc R . . C25 C 0.3305(3) 1.0868(4) 0.11935(15) 0.0193(11) Uani 1 1 d . . . C26 C 0.3943(3) 1.0143(4) 0.11029(16) 0.0224(12) Uani 1 1 d . . . H26 H 0.4511 1.0087 0.1279 0.027 Uiso 1 1 calc R . . C27 C 0.3750(3) 0.9493(4) 0.07536(15) 0.0190(11) Uani 1 1 d . . . C28 C 0.2912(3) 0.9609(4) 0.04983(14) 0.0198(12) Uani 1 1 d . . . C29 C 0.2883(4) 0.7986(5) 0.1593(2) 0.0381(15) Uani 1 1 d . . . H29 H 0.3380 0.8368 0.1522 0.046 Uiso 1 1 calc R . . C30 C 0.2176(5) 0.7739(5) 0.1294(2) 0.0445(18) Uani 1 1 d . . . H30 H 0.2179 0.7962 0.1020 0.053 Uiso 1 1 calc R . . C31 C 0.1457(4) 0.7170(5) 0.1386(2) 0.0432(18) Uani 1 1 d . . . H31 H 0.0962 0.6996 0.1175 0.052 Uiso 1 1 calc R . . C32 C 0.1451(4) 0.6848(5) 0.1784(2) 0.0424(17) Uani 1 1 d . . . H32 H 0.0960 0.6439 0.1849 0.051 Uiso 1 1 calc R . . C33 C 0.2173(4) 0.7130(4) 0.20907(18) 0.0323(14) Uani 1 1 d . . . H33 H 0.2164 0.6930 0.2367 0.039 Uiso 1 1 calc R . . C34 C 0.2906(4) 0.7700(4) 0.19974(17) 0.0296(14) Uani 1 1 d . . . C35 C 0.3700(4) 0.7987(5) 0.2324(2) 0.0473(19) Uani 1 1 d . . . H35A H 0.4254 0.7944 0.2205 0.057 Uiso 1 1 calc R . . H35B H 0.3752 0.7435 0.2546 0.057 Uiso 1 1 calc R . . C36 C 0.3633(4) 0.9138(5) 0.2505(2) 0.0448(18) Uani 1 1 d . . . H36A H 0.4215 0.9329 0.2681 0.054 Uiso 1 1 calc R . . H36B H 0.3513 0.9684 0.2280 0.054 Uiso 1 1 calc R . . C37 C 0.2091(4) 0.9504(4) 0.26227(16) 0.0268(13) Uani 1 1 d . . . C38 C 0.1066(3) 1.0048(4) 0.19900(15) 0.0221(12) Uani 1 1 d . . . C39 C 0.5920(5) 0.8095(6) 0.9807(2) 0.062(2) Uani 1 1 d . . . H39 H 0.5905 0.8696 0.9623 0.075 Uiso 1 1 calc R . . C40 C 0.6639(5) 0.7996(7) 1.0123(2) 0.082(3) Uani 1 1 d . . . H40 H 0.7089 0.8551 1.0166 0.098 Uiso 1 1 calc R . . C41 C 0.6707(4) 0.7083(7) 1.0378(2) 0.053(2) Uani 1 1 d . . . H41 H 0.7214 0.6986 1.0591 0.064 Uiso 1 1 calc R . . C42 C 0.6026(4) 0.6327(5) 1.03164(19) 0.0386(16) Uani 1 1 d . . . H42 H 0.6060 0.5697 1.0488 0.046 Uiso 1 1 calc R . . C43 C 0.5293(4) 0.6465(5) 1.00096(18) 0.0316(14) Uani 1 1 d . . . H43 H 0.4826 0.5931 0.9978 0.038 Uiso 1 1 calc R . . C44 C 0.5210(4) 0.7345(5) 0.97469(17) 0.0327(15) Uani 1 1 d . . . C45 C 0.4379(4) 0.7510(5) 0.94207(18) 0.0403(16) Uani 1 1 d . . . H45A H 0.3846 0.7266 0.9531 0.048 Uiso 1 1 calc R . . H45B H 0.4308 0.8306 0.9359 0.048 Uiso 1 1 calc R . . C46 C 0.4403(3) 0.6898(5) 0.90291(16) 0.0312(14) Uani 1 1 d . . . H46A H 0.4829 0.7260 0.8878 0.037 Uiso 1 1 calc R . . H46B H 0.4606 0.6132 0.9091 0.037 Uiso 1 1 calc R . . C47 C 0.3211(3) 0.7503(4) 0.84565(15) 0.0209(12) Uani 1 1 d . . . C48 C 0.1807(3) 0.7850(4) 0.79682(15) 0.0222(12) Uani 1 1 d . . . O17 O 0.5123(2) 0.2339(3) 0.26172(12) 0.0342(10) Uani 1 1 d . . . O18 O 0.6494(2) 0.3805(3) 0.25145(12) 0.0343(10) Uani 1 1 d . . . O19 O 0.9133(4) 0.5405(4) 0.19843(16) 0.0704(17) Uani 1 1 d . . . O20 O 0.7712(2) 0.6464(3) 0.15019(13) 0.0375(11) Uani 1 1 d . . . O21 O 0.1780(2) 0.7758(3) 0.91111(12) 0.0342(10) Uani 1 1 d . . . O22 O 0.2289(3) 0.5375(3) 0.90250(15) 0.0480(12) Uani 1 1 d . . . O23 O 0.3172(6) 0.9963(7) 0.7754(3) 0.039(2) Uani 0.50 1 d P A 1 O23' O 0.2908(6) 1.0103(7) 0.8009(3) 0.049(3) Uani 0.50 1 d P B 2 O24 O 0.5522(6) 0.9591(7) 0.2269(3) 0.046(2) Uani 0.50 1 d P . . O25 O 0.6315(6) 0.9959(8) 0.1141(3) 0.055(3) Uani 0.50 1 d PU C 1 O25' O 0.6332(8) 0.9446(11) 0.1337(4) 0.078(3) Uani 0.50 1 d PU D 2 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 0.0226(6) 0.0248(6) 0.0210(6) -0.0020(5) -0.0003(5) 0.0032(5) S2 0.0279(6) 0.0190(6) 0.0283(7) 0.0003(5) -0.0011(5) -0.0009(5) S3 0.0245(6) 0.0252(6) 0.0323(7) -0.0029(6) 0.0050(5) -0.0043(5) S4 0.0191(6) 0.0278(6) 0.0177(6) -0.0057(5) 0.0019(5) -0.0025(5) O1 0.0262(17) 0.0257(18) 0.026(2) -0.0023(16) 0.0015(15) 0.0007(15) O2 0.0275(18) 0.045(2) 0.028(2) 0.0029(18) 0.0013(16) -0.0111(17) O3 0.0280(17) 0.0325(19) 0.0203(19) -0.0014(16) 0.0050(14) 0.0031(15) O4 0.043(2) 0.032(2) 0.026(2) -0.0059(17) -0.0068(17) 0.0147(17) O5 0.0292(18) 0.0267(18) 0.024(2) -0.0020(16) 0.0005(15) -0.0004(15) O6 0.037(2) 0.0305(19) 0.033(2) 0.0102(18) -0.0077(17) -0.0076(17) O7 0.0242(17) 0.0205(17) 0.045(2) -0.0052(17) 0.0053(16) -0.0076(15) O8 0.044(2) 0.0261(19) 0.037(2) 0.0002(17) 0.0134(17) 0.0042(17) O9 0.0341(18) 0.0178(17) 0.0232(19) -0.0018(15) 0.0040(15) 0.0009(15) O10 0.071(3) 0.032(2) 0.083(3) -0.001(2) 0.053(2) -0.010(2) O11 0.0232(19) 0.058(3) 0.047(3) -0.018(2) -0.0112(18) 0.0067(19) O12 0.0225(17) 0.037(2) 0.024(2) -0.0076(16) 0.0026(14) 0.0006(15) O13 0.0274(18) 0.0330(19) 0.0161(18) -0.0057(16) -0.0011(14) 0.0022(16) O14 0.0236(17) 0.040(2) 0.024(2) -0.0073(17) 0.0053(15) -0.0024(16) O15 0.040(2) 0.0247(19) 0.032(2) -0.0080(17) 0.0062(17) -0.0051(16) O16 0.0187(16) 0.045(2) 0.025(2) -0.0120(17) 0.0005(14) 0.0005(16) N1 0.037(3) 0.036(3) 0.028(3) -0.004(2) -0.015(2) 0.015(2) N2 0.038(2) 0.036(2) 0.015(2) 0.006(2) 0.0016(18) 0.003(2) N3 0.0173(19) 0.032(2) 0.025(2) -0.002(2) -0.0015(17) 0.0025(18) N4 0.028(2) 0.023(2) 0.023(2) 0.0071(19) 0.0028(17) 0.0051(18) N6 0.022(2) 0.029(2) 0.018(2) -0.0022(19) 0.0019(16) 0.0033(18) N7 0.018(2) 0.046(3) 0.033(3) 0.007(2) -0.0004(18) -0.001(2) N8 0.021(2) 0.031(2) 0.023(2) 0.0053(19) 0.0032(17) 0.0031(18) N9 0.020(2) 0.035(2) 0.024(2) -0.002(2) 0.0012(17) 0.0067(18) C1 0.030(3) 0.021(2) 0.019(3) -0.001(2) 0.009(2) -0.001(2) C2 0.022(2) 0.024(2) 0.023(3) -0.002(2) 0.0071(19) 0.000(2) C3 0.018(2) 0.024(3) 0.026(3) -0.003(2) 0.0046(19) -0.0016(19) C4 0.019(2) 0.032(3) 0.016(2) -0.002(2) -0.0013(19) 0.005(2) C5 0.023(2) 0.022(2) 0.021(3) 0.001(2) 0.0058(19) 0.004(2) C6 0.019(2) 0.020(2) 0.019(2) -0.006(2) 0.0051(18) 0.0049(19) C7 0.021(2) 0.021(2) 0.019(3) -0.001(2) 0.0062(19) 0.0078(19) C8 0.027(2) 0.020(2) 0.022(3) -0.004(2) 0.003(2) 0.001(2) C9 0.024(2) 0.021(2) 0.023(3) -0.006(2) -0.002(2) -0.001(2) C10 0.024(2) 0.020(2) 0.023(3) -0.006(2) -0.007(2) 0.002(2) C11 0.028(3) 0.017(2) 0.024(3) -0.005(2) -0.002(2) -0.003(2) C12 0.029(3) 0.017(2) 0.024(3) -0.008(2) -0.002(2) 0.000(2) C13 0.026(2) 0.015(2) 0.017(2) -0.001(2) -0.0037(19) -0.0030(19) C14 0.031(3) 0.018(2) 0.016(3) -0.002(2) -0.002(2) -0.001(2) C15 0.019(2) 0.020(2) 0.023(3) -0.003(2) -0.0005(19) -0.0009(19) C16 0.023(2) 0.020(2) 0.017(3) 0.003(2) -0.0067(19) 0.002(2) C17 0.020(2) 0.023(2) 0.020(3) 0.002(2) -0.0053(19) 0.000(2) C18 0.019(2) 0.022(2) 0.022(3) 0.001(2) -0.0026(19) 0.000(2) C19 0.025(2) 0.016(2) 0.020(3) 0.002(2) -0.008(2) -0.001(2) C20 0.020(2) 0.019(2) 0.013(2) 0.003(2) -0.0028(18) 0.0020(19) C21 0.021(2) 0.021(2) 0.011(2) 0.006(2) -0.0030(18) 0.0027(19) C22 0.028(3) 0.022(2) 0.016(3) -0.004(2) -0.005(2) 0.003(2) C23 0.018(2) 0.022(2) 0.016(2) 0.001(2) 0.0037(18) -0.0022(19) C24 0.020(2) 0.017(2) 0.021(3) 0.002(2) 0.0031(19) 0.0005(19) C25 0.024(2) 0.018(2) 0.017(2) -0.004(2) 0.0090(19) -0.0072(19) C26 0.022(2) 0.020(2) 0.025(3) 0.007(2) 0.005(2) -0.001(2) C27 0.025(2) 0.017(2) 0.016(2) 0.004(2) 0.0060(19) -0.0015(19) C28 0.026(2) 0.023(2) 0.010(2) 0.000(2) 0.0038(18) -0.001(2) C29 0.046(3) 0.029(3) 0.045(4) -0.004(3) 0.023(3) 0.000(3) C30 0.064(4) 0.043(3) 0.028(3) 0.005(3) 0.010(3) 0.000(3) C31 0.047(3) 0.040(3) 0.037(4) -0.012(3) -0.006(3) 0.008(3) C32 0.036(3) 0.035(3) 0.059(4) -0.009(3) 0.017(3) -0.008(3) C33 0.050(3) 0.025(3) 0.023(3) 0.006(2) 0.010(2) 0.006(2) C34 0.038(3) 0.020(3) 0.030(3) -0.005(2) 0.008(2) 0.008(2) C35 0.039(3) 0.043(3) 0.052(4) -0.017(3) -0.012(3) 0.013(3) C36 0.030(3) 0.046(3) 0.051(4) -0.020(3) -0.011(3) 0.008(3) C37 0.031(3) 0.023(3) 0.022(3) -0.007(2) -0.006(2) 0.007(2) C38 0.030(3) 0.022(2) 0.014(2) -0.003(2) 0.001(2) 0.005(2) C39 0.076(5) 0.065(4) 0.038(4) 0.024(3) -0.010(3) -0.036(4) C40 0.077(4) 0.117(6) 0.043(4) 0.023(4) -0.015(4) -0.073(4) C41 0.035(3) 0.091(5) 0.029(4) 0.006(4) -0.005(3) -0.013(3) C42 0.049(3) 0.038(3) 0.031(3) 0.005(3) 0.013(3) 0.005(3) C43 0.028(3) 0.030(3) 0.040(3) -0.007(3) 0.014(2) -0.001(2) C44 0.041(3) 0.033(3) 0.023(3) -0.002(2) 0.004(2) -0.007(2) C45 0.045(3) 0.047(4) 0.027(3) -0.007(3) 0.000(3) 0.003(3) C46 0.027(3) 0.048(3) 0.016(3) 0.002(2) -0.004(2) 0.005(2) C47 0.017(2) 0.025(2) 0.020(3) -0.003(2) 0.0015(19) 0.000(2) C48 0.023(2) 0.026(3) 0.018(3) 0.000(2) 0.0033(19) -0.002(2) O17 0.0306(19) 0.043(2) 0.026(2) -0.0034(18) -0.0005(16) 0.0022(17) O18 0.0320(19) 0.036(2) 0.033(2) -0.0025(18) -0.0001(16) 0.0128(17) O19 0.089(4) 0.051(3) 0.053(3) -0.026(2) -0.034(3) 0.019(3) O20 0.032(2) 0.037(2) 0.044(3) 0.0062(19) 0.0089(17) 0.0002(17) O21 0.0320(19) 0.039(2) 0.034(2) 0.0070(18) 0.0137(16) 0.0072(17) O22 0.056(3) 0.036(2) 0.055(3) 0.007(2) 0.021(2) 0.002(2) O23 0.053(5) 0.035(4) 0.032(5) 0.008(4) 0.014(4) 0.004(4) O23' 0.038(5) 0.039(5) 0.065(7) 0.019(5) -0.002(4) -0.007(4) O24 0.041(4) 0.050(5) 0.050(6) 0.001(4) 0.015(4) -0.003(4) O25 0.041(4) 0.062(5) 0.062(5) -0.009(4) 0.007(4) 0.002(4) O25' 0.066(5) 0.084(6) 0.082(6) -0.013(5) 0.011(5) -0.006(5) _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 O4 1.450(4) . ? S1 O2 1.459(4) . ? S1 O3 1.462(4) . ? S1 C4 1.767(5) . ? S2 O8 1.453(4) . ? S2 O6 1.456(4) . ? S2 O7 1.461(4) . ? S2 C11 1.768(5) . ? S3 O10 1.439(5) . ? S3 O11 1.443(4) . ? S3 O12 1.458(4) . ? S3 C18 1.757(5) . ? S4 O15 1.448(4) . ? S4 O16 1.454(4) . ? S4 O14 1.459(4) . ? S4 C25 1.775(5) . ? O1 C7 1.363(6) . ? O1 H1 0.8400 . ? O5 C14 1.375(6) . ? O5 H5 0.8400 . ? O9 C21 1.382(6) . ? O9 H9 0.8400 . ? O13 C28 1.379(6) . ? O13 H13 0.8400 . ? N1 C37 1.309(7) . ? N1 C36 1.448(8) . ? N1 H1C 0.8800 . ? N2 C37 1.310(7) . ? N2 H2 0.9349 . ? N2 H2A 0.9028 . ? N3 C38 1.370(6) . ? N3 C37 1.389(7) . ? N3 H3 0.8800 . ? N4 C38 1.317(7) . ? N4 H4A 0.8281 . ? N4 H4B 1.0195 . ? N5 C38 1.300(6) . ? N5 H5A 0.9482 . ? N5 H5B 0.9025 . ? N6 C47 1.302(6) . ? N6 C46 1.475(6) . ? N6 H6 0.8800 . ? N7 C47 1.322(7) . ? N7 H7 0.6633 . ? N7 H7A 0.9054 . ? N8 C48 1.377(6) . ? N8 C47 1.384(6) . ? N8 H8 0.8800 . ? N9 C48 1.321(7) . ? N9 H9A 0.9414 . ? N9 H9B 0.8948 . ? N10 C48 1.321(6) . ? N10 H10A 0.9941 . ? N10 H10B 0.9070 . ? C1 C27 1.518(7) . ? C1 C2 1.536(7) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.386(7) . ? C2 C7 1.418(7) . ? C3 C4 1.399(7) . ? C3 H3A 0.9500 . ? C4 C5 1.377(7) . ? C5 C6 1.392(7) . ? C5 H5D 0.9500 . ? C6 C7 1.395(7) . ? C6 C8 1.519(7) . ? C8 C9 1.537(7) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.385(8) . ? C9 C14 1.408(7) . ? C10 C11 1.407(7) . ? C10 H10 0.9500 . ? C11 C12 1.385(7) . ? C12 C13 1.381(7) . ? C12 H12 0.9500 . ? C13 C14 1.388(7) . ? C13 C15 1.528(7) . ? C15 C16 1.517(7) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.399(7) . ? C16 C21 1.404(7) . ? C17 C18 1.376(7) . ? C17 H17 0.9500 . ? C18 C19 1.385(7) . ? C19 C20 1.404(7) . ? C19 H19 0.9500 . ? C20 C21 1.388(7) . ? C20 C22 1.523(7) . ? C22 C23 1.514(6) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.384(7) . ? C23 C28 1.421(7) . ? C24 C25 1.402(6) . ? C24 H24 0.9500 . ? C25 C26 1.379(7) . ? C26 C27 1.389(7) . ? C26 H26 0.9500 . ? C27 C28 1.397(6) . ? C29 C30 1.352(9) . ? C29 C34 1.382(8) . ? C29 H29 0.9500 . ? C30 C31 1.369(9) . ? C30 H30 0.9500 . ? C31 C32 1.382(10) . ? C31 H31 0.9500 . ? C32 C33 1.392(8) . ? C32 H32 0.9500 . ? C33 C34 1.389(8) . ? C33 H33 0.9500 . ? C34 C35 1.505(8) . ? C35 C36 1.533(9) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C39 C40 1.371(10) . ? C39 C44 1.394(9) . ? C39 H39 0.9500 . ? C40 C41 1.388(11) . ? C40 H40 0.9500 . ? C41 C42 1.368(9) . ? C41 H41 0.9500 . ? C42 C43 1.372(8) . ? C42 H42 0.9500 . ? C43 C44 1.371(8) . ? C43 H43 0.9500 . ? C44 C45 1.515(8) . ? C45 C46 1.503(8) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? 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 O4 S1 O2 113.2(2) . . ? O4 S1 O3 111.7(2) . . ? O2 S1 O3 111.0(2) . . ? O4 S1 C4 105.7(2) . . ? O2 S1 C4 106.4(2) . . ? O3 S1 C4 108.4(2) . . ? O8 S2 O6 114.4(2) . . ? O8 S2 O7 111.7(2) . . ? O6 S2 O7 111.2(2) . . ? O8 S2 C11 106.5(2) . . ? O6 S2 C11 106.4(2) . . ? O7 S2 C11 106.0(2) . . ? O10 S3 O11 114.1(3) . . ? O10 S3 O12 112.7(3) . . ? O11 S3 O12 110.2(2) . . ? O10 S3 C18 106.9(3) . . ? O11 S3 C18 106.8(3) . . ? O12 S3 C18 105.6(2) . . ? O15 S4 O16 112.1(2) . . ? O15 S4 O14 111.1(2) . . ? O16 S4 O14 112.6(2) . . ? O15 S4 C25 107.0(2) . . ? O16 S4 C25 106.1(2) . . ? O14 S4 C25 107.5(2) . . ? C7 O1 H1 109.5 . . ? C14 O5 H5 109.5 . . ? C21 O9 H9 109.5 . . ? C28 O13 H13 109.5 . . ? C37 N1 C36 127.6(5) . . ? C37 N1 H1C 116.2 . . ? C36 N1 H1C 116.2 . . ? C37 N2 H2 115.0 . . ? C37 N2 H2A 122.0 . . ? H2 N2 H2A 123.0 . . ? C38 N3 C37 126.5(5) . . ? C38 N3 H3 116.8 . . ? C37 N3 H3 116.8 . . ? C38 N4 H4A 106.3 . . ? C38 N4 H4B 127.5 . . ? H4A N4 H4B 123.9 . . ? C38 N5 H5A 116.1 . . ? C38 N5 H5B 122.4 . . ? H5A N5 H5B 121.5 . . ? C47 N6 C46 126.6(5) . . ? C47 N6 H6 116.7 . . ? C46 N6 H6 116.7 . . ? C47 N7 H7 122.3 . . ? C47 N7 H7A 118.4 . . ? H7 N7 H7A 119.2 . . ? C48 N8 C47 126.2(4) . . ? C48 N8 H8 116.9 . . ? C47 N8 H8 116.9 . . ? C48 N9 H9A 138.3 . . ? C48 N9 H9B 109.9 . . ? H9A N9 H9B 111.7 . . ? C48 N10 H10A 115.5 . . ? C48 N10 H10B 121.4 . . ? H10A N10 H10B 123.1 . . ? C27 C1 C2 112.8(4) . . ? C27 C1 H1A 109.0 . . ? C2 C1 H1A 109.0 . . ? C27 C1 H1B 109.0 . . ? C2 C1 H1B 109.0 . . ? H1A C1 H1B 107.8 . . ? C3 C2 C7 118.4(5) . . ? C3 C2 C1 119.7(4) . . ? C7 C2 C1 121.9(4) . . ? C2 C3 C4 120.2(4) . . ? C2 C3 H3A 119.9 . . ? C4 C3 H3A 119.9 . . ? C5 C4 C3 120.3(4) . . ? C5 C4 S1 120.4(4) . . ? C3 C4 S1 119.2(4) . . ? C4 C5 C6 121.4(5) . . ? C4 C5 H5D 119.3 . . ? C6 C5 H5D 119.3 . . ? C5 C6 C7 117.9(4) . . ? C5 C6 C8 122.0(4) . . ? C7 C6 C8 120.1(4) . . ? O1 C7 C6 117.6(4) . . ? O1 C7 C2 120.6(4) . . ? C6 C7 C2 121.7(4) . . ? C6 C8 C9 114.2(4) . . ? C6 C8 H8A 108.7 . . ? C9 C8 H8A 108.7 . . ? C6 C8 H8B 108.7 . . ? C9 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? C10 C9 C14 118.0(5) . . ? C10 C9 C8 119.6(4) . . ? C14 C9 C8 122.3(5) . . ? C9 C10 C11 120.5(4) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C12 C11 C10 120.0(5) . . ? C12 C11 S2 120.5(4) . . ? C10 C11 S2 119.3(4) . . ? C13 C12 C11 120.5(5) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C12 C13 C14 119.2(4) . . ? C12 C13 C15 120.3(5) . . ? C14 C13 C15 120.5(4) . . ? O5 C14 C13 117.0(4) . . ? O5 C14 C9 121.3(5) . . ? C13 C14 C9 121.7(5) . . ? C16 C15 C13 112.4(4) . . ? C16 C15 H15A 109.1 . . ? C13 C15 H15A 109.1 . . ? C16 C15 H15B 109.1 . . ? C13 C15 H15B 109.1 . . ? H15A C15 H15B 107.9 . . ? C17 C16 C21 117.7(4) . . ? C17 C16 C15 120.0(4) . . ? C21 C16 C15 122.2(5) . . ? C18 C17 C16 121.2(5) . . ? C18 C17 H17 119.4 . . ? C16 C17 H17 119.4 . . ? C17 C18 C19 120.4(5) . . ? C17 C18 S3 119.3(4) . . ? C19 C18 S3 120.2(4) . . ? C18 C19 C20 120.1(5) . . ? C18 C19 H19 119.9 . . ? C20 C19 H19 119.9 . . ? C21 C20 C19 118.8(4) . . ? C21 C20 C22 121.8(4) . . ? C19 C20 C22 119.5(4) . . ? O9 C21 C20 117.3(4) . . ? O9 C21 C16 120.9(4) . . ? C20 C21 C16 121.7(5) . . ? C23 C22 C20 114.9(4) . . ? C23 C22 H22A 108.5 . . ? C20 C22 H22A 108.5 . . ? C23 C22 H22B 108.5 . . ? C20 C22 H22B 108.5 . . ? H22A C22 H22B 107.5 . . ? C24 C23 C28 117.4(4) . . ? C24 C23 C22 120.3(4) . . ? C28 C23 C22 122.3(4) . . ? C23 C24 C25 120.1(4) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C26 C25 C24 121.7(4) . . ? C26 C25 S4 121.2(4) . . ? C24 C25 S4 117.1(4) . . ? C25 C26 C27 119.8(4) . . ? C25 C26 H26 120.1 . . ? C27 C26 H26 120.1 . . ? C26 C27 C28 118.6(4) . . ? C26 C27 C1 120.5(4) . . ? C28 C27 C1 120.9(4) . . ? O13 C28 C27 117.2(4) . . ? O13 C28 C23 120.4(4) . . ? C27 C28 C23 122.3(4) . . ? C30 C29 C34 122.2(6) . . ? C30 C29 H29 118.9 . . ? C34 C29 H29 118.9 . . ? C29 C30 C31 120.2(6) . . ? C29 C30 H30 119.9 . . ? C31 C30 H30 119.9 . . ? C30 C31 C32 119.9(6) . . ? C30 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? C31 C32 C33 119.3(6) . . ? C31 C32 H32 120.4 . . ? C33 C32 H32 120.4 . . ? C34 C33 C32 120.8(6) . . ? C34 C33 H33 119.6 . . ? C32 C33 H33 119.6 . . ? C29 C34 C33 117.5(5) . . ? C29 C34 C35 121.1(6) . . ? C33 C34 C35 121.3(5) . . ? C34 C35 C36 113.1(5) . . ? C34 C35 H35A 109.0 . . ? C36 C35 H35A 109.0 . . ? C34 C35 H35B 109.0 . . ? C36 C35 H35B 109.0 . . ? H35A C35 H35B 107.8 . . ? N1 C36 C35 111.9(5) . . ? N1 C36 H36A 109.2 . . ? C35 C36 H36A 109.2 . . ? N1 C36 H36B 109.2 . . ? C35 C36 H36B 109.2 . . ? H36A C36 H36B 107.9 . . ? N1 C37 N2 122.8(5) . . ? N1 C37 N3 117.9(5) . . ? N2 C37 N3 119.2(5) . . ? N5 C38 N4 121.4(4) . . ? N5 C38 N3 116.3(5) . . ? N4 C38 N3 122.2(5) . . ? C40 C39 C44 122.4(7) . . ? C40 C39 H39 118.8 . . ? C44 C39 H39 118.8 . . ? C39 C40 C41 119.8(7) . . ? C39 C40 H40 120.1 . . ? C41 C40 H40 120.1 . . ? C42 C41 C40 118.3(6) . . ? C42 C41 H41 120.8 . . ? C40 C41 H41 120.8 . . ? C41 C42 C43 120.9(6) . . ? C41 C42 H42 119.5 . . ? C43 C42 H42 119.5 . . ? C44 C43 C42 122.4(5) . . ? C44 C43 H43 118.8 . . ? C42 C43 H43 118.8 . . ? C43 C44 C39 116.0(5) . . ? C43 C44 C45 121.7(5) . . ? C39 C44 C45 122.2(6) . . ? C46 C45 C44 113.9(5) . . ? C46 C45 H45A 108.8 . . ? C44 C45 H45A 108.8 . . ? C46 C45 H45B 108.8 . . ? C44 C45 H45B 108.8 . . ? H45A C45 H45B 107.7 . . ? N6 C46 C45 108.7(5) . . ? N6 C46 H46A 110.0 . . ? C45 C46 H46A 109.9 . . ? N6 C46 H46B 110.0 . . ? C45 C46 H46B 110.0 . . ? H46A C46 H46B 108.3 . . ? N6 C47 N7 125.6(4) . . ? N6 C47 N8 115.2(4) . . ? N7 C47 N8 119.1(4) . . ? N9 C48 N10 121.7(5) . . ? N9 C48 N8 122.1(4) . . ? N10 C48 N8 116.1(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 C27 C1 C2 C3 -94.2(5) . . . . ? C27 C1 C2 C7 85.8(6) . . . . ? C7 C2 C3 C4 -0.4(7) . . . . ? C1 C2 C3 C4 179.5(5) . . . . ? C2 C3 C4 C5 -0.6(8) . . . . ? C2 C3 C4 S1 176.6(4) . . . . ? O4 S1 C4 C5 34.5(5) . . . . ? O2 S1 C4 C5 155.1(4) . . . . ? O3 S1 C4 C5 -85.4(5) . . . . ? O4 S1 C4 C3 -142.7(4) . . . . ? O2 S1 C4 C3 -22.1(5) . . . . ? O3 S1 C4 C3 97.4(4) . . . . ? C3 C4 C5 C6 1.4(8) . . . . ? S1 C4 C5 C6 -175.7(4) . . . . ? C4 C5 C6 C7 -1.1(7) . . . . ? C4 C5 C6 C8 177.2(5) . . . . ? C5 C6 C7 O1 175.7(4) . . . . ? C8 C6 C7 O1 -2.7(7) . . . . ? C5 C6 C7 C2 0.0(7) . . . . ? C8 C6 C7 C2 -178.3(5) . . . . ? C3 C2 C7 O1 -174.8(4) . . . . ? C1 C2 C7 O1 5.2(7) . . . . ? C3 C2 C7 C6 0.7(7) . . . . ? C1 C2 C7 C6 -179.2(5) . . . . ? C5 C6 C8 C9 95.9(6) . . . . ? C7 C6 C8 C9 -85.8(6) . . . . ? C6 C8 C9 C10 -92.7(6) . . . . ? C6 C8 C9 C14 89.1(6) . . . . ? C14 C9 C10 C11 -0.3(7) . . . . ? C8 C9 C10 C11 -178.5(4) . . . . ? C9 C10 C11 C12 -2.3(7) . . . . ? C9 C10 C11 S2 172.0(4) . . . . ? O8 S2 C11 C12 -34.0(5) . . . . ? O6 S2 C11 C12 -156.5(4) . . . . ? O7 S2 C11 C12 85.0(4) . . . . ? O8 S2 C11 C10 151.7(4) . . . . ? O6 S2 C11 C10 29.3(5) . . . . ? O7 S2 C11 C10 -89.2(4) . . . . ? C10 C11 C12 C13 1.8(7) . . . . ? S2 C11 C12 C13 -172.5(4) . . . . ? C11 C12 C13 C14 1.4(7) . . . . ? C11 C12 C13 C15 -177.0(4) . . . . ? C12 C13 C14 O5 173.7(4) . . . . ? C15 C13 C14 O5 -7.8(7) . . . . ? C12 C13 C14 C9 -4.1(7) . . . . ? C15 C13 C14 C9 174.3(4) . . . . ? C10 C9 C14 O5 -174.2(4) . . . . ? C8 C9 C14 O5 4.0(7) . . . . ? C10 C9 C14 C13 3.6(7) . . . . ? C8 C9 C14 C13 -178.3(4) . . . . ? C12 C13 C15 C16 91.9(5) . . . . ? C14 C13 C15 C16 -86.5(6) . . . . ? C13 C15 C16 C17 -90.6(5) . . . . ? C13 C15 C16 C21 89.6(6) . . . . ? C21 C16 C17 C18 1.5(7) . . . . ? C15 C16 C17 C18 -178.4(4) . . . . ? C16 C17 C18 C19 -1.9(7) . . . . ? C16 C17 C18 S3 173.3(4) . . . . ? O10 S3 C18 C17 29.4(5) . . . . ? O11 S3 C18 C17 -93.1(4) . . . . ? O12 S3 C18 C17 149.6(4) . . . . ? O10 S3 C18 C19 -155.4(4) . . . . ? O11 S3 C18 C19 82.2(4) . . . . ? O12 S3 C18 C19 -35.2(4) . . . . ? C17 C18 C19 C20 0.4(7) . . . . ? S3 C18 C19 C20 -174.8(4) . . . . ? C18 C19 C20 C21 1.6(7) . . . . ? C18 C19 C20 C22 -179.1(4) . . . . ? C19 C20 C21 O9 174.3(4) . . . . ? C22 C20 C21 O9 -5.0(6) . . . . ? C19 C20 C21 C16 -2.0(7) . . . . ? C22 C20 C21 C16 178.6(4) . . . . ? C17 C16 C21 O9 -175.7(4) . . . . ? C15 C16 C21 O9 4.1(7) . . . . ? C17 C16 C21 C20 0.5(7) . . . . ? C15 C16 C21 C20 -179.6(4) . . . . ? C21 C20 C22 C23 -86.8(6) . . . . ? C19 C20 C22 C23 93.8(5) . . . . ? C20 C22 C23 C24 -93.8(6) . . . . ? C20 C22 C23 C28 85.5(6) . . . . ? C28 C23 C24 C25 0.4(7) . . . . ? C22 C23 C24 C25 179.8(4) . . . . ? C23 C24 C25 C26 -2.5(7) . . . . ? C23 C24 C25 S4 177.1(4) . . . . ? O15 S4 C25 C26 119.1(4) . . . . ? O16 S4 C25 C26 -0.8(5) . . . . ? O14 S4 C25 C26 -121.5(4) . . . . ? O15 S4 C25 C24 -60.6(4) . . . . ? O16 S4 C25 C24 179.6(4) . . . . ? O14 S4 C25 C24 58.8(4) . . . . ? C24 C25 C26 C27 1.7(7) . . . . ? S4 C25 C26 C27 -177.9(4) . . . . ? C25 C26 C27 C28 1.1(7) . . . . ? C25 C26 C27 C1 -179.3(4) . . . . ? C2 C1 C27 C26 92.4(5) . . . . ? C2 C1 C27 C28 -88.0(6) . . . . ? C26 C27 C28 O13 173.7(4) . . . . ? C1 C27 C28 O13 -5.9(7) . . . . ? C26 C27 C28 C23 -3.2(7) . . . . ? C1 C27 C28 C23 177.2(4) . . . . ? C24 C23 C28 O13 -174.3(4) . . . . ? C22 C23 C28 O13 6.3(7) . . . . ? C24 C23 C28 C27 2.5(7) . . . . ? C22 C23 C28 C27 -176.9(5) . . . . ? C34 C29 C30 C31 -1.2(10) . . . . ? C29 C30 C31 C32 0.2(10) . . . . ? C30 C31 C32 C33 1.4(9) . . . . ? C31 C32 C33 C34 -1.9(9) . . . . ? C30 C29 C34 C33 0.7(8) . . . . ? C30 C29 C34 C35 -179.9(6) . . . . ? C32 C33 C34 C29 0.9(8) . . . . ? C32 C33 C34 C35 -178.5(5) . . . . ? C29 C34 C35 C36 87.0(7) . . . . ? C33 C34 C35 C36 -93.6(7) . . . . ? C37 N1 C36 C35 -92.8(7) . . . . ? C34 C35 C36 N1 68.7(7) . . . . ? C36 N1 C37 N2 167.2(5) . . . . ? C36 N1 C37 N3 -15.5(8) . . . . ? C38 N3 C37 N1 150.9(5) . . . . ? C38 N3 C37 N2 -31.7(8) . . . . ? C37 N3 C38 N5 163.7(5) . . . . ? C37 N3 C38 N4 -15.3(8) . . . . ? C44 C39 C40 C41 4.6(13) . . . . ? C39 C40 C41 C42 -2.8(12) . . . . ? C40 C41 C42 C43 0.0(11) . . . . ? C41 C42 C43 C44 1.1(10) . . . . ? C42 C43 C44 C39 0.5(9) . . . . ? C42 C43 C44 C45 -177.5(6) . . . . ? C40 C39 C44 C43 -3.3(11) . . . . ? C40 C39 C44 C45 174.6(7) . . . . ? C43 C44 C45 C46 -85.5(7) . . . . ? C39 C44 C45 C46 96.7(8) . . . . ? C47 N6 C46 C45 104.1(6) . . . . ? C44 C45 C46 N6 166.4(5) . . . . ? C46 N6 C47 N7 16.4(8) . . . . ? C46 N6 C47 N8 -160.4(5) . . . . ? C48 N8 C47 N6 -155.0(5) . . . . ? C48 N8 C47 N7 28.0(8) . . . . ? C47 N8 C48 N9 29.6(8) . . . . ? C47 N8 C48 N10 -152.5(5) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.748 _refine_diff_density_min -0.539 _refine_diff_density_rms 0.122 # Attachment 'SC5A+MFM.cif' data_SC5A+MFM _database_code_depnum_ccdc_archive 'CCDC 820615' #TrackingRef 'SC5A+MFM.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H81.50 N12.50 O32 S5' _chemical_formula_sum 'C45 H81.50 N12.50 O32 S5' _chemical_formula_weight 1470.03 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 'P 1 21/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.2990(17) _cell_length_b 20.408(2) _cell_length_c 22.893(2) _cell_angle_alpha 90.00 _cell_angle_beta 107.014(6) _cell_angle_gamma 90.00 _cell_volume 6388.2(12) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 18125 _cell_measurement_theta_min 1.50 _cell_measurement_theta_max 27.90 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.528 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3100 _exptl_absorpt_coefficient_mu 0.283 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9404 _exptl_absorpt_correction_T_max 0.9562 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator multilayer _diffrn_measurement_device_type 'Rigaku Saturn724 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.222 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 50620 _diffrn_reflns_av_R_equivalents 0.0463 _diffrn_reflns_av_sigmaI/netI 0.0475 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 27.91 _reflns_number_total 15220 _reflns_number_gt 13677 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r2 (Rigaku, 2009)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r2' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure 4.0' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2009)' _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^)+(0.0569P)^2^+6.8155P] 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 15220 _refine_ls_number_parameters 1046 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.0755 _refine_ls_R_factor_gt 0.0655 _refine_ls_wR_factor_ref 0.1559 _refine_ls_wR_factor_gt 0.1504 _refine_ls_goodness_of_fit_ref 1.184 _refine_ls_restrained_S_all 1.198 _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 S1 S 0.22013(6) 0.57221(3) 0.48337(3) 0.02475(16) Uani 1 1 d D . . S2 S 0.24942(6) 0.43442(3) 0.23674(3) 0.02484(16) Uani 1 1 d . . . S3 S 0.29899(5) 0.07455(3) 0.23268(3) 0.02290(15) Uani 1 1 d . . . S4 S 0.24966(5) -0.09520(3) 0.50157(3) 0.01627(14) Uani 1 1 d . . . S5 S 0.39660(5) 0.23397(3) 0.58649(3) 0.02085(15) Uani 1 1 d . . . O1 O -0.03553(15) 0.33963(10) 0.43184(9) 0.0225(4) Uani 1 1 d . . . H1 H -0.051(3) 0.3263(17) 0.4635(16) 0.034 Uiso 1 1 d . . . O2 O -0.09108(16) 0.29399(10) 0.27014(9) 0.0245(4) Uani 1 1 d . A . H2 H -0.151(3) 0.3212(18) 0.2627(16) 0.037 Uiso 1 1 d . . . O3 O -0.06516(15) 0.16136(10) 0.28054(9) 0.0223(4) Uani 1 1 d . A . H3 H -0.075(3) 0.2009(19) 0.2743(16) 0.033 Uiso 1 1 d . . . O4 O -0.02500(15) 0.12517(9) 0.42058(8) 0.0210(4) Uani 1 1 d . A . H4 H -0.068(3) 0.1184(17) 0.3869(16) 0.031 Uiso 1 1 d . . . O5 O -0.03258(13) 0.24491(9) 0.53123(8) 0.0181(4) Uani 1 1 d . A . H5 H -0.063(3) 0.2051(17) 0.5252(15) 0.027 Uiso 1 1 d . . . O6 O 0.2791(3) 0.57296(17) 0.44003(15) 0.0235(9) Uani 0.532(4) 1 d PD A 1 O7 O 0.2971(3) 0.56307(18) 0.54728(14) 0.0261(9) Uani 0.532(4) 1 d PD A 1 O8 O 0.1676(3) 0.62978(17) 0.48422(19) 0.0301(10) Uani 0.532(4) 1 d PD A 1 O6' O 0.1811(3) 0.61155(19) 0.42407(16) 0.0242(10) Uani 0.468(4) 1 d PD A 2 O7' O 0.3074(3) 0.5438(2) 0.49064(19) 0.0249(11) Uani 0.468(4) 1 d PD A 2 O8' O 0.1990(3) 0.60847(19) 0.53188(16) 0.0220(10) Uani 0.468(4) 1 d PD A 2 O9 O 0.25744(19) 0.49612(11) 0.26997(11) 0.0416(6) Uani 1 1 d . . . O10 O 0.23148(18) 0.44567(13) 0.17218(9) 0.0431(6) Uani 1 1 d . . . O11 O 0.33156(16) 0.39165(10) 0.26361(11) 0.0343(5) Uani 1 1 d . . . O12 O 0.36711(15) 0.12979(10) 0.24895(9) 0.0288(5) Uani 1 1 d . . . O13 O 0.27318(16) 0.06022(10) 0.16754(9) 0.0284(5) Uani 1 1 d . . . O14 O 0.33294(16) 0.01711(10) 0.27028(9) 0.0299(5) Uani 1 1 d . . . O15 O 0.32271(15) -0.09220(10) 0.46889(9) 0.0267(4) Uani 1 1 d . . . O16 O 0.18786(15) -0.15312(9) 0.48501(9) 0.0235(4) Uani 1 1 d . . . O17 O 0.29477(14) -0.08922(9) 0.56733(8) 0.0223(4) Uani 1 1 d . . . O18 O 0.40726(16) 0.24562(12) 0.52597(10) 0.0331(5) Uani 1 1 d . . . O19 O 0.43089(16) 0.16930(11) 0.60945(12) 0.0407(6) Uani 1 1 d . . . O20 O 0.43941(15) 0.28623(10) 0.62873(9) 0.0258(4) Uani 1 1 d . . . O21 O 0.63122(17) 0.13393(11) 0.63876(10) 0.0279(5) Uani 1 1 d . . . H21A H 0.650(3) 0.119(2) 0.6114(18) 0.042 Uiso 1 1 d . . . H21B H 0.577(3) 0.138(2) 0.6317(18) 0.042 Uiso 1 1 d . . . O22 O 0.27169(18) 0.76815(11) 0.95679(10) 0.0271(5) Uani 1 1 d . . . H22A H 0.248(3) 0.732(2) 0.9599(17) 0.041 Uiso 1 1 d . . . H22B H 0.232(3) 0.796(2) 0.9577(17) 0.041 Uiso 1 1 d . . . O23 O 0.21458(16) 0.91107(10) 0.66144(9) 0.0236(4) Uani 1 1 d . . . H23A H 0.236(3) 0.9113(18) 0.6319(18) 0.035 Uiso 1 1 d . . . H23B H 0.227(3) 0.9464(19) 0.6766(17) 0.035 Uiso 1 1 d . . . O24 O 0.36781(19) 0.24104(12) 0.78162(11) 0.0346(5) Uani 1 1 d . . . H24A H 0.354(3) 0.205(2) 0.773(2) 0.052 Uiso 1 1 d . . . H24B H 0.364(3) 0.270(2) 0.751(2) 0.052 Uiso 1 1 d . . . O25 O 0.47130(18) 0.61053(13) 0.74110(12) 0.0373(6) Uani 1 1 d . . . H25A H 0.493(4) 0.586(2) 0.770(2) 0.056 Uiso 1 1 d . . . H25B H 0.418(3) 0.595(2) 0.718(2) 0.056 Uiso 1 1 d . . . O26 O 0.24856(18) 0.64238(12) 0.74596(11) 0.0350(5) Uani 1 1 d . . . H26A H 0.255(3) 0.620(2) 0.720(2) 0.053 Uiso 1 1 d . . . H26B H 0.282(3) 0.630(2) 0.779(2) 0.053 Uiso 1 1 d . . . O27 O 0.3484(2) 0.02519(13) 0.39501(12) 0.0376(6) Uani 1 1 d . . . H27A H 0.383(4) 0.014(3) 0.413(2) 0.056 Uiso 1 1 d . . . H27B H 0.354(3) 0.020(2) 0.353(2) 0.056 Uiso 1 1 d . . . O28 O 0.5384(2) 0.31569(12) 0.48178(15) 0.0459(7) Uani 1 1 d . . . H28A H 0.504(4) 0.296(2) 0.500(2) 0.069 Uiso 1 1 d . . . H28B H 0.586(4) 0.302(3) 0.494(2) 0.069 Uiso 1 1 d . . . O29 O 0.2858(2) 0.57282(13) 0.65535(12) 0.0507(8) Uani 1 1 d . . . H29A H 0.266(4) 0.586(2) 0.615(2) 0.076 Uiso 1 1 d . . . H29B H 0.274(4) 0.532(3) 0.660(2) 0.076 Uiso 1 1 d . . . O30 O 0.4638(3) 0.47988(17) 0.04974(15) 0.0740(10) Uani 1 1 d . . . H30A H 0.5219 0.4926 0.0677 0.111 Uiso 1 1 d R . . H30B H 0.4676 0.4409 0.0373 0.111 Uiso 1 1 d R . . O31 O 0.4258(3) 0.4718(2) 0.16174(16) 0.0845(12) Uani 1 1 d . . . H31B H 0.4731 0.4935 0.1854 0.127 Uiso 1 1 d R . . H31A H 0.4214 0.4786 0.1246 0.127 Uiso 1 1 d R . . N1 N 0.4851(2) 0.35530(13) 0.96742(11) 0.0268(5) Uani 1 1 d . . . H1A H 0.536(3) 0.3800(19) 0.9847(17) 0.040 Uiso 1 1 d . . . H1B H 0.456(3) 0.3378(19) 0.9903(17) 0.040 Uiso 1 1 d . . . N2 N 0.5023(2) 0.36547(13) 0.87103(12) 0.0279(6) Uani 1 1 d . . . H2A H 0.562(3) 0.3859(19) 0.8879(17) 0.042 Uiso 1 1 d . . . H2B H 0.470(3) 0.3656(18) 0.8309(18) 0.042 Uiso 1 1 d . . . N3 N 0.37064(17) 0.30938(12) 0.88403(11) 0.0219(5) Uani 1 1 d . . . H3A H 0.368(3) 0.2902(17) 0.8498(16) 0.033 Uiso 1 1 d . . . N4 N 0.26463(19) 0.36447(12) 0.92625(11) 0.0225(5) Uani 1 1 d . . . H4A H 0.288(3) 0.4051(18) 0.9176(16) 0.034 Uiso 1 1 d . . . H4B H 0.224(3) 0.3651(18) 0.9452(16) 0.034 Uiso 1 1 d . . . N5 N 0.23744(17) 0.25514(11) 0.89821(10) 0.0212(5) Uani 1 1 d . . . N6 N 0.69442(19) 0.26998(12) 0.65791(11) 0.0236(5) Uani 1 1 d . . . H6A H 0.701(3) 0.2739(17) 0.6194(17) 0.035 Uiso 1 1 d . . . H6B H 0.680(3) 0.2314(18) 0.6719(17) 0.035 Uiso 1 1 d . . . N7 N 0.7334(2) 0.37812(14) 0.67743(12) 0.0337(7) Uani 1 1 d . . . H7A H 0.745(3) 0.386(2) 0.645(2) 0.051 Uiso 1 1 d . . . H7B H 0.731(3) 0.414(2) 0.6997(19) 0.051 Uiso 1 1 d . . . N8 N 0.70227(18) 0.31656(12) 0.75272(10) 0.0221(5) Uani 1 1 d . . . H8A H 0.726(3) 0.3491(18) 0.7767(16) 0.033 Uiso 1 1 d . . . N9 N 0.57238(18) 0.24325(13) 0.73894(11) 0.0232(5) Uani 1 1 d . . . H9A H 0.538(3) 0.2614(17) 0.7059(17) 0.035 Uiso 1 1 d . . . H9B H 0.554(3) 0.2048(19) 0.7501(16) 0.035 Uiso 1 1 d . . . N10 N 0.68530(17) 0.25583(11) 0.83385(10) 0.0199(5) Uani 1 1 d . . . C1 C 0.0215(2) 0.39458(12) 0.44596(11) 0.0183(5) Uani 1 1 d . . . C2 C 0.07621(19) 0.40830(12) 0.50619(11) 0.0172(5) Uani 1 1 d . A . C3 C 0.1361(2) 0.46319(13) 0.51716(12) 0.0200(5) Uani 1 1 d . . . H3C H 0.1749 0.4727 0.5576 0.024 Uiso 1 1 calc R A . C4 C 0.1398(2) 0.50432(13) 0.46948(12) 0.0247(6) Uani 1 1 d . A . C5 C 0.0818(3) 0.49132(14) 0.41060(12) 0.0286(7) Uani 1 1 d . . . H5C H 0.0821 0.5209 0.3786 0.034 Uiso 1 1 calc R A . C6 C 0.0233(2) 0.43594(13) 0.39759(12) 0.0227(6) Uani 1 1 d . A . C7 C -0.0399(2) 0.42062(14) 0.33319(12) 0.0263(6) Uani 1 1 d . . . H7C H -0.0935 0.3910 0.3356 0.032 Uiso 1 1 calc R A . H7D H -0.0700 0.4618 0.3136 0.032 Uiso 1 1 calc R . . C8 C -0.0141(2) 0.32943(13) 0.26269(11) 0.0205(5) Uani 1 1 d . . . C9 C 0.0151(2) 0.38891(13) 0.29299(11) 0.0226(6) Uani 1 1 d . A . C10 C 0.0962(2) 0.42024(13) 0.28394(11) 0.0234(6) Uani 1 1 d . . . H10 H 0.1176 0.4605 0.3042 0.028 Uiso 1 1 calc R A . C11 C 0.1461(2) 0.39402(13) 0.24617(11) 0.0204(5) Uani 1 1 d . A . C12 C 0.1162(2) 0.33504(13) 0.21622(11) 0.0195(5) Uani 1 1 d . . . H12 H 0.1506 0.3174 0.1901 0.023 Uiso 1 1 calc R A . C13 C 0.0362(2) 0.30185(13) 0.22451(11) 0.0192(5) Uani 1 1 d . A . C14 C 0.0044(2) 0.23709(12) 0.19262(11) 0.0186(5) Uani 1 1 d . . . H14A H 0.0162 0.2382 0.1521 0.022 Uiso 1 1 calc R A . H14B H -0.0668 0.2317 0.1858 0.022 Uiso 1 1 calc R . . C15 C 0.01709(19) 0.14138(13) 0.26692(11) 0.0177(5) Uani 1 1 d . . . C16 C 0.0570(2) 0.17807(12) 0.22784(11) 0.0175(5) Uani 1 1 d . A . C17 C 0.1443(2) 0.15723(13) 0.21962(11) 0.0195(5) Uani 1 1 d . . . H17 H 0.1738 0.1824 0.1949 0.023 Uiso 1 1 calc R A . C18 C 0.1896(2) 0.10016(13) 0.24698(12) 0.0202(5) Uani 1 1 d . A . C19 C 0.1459(2) 0.06210(13) 0.28159(11) 0.0187(5) Uani 1 1 d . . . H19 H 0.1755 0.0220 0.2985 0.022 Uiso 1 1 calc R A . C20 C 0.0589(2) 0.08188(12) 0.29186(11) 0.0177(5) Uani 1 1 d . A . C21 C 0.0085(2) 0.03739(13) 0.32656(11) 0.0182(5) Uani 1 1 d . . . H21C H -0.0587 0.0539 0.3207 0.022 Uiso 1 1 calc R A . H21D H 0.0030 -0.0069 0.3083 0.022 Uiso 1 1 calc R . . C22 C 0.03932(18) 0.07426(12) 0.43736(11) 0.0153(5) Uani 1 1 d . . . C23 C 0.05874(19) 0.03139(12) 0.39449(11) 0.0156(5) Uani 1 1 d . A . C24 C 0.12479(19) -0.01952(12) 0.41575(11) 0.0171(5) Uani 1 1 d . . . H24 H 0.1382 -0.0494 0.3874 0.020 Uiso 1 1 calc R A . C25 C 0.17154(19) -0.02725(12) 0.47794(11) 0.0160(5) Uani 1 1 d . A . C26 C 0.15258(18) 0.01623(12) 0.51976(11) 0.0157(5) Uani 1 1 d . . . H26 H 0.1853 0.0113 0.5621 0.019 Uiso 1 1 calc R A . C27 C 0.08567(18) 0.06722(12) 0.49990(11) 0.0139(5) Uani 1 1 d . A . C28 C 0.06077(19) 0.11319(12) 0.54507(11) 0.0151(5) Uani 1 1 d . . . H28C H 0.0769 0.0914 0.5855 0.018 Uiso 1 1 calc R A . H28D H -0.0105 0.1215 0.5317 0.018 Uiso 1 1 calc R . . C29 C 0.06706(18) 0.23889(12) 0.54703(10) 0.0143(5) Uani 1 1 d . . . C30 C 0.11409(19) 0.17821(12) 0.55195(10) 0.0150(5) Uani 1 1 d . A . C31 C 0.21612(19) 0.17776(13) 0.56621(11) 0.0170(5) Uani 1 1 d . . . H31 H 0.2496 0.1371 0.5693 0.020 Uiso 1 1 calc R A . C32 C 0.26944(19) 0.23574(13) 0.57588(11) 0.0174(5) Uani 1 1 d . A . C33 C 0.22133(19) 0.29573(12) 0.57306(11) 0.0166(5) Uani 1 1 d . . . H33 H 0.2581 0.3352 0.5807 0.020 Uiso 1 1 calc R A . C34 C 0.12018(19) 0.29802(12) 0.55919(11) 0.0158(5) Uani 1 1 d . A . C35 C 0.07034(19) 0.36412(12) 0.55812(11) 0.0165(5) Uani 1 1 d . . . H35A H 0.0006 0.3567 0.5550 0.020 Uiso 1 1 calc R A . H35B H 0.1007 0.3869 0.5973 0.020 Uiso 1 1 calc R . . C36 C 0.4543(2) 0.34537(14) 0.90865(13) 0.0226(6) Uani 1 1 d . . . C37 C 0.2895(2) 0.30937(13) 0.90452(11) 0.0196(5) Uani 1 1 d . . . C38 C 0.1385(2) 0.25582(16) 0.90497(13) 0.0270(6) Uani 1 1 d . . . H38A H 0.1423 0.2495 0.9480 0.041 Uiso 1 1 calc R . . H38B H 0.0998 0.2204 0.8805 0.041 Uiso 1 1 calc R . . H38C H 0.1073 0.2980 0.8909 0.041 Uiso 1 1 calc R . . C39 C 0.2784(2) 0.19004(14) 0.89270(14) 0.0306(7) Uani 1 1 d . . . H39A H 0.2477 0.1726 0.8517 0.046 Uiso 1 1 calc R . . H39B H 0.2655 0.1604 0.9232 0.046 Uiso 1 1 calc R . . H39C H 0.3491 0.1938 0.8996 0.046 Uiso 1 1 calc R . . C40 C 0.7087(2) 0.32085(14) 0.69411(11) 0.0207(5) Uani 1 1 d . . . C41 C 0.65199(19) 0.26982(13) 0.77490(11) 0.0180(5) Uani 1 1 d . . . C42 C 0.7878(2) 0.26241(14) 0.87014(12) 0.0230(6) Uani 1 1 d . . . H42A H 0.8260 0.2798 0.8444 0.034 Uiso 1 1 calc R . . H42B H 0.8135 0.2194 0.8861 0.034 Uiso 1 1 calc R . . H42C H 0.7925 0.2925 0.9043 0.034 Uiso 1 1 calc R . . C43 C 0.6238(2) 0.22237(16) 0.86545(13) 0.0305(7) Uani 1 1 d . . . H43A H 0.5548 0.2285 0.8426 0.046 Uiso 1 1 calc R . . H43B H 0.6360 0.2407 0.9066 0.046 Uiso 1 1 calc R . . H43C H 0.6393 0.1755 0.8684 0.046 Uiso 1 1 calc R . . O32 O 0.5574(3) 0.0784(2) 0.2507(2) 0.0338(10) Uani 0.50 1 d P . . N11 N 0.3727(4) 0.4858(2) 0.3965(2) 0.0261(11) Uani 0.50 1 d P B -1 H11A H 0.3398 0.4862 0.3575 0.031 Uiso 0.50 1 calc PR B -1 H11B H 0.3519 0.5090 0.4227 0.031 Uiso 0.50 1 calc PR B -1 N12 N 0.4872(4) 0.4158(3) 0.3795(2) 0.0293(12) Uani 0.50 1 d P B -1 H12A H 0.4564 0.4148 0.3401 0.035 Uiso 0.50 1 calc PR B -1 H12B H 0.5412 0.3929 0.3941 0.035 Uiso 0.50 1 calc PR B -1 N13 N 0.5003(4) 0.4467(2) 0.4768(2) 0.0202(10) Uani 0.50 1 d P B -1 H13A H 0.5269 0.4091 0.4918 0.024 Uiso 0.50 1 calc PR B -1 N14 N 0.5256(4) 0.5574(2) 0.4974(3) 0.0243(11) Uani 0.50 1 d P B -1 H14C H 0.5336 0.5912 0.5223 0.029 Uiso 0.50 1 calc PR B -1 H14D H 0.5293 0.5627 0.4600 0.029 Uiso 0.50 1 calc PR B -1 N15 N 0.5015(4) 0.4875(2) 0.5712(2) 0.0221(10) Uani 0.50 1 d P B -1 C44 C 0.4531(4) 0.4507(3) 0.4158(3) 0.0204(11) Uani 0.50 1 d P B -1 C45 C 0.5081(5) 0.4992(3) 0.5161(2) 0.0211(12) Uani 0.50 1 d P B -1 C46 C 0.5253(6) 0.5389(4) 0.6172(3) 0.0379(16) Uani 0.50 1 d P B -1 H46A H 0.5819 0.5637 0.6134 0.057 Uiso 0.50 1 calc PR B -1 H46B H 0.5408 0.5192 0.6580 0.057 Uiso 0.50 1 calc PR B -1 H46C H 0.4692 0.5684 0.6112 0.057 Uiso 0.50 1 calc PR B -1 C47 C 0.4612(5) 0.4267(3) 0.5886(3) 0.0278(13) Uani 0.50 1 d P B -1 H47A H 0.4352 0.3993 0.5524 0.042 Uiso 0.50 1 calc PR B -1 H47B H 0.4086 0.4375 0.6065 0.042 Uiso 0.50 1 calc PR B -1 H47C H 0.5130 0.4029 0.6187 0.042 Uiso 0.50 1 calc PR B -1 O33 O 0.4400(4) 0.4224(2) 0.6193(2) 0.0370(11) Uani 0.50 1 d P C -2 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 0.0400(4) 0.0147(3) 0.0262(3) -0.0004(2) 0.0200(3) -0.0028(3) S2 0.0290(4) 0.0204(3) 0.0200(3) 0.0035(2) -0.0008(3) -0.0072(3) S3 0.0254(4) 0.0233(3) 0.0220(3) 0.0031(3) 0.0101(3) 0.0041(3) S4 0.0159(3) 0.0144(3) 0.0191(3) 0.0022(2) 0.0062(2) 0.0025(2) S5 0.0143(3) 0.0213(3) 0.0251(3) -0.0014(2) 0.0028(2) -0.0019(2) O1 0.0222(10) 0.0243(10) 0.0189(9) -0.0015(7) 0.0027(8) -0.0061(8) O2 0.0284(11) 0.0217(10) 0.0274(10) 0.0019(8) 0.0144(9) 0.0002(8) O3 0.0221(10) 0.0199(10) 0.0275(10) 0.0045(8) 0.0113(8) 0.0030(8) O4 0.0220(10) 0.0178(9) 0.0192(9) 0.0001(7) 0.0000(8) 0.0056(8) O5 0.0144(9) 0.0141(9) 0.0247(9) -0.0001(7) 0.0039(7) -0.0004(7) O6 0.027(2) 0.0229(19) 0.0235(18) 0.0012(14) 0.0116(16) -0.0056(15) O7 0.027(2) 0.030(2) 0.0187(17) 0.0002(14) 0.0019(15) -0.0111(16) O8 0.028(2) 0.0133(18) 0.054(3) -0.0028(17) 0.019(2) 0.0007(15) O6' 0.029(2) 0.022(2) 0.021(2) 0.0047(16) 0.0066(17) -0.0075(17) O7' 0.012(2) 0.024(2) 0.041(3) -0.0036(18) 0.0103(18) 0.0011(16) O8' 0.032(2) 0.017(2) 0.019(2) -0.0057(16) 0.0112(18) -0.0079(17) O9 0.0511(16) 0.0203(11) 0.0490(14) -0.0035(10) 0.0075(12) -0.0128(10) O10 0.0405(14) 0.0642(17) 0.0196(10) 0.0098(10) 0.0012(9) -0.0272(12) O11 0.0267(12) 0.0238(11) 0.0464(13) 0.0058(9) 0.0011(10) -0.0047(9) O12 0.0255(11) 0.0305(11) 0.0323(11) 0.0010(9) 0.0118(9) -0.0001(9) O13 0.0372(12) 0.0309(11) 0.0202(9) 0.0010(8) 0.0132(9) 0.0077(9) O14 0.0326(12) 0.0290(11) 0.0298(11) 0.0078(9) 0.0120(9) 0.0089(9) O15 0.0245(11) 0.0289(11) 0.0322(11) 0.0094(8) 0.0170(9) 0.0083(9) O16 0.0217(10) 0.0140(9) 0.0334(10) -0.0002(8) 0.0058(8) 0.0017(8) O17 0.0222(10) 0.0246(10) 0.0173(9) 0.0027(7) 0.0013(7) 0.0060(8) O18 0.0210(11) 0.0543(15) 0.0258(10) -0.0071(10) 0.0095(9) -0.0063(10) O19 0.0178(11) 0.0243(12) 0.0744(17) 0.0065(11) 0.0046(11) 0.0017(9) O20 0.0187(10) 0.0282(11) 0.0245(9) -0.0029(8) -0.0030(8) -0.0033(8) O21 0.0239(11) 0.0336(12) 0.0261(10) -0.0044(9) 0.0071(9) 0.0016(10) O22 0.0380(13) 0.0146(10) 0.0358(11) 0.0018(8) 0.0220(10) 0.0014(9) O23 0.0289(11) 0.0220(10) 0.0199(9) -0.0013(8) 0.0071(8) 0.0008(9) O24 0.0466(15) 0.0271(12) 0.0323(12) -0.0084(10) 0.0148(11) -0.0100(11) O25 0.0266(12) 0.0408(14) 0.0420(13) -0.0105(11) 0.0062(11) 0.0042(10) O26 0.0311(13) 0.0384(14) 0.0308(12) -0.0034(10) 0.0016(10) 0.0043(10) O27 0.0482(17) 0.0284(13) 0.0408(15) 0.0007(10) 0.0203(12) 0.0024(11) O28 0.0581(19) 0.0247(13) 0.0699(19) 0.0081(12) 0.0420(16) 0.0040(12) O29 0.085(2) 0.0256(13) 0.0333(13) -0.0007(10) 0.0044(13) -0.0046(13) O30 0.066(2) 0.070(2) 0.073(2) -0.0186(17) -0.0006(17) 0.0095(18) O31 0.067(2) 0.123(3) 0.064(2) 0.011(2) 0.0197(18) 0.028(2) N1 0.0224(13) 0.0333(14) 0.0239(12) -0.0050(10) 0.0055(10) -0.0103(11) N2 0.0233(13) 0.0347(15) 0.0272(12) -0.0073(11) 0.0094(11) -0.0112(11) N3 0.0195(12) 0.0238(12) 0.0231(11) -0.0079(9) 0.0072(9) -0.0050(9) N4 0.0216(12) 0.0228(12) 0.0242(12) -0.0011(9) 0.0084(10) 0.0003(10) N5 0.0197(12) 0.0234(12) 0.0204(10) -0.0019(9) 0.0058(9) -0.0048(9) N6 0.0304(14) 0.0234(13) 0.0192(11) -0.0011(9) 0.0105(10) -0.0010(10) N7 0.0545(19) 0.0302(14) 0.0167(11) 0.0001(10) 0.0107(12) -0.0188(13) N8 0.0282(13) 0.0244(12) 0.0133(10) -0.0003(9) 0.0057(9) -0.0070(10) N9 0.0220(12) 0.0276(13) 0.0175(11) 0.0062(9) 0.0019(9) -0.0031(10) N10 0.0204(12) 0.0233(12) 0.0159(10) 0.0027(8) 0.0051(9) 0.0010(9) C1 0.0217(13) 0.0141(12) 0.0190(12) -0.0014(9) 0.0057(10) 0.0031(10) C2 0.0196(13) 0.0140(12) 0.0189(12) 0.0009(9) 0.0071(10) 0.0031(10) C3 0.0273(14) 0.0156(12) 0.0191(12) -0.0029(9) 0.0101(11) -0.0029(10) C4 0.0436(18) 0.0129(13) 0.0227(13) -0.0024(10) 0.0177(12) -0.0018(12) C5 0.055(2) 0.0157(13) 0.0197(13) 0.0003(10) 0.0180(13) 0.0019(13) C6 0.0344(16) 0.0178(13) 0.0158(11) -0.0013(9) 0.0072(11) 0.0066(11) C7 0.0382(17) 0.0242(14) 0.0139(12) 0.0008(10) 0.0034(11) 0.0112(12) C8 0.0275(15) 0.0185(13) 0.0157(11) 0.0040(9) 0.0067(10) 0.0016(11) C9 0.0338(16) 0.0184(13) 0.0135(11) 0.0029(9) 0.0037(11) 0.0050(11) C10 0.0351(16) 0.0152(13) 0.0153(11) 0.0014(9) 0.0001(11) 0.0014(11) C11 0.0258(14) 0.0170(13) 0.0157(11) 0.0039(9) 0.0016(10) -0.0007(10) C12 0.0238(14) 0.0191(13) 0.0142(11) 0.0029(9) 0.0034(10) 0.0005(10) C13 0.0257(14) 0.0160(12) 0.0144(11) 0.0014(9) 0.0035(10) 0.0009(10) C14 0.0232(14) 0.0161(12) 0.0167(11) 0.0013(9) 0.0061(10) -0.0017(10) C15 0.0191(13) 0.0193(13) 0.0132(11) -0.0027(9) 0.0024(9) -0.0015(10) C16 0.0232(13) 0.0154(12) 0.0141(11) -0.0013(9) 0.0059(10) -0.0010(10) C17 0.0268(14) 0.0182(13) 0.0140(11) -0.0013(9) 0.0069(10) -0.0028(11) C18 0.0224(14) 0.0218(13) 0.0174(12) -0.0022(10) 0.0077(10) 0.0003(11) C19 0.0227(14) 0.0188(13) 0.0134(11) 0.0003(9) 0.0036(10) -0.0002(10) C20 0.0229(13) 0.0168(12) 0.0123(10) -0.0001(9) 0.0032(10) -0.0038(10) C21 0.0224(13) 0.0168(12) 0.0140(11) 0.0015(9) 0.0034(10) -0.0023(10) C22 0.0150(12) 0.0107(11) 0.0194(11) 0.0035(9) 0.0036(10) -0.0002(9) C23 0.0164(12) 0.0151(12) 0.0148(11) 0.0022(9) 0.0038(9) -0.0035(9) C24 0.0191(13) 0.0145(12) 0.0191(12) -0.0008(9) 0.0078(10) -0.0021(10) C25 0.0153(12) 0.0143(12) 0.0186(11) 0.0026(9) 0.0052(10) -0.0010(9) C26 0.0147(12) 0.0152(12) 0.0167(11) 0.0012(9) 0.0040(9) -0.0022(9) C27 0.0138(12) 0.0127(11) 0.0154(11) 0.0009(9) 0.0045(9) -0.0034(9) C28 0.0168(12) 0.0126(12) 0.0164(11) 0.0003(9) 0.0057(9) -0.0014(9) C29 0.0129(11) 0.0177(12) 0.0120(10) -0.0006(9) 0.0032(9) -0.0001(9) C30 0.0176(12) 0.0166(12) 0.0115(10) -0.0008(9) 0.0052(9) -0.0009(10) C31 0.0172(12) 0.0167(12) 0.0162(11) -0.0002(9) 0.0037(9) 0.0001(10) C32 0.0157(12) 0.0198(13) 0.0159(11) 0.0003(9) 0.0033(9) -0.0002(10) C33 0.0193(13) 0.0143(12) 0.0162(11) -0.0005(9) 0.0052(10) -0.0027(10) C34 0.0203(13) 0.0153(12) 0.0129(10) 0.0008(9) 0.0066(9) -0.0010(10) C35 0.0201(13) 0.0128(12) 0.0180(11) -0.0002(9) 0.0075(10) -0.0019(10) C36 0.0186(13) 0.0219(14) 0.0268(13) -0.0064(10) 0.0058(11) -0.0009(11) C37 0.0181(13) 0.0231(13) 0.0159(11) 0.0006(9) 0.0021(10) -0.0010(10) C38 0.0230(15) 0.0354(16) 0.0232(13) -0.0032(12) 0.0076(11) -0.0081(12) C39 0.0347(17) 0.0218(15) 0.0353(16) -0.0070(12) 0.0104(13) -0.0040(13) C40 0.0196(13) 0.0256(14) 0.0166(11) 0.0020(10) 0.0047(10) -0.0020(11) C41 0.0176(13) 0.0204(13) 0.0171(11) 0.0017(9) 0.0069(10) 0.0007(10) C42 0.0237(14) 0.0253(14) 0.0170(12) 0.0006(10) 0.0013(10) 0.0020(11) C43 0.0344(17) 0.0360(17) 0.0228(13) 0.0082(12) 0.0109(12) -0.0037(14) O32 0.020(2) 0.034(2) 0.054(3) -0.004(2) 0.020(2) -0.0062(18) N11 0.019(2) 0.027(3) 0.026(2) -0.0063(19) -0.0019(19) 0.008(2) N12 0.033(3) 0.032(3) 0.021(2) 0.001(2) 0.005(2) 0.014(2) N13 0.020(3) 0.020(3) 0.019(2) -0.001(2) 0.004(2) 0.0049(19) N14 0.025(3) 0.022(3) 0.025(3) -0.004(2) 0.006(2) -0.003(2) N15 0.025(2) 0.024(2) 0.017(2) -0.0030(17) 0.0049(18) -0.0028(19) C44 0.022(3) 0.018(3) 0.019(3) -0.002(2) 0.003(2) 0.004(2) C45 0.011(3) 0.028(3) 0.021(3) -0.003(3) 0.000(3) -0.002(2) C46 0.053(5) 0.039(4) 0.020(3) -0.010(3) 0.007(3) -0.010(4) C47 0.029(3) 0.025(3) 0.029(3) 0.002(2) 0.008(3) -0.002(2) O33 0.039(3) 0.036(3) 0.044(3) 0.000(2) 0.024(3) -0.003(2) _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 O7' 1.342(4) . ? S1 O8 1.398(3) . ? S1 O8' 1.438(3) . ? S1 O6 1.479(3) . ? S1 O6' 1.535(3) . ? S1 O7 1.563(3) . ? S1 C4 1.768(3) . ? S2 O10 1.442(2) . ? S2 O11 1.448(2) . ? S2 O9 1.458(2) . ? S2 C11 1.760(3) . ? S3 O14 1.451(2) . ? S3 O13 1.457(2) . ? S3 O12 1.465(2) . ? S3 C18 1.769(3) . ? S4 O15 1.453(2) . ? S4 O16 1.458(2) . ? S4 O17 1.4591(19) . ? S4 C25 1.763(3) . ? S5 O20 1.450(2) . ? S5 O19 1.452(2) . ? S5 O18 1.457(2) . ? S5 C32 1.763(3) . ? O1 C1 1.369(3) . ? O1 H1 0.86(4) . ? O2 C8 1.369(3) . ? O2 H2 0.99(4) . ? O3 C15 1.364(3) . ? O3 H3 0.82(4) . ? O4 C22 1.366(3) . ? O4 H4 0.85(4) . ? O5 C29 1.369(3) . ? O5 H5 0.91(4) . ? O21 H21A 0.81(4) . ? O21 H21B 0.74(4) . ? O22 H22A 0.83(4) . ? O22 H22B 0.81(4) . ? O23 H23A 0.82(4) . ? O23 H23B 0.80(4) . ? O24 H24A 0.77(4) . ? O24 H24B 0.91(4) . ? O25 H25A 0.81(5) . ? O25 H25B 0.86(5) . ? O26 H26A 0.77(4) . ? O26 H26B 0.81(5) . ? O27 H27A 0.59(5) . ? O27 H27B 1.00(4) . ? O28 H28A 0.84(5) . ? O28 H28B 0.72(5) . ? O29 H29A 0.92(5) . ? O29 H29B 0.86(5) . ? O30 H30A 0.8525 . ? O30 H30B 0.8521 . ? O31 H31B 0.8554 . ? O31 H31A 0.8449 . ? N1 C36 1.303(4) . ? N1 H1A 0.88(4) . ? N1 H1B 0.84(4) . ? N2 C36 1.315(4) . ? N2 H2A 0.92(4) . ? N2 H2B 0.90(4) . ? N3 C37 1.373(4) . ? N3 C36 1.376(4) . ? N3 H3A 0.87(4) . ? N4 C37 1.320(4) . ? N4 H4A 0.94(4) . ? N4 H4B 0.82(4) . ? N5 C37 1.318(4) . ? N5 C38 1.468(4) . ? N5 C39 1.472(4) . ? N6 C40 1.307(4) . ? N6 H6A 0.92(4) . ? N6 H6B 0.90(4) . ? N7 C40 1.310(4) . ? N7 H7A 0.83(4) . ? N7 H7B 0.90(4) . ? N8 C40 1.374(3) . ? N8 C41 1.378(3) . ? N8 H8A 0.87(4) . ? N9 C41 1.311(4) . ? N9 H9A 0.86(4) . ? N9 H9B 0.89(4) . ? N10 C41 1.324(3) . ? N10 C43 1.461(4) . ? N10 C42 1.464(4) . ? C1 C6 1.398(4) . ? C1 C2 1.400(3) . ? C2 C3 1.388(4) . ? C2 C35 1.514(3) . ? C3 C4 1.390(4) . ? C3 H3C 0.9500 . ? C4 C5 1.386(4) . ? C5 C6 1.386(4) . ? C5 H5C 0.9500 . ? C6 C7 1.519(4) . ? C7 C9 1.519(4) . ? C7 H7C 0.9900 . ? C7 H7D 0.9900 . ? C8 C9 1.400(4) . ? C8 C13 1.402(4) . ? C9 C10 1.392(4) . ? C10 C11 1.380(4) . ? C10 H10 0.9500 . ? C11 C12 1.389(4) . ? C12 C13 1.390(4) . ? C12 H12 0.9500 . ? C13 C14 1.514(4) . ? C14 C16 1.520(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C20 1.400(4) . ? C15 C16 1.409(4) . ? C16 C17 1.383(4) . ? C17 C18 1.389(4) . ? C17 H17 0.9500 . ? C18 C19 1.383(4) . ? C19 C20 1.391(4) . ? C19 H19 0.9500 . ? C20 C21 1.520(4) . ? C21 C23 1.515(3) . ? C21 H21C 0.9900 . ? C21 H21D 0.9900 . ? C22 C27 1.398(3) . ? C22 C23 1.402(4) . ? C23 C24 1.393(4) . ? C24 C25 1.393(3) . ? C24 H24 0.9500 . ? C25 C26 1.389(4) . ? C26 C27 1.397(3) . ? C26 H26 0.9500 . ? C27 C28 1.514(3) . ? C28 C30 1.515(3) . ? C28 H28C 0.9900 . ? C28 H28D 0.9900 . ? C29 C30 1.398(3) . ? C29 C34 1.410(3) . ? C30 C31 1.399(4) . ? C31 C32 1.390(4) . ? C31 H31 0.9500 . ? C32 C33 1.397(4) . ? C33 C34 1.388(4) . ? C33 H33 0.9500 . ? C34 C35 1.523(3) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? N11 C44 1.317(7) . ? N11 H11A 0.8800 . ? N11 H11B 0.8800 . ? N12 C44 1.294(8) . ? N12 H12A 0.8800 . ? N12 H12B 0.8800 . ? N13 C44 1.365(7) . ? N13 C45 1.382(8) . ? N13 H13A 0.8800 . ? N14 C45 1.310(9) . ? N14 H14C 0.8800 . ? N14 H14D 0.8800 . ? N15 C45 1.316(7) . ? N15 C46 1.455(8) . ? N15 C47 1.471(8) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? 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 O7' S1 O8 147.8(3) . . ? O7' S1 O8' 121.7(2) . . ? O8 S1 O8' 47.3(2) . . ? O7' S1 O6 52.8(2) . . ? O8 S1 O6 114.5(2) . . ? O8' S1 O6 143.4(2) . . ? O7' S1 O6' 114.8(2) . . ? O8 S1 O6' 61.0(2) . . ? O8' S1 O6' 108.0(2) . . ? O6 S1 O6' 62.1(2) . . ? O7' S1 O7 57.2(2) . . ? O8 S1 O7 108.7(2) . . ? O8' S1 O7 65.7(2) . . ? O6 S1 O7 104.2(2) . . ? O6' S1 O7 149.8(2) . . ? O7' S1 C4 102.4(2) . . ? O8 S1 C4 109.7(2) . . ? O8' S1 C4 105.66(19) . . ? O6 S1 C4 110.82(17) . . ? O6' S1 C4 101.66(19) . . ? O7 S1 C4 108.48(17) . . ? O10 S2 O11 114.21(16) . . ? O10 S2 O9 111.13(15) . . ? O11 S2 O9 111.63(14) . . ? O10 S2 C11 107.24(13) . . ? O11 S2 C11 105.74(13) . . ? O9 S2 C11 106.33(14) . . ? O14 S3 O13 112.68(13) . . ? O14 S3 O12 112.87(13) . . ? O13 S3 O12 111.41(13) . . ? O14 S3 C18 106.82(13) . . ? O13 S3 C18 106.02(13) . . ? O12 S3 C18 106.48(13) . . ? O15 S4 O16 111.87(12) . . ? O15 S4 O17 111.11(12) . . ? O16 S4 O17 112.79(12) . . ? O15 S4 C25 107.17(12) . . ? O16 S4 C25 106.05(12) . . ? O17 S4 C25 107.45(12) . . ? O20 S5 O19 113.29(13) . . ? O20 S5 O18 111.90(13) . . ? O19 S5 O18 111.99(15) . . ? O20 S5 C32 107.11(12) . . ? O19 S5 C32 107.10(13) . . ? O18 S5 C32 104.85(12) . . ? C1 O1 H1 110(2) . . ? C8 O2 H2 112(2) . . ? C15 O3 H3 112(3) . . ? C22 O4 H4 113(2) . . ? C29 O5 H5 112(2) . . ? H21A O21 H21B 115(4) . . ? H22A O22 H22B 108(4) . . ? H23A O23 H23B 105(4) . . ? H24A O24 H24B 118(4) . . ? H25A O25 H25B 110(4) . . ? H26A O26 H26B 111(4) . . ? H27A O27 H27B 112(6) . . ? H28A O28 H28B 104(5) . . ? H29A O29 H29B 113(4) . . ? H30A O30 H30B 107.3 . . ? H31B O31 H31A 111.5 . . ? C36 N1 H1A 123(2) . . ? C36 N1 H1B 120(3) . . ? H1A N1 H1B 117(4) . . ? C36 N2 H2A 117(2) . . ? C36 N2 H2B 117(3) . . ? H2A N2 H2B 124(3) . . ? C37 N3 C36 125.5(2) . . ? C37 N3 H3A 119(2) . . ? C36 N3 H3A 115(2) . . ? C37 N4 H4A 122(2) . . ? C37 N4 H4B 121(3) . . ? H4A N4 H4B 117(3) . . ? C37 N5 C38 120.8(2) . . ? C37 N5 C39 122.8(2) . . ? C38 N5 C39 115.9(2) . . ? C40 N6 H6A 120(2) . . ? C40 N6 H6B 119(2) . . ? H6A N6 H6B 121(3) . . ? C40 N7 H7A 125(3) . . ? C40 N7 H7B 120(3) . . ? H7A N7 H7B 114(4) . . ? C40 N8 C41 126.5(2) . . ? C40 N8 H8A 116(2) . . ? C41 N8 H8A 117(2) . . ? C41 N9 H9A 123(2) . . ? C41 N9 H9B 118(2) . . ? H9A N9 H9B 119(3) . . ? C41 N10 C43 121.1(2) . . ? C41 N10 C42 124.1(2) . . ? C43 N10 C42 114.2(2) . . ? O1 C1 C6 117.1(2) . . ? O1 C1 C2 121.3(2) . . ? C6 C1 C2 121.7(2) . . ? C3 C2 C1 118.5(2) . . ? C3 C2 C35 120.8(2) . . ? C1 C2 C35 120.7(2) . . ? C2 C3 C4 120.6(2) . . ? C2 C3 H3C 119.7 . . ? C4 C3 H3C 119.7 . . ? C5 C4 C3 119.9(3) . . ? C5 C4 S1 119.8(2) . . ? C3 C4 S1 120.3(2) . . ? C6 C5 C4 121.1(3) . . ? C6 C5 H5C 119.4 . . ? C4 C5 H5C 119.4 . . ? C5 C6 C1 118.1(2) . . ? C5 C6 C7 121.8(3) . . ? C1 C6 C7 120.1(3) . . ? C9 C7 C6 114.2(2) . . ? C9 C7 H7C 108.7 . . ? C6 C7 H7C 108.7 . . ? C9 C7 H7D 108.7 . . ? C6 C7 H7D 108.7 . . ? H7C C7 H7D 107.6 . . ? O2 C8 C9 122.0(2) . . ? O2 C8 C13 116.3(2) . . ? C9 C8 C13 121.6(3) . . ? C10 C9 C8 117.7(3) . . ? C10 C9 C7 119.7(3) . . ? C8 C9 C7 122.5(3) . . ? C11 C10 C9 121.4(3) . . ? C11 C10 H10 119.3 . . ? C9 C10 H10 119.3 . . ? C10 C11 C12 120.3(3) . . ? C10 C11 S2 120.1(2) . . ? C12 C11 S2 119.5(2) . . ? C11 C12 C13 120.1(3) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C12 C13 C8 118.8(2) . . ? C12 C13 C14 120.2(2) . . ? C8 C13 C14 121.0(2) . . ? C13 C14 C16 113.8(2) . . ? C13 C14 H14A 108.8 . . ? C16 C14 H14A 108.8 . . ? C13 C14 H14B 108.8 . . ? C16 C14 H14B 108.8 . . ? H14A C14 H14B 107.7 . . ? O3 C15 C20 117.4(2) . . ? O3 C15 C16 121.5(2) . . ? C20 C15 C16 121.1(2) . . ? C17 C16 C15 118.2(2) . . ? C17 C16 C14 119.8(2) . . ? C15 C16 C14 121.9(2) . . ? C16 C17 C18 121.1(2) . . ? C16 C17 H17 119.4 . . ? C18 C17 H17 119.4 . . ? C19 C18 C17 120.0(3) . . ? C19 C18 S3 120.8(2) . . ? C17 C18 S3 119.0(2) . . ? C18 C19 C20 120.7(2) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? C19 C20 C15 118.7(2) . . ? C19 C20 C21 119.9(2) . . ? C15 C20 C21 121.3(2) . . ? C23 C21 C20 115.5(2) . . ? C23 C21 H21C 108.4 . . ? C20 C21 H21C 108.4 . . ? C23 C21 H21D 108.4 . . ? C20 C21 H21D 108.4 . . ? H21C C21 H21D 107.5 . . ? O4 C22 C27 116.4(2) . . ? O4 C22 C23 122.2(2) . . ? C27 C22 C23 121.4(2) . . ? C24 C23 C22 118.3(2) . . ? C24 C23 C21 119.2(2) . . ? C22 C23 C21 122.5(2) . . ? C23 C24 C25 121.0(2) . . ? C23 C24 H24 119.5 . . ? C25 C24 H24 119.5 . . ? C26 C25 C24 120.0(2) . . ? C26 C25 S4 121.65(19) . . ? C24 C25 S4 118.27(19) . . ? C25 C26 C27 120.3(2) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C26 C27 C22 119.0(2) . . ? C26 C27 C28 121.0(2) . . ? C22 C27 C28 120.0(2) . . ? C27 C28 C30 113.7(2) . . ? C27 C28 H28C 108.8 . . ? C30 C28 H28C 108.8 . . ? C27 C28 H28D 108.8 . . ? C30 C28 H28D 108.8 . . ? H28C C28 H28D 107.7 . . ? O5 C29 C30 122.7(2) . . ? O5 C29 C34 115.7(2) . . ? C30 C29 C34 121.6(2) . . ? C29 C30 C31 118.0(2) . . ? C29 C30 C28 123.5(2) . . ? C31 C30 C28 118.5(2) . . ? C32 C31 C30 121.2(2) . . ? C32 C31 H31 119.4 . . ? C30 C31 H31 119.4 . . ? C31 C32 C33 120.0(2) . . ? C31 C32 S5 120.0(2) . . ? C33 C32 S5 119.9(2) . . ? C34 C33 C32 120.4(2) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C33 C34 C29 118.8(2) . . ? C33 C34 C35 119.0(2) . . ? C29 C34 C35 122.2(2) . . ? C2 C35 C34 114.0(2) . . ? C2 C35 H35A 108.7 . . ? C34 C35 H35A 108.7 . . ? C2 C35 H35B 108.7 . . ? C34 C35 H35B 108.7 . . ? H35A C35 H35B 107.6 . . ? N1 C36 N2 122.9(3) . . ? N1 C36 N3 119.8(3) . . ? N2 C36 N3 117.2(2) . . ? N5 C37 N4 123.4(3) . . ? N5 C37 N3 118.0(2) . . ? N4 C37 N3 118.5(3) . . ? N5 C38 H38A 109.5 . . ? N5 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N5 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N5 C39 H39A 109.5 . . ? N5 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? N5 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N6 C40 N7 122.0(3) . . ? N6 C40 N8 121.7(3) . . ? N7 C40 N8 116.3(3) . . ? N9 C41 N10 122.5(3) . . ? N9 C41 N8 120.4(2) . . ? N10 C41 N8 117.0(2) . . ? N10 C42 H42A 109.5 . . ? N10 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N10 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N10 C43 H43A 109.5 . . ? N10 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? N10 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C44 N11 H11A 120.0 . . ? C44 N11 H11B 120.0 . . ? H11A N11 H11B 120.0 . . ? C44 N12 H12A 120.0 . . ? C44 N12 H12B 120.0 . . ? H12A N12 H12B 120.0 . . ? C44 N13 C45 122.7(5) . . ? C44 N13 H13A 118.6 . . ? C45 N13 H13A 118.6 . . ? C45 N14 H14C 120.0 . . ? C45 N14 H14D 120.0 . . ? H14C N14 H14D 120.0 . . ? C45 N15 C46 119.7(5) . . ? C45 N15 C47 123.9(5) . . ? C46 N15 C47 116.1(5) . . ? N12 C44 N11 122.8(5) . . ? N12 C44 N13 117.3(5) . . ? N11 C44 N13 119.8(5) . . ? N14 C45 N15 123.5(6) . . ? N14 C45 N13 118.6(5) . . ? N15 C45 N13 117.9(6) . . ? 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 177.1(2) . . . . ? C6 C1 C2 C3 -2.5(4) . . . . ? O1 C1 C2 C35 -2.7(4) . . . . ? C6 C1 C2 C35 177.8(3) . . . . ? C1 C2 C3 C4 1.5(4) . . . . ? C35 C2 C3 C4 -178.8(3) . . . . ? C2 C3 C4 C5 1.4(4) . . . . ? C2 C3 C4 S1 -177.4(2) . . . . ? O7' S1 C4 C5 -103.8(3) . . . . ? O8 S1 C4 C5 78.3(3) . . . . ? O8' S1 C4 C5 127.9(3) . . . . ? O6 S1 C4 C5 -49.1(3) . . . . ? O6' S1 C4 C5 15.2(3) . . . . ? O7 S1 C4 C5 -163.0(3) . . . . ? O7' S1 C4 C3 75.0(3) . . . . ? O8 S1 C4 C3 -102.9(3) . . . . ? O8' S1 C4 C3 -53.3(3) . . . . ? O6 S1 C4 C3 129.6(3) . . . . ? O6' S1 C4 C3 -166.1(3) . . . . ? O7 S1 C4 C3 15.7(3) . . . . ? C3 C4 C5 C6 -3.3(5) . . . . ? S1 C4 C5 C6 175.4(2) . . . . ? C4 C5 C6 C1 2.3(5) . . . . ? C4 C5 C6 C7 -179.3(3) . . . . ? O1 C1 C6 C5 -179.0(3) . . . . ? C2 C1 C6 C5 0.6(4) . . . . ? O1 C1 C6 C7 2.7(4) . . . . ? C2 C1 C6 C7 -177.8(3) . . . . ? C5 C6 C7 C9 80.7(3) . . . . ? C1 C6 C7 C9 -100.9(3) . . . . ? O2 C8 C9 C10 178.0(2) . . . . ? C13 C8 C9 C10 0.1(4) . . . . ? O2 C8 C9 C7 -3.8(4) . . . . ? C13 C8 C9 C7 178.3(2) . . . . ? C6 C7 C9 C10 -56.4(3) . . . . ? C6 C7 C9 C8 125.4(3) . . . . ? C8 C9 C10 C11 0.4(4) . . . . ? C7 C9 C10 C11 -177.9(2) . . . . ? C9 C10 C11 C12 -0.2(4) . . . . ? C9 C10 C11 S2 -179.0(2) . . . . ? O10 S2 C11 C10 -124.0(2) . . . . ? O11 S2 C11 C10 113.7(2) . . . . ? O9 S2 C11 C10 -5.1(3) . . . . ? O10 S2 C11 C12 57.1(3) . . . . ? O11 S2 C11 C12 -65.1(2) . . . . ? O9 S2 C11 C12 176.1(2) . . . . ? C10 C11 C12 C13 -0.4(4) . . . . ? S2 C11 C12 C13 178.40(19) . . . . ? C11 C12 C13 C8 0.9(4) . . . . ? C11 C12 C13 C14 -179.1(2) . . . . ? O2 C8 C13 C12 -178.7(2) . . . . ? C9 C8 C13 C12 -0.7(4) . . . . ? O2 C8 C13 C14 1.3(4) . . . . ? C9 C8 C13 C14 179.3(2) . . . . ? C12 C13 C14 C16 86.8(3) . . . . ? C8 C13 C14 C16 -93.2(3) . . . . ? O3 C15 C16 C17 175.5(2) . . . . ? C20 C15 C16 C17 -6.4(4) . . . . ? O3 C15 C16 C14 -7.6(4) . . . . ? C20 C15 C16 C14 170.5(2) . . . . ? C13 C14 C16 C17 -88.4(3) . . . . ? C13 C14 C16 C15 94.8(3) . . . . ? C15 C16 C17 C18 2.7(4) . . . . ? C14 C16 C17 C18 -174.3(2) . . . . ? C16 C17 C18 C19 2.0(4) . . . . ? C16 C17 C18 S3 177.9(2) . . . . ? O14 S3 C18 C19 -8.3(3) . . . . ? O13 S3 C18 C19 112.1(2) . . . . ? O12 S3 C18 C19 -129.1(2) . . . . ? O14 S3 C18 C17 175.9(2) . . . . ? O13 S3 C18 C17 -63.7(2) . . . . ? O12 S3 C18 C17 55.0(2) . . . . ? C17 C18 C19 C20 -3.1(4) . . . . ? S3 C18 C19 C20 -178.89(19) . . . . ? C18 C19 C20 C15 -0.6(4) . . . . ? C18 C19 C20 C21 176.1(2) . . . . ? O3 C15 C20 C19 -176.4(2) . . . . ? C16 C15 C20 C19 5.4(4) . . . . ? O3 C15 C20 C21 7.0(3) . . . . ? C16 C15 C20 C21 -171.2(2) . . . . ? C19 C20 C21 C23 71.9(3) . . . . ? C15 C20 C21 C23 -111.5(3) . . . . ? O4 C22 C23 C24 -179.5(2) . . . . ? C27 C22 C23 C24 1.0(4) . . . . ? O4 C22 C23 C21 -1.3(4) . . . . ? C27 C22 C23 C21 179.2(2) . . . . ? C20 C21 C23 C24 -93.0(3) . . . . ? C20 C21 C23 C22 88.8(3) . . . . ? C22 C23 C24 C25 -0.9(4) . . . . ? C21 C23 C24 C25 -179.2(2) . . . . ? C23 C24 C25 C26 -0.1(4) . . . . ? C23 C24 C25 S4 177.0(2) . . . . ? O15 S4 C25 C26 -126.8(2) . . . . ? O16 S4 C25 C26 113.5(2) . . . . ? O17 S4 C25 C26 -7.3(3) . . . . ? O15 S4 C25 C24 56.2(2) . . . . ? O16 S4 C25 C24 -63.5(2) . . . . ? O17 S4 C25 C24 175.7(2) . . . . ? C24 C25 C26 C27 1.0(4) . . . . ? S4 C25 C26 C27 -175.98(19) . . . . ? C25 C26 C27 C22 -0.9(4) . . . . ? C25 C26 C27 C28 177.2(2) . . . . ? O4 C22 C27 C26 -179.7(2) . . . . ? C23 C22 C27 C26 -0.1(4) . . . . ? O4 C22 C27 C28 2.2(3) . . . . ? C23 C22 C27 C28 -178.2(2) . . . . ? C26 C27 C28 C30 100.0(3) . . . . ? C22 C27 C28 C30 -81.9(3) . . . . ? O5 C29 C30 C31 177.7(2) . . . . ? C34 C29 C30 C31 -3.4(3) . . . . ? O5 C29 C30 C28 -4.7(4) . . . . ? C34 C29 C30 C28 174.2(2) . . . . ? C27 C28 C30 C29 128.6(2) . . . . ? C27 C28 C30 C31 -53.9(3) . . . . ? C29 C30 C31 C32 0.7(4) . . . . ? C28 C30 C31 C32 -177.0(2) . . . . ? C30 C31 C32 C33 1.8(4) . . . . ? C30 C31 C32 S5 -173.90(19) . . . . ? O20 S5 C32 C31 -146.5(2) . . . . ? O19 S5 C32 C31 -24.7(3) . . . . ? O18 S5 C32 C31 94.4(2) . . . . ? O20 S5 C32 C33 37.8(2) . . . . ? O19 S5 C32 C33 159.6(2) . . . . ? O18 S5 C32 C33 -81.2(2) . . . . ? C31 C32 C33 C34 -1.6(4) . . . . ? S5 C32 C33 C34 174.10(19) . . . . ? C32 C33 C34 C29 -1.1(4) . . . . ? C32 C33 C34 C35 178.4(2) . . . . ? O5 C29 C34 C33 -177.4(2) . . . . ? C30 C29 C34 C33 3.6(4) . . . . ? O5 C29 C34 C35 3.1(3) . . . . ? C30 C29 C34 C35 -175.9(2) . . . . ? C3 C2 C35 C34 -108.0(3) . . . . ? C1 C2 C35 C34 71.8(3) . . . . ? C33 C34 C35 C2 68.6(3) . . . . ? C29 C34 C35 C2 -111.9(3) . . . . ? C37 N3 C36 N1 35.3(4) . . . . ? C37 N3 C36 N2 -148.1(3) . . . . ? C38 N5 C37 N4 11.0(4) . . . . ? C39 N5 C37 N4 -160.3(3) . . . . ? C38 N5 C37 N3 -165.1(2) . . . . ? C39 N5 C37 N3 23.6(4) . . . . ? C36 N3 C37 N5 -149.0(3) . . . . ? C36 N3 C37 N4 34.8(4) . . . . ? C41 N8 C40 N6 -22.6(4) . . . . ? C41 N8 C40 N7 159.8(3) . . . . ? C43 N10 C41 N9 -14.8(4) . . . . ? C42 N10 C41 N9 155.2(3) . . . . ? C43 N10 C41 N8 162.1(3) . . . . ? C42 N10 C41 N8 -27.9(4) . . . . ? C40 N8 C41 N9 -31.1(4) . . . . ? C40 N8 C41 N10 151.9(3) . . . . ? C45 N13 C44 N12 146.5(6) . . . . ? C45 N13 C44 N11 -37.7(9) . . . . ? C46 N15 C45 N14 -7.3(10) . . . . ? C47 N15 C45 N14 166.0(6) . . . . ? C46 N15 C45 N13 169.8(6) . . . . ? C47 N15 C45 N13 -16.9(9) . . . . ? C44 N13 C45 N14 -40.5(9) . . . . ? C44 N13 C45 N15 142.2(6) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.91 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.490 _refine_diff_density_min -0.763 _refine_diff_density_rms 0.075